Regulation of the mTORC1 growth pathway by amino aci ds by MASSACHUSETTS INSTITUTE OF rECHNOLOLGY Zhi-Yang Tsun B.S. Bioengineering, Molecular Biology University of California, San Diego (2004) MAY 2 7 2015 LIBRARIES Submitted to the Department of Biology in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy at the Massachusetts Institute of Technology June 2015 @2015 Zhi-Yang Tsun. All rights reserved. The author hereby grants to MIT permission to reproduce and to distribute publicly paper and electronic copies of this thesis document in whole or in part in any medium now known or hereafter created. Signature of Author..................................... Signature redacted Departmqntof Biology Marob 14, 2015 C e rtifie d b y ................................................ Signature redacted David M. Sabatini Professor of Biology JI]hesis Supervisor A cce pted by ............................................ Signature redacted Midhael T. Hemann Professor of Biology Chairman, Committee for Graduate Students 1 2 Regulation of the mTORC1 growth pathway by amino acids by Zhi-Yang Tsun Submitted to the Department of Biology on May 22, 2015 in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy at the Massachusetts Institute of Technology Abstract: The mTORC1 kinase is a master growth regulator that responds to numerous environmental cues, including amino acids, to regulate many processes, such as protein, lipid, and nucleotide synthesis, as well as autophagy. Given that mTORC1 regulates a multitude of processes, it is not surprising that the pathway it anchors is deregulated in various common diseases, including cancer. The Rag GTPases interact with mTORC1 and signal amino acid sufficiency by promoting the translocation of mTORC1 to the lysosomal surface, its site of activation. The Rags are unusual GTPases in that they function as obligate heterodimers, which consist of RagA or B bound to RagC or D. We show that RagC/D is a key regulator of the interaction of mTORC1 with the Rag heterodimer and that, unexpectedly, RagC/D must be GDP-bound for the interaction to occur. We identify FLCN and its binding partners, FNIP1/2, as Rag-interacting proteins with GTPase activating activity for RagC/D, but not RagA/B. Given that many proteins known to signal amino acid sufficiency to mTORC1, including the Rag GTPases, localize to the lysosome and that intralysosomal amino acid accumulation is necessary for mTORC1 activation, we began our search for potential direct amino acid sensors at the lysosomal membrane. We identify SLC38A9, an uncharacterized protein with homology to amino acid transporters, as a lysosomal transmembrane protein. SLC38A9 forms a supercomplex with Ragulator, the Rag GTPases and the v-ATPase and is necessary for mTORC1 activation by amino acids, particularly arginine. Overexpression of the full-length protein or just its Ragulatorbinding domain makes mTORC1 signaling insensitive to amino acid starvation but does not affect its dependence on Rag activity. SLC38A9 reconstituted in proteoliposomes transports arginine, an abundant amino acid in the lysosome and necessary for mTORC1 pathway activity. These results place SLC38A9 between amino acids and the Rag GTPases and are consistent with the notion that amino acids are sensed at the lysosome. Thus, SLC38A9 is an excellent candidate for being an amino acid sensor upstream of mTORC1. Thesis supervisor: David M. Sabatini Title: Member, Whitehead Institute; Professor of Biology, MIT 3 Acknowledgements: Undertaking PhD training in David Sabatini's lab has been the most transformative years of my life. What inspires me most about David is that he leads by example. He engenders incredible work ethic in his trainees because he works harder than anyone in the lab. David has a piercing clarity of thought that instantly scrutinizes new data and develops consistent models, that is matched by his scientific rigor and fearlessness. David pursues the highest caliber of quality not just in experiments but also in data figures, writing, and in giving seminars. Attempting to emulate these qualities has pushed me to grow in ways I never expected. Perhaps the most valuable lesson that I've learned working with David is to pursue important problems, and thanks to my time in his lab, I finally have the confidence to tackle important but difficult problems. I would like to thank the members of my thesis committee, Steve Bell, and Bob Sauer, for the continued guidance and support throughout my journey. I am also grateful to Brendan Manning and Hidde Ploegh who are also part of my thesis evaluation committee. It is rare to find a lab with such talented and motivated people and yet have an environment that is equally exceptional in collegiality. Many thanks to Rich Possemato who mentored me during my rotation with inexhaustible patience, and Kris Wood, Yoav Shaul, Shomit Sengupta, Peggy Hsu, Doug Wheeler, Yasemin Sancak, Maki Saitoh for making the transition from undergraduate to graduate lab such a welcoming one. I also appreciate the incisive conversations with Tim Peterson, who started the work on BirtHogg-Dube syndrome, and whose DEPTOR paper helped convinced me to pursue my rotation here. Liron Bar-Peled and Lynne Chantranupong were wonderful bay-mates and tolerated my relentless questions when I first joined the lab. Lynne-mama, as we affectionately call her, has been an amazing bench-mate throughout my time here-so thoughtful and showed me what 'being industrious' means. Although Rachel Wolfson recently joined the bay, I have really appreciated her incisive feedback, vigorous discussions, and unconditional eagerness to help. I am grateful to Shuyu Wang, with whom I had the pleasure of sitting next to and work closely with, and who pushed me to think deeper about science and life. And many thanks to Kuang Shen who has taught me everything I know about experimental biochemistry. It has been a pleasure to work with everyone who has spent time in our bay, Tony Kang, Naama Kanarek, Bobby Saxton, and Jose Orozco. The way everyone so generously came to help during the two instances when we had to race to submit our manuscripts is a testament to how the lab really has become a family. Many people in the lab have made this an inspiring and rigorous place to train: Walter Chen for his constant encouragement and companionship as we joined the lab together; Larry Schweitzer for incisive feedback and help with my NRSA fellowship application; Carson Thoreen, Omer Yilmaz, Pekka Katajisto and Kris Wood for giving inspiring advice; Roberto Zoncu, who taught me how to work with microscopes and isolate lysosomes, and whose exemplar seminars have been inspirational; Mike Pacold, who has been a wonderful source of necessary and unnecessary information, as well as medical advice; Kivanc Birsoy, Bill Comb, and Do Kim for thoughtful discussions and advice; Kathleen Ottina, who makes it so effortless to do our best science in lab, and for sharing life advice; Amanda Hutchins, Sam Murphy, and Kevin Krupczak who ensure the lab runs smoothly; Edie Valeri, who always brightens the day and has been so reliable and responsive for everything non-science in the lab; Greg Wyant and Monther Remaileh for a seamless transition as I wrapped up in lab. I have been most fortunate to 4 have the opportunity to work with very talented students, Choah Kim, Tony Jones, Elizabeth Yuan, and Alice Chen, who have certainly taught me more than I could teach them. I especially want to thank Tim Wang who has become a dear friend and scientific colleague. I am grateful that we went through scientific races together, and what can only be described as a scientific coming-of-age, together. His intellectual and scientific prowess inspires me and his incisive feedback pushes me to grow. I would also like to thank Mounir Koussa, who has been my partner in crime as we embarked on this science and life journey 3 years ago. His companionship has kept me sane while also in many ways encouraged madness. He has been unnecessarily generous with his time in reviewing all my practice talks, grant applications, and manuscript drafts, and I am grateful for how he has shaped my personal and scientific development. I am very fortunate to have friends who have not only supported me but continue to inspire me: Nikhil Bhatla, Allen Cheng, Sasha and Masha Rayshubskiy Anna Chambers, Jason Yamada-Hanff, Pallav Kosuri, and Dr. Sheila Nutt. I would like to thank my parents, Maung-win Maung and Sau-Man Yang, and sister Zhi-Fang Tsun, who continue to support me unconditionally and made possible all the opportunities I am fortunate to have. And Charlie and Veronica Plovanich who have been my family here on the east coast. And of course my wife, Molly Plovanich, who not only supports and inspires me through every step of our journey, but also provided key scientific guidance during the most critical time. She is my better half who grounds me in life. 5 Table of Contents A b stra ct .................................................................................................... A cknow ledgem ents ..................................................................................... . .3 4 Chapter 1: Introduction I. Intro d u ctio n .............................................................................................. . .8 II. T he m T O R P athw ay................................................................................... 8 A. Rapamycin: a discovery tool and therapeutic........................................ 8 B. mTORC1 and mTORC2.................................................................... 9 C. Amino acid signaling machinery....................................................... 11 D. Downstream effectors of mTORC1.....................................................12 Ill. mTOR signaling in cancer..........................................................................13 A . U pstream of m T O R C 1........................................................................13 B. Birt-Hogg-Dub6 Syndrome...................................................................15 C. Outputs of mTORC1 Altered in Cancer.............................................. 16 D. Rapalogues in cancer therapy...........................................................17 IV . A m ino acid transport............................................................................... 19 A. History: digestion, protein absorption, and AA uptake in tissues.........19 B. SLC38 AA transporter family.............................................................21 C. Arginine transport at the plasma and lysosomal membranes.................. 23 V. Preface for work presented in this thesis.......................................................25 Re fe re n ce s ............................................................................................... . ..2 8 Chapter 2: The Folliculin tumor suppressor is a GAP for RagC/D GTPases that signal amino acid levels to mTORC1 S u m m a ry ...................................................................................................... 39 Introd u ction ................................................................................................... 40 R e sults ..................................................................... ................ . . 41 The RagC Nucleotide State Determines mTORC1 Binding to the Rag H e tero d im e r...................................................................................... . 4 1 FLCN Interacts with the Rags in an Amino Acid-Sensitive Fashion................43 FLCN is Necessary for mTORC1 Activation and Localization to the Lysosomal M e m b ra ne s ....................................................... . . ...................... . . 45 FLCN Co-Localizes with the Rag GTPases on the Lysosomal Surface in an Amino Acid-Sensitive Fashion....................................................................46 FLCN-FNIP2 is a GAP for RagC and RagD............................................ 47 D is c u s sio n ..................................................................................................... 50 F ig u re s ..................................................................................................... . . 52 F ig u re Leg e nd s ........................................................................................ . . 56 Experimental Procedures............................................................................. 60 R e fe re n ce s ............................................................................................... . ..6 6 S up ple m e nta l Info ........................................................................................ . 72 6 Chapter 3: Lysosomal amino acid transporter SLC38A9 signals arginine sufficiency to mTORC1 S u m m a ry ...................................................................................................... 79 Intro d u ctio n ............................................................................................... . 80 Re s u lts ..................................................................................................... . .81 SLC38A9 Interacts with Ragulator and the Rag GTPases......................... 81 SLC38A9, a Lysosomal Membrane Protein Required for mTORC1 Activation... 82 SLC38A9.1 Overexpression Makes mTORC1 Signaling Insensitive to Amino Acids..................... ................................. 83 Modulation of the SLC38A9-Rag-Ragulator Interactions by Amino Acids..........84 SLC38A9.1 is an Amino Acid Transporter...................................................85 D isc u s s io n ............................................................................................... . .. 8 6 F ig u re s ..................................................................................................... . . 88 F ig u re Le g e nd s ........................................................................................ . . 93 R e fe re n ce s ............ ................................................................................... . . 96 Experimental Procedures............................................................................. 99 S u p p le m e nta l Info .......................................................................................... 10 7 Chapter 4: Future directions and discussions I. T he R ag H ete ro d im e r..................................................................................119 11. Lysosomal amino acid concentrations in human cells........................................120 111. Nutrient sensing in the compartmentalized cell...............................................121 R e fe re n ce s .................................................................................................. 1 23 7 CHAPTER 1 I. INTRODUCTION Cell growth, or the accumulation of mass, is a resource-intensive process. As such, cells have evolved sophisticated systems to ensure that the rate of growth is controlled not only by the availability of nutrients, but also by signaling pathways that report growth factors and cellular stresses. One such system is the mechanistic target of rapamycin complex 1 (mTORC1) pathway. mTORC1 integrates a diverse set of signals, such as growth factors, nutrient and energy levels, to regulate many anabolic and catabolic processes, including protein, lipid, and nucleotide synthesis, as well as autophagy. Given that mTORC1 regulates a multitude of processes, it is not surprising that the pathway it anchors is deregulated in various common diseases, including cancer, diabetes, and aging. Therefore, understanding the molecular underpinnings of this pathway will be essential for therapeutic intervention. II. THE MTOR PATHWAY A. Rapamycin: a discovery tool and therapeutic In the 1970s, Rapamycin was isolated from Streptomyces hygroscopicus in a soil sample from Easter Island, also called Rapa Nui. Identified from an antibiotic screen performed in Ayerst Research Labs, rapamycin lacked antibacterial activity but had potent growth-inhibitory effects on yeast, causing G1 arrest (Robert and Gregory, 1996). These anti-proliferative effects also applied to human cancer cells, extending these effects from yeast to human (Eng et al., 1984). Rapamycin was also shown to have immunosuppressive effects in two mouse models of auto-immune disease. Once FDA approved rapamycin for use as an immunosuppressant in kidney transplant patients, several pharmaceutical companies developed derivatives, called rapalogues, with better bioavailability (Robert and Gregory, 1996). Rapamycin and its chemical derivatives, rapalogues, are also used as anti-restenosis agents in drug-eluting stents and in chemotherapy for cancer. Rapamycin extends lifespan in every model organism tested, and rapalogues are in pre-clinical trials for aging-related morbidities. 8 The Target Of Rapamycin: As a small molecule, rapamycin has an unusual mechanism of action. It binds to a small intracellular protein called FKBP12, and in the form of this complex, inhibits its target. To identify the target of rapamycin, screens in yeast were performed to isolate mutants that are resistant to its growth-inhibitory effects. Mutant alleles of three genes were identified-recessive mutations in FKBP12, and dominant mutations in TOR1, and TOR2 (Heitman et al., 1991; Koltin et al., 1991). The FKBP12 null cells did not recapitulate the growth arrest, whereas the TOR1/TOR2 double mutants mimicked the growth arrest imposed by rapamycin, suggesting that rapamycin inhibits the TOR proteins (Helliwell et al., 1994). Direct evidence that rapamycin inhibited TOR came from biochemical purification from mammalian sources. Sequence analysis of the proteins revealed homology to the yeast TORs (Brown et al., 1994; Chen et al., 1994; Sabatini et al., 1994; Sabers et al., 1995). We now refer to this protein as the mechanistic target of rapamycin, or mTOR. B. mTORC1 and mTORC2 We now know that mTOR is the catalytic kinase domain of two distinct complexes, mTOR complex 1 (mTORC1), and mTOR complex 2 (mTORC2). In response to growth factors and nutrients, mTORC1 regulates key cell growth processes, such as protein, lipid, and nucleotide biosynthesis, and autophagy. Considered part of the P13K-Akt pathway, mTORC2 is less well-understood but was found to be the elusive kinase for one of the two phosphorylation sites for Akt activation in response to growth factor signaling. Thus, as part of two distinct complexes, mTOR is both upstream and downstream of itself. mTORC2 Yeast TOR2, but not TOR1, had rapamycin-insensitive functions (Xiao-Feng et al., 1995). This issue was clarified with the discovery of two distinct complexes containing TOR2. TOR1 or TOR2 can associate with the rapamycin-sensitive TOR complex 1 (TORC1), which included KOG1 (homologous to human raptor) and LST8 (homologous to human GbL/mLST8). On the other hand, only TOR2 was found in TOR complex 2 (TORC2), which comprised of AVO1 (homologous to human SIN1), AVO2, AVO3 (homologous to human rictor) (Loewith et al., 2002). In mammals, there is one mTOR 9 protein and it is found in both complexes. mTORC2 is defined by its rictor component and also contains mLST8, SIN1 (Sarbassov et al., 2004). Deletion of TORC2 components in yeast and knockdown in mammalian cells showed actin cytoskeleton defects (Jacinto et al., 2004). Interest in the mTOR pathway escalated to a new high when mTORC2 was found to be the elusive kinase for full Akt activation. The PI3K/PTEN/Akt pathway mediates insulin signaling and is one of the most commonly mutated pathways in cancer. Full activation of Akt requires phosphorylation at two sites. PDK1 executes the first round of phosphorylation on T308, and mTORC2 phosphorylates S473 for full Akt activation (Sarbassov et al., 2005b). In turn, Akt drives cell growth, cell cycle progression, glucose metabolism, and survival by signaling to its targets TSC2, Cyclin1, GSK3, and BAD (Greer and Brunet, 2005). How mTORC2 is activated by P13K is still poorly understood. mTORC1 Concurrent with yeast studies, raptor was found to be a defining component of the nutrient-responsive, rapamycin-sensitive, mammalian mTORC1 (Hara et al., 2002; Kim et al., 2002). Raptor is not required for mTOR kinase activity in vitro, but is thought to help in substrate recruitment (Sabatini, 2006). As described above, GbL/mLST8 is also a component of mTORC1, but its function has been debated. PRAS40 is the final component of mTORC1 and is an insulin-sensitive inhibitor of mTORC1 (Sancak et al., 2007b). The mechanisms through which mTORC1 senses and integrates stimuli are of great interest. One key upstream factor is the Tuberous Sclerosis Complex, TSC1-TSC2 tumor suppressor, which suppresses mTORC1 activity in response to deprivation of growth factor or energy (Brugarolas et al., 2004; Castro et al., 2003; Corradetti et al., 2005; Garami et al., 2003; Inoki et al., 2003a; Inoki et al., 2003b; Ma et al., 2005; Reiling and Hafen, 2004; Roux et al., 2004; Saucedo et al., 2003; Stocker et al., 2003; Tee et al., 2003a; Tee et al., 2002; Tee et al., 2003b; Zhang et al., 2003). The TSC complex does so by inhibiting Rheb, a GTP-binding protein that is an essential activator of the mTORC1 kinase activity (Long et al., 2005; Sancak et al., 2007a). 10 C. Amino Acid Signaling Machinery The TOR pathway has been associated with nutrient sensing ever since treatment with rapamycin or TOR1/TOR2 deletion in yeast revealed a cellular response characteristic of starvation (Barbet et al., 1996). Amino acid starvation is sufficient to cause rapid dephosphorylation of both S6K and 4EBP1 in many cell types (Fox et al., 1998a; Fox et al., 1998b; Hara et al., 1998; Kimball et al., 1998; Krause et al., 2002; Patti et al., 1998; Wang et al., 1998; Xu et al., 1998). Leucine seems to contribute the most to the amino acid-responsive effects, followed by arginine. GATOR2 complex (A) Low amino acid levels (B) High amino add levels Svc Energy, GATORI complex Energy, oxygenoxygen lel evels acids Ragulator complex signaling signaling tyt GAPPN GEF "04"t .:GA GAP Folliculin complex TSC complex Figure 1: Lysosomal integration of nutrients and growth factor signals in the mTORCI pathway, adapted from Bar-Peled et al., 2013 Amino acids do not appear to signal through the TSC complex (Nobukuni et al., 2005; Roccio et al., 2006; Smith et al., 2005). Instead, emerging evidence indicates that mTORC1 activation by amino acids requires a lysosome-associated machinery, comprised of the vacuolar adenosine triphosphatase (v-ATPase), the Ragulator, GATOR1, and the Rag GTPases (Figure 1) (Kim et al., 2008; Sancak et al., 2010; Sancak et al., 2008; Zoncu et al., 2011). Like Rheb, the Rags are members of the Rasrelated GTP-binding superfamily of proteins, but they are unusual in that they function as obligate heterodimers of RagA or B (A/B) with RagC or D (C/D). RagA and RagB are highly homologous and redundant, as are RagC and RagD (Hirose et al., 1998; Sancak et al., 2008; Schurmann et al., 1995; Sekiguchi et al., 2001). The Rag nucleotide state 11 determines mTORC1 binding and localization to the lysosome (Sancak et al., 2008; Sancak et al., 2010). We have proposed that amino acids signal from within the lysosomal lumen to Ragulator, in a v-ATPase-dependent fashion. In turn, Ragulator activates RagA/B through its activity as a guanine nucleotide exchange factor (GEF). When RagA/B is loaded with GTP, the Rag heterodimer recruits mTORC1 to the lysosomal surface where it binds Rheb and becomes activated (Bar-Peled et al., 2013; Bar-Peled et al., 2012; Efeyan et al., 2012). To turn off amino acid signals, GATOR1 activates RagA/B GTPase activity, resulting in loss of mTORC1 binding and the loss of mTORC1 lysosomal localization. Interestingly, the TSC complex shuttles on and off the lysosomal surface in response to growth factors (Menon et al., 2014). P13K signaling activates Akt and in turn phosphorylates the TSC complex, resulting in its dissociation from the lysosome. Without the GAP activity of the TSC complex acting on Rheb, Rheb is activated to stimulate mTORC1 kinase activity. Thus, the lysosome has emerged as a signal integration hub for the mTORC1 pathway. D. Downstream Effectors of mTORC1: The mTORC1 pathway regulates cell growth by phosphorylating key regulators of anabolic and catabolic processes, such as protein, lipid, and nucleotide biosynthesis, and autophagy. Before the identification of mTOR, its key substrates 4E-BP1 and S6K1 were already known to be rapamycin-sensitive (Beretta et al., 1996; Chung et al., 1992; Kuo et al., 1992; von Manteuffel et al., 1996). Shortly after its identification, mTOR was shown to be kinase responsible for their phosphorylation (Brunn et al., 1997; Burnett et al., 1998; Hara et al., 1997; Isotani et al., 1999). Both S6K1 and 4E-BP1 regulate the formation of the translational pre-initiation complex (eIF4E, eIF4G, elF3) (Holz et al., 2005). eIF4E binds the 7-methylguanosine mRNA 5' cap and unphosphorylated 4EBP1 prevents the eIF4E-mRNA complex from binding to eIF4G. mTORC1 activation phosphorylates 4E-BP1 and diminishes its affinity for eIF4E, allowing translation to proceed. Activated S6K1 phosphorylates S6, a subunit of 40S ribosome, which permits its association with the pre-initiation complex and thus translation (Holz et al., 2005). 12 S6K1 also mediates other mTORC1-associated anabolic processes. mTORC1 regulates lipid synthesis through SREBP1 and 2, transcription factors that govern expression of genes involved in fatty acid and cholesterol synthesis, in a S6K1 and Lipin-1 dependent fashion (Laplante and Sabatini, 2012; Peterson et al., 2011). S6K1 regulates nucleotide biosynthesis by phosphorylating CAD, the enzyme responsible for catalyzing the first three steps of pyrimidine synthesis (Ben-Sahra et al., 2013; Robitaille et al., 2013). Importantly, S6K1 mediates a negative feedback loop that restricts growth factor signaling. S6K1 phosphorylates insulin receptor substrates (IRS), preventing them from activating the P13K lipid kinase. This negative feedback loop plays important roles in insulin resistance, as S6K1 null mice were resistant to obesity and maintained high insulin sensitivity (Um et al., 2004). Ill. MTOR SIGNALING IN CANCER A. Pathways altered in cancer upstream of mTORC1 RT K Downstreanstrea effector Teffector Cell growth trien Figure 2: Signaling cascade upstream of mTOR, adapted from Shaw and Cantley, 2006 Tumor suppressors associated with the mTORC1 pathway are mutated in both sporadic cancers and familial tumor-prone syndromes. Growth factor receptor tyrosine kinases 13 (RTK) activate the Ras and P13K signal transduction pathways (Figure 2), both of which are deregulated in cancer (Laplante and Sabatini, 2012). NF1 normally reverses the effects of Ras as a GTPase activating protein (GAP). Germline mutations in NF1 cause neurofibromatosis, a tumor-prone syndrome (Xu et al., 1990). Both Ras and RTKs activate the catalytic subunit p11 Oa of the P13K lipid kinase, which often harbors activating mutations or is amplified in cancer (Gupta et al., 2007). The most common mechanism of activating this pathway, however, is loss of the PTEN lipid phosphatase that reverses the action of P13K. PTEN is one of the most commonly mutated tumor suppressors after p53 (Salmena et al., 2008). Mutations in PTEN also cause a familial cancer syndrome called Cowden syndrome (Liaw et al., 1997). The tuberous sclerosis complex (TSC) integrates growth factor signals and ATP levels to regulate mTORC1 activation (Dibble and Manning, 2013). Growth factor signals are conveyed by AKT, a major effector of P13K signaling, and ATP levels are reported by AMP-activated protein kinase AMPK. To signal low ATP levels, AMPK needs to be activated by LKB1 (Shaw et al., 2004; Woods et al., 2003), which is frequently mutated in lung adenocarcinomas (Sanchez-Cespedes et al., 2002). Mutations in LKB1 and TSC1/2 cause the Peutz-Jeghers and Tuberous Sclerosis Complex familial cancer syndromes, respectively (Hemminki et al., 1998; Slegtenhorst, 1997). Growth factor signaling and ATP levels regulate TSC1/2 GAP activity towards Rheb, which in turn stimulates mTORC1 kinase activity at the lysosomal surface. Rheb represents the first half of a lysosome-based coincidence detector comprised of GTPases that controls activation of mTORC1. The other half, signals amino acid levels via the Rag GTPases, which bind mTORC1 and promote its lysosomal localization. Thus, the pathway ensures that appropriate growth conditions are met by independently regulating mTORC1 lysosomal localization and kinase activation via the Rag and Rheb GTPases (Bar-Peled and Sabatini, 2014). Amino Acid Sensing by mTORC1 Although the tumor suppressors involved in growth factor signaling are well established, emerging components of the amino acid signaling machinery are already implicated in cancer. Furthermore, mTOR itself was also recently appreciated to be mutated in cancer (Grabiner et al., 2014). The Rag GTPases are obligate heterodimers comprised of RagA 14 or RagB bound to RagC or RagD. GATOR1, the GAP for RagA/B, is mutated in gliobastomas and ovarian cancers (Bar-Peled et al., 2013). Mutations in FLCN, the GAP for RagC/D, cause the Birt-Hogg-Dube tumor syndrome (Tsun et al., 2013). B. The Tumor-prone Birt-Hogg-Dube Syndrome FLCN is conserved from yeast to human yet its molecular function remains unclear. Loss of function mutations in FLCN cause an inherited cancer syndrome called Birt-HoggDube (BHD) characterized by benign skin tumors (fibrofolliculomas), bilateral, multifocal renal neoplasms of different subtypes, and lung cysts (BIRT et al., 1977). BHD is autosomal dominantly inherited and loss of heterozygosity observed in humans, mouse and rat BHD models led to a proposed tumor suppressor function for FLCN (Hasumi et al., 2009; Khoo et al., 2002; Okimoto et al., 2004). The most common germline mutation, observed in over half of BHD patients, occurs in a tract of eight cytosines where either a cytosine is inserted (1 733insC) or deleted (1 733delC), resulting in a truncated protein (Toro et al., 2008). Missense germline mutations are rare, but a BHD canine model is caused by a mutation in a highly conserved residue, corresponding to H255R in human FLCN (Lingaas et al., 2003). Because genes (tscl/2, pten, Lkbl) linked to other hamartoma syndromes are all classical tumor suppressors that restrict mTORC1 activity (Inoki et al., 2002; Sarbassov et al., 2005a; Shaw et al., 2004), it has been proposed that FLCN is a negative regulator of mTORC1 activity. However, there have been conflicting reports, in mouse models of BHD (Baba et al., 2008; Chen et al., 2008; Hartman et al., 2009; Hasumi et al., 2009; Hudon et al., 2010) and cell-based studies (Baba et al., 2006; Cash et al., 2011; Hartman et al., 2009; Takagi et al., 2008), on whether it acts as a negative or positive regulator in the mTORC1 pathway. Therefore, although there is a clear connection for FLCN to the mTORC1 pathway, how it regulates mTORC1 activity is unclear. There is emerging evidence that FLCN has a role in nutrient sensing. The FLCN and TSC1/2 yeast orthologs have opposing roles in amino acid homeostasis (van Slegtenhorst et al., 2007). Furthermore, FNIP1 and 2, which are paralogs with 74% sequence similarity, directly interact with AMP-activated protein kinase (AMPK), an energy-sensing molecule that regulates mTORC1 activity through the action of TSC 15 complex (Baba et al., 2006; Hasumi et al., 2008; Takagi et al., 2008). However, the mechanism through which FLCN regulates nutrient signaling in the mTORC1 pathway has yet to be revealed. C. Outputs of mTORC1 Altered in Cancer Processes regulated by mTORC1 that affect amino acid pools, such as protein translation and autophagy, have been implicated in cancer. S6 kinase 1 (S6K1) and eIF4E-binding protein (4E-BP1) are well known mTORC1 substrates that regulate protein translation. Phosphorylation of 4E-BP1 by mTORC1 relieves its inhibition of the elF4E translation initiation factor, allowing translation to proceed (Sonenberg and Hinnebusch, 2009). The 4E-BP1-eIF4E axis, not S6K1, is emerging as the major downstream effector of mTORC1 in cancer (Hsieh et al., 2010). elF4E is amplified or overexpressed in various sporadic cancers and increased 4E-BP1 phosphorylation correlates with poor survival outcomes (Armengol et al., 2007; Bjornsti and Houghton, 2004). Expression of phosphorylation defective 4E-BP1 reduces tumor progression in KRAS and P13K driven tumors, suggesting elF4E plays an important role in maintaining cancer growth (Hsieh et al., 2010; She et al., 2010). Conversely, loss of 4E-BP1 and 4EBP2 increased tumorigenesis in p53 null mice (Petroulakis et al., 2009). How 4EBP1elF4E deregulation promotes oncogenesis is unclear but it is thought to increase translation of pro-oncogensis proteins for cell survival (Hsieh et al., 2010; Wendel et al., 2007) and cell-cycle progression (Dowling et al., 2010). Autophagy, or 'self-eating', is a stress-induced survival mechanism that degrades and recycles damaged or superfluous proteins and organelles in the lysosome. As amino acid levels are also influenced by autophagy, especially during metabolic stress (Noboru, 2007) the mTORCI pathway is a primary autophagy regulator, shutting the process off during abundant nutrient and growth factor signaling (Kroemer et al., 2010). Autophagy plays a dual role as an oncogenic and tumor suppressive process. On one hand, autophagy is activated during early tumor formation before adequate blood supply is established to buffer metabolic stress (Degenhardt et al., 2006), and contributes to chemotherapy resistance (Amaravadi et al., 2007; Carew et al., 2007). However, despite this pro-survival role, there is clear evidence that autophagy is tumor suppressive. Monoallelic loss of beclinI, an essential autophagy component, is frequently observed in 16 human breast, ovarian, and prostate cancer, and is sufficient to cause spontaneous tumor development in mice (Liang et al., 1999; Qu et al., 2003; Yue et al., 2003). Loss of other autophagy genes such as UVRAG, Atg4C, and Bif-1 also increases susceptibility to tumorigenesis (Liang et al., 2006; Marino et al., 2007; Takahashi et al., 2007). How autophagy suppresses tumor formation is still under investigation, but as an important contributor to cellular housekeeping, autophagy clears damaged proteins, damaged mitochondria, and reactive oxygen species, which can promote oncogenesis (Mathew et al., 2009). Furthermore, autophagy is thought to prevent necrotic death in apoptotic deficient tumor cells, thereby limiting local inflammation, which can increase tumor growth (Degenhardt et al., 2006). Finally, autophagy-deficient cells are prone to chromosome instability and DNA damage (Mathew et al., 2007). Thus, targeting autophagy in cancer will likely require context-specific and disease-stage specific modulation. D. Rapalogues in cancer therapy For a pathway so critical to growth, and with so much promising pre-clinical data to support anti-tumor effects, it is disappointing that rapamycin and its derivatives have limited use in cancer therapy. Rapamycin-or its chemical derivatives, rapaloguesextend survival for cancer patients with renal cell carcinoma, and mantle cell lymphoma (Wander et al., 2011). Probably the best indication for mTOR inhibition is blocking angiomyolipoma growth in tuberous sclerosis patients, where hyperactive mTORC1 signaling is the root cause of the disease (Crino et al., 2006). Indeed, in a Phase Ill clinical trial, treatment with rapalogue, everolimus, showed a 42% response rate of reducing angiomyolipoma size (Bissler et al., 2013). Why rapalogues haven't proved to be more effective has been widely debated. Fundamentally, it seems that effectors downstream of mTORC1 control cell growth, which is certainly a requisite for tumorigenesis, but inhibition of these processes is not sufficient to kill a cancer cell. In other words, rapalogues seem to have more of a cytostatic rather than a cytotoxic effect. For example, rapamycin treatment prevents further growth of established tumors in a NF1 mouse model (Johannessen et al., 2008), and the angiomyolipomas in patients with tuberous sclerosis continue to grow after cessation of sirolimus treatment (Bissler et al., 2008). This is also true in PTEN driven 17 endometrial tumors, where regression is rarely observed but disease is stabilized by 2644% (Colombo et al., 2007; Slomovitz et al. 2008). There is evidence that mTORC1 inhibition might, in some cases, even enable more aggressive tumor cell growth. As described earlier, mTORC1 activity negatively regulates Akt signaling, and rapalogue treatment has been shown to activate Akt in colorectal carcinoma (O'Reilly et al., 2006). Loss of mTORC1 signaling may even cause other proliferative pathways to compensate, such as MAPK upregulation seen in mouse model of prostate cancer treated with rapalogues (Carracedo et al., 2008). This compensation is not surprising given the incredible selective pressures that tumor cells face. Another issue that we now appreciate is that rapamycin inhibits mTORC2 in select cells and is a partial inhibitor of mTORC1. Long-term treatment with rapamycin, as is the case in chemotherapy, has been shown to disrupt mTORC2 assembly (Sarbassov et al., 2006). Thus, the response of cancer cells to rapamycin may in fact be due to mTORC2 inhibition and loss of subsequent Akt activation. Disassembly of mTORC2 does not correlate with efficacy of treatment, so it still unclear why this fraction of tumors are responsive. The development of ATP-competitive inhibitors of mTOR has revealed that rapamycin is not a complete inhibitor of mTOR (Thoreen et al., 2009). Rapamycin inhibits S6K1 well but 4E-BP1 phosphorylation is rapamycin-resistant. Given the emerging evidence that the 4E-BP1 - eIF4E axis is deregulated in cancer, the incomplete inhibition of this axis by rapamycin may also contribute to its poor efficacy. The contribution of these two possibilities will likely become more clear once there is sufficient clinical data for the mTOR ATP-competitive inhibitors currently in trials, although dosing will be limited by the narrow therapeutic window given the inhibition of both mTORC1 and mTORC2 (Benjamin et al., 2011). Perhaps it is not surprising that rapalogues have failed as a single agent therapy. After decades of chemotherapy trials, there are rare examples for durable remission for single agents against any target. It is increasingly clear that chemotherapy will need to involve multiple agents that accommodate the stage of disease and anticipate the rewiring of signaling pathways in response to therapy. Given the mTORC1's involvement in protein translation, perhaps its inhibition will prevent cancer cells from rewiring its signaling 18 networks. It will be interesting to see how rapalogue combination therapy trials will turn out (Wander et al., 2011). IV. AMINO ACID TRANSPORT A. History: digestion, protein absorption, and amino acid uptake in tissues Digestion: a chemical process Digestion was first demonstrated to be more than mechanical-a chemical processwhen Rene Reamur, in the 1750s, induced a bird to swallow an opened tube filled with food and observed that the food was partially digested. 30 years later, Lazzaro Spallanzani confirmed these results by feeding and forcing regurgitation of many animals-himself included-with perforated spherules containing food. Furthermore, he induced himself to vomit on an empty stomach and showed that digestion can take place in gastric fluid outside of the body, confirming that it was indeed a chemical process. But perhaps the most famous experiments came in the 1830s from William Beaumont, a self-taught physician largely known as the father of gastric physiology. The opportunity came when his patient suffered a shotgun wound that left a gastric fistula, allowing direct access into his stomach. Beaumont confirmed that digestion was a chemical process, both outside the body and in the stomach, and with the help of chemists, established that hydrochloric acid was the main component of gastric juice (Complete Dictionary of Scientific Biography, 2008). Meanwhile, the proteinogenic amino acids were just being discovered, although it wasn't appreciated yet that they were the building blocks of protein. First was Asparagine, isolated from asparagus (Vauquelin, 1807), and soon leucine was discovered from cheese in 1818 and arginine from lupin seedlings in 1886 (Plimmer, 1912). But it wasn't until -1895 that Emil Fischer and Albrecht Kossel showed that amino acids were hydrolysis products of protein. And together with Franz Hofmeister, Fischer demonstrated that amino acids are linked by peptide bonds in proteins (Fischer, 1906). 19 Protein absorption: intact or as amino acids As we learned that proteins were made of amino acids, another debate was being settled-how are proteins absorbed into the body? There were two schools of thought. Liebeg and Voit posited that proteins are absorbed directly, with no or little decomposition, arguing that it would not make sense to waste energy to decompose them only to reform them in tissues (Folin, 1905). On the other hand, Pflciger and colleagues insisted that proteins were chemically changed for adequate absorption (Slyke, 1917). This debate was settled when Otto Cohnheim isolated intestinal juices, termed erepsin, and demonstrated that proteins added to erepsin are digested into amino acids (Cohnheim, 1902). This work opened many lines of investigation, further confirming that amino acids are the "protein currency of the body" (Matthews, 1978). Emil Abderhalden fed dogs only amino acids and showed that they were able to maintain a positive nitrogen balance, and even deliver pups. From these experiments, he proposed that proteins are indeed rebuilt from absorbed amino acids (Wolf, 1996). Certain amino acids were shown to be essential when Willcock and Hopkins fed mice only plant protein; they died, but were rescued by tryptophan supplementation (Willcock and Hopkins, 1906). Uptake of amino acids into tissues The field focused next on how amino acids were incorporated into tissues. In a seminal study, Van Slyke and Meyer showed that amino acids are enriched, as much as ten fold, in tissues compared to serum (Slyke and Meyer, 1913). Insights into how this large gradient was achieved came when Halvor Christensen fed guinea pigs individual amino acids and examined the relative distribution of glycine and glutamine in plasma versus tissue (Christensen et al., 1948). They saw that a subset of fed amino acids reduced glycine or glutamine enrichment in tissues, suggesting competitive inhibition of limited transporters. Based on the subsets of amino acids that can affect the distribution ratios of particular amino acids-interpreted as the substrate preferences of the different transporters-distinct transport "systems" were defined, reviewed in (Brder, 2008). In 1957, before molecular characterization and any crystallographic insight, Peter Mitchell proposed an alternating access mechanism for transporters, which has largely turned out to be true (Mitchell, 1957). 20 Since the advent of expression cloning (Hediger et al., 1987), there has been an explosion of gene identification responsible for many transport activities, including amino acids. About 10% of the genome (-2,000 genes) is dedicated to transporting solutes across membranes. Half are represented by solute carrier (SLC) transporters, -35% are ion channels and the remaining 15% are ATPases, reviewed in (Hediger et al., 2013). B. The SLC38 Amino Acid Transporter family The SLC families are defined by sequence similarity of 20-25% (Hediger et al., 2004). The SLC38 family is comprised of sodium-coupled amino acid transporters. SLC38A1-5 reside on the plasma membrane, but SLC38A7 localizes to the lysosome (Chapel et al., 2013), while SLC38A8-11 have not been characterized. Interestingly, SLC38A9 has diverged over evolution from all other SLC38 members (Figure 3) (Schi6th et al., 2013). The SLC6, -7, and -36 families are the closest in sequence similarity to the SLC38 family. SLC38A1-6 SLC38A11 a.k.a. PAT 1-4 SLC38A9 SLC38A7-8 vesicular GABA/ Gly transporter SLC38A10 Figure 3: SLC38A9 is phylogenetically separated from other SLC38 family members, adapted from Schioth et al., 2013 21 Although the SLC families are segregated by sequence divergence, recent crystal structures of several SLC families, namely SLC6 and SLC7, show remarkable structural similarity, reviewed in (Forrest and Rudnick, 2009; Krishnamurthy et al., 2009; Perez and Ziegler, 2013; Schweikhard and Ziegler, 2012). The leucine transporter LeuT was the first to be crystallized among these and has laid the foundation for ion-coupled amino acid/polyamine transport (Yamashita et al., 2005). The LeuT fold represents one of five different structural architectures found in transporters (Schlessinger et al., 2010). C NSS (LeuT) N Repeat I Repeat 2 C NCS1 (Mhpl) ApcT (AdI) SSSP(SGLT) BCCT (BetP) Figure 4: Structurally conserved inverted repeat domain structure of LeuT across many SLC transporter families, adapted from Khafizov et al., 2010 The LeuT fold, found in the AdiC, vSGLT, BetP, GadC, MHP1, ApcT, DAT, and CaiT structures, comprises a ten transmembrane (TM) domain of inverted structural repeats, each 5 TM segments, suggesting a structural mechanism of alternative access. Remarkably, this structural fold is conserved despite substantial differences in sequence, coupling mode, and nature of substrate (Figure 4) (Khafizov et al., 2010). TM domains 1, 3, 6, and 8 are involved in substrate binding and TM1 and 6 have a break in 22 their alpha-helix structure to form a hinge that bends during transport. Although a crystal structure of an SLC38 family member has yet to be solved, the Drosophila dopamine transporter SLC6A3 (DAT) shows remarkable similarity to the related LeuT prokaryotic structures (Penmatsa et al., 2013). C. Arginine transport at the plasma and lysosomal membranes Arginine is used in the synthesis of many biomolecules, including creatine, urea, agmatine, nitric oxide and proteins. Arginine is considered a semi-essential amino acid because it is required during development but adult tissues, particularly the kidney, can synthesize it. However, during times of high demand, such as wound healing, sepsis, and growth, endogenous arginine may be limiting (Closs et al., 2004). Plasma membrane transporters that accept arginine as a substratel,2 Arginine transport Gene 3 Transport Na+ - system dependent Na+ - 3 Apparent Km dependent y+LAT2 + SLC7A6 4F2hc b0. AT rBAT ATBO,I SLC3A2 SLC7A9 4 SLC3A1 SLC6A14 No No No No - - 0.10-0.16 3.40-3.90 0.25-0.70 0.20-0.50 - - - - Yes No Moderate Moderate 12 12 12 13 y+L No 0.346 Yes 0.02 Yes 14 y+L No 0.12-0.147 Yes 0.20-0.30 Yes 15 0.08-0.20 0.10-0.15 No Yes + Cl- 0.30 0.01 Yes No 16, 17 18 + CAT-4 y' ND y+ y+ Ref. + y+LAT1 + 4F2hc SLC7A1 SLC7A2 SLC7A2 SLC7A3 SLC7A4 SLC7A7 SLC3A2 Transstimulation mmol/L mmoWlL CAT-13,4 CAT-2A3 CAT-2B3,4 3 CAT-3 5 Apparent Km - Protein Leucine transport bO.0 B , No Yes + Cl 1 Known carrier proteins for arginine are listed; only the most common name for each protein is given. Gene names are per HUGO. Apparent extracellular Km values are for arginine and, where applicable, the neutral amino acid leucine (for comparison). 2 Abbreviations: AT, amino acid transporter; ND, not defined. 3 Values are for human CAT proteins. Note that experimental Km values vary considerably. 4 CAT-1 and CAT-2 may also mediate activities of systems b1 and b2 (23). 5 No transport activity has been detected. 6 Value for arginine is 93 ytmol/L in the absence of Na 7 Km is independent of Na+ concentration. Table 1: Plasma membrane arginine transport, adapted from Closs et al., 2004 Arginine transport at the plasma membrane is largely mediated by the cationic transport system y+ (y from lysine, first substrate described for this system, + for cationic), comprised of cationic amino acid transporters CAT1-4, also known as SLC7A1-4 (Deves and Boyd, 1998; Fotiadis et al., 2013; Verrey et al., 2004; White, 1985). Recent kinetic experiments revealed other minor routes via other transport systems, summarized in Table 1. Unlike most plasma membrane transporters, which have high affinities in the 50-300 pM, range, CAT2, expressed in the liver, is a low-affinity (-4mM), high-capacity 23 arginine transporter thought to be responsible for cationic amino acid uptake following a meal (Closs et al., 1993). Arginine transport at the lysosomal membrane is relatively poorly characterized and is largely achieved through a distinct transport system, dubbed system c. This transports cationic amino acids lysine, arginine, ornithine, histidine, and ornithine, and its activity is ATP, pH gradient, and vATPase-dependent, but not Na-dependent (Pisoni et al., 1985; Pisoni et al., 1987; Ramirez-Montealegre and Pearce, 2005). Unlike many plasma membrane transport activities, no lysosomal transport has been reported to be Nadependent (Pisoni and Thoene, 1991). Interestingly, the Km of arginine uptake into lysosomes in fibroblasts is 300 pM, approximately 8 fold higher than that observed in the plasma membrane, indicating a much lower-affinity system at the lysosome. The orphan transporter SLC7A14 was recently proposed to participate in system c based on its lysosomal localization and substrate profile of a SLC7A2-SLC7A14 chimera (Jaenecke et al., 2012). However, more compelling evidence indicates that PQLC2 is largely responsible for lysosomal arginine efflux. C. elegans mutants defective in PQLC2 have excess arginine and lysine in their lysosomes, and transport studies of heterologously-expressed PQLC2 in oocytes, representing lysosomal-export activity, reveal a Km of -4 mM (Jezegou et al., 2012; Liu et al., 2012). Such a low-affinity transport activity for PQLC2 is consistent with a role in arginine/lysine export from the lysosome, when concentrations become high following autophagy or lysosomaldegradation of proteins. Because it was technically not possible to assay lysosomal import activity of PQLC2, it is unclear if PQLC2 is also responsible for the lysosomal import activity of arginine (Km 300 pM). It is likely that SLC7A14 and/or other transporters may be involved. 24 V. PREFACE FOR WORK PRESENTED IN THIS THESIS: How the mTORC1 pathway senses the multitude of inputs to stimulate growth only in the appropriate context has been of great interest. We now know that these signals are integrated at the lysosome by a coincidence detector comprised of the Rag and Rheb GTPases (Figure 5). Growth factors, energy levels and stresses regulate the activity of Rheb, which stimulates mTORC1 kinase activity. Amino acids, on the other hand, signal through the Rags, which regulate mTORC1 localization to the lysosome. Thus, by independently controlling the kinase activity and subcellular localization of mTORC1, these regulators ensure that mTORC1 is only active in appropriate growth conditions. Inputs: growth factors energy levels Input. amino stress acids Function: Function: stimulates mTORC1 kinase activity recruits mTORC1 to lysosome p Ls om Figure 5: The Rag and Rheb GTPases are key regulators of mTORC1 Whereas the upstream regulators of Rheb are relatively well characterized, the mechanisms of amino acid signaling are only beginning to emerge. The Rag GTPases interact with mTORC1 and signal amino acid sufficiency by promoting the translocation of mTORC1 to the lysosomal surface, the site of its activation. The Rags are unusual GTPases in that they function as obligate heterodimers, which consist of RagA or B (A/B) bound to RagC or D (C/D). We have proposed that amino acids signal from within the lysosomal lumen to Ragulator, the lysosomal scaffold for the Rags, in a v-ATPasedependent fashion. In turn, Ragulator activates RagA/B through its guanine nucleotide exchange factor (GEF) activity. When RagA/B is loaded with GTP, the Rag heterodimer recruits mTORC1 to the lysosomal surface where it can bind Rheb and becomes activated. 25 What is the role of RagC/D in the Rag heterodimer? Although the loading of RagA/B with GTP initiates amino acid signaling to mTORC1, the role of RagC/D was unknown. We discovered that RagC/D is a key regulator of the interaction of mTORC1 with the Rag heterodimer and that, unexpectedly, RagC/D must be GDP-bound for the interaction to occur. We identified Folliculin (FLCN) and its binding partners, FNIP1 and 2, as Rag interacting proteins. Mutations in FLCN cause the tumor-prone Birt-Hogg-Dube syndrome, yet the molecular function of FLCN had been elusive. We found that FLCN is necessary for mTORC1 activation by amino acids and that the FLCN-FNIP complex has GTPase activating protein (GAP) activity for RagC/D, but not RagA/B. Thus, we revealed a role for RagC/D in mTORC1 activation and a molecular function for FLCN (Figure 6). IP (inactive) FLCN-FNIP GAP activity towards RagCID +Amino acids Figure 6: FLCN-FNIP is a GAP for RagC/D What is the amino acid sensor(s)? Although there are many components being discovered in this amino acid signaling machinery, the actual amino acid sensor(s) has been elusive. Recent work demonstrated that amino acids signal from within the lysosomal lumen, through an unknown mechanism, to the Rags and Ragulator complexes, which reside on cytosolic side of the lysosomal membrane. We reasoned that candidate sensor(s) would be transmembrane protein(s) and interact with Rag and Ragulator, key components of the amino acid signal transduction machinery. 26 We identified SLC38A9, an uncharacterized protein with sequence similarity to amino acid transporters, as a lysosomal transmembrane protein that interacts with the Rag GTPases and Ragulator in an amino acid-sensitive fashion. The cytosolic facing, Nterminal region of 119 residues in SLC38A9 is sufficient for Rag/Ragulator interaction, which we call the Ragulator-binding domain, but the amino acid-regulated interaction requires the 11 transmembrane domains, where amino acid substrates are predicted to bind. In vitro liposome reconstituted SLC38A9 transports arginine with a high Km (-40mM) and seems to have a broad substrate profile. Loss of SLC38A9 represses mTORC1 activation by amino acids, particularly arginine. Overexpression of SLC38A9 or just its Ragulator-binding domain makes mTORC1 signaling insensitive to amino acid starvation but not to Rag activity. Thus, SLC38A9 functions upstream of the Rag GTPases and is an excellent candidate for being an arginine sensor for the mTORC1 pathway (Figure 7). amino v-ATPase 11 acids cytosol SLC38A9 lysosomal membrane lysosomal lumen amino acids Figure 7: SLC3BA9 Is a candidate amino acid sensor. 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(2011). mTORC1 Senses Lysosomal Amino Acids Through an Inside-Out Mechanism That Requires the Vacuolar*H+-ATPase. Science 334, 678-683. 37 CHAPTER 2 Reprinted from Cell Press: The Folliculin tumor suppressor is a GAP for RagC/D GTPases that signal amino acid levels to mTORC1 , Zhi-Yang Tsun, 2 , Liron Bar-Peled1 2', Lynne Chantranupong 1 ,2 , Roberto Zoncu, 2 2 3 Tim Wang1,2 , Choah Kim 1 ,2, Eric Spooner', and David M. Sabatini1, , 1Whitehead Institute for Biomedical Research and Massachusetts Institute of Technology, Department of Biology, Nine Cambridge Center, Cambridge, MA 02142, 2Koch USA Institute for Integrative Cancer Research, 77 Massachusetts Avenue, Cambridge, MA 02139, USA 3 Howard Hughes Medical Institute, Department of Biology, Massachusetts Institute of Technology, Cambridge, MA 02139, USA * These authors contributed equally to this work Correspondence should be addressed to D.M.S. Tel: 617-258-6407; Fax: 617-452-3566; Email: sabatiniawi.mit.edu Experiments Experiments Experiments Experiments Experiments in in in in in Figures 1, S1 were performed by LBP. Figures 2D were performed by LC. Figure 2C were performed by ZYT under guidance of TW. Figures 3A, 3B, S2 were performed by ZYT under guidance of RZ. Figures 2A, 2B, 2E, 2F, 3C, 3D, 4, S3 were performed by ZYT. 38 SUMMARY The mTORC1 kinase is a master growth regulator that senses numerous environmental cues, including amino acids. The Rag GTPases interact with mTORC1 and signal amino acid sufficiency by promoting the translocation of mTORC1 to the lysosomal surface, its site of activation. The Rags are unusual GTPases in that they function as obligate heterodimers, which consist of RagA or B bound to RagC or D. While the loading of RagA/B with GTP initiates amino acid signaling to mTORC1, the role of RagC/D is unknown. Here, we show that RagC/D is a key regulator of the interaction of mTORC1 with the Rag heterodimer and that, unexpectedly, RagC/D must be GDP-bound for the interaction to occur. We identify FLCN and its binding partners, FNIP1/2, as Raginteracting proteins with GAP activity for RagC/D, but not RagA/B. Thus, we reveal a role for RagC/D in mTORC1 activation and a molecular function for the FLCN tumor suppressor. PU.LCN-FNIP +Amino acids m TORCI FLCN-FNIP GAP activity towards RagC1D HIGHLIGHTS -RagC/D nucleotide state is a key determinant of mTORC1 binding to the Rag GTPases -FLCN-FNIP complex interacts with the Rag GTPases in an amino-acid sensitive fashion -FLCN is necessary for mTORC1 activation by amino acids -FLCN-FNIP complex is a GTPase activating protein (GAP) for RagC/D 39 INTRODUCTION The mechanistic target of rapamycin complex 1 (mTORC1) protein kinase is a master regulator of growth. It senses a diverse set of signals, such as growth factors, nutrient and energy levels, to regulate many anabolic and catabolic processes, including protein, lipid, and nucleotide synthesis, as well as autophagy. Given that mTORC1 regulates a multitude of processes, it is not surprising that the pathway it anchors is deregulated in various common diseases, including cancer (reviewed in Howell et al., 2013; Kim et al., 2013; Yuan et al., 2013; Zoncu et al., 2011b). The mechanisms through which mTORC1 senses and integrates stimuli have - been of great interest over the last few years. One key upstream factor is the TSC1 TSC2 tumor suppressor, which suppresses mTORC1 in response to growth factor or energy deprivation (Brugarolas et al., 2004; Castro et al., 2003; Corradetti et al., 2005; Garami et al., 2003; Inoki et al., 2003a; Inoki et al., 2003b; Ma et al., 2005; Reiling and Hafen, 2004; Roux et al., 2004; Saucedo et al., 2003; Stocker et al., 2003; Tee et al., 2003a; Tee et al., 2002; Tee et al., 2003b; Zhang et al., 2003). TSC1-TSC2 does so by inhibiting Rheb, a GTP-binding protein that is an essential activator of the mTORC1 kinase activity (Long et al., 2005; Sancak et al., 2007). mTORC1 is also acutely sensitive to drops in amino acid levels, but these nutrients do not appear to signal through TSC1-TSC2 (Nobukuni et al., 2005; Roccio et al., 2006; Smith et al., 2005). Instead, emerging evidence indicates that mTORC1 activation by amino acids requires a lysosome-associated machinery, comprised of the vacuolar adenosine triphosphatase (v-ATPase), the Ragulator, and the Rag GTPases (Kim et al., 2008; Sancak et al., 2010; Sancak et al., 2008; Zoncu et al., 2011 a). Like Rheb, the Rags are members of the Ras-related GTP-binding superfamily of proteins, but they are unusual in that they function as obligate heterodimers of RagA or B (A/B) 40 with RagC or D (C/D). RagA and RagB are highly homologous and redundant, as are RagC and RagD (Hirose et al., 1998; Sancak et al., 2008; Schurmann et al., 1995; Sekiguchi et al., 2001). We have proposed that amino acids signal from within the lysosomal lumen to Ragulator, in a v-ATPase-dependent fashion. In turn, Ragulator activates RagA/B through its guanine nucleotide exchange factor (GEF) activity. When RagA/B is loaded with GTP, the Rag heterodimer recruits mTORC1 to the lysosomal surface where it binds Rheb and becomes activated (Bar-Peled et al., 2013; Bar-Peled et al., 2012; Efeyan et al., 2012). Whereas much attention has focused on RagA/B, the role of RagC/D in mTORC1 signaling has remained a mystery. Here, we make the surprising finding that GDP-loading of RagC is necessary for the binding of mTORC1 to the Rag heterodimer, and that the nucleotide state of RagC affects the activation of mTORC1 in response to amino acids. Moreover, we identified the FLCN-FNIP complex as a potent GTPase activating protein (GAP) for RagC/D that interacts with the Rag heterodimer in an amino acid-sensitive fashion and localizes to the lysosomal surface upon amino acid starvation. Thus, we provide a molecular function for FLCN, mutations in which cause the BirtHogg-Dub6 hereditary cancer syndrome, and reveal a role for RagC/D in amino acid signaling to mTORC1. RESULTS The RagC Nucleotide State Determines mTORCI Binding to the Rag Heterodimer The binding of mTORC1 to the heterodimeric Rag GTPases in the presence of amino acids is a key event in the activation of mTORC1. Using two classes of Rag nucleotide binding mutants, we and others have shown that the interaction between the Rags and mTORC1 depends on the nucleotide configuration of the Rag heterodimer 41 (Gong et al., 2011; Sancak et al., 2008). The first class of mutations (RagBQ 9 9 Land RagCQ12 0L) is analogous to the oncogenic H-RasQ'1L mutant (Frech et al., 1994; Krengel et al., 1990) that abolishes GTPase activity and maintains RagB or RagC loaded with GTP (Bar-Peled et al., 2012; Sancak et al., 2008). Mutations of the second class (RagAT 2 1N, RagBT 54 N, and RagCS 7 5 N) disrupt the coordination of the magnesium co-factor (Feig, 1999; Feig and Cooper, 1988; John et al., 1993), resulting in mutants with much lower affinity for all nucleotides but with likely preferential binding of GDP over GTP within cells (Bar-Peled et al., 2012; Sancak et al., 2008). To test the contribution of each Rag to the binding of mTORC1, we expressed combinations of Rag nucleotide mutants in human embryonic kidney (HEK)-293T cells. 99 Consistent with previous reports (Gong et al., 2011; Sancak et al., 2008), RagBQ L_ CS 7 5 N co-immunoprecipitated the largest amount of endogenous mTORC1 (Figure IA). From these data, as well as the observation that RagAT 2 1N- or RagBT 5 4 N-containing heterodimers do not co-immunoprecipitate mTORC1, it has been supposed that RagA/B nucleotide state is the major determinant for mTORC1 binding (Gong et al., 2011; Sancak et al., 2008). To re-examine which Rag heterodimer is responsible for mTORC1 binding, we immunoprecipitated single Rag nucleotide mutants paired with wild-type partners. Surprisingly, RagB-CS 7 5 N, but not RagBQ 9 9 L-C, was sufficient to recover large amounts of mTORC1 similar to that of RagBQ 99 LCS 7 5 N, suggesting that the RagC nucleotide state determines mTORC1 binding (Figure 1A). Because the behavior of these mutants may not reflect that of nucleotide-loaded, wild-type Rags, we developed an in vitro assay in which we load purified Rag heterodimers with specified nucleotides and monitor their ability to bind to raptor, the Rag-binding subunit of mTORC1. Unexpectedly, wild-type Rags loaded with GDP bound more raptor than Rags loaded with GTP (Figure 1 B), suggesting that the GDP-bound state of one or both Rags promotes raptor binding. To determine which Rag in the 42 heterodimer is responsible for this effect, we employed another class of Rag nucleotide mutants that has base specificity for xanthine rather than guanine nucleotides (BarPeled et al., 2012; Hoffenberg et al., 1995; Schmidt et al., 1996). We term these RagBX and RagCX (RagBD1 63 N, RagCD1 81N), as they bind less than 2% of the amount of guanine nucleotides bound by their wild-type counterparts (Bar-Peled et al., 2012). Consistent with the results obtained in cells, the RagC nucleotide state determined raptor binding, as only GDP-loaded RagBx-C could bind raptor (Figure 1 C). Importantly, RagB-CX loaded with XDP also recovered raptor, suggesting that the state induced by the nucleotide diphosphate loading of RagC promotes raptor binding (Figure 1 D). Thus, unlike most GTPases, which activate their effectors in the GTP-bound state, it is the GDP-bound state of RagC that promotes raptor binding to the Rag heterodimer. Given that the nucleotide state of RagC is important for mTORC1 binding, we reasoned that expression of RagC nucleotide mutants might alter the sensitivity of the mTORC1 pathway to amino acid levels. Indeed, expression of RagCS 7 5 Nrendered mTORC1 activity resistant to amino acid starvation, as judged by phosphorylation of S6 kinase (S6K1), a canonical mTORC1 substrate (Figure 1E). Conversely, the GTP-bound mutant RagCQ 2 0L blunted mTORC1 activity, even in the presence of amino acids. Thus, RagC plays a pivotal role in mediating the binding of mTORC1 to the Rag heterodimer and manipulating the nucleotide state of RagC affects mTORC1 pathway activity. FLCN Interacts with the Rag GTPases in an Amino Acid-Sensitive Fashion Because RagC is critical for mTORC1 activation, we sought to identify regulators of its nucleotide state. We employed proteomic approaches that have successfully identified other mTORC1 pathway components (see Experimental Procedures). Mass spectrometric analysis of anti-FLAG immunoprecipitates prepared from HEK-293T cells stably expressing FLAG-tagged RagA, -B, -C, or -D, but not control proteins, 43 consistently identified peptides derived from Folliculin (FLCN) and its interacting partners, FNIP1 and FNIP2. FLCN is evolutionarily conserved, yet its molecular function remains unknown (Schmidt, 2012; van Slegtenhorst et al., 2007). Loss-of-function mutations in FLCN cause a familial cancer syndrome called Birt-Hogg-Dube (BHD), characterized by hamartomatous tumors of the hair follicle (fibrofolliculomas), kidney, and lung (BIRT et al., 1977; Nickerson et al., 2002). Given that TSC1/2, PTEN, and LKB1-genes linked to other hamartoma syndromes-are bona fide tumor suppressors that impinge on the mTORC1 pathway, FLCN is likely a regulator of the pathway (Baba et al., 2006; Guertin and Sabatini, 2007). In addition, there is emerging evidence that FLCN plays a role in mTORC1 nutrient sensing, potentially implicating the involvement of the Rags. For example, deletions of the fission yeast orthologs of FLCN and TSC1/2 have opposite effects on the expression of amino acid metabolism genes (van Slegtenhorst et al., 2007). Furthermore, a chemical genomic screen revealed that the deletion mutants for the budding yeast orthologs of FLCN (LST7) and the Rags (GTR1, GTR2) exhibited similar growth sensitivities to various environmental and chemical insults (Figure S1) (Hillenmeyer et al., 2008). FLCN forms a complex with either FNIP1 or FNIP2, paralogs with 74% sequence similarity (Baba et al., 2006; Hasumi et al., 2008; Takagi et al., 2008). The FNIPs directly interact with AMP-activated protein kinase (AMPK), an energy-sensor that monitors the AMP/ATP ratio. Given these results, the possibility that the FLCN-FNIP complex interacts with the Rags was of great interest. To begin to verify our mass spectrometric identification of FLCN and FNIPs as Rag-interacting proteins, we expressed them alone or in combination in HEK-293T cells. Endogenous RagA and RagC co-immunoprecipitated with FLCN when it was coexpressed with FNIP2, but not with metap2, or when FLCN or FNIP2 were expressed 44 alone (Figure 2A). This suggests that a FLCN-FNIP2 complex is required for either FLCN or FNIP2 to interact with the Rags. The Rags, Ragulator, and v-ATPase, established components of the mTORC1 nutrient-sensing machinery, all engage in nutrient-responsive interactions with each other (Bar-Peled et al., 2012; Efeyan et al., 2013; Zoncu et al., 2011 a). Like that of Ragulator and the v-ATPase, the interaction between endogenous FLCN and the Rag heterodimer, isolated through stably expressed RagB, strengthened upon amino acid starvation (Figure 2B). FLCN is Necessary for mTORC1 Activation and Localization to the Lysosomal Membranes Studies investigating the role of FLCN in the mTORC1 pathway in mammalian systems have yielded equivocal results. While in most cell-based systems acute loss of FLCN inhibits mTORC1 activation (Bastola et al., 2013; Hartman et al., 2009; Hudon et al., 2010; Takagi et al., 2008; van Slegtenhorst et al., 2007), deletion of FLCN in tissues in vivo, causes mTORC1 hyperactivation (Baba et al., 2008; Baba et al., 2012; Chen et al., 2008; Hasumi et al., 2009) (see Discussion for more details). In the cell-based assays we have used to study other mTORC1 components, we find that FLCN is indeed necessary for mTORC1 activation by amino acids. In HEK-293T cells, short-hairpin RNAs (shRNAs) targeting FLCN suppressed mTORC1 activation by amino acids, as read out by the phosphorylation of S6K1 (Figure 2C). This phenotype was recapitulated in Drosophila S2 cells treated with double stranded RNAs (dsRNAs) targeting the ortholog of FLCN, indicating that the function of FLCN is conserved (Figure 2D). Collectively, these results show that FLCN interacts with the Rag GTPases in a nutrientsensitive manner and is necessary for mTORC1 activation by amino acids. 45 A key event in the activation of mTORC1 by amino acids is its recruitment to the lysosomal surface by the Rag GTPases (Sancak et al., 2010). In HEK-293T cells expressing shRNAs targeting FLCN, mTOR failed to localize to LAMP2-positive lysosomes in response to amino acid stimulation (Figure 2E). Unlike Ragulator, the lysosomal scaffold for the Rags, FLCN was not required for Rag subcellular localization (Figure 2F). Thus, although the Rags localize appropriately to the lysosomal membranes in FLCN knockdown cells, mTORC1 is unable to be recruited there. These results are consistent with FLCN being required for mTORC1 activation by amino acids (Figure 2C). FLCN Co-Localizes with the Rag GTPases on the Lysosomal Surface in an Amino Acid-Sensitive Fashion Given that FLCN and FNIPs are enriched in membranes (Takagi et al., 2008) and that FLCN interacts with the Rag GTPases, we tested the possibility that FLCN itself may localize to the lysosomal surface. Indeed, in HEK-293T cells co-expressing HAFNIP2, GFP-tagged FLCN co-localized with RFP-tagged LAMP1, a lysosomal marker (Figure 3A), and this association persisted over time as lysosomes trafficked within the cell (Figure 3B). Consistent with previous reports (Takagi et al., 2008), FLCN-GFP was found diffusely throughout the cell when FNIP2 was not co-expressed (Figure S2), suggesting that FNIP2 is required for the lysosomal localization of FLCN. Despite detecting amino acid-sensitive interactions between the Rags and FLCN in co-immunoprecipitation experiments, initial tests using transiently co-expressed FLCN and FNIP2 did not reveal appreciable nutrient-responsive changes in their localization. We reasoned that overexpression might overwhelm endogenous regulatory mechanisms; therefore, we sought to probe the localization of endogenous FLCN using an anti-FLCN antibody. Although knockdown of FLCN expression did not diminish the immunofluorescence signal of most anti-FLCN antibodies we tested, we did identify one 46 antibody that showed both specific (lysosomal) and non-specific (nuclear) signals (Figure 3C). Using this antibody we found that, in HEK-293T cells, endogenous FLCN was enriched at the lysosomal surface during amino acid starvation and dispersed upon amino acid stimulation (Figure 3C). Furthermore, in HEK-293T cells treated with Torin1, an ATP-competitive inhibitor of mTOR (Thoreen et al., 2009), FLCN still dispersed from the lysosome upon amino acid stimulation (Figure 3D). Thus, FLCN localizes to the lysosomal surface during amino acid starvation, but leaves this site upon amino acid stimulation in an mTORC1 activity-independent manner. This regulated localization of FLCN to the lysosomes is consistent with the increased binding of FLCN to the Rags under amino acid starvation conditions (Figure 2B). FLCN-FNIP2 is a GAP for RagC and RagD Regulators of GTP-binding proteins commonly associate with either the GTP- or GDP-bound form of their cognate GTPases (Takai et al., 2001). To investigate the molecular function of the FLCN-FNIP complex, we asked if it exhibits any preferential binding to the Rag GTPase mutants. Different combinations of Rag mutants were coexpressed with FNIPs in HEK-293T cells. Interestingly, Rag heterodimers containing low affinity nucleotide mutants behaved in opposite ways; large amounts of endogenous FLCN co-purified with the RagBT5 4 N-C heterodimer, whereas little FLCN was recovered with RagB-CS 7 5 N (Figure 4A). In contrast, RagB-CS 7 5Nwas able to interact with mTORC1 and Ragulator, as detected through their raptor and p18 subunits, respectively. These binding properties are consistent with several possible functions for the FLCN-FNIP complex. The robust binding to RagBT 54 Nsuggests that the FLCN-FNIP complex might be a guanine nucleotide exchange factor (GEF) or GDP dissociation inhibitor (GDI) for RagB (Bos et al., 2007; DerMardirossian and Bokoch, 2005). Intriguingly, a recent report of the crystal structure of the FLCN C-terminal domain 47 revealed that despite having almost no sequence similarity, it shares structural similarity with the DENN domain, which has GEF activity towards the Rab GTPases (Nookala et al., 2012). Alternatively, although not mutually exclusively, the inability of FLCN to interact with RagCS 75 Nindicates that the FLCN-FNIP complex prefers binding to RagC in its GTP-bound state, a property shared by many GTPase activating proteins (GAPs) (Bos et al., 2007; Takai et al., 2001). Because the Rags function as obligate heterodimers, it was necessary to monitor the nucleotide state of one Rag at a time. To accomplish this, we assembled Rag heterodimers composed of a wild-type Rag with its appropriate RagX partner. Thus, loading with radiolabeled guanine and unlabeled xanthine nucleotides allowed us to selectively monitor the nucleotide state of the wild-type Rag, as previously described (Bar-Peled et al., 2012). Purified FLCN-FNIP complex did not stimulate or inhibit the dissociation of GDP from RagB or RagC when coupled with either a RagX or wild-type partner (Figures S3A-S3C). These results suggest that FLCN-FNIP does not have GEF or GDI activities towards the Rags. Instead, the strong binding to RagBT 5 4 Nmight indicate that RagB serves as a docking site for FLCN-FNIP on the Rag heterodimer. As RagB is GDP-bound during amino acid starvation, this behavior would be consistent with both the increased binding to the Rag heterodimer and lysosomal localization of FLCN under this condition (Figures 2B and 3C). We pursued the possibility that the FLCN-FNIP complex may be a GAP for RagC/D. To assay GTPase activating activity towards one Rag at a time, we prepared Rag heterodimers with a wild-type Rag partnered with a doubly mutated Rag that binds xanthine nucleotides but lacks GTPase activity, termed RagBQ 9 9 L-X and RagCQ12 0LX. expected, purified GATOR1, a GAP for RagA/B (Bar-Peled et al., 2013), strongly stimulated the GTPase activity of RagB, but not RagC or RagD (Figures 4B-4D). Conversely, purified FLCN-FNIP2 potently stimulated GTP hydrolysis by RagC and 48 As RagD, but not RagA, RagB, or Rap2A (a control GTPase), in a time- and dosedependent manner (Figures 4B-4E, 4G, S3D). Similar degrees of GAP activity were observed toward RagC when RagBx was loaded with either XTP or XDP, suggesting that the GAP activity towards RagC/D is not dependent on the nucleotide state of RagA/B (Figure 4F). The FLCN-FNIP1 complex was overall less active than FLCNFNIP2 and appears to prefer RagD instead of RagC (Figures 4B and 4C). The observed GTP hydrolysis was not due to contaminating phosphatases because addition of purified FLCN-FNIP2 to free GTP showed minimal hydrolysis (Figure S3E). Furthermore, an FLCN-FNIP2 complex with FLCN lacking its N-terminal region (Nookala et al., 2012), but that still interacts with the Rags, did not exhibit GAP activity, suggesting that this region is required for the GAP activity (Figure 4F). In contrast to a recent report that proposed that the leucyl-tRNA synthetase (LRS) acts as a GAP for RagD (Han et al., 2012), purified LRS did not increase basal GTPase activity of any of the Rags in any condition tested (Figures 4B-D). Lastly, purified FLCN or FNIP2 alone did not have GAP activity for the Rags, suggesting that an intact complex is required (Figure 4F). As RagC-GDP is required for mTORC1 binding to the Rag heterodimer (Figure 1), we asked if FLCN-FNIP2 GAP activity was sufficient to promote binding of mTORC1 to the Rags in vitro. Indeed, addition of FLCN-FNIP2, but not a control protein, caused RagBX-C loaded with GTP to bind raptor (Figure 4H). Together, these results indicate that FLCN-FNIP2 acts as a positive component of the mTORC1 pathway by promoting the binding of mTORC1 to the Rag heterodimer via its GAP activity for RagC and RagD. 49 DISCUSSION A growing body of evidence indicates that the Rags and Rheb are key components of a coincidence detector mechanism that ensures mTORC1 is active only in the appropriate growth conditions (reviewed in Dibble and Manning, 2013; Efeyan et al., 2012; Kim et al., 2013; Yuan et al., 2013). Through a Rag-mediated pathway, amino acids recruit mTORC1 to the lysosomal surface, where it can encounter Rheb. If growth factors and energy levels are sufficient, Rheb then binds to and activates the kinase activity of mTORC1. Our new findings support the idea that the Ragulator-Rag complex is a nutrient-regulated docking site for mTORC1 on lysosomes, in which the nucleotide state of RagC, and likely RagD, is the key determinant of mTORC1 binding. Our work raises a number of intriguing questions. First, given the importance of RagC in the binding of the Rag heterodimer to mTORC1, what is the role of RagA/B? It is clear that RagA/B plays a dominant role in mTORC1 activation as expression of a RagA/B mutant that is bound constitutively to GTP makes the mTORC1 pathway completely insensitive to amino acid starvation (Efeyan et al., 2013; Kim et al., 2008; Sancak et al., 2008). A likely possibility is that RagA/B controls a process that has not been recognized but is critical for mTORC1 signaling. For example, RagA/B may regulate the subcellular localization of the heterodimer, thereby controlling its access to mTORC1. While the Rag proteins appear to be constitutively localized to the lysosomal surface, there may be a pool of Rag heterodimers that cycle on and off lysosomes upon amino acid stimulation, enabling them to find and retrieve mTORC1 from its nonlysosomal location in amino acid-starved cells. This cycling could be controlled by the RagA/B nucleotide state, which would be consistent with the observation that the loading of RagA/B with GDP greatly strengthens the binding of the Rag heterodimer to Ragulator, its lysosomal scaffold (Bar-Peled et al., 2012). 50 Such a model could also help address a second conundrum. As mTORC1 and the Rags reside on the lysosomal surface in the presence of amino acids, why is FLCN found diffusely in the cytoplasm under this same condition? A possibility consistent with the above model is that FLCN activates RagC/D in Rag heterodimers that have come off the lysosomes upon amino acid stimulation and are on route to recruiting mTORC1. Alternatively, in amino acid starved cells FLCN might be poised at the lysosomal surface to activate RagC/D upon the restoration of amino acid levels, but such a scenario would require a mechanism to regulate the FLCN-FNIP GAP activity. A third question is why FLCN is a tumor suppressor and yet in most studies in cultured cells and whole organisms, including ours, it scores as a positive component of the TORC1 pathway (Baba et al., 2006; Bastola et al., 2013; Hartman et al., 2009; Hudon et al., 2010; Liu et al., 2013; Takagi et al., 2008; van Slegtenhorst et al., 2007). It is possible that in response to the suppression of mTORC1 signaling caused by FLCN loss, cells overdrive other pathways that more than compensate for mTORC1 inhibition. Indeed, in FLCN-null kidney tumors and cysts, as well as embryonic stem cells, the RasMAPK, Akt, and mTORC1 pathways all appear hyperactive (Baba et al., 2008; Cash et al., 2011; Chen et al., 2008; Hasumi et al., 2009), although this could reflect the proliferative state of the cells. Furthermore, in FLCN-null tumors there must be a mechanism to reactivate mTORC1, suggesting that there may be proteins that can compensate for FLCN loss. Candidates for such a role include C9orf72 and SMCR8, which have very little sequence homology with FLCN, but like it, are predicted to have DENN-like domains (Levine et al., 2013; Zhang et al., 2012). Lastly, it is likely that future studies will reveal that the FLCN-FNIP complex funnels so far unidentified regulatory signals to the Rag pathway so as to modulate amino acid sensing by mTORC1. 51 FIGURE 1: The RagC Nucleotide State Determines mTORC1 Binding to the Rag Heterodimer and Regulates Amino Acid Sensing by mTORC1 Input FLAG-raptor: RagC 01 20L: GTP hydrolysis mutant RagC S75N: low affinity for all nucleotides RagB 099L: GTP hydrolysis mutant RagB T54N: low affinity for all nucleotides transfected HA-ST-RagC: FLAG-RagB: cDNAs: FLAG-Rap2A: - W00120L - WT T54N +- - mTOR S75N WT 099L T54N WT S75N 0120L WT 099L WT pull-down: + 5 HA-GST-RagB + HA-RagC: NA-GST-Rap2A: in vitro binding + - + + + GST + bad fo l 1Ctd FLAG-raptOr assay ----- + + 5% C Rag Nucleotide Mutants + A HA-GST-RagBx AW HA-RagC HA-GST-RW2A raptor HA-GST-RagC HA-GST-Rap2A raptor HA-RagB + HA-RagB: HA-GST-Rap2A: + + GTP + - amino acida: FLAG-raptor in vitro binding I: -T389-S6K1 HA-GsT-RagC FLAG NA-GsT-Rap2A lysate FLAG-SOKI assay HA-GST-RagC HA-GsT-RagB HA-RagB 52 + R&g8 FLAG-S6K1 RagB + + RagB RagC RagCal"a RagC01? + "-+ GST + GTP XDP XTP & GOP _k - -- + + + + + transfected cDNAs: - FLAG-raptor: HA-GsT-RagC E + -+GDP HA-GST-RagC lysate pull-down: GST + FLAG-raptOr 4 mTOR 5% Input + - in vitro binding assay FLAG-Rap2A B pull-down: + + FLAG-raptOr: HA-GST-RagCx+ HA-RagB: HA-GsT-Rap2A: + 5% Input FLAG-RagB - IP: FLAG FIGURE 2: FLCN-FNIP2 is a Rag-interacting Complex and is Necessary for mTORC1 Activation by Amino Acids A B C ORMA: GFP FLCN1 transfectedt&*dl cDNA: M.sRA cells expressing* LG L* Ra s amino acids: - WWI" F - LN1FC_ + -+ FC R-gC 1p: FLAG - + " RaAFLCN IP: amino ackis: (9T3ag-4sK1 F!!1 + F FaaFMiLCA NAagO FLA-feta Ake RegANMA* lysale RsA111 FLCN 1006* R-gCO M" HA-FNIP2 -_j FLAG-MNP2 -yat pi -g 1"s _tm FA2,g FLA-tsp FLAG-ROPM4A E ShGPP antibody: mTOR -- LAMP2 dw6 F *hFLCN-2 mTOR LAMP2 EL antibody: ahGFP LAMP2 ShFLCN_2 LAMP2 flmTORar LAMP2 -A.&. for 0nin .yu T90d6 aL for LAMP2 &AL for TOR LAMP2 53 -Wmi LAMP2 "."aC FIGURE 3: FLCN Localizes to the Lysosomal Surface in an Amino Acid-Sensitive Fashion A C B shGFP antibody: -a.a. for 50min -a.a. for 50min +a.a. for 10min D DMSO antibody: *hFLCN_2 I I .CN LAMP2 merge FLCN LAMP2 merge Torin1 FL FLCN -a.a. for 50min I LAMP2 merge -a.a. for FLCN 50min LAMP2 +a.a. for merge 10min 54 FIGURE 4: FLCN-FNIP is a GTPase-Activating Protein Complex for RagC and RagD C RagBsO"-RagD A HA-FNIP1+ HA-FNIP2 8 B Rag8"-B-RagC Condition: buffer LAS FLCN GATORI FNIP2 FLCN Condition: buffer FNIPI LRS FLCN GATORI FFIP2 FLCN FNIP1 - transfected NA-GST-RagC: - WT W7 WT I -, RAG-RagS: - W. -IL 1, WT WI cDNAs: FLA-Rbp2A: + FLCN raptor a GDP GDP GTP GTP 0 PIS FLAG-RagS %GDP: 50,24 13,23 5., 17 000,0 %GDP: 201.S9 D 'LAG-fp2A reptor 400s am a M M4 Condition: buffer 1 52 3 FNIP2 FLCN FNi1 Rap2A Condition: buffer FLCN FNIP2 FLCN FMP1 GOP FLAo-RagB 087,*1 164,3 %GDP: 154,27 30 min 3.0% 84.5% 843% 5.6% 5,7% 3.8% 90 G Nueleotldes Loaded GTP, XDP GTP. XDP GTP, XTP GT, XDP GTP, XDP GTP. XDP - 0 -0'C..fafl H -tCF 5 in vitro binchng assay dao 030 20 20,07 36,06 FLAG-rapto: T s'o E 24,0 HA-as-Rap2A: FLAG-raptor W 6A-csT-RagD' HA-RagC HA-oST-Rap2AO 0 5 6 4 3 1 2 Molar Ptmio (Protein : RegEa'RagC) 55 7 '+ A4sT-wtagB' + HA-RagC: + 40,00 30 rain RagB--R8gC Condition Buffer only FLCN-FNIP2 FLCN-FNIP2 FLCN alone FNIP2 alone FLC~aN-trmn)-FNIP2 13,02 9 GTP - %GDP: FLAGO-fp2A 9, 9TP 9 C F GATOR FLCN 9 GOP HA-GST-RagC lysato LRS 36,0 21,01 E RagB-Ragca'4-x FLCN 6,14 30 min 30 nIn + FLAG # IIA.OST.RagC yPs M 0 4 -1,1 FIGURE LEGENDS Figure 1. The RagC Nucleotide State Determines mTORCI Binding to the Rag Heterodimer and Regulates Amino Acid Sensing by mTORC1 (A) Rag heterodimers containing RagCS75N co-immunoprecipitate the largest amount of endogenous mTORC1. Anti-FLAG immunoprecipitates were prepared from HEK-293T cells expressing the indicated cDNAs. Cell lysates and immunoprecipitates were analyzed by immunoblotting for the indicated proteins. (B) Raptor preferentially binds a GDP-loaded Rag heterodimer. In vitro binding assay in which recombinant HA-GST-tagged-RagB-RagC or -Rap2A were loaded with the indicated nucleotide and incubated with purified FLAG-tagged raptor protein. HA-GST precipitates were analyzed by immunoblotting for indicated proteins. Irrelevant lanes were removed and indicated by a dashed line. (C) Raptor only binds to the RagBX-C heterodimer when RagC is GDP-loaded. In vitro binding assay in which recombinant HA-GST-tagged-RagBX-RagC or -Rap2A were loaded with the indicated nucleotide and incubated with purified FLAG-tagged raptor protein and analyzed as in (B). (D) Raptor only binds to the RagB-CX heterodimer when RagCX is XDP-loaded. In vitro binding assay in which recombinant HA-GST-tagged-RagB-RagCx or -Rap2A were loaded with the indicated nucleotide and incubated with purified FLAG-tagged raptor protein and analyzed as in (B). (E) Expression of RagC S75N or RagCQ10IL renders the mTORC1 pathway insensitive to amino acid levels. HEK-293T cells expresssing the indicated cDNAs were analyzed as in (A). Irrelevant lanes were removed and indicated by a dashed line. Figure 2. FLCN-FNIP2 is a Rag-Interacting Complex and is Necessary for mTORCI Activation by Amino Acids 56 (A) Recombinant epitope-tagged FLCN-FNIP2 co-immunoprecipitates endogenous RagA and RagC. Anti-FLAG immunoprecipitates were prepared from HEK-293T cells expressing the indicated cDNAs in expression vectors and analyzed along with cell lysates by immunoblotting for indicated proteins. Irrelevant lanes were removed and indicated by a dashed line. (B) Amino acid starvation increases the amount of endogenous FLCN that co-immunoprecipitates with recombinant RagB. HEK-293T cells stably expressing FLAG-RagB were starved for amino acids for 50 min, or starved and stimulated with amino acids for 10 min. Anti-FLAG immunoprecipitates were analyzed as in (A). (C) FLCN is necessary for the activation of the mTORC1 pathway by amino acids. HEK-293T cells expressing a control shRNA or two distinct shRNAs targeting FLCN were starved for amino acids for 50 min, or starved and stimulated with amino acids for 10 min. Levels of indicated proteins and phosphorylation states were analyzed by immunobloting of cell lysates. (D) FLCN function is conserved in Drosophila cells. Drosophila S2 cells were transfected with a control dsRNA, or dsRNAs targeting dRagB, or dFLCN, starved of amino acids for 90 min, or starved and re-stimulated with amino acids for 30 min and analyzed as in (C). (E) Knockdown of FLCN prevents amino acid-induced translocation of mTOR to lysosomes. HEK-293T cells expressing the indicated shRNAs were starved or starved and re-stimulated with amino acids for the specified times before co-immunostaining for mTOR (red) and LAMP2 (green). (F) FLCN is not required for the lysosomal localization of RagC. HEK-293T cells expressing the indicated shRNAs were treated and processed as described in (E). In all images, insets show selected fields that were magnified two times and their overlays. Scale bars represent 10 pm. See also Figure S1. Figure 3. FLCN Localizes to the Lysosomal Surface in an Amino Acid-Sensitive Fashion 57 (A) FLCN localizes to the lysosomal surface. Spinning disk confocal image of a HEK-293T cell co-expressing FLCN-GFP, HA-FNIP2, and mRFP-LAMP1 (pseudo-colored red and green in merge, respectively). (B) FLCN associates with lysosomes as they traffic within cells. Time-lapse of FLCN- and LAMP1-positive lysosomes from the boxed region in (A) magnified by 2.5 times. Time intervals are in seconds. (C) FLCN localizes to the lysosomal surface upon amino acid starvation. HEK-293T cells expressing the indicated shRNAs were starved or starved and re-stimulated with amino acids for the specified times before co-immunostaining for FLCN (red) and LAMP2 (green). (D) Amino acid-sensitive localization of FLCN is independent of mTORC1 activity. HEK-293T cells treated with DMSO or Torin1 (250 nM) were starved or starved and re-stimulated with amino acids for the specified times before co-immunostaining for FLCN (red) and LAMP2 (green). In (C) and (D), insets show selected fields that were magnified two times and their overlays. All scale bars represent 10 pm. See also Figure S2. Figure 4. FLCN-FNIP is a GTPase-Activating Protein Complex for RagC and RagD (A) Rag heterodimers containing RagB T54N, but not RagCS75N, co-immunoprecipitate endogenous FLCN. Anti-FLAG immunoprecipitates were prepared from HEK-293T cells transfected with indicated cDNAs in expression vectors. Cell lysates and immunoprecipitates were analyzed by immunoblotting of indicated proteins. (B) FLCN-FNIP stimulates GTP hydrolysis by RagC. 5 pmol of RagB Q 99L-X-RagC was loaded with [a- P]GTP and incubated with indicated proteins (20 pmol). GTP hydrolysis was determined by thin-layer chromatography (see Experimental Procedures). Each value represents the mean SD (n=3). (C) FLCN-FNIP stimulates GTP hydrolysis by RagD. GAP assay was performed with RagB Q9L-X_ RagD as described in (B). 58 (D) GATOR1, but not FLCN-FNIP1/2, stimulates GTP hydrolysis by RagB. GAP assay was performed with RagB-RagCQ - as described in (B). (E) FLCN-FNIP does not stimulate GTP hydrolysis by Rap2A. GAP assay was performed with the Rap2A control GTPase as described in (B). (F) Nucleotide state of RagB does not affect FLCN-FNIP2 GAP activity towards RagC, FLCNFNIP2 complex is required for GAP activity, and N-terminal region of FLCN is required for GAP activity. GAP assays were performed as described in (B) with 10 min incubations of indicated proteins. Values represent an average from at least 2 experiments. (G) FLCN-FNIP2 stimulates GTP hydrolysis by RagC in a dose-dependent manner. GAP assay was performed as described in (B) with indicated molar ratios of FLCN-FNIP2 or control metap2 to RagBx-RagC. (H) In vitro, the FLCN-FNIP2 GAP activity is sufficient to cause raptor to bind to the Rags. In vitro binding assay in which recombinant HA-GST-tagged-RagBX-RagC or -Rap2A were loaded with the indicated nucleotide and incubated with purified FLAG-tagged raptor along with FLCN-FNIP2 or metap2 control protein. HA-GST precipitates were analyzed by immunoblotting for indicated proteins. See also Figure S3. 59 EXPERIMENTAL PROCEDURES Cell Lysis and Immunoprecipitation HEK-293T cells were rinsed once with ice-cold PBS and lysed with Triton lysis buffer (1% Triton X-100, 10 mM P-glycerol phosphate, 10 mM pyrophosphate, 40 mM Hepes pH 7.4, 2.5 mM MgCl 2 and 1 tablet of EDTA-free protease inhibitor (per 25 ml)). When amino acid-sensitive interactions were interrogated, cells were lysed in CHAPS lysis buffer (0.3% CHAPS, 10 mM P-glycerol phosphate, 10 mM pyrophosphate, 40 mM Hepes pH 7.4, 2.5 mM MgCl 2 and 1 tablet of EDTA-free protease inhibitor (per 25 ml)). The soluble fractions of cell lysates were isolated by centrifugation at 13,000 rpm in a refrigerated microcentrifuge for 10 minutes. For anti-FLAG-immunoprecipitations, the FLAG-M2 affinity gel was washed with lysis buffer 3 times and 50 [d of a 50% slurry of the affinity gel was then added to cleared cell lysates and incubated with rotation for 3 hours at 4 0C. The beads were washed 3 times with lysis buffer containing 150 mM NaCl. Immunoprecipitated proteins were denatured by the addition of 50 d of sample buffer and boiling for 5 minutes as described (Kim et al., 2002), resolved by 8%-16% SDSPAGE, and analyzed by immunoblotting. For co-transfection experiments, 2,000,000 HEK-293T cells were plated in 10 cm culture dishes. Twenty-four hours later, cells were transfected using XtremeGene 9 transection reagent with the pRK5-based cDNA expression plasmids indicated in the Figures in the following amounts: 100 ng HA-RagB; 100 ng HA- or HA-GST-RagC; 300 ng HA-GST-RagBQ 99 Lor 300 ng HA-GST-RagBT 5 4 N; 300 ng HA-GST-RagCS 7 5 Nor 300 ng HA-GST-RagCQ12 0L; 100 ng FLAG-Rap2A; 300 ng of FLAG-metap2, 300 ng of FLAG- FLCN, 300 ng of HA- or FLAG-FNIP2, and 5 ng Flag-S6K. The total amount of plasmid 60 DNA in each transfection was normalized to 2 pg with empty pRK5. Thirty-six hours after transfection, cells were lysed as described above. Amino acid Starvation of Cells HEK-293T cells in culture dishes or coated glass cover slips were rinsed with and incubated in amino acid-free RPMI for 50 minutes and stimulated with amino acids for 10-15 minutes. After stimulation, the final concentration of amino acids in the media was the same as in RPMI. A 1OX amino acid mixture used to stimulate cells, which was prepared from individual powders of amino acids. When Torin1 was used, cells were incubated with 250 nM of Torin1 or DMSO during the 50 minute starvation period and the 10 minute stimulation period. RNAi in Mammalian Cells Lentiviral shRNAs targeting FLCN and non-targeting controls (Sancak et al., 2008) were obtained from the TRC. The TRC number for each shRNA is as follows: Human FLCN shRNA_1: TRCN0000237882 Human FLCN shRNA_2: TRCN0000237885 shRNA-encoding plasmids were co-transfected with the Delta VPR envelope and CMV VSV-G packaging plasmids into actively growing HEK-293T cells using XtremeGene 9 transfection reagent as previously described (Sarbassov et al., 2005). Virus-containing supernatants were collected 48 hours after transfection and passed through a 0.45 um filter to eliminate cells. Target cells were infected in the presence of 8 pg/ml polybrene. 24 hours later, cells were selected with puromycin and analyzed on the 3 rd day after selection. Immunofluorescence Assays 61 Immunofluorescence assays were performed as described in (Sancak et al., 2010). Briefly, 400,000 of the indicated HEK-293T cells were seeded on fibronectincoated glass coverslips in 6-well tissue culture plates. Twenty-four hours later, the slides were starved or stimulated with amino acids as described above and fixed for 15 min with 4% paraformaldehyde in PBS at room temperature. The slides were rinsed twice with PBS and cells were permeabilized with 0.05% Triton X-100 in PBS for 5 min. After rinsing twice with PBS, the slides were incubated with primary antibody in 5% normal donkey serum for 1 hr at room temperature, rinsed four times with PBS, and incubated with secondary antibodies produced in donkey (diluted 1:400 in 5% normal donkey serum) for 40 min at room temperature and washed four times with PBS. Slides were mounted on glass coverslips using Vectashield containing DAPI (Vector Laboratories) and imaged on a spinning disk confocal system (Perkin Elmer). Live Cell Imaging 300,000 HEK-293T cells were seeded on fibronectin-coated glass bottom 35 mm dishes (MatTek Corp.). The next day, cells were co-transfected using XtremeGene 9 with the following plasmids: 90 ng FLCN-GFP (Clontech), 10 ng HA-FNIP2, 100 ng mRFP-LAMP1, 300 ng empty pRK5. The following day, cells were imaged on a spinning disk confocal microscope (Andor Technology) with a 488-nm and a 568-nm laser through a 60x objective. Purification of Recombinant Proteins for GAP and In Vitro Binding Assays To produce protein complexes used for GAP assays, 4,000,000 HEK-293T cells were plated in 15 cm culture dishes. Forty-eight hours later, cells were transfected with the following combination of constructs (all cDNAs were expressed from the pRK5 expression plasmid). For RagB-RagCQ120L-X: 16 pg HA-RagB and 8 pg Flag-RagCQ120L- 62 D181N; for RagBQ 99L-X-RagC: 8 pg FLAG-RagBQ 9 9 L-D1 6 3 Nand 16 pg HA-RagC; for RagBQ 9 9 L- X-RagD: 8 pg FLAG-RagBQ 99L-D 63 N and 16 pg HA-RagD; for RagBX-RagC: 8 pg FLAG- RagBD1 6 3 N and 16 pg HA-RagC. For Rags used in in-vitro binding: 8 pg HA-GSTRagBD1 6 3 N and 16 pg HA-RagC; 8 pg HA-GST-RagCD1 8 1N and 16 pg HA-RagB; 8 pg HAGST-RagC and 16 pg HA-RagB; GATOR1: 4 pg FLAG-DEPDC5 and 8 pg myc-NPRL2 and 8 pg myc-NPRL3 (Bar-Peled et al., 2013); FLCN-FNIP1: 8 pg FLAG-FNIP1 and 16 pg HA-FLCN; FLCN-FNIP2: 8 pg FLAG-FNIP2 and 16 pg HA-FLCN; FLCN(AN-term)FNIP2: 8 pg FLAG-FNIP2 and 16 pg HA-FLCN(AN-term) (Nookala et al., 2012). For FLCN-FNIP purifications, it is crucial to immunoprecipitate through the FNIP component to obtain stoichiometric complexes with high activities. For individual proteins: 10 pg Flag- or HA-GST-Rap2A, 15 pg of FLAG-Leucyl tRNA synthetase (LRS), or 10 pg FlagMetap2, 16 pg FLAG-FLCN, 16 pg FLAG-FNIP2. Thirty-six hours post transfection cell lysates were prepared as described above, with the exception that for all FLCN or FNIP containing purifications, EDTA-free protease inhibitor tablet was added to prevent degradation and for all GATOR purifications cells were lysed in 0.3% CHAPS buffer without MgC 2 . 200 pl of a 50% slurry of FLAG-M2 affinity gel or immobilized glutathione beads were added to lysates from cells expressing FLAG-tagged proteins or HA-GST tagged proteins, respectively. Recombinant proteins were immunoprecipitated for 3 hours at 4*C. Each sample was washed once with Triton lysis buffer, followed by 3 washes with Triton lysis buffer supplemented with 500 mM NaCl and finally, 4 washes with the CHAPS buffer. FLCN-FNIP complexes were rotated at 40C in the last Triton salt wash for 30 minutes for a cleaner purification. FLAG-tagged proteins were eluted from the FLAG-M2 affinity gel with a competing FLAG peptide for 1 hour as described above. All proteins were stored in CHAPS buffer supplemented with 10% glycerol, snap frozen with liquid nitrogen and stored at -80*C. 63 To remove the FLAG peptide, proteins were subsequently purified on a HiLoad 16/60 Superdex 200 FPLC column (GE) pre-equilibrated with CHAPS buffer supplemented with 150 mM salt. For FLCN-FNIP purifications, 4 protease inhibitor tablets were supplemented per 400mL of CHAPS buffer. The peak corresponding to the desired complex was concentrated in 10,000 MW CO columns (Amicon), snap frozen in CHAPS buffer supplemented with 10% glycerol and stored at -800 C. All proteins were verified by Coomasie staining on a 4-16% gel. Rag GTP Hydrolysis Assays GAP assays were performed essentially as described in (Bar-Peled et al., 2013). In brief, the indicated GTPases were bound at 40C to FLAG-M2 affinity gel. The resin was then washed to remove unbound protein, and the GTPases were loaded with XDP (or XTP where indicated) and [a- 3 2 P]GTP at room temperature followed by an incubation with MgC 2 to stabilize the nucleotide. The GTPases were subsequently washed to remove unbound nucleotide and eluted from the affinity gel with competing FLAG peptide. Protein concentrations were determined prior to use. For the TLC-based GTP hydrolysis assay, 5 pmoles of the indicated Rag heterodimer or Rap2a loaded with xanthine nucleotides and [a- 32 P]GTP were added to 20 pmoles of purified LRS, GATOR1, or FLCN-FNIP in 45 pl of GTPase wash buffer. The reaction was incubated at 250C for the indicated times and eluted samples were spotted on PEI Cellulose plates and developed for 2.5 hours in 0.5 M KH 2PO 4 pH 3.4. Plates were exposed to film and spot densities were quantified with ImageJ. ACKNOWLEDGEMENTS We thank Shuyu Wang, Larry Schweitzer, Mounir Koussa, Molly Plovanich, and Rich Possemato for critical review of the manuscript and all members of the Sabatini Lab 64 for helpful suggestions. This work was supported by grants from NIH (CA103866 and A147389) and Department of Defense (W81XWH-07-0448) to D.M.S., fellowship support from the NCI (F30CA180754) to Z.T., David H. Koch Graduate Fellowship Fund to L.B.P., National Science Foundation to L.C. and T.W., Jane Coffin Childs Memorial Fund for Medical Research to R.Z., and support from Howard Hughes Medical Institute (HHMI) to C.K. D.M.S. is an investigator of the HHMI. 65 REFERENCES Baba, M., Furihata, M., Hong, S.-B., Tessarollo, L., Haines, D.C., Southon, E., Patel, V., Igarashi, P., Alvord, W.G., Leighty, R., et a/. (2008). Kidney-targeted Birt-Hogg-Dube gene inactivation in a mouse model: Erkl/2 and Akt-mTOR activation, cell hyperproliferation, and polycystic kidneys. J Natl Cancer 1 100, 140-154. 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Nat Rev Mol Cell Bio 12, 21-35. 71 Supplemental Info A Homozygous co-ftness Interactions Top 10 InleracMora wtth GTRI by homozgous co-senilvIty: Qoq ry Ti at rrewo" 1 .78085 .74338 TRI _____ Enriched O Wrma .r kerucare _ ___ TRI .71567 * .54758 A3379 A203 1 TR1 * aulaphay (2e-03) Funcoon: SNone ______ ________.3833 .37561 9_ _QM _ Wo lasma membane transoort Component 1036 * vacuolar membrane (4e-041 # vacuolar membrane (sensu Funal) * vatoe M6-031 Figure S1, related to Figure 2. Yeast orthologs of FLCN and Rag GTPases have similar growth sensitivities (A) Top 10 interactors with GTR1 (Yeast RagA/B ortholog) include GTR2 (Yeast RagC/D ortholog) and LST7 (Yeast FLCN ortholog) in terms of growth sensitivities to various environmental and chemical insults. Output from querying "GTR1" at: http://chemogenomics.stanford.edu/supplements/cofitness/index.html (Hillenmeyer et al., 2008) 72 A Figure S2, related to Figure 3. FLCN requires FNIP2 to localize to the lysosomal surface (A) Spinning disk confocal image of a HEK-293T cell co-expressing FLCN-GFP and mRFP-LAMP1 (pseudo-colored red and green in merge, respectively). A B RagB-RagCx C RagBx-R8gC 0 7 RagB-RagC -_ V0 7L W 0. metap2 a- Ragulator FL N-FNIP2 7 00 0 2iX 21 2672 0 D 10 4 8 12 i 0m Time (min) Time (mn) RagBx-RagC E 0 12 4 8 12 Time (min) free GTP 8 aw metap2 - Condition: FLCN-FNIP2 buffer FLCN FNIP2 2 0 GDP 10 20 Time (min) 30 GTP % GDP: 0.5 30 min Figure S3, related to Figure 4. FLCN-FNIP2 does not have GEF activity towards the Rag GTPases, FLCN-FNIP2 stimulates RagC GTPase activity in a time-dependent 73 manner, and purified FLCN-FNIP2 does not contain significant contaminating phosphatases (A) FLCN-FNIP2 does not stimulate GDP dissociation from RagB. Dissociation assay in which RagB-RagCx was loaded with [ 3H]GDP, and incubated with FLCN-FNIP2, Ragulator positive control, or metap2 control protein. Dissociation was monitored by a filter-binding assay. Each value represents the average of a replicate. (B) FLCN-FNIP2 does not stimulate GDP dissociation from RagC. Dissociation assay with RagBX-RagC was performed as described in (A). (C) FLCN-FNIP2 does not stimulate GDP dissociation from wild-type RagB-RagC. Dissociation assay with RagB-RagC was performed as described in (A). (D) FLCN-FNIP2 stimulates GTP hydrolysis by RagC in a time-dependent manner. 5 pmol of RagBX-RagC was loaded with [a- 32P]GTP and incubated with indicated proteins (20 pmol) for indicated times. GTP hydrolysis was determined by thin-layer chromatography. Each value represents the average of two experiments. (E) Purified FLCN-FNIP2 does not contain significant amounts of contaminating phosphatases. The purified FLCN-FNIP2 used in Figure 4 was incubated with free [a32 P]GTP. This amount of hydrolysis is representative of separate FLCN-FNIP2 purifications. Value represents the quantification in the incubation shown. Supplemental Experimental Procedures Materials Reagents were obtained from the following sources: HRP-labeled anti-mouse and anti-rabbit secondary antibodies and LAMP2 antibody from Santa Cruz Biotechnology; antibodies to phospho-T389 S6K1, S6K1, phospho-S473-Akt, Akt, phospho-T398 dS6K, RagA, RagC, p18, mTOR, FLCN, and the FLAG epitope from Cell 74 Signaling Technology; antibodies to the HA epitope from Bethyl laboratories; antibodies to raptor from Millipore. RPMI, FLAG M2 affinity gel, ATP, GDP, and amino acids were from Sigma Aldrich; DMEM from SAFC Biosciences; XtremeGene9 and Complete Protease Cocktail from Roche; Alexa 488 and 568-conjugated secondary antibodies, Schneider's media, Express Five-SFM, and Inactivated Fetal Calf Serum (IFS) from Invitrogen; amino acid-free RPMI, and amino acid-free Schneider's media from US Biological; Cellulose PEI TLC plates from Sorbent Technologies; [a- 32P]GTP from Perkin Elmer; GTP, XTP and XDP from Jena Biosciences; nitrocellulose membrane filters from Advantec; DSP and Glutathione beads from Pierce. Torin1 from Dr. Nathanael Gray (DFCI). The dS6K antibody was a generous gift from Mary Stewart (North Dakota State University). Identification of FLCN, FNIP1, and FNIP2 as Rag-interacting proteins HEK-293T cells stably expressing FLAG-tagged metap2, RagA, RagB, RagC or RagD were subjected to FLAG-immunoprecipitation as described above. Proteins were eluted with the FLAG peptide (sequence DYKDDDDK) from the FLAG-M2 affinity gel, resolved on 4-12% NuPage gels (Invitrogen), and stained with simply blue stain (Invitrogen). Each gel lane was sliced into 10-12 pieces and the proteins in each gel slice digested overnight with trypsin. The resulting digests were analyzed by mass spectrometry as described (Sancak et al., 2008). Peptides corresponding to FLCN and FNIP1 and FNIP2 were detected in the FLAG-RagA, -B, -C, and -D immunoprecipitates, while no such peptides were detected in negative control immunoprecipitates of FLAGmetap2. 75 RNAi in Drosophila S2 cells dsRNAs against Drosophila FLCN were designed as described in (Sancak et al., 2008). Primer sequences used to amplify DNA templates for dsRNA synthesis for dFLCN including underlined 5' and 3' T7 promoter sequences, are as follows: dFLCN (CG8616) Forward primer CG8616_1F: GAATTAATACGACTCACTATAGGGAGA AGAATAACAATGCGATCTACAGCAG Reverse primer CG8616_1R: GAATTAATACGACTCACTATAGGGAGA GAAGGTGTGACTCAGGATGTGA Forward primer CG8616_2F: GAATTAATACGACTCACTATAGGGAGA GTACAAAATCATATCCGTGTCCAAT Reverse primer CG8616_2R: GAATTAATACGACTCACTATAGGGAGA GAAGGTGTGTGCTCCAGTAGTTAAT dsRNAs targeting GFP and dRagB (Sancak et al., 2008) were used as negative and positive controls, respectively. On day one, 4,000,000 S2 cells were plated in 6-cm culture dishes in 4 ml of Express Five SFM media. Cells were transfected with 1 pg of dsRNA per million cells using XtremeGene9. Two days later, a second round of dsRNA transfection was performed. On day four, cells were transferred to a fibronectin coated 6cm culture dish. On day five, cells were rinsed once with amino acid-free Schneider's medium, and starved for amino acids by replacing the media with amino acid-free Schneider's medium for 1.5 hours. To stimulate with amino acids, the amino acid-free medium was replaced with complete Schneider's medium for 30 minutes. Cells were then washed with ice cold PBS, lysed in Triton lysis buffer, and subjected to immunoblotting for phospho-T398 dS6K and total dS6K. 76 In Vitro Binding Assays For the binding reactions, 20 pl of a 50% slurry containing immobilized HA-GSTtagged proteins were incubated in binding buffer (0.3% CHAPS, 2.5 mM MgC 2, 40 mM HEPES [pH 7.4], 2 mM DTT, and 1 mg/ml BSA) with 2 pg of FLAG-raptor, FLAGmetap2, or FLAG-FNIP2-HA-FLCN in a total volume of 50 pl for 1 hr and 30 min at 40C. Where indicated, Rags were loaded with the indicated nucleotides as previously described (Bar-Peled et al., 2012). To terminate binding assays, samples were washed twice times with 1 mL of ice-cold binding buffer supplemented with 150 mM NaCl followed by the addition of 50 pl of sample buffer. Nucleotide Exchange Assays GEF assays were performed as described in (Bar-Peled et al., 2012). Briefly, the indicated purified Rag GTPases were loaded with XTPyS and [ 3 H]GTP at room temperature followed by an incubation with MgCl 2 to stabilize the nucleotide. To initiate GEF assay, purified FLCN-FNIP2, Ragulator, or metap2 proteins were added to Rags along with GTPyS. Samples were taken every 2 minutes and spotted on nitrocellulose filters, which were washed. Filter-associated radioactivity was measured using a TriCarb scintillation counter (PerkinElmer). Supplemental References Bar-Peled, L., Schweitzer, L.D., Zoncu, R., and Sabatini, D.M. (2012). Ragulator is a GEF for the rag GTPases that signal amino acid levels to mTORC1. Cell 150, 11961208. Hillenmeyer, M.E., Fung, E., Wildenhain, J., Pierce, S.E., Hoon, S., Lee, W., Proctor, M., St Onge, R.P., Tyers, M., Koller, D., et al. (2008). The chemical genomic portrait of yeast: Uncovering a phenotype for all genes. Science 320, 362-365. Sancak, Y., Peterson, T.R., Shaul, Y.D., Lindquist, R.A., Thoreen, C.C., Bar-Peled, L., and Sabatini, D.M. (2008). The Rag GTPases bind raptor and mediate amino acid signaling to mTORC1. Science 320,1496-1501. 77 CHAPTER 3 Reprinted from Science Magazine: Lysosomal amino acid transporter SLC38A9 signals arginine sufficiency to mTORC1 Shuyu Wang ,2,3,4,*, Zhi-Yang Tsun 1,2,3,4,*, Rachel Wolfson 1,2,3,4, Kuang Shen 1,2,3,4, Gregory A. 1234 2,3,4 12,34 Wyant1 ,Molly E. Plovanich , Elizabeth D. Yuan', Tony D. Jones,' , Lynne Chantranupong12, 4, William Comb 1,2,3,4, Tim Wang 1,2,3,4, Liron Bar-Peled1,2,3,4 t, Roberto Zoncu1 2,3,4:, Christoph Straub , Choah Kim 1,2,3,4, Jiwon Park 1,2,3,4, Bernardo L. Sabatini , and David M. Sabatini',2,3,4 Whitehead Institute for Biomedical Research and Massachusetts Institute of Technology, Department of Biology, 9 Cambridge Center, Cambridge, MA 02142, USA Howard Hughes Medical Institute, Department of Biology, Massachusetts Institute of I fTechnology, Cambridge, MA 02139, USA Koch Institute for Integrative Cancer Research, 77 Massachusetts Avenue, Cambridge, MA 02139, USA 4Broad Institute of Harvard and Massachusetts Institute of Technology, 7 Cambridge Center, Cambridge MA 02142, USA Department of Neurobiology, Howard Hughes Medical Institute, Harvard Medical School, 220 Longwood Avenue, Boston, MA 02115, USA 6 Harvard Medical School, 260 Longwood Avenue, Boston, MA 02115, USA *These authors contributed equally to this work tPresent address: Department of Chemical Physiology, The Scripps Research Institute, La Jolla, CA 92037, USA tPresent address: Department of Molecular and Cell Biology, University of California Berkeley, Berkeley, CA 94720, USA Correspondence should be addressed to D.M.S. Tel: 617-258-6407; Fax: 617-452-3566; Email: sabatinicwi.mit.edu Experiments in Figure 1A were performed by LBP. Experiments in Figure 1B were performed by SW. Experiments in Figure IC were performed by ZYT. Experiments in Figures 1D were performed by SW using reagents generated by ZYT. Experiments in Figures 1E, 1F were performed by RW. Experiments in Figure 2A were performed by ZYT. Experiments in Figures 2B were performed by LC and TW. Experiments in Figures 3A-B, 3D-3F were performed by SW using reagents generated by ZYT. Experiments in Figure 3C were performed by SW using reagents generated by RW. Experiments in Figures 4A, 4C were performed by SW. Experiments in Figures 4B were performed by ZYT. Experiments in Figures 5A, 5C, 5D were performed by ZYT. Experiments in Figures 5B were performed by ZYT under guidance of KS. Experiments in Figures 5E, 5F were performed by GAW. Experiments in Figures S1A, S3A S3B, S6A-D, S6F-G were performed by ZYT. Experiments in Figure S4A, S4B, S4D, S4E, S5 were performed by SW. Experiments in Figures S2, S4C were performed by SW using reagents generated by ZYT. Experiments in Figure S3C were performed by KS. Experiments in Figure S3D were performed by WC. Experiments in Figure S6E were performed by CS. Experiments in Figure S61 were performed by ZYT and EDY under guidance of MEP. 78 SUMMARY: The mTOR complex 1 (mTORC1) protein kinase is a master growth regulator that responds to multiple environmental cues. Amino acids stimulate, in a Rag-, Ragulator-, and v-ATPase-dependent fashion, the translocation of mTORC1 to the lysosomal surface, where it interacts with its activator Rheb. Here, we identify SLC38A9, an uncharacterized protein with sequence similarity to amino acid transporters, as a lysosomal transmembrane protein that interacts with the Rag GTPases and Ragulator in an amino acid-sensitive fashion. SLC38A9 transports arginine with a high Km and loss of SLC38A9 represses mTORC1 activation by amino acids, particularly arginine. Overexpression of SLC38A9 or just its Ragulator-binding domain makes mTORC1 signaling insensitive to amino acid starvation but not to Rag activity. Thus, SLC38A9 functions upstream of the Rag GTPases and is an excellent candidate for being an arginine sensor for the mTORC1 pathway. amino acids cytosol SLC38A9 lysosomal membrane I lysosomal lumen arginine 79 INTRODUCTION: The mechanistic target of rapamycin complex 1 (mTORC1) protein kinase is a central controller of growth that responds to the nutritional status of the organism and is deregulated in several diseases, including cancer (1-3). Upon activation, mTORC1 promotes anabolic processes, including protein and lipid synthesis, and inhibits catabolic ones, such as autophagy (4). Environmental cues such as nutrients and growth factors regulate mTORC1, but how it senses and integrates these diverse inputs is unclear. The Rag and Rheb GTPases have essential but distinct roles in mTORC1 pathway activation, with the Rags controlling the subcellular localization of mTORC1 and Rheb stimulating its kinase activity (5). Nutrients, particularly amino acids, activate the Rag GTPases, which then recruit mTORC1 to the lysosomal surface where they are concentrated (6, 7). Rheb also localizes to the lysosomal surface (6, 8-10) and, upon growth factor withdrawal, the tuberous sclerosis complex (TSC) tumor suppressor translocates there and inhibits mTORC1 by promoting GTP hydrolysis by Rheb (10). Thus, the Rag and Rheb inputs converge at the lysosome, forming two halves of a coincidence detector that ensures that mTORC1 activation occurs only when both are active. There are four Rag GTPases in mammals and they form stable, obligate heterodimers consisting of RagA or RagB with RagC or RagD. RagA and RagB are highly similar and functionally redundant, as are RagC and RagD (1, 6). The function of each Rag within the heterodimer is poorly understood and their regulation is likely complex as many distinct factors play important roles. A lysosome-associated molecular machine containing the multi-subunit Ragulator and vacuolar ATPase (v-ATPase) complexes regulates the Rag GTPases and is necessary for mTORC1 activation by amino acids (11). Ragulator anchors the Rag GTPases to the lysosome and also has nucleotide exchange activity for RagA/B (12, 13), but the molecular function of the vATPase in the pathway is unknown. Two GTPase activating protein (GAP) complexes, which are both tumor suppressors, promote GTP hydrolysis by the Rag GTPases, with GATOR1 acting on RagA/B (14) and Folliculin-FNIP2 on RagC/D (15). Lastly, a distinct complex called GATOR2 negatively regulates GATOR1 through an unknown 80 mechanism (14). Despite the identification of many proteins involved in signaling amino acid sufficiency to mTORC1, the actual amino acid sensors remain unknown. RESULTS: SLC38A9 Interacts with Ragulator and the Rag GTPases We have proposed that amino acid sensing initiates at the lysosome and requires the presence of amino acids in the lysosomal lumen (11). Thus, we sought to identify, as candidate sensors, proteins that interact with known components of the pathway and also have transmembrane domains. Mass spectrometric analyses of non-heated immunoprecipitates of several Ragulator components and, to a lesser extent, RagB, revealed the presence of isoform 1 of SLC38A9 (SLC38A9.1), a previously unstudied protein with sequence similarity to the SLC38 class of sodium-coupled amino acid transporters (16) (Fig. 1A). SLC38A9.1 is predicted to have eleven transmembrane domains, a cytosolic N-terminal region of 119 amino acids, and three N-linked glycosylation sites in the luminal loop between transmembrane domains 3 and 4 (Fig. 1B and fig. S1, A and B). When stably expressed in human embryonic kidney (HEK)-293T cells, SLC38A9.1 migrated on SDS-PAGE as a smear that collapsed to near its predicted molecular weight of 63.8 kDa after treatment with Peptide-N-Glycosidase F (PNGase F) (Fig. 1C). Isoforms 2 (SLC38A9.2) and 4 (SLC38A9.4) lack the first 63 or 124 amino acids of SLC38A9.1, respectively (Fig. 1B). As expected from the mass spectrometry results, immunoprecipitates of stably expressed FLAG-tagged SLC38A9.1, but not of three other lysosomal membrane proteins -LAMP1 (17), SLC36A1 (18), and SLC38A7 (19) - contained Ragulator (as detected by its p14 and p18 components), RagA, and RagC (Fig. 1D and fig. S2A). Indicative of the strength of the Ragulator-SLC38A9.1 interaction, the amounts of endogenous Ragulator that coimmunoprecipitated with SLC38A9.1 were similar to those associated with the RagB-RagC heterodimer (Fig. 1 D). In contrast, SLC38A9.2, SLC38A9.4 or a mutant of SLC38A9.1 lacking its first 110 amino acids (SLC38A9.1 Al 10) did not associate with Ragulator (fig. S2, B and C). The N-terminal region of SLC38A9.1 is sufficient for it to interact with Ragulator-Rag because on its own the first 119 amino acids of SLC38A9.1 coimmunoprecipitated similar amounts of Ragulator and Rag GTPases as did the full-length protein (Fig. 1 D and fig. S2C). Using alanine 81 scanning mutagenesis of residues in the N-terminal region conserved to the SLC38A9.1 homolog in C. elegans (F13H10.3), we identified 168, Y71, L74, P85, and P90 as required for the Ragulator-SLC38A9.1 interaction (Fig. 1E). The v-ATPase and its activity are necessary for amino acid sensing by the mTORC1 pathway and, like SLC38A9.1, it coimmunoprecipitated with stably expressed FLAG-tagged Ragulator (11, 20, 21). Indicating the existence of a supercomplex, stably expressed SLC38A9.1, but not LAMP1, associated with endogenous components of the v-ATPase in addition to Ragulator and the Rag GTPases (Fig. 1 F). Although SLC38A9.2 does not interact with Ragulator, it did co-immunoprecipitate the v-ATPase, albeit at lesser amounts than SLC38A9.1 (Fig. 1F). This suggests that the interaction between SLC38A9.1 and the v-ATPase is not mediated through Ragulator but directly or indirectly through the region of SLC38A9.1 that contains its transmembrane domains. Concordant with this interpretation, the N-terminal domain of SLC38A9.1, which interacts strongly with Ragulator, did not coimmunoprecipitate the v-ATPase (Fig. 1 F). SLC38A9 is a Lysosomal Membrane Protein Required for mTORC1 Activation Well-characterized members of the SLC38 family of amino acid transporters (SLC38A1-5) localize to the plasma membrane (22) but at least one member, SLC38A7, is a lysosomal membrane protein (19). This is also the case for SLC38A9.1, SLC38A9.2, and SLC38A9.4 as in HEK-293T cells all three isoforms co-localized with LAMP2, an established lysosomal membrane protein (Fig. 2A and fig. S3, A and B). Amino acids did not affect the lysosomal localization of SLC38A9.1 (Fig. 2A). As would be expected if SLC38A9.1 binds to Ragulator at the lysosome, a Ragulator mutant that does not localize to the lysosomal surface because its p18 component lacks lipidation sites (23) did not interact with SLC38A9.1 (fig. S3C). ShRNA- or siRNA-mediated depletion of SLC38A9 in HEK-293T cells suppressed activation of mTORC1 by amino acids, as detected by the phosphorylation of its established substrate ribosomal protein S6 Kinase 1 (S6K1) (Fig. 2B and fig. S3D). Thus, like the five known subunits of Ragulator (12, 13), SLC38A9.1 is a positive component of the mTORC1 pathway. We conclude that SLC38A9.1 is a lysosomal membrane protein that interacts with Ragulator and the Rag GTPases through its Nterminal 119 amino acids ('Ragulator-binding domain') and is required for mTORC1 activation. 82 SLC38A9.1 Overexpression Makes mTORC1 Signaling Insensitive to Amino Acids Given the similarity of SLC38A9.1 to amino acid transporters, we reasoned that it might act in conveying amino acid sufficiency to Ragulator and the Rag GTPases. In accord with this expectation, stable or transient overexpression in HEK-293T cells of SLC38A9.1, but not of several control proteins, rendered mTORC1 signaling resistant to total amino acid starvation or to just that of leucine or arginine, two amino acids that regulate mTORC1 activity in many cell types (24-26) (Fig. 3A and fig. S4A). Overexpression of SLC38A9.1 did not affect the regulation of mTORC1 by growth factor signaling (fig. S4, D and E). Commensurate with its effects on mTORC1, SLC38A9.1 overexpression suppressed the induction of autophagy caused by amino acid starvation (fig. S4C), a phenotype shared with activated alleles of RagA and RagB (6, 7, 28). Overexpression of variants of SLC38A9 that do not interact with Ragulator and the Rag GTPases, including SLC38A9.2, SLC38A9.4, and the SLC38A9.1 Al10 and SLC38A9.1 168A mutants, failed to maintain mTORC1 signaling after amino acid withdrawal (Fig. 3, B and C, and fig. S4A). Thus, even in cells deprived of amino acids, some of the overexpressed SLC38A9.1 protein appears to be in an active conformation that confers amino acid insensitivity on mTORC1 signaling in a manner dependent on its capacity to bind Ragulator and Rags. SLC38A9.1 overexpression also activated mTORC1 in the absence of amino acids in HEK-293E, HeLa, and LN229 cells, as well as in mouse embryonic fibroblasts (MEFs), with the degree of activation proportionate to the amount of SLC38A9.1 expressed (fig. S4B). Interestingly, overexpression of just the Ragulatorbinding domain of SLC38A9.1 mimicked the effects of the full-length protein on mTORC1 signaling (Fig. 3D), indicating that it can adopt an active state when separated from the transmembrane portion of SLC38A9.1. The gain of function phenotype caused by SLC38A9.1 overexpression offered an opportunity to test its relation to the Rag GTPases, mTORC1, and the v-ATPase. The Rag GTPases and mTORC1 both clearly function downstream of SLC38A9.1 as 2 or treatment expression of the dominant negative Rag heterodimer (RagBT 54 N-RagCQ OL) with the mTOR inhibitor Torinl (29) completely inhibited mTORC1 activity, irrespective of whether SLC38A9.1 was overexpressed or not (Fig. 3, E and F). In contrast, the vATPase has a more complex relationship with SLC38A9.1. Its inhibition with concanamycin A eliminated mTORC1 signaling in the control cells but only partially 83 blocked it in cells overexpressing SLC38A9.1 (Fig. 3F). These results suggest a model in which SLC38A9.1 and the v-ATPase represent parallel pathways that converge upon the Ragulator-Rag GTPase complex. Modulation of the SLC38A9-Rag-Ragulator Interactions by Amino Acids Amino acids modulate the interactions between many of the established components of the amino acid sensing pathway, so we tested if this was also the case for the SLC38A9.1-Ragulator-Rag complex. Indeed, amino acid starvation strengthened the interaction between stably expressed or endogenous Ragulator and endogenous SLC38A9 (Fig. 4A, fig. S5) and between stably expressed SLC38A9.1 and endogenous Ragulator and Rags (Fig. 4B). We obtained similar results when cells were deprived of and stimulated with just leucine or arginine (Fig. 4A). Curiously, although the N-terminal domain of SLC38A9.1 readily bound Ragulator, the interaction was insensitive to amino acids (Fig. 4B), suggesting that the transmembrane region is required to confer amino acid responsiveness. As amino acid starvation alters the nucleotide state of the Rag GTPases (6, 7), we tested whether SLC38A9 interacted differentially with mutants of the Rags that lock their nucleotide state. Heterodimers of epitope-tagged RagB-RagC containing RagBT 54 N which mimics the GDP-bound state (6, 7), were associated with more endogenous SLC38A9 than heterodimers containing wild-type RagB (Fig. 4C). In contrast, heterodimers containing RagBQ 99L, which lacks GTPase activity and so is bound to GTP (6, 7, 15), interacted very weakly with SLC38A9 (Fig. 4C). Thus, like Ragulator, SLC38A9 interacts best with Rag heterodimers in which RagA/B is GDP-loaded, which is consistent with SLC38A9 binding to Ragulator and with Ragulator being a GEF for RagA/B. These results suggest that amino acid modulation of the interaction of SLC38A9.1 with Rag-Ragulator largely reflects amino acid-induced changes in the nucleotide state of the Rag GTPases. Because the RagB mutations had greater effects on the interaction of the Rag GTPases with SLC38A9 than with Ragulator (in Figure 4C compare the SLC38A9 blots with those for p14 and p18), it is very likely that the Rag heterodimers make Ragulator-independent contacts with SLC38A9 that affect the stability of Rag-SLC38A9 interaction. 84 SLC38A9.1 is an Amino Acid Transporter We failed to detect SLC38A9.1 -mediated amino acid transport or amino acidinduced sodium currents in live cells in which SLC38A9.1 was so highly overexpressed that some reached the plasma membrane (fig. S6, A-E). Because these experiments were confounded by the presence of endogenous transporters or relied on indirect measurements of transport, respectively, we reconstituted SLC38A9.1 into liposomes to directly assay the transport of radiolabelled amino acids. Affinity-purified SLC38A9.1 inserted unidirectionally into liposomes so that its N-terminus faced outward in an orientation analogous to that of the native protein in lysosomes (fig. S6, F-H). We could not use radiolabelled L-leucine in transport assays because it bound non-specifically to liposomes so we focused on the transport of L-arginine, which had low background binding (fig. S61). The SLC38A9.1-containing proteoliposomes exhibited time-dependent uptake of radiolabelled arginine while those containing LAMP1 interacted with similar amounts of arginine as liposomes (Fig. 5A, fig. S61). Steady-state kinetic experiments revealed that SLC38A9.1 has a Michaelis constant (Km) of -39 mM and a catalytic rate constant (kcat) of -1.8 min- (Fig. 5B), indicating that SLC38A9.1 is a low-affinity amino acid transporter. SLC38A9.1 can also efflux arginine from the proteoliposomes (Fig. 5C), but its orientation in liposomes makes it impossible to obtain accurate Km and kcat measurements for this activity. It is likely that by having to assay the transporter in the 'backwards' direction we are underestimating its affinity for amino acids during their export from lysosomes. To assess the substrate specificity of SLC38A9.1, we performed competition experiments using unlabeled amino acids (Fig. 5D). The positively charged amino acids histidine and lysine competed radiolabelled arginine transport to similar degrees as arginine, while leucine had a modest effect and glycine was the least effective competitor. Thus, it appears that SLC38A9.1 has a relatively non-specific substrate profile with a preference for polar amino acids. Given the preference of SLC38A9.1 for the transport of arginine and that arginine is highly concentrated in rat liver lysosomes (30) and yeast vacuoles (31), we asked whether SLC38A9.1 may have an important role in transmitting arginine levels to mTORC1. Towards this end we examined how mTORC1 signaling responded to a range of arginine or leucine concentrations in HEK-293T cells in which we knocked out SLC38A9 using CRISPR-Cas9 genome editing (Fig. 5E). Interestingly, activation of mTORC1 by arginine was strongly repressed at all arginine concentrations while the 85 response to leucine was only blunted so that high leucine concentrations activated mTORC1 equally well in null and control cells (Fig. 5F). DISCUSSION: Several properties of SLC38A9.1 are consistent with it functioning as an amino acid sensor for the mTORC1 pathway. Purified SLC38A9.1 transports and therefore directly interacts with amino acids. Overexpression of SLC38A9.1 or just its Ragulatorbinding domain activates mTORC1 signaling even in the absence of amino acids. The activation of mTORC1 by amino acids, particularly arginine, is defective in cells lacking SLC38A9. Given these results and that arginine is highly enriched in lysosomes from at least one mammalian tissue (30), we suggest that SLC38A9.1 is a strong candidate for being a lysosome-based arginine sensor for the mTORC1 pathway. To substantiate this possibility it will be necessary to determine the actual concentrations of arginine and other amino acids in the lysosomal lumen and cytosol and compare them to the affinity of SLC38A9.1 for amino acids. If high arginine levels are a general feature of mammalian lysosomes it could explain why SLC38A9.1 appears to have a relatively broad amino acid specificity; perhaps no other amino acid besides arginine is in the lysosomal lumen at levels that approach its Km. The notion that proteins with sequence similarity to transporters function as both transporters and receptors (transceptors) is not unprecedented (32, 33). The transmembrane region of SLC38A9.1 might undergo a conformational change upon amino acid binding that is then transmitted to Ragulator through its N-terminal domain. What this domain does is unknown but it could regulate Ragulator nucleotide exchange activity or access to the Rag GTPases by other components of the pathway. To support a role as a sensor, it will be necessary to show that amino acid binding regulates the biochemical function of SLC38A9.1. Even if SLC38A9.1 is an amino acid sensor, additional sensors, even for arginine, are almost certain to exist as we already know that amino acid-sensitive events exist upstream of Folliculin (15, 34) and GATOR1 (35), which, like Ragulator, also regulate the Rag GTPases. An attractive model is that distinct amino acid inputs to mTORC1 converge at the level of the Rag GTPases with some initiating at the lysosome through proteins like SLC38A9.1 and others from cytosolic sensors that remain to be 86 defined (Fig. 5G). Indeed, such a model would explain why the loss of SLC38A9.1 specifically affects arginine sensing but its overexpression makes mTORC1 signaling resistant to arginine or leucine starvation: hyperactivation of the Rag GTPases through the deregulation of a single upstream regulator is likely sufficient to overcome the lack of other positive inputs. A similar situation may occur upon loss of GATOR1, which, like SLC38A9.1 overexpression, causes mTORC1 signaling to be resistant to total amino acid starvation (14). Modulators of mTORC1 have clinical utility in disease states associated with or caused by mTORC1 deregulation. The allosteric mTOR inhibitor rapamycin is used in cancer treatment (36) and transplantation medicine (37). However, to date, there have been few reports on small molecules that activate mTORC1 by engaging known components of the pathway. The identification of SLC38A9.1-a protein that is a positive regulator of the mTORC1 pathway and has an amino acid binding site-provides an opportunity to develop small molecule agonists of mTORC1 signaling. Such molecules should promote mTORC1-mediated protein synthesis and could have utility in combatting muscle atrophy secondary to disuse or injury. Lastly, there is reason to believe that a selective mTORC1 pathway inhibitor may have better clinical benefits than rapamycin, which in long-term use inhibits both mTORC1 and mTORC2 (38). SLC38A9.1 may be an appropriate target to achieve this. 87 FIGURE 1: Interaction of SLC38A9.1 with Ragulator and the Rag GTPases B C Metap2 RagB Ragulator: 0 2 p18 3 7 9 5 p14 c7orf59 HBX1P S, SLC38A9.4 100 kDa SLC3SA9.1 A110 70 kDa $C38A9. N-tfm 119 50 kDa D F E Transfecd ' cNAs: C.lls ... rssvl FLAG-SLC38A9.1 PNGase F: SLC38A92 # protein a5i SLC38A9.1 - SLC38A9.1 peptlde - IPed - A Y m r T UUUU. 38aASNMPa3*.?LTPADAL *EjD-PGELTM s gsALt IA9 y1#AW 9N1a PS Cels expreask: 1 PIS franseced cDNAs: RagC pie RagA P1 13 A -Vlm 4 IP FLAG v-ATPas* . p14 R&O RagC FLAo-LAMP1 lp: PLAo-SLC38A9. 1 'P RagA FLAG FLAG NuAn etMp2 FLA-LAMPi *1 FLAO-RagE PLAG-SLC38AS.1 Ao- SLC38A9.2 F AMPI SLC3A9.1 FLAO-SLC3SA9.1 1_1190 p18 ~ F.Aa-p14 ag p14 i4ARaC RagA m _ Cell M Cel tysate lysals FLAo-LAMP; nua-SLC3S.A9.1 ruoa4n@tp2 FLA-RagE nAo-SLC38A9.1 1-119 88 F"Ap16 FIGURE 2: Localization of SLC38A9.1 to the lysosomal membrane in an amino acid-independent fashion and requirement of SLC38A9 for mTORCI pathway activation by amino acids A FLAG-SLC38A9.1 LAMP2 FLAG- SLC38A9.1 -a.a. for 50 for LAMP2 Merge B C shRNA: amino acids: ' ®-T389-S6K1 +' 4 S6K1 .0,0 - O '"-+' 0 00 SLC38A9 -a.a. forFLAG50 mfo SLC38A9.1 dj!*'ytd raptor SLAMP2 +a.a. for 10 min Merge 89 ** #04 4* FIGURE 3: Stable overexpression of full-length SLC38A9.1 or its N-terminal Ragulator-binding domain makes the mTORC1 pathway insensitive to amino acid deprivation A B Ces expressing: ssing: amino aci : Be ucine: acids: -amino 4 -T389-36K1 - ar inine: - + - + - + Cells expre 6S6K1 c-T3a9 S6K1 S61 a Ra-SLC3WA.1As FLAG-SLC39AS.2 ULKI 1MO W 6 0 db* . 4 .- S65-4E-BP1 04 WOW0 M44 - *0 4* C V Cels expressing: amino acids: 4E-BP1 + + - -+ + ®-S757-ULKI T389-SK1 FLAO-SLC38A9.1 FLAG-LAMP1 FLAG-SLC3BA9.1 FLAOmetap2 D E FLA.56K1 & KATranstected Cells expressing: + RaagC*' ++ - arginine: R[ MW i"s '0 ®-T389-6K1 + FLAG FLAOSLC38A9.1 CeN lysate 1-119 Conc-nycin A DMSO treatment Torini - + - + - + - + - + - + Cells expressing: amino acids: S6K1 mA-SEC30A9.1 FLAG-metap2 F amino acids 1T38946K1 -T389-S6K1 40 f 40 96K1 FLAO-SLC38A9.1 FLA-metap2 90 4A-mtap2 t.RagcolL - + '- + - - + +o RagBt1 + amino acids: + SLC36A9.1 Metp2 Rag3"B cDNAs: 40 som40' s aft FIGURE 4: Modulation of the interaction between SLC38A9 and Ragulator and the Rag GTPases by amino acids FLAG- FLAG-pIS FLAG-p14 - - C agC u. Roo YS + leucine: argirnine: + + amino acids: metp2 + SLC38A9 Translected cDNAs: FLAG lysae [ ue p14 ~ Rag nucleobd binding mutanits AseYoknwy wam nuesohes] GTP hVdycyesmWnwi OTP hey**pi emfwt FLA.mtap2: - A-GAT-RagB: - SL FLAPI +- FLAO-1R0gC: - - - - - - WT WI WT S7QOIOL5n*O1O L wT lim oauL wT wI owt iset 3A9 SLC36A9 FLA-p1i (samea f FLAa-p14 Fp. FLAG B Cells expressing: amino acids: / xYe~e~ /~P/~ FuoAretp2 ams FLAG-RagC RagC mA-a-RagO RagA SLC38A9 d"4V"~ PLAaSLC38A9.1 PLAG-SLC3BA9.2 raptor ek Ceil FLAo-metap2 FLAGSLC3&A9.4 p14 WON Fuw-mWt2 1-119 FLAo-RagC m-AST-RagSB p14 RegA Cell lysate 4 a p14 p14 L raptor p18 p1S IP: FLAG - A Cells expressing: RagC Rua-SLC3SA9.1 FLAo-SLC3SA9.2 FLAa-fWtap2 FLAG-SLC36A9.4 ruLo-SLC3SA9.1 1-119 91 "W Oft w A -p.-. FIGURE 5: SLC38A9.1 is a low affinity amino acid transporter and is necessary for mTORC1 pathway activation by arginine B 4- R-(05uM) +IR'+20 mM R 0 - e 8~ 20 R*+50 mM R 1100- * SLC38A9.1 proteoliposomes 10- fi R'+10O0mM R R+400 mMR & A, 'a e. 6- 10-Km ~50 = 39 mM - 14- liposormes onl~y 2- 0 Time(min) 20 0 60 40 20 Skcat 0. C 40 Time (min) 300 200 100 0 60 1 .8 E C4 0SLC38A9 -E a 0 raptor g 4 S. FHEK-293T clone: sgAAVS1_ 0 %leucino in RPMI: 1 3 -w ®-T389-S6K1 10 100 0 im t 1 3 1 3 10 30 100 in RPMI S6K1 G so S ®-T389-S6K1 , w90 cytosol R 40 0 0 HEK-293T clone: % aglne 0 in RPMI: 1 ®-T389-S6K1 gAAVS12 3 10 30 100 0 amino acids membrane amino acids 92 sgSLC38A9-1 1 3 10 30 100 &gSLC38A9-2 1 3 10 30 100 s 4 6V W6K1 4% a 0 00, SLC38A9 ru &gAAVS1 1 1 3 10 30 100 0 0 ,i 00 *4 "-- 06 10 0 1 l ,04 v-ATPase tysosomai lumen M 0 SKI S I* *gSLC38A9_2 0 10 30 100 %arglnkn in RPMI G ® k-T389-S6K1 o - sgAAVS1_1 0 HEK-293T clone: 3 10 30 100 1 a ft so a HEK-293T clone: H KQ E M F L I A P Competitor amino acid sgSLC3BA9 I 30 S6K1 A %leucdne R 20 4110 . 100 15;0 200 Time 000 (min) 500 400 [Arg] (mM) D 0 min- 40 46 li 00 d 4k6 Figure Legends Figure 1. Interaction of SLC38A9.1 with Ragulator and the Rag GTPases. (A) The spectral counts of SLC38A9-derived peptides detected by mass spectrometry in immunoprecipitates prepared from HEK-293T cells stably expressing the indicated FLAG-tagged proteins. (B) Schematic depicting SLC38A9 isoforms and truncation mutants. Transmembrane domains predicted by the TMHMM (transmembrane hidden Markov model) algorithm (http://www.cbs.dtu.dk/services/TMHMM) are shown as blue boxes. (C) Effects of PNGase F treatment of SLC38A9.1 on its electrophoretic migration. (D) Interaction of full-length SLC38A9.1 or its N-terminal domain with endogenous Ragulator (p18 and p14) and RagA and RagC GTPases. HEK-293T cells were transfected with the indicated cDNAs in expression vectors and lysates were prepared and subjected to FLAG immunoprecipitation followed by immunoblotting for the indicated proteins. (E) Identification of key residues in the N-terminal domain of SLC38A9.1 required for it to interact with Ragulator and the Rag GTPases. Experiment was performed as in (D) using indicated SLC38A9.1 mutants. (F) Interaction of SLC38A9.1 with v-ATPase components VOd1 and V1 B2. HEK-293T cells stably expressing the indicated FLAG-tagged proteins were lysed and processed as in (D). Figure 2. Localization of SLC38A9.1 to the lysosomal membrane in an amino acidindependent fashion and requirement of SLC38A9 for mTORC1 pathway activation by amino acids. (A) SLC38A9.1 localization in cells deprived of or replete with amino acids. HEK-293T cells stably expressing FLAG-SLC38A9.1 were starved and stimulated with amino acids for the indicated times. Cells were processed and immunostained for LAMP2 and FLAG-SLC38A9.1. (B) Requirement of SLC38A9 for the activation of the mTORC1 pathway by amino acids. HEK-293T cells expressing indicated short hairpin RNAs (shRNAs) were deprived of amino acids for 50 min or deprived of and then restimulated with amino acids for 10 min. Cell lysates were analyzed for the levels of indicated proteins and the S6K1 phosphorylation state. Figure 3. Stable overexpression of full-length SLC38A9.1 or its N-terminal Ragulatorbinding domain makes the mTORC1 pathway insensitive to amino acid deprivation. (A) Stable overexpression of FLAG-SLC38A9.1 largely restores mTORC1 signaling during total amino acid starvation and completely restores it upon deprivation of leucine or arginine. HEK-293T cells transduced with lentiviruses encoding the specified proteins 93 were deprived for 50 min of all amino acids, leucine, or arginine and, where indicated, re-stimulated for 10 min with the missing amino acid(s). Cell lysates were analyzed for the levels of the specified proteins and the phosphorylation states of S6K1, ULKI, and 4E-BP1. (B and C) Overexpression of neither SLC38A9.2 nor a point mutant of SLC38A9.1 that fails to bind Ragulator rescues mTORC1 signaling during amino acid starvation. Experiment was performed as in (A) except that cells were stably expressing SLC38A9.2 (B) or SLC38A9.1 168A (C). (D) Stable overexpression of the Ragulatorbinding domain of SLC38A9.1 largely restores mTORC1 signaling during total amino acid starvation and completely rescues it upon deprivation of leucine or arginine. Experiment was performed as in (A) except cells were stably expressing FLAGSLC38A9.1 1-119. (E) The ability of SLC38A9.1 overexpression to rescue mTORC1 signaling during amino acid starvation is eliminated by co-expression of RagBT 5 4 N_ RagCQ 2OL, a Rag heterodimer locked in the nucleotide configuration associated with amino acid deprivation. Effects of expressing the indicated proteins on mTORC1 signaling were monitored by the phosphorylation state of co-expressed FLAG-S6K1. (F) Effects of concanamycin A and Torin1 on mTORC1 signaling in cells stably expressing SLC38A9.1. HEK-293T cells stably expressing the indicated FLAG-tagged proteins were treated with the DMSO vehicle or the specified small molecule inhibitor during the 50 min starvation for and, where indicated, the 10 min stimulation with amino acids. Figure 4. Modulation of the interaction between SLC38A9 and Ragulator and the Rag GTPases by amino acids. (A) Effects of amino acids on interaction between the Ragulator complex and endogenous SLC38A9. HEK-293T cells stably expressing the indicated FLAG-tagged Ragulator components were deprived of total amino acids, leucine, or arginine for 1 hour and, where indicated, re-stimulated with amino acids, leucine, or arginine for 15 min. After lysis, samples were subject to FLAG immunoprecipitation and immunoblotting for the indicated proteins. Quantification of SLC38A9 levels in the stimulated state relative to starved state, p14 IP: 0.75 (+AA), 0.79 (+L), 0.74 (+R); p18 IP: 0.56 (+AA), 0.57 (+L), 0.49 (+R). (B) Effects of amino acids on the interaction between full-length or truncated SLC38A9.1 and endogenous Ragulator and the Rag GTPases. Experiment was performed as in (A) except that cells stably expressed the indicated SLC38A9 isoforms or its N-terminal domain (SLC38A9.1 1-119). Quantification of indicated protein levels in the stimulated state relative to starved state, SLC38A9.1 IP: 0.43 (p18), 0.51 (p14), 0.61 (RagC), 0.58 (RagA); SLC38A9.1 1-119 IP: 94 0.99 (p18), 1.05 (p14), 1.04 (RagC), 1.09 (RagA). (C) Effects of the RagBT 5 4N mutation on association with endogenous SLC38A9. HEK-293T cells were transfected with the indicated cDNAs in expression vectors and lysates were prepared and subjected to FLAG immunoprecipitation followed by immunoblotting for the indicated proteins. Two different antibodies were used to detect endogenous SLC38A9. Figure 5. SLC38A9.1 is a low affinity amino acid transporter and is necessary for mTORC1 pathway activation by arginine. (A) Time-dependent uptake of [ 3 H]arginine at 0.5 pM by proteoliposomes containing 22.4 pmol of SLC38A9.1. To recapitulate the pH gradient across the lysosomal membrane, the lumen of the proteoliposomes is buffered at pH 5.0, while the external buffer is pH 7.4. (B) Steady-state kinetic analysis of SLC38A9.1 uptake activity reveals a Michaelis constant (Kn) of -39mM and catalytic rate constant (kcat) of -1.8min-1. (Left) Time course of [3H]arginine (R*) uptake, given fixed [ 3H]arginine (0.5 pM) and increasing concentrations of unlabeled arginine. (Right) Velocity, calculated from left panel, as a function of total arginine concentration. Data were fitted to the Michaelis-Menton equation. Experiment was repeated over 4 times with similar results and a representative one is shown. (C) Time-dependent efflux of SLC38A9.1 proteoliposomes following 1.5 hr loading with 0.5 pM [ 3 H]arginine. (D) Competition of 0.5 pM [ 3H]arginine transport by SLC38A9.1 using 100 mM of indicated unlabeled amino acids. In A-D, error bars represent standard deviation derived from at least 3 measurements. (E) HEK-293T cells null for SLC38A9 were generated using CRISPR-Cas9 genome editing using two different guide sequences and isolated by single cell cloning. The AAVS1 locus was targeted as a negative control. (F) Impairment of arginine-induced activation of the mTORC1 pathway in SLC38A9-null HEK-293T cells. Cells were starved of the indicated amino acid for 50 minutes and stimulated for 10 minutes using the indicated amino acid concentrations. The leucine and arginine concentrations in RPMI are, respectively, 381 pM and 1.14 mM. (G) Model for distinct amino acid inputs to the Rag GTPases in signaling amino acid sufficiency to mTORC1. 95 References 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. J. L. Jewell, R. C. Russell, K. L. Guan, Amino acid signalling upstream of mTOR. 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Rebsamen for suggesting the use of the Sigma antibody to detect SLC38A9. This work was supported by grants from the NIH (R01 CA103866 and A147389) and Department of Defense (W81XWH-07-0448) to D.M.S., and fellowship support from the NIH to Z.T. (F30 CA1 80754), to S.W. (T32 GM007753 and F31 AG044064), to L.C. (F31 CA180271), and to R.W. (T32 GM007753); an NDSEG Fellowship to G.A.W.; an NSF Graduate Research Fellowship to T.W.; an American Cancer Society - Ellison Foundation Postdoctoral Fellowship to W.C. (PF-13-356-01-TBE); a German Academic Exchange Service/DAAD Fellowship to C.S., and support from the Howard Hughes Medical Institute to T.D.J., C.K. and J.P. D.M.S. and B.L.S. are investigators of the Howard Hughes Medical Institute. 98 EXPERIMENTAL PROCEDURES Materials Reagents were obtained from the following sources: HRP-labeled anti-mouse, anti-rabbit, and anti-goat secondary antibodies and the antibody to LAMP2 from Santa Cruz Biotechnology; antibodies to phospho-T389 S6K1, S6K1, phospho-ULK1, ULK1, phospho-S65 4E-BP1, 4E-BP1, RagA, RagC, p14 (LAMTOR2), p18 (LAMTOR1), mTOR, and the FLAG epitope (rabbit antibody) from Cell Signaling Technology; the antibody to the HA epitope from Bethyl laboratories; the antibody to ATP6V1 B2 from Abcam; RPM I, FLAG M2 affinity gel, FLAG-M2 (mouse) and ATP6V0d1 antibodies, and amino acids from Sigma Aldrich; the PNGase F from NEB; Xtremegene 9 and Complete Protease Cocktail from Roche; AlexaFluor-labeled donkey anti-rabbit, anti-mouse, and anti-rat secondary antibodies from Invitrogen and Inactivated Fetal Calf Serum (IFS) from Invitrogen; amino acid-free RPMI and Leucine or Arginine-free RPMI from US Biological; siRNAs targeting indicated genes and siRNA transfection reagent from Dharmacon; Concanamycin A from A.G. Scientific; Torin1 from Nathanael Gray (DFCI); [ 14C]-labeled amino acids and Opti-Fluor scintillation fluid from PerkinElmer; [ 3H]-labeled amino acids from American Radiolabeled Chemicals; Egg phosphatidylcholine (840051C) from Avanti lipids; Bio-beads SM-2 from Bio-Rad; and PD-1 0 columns from GE Healthcare Life Sciences. The antibody to SLC38A9 from Sigma (HPA043785) was used to recognize the deglycosylated protein (according to NEB instructions except without the boiling step) in cell lysates and immunopurifications. A distinct antibody to SLC38A9.1 was generated in collaboration with Cell Signaling Technology and was used to detect the glycosylated protein in Ragulator immunopurifications but is not sensitive enough to detect it in cell lysates. Cell lines and tissue culture HEK-293T cells were cultured in DMEM supplemented with 10% inactivated fetal bovine serum, penicillin (100 IU/mL), and streptomycin (100 pg/mL) and maintained at 370C and 5% CO2. In HEK-293E, but not HEK-293T, cells the mTORC1 pathway is strongly regulated by serum and insulin (1). Mass spectrometric analyses Immunoprecipitates from 30 million HEK-293T cells stably expressing FLAGmetap2, FLAG-p18, FLAG-p14, FLAG-HBXIP, FLAG-c7orf59, and FLAG-RagB were prepared as described below. Proteins were eluted with the FLAG peptide (sequence 99 DYKDDDDK) from the anti-FLAG affinity beads, resolved on 4-12% NuPage gels (Invitrogen), and stained with SimplyBlue SafeStain (Invitrogen). Each gel lane was sliced into 10-12 pieces and the proteins in each gel slice digested overnight with trypsin. The resulting digests were analyzed by mass spectrometry as described (2). Amino acid or individual amino acid starvation and stimulation of cells Almost confluent cell cultures in 10 cm plates were rinsed twice with amino acidfree RPMI, incubated in amino acid-free RPMI for 50 min, and stimulated for 10 min with a water-solubilized amino acid mixture added directly to the amino acid-free RPMI. For leucine or arginine starvation, cells in culture were rinsed with and incubated in leucineor arginine-free RPMI for 50 min, and stimulated for 10 min with leucine or arginine added directly to the starvation media. After stimulation, the final concentration of amino acids in the media was the same as in RPMI. Cells were processed for biochemical or immunofluorescence assays as described below. The 1OX amino acid mixture and the 300X individual stocks were prepared from individual amino acid powders. When Concanamycin A (ConA) or Torin1 was used, cells were incubated in 5 pM Concanamycin or 250 nM Torin1 during the 50 min amino acid starvation and 10 min amino acid stimulation periods. Cell lysis and immunoprecipitations HEK-293T cells stably expressing FLAG-tagged proteins were rinsed once with ice-cold PBS and lysed in ice-cold lysis buffer (40 mM HEPES pH 7.4, 1% Triton X-100, 10 mM P-glycerol phosphate, 10 mM pyrophosphate, 2.5 mM MgC1 2 and 1 tablet of EDTA-free protease inhibitor (Roche) per 25 ml buffer). The soluble fractions from cell lysates were isolated by centrifugation at 13,000 rpm for 10 min in a microcentrifuge. For immunoprecipitates 30 uL of a 50% slurry of anti-FLAG affinity gel (Sigma) were added to each lysate and incubated with rotation for 2-3 hr at 40C. Immunoprecipitates were washed three times with lysis buffer containing 500 mM NaCl. Immunoprecipitated proteins were denatured by the addition of 50 uL of sample buffer and incubation at RT for 30 min. It is critical that the samples containing SLC38A9 are neither boiled nor frozen prior to resolution by SDS-PAGE and analysis by immunoblotting. A similar protocol was employed when preparing samples for mass spectrometry. cDNA manipulations and mutagenesis 100 The cDNAs for all human SLC38A9 isoforms, both native and codon-optimized, were gene-synthesized by GenScript. The cDNAs were amplified by PCR and the products were subcloned into Sal I and Not I sites of HA-pRK5 and FLAG-pRK5. The cDNAs were mutagenized using the QuikChange 11 kit (Agilent) with oligonucleotides obtained from Integrated DNA Technologies. All constructs were verified by DNA sequencing. FLAG-tagged SLC38A9 isoforms and SLC38A9 N-terminal 1-119 were amplified by PCR and cloned into the Sal I and EcoR I sites of pLJM60 or into the Pac I and EcoR I sites of pMXs. After sequence verification, these plasmids were used, as described below, in cDNA transfections or to produce lentiviruses needed to generate cell lines stably expressing the proteins. cDNA transfection-based experiments For cotransfection-based experiments to test protein-protein interactions, 2 million HEK-293T cells were plated in 10 cm culture dishes. 24 hours later, cells were transfected with the pRK5-based cDNA expression plasmids indicated in the figures in the following amounts: 500 ng FLAG-metap2; 50 ng FLAG-LAMP1; 100 ng FLAG-RagB and 100 ng HA-RagC; 300 ng FLAG-SLC38A9.1; 600 ng FLAG-SLC38A9.1 A110; 200 ng FLAG-SLC38A9.4; 400 ng FLAG-N-terminal 119 fragment of SLC38A9. 1; 200 ng FLAG-RagC; 200 ng FLAG-RagC S75N; 200 ng FLAG-RagC Q120L; 400 ng HAGSTRagB; 400 ng HAGST-RagB T54N; 400 ng HAGST-RagB Q99L. Transfection mixes were taken up to a total of 5 pg of DNA using empty pRK5. For co-transfection experiments to test mTORC1 activity, 1 million HEK-293T cells were plated in 10 cm culture dishes. 24 hours later, cells were transfected with the pRK5-based cDNA expression plasmids indicated in the figures in the following amounts: 500 ng HA-metap2; 50 ng HA-LAMP1; 200 ng HA-SLC38A9.1; 500 ng HASLC38A9.1 A110; 200 ng HA-SLC38A9.4; 100 ng HA-RagB T54N and 100 ng HA-RagC Q1 20L; 2 ng FLAG-S6K1. 72 hours post-transfection, cells were washed once prior to 50-min incubation with amino acid-free RPMI. Cells were stimulated with vehicle or amino acids (to a final concentration equivalent to RPMI) prior to harvest. Lentivirus production and lentiviral transduction Lentiviruses were produced by co-transfection of the pLJM1/pLJM60 lentiviral transfer vector with the VSV-G envelope and CMV AVPR packaging plasmids into viral 101 HEK-293T cells using the XTremeGene 9 transfection reagent (Roche). For infection of HeLa cells, LN229 cells, and MEFs, retroviruses were produced by co-transfection of the pMXs retroviral transfer vector with the VSV-G envelope and Gag/Pol packaging plasmids into viral HEK-293T cells. The media was changed 24 hours post-transfection to DME supplemented with 30% IFS. The virus-containing supernatants were collected 48 hours after transfection and passed through a 0.45 pm filter to eliminate cells. Target cells in 6-well tissue culture plates were infected in media containing 8 pg/mL polybrene and spin infections were performed by centrifugation at 2,200 rpm for 1 hour. 24 hours after infection, the virus was removed and the cells selected with the appropriate antibiotic. Mammalian RNAi Lentiviruses encoding shRNAs were prepared and transduced into HEK-293T cells as described above. The sequences of control shRNAs and those targeting human SLC38A9, which were obtained from The RNAi Consortium 3 (TRC3), are the following (5' to 3'): SLC38A9 #1: GCCTTGACAACAGTTCTATAT (TRCN0000151238) SLC38A9 #2: CCTCTACTGTTTGGGACAGTA (TRCN00001 56474) GFP: TGCCCGACAACCACTACCTGA (TRCN0000072186) For siRNA-based experiments, 200,000 HEK-293T cells were plated in a 6-well plate. 24 hours later, cells were transfected using Dharmafect 1 (Dharmacon) with 250 nM of a pool of siRNAs (Dharmacon) targeting SLC38A9 or a non-targeting pool. 48 hours post-transfection, cells were transfected again but this time with double the amount of siRNAs. 24 hours following the second transfection, cells were rinsed with icecold PBS, lysed, and subjected to immunoblotting as described above. The following siRNAs were used: Non-targeting: ON-TARGETplus Non-targeting Pool (D-001810-10-05) SLC38A9: SMARTpool: ON-TARGETplus SLC38A9 (L-007337-02-0005) Immunofluorescence assays HEK-293T cells were plated on fibronectin-coated glass coverslips in 6-well tissue culture dishes, at 300,000 cells/well. 12-16 hours later, the slides were rinsed with PBS once and fixed and permeabilized in one step with ice-cold 100% methanol (for 102 SLC38A9 detection) at -20'C for 15 min. After rinsing twice with PBS, the slides were incubated with primary antibody (FLAG CST 1:300, LAMP2 1:400) in 5% normal donkey serum for 1 hr at room temperature, rinsed four times with PBS, incubated with secondary antibodies produced in donkey (diluted 1:400 in 5% normal donkey serum) for 45 min at room temperature in the dark, and washed four times with PBS. Slides were mounted on glass coverslips using Vectashield with DAPI (Vector Laboratories) and imaged on a spinning disk confocal system (Perkin Elmer). Whole-cell amino acid transport assay HEK-293T cells (150,000/well) were plated onto fibronectin-coated 12-well dishes and transfected 12 hours later with the pRK5-based cDNA expression plasmids indicated in the figures in the following amounts using XtremeGene9: 400 ng LAMP1FLAG, 400 ng FLAG-SLC38A9.1, 400 ng SLC38A2-FLAG, 150 ng PQLC2-FLAG, and 50 ng GFP. Transfection mixes were taken up to a total of 2 pg of DNA using empty pRK5. Cells were assayed 48 hours later by washing twice in transport buffer (140 mM NaCl, 5 mM KCI, 2 mM MgCI2, 2 mM CaCl 2, 30 mM Tris-HCI, pH 7.4, 5 mM glucose), incubating in transport buffer for 5 min. at 370C before replacing the buffer with fresh buffer supplemented with amino acids (unlabeled and 0.1 pCi of [ 14C]leucine at a total concentration of 380 pM, or unlabeled and 0.1pCi of [ 14C]amino acid mix at total concentrations found in RPMI, or unlabeled and 0.2 pCi of [ 14C]arginine at a total concentration of 3 mM) at the indicated pH (pH 5 buffered by MES, pH 8 buffered by Tris) for 10 minutes at 370C. After uptake, cells were washed twice in ice-cold transport buffer and harvested in 0.5 mL of 1% SDS for scintillation counting. Protocol and amino acid concentrations used were informed by previous whole-cell assays to detect transport by SLC38A2 and PQLC2 (3, 4). Electrophysiology Whole-cell recordings were made from GFP-positive HEK-293T cells, prepared as described above, 48 to 72 hrs post transfection. Patch pipettes (open-tip resistance 34 Mf) were filled with a solution containing (in mM) K-gluconate 153, MgC 2 2, CaC 2 1, EGTA 11, HEPES 10, pH 7.25 adjusted with KOH, and tip resistance was left uncompensated. Cells were continuously superfused (- 2 ml/min) with extracellular solution containing (in mM) NaCl 150, KCI 3, CaCl 2 2, MgC 2 1, Glucose 5, HEPES 10, pH adjusted to 7.4 with NaOH. Once whole-cell configuration was established, a 103 homemade perfusion system consisting of several adjacent glass tubes (ID 252 pm) was used to locally perfuse extracellular solution pH 5.5 and to apply amino acids (in mM) leucine 1.6, arginine 2.4, glutamine 4. Membrane currents were amplified and low-pass filtered at 3 kHz using a Multiclamp 700B amplifier (Molecular Devices), digitized at 10 kHz and acquired using National Instruments acquisition boards and a custom version of ScanImage written in MATLAB (Mathworks) (5). Data were analyzed offline using Igor Pro (Wavemetrics), and amino acid-induced currents were quantified as difference in the average membrane currents for the 5 s-windows right before and during application. Proteoliposome Reconstitution HEK-293T cells stably expressing FLAG-SLC38A9.1 were harvested as described above for immunoprecipitations, except cells were lysed in 40 mM HEPES pH 7.4, 0.5% Triton X-100, 1 mM DTT, and protease inhibitors. Following a 3 hr immunoprecipitation, FLAG-affinity beads were washed twice for 5 min each in lysis buffer supplemented with 500 mM NaCl. Beads were equilibrated with inside buffer (20 mM MES pH 5, 90 mM KCI 10 mM NaCI) supplemented with 10% glycerol by washing them 5 times. FLAG-affinity purified SLC38A9.1 protein was eluted in glycerolsupplemented inside buffer containing 1 mg/mL FLAG peptide by rotation for 30 min. Protein was concentrated using Amicon centrifuge filters to about 1 mg/mL and snapfrozen in liquid nitrogen and stored at -80'C. Chloroform-dissolved phosphatidycholine (PC, 50 mg) was evaporated using dry nitrogen to yield a lipid film in a round bottom flask and desiccated overnight under vacuum. Lipids were hydrated in inside buffer at 50 mg/mL with light sonication in a water bath (Branson M2800H) and split into 100 pL aliquots in eppendorf tubes. Aliquoted lipids were clarified using water bath sonication and recombined and extruded through a 100 nm membrane with 15 passes (Avanti 61000). Reconstitution reaction (15 pg FLAG-SLC38A9.1 protein, 7.5 mg Triton X-100, 10 mg extruded PC, 1 mM DTT in inside buffer up to 700 pL) was initiated by rotating at 40C for 30 min. Glycerolsupplemented inside buffer was used in lieu of SLC38A9.1 protein in liposome only controls. Bio-beads (200 mg/reaction) were prepared by washing 1 time in methanol, 5 times in water and 2 times in inside buffer. Reconstitution reaction was applied to Biobeads for 1 hr, transferred to fresh Bio-beads overnight, and transferred again to fresh Bio-beads for 1 hr. Protocol was adapted from a recently reconstituted lysosomal 104 transporter and a recent review (6, 7). Floatation assay A three-step sucrose gradient was generated by first adding 3.8 mL of the middle buffer (35% glycerol in inside buffer) to the ultracentrifuge tube, then applying 1 mL of the bottom buffer (50% glycerol in inside buffer) with 100 pL of SLC38A9.1 proteoliposomes (or protein only) using a 2 mL pipette to the bottom of the tube, and finally layering 1.2 mL of the top buffer (0% glycerol, inside buffer) on top. For assays containing urea, the proteoliposomes were rotated in bottom buffer containing 6 M urea for 30 min. at 40C before generating the sucrose gradient with above buffers supplemented with 6 M urea. Gradients were topped with 2 mL paraffin oil and loaded into a SW32.1 rotor and centrifuged at 32,000 g for 24 hours. Fractions (500 pL, excluding the oil) were collected from the top and 20 pL of each subjected to anti-FLAG western analysis. Protocol was adapted from Wuu et al. (8). Trypsin protection assay Trypsin (1 pL of 0.05%, Invitrogen) was added to SLC38A9.1 proteoliposomes (15 pL) and incubated at 370C for 30 min. As indicated, 1% Triton X-100 was added and rotated for 30 min. at 40C before addition of trypsin. Reactions were subjected to antiFLAG western analysis. Protocol was inspired by Brown and Goldstein (9). In vitro amino acid transport assay All buffers were chilled and assays performed in a 40C cold room. For time course experiments, SLC38A9.1 proteoliposomes or liposome controls were applied to PD10 columns equilibrated with outside buffer (20 mM Tris pH 7.4, 100 mM NaCl) and eluted according to manufacturer's instructions. Amino acid uptake was initiated by the addition of 0.5 pM [ 3H]arginine and incubated in a 300C water bath. Time points were collected by taking a fraction of the assay reaction and applying it to PD10 columns preequilibrated with outside buffer. Columns were eluted in fractions or a single elution of 1.75 mL and added to 5 mL of scintillation fluid. Protein used in uptake assays was estimated by assuming 100% incorporation efficiency during reconstitution. To obtain accurate measures of amino acid concentrations, equal volumes of outside buffer was added to scintillation fluid in the standards. 105 For competition experiments with unlabeled amino acids, high concentrations of amino acids were required due to the high Km (-39mM) of SLC38A9.1 import activity. SLC38A9.1 proteoliposomes or liposome controls were centrifuged at 100,000 g for 30 min. in a TLA-1 00.3 rotor and resuspended in a smaller volume of outside buffer such that they could be added to a larger volume of 100 mM unlabeled amino acid (final concentration) supplemented with outside buffer components. We had to resort to this procedure due to the solubility limit of leucine at -130 mM. At such high concentrations, it is important to adjust all amino acid solutions to pH 7.4. Assays were initiated by addition of 0.5 pM [ 3 H]arginine to the amino acid buffer solution followed by the addition of SLC38A9.1 proteoliposomes or liposome controls. For steady-state kinetics experiments, time points were collected as described above and to assess substrate specificity, competition experiments were collected at 75 min. For efflux experiments, SLC38A9.1 proteoliposomes or liposome controls were loaded with [ 3H]arginine as described above for an import assay for 1.5 hrs. To remove external amino acids, the reactions were applied to PD10 columns pre-equilibrated with outside buffer, and time points were collected as described above. Scintillation counts from liposome controls were subtracted from that of SLC38A9.1 proteoliposomes. Generation of knockout clones using CRISPR/Cas9 The CRISPR guide sequences designed to the N-terminus (1-119 a.a.) of SLC38A9 or the AAVS1 locus using http://crispr.mit.edu were cloned into pX459 (10). AAVS1: GGGGCCACTAGGGACAGGAT SLC38A9_1: GGCTCAAACTGGATATTCATAGG SLC38A9_2: GGAGCTGGAACTACATGGTCTGG HEK-293T cells (750,000/well) were plated into 6 well dishes and transfected 16 hours later with 1 pg of pX459 expressing above guides using XtremeGene9. Cells were trypsinized 48 hours later, 2 mg/mL puromycin was applied for 72 hours, and allowed to recover for a few days. When cells were approaching confluency, they were single-cell sorted into 96-well dishes containing 30% serum and conditioned media. Clones were expanded and evaluated for knockout status by western analysis for SLC38A9. These clones were evaluated for amino acid response as described above. 106 SUPPLEMENTAL INFO Figure S1: Membrane topology of SLC38A9.1. A TMHMM output for human SLC38A9.1 1.2 0. 0.6 CL 0.4 0.2 residue number: o 100 200 transmembrane 300 inside -- P I v A ) B Scytosol I Iv Iy 0ue Av 107 vma 500 400 -- outside Figure S2: Ragulator and the Rag GTPases do not interact with all lysosomal amino acid transporter-like proteins. P~f% A N B B C 0 Transfected cDNAs: RgC 0 Transiected cDNAs ~ p18 R4q RagA RagA 4 p18 p14 IP: FLAG p1S 'P FLAG IP: p14 ReAC nuo-LAMP1 FPLASLC38A9.1 LA.SLC38A9.1 Alt0 Fu4oeWa2 FAOCSLC8A9.4 .A.LAMP1 LAG-SLCS8A9.1 FLAG FR0-SLC38A9.2 FnA-LAMPI FPAa-SLCMA9.1 nAomltap2 R9gC RagC A Cell lysate n.o-SLC36A1 RagA FLo-SLC38A7 FLAGLAMP1 PLA-SLC38A9.1 A110 FLA-SLC38A8.I p18 * RagC CoN lysate FLA-SLC38A.4 P14 PL&G-SLCUA1.1 ROgA p18 Col LAGLAMPI nAo-SLC38A9.1 ~ FtA-SLC38A9.2 p14 lysate FLAG-LAMPI Un-Ametap2 - F.A-SLC38A9.1 FiA-SLC38A7 FLAo-SLC36AI 4 108 FLAG- SLC38A9.2 FLAG-p14 + HA-HBXIP+ hA-MPI + -c7orf59 Transfected cDNAs: "Isa IA.p1s HA-SLC3SA9.1 LAMP2 uA-SLC38A9.4 H -- HA-SLC38A9.1 merge B PLAo-p14 IP: FLAG- FLAG "A-HBXIP SLC38A9.4 "A-Plie" HA-plO LAMP2 HA-MPl mu-c7orf59 merge mSLC38A9.1 D siRNA: amino acids: NA-SLC38A9.4 -+ cell -+ FLA*-p14 lysale (-T389-6K1 mA-HBXIP SOKI HA-plaA SLC38A9 sA.MP1 . 109 -4 A-c7orf59 + + C + A + Figure S3: Localization of SLC38A9 isoforms 2 and 4 and signaling effects of siRNAmediated SLC38A9 knockdown. Figure S4: (A) Transient overexpression of SLC38A9.1, but not truncation mutants lacking the N-terminal Ragulator-binding domain, makes the mTORC1 pathway insensitive to amino acid starvation. r ODN": LM'SLC8". ,"'."p2 COS expr.ssing: arginine starvation time (h): - chloroquine: % TransIected C nAG.SOK1 &liA. + - + - + -+ - + # eS Onmin, ack: FLAG -+ ++ +- - - 16K1 96KI LC3 BI A4.LAMP1 pG2 isA-SLC28A9.1 Ap2 PLASLC3SA1.1 A110 A-81CIIIIIA9A MA-SLC31IA9.1 B p5 -/- 2MT Ceexpssing amino rua~netmp2 . . HeLa MEFs :. adds: Cellsexpressing r= -+ + -+ ,p -ax - #AM. . CON lyeate ®-T238-6K1 arninomed' -BT311-4611 PLAG-SLC38AS pu.-SLCM8A9Wll amino acia: =+r="+""i -+ SGK1 jV ®T355-46K1[ S6KI FLA".LC3BAO PLua-Rap2A FLA&-Rap2 FLAG-RWp2 i 00M1, oil insulin: ®-T9-SSKI HEK-293T cells expressfg: VLf!!- ap2 treatment: Dtno ua2M =-+ amino scids: - HEK-293E Cellis expressing: - + - +" D2T32 6K1 K FLA-SLC26A9.1 suLa~ap2 -T306AkM AkM L~mABtAII 110 PLAG.sLC3aA.1 DB -+ MM" '- + -- MM D P"=d llll - + A Figure SS: Endogenous immunoprecipitation of Rag and Ragulator components recovers SLC38A9 in an amino acid-sensitive fashion. p18 + RagC RagA - +'- - IP antibody: control amino acids: -+ SLC38A9 (cn-r IP RagA Y SLC38A9 RagC RagA cell lysate L RpgA 111 Figure S6: SLC38A9.1 is a low-affinity amino acid transporter. D C B A 4000$2000, 1000. '10 /OPqt?~/ Transfectod J~~~%~. pH PH5 H F 0001 60-0 tin- 40- SLC36A9 LAMPISLC3&A. I FLA4-SLM3AS . ,0 pH 5 pH - . s 20so- SLOWV 0-20 Transfected cDNA: empty vector SLC38A9.1 SLC38A2 1s- G fraction from top of sucrose gradient: 1 2 3 4 5 6 7 8 9 10 11 12 FLAG-SLC38A9.1 proteollposomes FLAG-sLC38A9.1 protein only FLAG-SLC36A9.1 + I FLAG-LAMP1 lposomes proteolIposomS liposomes * WM Urea 3W0- E 82000F 1000- . FLAG-sLC38A9.1 + 0.5 1.0 1.5 2.0 Elution volume (mL) - Buffer only I+ Uposomes only 3 [ HJArg + + SLC38A9.1 proteoliposomes +0LAMP1 proteoliposomes 112 Figure S1: Membrane topology of SLC38A9.1. (A) Representation of the TMHMM topology prediction for SLC38A9.1. (B) Visualization of SLC38A9.1 topology as generated by Protter. Figure S2: Ragulator and the Rag GTPases do not interact with all lysosomal amino acid transporter-like proteins. (A) SLC38A9.1, but not SLC38A7 or SLC36A1, interacts with the Ragulator complex and the Rag GTPases. HEK-293T cells were transfected with the indicated cDNAs in expression vectors and lysates were prepared and subjected to FLAG immunoprecipitation followed by immunoblotting for the indicated proteins. (B and C) The interaction with Ragulator requires the presence of the intact Nterminal domain of SLC38A9.1, which is lacking in SLC38A9.2 (B), SLC38A9.1 A110 (C), and SLC38A9.4 (C). HEK-293T cells were transfected with the indicated cDNAs in expression vectors and processed as in (A). Figure S3: Localization of SLC38A9 isoforms 2 and 4 and signaling effects of siRNAmediated SLC38A9 knockdown. SLC38A9 isoforms lacking part (A) or all (B) of the Nterminal region of SLC38A9.1 still localize to the lysosomal membrane. HEK-293T cells stably expressing the indicated FLAG-tagged SLC38A9 isoforms were immunostained for FLAG and LAMP2. (C) The interaction between SLC38A9.1 and Ragulator occurs only when Ragulator is anchored at the lysosomal membrane through lipidation of the Nterminus of p18. Ragulator containing the lipidation-deficient p 1 8 G2A mutant fails to interact with SLC38A9.1. HEK-293T cells were transfected with the indicated cDNAs in expression vectors and lysates prepared and subjected to FLAG immunoprecipitation followed by immunoblotting for the indicated proteins. (D) Knockdown of SLC38A9 in HEK293T cells with a pool of short interfering RNAs suppresses the phosphorylation of S6K1. Figure S4: (A) Transient overexpression of SLC38A9.1, but not truncation mutants lacking the N-terminal Ragulator-binding domain, makes the mTORCI pathway insensitive to amino acid starvation. Cell lysates were prepared from HEK-293T cells deprived for 50 min for amino acids and, then, where indicated, stimulated with amino acids for 10 min. Cell lysates and FLAG immunoprecipitates were analyzed for the levels of the specified proteins and for the phosphorylation state of S6K1. (B) Stable overexpression of SLC38A9.1 in HeLa cells, LN229 cells, and MEFs makes the 113 mTORC1 pathway partially resistant to amino acid deprivation. Cells transduced with retroviruses encoding the specified proteins were deprived for 50 min of all amino acids and, where indicated, stimulated for 10 min with amino acids. Cell lysates were analyzed for the levels of the specified proteins and the phosphorylation state of S6K1. (C) Stable overexpression of SLC38A9.1 suppresses autophagy induction upon arginine starvation as indicated by detected by p62 accumulation and suppressed LC3 degradation. HEK293T cells stably overexpressing FLAG-SLC38A9.1 were simultaneously deprived of arginine and, where indicated, treated with 30 uM chloroquine for the indicated time. Cell lysates were analyzed for the levels of the specified proteins and the phosphorylation state of S6K1. (D) Stable overexpression of SLC38A9.1 in HEK-293E cells does not perturb the response of mTORC1 signaling to serum starvation and insulin stimulation. (E) Stable overexpression of SLC38A9.1 does not protect mTORCI signaling from the inhibitory effects of MK2206, which blocks growth factor signaling by allosterically inhibiting Akt. Figure S5: Endogenous immunoprecipitation of Rag and Ragulator components recovers SLC38A9 in an amino acid-sensitive fashion. Cell lysates were prepared from HEK-293T cells deprived for 50 min for amino acids and, then, where indicated, stimulated with amino acids for 10 min. Cell lysates as well as control, p18, RagA, and RagC immunoprecipitates were analyzed for the levels of the indicated endogenous proteins. Figure S6: SLC38A9.1 is a low-affinity amino acid transporter. (A) Immunostaining of HEK-293T cells transiently overexpressing SLC38A9.1 at levels that cause spillover to the plasma membrane. These cells were used for whole-cell amino acid transport assays and amino acid-induced current recordings. HEK-293T cells transiently expressing indicated cDNAs were incubated with [1 4C]arginine (B), [1 4C]amino acid mix (C), or [ 1 4C]leucine (D) containing buffer at the indicated pH and washed before harvested for scintillation counting. (E) (Left) Whole-cell recordings from HEK-293T cells expressing indicated cDNAs at -80 mV. Quantified is the change in steady-state current following local application of 2.4 mM arginine, 1.6 mM leucine, and 4 mM glutamine (4x DMEM concentrations). All recordings were performed at pH 5.5. Statistical comparison was performed by Kruskall-Wallis test, followed by Dunn's test. (Right) Representative examples of individual recordings. Grey bars indicate application of amino acids. (F) 114 Coomassie stain of FLAG-affinity purified LAMP1 or SLC38A9.1 from HEK-293T cells stably expressing respective protein. (G) Floatation assay shows successful insertion of SLC38A9.1 into proteoliposomes. Where indicated, 6 M urea was added following the reconstitution reaction. (H) SLC38A9.1 is unidirectionally inserted into proteoliposomes, with the N-terminus facing the outside of liposomes. Proteoliposomes containing Nterminally FLAG-tagged SLC38A9.1 were exposed to trypsin and immunoblotted for FLAG. The addition of 1% Triton X-100 did not reveal any protected FLAG-tagged fragments. (1) SLC38A9.1 proteoliposomes uptake [ 3H]arginine. 0.5 pM [ 3H]arginine was incubated with the indicated components for 60 min. and the reaction was applied to a column that traps free amino acids. Proteoliposomes pass through the column and fractions were subjected to scintillation counting and FLAG immunoblotting. To recapitulate the pH gradient across the lysosomal membrane, the lumen of the proteoliposomes is buffered at pH 5.0, while the external buffer is pH 7.4. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. Y. Sancak et al., PRAS40 is an insulin-regulated inhibitor of the mTORC1 protein kinase. Molecular cell 25, 903 (Mar 23, 2007). Y. Sancak et al., The Rag GTPases bind raptor and mediate amino acid signaling to mTORC1. Science 320, 1496 (Jun 13, 2008). Z. Zhang, A. Gameiro, C. Grewer, Highly conserved asparagine 82 controls the interaction of Na+ with the sodium-coupled neutral amino acid transporter SNAT2. The Journal of biological chemistry 283, 12284 (May 2, 2008). B. Liu, H. Du, R. Rutkowski, A. Gartner, X. Wang, LAAT-1 is the lysosomal lysine/arginine transporter that maintains amino acid homeostasis. Science 337, 351 (Jul 20, 2012). T. A. Pologruto, B. L. Sabatini, K. Svoboda, Scanimage: flexible software for operating laser scanning microscopes. Biomedical engineering online 2, 13 (May 17, 2003). C. Zhao, W. Haase, R. Tampe, R. Abele, Peptide specificity and lipid activation of the lysosomal transport complex ABCB9 (TAPL). The Journal of biological chemistry 283, 17083 (Jun 20, 2008). J. L. Rigaud, D. Levy, Reconstitution of membrane proteins into liposomes. Methods in enzymology 372, 65 (2003). J. J. Wuu, J. R. Swartz, High yield cell-free production of integral membrane proteins without refolding or detergents. Biochimica et biophysica acta 1778, 1237 (May, 2008). A. Nohturfft, M. S. Brown, J. L. Goldstein, Topology of SREBP cleavage-activating protein, a polytopic membrane protein with a sterol-sensing domain. The Journal of biological chemistry 273, 17243 (Jul 3, 1998). F. A. Ran et al., Genome engineering using the CRISPR-Cas9 system. Nature protocols 8, 2281 (Nov, 2013). 115 Figure S1: Membrane topology of SLC38A9.1. (A) Representation of the TMHMM topology prediction for SLC38A9.1. (B) Visualization of SLC38A9.1 topology as generated by Protter. Figure S2: Ragulator and the Rag GTPases do not interact with all lysosomal amino acid transporter-like proteins. (A) SLC38A9.1, but not SLC38A7 or SLC36A1, interacts with the Ragulator complex and the Rag GTPases. HEK-293T cells were transfected with the indicated cDNAs in expression vectors and lysates were prepared and subjected to FLAG immunoprecipitation followed by immunoblotting for the indicated proteins. (B and C) The interaction with Ragulator requires the presence of the intact Nterminal domain of SLC38A9.1, which is lacking in SLC38A9.2 (B), SLC38A9.1 A110 (C), and SLC38A9.4 (C). HEK-293T cells were transfected with the indicated cDNAs in expression vectors and processed as in (A). Figure S3: Localization of SLC38A9 isoforms 2 and 4 and signaling effects of siRNAmediated SLC38A9 knockdown. SLC38A9 isoforms lacking part (A) or all (B) of the Nterminal region of SLC38A9.1 still localize to the lysosomal membrane. HEK-293T cells stably expressing the indicated FLAG-tagged SLC38A9 isoforms were immunostained for FLAG and LAMP2. (C) The interaction between SLC38A9.1 and Ragulator occurs only when Ragulator is anchored at the lysosomal membrane through lipidation of the Nterminus of p18. Ragulator containing the lipidation-deficient p 1 8 G2A mutant fails to interact with SLC38A9.1. HEK-293T cells were transfected with the indicated cDNAs in expression vectors and lysates prepared and subjected to FLAG immunoprecipitation followed by immunoblotting for the indicated proteins. (D) Knockdown of SLC38A9 in HEK293T cells with a pool of short interfering RNAs suppresses the phosphorylation of S6K1. Figure S4: (A) Transient overexpression of SLC38A9.1, but not truncation mutants lacking the N-terminal Ragulator-binding domain, makes the mTORCI pathway insensitive to amino acid starvation. Cell lysates were prepared from HEK-293T cells deprived for 50 min for amino acids and, then, where indicated, stimulated with amino acids for 10 min. Cell lysates and FLAG immunoprecipitates were analyzed for the levels of the specified proteins and for the phosphorylation state of S6K1. (B) Stable 116 overexpression of SLC38A9.1 in HeLa cells, LN229 cells, and MEFs makes the mTORC1 pathway partially resistant to amino acid deprivation. Cells transduced with retroviruses encoding the specified proteins were deprived for 50 min of all amino acids and, where indicated, stimulated for 10 min with amino acids. Cell lysates were analyzed for the levels of the specified proteins and the phosphorylation state of S6K1. (C) Stable overexpression of SLC38A9.1 suppresses autophagy induction upon arginine starvation as indicated by detected by p62 accumulation and suppressed LC3 degradation. HEK293T cells stably overexpressing FLAG-SLC38A9.1 were simultaneously deprived of arginine and, where indicated, treated with 30 uM chloroquine for the indicated time. Cell lysates were analyzed for the levels of the specified proteins and the phosphorylation state of S6K1. (D) Stable overexpression of SLC38A9.1 in HEK-293E cells does not perturb the response of mTORC1 signaling to serum starvation and insulin stimulation. (E) Stable overexpression of SLC38A9.1 does not protect mTORC1 signaling from the inhibitory effects of MK2206, which blocks growth factor signaling by allosterically inhibiting Akt. Figure S5: Endogenous immunoprecipitation of Rag and Ragulator components recovers SLC38A9 in an amino acid-sensitive fashion. Cell lysates were prepared from HEK-293T cells deprived for 50 min for amino acids and, then, where indicated, stimulated with amino acids for 10 min. Cell lysates as well as control, p18, RagA, and RagC immunoprecipitates were analyzed for the levels of the indicated endogenous proteins. Figure S6: SLC38A9.1 is a low-affinity amino acid transporter. (A) Immunostaining of HEK-293T cells transiently overexpressing SLC38A9.1 at levels that cause spillover to the plasma membrane. These cells were used for whole-cell amino acid transport assays and amino acid-induced current recordings. HEK-293T cells transiently expressing indicated cDNAs were incubated with [1 4C]arginine (B), [14 C]amino acid mix (C), or [ 14C]leucine (D) containing buffer at the indicated pH and washed before harvested for scintillation counting. (E) (Left) Whole-cell recordings from HEK-293T cells expressing indicated cDNAs at -80 mV. Quantified is the change in steady-state current following local application of 2.4 mM arginine, 1.6 mM leucine, and 4 mM glutamine (4x DMEM concentrations). All recordings were performed at pH 5.5. Statistical comparison was performed by Kruskall-Wallis test, followed by Dunn's test. (Right) Representative 117 examples of individual recordings. Grey bars indicate application of amino acids. (F) Coomassie stain of FLAG-affinity purified LAMP1 or SLC38A9.1 from HEK-293T cells stably expressing respective protein. (G) Floatation assay shows successful insertion of SLC38A9.1 into proteoliposomes. Where indicated, 6 M urea was added following the reconstitution reaction. (H) SLC38A9.1 is unidirectionally inserted into proteoliposomes, with the N-terminus facing the outside of liposomes. Proteoliposomes containing Nterminally FLAG-tagged SLC38A9.1 were exposed to trypsin and immunoblotted for FLAG. The addition of 1% Triton X-100 did not reveal any protected FLAG-tagged fragments. (1) SLC38A9.1 proteoliposomes uptake [ 3H]arginine. 0.5 pM [ 3H]arginine was incubated with the indicated components for 60 min. and the reaction was applied to a column that traps free amino acids. Proteoliposomes pass through the column and fractions were subjected to scintillation counting and FLAG immunoblotting. To recapitulate the pH gradient across the lysosomal membrane, the lumen of the proteoliposomes is buffered at pH 5.0, while the external buffer is pH 7.4. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. Y. Sancak et al., PRAS40 is an insulin-regulated inhibitor of the mTORC1 protein kinase. Molecular cell 25, 903 (Mar 23, 2007). Y. Sancak et aL., The Rag GTPases bind raptor and mediate amino acid signaling to mTORC1. Science 320, 1496 (Jun 13, 2008). Z. Zhang, A. Gameiro, C. Grewer, Highly conserved asparagine 82 controls the interaction of Na+ with the sodium-coupled neutral amino acid transporter SNAT2. The Journal of biological chemistry 283, 12284 (May 2, 2008). B. Liu, H. Du, R. Rutkowski, A. Gartner, X. Wang, LAAT-1 is the lysosomal lysine/arginine transporter that maintains amino acid homeostasis. Science 337, 351 (Jul 20, 2012). T. A. Pologruto, B. L. Sabatini, K. Svoboda, Scanimage: flexible software for operating laser scanning microscopes. Biomedical engineering online 2,13 (May 17, 2003). C. Zhao, W. Haase, R. Tampe, R. Abele, Peptide specificity and lipid activation of the lysosomal transport complex ABCB9 (TAPL). The Journal of biological chemistry 283, 17083 (Jun 20, 2008). J. L. Rigaud, D. Levy, Reconstitution of membrane proteins into liposomes. Methods in enzymology 372, 65 (2003). J. J. Wuu, J. R. Swartz, High yield cell-free production of integral membrane proteins without refolding or detergents. Biochimica et biophysica acta 1778, 1237 (May, 2008). A. Nohturfft, M. S. Brown, J. L. Goldstein, Topology of SREBP cleavageactivating protein, a polytopic membrane protein with a sterol-sensing domain. The Journal of biological chemistry 273, 17243 (Jul 3,1998). F. A. Ran et al., Genome engineering using the CRISPR-Cas9 system. Nature protocols 8, 2281 (Nov, 2013). 118 CHAPTER 4: Future Directions and Discussions 1. The Rag Heterodimer The Rag GTPases are unusual in that they function as obligate heterodimers whereas most Ras-like GTPases are typically monomeric. This heterodimeric state is conserved from yeast to human. Why do the Rag GTPases function as heterodimers? Monomeric GTPases have two states-either GTP or GDP loaded. Therefore, a heterodimeric configuration affords four states. In cells, RagA/B must be bound by GTP for the Rag heterodimer to bind mTORC1, but the RagA/B-(GTP) - RagC/D-(GDP) heterodimer exhibits greatest mTORC1 binding (Sancak et al., 2008). In contrast, in vitro, RagC/D loaded with GDP is sufficient for the Rag heterodimer to bind mTORC1, suggesting that RagC/D is the primary determinant of mTORC1 binding (Tsun 2013). The fact that RagA/B-(GDP) - RagC/D-(GDP) does not bind mTORC1 in cells suggests that there must be other factors in cells that are not accounted for in vitro or that RagA/B-(GDP) is dominant over RagC/D nucleotide state. For example, in cells the Rags must both bind mTORC1 and localize to the lysosome. Interestingly RagA/B-(GDP), or amino acid starvation, shows weaker Rag interactions with Ragulator, its lysosomal scaffold, suggesting that the Rag heterodimers may dynamically localize to the lysosome. Although by immunofluorescence the Rags appear lysosomal, this static image does not provide information about the level of Rag turnover. Comparison of fluorescence recovery after photobleaching (FRAP) of photobleached lysosomes in cells expressing fluorescently tagged Rags, under amino acid starved versus stimulated state, will test this possibility. It would be ideal to use endogenously tagged Rags to avoid overexpression artifacts, especially because careful measurements of turnover will likely be required. If true, it could mean that RagA/B nucleotide state regulates lysosomal docking, whereas RagC/D regulates mTORC1 binding. If RagA/B is in the GDP state, it can never leave the lysosome and thus cannot bind mTORC1 in cells, regardless of RagC/D nucleotide state. Another possibility is that each Rag within the heterodimer can affect the nucleotide state of the other, as seen in the heterodimeric GTPases, signal recognition particle (SRP) and its receptor (SR) (Saraogi et al., 2011). 119 1I. Lysosomal amino acid concentrations in human cells The broad substrate profile and high Km (-40mM) of SLC38A9 raises several important questions. Given that intracellular concentrations of arginine are -100uM, how is SLC38A9 relevant for sensing arginine? We know that leucine and arginine are important for mTORC1 activity, yet loss of SLC38A9 seems to specifically affect mTORC1 activation by arginine. Given that a growth pathway should monitor the total cellular nutrient content, our current model proposes that the Rag GTPases integrate multiple amino acid inputs from both the lysosomal and cytosolic compartments (Fig. 1). SLC38A9 may be responsible for reporting lysosomal amino acid content, where arginine, more than any other amino acid, has been reported to be highly enriched (Harms et al., 1981). Thus, despite the broad substrate profile of SLC38A9, perhaps concentrations of no other lysosomal amino acid besides arginine reach its Km. v-ATPase amino AClds cytosol SLC38A9 lysosomal membrane lysosomal lumen amino acids Figure 1: SLC38A9 is a candidate amino acid sensor. Model for distinct amino acids inputs in the mTORC1 pathway To test this model, it will be necessary to measure lysosomal amino acid concentrations in human cells, which will require quantifying lysosomal amino acids as well as obtaining the lysosomal volume. Using the immunopurification method developed in the lab, capturing lysosomes using an epitope-tagged lysosomal transmembrane protein (Zoncu et al., 2011), it should be feasible to isolate lysosomes quickly for metabolite profiling. To measure lysosomal volume, a quick estimate would be to quantify the volume occupied by lysosomal membrane stain in confocal images, but of course this will be diffraction limited. Because lysosomes range from 0.1 - 1.2 um in diameter, super-resolution imaging of a lysosomal dye such as Lysotracker will obtain a more accurate 120 measurement. Given the lysosomal localization of many mTORC1 pathway components, this method will be instrumental in understanding how this pathway is regulated by amino acids and how lysosomal contents change in normal physiology and disease. Ill. Nutrient sensing in the compartmentalized cell The emerging picture is that the lysosome is a signal integration hub for the mTORC1 growth pathway. How did the mTORC1 pathway end up anchoring at the lysosome? What is the significance of the lysosomal surface? Fundamentally, we think the TOR pathway had to solve the problem of nutrient sensing in a compartmentalized cell, in which membrane bound compartments are used for storage. In prokaryotes, there is a single cytoplasmic compartment and no organelles for storage. If extracellular nutrients became limiting, the cell had to either stopped growing or perform the biosynthetic reactions to make the things it needs. Prokaryotes don't have a TOR pathway (van Dam et al., 2011). With the exception of malaria and microsporidium, both parasites, the TOR pathway can be found in all eukaryotes, which rely on membrane compartmentalization (van Dam et al., 2011). The lysosome or vacuole in yeast and plants are the major storage site for amino acids (Klionsky et al., 1990). The localization of TOR to this compartment is conserved from yeast to human (Dubouloz et al., 2005; Sancak et al., 2010). Now, when extracellular amino acids become limiting, growth doesn't need to stop if the cell has large amino acid stores. To make that decision, the cell requires a system like the TOR pathway that could regulate growth based on the availability of amino acids in both compartments: the lysosome and cytoplasm. And the lysosomal surface is an ideal place for this because it's at the interface between these two compartments (Fig. 2). There is increasing evidence that both cytosolic and lysosomal events are amino acid regulated. Zoncu et al, showed that amino acids have to be concentrated within isolated lysosome in order for mTORC1 to localize to the lysosomal surface, indicating that there is inside-out signaling of amino acids (Zoncu et al., 2011). On the cytoplasmic side, the FLCN-FNIP complex lysosomal localization is amino acid responsive and so is the sestrin-GATOR2 interaction (Lynne et al., 2014; Tsun et al., 2013). 121 Growth factors Figure 2: Integration of cytosolic and lysosomal amino acid inputs, as well as growth factor signaling, at the lysosomeal surface. With emergence of multicellular life, there was a need for growth factor based regulation. Nutrient sensing is the more ancestral branch and it has remained here from yeast to human so growth factor signaling likely represented another input that need to be integrated at the lysosome. 122 References Dubouloz, F., Deloche, 0., Wanke, V., Cameroni, E., and De Virgilio, C. (2005). The TOR and EGO protein complexes orchestrate microautophagy in yeast. Molecular cell 19, 15-26. Harms, E., Gochman, N., and Schneider, J.A. (1981). Lysosomal pool of free-amino acids. Biochemical and biophysical research communications 99, 830-836. 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