AN ABSTRACT OF THE THESIS OF Mohammad Farhad for the degree of Master of Science in Microbiology presented on May 21, 2013. Title: The Role of Salmonella typhimurium Type Three Secretion System (T3SS) and Effector Proteins in Chromatophore Cell Response. Abstract approved: Janine E. Trempy Bacterial contamination of food poses a great risk to human health worldwide. A chromatophore cell-based biosensor, utilizing B. splendens erythrophore cells, is an emerging technology that has shown potential to detect bacterial toxicity based on function-dependent mechanisms. Previous studies have investigated the response of erythrophore cells to foodborne pathogens, pesticides, and environmental toxicants. Numerous studies reveal that the chromatophore cell type, erythrophore, can rapidly detect, by aggregating their pigment organelles, several food associated bacterial pathogens, including Salmonella typhimurium. This study describes the Betta splendens erythrophore cells response to Salmonella typhimurium, including an analysis of the bacterial mechanism(s) that may be involved in this response. Previous studies using mutagenesis, identified genes of S. typhimurium that contributed to a response in erythrophore cells. The results indicated a potential role for the Type Three Secretion System (T3SS) apparatus coded for by the prgHIJK operon. In the current study, a mutation was identified in a region different from the mutation that disrupted the prgHIJK operon. However, both mutantions induced a similar but not identical response in erythrophore cells. The first objective of this study was to test the hypothesis that this second S. typhimurium (ST10) mutant has a mutation residing in either the gene(s) coding for the process regulating expression of the prgHIJIK operon or the gene(s) coding for the effector proteins secreted by the PrgHIJK apparatus. The S. typhimurium (ST10) mutant contained an insertional mutation in the hilD gene, a regulator involved in regulating the expression of the prgHIJK operon. Failure to express hilD in S. typhimurium impacts pigment organelle movement in erythrophore cells. The second objective of this study was to test the hypothesis that the effector proteins of T3SS (SipA, SopB, SopE2, SptP) are the components of S. typhimurium’s invading mechanism directly involved in inducing pigment organelles to undergo an aggregative response in erythrophore cells. Mutations in sopE2, sipA, or sptP did not change the erythrophore cell response to S. typhimurium as the magnitude and kinetics of the response was similar to that observed with wildtype S. typhimurium. A mutation in the sopB gene that encodes the SopB effector protein, which is involved in actin filament rearrangement, did change erythrophore cell response to S. typhimurium as the magnitude and kinetics of the response was different to that observed for the wildtype S. typhimurium. This is the first evidence in support of a direct role for the S. typhimurium SopB effector protein in pigment organelle aggregation in erythrophore cells. Results from this research effort suggest that hilD and sopB genes of S. typhimurium are involved in pigment organelle movement in a neuron-like pigment cell, an erythrophore cell of the chromatophore cell classification, isolated from the fish species, Betta splendens. The outcome to this research effort is to increase understanding of the biological basis of the erythrophore cell response to bacterial pathogens. Increased understanding will lead to better utility of erythrophore cells as biosensors for bacterial toxicity testing. © Copyright by Mohammad Farhad May 21, 2013 All Rights Reserved The Role of Salmonella typhimurium Type Three Secretion System (T3SS) and Effector Proteins in Chromatophore Cell Response. by Mohammad Farhad A THESIS submitted to Oregon State University in partial fulfillment of the requirements for the degree of Master of Science Presented May 21, 2013 Commencement June 2013 Master of Science thesis of Mohammad Farhad presented on May 21, 2013 APPROVED: Major Professor, representing Microbiology Chair of the Department of Microbiology Dean of the Graduate School I understand that my thesis will become part of the permanent collection of Oregon State University libraries. My signature below authorizes release of my thesis to any reader upon request. Mohammad Farhad, Author ACKNOWLEDGMENTS I would like to express my appreciation to my Major Professor, Dr. Janine Trempy, for her commitment, support and guidance in overcoming obstacles throughout my undergraduate and graduate academic career. Her contribution was not limited to my education. She made sure I preserved my culture, kept my long-term goals in sight and persevered through difficulties in my personal life. Working in her laboratory has been a life changing experience. I would also like to thank my committee members Dr. Bruce Geller, Dr. Martin Schuster and Dr. Jerry Heidel. It was an honor to work with Dr. Karen P. Dierksen. I have been lucky to benefit from her vast scientific knowledge and technical expertise. She was my primary source for overcoming experimental and scientific complications in the laboratory. She is kind and has incredible amount of patience. Her guidance and help was vital in finishing my graduate studies. I would like to thank all the Trempy lab members, especially Roberto Garcia and Holly Roach, with whom I had the honor to work side by side and for their friendship and support. I also would like to thank a previous graduate student in Dr. Trempy’s research program, Dr. Stephanie Dukovcic, whose prior research efforts in this laboratory helped me form new hypotheses, design experiments and interpret results. I would like to thank the Department of Microbiology and Dr. Janine Trempy for the financial support in completing my degree. I would like to thank Dr. Garry L. Adams in the College of Veterinary Medicine at Texas A&M University for providing me with Salmonella typhimurium effector protein mutant strains. I would like to thank the people who I love and cherish since I have come to the United States in pursuit of my education. I would like to say thank you to Mike Manaton for his unconditional love, support and encouragement. He has been an inspiration for me. I would not have made it to the United State if it was not for him. I would also like to thank my best friend, Jolie Drion for her love and support in times of stress and getting homesick. Finally, I would like to thank my family: my mother, my father, my sisters and brothers. I have been blessed to be part of a family so loving, strong, and wise. Thank you for believing in me. I would never forget your sacrifice. Mom and Dad: thank you for giving me the permission to come to the United State to study; I can not imagine how much pain and worry you have endured because of me being away from home. Sisters: thank you for being the best sisters in the world. Brothers: you are my heroes. You guys have provided me with everything to ease my journey of getting my education. Words cannot express my gratitude for all my family has done for me. CONTRIBUTION OF AUTHORS Dr. Janine E. Trempy and Dr. Karen P. Dierksen collaborated in experimental design, interpretation of results and editing of this manuscript. Dr. Karen P. Dierksen assisted in the laboratory preparation for experiments. Dr. Stephanie Dukovcic created the Salmonella typhimurium mutants. Holly Roach assisted in fish care as well as preparation and maintenance of Betta splendens chromatophore cell tissue cultures. Roberto Garcia assisted in general laboratory procedures necessary for this research effort. All the experiments in this study were conducted in Dr. Janine E. Trempy’s research program. TABLE OF CONTENTS Page 1. Introduction……………..…........................................................................................ 1 2. Literature Review…..................................................................................................... 3 Part 1: Food Associated Illnesses and Salmonella enterica................................. 3 Foodborne Illness…………….……………................................ 3 Salmonella Associated Foodborne Illnesses……….................... 4 Salmonella enterica……........................…………………….…. 5 Salmonella enterica servovar Typhimurium Pathogenesis…….. 7 Salmonellla Pathogenicity Islands………………………....…....10 Adhesion…………………………………………………….…..12 Invasion...………………………………………………………..13 SCV Maturation………………………………………………....15 Gram-negative Secretion system ……………………………….15 Type III Secretion System………………………………………17 Salmonella T3SS-1 Apparatus…………………………………..18 SPI-1 T3SS Secreted Effector proteins………………………….19 Part 2: Dectection Metohds and Chromatophore Cell-based Biosensors……….22 Detection Methods for Bacterial Pathogesn……………….….…22 Immunology-based Methods……………………………..……...23 Polymerase Chain Reaction-based Methods………………..…...24 Biosensors…………………………………………………..…...25 Chromatophore Cell-based Biosensor……………………….….26 TABLE OF CONTENTS (Continued) Page Chromatophore Cells and Pigmentation……………………….. 27 Betta splendens………………………………………………….30 Research Objectives……………………………………………………………..33 3. Materials and Methods…………..…………………………………………………....35 Fish Care…………………………………………………………….…………..35 Cell Culture…………………………………………………………….………..35 Response Assay and Computational Analysis…………………………………..38 Bacterial Growth Conditions…………………………………………………....39 Polymerase Chain Reaction (PCR).……………………………………………..41 Bacterial Transformations……………………………………………………….42 Identifying Transposome™ Insertion Site(s) and Sequencing…………….……46 Complementation…………………………………………………………….….46 4. Results..……………………………………………………………..............….……..49 The Physiological Response of Betta splendens Erythrophore Cells...................49 Betta Splendens Erythrophore Cell Response To Wildtype Salmonella Typhimurium And Salmonella Typhimurium ST10 Mutant.............................................................................................52 Identification Of hilD Gene Product And Complementation of hild Function........................................................................................55 Erythrophore Cell Response To Salmonella Typhimurium Wildtype, ST10 Mutant, ST10-pTA108 And ST10-pTA108-hilD............................58 TABLE OF CONTENTS (Continued) Page Betta Splendens Erythrophore Cell Response To Salmonella typhimurium Human Isolate And Salmonella typhimurium Bovine Isolate...................................................62 Betta Splendens Erythrophore Cell Response To Salmonella typhimurium With Mutations In Effector Protein SopE2, SipA, Or SptP Genes........................................................64 Betta Splendens Erythrophore Cell Response To Salmonella typhimurium With Mutations In Effector Protein SopB Or SipB/SopB Genes.............................................66 5. Discussion…………………………………………………………….……...............68 The Response Betta Splendens Erythrophore Cells To Salmonella typhimurium ST10 Mutant......................................................68 Salmonella typhimurium ST10 Mutant Complementation....................................73 Betta Splendens Erythrophore Cells Response To Salmonella typhimurium Effector Protein Mutants...................................75 Future Directions For This Research Effort...........................................................82 6. Conclusion.……………………………………………………….............…….……..83 7. Bibliography…………..………………………………………….............…….……..86 Appendix…………..………………………….…………………….............…….…….109 Biographical Information…………..……………………….............…….…….110 LIST OF FIGURES Figure Page 1. Betta splendens erythrophore cell response to Clonidine, MSH, and LB…...………………………………………………...….51 2. Betta splendens erythrophore cell response to wildtype Salmonella typhimurium and Salmonella typhimurium ST10 mutant. …………..….……………………..…….………… 54 3. Identification of the hilD gene……….………….………………………….……..…. 56 4. Cloning complementation of hilD gene ………………………………...….…….….. 57 5. Betta splendens erythrophore cell response to wildtype Salmonella typhimurium, Salmonella typhimurium ST10 mutant, ST10 containing pTA108, and ST10 containing pTA108-hilD (60 minutes) ……….……………………....……..….. 59 6. Betta splendens erythrophore cell response to wildtype Salmonella typhimurium, Salmonella typhimurium ST10 mutant, ST10 containing pTA108, and ST10 containing pTA108-hilD (90 minutes) ……….………………..…….……..….. 61 7. Betta splendens Chromatophore Cell Response to Salmonella typhimurium wildtype (human isolate) and Salmonella typhimurium wildtype (bovine isolate)..……………….……….….. 63 LIST OF FIGURES (Continued) Figure Page 8. Betta splendens erythrophore cell response to wildtype Salmonella typhimurium bovine isolate and specific effector protein mutants with mutations in sopE2, sipA, or sptP.….……….….. 65 9. Betta splendens erythrophore cell response to wildtype Salmonella typhimurium bovine isolate and specific effector protein mutants with mutations in sopB and sipA/sopB…...........................................................................................................67 10. Salmonella Pathogenicity Island 1 (SPI-1) Genetic Organization...............................70 11. A model of transcriptional regulation of SPI-1............................................................72 12. A hypothetical model as to how S. typhimurium might enter an erythrophore cell....................................................................................................81 LIST OF TABLES Table Page 1. Bacterial Strains and Plasmids used in this study…………………………….………41 2. Primers used in this study……...……………….………………………….…………43 For my Family Chapter 1 Introduction Bacterial and environmental toxicant contamination of food has been, and continues to be a threat to human health worldwide. Developing rapid and accurate methods to detect bacterial and viral pathogens in contaminated food is important for human health. In recent years, cell based biosensors, living cells that detect the presence of biological and chemical toxicants, have become the main focus of researchers (19, 192). The chromatophore cell-based biosensor is an emerging biosensor that has shown the potential to detect contaminants based on function-dependent mechanisms (202, 204, 207, 208, 231, 237, 238). Function-dependent mechanisms give the chromatophore cellbased biosensor the ability to respond to biological (a viable pathogen or associated toxins) and environmental stimulants (heavy metals, chemical) in a physiological manner that can be measured. Thus, this type biosensor overcomes the limitation of other molecular and immunology based methods. Chromatophore cell-based biosensors utilize a class of pigmented neuron-like cells called chromatophores. These cells are capable of moving their intercellular pigment organelles upon exposure to physiological stimuli. This property has made chromatophore cells valuable for their use in a detection system solely based on biological activity. Induction of pigment granule movement in chromatophore cells due to disrupted intracellular functions in response to different biological stimuli is measured and analyzed to assess the toxicity of a pathogen, whereas other detection methods can 2 only assess the presence but not toxicity of a pathogen (207, 208, 209). These pigment movements could be toward the peri-nucleus of the cell called aggregation or outward to the periphery of the cell called dispersion (208, 209). The degree, magnitude, and kinetics of chromatophore cell responses (aggregation and dispersion) vary depending on the different pathogens and toxic stimuli (208, 209). The similarity of chromatophore cells to neuron cells of other animal makes them of interest in detecting biological substances of concern to human health (210, 209). Betta splendens erythrophore cells have been used as cell-based biosensors for the detection of chemicals, bacterial exotoxins, pesticides, Gram-positive foodborne bacteria and more recently, Gram-negative foodborne bacteria (204, 207, 209, 231). More studies are essential to better understand the mechanism by which the Gram-negative bacterium, Salamonella typhimurium, triggers the response in B. splendens erythrophore cells. The objective of this study is to further investigate and increase our knowledge of B. splendens erythorophores for the detection of S. typhimurium. 3 Chapter 2 Literature Review The literature review chapter consists of two parts. The first part covers a brief introduction to food associated illness, and a much greater emphasis on the current understanding of Salmonella typhimurium pathogenesis. The second part briefly discusses different bacterial detection methods and focuses on the chromatophore cellbased biosensor. Part1: Food Associated Illnesses and Salmonella enterica Foodborne Illness Although detection technology has advanced, food associated illness caused by bacterial and viral contamination of food poses a significant global health concern. Each year in the United States, 5000 people die, 128,000 are hospitalized and 48 million report illness as a result of foodborne illness (232). The reported numbers of illnesses correspond to 17% of the U.S. population, which is remarkable considering the U.S. food supply is considered one of the safest in the world. The World Health Organization recently put forth an initiative to estimate the global burden of foodborne diseases (233). Not only is it difficult to estimate the global burden of foodborne diseases, it is also difficult to estimate the global incidence of foodborne diseases. Globally, diarrheal diseases are the leading cause of mortality and morbidity in children, with bacterial contaminated food and water being one of the major contributors to global diarrhoeal 4 diseases (234). The bacterial species of prime concern include Salmonella sp., Bacillus cereus, Campylobacter jejuni, Escherichia coli-producing toxin (including 0157:H7), Listeria monocytogenes, Clostridium perfringens, Shigella sp., Staphylococcus aureus, Vibrio parahaemolyticus, and Vibrio vulnificus (232). Salmonella Associated Foodborne Illnesses Salmonella enterica subspecies serovars are estimated to cause 1.3 billion cases of illness worldwide including 3 million deaths due to non-typhoidal Salmonella annually. Intestinal disease due to non-typhoidal Salmonella species is highest in third world countries but non-typhoidal Salmonella is also of concern in developing countries (1). Salmonella enterica subspecies are typically orally acquired pathogens that result in typhoid fever, diarrhea, bacteremia and chronic asymptomatic carriage (2). In the United States, Salmonella enterica causes about 1.4 million cases of salmonellosis, 19,586 hospitalizations, 378 deaths among humans and an economic loss of around $3.3 billion annually (3, 239, 240). Ingestion of more than 5x104 Salmonella in contaminated water or food will cause salmonellosis. Acute, crampy, abdominal pain and diarrhea with or without blood are salmonellosis symptoms that occur between 6 and 72 hours after ingestion. Other common symptoms are fever, nausea, and vomiting. Salmonellosis usually occurs in the ileum of the small intestine but it also causes inflammation in the large bowel, with rare infections in the jejunum, duodenum and stomach (7, 8). Salmonella is a major concern for the food industry. Salmonella is found in 5 poultry, uncooked meat, fish, shellfish and natural environments. Eradicating Salmonella from food processing environments and products has been a challenging task (10). Cattle infected with Salmonella can excrete up to 108 CFU/g of feces, which becomes the main source of further contamination of the environment and other uninfected animals. Cattle that are active carriers of Salmonella do not exhibit clinical symptoms, however they are able to excrete Salmonella in their feces. Contaminated feces is a problem in food production especially when cattle feces is recycled as manure or is not properly disposed (11). Studies have shown that swine shed S. typhimurium through their feces for up to 28 weeks after initial infection (12). Fresh fruits and vegetables contaminated with Salmonella have been associated with human salmonellosis. Salmonella, mostly from untreated irrigation waters, can contaminate fruits and vegetables through roots, stem scars, and leaves (14, 15). Pre- and post- processing food facilities may become contaminated with Salmonella through all these original sources of Salmonella such as poultry, cattle, fresh fruits and vegetables. Peanut butter, mangoes, cantaloupe, ground beef, dry dog food, and raw scrap ground tuna product are some of the most recent contaminated sources of Salmonella that have been associated with salmonellosis outbreaks in humans in the United States (13). Salmonella enterica Salmonella is a Gram-negative, non-spore forming, facultative intracellular anaerobe that belongs to the family of Enterobacteriaceae. Salmonella is a chemoorganotrophic organism; it is capable of degrading organic material and 6 compounds for energy. It is oxidase negative, catalase positive and produces hydrogen sulfide. Salmonella can decarboxylate lysine and ornithine and uses citrate as its sole carbon source (10). Salmonella is capable of growing in extreme and harsh environments due to its exceptional tolerance and adaptive characteristics. Salmonella is classified as a mesophile, optimally reproducing in a temperature range of 30 to 40o C. However, Salmonella can also reproduce in foods stored at temperatures of 2-4o C, which then classifies Salmonella as a psychrophile. Salmonella can survive the acidic environment of the stomach due its wide range tolerance for pH (4.6-9.5), and is thus able to invade the small intestine. It has a tolerance for salt concentrations of 3-4%; salt tolerance increases with increasing temperature (10). To overcome challenges of different environmental conditions, Salmonella detects changes in its environment and responds by orchestrated gene expression to adapt and survive. Altering the gene expression profile allows for adaptation to environmental stresses such as nutrients depletion, pH and temperature extremes, while virulence gene expression enables Salmonella to acquire resistance, evade, and systematically confront the elements of innate immunity of the host (16). Leon Le Minor and Michel Popoff contributed to the current understanding of the two species of Salmonella genus, Salmonella enterica and Salmonella bongori (9). Salmonella species are divided into subspecies, which are divided into serotypes/serovars; so far 2500 serotypes of S. enterica have been identified (1, 2). Serovars are conventionally distinguished through a species-specific antigenic scheme 7 classification based on somatic (O), flagellar (H), Capsular (K) antigens and virulence (Vi). In recent years, World Health Organization Center for Reference and Research on Salmonella has developed serotype-specific 16S rRNA and other gene sequence comparison schemes for Salmonella typing (4). The study of Salmonella intestinal infection had been restricted to studies using bovine ileal loop inoculations, intestinal epithelial cell cultures and oral infections, until a murine model of Salmonella enteropathogenesis was developed (5). The murine model made it possible to better understand the mode of Salmonella pathogenesis and different stages of salmonellosis. These studies revealed that virulent S. enterica localizes to the apical epithelium, triggers invasion and associated virulence gene expression to elicit significant inflammatory changes leading to local and diffuse polymorphonuclear leukocytes infiltrate, crypt abscesses, epithelial necrosis, edema and fluid secretion (1, 6). Salmonella enterica servovar Typhimurium Pathogenesis Salmonella enterica servovar Typhimurium infection starts with ingesting contaminated food or water. Salmonella typhimurium crosses the host’s digestive tract, and enters the stomach. To survive the low pH of the stomach, S. typhimurium expresses acid shock and outer membrane proteins through acid tolerance response (ATR). In addition to low pH, nutrient deprivation sigma factor (δs) can also induce the ATR response. After reaching the lumen of the small intestine, it expresses the virulence factors that grant S. typhimurium protection from antimicrobial peptides, bile salts, digestive enzymes, secretory IgA, and the innate host immune system, facilitating an 8 opportunity to transverse the intestinal mucus layer, and invade intestinal epithelial cells (22). Salmonella typhimurium expresses and utilizes fimbriae that give the bacterium the ability to adhere to intestinal epithelial cells (23). Further progression of infection in the specific host cell has staggering impact depending on which uptake mechanism, active or passive, is utilized (26). The following provides an overview of S. typhimurium pathogenesis. Each phase of S. typhimurium pathogenesis will be discussed in detail later in the literature review. Salmonella typhimurium is capable of infecting a wide range of cell types such as dendritic cells, phagocytes, and non-phagocytic epithelial cells of the gut. It can enter host epithelial cells in two ways: active or passive (25, 26). The active or “trigger” mechanism initiates rearrangement and ruffling of the host cell membrane by injection of virulence proteins into the host cell using Type III Secretion System which results in the internalization of the bacteria (21, 241). Salmonella has been viewed as prototype for pathogens using the “trigger” mechanism (18, 19, 20, 24). On the other hand, one or more bacterial surface proteins bind to one or more specific host cell receptors to induce the passive or “zipper” mechanism, consequently, initiating the internalization of the bacteria (241). Listeria monocytogenes has been viewed as prototype for pathogens using “zipper” mechanism (241). The “trigger” and “zipper” mechanisms phenotypically differ from each other. In addition to trigger and zipper mechanisms, host immune cells that have phagocytic characteristics can internalize Salmonella typhimurium. Upon adhesion (preferably) to microfold cells (M cells) in the intestinal 9 epithelium, S. typhimurium stimulates the inflammatory response, induces secretion of chemokine interleukin-8 (IL-8) and activates polymorphonuclear leukocytes (PMN) to move across the intestinal epithelial cell layer (27, 28, 31). M cells lack IgA, which becomes a bridge for Salmonella to get to underling tissues. Salmonella enters M cells using “trigger” mechanism by deploying SPI-1 T3SS that injects the effector proteins involved in rearranging the actin cytoskeleton (33, 34). M cells are specialized cells in the intestinal epithelium, important in inducing mucosal immunity through sampling of antigens using a pinocytosis mechanism. Using pinocytosis, M cells engulf S. typhimurium and deliver them to lymphoid cells in the Peyer’s patches beneath the epithelium (32). These events result in bacterial internalization and formation of Salmonella-containing vacuole (SCV), which acts as a protective niche for S. typhimurium survival and replication (29). Various markers on the vacuole are responsible for different phases of SCV maturation (30). The first phase of SCV maturation, biogenesis, occurs in less than 30 minutes and Salmonella controls most of the different markers on the vacuole (30). SCV moves through the cell, staying close to the Golgi in the perinuclear region of the host cell for 30 minute to 5 hours post infection. The final phase of SCV maturation is indicated by the formation of Salmonella-induced filaments (SIFs) (35). SIFs are long membranous tubules that diffuse away from SCV approximately 8 hours post infection. The tubular structures are enriched with lysosome-associated membrane protein 1 (LAMP1) and other markers which facilitates SCV fusion with endocytic vesicles, which act as nutrient sources vital to Salmonella intracellular replication (36, 37). During the phases of SCV 10 biogenesis, the SCV membrane is loaded with cholesterol, which is an important component required for Salmonella replication; inhibiting cholesterol production will stop bacterial growth (38). Another important component of Salmonella virulence is SPI-2 T3SS required for S. typhimurium intracellular survival. SPI-2 T3SS injects effector proteins across the SCV into the host cell cytoplasm, which prevents lysosomal fusion to SCV (39, 40). Salmonella pathogenesis is the coordinated work of greater than 30 effector proteins secreted by the T3SS-1 and T3SS-2 apparatus that reside on Salmonella pathogenicity island- (SPI-1) and Salmonella pathogenicity island- (SPI-2), respectively (18, 41). Salmonellla Pathogenicity Islands Pathogenicity islands are clusters of virulence genes in a confined region of the chromosome. The following three characteristics of pathogenicity islands suggest that Salmonella pathogenicity islands genes are acquired through horizontal gene transfer: 1) pathogenicity islands have different GC composition than the rest of the chromosome, 2) pathogenicity islands contain genes that are closely related and they are not found in nonpathogenic bacteria, and 3) transposon insertions are often localized around the pathogenicity island (42). Salmonella pathogenicity islands are essential for invading the host cell, intracellular survival, and pathogenesis. According to Hensel in a 2004 review article, 12 SPIs (SPI-1 – SPI-10, SGI-1 and HPI) have been described and most of them share 11 common motifs; however, size, structure and function of these SPI and their distribution in Salmonella subspecies and serovars varies significantly (43). SPI 7, 8, 9 or 10 are not present in S. typhimurium (43, 53). Another review by Fabian et al. in 2012 presents the conclusion that 21 SPIs (SPI-1 – SPI-21) have been identified in Salmonella and only SPI-1 to 6, 9, 11, 12, 13, 14, and 16 are present in S. typhimurium (61). Even though there is a difference in nomenclature of the SPIs in the two studies, they both agree that SPI-1 – SPI-6 are significant contributors in S. typhimurium pathogenesis. Only SPI-1 and 2 are relevant to this research and they will be described in detail. Salmonella pathogenicity island 1 is responsible for encoding a T3SS, which is an apparatus for injecting effector proteins into the host cell (43, 34). SPI-1 is 40 kb in size and is mostly conserved among all Salmonella species. Some of the SPI-1 effector proteins are involved in the invasion of non-phagocytic cells by Salmonella, through rearranging the host cell’s actin cytoskeleton. Other SPI-1 effector proteins are involved in eliciting inflammation of the intestinal epithelium, diarrheal symptoms and other entero-pathogenesis processes (44). Salmonella pathogenicity island 2 is 40 kb in size, composed of two distinct portions: a 25 kb portion that is exclusive to S. enterica and a 15 kb portion that is observed in S. bongori and S. enterica (45). The first portion has a G+C content of 43%. It plays a crucial role in systemic pathogenesis and encodes the T3SS-2 in S. enterica that is induced during intracellular survival and replication. The second portion has a G+C content of 54% encodes tetrathionate reductase (Ttr) used in anaerobic respiration (46). 12 Any bacterial products that are involved directly or indirectly in Salmonella pathogenesis are called Salmonella virulence factors. Adhesion, invasion, capsule formation, immune evasion strategies, and regulation of virulence gene expression are some of the mechanisms that are associated with Salmonella virulence factors. Although exhaustive investigations have been done on Salmonella virulence factors, this study will only review virulence factors that are direct contributors to successful Salmonella pathogenesis. Adhesion The presence of S. typhimurium in the mucosal cells and Peyer’s patches stimulates the signaling pathways of host cells, resulting in secretion of inflammatory cytokines, which act like physical barriers. Various adhesion factors of S. typhimurium such as fimbria, flagella, and lipopolysaccharide (LPS) interact with host-receptors (62, 63). Salmonella typhimurium uses 13 different fimbriae and 3 nonfimbrial adhesins for colonization, and their expression are controlled according to time and space (64, 61). Fimbriae (or pili) are inflexible, straight filamentous proteins, anchored on the outer membrane surface, and are recognized by the host cell receptor for initiating cell-to-cell contact, which results in signal transduction. These proteins are assembled through the Chaperone usher (CU) pathway. Non-fimbrial adhesins are mono- or oligomeric proteins on the outer membrane surface that function in the same general way as fimbriae adhesins, however, they are not assembled through the CU pathway (65). 13 Salmonella typhimurium also possess flagella that confer a complete adhesion of S. typhimurium to M cells. The propulsion and motility of S. typhimurium is due the chemotactic responses of flagella (73, 74). This flagella structure is assembled by proteins encoded by 30 genes that are controlled by three classes of promoters (75). A hydrophobic lipid A, a short non-repeating core oligosaccharide, and a distal polysaccharide (O-antigen) are the three main domains of LPS in S. typhimurium (66). The longer chain forms of O-antigen in LPS contribute to S. typhimurium resistance to neutrophils, phage lysis, and other host responses, adaptation and intestinal colonization (67-72). Six of the twelve SPIs present in S. typhimurium are involved in bacterial adhesion to the host cell prior to the onset of the disease (61). Invasion Following adhesion by S. typhimurium, invasion of the host begins. Invasion is encoded and controlled by SPI-1 that induces rearrangement and ruffling of the host cell membrane to internalize the bacteria (76). Salmonella typhimurium uses about 29 genes of SPI-1 to encode virulence factors to initiate invasion. These genes code for: a) avirulence factor A (Avr A), Salmonella secreted protein (Ssp) SipA, SipB, SipC and tyrosine phosphatase protein (SptP); b) SPI-1 genes expression regulator, HilA; c) Inv, Spa, and Prg and other T3SS proteins; d) the chaperone proteins important for injecting effector proteins into the host cell (77-79). SipA and SipC proteins are crucial to remodeling and rearrangement of host cytoskeleton to facilitate bacterial entry, which 14 triggers signal transduction to mobilize the polymorphonuclear leukocyte (PMN) through the intestinal epithelial layer (80, 81). SipB works as an effector protein that binds to cholesterol, crucial to formation of the translocon for translocating other SPI-1 effector proteins (82). SopE is responsible for activating the Cdc42 and Rac small G-proteins inside the host cell resulting in actin rearrangement and induction of inflammatory cytokines (78, 83-85). Salmonella pathogenicity island 1 is activated and controlled by HilA, a locus that resides within SPI-1 (86). HilA belongs to the OmpR/ToxR transcriptional activators family and binds to prg, inv/spa, and sip operon promoters (87). In response to an unsuitable intestinal lumen environment, hilA expression is induced through a BarA/SirA two component system (TCS). HilA expression is positively controlled by HilD, HilC and the RstA/RstB TCS (87). HilA is also responsible for inducing T3SS-1 expression and expression of encoded effector proteins (88). To insure its survival inside the host cell, S. typhimirum takes steps to keep the host cell alive. After S. typhimurium is internalized, the SptP-mediated process reverses the SopE related activity to repair the host cytoskeleton (78). HilA expression is blocked through PhoP/PhoQ system due to the low Mg2+ concentration level inside the vacuole (SCV) (89). In addition, RcsCDB phosphorelay system is also known to be responsible for repression of hilA, invF and invG SPI-1 gene transcription (90). Along with inhibiting SPI-1 gene expression and their activity through RcsB and the PhoP mechanism, the PhoP activates SPI-2 genes expression for commencing the next stage of Salmonella 15 systemic infection (87). SCV Maturation SopE and SopB (T3SS-1 effector proteins) and SpiC (T3SS-2 effector protein) are used as markers to prevent SCV fusion with endosomes or lysosomes, allowing SCV to go through the maturation phase (91, 92). SsrA/SsrB TCS (Ssr regulatory operon), T3SS/SPI-2 (Ssa operon), the secretion system chaperones (Ssc operon) and the secretion system effectors (Sse operon) are some of the 40 genes that reside and are encoded by SPI-2 in S. typhimurium (93,77, 94). The signal that activates SsrA/SsrB TCS to regulate sse, ssa, and ssc operons is unknown, however, it is well known that SsrA/SsrB TCS is regulated by pH and osmolarity change in OmpR/EnvZ-dependent pathway (95-97). The Salmonella-containing vacuole moves to the peri-nuclear region in close proximity of Golgi. This movement gives SCV the opportunity to obtain nutrients using SPI-2 effectors, SifA, SseG and SseF, from endocytic/exocytic transport vesicles (98). Following the localization of SCV and nutrient acquisitions, S. typhimurium replication commences (61). Gram-Negative Secretion Systems Gram-negative bacteria have evolved numerous secretions systems for transporting proteins to the outer membrane surface, extracellular space, or into the host cytoplasm (99). Some of these secretion pathways are complex and involve macromolecular structures to overcome the limitations of having an outer membrane. So 16 far, eight different secretion systems have been discovered and are classified in two categories: a) sec-dependent and b) sec-independent systems. The type II secretion system (T2SS), type V secretion system (T5SS), chaperone/usher system (CU), and the extracellular nucleation-precipitation system (ENP) are classified as Sec-dependent secretion systems. Type II secretion system secretes hydrolytic enzymes, toxins and type IV pili to the outer membrane (100-102). In T5SS, substrates facilitate their own secretion into the outer membrane after being targeted by inner transmembrane protein complexes (103, 104). The CU system, beststudied system in E. coli, uses an assembly foundation on the outer membrane that is created by a periplasmic chaperone, FimC and an usher, FimD (105, 106). In E. coli, ENP system is essential in secretion of curli, adhesive fibers, to the outer membrane. ENP is also important for the formation of biofilm (107, 102). Type I secretion system (T1SS), type III secretion system (T3SS), type IV secretion system (T4SS) and the twin-arginine secretion system (Tat) are classified as sec-independent secretion systems. Type I secretion system secretes proteins with high molecular weight that possess a C-terminal signal sequence directing them outside of the cell. The transport of these proteins occurs without the cleavage of the C-terminal sequence and it is best described for the exotoxin, α-hemolysin (HlyA), in pathogenic Echerichia coli (108). In contrast, Tat secretory system transports folded proteins with an N-terminal peptide signal composed of two arginines through an active transport system, proton-motive force (109). Type IV secretion systems are secretory systems that can 17 transport single-stranded-DNA-protein complexes in addition to proteins in two different ways: cell contact-dependent or cell contact-independent (110-112). Since T3SS is part of this study and it is induced in Salmonella sp. pathogenesis, it will be discussed in more detail. Type III secretion system Type III secretion systems are evolved specialized virulence devices that directly inject bacterial virulence proteins/effector proteins into the host cytoplasm in order to control and modify host cell functions (113). Delivery of these effector proteins into the host cell cytoplasm to alter host-cell cytoskeleton, membrane trafficking, cytokine gene expression, and signal transduction is a complex task that is carried out by a needle-like apparatus that projects outward from the bacterial outer membrane (114). This apparatus is comprised of 20 proteins divided into substructures consisting of: base, inner rod, needle and translocon. Base is a multi-ring structure that spans the inner and outer bacterial membranes. In addition, base functions as an anchor for the inner rod and hollow needle structure. The inner and outer membrane structures of the needle-like apparatus are evolutionarily related to the bacterial flagellar secretion apparatus and PulD family of type II secretion system, respectively (114-116). T3SS secretes translocon proteins that are embedded in the host cell membrane. Translocon proteins assemble a pore, and act as a needle apparatus target (117). The structures of the T3SS are highly conserved among different species of Salmonella, however, the effector proteins secreted by the T3SS varies across Salmonella species (118). The effector proteins are encoded 18 by sets of genes that reside on the same pathogenicity island (SPI-1) encoding the T3SS or somewhere else in the chromosome (113). Salmonella T3SS-1 Apparatus The base structure of Salmonella is composed of equal molar amounts of InvG, PrgH and PrgK, which are sec-dependent proteins. InvG is inserted into S. typhimurium outer most membrane. PrgH and PrgK linked to each other form a structure that is inserted into the inner most cytoplasmic membrane of S. typhimurium. PrgJ and PrgI proteins form the inner rod and hollow needle structures, respectively. Numerous other proteins such as InvC, InvA, SpaP, SpaQ, SpaR and SpaS lie within the PrgH/PrgK inner member ring that make up the effector protein export machinery. InvC is an ATPase that ensures an efficient translocation of the PrgJ and PrgI proteins by recognizing and unfolding them to form the inner rod and the hollow needle, respectively. Several chaperones and stabilizing proteins play critical roles in the formation of the apparatus but they are not part of the fully assembled apparatus. InvJ is not a permanent part of T3SS apparatus but it ensures the proper formation of the needle complex (119, 120). Another non-permanent T3SS related lipoprotein, InvH, translocates the InvG protein to assemble the outer most membrane ring in the base structure (121, 122). Type III secretion system uses a “substrate switching” mechanism that specifies what kinds of proteins are allowed to be delivered through the needle. The substrate switching is possible because InvJ plays a critical role in causing conformational changes in the secretion apparatus that allows PrgJ and PrgI to pass through the needle and block other 19 effector proteins (123). Other chaperones guide effector proteins to the T3SS apparatus. For example InvB escorts SipA, SopE, and SopE2 effector proteins (124, 125). SipB, C, and D are proteins that are secreted through the T3SS apparatus and form the translocon pore in the host cell membrane (126). According to recent studies, SipD is thought to be located at the tip of the needle complex, initiating a translocon assembly by associating itself with the host cell membrane upon contact (127, 128). SipB and SipC play a critical role in the assembly and proper function of the translocon pore; however, they were not observed immediately after the initial contact between the needle apparatus and host cell membrane (128). Since SipB has a high affinity for binding cholesterol, the location of translocon pore on the host membrane is most likely to be the cholesterol rich regions called the lipid rafts. SipB can also recruit cholesterol to the assembly site of the translocon pore on the host cell membrane (129). SPI-1 T3SS Secreted Effector Proteins The internalization of S. typhimurium into the host cell is facilitated by the collaborative work of SPI-1 T3SS effector proteins. SipA and SipC work in concert to remodel the host cell membrane (130). SipC binds and bundles microfilaments called Factins to trigger the formation of actin at the bacterial adhesion site. SipA enhances SipC activity by binding the actin filaments to induce polymerization and stabilize the actin filaments by up-regulating T-plastin activity, a localized actin bundling protein (131134). In addition SipC blocks host cell factors to prevent actin filament disassembly (135, 136). Other effector proteins such as SopE and SopE2, do not bind actin filaments 20 directly; they mimic the host cell guanine-nucleotide exchange factors (GEFs) to trigger Rho GTPase, Rac-1 and Cdc42 that ultimately cause host cytoskeleton remodeling and membrane ruffling through the Arp2/3 pathway (133, 137). SopB is an inositol phosphatase that contributes to extensive actin remodeling by targeting host GEFs to activate RhoG GTPase (138, 133). After internalization and formation of the SCV, SopB and SopD work together to seal the host membrane infolding (139, 133). SptP restores changes in the host membrane by reversing the activities of SopE, SopE2 and SopB effectors. SptP mimics the GTPase-activation proteins (GAPs) to deactivate Rho GTPase, Rac-1 and Cdc42 by hydrolysis of bound GTP to GDP (140-143). SptP also promotes host cytoskeleton recovery using its tyrosine phosphatase activity targeting tyrosine Kinase (ACK), a downstream effector of vimentin (an intermediate filament protein) and Cdc42 (144). A number of SPI-1 T3SS effector proteins that are involved in nonphagocytic cellular invasion, also induce the host immune system which results in acute intestinal inflammation. SopE activates Rac-1, and SopE, SopE2 and SopB work in a concert to activate Cdc42. The activation of Cdc42 and Rac-1 result in Raf1-dependent upregulation of the Erk, Jnk and p38 mitogen-activated protein kinase (MAPK) signaling pathways, which leads to activation of AP-1 and NF-κB transcription factors (150, 138, 133, 137, 152, 151). Subsequently, the activation of these pathways induces the transcription, translation and secretion of proinflammatory cytokine, IL-8 (also know as CXCL8), by the invaded host epithelial cells (138, 153). IL-8 act as a chemoattractant to recruit PMNs to the infection site. SopB, SopE, SopE2 and SipA facilitate the migration of PMNs 21 across the epithelium by disrupting tight junctions (154). In addition, SipA, and SopA trigger the Arf6 and Phospholipase D signaling cascades resulting in release of hepoxilllin A3 that contributes to PMNs recruitment and its migration across the intestinal epithelial layer (155, 156, 157, 158, 150, 132). The migration of PMNs coupled with fluid flux and secretion of chloride by the invaded epithelial cell contributes to diarrhea (154, 150, 133). SipB binds and activates caspase-1, which then triggers the production of other inflammatory cytokines such as IL-18 and IL-1β. In addition, Salmonella strives to block the infected cell from going through apoptosis by deploying effector proteins in order to allow bacterial survival and replication inside SCV (171). Salmonella effectors block apoptosis of the host cell by suppressing NF-κB-dependent gene expression in numerous ways. SspH1 effector protein binds PKN1 to stop NF-κB-dependent gene expression (172). Another effector protein, AvrA, makes host cell survival possible by blocking the JNK signaling pathway (173). SptP mimics ATPase activity to inactivate Raf1 that would downregulate MAPK signaling in order to reverse actin rearrangement by GAP activity (174). SopB is involved in preventing host cell apoptosis by activating Akt (175,176). SpvC, Phospho-threonine lyase, inactivates MAPK via beta-elimination reaction. It also reduces the mRNA level of proinflammatory cytokines by dephosphorylating ERK (177). SseL, a SPI-2 effector protein, decreases inflammatory cytokines by protecting Iκ-Bα, a NF-κB inhibitor, from degradation (178). It can be seen from the overview described in Part 1 that Salmonella pathogenesis 22 in a natural host system is highly complex and involves numerous effector proteins. Hutchison and Dukovcic have demonstrated that a Betta splendens (Siamese fighting fish) chromatophore based biosensor can detect and differentiate between pathogenic bacteria and closely related non-pathogens (204, 213, 231). What remains to be elucidated are the mechanisms by which cells that are not natural hosts for pathogenic bacteria respond to pathogens. The remainder of this review will discuss detection methods for bacterial pathogens in general, and the Betta splendens chromatophore based biosensor used in this research. Part 2: Detection Methods and chromatophore cell-based biosensor Detection Methods for Bacterial Pathogens Rapid and accurate detection methods for bacterial pathogens contaminating food and water are essential to identification, treatment and prevention of diseases that continue to plague humans and animals worldwide. Approximately two thirds of research efforts have been invested in developing pathogen detection applications for the food industries, clinical diagnosis, and water and environmental quality control (192). Most efforts in this field have been focused on developing rapid pathogen detection methods. Culturing and colony counting, immunology-based methods and Polymerase chain reaction (PCR), are three well established and most commonly used methods for pathogen detection. These methods are quite time consuming, however, and can only report on the presence, not toxicity, of the contaminating microorganism (192). 23 Immunology-based Methods Immunology-based methods provide various ways to analyze and detect a wide range of bacterial pathogens. One of the most well established immunology-based methods is Enzyme-linked immunosorbent assay (ELISA) that uses specially designed antibodies to bind specific target antigens (195). ELISA is used to detect cell surface antigens of target bacteria. Many companies provide antibodies used in ELISA for detecting toxins or spores of B. anthracis (196), extracellular lipopolysaccharides of Salmonella serovars (197), outer membrane proteins of Salmonella serovars (198), and other various bacterial antigens. In a typical ELISA, samples are added to a microtiter plate that contains immobilized antigen-specific antibodies that binds the antigens from the samples and then allows the rest of the sample to be washed away. This is followed by the addition of a second antibody tagged with an enzyme that will induce a color change upon binding. The color is then quantified by colorimetric methods. Although this is a very visible method that is easily quantified, this method can only report on the presence, not viability or toxicity, of contaminating bacteria. Another immunology-based method is immunomagnetic separation (IMS) that is used in concert with other detection methods. IMS is used to separate the target bacterial pathogen from a pool of bacteria using specific antibody coated magnetic beads that bind to the target bacteria (199). Optical, magnetic force microscopy, and magnetoresistance are some of the methods that can be used for further detection after the target bacteria is 24 captured and extracted by IMS (200, 201). Polymerase Chain Reaction-based Methods Polymerase chain reaction (PCR) methods are used for bacterial pathogen detection. PCR is based on the isolation, amplification and quantification of short DNA or RNA sequences of target bacteria. Real-time PCR, multiplex PCR and reverse transcriptase PCR are other PCR methods that have been developed for bacterial detection. These methods require a known nucleic acid template, specific primers, and other essential thermostable polymerization enzymes. PCR consists of a denaturation cycle of the purified DNA by heat, an extension cycle using specific primers, and DNA polymerase, followed by the exponential amplification of each new double stranded DNA. Then, gel electrophoresis is used to verify the presence of the new amplified DNA sequence (192). Even though PCR is a valuable method in detecting different types of bacterial pathogens, it has some limitations. For example, PCR does not provide information about the viability of the bacterial cells due the presence of DNA in both, dead and living cells. Additionally PCR cannot report directly on the toxicity of the contaminating bacteria. Also in some cases, PCR needs purified DNA or RNA as template, which often requires more than 24 hours to acquire an appropriate amount because culturing is still part of the process. RT-qPCR (reverse transcriptase-quantatative PCR) addresses some of these limitations. 25 Biosensors Biosensors are detection devices that utilize biological materials such as cells, tissues, organelles, microorganisms, cell receptors, antibodies, nucleic acids or enzymes. Biosensors also utilize biologically derived materials like engineered proteins and antibodies, or biomimic materials like synthetic catalysts, imprinted polymers and ligands (192). These materials are attached to a physiochemical transducer/transducing microsystem that can be electrochemical, optical, piezoelectric, magnetic thermometric or micromechanical and are used for biochemical interactions with targets for detection (192, 202). Biosensors have two main steps in detecting the target: immobilization of the target and analysis of the target (202). Biosensors have been very important in the pathogen detection field due to their ability to detect a wide range of microorganisms and assess their toxicity. However, cell-based biosensors have become the ideal detection method due to their distinguishable physiological behavior toward pathogenic and nonpathogenic bacteria (203-205). Unlike other detection methods that require DNA homology, antibody-antigen specificity, or structure recognition, cell-based biosensors’ physiological responses and their reaction to the environment are used as the detection tool (202). Cell-based biosensors can be divided into two categories: engineered cell-based biosensors and innate cell-based biosensors. Engineered cell-based biosensors are cells that are altered/engineered for a specific pathogen or target. The rat basophilic leukemia mast cell and the B-lymphocyte cell are the two examples of engineered cell-based 26 biosensors to detect foodborne pathogens that show high specificity (206). Even though the high specificity of engineered cell-based biosensors is preferred, it takes years of research to develop it. In contrast, innate cell-based biosensors are biosensors that do not need any modification; their use as a detection tool is reliant upon the quantifiable signal of their inherent physiological characteristics. These biosensors use their natural receptors to trigger an intracellular signal transduction pathway that can be measured. A prominent example of innate cell-based biosensors is the chromatophore cell-based biosensor. Chromatophore Cell-based Biosensor Chromatophore cell-based biosensors utilize a class of pigmented neuron like cells called chromatophores. These cells are capable of moving their intercellular pigment organelles upon exposure to physiological stimuli. This property has made chromatophore cells valuable in their use in a detection system solely based on biological activity. Induction of pigment granules movement in chromatophore cells due to disrupted intracellular functions in response to different biological stimuli are measured and analyzed to assess toxicity of a pathogen, whereas other detection methods can only assess the presence but not toxicity of a pathogen (207, 208, 209). These pigment movements could be toward the peri-nucleus of the cell called aggregation or outward to the periphery of the cell called dispersion (208, 209). The degree, magnitude and kinetics of chromatophore cell responses (aggregation and dispersion) vary depending on the different pathogens and toxic stimuli (208, 209). The similarity of chromatophore cells to 27 neuron cells of other animal makes them of interest in detecting biological substances of concern to human health (210, 209). Chromatophore Cells and Pigmentation Amphibians, crustaceans, fish and reptiles are poikilothermic animals that have pigmented cells, called chromatophores, located under their dermis layer. This class of neuron like cells is responsible for changing the animal’s overall body pigmentation and color intensity in response to environmental stress. Chromatophore cells are used as an integumentary system in Poikilothermic species, participating in survival, visual communication and mating processes (214-217). Chromatophore cells are named based on their intracellular pigment organelles: cyanophores (blue), erythrophores (red), iridophores (iridescent), leucophores (white), melanophores (brown), and xanthophores (yellow). Chromotaphore cells are subdivided into two major categories, light-absorbing and light-reflecting, based on their optical properties. Erythrophore, cyanophore, melanophore and xanthophore cells are light-absorbing and have a dendritic morphology. In contrast, iridophore and leucophore are light-reflecting and have non-dendritic, round shaped cells (218, 219). Except iridophores, the remaining five types of chromatophore cells contain motile pigment organelles called chromatosomes. These chromatosomes have the capability to exhibit different colors based on the absorption, or reflection in the case of leucophores, of different light wavelengths. Leucophores have (unidentified) whitish fibrous materials that scatter all the wavelengths, thus, deemed as light-reflectors (216). 28 Iridophores are the only chromatophore cells that do not contain chromatosomes, instead, they have stacked platelets of guanine crystals in the cytoplasm (216). Due to the high refractive index of these platelets, they give an iridescent color to many Poikilothermic species. Unlike other chromatophore cells, iridophores are not involved in changing color intensity through intracellular motile pigment organelles (216). Specialized cytoskeletal microtubules that spread from the center of the cell to dendrites, facilitates a movement route for chromatosomes through the activity of ATPase motor proteins; giving chromatosomes the ability to aggregate or disperse. Aggregation refers to movement of chromatosomes toward the center of the cell and dispersion refers to movement of chromatosomes toward the periphery of intracellular space. Aggregation is caused by the coupling activities of the first signaling messenger, neural or hormonal ligands, binding to receptor and the activation of G-protein, which in turn activates dynein, a eukaryotic microtubule motor protein. The resulting signal cascade is translated into the movement of pigment organelles toward the peri-nucleus of the cell along the microtubules (220). Chromatophore cells are generated in the neural crest of poikilothermic animals. The chromatosomes in chromatophore cells are controlled by the endocrine and neural systems via different hormones (216, 218). For example: the pituitary gland secretes melanophore stimulating hormone (MSH) that causes dispersion, movement of chromatosomes toward the cell periphery, in light-absorbing chromatophore cells. Interestingly, MSH causes aggregation in light-reflecting iridrophore and leucophore 29 chromatophore cells by means other than causing translocation of the chromatosomes. The hypothalamus secretes melanin concentrating hormone (MCH) and melatonin that cause aggregation, movement of chromatosomes to the peri-nucleus region of the cell, in light-absorbing chromatophore cells (218). Betta splendens possess sympathetic nervous system that is also involved in regulation of chromatosome motility in the chromatophore cells. Changes in the level of different intracellular ions concentration can cause a signal transduction, which affect the nervous system. Thus, the nervous system releases neurotransmitters to cause aggregation or dispersion (218). Physiological studies have shown that environmental stress is also responsible for the overall body color changes in fish, amphibians and crustaceans. The color changes in these animals are characterized as hyper – or hypopigmentation (225). The dermis layer of Poikilothermic animals that contain chromatophore cells act as the integumentary system of the animal and thus, is exposed to a variety of different environmental conditions (226). Toxicants, chemicals (e.g. industrial waste), and heavy metals are associated with depigmentation in fish, amphibians and crustaceans. For example: some studies have shown that mercuric chloride is responsible for hypopigmentation in rainbow trout (154), Rohu carp (226) and estuarine crab larvae (170). Environmental stress related depigmentation is also caused by bacterial pathogens or bacterial pathogens’ exotoxins. The depigmentation in numerous species of fish is exhibited as a primary symptom after exposure to bacterial toxin (198). 30 Betta splendens The use of Betta splendens (Siamese fighting fish) erythrophore cells to detect chemical and bacterial toxicity is a good example of a chromatophore cell-based biosensor. Positive controls, clonidine hydrochloride (Cl) and α-melanocyte simulating hormone (MSH), for aggregation and dispersion, respectively, were established in erythrophore cells from Betta splendens by Mojovic et al (209, 211). In other studies, erythrophore cells from B. splendens have been exposed to different pathogenic bacteria (e.g Bacillus cereus, Clostridium perfringens, C. botulinum and Salmonella enteritidis) and nonpathogenic bacteria (e.g. B. subtilis, B. cereus nonpathogenic mutant). Interestingly, erythrophore cells respond by aggregating in the presence of the pathogenic bacteria, yet remain nonresponsive to nonpathogenic bacteria (204, 213). In addition, erythrophore cells have been instrumental in detecting water contaminants, chemical agents and purified bacterial toxins (207, 209). Erythrophore cell-based biosensor is an emerging technology that exhibits the potential to detect toxic conditions not only caused by the presence of foodborne pathogens, but also toxic chemicals. Betta splendens have acquired worldwide popularity as ornamental fish due to their brilliant coloration. Rice farmers in Thailand domesticated and bred this species of fish for ornamental and sports purposes. B. splendens with long fins and bright colors are used as household ornamental fish. The brilliantly colored phenotype of the ornamental form of B. splendens no longer resembles the phenotype of wild B. splendens living in rice puddles or the B. splendens with short and round fins for sport fighting in Thailand 31 (183, 184 and 185). Betta splendens is of a great commercial value in Southeast Asia. Thailand alone exports about 3.6 million male B. splendens fish each year (184). Wild B. splendens are naturally found in Thailand and other Southeast Asian countries in the freshwater ponds, rice puddles and marshes (186, 183). These ponds and puddles make a perfect niche for these fish because of their shallow, high temperature (about 29.9 0C) and low in dissolved oxygen water (187). Genus Betta belongs to the family Osphronemidae and is classified as a freshwater ray-finned fish. Betta species possess lung-like organs that allow them to gulp air at the water surface, putting them under suborder Anabantoidei (the labyrinth fish) (188). Parental care characteristics, mouth-brooder or bubble-nest builders, are the distinguishing factors among different species of wild-type Betta. Betta splendens are the bubble-nest builders, a reproduction strategy that sets them apart from other fish species. Betta splendens coloration plays important roles in reproduction and protection of the offspring. The male B. splendens builds a bubble nest by gulping air at the water surface and starts initiating courtship with females (186). Males protect the bubble nest by projecting a territorial behavior and aggression toward the intruder or unwanted female by blazing its opercula (gill covers), spreading fins, and deepening his overall color (189, 186). The courtship and spawning process is divided into five phases: prespawning preparatory phase, courtship phase, clasp, swimming inhibition and postspawning phase 32 (190). Coloration is the main signal of prespawning for triggering courtship. The male B. splendens switches from being pale and dull color to a bright and uniformed body color to display for female. Female B. splendens changes from a pale color to a phenotype of deeply colored vertical bars on the body and a gold patch on the belly to signal the male that she is ready for courtship and spawning (190, 191). The female B. splendens work is done in the reproduction process after spawning. The male B. splendens picks the fertilized eggs in his mouth and places them in the bubble nest and continues to protect the eggs and newly hatched fry (190). Any faulty response from either of the two fish, male or female, in any of the above five phases results in interruption of reproduction (190). Betta splendens make an ideal organism for chromatophore cell-based biosensors. Betta splendens are readily available in any pet store and can be purchased throughout the year. Due to their small body size, Betta splendens are easy to maintain. Each fish can be placed in a small beaker and kept in a relatively small facility for the duration of 21 days before tissue culture. The large flowing fins provide large number of chromatophore cells that can be used for multiple experiments. In addition, tissue cultures from B. splendens are easy to maintain. Chromatophore cells are cultured in 6, 12, 24 or 48 well plates and stored on a flat surface at room temperature. The tissue culture remains viable and responsive for up to five weeks without addition of hormones or growth factors. 33 Research Objectives Previous research efforts using the chromatophore cell type, erythrophore, for detection of bacterial toxicity revealed this cell type could rapidly detect several food associated bacterial pathogens, including S. typhimurium. Previously tested hypotheses using mutagenesis to analyze the attributes of S. typhimurium that led to a response in erythrophore cells revealed a potential role for the T3SS apparatus coded for by prgHIJK. Although wildtype S. typhimurium rapidly induces pigment organelles to undergo an aggregative response in erythrophore cells, S. typhimurium containing a mutation in the prgHIJK operon does not induce the pigment organelles to undergo an aggregative response in erythrophore cells. A mutation identified in a region different from the mutation that disrupted the prgHIJK operon also had a similar impact on erythrophore cells. The first objective of this study was to test the hypothesis that this second mutation resided in either gene(s) coding for the process regulating expression of the prgHIJI operon or the gene(s) coding for the effector proteins that traveled through the PrgHIJK apparatus. The approaches used to test this hypothesis included sequencing the region containing the mutation and identifying the gene(s) impacted by this mutation through comparative sequence analysis, cloning the wildtype gene sequence and using this wildtype gene sequence to complement the mutant thereby demonstrating that the mutation is linked to the resulting biological outcome. The second objective of this study was to test the hypothesis that the effector proteins of T3SS are the components of S. typhimurium’s invading mechanism directly involved in inducing pigment organelles to undergo an aggregative response in erythrophore cells. The approach used to test this 34 hypothesis involved testing the response of erythrophore cells to S. typhimurium strains containing targeted, well characterized mutations in genes coding for T3SS effector proteins. The outcome to this research effort increased understanding of the role of the T3SS in chromatophore cell response. This understanding lead to better utility of chromatophore cells as biosensors for bacterial toxicity. 35 Chapter 3 Materials and Methods Fish Care Red male Betta splendens were purchased from the local Petco or Animal House (pet store), depending on availability. Fish were maintained individually in 1000 ml beakers that contained 900 ml conditioned tap water (3.5 L autoclaved tap water, 460 µL Stress Coat, 2.3 g Aquarium Salt, pH∼7.0) at 26 oC (80.6 oF) with alternating light and dark cycles for 14 and 10 hours, respectively. Fish were fed New Life® Spectrum Betta Formula pellets six days a week and blood worms on the seventh day. Once a week, they were dipped for 30 seconds in a 3% aquarium salt solution and transferred to a new beaker containing fresh water. These husbandry conditions were implemented in accordance with regulations of Oregon State University’s Institutional Animal Care and Use Committee (approval #4409). Fish were held at least 21 days before use in chromatophore cell extraction. Cell Culture Fish were euthanized in an ice water bath for approximately 20 minutes prior to chromatophore cell extraction. After discarding the ice water, the fish was briefly rinsed with phosphate buffered saline (PBS) [128 mM NaCl, 2.7 mM KCL, 10 mM Na2HPO4, 1.46 mM KH2PO4, supplemented with 5.6 mM glucose and 1% antibiotic/antimycotic (Invitrogen Cat# 15140122), in tissue culture grade H2O, pH 7.3] before transfer with sterile forceps to a petri dish containing 10mL of PBS. Anal, caudal, and dorsal fins were 36 clipped using sterile scissors and forceps and transferred to a second petri dish containing 10 mL of PBS. Using sterile forceps, the clipped fins were transferred to a 50 mL Falcon tube containing 10 mL of skinning solution (SK) [128 mM NaCl, 2.7 mM KCl, 10 mM Na2HPO4, 1.46 mM KH2PO4, 1 mM EDTA (FW=372.2), supplemented with 5.6 mM glucose and 1% antibiotic/antimycotic (Invitrogen Cat# 15140122), pH 7.3]. Fins were washed in 10 mL SK for 1 minute on a rocker plate. Skinning solution was then discarded carefully, using disposable pipets, and replaced with 10 mL fresh SK. The SK wash step was repeated nine times. The SK wash removes non-pigmented epithelial cells, protective mucus, and scales from fin tissues. After the last 10 mL SK wash was discarded, a digestive enzyme solution (ENZ) [15 mg collagenase (Worthington Biochemical Cat# LS004196), 1.5 mg hyaluronidase (Worthington Biochemical Cat# LS002594), 7 mL PBS] was added to the fins in the 50 mL Falcon tube to release chromatophore cells from fin tissue. Batch lots of collagenase and hyaluronidase were prepared, and aliquots of 15 mg/1 mL PBS and 1.5 mg/1 mL PBS, respectively, were stored at -200C in 1.5 mL microcentrifuge tubes (epitubes) for single-use. The exposure time of fins to ENZ varied depending on fish age, fin size, and the rate of fin digestion. The normal exposure time ranged from 1 minute up to 5 minutes. After fin digestion, ENZ with released chromatophore cells, was transferred to a 15 mL Falcon tube using a sterile disposable pipette. Chromatophore cells were then separated from ENZ by centrifugation for three minutes at 600 rpm in a swinging bucket centrifuge (IEC Centra CL3). The supernatant ENZ was added back to the remaining fin tissues for further digestion. The fin digestion and separation of ENZ from released chromatophore 37 cells steps were repeated until most of the chromatophore cells were released and the fin rays became visible. Usually, 1-4 digestion steps are performed. The first digestion time is short and typically the cells are discarded due to excessive scales. The pelleted chromatophore cells from each digestion were resuspended and washed in approximately 7 mL Leibovitz L15+ medium [L15+(Invitrogen Cat# 15090046), supplemented with 20 mM HEPES buffer (Invitrogen Cat# 15630080) and 1% antibiotic/ antimycotic (Invitrogen Cat# 15140122)] and then centrifuged for three minutes at 600 rpm in a bucket centrifuge. The supernatant was discarded and the chromatophore cell pellet was resuspended in 100-400 µL L15+, depending on the size of the pellet, and transferred to a 1.5 mL epitube. A 5 µL drop from each of the resuspended chromatophore cell pellets was visualized under the microscope to observe the concentration and scale presence. A 5 µL drop of chromatophore cells was placed in the center of each well of a 24well Falcon tissue culture plate. Chromatophore cells were left undisturbed for 15 to 20 minutes in order to attach to the bottom of the wells. One mL of L15+ medium was added to each well, and after 20 minutes of equilibration, 50 µL of fetal bovine serum (5%) (FBS, Sigma-Aldrich Cat# F2442) was added. After 24 hours, old media was replaced with 1.5 mL of L15+ with 5% FBS. Chromatophore cells were stored at room temperature (220C) and media was changed weekly to avoid accumulation of cellular waste products and debris. Chromatophore cells were maintained for 1-2 weeks before using them for any 38 experiments. Response Assays and Computational Analysis Red chromatophore cells (erythrophores) from B. splendens were tested to measure their physiological responsiveness to the control agents α-melanocyte stimulating hormone (MSH, Sigma- Aldrich Cat# M4135), which induced pigment dispersion and clonidine (Sigma-Aldrich Cat# C7897), which induced pigment aggregation prior to conducting each experiment. Frozen single-use aliquot stock solutions of both clonidine and MSH at a concentration of 1 µM were thawed prior to use. A 150 µL volume of L15+ medium (10% of well volume) was removed from the designated chromatophore cell culture well, and replaced by adding 150 µL of either MSH or clonidine (final concentration of 100nM). Luria-Bertani (LB) broth used for culturing different strains of Salmonella was also included as a control and added to chromatophore cells in the same manner as MSH and clonidine. A viewing field of chromatophore cells was observed for 60 to 90 minutes at 100X through a Leica (Leica, Inc., Wetzlar, Germany) DMIL inverted microscope (Bartels and Stout, Issaquah, WA, USA). After control agents or bacterial cultures were added, time-lapsed images were captured at specified time-points during the 60 to 90 minute interval with a SPOT Insight 320 color camera (Diagnostic Instruments, Inc., Sterling Heights, MI, USA) mounted on the Leica microscope and SPOT Advanced software version 3.5.6.2 (Diagnostic Instruments, Inc.). Time-points for capturing images pictures during the 60 to 90 minute time course for MSH, clonidine, LB and all subsequent bacterial cultures were as follows: every 15 seconds for the first minute (0, 39 15, 30, 45 seconds), 1 minute, 1.5 minutes, 2 minutes, 3 minutes, 4 minutes, 5 minutes, 7.5 minutes, 10 minutes, and every five minutes thereafter. Using Image Pro Plus 7.01 (Media Cybernetics, Bethesda, MD, USA) software, images captured at each time-point were analyzed and data were exported to Microsoft Excel for further analysis. The response of chromatophore cells was measured by calculating area change in pigment based on pixels using the following equation: Change in Pigment Area = – [(Ao – At)/Ao] x 100 Ao is the initial chromatophore cell pigment area at time zero, At represents the pigment area at any given time-point, and multiplying the fraction by 100 will give the change in the pigment area. The collected data were represented graphically in Microsoft Excel by plotting “Change in pigment area (%)” versus “Time (minutes)”. A positive change in pigment area correlates to a dispersion response as seen with the dispersive control, MSH. Whereas a negative change in pigment area correlates to a pigment aggregation response, as seen with the aggregative control, clonidine. Chromatophore cell response assays with the above specifications were conducted at least twice. Bacterial Growth Conditions Salmonella typhimurium strains were grown and maintained in Luria-Bertani broth [LB, 10 g tryptone, 5 g yeast extract, 5 g NaCl, 1L double distilled water, pH 7.4]. Bacterial stocks were stored at -80 oC in LB supplemented with 20% glycerol. Fresh bacterial cultures were streaked on LB agar plates and incubated at 37 oC overnight. For 40 every chromatophore cells response assay, 5 mL LB in a 25 mL flask was inoculated with an isolated colony of each Salmonella strain from the LB agar plate and incubated at 37 o C in a shaking chamber (150 rpm) overnight (Table 1). Luria-Bertani media was supplemented with an appropriate 50 µg/mL antibiotic: ampicillin (Amp), kanamycin (Kan) or nalidixic acid (Nal), when needed. Overnight cultures were back diluted 1:100 (50 µL of overnight culture in 4.95 mL of LB in 25 mL flask) in fresh LB media and grown at 37 oC in a shaking chamber for 4 hours. One hundred fifty µL of the backdiluted bacterial culture (10% final volume) was added to a well after removing 150 µL of L15+ medium. Images were captured and analyzed as described previously. Salmonella strains are Biosafety Level 2 (BSL2) bacteria. Thus, all the chromatophore cell response assays that involved Salmonella were conducted in a BSL2 facility, approved by the Oregon State University’s Institutional Biosafety Committee. Chromatophore cell response assays with each bacterial strain were performed on chromatophore cells from at least two different fish. 41 Table 1: Bacterial strands and plasmids used in this study. Strain/plasmid S. typhimurium ATCC 70020 S. typhimurium ST10 S. typhimurium ST10 pTA108 S. typhimurium ST10 pTA108HilD S. typhimurium ATCC 14028 S. typhimurium ZA9 S. typhimurium ZA10 S. typhimurium ZA11 S. typhimurium ZA15 S. typhimurium ZA26 E. coli JM101 pTA108 (plasmid) Relevant Characteristics LT2 wildtype Derivative of ATCC 70020, hilD::EZ-Tn5 Kanr ST10 with pTA108 Kanr, Ampr ST10 with wild-type hilD gene, Kanr, Ampr IR715 Nalr Derivative of ATCC 14028, SopE2 mutant, Nalr Derivative of ATCC 14028, SipA mutant, Nalr Derivative of ATCC 14028, sptP mutant, Nalr Derivative of ATCC 14028, sopB mutant, Nalr Derivative of ATCC 14028, SipA/SopB mutant, Nalr F´ traD36 proA+B+ lacIq Δ (lacZ)M15/ Δ(lac-proAB) glnV thi lacZΔM15 bla (Ampr), 1-5 copies per cell Source ATCC Stephanie Dukovcic’s dissertation (231) This Study This Study Adams’s Lab (254) Adams’s Lab (254) Adams’s Lab (254) Adams’s Lab (254) Adams’s Lab (254) Adams’s Lab (254) Lab stock Lab stock (230) Polymerase Chain Reaction (PCR) PCR reactions were run using either a Perkin Elmer Gene Amp PCR system (model 2400) or Eppendorf Mastercycler® gradient machine. PCR samples contained 50100 ng of DNA, 1-2 µL of (20 µM) each primer (Table 2) and Platinum® PCR Super Mix HiFi (Invitrogen Cat. No. 11306016) to a final volume of 50µL in a 0.5 ml PCR epitube. Two controls, a negative control lacking DNA template, and a positive control with known pertinent products, were used with each PCR performed in this study. PCR reactions were subjected to 95 oC for 5 minutes to ensure complete initial denaturation, 42 and then went through 30 cycles of denaturation (95 oC for 30 seconds), annealing (set at Tm (Table 2) for 30 seconds) and extension (72 oC for one minute for each kb product). A final extension was conducted for 10 minutes to ensure that all products were fully extended by the polymerase. The PCR products were then analyzed by 1% agarose gel electrophoresis in TAE buffer (0.8 M tris-base, 0.35 M glacial acetic acid, 20 mM EDTA) to verify the presence of an amplified product. DNA bands were visualized by ethidium bromide staining. PCR products were purified using QIAquick® PCR Purification Kit (Qiagen, Cat. No. 28104) or DNA bands were excised from the agarose gel using a Qiagen Gel Extraction Kit (Cat. No. 28704). Bacterial Transformations Escherichia coli JM101 was transformed following a chemical competency protocol (228). Briefly, an overnight culture of E. coli in 5 mL LB media in a 25 mL flask was incubated at 37 oC with aeration. The overnight culture was back diluted (1:100), the next day, in 5 mL LB in a 25 mL flask and grown to mid-log phase (2-3 hours of incubation). One mL of the culture was transferred to a 1.5 mL epitube for each transformation and control. Each epitube was centrifuged in a microcentrifuge at maximum speed for 1 minute. Supernatant was decanted and cells were 43 Table 2: Primers used in this study. 44 resuspended in ~50 µL residual medium. Then, 100 µL of cold TSS (10 g PEG 3350 or 8000, 0.5 g MgSO4 7H2O, 88 mL LB, 5 mL DMSO) was added to the cell suspension in each epitube. Cells were incubated on ice while adding 1µL of plasmid DNA (10-50 ng). Cells were incubated on ice for 20 minutes and then heat shocked at 42 oC for 1.5 minutes and immediately returned to ice for 3 additional minutes. Nine hundred µL of LB was added to each epitube and incubated at 37 oC for 1 hour to allow the cells to recover. The transformed culture was then diluted 1:10 and 1:100. One hundred µL of each dilution was plated on the appropriate selective media. Plates were incubated overnight at 37 oC. Several well isolated colonies were restreaked to fresh plates and incubated overnight at 37 oC. Plasmids were extracted from 5 mL overnight cultures using the QIAprep® Spin Miniprep Kit (Cat. No. 27106). The correct plasmid was verified by restriction digest of plasmid mini-preps and sequencing. Salmonella typhimurium was transformed following an amended electrocompetency protocol (227). A 5 mL overnight culture of ST10 (S. typhimurium mutant) was diluted into 500 mL LB (1:100) and transferred to a 1 L flask. The culture was incubated at 370C with heavy aeration (250 rpm) for 2 hours to bring it up to late log phase. From this point on, every step was performed on ice and all the materials/equipment and reagents were kept chilled. The culture was divided into centrifuge bottles and spun at 5,000 rpm for 15 minutes at 4 oC using a Beckman JA 12 rotor. Supernatant from the culture was discarded and cells pellets were resuspended in 100 mL sterile ice water. The cells were spun at 5,000 rpm for 15 minutes at 4 oC. Supernatant was discarded and cell pellets were resuspended in 50 mL sterile ice water 45 and combined into on centrifuge bottle. The cells were centrifuged under the same conditions. The cells were resuspended in 2 mL 10% glycerol and spun at 5,000 rpm for 15 minutes at 4 oC. In the final step, the cells were resuspended in 400 µL 10% glycerol. The electrocompetent cells were ready for immediate use. However, any left over cells could be frozen at -80 oC. Forty µL of electrocompetent cells were used for each electroporation. On ice, 50-100 ng DNA was added to electrocompetent cells and mixed well by pipetting up and down. The mixture was then transferred to a 0.2 cm prechilled electrocuvette and tapped to ensure the removal of any air bubbles. Using a BioRad Gene Pulser set at 1.5-1.8 kV, 25 µF and 200 Ω, a single electric pulse (4-5 ms) was applied. Immediately after discharge, 1 mL of LB was added to cells and they were incubated at 37 oC for 1 hour with heavy aeration (250 rpm) to allow the cells recover. The transformed cells were spread on LB plates containing 50 µg/ml ampicillin for each transformation sample and control as follows: a 10 µL, 100 µL and a concentrated 100 µL (900 µL remaining cells were spun and resuspended in 100 µL LB) aliquot. The LB agar plates were incubated overnight at 37 oC. Several well isolated colonies were restreaked on fresh LB plates containing 50 µg/ml ampicillin and incubated overnight at 37 oC. A 5mL overnight culture was used for mini prep using the QIAprep® Spin Miniprep Kit (Cat. No. 27106). The correct plasmid was verified by PCR of plasmid mini-preps, and sequencing. A 1mL glycerol stock of each confirmed transformant was prepared and stored at -80 0C. 46 Identifying Transposome™ Insertion Site(s) and Sequencing All sequencing was conducted by the Center for Genome Research and Biocomputing (CGRB, Oregon State University) using an ABI 3730 capillary sequence machine. Templates and primers concentrations were optimized to the specifications of the CGRB. All the sequences received from CGRB were then aligned and analyzed using BioEdit Sequence Alignment Editor version 7.0.9.0. To find the transposome insertion site in ST10 (S. typhimurium mutant), genomic DNA from ST10 was extracted using an Ultra Clean Microbial DNA Isolation Kit (Cat. No. 12224-50-SF). The extracted genomic DNA from ST10 was used as template for Random Amplification of Transposon Ends (RATE) PCR (229). The PCR products were run on a 1% agorose gel and samples with a visible band were purified by the QIAquick® PCR Purification Kit. The purified PCR product was then sequenced. The sequence was analyzed using BioEdit and sequence was identified using the BLAST program at NCBI (blast.ncbi.nlm.gove/blast.cgi) database. Complementation To complement the Tn5::hilD insertion in the S. typhimurium mutant ST10, the hilD gene including its promoter and part of the Fur box were cloned into a low-copy number plasmid (1-5 copies per cell), pTA108. Genomic DNA from S. typhimurium was amplified with specific primers (Table 2), cloned into the TOPO TA cloning vector using TOPO TA Cloning® Kit (Invitrogen™, Cat. No. K4575-01SC), and transformed into E. coli JM101. A 60µL and 150µL aliquot of the transformation mixture was plated on LB plates containing 50 µg/ml ampicillin. Several well isolated colonies were plated on fresh 47 LB plates containing 50 µg/ml ampicillin overnight at 37 oC. An overnight culture of a single white colony from the LB plates containing 50 µg/ml ampicillin was incubated at 37 oC with aeration. The next day plasmid was extracted from the overnight culture using QIAprep® Spin Miniprep Kit (Cat. No. 27106). M13 forward and reverse primers provided with the TOPO Kit were used in a PCR reaction to check for the insert, and the PCR products were run on a 1% agarose gel. The PCR product was then cleaned up with QIAuick® PCR Purification Kit (Qiagen, Cat. No. 28104), and sequence confirmed. Topo::hilD plasmid and pTA108 plasmid were double digested using the restriction enzymes Sal1-HiFi and EcoR1-Hifi from NEB. The double digested products were run on an agarose gel, and single bands were extracted from the gel using a Clontech Gel Extraction Kit. DNA Dephos & Ligation Kit (Roche, Ref. 04898117001) was used to perform a ligation on the double digested pTA108 and insert. Ligations were carried out at 16 oC overnight, then heat inactivated at 65 oC for 20 minutes. The ligated product (pTA108hilD) was chemically transformed into E. coli JM101, as described previously. An overnight culture of selected colonies from the transformation were prepared and QIAprep® Spin Miniprep Kit (Cat. No. 27106) was used to extract the plasmid. pTA108 screening primers were used in a PCR reaction to screen for pTA108hilD. The PCR product was run on a 1% agarose gel and the right size single bands were confirmed. The PCR products were then cleaned up and sequenced. The sequence was analyzed and confirmed pTA108hilD. The pTA108hilD plasmid was then electroporated into ST10 electrocompent cells. An empty pTA108 was also electroporated into ST10 as a control. Transformants 48 were selected on LB plates containing 50 µg/ml ampicillin and plasmid was extracted. The extracted plasmids were screened by PCR using specific hilD forward and reverse primers and correct products size was confirmed on a 1% agarose gel. The PCR products were then cleaned up, and sent to CGRB for sequencing, and sequences were confirmed against the S. typhimurium sequence at NCBI. A complementation assay on B. splendens erythrophores, as described in the Response Assay and Computational Analysis sections, was performed to determine whether or not the ST10-pTA108hilD transformant complemented the ST10 phenotype. 49 Chapter 4 Results The Physiological Response Betta splendens Erythrophore Cells The Betta splendens chromatophore cell type, erythrophore, a neuron-like cell with predominately red pigmented organelles, was used in this study. The erythrophore cell’s physiological responsiveness in primary tissue culture is well characterized (204, 208, 204, 213, 231, 237). Physiological responsiveness in primary tissue culture is assessed using the neurotransmitters, Clonidine (Cl) and α-Melanocyte Stimulating Hormone (MSH). Both neurotransmitters induce pigment organelle translocation in erythrophore cells in a characteristic fashion. Erythrophore cells were isolated from the fins of red B. splendens and maintained in primary tissue culture. Erythrophore cells were exposed to 100 nM Clonidine, 100 nM MSH and LB medium (Luria broth; used to culture bacterial cells) for 60 minutes. Erythrophore cell response to the bacterial culturing medium, Luria broth (LB), was assessed because subsequent studies in this research effort characterize erythrophore cell response to the bacterium, Salmonella typhimurium, cultured in LB medium. Figures 1A, B, and C illustrate erythrophore cell response to 100nM Clonidine, 100nM MSH, and LB at time zero (left panels) and 60 minutes (right panels) after exposure. The data described in Figure 1 were obtained from two different red B. splendens erythrophore cell preparations. Erythrophore cell response, upon exposure to 100nM Clonidine, was 50 characterized by the rapid aggregation of pigment organelles to the center of the cell within one minute, with this response plateauing by 5 minutes (Figure 1A and 1D). The aggregation response induced by Clonidine, and mathematically described as a negative percent pigment area change (Figure 1D), has been previously reported (204, 208, 204, 213, 231, 237). Erythrophore cell response, upon exposure to 100 nM MSH, was characterized by a slow and steady dispersion of pigment organelles to the edge of the cell, with this response plateauing by 30 minutes, (Figure 1B and 1D). The dispersive response induced by MSH, and mathematically described as a positive percent pigment area change (Figure 1D), has been previously reported (204, 208, 204, 213, 231, 237). Erythrophore cell response, upon exposure to the bacterial culturing medium, Luria broth (LB), was characterized by slight dispersion, but dispersion was negligible and not at the magnitude as the response observed upon exposure to MSH (Figure 1C and 1D). 51 A B D Change in pigment area (%) C 40 30 20 10 0 -­‐10 -­‐20 -­‐30 -­‐40 -­‐50 -­‐60 -­‐70 0 10 20 30 40 50 60 Time (minutes) Figure 1: Betta splendens erythrophore cell response to Clonidine, MSH, and LB. Erythrophore cells before (left panels) and after (right panels) exposure for 60 minutes to: (A) Clonidine, (B) MSH, and (C) LB. Magnification of erythrophore cells is at 100X. (D) Graphical representation of erythrophore cell area change (percent) in response to: (u) Clonidine, (¢) MSH, and (p) LB. A negative area change describes an aggregation response, and a positive area change describes a dispersion response. Data represent the mean values of two trials. Error bars represent the standard deviation. 52 Betta Splendens Erythrophore Cell Response To Wildtype Salmonella Typhimurium And Salmonella Typhimurium ST10 Mutant Previous reports describe Betta splendens erythrophore cell response to foodassociated bacterial pathogens, such as Bacillus cereus and Salmonella typhimurium, and nonpathogenic mutants of these bacterial strains (204, 208, 204, 213, 231, 237). In a previous study examining erythrophore cell response to S. typhimurium, mutants were generated using the commercially available EZ-Tn5 mutagenic vector system (231). Several mutants from the pool of EZ-Tn5™ mutagenized S. typhimurium were identified that appeared not to induce an aggregation response in erythrophore cells (231). One S. typhimurium mutant, ST10, was examined further. Erythrophore cells were exposed to wildtype S. typhimurium and S. typhimurium ST10 mutant. Figures 2A and B illustrate the erythrophore cell response to wildtype S. typhimurium and S. typhimurium ST 10 mutant at time zero (left panels) and 60 minutes (right panels) after exposure. The data described in Figure 2 were obtained from two different red B. splendens erythrophore cell preparations. Erythrophore cell response, upon exposure to wildtype S. typhimurium, was characterized by aggregation of pigment organelles to the center of the cell, with this response initiating approximately 30 minutes after exposure to this bacterial pathogen (Figure 1A and 1D). The aggregation response induced by S. typhimurium is mathematically described as a negative percent pigment area change (Figure 1D). In contrast, erythrophore cell response, upon exposure to S. typhimurium ST10 mutant, was characterized by slight dispersion of pigment organelles after 20 minutes exposure followed by slight aggregation that resulted in very little 53 change of pigment distribution after one hour of exposure to the ST10 mutant. The slight dispersion followed by the slight aggregation of pigment organelles upon exposure to the ST10 mutant, was negligible and not at the magnitude as the response observed upon exposure to the dispersive agent, MSH, or the aggregative agent, Clonidine, or wildtype S. typhimurium. 54 A B C Change in pigment area (%) 40 30 20 10 0 -­‐10 -­‐20 -­‐30 -­‐40 -­‐50 0 10 20 30 40 50 60 Time (minutes) Figure 2: Betta splendens erythrophore cell response to wildtype Salmonella typhimurium and Salmonella typhimurium ST10 mutant. Erythrophore cells before (left panels) and after (right panels) 60 minute exposures to: (A) wildtype Salmonella typhimurium, and (B) Salmonella typhimurium mutant ST10. Magnification of erythrophore cells is at 100X. (C) Graphical representation of Erythrophore cell area change in response to: () Salmonella typhimurium Wildtype, and (✕) Salmonella typhimurium mutant, ST10. A negative area change describes an aggregation response, and a positive area change describes a dispersion response. Data represent the mean values of two trials. Error bars represent the standard deviation. 55 Identification Of hilD Gene Product And Complementation Of hilD Function The S. typhimurium ST10 mutant does not induce, in erythrophore cells, pigment organelle translocation in a manner similar to wildtype S. typhimurium suggesting a mutation interrupted a gene whose product is involved in this process. Molecular analysis of the ST10 mutant, using RATE PCR and sequencing the products, revealed that the EZ-Tn5 mutagenic vector interrupted the hilD gene (Figure 3). As described below, complementation of the mutant phenotype was used to demonstrate that a mutation in hilD was responsible for the ST10 mutant phenotype. By adding back wildtype hilD gene to the ST10 mutant, presumably this would add back the ability to induce an aggregation of pigment organelles in erythrophore cells. The complete sequence of the hilD gene, including an upstream partial Fur box (FurB), was amplified from wild-type S. typhimurium genomic DNA using specific primers (Figure 4). hilD was cloned into TOPO TA cloning vector, using TOPO TA Cloning® Kit, and transformed into E. coli JM101. The confirmed TOPO::hilD plasmid and pTA108 plasmid were double digested using the restriction enzymes Sal1-HiFi and EcoR1-HiFi, followed by ligation. The pTA108-hilD recombinant plasmid was electroporated into ST10 mutant. As a control, the pTA108 vector was electroporated into ST10 mutant. Transformants were selected on LB-Amp25 and successful construction of pTA108-hilD and pTA108 were confirmed by restriction digest and sequence analysis (Figure 4). 56 Figure 3: Identification of hilD gene: Illustration of the EZ-Tn5™ transposome insertion in the hilD gene. EZ-Tn5™ was inserted using EZ-Tn5TM <KAN-2>Tnp Transposome™ Kit. RATE PCR was used to determine the location of the EZ-Tn5™. The EZ-Tn5™ was inserted in the middle of the hilD gene. 57 Figure 4: Cloning hilD: The complete sequence of the wildtype hilD gene and an upstream partial Fur box (FurB) was amplified from wild-type S. typhimurium genomic DNA. hilD was cloned into TOPO TA cloning vector and transformed into E. coli JM101. TOPO::hilD plasmid and pTA108 plasmid were double digested with Sal1-HiFi and EcoR1-HiFi, followed by ligation. The pTA108-hilD recombinant plasmid was electroporated into ST10 mutant. As a control, the pTA108 vector was electroporated into ST10 mutant. Transformants containing either pTA108-hilD or pTA108 were confirmed by restriction digest and sequence analysis of the isolated plasmids. 58 Erythrophore Cell response To Salmonella typhimurium Wildtype, ST10 Mutant, ST10-pTA108 and ST10-pTA108-hilD Betta splendens erythrophore cells were exposed to wildtype S. typhimurium, S. typhimurium ST10 mutant, ST10 containing pTA108, ST10 containing pTA108-hilD. Erythrophore cell response, upon exposure to wildtype S. typhimurium, was characterized by aggregation of pigment organelles to the center of the cell, with this response initiating approximately 30 minutes after exposure to this bacterial pathogen (Figure 5). The aggregation response induced by S. typhimurium is described as a negative percent pigment area change (Figure 5). In contrast, erythrophore cell response, upon exposure to S. typhimurium ST10 mutant, was characterized by slight dispersion of pigment organelles after 20 minutes exposure followed by slight aggregation that resulted in very little change of pigment distribution after one hour of exposure to the ST10 mutant (Figure 5). Erythrophore cell response, upon exposure to S. typhimurium ST10 mutant containing just the vector, pTA108, was similar to the erythrophore cell response to the ST10 mutant without the vector. Interestingly, Erythrophore cells response to st10 containing copy of wild type hilD gene did not show a response as to wildtype S.typhimurium, which led me to question my experimental design and let it go longer than the 60 minutes. 59 40 Change in pigment area (%) 30 20 10 0 -­‐10 -­‐20 -­‐30 -­‐40 -­‐50 0 10 20 30 40 50 60 Time (minutes) Figure 5: Betta splendens erythrophore cell response to wildtype Salmonella typhimurium, Salmonella typhimurium ST10 mutant, ST10 containing pTA108, and ST10 containing pTA108-hilD. Graphical representation of erythrophore cell area change in response to: () Salmonella typhimurium Wildtype, (x) Salmonella typhimurium mutant, ST10, () ST10-pTA108, and (u) ST10-pTA108-hilD. A negative area change represents an aggregation response, and a positive area change presents a dispersion response. Data represent the mean values of two trials. Error bars represent the standard deviation. 60 The experimental design of the previous experiment was modified to ensure that the result was not due to experimental artifact. Erythrophore cells were exposed to wildtype S. typhimurium, S. typhimurium ST10 mutant, ST10 containing pTA108, ST10 containing pTA108-hilD for 90 minutes instead of 60 minutes (Figure 6). Erythrophore cell response, upon exposure to wildtype S. typhimurium, was characterized by aggregation of pigment organelles to the center of the cell, with this response initiating approximately 30 minutes after exposure to this bacterial pathogen (Figure 6). The aggregation response induced by S. typhimurium is described as a negative percent pigment area change (Figure 6). In contrast, erythrophore cell response, upon exposure to S. typhimurium ST10 mutant, was characterized by slight dispersion of pigment organelles after 20 minutes exp osure followed by slight aggregation that resulted in very little change of pigment distribution after 90 minutes of exposure to the ST10 mutant (Figure 6). Erythrophore cell response, upon exposure to S. typhimurium ST10 mutant ontaining just the vector, pTA108, was similar to the erythrophore cell response to the ST10 mutant without the vector (Figure 6). Interestingly, after 90 minutes exposure to S. typhimurium ST10 mutant containing pTA108-hilD, erythrophore cell response appeared to be more similar to that induced by wildtype S. typhimurium. 61 40 30 Area Change Figure20 5: Betta splendens erythrophore cell response to wildtype Salmonella typhimurium, Salmonella typhimurium ST10 mutant, ST10 containing pTA108, and ST10 10 containing pTA108-hilD. Graphical representation of erythrophore cell area change in response0 to: () Salmonella typhimurium Wildtype, (x) Salmonella typhimurium mutant, ST10, () ST10-pTA108, and (u) ST10-pTA108-hilD. A negative area change -­‐10 an aggregation response, and a positive area change presents a dispersion represents response. Data represent the mean values of two trials. Error bars represent the standard -­‐20 deviation. -­‐30 -­‐40 -­‐50 -­‐60 0 10 20 30 40 50 Time (min) 60 70 80 90 Figure 6: Betta splendens erythrophore cell response to wildtype Salmonella typhimurium, Salmonella typhimurium ST10 mutant, ST10 containing pTA108, and ST10 containing pTA108-hilD. Graphical representation of erythrophore cell area change in response to: () Salmonella typhimurium Wildtype, (x) Salmonella typhimurium mutant, ST10, () ST10-pTA108, and (u) ST10-pTA108-hilD. A negative area change represents an aggregation response, and a positive area change presents a dispersion response. Data represent the mean values of two trials. Error bars represent the standard deviation. 62 Betta Splendens Erythrophore Cell Response To Salmonella typhimurium Bovine Isolate And Salmonella typhimurium Human Isolate Salmonella typhimurium strains containing mutations in sipA, sopB, sopE2 and sptP genes were created in a S. typhimurium bovine isolate strain. To confirm if there is any difference between the erythrophore cells response to S. typhimurim bovine isolate and S. typhimurium human isolate, erythrophore cells were exposed to each one of the two strains. Figure 7 illustrates erythrophore cell response to S. typhimurium bovine isolate and S. typhimurium human isolate. The data described in Figure 7 were obtained from two different red B. splendens erythrophore cell preparations. Erythrophore cell response, upon exposure to either S. typhimurium human isolate or bovine isolate, was characterized by aggregation of pigment organelles to the center of the cell, with this response initiating approximately 30 minutes after exposure to either isolate of this bacterial pathogen (Figure 7). The aggregation response induced by both S. typhimurium strains is mathematically described as a negative percent pigment area change (Figure 7). Erythrophore cell response, upon exposure to the bacterial culturing medium, Luria broth (LB), was characterized by slight dispersion, but dispersion was negligible and not at the magnitude as the response observed upon exposure to MSH (Figure 7). 63 40 Change in pigment area (%) 30 20 10 0 -­‐10 -­‐20 -­‐30 -­‐40 -­‐50 0 10 20 30 40 50 60 70 Time (minutes) Figure 7: Betta splendens erythrophore cell response to Salmonella typhimurium (human isolate), Salmonella typhimurium wildtype (bovine isolate), and LB. Graphical representation of erythrophore cell area change in response to: () LB, (u) S. typhimurium bovine isolate, and (¢) S. typhimurium human isolate. A negative area change represents an aggregation response, and a positive area change presents a dispersion response. Data represent the mean values of two trials. Error bars represent the standard deviation. 64 Betta Splendens Erythrophore Cell Response To Salmonella typhimurium With Mutations In Effector Protein SopE2, SipA, Or SptP Genes Erythrophore cells were exposed to wildtype S. typhimurium bovine isolate or isogenic mutants of this strain containing mutations in specific effector protein genes. Figure 8 illustrates erythrophore cell response to S. typhimurium bovine isolate and isogenic mutant strains containing mutations in either sopE2, sipA, or sptP. The data described in Figure 8 were obtained from two different red B. splendens erythrophore cell preparations. Erythrophore cell response, upon exposure to S. typhimurium bovine isolate is characterized by aggregation of pigment organelles to the center of the cell, with this response initiating approximately 30 minutes after exposure to either isolate of this bacterial pathogen (Figure 8). Mutations in sopE2, sipA, or sptP genes did not dramatically change erythrophore cell response to S. typhimurium as the magnitude and kinetics of the response was similar to that observed by wildtype S. typhimurium. 65 40 Change in pigment area(%) 30 20 10 0 -­‐10 -­‐20 -­‐30 -­‐40 -­‐50 -­‐60 0 10 20 30 40 50 60 70 Time (minutes) Figure 8: Betta splendens erythrophore cell response to wildtype Salmonella typhimurium bovine isolate and specific effector protein mutants with mutations in sopE2, sipA, or sptP. Graphical representation of erythrophore cell area change in response to: () wildtype S. typhimurium bovine isolate, () S. typhimurium sopE2 mutant, (¢) S. typhimurium sipA mutant, and (u) S. typhimurium sptP mutant. A negative area change represents an aggregation response, and a positive area change presents a dispersion response. Data represent the mean values of two trials. Error bars represent the standard deviation. 66 Betta Splendens Erythrophore Cell Response To Salmonella typhimurium With Mutations In Effector Protein SopB Or SipA/SopB Genes Erythrophore cells were exposed to wildtype S. typhimurium bovine isolate or isogenic mutants of this strain containing mutations in specific effector protein genes. Figure 9 illustrates erythrophore cell response to S. typhimurium bovine isolate and isogenic mutant strains containing mutations in either in sopB or sipA/sopB. The data described in Figure 9 were obtained from two different red B. splendens erythrophore cell preparations. Erythrophore cell response, upon exposure to S. typhimurium bovine isolate, is characterized by aggregation of pigment organelles to the center of the cell, with this response initiating approximately 30 minutes after exposure to this bacterial pathogen (Figure 9). Mutations in sopB or sipA/sopB genes did change erythrophore cell response to S. typhimurium as the magnitude and kinetics of the response was different to that observed for the wildtype S. typhimurium. Although slight aggregation of pigment organelles eventually occurred in the presence of either the sopB or sipA/sopB mutant strains, this response was not to the magnitude observed by wildtype S. typhimurium. 67 40 Change in pigment area (%) 30 20 10 0 -­‐10 -­‐20 -­‐30 -­‐40 -­‐50 0 10 20 30 40 50 60 70 Time (minutes) Figure 9: Betta splendens erythrophore cell response to wildtype Salmonella typhimurium bovine isolate and specific effector protein mutants with mutations in sopB and sipA/sopB. Graphical representation of erythrophore cell area change in response to: () wildtype S. typhimurium bovine isolate, (¢) S. typhimurium sopB mutant, and (u) S. typhimurium sipA/sopB double mutant. A negative area change represents an aggregation response, and a positive area change presents a dispersion response. Data represent the mean values of two trials. Error bars represent the standard deviation. 68 Chapter 5 Discussion The Response of Betta Splendens Erythrophore To Salmonella typhimurium ST10 Mutant Chromatophore cells isolated from Betta splendens exhibit great potential as a unique cell-based biosensor able to respond to the presence of biological and chemical toxicants by dispersing or aggregating their pigment organelles (202, 207, 208, 204, 231, 237, 238). Numerous studies reveal that the chromatophore cell type, erythrophore, can rapidly detect several food associated bacterial pathogens, including S. typhimurium (202, 207, 208, 204, 231, 237, 238). Previously tested hypotheses, using mutagenesis to analyze the attributes of S. typhimurium contributing to a response in erythrophore cells, revealed a potential role for the T3SS apparatus coded for by prgHIJK (231). Although wildtype S. typhimurium rapidly induces pigment organelles to undergo an aggregative response in erythrophore cells, S. typhimurium containing a mutation in the prgHIJK operon does not induce pigment organelles to undergo an aggregative response in erythrophore cells (231). A mutation (ST10 mutant) identified in a region different from the mutation that disrupted the prgHIJK operon had a similar, but not identical impact on erythrophore cells. The first objective of this study was to test the hypothesis that S. typhimurium mutant ST10 has a mutation residing in either gene(s) coding for the process regulating expression of the prgHIJIK operon or the gene(s) coding for the effector proteins traveling through the PrgHIJK apparatus. The approaches used to test this 69 hypothesis included sequencing the region containing the mutation and identifying the gene(s) impacted by this mutation through comparative sequence analysis, cloning the wildtype gene sequence, and using this wildtype gene sequence to complement the mutant phenotype thereby demonstrating the mutation is linked to the resulting biological outcome in erythrophore cells. Salmonella typhimurium mutant ST10 does not induce an aggregation response in erythrophore cells similar to that observed with the isogenic wildtype S. typhimurium strain. This suggested the mutation had interrupted a gene whose product(s) is involved in induction of aggregation in erythrophore cells. Molecular analysis of the ST10 mutant using the RATE PCR method revealed that the EZ-Tn5™ transposome had interrupted the hilD gene. The 1221bp EZ-Tn5™ transposome was inserted in the hilD open reading frame between nucleotide number 3018490 and 3018491 (NCBI, LT2 sequence numbering), which corresponds to amino acid number 220 (Serine) (253). The hilD gene resides between the hilA gene and the prgHIJK operon, with the hilA gene oriented in the same direction as hilD and prgHIJK in the opposite direction on Salmonella pathogencity island 1 (SpI-1) (Figure 10). Interestingly, most of other genes located on the SPI-1 reside in opposite orientation of the hilD gene (Figure 10). The regulatory region of the hilD gene contains a Fur box (putative Fur Box A at -191 to 163, and putative Fur Box B At -48 to -30) and a RNA polymerase binding site at -35 upstream of the start codon. HilD encodes a 309 amino acid protein with a described function as an invasion regulatory protein (253). The location of the insertion in the hilD gene and the orientation and regulatory features of this gene suggests the insertion has 70 only impacted hilD gene function, presumably through loss of hilD expression. A polar effect on the hilA gene, which is adjecent to the hilD gene and in the same orientation, was roled out for two reasons. One, hilA has its own promotor (255). Second, the distance between the two genes is more than one thousand base pair, which is greater than typical for genes in an operon. Figure 10. Salmonella Pathogenicity Island 1 (SPI-1) Genetic Organization. This figure shows the position of hilD on SPI-1. The blue colored arrows indicate the genes and orientation of the genes encoding structural proteins of Type Three Secretion System 1 apparatus. The red colored arrows indicate the genes and orientation of the genes encoding for transcriptional regulators. The blue outlined arrows represent the effector proteins and effector proteins related proteins The hilD gene product positively controls expression of hilA (87). HilA activates and controls expression of SPI-1 and is responsible for inducing expression of the T3SS1 apparatus genes, prgHIJK, and/or expression of genes encoding effector proteins (86, 88). With respect to the first tested hypothesis in this study, it appears that S. typhimurium ST10 mutant has a mutation residing in a gene coding for the process regulating expression of the prgHIJIK operon, and this mutation impacts pigment organelle movement. The impact of the hilD gene product on pigment organelle movement in erythrophore cells raises two intriguing questions especially in light of what is previously 71 known about the role of the hilD gene product in the invasion of mammalian host cells. First, why does a mutation in hilD result in failure of Salmonella typhimurium to induce aggregation of pigment organelles in erythrophore cells? And second, does the hilD gene product play a crucial role in inducing pigment organelle movement in erythrophore cells? Given that S. typhimurium has the transcriptional regulators HilC and RtsA, with similar function as HilD, presumably HilC and RtsA can potentially duplicate HilD function by positively controlling expression of hilA. The HilC and RtsA regulators are capable of regulating SPI-1 through hilA or by directly binding to invF, leading to SPI-1 activation (247, 248) (Figure 11). However, this apparent duplication of function is not enough to overcome the impact of a hilD mutation as it relates to pigment organelle movement in erythrophore cells. Perhaps, the reason the hilD mutant cannot induce pigment aggregation in erythrophore cells is due to other functions of the hilD gene product. For example, the hilD gene product belongs to the AraC/XylS family, which typically act as derepressors and not as typical activators of transcription (249). In S. typhimurium, the hilD gene product activates hilA by counteracting the effect of negative transcriptional regulators (e.g. Hha, HilE, Pag, and RNase E) that may repress hilA by binding to an upstream site located in the regulatory region of the hilA promoter (Figure 11). Boddicker D. et. al. concluded that hilD gene is required for activating hilA expression even when known negative regulators are absent (249), suggesting that hilD was an absolute requirement and its activity could not be replaced. Given this explanation, then presumably the failure to activate hilA expression through activity of 72 the hilD gene product would result in the failure to express the T3SS-1 apparatus genes, prgHIJK, and/or expression of genes encoding effector proteins regardless of other activating pathways. As demonstrated previously through mutational analysis, a mutation disrupting the prgHIJK operon impacts pigment organelle movement in erythrophore cells (231). Figure 11: A model of transcriptional regulation of SPI-1. Green arrows indicate a direct activation effect. Red lines indicate direct repression. The thick green and green outlined arrows indicate the pathway leading to SPI-1 activation (248) Salmonella typhimurium mutant, ST8, containing a mutation in the prgHIJK operon responsible for encoding the T3SS-1 needle-like apparatus, does not induce 73 pigment organelles to aggregate in erythrophore cells by one hour, but after four hours exposure to this mutant the pigment organelles do fully aggregate (231). This observation suggests a potential second pathway, possibly similar to that encoded by prgHIJK, for S. typhimurium to induce pigment organelle aggregation in erythrophore cells. Interestingly, S. typhimurium mutant, ST10, containing a mutation in the hilD gene responsible for regulating expression of hilA gene, does not induce aggregation of pigment organelles even after four hours. This observation suggests there is no other activity that can substitute for HilD and that this regulator is crucial to the S. typhimurium mechanism involved in aggregating pigment organelles in erythrophore cells. HilD positively regulates and enhances hilA expression, which is responsible for activating the prgHIJK and invF operons, SPI-1 operons encoding T3SS needle-like apparatus and effector proteins that lead to invasion, respectively. Similar to HilD, HilC (encoded within SPI-1) and RtsA can also regulate the expression of hilA. The transcriptional regulators, hilD, hilC, and RtsA regulate each other and themselves. Alternatively, HilD can directly activate expression of the SPI-1 operon, invF, without regulating hilA (243). Given the absolute requirement for the hilD gene product in the erythrophore cell response to S. typhimurium, and the hypothesis that there might be duplicative activity to backup the functions encoded by the prgHIJK operon, suggests there are other factors encoded by S. typhimurium involved in the erythrophore cell response. Salmonella typhimurium ST10 Mutant Complementation Complementing the mutant phenotype displayed by the ST10 mutant was used to demonstrate that a mutation in hilD was responsible for the ST10 mutant phenotype. 74 Presumably adding back a wildtype copy of the hilD gene would add back the ability to induce an aggregation of pigment organelles in erythrophore cells. The wildtype hilD gene, with partial Fur box (FurB), was cloned into a low copy number plasmid and transformed in to the ST10 mutant. As hypothesized, the ST10 mutant containing a wildtype copy of the hilD gene induced an aggregation response in erythrophore cells similar to that induced by the isogenic wildtype strain of S. typhimurium. However, erythrophore cell response to the ST10 mutant containing a wildtype copy of the hilD gene was delayed and the magnitude of pigment organelle aggregation was reduced compared to that induced by the isogenic wildtype strain of S. typhimurium. The delay in the erythrophore cell response, and the reduced magnitude in pigment organelle area change in erythrophore cells suggest that only partial complementation of the mutant phenotype was achieved. Partial complementation due to more than one insertional mutation was ruled out because the EZ-Tn5™ transposome was found only to be inserted in the hilD gene. Partial complementation might have been due to either the vector used or design of the insert used to clone hilD gene. Although the vector is a low copy number vector with an origin of replication estimated to produce 2-3 copies per cell, this copy number still might not have been low enough to express functional hilD under conditions not toxic to the complemented mutant. Alternatively, the isolated DNA fragment cloned into the low copy number vector coded for the full length open reading frame (ORF) of hilD but only contained a short upstream sequence coding for a partial Fur box (FurB). Perhaps, the fragment with the complete hilD gene needed to also contain a complete Fur box (Fur A/B) for full complementation of the mutant phenotype. Recent studies have 75 shown that the Fur (ferric uptake regulator) protein (in its metal form), an iron homeostasis regulator, binds to an AT-rich region (Fur A box) upstream of hilD promoter to enhance hilD expression (248). Fur protein activates SPI-1 expression by enhancing hilD expression (245, 246). Several reports suggest that Fur also negatively regulates HNS, a global regulator that negatively regulates all the transcriptional regulators, hilD, hilC, RtsA, and hilA (Figure 10) (247, 248). Teixidó et al. concluded that Fur, in its metal-bound form Fur.Fe2+, is needed to directly activate hilD expression (248). Therefore, complementing a mutant hilD phenotype as it relates to pigment organelle movement in erythrophore cells might require multiple layers of interactions between regulators that might be difficult to perfectly reconstruct through simple complementation of a mutant gene. Betta Splendens Erythrophore Cells Response To Salmonella typhimurium Effector Protein Mutants The second objective of this study was to test the hypothesis that the effector proteins of T3SS are the components of S. typhimurium’s invading mechanism directly involved in inducing pigment organelles to undergo an aggregative response in erythrophore cells. The approach used to test this hypothesis involved testing the response of erythrophore cells to S. typhimurium strains containing targeted, well characterized mutations in genes coding for specific T3SS effector proteins. Because these targeted mutations were in a S. typhimurium strain isolated from bovine rather than humans, it was necessary to first determine that erythrophore cells responded similarly to S. typhimurium regardless of the source of isolation. Erythrophore cells respond to S. 76 typhimurium strains by aggregating their pigment organelles within 60-70 minutes regardless of the source of isolation. Interestingly, the human isolate induces the aggregation of pigment organelles slightly faster than the bovine isolate. Mutations in sopE2, sipA, or sptP genes did not change erythrophore cell response to S. typhimurium as the magnitude and kinetics of the response was similar to that observed with wildtype S. typhimurium. Mutations in sopB or sipA/sopB genes did change erythrophore cell response to S. typhimurium as the magnitude and kinetics of the response was different to that observed for the wildtype S. typhimurium. Although slight aggregation of pigment organelles eventually occurred in the presence of either the sopB or sipA/sopB mutant strains, this response was not to the magnitude observed with wildtype S. typhimurium. Salmonella typhimurium sipA mutant induced an aggregation response in erythrophore cells similar to S. typhimurium wildtype. This result suggests SipA is not directly involved in pigment organelle movement in erythrophore cells. In leucocytes, SipA enhances SipC activity by binding actin filaments to induce polymerization and stabilize the actin filaments by up-regulating T-plastin activity, a localized actin bundling protein (131-134). Previous studies have shown that S. typhimurium sipA mutant slightly delay S. typhimurium invasion process of epithelial cells (85, 252). Similar to the result with the sipA mutant, the S. typhimurium sopE2 mutant induced an aggregation response in erythrophore cells similar to S. typhimurium wildtype (Figure 8). This result suggests SopE2 is not directly involved in pigment organelle 77 movement in erythrophore cells. Pigment organelles in erythrophore cells move along microtubule and actin filaments in an aggregation or dispersion response (250, 251). Previous reports showed in leucocytes, SopE2 stimulates host Rho GTPase proteins which are responsible for promoting the actin assembly and polymerization (138, 133). Presumably SopE2 should be an important effector protein in the aggregation response in erythrophore cells. Based on this prediction, a mutation in sopE2 might have had a dramatic impact on the aggregation response in erythrophore cells. However, this prediction was not realized with this experimental approach. Perhaps, because of the redundancy between sopE and sopE2, the lack of SopE2 was compensated for by SopE, thus, the sopE2 mutant’s ability to induce an aggregation response in erythrophore cells was not impaired. S. typhimurium sptP mutant also induced an aggregation response in erythrophore cells similar to S. typhimurium wildtype. This result suggests SptP is not directly involved in pigment organelle movement in erythrophore cells. SptP is involved in restoring changes in the host membrane and promoting cell cytoskeleton recovery after rearrangement of microfilaments and membrane enfolding. It was hypothesized that the lack of SptP in S. typhimurium would result in an increase in S. typhimurium invasiveness. In agreement with this hypothesis, we observed a slight increase in the magnitude of pigment organelle aggregation in erythrophore cells in response to S. typhimurium sptP mutant as compared to wildtype S. typhimurium. In contrast to the results observed with the sipA, sopE2, and sptP mutants, S. 78 typhimurium sopB mutant and sipA/sopB double mutant induced a response in erythrophore cells that was different in magnitude and kinetics to that observed for the wildtype S. typhimurium. Both mutants induced slight pigment organelle aggregation, after 55 minutes of exposure, in erythrophore cells; however, the magnitude of the response was less than that observed with the wildtype S. typhimurium. The fact that the sipA mutant is able to induce an aggregation response in erythrophore cells suggests that the inability of the sipA/sopB mutant to induce a similar aggregation response in erythrophore cells is due to lack of sopB. This is the first evidence in support of a role for the SopB effector protein in pigment organelle aggregation in erythrophore cells. Even though, it is clear the effector proteins secreted by T3SS-1 encoded by SPI-1 have a certain degree of redundancy and they work in concert to facilitate S. typhimurium invasion of the host cell, SopB appears to have a far more important role in inducing an aggregation response in erythrophore cells than previously characterized in mammalian host cells. SopB is an inositol phosphatase that contributes to extensive actin remodeling in mammalian host cells by targeting host GEFs (guanine-nucleotide exchange factors) to activate RhoG GTPase (138, 133). Additionally, SopB is involved in sealing the host membrane in folding (139, 133). Figure 12 illustrates a hypothetical model as to how S. typhimurium might impact pigment organelle movement in erythrophore cells. Expression of hilD, in S. typhimurium, is activated during late log growth phase. Fully expressed hilD, in turn, activates expression of hilA. Expressed HilA activates expression of invF and prgHIJK, SPI-1 operons. Alternatively, hilD can directly activate expression of the invF and 79 prgHIJK operons. Expressed InvF turns on the expression of genes responsible for encoding the T3SS-1 effector proteins on SPI-1 or elsewhere. Activated prgHIJK operon expresses the proteins that assemble in to the T3SS-1 needle-like apparatus. Presumably a mutation in prgHIJK or hilD had a similar impact on erythrophore cell response because both classes of mutations led to the failure to produce a needle like apparatus that could deliver T3SS-1 effector proteins. Hypothetically, the T3SS-1 needle-like apparatus is used to deliver the T3SS-1 effector proteins into the erythrophore cells whereby one or several of the effector proteins directly impact pigment organelle movement. The mutation in hilD had a more notable impact on pigment organelle movement, suggesting that this function is crucial, presumably due to the genes regulated by HilD, and no other regulatory protein can compensate for HilD function in S. typhimurium. As illustrated in Figure 12, if the T3SS-1 needle-like apparatus has made contact with the erythrophore cell, then effector proteins, such as SipA, SopB, SopE2, and SptP might be injected into the erythrophore cell. If S. typhimurium effector proteins do gain access to the erythrophore cell then how might they induce pigment organelle movement? Although the results from this research effort did not suggest a direct role for SipA and SopE2, given their function in leucocytes, these two effector proteins may be involved in pigment organelle movement but other effector proteins may have similar function to compensate for loss of SipA or SopE2 function. Additionally, S. typhimurium sptP mutant exhibited an aggregation response in erythrophore cells with slightly higher magnitude than the wildtype S. typhimurium. In leukocytes, SptP is secreted during the early stage of pathogenesis after Salmonella enters the Salmonella containing vacuole 80 (SCV) and it reverses the activity of other effector proteins such as SopB, SopE, SopE2. However, there is no evidence of SCV formation inside the erythrophore cell and the secretion of SptP may require more time than the response that is observed in wildtype S. typhimurium. This finding suggests that the internalization of S. typhimurium is not required for inducing pigment organelle aggregation in erythrophore cells. However, results from this research effort suggest SopB has a role in triggering the movement of the pigment organelles. SopB function may be mimicking function of proteins that are involved in transporting pigment organelles along microtubules towards the perinuclear region in erythrophore cell. Alternatively, SopB may affect the activity of a protein, such as Rho G, that is involved in rearrangement of host cytoskeleton, resulting in pigment organelle movement in the erythrophore cell. Results from this research effort suggest that certain aspects of S. typhimurium’s pathogenic mechanism are involved in pigment organelle movement in a neuron-like pigment cell, in this case an erythropore cell of the chromatophore cell classification, isolated from the fish species, Betta splendens. 81 a. b. Figure 12. (a) A hypothetical model as to how S. typhimurium might enter an erythrophore cell and the ensuing collaborative work of effector proteins of T3SS-1 to induce pigment organelle movement. (b) Aggregated pigment organelles in the center of an erythrophore cell. 82 Future Directions For This Research Effort This study provides insight into how S. typhimurium induces pigment organelle aggregation in B. splendens erythrophore cells. Previous studies have shown that S. typhimurium requires a functional T3SS-1 needle-like apparatus for inducing an aggregation response in B. splendens erythrophore cells. This study demonstrated that effector protein, SopB, secreted by the T3SS-1 needle-like apparatus may also play a role in pigment organelle aggregation in erythrophore cells. In addition, a major regulator of SPI-1 expression, hilD, plays a crucial role in pigment organelle aggregation in erythrophore cells. However, many factors involved in inducing a response in erythrophore cells remain unclear. Further investigations of effector proteins such as SipC and SipD will increase understanding and potentially reveal their involvement in pigment aggregation of B. splendens erythrophore cells. Collectively, answering the why and how erythrophore cells respond to S. typhimurium will result in better understanding as to how to use this cell type as a biosensor for bacterial toxicity. 83 Chapter 6 Conclusion This study describes Betta splendens erythrophore cells response to Salmonella typhimurium, including an analysis of the bacterial mechanism(s) that may be involved in this response. The outcome to this research effort is to increase understanding of the biological basis of the erythrophore cell response to bacterial pathogens. Increased understanding will lead to better utility of erythrophore cells as biosensors for bacterial toxicity testing. Erythrophore cell-based biosensor is an emerging technology that has the potential to respond to biological and environmental stimulants in a physiological manner that can be measured and quantified. Cell based biosensors have the potential to overcome the limitation of other molecular and immunology based methods that are not function based. This study tested the hypothesis that a S. typhimurium mutant, ST10, which no longer induced a response in erythrophore cells, carried a mutation in either gene(s) coding for the process regulating expression of the prgHIJI operon or the gene(s) coding for the effector proteins that traveled through the PrgHIJK apparatus. Characterization of ST10 mutant revealed that the EZ-Tn5™ transposome had interrupted the hilD gene. Salmonella typhimurium mutant, ST10, containing an interrupted hilD gene was no longer able to induce a response of pigment organelle aggregation in erythrophore cells. The hilD wildtype gene, with partial Fur B box sequence, was cloned and the hilD mutant, ST10, was complemented with this construct to demonstrate that the mutation is 84 linked to the resulting biological outcome of a mutant hilD. The result showed that complemented ST10 strain induced an aggregation response in erythrophore cells similar to the response induced by the wildtype S. typhimurium strain. However, the erythrophore cell response induced by the complemented ST10 strain was delayed and pigment organelle movement was reduced in magnitude as compared to that observed with the wildtype S. typhimurium strain. The second hypothesis tested in this study was that the effector proteins of T3SS are the components of S. typhimurium’s invading mechanism directly involved in inducing pigment organelles to undergo an aggregative response in erythrophore cells. To test this hypothesis, the response of erythrophore cells to S. typhimurium strains containing targeted, well characterized mutations in genes coding for T3SS effector proteins SipA, SopB, SopE2 and SptP were analyzed. Mutations in either the sipA, sopE2 or sptP genes resulted in S. tyhpimurium mutants with a phenotype similar to the wildtype S. typhimurium strain: all induced pigment organelle aggregation in erythrophore cells. This resulted suggested that the SipA, SopE2 and SptP effector proteins are not directly involved in the erythrophore response to S. typhimurium. In contrast, S. typhimurium sopB and sipA/sopB mutants induced a response in erythrophore cells that was different in magnitude and kinetics to that observed for the wildtype S. typhimurium. Both mutants caused some aggregation (after 55 minutes of exposure) in erythrophore cells; however, the magnitude of the response was lower than that of observed by S. typhimurium wildtype. 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Journal of Molecular Biology 357: 373-86. 109 Appendix 110 Biographical Information Mohammad Farhad was born on October 10, 1987 in Kabul, Afghanistan to Haji Gul Mohammad and Bibi Habiba. He was raised, until the age of six, in the middle of civil war between the different Mujahideen groups following the withdrawal of the Soviet army in 1989 from Afghanistan. The situation in Kabul worsened and his father’s life was in risk because he was a Colonel in the Afghan National Army. His family migrated to Quetta, Pakistan in 1995. His family suffered from extreme poverty in lawless regions of Quetta. His father and older brother insisted on educating Farhad and his younger siblings. He finished middle school, attended an English Language Center and worked in a local pharmacy in Pakistan. He speaks five languages: Pashto (native language), Dari, Farsi, Urdu and English. After the U.S. Army invaded Afghanistan, his family returned to Kandahar, Afghanistan in 2002. At the age of sixteen he was appointed as an instructor of computer software and hardware in a newly established Computer Institute for one year. While still attending High School, he worked for two years as an interpreter and translator for the U.S. Army in Afghanistan to minimize the misunderstanding between Afghanis and U.S Army. He graduated from Zahir Shahi High School in Kandahar in 2005. With the help of his friend, Mike Manaton, he came to the United States in 2006 in pursuit of his higher education. In June of 2008, he graduated from Portland Community College with an Associate of Science degree with highest academic honors. He was awarded the PCC Foundation Scholarship and the Dan and Kathy Moriarty scholarship for his academic 111 excellence. He received the first ever International Student Key Note Speaker Award. He was also a member of Phi Theta Kappa Honor Society. In 2008, he transferred to Oregon State University to pursue a Bachelor of Science degree in Biology with a pre-medicine option. He was awarded an International Cultural Service Program (ICSP) scholarship for educating people on the situation in Afghanistan. He joined the Honors College at Oregon State University. As part of his Honors College requirements he had to conduct research, write a thesis and defend it. He conducted his research in Dr. Janine Trempy’s laboratory in the Department of Microbiology as an undergraduate lab research assistant. He investigated diarrheal disease in rural villages on the outskirt of Kabul. He completed his research and defended his undergraduate thesis, titled: “Presence of Diarrhea and its Intensity due to Human Behaviors in Deh Sabz, Kabul, Afghanistan.” He was awarded two scholarships from the College of Science at Oregon State University: 1) Doc Gilfillan Scholarship and 2) Science Scholar Scholarship. Mohammad Farhad graduated in 2010 from Oregon State University with a Bachelors of Science degree in Biology with Honors. His compelling life story, as well as his successes at Oregon State University, was one of four student stories selected by Oregon State University’s President Ray to share at graduation commencement. In 2010, he was accepted into the Graduate Program in the Department of Microbiology at Oregon State University and awarded a Graduate Research Assistantship in Dr. Trempy’s laboratory to pursue his Masters of Science degree in Microbiology. In addition to his research, he also served as a teaching assistant for the Department of 112 Microbiology’s lab courses. He defended his master’s thesis, “The Role of Salmonella typhimurium Type Three Secretion System (T3SS) and Effector Proteins in Erythrophore Cell Response”, on May 21st 2013, and graduated from OSU on Jun 15th 2013. Mohammad Farhad was accepted into the Ph.D. Graduate Program in Molecular and Cellular Biosciences at Oregon Health and Science University in Portland, OR. He will begin his graduate studies for a Ph.D., September 2013. Manuscripts in Preparation 1. Dierksen, K.P., Roach, H.B., Hutchison, J.R., Dukovcic, S., Farhad, M., Garcia, R., and Trempy, J.E. 2013. Biosensors employing chromatophore cells: a comparative analysis of chromatophore cell types in the detection of food associated bacterial pathogens. Manuscript in prep. 2. Dukovcic, S., Farhad, M., Dierksen, K.P., Hutchison, J.R., and Trempy, J. E. 2013. The role of prgHIJI and hilD in the chromatophore cell response to Salmonella typhimurium. Manuscript in prep. 3. Farhad, M., Dierksen, K.P., and Trempy, J.E. 2013. Salmonella typhimurium effector proteins and their role in pigment organelle movement in chromatophore cells. Manuscript in prep.