RESEARCH LETTER A new antibacterial and antioxidant S07-2 compound produced by Bacillus subtilis B38 Olfa Tabbene1, Ines Karkouch1, Salem Elkahoui1, Pascal Cosette2, Maria-Luisa Mangoni3, Thierry Jouenne2 & Ferid Limam1 1 Laboratoire des Substances Bioactives, Centre de Biotechnologie de Borj-Cedria, Tunis, Tunisia; 2UMR 6522 CNRS, Faculté des Sciences, Université de Rouen, Rouen, France; and 3Dipartimento di Scienze Biochimiche, Università La Sapienza, Rome, Italy Received 25 October 2009; revised 26 November 2009; accepted 27 November 2009. Final version published online January 2010. DOI:10.1111/j.1574-6968.2009.01875.x Editor: Wolfgang Schumann MICROBIOLOGY LETTERS Keywords antibacterial; antioxidant; Bacillus subtilis ; cyclic peptide. Abstract An antibacterial compound, S07-2, was purified to homogeneity by hydrophobic interaction, anion exchange, C18 reverse-phase and HS PEG HPLC. The molecular mass of S07-2 was 905.6 Da as determined by MS. The S07-2 compound was resistant to high temperatures (up to 100 1C) and could withstand a wide range of pH from 3 to 10. In addition, its antibacterial activity was preserved after treatment with proteases. Biochemical characterization revealed its cyclic peptide structure. This compound showed a bactericidal effect against important foodspoilage bacteria and food-borne pathogens including Listeria monocytogenes and Enterococcus faecalis with lethal concentration values of 62.5 mg mL1 and against Salmonella enteritidis at a concentration of 31.25 mg mL1. However, no cytotoxic effect against human erythrocytes was recorded. Furthermore, the S07-2 compound displayed a remarkable Fe21-chelating activity (EC50 = 9.76 mg mL1) and 1-diphenyl-2-picrylhydrazyl-scavenging capacity (IC50 = 65 mg mL1). All these chemical and biological features make S07-2 a useful compound in the food industry as a natural preservative. Introduction The Gram-positive bacterium Bacillus subtilis produces a large number of bioactive peptides classified as ribosomal or nonribosomal peptides according to their biosynthesis pathway (Tamehiro et al., 2002). Nonribosomal bioactive peptides exhibit antimicrobial properties and play crucial roles in suppressing microbial competitors. Peptide antibiotics represent the predominant class of antimicrobial molecules produced by B. subtilis species (Hagelin et al., 2004; Stein, 2005). Moreover, these species produce other bioactive molecules such as siderophores with iron-chelating properties. The catecholic siderophore bacillibactin is produced under iron-limited growth conditions (May et al., 2001). Sequestration of mobile iron plays a crucial role in reducing the occurrence of free radicals (Lin et al., 2006; Moktan et al., 2008). Free radicals or reactive oxygen species are known to cause oxidative damage to biological macromolecules, leading to a number of disorders including cancer, atherosclerosis, cardiovascular diseases, aging and inflammatory diseases (Chew et al., 2008). Synthetic antioxidants that have been extensively used in industrial processing are 2010 Federation of European Microbiological Societies Published by Blackwell Publishing Ltd. All rights reserved c being investigated for their toxic and carcinogenic effects (Moktan et al., 2008; Thitilertdecha et al., 2008). Recently, the interest in finding natural antioxidant agents with low cytotoxicity has increased significantly (Thitilertdecha et al., 2008). Several studies have focused on plant compounds (Teow et al., 2007; Erkan et al., 2008). However, only a few reports have been conducted on the antioxidant power of microbial extracts (Moktan et al., 2008). In previous studies, we described the production of several antimicrobial compounds by a newly identified B. subtilis B38 strain (Tabbene et al., 2009a) as well as their optimization (Tabbene et al., 2009b). The present paper addresses the purification and partial characterization of the S07-2 compound along with an evaluation of its antibacterial and antioxidant activities. Materials and methods Bacterial strains and culture conditions The bacterial indicator strains used in this study are listed in Table 1. Bacterial growth was performed in Luria–Bertani FEMS Microbiol Lett 303 (2010) 176–182 Downloaded from http://femsle.oxfordjournals.org/ by guest on March 6, 2016 Correspondence: Ferid Limam, Laboratoire des Substances Bioactives, Centre de Biotechnologie de Borj-Cedria, BP-901, 2050 Hammam-lif cedex, Tunis, Tunisia. Tel./fax: 1216 79 325 728; e-mail: ferid.limam@cbbc.rnrt.tn 177 S07-2 compound from B. subtilis sp. B38 Thin-layer chromatography (TLC) analysis of the purified antibacterial agent MIC (mg mL1) MBC (mg mL1) 62.5 62.5 31.25 15.62 62.5 62.5 31.25 15.62 62.5 62.5 4 250 4 250 62.5 62.5 4 250 4 250 The HPLC-purified fraction was subjected to TLC using n-butanol–methanol–water (39 : 10 : 20, v/v/v) as the mobile phase. The bioassay was performed as described previously (Tabbene et al., 2009a) using P. aeruginosa as the indicator strain. S07-2 compound was detected by UV light at 254 nm or by exposure to iodine and subjected to ninhydrin and 4,4’-bis(dimethylamino)diphenylmethane (TDM) staining methods according to Yu et al., 2002. The iron-binding capacity of the S07-2 compound was determined using chrome azurol sulfonate (CAS) agar blue solution according to Schwyn & Neilands (1987). The CAS agar solution was poured onto the developed TLC plate. A positive reaction was revealed by a change in the color of the CAS–iron complex from blue to orange. A preliminary detection of the radical-scavenging activity was conducted as described previously (Sreenivasan et al., 2007). The developed TLC plate was sprayed with 0.1% w/v 1-diphenyl-2-picrylhydrazyl (DPPH) methanolic solution. The compound with antiradical activity appeared as a yellow spot against the purple–blue background. Bacterial strains Gram-negative bacteria Pseudomonas aeruginosa ATCC 27853 Klebsiella pneumonia CIP 105705 Salmonella enteritidis ATCC 13076 Escherichia coli ATCC 35214 Gram-positive bacteria Enterococcus feacalis ATCC 29219 Listeria monocytogenes CIP 82110T Staphylococcus aureus ATCC 29213 Bacillus thuringiensis sp. 15 LILM (LB) broth at 37 1C. The producer strain B. subtilis B38 was grown in tryptic soy broth (TSB) at 30 1C. Determination of antibacterial activity The antibacterial activity was assayed using the agar disk diffusion method as described previously (Tabbene et al., 2009a). The titer of antibacterial activity was expressed as activity units (AU) mL1 and corresponded to the reciprocal of the highest dilution showing growth inhibition of the Pseudomonas aeruginosa ATCC 27853 indicator strain. Purification of the antibacterial compound produced by B. subtilis B38 To purify the S07-2 compound, B. subtilis B38 was cultured in 1 L TSB as described previously (Tabbene et al., 2009a). The cell-free supernatant was subjected to methanol extraction. After centrifugation, the supernatant was evaporated and the resulting precipitate was dissolved in MilliQ water and fractionated onto a Sep-Pak plus C18 cartridge (Waters, Division of Millipore Corp., Bedford, MA) using a discontinuous gradient of acetonitrile (0%, 20%, 40%, 60%, 80% and 100%). The active fraction was applied onto a DEAESepharose column (Amersham Pharmacia Biotech). Elution was performed using 10 mM ammonium acetate buffers at different pH (7.5, 6, 5, 4 and 3). The active fraction was applied onto a C18 RP-HPLC column (250 4.6 mm). Elution was performed using a linear gradient of acetonitrile from 0% to 100% at a flow rate of 1 mL min1 for 70 min. All collected fractions were dried under vacuum, dissolved in methanol and tested for their antibacterial activity against P. aeruginosa. The active fraction was chromatographed once more, onto an HS PEG HPLC column (250 4.6 mm). Elution was performed using a linear gradient of acetonitrile from 0% to 100% in 10 mM ammonium acetate buffer, pH 6.8, at a flow rate of 0.8 mL min1 for 40 min. FEMS Microbiol Lett 303 (2010) 176–182 Physicochemical properties of the S07-2 compound Temperature stability was evaluated by incubating S07-2 compound at various temperatures from 30 to 100 1C for 30 min or at 121 1C for 20 min. Residual antibacterial activity was determined by a disk diffusion assay against P. aeruginosa. The effect of pH was determined using a pH range from 2 to 10 with diluted HCl or NaOH. After incubation for 2 h at 25 1C and neutralization to pH 7, the residual activity was tested. Resistance to proteases was tested by incubating S07-2 compound with proteinase K, trypsin or a-chemotrypsin at ratios of 1 : 10 and 1 : 5 (w/w) as described previously (Tabbene et al., 2009a). MS analysis MS experiments were carried out using a prOTOFTM instrument (Perkin-Elmer) operating in the reflectron mode and with an accelerating voltage of 16 kV. The matrix used was a-cyano-4-hydroxycinnamic acid. The instrument was calibrated with peptides of known molecular mass in the 1000–2500-Da range (PepMix1, LaserBiolabs, France). In typical measurements, the mass accuracy was 5 p.p.m. Determination of minimal inhibitory concentration (MIC) and minimal bactericidal concentration (MBC) values The MIC of the S07-2 compound on different bacterial strains was determined by microbroth dilution assay. 2010 Federation of European Microbiological Societies Published by Blackwell Publishing Ltd. All rights reserved c Downloaded from http://femsle.oxfordjournals.org/ by guest on March 6, 2016 Table 1. Antibacterial activity spectrum of S07-2 compound produced by Bacillus subtilis B38 178 O. Tabbene et al. Twofold increasing concentrations of the sample (from 3.9 to 1000 mg mL1) were tested on cell suspensions (106 CFU mL1) in LB medium. Control wells with 20% methanol were included. Plates were incubated at 37 1C for 24 h. Bacterial growth was determined by measuring the OD600 nm using a microplate reader (Bioteck, ELx 800). MIC was defined as the lowest concentration inhibiting bacterial growth. MBC was determined from the same experiments by removing 10 mL from wells without growth after 48 h of incubation. These aliquots were then spread onto LB agar plates for counting. MBC was defined as the lowest concentration causing 95% killing of the microbial population. DPPH radical-scavenging activity Free DPPH radical-scavenging activity was measured by the method of Erkan et al. (2008). Briefly, 0.2 mM of DPPH in methanol was mixed with 100 mL of twofold increasing concentrations of sample (1.95–250 mg mL1) and 50 mM Tris-HCl buffer, pH 7.4. The mixture was shaken vigorously and left at room temperature for 30 min in the dark. The A517 nm was then measured. L-Ascorbic acid was used as a positive control. The free-radical-scavenging activity was then calculated as the percentage of inhibition according to the following equation: % Inhibition ¼ ½ðAblank Asample Þ=Ablank 100; Hemolytic assay Determination of siderophore chemical nature The S07-2 compound was subjected to chemical assays, to investigate its siderophore nature. Catecholate-, hydroxamate- and carboxylate-type siderophores were measured according to Arnow (1937), Neilands (1981) and Shenker et al. (1992), respectively. Ferrous ion-chelating activity Fe21-chelating activity was evaluated according to Moktan et al. (2008). Twofold increasing concentrations of the S07-2 compound (0.24–125 mg mL1) were added to 0.5 mM ferrous chloride tetrahydrate solution. After a 5-min incubation at room temperature, 1.25 mM ferrozine was added. The mixture was incubated for 10 min at room temperature and the A562 nm was measured. EDTA was used as a positive control. The percentage of inhibition of ferrozine–Fe21 complex formation was given by the following equation: Ferrous iron-chelating activityð%Þ ¼ ½ðAblank Asample Þ=Ablank 100; where Ablank is the absorbance of the negative control and Asample the absorbance of the sample or EDTA. Chelating activity was expressed by the EC50, the effective concentration of the material causing a 50% chelating effect. 2010 Federation of European Microbiological Societies Published by Blackwell Publishing Ltd. All rights reserved c Results and discussion Purification of the antibacterial compound produced by B. subtilis B38 The S07-2 compound was purified to homogeneity and its activity was tested against P. aeruginosa. Data of the purification steps are summarized in Table 2. Extraction with methanol increased the specific activity to 400 AU mL1 and led to 100% recovery. The active compound was eluted from a SepPak C18 cartridge at 40% acetonitrile (F40) with a specific activity of 3200 AU mL1 and a 64% recovery. F40 was further loaded onto a DEAE-Sepharose column. The S07-2 compound eluted with 10 mM ammonium acetate, pH 3, showed a specific activity of 4000 AU mL1 and a 40% recovery. To achieve purification, the active fraction was further loaded onto a C18 RP-HPLC column. One major peak was separated from contaminants and subjected to a second HPLC run on a discovery HS PEG column. A single peak was purified to homogeneity (Fig. 1). Its specific activity was increased 3500 times, reaching a value of 7000 AU mL1. The purity of the S07-2 compound was controlled by TLC as reported in Fig. 1 Table 2. Activity recoveries of S07-2 compound at different purification stages Purification steps Growth medium Methanol extract Sep-Pak C18 cartridge DEAE-Sepharose C18 RP HPLC HS PEG HPLC Specific activity Total activity Purification Recovery (AU) fold (%) (AU mL1) 20 400 3200 20 000 20 000 12 800 1 20 160 100 100 64 4000 6000 7000 8000 6000 5600 200 300 350 40 30 28 FEMS Microbiol Lett 303 (2010) 176–182 Downloaded from http://femsle.oxfordjournals.org/ by guest on March 6, 2016 The hemolytic activity of the S07-2 compound on human erythrocytes was also determined (Mangoni et al., 2000). Briefly, blood was centrifuged and erythrocytes were washed three times with 0.9% NaCl. Increasing concentrations of the sample, ranging from 3.9 to 1000 mg mL1, were incubated with the erythrocyte suspension (1 107 cells mL1 in 0.9% NaCl) at 37 1C for 30 min. The extent of hemolysis was measured at 415 nm. Hypotonically lysed erythrocytes were used as a standard for 100% hemolysis. where Ablank is the absorbance of the blank and Asample the absorbance of the extract or L-ascorbic acid. Antioxidant activity was expressed as inhibitory concentration 50% (IC50), defined as the concentration of the material required to cause a 50% decrease of the initial DPPH concentration. 179 S07-2 compound from B. subtilis sp. B38 (see inset). A single spot with Rf 0.7 exhibiting antibacterial activity against P. aeruginosa (Fig. 1, inset a) was detected by both UV light at 254 nm and exposure to iodine reagent (Fig. 1, insets b and c, respectively). Physicochemical properties of the S07-2 compound a b c d 100 1 50 %B A (215 nm) 1.5 0.5 0 0 0 5 10 15 20 25 Retention time (min) 30 MS analysis The molecular mass of the S07-2 compound was determined by matrix-assisted laser desorption/ionization-time-offlight MS (Fig. 2). The mass spectrum confirmed the purity of the sample and showed one major peak at m/z 905.6. Expansion of the chromatogram also showed minor species at m/z 927.6 and m/z 943.6, the sodium and potassium adducts, respectively. Cyclic peptide antibiotics produced by B. subtilis species generally exhibit molecular masses 4 1000 Da, ranging from 1447.7 to 1519.8 Da in the case of the maltacine complex (Hagelin et al., 2004), from 800 to 1500 Da in the case of lipopeptides (Price et al., 2007) and equal to 3401.2 0.5 Da for the lantibiotic subtilosin A (Kawulka et al., 2004). Furthermore, some peptide antibiotics with lower molecular masses were identified in a B. subtilis strain and were estimated to be in the range 960–983 Da (Teo & Tan, 2005). 35 Fig. 1. HPLC profile of the S07-2 compound after HS PEG HPLC. Inset: TLCbioautography analysis of the purified S07-2 compound using Pseudomonas aeruginosa as an indicator strain (a). Detection of the S07-2 compound under UV light at 254 nm (b), after exposure to iodine (c) or staining with TDM (d). S07-2 compound (20 mg) was applied onto a TLC plate. Antibacterial spectrum of the S07-2 compound The antibacterial activity of the S07-2 compound was determined against eight strains of Gram-positive and Gram-negative bacteria as shown in Table 1. The S07-2 compound exhibited a potent antibacterial activity against Fig. 2. Mass spectrum profile of the S07-2 compound. FEMS Microbiol Lett 303 (2010) 176–182 2010 Federation of European Microbiological Societies Published by Blackwell Publishing Ltd. All rights reserved c Downloaded from http://femsle.oxfordjournals.org/ by guest on March 6, 2016 The optimal temperature and pH values of the S07-2 compound were also investigated. The compound conserved its antibacterial activity until 90 1C and lost 50% of its initial activity after autoclaving at 121 1C for 20 min. It was stable in the pH range from 3 to 10 and was resistant to proteases. The S07-2 compound showed a positive reaction with TDM reagent (Fig. 1, inset d), but was negative to ninhydrin. Data indicate the absence of free N-terminal amino group and the presence of peptide bonds. Therefore, the antibacterial compound could be a cyclic peptide antibiotic. A cyclic structure should increase the rigidity of the peptide, reducing its proteolytic degradation by hampering enzyme access to the cleavage sites. Various cyclic peptides containing N- and/or C-terminal blocked residues as well as unusual amino acids have already been described, such as maltacine complex (Hagelin, 2005), subtilosin A lantibiotic (Kawulka et al., 2004), and surfactin, iturin and fengycin lipopeptides (Tamehiro et al., 2002). 180 Hemolytic activity The S07-2 compound did not exhibit any hemolytic activity even at a high concentration (1000 mg mL1). Consequently, this compound would not appear to be a lipopeptide antibiotic that generally causes hemolysis (Volpon et al., 1999; Leclère et al., 2005). This was also supported by the inability of the S07-2 compound to exhibit antifungal activity (Tabbene et al., 2009a), the main feature of lipopeptide antibiotics (Leclère et al., 2005; Ramarathnam et al., 2007). The lack of hemolytic activity suggests that the S07-2 compound is devoid of cytotoxic effect. Cyclic peptide antibiotics produced by Bacillus species showed variable hemolytic activities. Indeed, subtilosin A was not hemolytic, whereas gramicidin S produced by Bacillus brevis possessed quite a high hemolytic capacity (Kondejewski et al., 1996; Huang et al., 2009). Ferrous-chelating activity The Fe21-chelating ability of S07-2 was preliminarily detected on a TLC plate. A positive reaction was recorded by the color change of the CAS reagent from blue to orange (Fig. 3 inset). The chemical nature of the siderophore was 2010 Federation of European Microbiological Societies Published by Blackwell Publishing Ltd. All rights reserved c Fe2+-chelating activity (%) 100 50 0 0 20 40 60 80 100 120 140 Concentration (µg mL–1) Fig. 3. Chelating activity of the S07-2 compound. Purified S07-2 compound () and EDTA (), used as positive control for chelating iron ions. Data are expressed as means SE and assays were performed in triplicate. Inset: iron-chelating capacity as revealed by CAS agar on a TLC plate. S07-2 compound (5 mg) was deposited on a TLC plate. also investigated. The S07-2 compound was negative to hydroxamate, catecholate and carboxylate chemical tests, suggesting that this compound does not correspond to any of these types of siderophores. In a quantitative assay, the chelating activity of the S07-2 compound was tested against Fe21 ions as reported in Fig. 3. The S07-2 compound exhibited a strong iron-chelating effect (EC50 = 9.76 mg mL1), which represents 62.5% of that corresponding to EDTA-positive control (EC50 = 6.1 mg mL1). Previous studies on purified peptide from fermented mussel showed similar chelating ability (Rajapakse et al., 2005). Other protein hydrolysates from leaf and wheat germ (WGPH) were found to exhibit a moderate iron-chelating ability (65.15% at 0.5 mg mL1 and 89% at 1 mg mL1, respectively) compared with EDTA (Zhu et al., 2006; Xie et al., 2008). Several studies have shown that iron is a key active species responsible for oxidant formation in cells, generating hydroxyl radicals, which in turn are responsible for cell damage, causing neurodegenerative disorders such as Parkinson’s and Alzheimer’s diseases (Kaur et al., 2003; Xie et al., 2008). Therefore, the iron-chelating compound produced by B. subtilis B38 might be a useful agent in the treatment of neurodegenerative diseases or other iron-induced disorders. DPPH scavenging activity DPPH radicals were widely used to investigate the scavenging ability of natural compounds (Zhu et al., 2006; Chen et al., 2008; Xie et al., 2008). A positive reaction was detected on TLC plate around S07-2 compound after spraying with DPPH solution (Fig. 4 inset). The antiradical activity was quantitatively assayed and compared with that of ascorbic acid (Fig. 4). The 50% DPPH scavenging activity of S07-2 compound (IC50 = 65 mg mL1) was four times lower than that of ascorbic acid (IC50 = 15 mg mL1). Similar data have been reported for purified peptides from fermented mussel (72% radical FEMS Microbiol Lett 303 (2010) 176–182 Downloaded from http://femsle.oxfordjournals.org/ by guest on March 6, 2016 the tested bacteria, except the methicillin-resistant Staphylococcus aureus and Bacillus thuringiensis B15 strains. Escherichia coli and Salmonella enteritidis were the most sensitive bacteria with MIC values of 15.62 and 31.25 mg mL1, respectively. It was also active against P. aeruginosa, Klebsiella pneumoniae and against the food-borne pathogens Listeria monocytogenes and Enterococcus faecalis strains with MIC values of 62.5 mg mL1. Furthermore, the S07-2 compound showed similar MIC and MBC values, which led to the conclusion that this antibacterial compound exerted a bactericidal effect on the bacterial strains used. These features make the S07-2 compound a good candidate in biotechnological applications for biocontrol of pathogenic and food-spoilage microorganisms. Many studies have underlined the importance of bacteriocins in the food industry. Indeed, both nisin and pediocin PA-1 produced by lactic acid bacteria have been approved as food additives in many countries (Cotter et al., 2005). These bacteriocins are generally active against Gram-positive bacteria, but not against Gram-negative bacteria (Castellano et al., 2001). Subtilosin A produced by B. subtilis was also considered as a good candidate in food preservation, as it showed a strong antimicrobial activity against food-borne pathogens, for example E. faecalis (MIC = 3.125 mg mL1) and L. monocytogenes (MIC = 12.5 mg mL1) (Shelburne et al., 2007). However, this bacteriocin showed a moderate activity against Gram-negative bacteria such as P. aeruginosa (MIC = 50 mg mL1) and E. coli (MIC = 100 mg mL1) and no activity against S. enteritidis and K. pneumoniae (Shelburne et al., 2007). O. Tabbene et al. 181 DPPH–scavenging effect (%) S07-2 compound from B. subtilis sp. B38 100 50 0 0 50 100 150 200 250 Concentration (µg mL–1) 300 350 scavenging activity at 200 mg mL1) (Rajapakse et al., 2005). However, a moderate DPPH radical-scavenging activity was observed for WGPH (IC50 = 0.8 mg mL1) and alfalfa leaf (IC50 = 1.3 mg mL1) when compared with that of the S07-2 compound (Zhu et al., 2006; Xie et al., 2008). Microorganisms are also potential sources of natural antioxidants, including various fermented products from Aspergillus (Wang et al., 2007), Rhizopus (Sheih et al., 2000) and B. subtilis (Moktan et al., 2008) species. Antioxidant activity was also correlated with the polyphenol content of the fermented products. In conclusion, we have isolated an S07-2 compound from B. subtilis B38 with a molecular mass of 905.6 Da. This compound displayed antibacterial activity against food-spoilage microorganisms, DPPH radical-scavenging activity and an iron-chelating capacity. Consequently, the S07-2 compound could serve as a food preservative and might be a good alternative to synthetic antioxidant compounds already used in medicine. To our knowledge, no bioactive peptides with the same characteristics as the peptide described in the present study have been reported previously from B. subtilis strains. Further investigations are in progress to determine its chemical structure as well as its mode of action. Acknowledgements This work was supported by grants from the Ministère de l’Enseignement Supérieur, de la Recherche Scientifique et de la Technologie of Tunisia. We thank Prof. E. Aouani for valuable discussion and critical reading of the manuscript. 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