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AR226-3101 ^3 - GWWJ Huntingdon CONFIDENTIAL DPT434/984093 BACTERIAL MUTATION ASSAY DuPont Specialty Chemicals, Jackson Laboratory, Chambers Works, Deepwater, NJ 08023, USA Research Laboratory Huntingdon Life Sciences Ltd., Eye, Suffolk, IP237PX, ENGLAND Final report issued 1 October 1998 / Company Sanitized. Does not contain TSCA CBI CONTENTS Page COMPLIANCE WITH GOOD LABORATORY PRACTICE STANDARDS ............................ 3 QUALITY ASSURANCE STATEMENT .................................................................................. 4 SUMMARY ......................;......................;................................................................................ 5 INTRODUCTION .................................................................................................................... 6 TEST SUBSTANCE ................................................................................................................. 8 EXPERIMENTAL PROCEDURE............................................................................................. 9 ASSESSMENT OF RESULTS .................................................................................................. 13 MAINTENANCE OF RECORDS ............................................................................................. 13 RESULTS ................................................................................................................................. 14 CONCLUSION......................................................................................................................... 14 REFERENCES ......................................................................................................................... 15 TABLES 1. Results obtained with S. typhimurium TAPS following exposure tc^HI^HH^............ 16 2. Results obtained with X %?fo"wyr/uwTA 100 following exposure t^^^^^^^^l........... 18 3. Results obtained with S. typhimurium TA1535 following exposure to^HfHHB-......... 20 4. Results obtained with S. typhimurium TA1537 following exposure tcf----------B.......... 22 5. Results obtained with E. coli CM89I following exposure t(xB----^^^l^^^^_.......... 24 APPENDIX ; .< 1. Historical control data......................................................................................................... 26 Company Sanitized. Does not contain TSCA CBE COMPLIANCE WITH GOOD LABORATORY PRACTICE STANDARDS The study described in this report was conducted in compliance with the following Good Laboratory Practice standards, with the exception stated below, and I consider the data generated to be valid. The United Kingdom Good Laboratory Practice Regulations 1997 (Statutory Instrument No .654). EC Council Directive 87/18/EEC of 18 December 1986 (Official Journal No L 15/29). OECD Principles of Good Laboratory Practice (as revised in 1997), ENV/MC/CHEM(98)17. In line with normal practice in this type of short-term study, the protocol did not require analysis of the dose form. Study Director, Huntingdon Life Sciences Ltd. Date Company Sanltaed. Doss not contain TSCA CBI QUALITY ASSURANCE STATEMENT The following have been inspected or audited in relation to this study: Study Phases Inspected Protocol Process Based Inspections Audit Plate Scoring Treatment Formulation Report Date of Inspection 3 August 1998 8 January 1998 6 April 1998 15 April 1998 14 July 1998 2 September 1998 Date of Reporting 3 August 1998 8 January 1998 6 April 1998 15 April 1998 14 July 1998 2 September 1998 Protocol: An audit of the-protocol for this study was conducted and reported to the Study Director and Company Management as indicated above. Process based inspections: At or about the time this study was in progress inspections and audits of routine and repetitive procedures employed on this type of study were carried out. These were conducted and reported to appropriate Company Management as indicated above. Report Audit: This report has been audited by the Quality Assurance Department. This audit was conducted and reported to the Study Director and Company Management as indicated above. The methods, procedures and observations were found to be accurately described and the reported results to reflect the raw data. G Goddard Auditor, Department of Quality Assurance, Huntingdon Life Sciences Ltd. ...2&.'?.....5fep^^.Be&..B.^ Date Company Sanitized. Does not contain TSCA CBt SUMMARY In this in vitro assessment of the mutagenic potential ofZonyl FS-62, histidine dependent auxotrophic mutants of Salmonella typhimurium, strains TA1535, TA1537, TA98 and TA100, and a tiyptophan dependent mutant of Escherichia coli, strain CM891 (WPluvrA/pKMIOl), were exposed to the test substance diluted in purified water, which was also used as a negative control. Two independent mutation tests were performed in the presence and absence of liver preparations from Aroclor 1254-iBduced-rats (S9 mix). The first was a standard plate incorporation assay, the second involved a pre-incubation stage. - ;. -i :..- .-.'. Concentrations of up to 5000 pg/plate were tested in the mutation tests. This is die standard limit concentration recommended in the regulatory guidelines this assay follows. Other concentrations used werei.a-series of GO half-Iogio dilutions of the highest concentration. No signs oftoxicity were observed towards the tester strains in either mutation test. No evidence of mutagenic activity was seen at any concentration oi^^^^UJ^Hin either mutation test. The concurrent positive controls demonstrated the sensitivity of the assay and the metabolising activity ofthe liver-preparations. It is concluded that, when tested in purified water,|l^|BB|^hows no evidence of mutagenic activity in this bacterial system. Company Sanitwsd. Does not contain TSCA CW INTRODUCTION f^lHUlBo This report describes a'study designed to assess the mutagenic potential system. The study was conducted in compliance with the following guidelines: a bacterial <w OECD Guidelines for Testing of Chemicals. (1997) No. 471: Genetic Toxicology: Bacterial Reverse Mutation T^est. .. EEC Annex to Directive 92/69/EEC. (1992) Part B : Methods for Determination of Toxicity, B. 13. Other effects - Mutagenicity: Escherichiaeoli - Reverse Mutation Assay. O.J. No. L 383 A, 157. EEC Annex to Directive 92/69/EEC. (1992) Part B : Methods for Determination of Toxicity, B. 14. Other effects - Mutagenicity: Salmonella typhimurium - Reverse Mutation Assay. O.J. No. L 383 A, 160. US EPA 40 CFR Part 799 (1997) -Toxic Substances Control Act Test Guidelines - Sub-section 799.9510, TSCA bacterial reverse mutation test. Federal Register, Vol. 62, No. 158. ; .. , The method described was also designed to comply with ICH (1996 & 1997), and followed the recommendations of the United Kingdom Environmental Mutagen Society (Gatehouse^ al 1990). The in vitro technique described by Ames and his co-workers, (Ames, McCann and Yamasaki 1975, Maron and Ames 1983) enables the mutagenic effect of a test substance to be determined by exposing specially selected strains of Salmonella typhimurium to the test substance. Normally S. typhimurium is capable of synthesising the essential amino acid, histidine, but the mutant strains used in this test are incapable of this function. When these strains are exposed'to a mutagen, reverse mutation to the original histidine independent form takes place in a proportion of the population. These are referred to as revertants, and are readily detected by their ability to grow and form colonies on a histidine deficient medium (supplemented with biotin, since these strains are also incapable ofbiotin synthesis). A technique based on similar principles has also been described by Green (1984). This system employs mutant strains of Escherichia coli which are incapable of synthesising the amino acid tryptophan required for growth. The strains used carry additional mutations which render them more sensitive to mutagens. The S. typhimurium strains have a defective cell coat which allows greater permeability of test substances into the cell. All the strains are deficient in normal DNA repair processes. In addition three of them possess a plasmid (pKMIOl) which introduces an error-prone repair process, resulting in increased sensitivity to some mutagens. Company Sanitized. Doss not contain TSCA CBE Many substances do not exert a mutagenic effect until they have been metabolised by enzyme systems not available in the bacterial cell. Therefore the bacteria and test substance are incubated in both the absence and presence of a supplemented liver fraction (S9 mix) prepared from rats previously treated wnh a substance (Aroclor 1254) known to induce a high level of enzymic activity. The protocol was approved by Huntingdon Life Sciences Management on 7 July 1998, (he Sponsor on 17 July 1998 and by the Study Director on 31 July 1998. The experimental phase of the studywas conducted between 3 and 17 August 1998. Company Sanitized. Does not contain TSCA CB8 Identity: Chemical name: . A r.. Appearance: Storage conditions: Lot number: Expiry date: Purity: Date received: TEST SUBSTANCE Room temperature 2 Years from date of receipt 23 June 1998 Company Sas^tjzsd. Does not contain TSCA CBE w EXPERIMENTAL PROCEDURE BACTERIAL STRAINS The following strains were used:- : ~S, typhimurium TA1535: contains a histidine missense mutation (hisG46) but is also deficient in a DNA repair system (uvrB) and has a defective lipopolysaccharide coat on ....,..-, , the cell wall (rfa mutation). It is reverted by many agents causing base- pair substitutions, but is not sensitive to frameshift mutagens. S. typhinwrium TA100: ..is the same as TA1535 but contains a resistance transfer factor conferring ampicillin resistance and increasing sensitivity to some mutagens (plasmid pKMIOl). In addition to base-pair substitutions, it is also able to detect certain frameshift mutagens. S. typhimurium TA1537: bears a histidine frameshift mutation (hisC3076). Like TA1535, it is defective in a DNA repair system and lipopolysaccharide coat. It is sensitive to agents causing frameshift mutations involving insertion or deletion of a single base-pair. 5'. typhimurium TA98: contains another histidine frameshift mutation (hisD3052). Again it has a defective DNA repair system and lipopolysaccharide coat but also contains the pKMIOl plasmid. It is reverted by agents causing deletion of two adjacent base-pairs (double frameshift mutations), but not by simple alkylating agents causing base-pair substitutions. E. coli CM891: (WP2uvrA/pKM101) contains an ochre mutation. It is reverted by many agents causing A-T base-pair substitutions at the trpE locus or by G-C base-pair substitutions in transfer RNA loci elsewhere in the chromosome. It is also deficient in a DNA repair system (uwA), and is more readily reverted by certain mutagens than its parent strain WP2. It also contains the pKMIOl plasmid. The strains of S. typhimurium were obtained from Professor B.N. Ames, University of California, Berkeley, California, USA. The strain of E. coli was obtained from the National Collections of Industrial and Marine Bacteria, Aberdeen, Scotland. Batches of the strains were obtained from master stocks held in liquid nitrogen. The test batches were aliquots of nutrient broth cultures and were stored,at -80C. Dimethyl sulphoxide (DMSO) was added to the cultures at 8% v/v as a cryopreservative. Each batch of frozen strain was tested, where applicable, for cell membrane permeability (rfa mutation), sensitivity to UV light and the pKMIOl plasmid which confers resistance to ampicillin. The responses of the strains to a series of diagnostic mutagens was also assessed. For use in tests an aliquot of frozen culture was added to 25 ml of nutrient broth (Merck No. 2) and incubated, with shaking, at 37C for 10 hours. These cultures provided at least 109 cells per ml which were measured by spreading aliquots (0.1 ml) ofalO"6 dilution of the overnight cultures on the surface of plates of nutrient agar. Company Sanitized. Does no! contain TSC& CBB POSITIVE CONTROLS In the absence ofS9 mix Identity: Supplier: Lot number: Purity: Appearance: Solvent: Concentration: //-Ethyl-^'-nitro-^-nitrosoguanidinefENNG) Sigma Chemical 20F-0235 >97% Pale yellow crystalline powder DMSO (Aldrich, A.C.S.^pectrophotomefric grade, ^99.9% pure) 5 pg/plate for strain TA1535 3 ug/plate for strain TA100 2 ug/plate for strain CM891 Identity: Supplier: Batch number: Purity: Appearance: Solvent: Concentration: Identity: Supplier: Batch number: Purity: Appearance: Solvent: Concentration: 9-Aminoacridine Sigma Chemical tfl8-Q358 99% Yellow powder DMSO (Aldrich, A.C.S. spectrophotometric grade, S99.9% pure) 30 ug/plate for strain TA 1537 2-Nitrofluorene Aldrich Chemical Company 012867 98% Beige powder DMSO (Aldrich, A.C.S. spectrophotometric grade, ^99.9% pure) I ug/plate for strain TA98 In the presence ofS9 mix Identity: Supplier: Batch number: Purity: Appearance: Solvent: Concentration: 2-Aminoanthracene Aldrich Chemical Company 52234-024 96% Green powder DMSO (Aldrich, A.C.S. spectrophotometric grade, ^99.9% pure) 2 ug/plate for strain TA 1535 10 ug/plate for strain CM891 Identity: Supplier: Batch number: Purity: Appearance: Solvent- Concentration: Benzo[a]pyrene Aldrich Chemical Company 67778-105 98% Yellow powder DMSO (Aldrich, A.C.S. spectrophotometric grade, >99.9% pure) 5 ug/plate for strains TA1537, TA98 and TA100 Company Sanitized. Does noS contain TSCA CB? PREPARATION OF S9 FRACTION Species: Sex: Strain: Source: Age: Weight: Rat Male -Sprague-Dawley derived HarianOlacLtd 7-8 weeks <300g S9 fraction was prepared from'a. group of ca 10 animals. Mixed function oxidase systems in file rat livers were stimulated by Aroclor 1254, administered as a single intra-peritoneal injection in Arachis oil at a tfosage^of 500-mg/kg-bodyweight On the fifth day after injection, following an. overnight starvation, the rats were killed and their livers aseptically removed. The following steps were carried out at 0-4C under aseptic conditions. The livers were placed in 0.15M KC1 (3 ml :KC1: 1 g liver) before being transferred to an Ultra-Tunax homogeniser. Following preparation, me hombgenate was centriiuged at 9000 g far 10 minutes. The supernatant fraction (S9 fraction) was dispensed into aliquots and stored at -80C until required. The efficacy of each batch of S9 fraction was tested in a bacterial mutation assay with me mutagenic precursors 7,12- dimethylbenzanthracene and 2-aminoanthracene before use. The sterility was also checked. Date of preparation: 9 June 1998 PREPARATION OF S9 MIX S9 mix contained: S9 fraction (10% v/v), MgC^ (8 mM), KC1 (33 mM), sodium ormophosphate buffer pH7.4 (100 mM), glucose-6-phosphate (5 mM), NADP (4 mM). All me cofactors were filter-sterilised before use. SELECTION OF SOLVENT AND FORMUIATION OFTEST''SlJBSTAIiCK; The solubility of the test substance was assessed at 50 mg/ml in purified water, in which it dissolved following warming to 35-40C with gentle stirring. Therefore purified water (obtained by the reverse osmosis of tap water) was used as me solvent for this study. All concentrations cited mthis report are expressed in terms of pureMUBI^^Bh.e. correction was made for the purity ox|BR <~rtwmanv Sanitized. Does nat contain TSCA CB1 MUTATION TEST PROCEDURE First test The test substance was added to cultures of the five tester strains at seven concentrations 'separated by ca half-logio intervals. The highest concentration of|HHB----posted was 50 mg/ml in the chosen solvent, which provided a final concentration of 5000 ug/plate. This is the standard limit concentration recommended in the regulatory guidelines this assay follows. The negative control was the chosen solvent, purified water. The appropriate positive controls were also included. An aHquot bfO.l ml of a lOhour bacterial culture and 0.5 nu S9 mix or 0.5 ml 0.1 M phosphate buffer (pH 7.4) were placed in glass tubes. An aliquot of 0.1 ml of the test solution was added, followed immediately by 2 ml of molten agar containing 0.5mM histidine/biotin/tryptophan. The mixture was thoroughly shaken and overlaid onto previously prepared petri dishes containing 25 ml minimal agar. Each petri dish was individually labelled with a unique code corresponding to a sheet, identifying the dish^s'cbntents. Three petri dishes were used for each concentration. Plates were also prepared without the. addition of bacteria in order to assess the sterility of the test substance, S9 mix and phosphate buSer. AIT plates were incubated at 37C for ca 72 hours. After ttus period the appearance of the background bacterial lawn was'examined and revertant colonies counted using a Domino automated colony counter. Any toxic effects of the test substance would be detected by a substantial reduction in revertant colony counts or by the absence of a complete background bacterial lawn. In the absence of any toxic effects the top concentration normally used in the second test would be the same as that used in the first. If toxic effects were observed a lower concentration may be chosen. It should be ensured that if a lower concentration was chosen, signs of bacterial inhibition are present at the top concentration. Ideally a minimum of three non-toxic concentrations should be obtained. Second test As a clear negative response was obtained in the first test, a variation to me test procedure was used for the second. The variation used was the pre-incubation assay in which the tubes were incubated at 37C for 30 minutes with shaking before the addition of the agar overlay. 5000 ug/plate was again chosen as the top concentration, but. only.five concentrations were used. ' STABILITY AND FORMULATION ANALYSIS The stability of the test substance and the stability of the test substance in the solvent were not determined as part of this study. Analysis of achieved conceiilraliun was not performed as part of mis study. Company Sanitized. Does not contain TSCA CBi ASSESSMENT OF RESULTS For a test to be considered' valid the mean of the solvent control revertant colony numbers for each strain should lie in die range stated in the appropriate Standard Operating Procedure. Also, the positive control compounds, must cause at least a doubling of mean revertant colony numbers over the negative control. '''' "_ _' The mean number of revertant colonies for all treatment groups were compared wHfi those obtained for the solvent control groups. The mutagenic activity of a test substance was assessed by applying the following criteria: a) If treaaaent with a lest substance produces an increase in revertant colony numbers of at least twice the concurrent solvent controls/with some evidence of a positive dose-relationship, in two separate experiments, with any bacterial strain either in the presence or absence of S9 mix, it is considered to show evidence of mutagenic activity7nthis test system. No statistical analysis is performed. b) If treatment with a test substance does not produce reproducible increases of at least 1.5 times the concurrent solvent controls in either mutation test it is considered to show no evidence of mutagenic activity in this test system. No statistical analysis is performed. c) If the results obtained fail to satisfy the criteria for a clear "positive" or "negative" response given in paragraphs a) and b), additional testing may be performed in order to resolve the issue of the test substance's mutagenic activity in this test system. Should an increase in revertant colony numbers then be observed which satisfies paragraph (a) the substance is considered to show evidence of mutagenic activity in this test system. No statistical analysis is performed. If no clear "positive" response can be obtained, the test data may be subjected to analysis tn determine the statistical significance of any observed increases in revertant colony numbers. The statistical procedures used will be those described by Mahon e( al (1989) and will usually be analysis of variance followed by Dunnett's test. MAINTENANCE OF RECORDS All experimental data arising from the study (including documentary raw data, records and other materials; collectively defined as the "materials") will remain the property of the Sponsor. Huntingdon Life Sciences shall retain the materials in its archive for a period of five years from the date of issue of the final report. After such time, the Sponsor will be contacted and their advice sought on the return, disposal or further retention of the materials. If requested, Huntingdon Life Sciences will continue to retain the materials, subject to a reasonable fee being agreed with the Sponsor. Huntingdon Life Sciences shall also retain a copy of the final report in its archive indefinitely. Company Sanitized. Doas not contam TSCA C8t RESULTS witlfUHBind The resultsObtained positive control compounds are presented in Tables 1 to 5. The mean values quoted have been corrected to the nearest whole number. The absence of colonies on sterility check plates confirmed the absence of microbial contamination. The total colony counts on nutrient agar plates (see Tables) confirmed the viability and nigh"cell density of the cultures of the individual organisms. , . . . . The mean. revertant colony.. counts for me solvent controls .were within, the ranges stated in me appropriate Standard Operating Procedure or quoted by Gatehouse et al (1990). Appropriate positive control chemicals (with S9mix where required) induced substantial increases in revertant colony numbers with all strains, confirming sensitivity of the cultures and activity of the S9 mix. FIRST TEST " -./.. .. . No substantial increases in revertant colony numbers over control counts were obtained with any of the tester strains following exposure tolllBB|Upt any concentration in either the presence or absence ofS9mix. HB^BBB No visible thinning of the background lawn of non-revertant cells was obtained following exposure to A top exposure concentration of 5000 pg/plate was therefore selected for use in the second test. SECOND TEST No substantial increases in revertantcolony numbers over control counts were obtained with any of the tjHUUly: tester strains following exposure ofS9mix. any concentration in either the presence or absence No visible thinning of the background lawn of non-revertant cells was obtained following exposure to CONCLUSION It is concluded that, when tested in purified water.pimjU|^hows no evidence of mutagenic activity in this bacterial system. Rnmnanv Sanitized. Doss not contaSn TSCA CBl REFERENCES AMES, B.N., McCANN, J. and YAMASAKI, E. (1975) Methods for detecting carcinogens and mutageas with the Salmonella/mammalian microsome mutagenicity test. Mutation Res. 31, 347. GATEHOUSE, D.G., ROWLAND, I.R., WILCOX, P., CALLANDER, R.D. andI FORSTER, R. (1990) Bacteria} mutation assays in: KIRKLAND, D.J. (Ed.). UKEMS Sub-committee on Guidelines for Mutagenicity Testing. Report. Part I revised. Basic Mutagenicity Tests: UKEMS Recommended Procedures, p. 13. Cambridge University Press, Cambridge. GREEN, M.H.L. (1984) Mutagen testing using tvp. reversion,in Escherichia coli in_.KILBEY, B.J., LEGATOR, M., NICHOLS, W. and RAMEL, C. (Eds.). Handbook of Mutagenicity Test Procedures. Second edition, p. 161. Elsevier Science Publishers BV, Amsterdam. ICH (1996) GeHoHSacity: .Guidance on Specific Aspects of Regulatory Genotoxicity Tests. ICH (1997) Genotoxicity: A Standard Battery of Genotoxicity Testing ofPharmaceuticaIs. MAHON, G.A.T., GREEN, M.H.L., MIDDLETON, B., MITCHELL, I.DE G., ROBINSON, W.D. and TWEATS, D.J...(1989) Analysis of data from microbial colony assays in: KIRKLAND, D.J. (Ed.). UKEMS Sub-committee - on Guidelines for Mutagenicity Testing. Report. Part III. Statistical Evaluation of Mutagenicity Test Data, p.26. Cambridge University Press, Cambridge. MARON, D.M. and AMES, B.N. (1983) Mutation Res. 113, 173. Revised methods for the Salmonella mutagenicity test. Company Sanitized. Doss not contain TSCA CBI TABLE 1 Results .obtained with Salmonella typhiiwirium TA98 following exposure l S9mix + present - absent. Revertant colony counts and means Test I A B C Mean sd 0 0 0 None; 10'6 dilution of overnight culture, plated on nutrient agar (total counts) 4-5 37 44 --42- 44 35 43 41 31 37 42 37 31 34 36 34 38 38 31 36 32 27 34 31 41 32 48 40 + 38 43 43 41 41 34 42 39 24 41 39 35 34 34 45 38 37 38 35 37 44 36 35 38 41 50 34 42 45 30 31 35 43 39 34 39 554 580 562 565 13 184 284 218 229 51 119 143 129 130 Contoanv Sanitized. Doss not contain TSCA CB6 ] TABLE 1 - continued Results obtained withSalmoneUllaattyvphimurium TA98 following-exposure Plate No. Addition (|tg) 1 None; sterility check 2 ZonylFS-62,(5000); sterility check TO^rifted wa^r (0:1 nd) 15iBenzo[a]pyrene (5) 16 2-Nitrofluorene (1) None; 10r-6 dilution of 17 fflnerni^tcuaun^plated on nutrient agar (total counts) sdlStandard deviation S9mix + present -absent Revertant colony counts and means Test 2 (with pre-incubation) A B C Mean ! sd 0 ' 0 34 38 37 37 42 34 37 42 27 39 42 42 37 20 39 36 37 36 35 38 29 28 41 38 32 37 37 30 44 37 35 37 39 43 32 41 478 471 484 246 306 304 0 36 2 38 4 35 8 41 2 .32 10 36 1 34 5 36 7 35 3 37 7 37 2 39 6 478 285 34 116 112 110 - 113 1 Company Sanitized. Does r^ contain TSCACBi TABLE 2 Results obtained with Salmonella tyyhimur'wm TA100 following exposure < Non^JQ^dHutionof overnight culture, plated on nutrient agar (total counts) Revertantcolony counts and means S9mix Testi - ;- + present A B C Mean sd -absent 0 0 .0 0 W9 93 --89- -97- 11 100 90 94 95 5 106 96 85 96 11 100 109 102 104 5 101 100 103 101 2 86 92 103 34 9 87 102 101 97 8 110 100 96 102 94 114 99 14 99 100 86 95 8 106 90 104 100 9 92 110 92 '98 10 106 108 106 107 I 109 67 82 86 21 108 94 94 99 8 118 107 96 + 412 377 426 107 II 405 25 370 386 413 390 22 135 130 130 132 Sanitized. Does r.ot c^ain TSCA CBS Company TABLE 2 - continued Results obtained withSalmonella fyghimurium TA100 following exposure 1 Plate No. Addition ("g) l|None;sterility check (sterility check 8JParifiedwater (0.1 ml) WPurifiied water .(0:1 nd) Benzo[a]pyrene (5) 16 ENNG (3) None; 10"6 dilution of 17 overnight cutttue, plated on nutrient agar (total counts) sd|Standard deviation S9mix + present -absent Revertant colony counts and means Test 2 (with pre-incubation) A B C Mean | sd 0 0 99 94 100 7 97 101 99 99 2 99 97 102 99 3 87 106 102 98 10 85 94 112 97 14 104 115 89 103 13 109 104 89 101 10 100 99 108 102 5 95 8S 96 93 95 109 102 102 95 90 8S 91 95 103 92 -97 - 391 480 414 428 46 384 387 395 389 106 107 107 107 Company Sanif^d. Does ^t c^ain TSCA CS< TABLE3 Results obtained with Salmonella typhinwrium TA1535 following exposure 1 S9inix + present - absent Revertant colony counts and means Test i A B C j Mean | sd 0 0 0 None; 10 dilution of overnight culture, plated on nutrient agar (total counts) 19 K 47- -IT- 15 20 23 19 15 19 16 17 22 16 16 18 .14 n 14 13 21 17 16 18 21 20 21 21 16 17 23 19 12 19 27 19 20 12 15 16 19 28 16 21 15 17 15 16 19 15 9 14 19 21 34 25 19 19 15 18 17 22 19 19 129 119 132 127 100 117 129 115 15 14i 129 139 136 . e*~~??Mi.^oe<>"Hi. DOoSss Wr-s.t cCOomnt-aasin TSCA CBI TABLE 3 - continued Results obtained with Salmonella typhimurium TA1535 following exposure to| Plate No. Addition (ug) 16 ENNG (5) None; 101-6.dilution of 17 overnight culture,' plated . on nutrient agar (total counts) sdjStandard deviation Revertant colony counts and means Test 2 (with pre-incubation) S9mix +; present A B C Mean sd - absent: 0 0 2fr 14 44- 46- 20 21 20 20 21 14 14 16 22 22 14 19 21 14 20 18 20 23 19 21 16 21 13 17 14 13 19 15 23 23 22 23 20 22 14 19 20 20 23 21 17 22 19 125 118 112 19" 118 90 123 117 110 18 121 111 117 116 S^ed.D,r,o.c-,-.l,lnTSCACB< CompsW aa' TABLE 4 Results obtained with Salmonella typhimurium TA1537 following exposure toj S9nux + present - absent + Revertant colony counts and means Testi A B C | Mean | sd 0 |0 0 8 10- -T 9 10 12 10 2 10 13 12 12 2 12 12 9 11 2 15 10 10 12 3 10 15 9 11 3 13 8 8 12 12 10 15 14 13 10 JL. 11 -L 14 i 16 10 16 14 3 12 12 9 11 2 12 13 13 13 1 10 12 10 11 1 10 12 6 9 3 13 9 12 10 14 13 11 _2_ 12 2 206 237 202 215 19 245 189 202 212 29 115 121 119 118 Company Sanded. Doss rsof contain TSCA CBS TABLE 4 - continued Results obtained wMiSalmonella typhimurium TA1537 following exposure tc Plate No. Addition (Ug) t4l?unfied:waterXO.T nd) 15|Benzo[a]pyrene(5) 16 9-Aniinoacridine (30) None; 10n-6.dilution of 17 pveradght oiritare; plated on nutrient agar (total counts) sd Standard deviation S9nux + present - absent + Revertant colony counts and means Test 2 (with pre-incubation) A B C Mean sd 0 9 12 10 10 16 9 6 10 12 9 8 15 12 14 12 12 12 8 7 8 12 8 8 14 8 12 13 12 10 7 12 10 -10 174 176 203 143 141 136 0 10 12 9 11 13 10 12 10 9 184 16 140 93 115 -108 105 11 C,n'" S.ni..zd. Do^ -. con..,n TSCA CB1 TABLES Results obtained with Escherichia coll CM891 following exposure to S9mix + present - absent Revertant colony counts and means Testi A B C Mean sd 0 0 None;10dilution of overnight culture, plated on nutrient agar (total counts) -96 100 99 1--99 111 94 119 108 90 108 107 99 106 96 97 100 102 103 115 101 95 + 96 107 110 102 100 109 119 108 86 108 109 100 99 87 ?2 81 112 109 104 93 88 110 88 96 107 95 112 435 474 415 768 758 740 123 110 117 -98- -2- 102 9 106 15 105 5 100 6 102 2 104 10 104 7 104 5 104 17 106 5 93 6 101 17 95 8 98 II 105 9 441 30 755 14 117 Company ganl.^.O"'^"0""""""061 TABLE 5 - continued Results obtained with Escherichia coli CM891 following exposure toj Plate No. Addition (ug) 14 Purified water <0;I nri) 15j2-Aminoanthracene (10) 16. ENNG (2) None; 10n-6 dilution of 17 overnight culture, plated on nutrient agar (total counts) sd|Standard deviation S9inix + present - absent Revertant colony counts and means Test 2 (with pre-incubation) A B C Mean sd 0 0 + 87 96 -96 -93- 100 93 103 99 94 96 101 97 115 125 114 118 + 102 114 115 110 102 100 109 104 102 100 78 107 118 128 93 13 118 11 101 90 107 99 9 97 104 101 101 4 115 102 114 110 7 112 m 93 112 19 443 402 465 437 32 842 886 900 876 30 123 124 111 119 Company Ssawa"n^<^- d.Oo^^"^08' APPENDIX 1 Historical control data Presented below are the historical control data from the period 1 April 1997 to 30 June 1998. Purified water solvent controls Strain . S9nux TA 100 i- j . - + tAlJ)35 , - + ,^-. CM8;91 - + TA9 8 - + TA15;?7 - + Minimum Maximum Mean No. of values 78 81 122 123 99:5 100.4 99 '" 99 12 33 18.7 95 10 29 18.8 95 79 164 112.0 31 73 211 121.3 31 26. . 27- 45 47 36.1 98 38.1 ?8. 7 21 12.1 --96 7 22 12.2 -.96. Positive controls Strain S9mix -' Minimum Maximum Mean No. of values TA 100 + -^ 190 1477 377.3 274 240 1231 510.8 273 TA1 535 - + 37 1243 193.8 268 80 533 233.3 267 CMiS91 - + 294 2312 1296.7 89 231 2097 723.1 89 17 .98 - + TA1537 - . - 117 649 243.7 271 (80 ug) (30 ug) 200 562 169 823 4532 384 488.8 1695.4 270 266 251.5 6 + 94 396 210.2 271 Company Sanitized. Does not contain TSCACBS