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AR226-3211 TRADE SECRET Study Title H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats Supplement No. 1 Laboratory Project ID: DuPont-2923 AUTHOR: Carol Finlay, B.A. STUDY COMPLETED ON: July 27, 2000 SUPPLEMENT NO. 1 COMPLETED ON: December 13, 2001 PERFORMING LABORATORY: E.I. du Font de Nemours and Company Haskell Laboratory for Health and Environmental Sciences Elkton Road, P.O. Box 50 Newark, Delaware 19714-0050 WORK REQUEST NUMBERjUByj SERVICE CODE NUMBERi H I Page 1 of 40 ^mpsny San%grf. CTo^^Eafh TSCACBt H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 CERTIFICATION We, the undersigned, declare that this report provides an accurate evaluation of data obtained from this study. Reviewed by; 'Paul M. Hinderiitcr, Ph.D. Postdoctoral Fellow /A-/^-^' Dale Reviewed by; (J^ibt^L ^ ^fcg^^ // JudiA C. Stadler, PhJD., D.A.B.T.Dale ' Director >6-^C-^OOf Igmed by Study Director: jl^X^A^ f (U[^ 'JCf/iIA^ CStaaffrSocienltRist <llay,B.A.0Date 2 - - Company Sanitised. Does not c-j.-iiam TSCA CBt H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 TABLE OF CONTENTS Page CERTIFICATION.........................................................................................................................! LIST OF TABLES .........................................................................................................................4 LIST OF FIGURES .......................................................................................................................4 LIST OF APPENDICES...............................................................................................................4 STUDY INFORMATION .............................................................................................................5 STUDY PERSONNEL...................................................................................................................? REASON FOR SUPPLEMENT NO. 1 ........................................................................................8 SUMMARY....................................................................................................................................9 MATERIALS AND METHODS................................................................................................10 RESULTS AND DISCUSSION ..................................................................................................10 A. Liver Weights....................................................................................................................10 1. Test Substance......................................................;............,,...................................................................10 2. Positive Controls.................................................................................................................................... 10 B. Liver Fluorine Data,...........................................................................................................11 1. Positive Controls.................................................................................................................................. -11 2. Test Substance........................................................................................................................................11 CONCLUSIONS..........................................................................................................................11 TABLES........................................................................................................................................12 FIGURES......................................................................................................................................16 APPENDICES ..............................................................................................................................22 -3- Company Sanitized. Does not contain TSCA CBI H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 LIST OF TABLES Page 1. MEAN BODY AND LIVER WEIGHTS.............................................................................................................13 2. MEAN LIVER FLUORINE LEVELS..................................................................................................................15 3. MEAN LIVER FLUORINE CONCENTRATION NORMALIZED TO DOSE..................................................15 LIST OF FIGURES Page 1. COMPARISON OF MEAN RELATIVE LIVER WEIGHTS: TEST SUBSTANCE AND NEGATIVE CONTROLS.........................;...............................................................................................................................17 2. COMPARISON OF MEAN RELATIVE LIVER WEIGHTS: TEST SUBSTANCE AND POSITIVE CONTROLS.........................................................................................................................................................18 3. COMPARISON OF RELATIVE LIVER WEIGHT AND MEAN LIVER FLUORINE CONCENTRATION FOR H-23961 AND NEGATIVE CONTROLS...................................................................................................19 4. MEAN LIVER FLUORINE CONCENTRATION NORMALIZED TO DOSE..................................................20 5. COMPARISON OF MEAN BLOOD AND MEAN LIVER FLUORINE CONCENTRATION NORMALIZED TO DOSE..................................................................................................................................21 LIST OF APPENDICES Page A. INDIVIDUAL FINAL BODY WEIGHTS, LIVER WEIGHTS, AND RELATIVE LIVER TO BODY WEIGHT.............................................................................................................................................................^ B. INDIVIDUAL FLUORINE LEVELS ..................................................................................................................34 Company Sanitized. Does not contain TSCA CBI H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats STUDY INFORMATION TEST SUBSTANCE: Substance 11 li il iBB^^Bj Synonyms/Codes.^* H-23961 Haskell Number: 23691 DuPont-2923 Supplement No. 1 POSITIVE CONTROL; Substance Testa Synonyms/Codes: i--H-24019 Haskell Number: Company Sanitized. Does not contain TSCA CB1 H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats STUDY INFORMATION (Continued) Compositjoi DuPont-2923 Supplement No. 1 POSITIVE CONTROL; Substance Tested: Synonyms/Codes: H-24020 Haskell Number: 24020 Compositio Known Impurities: Unknown Sponsor: E. I. du Pont de Nemours and Company Wilmington, Delaware 19898 U.S.A. Study Initiated/Completed: April 30, 1999 / (see report cover page) K-\ In-Life Initiated/Completed: May 30, 1999 / August 30, 1999 -6- Company Sanitized. Does not contain TSCA CBi H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 STUDY PERSONNEL Study Director: Management: Primary Technician: Carol Finlay, B.A. Judith C. Stadler, Ph.D., D.A.B.T. Richard P. Mathena Liver Fluorine Data Analysis: Paul M. Hinderliter, Ph.D. Management: Matthew S. Bogdanffy, Ph.D., D.A.B.T. Toxicology Report Preparation: Wanda F. Dinbokowitz Laboratory Veterinarian: Wanda L. West, D.V.M., A.C.L.A.M. -7- Company Sanitized. Does not contain TSCA CB! H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 REASON FOR SUPPLEMENT NO. 1 The purpose of this supplement is to present the results from analysis of selected liver samples from rats treated with the test substance (H-23961), 2 positive controls (H-24019 and H-24020), and 2 negative controls (corn oil and corn oil/acetone). -8- Company Sanitized. Does not contain TSCA CBI H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 SUMMARY The objective of this study was to evaluate the potential for H-23961, when administered by gavage, to be absorbed and to accumulate in a mammalian system. Six groups of 5 male Crl:CD(SD)IGS BR rats each were given 1000 mg/kg/day of H-23961. The test substance was administered to one group of 5 rats for 5 consecutive days and to 5 groups for 10 days. On selected days (5,10, 13, 24, 52, 94) 5 rats per group were euthanized and the blood and livers were collected. Livers were weighed and those collected on study days 10,13, and 94 were analyzed for total fluorine. This supplement includes liver weight data and the results of total fluorine analyses in livers. Additionally, 2 negative controls, corn oil and corn oil/acetone (80:20), and 2 positive controls, H-24019 (10 mg/kg/day) and H-24020 (20 mg/kg/day), were tested and analyzed as described for H-23961. The mean relative liver weights (liver/body weight) of rats dosed with the test substance, H-23961, were similar to the negative controls during the dosing and recovery periods. On day 10, the mean relative liver weight of rats dosed with the positive control H-24019 was up to 27% higher than the negative controls. By day 94, the mean relative liver weight was up to 28% higher than the negative controls. In rats given H-24020, the mean relative liver weight was up to 75% higher at day 10 than the negative controls. By day 94, the weights were similar. The concentration of fluorine in the livers from rats dosed with the test substance, H-23961, was 18.43 fJtMequivalents on day 10 and 3.50 {tM equivalents on day 94. On day 10, mean /xM equivalent concentrations of fluorine in the livers from rats dosed with the positive control materials were approximately 275-fold (H-24019) and 60-fold (H-24020) greater than the fluorine concentration in livers from rats treated with the test substance. By day 94, the concentrations were approximately 340x and 3x the fluorine concentration in rats treated with H-23961. The ftM equivalents of fluorine in the livers from rats dosed with the test substance were higher than levels in the blood. Under the conditions of this study, there was some absorption and retention of fluorine in the liver from rats dosed with H-23961. However, fluorine levels in the liver were significantly lower than levels in rats dosed with the positive control materials, H-24019 and H-24020. Liver weights were not affected in rats dosed with the test substance. 9 - - Company Sanitized. Does net contain TSCA C81 H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 MATERIALS AND METHODS Blood and livers were collected on days 5,10,13,24,52, and 94. The livers were weighed. Only the test day 10,13, and 94 livers were analyzed for total fluorine. These time points provided sufficient data to determine the accumulation and persistence of fluorine in the liver. See the original report for details of the analysis. RESULTS AND DISCUSSION A. Liver Weights (Table 1, Figures 1-3, Appendix A) As with body weights, comparison of absolute liver weights was complicated by the fact that there was a difference in age on test day 1 between rats dosed with the test substance and those dosed with the positive or negative controls. The rats dosed with the test substance, H-23961, were older and heavier in weight than the corn oil negative control and H-24020 positive control rats, but younger and lighter in weight than the corn oiVacetone negative control and H-24019 positive control rats. Therefore, liver weights relative to body weight are presented for comparison. 1. Test Substance The mean relative liver weights of rats dosed with the test substance, H-23961, were similar to the negative controls during the dosing and recovery periods. 2. Positive Controls The mean relative liver weight of rats dosed with one of the positive controls, H-24019, was 17% higher on day 10 than the liver weight of rats dosed with the test substance, H-23961. On days 13, 24, and 52 (recovery), the mean relative liver weights of rats dosed with H-24019 were 13-36% higher than the liver weights of rats dosed with H-23961. By test day 94 (end of recovery), the mean relative liver weight of rats dosed with H-24019 was 21% higher than the liver weight of rats dosed with H-23961. The mean relative liver weight of rats dosed with H-24020, the other positive control, was 60% higher on day 10 than the liver weight of rats dosed with H-23961. On days 13 and 24 (recovery), the mean relative liver weights of rats dosed with H-24020 were 60 and 33% higher than the liver weights of rats dosed with H-23961. On days 52 and 94, the weights were similar. The mean relative liver weight of rats dosed with H-24019 was up to 27% higher at day 10 than the negative control groups. By day 94, the mean relative liver weight of rats dosed with H-24019 was up to 28% higher than the negative controls. The mean relative liver weight of rats dosed with H-24020 was up to 75% higher at day 10 than the negative controls. The mean -10- Company Sanitized. Does not contain TSCA CBI H-23961: Biopersistence Screening DuPont-2923 10-Dose Oral Gavage Study in Rats__________________________________Supplement No. 1 relative liver weights of rats dosed with H-24020 began to decrease during the recovery period and were similar by test day 94 to the negative controls. Therefore, liver weights of rats dosed with the test substance, H-23961, were not affected. B. Liver Fluorine Data (Tables 2-3, Figures 3-5, Appendix B) 1. Positive Controls The positive controls were H-24019 and H-24020. The concentrations of fluorine in the livers on day 10 from rats dosed with the positive control materials were 5045.85 and 1127.25 pM equivalents for H-24019 and H-24020, respectively. At day 13, the liver concentrations were 4135.69 and 334.49 piM equivalents. By day 94, the concentrations were 1190.15 and 10.72 fJiM equivalents. 2. Test Substance Levels of total fluorine in livers from rats dosed with the test substance, H-23961, were lower than the levels in livers from rats dosed with the positive control materials. The total fluorine concentration in the liver from rats dosed with H-23961 was 18.43 p.M equivalents at day 10, 11.89 /xM equivalent at day 13, and 3.50 /zM equivalents at day 94. For the positive control H-24019, the liver concentrations were approximately 275x higher (day 10) and approximately 340x higher (end of study) than H-23961. For H-24020, the liver concentration was approximately 60x higher (day 10) and approximately 3x higher (end of study). The fJiM equivalents of fluorine in the livers from rats dosed with the test substance were higher than levels in the blood. CONCLUSIONS Under the conditions of this study, there was some absorption and retention of fluorine in the liver from rats dosed with H-23961. However, fluorine levels in the liver were significantly lower than levels in rats dosed with the positive control materials, H-24019 and H-24020. Liver weights were not affected in rats dosed with the test substanc. -11- Company Sanitized. Does not contain TSCA CBI TABLES 12Company Sanitized. Does not contain TSCA CBI Test Days 5 10 13 24 52 94 TABLE 1 MEAN BODY AND LIVER WEIGHTS (g) CORN OIL (NEGATIVE CONTROL) Absc)lute Body Weight Liver Weight 259.3 12.620 311.1 15.861 322.9 14.906 391.2 16.635 464.7 17.240 557.8 20.118 Mean Relative Liver Weight(% of Body Weight) 0.049 0.051 0.046 0.043 0.037 0.036 Test Days 5 10 13 24 52 94 CORN OIL:ACETONE (NEGATIVE CONTROL) Absolute Body Weight Liver Weight 313.4 13.632 356.5 15.597 377.6 17.715 423.5 17.172 527.6 21.275 567.8 18.447 Mean Relative Liver Weight(% of Body Weight) 0.043 0.044 0.047 0.041 0.040 0.032 Test Days 5 10 13 24 52 94 H-24019 (POSITIVE CONTROL) Absolute Body Weight Liver Weight 306.6 15.456 310.1 17.336 344.8 22.049 387.9 21.313 438.1 19.826 597.9 24.455 Mean Relative Liver Weight(% of Body Weight) 0.050 0.056 0.064 0.055 0.045 0.041 -13- Company Sanitized. Does not contain 7SCACB1 H-23961: B iopersistence Screening 10-Dose Oral Gavage-Study in Rats DuPont-2923 Supplement No. 1 Test Days 5 10 13 24 52 94 TABLE 1 (Continued) MEAN BODY AND LIVER WEIGHTS (g) H-24020 (POSITIVE CONTROL) A1^solute Body Weight Liver Weight 244.8 17.052 284.4 21.944 289.1 21.780 370.3 20.619 456.7 17.713 538.7 18.205 Mean Relative Lrver Weight(% of Body Weight) 0.070 0.077 0.075 0.056 0.039 0.034 Test Days 5 10 13 24 52 94 H-23961 (TEST SUBSTANCE) __B_o_d_y_W_e_igAhbt_s_o_l_uLtivee_r_W_e_ig_h_t __ 264.9 11.821 306.4 14.729 336.7 15.488 381.7 15.991 502.0 19.891 561.7 18.957 Mean Relative Liver Weight(% of Body Weight) 0.045 0.048 0.046 0.042 0.040 0.034 Company Sanitized. Does not contain TSCA CBI H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 TABLE 2 MEAN LIVER FLUORINE LEVELS Test Days 10 13 94 Negzitive Controls Corn Oil (ppm) Corn Oil: Acetone (ppm) <0.2 <0.5 0.6" I3 Positive Controls H-24019 (ppm) 328.18 (19.3)" 269.02 (10.1) 77.56 (10.1) H-24020 (ppm) 155.76 (29.2) 46.36 (10.7) 1.68 (0.3) a One value. Four of the values were below the level of detection (LOD). b Standard deviation is in parentheses. Indicates no value for this day. Test Substance H-23961 (ppm) 20.84 13.52 (2.7) (1.5) 4.12 (4.0) TABLE 3 MEAN LIVER FLUORINE CONCENTRATION NORMALIZED TO DOSE Test Days 10 13 94 Positive Controls H-24019 H-24020 /iM F Equivalents 5045.85 (296.91)3 pM F Equivalents 1127.25 (211.37) 4135.69 (155.38) 334.49 (77.70) 1190.15 (156.05) 10.72 (2.14) a Standard deviation is in parentheses. Test Substance H-23961 liM F Equivalents 18.43 (2.4) 11.89 (1.4) 3.50 (3.6) -15Company Sanitized. Does not contain 7SCA CBI H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 FIGURES -16- Company Sanitized. Does not contain TSCA CBI [-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats FIGURE 1 COMPARISON OF MEAN RELATIVE LIVER WEIGHTS: TEST SUBSTANCE AND NEGATIVE CONTROLS Test Day -17- Company Sanitized. Does not co H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats FIGURE 2 COMPARISON OF MEAN RELATIVE LIVER WEIGHTS: TEST SUBSTANCE AND POSITIVE CONTROLS Test Day -18- Company Sanitized. Does not cont 3961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats FIGURES COMPARISON OF RELATIVE LIVER WEIGHT AND MEAN LIVER FLUORINE CONCEN FOR H-23961 AND NEGATIVE CONTROLS Day 10 Day 13 Day 94 Day 10 Day 13 El Corn Oil (Negative Control) Corn OiLAcetone (Negative Control) D H-23961 (Test Substance) -19- Company Sanitized. Does not contai eo 83 : 8 3 " i i4 3 113 - 3 J i . Gao SER i 3 \ TE SB OE Behe Te | } sworeanba 4 wt 3961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats FIGURE 5 COMPARISON OF MEAN BLOOD AND MEAN LIVER FLUORINE CONCENTRATION NORMA 6000 5000 4000 3000 . _S "5 o" uj 2000 1000 Blood / Liver Blood / Liver Blood / Liver -21- Company Sanitized. Doss not co H-23961: Biopersistence Screening 10-DoseOralGavage Study in Rats^ DuPont-2923 Supplement No. 1 APPENDICES -22- Company Saniilzed. Does r.ot csssiffin TSCA. CB! APPENDIX A Individual Final Body Weights, Liver Weights, and Relative Liver to Body Weight -23- Company Sanitized. Does no; contain TSCA CBI H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 CORK1 OIL (NEGATIVE CONTROL) INDIV:IDUAL FINAL BC>DY WEIGHTS (g),. LIVER WEIGHTS (cr), AND RELATIVE LF^ER TO BODY WE I GHT OF MALE RATS Animal Number 627789 627801 627805 627810 627818 Final Body Wfc. 247.7 240.1 283.7 265.0 260.2 GROUP I Liver Wt. 11.428 12.216 14.081 13.395 11.981 Relative Liver to Body Wt. 0.046 0.051 0.050 0.051 0.046 Test Day 5 5 5 5 5 Animal Number 627793 627797 627799 627800 627808 Final Body Wt. 283.5 324.2 294.7 331.3 321.8 GROUP II Liver Wt. 15.292 15.803 14.285 16.344 17.580 Relative Liver to Body Wt. 0.054 0.049 0.048 0.049 0.055 Test Day 10 10 10 10 10 Animal Number 627796 627806 627807 627809 627816 Final Body Wt. 322.7 320.3 305.2 336.2 330.2 GROUP III Liver Wt. 13.404 15.413 14.935 14.967 15.811 Relative Liver to Body Wt. 0.042 0.048 0.049 0.045 0.048 Test Day 13 13 13 13 13 -24- Company Sanitized. Does not coniain TSCA CB1 H-23961: B iopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 CORKr OIL (NEGATIVE; CONTROL) mm/IDUAL FINAL BC)DY WEIGHTS (g) , LIVER WEIGHTS (cr), AND RELATIVE LP'\TER TO BODY WE:[GHT OF MALE RATS Animal Number 627791 627794 627804 627812 627817 Final Body Wt. 365.6 416.7 378.1 388.4 407.3 GROUP IV Liver Wt. 15.371 19.105 15.326 16.775 16.600 Relative Liver to Body Wt. 0.042 0.046 0.041 0.043 0.041 Test Day 24 24 24 24 24 Animal Number 627792 627798 627813 627814 627815 Final Body Wt. 496.8 517.3 416.8 386.9 505.9 GROUP V Liver Wt. 16.359 19.293 15.234 14.358 20.958 Relative Liver to Body Wt. 0.033 0.037 0.037 0.037 0.041 Test Day 52 52 52 52 52 Animal Number 627795 627811 627819 627820 627821 Final Body Wt. 485.0 511.6 653.1 618.0 521.5 GROUP VI Liver Wt. 16.649 17.405 21.828 26.766 17.943 Relative Liver to Body Wt. 0.034 0.034 0.033 0.043 0.034 Test Day 94 94 94 94 94 -25- Company Sanitized. Does sasi oisoSaaa TSCA CBi H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 CORN OIL,:ACETONE (NEGA^['IVE CONTROL) INDF/IDUAL FINAL BOiDY WEIGHTS (g),, LIVER WEIGHTS (cf), AND RELATIVE LP/ER TO BODY WEI GHT OF MALE RATS Animal Number 625361 625363 625364 625380 625383 Final Body Wt. 349.7 286.7 312.0 305.5 313.1 GROUP I Liver Wt. 16.800 11.236 13.845 13.253 13.026 Relative Liver to Body Wt. 0.048 0.039 0.044 0.043 0.042 Test Day 5 5 5 5 5 Animal Number 625355 625362 625367 625368 625378 Final Body Wt. 333.6 332.9 363.8 386.7 365.4 GROUP II Liver Wt. 14.409 14.363 16.139 17.745 15.328 Relative Liver to Body Wt. 0.043 0.043 0.044 0.046 0.042 Test Day 10 10 10 10 10 Animal Number 625357 625358 625370 625384 625385 Final Body Wt. 405.6 340.7 407.0 357.1 377.6 GROUP III Liver Wt. 20.091 12.954 21.654 16.520 17.355 Relative Liver to Body Wt. 0.050 0.038 0.053 0.046 0.046 Test Day 13 13 13 13 13 -26- Company Sanitized. Does not contain TSCA CBI H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 CORN Oil,:ACETONE (NEGATIVE CONTROL) INDI^/IDUAL FINAL BC)DY WEIGHTS (g) , LIVER WEIGHTS (cr), AND RELATIVE LPi/ER TO BODY WEI:GHT OF MALE RATS Animal Number 625354 625365 625371 625376 625381 Final Body Wt. 396.1 459.6 447.3 432.9 381.8 GROUP IV Liver Wt. 16.383 18.313 17.859 19.168 14.135 Relative Liver to Body Wt. 0.041 0.040 0.040 0.044 0.037 Test Day 24 24 24 24 24 Animal Number 625356 625359 625360 625372 625374 Final Body Wt. 533.7 530.3 555.4 506.2 512.3 GROUP V Liver Wt. 20.498 22.901 23.312 21.287 18.378 Relative Liver to Body Wt. 0.038 0.043 0.042 0.042 0.036 Test Day 52 52 52 52 52 Animal Number 625353 625369 625373 625375 625377 Final Body Wt. 565.3 514.8 673.7 588.8 496.6 GROUP VI Liver Wt. 18.655 17.379 20.073 18.869 17.261 Relative Liver to Body Wt. 0.033 0.034 0.030 0.032 0.035 Test Day 94 94 94. 94 94 -27- CcEipany SaufiadL Qaes aaS.essiMa. ISCA CBI H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 H-2^1019 (POSITIVE CONTROL) INDB/TDUAL FINAL BODY WEIGHTS (g) , LIVER WEIGHTS (cI), AND RELATIVE LI\^ER TO BODY WEI GHT OF MALE RATS ^ Animal Number 625322 625323 625336 625343 625349 Final Body Wt. 329.0 298.0 318.1 294.0 293.7 GROUP I Liver Wt. 16.409 14.830 16.545 13.809 15.685 Relative Liver to Body Wt. 0.050 0.050 0.052 0.047 0.053 Test Day 5 5 5 5 5 Animal Number 625320 625330 625332 625341 625350 Final Body Wt. 312.1 310.1 318.3 325.6 284.3 GROUP II Liver Wt. 18.845 16.343 17.528 18.254 15.709 Relative Liver to Body Wt. 0.060 0.053 0.055 0.056 0.055 Test Day 10 10 10 10 10 Animal Number 625321 625327 625342 625345 625348 Final Body Wt. 371.2 355.3 324.4 336.9 336.4 GROUP III Liver Wt. 22.322 22.259 20.718 24.403 20.541 Relative Liver to Body Wt. 0.060 0.063 0.064 0.072 0.061 Test Day 13 13 13 13 13 -28- Company Sanitized. Does not contain TSCA CBI H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 H-2-4019 (POSITIVE CONTROL) INDI\^IDUAL FINAL BOIDY WEIGHTS (g) , LIVER WEIGHTS (cr), AND RELATIVE LI1/ER TO BODY WEI GHT OF MALE RATS Animal Number 625325 625328 625338 625340 625352 Final Body Wt. 381.3 423.9 339.9 419.0 375.3 GROUP IV Liver Wt. 21.479 22.100 18.018 23.131 21.835 Relative Liver to Body Wt. 0.056 0.052 0.053 0.055 0.058 Test Day 24 24 24 24 24 Animal Number 625324 625329 625333 625334 625344 Filial Body Wt. 447.4 498.1 427.4 426.5 391.0 GROUP V Liver Wt. 20.900 20.911 20.508 19.144 17.666 Relative Liver to Body Wt. 0.047 0.042 0.048 0.045 0.045 Test Day 52 52 52 52 52 Animal Number 625326 625335 625346 626347 625351 Final Body Wt. 577.5 579.5 556.9 638.9 636.8 GROUP VI Liver Wt. 23.749 21.548 23.945 27.416 25.615 Relative Liver to Body Wt. 0.041 0.037 0.043 0.043 0.040 Test Day 94 94 94 94 94 -29- Company Sanitized. Does not contain TSCA CBI H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 H-2.4020 (POSITIVE CONTROL) INDI^/IDUAL FINAL BCDY WEIGHTS (g),, LIVER WEIGHTS ( g), AND RELATIVE LF/ER TO BODY WEI GHT OF MALE RATS Animal Number 627756 627767 627771 627773 627777 Final Body Wt. 237.5 248.6 239.6 262.3 236.0 GROUP I Liver Wt. 15.360 19.033 16.968 17.629 16.268 Relative Liver to Body Wt. 0.065 0.077 0.071 0.067 0.069 Test Day 5 5 5 5 5 Animal Number 627768 627774 627776 627782 627785 Final Body Wt. 293.5 338.2 254.4 268.2 267.9 GROUP II Liver Wt. 22.536 27.332 18.821 20.172 20.857 Relative Liver to Body Wt. 0.077 0.081 0.074 0.075 0.078 Test Day 10 10 10 10 10 Animal Number 627758 627763 627764 627787 627788 Final Body Wt. 308.7 285.8 306.7 234.9 309.4 GROUP III Liver Wt. 26.021 22.123 21.526 16.498 22.730 Relative Liver to Body Wt. 0.084 0.077 0.070 0.070 0.073 Test Day 13 13 13 13 13 -30- Company Sanitized. Does not contain TSCA CBI H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 H-2 4020 (POSITIVE CONTROL) INDF^IDUAL FINAL BC)DY WEIGHTS (g) , LIVER WEIGHTS ( g), AND RELATIVE LI1^ER TO BODY WE I ;GHT OF MALE RATS Animal Number 627759 627761 627770 627779 627786 Final Body Wt. 380.1 359.4 379.8 406.2 326.1 GROUP IV Liver Wt. 22.707 19.579 19.540 24.858 16.410 Relative Liver to Body Wt. 0.060 0.054 0.051 0.061 0.050 Test Day 24 24 24 24 24 Animal Number 627757 627760 627765 627772 627781 Final Body Wt. 436.7 456.5 455.6 513.5 421.0 GROUP V Liver Wt. 16.899 18.240 16.505 20.225 16.695 Relative Liver to Body Wt. 0.039 0.040 0.036 0.039 0,040 Test Day 52 52 52 52 52 Animal Number 627762 627769 627775 627778 627783 Final Body Wt. 528.6 609.6 552.8 445.3 557.2 GROUP VI Liver Wt. 17.732 19.324 17.296 15.628 21.044 Relative Liver to Body Wt. 0.034 0.032 0.031 0.035 0.038 Test Day 94 94 94 94 94 -31 H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 H-2 3961 (TEST SUB STANCE) INDI^/IDUAL FINAL BOE)Y WEIGHTS (g) ,. LIVER WEIGHTS (gr), AND RELATIVE LIV;ER TO BODY WE I GHT OF MALE RATS Animal Number 626876 626877 626885 626889 626890 Final Body Wt. 262.6 278.2 245.9 268.9 268.9 GROUP I Liver Wt. 12.535 12.834 10.960 11.468 11.306 Relative Liver to Body Wt. 0.048 0.046 0.045 0.043 0.042 Test Day 5 5 5 5 5 Animal Number 626871 626872 626875 626882 626888 Final Body Wt. 309.0 318.1 315.1 325.1 264.8 Animal Number 626868 626879 626886 626887 626891 Final Body Wt. 366.9 320.6 319.9 329.9 346.3 GROUP II Liver Wt. 16.809 15.772 15.102 14.461 11.499 Relative Liver to Body Wt. 0.054 0.050 0.048 0.044 0.043 Test Day 10 10 10 10 10 GROUP III Liver Wt. 16.841 15.748 14.966 13.393 17.845 Relative Liver to Body Wt. 0.046 0.049 0.047 0.041 0.052 Test Day 13 13 13 13 13 -32- Company Sanitized. Does not corAain TSCA CB! H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 H-:23961 (TEST SUI3STANCE) INDF/IDUAL FINAL BC>DY WEIGHTS (g) , LIVER WEIGHTS (c[), AND RELATIVE LF/ER TO BODY WE][GHT OF MALE RATS Animal Number 626864 626865 626873 626894 626895 Final Body Wt. 390.7 351.8 424.7 380.8 360.6 GROUP IV Liver Wt. 16.059 14.379 18.570 15.501 15.449 Relative Liver to Body Wt. 0.041 0.041 0.044 0.041 0.043 Test Day 24 24 24 24 24 Animal Number 626867 626880 626881 626884 626892 Final Body Wt. 478.7 470.8 533.9 507.8 518.8 GROUP V Liver Wt. 17.371 19.473 21.007 21.287 20.319 Relative Liver to Body Wt. 0.036 0.041 0.039 0.042 0.039 Test Day 52 52 52 52 52 Animal Number 626866 626869 626874 626893 626896 Final Body Wt. 565.5 507.0 654.5 539.5 541.8 GROUP VI Liver Wt. 19.198 17.216 22.444 16.143 19.786 Relative Liver to Body Wt. 0.034 0.034 0.034 0.030 0.037 Test Day 94 94 94 94 94 -33- LTSCA.CBS H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 APPENDIX B Individual Fluorine Levels -34- Cosnpeny Sare?tze& Does nal sanlain 7SOA CK % H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 Terms: Active % Active TERMS AND CALCULATIONS Mol Wt Active Formulation Dose % F in Active MolWtF Compound Calculations: Dose Active (mg/kg) The mg of fluorine containing compound administered per kg of animal body weight. = (% active/100) x Formulation Dose Dose Active (mmole/kg) The mmole of fluorine containing compound administered per kg of animal body weight = dose [mg/kg] / Mol Wt Active [mg/mmol] Dose F (mg/kg) The mg Fluorine administered per kg of animal body weight = (% F in active/100) x Dose Active [mg/kg] Dose F (mmol/kg) The mmole of fluorine administered per kg of animal body weight = Dose F [mg/kg] / Mol Wt F [mg/mmol] Molar Ratio (Active/F) The moles of fluorine containing compound per mole of fluorine = Dose Active [mmol/kg] / Dose F [mmol/kg] Formulation Dose Normalization Factor The formulation dose that would be required to administer the amount of active needed to achieve the normalized dose = (Normalized dose of Active [mmol/kg] / Dose Active [mmol/kg]) x Formulation Dose -35- Cci^paay SaEutizad. Does tiotcaatsiti TSCA CBI TERMS AND CALCULATIONS Individual Animal Measurement: ppm F in liver The ppm fluoride measured in liver Individual Animal Calculations: ppm F in Liver minus Bkg 0.2 ppm ppm F in Liver normalized to 0.1 mmol/kg Dose The ppm fluoride measured in liver minus the background fluoride measured in control animal liver. In this case the value was established at 0.2 ppm. The ppm fluoride minus background that would be expected if the active dose was 0.1 mmol/kg instead of the actual active dose. This assumes linearity between administered dose and liver fluorine levels, but is needed because different doses of active were used in the study. = (0.1 [mmol/kg] / Active dose [mmol/kg]) x (ppm F in liver minus background) j^molar equivalents of active in liver The /imolar [/zmol/L] concentration of fluorine containing compound in liver based on the ppm fluorine in liver normalized to 0.1 mmol/kg active dose. This assumes that all liver fluorine is derived from the fluorine-containing component in the formulation. Note: 1 ppm - Img/L = (Normalized ppm [mg/L] fluorine in liver / Mol Wt F [mg/mmol]) x molar ratio active/F [mmol active/mmol F] x 1000 ^imol/mmol -36- CoEnpany Sanitized. Does ncf cssiisaa TSCA CBS H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2923 Supplement No. 1 FACTORS INFLUENCING INTERPRETATION OF KINETIC ANALYSIS Considerations: - The data used for kinetic analysis was from a limited screen and extrapolation should be done cautiously. - Sample size is low - Analytical data used without validation - Steady-state not reached - Terminal phase may not be reached - Some compounds are mixtures of fluorinated compounds - Different active and formulation doses were used - Different vehicles were used to deliver formulations - Each compound may have very different potency for producing toxicity Assumptions: (May or may not be justified in all cases) - Liver fluorine concentrations are linear with respect to dose - Analytical method is appropriate for all types of compounds - Elimination kinetics can be determined based on total fluorine rather than on concentrations of individual components - Background Fluorine is 0.2 ppm - % F data is the % Fluorine of the active (Fluorine containing component(s) in the formulation) - Molecular weight is the molecular weight of the active component in the formulation -37- CGEipar.g Sanitized. DoasnatGantam TSCACBi H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats Data for H- 24019 DuPont-2923 Supplement No. 1 Given: Mol Wt. Active (g/mole): 497 Formulation Dose (mg/kg): 10 % Active (F Containing) in Formulation: 100 % P in Active: 65 Mol Wt. F (g/mol): 19 Calculated Values: Dose Active (mg/kg): Dose Active (mmole/kg): Formulation Dose Normalization Factor: 10 0.020 49.7 Dose F (mmol/kg): 0.342 Molar Ratio (Active/F): 0.059 Dose F (mg/kg):_____6.5 Rat Number Test Day Sample ppmF in Liver Group II 625320 10 625330 10 625332 10 625341 10 625350 10 319.4 355.4 338.4 305.0 322.7 Group III 625321 13 625327 13 625342 13 625345 13 625348 13 255.9 275.3 277.9 260.4 275.6 Group VI 625326 94 625335 94 625346 94 625347 94 625351 94 79.8 89.6 73.8 62.5 82.1 ppm F in Liver Minus Bkg 0.2 ppm 319.2 355.2 338.2 304.8 322.5 255.7 275.1 277.7 260.2 275.4 79.6 89.4 73.6 62.3 81.9 ppm F in Liver Normalized to 0.1 mmoles/kg Dose ^molar Equivalents of Active in Liver 1586.42 1765.34 1680.85 1514.86 1602.83 4910.77 5464.62 5203.08 4689.23 4961.54 1270.83 1367.25 1380.17 1293.19 1368.74 3933.85 4232.31 4272.31 4003.08 4236.92 395.61 444.32 365.79 309.63 407.04 1224.62 1375.38 1132.31 958.46 1260.00 -38- Company Sanitized. Does not contain TSCA CBI H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats Data for H- 24020 DuPont-2923 Supplement No. 1 Given: Mol Wt. Active (g/mole): 426 Formulation Dose (mg/kg): 20 % Active (F Containing) in Formulation: 100 % F in Active: 69 Mol Wt. F (g/mol): 19 Calculated Values: Dose Active (mg/kg): Dose Active (mmole/kg): Formulation Dose Normalization Factor: 20 0.047 42.6 Dose F (mmol/kg): 0.726 Molar Ratio (Active/F): 0.065 Dose F (mg/kg):_____13.8 Rat Number Test Day Sample ppmF in Liver Group II 627768 10 182.5 627774 10 109.0 627776 10 174.0 627782 10 147.5 627785 10 165.8 Group III 627758 13 627764 13 627787 13 627763 13 627788 13 61.5 40.5 33.3 51.3 45.2 Group VI 627778 94 627783 94 627762 94 627775 94 627769 94 1.9 - 1.2 1.9 1.6 1.8 ppm F in Liver Minus Bkg 0.2 ppm 182.3 108.8 173.8 147.3 165.6 61.3 40.3 33.1 51.1 45.0 1.7 1.0 1.7 1.4 1.6 ppm F in L iver Normalizedto 0.1 mmoles/kg Dose 388.30 231.74 370.19 313.75 352.73 130.57 85.84 70.50 108.84 95.85 3.62 2.13 3.62 2.98 3.41 /imolar Equivalents of Active in Liver 1321.01 788.41 1259.42 1067.39 1200.00 444.20 292.03 239.86 370.29 326.09 12.32 - 7.25 12.32 10.14 11.59 -39- Company SanifzecL Does not <^n. TSQA OK H-23961: Biopersistence Screening 10-Dose Oral Gavage Study in Rats Data for H-23961 DuPont-2923 Supplement No. 1 Given: Mol Wt. Active (g/mole): 27500 % F in Active: 40 Formulation Dose (mg/kg): 1000 Mol Wt. F (g/mol): 19 % Active (F Containing) in Formulation: 28 Calculated Values: Dose Active (mg/kg): Dose Active (mmole/kg): Formulation Dose Normalization Factor: 280 0.010 9821.4 Dose F (mmoVkg): 5.895 Molar Ratio (Active/F): 0.002 Dose F (mg/kg):_____112 Rat Number Test Day Sample ppmF in Liver Group II 626871 10 626872 10 626875 10 626882 10 626888 10 19.6 22.8 20.8 17.1 23.9 Group III 626868 13 626879 13 626886 13 626887 13 626891 13 15.7 13.4 12.4 14.3 11.8 Group VI 626866 94 11.3 626869 94 2.5 626874 94 1.6 626893 94 2.4 626896 94 2.8 ppmF in Liver Minus Bkg 0.2 ppm 19.4 22.6 20.6 16.9 23.7 15.5 13.2 12.2 14.1 11.6 11.1 2.3 1.4 2.2 ' 2.6 ppm F in Liver Normalized to 0.1 mmoles/kg Dose 190.54 221.96 202.32 165.98 232.77 152.23 129.64 119.82 138.48 113.93 109.02 - 22.59 13.75 21.61 25.54 /imolar Equivalents of Active in Liver 17.32 20.18 18.39 15.09 21.16 13.84 11.79 10.89 12.59 10.36 9.91 2.05 1.25 1.96 2.32 -40- Cosapany San.^sd.. Dass nctcoasam TSCA CBI