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TRADE SECRET Study Title H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats Supplement No. 1 Laboratory Project ID: DuPont-2926 AR226-3216 AUTHOR: CarolPinlay,B.A. STUDY COMPLETED ON: September 5, 2000 SUPPLEMENT NO. 1 COMPLETED ON: January 11, 2002 PERFORMING LABORATORY: E.I. du Pont de Nemours and Company Haskell Laboratory for Health and Environmental Sciences Elkton Road, P.O. Box 50 Newark, Delaware 19714-0050 WORK REQUEST NUMBER: SERVICE CODE NUMBER: K Page 1 of 40 Company Sanitized. Does not contain TSCA CBI CERTIFICATION We, the undersigned, declare that this report provides an accurate evaluation of data obtained from this study. Reviewed by: Paul M. Hhideriiter, PhJ5. Postdoctoral Fellow o^J^-w^ Date Reviewed by: /V^J^g6<^/,i.J^^ciULuO Judith C. Stadler.PhJ).. D.A.B .T. Director /O-TAfJ-760-^ Date Issned by Study Director: tfLAbL tiC^L/liA_________ Caroimnlay.BAj Staff Scientist J_L_A^L-^ ^ Wate ^te-.^ t^'- s -1- Company SanHlzed. Does not contain TSCA GB) H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 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...................................................................................................................7 REASON FOR SUPPLEMENT NO. 1........................................................................................8 SUMMARY...................................................................................................................................^ MATERIALS AND METHODS................................................................................................10 RESULTS AND DISCUSSION ..................................................................................................10 A. Liver Weights.....................................................................................................................10 1. Test substance.........................................................................................................................................10 2. Positive Controls .................................................................................................................................... 10 B. Liver Fluorine Data............................................................................................................II 1. Positive Controls ....................................................................................................................................11 2. Test Substance........................................................................................................................................11 CONCLUSIONS..........................................................................................................................11 TABLES........................................................................................................................................12 FIGURES......................................................................................................................................16 APPENDICES ..............................................................................................................................22 -3- Company Sanitized. Does not contain TSCA CBt 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 ANDMEAN LIVER FLUORINE CONCENTRATION FOR H-24002 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 ,4- Company Sanitized. Does not contain TSCA CBI STUDY INFORMATION TEST SUBSTANCE: Substance Tested: Synonyms/Codes: H-24002 Haskell Number: 24002 Composition Known Impurities: Unknown POSITIVE CONTROL: Known Impurities: Unknown -5Company Sanitized. Does not contain TSCA C^ STUDY INFORMATION (Continued) POSITIVE CONTROL: Synonyms/Codes: H-24020 Haskell Number: 24020 Composition: 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) In-Life Initiated/Completed: July 11, 1999/October 12, 1999 -6GompanySanded. Does not contah TSCA cm H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 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 Sanded. Does hot contain TSCACW H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 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-24002), 2 positive control (H-24019 and H-24020), and 2 negative controls (corn oil and corn oiVacetone). -8- CompanySanltbed. Does not contain TSCACBl H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 SUMMARY The objective of this study was to evaluate the potential for H-24002, 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 75 mg/kg/day of H-24002. The test substance was administered to one group of 5 rats for 5 consecutive days and to 5 groups for 10 days. Approximately 2 hours after the first dose, blood was collected from the orbital sinus of each rat from the 5-dose group. 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 and 94 were analyzed for total fluorine. This supplement includes liver weight data and the results of total fluorine analyses in liver. Additionally, 2 negative controls, corn oil and corn oiVacetone (80:20), and 2 positive controls, H-24019 (10 mg/kg/day) and H-24020 (20 mg/kg/day), were tested as described for H-24002. The mean relative liver weights (liver/body weight) of rats dosed with the test substance, H-24002, were similar to the negative controls. 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 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-24002, was 696.43 fiM equivalents on day 10 and 15.58 /xM equivalents on day 94. On day 10, mean ^M equivalent concentrations of fluorine in the livers from rats dosed with the positive control materials were approximately 7-fold (H-24019) and 2-fold (H-24020) greater than the fluorine concentration in livers from rats treated with the test substance. By day 94, the concentration in the livers from rats treated with the positive control H-24019 was approximately 70x fluorine concentration in rats treated with H-24002. The concentrations of fluorine on day 94 were similar in rats treated with the positive control H-24020 and the test substance, H-24002. The {JIM equivalents of fluorine in the livers from rats treated with the test substance, H-24002, were higher than levels in the blood. Under the conditions of this study, there was some absorption and retention of fluorine in the livers from rats dosed with H-24002. Fluorine levels in the livers from rats dosed with the test substance were lower than levels in rats dosed with the positive control H-24019. Fluorine levels in the livers from rats dosed with the test substance were lower on day 10 than levels in rats dosed with the positive control H-24020. On day 94, the fluorine levels were similar. Liver weights were not affected in rats dosed with the test substance. -9- Company Sanitized. Does not contain TSCA rwi H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 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 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 (Tables 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 H-24019 positive control or the corn oil:acetone negative control. 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-24002, were similar to the negative controls. 2. Positive Controls The mean relative liver weight of rats dosed with one of the positive controls, H-24019, was 12% higher on day 10 than the liver weight of rats dosed with the test substance, H-24002. On days 13, 24, and 52 (recovery), the mean relative liver weights of rats dosed with H-24019 were 22 or 33% higher than the liver weights of rats dosed with H-24002. 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-24002. The mean relative liver weight of rats dosed with H-24020, the other positive control, was 54% higher on day 10 than the liver weight of rats dosed with H-24002. On days 13 and 24 (recovery), the mean relative liver weights of rats dosed with H-24020 were 33 or 24% higher than the liver weights of rats dosed with H-24002. 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 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-24002, were not affected. -10- Corepany Sanitized. Does not contain TSCA CBI H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 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 ^iM equivalents for H-24019 and H-24020, respectively. By day 94, the concentrations were 1190.15 and 10.72 pM. equivalents. 2. Test Substance Levels of total fluorine in livers from rats dosed with the test substance, H-24002, were generally 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-24002 was 696.43 /AM equivalents at day 10 and 15.58 /xM equivalents at day 94. For the positive control H-24019, the liver concentrations were approximately 7x higher (day 10) and approximately 70x higher (end of study) than H-24002. For H-24020, the liver concentration was approximately 2x higher than H-24002 by the end of dosing. The concentrations were similar by the end of recovery. The pM. equivalents of fluorine in the livers from rats dosed with the test substance, H-24002, were higher than levels in the blood. CONCLUSIONS Under the conditions of this study, there was some absorption and retention of fluorine in the livers from rats dosed with H-24002. Fluorine levels in the livers from rats dosed with the test substance were lower than levels in rats dosed with the positive control H-24019. Fluorine levels in the livers from rats dosed with the test substance were lower on day 10 than levels in rats dosed with the positive control H-24020. On day 94, the fluorine levels were similar. Liver weights were not affected in rats dosed with the test substance. % 11Company Sanitized. Does not contain TSCA C81 H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 TABLES -12- :CompanySanitized. Does not contain TSCA CBI H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 Test Days 5 10 13 24 52 94 TABLE 1 MEAN BODY AND LIVER WEIGHTS (g) CORN OIL (NEGATIVE CONTROL) Absclute 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 OELACETONE (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 c 10 13 24 52 94 H-24019 (POSITIVE CONTROL) ___Bo_d_y_W__ei_gAhtb_s__o_luLitvee_r_W_e_ig_h_t __ i3r>0<6:.6c. 1ie5.4A5C6. 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) 0f\.0r\5cr0\ 0.056 0.064 0.055 0.045 0.041 13- Conipany Sanitized. Does not contain 7SCA CB) H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 TABLE 2 (Continued) MEAN BODY AND LIVER WEIGHTS (g) Test Days 5 c 10 13 24 52 94 H-24020 (POSITIVE CONTROL) __B_o_d_y_W_e_igAhbt_s_o_l_uLtivee_r_W_e_ig_h_t __ ^2A4 4^ . 8o 1i i7.f0\5e ^2 284.4 21.944 289.1 21.780 370.3 20.619 456.7 17.713 538.7 18.205 Mean Relative Liver Weight(% of Body Weight) 0f\.0f\7if0\ 0.077 0.075 0.056 0.039 0.034 Test Days 5 10 13 24 52 94 H-24002 (TEST SUBSTANCE) __B_o_d_y_W_e_i_gAhtb_s__o_lLuitvee_r _W_e_ig_h_t __ 266.5 13.716 308.1 15.379 322.1 15.490 371.9 16.724 532.7 19.962 593.9 20.154 Mean Relative Liver Weight(% of Body Weight) 0.051 0.050 0.048 0.045 0.037 0.034 -14- Company Sanitized. Does not contain TSCA CBI H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 TABLE 2 MEAN LIVER FLUORINE LEVELS Negative Controls Positive Controls Test Substance Corn Test Corn Oil Oil:Acetone H-24019 H-24020 H-24002 ""LO<02<0.5328.18 Days (ppm)_____(ppm)_______(ppm)____(ppm)_______(ppm) (19.3)13155.76 (29.2)125.4 (16.3) 94 0.6"______1"______77.56 (10.1) 1.68 (0.3) 3.0 (1.19) a One value. Four of the values were below the level of detection (LOD). b Standard deviation is in parentheses. TABLE 3 MEAN LIVER FLUORINE CONCENTRATION NORMALIZED TO DOSE Test Days 10 94 Positive Controls Test Substance H-24019 H-24020 H-24002 JU.MF Equivalents 5045.85 (296.91)' iiM F Equivalents____juM F Equivalents 1127.25 (211.37) 696.43 (90.76) 1190.15 (156.05) 10.72 (2.14)______15.58 (6.61) a Standard deviation is in parentheses. -15- .CpmpanySanitized. Does not contain TSCA CB1 H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 FIGURES - 16- Company Sanitized. Does not contain TSCA CBi )-- H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats FIGURE 1 COMPARISON OF MEAN RELATIVE LIVER WEIGHTS: TEST SUBSTANCE AND NEGATIVE CONTROLS 0.06 0.05 0.04 i:- & U 0 BS .0 0,03 0.02 0.01 0.00 Test Day -17- H-24002: 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- H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats FIGURES COMPARISON OF RELATIVE LIVER WEIGHT AND MEAN UVER FLUORINE CONCENTRA FOR H-24002 AND NEGATIVE CONTROLS Day 10 Day 13 Day 94 Day 10 II Corn Oil (Negative Control) Corn Oil:Acetone (Negative Control) D H-24002 (Test Substance) -19- H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats FIGURE 4 MEAN LIVER FLUORINE CONCENTRATION NORMALIZED TO DOSE 6000 5000 4000 s 3000 2000 1000 Day 10 Day 94 -20- H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats FIGURE 5 COMPARISON OF MEAN BLOOD AND MEAN LIVER FLUORINE CONCENTRATION NORMALIZE Blood / Liver Blood / Liver -21- Blood / Liver H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 APPENDICES -22- Company Sanrdzed. Does not contain TSCA CBf H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 APPENDIX A Individual Final Body Weights, Liver Weights, and Relative Liver to Body Weight -23- Company Sanitized. Does not contain TSCA CBl H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 CORN OIL (NEGATIVE (20NTROL) INDI\^IDUAL FINAL BODY WEIGHTS (g), LIVER WEIGHTS (g ) , AND RELATIVE LI\n3R TO BODY WEIG;HT OF MALE RATS Animal Number 627789 627801 627805 627810 627818 Final Body Wt. 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 contain TSCA CBi H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 0 ORN OIL (NEGATIVE; <CONTROL) INDIVIDUAL FINAL BODY WEIGHTS (g), LIVER WEIGHTS (g) ' AND RELATIVE LIVER TO BODY WEIG;HT 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 not contain TSCA CBH H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 CORN <3IL:ACETONE (NEGAT IVE CONTROL) INDIVIDUAL FINAL BODY WEIGHTS (g), LIVER WEIGHTS (g) l AND RELATIVE LIVER TO BODY WEIGHT OP 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 Live:r 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 CB' H-24002; Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 CORN lOIL:ACETONE (NEGAT:IVE CONTROL) INDIVIDUAL FINAL BODY WEIGHTS (g), LIVER WEIGHTS (g) / AND RELATIVE LIVER TO BODY WEIGHT 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 Live:r 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 Live:r to Body Wt. 0.033 0.034 0.030 0.032 0.035 Test Day 94 94 94 94 94 -27- Company Sanitized. Does not contain TSCA CBF H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 H-24 019 (POSITIVE (:ONTROL) INDIVI DUAL FINAL BOI3Y WEIGHTS (g), LIVER WEIGHTS (g ) , AND RELATIVE LIV ER TO BODY WEK3HT 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 CBf H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 H-241019 (POSITIVE CONTROL) INDIV?IDUAL FINAL BODY WEIGHTS (g) , LIVER WEIGHTS (g ) , AND RELATIVE LI\rER 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 Final Body Wt. 447.4 498.1 427.4 426.5 391.0 GROUP V Liver Wfc. 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 CBf H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 H-241020 (POSITIVE (:ONTROL) INDI\riDUAL FINAL BODY WEIGHTS (g), LIVER WEIGHTS (g ) , AND RELATIVE LI\FER TO BODY WEK3HT 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 SanRlzed. Does not contain T8CA CBi> H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 H-2'1020 (POSITIVE CONTROL) INDI\riDUKL FINAL BODY WEIGHTS (g),, LIVER WEIGHTS (gr), AND RELATIVE Ll\/ER TO BODY WEI 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- Company Sanitized. Does not contain TSCA CB1 H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 H-:24002 (TEST SUB;STANCE) IND][VIDUAL FINAL BO DY WEIGHTS (g), LIVER WEIGHTS (g ) , AND RELATIVE L^/ER TO BODY WEK3HT OF MALE RATS Animal Number 628192 628195 628207 628211 628212 Final Body Wt. 251.3 279.5 269.9 250.9 281.1 GROUP I Liver Wfc. 13.034 14.705 14.429 12.800 13.611 Relative Liver to Body Wt. 0.052 0.053 0.053 0.051 0.048 Test Day 5 5 5 5 5 Animal Number 628187 628188 628199 628209 628217 Final Body Wt. 314.4 328.1 315.3 299.3 283.4 GROUP II Liver Wt. 14.111 16.885 16.606 15.575 13.716 Relative Liver to Body Wt. 0.045 0.051 0.053 0.052 0.048 Test Day 10 10 10 10 10 Animal Number 628190 628202 628204 628206 628214 Final Body Wt. 314.2 318.6 361.0 320.0 296.9 GROUP III Liver Wt. 14.735 16.595 18.015 15.690 12.414 Relative Liver to Body Wt. 0.047 0.052 0.050 0.049 0.042 Test Day 13 13 13 13 13 -32- jCpmpanySanHIzed. Does not contain TSCA CB H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 H-;'4002 (TEST SUBSTANCE) INDIVI DUAL FINAL BODY WEIGHTS (g),, LIVER WEIGHTS (g ) , AND RELATIVE LI\TER TO BODY WE I GHT OF MALE RATS Animal Number 628197 628198 628201 628203 628216 Final Body Wt. 345.6 378.8 362.8 423.4 348.9 GROUP IV Liver Wt. 13.523 18.369 15.533 20.489 15.704 Relative Liver to Body Wt. 0.039 0.048 0.043 0.048 0.045 Test Day 24 24 24 24 24 Animal Number 628191 628196 628208 628210 628215 Final Body Wt. 498.3 565.9 543.3 542.0 514.0 GROUP V Liver Wt. 17.776 21.754 20.901 20.735 18.644 Relative Liver to Body Wt. 0.036 0.038 0.038 0.038 0.036 Test Day 52 52 52 52 52 Animal Number 628194 628200 628213 628218 628219 Final Body Wt. 578.2 556.4 609.7 633.8 591.2 GROUP VI Liver Wt. 21.190 16.602 21.672 22.255 19.050 Relative Liver to Body Wt. 0.037 0.030 0.036 0.035 0.032 Test Day 94 94 94 94 94 ^ -33- :Companf Sanitized. Does net contain TSCA CBI H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 APPENDIX B Individual Fluorine Levels -34. Company Sanitized. Does not contain TSCA CBI H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 Terms: Active % Active Mol Wt Active Formulation Dose % F in Active Mol Wt F TERMS AND CALCULATIONS Fluorine containing compound The % of formulation that is made up of fluorine containing components The molecular weight of the fluorine containing components (g/mole) The mg of formulation given per kg of animal body weight The % fluorine in the fluorine containing components of the formulation (weight basis) The molecular weight of fluorine g/mol 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 [mmbl/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- Company Sanitized. Does not contain T8CA CBI H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats DuPont-2926 Supplement No. 1 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/kgDose 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 blood minus background) ju,molar equivalents of active in liver The ^.molar [^mol/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 ^mol/mmol -36- Company Sanitized. Does not contain TSCA CR 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- Company Sanitized. Does not contain TSCA CP H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats Data for H- 24019 DuPont-2926 Supplement No. 1 Given: Mol Wt. Active (g/mole): 497 Formulation Dose (mg/kg): 10 % Active (F Containing) in Formulation: 100 %F in Aictive: 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 10 319.4 625330 10 355.4 625332 10 338.4 625341 10 305.0 625350 10 322.7 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 79.6 89.4 73.6 62.3 81.9 ppm F in Liver Normalized to 0.1 mmoles/kg Dose 1586.42 1765.34 1680.85 1514.86 1602.83 395.61 444.32 365.79 309.63 407.04 /imolar Equivalents of Active in Liver 4910.77 5464.62 5203.08 4689.23 4961.54 1224.62 1375.38 1132.31 958.46 1260.00 -38- jCompany Sanitized. Does not contain TSCA C91 H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats Data for H- 24020 DuPont-2926 Supplement No. 1 Given: Mol Wt. Active (g/mole): 426 Formulation Dose (mg/kg): 20 % Active (F Containing) in Formulation: 100 %F in Act ive: 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 627774 10 627776 10 627782 10 627785 10 182.5 109.0 174.0 147.5 165.8 Group VI 627778 94 1.9 627783 94 1.2 627762 94 1.9 627775 94 1.6 627769 94 1.8 ppm F in Liver Minus Bkg 0.2 ppm 182.3 108.8 173.8 147.3 165.6 1.7 1.0 1.7 1.4 1.6 ppm F in Liver Normalized to 0.1 mmoles/kg Dose 388.30 231.74 370.19 313.75 352.73 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 12.32 7.25 12.32 10.14 11.59 -39 H-24002: Biopersistence Screening 10-Dose Oral Gavage Study in Rats Data for H-24002 DuPont-2926 Supplement No. 1 Given: Mol Wt. Active (g/mole): 570 Formulation Dose (mg/kg): 75 % Active (F Containing) in Formulation: 47 % Fin Active: 51 Mol Wt. F (g/mol): 19 Calculated Values: Dose Active (mg/kg): Dose Active (mmole/kg): Formulation Dose Normalization Factor: 35.25 0.062 121.3 Dose F (mmol/kg): 0.946 Molar Ratio (Active/F): 0.065 Dose F (mg/kg):_____17.9775 Rat Number Test Day Sample ppmF in Liver Group II 628209 10 628187 10 628199 10 628188 10 628217 10 99.6 128.5 123.4 131.4 144.1 Group VI 628218 94 5.1 628213 94 2.3 628194 94 2.3 628200 94 2.6 628219 94 2.7 ppm F in Liver Minus Bkg 0.2 ppm 99.4 128.3 123.2 131.2 143.9 4.9 2.1 2.1 2.4 2.5 ppm F in L iver Normalize*ito 0.1 mmoles/kg Dose 160.73 207.46 199.22 212.15 232.69 7.92 3.40 3.40 3.88 4.04 /imolar Equivalents of Active in Liver 552.91 713.67 685.30 729.80 800.45 27.26 11.68 11.68 13.35 13.91 40- .CompanySanitized. Does not contain TSCA fw