A EPA EPA/635/R-22/277Fb www.epa.gov/iris IRIS Toxicological Review of Perfluorobutanoic Acid (PFBA, CASRN 375- 22-4) and Related Salts Supplemental Information—Appendices A through F December 2022 Integrated Risk Information System Center for Public Health and Environmental Assessment Office of Research and Development U.S. Environmental Protection Agency Washington, DC ------- Supplemental Information ofPFBA and Related Salts DISCLAIMER This document has been reviewed by the U.S. Environmental Protection Agency, Office of Research and Development and approved for publication. Any mention of trade names, products, or services does not imply an endorsement by the U.S. government or the U.S. Environmental Protection Agency. EPA does not endorse any commercial products, services, or enterprises. ii ------- Supplemental Information ofPFBA and Related Salts CONTENTS APPENDIX A. SYSTEMATIC REVIEW PROTOCOL FOR THE PFAS IRIS ASSESSMENTS A-l APPENDIX B. ADDITIONAL DETAILS OF SYSTEMATIC REVIEW METHODS AND RESULTS B-l APPENDIX C. ADDITIONAL TOXICOKINETIC INFORMATION IN SUPPORT OF DOSE-RESPONSE ANALYSIS C-l C.l. USE OF HALF-LIVES OF EXCRETION FOR DOSIMETRIC ADJUSTMENTS C-l C.2. MIXED MODELING TO ESTIMATE HALF-LIFE IN HUMANS C-7 APPENDIX D. BENCHMARK DOSE MODELING RESULTS D-l D.l. BENCHMARK DOSE MODELING APPROACHES D-l D.l.l. Modeling Procedure for Dichotomous Noncancer Data D-l D.l.2. Modeling Procedure for Continuous Noncancer Data D-l D.l.3. Modeling Procedure for Continuous Noncancer Developmental Toxicity Data D-3 D.1.4. Modeling Procedure for Dichotomous Noncancer Developmental Toxicity Data D-3 D.l.5. Data Used for Modeling D-3 D.2. RELATIVE LIVER WEIGHT—MALE RATS EXPOSED 90 DAYS (Butenhoff et al., 2012; van Otterdijk, 2007b) D-14 D.3. RELATIVE LIVER WEIGHT—P0 MICE (Das et al., 2008) D-23 D.4. LIVER HYPERTROPHY—MALE RAT (Butenhoff et al., 2012; van Otterdijk, 2007b) D-29 D.5. TOTAL T4—MALE RAT (Butenhoff et al., 2012; van Otterdijk, 2007b) D-32 D.6. INCREASED FETAL MORTALITY - MALE AND FEMALE Fi MICE (Das et al., 2008) D-36 D.7. DELAYED EYE OPENING—Fi MALE AND FEMALE MICE (Das et al., 2008) D-43 D.8. VAGINAL OPENING—Fi FEMALE MICE (Das et al., 2008) D-49 D.9. PREPUTIAL SEPARATION—Fi MALE MICE (Das et al., 2008) D-54 D.10. RELATIVE LIVER WEIGHT—MALE HUMANIZED PPARa MICE (Foreman et al., 2009) D-58 D.ll. RELATIVE LIVER WEIGHT—MALE RATS EXPOSED 28 DAYS (Butenhoff et al., 2012; van Otterdijk, 2007b) D-61 APPENDIX E. SUMMARY OF PUBLIC AND EXTERNAL PEER REVIEW COMMENTS AND EPA'S DISPOSITION E-l E.l. CHARGE QUESTION 1 - SYSTEMATIC REVIEW E-2 E.l.l. Overarching External Peer Reviewer Comments on Systematic Review E-2 E.l.2. Tier 1 Recommendations E-3 iii ------- Supplemental Information ofPFBA and Related Salts E.1.3. Tier 2 Suggestions E-4 E.1.4. Public Comments E-7 E.2. CHARGE QUESTION 2 - STUDY EVALUATION E-8 E.2.1. Overarching External Peer Reviewer Comments on Study Evaluation E-9 E.2.2. Tier 1 Recommendations E-9 E.2.3. Tier 2 Suggestions E-9 E.3. CHARGE QUESTIONS 3 AND 4 - HEPATIC EFFECTS E-ll E.3.1. Overarching External Peer Reviewer Comments on Hepatic Effects E-ll E.3.2. Tier 1 Recommendations E-ll E.3.3. Tier 2 Suggestions E-ll E.3.4. Public Comments E-15 E.4. CHARGE QUESTION 3 - THYROID EFFECTS E-16 E.4.1. Overarching External Peer Reviewer Comments on Thyroid Effects E-16 E.4.2. Tier 1 Recommendations E-17 E.4.3. Tier 2 Suggestions E-18 E.4.4. Public Comments E-20 E.5. CHARGE QUESTION 3 - DEVELOPMENTAL EFFECTS E-21 E.5.1. Overarching External Peer Reviewer Comments on Developmental Effects E-21 E.5.2. Tier 1 Recommendations E-22 E.5.3. Tier 2 Suggestions E-23 E.5.4. Public Comments E-24 E.6. CHARGE QUESTION 3 - REPRODUCTIVE AND OTHER EFFECTS E-25 E.6.1. Overarching External Peer Reviewer Comments on Reproductive and Other Effects E-25 E.6.2. Tier 1 Recommendations E-25 E.6.3. Tier 2 Suggestions E-25 E.7. CHARGE QUESTION 5 - CANCER HAZARD E-26 E.7.1. Overarching External Peer Reviewer Comments on Cancer Hazard E-26 E.7.2. Tier 1 Recommendations E-26 E.7.3. Tier 2 Suggestions E-27 E.8. CHARGE QUESTION 6 - NONCANCER TOXICITY VALUE DATA SELECTION E-27 E.8.1. Overarching External Peer Reviewer Comments on Noncancer Toxicity Value Data Selection E-27 E.8.2. Tier 1 Recommendations E-27 iv ------- Supplemental Information ofPFBA and Related Salts E.8.3. Tier 2 Suggestions E-28 E.8.4. Public Comments E-28 E.9. CHARGE QUESTION 7 - SUBCHRONIC REFERENCE DOSE E-29 E.9.1. Overarching External Peer Reviewer Comments on the Subchronic Reference Dose E-30 E.9.2. Tier 1 Recommendations E-30 E.9.3. Tier 2 Suggestions E-32 E.10. CHARGE QUESTION 8 - NONCANCER TOXICITY VALUE DOSE-RESPONSE MODELING E-32 E.10.1. Overarching External Peer Reviewer Comments on Noncancer Toxicity Value Dose-Response Modeling E-33 E.10.2. Tier 1 Recommendations E-33 E.10.3. Tier 2 Suggestions E-33 E.ll. CHARGE QUESTION 9 - TOXICOKINETICS E-34 E.ll.l. Overarching External Peer Reviewer Comments on Toxicokinetics E-34 E.ll.2. Tier 1 Recommendations E-34 E.ll.3. Tier 2 Suggestions E-35 E.11.4. Public Comments E-37 E.12. CHARGE QUESTION 10 - UNCERTAINTY FACTOR APPLICATION E-40 E.12.1. Tier 1 Recommendations E-40 E.12.2. Tier 2 Suggestions E-40 E.12.3. Public Comments E-42 E.13. CHARGE QUESTION 11 - CANCER TOXICITY VALUES E-44 E.13.1. Overarching External Peer Reviewer Comments on Cancer Toxicity Values E-44 E.13.2. Tier 1 Recommendations E-44 E.13.3. Tier 2 Suggestions E-44 APPENDIX F. QUALITY ASSURANCE FOR THE IRIS TOXICOLOGICAL REVIEW OF PERFLUOROBUTANOIC ACID AND RELATED COMPOUND AMMONIUM PERFLUOROBUTANOATE F-l REFERENCES R-l v ------- Supplemental Information ofPFBA and Related Salts TABLES Table B-l. Perfluorobutanoic acid (PFBA) database search strategy B-l Table B-2. Title/abstract-level screening criteria for the initial literature searches B-4 Table B-3. Example DistillerSR form questions to be used for title/abstract-level and full text-level screening for literature search updates from 2019 B-6 Table D-l. Sources of data used in benchmark dose modeling of PFBA endpoints D-3 Table D-2. Data received from study authors for Das et al. (2008) on full litter resorptions (FLR) D-3 Table D-3. Data received from study authors for Das et al. (2008) on fetal death (litters without full litter resorptions) combined with full litter resorptions D-4 Table D-4. Data received from study authors for Das et al. (2008)on delayed eye opening D-4 Table D-5. Data received from study authors for Das et al. (2008) on delayed vaginal opening D-7 Table D-6. Data received from study authors for Das et al. (2008) on delayed preputial separation D-12 Table D-7. Dose-response data for relative liver weight in male rats following 90 day exposure (Butenhoff et al., 2012; van Otterdijk, 2007b) D-14 Table D-8. Benchmark dose results for relative liver weight in male rats exposed 90 days —constant variance, BMR = 10% relative deviation (Butenhoff et al., 2012; van Otterdijk, 2007b) D-15 Table D-9. Benchmark dose results for relative liver weight in male rats exposed 90 days—nonconstant variance, BMR = 10% relative deviation (Butenhoff et al., 2012; van Otterdijk, 2007b) D-17 Table D-10. Benchmark dose results for relative liver weight in male rats exposed 90 days—log-normal distribution, constant variance, BMR = 10% relative deviation (Butenhoff et al., 2012; van Otterdijk, 2007b) D-18 Table D-ll. Benchmark dose results for relative liver weight in male rats exposed 90 days—log-normal distribution, constant variance, BMR = 1 standard deviation (Butenhoff et al., 2012; van Otterdijk, 2007b) D-22 Table D-12. Dose-response data for relative liver weight in pregnant mice (Das et al., 2008) D-23 Table D-13. Benchmark dose results for relative liver weight in pregnant mice—constant variance, BMR = 10% relative deviation (Das et al., 2008) D-24 Table D-14. Benchmark dose results for relative liver weight in pregnant mice—constant variance, BMR = 1 standard deviation (Das et al., 2008) D-28 Table D-15. Dose-response data liver hypertrophy in male rats (Butenhoff et al., 2012; van Otterdijk, 2007b) D-29 Table D-16. Benchmark dose results for liver hypertrophy in rats—BMR = 10% extra risk (Butenhoff et al., 2012; van Otterdijk, 2007b) D-29 Table D-17. Dose-response data for liver hypertrophy (slight severity lesions) in male rats (Butenhoff et al., 2012; van Otterdijk, 2007b) D-32 Table D-18. Benchmark dose results for liver hypertrophy (slight severity lesions) in male rats—BMR = 10% extra risk (Butenhoff et al., 2012; van Otterdijk, 2007b) D-32 Table D-19. Dose-response data for total T4 levels in male rats (Butenhoff et al., 2012; van Otterdijk, 2007b) D-32 Table D-20. Benchmark dose results for total T4 levels in male rats—constant variance, BMR = 1 standard deviation (Butenhoff et al., 2012; van Otterdijk, 2007b) D-33 Table D-21. Benchmark dose results for total T4 levels in male rats—nonconstant variance, BMR = 1 standard deviation (Butenhoff et al., 2012; van Otterdijk, 2007b) D-34 vi ------- Supplemental Information ofPFBA and Related Salts Table D-22. Benchmark dose results for total T4 levels in male rats—log-normal distribution, constant variance, BMR = 1 standard deviation (Butenhoff et al., 2012; van Otterdijk, 2007b) D-35 Table D-23. Dose-response data for increased fetal mortality (Das et al., 2008) D-36 Table D-24. Benchmark dose results for increased fetal mortality (male and female mice)—BMR = 1% extra risk (Das et al., 2008) D-38 Table D-25. Dose-response data for delayed eye opening in male and female mice (Das et al., 2008) D-43 Table D-26. Benchmark dose results for delayed eye opening in male and female mice—constant variance, BMR = 5% relative deviation (Das et al., 2008) D-44 Table D-27. Benchmark dose results for delayed eye opening in male and female mice—constant variance, BMR = 1 standard deviation (Das et al., 2008) D-48 Table D-28. Dose response data for delayed vaginal opening in female mice (Das et al., 2008) D-49 Table D-29. Benchmark dose results for delayed vaginal opening in female mice—constant variance, 5% relative deviation (Das et al., 2008) D-49 Table D-30. Benchmark dose results for delayed vaginal opening in female mice—constant variance, 1 standard deviation (Das et al., 2008) D-53 Table D-31. Dose-response data for delayed preputial separation in male mice (Das et al., 2008) D-54 Table D-32. Benchmark dose results for delayed preputial separation in male mice—constant variance, BMR = 5% relative deviation (Das et al., 2008) D-54 Table D-33. Benchmark dose results for delayed preputial separation in male mice—constant variance, BMR = 1 standard deviation (Das et al., 2008) D-58 Table D-34. Dose-response data for relative liver weight in male humanized PPARa mice (Foreman et al., 2009) D-58 Table D-35. Benchmark dose results for relative liver weight in male humanized PPARa mice —nonconstant variance, BMR = 10% relative deviation (Foreman et al., 2009) D-59 Table D-36. Dose-response data for relative liver weight in male rats following 28 day exposure (Butenhoff et al., 2012; van Otterdijk, 2007b) D-61 Table D-37. Benchmark dose results for relative liver weight in male rats exposed 28 days —nonconstant variance, BMR = 10% relative deviation (Butenhoff et al., 2012; van Otterdijk, 2007b) D-61 FIGURES Figure C-l. Mouse AUC after oral doses of PFBA C-l Figure C-2. Mouse Cmax after oral doses of PFBA C-2 Figure C-3. Rat AUC after oral doses of PFBA C-3 Figure C-4. Rat Cmax after oral doses of PFBA C-4 Figure C-5. Estimated human half-lives versus initial serum concentrations C-5 Figure D-l. Dose-response curve for the Exponential M3 model fit to relative liver weight in male rats exposed 90 days (Butenhoff et al., 2012; van Otterdijk, 2007b) D-19 Figure D-2. Dose-response curve for the Exponential M4 model fit to relative liver weight in pregnant mice (Das et al., 2008) D-25 Figure D-3. Dose-response curve for the Weibull model fit to liver hypertrophy in male rats (Butenhoff et al., 2012; van Otterdijk, 2007b) D-30 ------- Supplemental Information ofPFBA and Related Salts Figure D-4. Dose-response curve for the Nested-Logistic model fit to increased fetal mortality in male and female mice (Das et al., 2008) D-39 Figure D-5. Dose response curve for the Hill model fit to delayed eye opening in male and female mice (Das et al., 2008) D-45 Figure D-6. Dose response curve for the Hill model fit to delayed vaginal opening in female mice (Das et al., 2008) D-50 Figure D-7. Dose response curve for the Exponential 3 model fit to delayed preputial separation in male mice (Das et al., 2008) D-55 viii ------- Supplemental Information ofPFBA and Related Salts ABBREVIATIONS AND ACRONYMS ACO acyl-CoA oxidase HAWC Health Assessment Workspace ADME absorption, distribution, metabolism, Collaborative and excretion HED human equivalent dose AFFF aqueous film-forming foam HERO Health and Environmental Research AIC Akaike's information criterion Online ALP alkaline phosphatase HISA highly influential scientific information ALT alanine aminotransferase HPT hypothalamic-pituitary-thyroid AST aspartate aminotransferase IRIS Integrated Risk Information System atm atmosphere i.v. intravenous ATSDR Agency for Toxic Substances and IQ intelligence quotient Disease Registry IQR interquartile range AUC area-under-the-concentration curve ISI influential scientific information BMD benchmark dose IUR inhalation unit risk BMDL benchmark dose lower confidence limit LLOQ lower limit of quantitation BMDS Benchmark Dose Software LN log-normal BMR benchmark response LOAEL lowest-observed-adverse-effect level BW body weight MBq megabecquerel Cavg average concentration MOA mode of action Cmax maximum concentration NCEA National Center for Environmental CA Cochran-Armitage Assessment CAR constitutive androstane receptor NCV nonconstant variance CASRN Chemical Abstracts Service registry NIOSH National Institute for Occupational number Safety and Health CDR Chemical Data Reporting NIS sodium-iodide symporter CI confidence interval NOAEL no-observed-adverse-effect level CL clearance NPL National Priority List CLa clearance in animals NTP National Toxicology Program CLh clearance in humans OAT organic anion transporter CPAD Chemical and Pollutant Assessment OECD Organisation for Economic Co- Division operation and Development CPHEA Center for Public Health and OMB Office of Management and Budget Environmental Assessment ORD Office of Research and Development CV constant variance OSF oral slope factor CYP450 cytochrome P450 superfamily PC partition coefficient DAF dosimetric adjustment factor PBPK physiologically based pharmacokinetic DNA deoxyribonucleic acid PBTK physiologically based toxicokinetic DNT developmental neurotoxicity PECO Populations, Exposures, Comparators, DOD Department of Defense Outcomes EPA Environmental Protection Agency PFAA perfluoroalkyl acid EOP Executive Office of the President PFAS per- and polyfluoroalkyl substances ER extra risk PFBA perfluorobutanoic acid FLR full-litter resorption PFBS perfluorobutane sulfonate FTOH fluorotelomer alcohol PFCA perfluoroalkyl carboxylic acid GD gestation day PFDA perfluorodecanoic acid GFR glomerular filtration rate PFHxA perfluorohexanoic acid GGT y-glutamyl transferase PFHxS perfluorohexane sulfonate GRADE Grading of Recommendations PFNA perfluorononanoic acid Assessment, Development, and PFOA perfluorooctanoic acid Evaluation PFOS perfluorooctane sulfonate GSH glutathione PK pharmacokinetic PND postnatal day ix ------- Supplemental Information ofPFBA and Related Salts POD point of departure TRI Toxic Release Inventory PODhed human equivalent dose POD TSCA Toxic Substances Control Act PPAR peroxisome proliferator-activated TSCATS Toxic Substances Control Act Test receptor Submissions PQAPP Programmatic Quality Assurance TSH thyroid-stimulating hormone Project Plan TSHR thyroid-stimulating hormone receptor PT prothrombin time UCMR Unregulated Contaminant Monitoring PXR pregnane X receptor Rule QA quality assurance UDP-GT uridine 5'-diphospho- QAPP Quality Assurance Project Plan glucuronosyltransferase QMP Quality Management Plan UF uncertainty factor RBC red blood cell UFa animal-to-human uncertainty factor RD relative deviation UFc composite uncertainty factor RfC inhalation reference concentration UFd database deficiencies uncertainty factor RfD oral reference dose UFh human variation uncertainty factor RS Rao-Scott UFl LOAEL-to-NOAEL uncertainty factor SD standard deviation UFs subchronic-to-chronic uncertainty S-D Sprague-Dawley factor SE standard error Vd volume of distribution TD toxicodynamic VOC volatile organic compound TH thyroid hormone WOS Web of Science TK toxicokinetic TPO thyroid peroxidase x ------- Supplemental Information ofPFBA and Related Salts APPENDIX A. SYSTEMATIC REVIEW PROTOCOL FOR THE PFAS IRIS ASSESSMENTS 1 A single systematic review protocol was used to guide the development of five, separate 2 IRIS PFAS assessments (i.e., PFBA, PFHxA, PFHxS, PFNA, and PFDA). This "systematic review 3 protocol for the PFAS IRIS assessments" was released for public comment and subsequently 4 amended. The amended protocol and prior revisions can be found at the following location: 5 http://cfpub.epa.gov/ncea/iris drafts/recordisplay.cfm?deid=345065. 6 When the assessment references a particular section or page number in Appendix A, please 7 refer to that section in the systematic review protocol linked above. A-l ------- Supplemental Information ofPFBA and Related Salts APPENDIX B. ADDITIONAL DETAILS OF SYSTEMATIC REVIEW METHODS AND RESULTS Table B-l. Perfluorobutanoic acid (PFBA) database search strategy Search Search strategy Dates of search3 PubMed Search terms 375-22-4[rn] OR "Heptafluoro-l-butanoic acid"[tw] OR "Heptafluorobutanoic acid"[tw] OR "Heptafluorobutyric acid"[tw] OR "Kyselina heptafluormaselna"[tw] OR "Perfluorobutanoic acid"[tw] OR "Perfluorobutyric acid"[tw] OR "Perfluoropropanecarboxylic acid"[tw] OR "2,2,3,3,4,4,4-heptafluoro-Butanoic acid"[tw] OR "Butanoic acid, 2,2,3,3,4,4,4-heptafluoro-"[tw] OR "Butanoic acid, heptafluoro-"[tw] OR "Perfluoro-n-butanoic acid"[tw] OR "Perfluorobutanoate"[tw] OR "2,2,3,3,4,4,4-Heptafluorobutanoic acid"[tw] OR "Butyric acid, heptafluoro-"[tw] OR "Fluorad FC 23"[tw] OR "H 0024"[tw] OR "NSC 820"[tw] OR «PFBA[tw] OR "FC 23"[tw] OR HFBA[tw]) AND (fluorocarbon*[tw] OR fluorotelomer*[tw] OR polyfluoro*[tw] OR perfluoro-*[tw] OR perfluoroa*[tw] OR perfluorob*[tw] OR perfluoroc*[tw] OR perfluorod*[tw] OR perfluoroe*[tw] OR perfluoroh*[tw] OR perfluoron*[tw] OR perfluoroo*[tw] OR perfluorop*[tw] OR perfluoros*[tw] OR perfluorou*[tw] OR perfluorinated[tw] OR fluorinated[tw] OR PFAS[tw] OR PFOS[tw] OR PFOA[tw])) No date limit—7/19/2017 Literature update search terms (((375-22-4[rn] OR "Heptafluoro-l-butanoic acid"[tw] OR "Heptafluorobutanoic acid"[tw] OR "Heptafluorobutyric acid"[tw] OR "Kyselina heptafluormaselna"[tw] OR "Perfluorobutanoic acid"[tw] OR "Perfluorobutyric acid"[tw] OR "Perfluoropropanecarboxylic acid"[tw] OR "2,2,3,3,4,4,4-heptafluoro-Butanoic acid"[tw] OR "Butanoic acid, 2,2,3,3,4,4,4-heptafluoro-"[tw] OR "Butanoic acid, heptafluoro-"[tw] OR "Perfluoro-n-butanoic acid"[tw] OR "Perfluorobutanoate"[tw] OR "2,2,3,3,4,4,4-Heptafluorobutanoic acid"[tw] OR "Butyric acid, heptafluoro-"[tw] OR "Fluorad FC 23"[tw] OR "H 0024"[tw] OR "NSC 820"[tw] OR «PFBA[tw] OR "FC 23"[tw] OR HFBA[tw]) AND (fluorocarbon*[tw] OR fluorotelomer*[tw] OR polyfluoro*[tw] OR perfluoro-*[tw] OR perfluoroa*[tw] OR perfluorob*[tw] OR perfluoroc*[tw] OR perfluorod*[tw] OR perfluoroe*[tw] OR perfluoroh*[tw] OR perfluoron*[tw] OR perfluoroo*[tw] OR perfluorop*[tw] OR perfluoros*[tw] OR perfluorou*[tw] OR perfluorinated[tw] OR fluorinated[tw] OR PFAS[tw] OR PFOS[tw] OR PFOA[tw])) AND ("2017/08/01"[PDAT] : "2018/02/14"[PDAT]) 8/1/2017-2/14/2018 B-l ------- Supplemental Information ofPFBA and Related Salts Search Search strategy Dates of search3 Web of Science Search terms TS="Heptafluoro-l-butanoic acid" OR TS="Heptafluorobutanoic acid" OR TS="Heptafluorobutyric acid" ORTS="Kyselina heptafluormaselna" OR TS="Perfluorobutanoic acid" OR TS="Perfluorobutyric acid" OR TS="Perfluoropropanecarboxylic acid" OR TS="2,2,3,3,4,4,4-heptafluoro-Butanoic acid" OR TS="Butanoic acid, 2,2,3,3,4,4,4-heptafluoro-" ORTS="Butanoicacid, heptafluoro-" OR TS="Perfluoro-n-butanoic acid" ORTS="Perfluorobutanoate" OR TS="2,2,3,3,4,4,4-Heptafluorobutanoic acid" OR TS="Butyric acid, heptafluoro-" ORTS="Fluorad FC 23" ORTS="H 0024" ORTS="NSC 820" OR (TS=(PFBA OR "FC 23" OR HFBA) AND TS=(fluorocarbon* OR fluorotelomer* OR polyfluoro* OR perfluoro-* OR perfluoroa* OR perfluorob* OR perfluoroc* OR perfluorod* OR perfluoroe* OR perfluoroh* OR perfluoron* OR perfluoroo* OR perfluorop* OR perfluoros* OR perfluorou* OR perfluorinated OR fluorinated OR PFAS OR PFOS OR PFOA)) No date limit-7/20/2017 Literature update search terms ((TS="Heptafluoro-l-butanoic acid" OR TS="Heptafluorobutanoic acid" OR TS="Heptafluorobutyric acid" ORTS="Kyselina heptafluormaselna" OR TS="Perfluorobutanoic acid" OR TS="Perfluorobutyric acid" OR TS="Perfluoropropanecarboxylic acid" OR TS="2,2,3,3,4,4,4-heptafluoro-Butanoic acid" OR TS="Butanoic acid, 2,2,3,3,4,4,4-heptafluoro-" ORTS="Butanoicacid, heptafluoro-" OR TS="Perfluoro-n-butanoic acid" ORTS="Perfluorobutanoate" OR TS="2,2,3,3,4,4,4-Heptafluorobutanoic acid" OR TS="Butyric acid, heptafluoro-" ORTS="Fluorad FC 23" ORTS="H 0024" ORTS="NSC 820") OR TS=(PFBA OR "FC 23" OR HFBA) AND TS=(fluorocarbon* OR fluorotelomer* OR polyfluoro* OR perfluoro-* OR perfluoroa* OR perfluorob* OR perfluoroc* OR perfluorod* OR perfluoroe* OR perfluoroh* OR perfluoron* OR perfluoroo* OR perfluorop* OR perfluoros* OR perfluorou* OR perfluorinated OR fluorinated OR PFAS OR PFOS OR PFOA)) AND PY=2017-2018 2017-2018 Toxline Search terms ( 375-22-4 [rn] OR "heptafluoro-l-butanoic acid" OR "heptafluorobutanoic acid" OR "heptafluorobutyric acid" OR "kyselina heptafluormaselna" OR "perfluorobutanoic acid" OR "perfluorobutyric acid" OR "perfluoropropanecarboxylic acid" OR "2,2,3,3,4,4,4-heptafluoro-butanoic acid" OR "butanoic acid 2 2 3 3 4 4 4-heptafluoro-" OR "butanoic acid heptafluoro-" OR "perfluoro-n-butanoic acid" OR "perfluorobutanoate" OR "2,2,3,3,4,4,4-heptafluorobutanoic acid" OR "butyric acid heptafluoro-" OR "fluorad fc 23" OR "h 0024" OR "nsc 820" OR (( pfba OR "fc 23" OR hfba ) AND (fluorocarbon* OR fluorotelomer* OR polyfluoro* OR perfluoro* OR perfluorinated OR fluorinated OR pfas OR pfos OR pfoa ))) AND (ANEUPL [org] OR BIOSIS [org] OR CIS [org] OR DART [org] OR EMIC [org] OR EPIDEM [org] OR HEEP [org] OR HMTC [org] OR IPA [org] OR RISKUNE [org] OR MTGABS [org] OR NIOSH [org] OR NTIS [org] OR PESTAB [org] OR PPBIB [org] ) AND NOT PubMed [org] AND NOT pubdart [org] No date limit-7/20/2017 B-2 ------- Supplemental Information ofPFBA and Related Salts Search Search strategy Dates of search3 Literature update search terms @AND+@OR+("heptafluoro-l-butanoic acid"+"heptafluorobutanoic+acid"+"heptafluorobutyric+acid"+"kyselina+hept afluormaselna"+"perfluorobutanoic+acid"+"perfluorobutyric+acid"+"perfluor opropanecarboxylic +acid"+"2 2 3 3 4 4 4-heptafluoro-butanoic+acid"+"butanoic+acid+2 2 3 3 4 4 4-heptafluoro-"+"butanoic+acid+heptafluoro-"+"perfluoro-n-butanoic acid"+"perfluorobutanoate"+"2 2 3 3 4 4 4-heptafluorobutanoic+acid"+"butyric+acid+heptafluoro-"+"fluorad+fc+23"+" h0024"+"nsc+820"+@TERM+@rn+375-22-4("pfba"+"fc+23"+"hfba"))+( fluorocarbon*+ fluorotelomer*+polyfluoro*+perfluoro*+perfluorinated+fluorinated+pfas+pfo s+pfoa)+@RANGE+yr+2017+2018 2017-2018 TSCATS Search terms 375-22-4[rn] AND tscats[org] No date limit-7/20/2017 a Yearly spring updates are conducted following release of the draft for public comment; see also the docket ("EPA-HQ-QRD-2020-0675-0022") for studies identified after the last formal update preceding public release. B-3 ------- Supplemental Information ofPFBA and Related Salts Table B-2. Title/abstract-level screening criteria for the initial literature searches Inclusion criteria Exclusion criteria Populations Humans Standard mammalian animal models, including rat, mouse, rabbit, guinea pig, hamster, monkey, dog Alternative animal models in standard laboratory conditions (e.g., Xenopus, zebrafish, minipig) Human or animal cells, tissues, or organs (not whole animals); bacteria, nonmammalian eukaryotes; other nonmammalian laboratory species Ecological species Exposures Exposure is to PFBA Study population is not exposed to PFBA Exposure via oral, inhalation, dermal, intraperitoneal, or intravenous injection routes Exposure is to a mixture only Exposure is measured in air, dust, drinking water, diet, gavage, injection or via a biomarker of exposure (PFBA levels in whole blood, serum, plasma, or breastmilk) Outcomes Studies that include a measure of one or more health effect endpoints, including but not limited to, effects on reproduction, development, developmental neurotoxicity, liver, thyroid, immune system, nervous system, genotoxicity, and cancer In vivo or in vitro studies related to toxicity mechanisms, physiological effects/adverse outcomes, and studies useful for elucidating toxic modes of action (MOAs) Qualitative or quantitative description of absorption, distribution, metabolism, excretion, toxicokinetic or toxicodynamic models (e.g., PBPK, PBTK, PBTK/TD) Studies addressing risks to infants, children, pregnant women, occupational workers, the elderly, and any other susceptible or differentially exposed populations B-4 ------- Supplemental Information ofPFBA and Related Salts Inclusion criteria Exclusion criteria Other Structure and physiochemical properties Reviews and regulatory documents Not on topic, including: Abstract only, inadequately reported abstract, or no abstract and not considered further because study was not potentially relevant Bioremediation, biodegradation, or chemical or physical treatment of PFBA, including evaluation of wastewater treatment technologies and methods for remediation of contaminated water and soil Ecosystem effects Studies of environmental fate and transport of PFBA in environmental media Analytical methods for detecting/measuring PFAS compounds in environmental media and use in sample preparations and assays Studies describing the manufacture and use of PFBA Not chemical specific (studies that do not involve testing of PFBA) Studies that describe measures of exposure to PFBA without data on associated health effects MOA = mode of action; PBPK = physiologically based pharmacokinetic; PBTK = physiologically based toxicokinetic; TD = toxicodynamic. B-5 ------- Supplemental Information ofPFBA and Related Salts Table B-3. Example DistillerSR form questions to be used for title/abstract-level and full text-level screening for literature search updates from 2019 Used in title/abstract and full-text screening Used in full text screening only Source of If meets PECO and study if not endocrine identified Does the If meets PECO, Which PFAS outcome, which from database article meet what type of If supplemental, what did the study If meets PECO, which endocrine tags Question search? PECO criteria? evidence? type of information? report? health outcome(s) apply? apply? Answer options (can select multiple options) Source other Yes Human In vivo mechanistic or PFBA General toxicity, including Adrenal than HERO No Unclear Tag as potentially relevant supplemental Animal (mam- malian models) In vitro or MOA studies, PFHxA PFHxS PFNA body weight, mortality, Sex hormones (e.g., androgen; estrogen; progesterone) database search including non-PECO routes of exposure (e.g., injection) and populations and survival Cancer Cardiovascular, including in silico genotoxicity (e.g., nonmammalian) In vitro or in silico PFDA serum lipids Endocrine (hormone) Neuroendocrine Pituitary information PBPKor PK model studies (nongenotoxicity) ADME/toxicokinetic (excluding models) Exposure assessment or characterization (no health outcome) PFAS mixture study (no individual PFAS comparisons) Gastrointestinal Genotoxicity Growth (early life) and development Hematological, including nonimmune/hepatic/ renal clinical chemistry measures Hepatic, including liver Steroidogenesis Thyroid Human case reports or case series measures and serum markers (e.g., ALT; AST) Ecotoxicity studies Immune/ inflammation B-6 ------- Supplemental Information ofPFBA and Related Salts Used in title/abstract and full-text screening Used in full text screening only Question Source of study if not identified from database search? Does the article meet PECO criteria? If meets PECO, what type of evidence? If supplemental, what type of information? Which PFAS did the study report? If meets PECO, which health outcome(s) apply? If meets PECO and endocrine outcome, which endocrine tags apply? Environmental fate or occurrence (including food) Manufacture, engineering, use, treatment, remediation, or laboratory methods Other assessments or records with no original data (e.g., reviews, editorials, commentaries) Musculoskeletal Nervous system, including behavior and sensory function Nutrition and metabolic Ocular PBPK or PK model Renal, including urinary measures (e.g., protein) Reproductive Respiratory Skin and connective tissue effects ADME = absorption, distribution, metabolism, and excretion; ALT = alanine aminotransferase; AST = aspartate aminotransferase; HERO = Health and Environmental Research Online; MOA = mode of action; PBPK = physiologically based pharmacokinetic; PECO = Populations, Exposures, Comparators, and Outcomes; PFAS = per- and polyfluoroalkyl substance; PFBA = perfluorobutanoic acid; PFDA = perfluorodecanoic acid; PFHxA = perfluorohexanoic acid; PFHxS = perfluorohexanesulfonate; PFNA = perfluorononanoic acid; PK = pharmacokinetic. B-7 ------- Supplemental Information ofPFBA and Related Salts APPENDIX C. ADDITIONAL TOXICOKINETIC INFORMATION IN SUPPORT OF DOSE-RESPONSE ANALYSIS C.l. USE OF HALF-LIVES OF EXCRETION FOR DOSIMETRIC ADJUSTMENTS The pharmacokinetics ofPFBA have only been measured after direct administration of PFBA in single-exposure/single-day studies in animals fChang etal.. 20081. For the mouse, Chang et al. f20081 performed 24-hour toxicokinetic studies after 10, 30, and 100 mg/kg oral doses. Based on the area-under-the-concentration-curve (AUC) and maximum concentration (Cmax), the data also appear approximately linear below 30 mg/kg but show some saturation above that dose rate (see Figure C-l, Figure C-2). 9000 SOOO 7000 6000 E i" 5000 4000 D < 3000 2000 1000 0 * Male + Fan ale 0 i + Mouse 24-h AUC after oral doses of } 20 40 60 Dose (mg/kg) SO 100 Figure C-l. Mouse AUC after oral doses of PFBA. C-l ------- Supplemental Information ofPFBA and Related Salts 350 300 250 •|2t>0 | 150 u • Male + Fa^iale 100 5 I Mouse Cmax after oral doses of PFBA } } 50 0 0 20 40 60 Dose (mg/kg) SO 100 Figure C-2. Mouse Cmax after oral doses of PFBA. Chang etal. f20081 reported serum and liver concentrations in male rats and serum concentrations in female rats given a 3-300 mg/kg oral dose ofPFBA at 24 hours after dosing. Although the time point for these measurements is not ideal given the short half-life of PFBA, the data indicate that the dosimetry is approximately linear up to 100 mg/kg in male rats and up to 30 mg/kg in female rats (see Figure C-3, Figure C-4). Tissue levels then appear to saturate or decline; this might be due to incomplete absorption at higher doses, saturable renal resorption, or both, whereby excretion is more rapid for concentrations above the level of saturable resorption in the kidney. With the half-life in female rats being ~3 hours, the female serum 24-hour data are particularly subject to experimental noise, but at least provide an indication that use of the half-life measured using a 30 mg/kg dose is applicable to BMD levels from bioassays at or below this dose rate. C-2 ------- Supplemental Information ofPFBA and Related Salts 72 to 60 ° 48 E 36 s o £ 24 c OJ u 312 • Serum + Lr/er I i 0 * 0 ¦i x 5 Male rat tissue concentrations 24 h after an oral dose of PFBA 50 100 150 200 Dose (mg/kg) 250 300 Figure C-3. Rat AUC after oral doses of PFBA. C-3 ------- Supplemental Information ofPFBA and Related Salts E 1 e o % ai 0.4 0.35 0.3 0.25 0.2 0.15 o 0.1 0.05 0 Female rat serum concentration 24 h after j an oral dose of PFBA i L ! -1 « r - * 0 50 100 150 200 Dose (mg/kg) 250 300 Figure C-4. Rat Cmax after oral doses of PFBA. For the human data analyzed by Chang et al. f2008I detailed toxicokinetic parameters are not available, but one can evaluate the relationship between the initial concentration and ti/2. Here only data for subjects in which the final concentration is greater than the limit of quantification is considered to avoid statistical artifacts due to limited observational data. Although the lower half-life of the subject with the highest initial concentration indicates a possible negative trend, the half-life is in the range of subjects with lower initial concentrations. Thus, these data do not show a clear dose dependence for half-life and are interpreted as only showing interindividual variation (see Figure C-5). The human data appear consistent with first-order clearance across the range of concentrations observed. C-4 ------- Supplemental Information ofPFBA and Related Salts 160 140 120 i 100 Ol = SO <•1 « 60 40 20 0 t Human half-life vs. initial concentration * • • • • • • • } 20 40 60 SO Initial concentration (ng/ml) Figure C-5. Estimated human half-lives versus initial serum concentrations. Chang etal. f20081 only evaluated one PFBA dose in monkeys, so determining whether the biphasic clearance pattern is due to the classical distinction between distribution and excretion phases or a nonlinearity in clearance is not possible. The data show linear clearance from 1-7 or 10 days after the i.v. dose was given, however, when serum concentrations were below 100 ng/mL. Thus, interpreting these data as showing linear kinetics for serum concentrations below 100 ng/mL under long-term exposure conditions seem reasonable. Because the highest initial condition of the human subjects in Chang etal. (20081 was 72 ng/mL, to the extent that kinetics in monkeys can be extrapolated to humans, the results for monkeys confirm the conclusion that human kinetics are also reasonably assumed linear below ~100 ng/mL. This is approximately 1,000-fold below the range of linearity in mice and rats, however, so uncertainty exists as to whether the range of linear kinetics in humans and monkeys extends into the range of rodent-based points of departure. Russell etal. (20151 attempted to evaluate the kinetics ofPFBA as a metabolite of 6:2 fluorotelomer alcohol (FTOH) during a 1-day inhalation study (6-hour exposure, 24-hour observation) and at the end of 23 days of exposure. The half-life of PFBA, however, could not be estimated from the single-day data for male rats and could be estimated only for the high-level exposure in female rats, with yields of PFBA 0.2% in males and not detectable or 0.02% in females. Also, three metabolic intermediates occur between 6:2 FTOH and PFBA, but the model appears to have assumed direct, instantaneous transformation through the first two steps. Assumptions about the volume of distribution were made by (Russell etal.. 20151. These simplifications in the model likely explain the large discrepancy between the PFBA half-life determined from the single-day exposure 6:2 FTOH for female rats (19 hours) and the half-life obtained for direct exposure to PFBA (1.4-hour average) by f Chang etal.. 20081. Russell etal. f20151 used only male rats in the 23-day C-5 ------- Supplemental Information ofPFBA and Related Salts 6:2 FTOH inhalation study, from which they estimated a half-life of 27.7 hours, over three times higher than the average obtained by (Chang etal.. 20081. The discrepancy also could be due to an underestimation of the metabolic yield from the 1-day experiments. In summary, whereas Russell etal. f20151 described measurements ofPFBA in male rats from 23 days of exposure to 6:2 FTOH, the results for female rats after a single exposure are completely inconsistent with the results of f Chang etal.. 20081. Therefore, the conclusions from the multiday study are considered too unreliable to be used. The other long-term data available on internal dosimetry are from the bioassays (Butenhoff etal.. 2012: Das etal.. 2008: van Otterdiik. 2007bl. Serum concentrations in nonpregnant female mice after 17 days of exposure (24 hours after the last dose) are 2.0 ± 1.0 and 2.4 ± 1.7 [ig/mL, and for pregnant mice are 3.8 ± 1.0 and 4.4 ± 0.7 [ig/mL, for the 35- and 175-mg/kg dose groups, respectively fDas etal.. 20081. For female mice dosed with 30- and 100-mg/kg PFBA, Chang et al. (20081 reported 4.1 ± 1.7 and 6.4 ± 3.9 |J.g/mL in serum 24 hours after the dose; using linear extrapolation based on the difference in dose, one might expect 4.8 and 11.2 |J.g/mL at 24 hours after doses of 35 and 175 mg/kg, given these data. Although the concentrations in the Das et al. (20081 study are somewhat lower than these projections, the difference, especially at the low dose, is within the range of uncertainty and precision expected for PK analysis. Of note is that, given an average clearance of 28 mL/kg-hour obtained by Chang et al. f20081 after 10- and 30-mg/kg doses, the predicted average serum concentrations for a 35-mg/kg dose is 52 [ig/mL. This average concentration reflects the much higher concentrations expected in the first few hours after each dose. For male rats, Butenhoff et al. (20121 measured end-of-treatment serum levels of 38 ± 23 and 52 ± 25 |J.g/mL after 28 and 90 days, respectively, at 30 mg/kg-day; EPA presumes these measurements were made 24 hours after the last dose. The corresponding values reported by Chang etal. f20081 for a 30-mg/kg oral dose in the dose-range and time-course studies are 16 ± 3 and 29 ± 13 [ig/mL, respectively. Although again, some discrepancy is found between the short-term PK data and the bioassay measurements, the difference is that it is roughly within a factor of 2, which is acceptable for PK analysis and does not indicate a strong time dependence in the PK. One should keep in mind that the estimated clearance and half-life values are based on multiple time points at which the serum concentration is measured, while the comparisons above use only a single time point, 24 hours after dosing, when the result will be sensitive to experimental variation. Given these data and results, the half-life or clearance ofPFBA measured in single-day exposures by Chang etal. (20081 will be assumed to predict dosimetry after repeated exposures that occur in bioassays. This is a common assumption for chemicals with relatively short half-lives because pharmacokinetic studies are typically confined to a single day or less. Clearance in rats and mice might include a slower beta phase, like that observed in monkeys. If a slow clearance phase exists, internal dose from long-term exposure will be higher than is effectively estimated using the C-6 ------- Supplemental Information ofPFBA and Related Salts clearance rate determined from single-day exposures, which would increase the HED compared with the current prediction. Using an animal-human ratio of clearance values to estimate the HED relies only on the assumptions that the average serum concentration (Cavg) is predictive of systemic effects in adults and that the relationship between Cavg and dose rate is linear with the proportionality determined by the clearance values estimated here (i.e., the clearance from single-day experiments is predictive of bioassay conditions). The human half-life estimates were from subjects who had been occupationally exposed to PFBA, with the duration of the PK observation 7-10 days. Thus, those results are reasonably expected to represent clearance under (subsequent to) chronic exposure conditions. The primary uncertainty in predicting human clearance comes from assuming a volume of distribution equal to that estimated for monkeys, which is thought modest given the physiological similarity between monkeys and humans. Thus, the overall uncertainty from using the animal-human clearance ratio to predict the HED for systemic effects in adults appears modest, especially compared to the case where PK data such as used here are not available. Because developmental effects are usually presumed to depend on peak concentration rather than average concentration, it must be noted that use of the clearance ratio to estimate HEDs for those endpoints also involves an assumption that the absorption rate in humans is similar to that of animals. For PFBA, the absorption rate in mice and rats is fairly rapid, with the peak concentration occurring 0.6-4 hours after bolus oral doses fChang etal.. 20081. That absorption in humans would be faster than in rodents seems unlikely, and exposures are more likely spread out over the day than in the animal bioassays. Therefore, the most likely case is that the peak concentration in humans exposed at the HED will be lower than the peak concentration in mice or rats at the corresponding dose rate. Thus, although this assumption creates uncertainty in the dose extrapolation, the result is not expected to underpredict human health risks. C.2. MIXED MODELING TO ESTIMATE HALF-LIFE IN HUMANS A linear mixed-effects model was additionally used to estimate a ti/2 for PFBA according to methods described in (Li etal.. 2018). Briefly, linear mixed-effect models are extensions of simple linear models that use the best linear unbiased prediction estimator to estimate random and fixed effects for clustered data. One important consequence of clustering is that measurements of serum PFBA units within the same person (cluster) are more similar than measurements on serum PFBA in different people (i.e., other clusters). Failure to account for the intracluster correlation would result in misleading inferences. Each individual in Chang etal. (2008) was assumed to have been selected randomly from a larger population. Below is the mixed model formula used for estimating the half-life of serum PFBA: ln(PFBAjy) = (apop + at) + (/cpop + kt) x ty + (C-l) C-7 ------- Supplemental Information ofPFBA and Related Salts where ln(PFBA,y) is the natural logarithm of the serum PFBA concentrations measured at the jth time point for the ith subject, crpop is the population mean (also known as the fixed intercept for the population); ai ~ N (0, o2a) is a random intercept for the ith subject; /fpop is the fixed slope for the population (also known as the average excretion rate constant for serum PFBA for the whole population); ki ~ N (0, a2k) is the random slope for the ith subject that allows the excretion rate to vary by individuals; t,y represents the observation time for the jth measurement of serum PFBA for ith subject; and £,y ~ N (0, g2£) is the random-error effect (residual) for jth measurement of ith subject Of note, the small sample sizes (due to the exclusion of the only two subjects identified as females) limited our ability to draw clear conclusions in gender-stratified comparisons. The subjects from Chang etal. f20081 used in this analysis and the half-lives estimated by Chang etal. f20081 are listed in the following table. As explained in section 5.2.1, Approach for Animal-Human Extrapolation of Perfluorobutanoic Acid (PFBA) Dosimetry, subjects whose second concentration measurement was below the lower limit of quantitation (LLOQ) were excluded from analysis because the half-life for these subjects is highly uncertain. This choice is expected to bias the analysis towards higher half-lives but given the small number of human subjects for which data are available, and that variability in clearance among the human population is expected, this is considered a reasonably health-protective choice. Subject Sex Reported half-life (h) Cottage Grove Subject 1 NS 105.3 Cottage Grove Subject 1 NS 109.7 Cordova Subject 2 M 53 Cordova Subject 3 M 72 Cordova Subject 4 M 44 Cordova Subject 6 M 152 Cordova Subject 8 M 63 Cordova Subject 9 M 47 The half-life of serum PFBA for the study population (ti/2,pop) then was estimated as: t 1/2,pop lll(2) '•pop (C-2) The mixed-effects model estimated /fpop to be -0.010, therefore resulting in an estimated ti/2 of 67.9 hours. Of the estimated half-lives reported by Chang etal. (2008). including those excluded from analysis by EPA, five values (42% of the population) were greater than 67.9 hours and seven (58% of the population) were below. This value also matches very closely to the median value calculated when not taking clustering into account, and therefore was considered a reasonable estimate of the population mean and was used in estimation of clearance in humans. C-8 ------- Supplemental Information ofPFBA and Related Salts APPENDIX D. BENCHMARK DOSE MODELING RESULTS D.l. BENCHMARK DOSE MODELING APPROACHES As discussed in Section 5 of the body of the Toxicological Review, the endpoints selected for benchmark dose (BMD) modeling were relative liver weight, liver hypertrophy, total T4, and thyroid follicular hypertrophy incidence from Butenhoff et al. f20121 and relative liver weight, full litter resorption, delayed eye opening delayed vaginal opening, and delayed preputial separation from (Das etal.. 20081. The animal doses in the study were used in the BMD modeling and then converted to human equivalent doses (HEDs) using the ratio of animal-to-human clearance values; the modeling results are presented in this appendix. D.l.l. Modeling Procedure for Dichotomous Noncancer Data BMD modeling of dichotomous noncancer data was conducted using EPA's Benchmark Dose Software (BMDS, version 3.1.2). For these data, the Gamma, Logistic, Log-Logistic, Log-Probit, Multistage, Probit, Weibull, and Dichotomous Hill models available within the software were fit using a benchmark response (BMR) of 10% extra risk (see Toxicological Review, Section 4.2.1 for justification of selected BMRs). The Multistage model is run for all polynomial degrees up to n - 2, where n is the number of dose groups including control. Adequacy of model fit was judged on the basis of x2 goodness-of-fit p-value (p >0.1), scaled residuals at the data point (except the control) closest to the predefined benchmark response (absolute value <2.0), and visual inspection of the model fit. In the cases where no best model was found to fit to the data, a reduced data set without the high-dose group was further attempted for modeling and the result presented with that of the full data set. In cases where a model with several parameters equal to the number of dose groups was fit to the data set, all parameters were estimated, and no p-value was calculated, that model was not considered for estimating a point of departure (POD) unless no other model provided adequate fit. Among all models providing adequate fit, the benchmark dose lower confidence limit (BMDL) from the model with the lowest Akaike's information criterion (AIC) was selected as a potential POD when BMDL values were sufficiently close (within threefold). Otherwise, the lowest BMDL was selected as a potential POD. D.l.2. Modeling Procedure for Continuous Noncancer Data BMD modeling of continuous noncancer data was conducted using EPA's Benchmark Dose Software (BMDS, version 3.1.2). For these data, the Exponential, Hill, Polynomial, and Power models available within the software are fit using a BMR of 1 standard deviation (SD) when no toxicological D-l ------- Supplemental Information ofPFBA and Related Salts information was available to determine an adverse level of response. When toxicological information was available, the BMR was based on relative deviation, as outlined in the Benchmark Dose Technical Guidance fU.S. EPA. 20121 (see Toxicological Review, Section 5.2.1 for justification for using BMRs); when a BMR based on relative deviation was used, modeling results using BMRs based on SD are included for reference. An adequate fit is judged on the basis of x2 goodness-of-fit p-value (p > 0.1), scaled residuals at the data point (except the control) closest to the predefined benchmark response (absolute value <2.0), and visual inspection of the model fit In addition to these three criteria for judging adequacy of model fit, a determination is made on whether the variance across dose groups is homogeneous. If a homogeneous variance model is deemed appropriate based on the statistical test provided by BMDS (i.e., Test 2), the final BMD results are estimated from a homogeneous variance model. If the test for homogeneity of variance is rejected (p < 0.05), the model is run again while modeling the variance as a power function of the mean to account for this nonhomogeneous variance. If this nonhomogeneous variance model does not adequately fit the data (i.e., Test 3; p < 0.05), alternative approaches were assessed on a case-by- case basis. For example, in cases where neither variance model fit, or constant variance did not fit (with adequate Test-4 p-value) and nonconstant variance did fit (with inadequate Test-4 p-value), the log-normal distribution was attempted. In cases where a model with several parameters equal to the number of dose groups was fit to the data set, all parameters were estimated, and no p-value was calculated, that model was not considered for estimating a POD unless no other model provided adequate fit. Among all models providing adequate fit, the BMDL from the model with the lowest AIC was selected as a potential POD when BMDL estimates differed by less than threefold. When BMDL estimates differed by greater than threefold, the model with the lowest BMDL was selected to account for model uncertainty. In situations where there are multiple, related continuous endpoints in an organ system, or endpoints that inform a generalized effect to the exposed organism (e.g., developmental delays in multiple organ systems), modeling a combined endpoint of "total affected" animals was not pursued. Such a systematic multi-endpoint modeling approach is not currently available in BMDS other than the MS-Combo model that requires an assumption that the endpoints are independent; such an assumption is likely not valid with respect to continuous non-cancer endpoints in the PFBA toxicity database. Further, with respect to combining multiple continuous and dichotomous endpoints outside of a specific multi-endpoint model, first a cut-off value would need to be established for continuous endpoints to determine when an animal has "responded" (i.e., the continuous data would need to be "dichotomized"). Such dichotomization of continuous data results in a loss of precision and is recommended against in the BMD Technical Guidance (U.S. EPA, 2012). D-2 ------- Supplemental Information ofPFBA and Related Salts D.1.3. Modeling Procedure for Continuous Noncancer Developmental Toxicity Data For continuous developmental toxicity data, data for individual animals were requested from the study authors when possible. The use of individual animal data allows for the correct measure of variance to be calculated. When a biological rationale for selecting a benchmark response level is lacking, a BMR equal to 0.5 SD was used. The use of 1 SD for the BMR for continuous endpoints is based on the observation that shifting the distribution of the control group by 1 SD results in ~10% of the animal data points falling beyond an adversity cutoff defined at the ~1.5 percentile (Crump. 19951. This approximates the 10% extra risk commonly used as the BMR for dichotomous endpoints. Thus, the use of 0.5 SD for continuous developmental toxicity endpoints approximates the extra risk commonly used for dichotomous developmental toxicity endpoints. D.1.4. Modeling Procedure for Dichotomous Noncancer Developmental Toxicity Data For dichotomous developmental toxicity data, data for individual animals were requested from the study authors when possible. This allowed the use of the nested logistic model, which statistically accounts for intralitter similarity (the propensity of littermates to respond more like one another than pups from another litter) by estimating intralitter correlation and using litter-specific covariates. Other models (Rai and van Ryzin, NCTR) that also account for intralitter similarity were not considered in modeling dichotomous developmental toxicity data as they are not currently implemented in BMDS 3.2. Judging model fit for this model is identical to the procedure used for regular dichotomous models. D.1.5. Data Used for Modeling The source of the data used for modeling is provided in Table D-l. For endpoints from the Das etal. f20081 study, the study authors kindly provided individual dam-level data to facilitate modeling and to provide corrected data where needed. These data also are included in full in the tables below. Table D-l. Sources of data used in benchmark dose modeling of PFBA endpoints Endpoint/Reference Reference Location HAWC link Relative liver weight Butenhoff et al. Appendix 1, page 37 (van Otterdiik, 2007b) https://hawcprd. eoa.gov/ani/endDoint/ (2012) 100507453/ Relative liver weight Das et al. (2008) Figure 2, page 175 https://hawcprd. eoa.gov/ani/endDoint/ 100507508/ Liver hypertrophy Butenhoff et al. Table 9, page 523 httos://hawcord. eoa.gov/ani/endooint/ (2012) 100507383/ Total T4 Butenhoff et al. Table 8, page 522 httos://hawcord. eoa.gov/ani/endooint/ (2012) 100507375/ Full litter resorption Das et al. (2008) Table D-2 D-3 ------- Supplemental Information ofPFBA and Related Salts Endpoint/Reference Reference Location HAWC link Fetal mortality (full litter resorptions combined with fetal death from litters without full litter resorptions) Das et al. (2008) Table D-3 Eyes opening Das et al. (2008) Table D-4 Vaginal opening Das et al. (2008) Table D-5 Preputial separation Das et al. (2008) Table D-6 Table D-2. Data received from study authors for Das et al. (2008) on full litter resorptions (FLR) Dose (mg/kg-d) Number of implants FLR 0 8 0 18 35 2 175 2 175 2 175 9 175 5 350 3 350 2 350 13 350 13 350 3 350 14 350 13 Table D-3. Data received from study authors for Das et al. (2008) on fetal death (litters without full litter resorptions) combined with full litter resorptions Dose (mg/kg-d) Number of implants Number of dead Dam weight on GDI (litter- specific covariate) 0 16 1 30 0 16 1 28.2 0 11 2 27.7 D-4 ------- 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 35 35 35 35 35 35 35 35 35 35 35 35 35 35 35 Supplemental Information ofPFBA and Related Salts Number of implants 11 12 11 15 14 12 14 16 13 17 14 13 11 18 15 13 13 14 15 13 12 13 14 16 13 15 13 14 Number of dead 18 Dam weight on GDI (litter- specific covariate) 27.4 25.9 24.1 29.2 28 27.1 26.8 26.6 25.1 30.1 29 27.5 28.1 26.9 26.7 23.3 25.8 31.4 28.1 29.3 27.4 27 26.9 25.7 31.6 29.2 27.7 27.5 28.1 25.5 30.3 27.5 28.1 D-5 ------- 35 35 35 35 35 35 35 35 175 175 175 175 175 175 175 175 175 175 175 175 175 175 175 175 175 175 175 175 Supplemental Information ofPFBA and Related Salts Number of implants 13 11 10 13 13 13 12 14 15 14 14 15 14 15 16 11 16 11 13 11 15 14 13 12 16 11 14 Number of dead Dam weight on GDI (litter- specific covariate) 27.9 26.4 27.4 27.9 26.1 24.8 24.8 23.1 28.1 27.5 27.4 27.5 29.4 27.5 26 26.2 23.4 29.1 28.2 25.8 26.8 26.9 25 26.7 25.5 25.4 29 25 29.2 26.3 27.4 25.1 25.3 D-6 ------- Supplemental Information ofPFBA and Related Salts Dose (mg/kg-d) Number of implants Number of dead Dam weight on GDI (litter- specific covariate) 350 12 1 29.5 350 16 2 28.8 350 17 2 26.2 350 12 2 26.2 350 16 0 27.3 350 9 3 27.6 350 13 0 27.7 350 13 0 27.4 350 13 1 26.4 350 7 1 24.6 350 3 3 21.5 350 2 2 23 350 13 13 25.8 350 13 13 24.6 350 3 3 25.1 350 14 14 28.2 350 13 13 29.2 350 1 1 25.4 Table D-4. Data received from study authors for Das et al. (2008)on delayed eye opening Dose (mg/kg-d) Average day of eye opening 0 16.27 0 15.57 0 15.22 0 15.27 0 14.55 0 14.91 0 17.64 0 15.69 0 15.00 0 17.57 0 17.71 D-7 ------- 0 0 0 0 0 0 0 0 0 35 35 35 35 35 35 35 35 35 35 35 35 35 35 35 35 35 35 35 35 35 35 Supplemental Information ofPFBA and Related Salts Average day of eye opening 14.91 16.50 17.58 16.50 16.25 15.20 17.25 18.00 18.00 16.00 17.31 18.00 17.23 17.23 16.82 18.78 17.31 17.57 17.53 18.00 15.25 17.00 17.82 18.09 17.70 16.11 18.29 17.50 17.55 17.60 17.78 17.69 17.67 D-8 ------- 175 175 175 175 175 175 175 175 175 175 175 175 175 175 175 350 350 350 350 350 350 350 350 350 350 350 350 350 350 350 Supplemental Information ofPFBA and Related Salts Average day of eye opening 15.71 17.77 16.91 18.00 17.69 17.27 17.17 17.64 18.00 18.00 18.09 18.88 18.00 18.00 18.20 15.00 18.64 17.85 17.64 18.00 17.36 17.85 17.93 18.00 18.00 18.00 18.60 18.00 18.09 18.00 D-9 ------- Supplemental Information ofPFBA and Related Salts Table D-5. Data received from study authors for Das et al. (2008) on delayed vaginal opening Dose (mg/kg-d) Average day of vaginal opening 0 32.40 0 27.00 0 30.80 0 30.20 0 34.17 0 33.67 0 30.33 0 28.00 0 30.14 0 33.67 0 28.00 0 31.90 0 32.50 0 34.00 0 29.25 0 28.00 0 29.33 0 35.57 0 34.83 35 28.20 35 34.00 35 37.25 35 34.00 35 31.00 35 31.20 35 35.67 35 34.25 35 35.38 35 30.00 35 31.50 35 31.20 D-10 ------- 35 35 35 35 35 35 35 35 35 175 175 175 175 175 175 175 175 175 175 175 175 175 175 175 175 175 350 350 350 350 350 350 350 Supplemental Information ofPFBA and Related Salts Average day of vaginal opening 33.50 32.50 37.67 35.00 35.20 33.00 34.50 38.50 34.30 31.60 29.40 33.67 31.67 34.20 34.50 37.00 32.22 38.00 34.50 34.33 34.67 37.86 33.00 36.50 35.33 39.25 35.00 36.00 33.80 33.00 32.00 31.17 33.57 D-ll ------- Supplemental Information ofPFBA and Related Salts Dose (mg/kg-d) Average day of vaginal opening 350 34.10 350 33.33 350 38.70 350 36.33 350 36.00 350 37.25 350 35.00 350 38.50 Table D-6. Data received from study authors for Das et al. (2008) on delayed preputial separation Dose (mg/kg-d) Average day of preputial separation 0 29.00 0 28.20 0 28.20 0 28.00 0 31.80 0 29.20 0 28.71 0 30.00 0 31.00 0 28.29 0 30.00 0 29.80 0 31.00 0 29.50 0 29.00 0 31.00 0 29.67 35 27.40 35 33.40 35 28.20 35 31.80 D-12 ------- 35 35 35 35 35 35 35 35 35 35 35 35 35 35 35 35 35 175 175 175 175 175 175 175 175 175 175 175 175 175 175 175 175 Supplemental Information ofPFBA and Related Salts Average day of preputial separation 30.00 31.33 35.50 30.22 33.17 30.00 29.00 30.14 30.29 29.80 30.43 30.00 27.50 28.20 28.57 29.25 30.17 26.60 28.80 30.50 31.71 31.11 32.33 28.00 31.00 35.00 30.60 30.13 29.50 30.00 31.60 31.00 30.17 D-13 ------- Supplemental Information ofPFBA and Related Salts Dose (mg/kg-d) Average day of preputial separation 175 31.50 350 28.00 350 31.80 350 31.50 350 32.40 350 31.83 350 30.80 350 31.17 350 33.80 350 34.00 350 30.33 350 30.00 350 33.17 350 32.00 350 32.80 D.2. RELATIVE LIVER WEIGHT-MALE RATS EXPOSED 90 DAYS fBUTENHOFF ET AL.. 2012: VAN OTTERDIIK. 2007B11 Table D-7. Dose-response data for relative liver weight in male rats following 90 day exposure fButenhoff et al.. 2012: van Otterdiik. 2007bl Dose (mg/kg-d) n Mean SD 0 10 2.11 0.13 1.2 10 2.29 0.14 6 10 2.26 0.16 30 10 2.8 0.32 'Throughout this document, if a model was selected as appropriately fitting the modeled data, that model's entries in the tables are in green shaded cells and the text is bolded. D-14 ------- Supplemental Information ofPFBA and Related Salts Table D-8. Benchmark dose results for relative liver weight in male rats exposed 90 days —constant variance, BMR = 10% relative deviation fButenhoff et al.. 2012: van Otterdiik. 2007bl Models Restriction3 10% Relative deviation p-Value AIC BMDS classification13 BMDS notes BMD BMDL Constant variance Exponential 2 (CV—normal) Restricted 11.3634 9.4685 0.1720 -8.8244 Questionable Constant variance test failed (Test 2 p-value < 0.05) Modeled control response SD >| 1.51 actual response SD Exponential 3 (CV—normal) Restricted 11.3634 9.4572 0.1720 -8.8244 Questionable Constant variance test failed (Test 2 p-value < 0.05) Modeled control response SD >| 1.51 actual response SD Exponential 4 (CV—normal) Restricted 10.4110 4.8569 0.0584 -6.7628 Questionable Constant variance test failed (Test 2 p-value < 0.05) Goodness-of-fit p-value <0.1 Modeled control response SD >| 1.51 actual response SD Exponential 5 (CV—normal) Restricted 10.4033 4.8563 0.0584 -6.7621 Questionable Constant variance test failed (Test 2 p- value < 0.05) Goodness-of-fit p-value <0.1 Modeled control response SD >| 1.51 actual response SD Hill (CV—normal) Restricted 6.6152 6.0656 NA -4.1913 Questionable Constant variance test failed (Test 2 p-value < 0.05) Modeled control response SD >| 1.51 actual response SD df = 0, saturated model (goodness-of-fit p-value cannot be calculated) D-15 ------- Supplemental Information ofPFBA and Related Salts Models Restriction3 10% Relative deviation p-Value AIC BMDS classification13 BMDS notes BMD BMDL Constant variance Polynomial (3 degree) (CV—normal) Restricted 12.8952 8.4671 0.0624 -6.8714 Questionable Constant variance test failed (Test 2 p-value < 0.05) Goodness-of-fit p-value <0.1 Modeled control response SD >| 1.51 actual response SD Polynomial (2 degree) (CV—normal) Restricted 12.1463 8.4560 0.0611 -6.8370 Questionable Constant variance test failed (Test 2 p-value < 0.05) Goodness-of-fit p-value <0.1 Modeled control response SD >| 1.51 actual response SD Power (CV—normal) Restricted 10.4151 8.4328 0.1668 -8.7631 Questionable Constant variance test failed (Test 2 p-value < 0.05) Modeled control response SD >| 1.51 actual response SD Linear (CV—normal) Unrestricted 10.4151 8.4328 0.1668 -8.7631 Questionable Constant variance test failed (Test 2 p-value < 0.05) Modeled control response SD >| 1.51 actual response SD a"Restriction" column denotes the restriction status of applied models. ^'Classification" column denotes whether a model can be considered for model selection purposes. See BMDS User Guide: https://www.epa.gov/bmds. D-16 ------- Supplemental Information ofPFBA and Related Salts Table D-9. Benchmark dose results for relative liver weight in male rats exposed 90 days—nonconstant variance, BMR = 10% relative deviation fButenhoff et al.. 2012: van Otterdiik. 2007bl Models Restriction 10% Relative deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Nonconstant variance Exponential 2 (NCV—normal) Restricted 11.3982 9.0908 0.0362 -15.2001 Questionable Goodness-of-fit p-value <0.1 Exponential 3 (NCV—normal) Restricted 11.3962 9.0911 0.0362 -15.2001 Questionable Goodness-of-fit p-value <0.1 Exponential 4 (NCV—normal) Restricted 10.5179 5.2058 0.0096 -13.1325 Questionable Goodness-of-fit p-value <0.1 Exponential 5 (NCV—normal) Restricted 10.5091 5.2055 0.0096 -13.1313 Questionable Goodness-of-fit p-value <0.1 Hill (NCV—normal) Restricted 11.1854 7.9783 0.0090 -13.0126 Questionable Goodness-of-fit p-value <0.1 Polynomial (3 degree) (NCV—normal) Restricted 12.7313 8.1751 0.0104 -13.2674 Questionable Goodness-of-fit p-value <0.1 Polynomial (2 degree) (NCV—normal) Restricted 11.9089 8.1513 0.0100 -13.2065 Questionable Goodness-of-fit p-value <0.1 Power (NCV—normal) Restricted 10.5174 8.1228 0.0350 -15.1326 Questionable Goodness-of-fit p-value <0.1 Linear (NCV—normal) Unrestricted 10.5179 8.1236 0.0350 -15.1326 Questionable Goodness-of-fit p-value <0.1 D-17 ------- Supplemental Information ofPFBA and Related Salts Table D-10. Benchmark dose results for relative liver weight in male rats exposed 90 days—log-normal distribution, constant variance, BMR = 10% relative deviation fButenhoff et al.. 2012: van Otterdiik. 2007bl Models3 Restriction 10% Relative deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Log-normal distribution, constant variance Exponential 2 (CV— log-normal) Restricted 11.5672 9.5455 0.1004 -14.1752 Viable- Alternate Modeled control response SD >| 1.51 actual response SD Exponential 3 (CV—log-normal) Restricted 11.5672 9.6019 0.1004 -14.1752 Viable- Recommended Lowest AIC Modeled control response SD > 11.51 actual response SD Exponential 4 (CV—log-normal) Restricted 10.6449 5.1404 0.0311 -12.1242 Questionable Goodness-of-fit p-value < 0.1 Modeled control response SD >| 1.51 actual response SD Exponential 5 (CV—log-normal) Restricted 10.6419 5.1401 0.0311 -12.1239 Questionable Goodness-of-fit p-value < 0.1 Modeled control response SD >| 1.51 actual response SD Hill (CV—log-normal) Restricted 10.5728 4.9799 0.0976 -14.1178 Questionable Goodness-of-fit p-value < 0.1 Modeled control response SD >| 1.51 actual response SD Polynomial (3 degree) (CV—log-normal) Restricted 12.6948 8.5635 0.0328 -12.2144 Questionable Goodness-of-fit p-value < 0.1 Modeled control response SD >| 1.51 actual response SD Polynomial (2 degree) (CV—log-normal) Restricted 11.9903 8.5515 0.0321 -12.1783 Questionable Goodness-of-fit p-value < 0.1 Modeled control response SD >| 1.51 actual response SD D-18 ------- Supplemental Information ofPFBA and Related Salts Models3 Restriction 10% Relative deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Log-normal distribution, constant variance Power (CV— log-normal) Restricted 10.6452 8.5334 0.0979 -14.1242 Questionable Goodness-of-fit p-value < 0.1 Modeled control response SD >| 1.51 actual response SD Linear (CV—log-normal) Unrestricted 10.6452 8.5334 0.0979 -14.1242 Questionable Goodness-of-fit p-value < 0.1 Modeled control response SD >| 1.51 actual response SD Frequentist Exponential Degree 3 Model with BMR of 0.1 Rel. Dev. for the BMD and 0.95 Lower Confidence Limit for the BMDL 3.1 Dose Figure D-l. Dose-response curve for the Exponential M3 model fit to relative liver weight in male rats exposed 90 days (Butenhoff et al.. 2012: van Otterdijk. 2007b). D-19 ------- Supplemental Information ofPFBA and Related Salts User Input Info Model frequentist Exponential degree 3 vl.l Dataset Name Butenhoff_90_Lweight_rel User notes [Add user notes here] Dose-Response Model M[dose] = a * exp(±l * (b * dose)Ad) Variance Model Var[i] = alpha Model Options BMR Type Rel. Dev. BMRF 0.1 Tail Probability - Confidence Level 0.95 Distribution Type Log-normal Variance Type Constant Model Data Dependent Variable [Dose] Independent Variable [Mean] Total # of Observations 4 Adverse Direction Automatic D-20 ------- Supplemental Information ofPFBA and Related Salts Model Results Benchmark Dose BMD 11.56718731 BMDL 9.60187006 BMDU 14.67526197 AIC -14.17517344 Test 4 P-value 0.100441772 D.O.F. 2 Model Parameters # of Parameters 4 Va ria ble Estimate a 2.171112769 b 0.0082397 d Bounded log-alpha -5.045994496 Goodness of Fit Dose Size Estimated Median Calc'd Median Observed Mean Estimated GSD Calc'd GSD Observed SD Scaled Residual 0 10 2.171112769 2.10600663 2.11 1.08352413 1.063487 0.13 -0.17835832 1.2 10 2.192686432 2.28573248 2.29 1.08352413 1.062982 0.14 0.284010771 6 10 2.281146197 2.25435749 2.26 1.08352413 1.073268 0.16 -0.061715421 30 10 2.779944166 2.78189148 2.8 1.08352413 1.120657 0.32 0.058533184 Likelihoods of Interest # of Model Log Likelihood* Parameters AIC A1 12.38576382 5 -14.771528 A2 15.32442666 8 -14.648853 A3 12.38576382 5 -14.771528 fitted 10.08758672 3 -14.175173 R -8.71328445 2 21.4265689 * Includes additive constant of -70.8323. This constant was not included in the LL derivation prior to BMDS 3.0. Tests of Interest -2*Log(Likelihood Test Ratio) Test df p-value 1 48.07542222 6 <0.0001 2 5.877325671 3 0.11773355 3 5.877325671 3 0.11773355 4 4.596354207 2 0.10044177 D-21 ------- Supplemental Information ofPFBA and Related Salts Table D-ll. Benchmark dose results for relative liver weight in male rats exposed 90 days—log-normal distribution, constant variance, BMR = 1 standard deviation fButenhoff et al.. 2012: van Otterdiik. 2007bl Models Restriction 1 Standard deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Log-normal distribution, constant variance Exponential 2 (CV— log-normal) Restricted 9.7357 7.6047 0.1004 -14.1752 Viable- Alternate Modeled control response SD >| 1.51 actual response SD Exponential 3 (CV—log-normal) Restricted 9.7356 7.6049 0.1004 -14.1752 Viable- Recommended Lowest AIC Modeled control response SD > 11.51 actual response SD Exponential 4 (CV—log-normal) Restricted 8.8962 0.0000 0.0311 -12.1242 Questionable Goodness-of-fit p-value < 0.1 Modeled control response SD >| 1.51 actual response SD Exponential 5 (CV—log-normal) Restricted 8.8943 6.9746 0.0311 -12.1239 Questionable Goodness-of-fit p-value < 0.1 Modeled control response SD >| 1.51 actual response SD Hill (CV—log-normal) Restricted 8.8323 4.0523 0.0976 -14.1178 Questionable Goodness-of-fit p-value < 0.1 Modeled control response SD >| 1.51 actual response SD Polynomial (3 degree) (CV—log-normal) Restricted 10.7197 6.8148 0.0328 -12.2144 Questionable Goodness-of-fit p-value < 0.1 Modeled control response SD >| 1.51 actual response SD Polynomial (2 degree) (CV—log-normal) Restricted 10.1369 6.8036 0.0321 -12.1783 Questionable Goodness-of-fit p-value < 0.1 Modeled control response SD >| 1.51 actual response SD Power (CV—log-normal) Restricted 8.8972 6.7871 0.0979 -14.1242 Questionable Goodness-of-fit p-value < 0.1 Modeled control response SD >| 1.51 actual response SD Linear (CV—log-normal) Unrestricted 8.8972 6.7871 0.0979 -14.1242 Questionable Goodness-of-fit p-value < 0.1 D-22 ------- Supplemental Information ofPFBA and Related Salts Models Restriction 1 Standard deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Log-normal distribution, constant variance Modeled control response SD >| 1.51 actual response SD D.3. RELATIVE LIVER WEIGHT-Po MICE fDAS ET AL.. 20081 Table D-12. Dose-response data for relative liver weight in pregnant mice fDas et al.. 20081 Dose (mg/kg-d) n Mean SD 0 6 8.04 0.66 35 6 8.76 1.37 175 7 10.28 0.75 350 6 10.65 0.62 D-23 ------- Supplemental Information ofPFBA and Related Salts Table D-13. Benchmark dose results for relative liver weight in pregnant mice—constant variance, BMR = 10% relative deviation fDas et al.. 20081 Models Restriction 10% Relative deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Constant variance Exponential 2 (CV—normal) Restricted 130.2877 98.9543 0.0486 73.1479 Questionable Goodness-of-fit p-value < 0.1 Exponential 3 (CV—normal) Restricted 130.2877 99.1362 0.0486 73.1479 Questionable Goodness-of-fit p-value < 0.1 Exponential 4 (CV—normal) Restricted 36.1911 15.1545 0.8612 69.1285 Viable- recommended Lowest AIC Exponential 5 (CV—normal) Restricted 39.4346 15.2398 NA 71.0979 Questionable df = 0, saturated model (goodness-of-fit p- value cannot be calculated) Hill (CV—normal) Restricted 38.7873 12.3846 NA 71.0979 Questionable df = 0, saturated model (goodness-of-fit p- value cannot be calculated) Polynomial (3 degree) (CV—normal) Restricted 115.5880 84.4884 0.0736 72.3159 Questionable Goodness-of-fit p-value < 0.1 Polynomial (2 degree) (CV—normal) Restricted 115.5878 84.4883 0.0736 72.3159 Questionable Goodness-of-fit p-value < 0.1 Power (CV—normal) Restricted 115.5870 84.4876 0.0736 72.3159 Questionable Goodness-of-fit p-value < 0.1 Linear (CV—normal) Unrestricted 115.5882 84.4875 0.0736 72.3159 Questionable Goodness-of-fit p-value < 0.1 D-24 ------- Supplemental Information ofPFBA and Related Salts Frequentist Exponential Degree 4 Model with BMR of 0.1 Rel. Dev. for the BMD and 0.95 Lower Confidence Limit for the BMDL i CS—1 Estimated Probability Response at BMD O Data BMD BMDL Dose Figure D-2. Dose-response curve for the Exponential M4 model fit to relative liver weight in pregnant mice (Das etal.. 2008). D-25 ------- Supplemental Information ofPFBA and Related Salts User Input Info Model frequentist Exponential degree 4 vl.l Dataset Name Das_p_Lweight_rel User notes [Add user notes here] Dose-Response Model M[dose] = a * [c-(c-l) * exp(-b * dose)] Variance Model Var[i] = alpha Model Options BMR Type Rel. Dev. BMRF 0.1 Tail Probability - Confidence Level 0.95 Distribution Type Normal Variance Type Constant Model Data Dependent Variable [Dose] Independent Variable [Mean] Total # of Observations 4 Adverse Direction Automatic D-26 ------- Supplemental Information ofPFBA and Related Salts #NAME? Benchmark Dose BMD 36.19110286 BMDL 15.15446485 BMDU 87.70968183 AIC 69.12846157 Test 4 P-value 0.861196136 D.O.F. 1 Model Parameters # of Parameters 4 Variable Estimate a 8.018710905 b 0.009531749 c 1.342753894 log-alpha -0.39273843 Goodness of Fit Dose Size Estimated Median Calc'd Median Observed Mean Estimated SD Calc'd SD Observed SD Scaled Residual 0 6 8.018710905 8.04 8.04 0.82170879 0.66 0.66 0.063462168 35 6 8.798356028 8.76 8.76 0.82170879 1.37 1.37 -0.114338192 175 7 10.24876199 10.28 10.28 0.82170879 0.75 0.75 0.100580637 350 6 10.66937939 10.65 10.65 0.82170879 0.62 0.62 -0.057769406 Likelihoods of Interest # of Model Log Likelihood* Parameters AIC A1 -30.54894422 5 71.0978884 A2 -27.8068244 8 71.6136488 A3 -30.54894422 5 71.0978884 fitted -30.56423079 4 69.1284616 R -42.8486201 2 89.6972402 * Includes additive constant of -22.97346. This constant was not included in the LL derivation prior to BMDS 3.0. Tests of Interest -2*Log(Likelihood Test Ratio) Test df p-value 1 30.08359139 6 <0.0001 2 5.484239634 3 0.13958431 3 5.484239634 3 0.13958431 4 0.030573129 1 0.86119614 D-27 ------- Supplemental Information ofPFBA and Related Salts Table D-14. Benchmark dose results for relative liver weight in pregnant mice—constant variance, BMR = 1 standard deviation fDas et al.. 20081 Models Restriction 1 Standard deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Constant variance Exponential 2 (CV—normal) Restricted 141.5518 104.9937 0.0524 73.6332 Questionable Goodness-of-fit p-value < 0.1 Exponential 3 (CV—normal) Restricted 141.5511 104.9942 0.0524 73.6331 Questionable Goodness-of-fit p-value < 0.1 Exponential 4 (CV—normal) Restricted 37.2658 16.6945 0.5517 70.0879 Viable- recommended Lowest AIC Exponential 5 (CV—normal) Restricted 40.3641 16.7699 NA 71.7337 Questionable df = 0, saturated model (goodness-of-fit p-value cannot be calculated) Hill (CV—normal) Restricted 39.5789 13.8731 NA 71.7337 Questionable df = 0, saturated model (goodness-of-fit p-value cannot be calculated) Polynomial (3 degree) (CV—normal) Restricted 124.9178 90.1236 0.0725 72.9822 Questionable Goodness-of-fit p-value < 0.1 Polynomial (2 degree) (CV—normal) Restricted 124.9176 90.1235 0.0725 72.9822 Questionable Goodness-of-fit p-value < 0.1 Power (CV—normal) Restricted 124.9169 90.1256 0.0725 72.9822 Questionable Goodness-of-fit p-value < 0.1 Linear (CV—normal) Unrestricted 124.9180 90.1238 0.0725 72.9822 Questionable Goodness-of-fit p-value < 0.1 D-28 ------- Supplemental Information ofPFBA and Related Salts DA. LIVER HYPERTROPHY-MALE RAT rBUTENHOFF ET AL.. 2012: VAN OTTERDIIK. 2007B1 Table D-15. Dose-response data liver hypertrophy in male rats (Butenhoff et al.. 2012: van Otterdijk. 2007b) Dose (mg/kg-d) n Incidence 0 10 0 1.2 10 0 6 10 0 30 10 9 Table D-16. Benchmark dose results for liver hypertrophy in rats—BMR = 10% extra risk fButenhoff et al.. 2012: van Otterdiik. 2007bl Models Restriction 10% Extra risk p-Value AIC BMDS classification BMDS notes BMD BMDL Gamma Restricted 16.2946 5.3859 1.0000 8.5017 Viable—alternate Log-logistic Restricted 23.5001 5.4486 1.0000 10.5017 Viable—alternate Multistage 3rd Restricted 10.8404 5.0184 0.9796 8.8673 Viable—alternate Multistage 2nd Restricted 6.8934 3.6966 0.8078 10.2814 Viable—alternate Multistage 1st Restricted 2.4428 1.4091 0.0817 18.5672 Questionable Goodness-of-fit p-value < 0.1 Weibull Restricted 25.2757 5.3801 1.0000 8.5017 Viable- recommended Lowest AIC Dichotomous Hill Unrestricted 23.4994 5.8336 0.9995 12.5017 Viable—alternate Logistic Unrestricted 23.4727 8.4278 1.0000 8.5017 Viable—alternate Log-probit Unrestricted 20.1374 5.4722 1.0000 10.5017 Viable—alternate Probit Unrestricted 21.2661 7.6123 1.0000 10.5017 Viable—alternate D-29 ------- Supplemental Information ofPFBA and Related Salts Frequentist Weibull Model with BMR of 10% Extra Risk for the BMD and 0.95 Lower Confidence Limit for the BMDL 1 0.9 0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0®- e- -e- 15 Dose Estimated Probability Response at BMD O Data BMD BMDL Figure D-3. Dose-response curve for the Weibull model fit to liver hypertrophy in male rats (Butenhoff et al.. 2012: van Otterdijk. 2007b). D-30 ------- Supplemental Information ofPFBA and Related Salts User Input Info Model frequentist Weibull vl.l Dataset Name Butenhoff_90_Lhypertrophy User notes [Add user notes here] Dose-Response Model P[dose] = g + (l-g)*[l-exp(-b*doseAa)] Model Options RiskType Extra Risk BMR 0.1 Confidence Level 0.95 Background Estimated Model Data Dependent Variable Dose Independent Va riable Incidence Total # of Observations 4 Model Results Benchmark Dose BMD 25.27565904 BMDL 5.380065202 BMDU 26.31774355 AiC 8.501660382 P-value 1 D.O.F. 3 Chi2 4.56905E-07 Model Parameters # of Parameters 3 Variable Estimate g Bounded a Bounded b 5.94337E-27 Goodness of Fit Dose Estimated Probability Expected Observed Size Scaled Residual 0 1.523E-08 1.523E-07 0 10 -0.00039 1.2 1.523E-08 1.523E-07 0 10 -0.00039 6 1.52306E-08 1.52306E-07 0 10 -0.00039 30 0.899999999 8.999999992 9 10 8.003E-09 Analysis of Deviance Model Log Likelihood # of Parameters Deviance Test d.f. P Value Full Model -3.250829734 4 - - - Fitted Model -3.250830191 1 9.1381E-07 3 1 Reduced Model -21.32655363 1 36.1514478 3 <0.0001 D-31 ------- Supplemental Information ofPFBA and Related Salts Table D-17. Dose-response data for liver hypertrophy (slight severity lesions) in male rats fButenhoff et al.. 2012: van Otterdiik. 2007bl Dose (mg/kg-d) n Incidence 0 10 0 1.2 10 0 6 10 0 30 10 4 Table D-18. Benchmark dose results for liver hypertrophy (slight severity lesions) in male rats—BMR = 10% extra risk fButenhoff et al.. 2012: van Otterdijk. 2007b) Models Restriction 10% Extra risk p-Value AIC BMDS classification BMDS notes BMD BMDL Gamma Restricted 23.1357 5.6717 1.0000 15.4602 Viable—alternate Log-logistic Restricted 27.1575 5.5461 1.0000 17.4602 Viable—alternate Multistage 3rd Restricted 17.7871 5.5407 0.9978 15.5422 Viable—alternate Multistage 2nd Restricted 13.9892 5.1121 0.8984 17.8741 Viable—alternate Multistage 1st Restricted 8.1158 3.9098 0.5376 19.5942 Viable- recommended Lowest BMDL Weibull Restricted 27.4811 5.6718 1.0000 17.4602 Viable—alternate Dichotomous Hill Unrestricted 27.1562 5.2830 0.9995 19.4602 Viable—alternate BMD:BMDL ratio > 5 Logistic Unrestricted 26.9449 13.6106 1.0000 15.4602 Viable—alternate Log-Probit Unrestricted 24.8237 5.3131 1.0000 17.4602 Viable—alternate Probit Unrestricted 25.5166 12.1561 1.0000 17.4602 Viable—alternate D.5. TOTAL T4—MALE RAT fBUTENHOFF ET AL.. 2012: VAN OTTERDIIK. 2007B1 Table D-19. Dose-response data for total T4 levels in male rats (Butenhoff et al.. 2012: van Otterdijk. 2007b) Dose (mg/kg-d) n Mean SD 0 10 5.27 0.71 1.2 10 5.97 1.08 6 9 4.46 0.88 30 9 3.23 0.55 D-32 ------- Supplemental Information ofPFBA and Related Salts Table D-20. Benchmark dose results for total T4 levels in male rats—constant variance, BMR = 1 standard deviation fButenhoff et al.. 2012: van Otterdiik. 2007hl Models Restriction 1 Standard deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Constant variance Exponential 2 (CV—normal) Restricted 9.2322 6.5166 0.0138 104.3816 Questionable Goodness-of-fit p-value <0.1 Exponential 3 (CV—normal) Restricted 9.2324 6.5166 0.0138 104.3816 Questionable Goodness-of-fit p-value <0.1 Exponential 4 (CV—normal) Restricted 4.9496 2.5239 0.0075 104.9572 Questionable Goodness-of-fit p-value <0.1 Exponential 5 (CV—normal) Restricted 5.7655 3.5138 NA 103.5642 Questionable df = 0, saturated model (goodness-of-fit p-value cannot be calculated) Hill (CV—normal) Restricted 5.5394 3.2999 NA 103.5644 Questionable df = 0, saturated model (goodness-of-fit p-value cannot be calculated) Polynomial (3 degree) (CV—normal) Restricted 11.5906 8.7704 0.0090 105.2374 Questionable Goodness-of-fit p-value <0.1 Polynomial (2 degree) (CV—normal) Restricted 11.5906 8.7704 0.0090 105.2374 Questionable Goodness-of-fit p-value <0.1 Power (CV—normal) Restricted 11.5906 8.7706 0.0090 105.2374 Questionable Goodness-of-fit p-value <0.1 Linear (CV—normal) Unrestricted 11.5906 8.7704 0.0090 105.2374 Questionable Goodness-of-fit p-value <0.1 D-33 ------- Supplemental Information ofPFBA and Related Salts Table D-21. Benchmark dose results for total T4 levels in male rats—nonconstant variance, BMR = 1 standard deviation fButenhoff et al.. 2012: van Otterdiik. 2007bl Models Restriction 1 Standard deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Nonconstant variance Exponential 2 (NCV—normal) Restricted 11.3786 7.8978 0.0182 102.5921 Questionable Goodness-of-fit p-value <0.1 Exponential 3 (NCV—normal) Restricted 11.3789 7.8977 0.0182 102.5921 Questionable Goodness-of-fit p-value <0.1 Exponential 4 (NCV—normal) Restricted 5.8707 2.9606 0.0104 103.1558 Questionable Goodness-of-fit p-value <0.1 Exponential 5 (NCV—normal) Restricted 5.8297 3.9098 NA 102.1810 Questionable df= 0,saturated model (goodness-of-fit p-value cannot be calculated) Hill (NCV—normal) Restricted 5.8562 3.7033 NA 102.1809 Questionable df= 0,saturated model (goodness-of-fit p-value cannot be calculated) Polynomial (3 degree) (NCV—normal) Restricted 13.7327 10.1890 0.0130 103.2666 Questionable Goodness-of-fit p-value <0.1 Polynomial (2 degree) (NCV—normal) Restricted 13.7329 10.1889 0.0130 103.2666 Questionable Goodness-of-fit p-value <0.1 Power (NCV—normal) Restricted 13.7325 10.1890 0.0130 103.2666 Questionable Goodness-of-fit p-value <0.1 Linear (NCV—normal) Unrestricted 13.7332 10.1889 0.0130 103.2666 Questionable Goodness-of-fit p-value <0.1 D-34 ------- Supplemental Information ofPFBA and Related Salts Table D-22. Benchmark dose results for total T4 levels in male rats—log-normal distribution, constant variance, BMR = 1 standard deviation fButenhoff et al.. 2012: van Otterdiik. 2007bl Models Restriction 1 Standard deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Log-normal distribution, constant variance Exponential 2 (CV— log-normal) Restricted 12.0074 7.6347 0.0223 98.5676 Questionable Goodness-of-fit p-value <0.1 Exponential 3 (CV—log-normal) Restricted 12.0074 7.6347 0.0223 98.5676 Questionable Goodness-of-fit p-value <0.1 Exponential 4 (CV—log-normal) Restricted 5.7060 2.5325 0.0200 98.3698 Questionable Goodness-of-fit p-value <0.1 Exponential 5 (CV—log-normal) Restricted 5.9263 3.4425 NA 97.5382 Questionable df= 0,saturated model (goodness-of-fit p-value cannot be calculated) Hill (CV—log-normal) Restricted Questionable df= 0,saturated model (goodness-of-fit p-value cannot be calculated) Polynomial (3 degree) (CV—log-normal) Restricted Questionable Goodness-of-fit p-value <0.1 Polynomial (2 degree) (CV—log-normal) Restricted Questionable Goodness-of-fit p-value <0.1 Power (CV—log-normal) Restricted - - - - Questionable Goodness-of-fit p-value <0.1 Linear (CV—log-normal) Unrestricted - - - - Questionable Goodness-of-fit p-value <0.1 D-35 ------- Supplemental Information ofPFBA and Related Salts D.6. INCREASED FETAL MORTALITY - MALE AND FEMALE Fi MICE fDAS ETAL.. 20081 Table D-23. Dose-response data for increased fetal mortality (Das et al.. 2008) Dose (mg/kg-d) n (No. of implants) No. of dead fetuses/neonates by PND21 Litter-specific covariate (Maternal weight on GDI) 0 16 1 30 0 16 1 28.2 0 11 2 27.7 0 11 0 27.4 0 12 3 25.9 0 11 0 24.1 0 15 0 29.2 0 14 1 28 0 12 3 27.1 0 14 0 26.8 0 16 1 26.6 0 13 2 25.1 0 17 3 30.1 0 14 0 29 0 6 0 27.5 0 9 2 28.1 0 6 0 26.9 0 13 1 26.7 0 11 0 23.3 0 8 8 25.8 0 18 18 31.4 35 15 3 28.1 35 13 0 29.3 35 13 0 27.4 35 14 1 27 35 15 2 26.9 35 13 2 25.7 35 12 4 31.6 35 13 0 29.2 35 14 1 27.7 D-36 ------- 35 35 35 35 35 35 35 35 35 35 35 35 35 35 175 175 175 175 175 175 175 175 175 175 175 175 175 175 175 175 175 175 175 175 Supplemental Information ofPFBA and Related Salts n (No. of implants) 16 13 15 13 14 13 11 10 13 13 13 12 14 15 14 14 15 14 15 16 11 16 11 13 11 15 14 13 . of dead fetuses/neonates by PND21 0 Litter-specific covariate (Maternal weight on GDI) 27.5 28.1 25.5 30.3 27.5 28.1 27.9 26.4 27.4 27.9 26.1 24.8 24.8 23.1 28.1 27.5 27.4 27.5 29.4 27.5 26 26.2 23.4 29.1 28.2 25.8 26.8 26.9 25 26.7 25.5 25.4 29 25 D-37 ------- Supplemental Information ofPFBA and Related Salts Dose (mg/kg-d) n (No. of implants) No. of dead fetuses/neonates by PND21 Litter-specific covariate (Maternal weight on GDI) 350 7 2 29.2 350 12 1 26.3 350 16 3 27.4 350 11 0 25.1 350 14 2 25.3 350 12 1 29.5 350 16 2 28.8 350 17 2 26.2 350 12 2 26.2 350 16 0 27.3 350 9 3 27.6 350 13 0 27.7 350 13 0 27.4 350 13 1 26.4 350 7 1 24.6 350 3 3 21.5 350 2 2 23 350 13 13 25.8 350 13 13 24.6 350 3 3 25.1 350 14 14 28.2 350 13 13 29.2 Table D-24. Benchmark dose results for increased fetal mortality (male and female mice)—BMR = 1% extra risk fDas etal.. 20081 Models Restriction 1% Extra risk p-Value AIC BMDS classification BMDS notes BMD BMDL Nested logistic (lsc+ilc+) Restricted 19.5989 5.7383 Infinity 0.2633 Viable- Recommended Lowest AIC BMDL 3x lower than lowest non- zero dose Nested logistic (Isc+ilc-) Restricted 326.9633 170.7455 Infinity <0.0001 Questionable Goodness of fit p- value < 0.1 D-38 ------- Supplemental Information ofPFBA and Related Salts Models Restriction 1% Extra risk p-Value AIC BMDS classification BMDS notes BMD BMDL Nested logistic (lsc-ilc+) Restricted 50.4014 10.1822 Infinity 0.0833 Questionable Goodness of fit p- value < 0.1 BMDL 3x lower than lowest non- zero dose Nested logistic (Isc-ilc-) Restricted 191.2272 81.9934 Infinity <0.0001 Questionable Goodness of fit p- value < 0.1 Frequentist Nested Logistic Model with BMR of 0.01 Std. Dev. for the BMDand 0.95 Lower Confidence Limit for the BMDL 0.6 Dose Figure D-4. Dose-response curve for the Nested-Logistic model fit to increased fetal mortality in male and female mice fDas et al.. 20081. D-39 ------- Supplemental Information ofPFBA and Related Salts User Input Info Model frequentist Nested Logistic_lsc+ilc+_ v2.2 Dataset Name Das FLR Fetal Death User notes [Add user notes here] Dose-Response Model P[dose] = alpha + thetal*Rij + [1 - alpha - thetal*Rij]/[l+exp(-beta-theta2*Rij-rho*log(dose))] Model Options Risk Type Extra Risk BMR 0.01 Confidence Level 0.95 Litter Specific Covariate Overall Mean Intralitter Correlation Estimate Background Estimate Model Data Dependent Variable Dose Independent Variable Incidence Total # of Observations 87 D-40 ------- Supplemental Information ofPFBA and Related Salts Model Results Benchmark Dose BMD 19.59891366 BMDL 5.738265629 BMDU - AIC 688.92042 P-value 0.263333333 D.O.F. 78 Chi2 96.74138773 Model Parameters # of Parameters 9 Va riable Estimate alpha -0.5312932 beta 16.8290783 thetal 0.024711312 theta2 -0.913645475 rho 1.08467654 phil 0.368252856 phi2 0.135465621 phi3 0.509745798 phi4 0.576861839 Bootstrap Results # Iterations 1000 Bootstrap Seed 1599045577 Log-likelihood -335.46021 Observed Chi-square 96.74138773 Combined P-value 0.263333333 Bootstrap Runs Run Bootstrap Chi-square Percentiles P-Value 50th 90th 95th 99th 1 0.285 85.65851617 109.848694 117.6 134.18995 2 0.258 85.12942257 110.722914 119.0851 131.33939 3 0.247 85.05473338 108.751327 115.9296 137.48443 Combined 0.263333333 85.30000651 109.644757 117.9646 135.17128 Scaled Residuals Minimum scaled residual for dose group nearest the BMD -0.50395 Minimum ABS(scaled residual) for dose group nearest the BMD 0.503952 Average Scaled residual for dose group nearest the BMD -0.50395 Average ABS(scaled residual) for dose group nearest the BMD 0.503952 Maximum scaled residual for dose group nearest the BMD -0.50395 Maximum ABS(scaled residual) for dose group nearest the BMD 0.503952 D-41 ------- Supplemental Information ofPFBA and Related Salts Litter Data Dose Lit. Spec. Cov. Est. Prob. Litter Size Expected Observed Scaled Residua 0 23.3 0.044480361 11 0.489284 0 -0.330689547 0 24.1 0.06424941 11 0.706744 0 -0.401615664 0 25.1 0.088960722 13 1.156489 2 0.353012617 0 25.8 0.10625864 8 0.850069 8 4.33673202 0 25.9 0.108729771 12 1.304757 3 0.699492477 0 26.6 0.126027689 16 2.016443 1 -0.299772055 0 26.7 0.12849882 13 1.670485 1 -0.238711127 0 26.8 0.130969952 14 1.833579 0 -0.603802545 0 26.9 0.133441083 6 0.800646 0 -0.570250323 0 27.1 0.138383345 12 1.6606 3 0.498243205 0 27.4 0.145796738 11 1.603764 0 -0.633212408 0 27.5 0.14826787 6 0.889607 0 -0.606305933 0 27.7 0.153210132 11 1.685311 2 0.121734257 0 28 0.160623525 14 2.248729 1 -0.377819018 0 28.1 0.163094657 9 1.467852 2 0.241698202 0 28.2 0.165565788 16 2.649053 1 -0.434253259 0 29 0.185334837 14 2.594688 0 -0.741848906 0 29.2 0.190277099 15 2.854156 0 -0.756724162 0 30 0.210046149 16 3.360738 1 -0.567256611 0 30.1 0.21251728 17 3.612794 3 -0.138387912 0 31.4 0.244641985 18 4.403556 18 2.76675012 35 23.1 0.420439493 2 0.840879 2 1.558208765 35 24.8 0.193667312 12 2.324008 1 -0.612920728 35 24.8 0.193667312 13 2.517675 1 -0.657368032 35 25.5 0.160429819 7 1.123009 3 1.435714172 35 25.7 0.15539473 13 2.020131 2 -0.009511434 35 26.1 0.149721705 13 1.946382 0 -0.933727752 35 26.4 0.148530963 11 1.633841 0 -0.902727468 35 26.9 0.150776303 15 2.261645 2 -0.110930327 35 27 0.151716296 14 2.124028 1 -0.503951928 35 27.4 0.156698447 13 2.03708 0 -0.959178264 35 27.4 0.156698447 10 1.566984 1 -0.331093052 35 27.5 0.158199979 16 2.5312 0 -0.995853056 35 27.5 0.158199979 13 2.0566 0 -0.964622031 35 27.7 0.16145156 14 2.260322 1 -0.550928027 35 27.9 0.164988496 13 2.14485 1 -0.527947549 35 27.9 0.164988496 13 2.14485 1 -0.527947549 35 28.1 0.168763344 15 2.53145 3 0.189788804 35 28.1 0.168763344 14 2.362687 1 -0.585185094 35 28.1 0.168763344 13 2.193923 2 -0.088622513 35 29.2 0.192293335 13 2.499813 0 -1.08570969 35 29.3 0.194583201 13 2.529582 0 -1.093706422 35 30.3 0.218173919 15 3.272609 1 -0.834803748 35 31.6 0.249793258 12 2.997519 4 0.423637452 175 23.4 0.753292803 11 8.286221 0 -2.346999161 175 25 0.450913899 14 6.312795 1 -1.033293673 175 25 0.450913899 5 2.254569 5 1.415449135 175 25.4 0.381299381 2 0.762599 2 1.466122666 175 25.5 0.365523168 2 0.731046 2 1.516399081 175 25.8 0.322690467 13 4.194976 0 -0.932876612 175 26 0.298046899 15 4.470703 0 -0.884741991 175 26.2 0.276550941 16 4.424815 2 -0.460908554 175 26.7 0.235805287 13 3.065469 1 -0.505849379 175 26.8 0.229690589 11 2.526596 2 -0.152863219 175 26.9 0.2241858 15 3.362787 1 -0.512836334 175 27.4 0.204707536 14 2.865906 0 -0.687383811 175 27.5 0.202204115 14 2.830858 1 -0.441145101 175 27.5 0.202204115 14 2.830858 1 -0.441145101 175 27.5 0.202204115 15 3.033062 0 -0.683561326 175 28.1 0.194568014 14 2.723952 1 -0.421446879 175 28.2 0.194300585 11 2.137306 0 -0.659587572 175 29 0.199087513 9 1.791788 9 2.670218904 175 29.1 0.200338227 16 3.205412 3 -0.043633258 175 29.4 0.204695235 15 3.070429 2 -0.240145327 350 21.5 0.971795484 3 2.915386 3 0.201065485 350 23 0.901250165 2 1.8025 2 0.372789514 350 24.6 0.695111669 13 9.036452 13 0.848375256 350 24.6 0.695111669 7 4.865782 1 -1.502678856 350 25.1 0.601246578 3 1.80374 3 0.961150815 350 25.1 0.601246578 11 6.613712 0 -1.565382323 350 25.3 0.562306321 14 7.872288 2 -1.085132125 350 25.4 0.542866281 1 0.542866 1 0.91764604 350 25.8 0.467290016 13 6.07477 13 1.367719528 350 26.2 0.398842995 12 4.786116 2 -0.606043119 350 26.2 0.398842995 17 6.780331 2 -0.740295677 350 26.3 0.383300844 12 4.59961 1 -0.788584398 350 26.4 0.368470315 13 4.790114 1 -0.774204472 350 27.3 0.269132881 16 4.306126 0 -0.781258285 350 27.4 0.261775084 13 3.403076 0 -0.762807027 350 27.4 0.261775084 16 4.188401 3 -0.217527974 350 27.6 0.249017755 9 2.24116 3 0.246847242 350 27.7 0.243559594 13 3.166275 0 -0.726875687 350 28.2 0.224244443 14 3.139422 14 2.387132337 350 28.8 0.214724836 16 3.435597 2 -0.281313821 350 29.2 0.214117934 13 2.783533 13 2.454127084 350 29.2 0.214117934 7 1.498826 2 0.218630258 350 29.5 0.215777472 12 2.58933 1 -0.411519634 D-42 ------- Supplemental Information ofPFBA and Related Salts D.7. DELAYED EYE OPENING-Fi MALE AND FEMALE MICE fDAS ET AL.. 20081 Table D-25. Dose-response data for delayed eye opening in male and female mice (Das et al.. 2008) Dose (mg/kg-d) n Mean SD 0 20 16.28 1.19 35 22 17.38 0.79 175 17 17.69 0.68 350 15 17.8 0.83 D-43 ------- Supplemental Information ofPFBA and Related Salts Table D-26. Benchmark dose results for delayed eye opening in male and female mice—constant variance, BMR = 5% relative deviation fDas etal.. 20081 Models Restriction 5% Relative deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Constant variance Exponential 2 (CV—normal) Restricted 252.3387 178.6688 0.0008 211.1176 Questionable Goodness-of-fit p-value < 0.1 | Residual at control | >2 Exponential 3 (CV—normal) Restricted 252.3380 178.7347 0.0008 211.1176 Questionable Goodness-of-fit p-value < 0.1 | Residual at control | >2 Exponential 4 (CV—normal) Restricted 20.4436 0.0000 0.7270 198.8811 Unusable BMD computation failed; lower limit includes zero BMDL not estimated Exponential 5 (CV—normal) Restricted 175.5239 0.0000 NA 215.6060 Unusable BMD computation failed; lower limit includes zero BMDL not estimated | Residual at control | >2 df = 0, saturated model (goodness-of-fit p-value cannot be calculated) Hill (CV—normal) Restricted 16.1508 4.8878 0.8659 198.7878 Viable- recommended Lowest AIC BMDL 3x lower than lowest nonzero dose Polynomial (3 degree) (CV—normal) Restricted 247.2477 172.9292 0.0008 210.9441 Questionable Goodness-of-fit p-value < 0.1 | Residual at control | >2 Polynomial (2 degree) (CV—normal) Restricted 247.2476 172.9292 0.0008 210.9441 Questionable Goodness-of-fit p-value < 0.1 | Residual at control | >2 Power (CV—normal) Restricted 247.2483 172.9366 0.0008 210.9441 Questionable Goodness-of-fit p-value < 0.1 | Residual at control | >2 Linear (CV—normal) Unrestricted 247.2471 172.9288 0.0008 210.9441 Questionable Goodness-of-fit p-value < 0.1 | Residual at control | >2 D-44 ------- Supplemental Information ofPFBA and Related Salts Frequentist Hill Model with BMR of 0.05 Rel. Dev. for the BMD and 0.95 Lower Confidence Limit for the BMDL Dose Figure D-5. Dose response curve for the Hill model fit to delayed eye opening in male and female mice (Das etal.. 2008). D-45 ------- Supplemental Information ofPFBA and Related Salts User Input Info Model frequentist Hill vl.l Dataset Name Das EO litter SDs User notes [Add user notes here] Dose-Response Model M[dose] = g + v*doseAn/(kAn + doseAn) Variance Model Var[i] = alpha Model Options BMR Type Rel. Dev. BMRF 0.05 Tail Probability - Confidence Level 0.95 Distribution Type Normal Variance Type Constant Model Data Dependent Variable [Dose] Independent Variable [Mean] Total # of Observations 4 Adverse Direction Automatic D-46 ------- Supplemental Information ofPFBA and Related Salts Model Results Benchmark Dose BMD 16.15084927 BMDL 4.88775303 BMDU 58.67497527 AIC 198.7877861 Test 4 P-value 0.865852068 D.O.F. 1 Model Parameters # of Parameters 5 Variable Estimate g 16.28027637 V 1.557732828 k 14.75612987 n Bounded alpha 0.771309051 Goodness of Fit Dose Size Estimated Median Calc'd Median Observed Mean Estimated SD Calc'd SD Observed SD Scaled Residual 0 20 16.28027637 16.28 16.28 0.87824202 1.19 1.19 -0.001407337 35 22 17.3760338 17.38 17.38 0.87824202 0.79 0.79 0.021182211 175 17 17.71687421 17.69 17.69 0.87824202 0.68 0.68 -0.126167037 350 15 17.77499146 17.8 17.8 0.87824202 0.83 0.83 0.110285841 Likelihoods of Interest # of Model Log Likelihood* Parameters AIC A1 -95.37962446 5 200.759249 A2 -91.88601151 8 199.772023 A3 -95.37962446 5 200.759249 fitted -95.39389305 4 198.787786 R -109.7197233 2 223.439447 * Includes additive constant of -68.00145. This constant was not included in the LL derivation prior to BMDS 3.0. Tests of Interest -2*Log(Likelihood Test Ratio) Test df p-value 1 35.6674235 6 <0.0001 2 6.987225901 3 0.07230604 3 6.987225901 3 0.07230604 4 0.028537187 1 0.86585207 D-47 ------- Supplemental Information ofPFBA and Related Salts Table D-27. Benchmark dose results for delayed eye opening in male and female mice—constant variance, BMR = 1 standard deviation fDas etal.. 20081 Models Restriction 1 Standard deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Constant variance Exponential 2 (CV—normal) Restricted 289.0417 204.0632 0.0008 211.1176 Questionable Goodness-of-fit p-value <0.1 | Residual at control | >2 Exponential 3 (CV—normal) Restricted 289.0397 204.0631 0.0008 211.1176 Questionable Goodness-of-fit p-value <0.1 | Residual at control | >2 Exponential 4 (CV—normal) Restricted 23.0895 12.5328 0.7270 198.8811 Viable- recommended Lowest AIC Exponential 5 (CV—normal) Restricted -9,999.0000 0.0000 NA 215.6060 Unusable BMD computation failed BMD not estimated BMDL not estimated | Residual at control | >2 df= 0,saturated model (goodness-of-fit p-value cannot be calculated) Hill (CV—normal) Restricted 19.0723 0.0000 0.8659 198.7878 Unusable BMD computation failed; lower limit includes zero BMDL not estimated Polynomial (3 degree) (CV—normal) Restricted 284.0211 198.2059 0.0008 210.9441 Questionable Goodness-of-fit p-value <0.1 | Residual at control | >2 Polynomial (2 degree) (CV—normal) Restricted 284.0211 198.2059 0.0008 210.9441 Questionable Goodness-of-fit p-value <0.1 | Residual at control | >2 Power (CV—normal) Restricted 284.0218 198.2009 0.0008 210.9441 Questionable Goodness-of-fit p-value <0.1 | Residual at control | >2 Linear (CV—normal) Unrestricted 284.0204 198.2054 0.0008 210.9441 Questionable Goodness-of-fit p-value <0.1 | Residual at control | >2 D-48 ------- Supplemental Information ofPFBA and Related Salts D.8. VAGINAL OPENING-Fi FEMALE MICE fDAS ET AL.. 20081 Table D-28. Dose response data for delayed vaginal opening in female mice fDas et al.. 20081 Dose (mg/kg-d) n Mean SD 0 83 31.59 5.386 35 97 33.598 5.715 175 89 34.292 5.714 350 87 35.023 5.188 Table D-29. Benchmark dose results for delayed vaginal opening in female mice—constant variance, 5% relative deviation (Das et al.. 2008) Models Restriction 5% Relative deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Constant variance Exponential 2 (CV—normal) Restricted 199.6149 137.1410 0.0106 348.8761 Questionable Goodness-of-fit p-value < 0.1 | Residual at control | >2 Exponential 3 (CV—normal) Restricted 199.6216 137.1431 0.0106 348.8761 Questionable Goodness-of-fit p-value < 0.1 | Residual at control | >2 Exponential 4 (CV—normal) Restricted 17.1139 0.0000 0.6944 341.9320 Unusable BMD computation failed; lower limit includes zero BMDL not estimated Exponential 5 (CV—normal) Restricted 30.5201 0.0000 NA 343.9392 Unusable BMD computation failed; lower limit includes zero BMDL not estimated df = 0, saturated model (goodness-of-fit p-value cannot be calculated) Hill (CV—normal) Restricted 13.5161 3.7929 0.8401 341.8184 Viable- recommended Lowest AIC BMDL 3x lower than lowest nonzero dose Polynomial (3 degree) (CV—normal) Restricted 193.4400 130.5619 0.0115 348.7113 Questionable Goodness-of-fit p-value < 0.1 | Residual at control | >2 D-49 ------- Supplemental Information ofPFBA and Related Salts Models Restriction 5% Relative deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Polynomial (2 degree) (CV—normal) Restricted 193.4443 130.5615 0.0115 348.7113 Questionable Goodness-of-fit p-value < 0.1 | Residual at control | >2 Power (CV—normal) Restricted 193.4434 130.5626 0.0115 348.7113 Questionable Goodness-of-fit p-value < 0.1 | Residual at control | >2 Linear (CV—normal) Unrestricted 193.4436 130.5610 0.0115 348.7113 Questionable Goodness-of-fit p-value < 0.1 | Residual at control | >2 Figure D-6. Dose response curve for the Hill model fit to delayed vaginal opening in female mice fDas et al.. 20081. D-50 ------- Supplemental Information ofPFBA and Related Salts User Input Info Model frequentist Hill vl.l Dataset Name Das VO litter SDs User notes [Add user notes here] Dose-Response Model M[dose] = g + v*doseAn/(kAn + doseAn) Variance Model Var[i] = alpha Model Options BMR Type Rel. Dev. BMRF 0.05 Tail Probability - Confidence Level 0.95 Distribution Type Normal Variance Type Constant Model Data Dependent Variable [Dose] Independent Variable [Mean] Total # of Observations 4 Adverse Direction Automatic D-51 ------- Supplemental Information ofPFBA and Related Salts Model Results Benchmark Dose BMD 13.51609885 BMDL 3.792905489 BMDU 58.81907947 AIC 341.8183924 Test 4 P-value 0.840124836 D.O.F. 1 Model Parameters # of Parameters 5 Variable Estimate g 31.25160173 V 3.782877454 k 19.2052612 n Bounded alpha 6.040525655 Goodness of Fit Dose Size Estimated Median Calc'd Median Observed Mean Estimated SD Calc'd SD Observed SD Scaled Residual 0 19 31.25160173 31.25 31.25 2.45774809 2.62 2.62 -0.002840717 35 21 33.69418217 33.71 33.71 2.45774809 2.59 2.59 0.029493016 175 17 34.66038453 34.57 34.57 2.45774809 2.59 2.59 -0.151628625 350 15 34.83770206 34.92 34.92 2.45774809 2.23 2.23 0.129687238 Likelihoods of Interest # of Model Log Likelihood* Parameters AIC A1 -166.8888479 5 343.777696 A2 -166.5982185 8 349.196437 A3 -166.8888479 5 343.777696 fitted -166.9091962 4 341.818392 R -177.364099 2 358.728198 * Includes additive constant of -66.16357. This constant was not included in the LL derivation prior to BMDS 3.0. Tests of Interest -2*Log(Likelihood Test Ratio) Test df p-value 1 21.53176107 6 0.00147157 2 0.581258883 3 0.900709 3 0.581258883 3 0.900709 4 0.040696527 1 0.84012484 D-52 ------- Supplemental Information ofPFBA and Related Salts Table D-30. Benchmark dose results for delayed vaginal opening in female mice—constant variance, 1 standard deviation fDas etal.. 20081 Models Restriction 1 Standard deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Constant variance Exponential 2 (CV—normal) Restricted 316.9350 218.4320 0.0106 348.8761 Questionable Goodness-of-fit p-value < 0.1 | Residual at control | >2 Exponential 3 (CV—normal) Restricted 316.9457 218.4320 0.0106 348.8761 Questionable Goodness-of-fit p-value < 0.1 | Residual at control | >2 Exponential 4 (CV—normal) Restricted 35.1705 15.4720 0.6944 341.9320 Viable- recommended Lowest AIC Exponential 5 (CV—normal) Restricted 34.9991 15.4632 NA 343.9392 Questionable df = 0, saturated model (goodness-of-fit p-value cannot be calculated) Hill (CV—normal) Restricted 35.6204 0.0000 0.8401 341.8184 Unusable BMD computation failed; lower limit includes zero BMDL not estimated Polynomial (3 degree) (CV—normal) Restricted 311.4806 211.1287 0.0115 348.7113 Questionable Goodness-of-fit p-value < 0.1 | Residual at control | >2 Polynomial (2 degree) (CV—normal) Restricted 311.4877 211.1313 0.0115 348.7113 Questionable Goodness-of-fit p-value < 0.1 | Residual at control | >2 Power (CV—normal) Restricted 311.4864 211.1303 0.0115 348.7113 Questionable Goodness-of-fit p-value < 0.1 | Residual at control | >2 Linear (CV—normal) Unrestricted 311.4866 211.1307 0.0115 348.7113 Questionable Goodness-of-fit p-value < 0.1 | Residual at control | >2 D-53 ------- Supplemental Information ofPFBA and Related Salts D.9. PREPUTIAL SEPARATION—Fi MALE MICE fDAS ET AL.. 20081 Table D-31. Dose-response data for delayed preputial separation in male mice fDas etal.. 20081 Dose (mg/kg-d) n Mean SD 0 17 29.55 1.14 35 21 30.21 1.99 175 17 30.56 1.84 350 15 31.88 1.72 Table D-32. Benchmark dose results for delayed preputial separation in male mice—constant variance, BMR = 5% relative deviation (Das et al.. 2008) Models Restriction 5% Relative deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Constant variance Exponential 2 (CV—normal) Restricted 254.8183 179.1436 0.6004 277.5960 Viable—alternate Exponential 3 (CV—normal) Restricted 254.8005 179.1431 0.6004 277.5960 Viable—recommended Lowest AIC Exponential 4 (CV—normal) Restricted 252.8480 102.0115 0.3080 279.6149 Viable—alternate Exponential 5 (CV—normal) Restricted 252.5410 101.9527 0.3076 279.6166 Viable—alternate Hill (CV—normal) Restricted 194.2094 175.4639 0.2286 280.0252 Viable—alternate Polynomial (3 degree) (CV—normal) Restricted 276.4524 176.5648 0.3427 279.4759 Viable—alternate Polynomial (2 degree) (CV—normal) Restricted 269.5337 175.9153 0.3268 279.5372 Viable—alternate Power (CV—normal) Restricted 252.7648 175.1179 0.5950 277.6140 Viable—alternate Linear (CV—normal) Unrestricted 252.7653 175.1182 0.5950 277.6140 Viable—alternate D-54 ------- Supplemental Information ofPFBA and Related Salts Frequentist Exponential Degree 3 Model with BMR of 0.05 Rel, Dev. for the BMD and 0.95 Lower Confidence Limit for the BMDL 34 33 32 — tstimated Probability Response at BMD O Data — BMD BMDL Figure D-7. Dose response curve for the Exponential 3 model fit to delayed preputial separation in male mice fDas et al.. 20081. D-55 ------- Supplemental Information ofPFBA and Related Salts User Input Info Model frequentist Exponential degree 3 vl.l Dataset Name Das PS litter SDs User notes [Add user notes here] Dose-Response Model M[dose] = a * exp(±l * (b * dose)Ad) Variance Model Var[i] = alpha Model Options BMR Type Rel. Dev. BMRF 0.05 Tail Probability - Confidence Level 0.95 Distribution Type Normal Variance Type Constant Model Data Dependent Variable [Dose] Independent Variable [Mean] Total # of Observations 4 Adverse Direction Automatic D-56 ------- Supplemental Information ofPFBA and Related Salts Model Results Benchmark Dose BMD 254.8005164 BMDL 179.1431485 BMDU 443.2041287 AIC 277.5960319 Test 4 P-value 0.600364435 D.O.F. 2 Model Parameters # of Parameters 4 Variable Estimate a 29.74458616 b 0.000191484 d Bounded log-alpha 1.042066246 Goodness of Fit Dose Size Estimated Median Calc'd Median Observed Mean Estimated SD Calc'd SD Observed SD Scaled Residual 0 17 29.74458616 29.55 29.55 1.68376629 1.14 1.14 -0.47649088 35 21 29.94460185 30.21 30.21 1.68376629 1.99 1.99 0.722313504 175 17 30.75820529 30.56 30.56 1.68376629 1.84 1.84 -0.485353184 350 15 31.80636595 31.88 31.88 1.68376629 1.72 1.72 0.169372344 Likelihoods of Interest # of Model Log Likelihood* Parameters AIC A1 -135.2877975 5 280.575595 A2 -132.4445224 8 280.889045 A3 -135.2877975 5 280.575595 fitted -135.7980159 3 277.596032 R -142.6419354 2 289.283871 * Includes additive constant of -64.3257. This constant was not included in the LL derivation prior to BMDS 3.0. Tests of Interest -2*Log(Likelihood Test Ratio) Test df p-value 1 20.39482594 6 0.00235492 2 5.686550161 3 0.12789698 3 5.686550161 3 0.12789698 4 1.020436835 2 0.60036443 D-57 ------- Supplemental Information ofPFBA and Related Salts Table D-33. Benchmark dose results for delayed preputial separation in male mice—constant variance, BMR = 1 standard deviation fDas et al.. 20081 Models Restriction 1 Standard deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Constant variance Exponential 2 (CV—normal) Restricted 287.5467 201.6707 0.6004 277.5960 Viable—alternate Exponential 3 (CV—normal) Restricted 287.5612 201.6697 0.6004 277.5960 Viable—recommended Lowest AIC Exponential 4 (CV—normal) Restricted 286.3951 198.7931 0.3080 279.6149 Viable—alternate Exponential 5 (CV—normal) Restricted 286.1679 197.6553 0.3076 279.6166 Viable—alternate Hill (CV—normal) Restricted 201.3711 94.7311 0.2286 280.0252 Viable—alternate Polynomial (3 degree) (CV—normal) Restricted 302.3780 199.5688 0.3427 279.4759 Viable—alternate Polynomial (2 degree) (CV—normal) Restricted 297.6581 198.8516 0.3268 279.5372 Viable—alternate Power (CV—normal) Restricted 286.2526 197.9759 0.5950 277.6140 Viable—alternate Linear (CV—normal) Unrestricted 286.2531 197.9763 0.5950 277.6140 Viable—alternate D.10. RELATIVE LIVER WEIGHT-MALE HUMANIZED PPARA MICE fFOREMAN ET AL.. 20091 Table D-34. Dose-response data for relative liver weight in male humanized PPARa mice fForeman et al.. 20091 Dose (mg/kg-d) n Mean SD 0 10 4.07 0.261 35 10 5.62 0.719 175 10 6.65 0.784 350 10 7.38 0.719 D-58 ------- Supplemental Information ofPFBA and Related Salts Table D-35. Benchmark dose results for relative liver weight in male humanized PPARa mice —nonconstant variance, BMR = 10% relative deviation fForeman et al.. 20091 Models Restriction 10% Relative deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Nonconstant variance Exponential 2 (NCV—normal) Restricted 77.3820 62.7400 <0.0001 107.4138 Questionable Goodness-of-fit p-value <0.1 | Residual at control | >2 Modeled control response SD >| 1.51 actual response SD Exponential 3 (NCV—normal) Restricted 77.3912 62.7399 <0.0001 107.4138 Questionable Goodness-of-fit p-value <0.1 | Residual at control | >2 Modeled control response SD >| 1.51 actual response SD Exponential 4 (NCV—normal) Restricted 6.7656 4.8076 0.0951 80.0462 Questionable Goodness-of-fit p-value <0.1 BMD 3x lower than lowest nonzero dose BMDL 3x lower than lowest nonzero dose Exponential 5 (NCV—normal) Restricted 6.7678 4.8076 0.0951 80.0462 Questionable Goodness-of-fit p-value <0.1 BMD 3x lower than lowest nonzero dose BMDL 3x lower than lowest nonzero dose Hill (NCV—normal) Restricted 5.4945 4.4070 0.2883 78.3878 Viable- recommended Lowest AIC BMD 3x lower than lowest nonzero dose BMDL 3x lower than lowest nonzero dose Polynomial (3 degree) (NCV—normal) Restricted 59.5695 46.0032 <0.0001 104.4698 Questionable Goodness-of-fit p-value <0.1 | residual for dose group near BMD| >2 | residual at control | >2 Modeled control response SD >| 1.51 actual response SD D-59 ------- Supplemental Information ofPFBA and Related Salts Models Restriction 10% Relative deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Nonconstant variance Polynomial (2 degree) (NCV—normal) Restricted 59.5723 46.0033 <0.0001 104.4698 Questionable Goodness-of-fit p-value <0.1 | residual for dose group near BMD| >2 | residual at control | >2 Modeled control response SD >| 1.51 actual response SD Power (NCV—normal) Restricted 59.5691 46.0034 <0.0001 104.4698 Questionable Goodness-of-fit p-value <0.1 | residual for dose group near BMD| >2 | residual at control | >2 Modeled control response SD >| 1.51 actual response SD Linear (NCV—normal) Unrestricted 59.5725 46.0031 <0.0001 104.4698 Questionable Goodness-of-fit p-value <0.1 | residual for dose group near BMD| >2 | residual at control | >2 Modeled control response SD >| 1.51 actual response SD D-60 ------- Supplemental Information ofPFBA and Related Salts D.ll. RELATIVE LIVER WEIGHT-MALE RATS EXPOSED 28 DAYS fBUTENHOFF ET AL.. 2012: VAN OTTERDIIK. 2007B1 Table D-36. Dose-response data for relative liver weight in male rats following 28 day exposure (Butenhoff et al.. 2012: van Otterdijk. 2007b) Dose (mg/kg-d) n Mean SD 0 10 2.42 0.17 1.2 10 2.55 0.25 6 10 3 0.33 30 10 3.59 0.46 Table D-37. Benchmark dose results for relative liver weight in male rats exposed 28 days—nonconstant variance, BMR = 10% relative deviation (Butenhoff et al.. 2012: van Otterdijk. 2007b) (Das et al.. 2008) Models Restriction 10% Relative deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Nonconstant variance Exponential 2 (NCV—normal) Restricted 39.0522 30.9899 0.0010 30.9052 Questionable Goodness of fit p- value < 0.1 | Residual for Dose Group Near BMD| >2 Modeled control response std. dev. >| 1.51 actual response std. dev. Exponential 3 (NCV—normal) Restricted 39.0519 30.9899 0.0010 30.9052 Questionable Goodness of fit p- value < 0.1 | Residual for Dose Group Near BMD| >2 Modeled control response std. dev. >| 1.51 actual response std. dev. Exponential 4 (NCV—normal) Restricted 9.9467 6.3433 0.9596 19.1475 Viable - Recommended Lowest AIC Exponential 5 (NCV—normal) Restricted 10.1350 6.3447 NA 21.1450 Questionable d.f.=0, saturated model (Goodness of fit test cannot be calculated) D-61 ------- Supplemental Information ofPFBA and Related Salts (Das et al., 2008) Models Restriction 10% Relative deviation p-Value AIC BMDS classification BMDS notes BMD BMDL Nonconstant variance Hill (NCV—normal) Restricted 9.9219 5.3433 NA 21.1450 Questionable d.f.=0, saturated model (Goodness of fit test cannot be calculated) Polynomial (3 degree) (NCV—normal) Restricted 31.8784 23.5467 0.0028 28.8760 Questionable Goodness of fit p- value < 0.1 | Residual for Dose Group Near BMD| >2 Polynomial (2 degree) (NCV—normal) Restricted 31.8784 23.5468 0.0028 28.8760 Questionable Goodness of fit p- value < 0.1 | Residual for Dose Group Near BMD| >2 Power (NCV—normal) Restricted 31.8784 23.5470 0.0028 28.8760 Questionable Goodness of fit p- value < 0.1 | Residual for Dose Group Near BMD| >2 Linear (NCV—normal) Unrestricted 31.8784 23.5468 0.0028 28.8760 Questionable Goodness of fit p- value < 0.1 | Residual for Dose Group Near BMD| >2 D-62 ------- Supplemental Information ofPFBA and Related Salts APPENDIX E. SUMMARY OF PUBLIC AND EXTERNAL PEER REVIEW COMMENTS AND EPA'S DISPOSITION The Toxicological Review of Perfluorobutanoic Acid and Related Salts was released for public comment in August 2021. Public comments on the assessment were submitted to the U.S. Environmental Protection Agency (EPA) by November 8, 2021. The Toxicological Review has also undergone a formal external peer review in accordance with U.S. Environmental Protection Agency (EPA) guidance on peer review fU.S. EPA. 20151. A public, external peer-review meeting was held February 22 and 23, 2022, which included another opportunity for public comment. The external peer reviewers were tasked with providing written answers to general questions on the overall assessment approach, key conclusions, and areas of scientific controversy or uncertainty. A summary of comments made by the external peer reviewers and public commenters, as well as EPA's responses to these comments, are arranged by charge question as follows. In many cases, the comments of the individual external reviewers have been synthesized and paraphrased for brevity (please consult the final peer review report for the full text of the panel's comments: Peer Review Report! External Peer Reviewers were asked to prioritize their comments to indicate their relative importance. The prioritization instructions are duplicated below from the IRIS PFBA charge questions to the peer reviewers, which can be found in the public EPA docket: EPA-HO-QRD-2020- 0675: Tier 1: Recommended Revisions - Key major recommendations necessary for strengthening the scientific basis for the Toxicological Review ofPFBA. The implication of such key Tier 1 recommendations is that the assessment conclusions are not adequately supported without addressing the recommendations and need to be reconsidered or better substantiated. For Tier 1 recommendations, please describe the specific revisions necessary to modify or better substantiate the most scientifically appropriate assessment conclusions. Tier 2: Suggestions - Recommendations that are encouraged to strengthen the scientific analyses and conclusions in the Toxicological Review ofPFBA. That other factor (e.g., timeliness) also may also be considered before deciding to address or incorporate Tier 2 suggestions is understood. For Tier 2 recommendations, please provide specific suggestions to strengthen the scientific basis for assessment conclusions or improve the clarity of the analyses and presentation. Tier 3: Future Considerations - Scientific exploration that might inform future work. These recommendations are outside the immediate scope or needs of the current document under review but could inform future toxicological reviews or research efforts E-l ------- Supplemental Information ofPFBA and Related Salts Appendix E lists all Tier 1 recommendations and Tier 2 Suggestions from the external peer reviewers organized by charge question. For Tier 3 Considerations, please refer to the external peer review report linked above. Where public comments were made on topics raised by the external peer reviewers, they are noted alongside the external peer review comments. All Tier 1 recommendations were implemented in this revised assessment, either through revision or addition to the peer reviewed analyses or text. Tier 2 suggestions were considered in light of the extent to which those suggestions would impact the conclusions or quantitative analyses of the assessment, consistency across panelists in raising the suggestion, and the level of effort to implement For this assessment, all Tier 2 suggestions deemed to be impactful to the toxicity value conclusions were implemented in this revised assessment Additional public comments not raised by the peer reviewers are included in a separate section at the end of each charge question section. Where possible, the public comments have been reproduced in this Appendix as they were submitted, but in some cases have synthesized and paraphrased for brevity. A summary document collating all public comments was provided as a courtesy to the external peer review panel. Please see docket EPA-HO-QRD-2020-0675 for both this summary document and the full text of the submitted public comments. External peer reviewer and public comments regarding requests for additions of clarifying text or editorial or grammatical corrections have been made throughout the assessment as appropriate; these comments and responses have not been tracked in this Appendix. E.l. CHARGE QUESTION 1 - SYSTEMATIC REVIEW The Toxicological Review describes and applies a systematic review process for identifying and screening pertinent studies that is described in detail in Section 1.2.1 (Literature Search and Screening) and Appendix A (Systematic Review Protocol for the PFBA, PFHxA, PFHxS, PFNA, and PFDA IRIS Assessments). Please comment on whether the search strategy and screening criteria for PFBA are appropriate and clearly described. Please identify additional peer-reviewed studies ofPFBA that the assessment should incorporate2. E.l.l. Overarching External Peer Reviewer Comments on Systematic Review "All reviewers agreed that the literature search was well done, noting that it was comprehensive and that the methods used were appropriate and clearly described. They also stressed how challenging it is to conduct a thorough literature search in such a rapidly evolving field, where information may be out of date in a matter of months or even weeks." 2 Newly identified studies (i.e., studies identified by EPA or the public that meet PECO criteria but were not addressed in the external review draft, for example due to recent publication) will be characterized by EPA and presented to the peer review panel. This characterization will focus on EPA's judgment of whether the studies would have a material impact on the conclusions (i.e., identified hazards or toxicity values) in the external review draft. The peer review panel is asked to review EPA's characterization and provide tiered recommendations to EPA regarding which studies, if any, to incorporate into the assessment before finalizing. E-2 ------- Supplemental Information ofPFBA and Related Salts E.1.2. Tier 1 Recommendations Comment: EPA should clarify when and how papers identified from the related systematic reviews for the other PFAS compounds were included in the PFBA toxicological review. EPA could provide this clarification by adding a small section and/or a table describing how the health effects text in the PFBA report was similar or was supported by the application of information from the review of related PFAS compounds. EPA Response: Section 1.2.1 "Literature Search and Screening" describes the identification of studies during problem formulation, scoping and title/abstract screening for other PFAS that are relevant to the PFBA toxicological review. Specifically, some studies relevant to PFBA were identified by searches focused on the other four PFAS currently being assessed by the Integrated Risk Information System (IRIS) Program (i.e., PFHxA, PFHxS, PFNA, and PFDA) or from other authoritative reviews (e.g., final EPA reviews). This mostly applied to epidemiological studies as animal and mechanistic studies on specific PFAS are better indexed by specific PFAS. In addition, Table 4-2 has been added to Section 4.1 to demonstrate similarities and differences (contingent on the availability of data) in the health effects observed across the EPA PFAS human health assessments published at the time of finalization of the PFBA assessment As EPA finalizes more PFAS assessments, this table will be expanded in subsequent IRIS assessments. Comment: Multiple reviewers recommended EPA update the literature search to include the most up-to-date set of studies. Specifically, one reviewer recommended that EPA incorporate the Weatherly etal. (2021) study before finalizing the Toxicological Review. Multiple public comments were also received recommending that EPA update its literature search and incorporate relevant studies (including Weatherly et al., 2021). Public comments also recommended that EPA explicitly state the date of the last literature search used for the Toxicological Review. EPA Response: The date of the last literature search used for the Toxicological Review (April 2021) was added to Section 2.1. Updates to the literature incorporated into the public comment draft (after the last literature update) are reflected in a separate document posted to the docket ("EPA-HO-ORD-2020-0675-0022") and provided to the peer reviewers. This document describes the consideration of the studies deemed relevant based on the methods laid out in the protocol and documents the justification for the subset of those incorporated into the revised assessment. A specific charge question was posed to the peer reviewers on these decisions and no disagreements were noted in the panel's final comments. The Weatherly et al. (2021) study was added to the assessment given it was specifically identified by the peer review panel (see Sections 3.2.2, 3.2.5, and 5.2.1). E-3 ------- Supplemental Information ofPFBA and Related Salts Comment: To improve access to the studies identified, one reviewer recommended that EPA (1) develop a simple table explicitly listing all the in vitro, in silico, or nonmammalian model "supplemental material" studies that were considered and selected, and (2) develop a simple table listing all the studies that were considered but not selected, that also briefly identifies the reasons for rejecting each of these studies. Public comments were also received requesting EPA make available the lists of included and supplemental studies and to ensure that the list of studies in HAWC are accurate. EPA Response: The included, excluded and supplemental studies can be found in HERO (https://hero.epa.gov/hero/index.cfm/proiect/page/search/true/isws/false/proiect id/26 32 /1. With respect to inclusion or exclusion, studies are excluded if they do not meet all PECO criteria. During screening, most studies are excluded because they do not meet any or only meet a few of the PECO criteria. Thus, a single screened out study typically has multiple reasons for exclusion which is unwieldy to document, especially at the title and abstract level when screening may be needed for thousands of studies. The annotation used in the assessment is consistent with the convention in systematic review (Page etal.. 20211. Note also that multiple tags may be applied to a single study (e.g., tagged "supplemental" during title/abstract and "in vitro" during full-text screening) which results in potential discrepancies when cross referencing numbers between HERO and the literature flow diagrams or HAWC study evaluation heatmaps. E.1.3. Tier 2 Suggestions Comment: EPA should add an introductory preview on how it is approaching PFBA in relation to other forms of PFAS that have been much more extensively studied. EPA Response: Text was added to Section 1.2.1 "Literature Search and Screening" explaining that relevant literature on PFBA was identified by searches focused on the other four PFAS currently being assessed by the Integrated Risk Information System (IRIS) Program (i.e., PFHxA, PFHxS, PFNA, and PFDA) or from other authoritative reviews (e.g., final EPA reviews). Table 4-2 has been added to Section 4.1 to demonstrate similarities and differences (contingent on the availability of data) in the health effects observed across the EPA PFAS human health risk assessments published at the time of finalization of the PFBA assessment As EPA finalizes more PFAS assessments, this table will be expanded in subsequent IRIS assessments. Comment: One reviewer suggested, as an enhancement to the added table (listing all the in vitro, in silico, or nonmammalian model "supplemental material" studies) recommended in the Tier 1 recommendation above, EPA should incorporate columns (a) summarizing qualitatively the confidence (low, medium, high) associated with the information presented E-4 ------- Supplemental Information ofPFBA and Related Salts in each study, and (b) listing potential outcomes associated with the "supplemental material" studies. EPA Response: Confidence in studies meeting PECO criteria is documented in HAWC fhttps: //hawc.epa.gov/study/assessment/100500073/1. and several additions were made in this revised assessment to ensure that the health outcome-specific confidence for these studies is conveyed in the figures or text of the relevant synthesis sections. Studies that are identified as potentially relevant supplemental material (e.g., mechanistic, pharmacokinetic) can be found in HERO. Comment: Numerical inconsistencies in the number of studies listed in Figures 2-1, 2-2, and 2-3, the number of studies discussed in the text of the Toxicological Review, and the number of studies listed in HAWC should be corrected (a Tier 1 recommendation on this topic was also provided under Charge Question 2 below). Public comments were also received recommending that EPA ensure that all numbers of studies are properly reported within the document, figures, tables, and associated meta-data. EPA Response: Eight epidemiology studies and seven animal studies were identified as meeting the PECO criteria following full-text review. Nine animal studies are listed in Figure 2-1 which includes the Butenhoff et al. (20121 study which reported the findings of two unpublished industry reports: a 28-day and 90-day gavage study fully reported in (van Otterdiik. 2007a. b). These industry reports were conducted at the same facility and largely by the same staff but independently of one another and at different times: July 26, 2006, through September 15, 2006, for the 28-day study and April 5, 2007, through August 6, 2007, for the 90-day study. Throughout the Toxicological Review, both fButenhoff et al.. 20121 and the relevant industry report are cited when discussing effects observed in these reports. However, only one study evaluation was performed for this group of citations in HAWC (see Figure 2-2), the overall confidence level of high applies to both the 28-day and 90-day reports and grouping of these studies accounts for the discrepancy between the number of animal studies in Figures 2-1 and 2-2. Comment: EPA could add a statement about what kind of information would be required to change the overall analysis/conclusions, with a clearer description of when updates will be made. EPA Response: With respect to information to change overall analysis or conclusions, this is implicit in the evidence synthesis and integration analysis. For example, conclusions of "evidence inadequate" are reached after describing specific limitations to the evidence base. These limitations can be translated by the research community into information gaps that, if filled, could potentially change an overall analysis or conclusion. Presentation of uncertainty E-5 ------- Supplemental Information ofPFBA and Related Salts factors is another area in the IRIS assessment that provides an indication of information that could be impactful to change an overall analysis/conclusion. Once the IRIS Toxicological Review of PFBA is finalized, the IRIS program has no immediate plans on updating the assessment. Given the finite resources of the IRIS Program, IRIS assessment activities are based on the priority needs of EPA National Program and Regional Offices identified through a structured internal (to EPA) nomination process. Comment: EPA could consider providing a brief discussion of what is known (and not known) to help inform animal-to-human extrapolation. For example, the relevance of PPAR as a mode of action is an important point and the degree to which it is or is not relevant to humans could be mentioned at the outset Similarly, the dramatic sex differences in some rodents are clearly not applicable to humans for other forms of PFAS and presumably not for PFBA either. EPA Response: The human relevance of the animal data is explicitly addressed within the context of the evidence available to inform each individual hazard. However, without specific evidence to the contrary, effects in animals are presumed relevant to humans (U.S. EPA. 2005.1998.1991). Once a determination is made that an effect is considered relevant to humans using the currently available evidence, the quantitative implications of the remaining uncertainties in extrapolation are addressed through dosimetric adjustment and application of the UFa during dose-response analysis. Comment: EPA could consider adding a section that discusses available information on PFBA's potential immunomodulation (immunosuppression) effects. Existing studies most probably cannot support derivation of relevant reference values, but compilation and evaluation of the available information can provide an initial framework for addressing this challenge in future revisions. EPA Response: A discussion of potential immunomodulation was added to Section 3.2.5 "Other Non-Health Effects." Comment: PFAS information submitted to IRIS should be available to all EPA programs and vice versa. EPA Response: IRIS assessments rely on publicly available information in the published literature and can potentially include information submitted to EPA programs (e.g., TSCA), if those data can be made publicly available. E-6 ------- Supplemental Information ofPFBA and Related Salts Comment: EPA should correct the PECO element Exposures statement that incorrectly suggests that the 6:2fluorotelomer is metabolized into two analytes; it is in fact multiple analytes. EPA Response: The IRIS PFAS protocol states (text of interest underlined) the following: "[Note: although while these PFAS are not metabolized or transformed in the body, there are precursor compounds known to be biotransformed to a PFAS of interest; for example, 6:2 fluorotelomer alcohol is metabolized to PFHxA and PFBA (Russell etal.. 20151. Thus, studies of precursor PFAS that identify and quantify a PFAS of interest will be tracked as potential supplemental material (e.g., for ADME analyses or interpretations)]". This text does not preclude that this compound can be metabolized to other analytes; it is simply emphasizing those analytes of interest to the protocol, namely PFBA, PFHxA, PFHxS, PFNA, or PFDA. However, a small editorial change to the text was made for clarity. E.1.4. Public Comments Comment: EPA improperly excluded its own relevant studies (i.e., Das et al., 2008) in developing the draft IRIS review. In the Draft IRIS Review, EPA made numerous comparisons between PFBA, a four carbon perfluoroalkyl carboxylate, and perfluorobutanesulfonate (PFBS), a four-carbon perfluoroalkyl sulfonate congener. While both PFBA and PFBS have generally been considered short-chain PFAS compounds given the relatively short serum elimination half-lives in the species evaluated (rodents, non- human primates, and humans), EPA leaned too heavily on this similarity and ignored relevant data available for PFBA itself. EPA Response: This comment implies that the draft assessment did not include the Das et al. f20081 mouse developmental toxicity study in the PBFA assessment This is incorrect. Section 5 indicates that multiple effects from Das etal. f20081 were modeled and considered for RfD derivation. Additionally, the consideration of data regarding the toxicological effects of PFBS in the PFBA Toxicological Review is consistent with methods described in Appendix A (Protocol) supporting the consideration of data on similar chemicals to inform PFBA-specific data gaps. Thus, PFBS data is described in the PFBA assessment in cases where data was lacking for PFBA or when drawing parallels between chemicals was useful in discussing potentially consistent toxicological effects across PFAS. That said, PFBS data were not used in the PFBA assessment for quantitative purposes or toxicity value derivation, nor were they necessary to draw the evidence integration conclusions regarding PFBA, which were sufficiently supported by PFBA-specific data. E-7 ------- Supplemental Information ofPFBA and Related Salts Comment: In analyzing the potential health effects of PFBA, the draft assessment makes several comparisons to data available for other PFAS. While such a "read-across" approach can be a useful in qualitatively assessing the potential for a compound to impact health endpoints, it is important that the comparison be made to compounds that are as structurally similar to the compound of interest as possible and, when appropriate, to indicate how structural differences may impact ability to compare the toxicokinetics, target organs, critical effects, potential molecular targets, and shapes of the dose-response curves. In the case ofPFBA, other short-chain (<8 carbons) carboxylates are the most appropriate for comparison. Consequently, comparison to perfluorohexanoic acid (PFHxA) would be more appropriate than to a sulfonic acid like perfluorobutyl sulfonate (PFBS). In this regard, the lack of observed significant developmental effects associated with PFHxA is noted. EPA Response: As noted above, the IRIS PFBA assessment considers the data available on other PFAS to inform PFBA-specific data gaps, with an emphasis on and increased use of data and judgments on PFAS for which EPA has available a final assessment at the time of developing the PFBA assessment. It is important to emphasize that EPA has not reached a final conclusion on whether the evidence supports a "lack of observed significant developmental effects associated with PFHxA." EPA's IRIS PFHxA assessment is still under development Comment: EPA should provide further clarification and better reporting when multiple publications of the same data are included. For example, the studies reported as van Otterdijk 2007c and van Otterdijk 2007d are industry documents available in EPA's HERO database but have also been published in the peer reviewed literature in the study by Butenhoff etal. 2012. That these studies contain overlapping and duplicative data, should be more clearly noted in the literature flow diagram (Figure 2-1) and the discussion of Study Evaluation Results in Section 2.2. EPA Response: This is noted in Section 3.2.1 "Non-Cancer Evidence Synthesis and Integration" (footnote 11). Additional clarification was also added to Study Evaluation Results in Section 2.2: "The studies meeting PECO criteria at the full-text level included eight epidemiological studies, nine animal studies (including one published study [Butenhoff et al. (2012)] that reported on the same data in two unpublished industry reports [fvan Otterdiik. 2007al and fvan Otterdiik. 2007bl]." E.2. CHARGE QUESTION 2 - STUDY EVALUATION The Toxicological Review describes the results of the evaluations of individual studies in Section 2.2 (Study Evaluation Results) and presents and analyzes the findings from those studies deemed informative in the relevant health effect-specific synthesis sections. E-8 ------- Supplemental Information ofPFBA and Related Salts a. Please comment on whether the study confidence conclusions for the PFBA studies are scientifically justifiedgiving appropriate consideration to important methodological features of the assessed outcomes. Please specify any study confidence conclusions that are not justified and explain any alternative study evaluation decisions. b. Results from individual PFBA studies are presented and synthesized in the health system- specific sections. Please comment on whether the presentation and analysis of study results is clear, appropriate, and effective to allow for scientifically supported syntheses of the findings across sets of studies. E.2.1. Overarching External Peer Reviewer Comments on Study Evaluation "Reviewers agreed that the confidence conclusions were scientifically justified, and that Section 2.2 was well done. Reviewers noted that the scientific justification presented was clear and effective, and found that the interactive visualizations provided a convenient overview. [One reviewer] also found it very beneficial that EPA presented the logic for giving more or less attention to particular studies and specific outcomes." E.2.2. Tier 1 Recommendations Comment: EPA should correct numerical inconsistencies in the number of studies listed in the Figures 2-1, 2-2, and 2-3, the number of studies discussed in the text of the Toxicological Review, and the number of studies listed in HAWC. (a Tier 2 suggestion on this topic was also provided under Charge Question 1 above). EPA Response: See EPA Response to Charge Question 1 above and referenced in footnote 11 of the Toxicological Review which states "Eight epidemiology studies and seven animal studies were identified as PECO relevant following full-text review. Nine animal studies are listed in Figures 2-1 which includes the Butenhoff et al. f20121 study which reported the findings of two unpublished industry reports: a 28-day and 90-day gavage study fully reported in fvan Otterdiik. 2007a. b). These industry reports were conducted at the same facility and largely by the same staff but independently of one another and at different times: July 26, 2006, through September 15, 2006, for the 28-day study and April 5, 2007, through August 6, 2007, for the 90-day study. Throughout the Toxicological Review, both Butenhoff et al. f20121 and the relevant industry report are cited when discussing effects observed in these reports. However, only one study evaluation was performed for this group of citations in HAWC (see Figure 2-2), the overall confidence level of high applies to both the 28-day and 90-day reports and accounts for the discrepancy between nine animal studies in Figures 2-1 and 2-2." E.2.3. Tier 2 Suggestions Comment: Comparison of effects in males and females is a common theme in the document and sometimes tentatively related to the pharmacokinetic differences ofPFBA in females E-9 ------- Supplemental Information ofPFBA and Related Salts (more rapid clearance) than males (slower clearance). EPA could select an administered dose in males that is nearly equivalent to females based on pharmacokinetic dose metrics and compare toxicity outcomes, as it may provide a clearer picture of the role that pharmacokinetics plays in toxicity in male and female lab animals. EPA Response: A brief comparison and discussion of pharmacokinetic parameters and relative responses for liver and thyroid endpoints at a constant dose has been added to Section 4.3 (Conclusions Regarding Susceptible Populations and Lifestages). Comment: While the information on the available epidemiologic studies is provided in the HAWC table, EPA could provide text that briefly notes the nature of the studies in general, and since these studies are so few in number, a sentence or two about each. It could be as little as 2-3 sentences that gives a synopsis of what was done (the PECO attributes), key methodologic limitations, and overall assignment regarding its quality. This is editorial in nature but would help make this a more transparent, user-friendly document Those who want the full details could look to HAWC and appendices as needed. EPA Response: Confidence in studies meeting PECO criteria is documented in HAWC fhttps://hawc.epa.gov/assessment/100500073/). and several additions were made in this revised assessment to ensure that the health outcome-specific confidence for these studies is conveyed in the figures or text of the relevant synthesis sections. Because study evaluations in IRIS are outcome-specific, the revised draft assessment does not include text summarizing the studies and their strengths/limitations in an outcome-nonspecific manner. Further, the health outcome-specific syntheses attempt to distill the available (epidemiological or other) evidence to those aspects of the studies (e.g., design; confidence) most pertinent to drawing hazard judgments; they intentionally try to avoid study-by-study summaries. This focus on developing concise IRIS assessments is based on feedback from reviewers over many years. Comment: The Toxicological Review states that most of the animal studies evaluated for study confidence were adequate, but the specific rationale for the analyses was unclear because the interactive HAWC link did not work. Ultimately it was unclear how the study confidence conclusions were determined, other than professional judgement. This chapter could be improved by writing more about the overall confidence conclusions in the chapter, even if the information is found in links. EPA Response: The HAWC site is now public fhttps: //hawc.epa.gov/assessment/100500073 /1. Links were checked and fixed throughout the revised assessment, and the study confidence conclusions are detailed there. Please see responses above about text additions relating to study confidence ratings. E-10 ------- Supplemental Information ofPFBA and Related Salts E.3. CHARGE QUESTIONS 3 AND 4 - HEPATIC EFFECTS For each health effect considered in the assessment and outlined below, please comment on whether the available data have been clearly and appropriately synthesized to describe the strengths and limitations. For each, please also comment on whether the weight-of-evidence decisions for hazard identification have been clearly described and scientifically justified. • For hepatic effects; the Toxicological Review concludes that the available evidence indicates PFBA exposure is likely to cause hepatic effects in humans given relevant exposure circumstances; on the basis of a series of short-term, subchronic, and developmental studies in rats and mice demonstrating consistent and coherent effects with a clear biological gradient. Although the available mechanistic information indicates the effects in rodents are relevant to humans, some uncertainty remains regarding potential differences in sensitivity across species due to evidence for the involvement of both PPARa-dependent and PPARa-independent pathways in these effects (see Charge Question 4 requesting input specific to this latter uncertainty). Appendix A (Systematic Review Protocol for the PFBA PFHxA, PFHxS, PFNA, and PFDA IRIS Assessments) identifies the human relevance of hepatic effects in animals that involve peroxisome proliferator-activated receptor alpha (PPARa) receptors as a key science issue. To the extent supported by the PFBA literature (and to a lesser extent, literature for other PFAS), the Toxicological Review evaluates the evidence relevant to the potential involvement of PPARa and non-PPARa pathways with respect to the reported hepatic effects. The Toxicological Review ultimately concludes evidence from in vivo and in vitro studies support that multiple modes of action (MOA) are operant in the induction of hepatic effects by PFBA exposure and the relative contribution of these different MOAs cannot be concluded with confidence from the available data. Please comment on whether the available animal and mechanistic studies support this conclusion and whether the analysis presented in the Toxicological Review is clearly documented. E.3.1. Overarching External Peer Reviewer Comments on Hepatic Effects "All reviewers agreed that the PFBA document clearly and appropriately synthesizes available data to describe the strengths and limitations of hepatic effects. [One reviewer] commented that "The evidence integration section is well done and supported by a great summary in Table 3-8." All reviewers also found the document supported the conclusion that MOAs are operant in the induction of hepatic effects by PFBA exposures, and the relative contribution of these different MOAs cannot be concluded with confidence. [The same reviewer] commented that "EPA did a great job in describing the complications" of the data, and another stated that "the available animal and mechanistic studies are clearly documented, and the conclusion is supported."" E.3.2. Tier 1 Recommendations Reviewers had no Tier 1 recommendations. E.3.3. Tier 2 Suggestions Comment: EPA could consider adding tables and/or figures that would help readers visualize important EPA conclusions, such as coherence of liver histopathology with liver E-ll ------- Supplemental Information ofPFBA and Related Salts weight effects (cited in Table 3-8), since these results are only presented in separate tables within the document (i.e., Table 3-7/Figure 3-6 for histopathology and Table 3-6/Figure 3-5 for liver weight changes). EPA Response: A data pivot chart has been created in HAWC displaying liver histopathology and liver weight effects together for ease of assessing the consistency and coherence of liver effects across species, sexes, durations of exposure, and study types. A link to this chart has been added to Section 3.2.2 of the assessment. Comment: The EPA should resolve an apparent discrepancy where statements regarding serum biomarker data are incoherent. Observations for serum biomarkers of altered liver function or injury appear as a factor that decreases certainty in Table 3-8 (p. 3-40) which contradicts statements in Section 3 that state that the inconsistent serum biomarker results did not influence the evidence integration judgements. EPA Response: The statement in Table 3-8 those incoherent observations across serum biomarkers (e.g., increased ALP but decreased bilirubin) decreased certainty is in reference to the certainty in the evidence for the serum biomarkers specifically. For the overall evidence integration judgment about hepatic effects, the noted incoherence across some of the biomarkers findings was not influential, but rather this judgment was based on the strong evidence of consistent and coherent effects on liver weights and liver histopathology. The text in Section 3 has been revised to provide more clarity on exactly how the serum biomarker evidence was used in drawing the overall evidence integration judgment Comment: EPA should explicitly state the meaning of "consistent effects" in the sentence: "The available animal evidence for effects on the liver includes multiple high and medium confidence studies with consistent effects across multiple species, sexes, exposure durations, and study designs...". This phrase could have several meanings (e.g., all the same effects occurred at the same or similar doses across multiple species, sexes, exposure durations, and study designs; one or more hepatic effects were consistently found at he some dose across studies though the specific effects observed may vary across studies) and different readers can/will interpret it differently. EPA Response: As described in the protocol, 'consistency' generally relates to findings for a given outcome (e.g., liver weight), while 'coherence' reflects the observed findings across related (e.g., through biological understanding or MOA) outcomes, such as effect on liver weight, and separately, histopathology, within individual studies or across multiple studies. Further, consistency is judged based on the pattern of findings across studies and comparisons and can range from consistency in the direction of the response to something more specific such as consistency in the magnitude of change in response at a given E-12 ------- Supplemental Information ofPFBA and Related Salts exposure level (while the latter can provide stronger evidence of consistency, it is neither expected nor required). In the context noted in the comment, the summary statement about consistency in the evidence integration section reflects the analyses presented in detail within the preceding synthesis sections on individual liver outcomes. An edit was made to clarify consistency refers to the findings of increased liver weight and, separately, increased liver histopathology incidence across the available studies. Comment: EPA should consider differences in metabolic pathways between species when comparing rodent to human exposures. The data on exposure obtained from the mouse used a humanized mouse model. Caution is always required when using data from a "humanized model" when the humanized model is limited to a single gene replacement As noted in the public comments, only a single nuclear receptor was humanized (PPARa) and that there are other nuclear receptors exist in the rat that can be induced and may lead to hepatocellular hypertrophy. This would not necessarily lead to a similar effect in humans at similar doses. This Tier 2 comment was also provided under Charge Question 6; responses to both instances of this Tier 2 comment are provided here for brevity's sake. EPA Response: Due to reported cross-species differences in PPARa signaling potency and dynamics, the potential human relevance of some hepatic effects has been questioned. Thus, the Foreman etal. f20091 study is informative in providing evidence on the relative contribution that PPARa has on PFBA-induced liver effects. While true that only PPARa was humanized in the Foreman etal. (20091 study, given the response in the humanized mice, including mouse PPARa-independent increases in hepatocellular hypertrophy and vacuolation, Foreman etal. (20091 provides evidence that rodent PPARa is not necessary for PFBA to induce some liver effects. The assessment indicates the data from Foreman et al. f20091 is largely used in qualitative analyses; thus, no claim is made that similar effects, whether in type or magnitude, would be observed in humans as in rats at similar doses. The mechanistic section discusses the activation and human relevance of other nuclear receptors (PXR, CAR) that might also contribute to the hepatic effects ofPFBA. Comment: The one issue that may call for more comment concerns the absence of evidence that PFBA affects liver enzymes (ALT, etc.) because that is the one human health endpoint that has consistently been found to be associated with other forms of PFAS. EPA should consider whether that contrast between an absence of an effect for PFBA in rodents and an apparent effect for PFOA and PFOS for humans has relevance to the final judgment EPA Response: The IRIS assessment does not conclude there is no evidence that PFBA exposure affects liver enzymes. The currently available data for PBFA on this endpoint are inconclusive. Specifically, only one epidemiology study was available and, although this study did not find any associations between serum biomarker levels and PFBA exposure, it E-13 ------- Supplemental Information ofPFBA and Related Salts was considered deficient with respect to sensitivity and likely biased towards the null. Additionally, while the two animal studies were also ultimately inconclusive with regard to ALT and other enzymes, some effects on related biomarkers were observed. Specifically, while no effects were observed after 28 days of exposure, changes in several serum biomarkers potentially indicative of liver injury (e.g., increased ALP) were observed after 90 days ofPFBA exposure, along with some incoherent findings (e.g., changes in the opposite direction as expected for bilirubin). Although uncertain, the serum biomarker data specifically were inconclusive and thus not necessarily in contrast to the findings for PFOA and PFOS. Regardless, in the case of PFBA, there is sufficient evidence on liver weight increases and increased histopathological lesions, as well as data informing mode-of-action, that the serum biomarker data, including if one were to more explicitly consider the serum biomarker data for other PFAS, would not change the overall evidence integration judgment of "evidence indicates (likely)" for PFBA. Comment: Because the entire Toxicological Report rests on animal-to-human extrapolation, to the extent that there are mechanisms in animals known not to apply to humans, this should be explained and factored into the report. EPA Response: A primary purpose of the Mechanistic Evidence and Supplemental Information section for hepatic effects is to evaluate the currently available mechanistic evidence informing whether the hepatic effects observed in rodents are relevant to human health (and thus suitable as the basis for reference value derivations). It is unclear what mechanisms in animals the commenter is referring to as "known" not to apply to humans, but given the focus on PPARa activation for PFAS, this is the mechanism of interest this response assumes. However, to clarify, activation of PPARa by other compounds can contribute to toxicity in humans and furthermore PFBA appears to be a ligand for PPARa in humans, given the data from the humanized PPARa mice and the observed interaction between PFBA and the human receptor in vitro. The concern is rather one of a differential response magnitude based on the presumption that hepatic responses to PPARa activation are exaggerated in rodents as compared to humans and thus may generally be more difficult to interpret as relating to a significant change in hepatic effects in most human exposure scenarios. Focusing on this concern, a key science issue addressed by the section noted above is whether the available data are sufficient to support dependence on PPARa activation for the observed hepatic effects of PFBA, or whether it is possible that the hepatic effects can also be mediated through non-PPARa modes-of-action. The other potential mechanisms discussed in this section are also considered in light of the available evidence on their human relevance, with a general assumption that animal mechanisms are relevant to humans without data to the contrary. The final conclusion, which is also supported in the peer review comments, is that PFBA's liver effects appear to be mediated through both E-14 ------- Supplemental Information ofPFBA and Related Salts PPARa-dependent and -independent pathways and that the observed liver effects are relevant to human health. As this is already extensively discussed and explained (similarly to the explanations in the above response) in the peer reviewed draft, additional discussion on this topic was not added to this revised assessment E.3.4. Public Comments Comment: EPA improperly characterizes liver hypertrophy in rats as an adverse effect of PFBA exposure. This conclusion is not consistent with EPA's own guidance, which states that reported liver hypertrophy is not an adverse effect As noted in the EPA Office of Pesticide Programs Health Effects Division Guidance Document# G2002.01 on Hepatocellular Hypertrophy (U.S.EPA, 2002), liver hypertrophy does not necessarily represent liver toxicity, nor is it necessarily a precursor to a particular outcome of toxicity. In fact, Guidance Document # G2002.01 recommends a weight-of-evidence approach for determining whether a liver effect should be characterized as adverse. This approach includes evaluation of other findings, such as: (1) type and severity of observed effects; (2) onset, duration, and progression of effects; (3) study method and design; and (4) other relevant effects and data. This guidance states that liver size or weight changes may be "indicative of adaptation which, by itself, is not necessarily adverse." EPA Response: The HED guidance document does not state that "liver hypertrophy is not an adverse effect" but rather, as the comment itself points out "[hepatocellular hypertrophy (and its corresponding increased liver size/weight) may be indicative of adaptation which, by itself, is not necessarily adverse. However¦, it might be associated with other more severe changes [emphasis added]. These changes are usually accompanied by alterations in relevant clinical chemistry parameters and/or histopathology." The HED guidance document recommends a weight-of-evidence approach to determine whether hypertrophy and related liver weight changes are considered to reflect an adverse hepatic response. Consistent with the protocol, to judge the adversity of the observed liver effects, the PFBA IRIS assessment considered the panel recommendations outlined by Hall et al. (2012) and the HED 2002 Guidance document Ultimately, using this paradigm, the assessment concluded "application of the recommendations from Hall etal. (2012) supports the conclusion that the multiple and interconnected effects observed in the livers of exposed animals meet the criteria for adversity" (i.e., the conclusion of adversity is not based on liver hypertrophy alone). This conclusion was unanimously supported by the external peer review panel as noted in the final Peer Review Report: "[a] 11 reviewers agreed that the PFBA document clearly and appropriately synthesizes available data to describe the strengths and limitations of hepatic effects." E-15 ------- Supplemental Information ofPFBA and Related Salts Comment: The reported liver hypertrophy in rats with PFBA exposure is an adaptive response occurring through increased activation of PPARa and CAR nuclear receptors. The activation of PPARa and CAR can lead to expansion of the smooth endoplasmic reticulum in the liver cell, and this added intracellular mass is reflected in the overall liver weight macroscopically and hypertrophy microscopically. Another consequence of PPARa and CAR/PXR activation in rodents is the potential stimulation of cell division (hyperplasia] and a decrease in the normal process of removal of worn-out cells (apoptosis). These processes also increase liver mass and can potentially lead to tumor formation in rodents. However, it is important to note that the hyperplastic processes are not present in mice with humanized PPARa expression (Foreman et al., 2009). Therefore, the processes that lead to tumor formation in rats as a result of PFBA exposure are not applicable to humans. In addition, Foreman et al. also demonstrated that activation of the human form of PPARa with PFBA does not produce frank liver toxicity. Moreover, Bjork and Wallace (2009) demonstrated that human hepatocytes did not respond to PFBA-induced PPARa activation at concentrations up to 200 |j.M (42,600 ppb); rat hepatocytes responded at PFBA concentration of 25 |j.M (5,325 ppb) and above. EPA Response: Please see responses above relating to the adversity and human relevance of the hepatic changes observed in rodents following PFBA exposure, noting that the assessment does not draw a conclusion regarding the potential for PFBA exposure to lead to tumor formation (i.e., the available carcinogenicity evidence was judged as inadequate). E.4. CHARGE QUESTION 3 - THYROID EFFECTS For each health effect considered in the assessment and outlined below, please comment on whether the available data have been clearly and appropriately synthesized to describe the strengths and limitations. For each, please also comment on whether the weight-of-evidence decisions for hazard identification have been clearly described and scientifically justified. • For thyroid effects; the Toxicological Review concludes that the available evidence indicates PFBA exposure is likely to cause thyroid toxicity in humans given relevant exposure circumstances; primarily on the basis of short-term and subchronic studies in male rats reporting a consistent and coherent pattern of thyroid effects following PFBA exposure, but also drawing from the consistency of effects when considering evidence from structurally related PFAS. The Toxicological Review concludes the thyroid effects are considered relevant to humans in the absence of evidence to suggest otherwise. E.4.1. Overarching External Peer Reviewer Comments on Thyroid Effects "Six of the seven reviewers found the conclusions for thyroid effects to be clearly described and scientifically justified. For example, [One reviewer] wrote: "The data leading to the conclusion E-16 ------- Supplemental Information ofPFBA and Related Salts that the thyroid effects are considered relevant to humans were appropriately synthesized and their strengths and limitations were adequately described; the weight-of-evidence decisions for hazard identification have been adequately described; the weight-of-evidence decisions for hazard identification have been adequately described and justified." The seventh reviewer commented that there was a "lack of clarity on human exposures."" E.4.2. Tier 1 Recommendations Comment: One reviewer recommended that EPA provide a table presenting lab animal and human citations and data that show connections between a percent decrease in serum T4 and adverse outcome, relating percent change with adversity in humans especially. This reviewer noted that, "This argument needs to be solid and presenting data will help" to relate thyroid effects in rats and humans quantitatively. EPA Response: To our knowledge, there is only limited information from human studies that demonstrate what percent decrease in T4 leads to adverse outcomes such as neurodevelopmental outcomes (note: these outcomes are the focus of this response and discussions in the assessment since these associations are the best studied). This is mainly due to the nature of epidemiological studies, typically with representative samples analyzed post hoc; many also bin data by "hypothyroid, euthyroid, hypothyroxinemic" based on reference ranges, and then correlate to adverse outcomes. There are a few human studies Tansen etal. (20191: Levie etal. (20181: Korevaar etal. (20161 where the sample sizes are large enough to capture a wide range of TSH and/or T4 values, which were then correlated to various neurodevelopmental outcomes that could be quantified. However, these studies still do not make direct comparisons from a percent decrease in hormones that would lead to an adverse effect; rather, they stratify their hormone samples by standard deviation to the mean/median, quartiles, etc. Therefore, it's difficult to make a conclusion in humans regarding what percent of hormone dysfunction is adverse, as those kinds of data are not generated. Additionally, there are no conclusive values from animal studies regarding to what degree of T4 reduction is adverse. This is due to several factors, including the existence of multiple thyroid-dependent processes in the brain, which likely have differing spatiotemporal sensitivities. But there are studies that show how graded reductions in T4 can lead to neuronal heterotopia Gilbert etal. f20141. synaptic transmission defects Gilbert and Sui f20081 and differential gene expression. When unable to estimate the BMR based on an evidentiary approach, the EPA takes a default approach as outlined in the Benchmark Dose Technical Guidance (U.S. EPA. 20121. Given the limited and inconsistent information available from human and animal studies, the assessment uses a standard deviation definition for the BMR (see Toxicological Review, Section 5.2.1 for justification for using BMRs). The Mechanistic Support and Supplemental Information section for thyroid effects E-17 ------- Supplemental Information ofPFBA and Related Salts has been revised to more thoroughly discuss the nature of the available human and animal evidence. E.4.3. Tier 2 Suggestions Comment: Related to the Tier 1 recommendation above, the same reviewer re-iterated that the thyroid findings in rats are relevant to humans but proposing how to relate rat thyroid effects to humans in a quantitative manner (dose-response) is the challenge. This reviewer suggested a brief discussion on this topic would be useful. EPA Response: Please see the responses provided to the Tier 1 Recommendation above as well as the public comment on this topic below. Comment: One reviewer noted that, although Butenhoff et al. (2012) do not report statistically significant changes in serum TSH related to PFBA exposure, the coefficient of variation for TSH measurements in controls ranges from 40% to 72% in the two studies this group reports. The reviewer suggested that this means that detecting relatively small changes in serum TSH is difficult with this assay assembled from the reagents provided by the NIH Pituitary Program and that it is more likely, as pointed out in the Agency report, that the effect of PFBA exposure on thyroid histology reflects an increase in serum TSH that was not detected in this assay. This reviewer suggested the EPA consider evaluating the issue of the TSH assay using the reagents characterized in the Butenhoff studies and rather than emphasize the comparison with "hypothyroxinemia" (a clinical term that doesn't translate perfectly to animal studies), describe the situation as one in which serum T4 is low and TSH levels have increased. EPA Response: The description of PFBA exposure on thyroid effects now includes discussion of the potential lack of detectable increases in serum TSH levels with corresponding decreased T4. Lack of detectable increase in serum TSH levels may be related to the specific assay utilized in the Butenhoff et al. f20121 study, and text has been added to the assessment noting this possibility. Comment: One reviewer suggested that it is important to discriminate between "thyroid function" and "thyroid hormone action." This reviewer noted that evidence presented in Butenhoff et al. (2012) shows that PFBA decreases both serum total and free T4 while also showing an increase in thyroid hormone action in the liver. This reviewer further notes that this scenario is highly reminiscent of the effects of PCB and PBDE exposure on TH signaling in which measures of TH action indicate an increase in TH action in the liver despite a reduction in serum total and free T4 (Giera et al., 2011; Bansal et al., 2014). In the case of PCBs, this pattern of effects on serum hormones and gene expression in the liver was coincident with a complex pattern of effects on thyroid hormone action in brain (Zoeller et E-18 ------- Supplemental Information ofPFBA and Related Salts al., 2000; Bansal and Zoeller, 2008). Finally, this reviewer noted that Butenhoff etal. 2012 reports thatPFBA exposure also decreases serum cholesterol (Table 7), and thyroid hormone is known to reduce serum cholesterol in rodents and humans (Mullur et al., 2014). Ultimately this reviewer suggested that "[although paradoxical ... that PFBA reduces serum total and free T4 while the liver appears to be responding to increased thyroid hormone action, it is recommended that the Agency incorporate all measured endpoints of thyroid hormone action in their analysis." EPA Response: A brief description of reduced thyroid function (decreased serum total and free T4) and increased thyroid hormone action in the liver (decreased serum cholesterol) has been added to Section 3.2.1 (Thyroid Effects). Comment: One reviewer agreed that decreases in serum total and free T4 are very clearly associated with developmental and physiological deficits: "In both humans and experimental animals, low TH is related to permanent neural and cognitive deficits (e.g., (Zoeller and Rovet, 2004; Rovet, 2014; Stagnaro-Green and Rovet, 2016a). This is likely to be true for several (if not all) organs including heart, bone, lung and intestine (Bizzarro and Gross, 2004; Bassett et al., 2007; Mochizuki etal., 2007; Wexler and Sharretts, 2007). Much of the experimental literature on this topic makes use of models of severe hypothyroidism (Crofton et al., 2005; Crofton and Zoeller, 2005). However, graded effects of thyroid hormone insufficiency have become the focus of increased attention in experimental systems (Gilbert et al., 2020). This experimental interest reflects the degree to which subclinical hypothyroidism should be viewed as a disease state (Cooper, 2001). Thus, a preponderance of information indicates that even a small degree of thyroid hormone insufficiency is associated with cognitive deficits in children (Haddow et al 1999; Rose et al., 2006; Nakamizo etal., 2007; Oerbecketal., 2007; Korevaar etal., 2016)." This reviewer suggested that the EPA document more fully the sensitivity of the human brain to thyroid hormone insufficiency as it may strengthen the support for this choice. EPA Response: Additional references which support an association between subclinical hypothyroidism and cognitive deficits have been added to Section 3.2.1 (Thyroid Effects). Comment: One reviewer suggested that the EPA could consider a broader context of PFBA impacts on the thyroid system, including considerations on genetic deficits in specific proteins related to the thyroid hormone system. EPA Response: Text was added to Section 3.2.1 (Thyroid Effects) which includes a brief discussion ofPFBA effects and genetic differences in thyroid hormone system-related proteins. E-19 ------- Supplemental Information ofPFBA and Related Salts E.4.4. Public Comments Comment: One commenter noted that the significance of changes in T4 levels in rodents to human risk assessment has been questioned by the National Academy of Sciences (NAS) and others because of the significant differences in binding proteins and affinities among species. These differences in binding proteins, binding affinities of the proteins for the hormones, turnover rates of the hormones, and thyroid stimulation lead to important quantitative differences between rats and humans. As a result, NAS concluded that "rats are much more sensitive to agents that disturb thyroid function than are humans, so the relevance of rat studies in quantitative terms to humans is limited." NAS further noted that "[t]he committee does not agree that transient changes in serum thyroid hormone or TSH concentrations are adverse health effects; they are simply biochemical changes that might precede adverse effects. EPA Response: As noted above, six of the seven peer reviewers indicated the T4 effects are significant and relevant to humans. One of the external peer reviewers further specified that decreases in serum total and free T4 are very clearly associated with developmental and physiological deficits: "In both humans and experimental animals, low TH is related to permanent neural and cognitive deficits (e.g., Stagnaro-Green and Rovet f20161: Zoeller and Rovet (200411. This is likely to be true for several (if not all) organs including heart, bone, lung, and intestine (Bassett et al. (20071: Mochizuki et al. (20071: Wexler and Sharretts (20071: Bizzarro and Gross (200411. Much of the experimental literature on this topic makes use of models of severe hypothyroidism (Croftonand Zoeller. 2005: Crofton etal.. 20051. However, graded effects of thyroid hormone insufficiency have become the focus of increased attention in experimental systems f Gilbert etal.. 20201. This experimental interest reflects the degree to which subclinical hypothyroidism should be viewed as a disease state fCooper. 20011. Thus, a preponderance of information indicates that even a small degree of thyroid hormone insufficiency is associated with cognitive deficits in children (Korevaar etal.. 2016: Nakamizo etal.. 2007: Oerbeck. 2007: Haddowetal.. 19991. The majority of the panel concluded that the conclusions for the thyroid effects to be clearly described and scientifically, with another panel member stating that "the data leading to the conclusion that the thyroid effects are considered relevant to humans were appropriately synthesized and their strengths and limitations were adequately described." In response to this comment, however, the assessment has been revised to include a more detailed discussion on the relationship between thyroid hormone status and neurotoxicological effects to further support assessment conclusions. Regarding the NAS (2005) report on the Health Implications of Perchlorate Ingestion, the conclusions of that report should be considered narrowly in the context of health effects due to exposure to perchlorate and not generally as broad statements on the human E-20 ------- Supplemental Information ofPFBA and Related Salts relevance of thyroid effects observed in animals. The statement that the "committee does not agree that the transient changes in serum thyroid hormone or TSH concentrations are adverse health effects; they are simply biochemical changes that might precede adverse effects" is made regarding what endpoints to base the reference dose value on for perchlorate given the presumed chemical-specific mode of action. This mode of action is not pertinent to PFBA or other PFAS. Comment: EPA failed to consider studies where quantitative histomorphometric analysis on thyroid function after PFBA exposure did not report statistically significant changes. Histomorphometric analyses of thyroid follicles provide a more quantitative indication of thyroid response than histopathological assessments. To conduct a thorough and defensible risk assessment for PFBA, EPA must consider this and similar studies. EPA Response: The quantitative histomorphometric analyses from Butenhoff et al. T20121 are discussed in Section 3.2.1 (Thyroid Effects). E.5. CHARGE QUESTION 3 - DEVELOPMENTAL EFFECTS For each health effect considered in the assessment and outlined below, please comment on whether the available data have been clearly and appropriately synthesized to describe the strengths and limitations. For each, please also comment on whether the weight-of-evidence decisions for hazard identification have been clearly described and scientifically justified. • For developmental effects¦, the Toxicological Review concludes that the available evidence indicates PFBA exposure is likely to cause developmental effects in humans given relevant exposure circumstances; on the basis of a coherent pattern of delays in acquisition of three different developmental milestones in a single study in mice, with the findings presumed relevant to humans in the absence of evidence to suggest otherwise. The assessment discusses similar effects observed for structurally related PFAS. E.5.1. Overarching External Peer Reviewer Comments on Developmental Effects "Most reviewers agreed that the available data were clearly and appropriately synthesized and concurred with EPA's conclusion. [One reviewer] commented that "in several but not all ways" the available data on developmental effects were clearly and appropriately synthesized to describe the strengths and limitations but noted that the document lacked a discussion of "relevant mechanistic information or information on the conserved biological processes causing the developmental effects observed in mice to be considered relevant to humans." [The same reviewer] noted that such discussions "would inevitably lead to a more complete and transparent description of the strengths and limitations of the available data relevant to developmental effects."" E-21 ------- Supplemental Information ofPFBA and Related Salts E.5.2. Tier 1 Recommendations Comment: One reviewer stated that EPA should add information supporting the human relevance of the developmental effects to the assessment (e.g., the Evidence Integration Summary) in order to "... more fully and clearly support applicability of the weight-of- evidence decision." This reviewer noted that, currently, the text of the assessment lacks sufficient discussion of "...the conserved biological processes between mice and humans that the EPA considers relevant to the observed developmental effects (e.g., for delayed vaginal opening and preputial separation), whether the mouse has been shown to be a good laboratory animal model for assessing potential human developmental effects, or what human developmental endpoints (e.g., delayed onset of puberty) may be presumed to be correlates of some of the PFBA-induced developmental effects observed in the single mouse study (e.g., delays in vaginal opening and preputial separation in Das et al. 2008)." This reviewer further noted that some of this information could found later in the document (i.e., Section 5.2.1) and this information could be included and expanded on in Section 3. Public comments were also received regarding whether delays in vaginal opening and preputial separation whether "these endpoints accurately reflect pubertal development" and stating that "the biological basis for this assumption is lacking and reviews suggest that these measurements accurately reflect pubertal development in the rat but not the mouse." Public comments further stated that "mouse "puberty" has been used for POD calculations in some of the PFAS documents and I question that this is biologically correct, and the Agency may want to reconsider this. Clearly these are valid developmental landmarks in the mouse like eye-opening and etc. but they may not be valid indices of puberty." EPA Response: An expanded discussion of the conserved biological processes between mice and humans that is considered relevant to the observed developmental effects (e.g., for delayed vaginal opening and preputial separation) has been included in Section 3 and updated in Section 5.2.1. to include supporting references. "The onset of puberty in humans is driven by surges in the levels of estrogen in females and testosterone in males, so the timing of puberty can be altered by exposure to endocrine disrupting chemicals that mimic or antagonize these hormones In female rodents, pubertal markers include vaginal opening (indicative of the first ovulation in rats, but not mice) and the subsequent first estrus and onset of regular estrous cyclicity (rats and mice) [Prevot, V., Puberty in Mice and Rats, in Knobil and Neill's Physiology of Reproduction, T.M. Plant and A.J. Zeleznik, Editors. 2015 p. 1395-1439], Since Das etal. (2008). found delayed vaginal opening in mice (not rats), this is not a direct correlate to puberty in humans. However, the Reproductive Guidelines state that both accelerations and delays in the timing of reproductive milestones can be considered adverse. E-22 ------- Supplemental Information ofPFBA and Related Salts Comment: One reviewer recommended that references to the developmental toxicity effects of other PFAS should be documented in a chart and/or link to a chart/table. EPA Response: This information can be found in three recently published reports Carlson etal. (2022}: Radke etal. f20221.and Pelch etal. f20221. and that outline the available references of developmental effects following hundreds of other PFAS. Additionally, Table 4-2 has been added to the assessment (see Section 4.1) to facilitate comparisons of developmental toxicity hazard conclusions across EPA PFAS assessments. Comment: One reviewer recommended emphasizing statements on the observation of fetal effects in the absence of maternal toxicity and data gaps regarding information on the thyroid and nervous system following gestational exposures. EPA Response: This data gap is now discussed in the evidence integration summary of Section 3.2.3. (Developmental Effects); specifically, Section 3.2.3 notes that developmental delays consistent with delayed sexual maturation are observed in the absence of body weight or maternal effects, thus strengthening the certainty that the observed effects are adverse fetal effects. E.5.3. Tier 2 Suggestions Comment: One reviewer suggested that the EPA could opine on a thyroid-mediated mode- of-action in young animals based on evidence in adult rats (i.e., thyroid histopathology and serum T4 decreases in adult animals). EPA Response: There is insufficient available data supporting a direct link between a thyroid-mediated mode-of-action in young animals based on evidence in adult rats. Comment: One reviewer commented that "[w]hile the rationale [for developmental effects] is well-explained, the tone of the report implies notably weaker support than for thyroid or hepatic effects. It seems odd to put them into the same ultimate bin when there is such a sharp contrast in the evidence and even in the way that the evidence is interpreted and expressed." This reviewer suggested further explanation in the report why developmental effects "ended up in the same level" despite a weaker evidence base. EPA Response: Additional references have been incorporated in Section 3.2.3 to further support the rationale for the evidence integration judgment for developmental effects. Please note that the methods for drawing the evidence integration judgments and determining the levels of certainty regarding potential hazard are outlined in Appendix A. These methods do allow for a range of evidence scenarios with some variation in "strength" to ultimately lead to the same overall judgments. E-23 ------- Supplemental Information ofPFBA and Related Salts E.5.4. Public Comments Comment: The discussion of the effects of PFOA on timing of vaginal opening and preputial separation in mice reported by Lau et al. (2006) is incomplete and appears to be inappropriate. Lau et al. (2006) reported a non-monotonic dose-response for both day of vaginal opening and day of preputial separation in mouse offspring from dams treated with PFOA on gestational day (GD) 1-17. Vaginal opening was accelerated at the lowest dose (1 mg/kg/day) and delayed, at higher doses (3-20 mg/kg/day), with a greater delay with increasing dose. More notably, preputial separation was accelerated, rather than delayed, at all doses (1, 3, 5, and 10 mg/kg/day) except the highest dose (20 mg/kg/day). The acceleration of preputial separation was greatest at the lowest dose (1 mg/kg/day) and the magnitude of this effect decreased with increasing dose from 1-10 mg/kg/day. At 20 mg/kg/day, the only dose at which preputial separation was delayed, there was severe toxicity including full litter resorptions in 88% of dams and approximatelyl0% survival (i.e., ~90% mortality) of offspring at postnatal day (PND) 23. As such, the statement that the observations in male offspring treated with PFOA from Lau et al. (2006) are part of a "consistent pattern of delayed pubertal milestones...folio wing exposure to related PFAS" does not appear to be supportable. EPA Response: The relevant text in the Toxicological Review has been updated to indicate, where appropriate, markers of sexual maturation were delayed or accelerated. Specifically, to the comment that the dose-response for vaginal opening observed in Lau etal. (2006) was non-monotonic: while the mean value of time to vaginal opening was slightly lower in the lowest exposure group (compared to controls), this difference was not statistically significant and is more appropriate characterized as "no effect" rather than "accelerated". Comment: The Reproductive Toxicity Guidelines (U.S. EPA,1996) state that alterations in the age at puberty should be considered as adverse effects. Citing this, the Toxicology Review of PFBA uses delays in vaginal opening and preputial separation in the mouse for RfD, assuming that these endpoints accurately reflect pubertal development. However, the biological basis for this assumption is lacking and reviews suggest that these measurements accurately reflect pubertal development in the rat but not the mouse. This species difference is described in Chapter 30 "Puberty in Rats and Mice" by Vincent Prevot (Knobil and Neil's Physiology of Reproduction. Elsevier Science and Technology, 2015) and in a publication in Scientific Reports (2017) by Gaytan etal. (DOI:10.1038/srep46381). Related Comment: In rats, but not mice, vaginal opening is normally associated with maturation of the HP axis, ovulation and the initiation of reproductive cycles. Mouse "puberty" has been used for POD calculations in some of the PFAS documents and this may not be biologically correct and the Agency may want to reconsider this. Clearly these are E-24 ------- Supplemental Information ofPFBA and Related Salts valid developmental landmarks in the mouse like eye-opening but they may not be valid indices of puberty. EPA Response: As noted by the commenter, alterations in the timing of reproductive development (whether delayed or accelerated) are considered adverse in accordance with the EPA Reproductive Guidelines. While vaginal opening in mice may not be a direct correlate to puberty in humans (as it is in rats), alterations in reaching reproductive or developmental milestones are considered adverse and relevant to human health. However, the linkage of these delays in acquisition of these milestones to "puberty" has been removed in this revised assessment E.6. CHARGE QUESTION 3 - REPRODUCTIVE AND OTHER EFFECTS For each health effect considered in the assessment and outlined below, please comment on whether the available data have been clearly and appropriately synthesized to describe the strengths and limitations. For each, please also comment on whether the weight-of-evidence decisions for hazard identification have been clearly described and scientifically justified. • For reproductive effects and other noncancer effects (i.e., cardiometabolic effects, renal effects, ocular effects, body weight), the Toxicological Review concludes there is inadequate evidence to determine whether PFBA exposure has the potential to cause these effects in humans on the basis of the sparsity of available evidence. E.6.1. Overarching External Peer Reviewer Comments on Reproductive and Other Effects "All reviewers concurred with EPA's conclusion that there is insufficient evidence to determine if PFBA can cause reproductive or other noncancer effects." E.6.2. Tier 1 Recommendations Reviewers had no Tier 1 Recommendations. E.6.3. Tier 2 Suggestions Comment: One reviewer suggested that EPA consider adding a recent study by Ou et al. (2021) that indicates some PFAS may increase the risk of heart defects. EPA Response: While the Ou et al. (2021) study does suggest that some PFAS are associated with increased odds of septal defects, for PFBA specifically, odds ratios were not statistically significantly increased or decreased for septal defects, conotruncal defects, and all congenital heart defects. Hence, given that no defects were observed to be associated with PFBA exposure, discussion of this study was not added to the assessment given that consideration of its observations would not materially change the evidence integration conclusion for reproductive or developmental effects. E-25 ------- Supplemental Information ofPFBA and Related Salts Comment: One reviewer suggested that EPA consider including supporting mechanistic evidence or supplemental information for reproductive and other noncancer effects for a fuller description of the strength and limitations of the available information for reproductive and noncancer effects. EPA Response: There is inadequate evidence to determine whether PFBA exposure has the potential to cause human reproductive effects (aside from the delays in sexual and/or reproductive development discussed in Section 3.2.3: Developmental Effects) or the "other noncancer effects" discussed in the draft assessment. In general, and as in this case here where there is only limited (or none) supplemental information on these outcomes, there is not clear added value in delineating the potentially relevant mechanistic information on health effects for which toxicological evidence is generally lacking. Therefore, no additional discussions of mechanistic or supporting evidence for reproductive and other noncancer effects were added to this revised assessment. E.7. CHARGE QUESTION 5 - CANCER HAZARD The draft assessment concludes there is inadequate evidence to assess carcinogenic potential for PFBA and that this descriptor applies to oral and inhalation routes of human exposure. Please comment on whether the available animal and mechanistic studies, and the analysis presented in the Toxicological Reviewsupport this conclusion. E.7.1. Overarching External Peer Reviewer Comments on Cancer Hazard "All reviewers concurred with EPA's conclusion that there is inadequate evidence to assess carcinogenic potential for PFBA for either oral or oral inhalation exposure. [One reviewer] noted that the "evidence that PFBA is carcinogenic is sparse and continues to be sparse according to a recent review of PFAS and cancer (Steenland and Winquist 2021)." E.7.2. Tier 1 Recommendations Comment: One reviewer commented unlike the other sections with limited data, no discussion was included in the carcinogenicity section about how other studies of PFBA- related compounds could or could not inform the data gaps for carcinogenicity or genotoxicity. This reviewer recommended that EPA should include a short section to address this missing component in a manner similar to the other sections of the report EPA Response: A short explanation that the evidence for carcinogenicity due to PFBA exposure is non-existent and is limited for other related PFAS has been added to Section 3.3. In addition, the carcinogenicity conclusions from other EPA PFAS analyses that have been finalized have been included in Table 4.2, although they are not influential to the carcinogenicity judgment for PFBA. Conclusions from other ongoing IRIS assessments have E-26 ------- Supplemental Information ofPFBA and Related Salts not been added because they have not yet been finalized. Although not currently available, future efforts on PFAS (see PFAS Strategic Roadmap {U.S. EPA, 2021,10002133@@author- year), potentially including additional studies on PFBA, may help to inform this data gap. E.7.3. Tier 2 Suggestions Reviewers had no Tier 2 suggestions. E.8. CHARGE QUESTION 6 - NONCANCER TOXICITY VALUE DATA SELECTION For PFBA, no RfC was derived. The Butenhoff et al. (2012) 90-day rat study was the study chosen for use in deriving the RfD on the basis of an increased incidence of hepatocellular hyperplasia and decreased total T4 in male rats. Is the selection of this study and these effects for use in deriving the RfD for PFBA scientifically justified? a. If so, please provide an explanation. b. If not, please provide an alternative study(ies) or effect(s) that should be used to support the derivation of the RfD and detail the rationale for use of such an alternative. c. As part of the recommendations in "a" or "b" above, please comment on whether the effects selected are appropriate for use in deriving the RfD, including considerations regarding adversity (or appropriateness in representing an adverse change) and the scientific support for their selection. More specifically, Appendix A identifies interpreting the adversity of certain outcomes observed in rodents, including some hepatic effects, as a key science issue. Please consider in your recommendation the narrative in the Toxicological Review related to the decision that the observed hepatocellular hypertrophy, when considered within the broader constellation of effects, is representative of an adverse change in the organ. d. Given the lack of studies on inhalation exposure to PFBA, no reference concentration (RfC) is derived. Please comment on this decision. E.8.1. Overarching External Peer Reviewer Comments on Noncancer Toxicity Value Data Selection "All reviewers concurred: (1) with the selection of the Butenhoff et al. (2012) study as scientifically justified for derivation of an RfD for PFBA; (2) that the critical effects selected were appropriate for use in deriving the RfD; and (3) that the decision to not derive a reference concentration (RfC) was justified, given the lack of studies on inhalation exposures to PFBA." E.8.2. Tier 1 Recommendations Comment: One reviewer recommended adding a discussion of other carcinogenicity studies across the structurally related perfluorinated compounds to Section 5.2. E-27 ------- Supplemental Information ofPFBA and Related Salts EPA Response: A short explanation that the evidence for carcinogenicity due to PFBA exposure is non-existent and is limited for other related PFAS has been added to Section 3.3. In addition, the carcinogenicity conclusions from other EPA PFAS analyses that have been finalized have been included in Table 4.2. E.8.3. Tier 2 Suggestions Comment: One reviewer commented that identification of hepatic effects observed in rodents as a key scientific issue is a very conservative approach and that the conclusion is in contradiction with Hall etal. (2012), stating "The results of this workshop concluded that hepatomegaly as a consequence of hepatocellular hypertrophy without histologic or clinical pathology alterations indicative of liver toxicity was considered an adaptive and a non- adverse reaction." This reviewer stated that this conclusion should be reached by an integrative weight of evidence approach. EPA Response: An integrative weight of evidence approach is the approach taken in Section 3.2.2. The conclusions in Section 3.2.2 are entirely in-line with the recommendations of {Hall, 2012, 2718645@@author-year} that coincident histological evidence of liver injury/damage can be used to support the conclusion that liver weight and hypertrophic changes are adverse. Specifically, for PFBA, liver weight changes and hypertrophic lesions are accompanied by other lesions such as necrosis and vacuolation, supporting their adversity along a progression to more severe effects. Thus, no revision was made. See related responses to comments on charge question 3. E.8.4. Public Comments Comment: The Das study was not considered as the critical study because it did not measure serum thyroid hormones. This decision does not withstand scrutiny from the scientific community. Serum thyroid hormones are subject to a great degree of variability due to the assay issues, diurnal variations, and even husbandry conditions, and thus are not suitable grounds upon which to exclude a relevant study. The Das study evaluated important key functional aspects of pregnancy outcomes as well as neonatal development into young adults and should have been considered as the critical study in the Draft IRIS Review for PFBA. Further, given the current Draft IRIS Review's emphasis on developmental toxicity with exposure to PFBA and the availability of relevant studies, EPA should rely on its own developmental study for PFBA as the critical study to develop the reference value for PFBA. EPA Response: It is not accurate to state that the Das study was not considered as the critical study because it did not measure serum thyroid hormones. Endpoints from both Das etal. (20081 and Butenhoff etal. (20121 were considered for POD derivation. Ultimately, as E-28 ------- Supplemental Information ofPFBA and Related Salts liver and thyroid effects from (Butenhoff etal.. 20121 were interpreted with the highest confidence and resulted in lower PODs, the candidate values for these endpoints were selected for the RfD. Additionally, the candidate value for developmental delays from Das et al. f20081 was selected for the subchronic RfD (see below). Comment: It is suggested that the rationale for not considering hepatic effects in male mice exposed to PFBA for 28 days in Foreman et al. (2009) as the basis for Reference Dose (RfD) development be reconsidered. It (i.e., the assessment) is stated that the subchronic (90 day) study in rats (Butenhoff et al., 2012b) and the developmental study in mice with 17 days of exposure (GD 1-17; Das etal., 2008) were considered for RfD development because these study designs can "estimate potential effects of lifetime exposure, as compared to short- term [i.e., 28 day] or acute studies." However, the preference for developmental studies over short term (i.e., 28 day) studies does not appear to be supportable for RfDs based on systemic effects such as increased relative liver weight or histopathological changes in the liver. Specifically, Table 3-5 shows that both wild-type and humanized PPAR-alpha male mice exposed to PFBA for 28 days (Foreman et al., 2009) are more sensitive to increased relative liver weight (i.e., a greater increase at the same or similar dose) than pregnant and non-pregnant female mice exposed for 17 days (Das et al., 2008) and are also more sensitive than male rats exposed for 28 and 90 days (Butenhoff et al., 2012b). EPA Response: For the purpose of deriving chronic non-cancer reference values, subchronic exposure studies are preferred over short-term studies when chronic studies are lacking in the toxicity database. Also, developmental toxicity studies are useful for evaluating the potential for increased susceptibility in pregnant animals or their offspring during this sensitive lifestage, when short periods of exposure during critical windows of development can be considered more relevant to identifying sensitive health effects from a lifetime of exposure than subchronic or chronic exposure durations. This latter consideration does not necessarily apply to all health endpoints, likely including the hepatic effects of PFBA. A greater amount of uncertainty exists in extrapolating from short-term to chronic durations and thus, given the availability of preferred studies in the PFBA database, the results of short-term studies are only considered as supporting information for toxicity value derivation. E.9. CHARGE QUESTION 7 - SUBCHRONIC REFERENCE DOSE In addition, for PFBA, an RfD for less-than-lifetime ("subchronic") exposures is derived. No "subchronic" RfC was derived. The study chosen for use in deriving the subchronic RfD is the gestational exposure mouse study by Das et al. (2008) with the RfD based on delayed acquisition of developmental milestones¦, as indicated by delayed time to vaginal opening, eye opening, and preputial E-29 ------- Supplemental Information ofPFBA and Related Salts separation in exposed male and female offspring. Is the selection of this study and these effects for the derivation of the subchronic RfD for PFBA scientifically justified? a. If so, please provide an explanation. b. If not, please provide an alternative study(ies) or effect(s) that should be used to support the derivation of the subchronic RfD and detail the rationale for use of such an alternative. c. As part of the recommendations in "a" or "b" above, please comment on whether the effects selected are appropriate for use in deriving the RfD, including considerations regarding adversity (or appropriateness in representing an adverse change) and the scientific support for their selection. d. Given the lack of studies on inhalation exposure to PFBA, no "subchronic" RfC is derived. Please comment on this decision. E.9.1. Overarching External Peer Reviewer Comments on the Subchronic Reference Dose "All reviewers concurred that selection of the Das et al. (2008) study is scientifically justified for derivation of the subchronic RfD. [One reviewer] noted that a subchronic RfD based on developmental effects resulting from a shorter exposure duration "will provide a useful risk assessment complement to the chronic RfD, furthering risk assessment and risk communication." "Most reviewers concurred that the selection of effects were justified for derivation of the RfD, although [one reviewer] commented that EPA should consider improving the scientific justification to the extent possible for certain effects." "All reviewers concurred that the decision to not derive a subchronic RfC was justified." E.9.2. Tier 1 Recommendations Comment: One reviewer recommended that a discussion be included regarding how inclusion of delayed eye opening would or would not change the RfD. EPA Response: The candidate value for delayed eye opening is included in the endpoints considered for final RfD selection in Table 5-7 of the assessment. As can be seen from the values presented in this table, selection of this endpoint would result in an RfD 33% higher than currently selected (8 x 10-3 mg/kg-day vs. 6 * 10:i mg/kg-day) and was not interpreted with greater confidence, and thus would be inadequately protective of human health. A brief discussion to this effect has been added. Comment: One reviewer commented that they were surprised that the cumulative endpoint of "total affected implants" was not reported or evaluated. This reviewer E-30 ------- Supplemental Information ofPFBA and Related Salts recommended that the Toxicological Review add a paragraph discussing further several of the decisions to not look at the endpoint of all affected, why the Rai and Van Ryzin model was not used and discuss the importance of looking at this cumulative endpoint This paragraph should specifically discuss whether these suggestions would have changed the calculation of the subchronic RfD. EPA Response: A short discussion of this topic, including an explanation for why the cumulative endpoint was not modeled, has been added to the assessment in Appendix D.1.2 and as a footnote to Table 5-1. The Rai and van Ryzin model are a nested dichotomous model that can account for intralitter similarity (via estimation of intralitter correlation and use of litter specific covariate parameters). Functionally, this model has the same capabilities of the nested Logistic model, which is currently implemented in BMDS 3.2 and was used to model the embryo/fetal mortality endpoint How modeling "total affected implants" would ultimately impact the final RfD derived is difficult to characterize but given that fetuses that lived to parturition and experienced some delay in developmental milestones would be counted as "responding" alongside fetuses that died in utero, the total incidence of "affected fetuses" would be greater per dose group than for the individual endpoints, thus resulting in a lower BMD and BMDL. This would result in a lower POD. Comment: One reviewer commented on the need to add a paragraph that expands the discussion of what the lack of a functional reproductive or neurodevelopmental assessment means for the application of the current uncertainty factors in this incomplete toxicological assessment package. The signals from the Das et al 2008 study should raise concern of this lack and require additional assessment of what this widespread environmentally relevant compound and metabolic common breakdown product means to the overall IRIS assessment report across the structurally related perfluorinated compounds. EPA Response: The lack of a functional reproductive or neurodevelopmental study in relation to selecting the uncertainty factors is discussed in Section 5.2.1. Briefly, the lack of a functional reproductive study was not considered a key quantitative data gap in the PFBA database, in part given the general lack of evidence for sensitive reproductive effects for some other similar PFAS (see Table 4-2). Regarding the lack of a functional neurodevelopmental study, while this is identified as a key data gap in the PFBA evidence base, concerns over developmental neurotoxicological effects presumed to result from thyroid hormone insufficiency are mitigated given evidence from PFBS (i.e., PODs for effects in dams and offspring are almost identical for thyroid hormones). However, concern over developmental neurotoxicity independent of a thyroid hormone-mediated mechanism remains an important uncertainty accounted for via application of a UFd = 3. E-31 ------- Supplemental Information ofPFBA and Related Salts Comment: One reviewer reiterated their previous Tier 1 Recommendation (see Section E.5) that EPA should consider improving scientific justification (e.g., expanded to other developmental effects) to the extent possible, particularly for the critical effect. Specifically, this reviewer requested that EPA expand discussion on the conserved biological processes between mice and humans that the EPA considers relevant to the observed developmental effects (e.g., for delayed vaginal opening and preputial separation), whether the mouse has been shown to be a good laboratory animal model for assessing potential human developmental effects, or what human developmental endpoints (e.g., delayed onset of puberty) may be presumed to be correlates of some of the PFBA-induced developmental effects observed in the single mouse study (e.g., delays in vaginal opening and preputial separation in Das etal. (2008)). EPA Response: A discussion on the known similarities and differences in the development of these outcomes between rodents and humans has been added to the assessment (see Section 3.2.3). It is important to emphasize, as described in EPA guidelines, that it is not expected that the effects that manifest in animal studies will manifest similarly in humans, although outcomes that are strongly correlated across species can provide strong evidence. Likewise, in the absence of evidence to the contrary, effects observed in animal models are considered relevant to humans. Comment: One reviewer noted that it appeared to them that the "...document supports use of delayed eye opening and embryo/fetal mortality more strongly than other developmental effects. While these effects provide candidate subchronic RfD values similar to that selected for the proposed final subchronic RfD, delays in vaginal opening observed in Das et al. (2008) apparently provides the most specific basis for thatvalue (Table 5-10, p. 5-24), the adversity of which does not appear to be fully addressed in the document." This reviewer recommended that relevant information to support the adversity of the critical effect ultimately selected for the determination of the subchronic RfD be added to the assessment. EPA Response: A discussion regarding the adversity of the observed developmental delays has been added to the assessment in Section 3.2.3. E.9.3. Tier 2 Suggestions Reviewers had no Tier 2 suggestions. E.10. CHARGE QUESTION 8 - NONCANCER TOXICITY VALUE DOSE- RESPONSE MODELING EPA used benchmark dose modeling (U.S. EPA, 2012) to identify points-of-departure (PODs) for oral exposure to PFBA. Are the modeling approaches used, selection and justification of benchmark E-32 ------- Supplemental Information ofPFBA and Related Salts response levels, and the selected models used to identify each POD for toxicity value derivation scientifically justified? E.10.1. Overarching External Peer Reviewer Comments on Noncancer Toxicity Value Dose- Response Modeling "The reviewers who responded to this charge question supported the modeling approach used and the justification provided, with some reviewers noting enthusiastic support for the approach." "Several reviewers noted that benchmark dose modeling is not their area of expertise and declined to comment." E.10.2. Tier 1 Recommendations Reviewers had no Tier 1 recommendations. E.10.3. Tier 2 Suggestions Comment: One reviewer suggested that EPA attempt to strengthen the benchmark response (BMR) justification for vaginal opening delays beyond historical precedence (to the extent possible) given that it is ultimately the critical effect used in determining the sub chronic RfD. EPA Response: The selection of a BMR = 5% relative deviation for delayed vaginal opening is not based on historical precedence, but rather is based on a determination of what level of change in this effect has been judged to be a relevant response level (i.e., a minimally biologically significant response) in the EPA Endocrine Disruptor Screening Program. In addition, this approach in defining a BMR for continuous endpoints based on biological information is consistent with the recommendations of the BMD Technical Guidance fU.S. EPA. 20121. A full discussion of the selection of the BMR for developmental delays is included in Table 5-2. Comment: One reviewer commented that the model selected for liver hypertrophy should possibly be the log-logistic model vs the currently selected Weibull model based on equal Akaike Information Criterion values and a BMDL value that appears to better agree with the actual study data. EPA Response: After consideration of the shape of the dose-response curve for this dataset, it was determined that the minimum-maximum characteristic of the data (i.e., response going from 0/10 to 9/10 between the mid- and high-dose groups precludes modeling this dataset (consistent with the BMD Technical Guidance (2012) document (U.S. EPA. 2012)). Thus, the NOAEL/LOAEL approach was used instead for this endpoint This E-33 ------- Supplemental Information ofPFBA and Related Salts change in POD derivation methodology does not have a large impact on the assessment as the NOAEL (6 mg/kg-day) is very close to the BMDL (5.4 mg/kg-day). E.ll. CHARGE QUESTION 9 - TOXICOKINETICS Appendix A identifies the potential for toxicokinetic differences across species and sexes as a key science issue and lays out a hierarchy for using relevant toxicokinetic data in extrapolating doses between laboratory animals and humans. Given what is known and not known about the potential interspecies differences in toxicokinetics of PFBA, EPA used the ratio of human-to-animal serum clearance values to adjust the POD to estimate a human equivalent dose in the derivation of the respective RfDs. a. Is applying the ratio of human-to-animal serum clearance values for PFBA scientifically justified? If not, please provide an explanation and detail on a more appropriate approach. b. Do the methods used to derive toxicity values for PFBA appropriately account for uncertainties in evaluating the toxicokinetic differences between the experimental animal data and humans? E.ll.l. Overarching External Peer Reviewer Comments on Toxicokinetics "The reviewers concurred that the application of the ratio of human-to-animal serum clearance values for PFBA was scientifically justified. [One reviewer] commented that applying the ratio is a more appropriate choice than scaling doses allometrically using body weight (BW)3/4 methods." E.11.2. Tier 1 Recommendations Comment: One reviewer suggested that another approach to help justify or strengthen the animal to human extrapolation is to use kidney filtration (GFR) and that comparison of excretion ratios (i.e., clearance/GFR) could be compared to other PFASs where data exist This reviewer stated that these analyses may be insightful for characterizing the degree of renal/hepatic reabsorption and ultimately increase the confidence in the calculated human CL. EPA Response: Two paragraphs were added to Section 3.1.5 comparing the clearance values to species-specific average GFR values for mice, rats, and humans, with or without including the impact of serum binding (i.e., GFR*free). A comparison across PFAS was not made in the revised PFBA assessment (a preliminary analysis of results across draft and final assessments indicates that there is not a consistent, predictable pattern, so any such discussion would not be straightforward or brief]. However, this is taken as a useful research note for future applications. E-34 ------- Supplemental Information ofPFBA and Related Salts Comment: One reviewer recommended that EPA clarify sections on PFBA toxicokinetics with respect to the consistency of the linearity assumptions with the presence of saturation processes. This reviewer specifically noted that EPA stated that dosimetric adjustments are made "assuming the exposure being evaluated is low enough to be in the linear (or first- order) range of clearance" in one part of Section 5, but in another part stated that "results for both male and female mice [from Chang et al., 2008] show a dose-dependent increase in clearance across all dose levels, consistent with the hypothesis of saturable renal resorption." EPA Response: Given the limited PK data available, an extensive analysis of this issue is not possible. However, a paragraph has been added to Section 3.1.5 explaining that the mouse data appear to be reasonably consistent with constant CL at < 30 mg/kg-day, and the plotted rat data for the same dose in Chang etal. f20081 appear likewise, so linearity will be assumed valid for dose levels below that, not above. A statement was also added in Section 5, where the approach for extrapolation is described. E.11.3. Tier 2 Suggestions Comment: One reviewer suggested that EPA could use dosimetrically adjusted doses rather than a ratio of clearance values, and that this could be considered to see if such calculations would make significant differences. EPA Response: If the dosimetric adjustment still involves use of a single clearance value, then changing the order of dosimetric adjustment and dose-response analysis will not change the outcome. Such an approach could make a significant difference if the adjustment is dose-dependent However, such an approach would significantly complicate the analysis. Clearance will not be a function of dose directly, but rather a function of blood concentration or internal dose, which in turn both depends on dose and time. Thus, a nonlinear PK model would need to be developed, validated, and applied to properly account for the time- and dose-dependence in a bioassay. The comment suggests consideration of a simpler approach, with clearance just assumed to be a nonlinear function of dose, but this would require picking a function form and then using it to interpolate between and extrapolate above doses used in the mouse PK studies, which has its own uncertainties. Further, since the PK study for rats only used a single dose level, the approach can't be used directly for that species. Given these considerations, development and application of a nonlinear PK model was not attempted. Comment: One reviewer noted that, while the Chang et al. (2008) occupational exposure data provide important insights into PFBA pharmacokinetic behavior, these data are not sufficiently robust for calculating pharmacokinetic parameters, and that EPA uses a half-life E-35 ------- Supplemental Information ofPFBA and Related Salts that is sufficiently long to encompass most adults from the study. This reviewer suggested showing how the half-lives were determined with the data and the logic for selecting a specific value. EPA Response: Details of the analysis were previously provided in Appendix C.2. The rationale for excluding subjects for whom the second measurement was below the LLOQ were provided in Section 5.2.1 but are now restated in Appendix C.2. A table listing the subjects used in EPA's analysis has been added to Appendix C.2. Of those eight subjects, four had half-lives greater than the estimated half-life, 67.9 hours, and four were below. Of the four excluded subjects, one had an estimated half-life greater than 67.9 hours. Hence, while it may be true that 7 of the 12 total subjects (i.e., "most") had half-lives lower than EPA's estimate, this is only 58% of the study population. Therefore, the assessment concludes that the estimated mean in this estimate is reasonable. While it is recognized that there is uncertainty inherent in the use of these data, but they are nonetheless human elimination data. The alternative to use of these human elimination data is to estimate the human half-life based on BWy> scaling, which leads to predicted half-lives of 38 hours in men and 7 hours in women, which are within a factor of 2 of the value from EPA's analysis (67.9 hours) for men and within a factor of 10 of that estimates for women. Given that PFAS are generally known to be subject to renal resorption, use of 67.9 hours is therefore considered both biologically plausible and modestly health-protective compared to use of BW% scaling. The presumption is that it provides an average elimination, hence clearance rate for humans and that uncertainty in this value is addressed by the portion of UF_H assigned (i.e., factor of 3). Comment: One reviewer commented that, under steady-state exposure to humans (e.g., drinking contaminated water) the bioaccumulation would depend on the half-life but no matter how quickly it's cleared, it is steadily replaced. This reviewer further stated that humans don't receive a single dose and stop being exposed, so slow or rapid clearance would be less influential than in the typical laboratory situation. This reviewer suggested that this could be explained in the report, indicating how the steady-state exposure to humans bears on the evaluation. EPA Response: If humans are exposed to a regular (daily) dose, D, then use of the estimated human clearance (CLh) leads to a prediction of an ongoing blood concentration equal to D/CLh; i.e., that is the steady-state or average blood concentration given the daily dose, D. Hence, this evaluation assumes that the steady-state level increases or decreases in direct proportion to D, with 1/CLh being the proportionality constant. This is now stated in the section on dose extrapolation. E-36 ------- Supplemental Information ofPFBA and Related Salts E.11.4. Public Comments Comment: The assessment uses a worst-case estimate for the serum excretion half-life (tl/2) of PFBA in humans which is confounded by potential co-exposure to other PFAS molecules. The draft IRIS assessment assumes a tl/2 of 67.9 hours based on a study of workers exposed to other PFAS believed to be metabolized to PFBA by Chang et al. (2008). The authors [i.e., Chang et al., 2008] note, however, thatthe data need to be interpreted cautiously, because the workers were not exposed directly to PFBA and were exposed to materials that, given their chemical structures, likely are metabolized to PFBA via oxidation or hydrolysis. Moreover, the draft assessment rejects the default body weight (BW0.75) approach which would generate a half-life of 37.8 hours - within a factor of two of that derived from Chang etal., 2008. EPA Response: Given the lack of controlled PK studies of PFBA in humans, the only empirical data one can use are those potentially confounded with possible ongoing exposures or metabolic production from precursors. Environmental epidemiological analyses, in which observed blood concentrations are correlated with estimated exposure levels, have an inherent uncertainty in that the exposure is not exactly known. Given that any estimate of human elimination has uncertainty, the EPA considers the use of a health- protective estimate to be reasonable, while noting that 67.9 hours is in fact not an upper bound of the Chang etal. (20081 data: five of the 12 subjects had estimated half-lives greater than that, as noted above. It is also noted that for subjects 1 and 2 of the Cottage Grove group in Chang, for whom multiple time-points are shown in Figure 6, the decline is very close to log-linear. If there was significant ongoing exposure or metabolic production, the decline would asymptotically approach a plateau, the steady-state level given that exposure. Further, the tl/2 values for these two subjects are above the average obtained. In summary, the results do not represent a worst-case scenario, which would involve use of an upper-bound half-life estimate from these data. While it is possible that the true average is lower, there are no specific data to support this possibility, for example that PFBA elimination is reduced in this population due to co-exposures to other PFAS. Further, EPA guidelines U.S. EPA (20111 support the use of such empirical data over default BW% scaling when such data exist. Comment: The approach taken in the draft assessment for calculating a dose adjustment factor (DAF) for the animal data overestimates serum concentrations which leads to an over prediction of the toxicity ofPFBA. Although using the ratio of clearance rates to generate the DAF is preferable to using the ratio based on half-life, the uncertainty around the tl/2 estimate raises significant questions about the decision to use it to derive the human equivalent dose (HED). Given this uncertainty, using the default body-weight scaling E-37 ------- Supplemental Information ofPFBA and Related Salts method to develop the DAF is more appropriate. Failing that, the assessment should include additional discussion of the uncertainty in the clearance model that is chosen. EPA Response: As noted above, EPA guidelines U.S. EPA f20111 state that extrapolation based on chemical-specific data is preferred over default scaling. Discussion of the uncertainty in the human half-life estimate has been augmented in the revised assessment (see Sections 3.1.4 and 5.2.1), including discussion of the potential for ongoing exposure or metabolic production ofPFBA, although noting that there is no clear indication of this occurring. The 2-fold difference between the estimated clearance and that predicted from BWA% is well within the range of uncertainty that would be expected for either value. Comment: The body weight values for the animals in the study that is being evaluated, if available, should be used instead of default body weight values to derive dosimetric adjustment factors (DAFs) based on body weight3/4. EPA Response: In general, study-specific body weight (BW) should be used when extrapolating dosimetry for a given toxicological observation. However, use of a DAF based on clearance builds in a BW adjustment, in that clearance is a rate per kg BW. While some intra-species variation in CL may occur with BW, the data available are not sufficient to demonstrate such variation, such variation will not have a significant effect on the outcome, and as addressed above, BW3/4 scaling was not determined to be the best approach for PFBA. Comment: A recent paper, Abraham et al. (2021), that investigated the distribution of PFBA in human tissues and came to conclusions that differ from those of Perez et al. (2013). should be cited. See: Abraham etal. (2021). Perfluorobutanoic acid (PFBA): No high-level accumulation in human lung and kidney tissue. International Journal of Hygiene and Environmental Health, 237,113830. EPA Response: First, the term "accumulation" is interpreted as an increase in tissue levels over time, given ongoing exposure. The determination of whether or not accumulation in that sense occurs requires longitudinal samples of the same individual over time while carefully monitoring exposure. Both Perez etal. (2013) and Abraham etal. (2021) only reported single time-point samples; hence, neither paper contains data that can be used to demonstrate or refute accumulation (e.g., a high tissue concentration can occur due to high exposure without accumulation). Second, the subjects of Perez etal. f20131 were from T arragona County (Catalonia, Spain), while those analyzed by Abraham etal. f20211 were from France, collected 3-6 years later than Perez, so there were likely differences in their exposure levels. That being said, the enormous differences in reported tissue levels certainly raises questions about the respective analytic methods, and so the results of E-38 ------- Supplemental Information ofPFBA and Related Salts Abraham are now also provided in the revised assessment (see Section 3.1.2), noting the discrepancy given these caveats about unknown differences in exposure. A recently published paper by EPA authors Bangma etal. f20211 did identify an endogenous compound in placenta that is a likely analytic interferent, and this has been added to the document The interfering compound identified by Bangma etal. f20211 would have to be present in human tissues but not in the pig tissues used for QA by Perez etal. T20131 in order to explain the discrepancy. Importantly, as noted in the revised assessment, Abraham etal. (20211 paper does not report some necessary methodological information including whether matrix-matched calibration curves were used or what QA/QC measures were taken (i.e., duplicates, method blanks, continuous calibration verification, etc.). Perez etal. f20131 state that matrix matched calibration was used for each tissue type using pig brain, liver, bone, and kidney; that reagent blanks, sample blanks, a repeated measures were conducted. The Perez etal. (2013) study also states that their method was validated, which is not reported by (Abraham etal.. 2021). Hence, based on details provided in the published papers, EPA's evaluation yields much higher confidence in (Perez etal.. 2013) than (Abraham etal.. 2021). Since the results of Perez etal. f20131 are not used in the quantitative assessment, this notation will only have a qualitative impact on the Toxicological Review. Comment: The toxicokinetic differences between wild-type, PPAR-alpha null, and humanized PPAR-alpha mice reported by Foreman et al. (2009) are unlikely to result from differences in PPAR-alpha status and are potentially relevant to interpretation of differences in susceptibility to toxicity among these strains. Suggest adding serum and liver concentration data from Foreman et al. (2009) to Table 3-1. EPA Response: While some of the differences between strains reported by Foreman etal. f20091 are not easily attributable to PPRAR-alpha status, this is not true for all of the differences. For example, the lower liver concentrations in null mice compared to wild-type is explainable as the lack of binding to PPAR-alpha in the null mouse liver. Other differences may be secondary to differences in hepatotoxicity (i.e., that this toxicity may be more severe in PPAR-alpha-carrying mice, but not in null mice). That both serum and liver concentrations in the humanized mice at 175 mg/kg were lower than at 35 mg/kg is more difficult to explain, as it suggests significantly higher clearance in this strain at that dose compared to lower doses. The data indicate, though, that PPAR-alphas status has a minimal effect on liver:serum distribution. This now stated and the data have been added to Table 3- 1. E-39 ------- Supplemental Information ofPFBA and Related Salts E.12. CHARGE QUESTION 10 - UNCERTAINTY FACTOR APPLICATION EPA has evaluated and applied where appropriate uncertainty factors to account for intraspecies variability (UFh), interspecies differences (UFa), database limitations (UFd), duration (UFs), and LOAEL-to-NOAEL extrapolation (UFl) for PFBA. a. Has uncertainty been adequately accounted for in the derivation of the toxicity values? Please describe and provide suggestions¦, if needed. b. For uncertainty in interspecies differences (UFA), a value of 3 is applied to extrapolate between effects in laboratory animals and in humans. Although PPARa dependence might support a value of UFA = 1 if that were the sole mode of action, evidence for non-PPARa MOAs is available in the PFBA (and larger PFAS) database. Thus, uncertainty remains regarding the potential differences in sensitivity across species due to the involvement of both PPARa- dependent and PPARa-independent mechanisms. Further, data are lacking to determine with confidence the relative contribution of these competing MOAs. As such, the Toxicological Review concludes the available data are not adequate to determine if humans are likely to be equally or less sensitive than laboratory animals with respect to the observed hepatic effects and that a value ofUFA=3 is warranted to account for the residual uncertainty in toxicodynamic differences across species. Please comment on whether the available animal and mechanistic studies support this conclusion and whether the analysis presented in the Toxicological Review is clearly documented. c. For uncertainty in extrapolating from subchronic to chronic exposure scenarios (UFS), a default value of 10 is applied. The assessment concludes there is conflicting evidence on whether effects manifest at lower exposure levels or are more severe at equivalent exposure levels when comparing findings across short-term and subchronic exposure durations. Thus, to account for the potential for some effects to worsen with longer durations of exposure (subchronic vs. short-term) and the lack of data on whether effects from subchronic exposures might worsen in a chronic exposure scenario, a UFS=10 is applied in the Toxicological Review. Does the provided scientific rationale support this decision? Please explain. d. To inform uncertainty in intraspecies variability (UFH), the assessment evaluates and considers the available evidence on potential susceptibility to PFBA within different populations or lifestages, including any potential human health impacts from early life exposure. Are the available information and data appropriately considered and the resultant UFH values scientifically justified and clearly described? e. Does the provided scientific rationale support the application of the remaining uncertainty factors (UFL, UFD)? Please explain. E.12.1. Tier 1 Recommendations Reviewers had no Tier 1 recommendations. E.12.2. Tier 2 Suggestions Comment: One reviewer suggested that the selection of a value of 3 for UFa should be evaluated and considered as an alternative to a value of 10 (rather than a value of 1) as our E-40 ------- Supplemental Information ofPFBA and Related Salts current understanding of interspecies differences in PFAS toxicokinetics and toxicodynamics has very significant gaps. EPA Response: A value of UFa = 10 is not supported given that interspecies differences in toxicokinetics are accounted for in the application of the dosimetric adjustment factor (DAF). In the case of the PFBA assessment, this DAF explicitly accounts for differences in the toxicokinetics (i.e., serum clearance values) between rodents and humans. However, the data gaps in understanding ofPFBA toxicokinetics remain highlighted in the revised assessment as an area deserving of additional research. Comment: One reviewer noted that, while hepatocellular hypertrophy exhibited exposure duration dependence when comparing 28- and 90-day results, there were no apparent increased sensitivity with longer exposure durations for liver weight or thyroid hormone measures. This reviewer commented that a UFs of 10 for liver weight and thyroid hormones may then not be justified and their corresponding candidate RfDs may be unjustifiably low. This reviewer suggested that the EPA consider additional justification for the selection of the UFs for these endpoints. EPA Response: Although no increase of effect was noted in liver weight endpoints or thyroid hormone levels when comparing short-term (28-day) and subchronic (90-day exposures), this is not sufficient evidence to conclude that effects would not worsen at the same exposure level or become evident at lower exposure levels with chronic exposure. It should be noted that the increase in exposure duration is approximately 8-fold when comparing chronic exposures to subchronic exposures and only 3-fold when comparing subchronic exposures to short-term exposures. A short discussion of this matter has been added to Section 5.2.1 of the assessment and a value of UFs = 10 is retained for all non- developmental toxicity endpoints. Comment: One reviewer commented that the UFa of 3 did not account for interspecies differences in thyroid toxicity or developmental effects related to thyroid hormone insufficiency. This reviewer suggested that the EPA consider increasing the UFa from 3 to 10. EPA Response: As noted in Table 5-5, after application of the chemical-specific DAF (based explicitly on differences in rodent and human serum clearance values), residual uncertainty regarding toxicodynamics remains and is accounted for in the application of a UFa= 3. EPA is unaware of any chemical-specific data that would support increasing the UFa to 10 to account for differences in toxicodynamics regarding PFBA-induced thyroid or developmental effects. E-41 ------- Supplemental Information ofPFBA and Related Salts E.12.3. Public Comments Comment: The draft assessment applies a total uncertainty factor of 1,000 to generate the chronic reference dose (RfD). This includes a 10-fold adjustment for a subchronic-to- chronic exposure adjustment (UFS), and a 3-fold adjustment for database uncertainty (UFD). The data from the study by Butenhoff et al. suggest, however, that PFBA levels have reached steady state conditions in rat livers after 28 days. As a result, the draft assessment notes that "[i]ncreased duration of exposure might not elicit increased effects in the target tissue." In the absence of a chronic study, however, the draft concludes that liver effects may increase with prolonged exposure and that includes a UFS of 10. EPA's conclusion is based on evidence that hepatocellular hypertrophy was observed at lower doses after 90 days when compared to the 28-day results, despite the fact that the lowest observed adverse effect level (LOAEL) for increased liver weight (likely resulting from hypertrophy) was the same in both the 28 and 90 day study and the clinical chemistry was inconsistent across endpoints and durations of exposure. EPA's conclusion is also not supported by the studies with perfluorooctanoic acid (PFOA), a structurally similar compound. While hypertrophy was observed in chronic studies of male rats exposed to PFOA, the concentrations required were 10-fold higher than those eliciting a response in the subchronic studies. Consequently, the addition of a UFS of 10 for liver effects is not supported by the available evidence. While a study of chronic exposure to PFBA is not available, the chronic data from studies with PFOA indicate that a UFS of 1 is more appropriate. EPA Response: For PFBA, there is chemical-specific data that demonstrates, for some endpoints (i.e., hepatocellular hypertrophy), an increase in duration results in observation of effects at lower doses. While this data is missing for other effects (liver weight, thyroid hormone levels), it is consistent with EPA guidelines U.S. EPA f20021 to apply a UFs = 10 to account for the possibility of increased effects at lower doses when considering chronic exposures. Application of a UFs = 10 for liver effects in adult animals is consistent with other recent EPA assessments of PFAS, including GenX U.S. EPA (2021). with the justification for this decision documented in Section 5.2.1 of the revised assessment. Comment: For the candidate RfDs for both chronic and subchronic effects, the draft assessment includes a UFD of 3 based on concern for neurodevelopmental effects independent of a thyroid hormone-related mechanism. Agency guidance explains, however, that a database uncertainty factor is applied when reproductive and developmental toxicity studies are missing since they have been found to provide useful information for establishing the lowest no adverse effect level. The guidance notes that, for a reference dose (RfD) based on animal data, a factor of 3 is often applied if either a prenatal toxicity study or a two-generation reproduction study is missing, or a factor of 10 may be applied if both are missing. In deciding whether to apply an UFD, EPA advises that the assessor should E-42 ------- Supplemental Information ofPFBA and Related Salts consider both the data lacking and the data available for a particular organ system as well as life stages. As noted in the draft assessment, a high confidence developmental study is available for PFBA; the draft also notes that the lack of a multigenerational reproductive study "is not considered a major concern." Therefore, EPA's proposal to add an uncertainty factor to address concern about neurodevelopmental effects is not supported by its own analysis. EPA Response: EPA's A Review of the Reference Dose and Reference Concentration Processes (U.S. EPA. 20021 states that the "database UF is intended to account for the potential for deriving an underprotective RfD/RfC as a result of an incomplete characterization of the chemical's toxicity." This comment itself acknowledges that the RfD/RfC document recommends "...the assessor should consider both the data lacking and the data available for particular organ systems as well as life stages" when determining the value of the UFd. Therefore, it is wrong to conclude that the recommendations for application of the UFd state that this uncertainty factor is intended to only account for the lack of developmental or reproductive studies. Given residual uncertainties regarding the potential for reproductive, developmental neurotoxicity, immunotoxicity, or mammary gland effects, a UFd = 3 is applied and this is consistent with EPA's RfD/RfC recommendations. Comment: Uncertainties are not appropriately accounted for. In the recent Human Health Toxicity Values derivation for PFBS, EPA included a database uncertainty factor of 10, citing a lack of chronic studies and neurodevelopmental and immunotoxicity studies as well as a lack of mammary gland studies. The same deficits were noted by EPA for PFBA. It is therefore unclear why EPA drew a different conclusion in the draft toxicological review of PFBA, deciding to only apply a partial database uncertainty factor of 3. EPA Response: The rationale for the selected UFd = 3 in the PFBA assessment is extensively discussed in Section 5.2.1 and the considerations that inform the final selection of UFd = 3 (lack of developmental neurotoxicity, immunotoxicity, and mammary gland toxicity studies) are consistent with the rationale for a higher UFd provided in the PFBS assessment The PFBS assessment additionally considers the lack of a chronic study in the final selection of a UFd = 10; this is considered and, as necessary, addressed by the UFs in the PFBA assessment For PFBA, the selection of UFd = 3 was supported by the external peer reviewers and is retained in the revised assessment Comment: Biomonitoring studies demonstrate that Americans have chronic exposure to multiple PFAS chemicals throughout their lifetimes. Therefore, it is impossible to be exposed to PFBA and no other PFAS chemicals. CDC's NHANES studies reveal that nearly every American has detectable concentrations of four PFAS chemicals in their bloodstream (PFOS, PFOA, PFHxS and PFNA). Multiple other PFAS have been detected in NHANES and E-43 ------- Supplemental Information ofPFBA and Related Salts state biomonitoring programs. Toxicity assessment (i.e, the PFBA assessment) should account for simultaneous exposure to other PFAS chemicals that impact the same target organs. EPA must promote similar assessments for other PFAS related health outcomes with potential for additive toxicity, including kidney and liver toxicity, lipid metabolism, birth outcomes, immunotoxicity and developmental effects. At the very least, EPA should add an additional uncertainty factor to account for the high likelihood of additive effects with other PFAS. EPA Response: The PFBA assessment derives organ or system-specific reference doses and states "... these toxicity values might be useful in some contexts (e.g., when assessing the potential cumulative effects of multiple chemical exposures occurring simultaneously)." Therefore, when assessing cumulative risk, the values presented in the PFBA assessment can be used by risk assessors in conjunction with values in other PFAS human health risk assessments (and separately conducted exposure assessments) to account for exposures to multiple PFAS simultaneously. E.13. CHARGE QUESTION 11 - CANCER TOXICITY VALUES Given the conclusion there was inadequate evidence to assess carcinogenic potential for PFBA (Charge Question 5), the Toxicological Review does not derive quantitative estimates for cancer effects for oral or inhalation exposures. Is this decision scientifically justified? E.13.1. Overarching External Peer Reviewer Comments on Cancer Toxicity Values "All reviewers concurred with the decision to not derive quantitative estimates for cancer effects due to inadequate evidence to assess carcinogenic potential for PFBA. Additionally, [one reviewer] commented that "no robust scientific foundation has been laid, critically reviewed and broadly accepted by the scientific community for the use of any surrogate PFAS with carcinogenicity data (e.g., PFOA) for this purpose."" E.13.2. Tier 1 Recommendations Reviewers had no Tier 1 recommendations. E.13.3. Tier 2 Suggestions Reviewers had no Tier 2 suggestions. E-44 ------- Supplemental Information ofPFBA and Related Salts APPENDIX F. QUALITY ASSURANCE FOR THE IRIS TOXICOLOGICAL REVIEW OF PERFLUOROBUTANOIC ACID AND RELATED COMPOUND AMMONIUM PERFLUOROBUTANOATE This assessment was prepared under the auspices of the U.S. Environmental Protection Agency's (EPA's) Integrated Risk Information System (IRIS) Program. The IRIS Program is housed within the Office of Research and Development (ORD) in the Center for Public Health and Environmental Assessment (CPHEA). EPA has an agency-wide quality assurance policy and that policy is outlined in the EPA Quality Manual for Environmental Programs (see CIO 2105-P-01.11 and follows the specifications outlined in EPA Order CIO 2105.1. As required by CIO 2105.1, ORD maintains a Quality Management Program, which is documented in an internal Quality Management Plan (QMP). The latest version was developed in 2013 using Guidance for Developing Quality Systems for Environmental Programs (OA/G-11. An NCEA/CPHEA-specific QMP also was developed in 2013 as an appendix to the ORD QMP. Quality assurance for products developed within CPHEA is managed under the ORD QMP and applicable appendices. The IRIS Toxicological Review ofPerfluorobutanoicAcid and Related Salts has been designated as Influential Scientific Information (ISI) and is classified as QA Category A. Category A designations require reporting of all critical QA activities, including audits. IRIS assessments are developed through a seven-step process. Documentation of this process is available on the IRIS website: https://www.epa.gov/iris/basic-information-about-integrated-risk-information- svstem#process. Specific management of quality assurance within the IRIS Program is documented in a Programmatic Quality Assurance Project Plan (PQAPP). A PQAPP was developed using the EPA Guidance for Quality Assurance Project Plans (OA/G-51. and the latest approved version is dated June 2022. All IRIS assessments follow the IRIS PQAPP, and all assessment leads and team members are required to receive QA training on the IRIS PQAPP. During assessment development, additional QAPPs may be applied for quality assurance management. They include: F-l ------- Supplemental Information ofPFBA and Related Salts Title Document Number Date Program Quality Assurance Project Plan (PQAPP) for the Integrated Risk Information System (IRIS) Program L-CPAD-0030729-QP-1-5 June 2022 An Umbrella Quality Assurance Project Plan (QAPP) for Dosimetry and Mechanism-Based Models (PBPK) L-CPAD-0032188-QP-1-2 December 2020 Quality Assurance Project Plan (QAPP) for Enhancements to Benchmark Dose Software (BMDS) L-HEEAD-0032189-QP-1-2 September 2020 Umbrella Quality Assurance Project Plan for CPHEA PFAS Toxicity Assessments L-CPAD-0031652-QP-1-4 October 2021 During assessment development, this project underwent four quality audits during assessment development including: Date Type of audit Major findings Actions taken August 2022 Technical System Audit No findings None July 2021 Technical System Audit No findings None August 2020 Technical System Audit No findings None August 2019 Technical System Audit No findings None During Step 3 of the IRIS Process, the IRIS Toxicological Review was subjected to external reviews by other federal agency partners including the Executive Offices of the White House. Comments during these IRIS Process steps are available in the Docket EPA-HQ-ORD-2020-0675 on http:/www. regulations.gov. During Step 4 assessment development, the IRIS Toxicological Review of Perfluorobutanoic Acid and Related underwent public comment from August 23, 2021, to November 8, 2021. Following this comment period, the toxicological review underwent external peer review by a contractor-led panel performed by ERG from October 2021 to June 2022. The peer-review report is available on the peer review website. All public and peer-review comments are available in the docket EPA-HQ-ORD-2020-0675. Prior to release (Step 7 of the IRIS process), the final toxicological review is submitted to management and QA clearance. During this step the CPHEA QA Director and QA Managers review the project QA documentation and ensure that EPA QA requirements are met. F-2 ------- Supplemental Information ofPFBA and Related Salts REFERENCES Abraham. K: El-Khatib. AH: Schwerdtle. T: Monien. BH. (2021). Perfluorobutanoic acid (PFBA): No high-level accumulation in human lung and kidney tissue. Int J Hyg Environ Health 237: 113830. http://dx.doi.org/10.1016/i.iiheh.2021.113830. Bangma. IT: Reiner. 1: Fry. RC: Manuck. T: Mccord. 1: Strvnar. Ml. (2021). Identification of an Analytical Method Interference for Perfluorobutanoic Acid in Biological Samples. Environ SciTechnol Lett 8: 1085-1090. http://dx.doi.org/10.1021/acs.estlett.lc00901. Bassett. THD: Clement-Lacroix. P: Samarut. 1: Chassande. 0: Williams. GR: O'Shea. PI: Sriskantharaiah. S: Rabier. B: Bovde. A: Howell. PGT: Weiss. R. ovE: Roux. TP: Malaval. L. uc. (2007). Thyroid hormone excess rather than thyrotropin deficiency induces osteoporosis in hyperthyroidism. Mol Endocrinoll095-1107. http://dx.doi.org/10.1210/me.2007-0033. Bizzarro. Ml: Gross. I. (2004). Effects of hormones on fetal lung development [Review], Obstet Gynecol Clin North Am 31: 949-961, xii. http://dx.doi.Org/10.1016/i.ogc.2004.08.001. Butenhoff. 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