Document 2RBEyXne7qqZ6V9qQG5xBGg46

Extraction of Potassium Perfluorooctanesulfonate from Red Blood Cells and Serum for Analysis Using HPLC-Electrospray/Mass Spectrometry DATA REQUIREMENTS Analytical Method Requirements Sean Gallagher ANALYTICAL REPORT DATE June 2, 2003 PERFORMING LABORATORY / TESTING FACILITY 30E3x8ygReesneRaerscehaDrrcihve State College, PA 16801 Phone: 814-272-1039 STUDY SPONSOR 3M Environmental Technology and Safety Services Building 2-3E-09 PO Box 33331 St. Paul, MN 55133-3331 PROJECT Exygen Protocol Number: 01P-023-066 Exygen Study Number: 023-066 Total Pages: 98 Exygen Study No. 023.066 GL OODABO PRR ACTICA ECOMT PLIAO NCESR TATEY MENT Exygen Swdy Number Perfluorooctanesulfonate from 023066, Red Blood cniled Cells and "Exraction of Potassium Serum for Analysis Using HPLC- Electrospray/Mass Spectrometry," conducted for 3M Environmental Technology and Safety Services, was performed in compliance with US EPA TSCA Good Laboratory Practice Standards (40 CFR Part 792) by Exygen Research. ily R. fecker Principal thvestigator Exygen Research Are be Sean Gallagher . Study Director Wildlife Intemational, Lid. / 7 Johy/Rewsted Spbfsor Representative: Eitri, Inc. Exygen Research _DatGe fofey DatebMlley cf los Date Page 20198 Exygen Study Noa 023-066 QUALITY ASSURANCE STATEMENT Exygen's Quality Assurance Unit reviewed Exygen Study Number 023-066, entitled, "Extraction of Potassium Perfluorooctanesulfonate from Red Blood Cells for Analysis Using HPLC-Elcctrospray/Mass Spectrometry". All reviewed phases were inspected for calolndaupcptlicaacbcloerdGiongodtoLEaxbyogreanto'rsySPtraancdtaircde OSptearndaatridnsg.PrAolcledufrinedsi,ngtshewSetruedyrePproorttoecdol1,0 atnhde Study Director and to management. Phase 1. Protocol Review 2. EFoxrutaicftiicaotni,on 3 RawDaaReview 4 Raw Data Review 5 DRervfiteRwepon G FRemvliRewopor Date DateERwepgoernted to SDtautdey RDeirpeocrttoerdatnod Inspected Management Sponsor Management 5122001 ean wisn sa ann ison 646801 7/1301 orion $7901 2100 orn LISIGIN 120501 02002 OWIL2I03 060203 060203 QLuyadliitay AsSspfuterrance Auditor Dae0s/02]e3 Exygen Research Page 30f98 Exygen Study No.: 023-066 CERTIFOIFCAUATHTENITIOCINTY `This report, for Exygen Study Number 023-066, is a true and complete representation of the raw data for the study. `Submitted by: Exygen Research 3058 Research Drive State College, PA 16801 (814) 272-1039 Principal~In~vestigator, Exygen: ScieinltyisR.t fecket Exygen Research CY Date Exygen Facility Management: ou Gude-- Richard A. Gr ph.D. President gen Ph Exygen Research 2-03 Date Study Director, Wildlife Intemational: Ai, t A os Sean Gallagher `Wildlife International, Ltd. Dae Gary Sponsor Representative, Entrix: o JEonhind Nested Exygon Research 6/13/03 Date Page 4198 Exygen Study No: 023.066 STUDYIDENTIFICATION Extraction of Potassium Perfluorooctanesulfonate from Red Blood Cells and Serum for Analysis Using HPLC-Electrospray/Mass Spectrometry EXYGEN PROTOCOL NUMBER: 01P-023-066 EXYGEN STUDY NUMBER: 023-066 TYPE OF STUDY: Analytical SAMPLE MATRIX: Mallard and Quail Red Blood Cells and Serum TEST SUBSTANCE: Perfluorooctanesulfonate (PFOS) SPONSOR: 3M Environmental Technology and Safety Services Building 236-09 PO Box 33331 St.Paul, MN 55133-3331 STUDY DIRECTOR: Sean Gallagher Wildlife International, Lid. 8598 Commerce Drive Easton, MD 21601 SPONSOR REPRESENTATIVE: John Newsted Enix, Inc. 4295 Okemos Road, Suite 101 Okemos, MI 48564 TESTING FACILITY/PRINCIPAL: Emily R. Decker INVESTIGATOR Exygen Research 3038 Research Drive State College, PA 16801 ANALYTICAL PHASE TIMETABLE: Study Initiation Date: Experimental Start Date: Experimental Termination Date: Analytical Report Date: 04123001 05/18/01 07/28/01 06/02/03 Exygen Research Page Sof 98 Exygen Study No: 023.066 PROJECT PERSONNEL `The Study Director for this project was Sean Gallagher at Wildiife Intemational, Lid. `The following personnel from Centre Analytical Laboratories, Inc., were associated with various phases of the study: Name Emily Decker Dave Bell Karen Risha Ling Ling Liu Marcia Swartzwelder Xiaoming Zhu Mitra Arjmand Lawrence Ord Ed Cames Shawn Robb Title Scientist Scientist Scientist Technician Technician Technician Technician Sample Custodian Sample Custodian Sample Custodian Exygen Research Page 6.098 Exygen Study No: 023.066 TABLE OF CONTENTS TUEOMIE osmmmismmmimasnsin ponmap----P1age GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT... 2 QUALITY ASSURANCE STATEMENT... CERTIFICATION OF AUTHENTICITY... 3 -- STUDYIDENTIFICATION... -------- PROJECT PERSONNEL... ss------------" TABLEOFCONTENTS... -- nen LI OFTS ABLET S... ss------------" LIST OFFIGURES............. ------ nnn 10 LIST OF APPENDICES... sms] 1.0 SUMMARY... s------ 20 OBJECTIVE............. a------------ 12 nn 12 3.0 INTRODUCTION... 4.0 TEST SYSTEM....... s---- s-------- nn 12 wn iS 5.0 REFERENCE MATERIAL........... sms 6.0 DESCRIPTION OF ANALYTICAL METHOD .......c.cc. 1d 6.1 EXIFACUON PROCCAUIE....o msm 6.2 Preparation of Standards and FORfication SOIUONS cu... 14 6.3 ChIOMAIOGEAPHY....r wsmm--------1 6.4 Instrument Sensitivity............. ------ 15 6.5Description of Instrument and Operating CONAIIONS............oovonsns 15 6.6 Quantitation and Example Calculation... ANA 7.0EXPERIMENTAL DESIGN... ---- 30 RESULTS. .ommmmmnns s---- NT] 9.0 CONCLUSIONS... smo 10.0 RETENTION OF DAA NDST AMPLEA S... nnn 19 Exygen Research Page 7 0f98 Exygen Study No: 023-066 TableT. Table II. Table Il. Table IV. Table V. Table VI. Table VIL `Table VII. Table IX. Table X. Table XI. Summaroyf PFOS Summary of PFOS Summary of PFOS Summary of PFOS SummoafPrFOyS Summoaf PrFOyS Summary of PFOS Summary of PFOS Summoaf PrFOyS Summary of PFOS Week 5 Summary of PFOS LIST OF TABLES in Reagent Blanks......... Page --) in Mallard Red Blood Cell Blanks......... 2 in Mallard Serum BIAnks.................. 2 in Quail Red Blood Cell Blanks 2 in Quail Serum BIGOKS corre 23 Recoveries in Mallard Red Blood Cells ..........c..... 24 Recoveries in Mallard Serum ... nS Recoveries in Quail Red Blood Cells ........vovurn 26 Recoveries in Qual Serum ...............ouscns 21 in Mallard Red Blood Cell Samples at 0 ppm a.i. for A -------------------------- 23 in Mallard Red Blood Cell Samples at 10 ppm a. for `Table XII. Summary of PFOS in Mallard Red Blood Cell Samples at 50 ppm a. for Weeks. ---------------- 30 Table XII. Summary of POS in Mallard Red Blood Cell Samples at 0 ppm ai. for Week 10 rn s---------- `Table XIV. Summary of POS in Mallard Red Blood Cell Samples at 10 ppm ai. for otk Wms sess 3] "Table XV. Summary of PFOS in Mallard Red Blood Cell Samples at 0 ppm a.. for Werik mma nmmnom---------3 `Table XVI. Summary of PFOS in Mallard Red Blood Cell Samples at 10 ppm as. for Week 15 -------- scnsmmnnn3 `Table XVII. Summary of PFOS in Mallard Red Blood Cell Samples at 50 ppm ai. for TERM wisn ---- 33 `Table XVIIL Summary of PFOS in Mallard Serum Samples at 0 ppm a.. for Week 5 ...34 `Table XIX. Summary of PFOS in Mallard Serum Samples at 10 ppm a.. for Week 5....35 Table XX. Summary of PFOS in Mallard Serum Samples at 50 ppm a.i. for Week 5....35 `Table XXI. Summary of PFOS in Mallard Serum Samples at 0 ppm a.i. for Week 10....36 Exygen Research Page 8.0798 Exygen Study No. 023.066 `Table XXII. Summary of PFOS in Mallard Serum Samples at 10 ppm a.. for Week `Table XXII Summary of PFOS in Mallard Serum Samples at 0 ppm a.i. for Week 15... ---- 38 Table XXIV. Summary of PFOS in Mallard Serum Samples at 10 ppm a.i. for Wetk DBiusmmmmmmmmsniin mem `Table XXV. Summary of PFOS in Mallard Serum Samples at 50 ppm a. for TERM......... ars---- ssn `Table XXVI. Summary of PFOS in Quail Red Blood Cell Samples at 0 ppm a. for Week 5 ..... ---------- nnn40 `Table XXVIL Summary of PFOS in Quail Red Blood Cell Samples at 10 ppm a.i. for Week5 ------ | `Table XXVIII Summary of PFOS in Quail Red Blood Cell Samples at 50 ppm a.. for WSs asmmmmm----=--g `Table XXIX. Summary of PFOS in Quail Red Blood Cell Samples at 0 ppm a.. for Wotlk Wann cS ------------ 42 `Table XXX. Summary of PFOS in Quail Red Blood Cell Samples at 10 ppm ai. for Week 10 ---- nes43 `Table XXXL Summary of PFOS in Quail Red Blood Cell Samples at 0 ppm ai. for LL osmmmmm-- `Table XXXIL Summary of PFOS in Quail Red Blood Cell Samples at 10 ppm a.i. forWeek 15.......... ---- -- `Table XXXIIL Summary of PFOS in Quail Red Blood Cell Samples at 50 pp a. for TERM... s---- 45 `Table XXXIV. Summary of PFOS in Quail Serum Samples at 0 ppm a.i. for Week 5....46 `Table XXXV. Summary of PFOS in Quail Serum Samples at 10 ppm a.i. for Week 5...47 `Table XXXVI. Summary of PFOS in Quail Serum Samples at 50 ppm ai. for Week 5 a-- ---- a7 `Table XXXVIL. Summary of PFOS in Quail Serum Samples at 0 ppm a.i. for Week 10... ------ nnn48 `Table XXXVILL Summary of PFOS in Quail Serum Samples at 10 ppm a.. for Week10........... s---- smc) `Table XXXIX. Summary of PFOS in Quail Serum Samples at 0 ppm a.i. for Week 15...50 Table XL. Summary of PFOS in Quail Serum Samples at 10 ppm ai. for Weck 15 ....51 Table XLL Summary of PFOS in Quail Serum Samples at 50 ppm a.i. for TERM ......51 Exygen Research Page 9.0f98 Exygen Study No: 023.066 Figure 1. Figure 2. Figure 3. Figure 4. Figure 5. Figure 6. Figure 7. Figure 8. Figure 9. Figure 10. LIST OF FIGURES Page Typical Calibration CUrVe fOr PROS... 53 Chromatogram Representing a 0.1 ng/mL standard for PFOS .................54 Chromatogram Representing a 1.0 ng/mL standard for PROS ..............55 Chromatogram Representing a Reagent Blank for PFOS (Exygen ID Reagent Blank A, Set: 051801A) .rvrvnrvre 36 Chromatogram Representing Control Quail Red Blood Cells for PEOS (Exygen ID: 0107376 Blank A, Set: 0518014) -- Chromatogram Representing Control Quail Serum for PFOS, (Exygen ID: 0107375 BlankA, Set:072301C) vr 38 Chromatogram Representing Control Quail Red Blood Cel fortified with 10 ng/mL. of PFOS (Exygen ID: 0107376 Spk A, Set: 051801DR)......59 Chromatogram Representing Control Quail Serum fortified with 10 ng/mL. of PFOS (Centre ID: 0107375 Spk A, Set: 072301D)........ 60 Chromatogram Representing Quail Red Blood Cell Sample (Exygen ID: 0107084, Sponsor ID: 454-108-401 WKS, Set: 05180IDR).......r..... 61 Chromatogram Representing Quail Serum Sample (Exygen ID: 0107207, `Sponsor ID: 454-108-407-WK1S, Set: 072301DD) 62 Exygen Research Page 10098, Exygen Study No: 023-066 LIST OF APPENDICES Page Appendix A. Study Protocol 01P-023-066 (Exygen Study No. 023-066) and AMENAMENtS ad DEVIRONS...rrrror en 63 Exygen Research Page 110198 Exygen Study No. 023-066 1.0 SUMMARY Exygen Research (Exygen) extracted mallard and quail red blood cell samples and serum samples for the determination of perfluorooctanesulfonate (PFOS) according to protocol 01P-023-066 (Appendix A). `The limit of quantitation for mallard red blood cells and serum was 10 ng/mL. The limit of quantitation for quail red blood cells and serum was 10 ng/mL. The LOQ for cach `matrix was determined in a method verification study performed at Centre (Centre Study: 023-065). PFOS in the mallard red blood cell samples ranged from non-quanitifiable levels to 418 pg/mL. PFOS in the mallard serum samples ranged from non-detected levels to 685 pg/mL. PFOS in the quail red blood cell samples ranged from non-quantifiable levels to 361 g/mL. PFOS in the quail serum samples ranged from non-quantifiable levels to 514 ng/mL. The average percent recoveries + standard deviation for PFOS in mallard red blood cell samples and scrum samples were 90% + 9% and 99% % 13%, respectively. The average percent recovery + standard deviation for POS in quail red blood cell samples and serum samples were 100% + 10% and 102% + 20%, respectively. 2.0 OBJECTIVE "The objective of this study was to determine levels of perfluorooctanesulfonate (PFOS) in specimens of mallard and quail red blood cell samples and serum samples using the analytical method described in protocol 01P-023-066 3I.0NTRODUCTION This report details the results of the analysis for the determination of PFOS in mallard and quail red blood cell samples and serum samples, using the analytical method entitled, "Extraction of Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds From Serum for Analysis Using HPLC-Electrospray/Mass Spectrometry". The study was initiated on April 23, 2001, when the study director signed Exygen protocolnumber 01P-023-066. The experimental start date was May 18, 2001, and the experimental termination date was July 28, 2001 Exygen Research Page 120198 Exygen Study No: 023-066 4.0 TESTSYSTEM The control mallard and quail red blood cells and serum used for the matrix blanks and matrix fortifications were received chilled on blu ice on May 17, 2001 from Wildlife Intemational Lid., Easton, MD. They were assigned the following Exygen ID numbers: Matrix Quail Serum Quail Blood Mallard Serum Mallard Blood ExygenID 0107375 0107376 0107377 0107378 Seventy-seven quail red blood cell samples and seventy-six quail serum samples were received chilled on blue ice at Exygen on May 17, 2001 and logged in by Exygen personnel and placed in frozen storage. Seventy-three mallard red blood cell samples and seventy-two mallard serum samples were received chilled on blue ice at Exygen on May 17,2001 and logged in by Exygen personnel and placed in frozen storage. Sample log-in and chainofcustody information can be found in the raw data package associated with this study. Storage records will be kept at Exygen and a true copy of the storage records can be found in the raw data package associated with this study. 5.0 REFERENCE MATERIAL The analytical standard PFOS was received at Exygen on June 3, 2000 from 3M Environmental Technology and Services. The available information `material was stored frozen for the reference material is listed below. The reference Compound PFOS ExygenControlNo. TCRNo, Purity (%) Expiration Date 00.023042 TCRO00I746 97.9 08/31/01 Exygen Research Page 13 0f 98 Exygen Study No: 023-066 `The molecular structure of PFOS is given below. PFOS Chemical Name = Perfluorooctanesulfonate Molecular weight = 499 (CsFinSOs) o Cefn| --O I Note: The neutral molecule and standard form from which PFOS (anion) is derived, is potassium perfluorooctanesulfonate [CsF:SOsK], molecular weight 538. 6.0 DESCRIPTION OF ANALYTICAL METHOD Analytical method entitled "Extraction of Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds From Serum for Analysis Using HPLC-Electrospray/Mass Spectrometry" was used for this study. 6.1 Extraction Procedure A 100 uL aliquot of the red blood cells and serum was used for the extraction procedure. After fortification of appropriate samples, the samples were vortexed for ~ 15 seconds. An aliquot of 0.5 milliliter of 0.5 M tetrabutylammonium hydrogen sulfate was added to the samples. One milliliter of 0.25 M sodium carbonate/sodium bicarbonate was added to the samples. Five milliliters of MTBE were added to the samples. Each sample was placed on wrist-action shaker for ~ 20 min. and then centrifuged for ~ 15 min. Four milliliters of the organic layer were taken and dried on a nitrogen evaporator and then reconstituted with 1 milliliter of methanol. Each sample was analyzed by LC/MS/MS electrospray. 62 Preparation of Standards and Fortification Solutions Standard solutions were prepared on March 14, 2001 as specified in Exygen protocol O1P-023-066. An individual stock standard solution of PFOS was prepared al a csaolntcecnotnrteantti)oninofme1t0h0anpogl/.mLFrboymditshissolsvoilnugti1on0,mgo1f.0tphge/msLt.anfdoarrtdif(iccaotriroenctsetdanfdoarrpdursiotlyutainond was prepared methanol. by taking 1 mL of the stock and bringing the volume up to 100 mL with A 0. pg/mL fortification standard was prepared by taking 10 mL of the 1.0 pg/mL fortification standard and bringing the volume up to 100 mL with methanol. A 0.01 Exygen Research Page 14.0f98 Exygen Study No: 023-066 pg/mL standard was prepared by taking 10 mL of the 0.1 pg/mL standard and bringing to 100 mL with methanol, A sat of standards containing PFOS was prepared by serial dilution of the 0.1 pg/mL and 0.01 pg/mLTsoTlutiTons inFtaheifonlltowrineg meannLeRrETE peepeeeres Tnitial Conc. (ug/mL)' Volume (mL) Diluted to (mL) _Final Conc. (g/mL) or 5 100 0.005 ol 2 100 0.002 ol 1 100 0.001 001 5 100 0.0005 001 2 100 0.0002 001 1 100 0.0001 "of PFOS The stock standard solution and all fortification and calibration standard solutions were stored in a refrigerator (4 + 2C) when not in use. Documentation of standard preparation can be found in the raw data associated with this report. 6.3 Chromatography Quantification of PFOS was accomplished by LC/MS/MS electrospray. The retention time of PFOS was ~ 4.4 min. Peaks were detected in the control matrices corresponding ( the analyte retention time, but the amounts detected were only significant enough to alter several fortification recoveries and the rest were less than the lowest calibration standard (0.0001 pg/mL) 6.4 Instrument Sensitivity The smallest standard amount injected during the chromatographic run had a concentrationof0.0001 pg/mL of PFOS. 6.5 Description of Instrument and Operating Conditions Instrument: PE SCIEX API 3000 Biomolecular Mass Analyzer Interface: SCIEX Turbolon Spray Liquid Introduction Interface Computer: Dell UltraSean P1110 Software: HPLC: PESciexAnalyst version 1.1 Windows NT, version 4 Hewlett Packard (HP) Series 1100 HP Quat Pump HP Vacuum Degasser Exygen Research Page 15of98 Exygen Study No: 023-066 HP Autosampler HP Column Oven HPLC Column:Genesis Cs (Jones Chromatography), 2.1 mm x 50 mim, 41 Column Temp.: 35C Injection Vol.: 10 uL. Mobile Phase (A): 2 mM Ammonium Acetate in ASTM type I water Mobile Phase (B): Methanol Flow Rate: 0.3 mLmin. Ti0me %60A %4B0 10 0100 70 0100 7560 40 10 60 40 Tons monitored: Analyte PFOS Mode negative Transition Monitored 499599 Approximate Retention Time (min; 420 Tune File Parameters Controls Set IS-Tospray 42000 DP-Declustering Potential 510 FP-Focusing Potential 2300 EP-Entrance Potential 100 `CE-Collision Energy 10 CXP-Collision Cell Exit Potential 5 DF-Deflector 300.0 CEM-Channel Electron Multiplier 28000 Gas Flows Set Nebulizer Gas 12 Curtain Gas 13 Collision Gas 4 TIS Temperature: 350C 6.6 Quantitation and Example Calculation "pTeeankmiacrreoaliwtaesrsmoefassaumrpeldeaonrdcatlhiebrsattainondasrtdancduarrvdewwearse ignejneecrtaetdeidnt(oustihnegL1Cx/MfSit/MwSei.ghTtheed Exygen Research Page 16.0198 Exygen Study No.: 023-066 linear regression) by Analyst software using six concentrations of standards. The concentration was determined from the equations below. Equation 1 calculated the amount of analyte found (in ng/mL, based on peak area) using the standard curve (linear regression parameters) generated by the Analyst software program. Then Equation 2 calculated the amount of analyte found in pg/mL (the quations for serum are shown) Equatio1n Analyte found (ng/mL) =(Paslroee pae-ina terck ept) Equation 2 Analyte found (ug/mL) = (anal. found (ng/mL) x EV (mL) x DE x EV (mL) x1ug Where: (AV (mL) x sample vol. (mL) 1000 ng FV = Final Volume DF = Dilution Factor EV = Extraction Volume AV = Aliquot Volume For samples fortified with known amounts of PFOS prior to extraction, Equation 3 calculated the percent recovery. Equation 3 Recovery (%) = (anal. found (g/m-aLvg). anal. in ctrl (ug/mL)) x(1000 ng/1 ug)x 100 amount added (ng/mL) An exampleof acalculation using an actual sample follows: Mallard serum sample Centre TD 0003803 Spk A (Set: 112100B), fortified at 10 ng/mL with PFOS, where: peak area = 6558 intercept = sis slope = m0 dilution factor =1 ngadded (fort level) = Ing avg amtincontrols = 0 (Not quanifiable) final volume = mL extraction volume = SmL aliquot volume = am sample weight (volume) = 0.1 mL Exygen Research Page 17098 Exygen Study No: 023.066 From equation 1: Analyte found (ng/ml) = From equation 2: Analyte found (ug/ml) = [6558-515] 7740 08ngmL = (O8ng/mLx 1 mLx 1x5mL)x lug (4mLx0.1 mL) 1000 ng From equation 3: = 000976 pg/mL % Recovery = (0.00976 g/mLx=0ug/mL)x1000) x 100 10 ng/ml. = 98% 7.0 EXPERIMENTALDESIGN Each set of samples (red blood cells or serum) consisted of one reagent blank, one matrix blank, two matrix blanks fortified at known concentrations, and ~ 20 samples. Each sample was extracted using the appropriate method and then analyzed in duplicate. 8.0 RESULTS `The amount of PFOS found in the reagent blanks are listed in Table I. The amount of PFOS in the mallard red blood cells and serum blanks are given in Tables II & IIL. The amount of PFOS in the quail red blood cells and serum are given in Tables IV& V. Peaks were detected in the control matrices corresponding to the analyte retention time. The amounts detected were only significant enough to alter several fortification recoveries and as a result are reported. The rest of the samples were less than the lowest calibration standard (0.0001 pg/mL) and not quantifiable. Individual recoveries for PFOS in the mallard red blood cell and scrum samples are detailed in Tables VI & VIL The average percent recoveries + standard deviations for PFOS in mallard red blood cell and serum samples were 90% * 9% and 99% + 13%, respectively. Individual recoveries for PFOS in the quail red blood cell and serum samples are detailed in Tables VIII & IX. The average percent recoveries + standard deviations for PFOS in mallard red blood cell and serum samples were 100% + 10% and 102% + 20%, respectively. PFOS in the mallard red blood cell samples ranged from non-detected levels to418 g/mL. Individual results are listed in Tables X-XVIL PFOS in the mallard serum Exygen Research Page 180198 Exygen Study No: 023-066 samples ranged from non-detected levels to 685 pg/mL. Individual results are listed in Tables XVITEXXY. PFOS in the quail red blood cell samples ranged from non-detected levels to 361 pg/mL. Individual results are listed in Tables XXVI-XXXIIL PFOS in the quail serum samples ranged from non-detected levels to 514 pg/mL. Individual results are listed in Tables XXXIV-XLL 9.0 CONCLUSIONS "The mallard and quail red blood cell and serum samples were successfully extracted and analyzed according to protocol 01P-023-066. 10.0 RETENTION OF DATA AND SAMPLES `When the final report is complete, al original paper data generated by Exygen will be shipped to the sponsor. This does not include facility-specific raw data such as instrument logs, however exact copies of temperature logs will be submitted. Exact copies of all raw data, as well as a signed copy of the final analytical report and all original faclity-specific raw data, will be retained in the Exygen archives for the period of time specified in 40 CFR Part 792. Retained samples of reference substances are archived by the sponsor. Exygen Research Page 19.0f 98 Exygen Study No. 023-066 Exygen Research Page 20 0f 98 Exygen Study Nos: 023-066 Table I. Summary of PFOS in Reagent Blanks Sponsor Centre n ne ReagenBlkA Mm ReagenBlankA no ReageniBlkA2 wm ReagenBlankA2* mo RegenBlukA mo ReagenBlankA mmoo RReeaggeemnBBllarkkAAt nm RegemBlukA mo ReagemBlkAt mo RegenBlkA no ReagenBlankA* m ReagemBlnkA nm ReagenmBlank A mo RegenBlnkA m ReagemBlnk A mo RegenBlukA mo RegemBlankA* no ReagenBlankA2 ma ResgemBlank A wo RegenBlnkA na ReagemBlankA na ResgemBlankA2 a ResgemBlnkA2e mo ReagemBlkA3 om ReagemBlank AS Se Number 0SISOIA OSISOIA 0SISOIB OSISOIB 001A 0S0IA 00502000188 0S20IA 082014 052008 052018 0S20IC 0S20IC O7190IA 071014 070014 O72001A 0720008 072008 073014 O7230IA 0723018 072018 072301C 07230IC Extraction ___Date SOI S801 1801 S801 S522U100I1 S2U0I S201 52200 52201 52201 52201 52201 52200 719001 719001 72000 72001 72001 72000 72301 72301 72301 72301 72301 72301 Analysis Date S/1s-1901 Sns-1901 s/1901 Soni ssnn2a0011 sn201 snan1 Sasol sn301 sn3n01 spat snl sns0l 119.2001 19.2001 101 101 R1.22001 122001 sion nsiol R401 0401 R42501 n42501 AVERAGE: STANDARD DEVIATION: Analyte Found (g/m) NNoo No xo xNoQ No xq xo NQ xq ~Q No NNoD NNDD ND No ND No No No No NNo NO NQ * Duplicate injection NbuQt w=asNoltesQsuatnhatniftihaeblleow(eAstpecaokncwenatsradteitoenctoefdtahtetchaelciobrrarteisopnosntdainndgaradnasl(y0t.e0r0e0t1enptgio/nmtLi)me. ND = Not Detected (A peak was not detected at the corresponding analyte retention time) For values recorded as NQ, 0.00005 pg/mL (half the value of the lowest calibration standard, 0.0001 pg/mL) was used to calculate the average and standard deviation. LOQ = 0.01 pg/mL for red blood cells and serum Exygen Research, Page 21 of 98 Exygen Study No.: 023-066 Table Il. Summary of PFOS in Mallard Red Blood Cell Blanks Sponsor Centre 1D mn Comol OATSBnkA conrol OI0778BlmkA comol OlTSBlnkA conrol OI0778BlmkA* convol OI7TSBlmkA2 cool OIO7SBlnkA2 conrol OIOTTSBlnkB __comol__OI07378 Blank B Set Number 020018 O2000B 0S201A 02201A 0522018 0S201B 0201C 052201C Extraction Ambsis Date Date S2IOL 522000 SRUDL 52201 52201 52301 S2201 52301 S2200 52301 S201 SPOL S201 S201 572001 sno AVERAGE: STANDARD DEVIATION: Analyte Found (ug/ml) No No No 00N0o24 000184 NNOo 0.000548 0.000927 Table II. Summary of PFOS in Mallard Serum Blanks Sponsor Centre Set Extraction Analysis Analyte m mn Number Date Date _ Found (g/mL) comol 010377BlkA3 710A 71901 7192001 000325 comrol 0107377 Blnk AS O710IA 901 7192000 000331 como OIOT77BlnkA OMIA 72001 T2UO1 000277 conrol OIOT3TBkA OR00IA 72000 201 000312 comol 0107377 Blank A2 0720018 72001 T2L2201 000188 conrol __0I07377 Blank A2 07200870001 721.2200 000214 AVERAGE: 0.00275 STANDARD DEVIATION: 0.000605 * Duplicate injection NQ = Not Quantifiable (A peak was detected at the corresponding analyte retention time but was less than the lowest concentration of the calibration standards (0.0001 pg/mL) LOQ = 0.01 pg/mL for red blood cells and serum For values recorded as NQ, 0.00005 pg/mL (half the value of the lowest calibration standard, 0.0001 pg/mL) was used to calculate the average and standard deviation. Exygen Research Page 22098 Exygen Study No: 023-066 Table IV. Sponsor iy Conia conmol conrol conol conol cool conol consol Summary of PFOS in Quail Red Blood Cell Blanks Centre ry OITSTGBlnkA | 0107376 Blank A 0I07376BInkA2 DIOTV6BlankA2 OI0776BlnkA OI07376Blank A O0T6BUmkA 0107376 Blank A___ Set Extraction Number Date OSISOIA SASOL OSISOIA SASOI O0SISOIB SASOI OSISOIB SANOI O2U01A S2UOL O2101A SRUOL 0S20IC S2201 052201C___5paiol STANDARD Analysis Date 5718-19001 S/IS-19001 S901 S901 S200 S52230001 sno AVERAGE: DEVIATION: Analyte Found (apm) NQ NQ NQ No NQ NNQQ Ng. NQ NQ Table V. Summary of PFOS in Quail Serum Blanks Sponsor 1 onwol | coniol conwol comol conol conol Centre Set Im Number Ol0775BlankA O72301AD OI07TSBlnkA* O720IAD OITSBlankA2 0073S Blank A 0077223300115B OIOTSBnkA3 O730IC 0107375 Blank A3___07230IC___ Extraction Analysis Date Date 2301 72601 2301 72601 7722330011 77224400000 T2301 7242500 R301 0425001 AVERAGE: STANDARD DEVIATION: Analyte Found (ig/ml) 0.00309 0002 NNQo No NQ 0.00100 0.00148 * Duplicate injection NQ = Not Quantifiable (A peak was detected at the corresponding analyte retention time but was less than the lowest concentration of the calibration standards (0.0001 pg/mL) LOQ = 0.01 pg/mL for red blood cells and serum For values recorded as NQ, 0.00005 pg/mL (half the value of the lowest calibration standard, 0.0001 pg/mL) was used to calculate the average and standard deviation. Exygen Research Page 230198 Exygen Study No: 023-066. Table VI. Sponsor iy cool conol conrol convol convol comrol conrol comrol comrol comrol conrol control comol control Summary of PFOS Recoveries in Mallard Red Blood Cells Centre n OIO7V8SpkA 0107378SpkA Ol07VSSpkB 01078 SpkB OIO7VTSSpkA OO7378SpkA* OIOTSSpkB O07378SpkB* OO7378SpkA2 OlO73SSpkA2 OI07378SpkB2 007378 SpkB2* OWO78SpkB __0I07378 SpkB* Set Number 0521018 0210 0S2101B 021018 0S201A 022014 052014 052201 05220B 052018 022018 05201B 05201C _0520IC__ Extraction Analysis Amt Date Date Added (ng/ml) S2UOL 522000 10 S2UOL 522001 10 S2UOL 522/01 50000 SRUOL 522001 50000 S201 523/01 10 S201 S301 10 SRL S301 50000 S201 R301 50000 52201 S301 10 S220L 2301 10 52201 52301 50000 $2201 52301 50000 S2201 2301 50000 522015301 50000 AVERAGE: STANDARD DEVIATION: RELATIVE STANDARD DEVIATION: % Recovery us 8 91 95 8 8 I) 0 7 101 105 102 101 90 9 11 -- LOQ = 0.01 pg/mL for red blood cells and serum Exygen Research Page 24 0f 98 Exygen Study No. 023.066 Table VIL. Summary of PFOS Recoveries in Mallard Serum Sponsor Cente i Comrol OIOTTTSPAS conwol OIOTSTISpAS conol OIOTTISIKBI conol comol OIOTSTISKB3 OIOTISHkA conol cool OIOTTISpKA OOTISpKB conol conwol 0O0I7O3T7T7ISSppkkBAe2 conwol conrol OIOTSTSpkA2 OIOTTISpKB2 conrol 0107377 SpkB2* * Duplicate infection Set Extraction Analysis Amt Number Date Date Added (nyml) O7TI90IA 71901 719-2000 0 OTISOIA A901 719.2000 10 OTIOIA TOI 7192001 500000 GTI90IA 02001A TI901 T2001 7192001 T2101 500000 0 OOTT00IIAA 2T2000011 7T22010011 50100000 0OT02010IAB T722000011 72T12.U202L00 500000 10 OT2000B OT00IB T2001 T2001 721-2200 721.2201 10 500000 0720008720001 _701.20001 500000 AVERAGE: STANDARD DEVIATION: RELATIVE STANDARD DEVIATION: LOQ =0.01 pg/mL for red blood cells and serum % Recovery 50 5 ww n 7 ur 19017 10 0 99 13 13 Exygen Research Page 25 0798 Exyen Study No. 023-066 Table VIL Summary of PFOS Recoveries in Quail Red Blood Cells Sponsor Conuol coniol convol contol coniol connol conuol conirol conrol convol comrol conol conrol coniol Centre Se Etracion Analysis Amt It) Number Date Date __ Added (ogiml) OIOTST6SPkA OSIGOIDR S801 21-2200 0 0107376 Spk A* OSISOIDR S801 521.2200 OIO73T6SpkB OSISOIDR 5/1801 21.2201 1500 OIO7376SBpk OSISOIDR S801 21.2201 0 0I07376SpkA2 OSISOIDR S801 521.2201 OLO7ST6SpkA2 OSISOIDR S801 21-2200 00 OIOTST6SPkB2 OSISOIDR 5/1801 21.2201 50 0l07376 Spk B2 OSISOIDR S/IBOL 5121-22000 OIOTST6SpKA 0S2101A SPUOI S200 100 OIO7YT6SpkAT 0S2I0IA S2MOI S200 0 OIO7I6SpkB OSOIA S2UOL 52200 50000 007376 SpkB* OS0IA S2UOL 52201 50000 OIOTHI6SPkA 0S201C P20 S301 10 0107376 SpkA_0S2201C__5n2001 ssl 10 AVERAGE: STANDARD DEVIATION: RELATIVE STANDARD DEVIATION: " Recovery 102 m3 1m 1nso 1 104 01 9 9% 91 100 10 10 * Duplicate injection LOQ = 0.01 pgm.for redbloodcells and serum Exygen Research Page 26.0198 Exygen Study No. 023-066 Table IX. Summary of PFOS Recoveries in Quail Serum Sponsor. Centre Set in iy Number conrol 0079S SpkA OZ30IAR coniol 0IO7375SpkA O30IAR conrol 0107S SpkB OZ30IAR conrol 0I07375SpkB* O301AR conrol 0I07TSSpkA2 07230ID contol 0107375 Spk A2 72301D convol convo OWO7ITSSpkB2 0723018 OI0737SSpkB2 0723018 comol contol OIOTISSpkA3 07230ID OIOTITSSpkAS 07230ID conrol OWTISSpB3 O730IC conrol__0I07375SpkB3*_O072301C * Duplicate injection Extraction Analysis Amt Date Date Added (ng/mL) _ 72301 725001 10 T2301 7501 10 72301 7501 500000 72301 72501 500000 72301 72627001 10 T2301 26.27/01 10 72301 724010 500000 72301 72401 500000 T2301 7262700 72301 262701 10 10 W230 242501 500000 72301 7042501 500000 AVERAGE: STANDARD DEVIATION: RELATIVESTANDARD DEVIATION: % Recovery 104 107 2 13 2s 126 106 105 100 101 102 20 20 LOQ=001 pg/mL for red blood cells and serum Exygen Research Page 27 0f98 Exygen Study No. 023.066 Table X. Summary of PFOS in Mallard Red Blood Cell Samples at 0 ppm a.i. for Week 5 Sponsor m ISEIDOWS 4S41093UOWES 4541003251WKS 4S4109DSIWESS SSEIDRDWES ASI0022WKst SSLIRSIWES ASLIODSIWEST 4541003254WKS 4SHI003254WKS SSLIRSSWES 4541093255WES 4541003256WhS 4541093256 Whs*_ Centre m 0107230 010730 00231 010731 0102 0107232 01023 0107233 O03 007234 00235 0107235 01023 010723 Se Extraction Analysis Analyte Number Date Date Found (ug/ml) 020008 S2U0L 522000 No O200B 0S20IB S20 SpUOL 5S2220011 00N01o97 OR00B S210 52201 02008 S201 52200 000167 NQ 0S101B S210 52200 ~Q 0208 S2U0L 52200 No 020008 S20 0SOIB SRUOL 52201 S200 xo xq OSI0IB S2IOL 52201 NQ 02008 S2U0L S200 000143 OR00B S210 52201 No OS2OIB SRUOI S200 Q 02108 Spu0L____ 520001 Ng AVERAGE: 0.000401 STANDARD DEVIATION: 0.000706 * Duplicate injection NQ = Not Quantifiable (A peak was detected at the corresponding analyte retention time but was less than the lowest concentration of the calibration standards (0.0001 pg/mL) LOQ = 0.01 pg/mLforredbloodcells and serum Fstoarndvaarldu,es0.r0e0c0o1rdpegd/amsLN)Qw,a0s.u0s0e0d05topcga/lcmuLla(thealfthtehaevevraalugee oafndthsetalnodwaersdt dceavliiabtriaotni.on Exygen Research Page 28.0198 Exygen Study No.: 023.066 Table XI. Summary of PFOS in Mallard Red Blood Cell Samples at 10 ppm a.i. for Week 5 Sponsor Centre n Jo) AS4I093280WKs 0107237 4541093280-WkS* 0107237 4SLI90WKS 0107238 45109-290-WkS* 0107238 ASLIONILWKS 0107239 454109.291Wks* 0107239 4SEI9292WKS 0107240 454109-292WkS* 0107240 4S4109-293WKS 0107241 450109-293Wks* 0107241 4S41093294WKS 01042 4541003294.WKs 0107242 454-109-3205WKS 010243 4541003095 WKS 0107243 4541093296.WkS 0107244 4541093296WKS 0107244 Set Number 0S2001BD 0S2101BD 0S210IBD OS20IBD OSOIBD 0S2101BD 0S2101BD OS2101BD 0S2101BD OS201BD 0S2101BD 0S210IBD 0S210BD 0S2101BD 0S2101BD 0S2101BD Extraction Analysis Date Date S210 301 S101 2301 S2101 2301 2101 301 S210 S301 2101 301 S210 301 52101 S301 52101 sn301 S101 301 S210 2301 S101 301 521001 S301 521001 sa301 521001 S301 __sp1i01 2301 AVERAGE: STANDARD DEVIATION: Analyte Found (ug/ml) 244 2u7 na 100 ns 123 151 131 301 308 488 395 189 188 264 285 178 880 * Duplicate injection LOQ = 0.01 pg/mL for red blood cells and serum Exygen Research Page 290f98 Exygen Study No. 023.066 Table XII. Summary of PFOS in Mallard Red Blood Cell Samples at 50 ppm ai. for Week 5 Sponsor Centre Ii) SSEI0930WEs 0107245 SSEININOWES 00745 ASHIINOWES 0107246 SSE10I0WES' 0107246 Se Number 052201CD 0220ICD 0S20ICD 09201CD Extraction Analysis Date Date 52201 52400 52201 dnl S201 S200 Spo snamt AVERAGE: STANDARD DEVIATION: Amiyte Found (agin) 589 @2 2 123 8 EY `Table XIII. Summary of PFOS in Mallard Red Blood Cell Samples at 0 ppm a.i. for Week 10 Sponsor. Centre Se m Ii Number SSI ROWED 0107250 | 020A SSLIDIAIWKIOT 0107250 0S20IA 4S41003250WKIO SSEIPIOWKIOH 0107251 0107251 0S201A 0S20IA ASLIORSIWKIO SSLIPDSLWKIOT 0107252 01022 020A 020A SSLI09R2WKIO SSEIDDRWKIOT 0107255 010253 0201 0S20IA SSLIORSIWKIO 0107254 020A SSEIPIIWKIOT SSLI09RSAWKIO 007254 0105S 0S20IA 020A 4S109056WKI ASLIORSSWKIO 0011007722555 00S22001AA ASLIRSSWKI ASLIRSCWKID 0010077225567 00522001AA 454109256:WKI0 0107257 0s201A * Duplicate injection Extraction Analysis Date Date 52200 sn301 52201 sn301 52200 52201 snot 52301 S200 52201 snl sn301 52200 52201 S230! sal 52200 snl 52201 5301 52200 52301 S52220010 s52s30l1 5522220000 ssessl! 52201 sn3ol AVERAGE: STANDARD DEVIATION: Analyte Found (ugiml) No No No No No No No No NQ NQ NQ No No NNQQ 000245 0.000200 0.000600 NbuQt w=aNsoltesQsutahnatniftihaeblleow(eAstpecaonkcwenatsradteitoenctoefdtahtetchaelicborrarteisopnosntdainndgaradnsal(y0t.e0r0e0t1enptgio/nmtLi)me LOQ = 0.01 pg/mL for red blood cells and serum For values recorded as NQ, 0.00005 pg/mL (half the value of the lowest calibration standard, 0.0001 g/mL) was used to calculate the average and standard deviation, Exygen Research Page 300198 Exygen Study No.: 023.066 Table XIV. Summary of PFOS in Mallard Red Blood Cell Samples at 10 ppm a.i. for Week 10 Sponsor i 4S41093280WKI0 454109-3280-WKI0 4S4109-3290WKI0 454109-3290-WKI0 4SE1093291WKIO 45109-3291-WKI0 4S109-292WKI0 4S4109-202-WKI0 4S109-293WKI0 4S109-203WKI0H 4S1093294WKI0 4541003294WKIOY 4S4109-3295WKI0 454109.3205WKI0 4S4109-296WKI0 454109.3296-WKI0 Centre mn 0107258 0107258 0107259 0107259 0107260 0107260 0107261 0107261 007262 0107262 007263 0107263 0107264 0107264 0107265 0107265 * Duplicate injection Set Extraction Analysis Number Date Date O52201AD S201 52324000 05201AD 52201 23-2401 OS201AD 52201 5232401 O05201AD 52201 23-2401 OS2201AD 2201 52324001 O0S2201AD S220 23-2401 OS20IAD S220 52324001 0S2201AD 52201 SR3:2401 OS2201AD S201 52324001 0S2201AD 52201 P3241 OS2201AD 2201 52324001 0S201AD S201 52324001 OS2201AD R201 52324001 05201AD S220 23-2401 OS2201AD 52201 5232401 052001AD__ Sn201 53-2401 AVERAGE: STANDARD DEVIATION: Analyte Found (g/mL) 193 196 204 202 11 149 613 660 ns 2 08 589 161 160 16 ug 303 207 LOQ = 0.01 pg/mLforred blood cells and serum Exygen Research Page 31 of 98 Exygen Study No.: 023.066 Table XV. Summary of PFOS in Mallard Red Blood Cell Samples at 0 ppm a.i. for Week 15 Sponsor Centre ry HS4I0020WKIS 0107266 4541093249-WKIS* 0107266 4S4I0900WKIS 0107267 SSEIDS0WKIST 010726) SSEI090SIWKIS 0107268 4SHI093251WKIS SSLIOR2WKIS 0107268 010260 ASLI022WKIS SSEIORSIWKIS 0107260 007270 ASEIRSIWKIST 007270 SSEI0RSAWKIS 00771 454109254WKIS 0107271 4SeI9ISWEIS 00722 4541003255WKISS 0107272 454100256WKIS 0107273 SSEI09SOWKIST 0107273 4541003236WKIS 454100236WKIS 0107274 0107274 Set Extraction Analysis Analyte Number Date Date Found (ug/m.) 052201 522000 2300 No 0S201B 522001 Saal 022018 52200 spon NQ No 0208 52201 sno 022018 52200 spol No 000179 052201 0208 52200 2200 sn301 sno 0001s No 02018 02208 S200 52200 sn301 spol No No 02018 2200 snon 0208 52200 sn301 No ND 05201 52201 ses! 0208 52200 sno ND No 0S20IB 52201 sno No 0S201B 522001 sn301 0208 52200 sno1 NQ No 052018 0522018 5200 sail sep3a0t1 NNQQ. AVERAGE: 0.000243 STANDARD DEVIATION: 0.000613 * Duplicate injection ND= No peak detected bNuQt w=aNsoltesQsuatnhtainftihaeblleow(eAstpecaonkcwenatsradteitoenctoefdtahtetchaelciobrrarteisopnosntdainndgaradnsal(y0t.e0r0e0t1enptgio/nmtLi)me LOQ = 0.01 pg/mL for red blood cells and serum Fstoarndvaarldu,es0.r0e0c0o1rdpegd/amsLN)Qa,nd0.f0o0r0N0D5,pzge/rmoLw(ahsalufstehde tvoaclaulecuolfattheetlhoewaevsetrcaagleibarnadtisotnandard deviation. Exygen Research Page 320198 Exygen Study No.: 023-066 Table XVI. Summary of PFOS in Mallard Red Blood Cell Samples at 10 ppm a.i. for Week 15 Sponsor Centre In m 4S4I0932WKIS 0107275 4541093289-WKIS* 00775 4541093200WKIS 0107206 4SH1003200WKIST 0107276 4S41093201WKIS 00277 4SHI093DIWKIST 0107277 4541003292WKIS 0107278 4S41003202WKIS 0107278 454100293WKIS 0107279 454100293WKIS 0107279 4541003294.WKIS 007280 4541093294-WKIS 007260 4541003295WKIS 007281 4541093295-WKIS* 007281 4541093296WKIS 007282 454100296 WKIS 0107282 set Number 02201BD OS20IBD O0201BD 0S201BD 02201BD 05201BD 02201BD 05201BD 0S201BDR 0S201BDR 05201BDR 0S2201BDR 05S201BDR 0S201BDR 0S201BD 05201BD Extraction Analysis Analyte Date Date Found (ug/mL.) sn20l 523.2400 55 S201 5232400 a2 S201 523.2400 S201 S232400 398 344 52201 523.2400 09 52201 5232400 ols S201 523-2400 965 S2201 5232400 89 5122001 sna 13 5122001 snaol 16 5/22/01 snr 154 522001 snail 5122001 Spal Lol 803 5122001 spat 656 S201 523.2400 063 __snoi01___sp324n 0505 AVERAGE: 311 STANDARD DEVIATION: ~~ 398 Table XVIL Summary of PFOS in Mallard Red Blood Cell Samples at 50 ppm a.i. for TERM Sponsor. Centre mn 1D 4S41005297TERM SSLI9S9TTERMS 010283 0107283 4541093298TERM 01084 454-109-208TERM 0107284 * Duplicate injection Set Number. 0S2201CD 0S20ICD O20IBDR __052201BDR___ Extraction Analysis Date Date 2200 S400 22001 sna 22001 snarl 52201 spat AVERAGE: STANDARD DEVIATION: Analyte Found (ug/ml) 275 m 406 ais 343 50 LOQ = 0.01 pg/mL for red blood cells and serum Exygen Research Page 33 of 98 Exygen Study No: 023-066 Table XVIII Summary of PFOS in Mallard Serum Samples at 0 ppm a. for Week 5 `Sponsor Centre n m 454109-324-WKs 0107303 4541003249-WhS 010703 4541093251WKS 010304 4541093251WKST 007304 SSEIDRWES 010705 454100252Whs 0107305 4SH1093253WKs 0107306 SSEIDISIWES 00706 ASLIDSAWES 010730) 454100254Whs 01007 454I090SSWES 00TH 4541003255WhS 0107308 4541093256WKS 010300 454100.3256-WKS 0107309 * Duplicate injection Set Number 072001A 0720014 O2001A 072001 070014 072001A OT0IA 07001A 000A 072001A 020A 072001A O2001A __072001A Extraction Analysis Date Date 70001 721000 72001 72100 72001 72100 72001 72000 72001 72101 72001 72100 T2001 72100 T2001 72100 2001 T2101 72001 72100 2001 72101 72001 72100 70001 72100 72001 72101 AVERAGE: STANDARD DEVIATION: Analyte Found (ug/ml) 000414 000417 000566 000599 000878 000943 000516 000499 000432 000444 000462 000392 000544 000516 0.00544 0.00167 LOQ =001 pg/mLforredbloodcells and serum Exygen Research Page 34098 Exygen Study Nos 023-066 `Table XIX. Summary of PFOS in Mallard Serum Samples at 10 ppm ai. for Week 5 Sponsor Centre Se m Number ISHIOHWS 0107310 OT00IAD SEIPIWES SLI0IVOWKS 0O0I703T1HI0 0RO0T00IIAADD 4SEI9I0WES SSLIOIDLWES 0O002 0ORT000IIAADD 4S4109001WEST SLI002WIS 0107312 007313 O001AD OT0IAD SLIDAVIWES OITA 0200IAD SSLIOIVIWES OOM OT0IAD 454109003WEST SLI004WKS 010734 OI0T3IS OT0IAD OT0IAD 4SLI09DVAWES SS4109320SWES OOIIO0T7I3HIS6 OOZTO00IIAADD 5100095 WESOI0T3I6___0R00IAD Extraction Analysis Date Date 70001 722000 T720000011 72201 72200 T2001 90001 72201 72200 2001 722000 72001 72200 T2001 72201 70001 72200 2001 72200 72001 72200 2R000011 77222200000 72001712001 AVERAGE: STANDARDDEVIATION: Analyte Found (ugiml) 128 6120 942 104 110 834 55s 504 766 06 515 73 765 864 222 Table XX. Summary of PFOS in Mallard Serum Samples at 50 ppm a. for Week 5 Sponsor Centre m ISEIIOWES 00317 4SEI093NOWEST SLI0ITOWES O07 007318 $54-10930-WkS" _0IOT3IS Sa Number O0OIAD O700IAD 072001AD O2001AD Extraction Analysis Date Date 72001 72200 T2001 722000 7720000011712072020010 AVERAGE: STANDARD DEVIATION: Analyte Found (ug/ml) 376 0 232%0 347 50 * Duplicate injection LOQ =0.01 pg/mL. for red blood cells and serum Exygen Research Page 350198 Exygen Study Noa 023-066 Table XXI.Summary of PFOS in Mallard Serum Samples at 0 ppm a.i. for Week 10 Sponsor CoIDre SSHHIO2R0OWWKO0 00007222 S4SLLDI9ODW0WKKOO 0000773233 SSLSILOIROSSSLIWWKKIOO O0007244 SSLSILGIORIRWWKKOO 0007725 S4SSLLIIDORRSSWWKOO 0000772266 SSSHLOIDOSISWEKWIKOO 00007733277 SSSSLLIIOOSSSSWWEOOT 0O007288 SSLSIHIODRSSC6WHWIEOO 00007752290 NeSwaber BaDcueon AmDabtses FounAdmaliGeym 00720008 70200010 7T221220000 0000007517 00020080 7722000011 7T211220010 000000676266 007720000188 70200010 7722112220001 000000655300 (O00BB 7T2000001 7T2202220001 00000098490 0020008 722000011 T7211220010 00000051i7 0O200008 772000011 772211.22220001 NNDD 0022000088 7722000011 1T202011 00000030337 0070000188 T72000010170712212220010 0o000iMse STANDARD DEAVVIEARTAIGOEN:: 00..0000427666 * Duplicate nection ND = No peak detected NQ = Not Quantifiable (A peak was detected at the corresponding analyte retention time but was less than the lowest concentration of the calibration standards (0.0001 pg/mL) LOQ = 0.01 pg/mLfor redbloodcells and serum For values recorded as NQ, 0.00005 pg/mL(half the value of the lowest calibration standard, 0.0001 pg/mL) and for ND, zero was used to calculate the average and standard deviation. Exygen Research Page36.0 98 Exygen Study No: 023-066 `Table XXII. Summary of PFOS in Mallard Serum Samples at 10 ppm a.i. for Week 10 Sponsor Centre n m 454109-3289-WKID 0107330 4541003280WKIO 0107330 4541093290WKI0 0107331 454109200WKIO 0107331 4SEI9I9LWKIO 007332 454100291WKIOT 00732 454109-292WKIO 0107333 4S193202WKIO 007333 4SEI93293WKI0 010733 454100293WKIOT 0107334 4SH1093204WKIO 0107335 454100204WKIO 0107335 454109-3205-WKIO 0107336 454100205-WKIO 010733 454109206WKIO 0107337 454-1093206-WKIO 0107337 Set Number. 072000BD 0200IBD 072000BD OR00IBD OR00BD O200IBD 07200BD 0700IBD OR00BD OD00IBD 072001BD OL00IBD 07200IBD OL00IBD 0200IBD __072001BD Extraction Analysis Date Date 72001 712200 72001 72200 72001 72201 72001 72200 72001 72201 72001 722010 72001 72200 72001 72200 72001 72201 72001 72201 7001 722000 T2001 72200 72001 72200 72001 72200 72001 72200 72001 722001 AVERAGE: STANDARD DEVIATION: * Duplicate injection LOQ=0.01 pg/mL for red blood cells and serum Analyte Found (ig/ml) 145 21477 25 95 102 107 nm 12 136 853 864 112203 Im 2 105 338 Exygen Research Page 370f98 Exygen Study No.: 023-066 Table XXIII Summary of PFOS in Mallard Serum Samples at 0 ppm a. for Week 15 Sponsor ConItDre SISSLIIO9I23W6KWIASS OOI0T73 SSELIIODNOWGASS O007T39 ASSSLLIIOORDSO0WWKKSS 00I00T7HH0 SSSSLLIIOONSSSILLWWKKSS OOT0THMI SSSHHIIORRNWESS 000302 SSSLHIIOORRSSWWESS 000007 SSSSHLIIOODRSSEEWWKKSS 0O0T4 SSSLLIIOODRISSSWWAESS 000077M5S SSSSLHIIOODDSSCEWWAHISS 00100773466 * Duplicate nection NeSmtber Excon Date Ams Date 0O70I910AIA T711990011 771199.22000011 O007I0AA 990010 T7992200000 0O771199001I4A 7711990011 771199..22000011 OO7T0I0IIAA 77109001 1719922000001 009900AA 7711990011 771199..22000011 00711900A1 TTAI0N1 79922000011 0O701910IAA TTAA09011 771199..22000011 0010910A1 7TI09011 T7119922000011 O07719109IA01471790011 _7_179192.0200011 STANDARD DEAVVIEARTAIGOEN:: Amiyie Found Gumi) xNDD 0000010729 >xp 000000444616 N>D 00000062839 NNDD 0000023939 00x1p5 000.0000651063 ND = No peak detected NQ = Not Quantifiable (A peak was detected at the corresponding analyte retention time but was less than the lowest concentration of the calibration standards (0.0001 pg/mL) LOQ'= 0.01 pg/mL for red blood cells and serum deviation For values recorded as NQ, 0.00005 pg/mL (half the value of the lowest calibration `standard, 0.0001 pg/mL) and for ND, zero was used to calculate the average and standard Exygen Research Page 38 of98 Exygen Study No. 023-066 Table XXIV. Summary of PFOS in Mallard Serum Samples at 10 ppm a.i. for Week 15 Sponsor Contre ID SSSHDIOHRWOKWSS 000077377 S4SSLLII0B3O0NWKKIISS 0OI007SMS SSLSILIODIRBOILWWKKIISS 0O0I70374H9Y ISSSLLIIOONDOWWKKIISS 0O007300 SSSHLIIDRNBSIIWWKKISS OO0017 SSLLIIROHVEAWWKKIISS 0000773322 SSSSLLIIDDIRBVSSWWKKIISSS O0O0T3Y SSSLIIDOSVHEGWWKKIISST 0010077335S4 Sa Exacion Amis Nember Due Date OO7II00IIAADD | 7T1N90L1 77220022100011 OOTT0IIOIAADD 771990011 772200221000010 OO7AI0IDAD TTIAON0I1 77220022010011 O7I0IAD OTI0IAD 7901 7901 7202101 7202101 OO77II00IIAADD TTII990011 77220022100011 OOT7IUS00IIAADD 7T1I990011 77220022100011 OO77II00IIAADD 771990011 77220022110011 OOTII0SOIIAADD 771990011 77220022110001 STANDARDDEVAIVAETRIAOGNE: Awayte Found Gm) 116522 5o7n5 152 jos 11s 607 iwsr 915126 71335 673 Table XXV. Summary of PFOS in Mallard Serum Samples at 50 ppm a.i. for TERM Sponsor Centre ID SSSELIIDDROTLTTEERRMMS 00I10077S3S8S5 4S5S4L10I0R2O9S6TTEERRMMS 01O0IO7T3S566 " Duplicate nection St Nember 0O77001IAADD _0O2T0N001IAADD Execton Amis Date Date 7722000011 7722220001 77220001017270220011 STANDARD DEAVVIEARTAIGOEN:: Amiyte Found mi) aass aawo 64338 LOQ =0.01 pg/mL for red blood cells and serum Exygen Research Page 390f 98 Exygen Study No: 023-066 Table XXVI. Summary of PFOS in Quail Red Blood Cell Samples at 0 ppm a.i. for Week 5 Sponsor. Centre iy 54105361WKS 0107077 4S410836LWKS 0107077 AS4I08362WKS OI0I0TS ASLI0S3QWEST 0107078 SSEI0SIGWES 0009 45410636-WKS 0107079 4S4I0SIAWES 0000 4SLIBIGLWKS OI0T0S0 4S4I08365WRS OLOTOSL SSLISIGSWES OIOTOSI 4S108366WKS 0107082 454108366WKS OI0T0S2 4SHI08365WKS 0107083 4S4I0836SWKS 0107083 Set Number OSIOLA OSISOIA OSISOIA OSISOIA OSISOIA OSISOIA OSISOIA OSISOIA OSISOIA OSISOIA OSISOIA OSISOIA OSISOIA OSISOIA Extraction Analysis Date Date SSO1 58.19/00 SASL S/IS-I901 SSO SS.19001 SASOL S/AS-19001 SASOL S891 SASOL SA8.19001 SASOL S891 SASOL SS-19000 SASOL SA8.19001 SASOL S891 SASOL S/IS-19001 SASOL SA8.19/01 SASOL 58.19/01 _SISOL___SN8-19/01 AVERAGE: STANDARD DEVIATION: Analyte Found (ug/ml) NQ No No NQ xq NQ xo No NQ NQ 000292 000264 NQ NQ 0.000440 0.000993 * Duplicate injection NQ = Not Quantifiable (A peak was detected at the corresponding analyte retention time but was less than the lowest concentration of the calibration standards (0.0001 pg/mL) LOQ=0.01 pg/ml for red blood cells and serum For values recorded as NQ, 0.00005 pg/mL (half the value of the lowest calibration standard, 0.0001 pg/mL) was used to calculate the average and standard deviation. Exygen Research Page 40 of 98 Exygen Study Noa 023-06 Table XXVIL S10umpmpamray.offoPrFWOeSekin5Quail Red Blood Cell Samples at Sponsor Centre i ASSLIISOS0AOILWWESS 0O0I700TO3S5S 4SSSLCII0O8S4A0W2KWKSS* 000l70T008S5S SSLSIHOISOOSSOMWWKKSS OOII00TTO0SS66 SSLIHAOILWMKS 0O0I70008S77 SSSSLHIIO0SSAM0SSWWKKSS OOIl007T0OSSSS SSIS0LI504S0066WWKKSS 0Ll00700889 SASSLHIIOOSSA0O-MWWEKSS' I001O09 44SSHHII0O4S0O80SWWEKSS* 0010I70009911 St Number OOSSIISSOOIIDDRR OOSSISSOOIIDDRRDD OOSSIISSOOIIDDRR OOSSIISSOOIIDDRR OOSSIISSOOIIDDRRDD OOSSIISSOOIIDDRRDD OOSSIISSOOIIDDRRDD __O0SSIISSOOIIDDRRDD Extraction Analysis Date Date___ SSS8O0 552211..22220011 sSSsOo p5222001 SSSSOO 552211..22220011 SSSSOO 552211..22220011 sSs/Sool 5522220011 SSSSOO SS220011 sS/sSOol s$2e2a0l1 S_s/SisOo1 52201 span STANDARD DEAVVIEARTAIGOEN:: Analyte Found (rym) 110 3351 530054 22598 7ais 1100500 5sot isi p3e6i9 324 * Duplicate nection LOQ = 0.01 pg/mL for red blood cells and serum Exygen Research Page 410f 95 Exygen Study No: 023.066 `Table XXVIIL Summary of PFOS in Quail Red Blood Cell Samples at 50 ppm a.i. for Week 5 Sponsor Centre m m SSEISMIWKS 00792 SSEIOSMLWKS SEI0SHRWKS 007092 007093 ASLI0S4QWKST 007093 Set Number 0S20ICD 0S20ICD 0S220ICD 0S20ICD Estacion Analysis Date Date 52200 S240 S201 SP40I S220 Snail Sn201 span AVERAGE: STANDARD DEVIATION: Analyte Found (uml) 166 163 108 103 135 3 Table XXIX. Summary of PFOS in Quail Red Blood Cell Samples at 0 ppm ai. for Week 10 Sponsor Centre m m SSEISIGLWKIO 007100 SSEI0SIGLWKIOT SSEISIQWKIO 007100 0070 SSHISIQWKION SSLISIGRWKIO 00701 007102 SSEISIGWKION 007102 SSEISIGEWKIO 0I07IOS 4SEISILWKION 007103 4SLI8IESWKIO SEI0SIGSWKIOT OlO7I0S 0I07I04 4SLIS3GCWKIO 4SE108366WKIOT OIOTI0S 0107105 4SLISITWKIO 0I07M06 44SSLEIISSIITSWWKKIIOON 000077100067 454108365 WKIO 0107107 * Duplicate infection Set Extraction Amlysis Analyte Number ___ Date Date Found (ug/ml) OSISOIB SASOL 5/9001 No OSISOIB SASOL OSISOB SASO1 S901 5/9001 No No OSISOIB SAS0L OSISOIB SASOL SA9001 5/1901 No No OSISOIB SAM0L S901 OSISOIB SASOL 5/1901 No NQ OSISOIB SSOl A901 OSISOB SASOI S901 No No OSISOIB AOL OSISOIB SASOI S901 S901 ~Q No OOSSIISSOOIIBB ASAOSOLI S5/9900011 NNQo OOSSIISSOOIIBB SSAISSOOL AS990011 NNoo 0SISOIB__ S801 s/ionL No AVERAGE: STANDARD DEVIATION: ~~ NNOQ NbuQt w=asNoltesQsuatnhtainftihaeblleow(eAstpecaokncwenatsradteitoenctoefdtahtetchaelciobrrarteisopnosntdainndgaradnsal(y0t.e0r0e0t1enptgio/nmtLi)me LOQ = 0.01 pg/mL for red blood cells and serum sFtoarndvaarldu,es0.r0e0c0o1rdged/masL)NQw,a0s.u0s0e0d05topcga/lcmuLla(thealtfhethaevevraalugeeofantdhestalnodwaersdt dceavliiabtriaotni.on Exygen Research Page 420198 Exygen Study Nos 023-06 `Table XXX.Summary of PFOS in Quail Red Blood Cell Samples at 10 ppm ai. for Week 10 Sponsor n SSSSLII0OGSAA0OLLWWAKII0O S4LSIL0ISSA2AWWKKIIOON SSLSILIOOLSOALBWWKAIIOO SSLSILIOOSSA0LLWWAKIIOO SSSSLLIIOOSSAOSSWWKAIIOO SSLSILI0OSH00C6WWKKIIOO SSLSIHIOOSOIMWWKKIIOO ASSLSIL0IO4O0SWWKHIOO * Duplicate nection Centre 0O10771805 00110077110099 OOII00T7ILI00 OOII0OT7HILI OOII00771I22 OOIIO0TTIIIIS3 OOIL0077TLIAE 0OlI00771L1ISS _ St Number GGSSIISSOOIIDDRRDD OOSSIISSOOIDDRRDD OSOISSIOOIIDDRR OOSSIIOSOIIDDRR OOSSIISOOIIDDRR OOSSIISSOOIIDDRR OOSSIISSOOIIDDRR 0OSSIISSOOIIDDRR Extraction Analysis Date Date __ SS8A0O1 5522220011 SS/SSOoIl S52220011 SSAASSOOIl 552211..22220001 SSSSOL S5211.222001 SSSSOL SS211.222001 SA8S0O1 552211.22220011 SSNASSoOlI $52211.22220011 S_s8ns0ol 5s21i.2a20n1 STANDARD DEAVVIEATRIAOGNE: Analyte Found (rpm 2an) 21500 22007 211920 210800 15095 2283 002s 212209 LOQ= 0.01 pg/mL for red blood cells and serum Exygen Research Page 430f95 Exygen Study No. 023-066 `Table XXXI. Summary of PFOS in Quail Red Blood Cell Samples at 0 ppm ai. for Week 15 Spoor ISTI036LWKIS ASSLEIIO3SRI6WLKWIKISS SSSSLHII0ISIGRWWKKIISS SSSSLHII0OSSIGLEWWKKIISS SSSSLLIIOOS3IGGSLWWKKIISS SSLIBISWKIS SL0S36GWKS SASSHLIIS0S3S6E6OWWKKISS SUOSEWKS SSLIOSIESWHS SSSSLHIISSIIBBWWKAISS ASLISITIWKIST Centre n 0107116 OOW007THIG 0O007T1H7S O0T0ITSH 0O0I70172H09 007120 00721 000077222 00712 00712) 00007712263 0107124 Sa Etracion Number Date Analysis Date Analyte Found (rym) 0S2100A S201 OS0IA S2Uol 52201 spl No xo 001A 00 szuol S2U0l S201 Spal No No 0O0sa10lAA Ss2zUu0oLl sSppaonl 000000222s6 Osa0IA szuol Spam 001A SRUOL 52201 000127 No 0Os0a00I1A sSz2uUo0lL s22p0l1 000000379015 os0IA OIA sauol s2i0l sna San No No 020A 020i sol saol S200 Spa 000795 000816 O2W0IA 0SH0IA sol S2U0L spa spol xo No 00s220001AA__ ssapouln Ssp2a0w0n 00N01o30 STANDARD DEAVVIEARTAIGOEN:: 00..0000139084 * Duplicate nestion ND = No peak detected NQ = Not Quantifiable (A peak was detected at the corresponding analyte retention time `but was less than the lowest concentration of the calibration standards (0.0001 ng/mL) LOQ = 0.01 pg/mL for red blood cells and serum For values recorded as NQ, 0.00005 pg/mL(half the value of the lowest calibration standard, 0.0001 pg/mL) and for ND, zero was used to calculate the average and standard deviation. Exygen Research Page 44.0798 Exygen Study No. 023.066 `Table XXXII. S10umpmpamrayi.offoPrFWOeSekin1Q5uail Red Blood Cell Samples at Sponsor n Centre SSLSCOILOAMOOLLWWKKIISS 001007712255 SSLSLIIOOLNAORZWWKKIISS 0010077112266 SSSSLLIOOLSOAAMWWKIASS 00007711277 ISSSLLIOOSAAD0LWLKWIASS 001707S8 SSLLIILOASOSSWWKKIISSt 000077112200 SSSSHLIISOS0O6GWWKKIISS 0O0I7073I00 SUSSLLIIOOLLA0WIKWIKSISS 0O0I0773TI13 SSHLOOLLOOSSWWKKIISS 00I0072I2 SSSSLIHSBIEIWWKKISS' 00100771333 NSoemtb.er Date Extraction AnaDlyasties.___FounAdnal(ytrepm) OOSSO0IAADD| sS2OIUoLl 5$2222.22330001 n12 OORS100IIAADD SS2DIDLI $S2222.233001 21366s 00RRAI0IIAADD Ss2aIuDoLl 5S2222.22330011 21828 OORSIO0IIAADD SS22UUOOLL SS222222330011 1230 OOSSOOIIAADD SSADUUDOIL 5S222222330011 11598 OOSRUA00IIAADD SSA2IIODL 557222..22330011 3I61 OORSU00IIAADD SSO2UIOLL $52222.22330001 915303 002020D1 SS2oIuOlL sS4a0o1 11254s O0R0R01DAD__sS2puUo0lL _ 5s2m2a2o3s0m0n 5sa6l7 STANDARDDEVAIVAETRIAOGNE:: 220438 Table XXXIIL Summary of PROS in Quail Red Blood Cell Samples at 50 ppm a.i. for TERM Sponsor Centre SSSILOIRGAOOTTEERRMMS O01T07N4 SSIS0LSIASIAOITOTEERRMMY 0010077113355 * Duplicate nection NuSmtber 00SS2I001ICCDD 00R0200i1CCDD ExtDraatcteion AnDaaltey__s_is FouAnndal(ytpem) SS220210 s52p4o0l1 336516 sSp2o2l0 Ssp4a1n h10n6 STANDARD DEAVVIEARTAIGOEN:. 213444 LOQ =0.01 pg/mL for red blood cells and serum Exygen Research Page 45098 Exygen Study No. 023.066 `Table XXXIV. Summary of PFOS in Quail Serum Samples at 0 ppm a.i. for Week 5 Sponsor 13 SSEI0S6IWRS SSEIOSIGLWES SSEISIQWES ASEIBIRWAS' SLISIGWES 4SEI0SIGWES SLISIGLWKS 4SLI0SI4WES SLIS366WRS SSEI0SIGWES ASEIOSISWKS SLIOSILWES' Centre m 0107154 OI07IS4 OI07ISS OI07ISS OO7IS6 OOOITOITSITS 0O0IO7T1ISST OIOTIS OI07IE 0107160 * Duplicate injection Se Number O7230IAR OTB0IAR OR30IAR 0230IAR OTBOIAR OOM7B300IIAARR OO7T3B0OIIAARR OTB0IAR OTB0IAR OT230IAR Extacton Analysis Date Date 72301 25001 72301 2501 72301 S01 92301 72500 72301 2501 7T22330O1L 7722550000 R301 92301 72501 72501 R301 72500 92301 72500 70301 7nsi01 AVERAGE: STANDARD DEVIATION: Amiyee Found (uml) 0082 00205 00149 oo1ss 00198 00000156160 000535 oo13s 00120 oo138 00156 00156 0.00746 LOQ = 0.01 pgmforred bloodcells and serum Exygen Research, Page 46.0198 Exygen Study No.: 023.066 `Table XXXV. Summary of PFOS in Quail Serum Samples at 10 ppm a. for Week 5 Sponsor ASHI08402WES 4S108402WKS* 4S108403WKS 4S108403WKS* 4SL108404WKS 454108404WKS* 4S108405WKS 4S4108405Whs* 4S4-108406WKS 454108406WES ASLI0S407WKS 454108407-Whs* 4S4-108409WKS 454-108-408.WKS* Centre In 0107162 0I07IG2 0107163 010763 007164 010TH 0107165 0107165 0107166 O107IG6 0107167 0107167 0107168 0107168 set Number 072301AD 072301AD O72301AD OT2301AD O7201AD 072301AD O72301AD 072301AD O7T2301AD 072301AD O7230IAD 072301AD O72301AD _072301AD Extraction Analysis Date Date 72301 726001 T2301 72601 72301 7726001 T2301 72601 72301 72601 72301 72601 72301 7726001 T2301 72601 72301 72601 72301 72601 72301 72601 72301 72601 72301 72601 70301 72601 AVERAGE: STANDARD DEVIATION: Analyte Found (ug/ml) ass 56 us 128 104 983 138 129 106 107 24 363 76 844 898 350 Table XXXVI. Summary of PFOS in Quail Serum Samples at 50 ppm a.i. for Week 5 Sponsor Centre i ID ASEI0S4LWES 0107092 4SH10844LWES 0107092 4SE108442WKS 0107093 454.108.4420WhS* 0107093 * Duplicate injection set Number O72301AD OT2301AD O7201AD 0T2301AD Extraction Analysis Date Date 72301 726001 72301 72601 72301 72601 72301 72601 AVERAGE: STANDARD DEVIATION: Analyte Found (ug/ml) El s62 59 520 sat 19.4 LOQ =0.01 pg/mL for red blood cells and serum Exygen Research Page 47098 Exygen Study No.: 023-066 Table XXXVIL. Summary of PFOS in Quail Serum Samples at 0 ppm ai. for Week 10 Sponsor Centre n Io) 4S10836LWKIO 0107177 4SC10836LWKIOT 0107177 4S108362WKIO 0107S 4S108362WKIOT 0107178 4S10836RWKIO 0I07I79 4SC108363WKIOT 0107179 4S4108364WKIO 0I07ISO 4S108364WKIOT OI07IS0 4S4108365WKIO OIO7ISI 4S-10836SWKIO OIO7ISI 4SH108366WKIO 0I07IS2 4S108366WKIO 0107182 4S4108367WKIO 0L07ISS ASLI08367WKIO 0107183 4SH108365WKIO 0L07ISe 454108368 WKIO 0107188 set Number 072301B O7T230IB 07230B O7T230IB 072308 O7T230IB 07230B O7230B O7230B O7T230B O7230B OT230B O72301B O7T230B O72301B 0T230IB Extraction Analysis Date Date 72301 724/00 72301 724001 72301 724001 72301 724000 72301 72401 T2301 724001 72301 72400 T2301 724001 72301 72400 72301 724000 72301 724001 70301 724000 72301 724001 72301 724001 72301 724001 70301 7724/01 AVERAGE: STANDARD DEVIATION: Analyte Found (ug/ml) 0.0083 000489 0.00295 0.00249 0.00467 000521 0.00390 0.00375 000271 000292 000439 000437 000563 000542 000537 000526 0.00430 0.00105 = Duplicate injection LOQ =0.01 pg/mL for red blood cells and serum Exygen Research Page 48 of 98 Exygen Study No.: 023-066 Table XXXVIII Summary of PFOS in Quail Serum Samples at 10 ppm a.i. for Week 10 Sponsor Centre mn iy 454-10840LWKIO 0107185 454-10840LWKIO 0107185 454108402WKIO 0107186 4S108402WKIO 0107186 454108403WKIO 0107187 4S4-108403WKIO* OI07IST 4S4108404WKIO 0L07ISS 454108404WKIO OL07ISS 454108405WKIO 0107189 4S4-108405WKIO* 0107189 4S4108407-WKIO 010790 454-108407-WKIO* 010719 454108408WKIO OI07I91 454-108-408WKIO 0107191 set Number 07230IDD 07230IDD 07230IDD 07230IDD 07230IDD 07230IDD 07230ID 07230ID 07230IDD 07230IDD 07230IDD 07230IDD 07230IDD 072301DD Extraction Analysis Date Date 72301 727.2801 72301 727-2801 72301 72-2801 T2301 7727-2801 7231 7272801 72301 727-2801 72301 727-2801 72301 727-2801 72301 7727-2801 72301 727-2801 72301 7720-2801 72301 7727-2801 72301 7727-2801 703/01 __ 7727-28001 AVERAGE: STANDARD DEVIATION: * Duplicate injection LOQ = 0.01 pg/mL for red blood cells and serum Analyte Found (ug/ml) 213 207 536 527 148 mm 194 203 157 147 105 110 970 97 4 624 Exygen Research Page 49 0f98 Exygen Study No: 023.066 Table XXXIX. Summary of PFOS in Quail Serum Samples at 0 ppm a.i. for Week 15 Sponsor SSEIBIGLWKIS SEIOSIGLWKIS 4S4I06362WKIS 4SEISIQ WRIST SSEISIGLWKIS 4S4I08363WKIS SSEIBIGEWKIS 4S4I0836HWKIS SSEIBIGSWIS 4S4I08365WKIS 4SEISIGCWKIS 4SLISIGEWKIS 4SEI0636TWKIS 4S4I08367WKIST 4SEI0S3GEWKIS 4SHI036SWKIS 4S4I0833-WKIS 45108339WKIS Centre 0107192 007192 OI0TIS3 007193 0l07I 0107194 OIO7I0S 0107195 0107196 0107196 0107197 007197 010718 0107198 010719 OL07I9 0107200 0107200 Set Extraction Analysis Analyte Number Date Date Found (ug/ml) 07230IC 72301 7242500 NQ O0R30IC T2301 242500 No OT20IC 2301 7242501 No O07230IC T2301 242500 T230IC T2301 7242501 No 000154 OT20IC 2301 7242501 000160 0T0IC T2301 7242501 No OT20IC 0T230IC 72301 T2301 77224422550001 NNoo O7T230IC 92301 72425001 0T0IC 72301 7242501 No No 07230IC O7230IC T2301 7242500 72301 7242500 No 000227 O7T230IC 2301 7242501 000249 O720IC T2301 7242501 O720IC 72301 7242500 000253 000255 O7280IC 0301 72425010 072301C 0301 72425000 000162 000160 AVERAGE: 0.000928 STANDARD DEVIATION: 0.00105 * Duplicate injection NbuQt w=aNsoltesQsuatnhtainftihaeblleow(eAstpecaokncwenatsradteitoenctoefdtahtetchaelciobrrarteisopnosntdainndgaradnasl(y0t.e00re0t1enptgio/nmtLi)me LOQ = 0.01 ug/ml for redbloodcells and serum Fstoarndvaarldu,es0.r0e0c0o1rdpegd/amsLN)Qa,nd0.f0o0r0N0D5,gz/emroLw(ahsalufstehde tvoaclaulecoulfattheetlheowaevsetrcaagleibarnadtisotnandard deviation. Exygen Research Page 50 0f 98 Exygen Study No. 023.066. Table XL. Summary of PFOS in Quail Serum Samples at 10 ppm a.i. for Week 15 Sponsor 4S410840LWKIS 454-10840LWKIS* 454108402WKIS 45108402WKIS 454-108405WKIS 454108403WKIS 4S108404WKIS 454.108404-WKIS* 4S4-10840SWKIS 454108405-WKIS* 4S4-108406WKIS 454.108406-WKIS 4S4108407-WKIS 454108407-WKIS 454-10840WKIS 454-108408-WKIS* 454108383-WKIS 454108383WKIS Centre m 0107201 0107201 010702 0107202 0107203 0107203 0107204 0107204 0107205 0107205 0107206 0107206 0107207 0107207 0107208 0107208 0107209 0107200 set Number 07230IDD 0730IDD 07230IDD 0730IDD 07230IDD 07230IDD 07230IDD O720DD 07230IDD 07230DD 07230IDD 07230DD 07230IDD 07230DD 07230IDD 07230DD 07230IDD 07230DD Extraction Analysis Date Date 723001 727-2800 72301 727-2801 72301 727-2801 T2301 727-2801 72301 727-2801 T2301 7727-2801 72301 727-2801 72301 7272801 72301 7272801 72301 727-2801 72301 727-2801 72301 71272801 72301 727-2801 72301 7272801 72301 727-2801 72301 7272801 72301 72728001 723/01 7127-2801 AVERAGE: STANDARD DEVIATION: Analyte Found (ugim. 181 150 821 845 246 239 11 107 1 156 704 698 107 na 102 891 31 143 950 66 Table XLI. Summary of PFOS in Quail Serum Samples at 50 ppm a.i. for TERM `Sponsor Centre In n GSH108410TERM 0107211 45410841TERMY_ 0107211 * Duplicate injection set Number 072301DD 07230IDD Extraction Analysis Date Date 72301 727-2801 723/01 7127-28001 AVERAGE: STANDARD DEVIATION: Analyte Found (ug/ml) 3 sis 495 2%9 LOQ = 0.01 pg/mL for red blood cells and serum Exygen Research Page 510f98 Exygen Study No: 023.066. Exygen Research Page 52.098 Exygen Std No: 023.066 Figure 1. Typical Calibration Curve for PFOS SR SA o E HURT HS a, Jo . si wou i" . wou oon] ed 2404] = 20041 1.804. 160s i I ou] J one] A 8000.01 ' wna] JS / / / /J */ Sf{ wl I Fagg Rescarch Page 53015 Figure2. Iss Exygen Study No. 023-066 Chromatogram Representing a 0.1 ng/mL standard for PFOS = El, EL - | : od 3 | | 3 | ] 3 | ]: | 3 2ed .[--= Th VARA | | odorpagar, ee RL | Eugen Research Page tors Exygen Study Noa 023-06 Figure 3. Chromatogram Representing a 1.0 ng/mL standard for PFOS mala EE. i 2 | [Ee HE = | 3 | = J IE | = | | FE | I] || | g Io : hc pn son, Hem 2 pp gamed, EIR Exygen Research Page 55 of98 Exygen Study No. 023-066 Figure 4. Chromatogram Representing a Reagent Blank for PFOS (Exygen ID Reagent Blank A, Set: 0518014) Jm E r ~~ | EEE iC | || ad | | ho | pboooo 1. i3] . Li a 4 1 | h1 1 {iim- wir] Ihaem wlFlit) weTI l 1hi a ieTawim] | WAC | Exygen Research Page 560198 Exygen Study No.: 023-066 Figure. Chromatogram Representing Control Quail Red Blood Cells for PFOS (Exygen ID: 0107376 Blank A, Set: 0518014) Ise : | ] : | | 10 T -| | Werle Pr3 flif TH. ]1 || Iil iJiIlI | 4S0| L fmI Te L | |1 i i HiyI 4 lL || 1a0 fHwR! | -l V 1 1. Ti= | {4oTllH mem T-- Thl | Exygen Research Page 570198 Exygen Study No.: 023-066 Figure 6. Chromatogram Representing Control Quail Serum for PFOS, (Exygen ID: 0107375 Blank A, Set: 072301C) Ermr e EE Ge 3 | B| o-#y oFi = | 1 | 2 - 5 | 3::] If| o | i| | a J J TRII TE J Te a pm EE 1h on] nw nWaAtY | phan ee Bpgen Roseuch Page 380198 Exygen Study No. 023.066 Figure 7. Chromatogram Representing Control Quail Red Blood Cells fortified with 10 ng/mL of PFOS (Exygen ID: 0107376 Spk A, Set: 051801DR) |e a EEfeE fe || FE ES | SEE Eo | | 3 {3 + |3 | 7 Exygen Research | | Nem | Page 590198 Exygen Study No.: 023-066 Figure 8. Chromatogram Representing Control Quail Serum fortified with 10 ng/mL of PFOS (Exygen ID: 0107375 Spk A, Set: 072301D) IEEE EEE | 13 ol = 43 3 | 2 Lo em 3 Exygen Research | | | || | MiS ntoE nar E cme Page 600108 ExygenStudyNo.: 023-066 Figure9. Chromatogram Representing Quail Red Blood Cell Sample (Exygen ID: 0107084, Sponsor ID: 454-108-401 WKS, Set: 051801DR) EEE. Eff : EEFeeasHH,EE =----- ||| | = | - | E | | 5 = | | 2 |I _ ew] Exygen Research Page 61 of 98, Exygen Study No.: 023.066 Figure 10. Chromatogram Representing Quail Serum Sample (Exygen ID: 0107207, Sponsor ID: 454-108-407-Wk15, Set: 072301DD) 0107207 454-108-4071)OF 5000 1o0r0zo)rooetssma a = aVuozroaCnGthrarrirs7 Fat | Taw sw | aw Ew ek Teayo Exygen Research Page 62098 Exyaen Study Nos 023-066 Study Protocol 01P-023-066 (Centre Study No. 023-066) and Amendments and Deviations Exygen Research Page 630198 Exygen Study No. 023-066 Cente Proce No, 1P-023.066 i | ANALYTICAL PHASE PROTOCOL i i ANALYTICAL PHASE TITLE t } | EXTRBALCOTOIDONCEOLFLPSOFTOARSSAINUAMLYPSSPEIESRCTUFSRLIOUNMGEOHTRPROLYCOECLTEACTNREOSSPURLAFFYRMOOANSMASRTEED | i i| { ME STPeOtNSORdy Sri | Building 232.09 i St.PauPlO, MBoNx 5335313313331 i "DATA REQUIREMENTS i AnsyicalMethodRequirements | i PERFORMINGLABORATORY i StateColReegsc,uPeA.br16e801 i Phone 814-231-8032 { i PROTOCOLIDENTIFICATION NUMBER || 01P023-066 i CenteAnataLibor, ne. Exygen Rescarch Pugs 10129 i Page64.0 95 Snes ; SRT |: `TABLE OFCONTENTS t; SE -- ! % memmeAToNFORTSacOn OFTETESTEs | i S. PERFORMINGLABORATORY ...cooosmmrummmssssnemmsssmsssmsne { 6. PROPOSEDEXPERIMENTALTIMEFRAME... eed | | 11. PROTOCOLAMENDMENTSAND DEVIATIONS coon 11 i 514. ARCHVESTATEMENT. ooo 0 DA ANDT REPA ORT ...cocormmmsssssmsmmssmssmmssmssssss 18 !| 16. REFERENCES... mms a ---- i | J | CenteAnayaLaboratories, ne. Exygen Research Page20129 i Page 65 of 98. [-------- CoePrac p05 | BTiEle:mAcTiON OF OTASSIAOM h PToERRFLRy USOT ROOCTA UANTEOSAUTS LFFFROOONMNARTESD 1 rhuepmouspes i syissys ldandqu odclssls :t 1 !! for residues of perfluorooctanesulfonate (PFOS) SiCotmoypsyFOruoammaFmoieaEnESon), "Extraction Of Potassium Perfluorooctanesulfonate hapeeoarpem using method entitled, Or Other Fluorochemical i ; Th spi pha willbecodcd ndecEPATSCAGodLarry | Practicestandards40 CFRPart792(1). | R---- i | T[ h lignT itesr i i [o icnwk oemwa or] : ; CCrhhoeomsmiietoanmse: sve of hecompospsn. Petvonseanelonsc {| | TUPACName: CNoaesmeie 9BKe1CYvR-seOonnc,)atpciado,1ns2.c2h3s34u4,l5.5f66o17n88c8- i ! ; ! an i |! :| Not The ml lee snd seni rom whch PROS anion) obbtaineed is peruorooctancsulonste potassium salt [CiFySOK], molecular Aoo festndmfn ensce n siress esp,ssCcodoondnsnddoenordd CoeAnt Less san Euygen Research Page 660195 Exygen Study No. 023-066 CateProtocol No. O1P-023066 sudbosctuamnecnetsiwnigclhlabieni-nocflucduesdtaosdpyaranodftshheiprpaiwndgatraecpocradsgef.or racking of the test 1 + uAlnliqsutealnadbaerldsoresntumsbeurobn sthaectnodnaataninynpecrrepoeracrresodsss-refoerenlcmeudustt0bttehecidoiennttaiofiineednrwitsha ; | HAZARDINFORMATION i |! AtesctuirnrgefnatciMliStyD. S fothechemmical(s)usd in this study will be maintained a the i i 3. SPONSOR B3uMilEdnivnigr2on3mEe.n0t9al TechnologysndSafety Services 1{ PStO PBaoulx, 3M33N31551333331 ; i| T`RSoEpcLohnEeslPolrHeROReNoprEbe:isaene6t5aa1t.i7ve7:8.7065 }; | FAX NUMBER: 651.776.6176 i 4. TESTING FACILITY | `8W5i9l8diCfoemImnteermcateioDnrailv,eLid. Easton, MD 21601 EE -- i i SSeTaUnDGaYllDaIgRheErCTOR: || TFEALXENPHUOMNBEE:R:441100-.862222-.80660302 || 5. PERFORMING LABORATORY i| | 3SCe0tn4at8troRCoeAlsnleaealgryetc,ihcPDaArliLva1eb6o5r0a1tories, Inc. (Centre) fi i TEmEiLlEyP.HOSNtaEu:ffer, 8C1e4n-tr3e31-8032 FAX NUMBER: 814.231.1580 { 6. PROPOSED EXPERIMTEIVNEFTRAAMLE AnAanlaylyttiiccaall STearrmtiDnaatteion Date April23,2001 "April 30,2001 Report sued May 31,2001 Centre AnalyticalLaboratories,nc. Pagers i Exygen Research Page 670198 Exygen Study No. 023.066 Centre ProNo.cO1P-o023l066 7. JUSTIFICATION FOR THE SELECTION OFTHETESTSYSTEM i . Mwillabealunsdeqlduaaiaslethdreblanodaoldyticclals ssaammpplleess cfoolrletchtiesd bpyhaWsie.ldiMfaelIlunrtdesmaatnidoqnuLaadill.,s i threepyrdesoentwewlilldibnirdabpoorpsuloartyioennsviarnodnmtehnety.arQeEuaPilAharbeitcaotmsmienncdluedde sbpueschiyspabsetcuaruess,e i| rassy roadsides, famiands and open woodlands, an they are considered land | cgdreatozeenrnns.inse MiisfaqlPdulRaaOrtedSrgwhraaaebzsietrddaset.psosiiTnthceleduduienstephooenfdwtsh,hoelsleaekbmelasotoradinocdfemsmafatorisrhnteghse,adsuatlnutdsdyttawhteaywsetarroee |i 1 fedPEOS. : | i4As5c4od-om1cp0ul5meetanentddeedQsuciarnilptMPiaroolntolofrcdotlhePNroot.etsotc4os5ly4s0Nt1oe0.m64a0lS0o4/n1Qg0PwI1iS0tU0hB0a4/lSlMo4Pf,ItShPUreBoiAjnSe-i4tf,eNoP.prao4rj5ae4mt-e1t0Ne4or,.s |1 This rjc the aoy rionoftha o sais i | 8. SNoAMprPcLeEsiPngwiRlbeO eqCSTfOoErRtAhGSsEAoS NDtIeI DsEaNmpTNlIesF.IGCAT,ION i| | i E`wahcihchswamipllebewisleldbefo sstirgancekdinga aunndiqiudeenstaifmipclaetioindoenfttifhiecatsiaomnplneusm.beTrhatsCsmeprle,s i! : w`iwlhlenbersetmoorvededinfaorteemxtprearcattioune-amnodniaonraelydsfirseeazser,demsacirnitbaeidneidn atthe< -m1e0thoCd,.excTehpet samples wibelkelpt iolaied frthoetemtsubstancecuring storage. |! dSwoiactmuhpmaleenutnreiedqc.euieptAlalablenlsdaomsrptsolraeamsgpelaenldoncuaamntbiyeornr.easnuSdluiccnhognsiddiaetmniptoilnfesiceadxtutirroiancntwgsiltlwhieblecstbiuetdeyirdeownintlilftibheeed | conotrcarosisenfereencred othe container. | 5. ANALYTICAL METHOD | i AOlfl sPaomtpalsessiuwmillPebreluaonraoloyczteadnaccscuolrfdoinnagteotOhreaOntahleyrticFallormoecthheomdiictaeld C"oExmtproacutnidons From Serum For Analysis UsingHPLCElectrosprayMass Specromety> GM ;i i `method numberETS-34.1 with the following modifications: f |i s1t.ocTk,hefroretiwfiilclatiboen,anondscuaoligbartateiosntasntdaanrddarudssewdililnbtehpereexptarraecdtiaonfporlolocwesd:ure. The |i SaPnrtaeolpcyaktriSecoaasllusotticaonkndasrodlcutoiroeneotfePdFfOorSpat e100rspaglc/amnLe.d pbneyrcwteenitghpuirnigtyo)u.tA1d0j.u0stmgfionafl it volume to 100 mL with methanol in a 100-mL volumetric Ask. Sore his i CenteAnya Labrsoriesn,e. Pagesof20 | Exygen Research Page 68.0198 Exyeen Study No. 023-066 Conte Protocol No. 01P023.066 s`tomckassoaupieornioidno1f265m-omnLthLsDfPrEobmtohtesd)ateionfapreefpagrteiront.aot2C to 6Cfor a i . Fortification Solutions i a. LSoOluutgi/onmLnFtoorti8fic1a0t0ioTnSLoluvtoilounme-tPtiipetitsek.1.0mBLrionfgthuep 1t0o0 vpogl/ummLestwoiclkh. ki 1 `methanol, | i b.0vf.oo1lrudgmfeicawoitnFhosmroeiltufhtacinaoonilo.intoSa8lu1o0n0m-. vpoeltumeet1ri0c0mflLaskofatndhebri1n0g pugp/m(l0 i|i . 0vf.oo0lr1utumcegaiw/iotlnhFmsooerltiuhtfaiinoconaliionfnoSo&lu1ti0on0-mPviopleutmeet1r0i.c0mfila.skof81tdhe0bi.n1gp4gp/m0L. i|i dSeattfoeirogefoapltlroefproarratatitf2iiocCant.iofno s6t<aCndfaorrd somluatxioinmsu(minpe1r2i5o-dmoLf L6DmPoEnbsottlferso)minthea ii} 1| CPraelpiabrreatsiioxnLSOtaMnSdaIrMdSs calbrstion standards in methanol via dilion of t|! 10.1 pg/mL. 4nd0.01 pg. orion solutions. i Tnheissdeid.a typical example adiional concentrations may be prepared as i|! a Conoer. Gg) Volum5e (a) DeTdooa) FilCo0n0e05 Gg) 01 2 100 oo |{| 00011 ool 5i 2 11000 10 00000015 00002 !!i 001 1 1% 0001 ! dSeatfotirgoerfatlplorrceaalaritabriaotCni.ontos6a<nCdfror somltaoxnismuimn p1e2ri5o-dmoLfL6DmPoEntbhotfsr)ominthe ||{ 1ii 3. Ta0hm2oe5usnaMtmopsflo0ed.iv5uomMluTcmaBebAfoonrastdchdheeorddteidutbhmleosbioacdmacpreblloenlwasitleslabmbupflf0ee.rs5wmaidlLdleabdnewdit1lh0e0baemuLo1.u0ntTmhLoe.f i . { hesample will nbey ilred with 02 um nylon sh fiif ceesarr. i 4. The sampleswilbe analyzed undertefollowing conditions: Contre Antic Lorre, Inc. Pusesor | Exygen Research Page 69 of 98 Exygen Study No.: 023-066 Cons Prot No. 01P025066 LCMSIMS SystemandOperating Conditions Furbolonspray) ii Mass Spc: PE SCIEX AP13000 BiomolecularMass Analyse ; ntetace: HaSrCvIaErXdTiunfbuosiloonnuSppryLiquid Invoduction Itecsce ; i;!| Computer: DellUltraScan P1110 Sofa: PWiEnSdcoewxsANmTlyt 11 !ii i |! HPLC: `HewlettHHPPPacVQkuaaarctdo(PuHumPmpD).eSegraiseesr1100 KP Autoamplr HPCalum Oven i |! HTCnoPjlLsuCimonCnoTVleoomm:p1G03Ke5LnC eCysGoiness Chromatography) 2.1mm 50mm, i Nobile Phas MFolboiwlReaPih:ase (1! (B0):3 3M Ammonium mMeitnhiann.ol Ace n ASTM tyIwpateer i: i ;| Tn wimeoo o%@A w%iwBm } |! Hio sowd i | iiImnmasxye3bt0e npoeemcre)tsosraamrnaydnetoso.laadmCjnusos.tttfahoesm.HvPidlL,Cfcgreaditmenat dninuosrrdeeorsto((oppi3omni1zee f OBhetiansieldC.ys etc.) can be used, provided equivalent chromatography is i} i Tons sonia Approximate | BOS Analyte nMeogdieve 4959 TransitionMonitored Pr RetentionTime(min) 1 hOne ba tdahy-otfom-odbaiylbeaspish,atshee retention times may vary slightly depending on ! CenteAyia Laorts, Exygen Research Pera Page 100198 Exygen Study No. 023-066 CenteProtocol No. 01P023066. } "EiTxhnaemfspollteoTwrtuinonugienFmvsatllreueuemnPseanattrr.aepmArelotsveoir,dstehdessesvsanlesxamaplyeb.eAcchtaunaglevdaflruoems mamye v0arymferoimn + onder oplimize for gestes easiviy. } O"Tnhciestthneiinlseiuimtehnetnssteadndd,inthgeoropuitminiezaendaplayrsaism.etTerhsatnisnavgpedraoc"uendmeafuylrb"e, repeated asnecessary oensure optimalsensiiviy: }i: || TuneFileParameters } i i DP-DecClSuo-slntorosiplnrgsayPoteatal 42S0et00 "510 i 1i ECFPPE-EFCoonclultsiisenognPPoEottneeennrttiigaayll 21E30000 i CXP-Collision Cel Exit Font 5 ! { DF-Deflecor 3000 i i `CEM-Channel Electron Multiplier 28000 ' NGebausliFzleorwGsas sa1t | CCoulrltiasionnGGaass 14 TIS Temperature ssc | { Calibraation PrIoncjeecdtutrheessamevolume (between 1010 20 uL) of ach calibration standard(preparedinMeOH)inothe LCIMSAS. i b. sUutssaienndglaitrnhdeeac,aupxrpvreowsperiiagarhetetgesedonsfettrawantrdeeadrsdyfoscrtueremva.ecshfAosnretyqubcaaynltiilbfirinacetaaitroinornse.igarLneidsnaseriaorsn }!{ fbaelleixncglouudtesdidfero+m3t0he%,cabliabsreadtioonncuusrvcea,lcHuolwateevderco,nctehenttraatlioun,mbmaeyr ofclibradonstandardsthatmaybeexcludedmstnotexceed 20% i `of the total numofsbtanedarrds injected. ! |ii TmThuisettsb,ceohn2ee0nl.a9ai9po2rn5opc(r2o0an.tf9ec8ei5n)ct.pI(fs)chufloard clbaelilibrranebtsuilot0nrs cfvaaulrtvteosutmisgiedenoetchrennesde i operation,andtherelevantseofsamplesmustbe reanalyzed. } ContesAnyaLaboratories I. Exygen Research Psion i Page 710f98 `Exygen Study No.: 023-066 CenteProtocol No. 01P023065 oSIfnajmsecpcthlethseAanmsapallmeye,sevfoorltiufmiecuatsioend, fcoornttohl,ceacl.ibirtaotiotnhesLtaCn/dMarSd/sMbSe.wEeaecnhs1u01m0.p20luusLe)t ! bearded in duplicate i . nt nce of sts 5) ogi of tm em nd t! a iSntcalnuddaerddisnacnorarneaslpytoincdailngset.to at least six concentrations must be ? iinnjjecctiosntsanmdardsubeinbtrsearcskpetetrseeddbyabstoaundeavredrynj5ct1o0nss.amples All unple | . Bocoanncethrosrlee,atgoeafntndscamoptnlwreols am(neaaxlttyrizacetdico(onnnottsroo0llevexncstaesmepodln2ey5s)),mfaosrttilfeiaiesndtclouandee akmtnaftoerwisnxt | i E"a`Tcycophnecec[ntiHamOiuosnbtsaanalkno.dicnacmluideedattlheoaustgohntchmeeptrhoacneodlurbela0nkvsenrdyonreecAovSeTryM. ii 4 Tnthelermycioninecndeafnlrtosamtiaonnhdaerodsfstaicnnadjcachrtdesdcaudmrupvrleien,bgafasoecrtdti.ofincTatthiheons,pteacnaodknaatrodelr,seostpcfo.ntsheiess i} mnheuesssetusnabrdryaa,crkdiectlurruevstporhnasnsegse aof tmahendprerse.iladnuaeleyfzoeusnd0 ignitvhaee rseasmppolnesesewti.thiInf . Forificaion recovers within 80 to 120% are sccpuble for ii afLno0rdQti.fficlFaltaiirolenusarnetaatloymtshieesoefLhOthQesaef(f1re0tctenedgdi/amsLarm)pelaegns.duatanlevveelsgsreiatgeraothftacnoavtnhee : | . Sumple in yh eke ae dete the competing se b i1 w`rbieWulthtleincabthreiepornleeeastspismtoeahsrarenawtsdtiheleNtleQdcbrteee(sdorptesoqptonutrshatoeeenfc.dtotamihselesNelp.oDowned(sintontsgtdaaenntdaealcrytdetde)(.T0t.e0Sn0ai1moppnliegeisnsLi)n ;i i |i & cBusaoectdke1gsrpoocunondmdeotlevvfaeollrusteisocbaftliaoonnwalryhetceeovLfeOroiGuen,sd.biun rceonstirlllbqluaanntkifsiaamblpelewsillthbaot i {i Hh. 12afsrCa1me0pxtl6reasCcaterud,nnlsoatamlnpollaeydsiesdmounnsdtthabenieanlssyttzorerudemdperneetffteiorbgseeltyawneiadtlhyazitendstpwphereeodkxa.imyattheelyy i CenteAnaya aborts, Exygen Research Pugs9or Page 720198 Exygen Study No 023-06 Cee ProtocolNo.01P023.066 10. EXPERIMENTAL DESIGN || ASexnupsnelpcyliieecsdalionbLttahabeionsretdtoybreyss,WiIlhcda.itffweoouIalnnedamlayastiosf.natflhTehLreiredes.cuaswrioelflnobieskSnstohuwiypn.pecdontaomCiennatnrse ; i: COnelnytrthsocsceonstaimnpgletso dmeestihgonda,te"dExbtyratchteiSonpoOnfsoProtwialslsibuemePxterfalcutoedroaancdaanncaeluyozneadtast |} i Or Other Fluorochemical Compounds From Serum For Analysis Using HPLC- F ii moEdliefcitrcoastpiroanys/lMasssd SnpeScetcrtoimoetnr,y" (3M method number ETS-84.1) with the : | Mfi oertihfoidcsaiotno oocfounntstoelstbeindsscornwtirlolol isnacmlopulvdeesisstsosoambytaoifnBcuon,vraetreydodfactoaB,ntaorldoseamptplee:es, | ii tFhtheoerLtcOeasQitioteonfarbewinolcvleebmtshauebdshtiegahnectsethrweeislimduabeetfsaopuppnldri.eoTdtsho(e0cfotxrhttrifcidiceaostinigsonnavtseoedlultSiroaannmcgoipnntgaivnfiiaongm. i! !i s`cHcaulatcoyn. singe, mieroppet pipet,co ages, 1 mao Comorrency }i b"eeThnecatalvceumrlaaatgyeedb.reecIeFoxnvceelcreuysdaseadnryfr.reolamatitpvheaspstsatanaldnsadraydsrddviatsmstibooinr.oofuttAlhileesrs,o. rt1ihefaeandvoesraugmeprlreeesxswicitlo,l found and standard deviationfosch mwia llbecus le. i "TEhqeuatfoilolnow1:ing equations wil be sedforthe aula. i| Assy found (n=(Pp akaran .int) eret) ; {i sore i 1 `Equation 2: 7 Analyte foundL(aung/am.l()fAo=VunmdL()og/smaLm)pFleVvo(lm. L()aX)DEXEV(mi)x1L0u0gg i |i FWVherF:inal Volume DF =Dilution Factor || EAVV==ExAtlriaqcutoitoVnoVloulmueme FEoqruastaimopnl'estofocrfaicdlwictthheupkenlrocweinntarmeocuonvtesryofPFOSpriorto extraction, use. Conte Asti Laboratories, Te. Exygen Research Page 100129 i Page 73 of98 Exygen Study No: 023-066 Cente Protocol No. 01P023065 Equaion 3: i! . Recovery (%)= (anal. ound (g/-mLvg). anal. inculGug/mL) x (1000 ng ygx) 100 : `amountadded(nginL) IL PROTOCOL AMENDMENTSANDDEVIATIONS f :| RAbeengyededoseccvnuitmasetiinvotene.sdfPralonamdnntehredepcporrohtcoadconplrtgooormefphrtsioslmyptrhtooteoctaohnlealoySrttticuoadltymheeDtainhraeolcdyttaoisrcalaprnmodevtihSdopedodnwwsiiollrll E | tbdheeevimaSattdiueodnsyiwniDwlilriebncetgoar,3spaanndpamtoheeetndiSmnspeopnnrtdsoaotnroecdoRaleppdaprnerdsoevnnetdatbcivyet.hnhthPArenidynf.ciinpaaealmleInpnddovmeres.natgsaoro,f i| 1. Pdtrhooectcuohmcieonnlgtaeem,daennbdydmiaemmnpetanscd:tmoePnnltatshnenstethduadcylh.aarnAglmeyesndd1e0mscetinhbteestshwpepcrhiobaveensldgiegp,nlrjoeutdsoatcniofdlicdasthiiatolenl obbrey | |: otfheaPmreinncdimpealntIsnvweislltgbaeors,eSttudtyhDeirqeuacltiotry,saunrdaSnpconesnoirR.epresentative. Copies ; 2. Ptdrehovetioantsaitsounrdseefoovfmothtnehe:dperPvoritoaottcoiocolno,,lshdpaeolvtlieanbtteiidoanlosc,cufwfmhcietcnhotraeiridenmnpthaeectttioomnye tarhenecdorsudtnsup,dlyn,ainannnegdd f PcrreoivmnieceitwpieavldebaIycntQvieAosnUi,gifuorerq,uirSetdu.dyProDtiroeccotlord,eviaantdionSspaornessoirgnReedpraensdendtaatteivdeb.yatnhde i 1. RREeCOsRDtSo be sind coe, bk um vo nied Ou flows 8 | spp21uoSSpaarmmippntlleee)t:raecckeiipntgreschoeredtss,)storage history, and choifcnustsody } 345...HDIinsesttsorrucymreanintdpropufirnaeopsnhanyereamttsi,oobneodnfscthiasnhdfeaertctdosstaoh(resomlooegknts,hfsoodrtification, calibration) 1: i1 7. AAlnlalcyhtriocmalatdoagtraabplheisc:and instrumental conditions 8 Sample extraction andanalysisdes i ! 11091..ACcnhoryomnptolhloeegitdcaislapnireecsoeesnfnstsaatrtguyidofynorpoftearhlseoenscetoulnd,syiscirogunmtaeitsuoprnoeosnfdstennhdcsietuidly i Al chromatogramswilconthetfolliowinng: } CentreAnaya Labor,nc. Page 1129 i Exygen Research Page 74.0198 Exygen Study No.: 023-066 Con Prot No. 017023066 ) . SiAundmedp,innedn,ijcaoaioincns,suomdnbatsee,rwciaohmoemsipodroentnegtre itfnhoderiircfanctiaotnioonflheveel aofetoef Annayya sanded chromsogums wil addidonly ncude te | i | EPaxahmeu`tcinon,cgentcrawtiinolnsct(no.gn.n,enjn1gp/fmlu,rnemg/som,Ln,papodbn,pep,memtce.p)t. eprsooer, coun ||i | I. QUALITYASSURANCE |i; dCaoecnunmeaQtAsanirUomnndteG.nwiclCaldovinnitgeGwToAwthUeGniptsrowstilnold)n,mpuledtetahoosr)dd1yy ecrominerdnleatnaotde isOlLfyoY i! sPrinscipacloInmvpesoitgaetoar, CGeLntEroeyMa1ndagweimlentp, randhthee SntduidnyDgisreocftohre. ses te |} || 14. DAANDTREPOART | co emer dover st pt tee 1. fIAialboarTtwoirsdyaecbusoanodkitshe,nrncilyghiecsligrnaenoddpoarroas!moemwiniodlnmbepene,mpinersaosioonncdsiundmotvhpeinhsioayn; | nohfcdtCnoyoudayhyrhephtsEo,rpmo,elosec dwuorekcshui e.swiloRlomwdeodo vcgsusao ,sdcrwaihtonScmutes ||i | 2.TeAnrpdeeprhorectonSwtpeonntibsseosirlhsoRsuuledecbuyrdCe,nutre,nsopptrliovieecdedann1d0fsoigmneedbsytohenStsyBEDiArecTthoer | | 21OAbjnecstiyvsesaannddpbrociedcuresmestahtoeddsinwtdheprotocol | 3. Snes Reference materials identified by name, lot, purity, andother 54.. SNatmeeeofpnecefporemiengalnadbogratnorybayndhanqaolsyticalostarrt annd twernmination dates iii Tits coring a spndus i| 7EA. Aclol cmptre HogmofsCo5esmegnadrnyapgelrcsioonicns | mSReppokrnessovernitRasetpiorvnees,ewnnhtdaotfiviel.ieTuhhe CooeenrtrsewGpirAthwuhniekscopipolrmvcaoeln,dauchCtoeannSsseeoAditnDoyfiiofonuid dt report andr dtspackagetosrs acura and GLPcompre, Tot | CentreAnalytical Laboratories, Inc. Page 12029 t Exygen Research Page 50198 Exygen Study No. 023-066 Conte Procol No01P 023.066 } 0rceopmopsrltiigmsannscete.wbe abiApepirslnotcvleeumldebenydttnhteofhStQuidnAaylUDiEripencostpnoercniodnsSpaondso4r Rsetpareemsecnattaiovfe pOeLoDr Any corrections or addins to the final report shal be in the form of an ; i i aIhcovemneeescpintagidroamnt.oref,bnSyttt"huTethdheyfeiDniPaarrmlieencrncteidoppmroareltanIntndtvheSstsphtoaiInlglsaotbboreerR.iesnpigTrgehcnseoeenmadtematetnenidvddem.deaannttdesdthhbaelylJcolehaserltPyieindnecnitpiffosyr !& | i; REPOOrRigTinaDlI:STSRuIBdUTDIiOrNe:c Copy Sponsor Representative | Copy: Contre Arches | 15. ARCHIVE STATEMENT i CSahtwruodmydaarttaeo,cgorroadbmssse,trovsabtpeieocmniasmienrtneacitonsredcdek:dinRdgeucrioinrnfdgosrmhtaoetiboceno,nmdanuicdnttasoitfnuedtdyfheorrstehded,sctdoaomdcyeasipmnoecnnldutdeienocanel,l i c"Thhaisraicniciluzdaeison& ddeastcrainptdiaonnyofsheiqpupiinpgmreenctorvdisedsduhrbieanrtelhtislnon.doct of th suds. AT |i| Ddobaoemcceucunmrdmemeinenentttdahsr,aicshvaianevdesesx:hIaeUcFtpTociosanpelyc.cormeepCsploaaerttnyieoatnnowdsoifulabtmrsheeeitnatdsietnmuefdcny,tosytyhsefhoesatlluadenbydogreoecnonagrdoesa,dlrsperca1oontrod,hcoel waSinlMdl py : | ofthe finalreportandraw data package. i | 16. REFERENCES f 1 GU.oS.odELvaiborroantomreynPtracPtriocteecSttiaonndaArgdesn.cyF.inaTloR xic Su4u0bsCtFanR, cePssCon1t9r2ol Act (TSCA). :i { Cone osc Loto, oc Exygen Research i Pe 1320 i Page 76.0195 Exygen Study No. 023-066 ConePres No.O1P023.06 17. PROTOCOL APPROVAL | QuayAssurance Reviewer, Contre i ! TLhias bprootorcolTo was audited by the Quality Assurance Unit of Centre Analytical .:| foraRe | `Principal Investigator, Centre lef le | } Ea Faclty Managemen, Centre | CHhuhaonoMtalgeir] i StudyDirector, WildlifeInternationalLid. Aes/ 2 nude Enis ii Sponsor3M, |} To -- IAL Efironmental Tethnologist [eR ---- Exyaen Research 7TH we ; BaPotty | dale i|i i Pdr b Page 77 or Exygen Study No.: 023-066 Centr ProtocolNo O1P423.065 i APPAE.NDCBoIamXp:couoAnNndAsoLfFPYroTotmIsCSsAieLurmMPoEerTcAfHnuaOolDyrsoiostUasinnegsHulPfLnCoaErtOltehcetrrFloosrpoMcrahaesymsical Spectrometry" i + | i || i i Cente Ansyicl Labrie, oc. Exygen Research ! i| Page 150129 i Page 780198 ExStyudygNo:e023.n066 Cons PrNo,OoPTtI [ i : Do ---- i ! 2 SMEvROwmALLBowtory f , Fr mm i i "= EPLmURCoHEnMICoArLm PCOoMFsOsUNo DSrFaROmMoSb ERRoUcMoFmCOi aTRAnINBALSYSTSIUs0St%OvOoNrTprEcA. | weil 2gAio Mert3on ! [ESivT Asn Ip Oo oriDAK o8 dSpss - Nor || SLoabe J >SDes ;|| adalslses Tsii fdic& is };} 2 ScsB oersmare vcinon aes - Wride2, f {| . 1152 fArvploatti-- cmponnd:F -- e okeeb eoteeOe ottiotcpr optai i J Sars Lm cl roa ! Conte Asli Lorie Exygen Research Paget6or i Page 79018 Exygen Study No: 023-066 Con rooNo.012025066 | Ts e OUTa R E C E eR e r Mei iB n EE : - . | DCEE : oe ; |y ra5 ay Tr imethoddesis he eee procedure fo extractingpotassium perflucrooctaneslfonate. i | = Ea &n emTmT i ET tt~ ||! fr2a Fri FrEOvo:p beronceehriwStaropo a Cn F507 ~ ;|/ O EI 35 sS -- ects-- e --mn atilnogcscoyurmtroly 5376 MSispetOF,nSOtNGN1CH.CO20R)p|t/e, bee c | | f4=8 ViSncemameina TES 413 emit plyMos : viin || i ST Sr 5S1o Trheomseem ner mor &iSl)R i| 1 hllowingeqiemtpmen ie ein met.Ee i ii ! OD a611133 VCsorutexoeihevnieYoVnR,tvoVonwre6Gee? .. ; } EEm.r.. tun ConteAnyi Laertorics, nc. Lens | Exygen Research Page 800198 `Exygen Study No.: 023-066 . Ce ComPomaNetponNs | 2 we Se SE "or elie `i tog SRT EE ; | DLE5 BNaimmaecapriran,Open : :! pms : i Damimsomdns 0c C t ; ~ 137 Bpp etri |i| 73 73 i YSloiucembaotlsg,m paocaofbpiasn250ml.sd 11. Lds ; ; 1 . 76 Comni Dptpipbrpiaonseal 77 Libel : ! |i i[s ne otentbie gyeeet 0n b ooyd.san. i|[ i ; 7T0AI2 135 STyitaogpss,hep, oosnet" 302X aa m Ot meomissnten ZF ) an SA Note:PrM iortoQuPsl ingtgelra,sRswiareeyanrdibnoeusle,iriise 3ieofswitehse fhhmeta shnadnn e3,ti3a maeswsl ithory i| e Sna y y o |i 1 2 3534 Sofiabydroeide STaetnebsyslemnon (NaOF),1T Bakeorcquivalet Gytroge0 n DISlIrCTR7 A),Kionkor ee xslt 1 pi f ii 8856 SMafeiyncbBuoyaBtieer(,OVmAiHgCBsaOke)lre,dciTmi.LcCtgi Py i i 187 Somat tomar Methanol, Omisoly,glassdisiled orHPLCgrade -eT |i i CD) ) 29 F1la9o2rocFhoeSmtiAcaolGsMtaSndaalrdtsyGCheke Divi beige : msec weigh 59 kt snBg- rTer | . -- ener URRY Cente yi Labortoris, ---- i Exygen Research Page 81 of 98 Exygen Study No.: 023-066 . Ce comPmoeorasos | wi ER ERSO ER i i D 93 OSAOMpelyCorio Divi),mcs wig 15 | 357x,)1519496.5TEuISFpOESoENOmHGGaMnpdeCcyalCeyCtthiteneDeivinssimotnoavscaeilcswei5g1ht 570 i i| { NL > 0407 S 336OM Specialty p cCheum i iisn1 #4 GFSOH)molarweight =428 Re | |i "0CH0OpTS!EpEepo ra eositpti t gn c,set, ere po Ryi Ie |f ! LRESERnR |! RIeNERT mNenee a e deso ; EE 103 05 Mtetrabat sulfie(TBA): Weigh sppronizmatel1y rea) 9 f [raS tviuA ce ihT sea sSEEEl Nr |il 4 n F p 2 i E e re Py-- . | 51 SeS11eeF entrrtaaeesea bsteen.h eri ME ooi | ED solutioncontaining1.00ps FOS, 02pp ' 2) PFOSA,01987pregPEOSARYsnd. | i TT 113 Weigh ppronimately 100mg of PFOS ato 8 00mL volemetreOak od rad. sy omEEN 114 Bing van i ctrli ck sda pinay1000p i ii 1i 9 fe `8.115Dilte thestocksolutionwithmethanolforawockingstandard 1soluton'of rh 116Ditwringsic vithmenoswin at 2 ont ii Po L ti oea mss ; I = Rew HES SHE oo [SR -- Pas potzs | Exygen Research Page 82of 98 Exygen Study No.: 023-066 Cone ors. i Sn agi TEs Lge Lt 8 i: 0 11.7Dsipow0or5k0ipnp.ded 1 wi boofraworkssisi elton i {0 Sneinaanme ! 812.1 Weigh proximately 50-60mgofs standard 15,18,2:4,28 i ; Comm mementos eesr op ecRot Et at trp Bo et fT a ry i| 2 a Nene menrn i 0. immpetu i 10.1 SolventBlanks,Methodplas20dmatrixblak 11001121EAnxsiqeuott ofe1.l0mls. mseifBootiFsUdPssvsioslvles oieg.dsposts i :i: [p 10.4--Ema xat cttgwo 1.0t amaqua of estnrSi7n inprmoadcsieerss.i i| i00229`bp maiereceivee e dwitheachsamo ple eset. r os&tY yJnaer ; i| | . Nsoiti syle may wrepn i i 103 Co1p0n2t4oPpT ersepisscaeo mnaisdsE piskieodmbitasitk repicis pe 0eSneehSande,uir ii 1098Fp te act pi1 ; | 1 0 1099 Fhmn nkeo p-- cxmpl, i amplest= 34, fou checksseppdsed exc. we mesopert } yim speEe rss : RI pe Aa `Centre AnalyticalLaboratories,Inc. Page20029 : ! Exygen Research Page 83of98 Exygen Study No.: 023-066 [A VC meme ; i Mie Ee EE a i 1000Thecptonions i vi te pe i, ; Fa Ee iceTE ey ae rat p=ray i | Rime. | %NomFo, SSpem,. + He "Pirate aLstse1ssactpots ~ |{! Ta0s0.E fgectE inmS iweenT a0lcrI stocttwist yi ; i 11112443Ti w.l foee pteia o ssen cvef smee, S,sy ces | i ! HLGS eRrnri simlne,Ta EFh54b0, FodTe.se5e0b.3,ewicr h tsewosing i 2 HLL Uf seArrseDah1r 0dnm cioteiang e heice h omit ohmv wisng `calibrationstandards. A ! 112 TRSR To cachstandad, lank,orcontissing addSpgroptiste amooufsnuto |{ 13 Beetbtexhmtt etes8tom 15.0 etd eit i i {y ! [@} ; : Hy i . : Na senha Ex Cn AnalyticalLabrsoislo. Exygen Research NR:en i Hg ! Pge2tol i Page 84.0798 Exygen Study No.: 023-066 ---- EE -- CenireProNto.o01Pc-0o 230l66 or ae | | Spd aE CR Ce ] ha A" Apres ptesamsmodstdpe i!I ]i oI o[Com--|-- NEEa S EeLB| iene] . | oe -- | i i [Comp LL me [Sooper 070m | r i i Cope a0| top | 121 Obtainfiz npn2dall fo haw fostempest in akev, 0 LEE T osm1 i m stbmne 05 gepit 5 ; 123 Rur nes mic ples fee sh coeTAaYmore. i||| 123 o ible t victhabessh ityenroe,e sale 0, ia Ses 126. Splemrieespconte ot ct,sty coEf er i| nr 128 ca onmgmac itpsc tofnnde ssSeba Vocmi iesatcrsremic eseod a 1. ra cgi | mr HE, i ; Le 112290CThokhsmpelt1ed0151M0TB3AMrTEsAtt2mHL100.2o5Mtfdntsccnoigny?n. ie f mt | 1 TE2Z0CUosp OenloDeipms, e5emtotrno0ses.r 0 tn. . i 0 1243CCoriinpor20102ivetiof 50070 ml nl i i pee ir ContreAnalytics Labor I. i fey f Exygen Research Page 85of 98 Exygen Study No. 023-06 Cont ProcolNo.OIPOZ3066 | GEA A TE es REL : | ) 1h Lk 15 contevin ee ion sn 15. 1215 Revove 40aofthe ric artotiscle 1 lcci. i : 6Dh sa sgoe pie EE, .I | 112L 01V800i802n sritns. cr t rem od i Be mie. . |J | 1220 1122230 Tel} OCnomtpee pc pei tere wihthestedysurmber,animalnumberaodgeoder,simple choe diosdthe i |i i [TRtVleEXrNi rer = 11 Caan 3 i} S oE S DI rs, de cts o . !, o J Ler | Ee STLey [EFA i ovr { 141 Themethoddetection init(MDL)isanalytesodmikix specific. RetfoMeDrL | 142 The21ebMioenl avlsyil cwodstmipcka .msemia ticcSLkNofS orice b 11442233MoT isgt_ yeel aT tes it oicrtstlemibdemreA= Sin Treen. ii 143Reetein 615frm8odp.re3cc1ei NBN ! |} oN) [ IS SSRtoTRneDwEetietste dnktanpcom wae pledvetvpe Gcrde : so Fo r-- i Contre AssitLaborsre, P22 | Exygen Research Page 86.019 Exygen Study Nos 023.066 Cone PNe,e 012025086 | Bond Lad ea Bi ee cin ae AR ie ; &I Ey 161 cxtracionworksheet tachedto hismethod,10d peinth i: .| a 1T7H5T" AA LEAr CBot itots perosteyertn } -- | 5 py | Bp im a 2 - 12 FACTMA,licenoeOe idBsfr ares ing i ! : 04 E BeRIotoREeB INee Pewo Q F BE p ae md- i havi i EReT e ttm Section 12.13Added pris the shakes speed #5 77 T || 4oO i| |i| 9 : J ,i ye -* i : i otamTeu m IPassa FE Pusher Exygen Research Page 87of 98 Exygen Study No. 023066 . Cent PrNoo.c012o023l066 EEE | J| a dicAhi a SreE ; JE =r TE | Em : STeEEEEE i| E e aa t rt t r }i nt 1 ------ :i tr || a f tt t t i| ee a e t ht e t t r ; O f e r er e t f i i! rt e Ee e |!| peerp EE-- ! _------ = = ea iii Ew ee -- | i:i fmm | ee || E -_-- E = ! i LAlnite Gr ae F me sei 5 rai i CentreAnalytical Laboratories,Ine. Page 25029 ! Exygen Research Page 88.0195 Exygen Study No.: 023-066 Cents ProNotOIePO2s30t6 i| SsEeErRie LEe E cEan EERE HE oo rer| ; i OQ 01100reo this : | i i Fh o=m ArprmaCtaebe raen Ca are geperr i ae t | | [SSE 57L] E s 5T5a2[[ Spbs 000geins]| re eS reamSiC endnother | meee Pests oye i \ a | 0 SF A ~pYEN 0; | i . {> b : LL pu i | YE i t , J ---- ma CentreAnalytical Laboratories, Inc. Exygen Research frre An ` Page26029 i Page 89.098 gen Sad No: 02366 CenteProNto.o O1Pc-02o3-0l66 SEE ETE ;| i GH ade hein abe TERE de HET LEE 1 Si T OJ Fchcaoimns TxE z i i | Rabbi Sen Range i | [[0[gAoaEn[ | orromn o reonrnee| ||orn | |m| e|r|| i [o|rr e |oom|m os| |; | sCompens: snr|oEs e TE ! [Fim{mr coo om | :! o EeToLoe | EEE Compra, 5 ff[oFreemremee|or [rwoesnne ||w|ea Twnaedn]e)i) ;! : ; ! ge . } J: emg ee } ee BEE ne ; CentreAnalyticalLaboratories,Inc. Page27af29 | Exygen Research Page90of 98 Exygen Study No.: 023-066 companions : oo | FEE | Prepared ings Keo Bo lasmor| | [[es=tei iareeT| roen |aonmTiwn]] : | pe---- oe[TE = i EEE O [[m[ Bem[oeroo nTTvowvnelo[gm ggiowvooa]rn] | P------ XnDer EEE | Ee Te re Fah) : [oom[no me[oreoi mna| wi T|e omwing : } To Ton oefon] 42 a, i 1 oO . ] IBAA or Ic "men | ---- nes Exygen Research Page 91 of 98 Exygen Study No. 023.066 Cente Pros No.OP023.068 | FAS aE rh a ERAS FER Ep | 0 . TonPie Standird Curves Fis ed i " Soadartmabe k i Saoepleemas| 0 Pe err ini I i T agEmes BCmbttdapp0r.500opp.m: re . 1 ce es andards 1 34FCmis i !| [oCsee rsotoor sto araa rTearr Teomee ] aor] | : F EE ear par rara taer e e a e } O B teEr rare bage m re e Colt concentofrsaadtarisosnsvi | i F [E oeae r 0 re e e ee2 Ty i! BEE Fess aw ! alltrong prt costo - > i i| fe fm e ms es s Ss 2D ao : } Atm artsOT BinrTsiami 5: repe i . aT HE? whiz pi i CentreAnalytical Laboratories, Inc. Page 29029 | Exygon Research Page 92098 Exygen Study No: 023-066 CAN Centre Analytical i 548ReacehDrive,SseCollg LPAaTOL.borPahot(o1r0i2ec3isn,1eG410I331n1,c25. y| PROTOCOL AMENDMENT Page tor] i || EAfmfeecntdivmeeDnatteN:um0b6e2r:70|1 Cone Sty Number: 022.066 Conve Protocol Number: QLP-023066 "DESCOFRAMIENPDETD SIECOTINON 1.87: JustificationforthSelectoifothne Test System i i AMENDEDTO i Chatnhegfiet sentteonrceaed: i TMoatlelramratdiaonnadl,quLadl. rweidlbbleouosdecdlsls atnhed asnearlyutmicsaalmspalmepslcelslocrtteidsbyphWaisel.ife RATIONALE : 1. Attherequestofthesponsor,lserum samplesaetobeanalyzedwiththisstudy. ||| IMPONTAHECSTUTDY. 1. Nonegaive impaonctth sty: | Ai/t - 920 Anloy | StodyDirector Signature Dae i| . gq So= m naive Signature Date L/L /a-- | | } Centre QAUReview_Lbi_1/jr T2501 Exygen Research Page 93.0198 Exygen Study No 023066 . Xysen.. oR, i PROTrOoCaOaLmAeMEhNaDnMENT rr ||| | . ExygenSuy Naber, 023088 Effective Date: 03724703 Pret umber F-23061 !i 2. SponsorRepresentative i ~ AMENDEDTO || 1.SonrmRseryeaode, Enc, i57oe133, || i 1. Titleshouldread"ExtraofcPottaissoiunm Perfluorooctanesulfonate from Red Blood Cells i P-------- \ | FACTORS: | | 1-2. Nonegative impoansctudty. A i [ld0 a Teck, i VE lao =oe | der ! | f Jud swall" \ | w5/a15/0h 3 i | ee we ExyQAgReevinew | LTS 04] 11[a3 Exygen Research Xz nnoy | Page 04 98 Exygen Study No: 023.066 CAN Centre Analytical 208Rear.Dei,SeCollePALTOaL.borPhat810o)23r18i05 eFrsc.s019I3n11c2.5 |; PROTDeOviCnOioLaNuDmEbVeIrA1TION |{ ) : DateofOccurence: (12) 057263)0057124,01 ; | Cone Sty Number: 023.066 ConeProtocol amber: OIP023.066 ! i "DESCROIFPDETVIIATOIONN 1. e$ct9iAonwhnenateMlectonhycoedn,ttSaaimoipnlsecAwenresagyeslst4e: QauannthifioedCheentiegshaemspslaen0d1072n61aSn0d5s22d0u1pAliDc,ate | | 2C.e$n9Asampule 01Ms0e7t57h8oySdpScuAipseAcSey5t2:2015.ceedrecoveryof 16J5ogr@e n dut iotriono i |i 2S.ned1c.ocszi9anuA npcio:ctenjMeectthia oond,wShuemy pheAncoa snysesn:iionQsuawnteirfierdCeeeshsaanmpthlefs0h1e070i9g2hada01r071d34 i|i ios frhSOeF d sion... 15. Protocoldevinsed. : Recors Byte: --_-- i EAT NTE STUDY |} 13. Nonsguin impact because eas wee < 5% ese hanteihe snd. ! 2 None impactbecausete avertaverseof fhe oiicaonsweewit th i|i sepa ane EovfoigEhor Sgt || SidDiren n Sibglna ole Buedolex ! Spc Maunv.age sigs -- Te 5/570" 3 7 CALQAUReview___ lei, Gfdle Fn } `thigsdaedlaoGnrd1o6bbGeirggrei. due to suspedd [s ofotlhe i Exygen Research Page 95 0198 Exygen Study No. 023-066 CA Centre Analytical 300Rar Dre,Se Cle PLATSa. borPhaet10o2r30i8 eFsue.010I2n1.c13.59 i PROTDOevCiOiLonDNuEmVbeIrA2TION ii i Centre Study Number: 023-066. CentreProtocol Number: 01P-023-066 i : DESIONCOFRDEVIIATPION |i 112.001$070983AsiweareM0e.0t5oh.0S.l0ail0e.0l25uOnl dnd 0f.r3C5aonLeseasmppleecsie10TH, 107G, 10708, | -- esetACTIONSST0AK8EN nc. ||! Recorded By/Date: -- -- amt. t TEAC ONESTUY i 1. Nonegaive impactbecassthesclvous was ued inth celts. i| [APaddenefiDgs Sgneaerel Daselp |: } 5DAireyc S2i. rebdo. -- Bielol ii| of sn Si De _S/ales { CALQAURepevc,i4eldwlo_ n __ ! Febouary 12.1998 i{ `tphiscsdeoxkt@1tf5inboenfitnlye-i duet"o Asuspected (oss of NR i 04@ ofl ' | Exygen Research Page 96of 98 Exygen Study No. 023-066 CAN Centre Analytical 906 Res eDee,Sue Clee PLATaS.borPhat31o02r10i0 eFasi,l (01I03n1-c43.5 | i PRODTevOiCaiOoLnNuDmEbeVr:IA3TION i i i : `Date of Occurrence: (1) 723/01 t | Centre Study Number: 023-066 Ceatre Protocol Number: 01P-023-066 i ESON OR F DEVIF ATION | 1. 9Analytica Method,3. aSndpl010v7o2l0u9wneersese0d05fmorLC.eesaples 010713,0107167,0IOTIG, i EE A-- | } Recoeawyomes } EAONTGE ST TUY 1. Nonegaive impact bectheastsl von was ued the cleans |i |VE qcche)figRor SmDaerfrey SBees ii 1 SaNyDoriee SQg.nNaeab, aeSlrle3 i| Sponge M/oma: Sinan Be botox | i| CALQAUluRcee AlvleFi o ew i Exygen Research i Page 970798 Exygen Study No. 023-066 RR | |J \ PROToOmCOsLnDEmVbIrA,TI4ON Fa i!} One Goce, TET |i| EvenShy Number, 021086 ProcolNmber. 01273086 i scion. Samplerats. ALN ever of FEALTeal126 Se 7. | i || otsot cannon"SACTAIONSTAKEN inae. |t: | | onieRneacctstoonsotiurdyfbeecaul[e Smfaeg rsTeoeccnensiin he owe |Helo etwrewith cpa | are \ i | : ------ |H mttbTh R itsDecks 3 oi ols ii vAiral bh, owSle o3 i| aLnl)a Shpnee JOT | S/LELR 1 Exy0AgReevinew LTS ga lulus. i Exygen Research ROE Bor, usa \E:sonB2p1o2n,v0 | Page 95.0195