Document gbbR540LvJvwE8mN7qOyaaz43

STUDY TITLE Extraction of Potassium Analysis Perfluorooctanesulfonaie from Red Blood Cells Using HPLC-Electrospray/Mass Spectrometry and Serum for DATA REQUIREMENTS Analytical Method Requirements STUDY DIRECTOR Sean Gallagher ANALYTICAL REPORT DATE June 2, 2003 PERFORMING LABORATORY / TESTING FACILITY Exygen Research 3058 Research Drive State College, PA 16801 Phone: 814-272-1030 STUDY SPONSOR 3M Environmental Technology and Safety Services Building 23E-09 PO Box 33331 St Paul, MN 55133-3331 PROJECT Exygen Protocol Number: 01P-023-066 Exygen Study Number: 023.066 Total Pages: 98 C0120 Exygen Sudy No. 023.066 GOODLABORATORYPRACTICECOMPLIANCE STATEMENT EPexryfgleunorooctaSnuedsyulfonNautembferrom Re0d23.B0l6o6o,d Celclnsiaendd Ser"uBmxtfuocrtiAonnalysiosfUsinPgotHaPssLiCu:m BSalfeecttyroSseprrvaiyc/eMsa,sswaSspepcetrrfoomremterdy."in ccoonmdpulcitaendcefowrit3hMUSEnEviPrAonmTeSnCtaAl GToeocdhnLoalboogryataonrdy Practice Standards (40 CFR Part 792) by Exygen Research. PriniclyipRal hefsetckiergator Exygen Research Aer tN . SSteuadnyGDailrleacgthoerr Wildl Intemational, Lid. / 77 TSpohhflsorReRsetperdesentative Ein. nc. Exygen Research _Daeof2ly Em6M\ae\ea / 1/2 . 0> Date Page20098 ender Exygen Study No: 023.066 QUALITY ASSURANCE STATEMENT Exygen's Quality Assurance Unit reviewed Exygen Study Number 023-066, entitled, "UEsxitnrgacHtPiLonC-oEflePcottraossspiruamy/PMearsfsluSopreocotcrtoamneetsruyl"f.onatAlel from Red reviewed Blood phases Cells were forAnalysis inspected for caolndaupcptlicaacbcloerdGiongodtoLEaxbyorgaetno'rsyStPraancdtaircde OSptearnadatridnsg.Pr~oAclledufirnedsi,ngtshewSetruedyrePproorttoecdolt,o atnhde Study Director and to management Phase 1 ProtocolReview 2. FEoxraticfticoanti,on 3 RawDiuReview 4. RawDaaReview 5 DReavfiteRwepot 6. FRienvaileRweport Date DateERwepgoernted to SDuatde RDeipreocrttoerdatnod ospected Management SponsorManagement 5122/01 col aso p01 Gaol @1s01 646301 71301 ornon 87901 2101 ormoL 1UISIGIN0N 120501 0102 animes ogo 0610203 Lydia Sphffer Quality Assurance Auditor Dat0e 6/02/43 Exygen Research Page 3 0f98 Ghd Eve Sty os 5000 CERTIFICATION OF AUTHENTICITY Teisoeposr, foor Exypgn Std Number 2506, re and complete epee of `Submitted by: Exygen Research 3St0a5t8e RCoelsleeagrec,hPDAri1v6e801 (814) 272-1039 Princippvyege, Eger . Ciily R. ecke Exygen Research Buyin FactiyMmgement fz, ? Date Kean ost PErexsyigdeenntReseg arceh nt sees Study Director, Wildlife Intemational: SVnGaalimg,iaetron, Lu Lat nd, \ Sponsor Reprsensin, Eni lg loa) John Nepsted ose esr = ony 6/1/03 Date ------ Geta Exygen Study No: 023-066 STUDY IDENTIFICATION 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: TEST SUBSTANCE: SPONSOR: Mallard and Quail Red Blood Cells and Serum Perfluorooctanesulfonate (PFOS) 3M Environmental Technology and Safety Services Building 2.3E-09 PO Box 33331 St. Paul, MN 55133-3331 STUDY DIRECTOR: Sean Gallagher Wildlife Intemational, Lid. 8598 Commerce Drive Easton, MD 21601 SPONSOR REPRESENTATIVE: John Newsted Entix, Inc. 4295 Okemos Road, Suite 101 Okemos, MI 48864 TESTING FACILITY/PRINCIPAL: Emily R. Decker INVESTIGATOR Exygen Research 3058 Research Drive State College, PA 16801 ANALYTICAL PHASE TIMETABLE: Study Initiation Date: Experimental Start Date: Experimental Termination Date: Analytical Report Date: 0423/01 05/18/01 07/28/01 06102103 Exygen Research Page 5.0798 cnLnt Exygen Study No. 023-066 PROJECT PERSONNEL The `The Study Director for following personnel tfhirsomprCoejnecttrewAansalSyetiacnalGaLlalbaorgahteorriaets,WiIlndc.l,ifweerIentaesmsaotciioantaeld, Lid. with various phases of the study: Name Emily Decker Dave Bell Karen Risha LingLingLiu Marcia Swartzwelder Xiaoming Zhu Mitra Armand Lawrence Ord Ed Cames Shawn Robb, Title Scientist Scientist Scientist Technician Technician Technician Technician Sample Custodian Sample Custodian Sample Custodian Exygen Research Page 6 of 98 Exygen Study No: 023.066 TABLE OF CONTENTS TUNE PMI ets tA Page GQUOAOLDITLYABAOSRSAUTROARNYCEPRSATCATTIECEMECONMTP.L.I.ANCE STATEMENT ............ 2 3 CSETRUTDIYFIIDCEANTTIIONFIOCFAATUITOHNE.NT.I.CITY. -- r-- A PROJECT PERSONNEL..... TAOFB CONTL ENTSE ... on -------------- sss 1 LIST OFFIGURES cocoons 3 10 LILOSTSOUFMAMPAPREYNDc ICES ................ s N-- s --12 20 30 OBJECTIVE...... INTRODUCTION. o.oo wn sm--rrs rm--s1 --2 -- 4500 TREESFTERSEYNSTCEEMM.AT.cEcRoIcAsLr.sramsmsmsmscmismsmsmsonene--ne--os--es ------e--so--s1]13 6.0 DESCRIPTION OF ANALYTICALMETHOD . 6.1 Extraction Procedre......... wga-- rs-- 1 r-- 6.2 Preparation of Standards 63Chromatography....... and FOrfication pm-- SOIONS .......oc.neereornroror rs------ 14 66..45DIeNsScUrUipMtEiNonSEofNSIHnIsVtIrLumenr t and Ope eratings COndHts ions......s.s.e.s.s.e.s.o.e.e.s.ee.norrnreoor 15 15 7.60.6EQXUPAENKRtIatMiEoNnTaANdLEDXEGSMIGPNE..C.alculationr....e ......ces .coemees eorrr emer 16 18 80 RESULTS... 9.0 CONCLUSIONS ove em -- ns ----19 10.0 RETENTION OF DATA AND SAMPLES... 19 Exygen Research Page 7of98 Cnt Exygen Study No: 023.066 LIST OF TABLES Table. Summaryof PFOS in Reagent Blanks Page rss) Table II. Summary of PFOS in Mallard Red BI00d Cell BIANKS.........c.cccr 22 Table I. Summary of PFOS in Mallard Serum Blanks..... ssl Table IV. SummoafPrFOyS in Quail Red Blood Cell Blanks ........... anni Table V.. SumomfaPFrOSyin Quail Serum Blanks. mmm Table VI. Summary of PFOS Recoveries in Mallard Red Blood Cells. on 24 `Table VIL Summary of PFOS Recoveries in Mallard Serum ...c.c.ccvrvrnnns 25 `Table VIL Summary of PFOS Recoveries in Quail RedBI00dCells... 26 Table IX. Summaryof PFOS Recoveries in QUl Serum ......oucurcvuorivrnies 21 Table X. Summary LL of PFOS in Mallard Red Blood Cell Samples at 0 ppm a.. for emi 8 Table XI. Summary WORKS of PFOS in Mallard commie Red Blood Cell Samples eer at 10 sw ppm a.i. for 29 `Table XIL. Summary of PFOS Week Summ in Mallard Red Blood Cell ws---- Samples at 50 ppm A a. for en30 `Table XII. Summary of PFOS LS in Mallard Red Blood Cell Samples at ram 0 pprm a.i. for win) `Table XIV. Summary of PFOS in Mallard LZ S-- Red Blood Cell Samples at 10 ppm a. for rrrss-----------"y Table XV. Summary of PFOS in Mallard Red Blood Cell Samples at 0 ppm a. for A `Table XVI Summary Week 15 of PFOS in ro. Mallard Red Blood Cell wn Samples at 10 ppm a.i. for ----------------"_3 `Table XVII Summary of PFOS TERM smn in Mallard Red Blood m---- Cell Samples mn at 50 ppm a.i. for smn33 Table XVIIL Summary of PFOS in Mallard Serum Samples at 0 ppm a.i. 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.. for Week 5....35 `Table XXL. Summary of PFOS in Mallard Serum Samples ai 0 ppm a. for Week 10.36 Exygen Research Page 8.f98 Gh Exygen Study No. 023.066 `Table XXIL Summary of PFOS Drs in Mallard Serum Samples at 10 ppm a.. for Week on------------3T `Table XXIII Summary of PFOS Week I5.......... in Mallard Serum Samples at 0 ppm om-------------- a.i. for mmo 38 `Table XXIV. Summary of PFOS in Mallard Serum Samples at 10ppm ai. for Table XXV. Summary of PFOS in Mallard Serum Samples at 50 ppm a.i. for A `Table XVI. SRumEmaWrySof PFOScionnQmumamimlmRmmeidmBelsotoadmmCealrlonSsamples at 0,-- ppm a.. Table XXVIL. Summary of PFOS in Quail Red Blood Cell Samples at 10 ppm a. for `Table XXVIIL Summary of PFOS in Quail Red Blood Cell Samples at 50 ppm a. for `Table XXIX. Summary of PFOS Week10..... in Quail Red ws-- Blood Ces ll Sampm les at-- 0ppm-- a.. for-- `Table XXX. Summary Week 10. of PFOS in Quail Red we; Blood Cell Samples at 10 ppm ai. for pre-----3 `Table XXXL SWuemtmaUrBy,osf PmFaOSrintQunaileRsedsBlood CellrSramples at 0 p-- pm a. fr or `Table XXXIL Summary forWeek of 15 PFOS in e Quailr Red n BloodrCells Samp-- les a-- t 10 p--pm a-- . -- `Table XXXII Summary of PFOS for TERM........ in Quail Red wm Blood Cell Samples at 50 ppm a. rnansmm---- Table XXXIV. Summary of PFOS in Quail Serum Samples at 0 ppm a. for Week 5....46 `Table XXXV. Summary of PFOS in Quail Serum Samples at 10 ppm a. for Week 5...47 `Table XXXVL. WSeuemkm5a.ry of PFOSoin nQuai--l Se--rum--Sam--ple--s at--50 --ppm--a.i. --for--l] `Table XXXVIL WSuRmma1r0y.ocfcPrFmOSrminrQeunairlrSsersusmmSmasmpmlmesseate0rpepemsae.i.erfomr msmsn ll Table XXXVILL Summary Wok 10 of PFcOSrrinrQmumairlsSsermusmmSmasmpelnesssats1e0eprpemeain.efeorrmrsn i `Table XXXIX. Summaroyf PFOS in Quail Serum Samples at 0 ppm ai. for Week 15...50 Table XL. Summary of PFOS in Quail Serum Samples at 10 ppm a.i. for Week 15 .....51 `Table XLL SummoafPrFOyS in Quail Serum Samples at 50 ppma.. for TERM... 51 Exygen Research Page9of 98 Chlntl Exygen Study No: 023.066 Figure 1. Figure 2. Figure 3. Figured. Figure 5. Figure 6. Figure 7. Figure 8. Figure 9. Figure 10. LIST OF FIGURES Page Typical Calibration CUVE fOr PFOS......ceornonrererninirins 53 Chromatogram Representiang 0.1 ng/mL standard for PFOS ................ 54 Chromatogram Representinag 1.0 ng/mL standard for POS... 55 C(EhxryogmeantoIgDrRaemaRgeepnrteBselnatniknAg,aSReet:ag0e5n1t8B0l1a4n)k for PFOS smn C(EhxryogmeantoIDg:ra0m10R7e3pr7e6seBnltainnkgAC,onSettr:ol05Qu1a8i0l14R)ed.B..l.o..o..d..C..ells for PFOS--- C(EhxryogmeantoIDg:ra0m10R7e3pr7e5seBnltainnkgAC,onSettr:ol0Q7u2a3i0l1SCe)rumcforcPFcOS, 58 Cwihtrhom1a0tnogrgam/oRfemPprFeOLseSnt(iEnxgygCeonntrIDo:l 0Q1ua0i7l37R6edSpBkloAo,dSCete:ll0s51f8o0r1tDiRf)i..e.d.. 59 Cwihtrhom1a0tnogrgam/oRfemPprFeOLseSnt(iCnegntCroentIrDo:l0Q1u0a7i3l7S5eSrpukmAf,oSrteitfi:e0d72301D).........60 C01h0r7o0m8a4t,ogSproanmsoRrepIrDe:se4n5t4i-n1g0Q8u-a4i0l1 RWeKdS,BlSoeto:d 0CeSl1l80S1aDmRp)l.e..(.E.x.ycgrecnrIcDr:c 61 CShpronosmoartoIDg:ra4m54R-e1p0r8e-s4en0t7i-nWgK1QuSa,ilSetS:er07u2m30S1aDmDp)l.e..(.E.xygen ID: 0n1m07207, Exygen Research Page 100798 Gary Exygen Study No: 023.066 LIST OF APPENDICES Page Appendix A SAtmuednydPmreontotcsolan0d1PD-e0v2V3i-at0i6o6n(sE..x.y.g.e.n.S.t..u.d.y.N.o... 023-066) amnd nd8 Exygen Research Page 110f98 Cox. Exygen Study No. 023.066 1.0 SUMMARY Esaxmypgleens Rfeosretahrechde(tEexrymgienant)ieoxntroafctpeedrfmlaulolraorodctaanndesquulafiolnarteed (bPloOoSd)celalccsoarmdpilnegs taonpdrosteorcuoml OLP-023-066 (Appendix A) "oTfhequlainmtiittoaftiqounanftoirtqautaiioln for red mallard red blood cells blood cells and serum and was serum was 10 ng/mL. 10 ng/mL. The LOQ The for limit each `matrix was 023.065). determined in a method verification study performed at Centre } (Centre Study: PFOS in ng/mL. the mallard red blood PFOS in the mallard cseelrlusmamspalmepslersanrgaendgefdrofmronomn-nqouna-ndiettieficatbelde levels levels to to 418 685 ng/mL. PFOS ng/mL. in the quail PFOS in red blood cell the quail serum samples samples ranged ranged from from non-quanifiable non-quantifiable levels levels to to 361 514 nem. The average percent recoveries + standard deviation for PFOS in mallard red blood cell spearmcpelnetsraencodvseeryrumsstaamnpdlareds dweevrieat9io0n%for 9PF%OaSndin9q9ua%il+re1d3%b,loroedspceecltlivsealmyp.leTshaendavseerraugme samples were 100% + 10% and 102% 20%, respectively. 2.0 OBJECTIV] "sTpheecoibmjeencstiovfemoafllthairsdsatnuddyquwaaisl troeddebtleoromdicneelllesvaemlsploefspaenrdflsueorrouomctsaanmepsluelsfounsaitneg(tPhFeOS) in analytical method described in protocol 01P-023-066. 3I.0NTRODUCTION Tahnidsquraeiplorrteddebtlaiolosdtcheellrsesaumlptlseosfatnhde saenraulymsissamfpolrest,heusdientgertmhienaatnailoyntiocfalPmFeOtShoidn emnatiltllaerdd, "Extraction of Potassium From Serum for Analysis UPseirfnlguoHrPoLoCc-tEalneescutlrfoosnpartaeyo/rMaOstsheSrpeFclturoormoectrhye"n.ical Compounds Tprhoetocsotludnyumwbaseri0n1itPi-a0t2e3d-0o6n6.AprTilhe23e,xpe2r0i0m1e,ntwahlesntartthedastetuwdaysdiMraecyto1r8,si2g0n0e1d, Exygen and the experimental termination date was July 28, 2001 Exygen Research Page 120198 eat Exygen Study No. 023-066 4.0 TEST SYSTEM "mTahtericxonftorrotlifmiaclatliaornds awnedrequraeicleirveeddblchoioldlecdelolsn abnldueseicreumonusMeadyfor17t,he20m0a1trfixrobmlaWniklsdlainfde Intemational Lid., Easton, MD. They were assigned the following Exygen ID numbers: QuMaaitl rSiexrum Quail Blood Mallard Serum Mallard Blood Ex0y1g0e73n7I5D 0107376 0107377 0107378 Seventy-seven quail received chilled on red blood cell samples blue ice at Exygen on and seventy-six May 17, 2001 quail serum and logged samples were in by Exygen pseervseonntnye-ltwaondmaplllaacredd sienrfurmozseanmsptloersagew.ereServeecnetiyv-etdhrceheilmlaeldlaornd brleude bilcoeoadt cEelxlysgaemnpolnesMaanyd 17,2001 and logged in by Exygen personnel and placed in frozen storage. `Sample log-in associated with and this chain study. of custody information can be found in Storage records will be kept at Exygen the and raw data package a true copy of the storage records can be found in the raw data package associated with this study. 5.0 REFERENCE MATERIAL TEnhveiraonnamleytnitcaall TsetcahnndoalrdogyPFaOndSSewravsicerse.ceived at Exygen on June 3, 2000 from 3M Tmahteeriaavlaiwlaabslestoirnefdorfmroazteino.n for the reference. material is listed below. The reference Compound PROS ExvgenComrolNo. TCRNo. 00023-0422 TCROOI7-46 Purity(%) Expiration Date 97.9 0831/01 Exygen Research Page 13098 oats Exygen Study No. 023.066 `The molecular structure of PFOS is given below. PFOS Chemical Name = Perfluorooctanesulfonate Molecular weight = 499 (CiFyS05") CaFuIl s--0 4 Ndeortiev:ed,Thisepnoetuatrsasliummolpeecrufllueoaronodctstaannedsaurldfofnoatrem [fCryoFm1wyhSOiscKh],PmOoSlec(ualnaiornw)eiisght 538. 6.0 DESCRIPTION OF ANALYTICAL METHOD AFnlauloyrtoicchaelmimceatlhoCdomenptoiutlnedds"EFxrtoramctSieonruomf PfoortaAsnsailuymsisPeUrfsliunogroHoPctLaCn-eEsluelcftornaotseproary/OMtahsesr Spectrometry" was used for this study. 6.1 Extraction Procedure AAft1e0r0fporLtiafilciaqtuiootnoofftahpeprreodprbilaotoedscaemlpllseas,ndthseersuammpwlaess uwseerdefovrorttheexeexdtrfaocrti~on15prosceecdounrdes.. Athne saalmiqpuloets.ofO0n.e5 mmiilllliilliitteerr ooff0.50.25MMtseotdriaubmutcyalrabmomnoantieu/msohdyidurmobgiecnarsbuolnfaattee wwaass aaddddeedd ttoo tphleacseadmpolnesw.risFti-vacetimoinllislhiatekresrofforM~TB20E mwienr.eaandddetdhentoctehnetrsiafmupgleeds.forE~ac1h5 smaimnp.leFwoausr milliliters of reconstituted the organic layer with 1 milliliter were taken of methanol. and dried on a Each sample nitrogen evaporator and then was analyzed by LC/MS/MS electrospray. 62 Preparationof Standards and Fortification Solutions Standard solutions O1P-023-066. An were prepared on individual stock March 14, 2001 as specified standard solution of PFOS in Exygen protocol was prepared af a csaolntcceonnttreantti)oninofme1t0h0anpogl./mLFrboymditshsisolsvoilnugti1o0n,mag1o.0f pthge/smtLanfdoarrtdif(iccaotriroenctsetdanfdoarrpdursiotlyutainodn was prepared methanol. by taking 1 mL of the stock and bringing the volume up to 100 mL with Afort0i.f1icgat/iomn Lstafonrdtairfdicaatnidonbsrtianngidnagrdthweasvoplruempeareudp by to taking 10 mL of the 1.0 100 mL with methanol. pg/mL A 0.01 Exygen Research Page 14.0798 Gan 2 Exygen Study No: 023.066 ng/mL standard was prepared 100 mL with methanol. by taking 10 mL of the 0.1 pg/mL standard and bringing to 0A.0s1etpogf/smtLansdoalrudtsiocnosntinaitnhienfgoPllFoOwSinwgamsanpnreerp:ared by serial dilution of the 0.1 pg/mL and Initial Conc. (ug/ml) or Volume (mL) 5 Diluted to (mL) Final Cone. (uml) 100 0.005 01 0.1 2 100 1 100 0.002 0.001 001 001 5 2 100 100 0.0005 0.0002 0.01 of PFOS 1 100 0.0001 `The stock stored in standard solution and a refrigerator (4 + all fortification 2C) when not and in calibration standard solutions were use. Documentation of standard preparation can be found in the raw data associated with this report 6:3 Chromatography Quantification time of PFOS of PFOS was ~ 4.4 was min. aPcecaokmsplwiesrheeddebteyctLeCd/iMn St/heMcSonctlreocltrmoastprriayc.es The retention corresponding a1l0tetrheseavnearlaylteforrettiefnitciaotniontimree,cobvuetrietshe amounts detected and the rest were were only significant less than the lowest enough to calibration standard (0.0001 pg/mL). 6.4 Instrument Sensitivity cTohnecenstmraaltlieosntofs0t.a0n0d0a1rdg/ammLo.unotf PFiOnjSe.cted during the chromatographic run had a 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: Exygen Research PE SciexAnalyst version 1.1 Windows NT, version 4 Hewlett Packard (HP) Series 1100 HP Quat Pump HP Vacuum Degasser Page 15 of98 C431 Exygen Study No: 023.066 HP Autosampler HP Column Oven HPLC Column:Genesis Cy (Jones Chromatography), 2.1 mm x 50 mm, du CInojlecutminonTVeomlp..: 103u5LC Mobile Phasc (A): 2 mM Ammonium Acetate in ASTM type I water Mobile Phase (B): Methanol Flow Rate: 0.3 mUmin. Time %A %B 0 60 40 010 00 110000 n75 oe60 4400 Tons monitored: Amie Mode Transition Monitored PFOS. negative 499 99 TPunaerFialemeters Controls 1S-lospray DP-Declustering Potential [FP-Focusing Potential EP-Entrance Potential CE-Collision Energy CCXP-Collision Cell Exit Potential DF-Deflector CEM-Channel Electron Multiplier , RetenAtpipornoTxiimmaet(emin) 420 Set 4200.0 -510 230.0 100 -70 -5 300.0 2800.0 Gas Flows Set Nebulizer Gas 12 CCoulrltisaiionnGGass 143 TIS Temperature. 350C 6.6 Quantitation and Example Calculation "pTeeankmaicrreoaliwtaesrs moefassaumrpeldeoarncdaltihberasttiaonndasrtdancduarrvdewwearse ignejneecrtaetdedint(oustihnegLO1/MxSf/itMwSe.ighTiheed Exygen Research Page 160798 Gait Exyeen Study No: 023.066 lcionnecaerntrreagtrieosnsiwoans) dbeyterAmnianleydstfrsoomfttwhaereequuastiinognssbiexlocwo.ncentrations of standards. The 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 equations for serum are shown) Equatio1n: Analyte found (ng/mL) = (Peak area - intescepy) slope. Eq`uAanatliyto2en.found (g/mL) = (anal. found (ng/mL) x EV (mL) x DEXEV (mL) Where: (AV (mL) x sample vol. (mL) FV = Final Volume DF = Dilution Factor EV = Extraction Volume AV = Aliquot Volume x 1ug 1000 ng For samples forified with known amounts of PFOS prior to extraction, Equation 3 calculated the percent recovery. ReEcqouvaetriyo3n(:%) = (anal. found (g/m-Lav)g. anal. in cil (ug/mL) x (1000 ng/L pg)x 100 `amount added (ng/mL) An example of a calculation using an acwal sample follows Mallard serum sample Centre ID 0003803 Spk A (Set: 112100B), fortified at 10 ng/mL with PFOS, where peakarea = sss ismleorpceept == msiso dilution factor =1 ngadded (fort level) = Ing avg. amuinconwols = 0 (Not quantifiable) final volume = am extraction volume = Sm aliquot volume. = am sample weight (volume) = 0.1 mL Exygen Research Page 170798 oan Exygen Study No. 023-066 From equation 1: Analyie found (ng/mL) = From equation 2: Analyte found (ug/ml) = [6558-515] 7740 08ngmL = (08ng/mLx1mLx1xSmL)X lug (mLx0. mL) 1000 ng From equation 3: = 0.00976 pg/ml. % Recovery = . (0u.g/m0 1L0xn=g0/0muL9 g/ml7 )x10600) x 100 = 98% 7.0 EXPERIMENTAL DESIGN Each set of samples (red blood cell 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 & HII. 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 us 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 serum 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 (0 418 pg/mL. Individual results are lisintTaebldes X-XVIL PEOS in the mallard serum Exygen Research Page 180f 98 Gain? Exygen Study No: 023.066 samples ranged from non-detected levelsto 685 pg/mL. Individual results are listed in Tables XVIII-XXV. POS in the quail red blood cell samples ranged from non-detected levels to 361 pg/mL. Individual results are lsted in Tables XXVI-XXXIIL PFOS in the quail serum samples ranged from non-detected levels (0 514 pg/mL. Individual results are listed in Tables XXXIV-XLI 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, all 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 facility-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. Enygen Research Page 19.098 Exysen Sudy Noi 023.066 Exygen Research Page 200195 G47 Exygen Study No: 023-066 Tablel. Summary of PFOS in Reagent Blanks Sponsor Ins Centre I) Se Number nm Regen BlmkA OSI0IA rm RegewBlnkA OSIOIA mo ResgenBlakA2 SISO mo mo RReepegneimBBllnnkkAA OSIOIB O2001A no nm ReagewBlnkA RegenBlnkA OR00IA 0200 nm ReagewBlkA OR00B mo mo RReesggeemnBBllnnkkAA 020A OSZOIA mo RegemBlukA 0208 mo mo ResgenBlukA RegemBlakA 0S20IB 020 mo ReagewBlkA 0920C mo no ReRgeesgneBwlBlnnkkAAd O790IA O71S01A mo mo RReessggeewmBBllkkAA 02004 O200IA nm RegewBlrkA2 02008 mo mo RegenBlankA2t ResgemBlukA 020008 023014 mo mo ResgewBlankA RegwBakA2 023014 O08 mo mo RegnBinkAZ RegwBnkAd 07308 O730C nm Regen Blank AS07301 Extraction Date S801 S801 51801 S801 SS220011 5S2211001) 52200 52200 52200 52200 52200 52201 70900 71901 72000 7722000000 72000 72300 72300 7200 72300 702330000 Analysis Analyte Dae Found (p/n S718-1901 No sns.1901 S901 No No shor No ssnn220011 NNoo ssna20n1, NNoo snl Sasol No No sas No span Sasol No No sn301 19.2001 No ND 9.2001 101 n> ND 11.022100 NNoD 1.2200 ND nsi01 nsion No No 401 n24001 No xo 42202550010 xxoo STANDARD AVERAGE. DEVIATION: ~~ NO. NQ * Duplicate nection bNuQt w=asNoltesQsuatnhtainftihaeblleow(eAstpecaokncweantsradteitoenctoefdtahetchaelciborrarteisopnosntdainndgaradnsal(y0t.e0r0e0t1enutgi/onmLt)i)me ND = Not Detected (A peak was not detected at the corresponding analyte retention time) sFtoarndvaarldu,es0.r0e0c0o1rdpegd/amsLN)Qw,a0s.u0s0e0d05topcga/lcmuLla(thealtfhethaevevraalguee oafndthsetlanodwaersdt dceavliiabtriaotnio.n LOQ = 0.01 g/mL for red blood cells and serum Exygen Rescarch Page 21 of98 CoLL.40 Exygen Study No.: 023.066 Table Il. Summary of PFOS in Mallard Red Blood Cell Blanks `Sponsor In comol | comol comol comol comrol comol conol __conwol___ Centre n OIOSBrkA OO7SBlnkA* OIOTVSBlnkA OO7VEBlamkA Ol7VSBnkA2 OIO7SBlnkA2 OIOTSBlnkB O08 Blank B Set Number 021005 O2A0IB OS201A OS201A 05201B 02018 0201C 052201C Extraction Date S201 S2U0L S200 S201 S201 52201 | 52201 50200 STANDARD Amiysis Date _ 52200 522001 S23 SS230011 2301 S301 snl AVERAGE: DEVIATION: Analyte Found (ug/ml) No No No 00N02o24 000184 No No 0.000548 0.000327 Table Il. Summary of PFOS in Mallard Serum Blanks Sponsor ID omol comol comol comol comol comol Centre n OI07377BlankA3 OMT BlmkA OIOBIBakA 007377 BlwkA* 00777 BlmkA2 0107377 Blank A Set Nomber O71S0LA O7101A 0RMIA ORMIA 07001B 07001B Extraction Analysis Analyte Date Date _ Found (ug/ml) A901 719.2000 000325 7901 7192001 000331 T2001 201 000277 T2001 201 000312 2001 7212201 0001S 70001 721-2201 0002s AVERAGE: 0.00275 STANDARD DEVIATION: 0.000605 * Duplicate infection NQ = Not Quantifiable (A peak was detected at the corresponding analyte retention time `out was less than the lowest concentration of the calibration standards (0.0001 pg/mL) LOQ= 0.01 pg/mLforredbloodcells 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 220198 Gani Exygen Study No: 023-066 Table IV. Summary of PFOS in Quail Red Blood Cell Blanks Sponsor in Conwol comol comol contol comol como cool comol _ Centre Set Number OIOTNGBlkA | OSISOIA 0I076BlakA OSISOIA 0IO7376BlankA2 OSISOIB OI07376Blnk A2 OSISOIB OOT6BAKA ORI0IA OIO7376BlankA O20IA 00I0I773766BBiunkk AA*___0s20O1SC2_O_I_C Extraction Analysis Analyte Date Date Found (uml) SASO1 S/A8-1901 NO SOL SA8-1901 No SN801 S901 No SASO S901 S2U0I S201 NNoo 52101 S700 Q S200 0201 s__psry2030L1 | NNQQ. STANDARD DEAVVIEARTAIGOEN:: NQ NQ Table V. Summary of PFOS in Quail Serum Blanks Sponsor ID Conwol | comrol ccoonvmool conrol conrol Centre Set n Number OIOTSBankA OITISBlankA | 072301AD O72301AD OIO0ITTWSSBBaankkAA22* 0O733008 01O0I73T7I5ISBlBalnnkkAA33 *__O2O32030IICC Extraction Analysis Analyte Date Date __Found (ug/mt) 72301 72301 722660011 000000237029 292330011 20440011 NNQo T2301 7242500 R301 7724-25001 NQ No AVERAGE: 0.00100 STANDARD DEVIATION: 0.00148 * Duplicate injection NbuQt w=aNsoltesQsuatnhiainftihaeblleow(eAstpecaokncwenatsradteitoenctoefdtahtetchaelciborrarteisopnosntdainndgaradnsal(y0t.e0r0e0t1enptgio/nmtLi)me LOQ = 0.01 pg/mL for red blood cells and serum Fstoarndvaarldu,es0.r0e0c0o1rdpegd/umsLN)Qw,as0.u0s0e0d0510gc/almcuLla(thealtfhethaevevraalguee oafndthsetalnodwaersdt dceavliiabtriaotni.on Exygen Research Page 230f98 oNLnal Exygen Study No.: 023.066 Table VI. Sponsor 1 como comol comol comol comol comrol conrol comrol convol convol comol comol comwol conrol Summary of PFOS Recoveries in Mallard Red Blood Cells Centre OI0TTSSpkA 0107378SpkA* OITSSkB OI778SpkB* OITVESPKA OITTSSpkA* OOTMSSpKB OlO7I8SpkB* OIO7T8SpkA2 OI0TSSpkA2+ 0I07378SpkB2 OI07378SpkB2 OITESKB __OI07378SpkB* Set Number 052008 0S210B 0S210B OS2A0IB OS20IA OSA OS201A 0S201A OS20IB 0522018 0S201B 0S20IB 0S20IC 0520 Extraction Analysis Amt Date Date Added (nimi) sRl0L 522000 10 S2LOL 52200 10 S2LOL 2201 50000 S2LOL 52201 50000 S220 S301 10 52200 S301 10 S2200 S301 50000 52201 52301 50000 52201 5/2301 10 52201 SR30I 10 2201 2301 50000 SP201 2301 50000 52201 2301 50000 S201 52301 50000 AVERAGE: STANDARD DEVIATION: RELATIVE STANDARD DEVIATION: % Recovery 5 88 91 95 8 0 8 8 0 7% 101 10s 102 101 90 9 11 * Duplicate injection LOQ = 0.01 pg/mL for red blood cells and serum Exygen Research Page 240 98 cna Exygen Study No: 023-066 Table VIL. Summary of PFOS Recoveries in Mallard Serum Sponsor Centre Set Extraction Analysis Amt % In mn Nomber Date Date Added (ng/ml) Recovery conrol | OI0737TSpkA3 O7IS0IA 71901 719.2001 10 % conrol conrol 0107377 Spk A3 O710IA OIOTITISPKBI OTIS0IA 1901 T1901 719-2001 192001 10 500000 8 in convo conrol OIOTITISpKB3* O7IS01A OLOTNTSpkA O7X0IA 7721090001 717922100101 50010000 n76 conrol conol OIOTIITSpkA OI0T37ISpKB 0O772X000I1AA 7722000000 7271210011 50010000 wm conol conol OIOTITISPKB OT001A 72001 72101 OIOT3TISpkA2 072001 72001 72122001 00000 10 9 107 convol conrol 0L07377Spk AZ OROOIB 72001 721.2200 OI0TI7TSpkB2 O72001B 72001 212201 10 500000 10 2 conrol 007377 Spk B2+ 0720018 720/01 721.2201 500000 5 AVERAGE: 99 STANDARD DEVIATION: 13 RELATIVESTANDARD DEVIATION: 13 * Duplicate injection LOQ = 0.01pg/mLfor red blood cells and serum Exygen Research Page 25 of 98 onto Exygen Study No.: 023-066 `Table VIII. Summaryof PFOS Recoveries in Quail Red Blood Cells Sponsor n cool comol comol cool comol conrol comol conol como convol comol comol comvol convol Centre. Set ID Number OI0T36SpkA OSISOIDR 0107376 Spk A" OSISOIDR Ol07376SpkB OSISOIDR 0I07376SpkB* OSISOIDR 0107376 Spk A2 OSISOIDR 0107376 Spk A2* OSISOIDR 0107376 SpkB2 OSISOIDR 007376 SpkB2* OSISOIDR OI0T6SpkA OS101A OI076SpkAT OS210IA OI0736SpkB OS2A0IA OIO736SpkB 021014 OOTV6SpKA 0S20IC 0107376 Spk A_052201C Extraction Analysis Amt Date Date Added (ng/ml) SASO1 521-2200 10 SASOL S21-22001 10 SISOL 521-2201 50 S/ISOL 5721-22001 50 S/ISOI 521-2201 10 S/IBO1 5721-2201 10 1801 721-2201 s0 S/I801 721-2201 50 SRUOL 522000 10 S211 52201 10 S210 5122001 50000 S201 52201 50000 S201 523001 10 50201 5/23/01 10 AVERAGE: STANDARD DEVIATION: RELATIVESTANDARD DEVIATION: % Recovery 102 9 m m m3 110 109 104 8 w 91 91 %0 94 100 10 10 = Duplicate infection LOQ = 0.01 pg/mL for red blood cells and serum Exygen Research Page 26 098 aLnil Exygen Study No. 023.066 Table IX. Summary of PFOS Recoveries in Quail Serum Sponsor Centre ID m comol | Ol0TTSSpkA convol 0107S SpkA conrol OTSSkB conrol OI0TIISSpkB conol OIOTIISSpkA2 conol comrol 0073S Spk A2* OI07TSSkB2 conwol OI0TVSSpkB2* conol OI0TSSpkA3 conrol 007375 Spk AY cowol OIOTSSpkBI convol 007375 SpkB3* Se Number O7301AR O7230IAR O70IAR O2301AR 07230ID 07230ID O0223300I8B 07230ID O230ID O7230IC O7230IC * Duplicate nection Extraction Analysis Amt Date Date Added (ng/ml) 72301 25000 72301 2501 10 10 T2301 SOL T2301 72500 500000 500000 2301 72627001 72301 72627001 10 10 2301 2301 2400 72400 500000 So0000 72301 72627101 10 2301 72627101 72301 242501 10 500000 7230170425001 500000 AVERAGE: RELATIVE SSTTAANNDDAARRDD DDEEVVIIAATTIIOONN:: LOQ =0.01 pg/mLforred blood cells and serum % Recovery o @ 104 107 2 312 126 106 105 100 110012 20 20 Exygen Research Page 27of98 Cnazag 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 CIen'tSre SISLCIO00D32O00WWkSs 00100722300 SSLI0RSLWES 00731 SSLSILOIDOSLRWWSST 00003212 ASSLLII0TRWSS 0O1l0o72M3R3 S4SLLISIRSEWSKS 0000374 SSLIHGIRISEMWS 000077334S SSSLHIRISNSWSST O00T3S6 541956 Wks 0107236 St Number Exracion ___Date Amaiysis Due Analyte Found gmt) 0s2101D 0210 sauol S20 52200 sp201 No No GAO 00D szuoL s2u0l $2200 S201 0o0o001i967r 0o2s0o8 sszzuuobll sspeaan NNoo GS20B ool smuol sauol S220 S200 NNoo OO02I0B Ssa2uo0l Ss2e2a0n NNoo OSA0B ONO sauol spuol span span 00~01o43 005S2U1001B8 Ss21o0 inS2s01 NNoo STANDARD DEAVVIEARTAIGOEN:: 0.000401 0.000706 * Duplicate necion 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 red blood cells and serum Fstoarndvaarldu,es0.r0e0c0o1rdpegd/amsLN)Qw,a0s.u0s0e0d05topcga/lcmuLl(ahtaeltfhetheavevraalguee oafndthsetlanodwaersdt dceavliiabtriaotnio.n Exygen Research Page 280198 GOAL? Exygen Study Nos 023.066 Table XI. Summary of PFOS in Mallard Red Blood Cell Samples at 10 ppm a.i. for Week 5 Sponsor Care iD ID SSLWOWES 00007 ISSSALIO0IP0OWWESS OOTTIISS SSSLHBOIOLWWESS 00007T3H9 SSLOOWWS 0O0072M0O SSILOOWNSS 0000774411 SSeHI0ONOWNESS O00l2o8T22 SSOI0USSWWEISS O00Tm 4AS1H0I7N0S6EWWEKSS 000l7o2T4a4s St Nmber 00S2200IBBDD U0SsIoOlIBBDD 0os0uoDmD 00SSUN00IBBDD 00SsU00BBDD O0S2U0I0B8D0 00SSUUO0IIBBDD 0_0Ss22I100I0B8DD Euan Amys Due Date SSaoionl S2233000r SsaOuIl SS27300r sSoouul Ss2a3l0 SS2U0 2$2330001 SSaOuLl 5$223001 SSOoLU SS220000 SS2O0L Ssaavonn sSu2Uo0 ss2ovonl STANDARDDEVAIVAETRIAOGNE: Amaiyte Found gym) 22074 1n0e0 1n2s3 11511 S50018 aassss 11889 226s4 187380 +Duplicate jection LOQ = 0.01 pg/mL for red blood cels and serum Exygen Research Page 290198 Corn Exygen Study No: 023.066 Table XII. Summary of PFOS in Mallard Red Blood Cell Samples at 50 ppm a.i. for Week Sponsor mn Centre iy SEIDEN 007245 4SS4CI0I932O9-TWKOST 0107245 0107246 454109-3330-WES*_ 0107246 Se Nomber 020ICD 0S20ICD 0S20ICD 052200CD Exracion Amaysis Date Date S201 S400 S201 sal S200 40l 52001 ___ span AVERAGE: STANDARDDEVIATION: Analyte Found (ug/ml) 589 2 n 123 89 3 `Table XIII. Summary of PFOS in Mallard Red Blood Cell Samples at 0 ppm a.i. for Week 10 Sponsor Centre n m SASS4EI0I9W32O4W9KWKIIO0 0107250 0107250 S4SS4EII09R2S5O0W.WKKIIOO 0I072S1 0107251 SAESIE0I0SSRSILWWKKIIOON 0107252 00252 445S441100993235222WWKKII000 0107283 OOS) 4SEI09SIWKIO 0l07S4 44SS44I1009923S25I4WWKKIIOOT 0OTSE 010755 SSSSEEIIB0RMSSESWWKIIOO 010255 010725 4A5SE1I0D9I5BC5WWKKIIOOT 00110077225876 451093256WKI0 0107257 * Duplicate injection Set Extraction Analysis Analyte Number Date Date Found (ugmL) 052014 0s20IA 5722000 2200 S300 ssl No No 00SSRROOIIAA SS220000 ssnnaiol NNoo OSROIA OS20IA 2200 52200 Sasol snso1 No NQ 0s201A 0S201A si22i00 S200 spon snl Ne No 0s201A sail 0s201A S200 spon smal NQ No 02014 02014 522000 S200 52301 52301 NQ No 0S20IA 0S201A S220 201 52301 ssl No No 052004 __osnoia $2200 snail 52301 snsol No 0.00245 STANDARD DEAVVIEARTAIGOEN:: 0.000200 0.000400 NbuQt w=aNsoltesQsuatnhtainftihaeblleow(eAstpecaonkcwenatsradteitoenctoefdtahtetchaelciborrarteisopnosntdainndgaradnsal(y0t.e0r0e0t1enptgio/nmtLi)me LOQ = 0.01 pg/mLforred bloodcells and serum Fstoarndvaarldu,es0.r0e0c0o1rdged/masL)NQw,a0s.u0s0e0d05togc/almcuLla(thealfthteheavevralaugee oafndthsetlaonwdeasrtd dceavliibartaitoinon Exygen Research Page 300f98 Chana 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 iS GSLIDROW0 SASLEIOIIOKWKIOO SASLLIOIILWKMIO SSUSILOII0DZRLWWKAI0OT SSLSIE0IMODTWBWKKIIOOY ASSLLIIOONNDIWWKKIIOOY SALSIEOIBOATWSNWIIOOT SSLSILIOOTTOGSWWKIIOS 501003096 Whio * Duplicate nection centre St Exracton Analysis Number Date Date 0107255 | OI0DSS 0SI0IAD 0S0IAD S220 Smo 5232400 sm32400 O000275 00S22001AADD Ss2z22001 Ssme3a224d0n1l 00110077226600 00SSZ200I1AADD Ss2z22001 5s3es2a4dopl O06 O06 OGSSRR0OIIAADD sspz2o0lL 223322440011 0072 OT OSROIAD 00D sz20l S201 232401 232001 001100772663) 00SZ00IDAD SSz222001 5s2m3a2z4s0o0l 0O1I0O7T6I86 SOS0NIOIAADD Ssmaao0I s32n33.2a4o0l1 0O1I00772E6S5 __ 0SsR2O0I1ADAD___ssmmoa01__ssnn3azzdoonl STANDARDDEVAIVAETRIAOGNE:: Anaiyie Found g/m) 13 4196 2141 a1435 6n0s 4w2s 518619 116s0 31073 207 LOQ=0.01 pg/mL for red blood cells and serum Exygen Research Page 31of98 Gite Exygen Sudy No: 023-066 Table XV. Summary of PFOS in Mallard Red Blood Cell Samples at 0 ppm a.i. for Week 15 Sponsor ID Centre 1D set Number Extraction Date Analysis Date Analyte Found (pg/mL) 4541093249.WKIS 0107266 ASHI0924-WKIS 007265 0S201B 0208 322000 S201 San 300 NQ No 4S4I09250-WKIS 010267 SSLIDRSOWKIST 0026 0S20B 0S201B S200 S201 spon S301 NQ NQ 44SS4A1I00992N5S1I-WWKKIISS 0107268 0107268 0S20IB S208 S200 sma01 sno sno 000179 000188 44SS441100990022WWKKIISS 00110077226609 0522008 + 0S208 52000 3201 sno snl No NQ A4SSE4II009N3S2I5WVKWIKISST 00270 010270 0208 0208 S220 20 smal sol No No 4ASS4EII00992SSEEWWKKIISST 007271 0107271 0S20B OS0B 2200 S220 301 se300 ND ND A4SSE4II0S9R2SSSSWWKKIISS 001002277122 00S20010B8 san S201 sn301 sno No No : AASS4AII00992SS66WWKKIISST 0107273 010273 0s201B 022018 S201 smn snsi01 snl No NQ 445S4410I90392336B:6WWKIISS 00110077227784 o0s5n0o1i0B sspnaan sspmant NNQQ. STANDARD DEAVVIEARTAIGOEN:: 0000203 0.000613 * Duplicate nection ND = No peak detected NbuQt w=asNoltesQsuatnhtainftihaeblleow(eAstpecaokncweantsradteitoenctoefdtahtetchaelciborrarteisopnosntdainndgaradnsal(y0t.e0r0e0t1enptgio/nmtLi)me LOQ =0.01 pg/mL for red blood cells and serum Fsotranvdaalureds,r0e.0c0o0r1dpegd/amsLN)Qa,nd0.f0o0r0N0D5,gz/emroLwa(hsalufstehde tvoaclaulecuolfattheetlheowaevsetrcaagleibarnadtisotnandard deviation. Exygen Research Page 32 of98 6RLn tL Exygen Study No: 023-066 `Table XVI. Summary of PFOS in Mallard 10 ppm a. for Week 15 Red Blood Cell Samples at Sponsor 1D SSSCCIIONOWKNISST SSLSLII9OOIWVOKWIKSITS SSLLIIOOIILVWWKKISS S4LSLIIOOINWWKKIISS SSSSLHIIOONRIDWWKKIISS SSLSILOITOIEWWKKISS SSHSILIOOSSIVSSWWKKIISS ASSSLSHLIIIOGOEIGWVWKCKIIWSS Centre ID 001007727755 0011007727766 00007277 OO0088 0000727799 OI07260 00110077801 O01002871 00110072882 St Number 00sS22008BDD 00Ss2200BBDD 0os2m0oBmDD 20200BDD OOSSZHOOIIBBDDRR OOSSZR0OIBBDDRR OOSSRROOIBBDDRR 000Ss22P2000IB1BDDD Exeacion Analysis Date Date 52s2p0210 5s2p33224o0l1 Ss2pu2o0r 5s2z33224a0d0l Ss2aa0o0l ssm23s224a0001 sspzoa0ll ss22s3a2seoonl Sspmool ssppuorl 52200 sp20i span spol SS2222000 sspaoll s5spo0o1ol ssspem3sz2auem0nl STANDARD DEAVVIEARTAIGOEN:: Anaiyie Found (gmt 55 8a29 swus os 98675 1116 154 810613 o65e6 os035e10s15 398 Table XVII Summary 50 ppm a.i. of PFOS in for TERM Mallard Red Blood Cell Samples at Sponsor n Cone SSSCLIIOOSROTTTEERRMMS 00002788 ASSSUSLILII0I9OO3SD0HS8ETTTEERRMM::_O00I1007T28H4 * Duplicate nection Sa Number Exeacion Date Anais Date 00S2Z001C0D0 5S2m2a0l1 ssiaoln O_SO_SM0IOSO2I0IS1BBDDDRR_ sSsm2un2oa0l___s_mssappaoonli STANDARDDEVAIVAETRIAOGNE: Analyte Found (ym 7m5 awias8s 3$903 LOQ = 0.01 pg/mLforred blood cells and serum Exygen Research Page 330198 Canin Exygen Study No.: 023.066 `Table XVIIL Summary of PFOS in Mallard Serum Samples at 0 ppm ai. for Week 5 Sponsor --e ASEIDIe OD -WES 454100349Wks ASEIDISIWES 4541093251WKse ASEIDISIWKS ASEIDSLWKS 454109253WKS ASEI0DSIWKS 4455441100003325245-4WWkKsSt 4SIDSSWAS 4541003255-WKS ASLI9SCWES 4541003256:Ws Centre 0I10mD7n303 007303 0107304 0107304 007305 0170S 007306 0107306 007307 0107307 0107308 0107308 0107309 0107309 * Duplicate injection set NOuN7um2m0bb0ee1rAr 072001A 070014 072001A 072001A ORLA 072001A O72001A 0OT7220000I1AA OTA O7200A O7T00A 072001A Extraction Analysis DD7a2a0tt0ee0 D7a2D1at0t0ee0 72001 721000 72001 721000 72001 72100 72001 721010 2000 72100 72000 72100 72000 7200 72000 72000 721010 72100 2001 72100 72001 721000 72001 72100 72001 32101 STANDARD DEAVVIEARTAIGOEN:: Analyte FFoouun0n0dd04g1i4m@ugilmt)) 00017 000566 000599 000878 000043 000516 000499 000432 00044 00062 000392 000544 000516 0.00544 0.00167 LOQ = 0.01 pg/mLforred blood cells and serum Exygen Research Page 34.0798 cand Exygen Study No. 023.066 Table XIX. Summary of PFOS ai. for Week 5 in Mallard Serum Samples at 10 ppm Sponsor Cae ID SAEIID0IIHWWISS 00007331100 4SSSHEIIDBI0OWWEKSS 00003 SSSHHBBILWES 000022 SSII0NRQRWWEESS OOT0I3S SSELI0ORWIWSS 00003D4 4SSSHIIGBRAOALWWESS OOTOISS SSS1HI5O00SWWEESS 00100733166 Set Number 0GT200IDAD 00mn0000liAADD 0022000IlAADD OOEE0OIIAADD O0EO0IADD O0720000IIAADD 007R200001AADD Exracion Dae Anas Date Amite Found (agmi) 172000017 7722220071 128 10 77000011 m22a0 6uz 2R000011 7M22001 . 1i0o8 22000011 772200010 64 858 T22000011 7722020001 E76n6 R7000011 772222001 6sts 7722000101707202010 n76a5 STANDARD DEv VIATIe ON: mso 2e22 s Table XX. Summary of a.i. for Week PFOS 5 in Mallard Serum Samples at 50 ppm --D S-- AISOpioNnnsOoWr ES 0C0o7In3tDr1e7 NONTeu0SmbbeIeArrD b ED7xD2at0a0eoe1n AD7D2mua2it0eers FFoouuAnnmd3d7ig6egGumgmyy SSSHLIOOIOWWESS OTT 0071S S5410030West 0107318 OOZE000IIAADD 0T001AD__ 72000 R001 T2200 22000 7200172000 "0 220 CT STANDAaRD vDEVeIATmIONe: s aw50 * Duplicate nection LOQ = 0.01 pg/mLforredbloodcells and serum Exygen Research Page 350798 cork Exygen Sudy No. 023.066 `Table XXI.Summary of PFOS in Mallard Serum Samples at 0 ppm a.i. for Week 10 Sponsor Centre m m SHI 2OW0 02 SSSSLOII0O9R5A0WWKKIIOO 00100772232 SSLIPOLWKIO 010723 SSEI9SLWKIO 00724 SLI00SIWKIOS 010724 SU1093252WKI0 0072S SSLIOSWKIOT 00725 SSMI0DSIWKO 00726 SSLINISIWKIO 007326 SSCISEWKIO 0107327 SSCI0SAWKIOT 007321 SSLI9SSWKIO 00728 SLI0925SWKIO OIOTRE ASLIISCWKIO 00729 454100 256-WKI0r 010729 Se Extraction Analysis Number ____ Date Date 020018 2000 7212200 OPOIB 2001 21200 OR00IB 72001 I20200 ORO00IB 72001 JRL201 OROIB J2001 T21200 ON00IB 2001 212200, O700IB T2000 T2220 ON00IB 72001 T2A2200 0018 T2001 212200 ONE 72001 I202201 0RIB 72001 7212200 0001 T2001 721.2200 OR00IB 72001 212201 OR00IB 2001 212201 ON00IB J2001 T2200 020018 00017212201 AVERAGE: STANDARD DEVIATION: Analyte Found (igml) 00027! 000 000726 000666 000659 000530 000899 000940 000S1T 00082 ND 00037 000403 000419 000384 0.00476 0.00266 Duplicate nection ND = No peak detected NQ = Not Quaniifiable (A peak was detected a the corresponding analyte retention time but was less than the lowest concentration of the calibration standards (0.0001 pg/mL) LOQ = 0.01 g/mLforred 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 36 of98 Coa ls Exygen Study No.: 023.066 Table XXII. Summary of PFOS in Mallard Serum Samples at 10 ppm au. for Week 10 Sponsor ID 454-109-3289-WkI0 454-109.3269-WKI0 4541093290WKI0 454-109-3200WKIO 4541093201WKIO 454-109-3291-Wk10 454-109-3202WKI0 454-109-3292-WKIO* 454.109-3293-WKI0 454-109.3293-WKI0* 454-109.3294-WKIO 454-109-3294-WKI0* 454109-3295-WKI0 454109-3295-WKIO 4561093206WKIO 454.109.3296 WK10* Centre in 0107330 0107330 0107331 0I07331 0107312 0107332 0107333 0107333 0107334 0107334 0107335 0107335 0107336 0107336 0107337 0107337 Set Extraction Analysis Number Date Date 072001BD 72001 72201 072001BD 72001 72201 072001BD T2001 T2201 O072001BD 72001 72201 072001BD 72001 7722000 072001BD 72001 72201 072001BD 72001 722001 072001BD 72001 72201 072001BD 72001 72201 072001BD 72001 7122001 072001BD 72001 72201 072001BD 72001 7722001 072001BD 72001 7220 072001BD 72001 72201 072001BD 72001 73201 OT2001BD 72001 ___ 7722001 AVERAGE: STANDARD DEVIATION: * Duplicate injection LOQ =0.01 pg/mLfor red blood cells and serum Analyte Found (uml) 145 147 27 2s 935 102 107 mn 132 136 853 864 123 120 1s u2 105 38 Exygen Research Page 370198 ents 6 Exygen Study No: 023.066 `Table XXIIL Summary of PFOS in Mallard Serum Samples at 0 ppm a.i. for Week 15 Sponsor Cre iD ID SSI BEWKIS SSLIOTIGWKIST O07 01073 SASSHLII0O0R3OUWOKWIKISST 0I10O70 SSSLLIIOOR0DWOKWISST 0010077H300 SSSSLLIIOORISLSWLKWIASST 001007711 SSSSLHII9ORRWRKWIKSST 001007232 4SIODSIWKS SSHIORSIWKIST 00733 01073 SSESILOIROSSSEEWWKKIISST 0010077344 SSSSLCIIBOASSSWWKKIISS 0OI00774MSS ASS1S0L9IO2S5EWWKKISS" 001I00773M466 Sa Nmber Exacton Amis Date Date OOVTI0S0IIAA 1I9N0I1 771199..22000011 OOTU0OIAA 7IN0I S7192O001 OOTI0IAA MT9I0N1 771199.22000011 OONNS00IIAA 7T1990011 TTA992200001 0O9T0AA 9TI09N1I 71199.-22000010 OOU0SIOIAA ITOSMOI 719200011 OOUI0IAA AT9O0I1 771199..22000001 0O1700IAA A99001 T1992000011 Oo7Ii0AlA A11990011 __T7199.0200011 STANDARD DEAVVIEARTAIGOEN:: Amie Found gpm) NNnD 0000017229 >n> 0000004446!6 IND 00000067839 xNDD 0000026939 00N1D95 0.000503 00616 Duplicate injection NNQD == NNootpQeuaakntdietfeicbtleed(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 38.0198 ents Exygen StudyNo.: 023.066 `Table XXIV. Summary of PFOS in Mallard Serum Samples at 10 ppm ai. for Week 15 Sponsor Centre mm D 4541003280 WKis 0107347 4541093269-WKIS* 0107347 4541093290-WKiS 0107348 4541003200-WKIS* 0107348 4541093291WKIS 0107349 4SHI003291-WKISH 010749 4541093292WKIS 0107350 4S41003202.WKIS* 0107350 4541003293WKIS 010731 4S41093203-WKIS* 0L073SL 4541003204WKIS 010732 4541093204-WKIS 0107352 4541093295 WKIS 0107353 4541003295-WKIS* 0107S} 4541003206 WKIS 0107354 454109-3296-WKIS* 0107354 Set Number O7I0IAD O710IAD O7ISOIAD O7190IAD O7ISOIAD O7101AD O7190IAD O7I90IAD O7ISOIAD O71901AD O7ISOIAD O7I0IAD O71S01AD O7190IAD O7ISOIAD O71901AD Extraction Analysis Date Date 719001 7202100 71901 7202101 9001 7202100 1901 7202101 901 7202101 INL 7202101, 7901 77202100 71901 77202101 7901 7202101 71901 7202101 7901 7202100 71901 7202101 71901 7202100 71901 7202101 71901 7202100 71901 7202101 AVERAGE: STANDARD DEVIATION: Analyte Found (ug/ml) 152 162 101 875 152 102 1 i 128 132 613 as nr 116 952 13 7s 13 Table XXV. Summary of PFOS in Mallard Serum Samples at 50 ppm au. for TERM Sponsor Centre ID D 4S4-1093297-TERM 0107355 454100297TERM= 0107355 454-1093298-TERM 007356 454.100 DORTERM 0107356 * Duplicate injection Set Number O7200AD OT2001AD OT00IAD 072001AD Extraction Analysis Date Date 72001 7722001 72001 7122001 72001 722001 720001722001 AVERAGE: STANDARD DEVIATION: Analyte Found (ug/ml) 85 01 66 601 638 a LOQ =0.01 pg/mLforredbloodcells and serum Exygen Research Page 39.01 98 cole `Exygen Study No.: 023-066 `Table XXVI. Summary of PFOS in Quail Red Blood Cell Samples at 0 ppm ai. for Week 5 Sponnsor Ceintre SSAIIOBIGILWEES 000070077 ASSIIO0SBIWRWSS 0O00007T6E SSUSILOLIIGSWWESS 00000009 SSLIIBGIRIAAWWKKSS 00000000 SSSIIOBRIISSWWISS 000I0008S1I SSSOIISBII66WWESS 00000022 SSEIISOIRSIWEEWSS 0000700683 NuSmtber ExDaatce t AnDaluycsis FouAndna(lgym) OOSSIIBSO0IIAA SSAEBTI SSss1o9mmnr NIo) OOSSIISBOOIIAA SSuuBsOOLl saSss.ioomnnn Nxoo OOSSIISOOIIAA SSuuss0Dll sssoiooonn xNoo OOSSIISSOOIIAA SSSSDDII sSnos.oionmn xNoo OOSSIISSOOIIAA SSUuSSOOll ssosonn NNoo OGSSIISSOOIIAA SSiISSOOlI SSaAlSIoOo0nL o00o06ms OOSSIISS0OIIAA sSiUsSOil sasatso.n Nxoo STANDARD DEAVVIEARTAIGOEN:: 00.000000494903 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. or red blood cels and serum sFtoarndvaarldu,es0.r0e0c0o1rdged/masLN)Qw,a0s.u0s0e0d05opcga/lcmuLla(thealtfhteheavevraalguee oafndthsetlanodwaersdt dceavliiabtriaotni.on Exygen Research Page 400198 CnLy 2 Exygen Study No.: 023.066 `Table XXVII Summary of PFOS in Quail Red Blood Cell Samples at 10 ppm a.i. for Week 5 `Sponsor Centre Set Extraction Analysis Analyte n ID Number Date Date Found (g/mL) 454108401WKS 007088 4S4-108401-WKS 0107084 OSISOIDR SABI OSISOIDR SASOI 521-2200 5212201 13 107 454.108402WKS 007065 OSISOIDRD 5/1801 454-108402-WKS* 0107085 OSISOIDRD S/1801 S201 sn201 353 351 454108403WKS 0107086 4SH108403WKS 0107086 OSISOIDR SARI OSISOIDR SASOI 2122000 521-2201 305 304 454108404WKS 007087 454108404WKS 0107087 OSISOIDR OSISOIDR SNSOI SASOI 521-2200 521-2201 2%9 28 454-108.405WkS 454-108405WKS* 0107088 007088 OSISOIDRD OSISOIDRD S/181 S/ISII S201 sr201 ats a 454.108406.WKS 454.108406.WKS OLOT09 0107089 OSISOIDRD OSISOIDRD S180! S/O S201 sa201 1050 10i0 454.108407.WKS 0107090 OSISOIDRD SN&0I 454-108407-WKS 010700 OSISOIDRD S/1801 sp201 S201 405 sol 454108408WKS 454-108408WKS 007091 0107091 OSISOIDRD S801 __OSISOIDRD _ S/1801 201 522001 asi an AVERAGE: 39 STANDARD DEVIATION: 2 " Duplicate injection LOQ = 0.01 pg/mL for red blood cells and serum Exygen Research Page 41098 GOL Exygen Study No: 023.066 `Table XXVIII Summary of PFOS in Quail Red Blood Cell Samples at 50 ppm a.i. for Week 5 Sponsor SSEIRAIWES SSCIBHLWES SSEIOS4LWES SS1040.WES' Centre Set Number 0107092 | 0S20CD 010702 020ICD 007093 0S220ICD 0107093 020iCD Extraction Analysis Date Date S201 san sn sso S201 spel som spat AVERAGE: STANDARD DEVIATION: Anaiyte Found (apmt) 166 16 108 103 135 3 Table XXIX. Summary of PFOS in Quail Red Blood Cell Samples at 0 ppm ai. for Week 10 Sponsor n SSEI0SI6IWKI0 4SLILILWKION SSLILIRWKIO SSLSIL0I8R3I2GWWHKIIOOT 4SLISIGLWKIN 4SEI0SI6LWKIO 4SEI08IGHWKIN 4S4I0836SWKIO 4SHI0L36SWKIO S4LSLIIB0I8636W6KWIKOION 454108367-WKIO S4SSE4I0IS033G6RWWKKIIOOS SSEI0BI6LWKIO Centre Ir 0107100 0107100 0I07IOl 0O0I7070I002L 007102 0107103 OIO7I03 0107104 0I07104 0010077100055 0107106 0010077110076 007107 * Duplicate injection Set Extraction Analysis Analyte Number Date Date Found (ml) GSISOIE SASOL OSIIOIB SAO S900] sol NNoo OSIBOIB SASOI ssl OSIOIB SAMO sgn No No OSISOIB SAROI 0SISOIB SUROI S91 s/1on01 NNoo OSISOIB OSISOIB SASOI SUSOL SS99011 NNoQ OSISOB SMSO OSISOIB SASOI snow sno No NQ OSISOIB O0SISOIB SAO SASOL S901 S901 ~Q No OSISOIB SASL OSISOIB SASOL sor sol No No OSISOIB SASOL OSISIB sisi sor snom No Q AVERAGE: STANDARD DEVIATION: NQ NQ NbuQt w=asNoltesQsuatnhtaniftihaeblleow(eAstpecaokncweantsradteitoenctoefdtahtetchaelciborrarteisopnosntdainndgaradnsal(y0t.e00re0t1enptgio/nmtLi)me LOQ=001 pg/mL for red blood cells and serum sFtoarndvaarldu,es0.r0e0c0o1rdged/masLN)Qw,a0s.u0s0e0d05togc/almcuLla(thealtfhethaevevraalugee oafndthsetlaondwaersdt cdeavliiabtriaotni.on Exygen Research Page 420f98 anty as Exygen Sudy No: 023.066 Table XXX.Summary of PFOS in Quail Red Blood Cell Samples at 10 ppm a.i. for Week 10 Spionnsor CoInDte SSSSEHIO0HHOOLLWWKIOO| 00I00771I0088 SSSLCOROWRKO 00007710099 SSEUII00LGWIKWIKOOT OOOO7THUOO SSSSLEOILOOBLAWOLKWIKOOT OOIT0TTII ASSSLHIIOBBAASOWSKWIKOO 0000771122 ASSSLLIBAWKIO O0I0O7Us3 SSCSIIOBWIWKKOOT OOIIO07TIISE SS54UI0S80W8WKKIOO_0I0OTT1IISS *Duplscnecion MeSmebter GOSSIIOS0IIDDRRDD GOSSIISOOIIDDRRDD GSGISBIOOIIDDRR OOSSIIBOOIIDDRR OOSSIIOBIODDRR OOSSIIBOODIDRR OOSSIISOOIDDRR _O_SOSIISSOOIIDRD_R_ BiDuoen ADmaies SSa1sso0lr 552220011 ssaovolr $522220011 Ssanssooll s2712.12.2020001 Ssanswooll s5n21122220000 ssaavvooll 5s021122220011 ssaavsoorl 532011.22220011 Ssaasvoolr 5$2a11..22220011 ssaavwo)r s5p21r.z2a2n0n1 STANDARDDEAVVIAETRIAOGNE: FounAdmgiem [anA 09s 220570 211920 0180 ass0s 225s 530042 212209 L0Q = 0.01 g/m. for red blood cells and serum ExygenResearch Page 43019 ons Exygen Study No 023.066 Table XXXI. Summary of PFOS in Quail Red Blood Cell Samples at 0 ppm a.i. for Week 15 Sponsor Care St Ewcion Amb Awe SG OILW WS OO0ToIiTe oGmsozii0AA ssaovoonr SCIONS ol 20a sol ssamaan smal NNoo No SSOO0SSRIGWWIKSS OoOomS G0i2o0iAa ssoaiull ssoml SSIGWKS OOS osmiolA Sou sma ooxzoe aos SSsLesOdeWWkSs oomTy oo22ii00llaA sSmaoo SUGSWKS 0720 oRi0lA Sao ssoomm smo oNooo 0000s SSLUISSIWEWAASS 007720 oomiiooliAA sSoaoon SU06WKS oT oon saol ssmaaml smal rNeoe No SSLLOOWWSS 00722 GomiiloiaA SSouoel ssmmaol SLISIEWKS 002 020A saul save oooamsrisc xo SSL0OISEIWWKASS 00002D6 oossoo sSo2l0o1 ssammatl selsIWAS 0012s osmioa savor spr omxiso N STRAT OIOTI2d| OS2101A SSTRAMNODNARDDSEA2VVI0EART1AIGOEN:: 00N0000Q139088 * Duplicate jection ND = Nopeakdetected NQ = Not Quantifizble (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 red blood cells and serum deviation. For values recorded as NQ, 0.00005 g/mL(half the value of the lowestcalibration standard, 0.0001 pg/mL) and for ND, zero was used to calculate the average and standard Exygen Research Page 4.198 cans Exygen Study No: 023.066 `Table XXXIL Summary of PFOS in Quail Red Blood Cell Samples at 10 ppm a.i. for Week 15 Sponsor ISEIRLOLWKS ASSESILSOILWWKKISS SSLSILIAOROWLKWIKISST SSSHLIIOALIOLWWKKIISST SSSSLHIIOAAOOLSWWKKIISST S4SSEeI1R0A8O40S6WWKKIISSS SSSSLUIIBLAO6TWWKAIISST ASSSELIIOOBLAOTSWWKHIISSS SSSSHIHBIAROSIWBKWISST SSEISIBWKIST Centre 0107125 0011007712265 0010077112276 000077112278 0011007712280 0O0I7017I2390 00100771330 O01007312 0010077332 0107133 Se Exiracion Analysis Number Date Due OS2I0IAD| 02101AD S210 S2I01 557222.3230000 O0SUO0IIAADD Ss2mUIODLL 5s2m2222330000 OORNUO0IIAADD Ssm2uIo0l1 S52222030 OOSUNOOIIAADD. SS2EULOOLL 552222.2330001 GSOIAD 0SOIAD S2UO S2UOL 52222.22330000 O0S2I10IDAD Ssz2UD0I 55222222330011 OOSSAN0OIIAADD SS22UUOOLL 552222..22330010 0S20ICD OS20ICD sauol szuol Spal Sao O0A201I0A1DAD__SsApUuDo1_s5m2222a3a0o1 STANDARD DEAVVIEARTAIGOEN:: Analyte Found qugmt 7122 213665 21825 11320 11598 3261 516303 112565 5su6l7 203 248 Table XXXIIL Summary of PFOS in Quail Red Blood Cell Samples at 50 ppm a.i. for TERM Sponsor Centre n SSLCIITSAEDTRERMMS 0O1I00771I4d SSCS1L0I8G4M1I0GTTEERRMM 001007713355 * Duplicate nection Sa Number 00SS200IICCDD 005S22200iICDC_D_ Exacion Analysis Date Date 5s2a20o0 2Sp4a0n1n S2200000 Ss4p0a1m STANDARD DEAVVIEARTAIGOEN:: Analyie Found gmt) 336516 110s5 213444 1OQ = 0.01 pg/mL for red blood cells and serum Exygen Research Page 45.0198 caLys Exygen Study No.: 023.066 Table XXXIV. Summary of PFOS in Quail Serum Samples at 0 ppm a.i. for Week 5 Sponsor m Centre D Set Extraction Analysis Analyte Number. Date Date Found (ym) 454108361WKS 0I07Is4 OT2301AR 4SEI08361WES 007154 O7B0IAR 72301 T2301 725001 7501 00282 0.0295 454108362WES OIO7ISS O70IAR 72301 72501 45EI0832WEST 0107155 OT30IAR T2301 72501 00149 00134 4SHI08363WES O0IO7IS6 4SHI08363WKS OIOTIS6 OT2301AR O7NOIAR 72301 2301 90501 0SOL , 00198 00166 4S4I08364WES OIOVIST 456108364WKST 00717 O7230IAR OT0IAR 72301 T2301 702501 725001 000510 000835 4SHI08366WKS 010719 OT20IAR 454108366WES 010710 OT20IAR T2301 72301 72501 725001 0013 00120 4SHI0SI6EWKS 007160 OT20IAR 72301 72501 454108368WKS 0107160 072301AR 70301 725/01 00138 00156 AVERAGE: 00156 * Duplicate injection STANDARD DEVIATION: 0.00746 LOQ = 0.01 pg/mLforred blood cells and serum Exygen Research Page 46of 98 Gris Exygen Study No: 023-066 Table XXXV. Summary of PFOS in Quail Serum Samples at 10 ppm a. for Week 5 Sponrsyor SSESIEI008L4422WWEESS SSEIBMOLWES SSHI0SBWIS SSLISOLWIS SLIOSAOLWKST SSLIOMOSWIS ASLIOSAOSWIST SLI0S40GWIS SSCI0BM06WKS SLILOIWS SLIT _ASSSISE0LIIB00ABS04O0LSWWWIIESSST CenItDee 001I0071T6I2 OIOTIGS 0107163 007161 0010077166s8 00II007T1I6GSS 0O0I7017I6G76 0O1I007T1I6G7S O0I1O0T7I1G6S8 NeSmuber Extraction Dae Amalyis Date 0O772233001IAADD | 722330011 770660011 OZ30IAD 07301AD 301 2301 0601 73601 O7B0IAD O0IAD 2301 201 72601 72601 O70IAD O30IAD 72301 T2301 72601 70601 OT0IAD OZ30IAD T2301 2301 72601 92601 0730IAD 00D T2301 T2301 72601 70601 O_02772000II01AAADDD 7T20M30O31L017m672e06o011L STANDARD DEAVVIEARTIAOGNE: Analyte Found agin) 5is8s us 8 918034 18 1=06 2I4 73663 s8sa98ss 35.0 `Table XXXVI. Summary of PFOS in Quail Serum Samples at 50 ppm a. for Week 5 Sponsor IS SUIOLMIWES SHISMILWST SSLI0842WKS _ASSLII0OG8A4O-2WWISS * Duplicate injection Centre Se Edracion Amlsis ID Number Dae 00092 O730IAD| 7avol Date 72601 0O1I001T009923 0O2T0ZOIIAADD T22330011 07660011 O01070093)00070I0A1ADD 10M30017A2Va6EsR0Ao1GE: STANDARD DEVIATION: Amalie Found (agin) 551 5s2e9 ss5ao2t0 19.4 LOQ=0.01 pg/mL for red blood cells and serum Exygen Research Page 470198 COLYSEG Exygen Study Nos 023.066 `Table XXXVII. Summary of PFOS in Quail Serum Samples at 0 ppm a. for Week 10 Sponsor SSSSHIOIIL6WIKWKOOT SSLSIHIIRRIWQKWOK0O0T SSHHGINWOT SSIS0ISBIIEWWKKIIOOT SS44IIB0IWSSWWEHIIOO 4SSL4II00883I666WWAIIO0 ASSSHLOIILOIOWWKKOOT ASSSSSLIUI0IS8OI3L6GISWWKIKOOOY CoImDre 007177 O00T7I7S7 O0T0S9 007 O00V71I0 0OO0T7I8S1I 000077122 0000SS 0000007718Si4 * Duplicate injection NuSmeber 07008 007700m 005700Bm 0B 03300 00300 OOT7B0 moonmo 000T7BmO0mImB Exracton Due Analyls Date Rye Twn 7240n um vTveerr ammaim mvy0e 0d40r1 TTa2yvo0 dTeln 7T22330011 7e20n00 723300 e04n00 TTvyeor aammi 11v2ov30l011 amau0non STANDARD DEAVVIEARTIAOGNE: Anslyie Found gm 000i83 000000i28995 0o0002i6607 000521 000000337950 r00e0e% 000000443397 00000055623 o0oo0o0s5os3e7 00..0000413005 LOQ =0.01 pg/mL for red blood cells and serum Exygen Research Page dof 98 corns Exygen Study No 023.066 `Table XXVIII Summary of a. for Week PFOS 10 in Quail Serum Samples at 10 ppm Sponsor CoIDre NSeam ExDcuieon ADmoies FouAnwadiygiem) 4SSS4I1O0S5A4O0IW1KWIKOO | 0OI100T7ESS TGoODD 272330011 772277..22880017 SSUI0LARWKO 00718 0mODD 2301 727.2800 u21n3 56 SAS4LII0OROSWWKKOI0O 0Ol0077I8S7S 0OiT0IiOIDDDD 3230011 77227.8208011 517s SS4S14I008440WWKKOI0T 00007188S7 O0O0DD + 77203011 772277.22880000 1m94 SSSS44II0B8A40ASWWKKII0O 00110077118898 0073300IIDDD 072330011 772277.20880000 210573 SSSL4II00BA40WSKWIKIOO 0011007719805 a0TT0OI0DDDD SOISAWKIOT 00790 aTODD 7722330011 2301 772277..22880010 727.2801 1w0r5 110 -444S14S013048L0480W8KWIIKO0'S0O1MI007T1I9910 1 L 00T7723O3W 01DIDDDD_DK_ In772293Oy0011 __l_ 790o277..028I n80011 OT9757I0 L STANDARDDEAVVIEARTAIGOEN:: 114 63.4 +Duplicate injection L0Q= 0.01 pg/mL for red blood cells and serum Exygen Research Page d9of98 COLnES Exygen Study No: 023.066 `Table XXXIX. Summary of PFOS in Quail Serum Samples at 0 ppm a.i. for Week 15 Sponsor in SALSIA0IBOIIE6LLWWKKIISST S4ESIEI00L83IWQHWIKISST AASSCLII0OLIIBGWWKKIISSS ASSSLLIIBBIIGGEAWWKKIISSS SSLSIL0IBBIGISSWWKKIISST ASSSGEII008I36666WWKKIISS 44SSI40IS0I83WWKKIISSS a4S5L1I0B8I36E5WWHKIISS SASSLCIIOBRIIBBWWAKIISS Centre I 0107192 007102 0107193 007193 010714 OI07TI94 010795 0071S 0107196 007196 0107197 0107197 0107198 0107198 0010077119999 0107200 0107200 * Duplicate injection Set Extraction Analysis Number ___ Date Date O730IC ODS0IC 72301 2301 7242501 7242500 OT30IC 0230IC 72301 201 7242501 7242501 O230IC OT20IC 01 TAWOL 242500 T242S01, 0230IC ORI0IC 2301 301 7242501 242500 0230IC ORNIC 2301 2301 7242501 7242501 0G2030IICC 2T2330011 772244225500001 07230IC 0720IC T2301 IIL 262501 42501 0O7T2Z300IICC 2301 TW0I 7242501 722500 O730IC 07301 21320310170422452050011 STANDARD DEAVVIEARTAIGOEN:: Analyte Found (ug/ml) No No No No 000184 000160 No NQ No NQ NNoo 000227 00000022593 000255 00016 000160 0.000928 0.00105 IbuNtQ w=aNsoltesQsutahnainiftihaeblleow(eAstpecaokncwenatsradteitoenctoefd tahtetchaelciborrarteisopnosntdainndgaradnsal(y0t.e0r0e0t1enptgio/nmtLi)me LOQ = 0.01 ug/ml.forred blood cells and scrum Fstoarndvaarldu,es0.r0e0c0o1rdpegd/amsLN)Qa,nd0.f0o0r0N0D5,gz/emroLw(ahsalufstehdetovaclaulecoulfattheetlhoewaevsetrcaagleibarnadtisotnandard deviation. Exygen Research Page 50.0f98 GOL ExygenStudyNo. 023.066 Table XL. Summary of PFOS in Quail Serum Samples at 10 ppm a.i. for Week 15 Sponsor Centre m Ir 4SSS4LII100S844001WWHKIISS 0011007720011 S4SHLII0LR40W2KWIISST 0010077220002 4S5L1I0O8S4O0L3WWKKISS 00110077220033 SSLIOS0LWKIS SHI0LWKIS 0107204 010204 4ASS-L1I0O8S4A05O-SWWKKIISS 00110077220055 4SSLLIIO0S0A06GWWKKIISST 00110077220066 4SSSHIHOIS0AIOTWWKKIISST 000170220077 44SSHLIIO0B4A00SSWWIKIISS 0010077220088 SSSSLUIIS0I3BIBWWNAISS 00110077220000 Se Number 0O772030I1DDDD 00700IDDD 00220300IIDDDD 0230IDD 703700IIDDD 00772230001IDDDD 0077223300IDDDD 07230IDD O077300IIDDDD 0730DD 0730DD__ Extraction Date 7T223300011 2R330011 T722330011 + 301 722330011 27233011 T22330011 2301 R23Y0O1 2301 0301 STANDARD Amalysis Date 27207..22880011 772277..22880011 772277.22880010 727.2800 772270.22880010 772277..22880010 772277..22880011 721.2801 7772211-:22880011 7121-2801 A7V27E.R2A8G0E1: DEVIATION: Analyte Found gm) 118810 s2a1s 22436 11 110417 710586 61097 1s 819012 1 91530 866 `Table XLI. Summaryof PFOS in Quail Serum Samples at 50 ppm a.i. for TERM Sponsor Cenmtnre SSSSSEUIIO0OS44AI1I0OO-TTTEERRMMY 000O1I0707722211111 * Duplicate nection Se Number 000T7722033I0011D00D00 Extraction Date Analysis Date 77p2233y0011 m7702a270s2288o0011n STANDARDDEVAIVAETRIAOGNE:: Anaiyte Found (ym) sp"ii6a 495 269 LOQ = 0.01 g/mL for red blood cells and serum Exygen Research Page Sof95 GNLG0 Exygen Study No.: 023.066 Exygeenn ReResseearrccth Page 520f 98 ainan Exygen Study No: 023.066 Figure 1. Typical Calibration Curve for PFOS GSI001A1 (PROS) LinearRagssion (1 wendy 76267 x 178241 09969158) s4cao,t J. aor ates ato . aes a0 a2e0]] 2a] 2200] / - xVs 10s] . 40a J rane] rong son] A wmf | ml OT Te TE ng? BW Exygen Research Page 530198 CNL Exygen Study No.: 023-066 Figure 2. Chromatogram Representing a 0.1 ng/mL standard for PFOS Er i a | - = | x I.2 pe 3 | a3 Co| 4 p 3: i | PLT Exygen Research | i| J| | T Foro oR= ol fN | Page 54 of 98 0133 Exygen Stay No: 023066 Figure 3. Chromatogram Representing a 1.0 ng/mL standard for 4 PFOS Br =F | | Hi | : : | | g Eugen Reseach | | | | Pages 0098 cana Exygen Study No.: 023-066 Figure 4. Chromatogram Representing a Reagent Blank for PFOS (Exygen ID Reagent Blank A, Set: 051801) [Sa = | | 3 | | 3 3] 3 PI T2 e - 1 | | | 10 10 1 o | :Al | 2g) eee 1a 01 T i | nl L1 Hnr irun hdy Bea assets Ghlnsl Exygen Study No.: 023-066 Figure 5. Chromatogram Representing Control Quail Red Blood Cellsfor PFOS {(Exygen ID: 0107376 Blank A, Set: 051801A) Isr | I :| | | Efi1al1 | 2 Cli1 al | 100 i | fbl7 em afe . I 1 | Tr | | {eeLEoeE | ChHlnas Exygen Study No.: 023-066 Figure 6. Chromatogram Representing Control Quail Serum for PFOS, (Exygen ID: 0107375 Blank A, Set: 072301C) a Egy f ho ' | | : 13 to | 3 | : 3 | : re | a {i i ||| 0|1 lT iem om e Te 3Er fiim "Ay | ThoTt Bem t tr md |id ExygenResearch Page 18 GnLns? Exygen Study No: 023066 Figure 7. Chromatogram Representing Control Quail Red Blood (CeElxlysgfeonrtIiDf:ie0d 1w0i7t3h7160Snpgk/Am,L Soeft:P0F5O1S801DR) IEE | EF : | fEFeEe mo. || | z i: | E | J { - | 3 J | 7] 4 | = | 7 Exygen Research | | ! | | | Ceprer Page 59.0198 GOALS Figure8. Chromatogram Representing Control Quail Serum IEE fortified with 10 ng/mL of PFOS (Exygen ID: 0107375 Spk A, Set: 072301D) | 3: |; | 3 | = || = | | | | | | CRAG Exygen Sady No: 023.066 Figure 9. Chromatogram Representing Quail Red Blood Cell Sample (Exygen ID: 0107084, Sponsor ID: 454-108-401 WKS, Set: 051801DR) IEEE = || | = | : |E || 3= Expgen Reseach || | . Page 1 019% [Lp sil Exygen Study No.: 023-066 Figure 10. Chromatogram Representing Quail Serum Sample (Exygen ID: 0107207, Sponsor ID: 454-108-407-Wk15, Set: 072301DD) oor 45108-40715)OF500 oc-noessnom aa awwo ahsoe oasrar Kd Taw a am iw ek ik ae Exygen Research Page 62019 oan Exygen Sudy No. 023.066 Study Protocol 01P-023-066 (Centre Study No. 023-066) and Amendments and Deviations Exygen Research Page 630198 CAlESR Exygen Study No: 023-066 ConProt No.01P023.68 |! ANALYTICAL PHASE PROTOCOL ANALYTICALPHASE TITLE ! |1 EXTRBALCOTOIDONCEOLFLPSOFTOARSASNIAULMSPYEEESRCEFTULRSUIOONMRGEOTOLRCYETAENLESULFSOhNhATEFRnOMeRED |i| ME sTpoonspordeySic |b l SPDFRuOlBiNonNg133331533.330135551 !| ; ; DATAREQUIREMENTS Rosy MethodResumes i! PERFORMINGLABORATORY || ! Cn AsguN iLeCail sr Bhe1.01 ene ! : `Phone 814-231-8032 { i | FROTOCOL IDENTIFICATIONNUMBER oraz ! | CoeAniLiens. Exygen Research rae a129 } Page 4198 Gnas yan Say No: 02.066 Comat pss i| TE Cr AAESEeREiohocT ESLFONT ROM !j p-- !i ] 5. PERFORMINGLABORATORY ce ! F + SAMPLEPC ROCESSING, STORAGEADD--BNT--IR--CA--TIO--N... 8 10. EXPERIMENTALDESION.......cocecccmmmreessnmssesmsesnsmmmen 10. ! | | 11. 12 RECORDS cee11 PROTOCOLAMENDMENTSANDDEVIATIONS...........c.oooescen1ee1 i i 14. DA ANDT REPORA T... mmsmmmssssssssssms meson 12. { CentreAnalytical Laboratories,Inc. FR. Page20(29 + Pagescron Gadi Bxygen Study No: 023.066 Cone PrNe,o 01.23t .06 | ETXitTleR:BALCOTOIDONCEOLFLSPFOTOARSASNIAULMYSPSPEIESRCTFURSLIONUMGEOTMRRLYOCOBCLTEACNREOSSUALFAROONeMARTEDE i 1 PuReosE ! i|i: Thf"CoEoerxmpipursoercuspiniooddsnuseeosOfFFtorifPosomstptueuSsrdiclyuuiumosmrtFooecaFrcnoularnloeyszsAaelcmnoauntlnsleciairod(anUPnstRdiiOnqSegu)aOHlrwPirLeOndgCblltmoeodcecoeedpllesarseyabmnpiodloe,ns f; SSEpheicoonmse,ny" (IMmetnohrEToS.8-d4.1)wis the modicutBooants i PThoeana alytical l phasCewoils lbecFonRductedunderEPATSCAGoodLaborsicry || 2 "TRhEefFoEllRoEwNinCgEanaMlAytTicEaRlsItAanLdardwillbeused: I } Pury (%) ros {rcwoonas | w9 |am | ` ii ChPCehRmeOimScicaa Naammee:1d cur of he compoundisprs Peflsoroosanessfonste elo. TUPACName: 1. Ocunculonc Att1..2233445.5661788. ||i CMoAlSeNcuumlbeeWre.ight H34e3p9t5aCde.3caFllou0or)spossi sh i i i Cong !| | Mot: The net molecule snd sundad frm which the PFOS (anion) is i| weoibtgahinesd3.is perorooctancsulions. potassium alt [CiFSOK), malecsar i oAf cwoidwoiflltebteanmdineienend ssutbsCtoannceerecAipM,sYtsLacboorsntoddei,asdoncFsra,mt CenteAnyi Liber,bo. Pesos i Exygen Research Page66.09% GLEE Exygen Study No: 023.066 Centr Proc No. O1P023066 sduobsctuamnceenswiinllcbheininocfl<uduesdo8d5pyrt1do.ftshheiupiwndgaraepcaocrdksagfeo,r aching of the test { "Al nisetanbdearodfneutmsubbesrtaoncehseacoodntnayinperreoparreodssoelfuteieonncsmeuds1ttbendcoimeaditwitha. : i i| HcAZeAnRDNINDFSORfoMAtTeIOhN owid)hs testing fay. dywil bemine | i 5 sronsor ii 3BuMilEdnivnigr2o3n5me.n0t5al Technologyand Safty Services POBox 331 | Spal, MNSS132:3831 : i:i R`TFoSEAcpLoXhnEseNPosUrHMORReNBpoErEed:Rsee:n4nt86a1t5i-1v7e77:58--76016756 |!|} 4. Ti8l5E5dS8iTfCIeoNImGnmFeeArrCtIDLorIinvTseYLla, i Easton,MD 21601 || SSSTeEUDnSYcEDaIRrECTO0R: 5600 FAXNUMBER: $10-72.0652 | 5 PERFORMING LABORATORY i | | feSiunstteeoCoAmlnleaelgiyet,yiPctaAloLy1a6b6o0r1trics, Ic. (Cen) i:i pETmEiaLlEyrR.OaSNuEap:fvere,sSCTieeonATo8R03:2 i i FAXNUMBER: 814251158 i PROPOSED EXPERIMTEIVNE TRAAVLE: i A`RAennpsaolyrytttlicaclasuSTeiedamriDnaaei:on Date "ApArpiil 220,,22000010 May 31,200 CentsAnyaLane,Tn Psat i Exygen Research Page 670198 Exygen Study No. 023.066 Cente Procol No. O1P023066 TT 7. JUSTIFICATIONFORTHE SELECTION OFTHE TEST SYSTEM i wrMielprlaebseenultaswniedlldqduaabsiaildethdrepoapaludlloyadtticcoalnlsssasanadmmppelleeyssacofeloErletPchtAiesdrpebhcyaosWme.miednMdeeIadnrlsmpaeltcaiieoensndarbleq,dcLuuiasdsl.e ;] i thgreaasyesrdyso.rowaedMsliadielnsa,adfaabamoblratinoedrssy aeinnnvdciolrupodneemnepnowtno.dosdQ,lualniidlkse,hsanabndidathmeiaynrscahrleusc,obnuassnihddyephreaedsyteawsne,d i?i |i; dcfeoetneasimrdioenSree.disfqPuFaOlSlgwaasedrespo.siTthedewfntehoefwhtahleesbelmoatoidcoefsmfatoirngthdesltsudtyhwaiwsetroe |: : i| A4is54cd-oo1mtc0pu5lmetetanentddei edQsucairinilptMPiarolonltoaofrctodhloePtNrooiet.toc4osSloy4sfDNtbIoe.OmSl40o50n4sQg/,P0Iw1iS0tU6hB0Aa0lSMlSPo,fItSPUhrBojAneSci#t,fNoP.prao4jre5acm4te-t1Ne0or5.s ; | No processing wbierelquilred oetheany of thesamples. | i Ewwahicilhcbhsewasmioplrlebedeiwisnlel dbeemopraesstaiatgcnrkeeidngmaoannniidtqoiurdeeendstiaffmripcelaeetri,oindomefnaiitfncetaatsiiaonmnepaldsteus<.b1e0TrheaC,sCaeemxnpctlerep,st }i : wsahmepnlersewmoviebde fkloeptesxltaratcetdiofnronmdt.heanaelsytssisuabsdeescurriibnedg siinoathgee.mehod. The |! Sdwoaicmtuphmlaeenutnreiedcqe.uieptLAlaalenldsoarmsptsolareamsgpelnedloncuaamntbyoenrr.essunSldtuiccnhognidsdiatemiapoilnfesceadxiuoarincntwgsiltlwhiebllestbeaietdhyderewoiilflitebhdee i conseror cosreferenced 0tecontains. 3 | 5. ANALYTICALMETHOD i AOfl sPaomtpalsessiuimlPebselsnoaryozocetdanaescllocnatoteontOretaOntiahleynrtegFslsomrcheentictealdhC"oEmxoptrocudinodns ; mFertohmodSeurmubmeFroErTSA-na8l.y4s.i1s) wUistihngheHPfLolCl-oEwliencgrmoosdpirfaiyca/tMiaosns: Spectrometry" (BM. !i { | s1t.ocTk,hefroretwifiilclatbioen,naondsucamloibgraattisotnasntdaanrddaurdssewdiillntbehepreexptarraectdiaosn fporlolcoewdsu:re, The i| PrSstenoplcaykrieSaoaltusttoiaconnksdlru(icoonmoecfePdEfOoSapetrc1e0nt0sulg/nLdbpyrweetighpiunrgtoy,utA1d0jo0stmgfooafl ii volume 10100 ml with ethan! in 8 100-mL. volumetric lk. Scr this Coote Anyi Labtec Presson ! Exygen Research Page 68.0198 CHR Exygen Study No: 023.066 Con ProcNea OP 75066 oocisupoon(di o1f265mmo,rLsDfPrEobole)eofeefpigseornor12 0 6C Fors | P-- r || a LlOauatgn/onm.laForti3fic1a0t0ionSoluvtoilonum-ePispettesk1.0mBLionfgthuep 1100pegs/amLsstwocikh }I | i b. 0fV.1ooriuhgea/wsmoilrhFaeorttiifoilcnatiioniSo3lu1ti0on0~.Pivpoetltuem1e0s.0 TmsLkoafndtheri1n.g0 pogp/m1l0 ii {0.o0n1uig/cml.oFotniifoicnati1osnSo+lu1ti0on0.~Piv pette 10o .0TmsLkofu 1t0he600.01s pogp/mL. | `volume with methanol |;| eC Stiorge lelng fx8iiaiCo1n6sanfdor smlsstiicns Gnpe125omfL6DPoEnbofio)mfnhea \|: | L i FCeailgbiburraptsiaxolnL.StOaMndSa0rI0dS1s cflbarailoonnishtcannidoanrdsslinummv.anol via dion of bf i fThiisoi pial example; airs concencaions maybe prepared 8 |j| CoSoir r) Vl5 2 I0eol 1 Fe CaosGat. ow i |! 0oa0o11r 5:i 11i0% S0Ga0no0tos i dor i 1% Gooor ! tStoofgrepe1prascra1lii2or5inontosnCfdorsmoairnis Gnp1o2d5i,fLDmPE botr)ominhea { |i! 5. Tm7h3oe5usnatmspofolde0vi3oumlNcEuTumObefoAonraatiicedhraoeddmebtosinadpmcpoellewislabmbpeelers3wmidileladbdewi1lh0e0be11.u0nmTthLoef i i | The spe will oble yrd wit 02 pon ih lIefseces } 4.The samples will beanlundyer hoeFoellowding condions CenteAnsys! LabortcicIsc,. Exyen Research Page6er20 | Page 090198 601% 7s Exygen Study No.: 023-066 \ Cente Proce No. 01P023.065 LCMS/MS SysndOtpereatimng Conditions (Turbelonspray) i Mass Spes: PE SCIEXAPI3000 BiomolMeascsAunlalayzrer ; Ioecfics: ~~SHCarIvEaXrTduirnbfoulsioonn pSpurmapyLiquidInodacionncfce :i } Computer. Dell UtraSean P1110 ! i Software: PWEinSdcoiwesxNAnTsys LL t |!; HPLC: HewlettHHPPPacQVkuaaacrtduPu(umHPmD)peSgearsiseesr1100 HHPP ACvoolsuammnpOlveern { | HCnPjoLelcuCtmCononTlVeoommlpa:.:1Ge03n15e.siCsCy (JonesChromatography),2. mm x 50mm, 4 :} MMoobbiilleePPhhassee (8A)):: M2emthMaA nol mmAceloateinnASi TMtyu peIwmer i i FlowRae: 03 ml/min ! :iii Ti00m. e00%@A %aB Wo iw } {] is 060 44 i | i1nsmtaryumbeent npeecrefsosramrayncteo.adjCuonltutmhnesHEwiLthCgdrfalderieenntt diinmoenrsieonoso(p0ti.mi2ze BGmbmaiiunxed.3C0amem)) ainnd be a columns provid svn cmogghy from different manufacturers (Keystone i i Tons honored: Agprosimae || AnFalOvSie neMgomdieve Transit4i9on9M3o9n9itored wo RetentionTime(min) i ! Ohnebaudchaofymo-bibltaespiohsa,ts-he,eirdet.eantiyon timesmayvaryslightlydepending on ConeAnalytical abort,ne. Exygen Research Pue7orzs Page 70098 GOS Exygen Study No. 023.066 ContreProc No. O1POZ3065 \ iEThxeanmfpsolllecoTwu0iunngnemsvFiaeeliuuemenPseanatrtr.aempeArltooev,ridsheedsavnloeexmamapyleb Acchtaunaglevdaflruoesm mGaeyvtaoyifroimn ordrto optimizeforgressiy. : i O"Tcicseutnhee repested fnleumstaen s 1 cesar to endeudribneg rooputtiinmeiaednpyarsa.meTh evar optimalseni. Gainagvpdr1 o caeemdauIyroee `I! | Tune Fl Parameters ! i } DP DecClSuo-sdnorsoiplnrgasyPotential 4s2st0et0o0 i FECPEP.-FECooncluahssciontng PPBotnoecnctgiyaal 21%0000 i { CX-CallsDiFoDneCfilecEoxirt Potential 30300 I{ ! (CEM.Channel Electron Maliplier 2000 t ! NeGbausliFzleormGs s sa1 i ] TCSCaloTlrseiimonnpGGeaasrss 1` 0c i|i Calibraa."don PsrtjoacenedtdaurrtdheesrseupmueevdolinuMmee(OcHt)weinsnt1he0L0O2M0S1A)ASofexch calibration i! b sUtiandlardncutrvnewseaieghegdesnceafor ean chfscetodmbytToiie naornpreLsotoen |! i[ funllgngtohuaipAdi perop3r0i%,sobfear wsaerdeosnCiys.calcrAlniyedecaciobprnaconersnn,aermeCasyA ; oofftcrltuaalnamsbaendrufdsstahantdmarybmeeteexcdl.uded stntenced 20% !: ii i TJmuhisemtsh,coetmh2ee0lna9si9op2np5rc(oo4er2fs0f9ei8ci5se)cn.tps(I9Fh)cuaflbobdrebacetailoitbnarkeaetniso1nlcafulrolvteostsgiecnrertahtteesde ; opesion,and he elevantstofsamplesmustbereamed. i (Cees AnalyticalLaboratories,Inc. Exygen Research Page Bor | Page 710f98 CaruNg Exygen Study No.: 023-066 ContreProc No. 01P0Z3.065 . oSIfunspjclhethsAanmsapallmyese,ifsvoorlfuimaeiufsono,rctomhoe, atcl. antionthestLaOndMaSrdIsM(Se,wEeaecnhs1u0m0p.l2e0muLs)t i beamyaedin duplica. : |! 5. Sundards comeponding to a least six concentrations ust be includedinananalyticsaetl. : i | b. Iiinnnjjeeectetiaosnntesannmdtuaisrrdtesbseiebntotefrasstpaerncsdeadsbrkydhssott(tasnixdoe)avreadtryrthjSec1bi0eogsnian.nmipnlge.ofAthle rsuunpalnde 3 |;i Gachcoonneolree,tagoefnntsdacmtopnwlteooslma(anacnliiyrxctc(oononttsoollvxseacrmsepealdne2ys)), afusotJreinsictluodaneeJaToeoaswxtn |i E`conacesnetcrmatuhisotnsalasnodncacrreied athsrotughonteheeptrhoacneodlubreantocavenrdifymreecAovSerTyA. ; | "Type 1 HzO blank. |] 4 dTenhcerlmiccnomecsaelnfrsoattmaotnndearodsfsaicdnaajcchiedscadumuprrlieen,bgasfercditc.otTnihtohens,apnckdomao,nspcooifnct.shees !|i hmnueescsbeaasnc,kddcirotevsetprhoansgasemopfletsh4ee2r-esaidnueyfozun1ed0 ginithvee ssapmopnlseesewinIf . Forificaion recovers within 80 to 120% are csepable for i anfLo0drtQai.ficuFaltieoanslrayttotmhoeeoLftOthhQesef(c1e0trengde/smaLrm)epqaulinerde.satanleivveelss ggreaaitenrotfhcanoutshee : ! SeVaiAmepnClieopsneismnkewahsriecwhdilnelosbpeeearkefspheoarcrteoedmet4s3cpiNoeDd.nda(tniottnhedmceotlmeecestpeadentdcSionagomnpaemmsletisen i!! But re ls han te responofth lowest andar (60001 py) willbereported as NQ(not quantifiable). i & Bcaocikmgsrpoounndd1levvaellssobfelaonwatlhye LfOoGu,nbitn rcsonivlollbqluaankntsiamlpelweisllthbaet | used to correct fortification recoveries. i| a2scCa0mi6prlaeCeanr,iolsatamonpalaedlsymauonsndtthsebnelnytssroeurdmeepnerttee0irgsbeleysaenwdyiB.ts4hptpehioeerkndi.amyALhCelyy CentsAnyaLabor Exygen Research Pesan Page 720198 GALT Exygen Study No: 023.066 Contr Proc No, 017.023.066 10. EXPERIMENTAL DESIGN | ) CxASpanemctptlieecsdanbLieinboedsttoybiysr,WilIndhcl.itfwoeoruIlandermfaalboe.nalTheLeirdle.srwielolfniobeknsohdiwyps.pecdco1tumCiennatnes : :i OnCelnyttehossceosraimnplgetsodemstihgenadt,ed"bEyxctahceioSnpOonfsoPrawislsiboenexPteradcotredoaunidaanneaslyozoendsaet i |1i mEOolrdciOtftoihscephrirFoalnyusMoiarioecsdheSmiipceSacelucodCmooemnipr,yo"un(dsOMFrmoemthSoedrummamFboerrAnEalTySs.i8s4U.s1ingwiHsPLhCe ! |] Mfaerntihycotsdisoontfo ofcfoournnitcioeclsdtbeiadsmscpolvneitlsoll 1isnacmlppurldoeevsida1essaamyvniaofinndruisncoaevtesorreydodfcaoyenrpaodleucseaimppileyese,, | i F1toeriLtf0iecQsatd0iofnsehweoilnvleebehsmeubhasitgeahnectset heimdatei wll be osupppnrlidi.eTdh1e0exhtorecacctdiaeonsitgnsleetvdelossnrauncgeoinignfviioanmg3 ;| !| sHacnrlo.n syringe, micropipete,ps or cquvint, 0 mani conten and i; "beTenhclviceuortngeyed,rbeecTFoxvnceceassnadryor,emalpiphvleey aasannuddaiardevisisayttfsioo.nolfcAhsle.of1hoeraadnvosenaigmerplrexaiwidielsdl i ound ndsteaddeviiofosshmats illcule. i "ETnhifoolnlo:win cquaions will be fosthe elation. ii| Any found (g/mL) =Bcsacnaci el ;i || Equation 2: Anite ound unt) = Wie Lam AfVoun(dnolyu/nalmXpFYv(lmLG)xLDE XEV(nl)L1u0g0m }i i|| PDVFE=DiFilnoailoVnoFlaucmteor EV = Bxacion Volume | AV Alu Volume EFqourastaimopnl'estoocialeliwihthekpneorcwenntscmouwrtyo.fPFOS pro exact, we ConteArptLibris, Exygen Research Fae100129 ; Page T3of98 Goren Bxygen Study No. 023066 Conte PNr o0802e 5086 `Equation 3: i| . Cn Tod Recovery (%)= (nL) sev,n inct Gm) (1000031 pg) x 100 ; iL PROTOCOL AMENDMENTSANDDEVIATIONS f i}iJ 1SARntyeddeoeveoinamti,eoindsnfPgrwhodomsntenhTderpmmreeoetsgocesorlnoorfsmrnopdmpsttoh.eepbaneealyitbiychalaiemeDBtAhoAcdaspnrpootvidSennd twill ! | ioSntsywDiileen,pe1nddedteh sSproorcRengd ent. p oy vms i|i 1.IPSCrrhHeoetomrh oecmonltdaemaaeanbvndymewmenpnigtusrla:tse nPotolSaenndysseadtdbcaahr arAnygsersde trnoodctSheepm oaiBpoeprSreohFveedtghpreraoottoacnonnldcssheanlel bbdre i i! 2. PrG1rohtoiotcionlrndesvooiifamotinhoren.sG:oqPoruoetisolnco,lhdpBaevloilaebtntiod nsoc,wlheio ascohafremsopnt ectn iomeaent tdrsunalpylawnoninenkdg | tPaonwnead bIy AnLca, Sudy Decor, nd Shomer Repescasine i | 12. RECORDS RReSceoornsdsaltovbienmgaihntoitne)d include, but are not limited the following (ss !!i} 2Sample rds rage istry, ndchofistnd | i 34&L.HDhiistooreyAiandpfkryeerpsmdairnopfcasntttaoniidnaosrsdnsote(stotcnrk,ofnortification, calibration) 4!I 5. A hromorahic nd seal oni || Scpoemc p Tsmaiofeni adg pensos, garndnel i 10. Chronologicaasl pmresenytationoorfe allstudycorree spondence iy { Al chromsogams wil coin he following i ---- Pee i Egon Research Page 40158 G01LHE Exygen Study No.: 023-066 ConePots No 01P73068 +. 5. iSAdandmeipsolne,aladlneydn,ujfiTocoariinofnc,aniuodmntbs,erwcialmoonnaeodrseobpheoreothinfneodiiircfanucniaoinonofltehveel aofethoef 1 c aAnmaliyytei.cl sundud_chommogums wil adiionally include the ; i `concentration (.g., pg/ml, ng/mL, ppb, ppt, etc.). + | pEaxrcahmdeatetrass, geaswesi,llinsctornutmaeinnt iparanmetferso,oanrnditnmesmtpareurmatetnutrietsyp,oef,lenotw.rats,column |: I. QUALITY ASSURANCE i em Co a Gl ee ty pn, 81 OL ;i edoncuemenQiAaiUonntGawcilludviingewrowhedaptrsta4codl,fsluitrteeprs)t1ycscoart ahntd taelsOuLdSy iii ParsisnucriepaclomInpvleisatnigcaetotro, CGeLnPt'rse,Maannadgweimlelnrte,paonrtdtthheeSftiunddyingDsireocftotrh.e audits to the 14 | 14. DATA AND REPORT + 1. AfIlallborrTwthodsyaandoatatenabdooitknhsce,lguadenosalltyhteessigpnsrenoddcpaorrlotdoacsomleonwodimlolenbptesr,ierpioaed,lminpdteciensihoanyse, ; ionnfdcansyyttlee.rshTshepe,rresaasimopnnleodrwscrgkiesnoercdtw,.ilclRodaowodvmomopto,dv.iecduwrialtboensceurdv ii | 2.fAerpeprroceoSwnpiloelnsbseosrhfRoeeupddrisbnyecCtldaeeveebu,t42op0ptrsmoovfiefdeintdfosignme obyotneS1i0udEyPiA.coThne :| 23. AORenbfleyiriecee]maadadpiisnreetonmeestcdhaobdddsvncaehdeprort stp!y, ndath } 45. NSAaihmmoafepepnrfeoprmeinsgnIdabsoirgtnoerdybsyndhesnlaytliyclssaatraedetvcorninaton dics: I i! 657.. TAclaolblmcephsrlocemoattnosgnriianpgnhaoiglcfCasnpdeplioensatsbreucymaenttpaalrcoondmitions 1 CRmeeanptkreiewniitsliilonengsn,dawhnaocfowilyloirftathehebpdeoarrttwerpietpotwritetthosctophmevmeaSnlttuosfy.DhCieerneStcaetoyAmaDnaedlcSipooernswsnioldlr ; Sponsor Repescuive. The Cenue QA ut will ont an So ofBe fv draft report and raw data package to assure accuracy and GLP compliance. The i [Ey ---- Pag 120120 i Exygen Research Page 75.09% [GEEEE! Een Sy Nos 073006 co toms O SireTT prt7 fTeo rr -- Snr ; E feTaGpei pp an mttyn | | pe od ey co ee thepartofthefinalreportthatisbeingcorrectedand the justificationfor I Investigator, Study Director nd Sponsor Representative. t i raZ SonrsT i o,ne ! i |! 15. SS SStARrhCyHsIVe eEntSyeTArs mTEMEtNi TeR sfHSoemo ahnmwis dteyo wydycry oiienn || |: oISmmtetidFeyind dfoers iennm T t mn s rl ds Documentarchives: Upon completionofthe study, the study records, protocol and i| 1.fhenafinralmrnepcoret nsd awdaapackage. }i i 1 US. Environmental Protection Agency. Toxic SubstancesControl GoodLaboratory Practice Standards. Final Ru40lCFeRPa,rt 792. Act (TSCA). i { | ; CentreAnalytical LaboratoriIensc,. FI Page 13029 + rh 0x Exyaen Study No: 023.066 ConePrNo.o01702t3068 17. PROTOCOLAPPROVAL. | Thfispriotocaol was audited bythe Quality AssuranceUnit ofCentreAnalytical | QultyAssurance Reviewer, Cire i i i | QUI Assurance Auditor : ls [1 i Principal avestgator,Centre | | | Scent | llr ; = : FacltyManager, Centre Hho ali] i OperationsManager Poly "e . | StudyDirector,Wilde InternationalLid. } / oo . nnn =dslet i|| Sponsor wes i CT Aes i ~Efironmental Tekhnologist ConeAyiaLabora nc. Psat : Exyeen Research Page 770198 G0OLnAG Exygen Study No. 023.066 Cent PrNoo.01cP023e066 i APPA.EN"CDoImEXp:oxuAnaNdAsocLFfYrtoTomsiIsCSoieAorLnmumMPEorTeAnHafOlylDsiss UosirngoHPoLsCoEraOltnhoeeorFssoplrcrbfhuienysssiatl Spectomeny" i! }' i| | } i || i i Cone Ania LarnIe. Exygen Research i| Page 150029 i Page 78 0f 98 6RLE HY Exygen Study No: 023066 BEST COPY AVAILABLE CootePr NoOpo a 0, _ 5) ; { :! T{ R ae wt ; ' MErmowmusLlsouey b ; FNgp ! ;i C7 7 ExeiracpnonoapaPcooTsuammssotiohmumsPeEmRmoIeoLnUSORctiOOnCTmerAoNEASraUrLaIOvNcaA voimOTmH,EaRp. | slBe ; FR i | Fe ) mommy - Reei, 4579) 7 Amoi ~ . ! 0 vyVD ag 5 ME Ny firs . i: wiYiLe 1 >tPoSuronna, ||| aPfa)l faidi,& s ;|| : A. i| 113 13 MI AinT rtie:cRh i ornetee e r ee n tr ete rr eet i J Joes r| emane Juyo ! CentreAnalyticalLaboratories,Inc. EygenResearch Page 16.029 Page 90198 conn BESTCOPYAVAILABLE Exygen Study No: 023066 ConeBrNao.00e3.0t66 R CheH UcR hai BRale aie . . a re i 2 20 sania ' ' re Thismethoddescribestheprocedureforextractingpots i prima bia ;} A on, ATER i Ani Se EE | Eisen re | 4 3 705pent fie 75 . t i "32. 33 EpPrRoORsSaAS ;A petroonct nullesGcFh,yScONtE,sCFSONCHCRYTHCO; {i OQ,2365 IshOeLcoAaiscoxut CICots ones|o e&r,e goSOHCR 37 Suo andga:1a H-1Ht -2H-e 2H, Seria | sma || a7 Somcmmtcnanimoni F= S ; i LI Uskudversalprecesions,especialy borsoeycous, goggles,a loves .& i ; 550noT mazminh gy teme more = E3E.N i;i : | SE e e-- ed 127 VCeonrte Vamriineas . | OD 63 Semen i me mtn CeatreAnalyticalLaboratories, Inc. ExygenResearch . Page 17029 b Page 80.0108 CO1539 BEST COPY AVAILABLE * . ere `Exygen Study No.: 023-066 CentreProtocol No.01P-023-066 - | Ee EE ae SRT CE : i 9 B5E B-- umeaing L 2 = ! {mn pr | -- 17Bite pie { 73 Ach capae ofbib og25e 0mLs, d11. | Sia i 74 i Bus,gh, 0 A. i n ;! : E 7L % Y a nly7 ese,15ml. : ii | 5 ree i ]i 7 Gata f i 7TH2 SSe y Snrpiile i 30n 3 i i. OiI cTimmeerpsiritntoAn eT7P. a | 5ete Pf iomsps ir gRirMoers t ssesyri cneT sN 8Beet ei nges: re k !{i a 55 54 ST too1om,E cyote eee wCateOer,n 1ga 1r .aBlr`ore i rirKotlo rveteeveEvisi s e1)ra !|i i : 55 86 atm oa (UHCO)17Bt rpieest Moly Bey trOnl, doled PLCpds "abSED, ho |i ii 72 PSMeeleoa,Onnnuceotmgbasrsadni,ieocHPLCpd :`: .& i i J J "83.1 53 PPFEOSSAGOMMSpSepceicalitaylyhCeemlrectaDDiviivsiisoi)om,eaclsrwewiegihgtht 538. 499 i a t | St bse me ; CenteAnyaLarneI. Pagethar i Exygen Research Page 81 of 98 annin BESTCOPY AVAILABLE ~ Exyeen Study No:023.066 ConPio pois sd i Dn ai il EET i ; 0 19834. ErROoSA OMSpeiltayCyocmeidceDin ciewig (FN 123 PROSEGMSpec }i ;i F19S 6 [(Pi77osS R nsmspam p yi ComrmCim oamDivaoieea v,ismmeeoeta* ewn rei5t7a3731 i i;| ; S0| 0 S g oE a e i e tc e ns T o ie pwc ir e e i Hig g =e.r ! || r 0 E INSEe RT 0E DsD e ANI110eO Moet0tN o cro i! o |I E T EE E m ie rRem aatee pe i 0 810305M rlfate(TBA): Weigh approximate eE stTt piioatnet srCeeTyyccorocotrseten, aeevse |!;| | 1 SiusipD mF preb ee(Up1iao 6tHm.Ctn)T oee firusode1s t1ocluvboohe tyremsaeost(0i0,k0,15tbaei5dn~g14~5voehfcsco :;} 1I 13 Whriot amg 508sPm emi EhEr. | E114B thoschalweightifoo cksitetok penly 1o 000p Bn i| !: Q fy 8115Dileethe stocksolutionwithmethofor working standard | olwion'af pi 11.6Dit sie vit tbefrvoi init sf. . DL ean in pts . Cte iets,be J. | Exygen Research Pige82018 CondL Exygen Study No: 023-066 BEST COPY AVAILABLE Cent ProtocolNo 1POZ3.066 i: a SUREEETE | 03777 S51 nStfeorriesgivdanerepdritin;tfrwin et tet |f Fo Cv i rept sint 12038. | ; LEAC R: p -- orEe te ey i | Fe opie wtessSi mtTes oetS er T-- . i} 9513 NAlhsseogl ierBe imcdo mep ttofrs ciln.b is en !i i 1a01 oSuonldBk 4H moiSs ii B 10101121ABnt e 00 n saVPc voetli* Seprs : 1--01 --m gateE sten d $ssd r ions |i 11003213 PDrPeaperscn dhi it egigepieeedet byflttSy EcnR mr :i ii 110022p43PEa xepeectotedncoamnnrsuiioneswl mnaS ieiieceiopf oOivfiiSnI01Nave. ||: . 103 Cotirn in brainchy es 0 Ft 1031 tperFigei n gesdkmkit eeerresy ati i|| 11002939 Pyr t imi,gciniho ick ecpeo iOesai,s BC : i 0 Se bi ; 2 5 tnErsadt tem sae : HE et he 2 ConeAnyi Laon,I. Poa || Exygen Research Page 3019 oan Exygen Study No.: 023-066 SE i A LNT EL i 0 103S4TS o pEdE cRcnaR vieit E ge i; ee Wr Set iomn LE - i 15, APS fiip2eM moattE escsnatbn setE smasesaare.s mct onaneielry ie ; 1 1143 Per to so cishs i i 11.04 Two 1 outer spoir,sep ve1 etict sks, | { fiemI re |! ight sadars, Saibank, odtomethodblk. . DO He tm a ee Seeu G EmEb i rm yt S E pe e Te e<i mt n r, y ; i 113 Extractspikedmatixstandardsfollowing 1261216 FratbodUsethesesundaes i | ; Qa, . | i :: AGon > - Dell = ote itLin oo i e3en -- yg Reach se stcrsn on BESTCOPY AVAILABLE Exygen Study No: 023.066 -- ee CornBrNo.OoUP t0N6 | __ : st nieondgtn SN NOE. : :| S 0 e ee Sl5 in TOP { |; = Aertel serirteit Sr !!f i [re i Esmee svar] | E 7) ee e | i | i en | o LEE NE cr ae ree . 122 13 e eVrersmk1r etsfdo reseh m51 et erStAse fr rr i 125 LS ie teviR ggt I e Aree i. Sct | 156. Spt earns nn ihoe ref i 17 Secuvis LER pistsdTeCSe tnTbe |{ 128 125" VCr orommixiee esagnet8a caTvOesAppe,tmatics1pklmkpl,so cotnosgiT. E i! j 110 TTeaome asintml025 moms ton |!i O5511221Ca Vping OtpttrDipsp e3keLtmiegs0ae th enens . | L mein rr ConsAnyi Listes, fae i Exygen Research Page 85.098 GOL BEST COPY AVAILABLE Exygen Study No.: 023-066 or A DES ree ; Oh ti 5 csienti IA15E Remove407mlr ofheara ai yertotisecme 1o 5mi tief n ben. s | ! | | p eL r n s eo e fcy it teshst s ts, e sceme i - ra | i! 111252 0CSlECeCearer cme oemietotnaeatsPenetyenorenmsy }| ! HBaL ErmeisrGsLPFOS, oar rplsicablesams : !| o rm a |i1 I re re Br BS el l 41 o ThemM ethoe ddetecm tionig it(Mo DL)rsam tsoTr d ioio sTse2m lf.Rs _ efere toMDc Lrepor rt + !i | F 1MEeaedsS mies versie FNgh t ; 23 eete e trefuses, ! 13RetrbeinJolETS 31 ormodpte ie || re LE f! L0 B Ea e ross pet : mn ti : Coe iarr, Expo Research [A -- Chui; Exysen Study No: 023066 BEST COPY AVAILABLE commpoccirocinoss i La. . i Dan4cS o m : ey :v ; i 10% er i FA A Collationtani ocewaebns: | wa | w[i e En e i | ESE | 0 1 im mT mm RTa : Es i EER 1 i Loo "i OO @ : : ,. } he Lo Si fe CentreAnalyticalLaboratories, Inc. Exysen Reseach Page240129 i Page 70098 CRED EaSyayNgo:e023n066 BEST COPY AVAILABLE . Corpor oP | f3i 2 RS AREALpl Si E : : Ee EEE EEE ! NE 1 ---- Eee i a s _-- r tf r --+-- -- |:|! i = esr | 0e E t t E a e e t e ! F a p | e --_-- sa r: i| EEee :| ii -- Cary, eRe TuA} ib Er_-- -- ---- {| EEa e = i O . i sm me ap i CenireAnalytical Laboratories,In. Page250f29 ! Exygen Research | Page 88 of 98 Gonna BEST COPAYVAILABLE Exygen Study No. 023-066 Con PrNoo 01702t306. | Bae Lie, eg r NbELm i i QO MD mietor G tar ; i 5 OM)| (om |Appt eseraog 0 ewe prepa ae ! Em poop ! Ee ey ESemma e I e re me } [M61760s Toa[ppb toooph | { PeLQsry MDE ly BT 4.401850 rf msi. hy i i 0 , E viii, mE mei ~ TARR Se : Centre AnalyticalLaboratories,Inc. Page260129 i ExyeenReseach Page89098 CARDS [---- BEST COPY AVAILABLE dota... SER oh deel LT 1 07 coin T: E 5h i F mp| 6 ' i! i [ft [or[wom|om|o| EEEts | i EEE = i [oon m | ong |wer] Composst: rrosl 2, ; --_-- i CE ro em : 0 E Ee TeS te Ty i [ome on |ion ron ; f pose Fre fam) ! 2 i ! } Ea i ACA me eae -- x. ---- ns -- Stat ---- = CentreAmalyticalLaboratories, nc. Page 27029 } . rass0ct58 TC crazan Exygen Study No.: 023-066 PY AVAILABLE BESTco CentreProtocol No. 01P-023-066 :i E Eg NR g wl og i: ! Donne ) ; ; r[i858 lom FonE ||E | x] CE=rerr TErerermTe] : | (oaoon ow] : :| ERE eS --. a . i j ! O [fIi[ BEme[oormnnm [Laabwnoiwap[lgen hgwn| |on|| (o vnfom m ow| [C FEEe [LF] ;! E [[rFreerr ees[eormme osp eemi||r ewow[ [ew|d|y By . i :: i } Oo 3 wi i . - Amada B: MDLLOQSummary Se tes Thee | cms an Exygen Research Page 91of 98 GLa ST COPY AVAILABL Exygen Study No: 023.066 Corr rotcaNo,01P023066_ || fFeES A e gS adl SesRBLe IEREAR Lg : . | i 0 | tmaadi Fh |* J: TonPteStSaanCntardsvoeitr rtds Pemetree: . i i f wm i EC mind pr. 0.300ppm: i SReAndRai . i trades 0madards1adeFCsts . i || F Fe ere ia traa r a e a saeTar) i 0 Ere ee BErbaratars] : Clete contrat a santasts Sais |;i E E Ea es r rae ee ee Bee > f C R apaL ] 4 D : ii ii E E e T-- ---- -- ) chem Contre Anyi) Lastories,c Exygen Research ois ; Pager i Page 92198 GOLE0L Exygen Study No: 023.066 CAN Centre Analytical 50 Rfro Dr,SeClg PLALOaL.borPeant0o1r0ier1s0e,000I51n5,c5. ii PROTOCOL AMENDMENT Perot] } |i | EAfmfeecntdimveeDnatteN:um0b7e2c7:0011 i Centre StudyNumber:023.066 CentreProtocol Number:1-02-06 DESCROFAIMEPNDTEDISECOTINON 1 87: ustcaton fortheSelectionofthe TestSystem i i AMENDEDTO Changethefi semence read: i i MTnatlelmaaridoannadl,qLuidi.rweidlbblooadecdeslsnhedansaelyrtaicsalleempslcolfloectedisbyphWasiel. de RATIONALE 1. Ath requestofthsponsor, llseusamplesar beanalyzedwiththissty. i PAONTC HE STT UDY M Al, ONA, Std Dict Signature Dae Ae ! a ---- i| S-- pomsZsperdicnaZivSiignanturees ES por |i i CenQAtURervieew, Lhe fFaryur FLT Exygen Research Page 930198 GOLB: Exygen Sudy No: 023066 ; Exygen., ark. :i PROTOCOL AMENDMENT Fe 39 j| | \ ---- AmendmTeent Number S2 m ------ er EE i ; i| surg DESCROIFPAMTENIDEODN SECTION {| 1. Tethoukd redExitractieonofPete sFee mot ctanen fonate romRedBloodCl i: | 2.Soroepochbs JtNewt, En, (517) 21.1404, ! er Genter smekrN g RATIONALE" ! i| \ 2. Nonemive npc nso EEACTOSTUEY ; i | E hDeTer sA as Thooie T i = -- t =e e || i| [Jidte apsad" S=vlstos | tho ---- ! Soon cnt eon LTSfiles Exygen Research Neos gBnr, i Pageos ots ents Exygen Study No. 023.066 e2Drs eSi Cop PCLATeaO.nbtorrhaent1oAnr1aile0 yst,i1 cInacl. | > :i PROTDeOviCatOioLn NDumEbVerI:A1TION i ) : DreofOccurs: (12052301, 052401 ! ! ConteSty Number, 023.068 Centr retoolNumber: 01.023066 ! | ERRGFEOTR j 1i.c49oAnnyeineMceotnt,rmSiclneswAinyeise QhunaitodfCennsun e010726S1 ededtpc | i FECentresample010757 SpkA2inSe 052201. ---- {").J | | 1,12Ari Vet,eeArs QtCn apes1707 1734 ii 1i pry 2ndtheirduplicateinjectionswhentheconcentrationsweregreaterthan thatofthehigheststandard in +; JR 13. Prot dinioniowet. eect Bou rene : | 15. No egies ca GTO TET iesvee < 5% ren igh snd | 2. JNoeomite mtpcbc eave aves allof efi were withinte } fi5 gTde uke ele i1 5 i-s SmJ Be<alox ! 5 r2in Se To 54 $7"03 ! `CALQAUReview MCL, Qfyglee a i "WSisigdendagtiiGodaLebiaa(f6ictoowd dfot 5ua7edd Bes ofthe i| Exygen Research Page 950198 onLu Exyaen Sudy No. 023.066 CAN Centre Analytical 50Relhe Dr StColl FLATa,borPa01tordia ePast,t 10-I5n1 c. | | PROTDOiCoOnL uDmEbVerIA7TION |i . * `DateofOccurrence: (1)S/18/01 i { Potrt | ; TONG BEVIN CentreStudy Number: 023-066 CentreProtocol Number: 01P-023-066 ! |i od13Gi0emrnoeg 00a5gOelLhooymews0dCog ne1rorihs ni, | JTR OS . }| ACTGTRE TOT Recorded By/Date: --_-- } 1. Mo epive patbce hestlvlanwas edin clans. lls | }i ZARtrD rTe Bsaregs i: i SodAisc,iSi.gTe d. Biecola || Mi Be i : CALQA Review, PRY om ; !{ YhSispat okt galsofanly(e-id dueto Sus#pected (05s of } : 0@4 dla : : Expgen Research i Page960798 GRA: Exygen Study No. 023.066 Centre Analytical 508RaecDre,St Coll PLALa.borPoanst41o02r08i0 Feuse.010I91n1c25. | PROTDeOvCiaOioLn NDeEeVrI:A3TION i| |} DateofOccomence: (1772301 { Centre Sady Numer: 023.066 CentreProtocolNumber: 01P.023.065 i i DESCRIPTIONOFDEVIATION 1. 9AnayicalMethod,3. aSadmp0l1e07v2o0l9umweesruesd005ormCL.ente samples 107155, 0107167, 0107168, ---- | ! iTsEucRd S0E8 ia n. | ! Recowcammue } HAPAONCTHTE STUDY 1. Noacgative impact because the stl vee was ued nh clelaions. | PpEo fir gms we i ' StAedaDiave,co9r0S.igmiaregh Ls, Bue Slrfo3 ii MaisgetrmenlSigatas wo lan || CALQAUReview, fee algle. [ox= ii Exygen Research Page 97 of 95 COLGDn Exygen Study No. 023.066 Exygen., . Poeriish. ! \ } \ PROTDOCoOLaDEbVneIrAT4ION TTT OoCoren, SRT |}i | EgonSy mbar, 100 PriscoNomom: or01108 i || \ || satin> ET ACTIONS TAKEN t:i nest Su) Te one Yel i! hpotiestv mpacton sty eck mengrec Gi estwirevith scape i1 \\ i| leith TZ Jer]of 0] i o Spr er, = ool\o3 | [tats btin) pJlvgl= NR v/2T/A | - !i EE -- Soren mio LT gully ; : si | Kez ; RnBa , | Exygen Research Page 98.01% cranny