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1f @ i ARRR_G 3406 10 000133 | RE | | D | ! HD RAG HHO6 BIOMALYTICALREpORT Tite: Das: Authors: PreparedFor. AvoaTipmtNo: QPuaetictitveuDecterrm(ioAnaFtoFiOonc)o,tMfeAasmszeoecdratsethee SPtudey DcWOuUsoogTArnwiboono(lPooFOAScp)r,aiytnLHOaumManSn MSeoSrusmfreom 30Septemb20e0r3 DSavuidJsALnadMerusrnopnh,ayM,SB.hS. TeL.Roamacs y,MPeS. 1Ad5vCioanhBriwooScoideRnoceasd, a. Ithaca, NewYork 14850 EDnuvPioroontmHeanstkaelllSLciacocbe orfoarHteaoltraynd + 2100.30Boxio0nRNoeawda.rk,DE 1971JMR GZIADIADUDOC `Advion Intecaal Study ID: DWo4. Number ofPages: 1 Tem "pTehceiocronoooscatraantoisotnsoafmaomenm(oPnFiOoAm)p, aescdetlezmuinre oi(bAoPuFncOa)ts,meemraesosuarnmdpaltetsshceollec duervielnogptehdeSbtyuAddyviDoWnOBSisiSngcseiloncccti.ov,saeecacs,rNe,Y,.odreproducible anlyialmethod 10HiusnoalantseePrFumOsAaamnpdlehse(0i.n0te2r5nmaEls)twdearde(xOtFracbteedxbaydecliaqiuiudo-lrioquniedemxatrnaaocciticdo,n procedire lSiHquLiEdDcFNAh).Frolloowinmg reaconmstattsusioosnp,egcstarmormpelteraeyxt(rLapcOtsMwSheIrMeySs)aiahnlytzheeadnbegynatirvhdeoioonenmsodpnea.y A2l8l0s.a0m5plegswfe.rfsourcPcFeOsfAu.lTlyheaplryecziesdiwointohfitnoiseassoaay.T(hCVe)laoswdeertleirmtinoefdfqruaonmtitthaetion alysisof quality contol (QC) samplesforPFOA:was 4.11%. `CompanySahitized.Doesnot containTSCACBI 600134 sovonmoscnces SIGNATURE PAGE Tite: Q(uAaPnFtOit)a,tMiveeasDureedtaszthmePeioffinAomraamootcntiiazuonmstPeeAfnuioornoo(cPtFzaOoAs)tiea FLuomaMnSMSSunfomStudyDWO4Usiag TwolonSpray Advion Report No.: 02331ADIA_DUJ Reportedby: AW lL DMavaid.nofaBiogwaieAyiSs 3pseD 2003 Date Authorized for Releaseby: To$e02 ~B DTiormectofrpeflBoinoa,naPlyDs.is Bue. ||| | Psezatts sian pos0e 600135 @ | | QaU STATEMENT eT tmcpte----T QualityAssurance UnitofAdvionBioSciences(Advion). [Spletogobinder [DemBeiew Tilman? TS Decombur2002 [simmons | 31 December20z | S E n R -- {pits Quality AssuranceAaditor | oo ssn 000136 | pp-- QA STATEMENT cccmmrerererrssmmsmsssssmmmmmsmesssmemsomersmnd `TOA FCOBNTELNTSE creesenmssmssssmssmssrmmmmsmssssmamendh LIST OFTABS ccmmmmmrrremmssmsmmsrmsmmmmmmessmosommismammnsaonS LIST OF FIGURES commensal 1.1. StudyDESCE20diOBpJ6CoHVnE crores sommes 2.1. Analytical PROCEUHS) erences 22. AS SIEe R gress -------- 32. AnaRleSuyltstorSiOcYDaWOlS c.ecomemremmennnd 4 DATARETRIEVAL ccersorsmsmmesmmrmmssssmssmssssmssmsmsmesrmned LI AJ 7. FIGURES cosossrssmrt smsmsssmmsmssssnes ws ssserseens 16. . Pagers @s31ADIADUDOC 000137 ustorTamas Table 1: SummofaSermpylemdAssay Iaformaion for StudyDWOS cv 10 Table2: PrL essionandAccuracyforPFOAQualitA yControlSamplesin Hum Seu Tie: PE dronsndArcam fePOAClfA rlon Sunde omen Snr `Table 4;Ca0li8bSr0a2t8ioDnCWuOrRv.eStc atistice s forthseDsetmersmirnatmiomnoefsPsFOsAisnmHuemamnnSerum 13 Table S: ConcenotfrPFaOAtiinHounmasn Secu Samples romStudy DWOA......14 Pages asnaDiapuDOC 000138 $ LIST OF FIGURES Figure 1:S`eStiacntdeadrRdeiancCtoinotnroMloBnlitaokriBngaClniomSteogeEaXmUsGoEfPFvrOAoanrdheeIntrernael 16 Figure2:S`eSlteacntdeadrdfReraocmtioHn uMamraitnoSreiraugmChErxotmraatoCgornatmasinoifnPgFlaOtAeresnaldStthaendIanredOaslly Figure 3: S`eStlacntdeadrRdearcotmionSMtoannidatrodri|nHguChmraonmSaetrogurmaEmxstorafctPF(O0A.05eBndLthe)Intcuavlee 18 Figure 4:S`eSltoatndeadrRdearcotmioanSMtoannidatrodri9nHgCuharonmSateoguramEsXoTfAPEF(1O0ABanLd)therntoemael 19 | Pcsocis sonps0 000139 . i9 : i | | || | + mmopvertan 11. StudyDescrisnpd Otbjiecotinve p`eTrhfelaoobrjoecotcitvaenoofatthei(ssAtPuFdOy)w,maseatsoduerteeramsitnehtpheercfleuncerconoactiaonnosioesfeaiomnm(oPnFiOuAm), ihuman. s`eBirouSmcsiaenmcpelsesncco.l(lAedctveidodnu)rfioognSttudly DtWraOck4i.nTg hpeusrtpuodsyeI. DH was guseernum mesarbma apylAtedsven iwoednre atnaanldyezmemdasssisnpgecstelreocmteivteryi(gLiOd-MiSq/uMiSd )exatrsaacyti.oTn,htebwoorkodn speraycliiqnuritdhciihsrboibmoamtmoaeglyrtadcpahly! reportwasconductedin ccordancewith Advionstandardoperatingprocedures (SOP). 2 METHODS | 21. Analytical Procedures) L"CP/FOMASc/onMcSeamtertathioodus(w1)e.rSeedreumeasiamnpeldeisn(h0.u0m2a5mnLse)rwuemarceceoxrtdriancgefdobtyhevlailgiidda-tleidquid Feoxltlraocwtiionngprrecoocnesdtiutruetiooni,ssolaamtpetlheeextraalctyswaenrdeinsteepraaraaltesdtbanydreve(r1s5e)fdr-pohmase mansen. Bcehlrloemfaotnotger,aPpAh)ywointhaa2.ni50t1ammmo(5ljeap)hBaesteaosf 4C5y%cElouleaat (BT(h9e0c:m1o0Fmyeptehransoilk:Keystone, 928mhMeaxsaodmeocnaifulmuaocreoanota)aaunacdi3dc5(% ElSnaFA (-1w0a:5sE0wmeetdDhaansoFlth:eI2NSmfMorAamPmF)oOnAi.uPmFacOeAtate). csopneccetnrtormaettiroyn(sweLredCele/iinnMetdhbeSnyetgab/toivMefoinosSnpmroad)ye.quidchromatographyademmass Fsoalmlpolewsi)n,gstbuadcyksgaromupnldesucbotnrcaectpitoin(oonrswcearliebdratteiconnsitnaenddfarodsm,QaCwseaimgphlteeds,(1n/cd)2,q0uadratic r`eBgormeisnsailocnoofpenakcareeorfantniionste(cpaerlaibararteitsonosiftPanFodOa/rndpse.Takhaerenaoomifna9l5-cHoDnFcNbAn)tveartsiuosfotnhse calibration standardswere 0.05,01,025,0.5,1,2,5,7.5 0d 10gal,PFOA. c"oTnhterloqlw(eQsCi)nsiutuofmqsuaanmtpiltaetsiaotn(tLhLreAeQd)iffoertciatscaosnscayewpatsi0o.n0s5(0g./15m,L3,PmFdOA8. gQufal,ity PFOA)wereanalyzedinreplicate of three. cTahliebarcactieopntsatnacnedcairtdesimaufsotcraelciwbriaatoiotnhsteacnaldiabrrattsitoinpcuulravteetfhoraeaatchfemaatltihrceae-lforuur.thsofthe Calibration standardsmaybe rectedif theyshow deviations>15% fomtheirnominal `concentration(20%attheLLQ):The coofficientofdetermination ()mustbe20.98. iTnhdievaicdcueapltQanCcsecarmiptleersiamfuorstthebequwailtihtiynco1nt5r%olosfatmhpelneosmstiinpaullactoendc(eanttrattwioo-nt,whiddsaotfltehaest Petts a2s31ADiA UDO 000140 | ID | | | crf tn Concentration. io ite19 TspumlmaarsyowfetheeprsecpsaprleedmadtAadsvsiaoyninifoamdavtaisocneofforhSeacdolyleDcYtWioOn4oifssgeirvuemnsTeabples1.is "TShteyp,urTphoseetiofptblhanikpswbelarnkpsrweapasreadbyrseicdaisnogcnoanrtyrmoelahnusma0nsmoreittrocoraplotlenitnialbes. contoaf stmudysiamnpleasdatriogishiopmennt. 22 Assaysie Alsampleswereanalyzed a AdvionBioSeicacs, oc, aca,NY. 23. DaaProcessing I aTrocdsawtearweeirlegglaelcetdebdy tshienAgptplbisdfoBiosSpyrsatyeLmOspIrMoSg/rMaSmMiatchCeQunaenga,tvievresiioonnm1o6d,ee.siPdeinsg o`nMacMQcuianntwoesrhscaovmepdutaert.eFxotllleosw,iwnhgipcehawkeareausnelgtroapieocnf,otrhabFaocukglrsoaubnldessufbtoramction, A`vBaickgroSulnd:ssivbetrawchteerddeaatawweeirgehseadv(e1d11)sqMuaacdQruatainctreexgrtefsisleisoanvnidsuppleorafdorme(d0utshieng the softwarepackage Watson (v 6.1.0.03, InnaPhaseCorp.,Philadelphia,PA). Concentration `ddoawtanwleoraeddeodwfnolroaaWdaetdsfornowmitWhattrsoenswdietchimtharlelesaicgenisfaicdanrtofuingduereds.1S0ttatrisetiscisgwiefriec.ant pres priororeporting. 3 RESULTS 31. AssayPerformance dTohceapmeernftomeadnncTeaobflteh2e.aTshseyinftorraP-aFsOsAayspsredceitseiromni(nCeVd)foofmQCth saalmpylseissroafnQgeCdfsraommpl3e.s14is 10.4.11% oxPFOA.Therewasnomnked nscuracyinth resulsfomtheseQC `samples;meanaccuracy(RE)rangedfrom -10.7 10 -6.33%. `Tmhaerpkeecdtionrsmcaenacreacoyifndtahleyrceaallfrsafioonmtcuhrevseessitsadndoacrudmse;mseiadnfsoTcaubelaecy3.rTahnegeesdwraos52060 500%. rectors amopusoc 000141 esi, no, tis stn rtespine preseacTatbleed4. The valuewas0.9958for PFOAinhumanserum. ADAedditiobyceosenrd5sshirgesedsodtslhyediphlse fco eicesgrR eti woefel iBdsoy onwr Festsinsle y ros A: Fe4e5pessrootdmpFesete,3fRoarprPtOaeiAvceocneomokposd So0sn PpFlOAwsasnpriesse|d 32. Anal Resuy ltst fori Stucdya DWl 04 TPFohOneAeocioyancekmsneimaimaonne1rrnioAmmoSotytsEDVOI3O8040b3reo4prr3e0tg1e0di TaTee.A.L | + DATARSTRIEVAL ~3 FEpOevtseivtbeamcrteroni5 heaisofaio Bos.--o--yM--a--nNY || 5. ReE FmRENCES S -- ValidationfortheQuantitation ofAmmoniumPerfluoroocta(nAPoFaOt)e, CommonRong) HonSam vy uno SyrayLERGSIS. MeasuredasthePerflnoAr nioon(oPFcOAt,0a.05ntoo10apgt/emL | 12July2002. A cmanpoze 000142 i| & | ria ---- | i | Ay tori: i || -~D | || 6 TaBLES TbIeL: SummaryofSpl nd Asay nformatin forSeyDRA SampleCollectionaad Storage formations ADanSltooemngReeacTegielvemdSpaeAebdrvesatirtA:duvirone: Number ofStudySeplesRoaived: N1o0t0scpltibcee2002 3000 NumbecofStudySuplesAmayect. 65 - AssayPeriod: Ansty AcalyticalStandart: SLoomtei:: trLloStNaon:at Source: CalibrRaWeteigiorngeRhsaiinooggaeF:atoo:d: LoUwberpLineitoroffQQLuueittiitmoinokn:: 29October2002 Pros GpeenaboarroscianoAesPctFt,i Sign-Aldich 9NoHneEaDvRaiNlAable: Sigma-Aldrich Quueiric 0{.0p5rgits, Potts aman puso 000143 o - | B Belaslzzg :{| Ep 55 2<Z<a8 5 z :3< EEE, fl lza 2. g "TH leziid 1 EH paz g 2 ; * 000144 @ Tbe: CEvaa SlCleatovSeaaetyoeDmf8orte DescaonPFsOAofn [ein[om|== [oi RunNumber| Quadratic Linear Intercept (C) Coefficient of Y=ATFBx|+C,owemieghat1e7|d,afoerbwacekgrnoun|dsuoblrawction | ow D i | ! Page 130119 O31ADIA_DUDOC 000145 8 1 | ~~ || EE StmdyDWo4 SNuubmjbeecrt PFOAC(ogmreanlt)iation STS 0.168 S5717890. 00.1077358 Ss7n8g1 <16Q5 sas 57184 <Q <Q snes 00561 57186 <a ssnng 1L1i3 : 57189 <Q 57190 <uQ 5s7n19o1 <<uQ 7193 <q 57194 <uQ 57195 571o9r6 a0<0i5Q4g3 - 5757119998 00.3094778 57200 0.127 57201 00834 77220023 000257076, 5S7T220045 00223973 . 5577220067 000157247 mos 1s 57209 57210 0<05Q65 5711 0210 212 <r 57213 <wq sua 0658 _ .contoned Pa ots IADIADUDOC 000146 . J| D Tables: (SCtoudnytDanOe)AConcenraonsofPFOA FrSern Samplerm "SNEumber SSaattse sshwoonteo TOACroe en 00501700 Saigg 98039. <uQ sS9aa8ua0d4t0 o<0s2Q4s Sense Ye . ss9au800ss4es9 <oaiu1sQ ssaen1s3a3 ra=ro] sasusizss 0022226 soantiszsr 0i3m55 psraetasn oaeisg rsaote o02n66 Ssaa1i6ds barrg sfagds oautgs TQsaiL er Tb vaToprr Quin(0t08poodn) J eniaonpuso 600147 . 5 | ---- Figur1e: TSnetleecrtaedlRSetaacntdiaorndMoiniCtoonrtirnoglCBahnrk HounmaanSteorofuPmgBFrOraAesatumdtshe wne1300mr 10.FEON jp. w g 1 3 Tene imin rems50-sies,mRNA 09 7 jp. @ 09 Tart18an = : ControlBlank,Run1,Injection 7 | frm cman puso | 000148 B | ) | Fie: Sh Lecot-- Recoe nhMoeningChramatgr PO sd espnsemen wn . . . Eg = }iii memeAsi I: l sn 3. " 20 C=T ZeroSam Runp1,l Injece tion, 93 | Page 170619 C2331ADIA_DUDOC 000149 Sr mT TIL (0.05 pg/mL) semen non on w w 2. | ii ems maema-mma== sin | & DcE "" w . { Tn 5 Smt snire J one 000150 Bb Fuet: SdcttReconMostraCrates 504a Internal Standard [ar from aStandard 9 Human Serum Extract B=4130 w=1690,PROM Lots 3 " . " . i iy g D " 3 3mE 50 we3009, Time,min ADEA 15) seh i i " 2 @ Tomwo a zn | Standard 9,Rua 1,Injection16 | | | Page 1919. @3tADIADUDOC 000151