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m-- t 1 AR223-0079 El-17 1 _-- LaboratoryReport 1 Analysis of Fluorochemicals in Wild Bird Livers 1 Laboratory Report No. FACT-GEN-010 LR U2392 1 oo TestingLaboratory i 3MEnviro3nMmeEnntvailrToenmcehnntoallogLayb&orSaatfoertyy Services Fluorine Analytical Chemistry Team (FACT) 1 2-3E-09 935 Bush Avenue, 1 St. Paul, MN 55106 EE a Laboratory Contact ---- Hn || n FS KriBsldHga.ns2e-n3,B-P0h9D. St PauPl.,0M.BNox535313331-3331 `Phone: (651) 778-6018 FAX: (651) 778-6176. Requester S---- n un 000520 | H" WMERO`NRMEPEONRTTNAOL.LFuAbCOTRGAETNOORIY0 n S`iSnutorolcihveemriscaamlpsl.eTshceolbliercdtesdwferroemcvlaasrsiifuisesdpaecccioersdoinfgbtiorsdspweceireacdhrgaecoegrriazpehdicwiltochartieosnp.eScix0ssppeceicfiioecfs BbrirodwsnaPeerleipcraensse,GnrteedatnBtliuseHseurdo,nsin,calnuddiBnrgaSnda'nshlClorCrmaonresa,sD.oTuhbelbeiCrrdewsteerdeCfoorumnordaantsv,arWiheityteoPfesliitceasn:s, I'l aFclroorsidsat.heIUnngietneedSra,tehse icacuis nogfdNeeabtrhasotkhae,sNeebwirMdesxiicuon,kFnoowrn.dD,eAcraizlosnaa,bCuatltihfeolronicaa,tLoonvciascihabni,ernddvas foundan aboutthecauseofdeath iknow) reincludedinAppendix Coftisreport. x L`iwvereerqsuaanmtpilteatsiwveerleyanhaolmyozgeednfiozrePaFnOdSeaxtnrdacPtFeOduSsAinusgianngihoing-hpaprriensgsuerxetrlacitidonprocedure,Theextracts n stcandharrdcurovemextraacttedfroomtgaranbdbriemlamivaesrp,sAsnptaelcytytriocmae/ltrdyee(taHlllLsPaCre/eaEvScaMiaStbMlSe)ri,ahnoedsetsvuadlypabtienrddveamsuisnytaaoed cboyntFaAmCiTnainnstahoed3mMeEtanbovliitreos n(mPFeOnSLtAaAl.,TMh55e6pr,eMsSenTcOe,aPOaAbsAe,ncMeSo1f3o,thPeFrkHnS,owandfuPoFrDoSc)hweaiscdaeltermined n bsyitnspeacitnicoAnpophfenHedPiLxdCB/.ESMISMSanalysisof 2birdliveswhaechgroup. Aful stofaconyrmis: `Withthexception ofmotof theSavillCranesan asingleBrowaPelicanfomCalifia,thecats o Tmt pn ne a Sir (exMtrDacLts=c1o0nptapin.edEsPtFrOacStlsevfreolmsvtehreylnievaerrstohfethMrDeLo.f 15SandhillCanesshowedsomePFOS;twoof these nu sEhxtorwacetdsPfRroOmSolneeeBsriangcr'eaCtoexmoocsraonffthoosm dSeatneDrimeignoe,dCnAtahedeoxtnraecWtshfitoemPoetlhiecranb,ifrrdsomwCialniatthieas,aCmeA: classification(20xforthecommorant an eary10%fo thepelican).Ifthesetwocutlpyoiisnagre un t`hreemgoevogerdaapntdicPaFlOlSoclaetvieolnsowfitthheibniarpdarhtaibciutlaatrclcaasnsbifeimcaatdioen.are averaged,somegeneralobservationsbasedon nu `DWiietghot,hCAc,xsCpltiioaniaof,thCeASensdhhoiwl rCealanteisv,eliynlgoewnleervaell,siovferPfFrOoSm,bwiidtshaconlalveectreadgferofm ethewheasnte5r0 npUbS.(LSiavners " from birdscollectedontheEastCoastoftheUS(Mia,Naples,andPL.Ladera,FL)showmoderate u P`wFeOreSdleetveerlsm,inaedpfporcoonxtaiinmt1ah0teh5eipglphbye.stElxetvrelasctoffPrRomOSb,iradppvreorxsizcaotlelleycte3d0f0rpopmbt.heCentalUS (LAandNV) mIotrseuntlhiakneolyntehintstthaencdei,fftehrenscmeseasspseocciiaetseofwbiitdhPliFvOinSglienvaeldsifftrheeatevnevrirsoanmpeunrteslhyaowfeudcsigoanioifcsaptelcyies. Tn ou cdoifnftearienntaPn aRvOeSrlaegveePlsF,OFSocroenxcaemntprlaet,iovneorfs5c8llpepbc,twdhfirloemvehrist coplelleicctaendsfirnomCaWlihfiotrneiPaewleicrandseien rNeivoaedda1 = sihvoewredraovmetrhaegseebPiFrOdSswleerveeldseotfeorvmeirn3ed50opbpe.wnSiafonrhallyllCoawniensPaReOSan,erxecgeaprtdiloenssofttihsegcehosgerravpahtoinc,laoctahteon. ofthebinds. u fies aes teaia cachcaswieredietercminead 0ciontaoinPFnDS.Live extractsfom severalspecies,inching 1 u d`eSatnedaumiillnCerdatnoec,ownetraeidnetselrmlinaemdotuonctoontfaPinEOasSmAa.lNlaomoPuOnAtAo,fMPFSHIS3.,NMeSaSr6l,yM2S0T%)o,fotr ePlRiOveSrAexAtwraacst.swere: detectedinthe iverextracts romamyofthebids.AppAceontnaintdheseiresuxlts. nu `Taindsfdearifonroichtemtihcaaplsemtaaylbeetoragcaepabilcebryechdasraacsteorciizatteidonwioftohwe eevveil oofmheenseacodmipsobuuntidosaionfanPiFmOalS tissuesamples. 000521 H 5 woRera0r.FmacoecEsnrtlo on P`ArlGotochoeoddLuuagrbheorrsiawgteoorrreoyusPfoqrllatowceydt,.ctohTnehtiaoslcdimsteisiosennsootfasnhai b3dMeatEfnowvaidrsionsnonmtebnnutetacolenLsa0abalonryyagctooolrlvyeecStraemndedanecrtcoargOtepinencrgyai0tniadnpegpfiecnasbeloef n pHrioghdeusctcsuuiltatbyilidtay orvseya.lReasutlitsstimoeu.ld beconsideredto besemi quaniaive. Da presbeerenhte. oN " LMOaendbi,c1si5an/me9p),blJeyeawSnceBorteutrP,osHafcrndosmef3nrMofeOtnch.ecuTNpahtaeitsoianomanlpallWMeesidwlieceirnHoeradgelilnitavleClryeedsretnhiettnboMiGneaadrvyeoesO,alWmsipeslnc(e3osMstioOnt.hseEentvirroan]mcaal u "Therei oholding imecriteriaasociatedwiththesesamplesforLCESMSMSanalysis. ou Anl"yFtAiCcTaMl-m1e0t,hEoxdtsractionofPotassiumPecooctancefonteorOtherAvior Foceosbemical SuFrAfaCcTt:aMnt:s2f0r,oAmLsiivseirsfoofrAFnuarlyoscihseUmsiicnagsHiPnLLiOvEerSEMxSact Using HPLCEloctosprayMassSpectrom o SaAmmpalyetperiepcarxaaticoenf- oaqmuaeosuasmspalmepmlaest,iHPwiLtCh/oEpSiMSnMgS:reiaogne-nptarsintgoexttraacmtimoon hydrogenslit uo (OTnBcAeYthienaanpotnTcoBnArolaliedienfvoirromnem,enht.eTahlectatisotnaincrseeargeendtvetloecti5valyotalrrgetsgaanoinsefanotroc(hiepmlicals. . acta)dried,adrconstittdinmethanolforMS lysis . o BPILcnoCl/EumEPnSL.,MBaaSssaeladidoqnuHotthoefPacffrinaLitcyoifOstihnejEaencftaoelrdSydatenetdaiMpolraetsdhsSqeeusdatltiMotouatngiShyvepawrhoe:avrsekersnepehasceliquidcehlratoimvaettoogtrhaepihiicd o s`omloubtiilonphPaFsOe,Stmeaaynahlycaits re0imniemefsor.aRcehtaernatciioenistimceasmboeutnwteeonf iest.andFaorrdcPaROmSes,oliuntaiosntaannddahred . analyteextracedfomfiver this analysiswerematchedontheHPLCsytem 0within 1% FollowingHPLCscparaion,ESMSMSprovides aapdndaratemeans foranalyzingaviderangeof |]. a`donertdgeaacntpiicrocinmoafromylonme, chpianracoclontuesdr,iiu nssgtgifcen lnouefortrad holeclhayenosmapilecyrat,laes,t.iesdEasetllleecitcvedet.Tlrhyiomsasndoiponntrisezapabetyorimos,bntartredsee.dMcwoihlhuhsneiedgsihpreaqinrmeeaurcrgiylezgy af,sor, u dbesoeednt colons retesalle secondary onicagentswetthepinyin,which are " un i{FhsoeBrsaegxmaemonpntldeea,droynrforPoaRgbOmeeSrn(tisoCinassdFuctyh12d5aS8na00nlayd5sics)a,in(obcnoevm4s9pd9oinstdosiienlgetc1teeSda05t)h,ePcnRdhOS7a30rraorammoc(tphriCimcsao5rtmypiio0oucnEn.a)dTchthi.aostfion n msiegcohntdhaarvyeothnefsaagrreescthaatriaocnteraitsees49.9 csprimeyin,but fenchemical compositionsand n 000522 o3l EO"REeroFLAsrcoTrrmsTvoln,r . 5.1 Calibration oi tihAnemsiexciphesecttle,dvedxeatfrl.a.cCtaeldbmartartioxnccahleibcrkatsitoanncdhaercdksastrancdaordmipsaenailynsznaemendtaelvery 5-1e0ssoanmspeleisstwoitmhoinnit+o.r 0% of ou ``sQMpuaeatcntiiifxtiacctaiuovnegsobfhrtaahceiktoeantrisgniegtnacgntaahclehygtmresouiuslpboaefsserademosppnlolenissn.eeoaQriuracegrrrkiecsntsgiomononoafndacleayoscfihsah,nweaeliygrthaetmsebedaUtsx.e,dTonhftetwshocecrxeotsnrpdaoccnatrevdoe.f 2 _ `asnotused forPFOSdetermination;bracketingcalibrationcheckswereallcompliant, 5 thisexclusion 7] `doesnotadverselyaffectthedataquality. 52 Blanks uo `AiTdtwdhoiexsatcorhancet,iicotnhwboolfasssakamsm,ppullteeissloaifznbidnacgwunarktvmeears.atsis,uuTosgdaftoemttherc,xataeceexdtcrlabcrteadtwiiotnh ccuarvcehsb,atrceheoxftsraacmtpeldeasl.ong ou {`hBilsanstkusdayr,ecaolmlplnikantwiefrneotcaormgpetiannta.lyteisdetectedabovethe limitofdetectionforaspecificanalyte. Tn | 53 Surrogates nu Teahyoporocane fc iswd a5 8supinthis rls. Sugerespons:is `monitoredto confirm grossinstrumentalfailure,ifnecessary. n 54 Matrix Spikes `Duplicatematrixspikenyse wing olltargetanlyteswerepreparedandanalyzed romSacil `craneliver.RecoveriesofPFOSandPFOSAwerewithintheacceptable rangeof70-130%. nu 55 Laboratory Control Samples LaboratoryConrolSamplesar notacomponentoftis dy, Nn 5.6 Sample Related Comments `Matrixspikeswerepreparedfor asinglespecieofbird. It iassumedthatspikerecoveworuildebse: uN r`eassoniafbomlreairleltlsenpteaicoinerst.iNmeoasntdarnedaasrodnmaabtleeridaalufgohrtePrFfDoSnisspaveaicluab.lUe.sCtolms pouna dimdenatn itfiicaitd isoanviislr baabsleed on identification of thisanalyteshouldbe considered tobepreliminary. uN {``hQwuaeasnootibetsaretritoavnregdfewotrhPeyRnOemoSsnwiaatroserciiosnngtdetuhcbetee4l5do9b,y>mo8n0ittorarnisnigttihonetratnhsitbiionn4v9e9rm>at9r9i,xS.oTrmaenpsiotsiioinvpeairnatmecefteerresaocer n 000523 n] F Tone -- Lon on a . Cempont| Pe| | Tenn `Table1:AnalyteTransitions for HPLC-ESMSMSAnalysis on [ws|| 1&0 | [msT= |] u pe pdra OSde emt t `Withtheexception ofmostoftheSandhillCranesand asingleBrownPelicanfromCalifornia,theextracts from theliversofallofthebirdsweredeterminedtocontainPFOSabovethemethodlimitofquantitation n A `extractscontainedPFOSlevelsvery nearthe MDL. `ExtractsfromoneBrandt'sCormorantfromSanDiego, CA andoneWhitePelican,fromCalipatria,CA on trh` eemgocevoegldraaa pnhdi(s cP>aF2ls Ol0oxSclfi aeotvrief otlnhosewi fcitothc rehmibona irarapdnastrt'tahini acdublnio aeraarcn cllaaynssb1ie0ixmcfaeordriteohn.earpelaivcearna)g.eId,ftshoemssetgewnoeoraul otbslecpvyoaitinitosnnasbgraesed on WDiietghot,hCeAex,cCeaptlipoantoifat,hCeAS,asndhhoiwllrCerlaanteivse,liynlgoewnleeravle,llsiovferPfRrOoSm,biirtdshcaonlalevcetreadgferaofmtehssewtheasnt5er0npUpSb,(SLaivners ou frombirdscollectedontheEastCoastoftheUS(Miami,Naples,and Pt. Lauderdale,FL)showmoderate un is lilE y tmeeilestI h p vi ROSlo olS s rhesvmeS seb asoplsyeectSEionhoefesyi. In `Weredetermioedtocontainthehighestlevelsof PFOS,approximately300ppb. `contain anaveragePFOSconcentration of58ppb,while liverscollected from WhitePelicansin Nevada ou `showedaveragePFOSlevelsofover 350ppb. San Crand esah reai n exl ceptl iontothis observation,asthe: Ta nkware delon 5swhirl lowinPFOS,regardlessofthegeographic location un `Withthe exceptionof th SandhillCranes, ive extractsfrom lastaneofthetwobirdsscreenedwithin " `eachclassificationweredeterminedtocontainPFDS.Liverextractsfromseveralspecies, including 1 n4 es `SandhillCrane,weredeterminedtocontain asmallamountofPFHS.Nearly20% oftheLiverextractswere determinedtocontain a smallamountofPFOSA.NoPOAA,M513,M556,M570, or PFOSAAwas | 000524 EHA oH ] || || BOr OBrLboRr ATORY Thisdataindicatesthatpotentialgeographictrendsassociatedwiththeenvironmental distribution ofPFOS derMocrosteicalsmaybe Gadble by characterizationof ow eve of hee composi anal `Thisreportreflects themost accuratedataavailablea this time.Allmumbersshould be consideredfo besemi- `Thisdataindicatesthatpotentialgeographictrendsassociatedwith heenvironmental istibuation of PFOS `maybetraceablebycharacterizationoflow-levelfluorochemicalsinanimal tissuesamples. wm `Samplesandextractswillberetainedforfisture evaluation,ifnecessary. un 51 92 AAtdtaachhment BA:DTeflitifonQsofllaodrocQhueAicrtoinecymlRse AnsofLv Sls = 59:34 AAttatchmtenDtasC:ESxactmopcltheiodeusmcdrAipetitonnaanddtsaemaplereceiptdaa un EEE Hu ou the Lg \ % `Harold Johnson, | Chemist uo " 22 4 4(z(an Date 42% [55 H . nu n " 000525 q : 1007 '99 08:43 ID:A@naETlEySsi4s2-2o8f Wild Bird LiFvAeXr:s6.12-778-4468 [3 #=notdetected NA =notanalyzed x = detected LOQ=Limi ofQuantiation [= A-- ui [= faa Tr [wsyem pees] Meta Tv Fs SandhillCana T Choos GoiTle roo--T4--He--] n [iTTsmaic ran eee huhu) -- TT Tm a [27SuudhiiCran s [QhochiseCo,AZ |<00T<to0Tva--Tma--] . : fA White Pelican TCalipaminCA 135__T<to0--Tx--Tx--] n h [EaN Wh1in7e B7el7lenS 1 CaliS oamisCAI2 I 3 T<to0 [7 x T7x9 ] . [LTWhite Pelican T calpainCA [1s 100 Ta a] |Brandt's Comonnt Brine Corona |SanDiego,CA | 0 SunDieseCAT46-- Tai ha--] Renee [nedLts 1 a] n [F2E Te oiownT PelisSn --TaCmTi F S--eSsYTio-- h I o] EC rT TP I so CECC T2S-- -- rTTT 0 | rs Se EC un [52 ViePetess--------1[FNiVllaD 36s a 160 re ----] E--haepm e enage] ST Whi Bellew Fallon, NV T9371 | <toOgQ TNA--ThA 1 :| [35 Whlepelicsn | Fallon,NV [391] LQTNATha| n fet |S 1 BrownPelican [BrownPelican imi ET T"FtLouderduie, Ls Te Th fa | Ft Lauderdale,FL OQ TNA S058 J ---- NE ne nN quantitativerealsof theanalysisofwidbird vers NsovaeER sacs 1ocATIon_| 7Lroiseyops |irrospao prose | pry =CY -- -- -- BN eee [oC sm T Be-- coms suber aT ---------------- T I Cr r I = =a o - S C -- --||| c a e| on C osomm smemmmeT [m in nS w im T] C oem em7 i S n oTem [Ce cme Nl, Tan pT] o. [Ioi Csss trem=rm=Tope mior r w oa5 eT] T | [[itoosIr ppb bT tem [MMameetTAA T 20 r 1] ] Y Cr c -- ---- | n T C Topo] 3 sP n7 ic0 mS W mO 7 o -- -- | Quin dipempt) MDSmBmse 6% 6% un 000527 BW concn [858 | wm cm= | sooner [on] ew|oo | ro E 5 TT S YS SSoo S| [eI Cmos |I= heen-- ClY ieoSA|----17--|ortey =TEa rcos] ITwSy P| [iI ol |7 Sabie me 5MieA 11x --x--| un [[i0z2Cs00e0s || edoboelreid ccoorrmmss[|Y 5StbMartimr iilte.TAA|| 150356 T |ste y eT d[r x mey n]] |J [oCoenee n or mpier m v Meir n oTx y] pr | [sm I ot -- opin--1--Mao ni-- n{-- --T 6 T oocy r eed rmey ne] [imC soor| ate-- | eecomr i O --------oe--) mses cme--Viie Go 0 | 00Tt need | men] [[[mmooomtre| || inbtmiieecccnsdoatccmoomorrnmss|||o oatmol r|o mset Tsr mw e ] rman]| |][[0m o00 n 7 I | | intttiiaesiccnoomremrss| | |Gi lamatFcLLi{| 10i175e0 TTTo=ottx meneee{attx mmaenrr|| soo bmpim 1Glwiaca 5x] [[ssiooin| | bhmeomasgtetiinn | |CClpincGh| | 57 TTootceom {{actmene] = VS un [[[iost0oi0 oro8r | T 1 p pprbettbcheebioreson [iioor Tp |5StNMMairrilieTtAAA||| 121676105 5Moi TA | 17 |osw ttmereedx {[amtemnetn|]] ot atmor nn [CEomrmmmssT | wep pion m Riom n a mea atTx --oren] [[mmoosrt | | [mons | owShwhisoipmeiionne| m| --Fi ebiinaV VT T | 1o0tT Tottw mm d{[ aattmce| ne] [mmEoaslmoen | heeoemnnmttoomn P baLaiY neiFL|T 50 otmenred[aatmmaennedr]a ||' Como PROSAR, S56 Ma ET, FT OvAoR,mspdeM5n13waTrthdeCciditee rrTofsnobrs.to a mee] 000528 L JV---- Fluorine Analytical Chemistry Team n PFS's nN PFHS `perfluorohexanesulfonate C6F13503- PFOSA PFOS perfluorooctanesulfonate nN PFOSAA CC88FF1I775S0032-NH2 C8F17S02N((CH2CH3)(CH2C00))- MM557506 CC88FF1177SS0O22NN((((HC)H(3C)H(2CCH020C)0)0-))- BM rosea pertuorcorsmenifonyietyt Et-FOSE-OH snide C8F17S02N((CH2CH3)(H) C8F17S02N((CH2CH3)(CH2CH20H)) BW PDS perfuorodecmmeitonate CIOF21503-++ PECA's WM ohn retoenons MSI3 perforodecancate By VB petuordodecaone MM46633 HB we C7F15000COF19C00ClIF23C00CCI80FF1271CCO000-C6F13C00- -- BW ors petuonimet mito PFCA = perfluorinated carboxylic acid n 10 standard material availableforconfirmation; Hn 000529