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LaboratoryReport
Analytical Report of Data for PFOS Dietary LC50 Study with Mallards
(Sera and Liver)
:
Laboratory Report No. FACT-TOX-130 (W1902)
Attachment A Sera TDaayob8fRelsulets
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Laboratory Report
Analytical Report of Data for
PFOS Dietary LC50 Study with Mallards
(Sera and Liver)
3
Laboratory Report No, FACT-TOX-130 (W1902)
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LaboratoryReport--Revision 1
Analytical Report of Data for PFOS Dietary LC50 Study with Mallards
(Sera and Liver)
1
Laboratory Report No. FACT-TOX-130 (W1902)
Testing Laboratory 3M Environmental Technology & Safety Services
3M Environmental Laboratory Fluorine Analytical Chemistry Team (FACT)
23609 935 Bush Avenue, St. Paul, MN 55106
Laboratory Contact
KriBsldHga.ns2e3nE,-P0h9.D.
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P.0.Box 3331
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St. Paul, MN 55133-3331
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Phone:(651) 778-6018
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FAX: (651) 7786176
Revision Date: March 19, 2001
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1 Introduction
wes LR
a T3h9i-3s)sInvdeswaisndheesisegrnaeadtdoiqvuearnioafmiavlellardasdsoecsksspeexfpuocsreodoictPoReOsuStlohaotueg(hPRdiOeSt.,DCBFeI7Sao0f3dl-o,sCisnAgS #2135
Cotnedimtaiionosn,al)aiadlacehesrovtaitoiconhsosdddinttihsrrteopxoircti.tSyduaestweorftehgeeianreegrdobuypthofitnestfaentiemsatlinsgwfearcielsiatycr(ifWiicefdoen
Ednavyi'rsomnedndtaayl2L,abpoasotddsooea.lySzeednquanntiitvaeticvoellylefcotrePdFrOoSm. tThisssaucerifircoemdssmoamelawielrssetnatt dtiedebeSfMore the:
scheduledsacred werecolted aod lyzedalos ul aemcd isreport
AWdidtihffoenwleyx,ceoptnisondse,oPEgtOhSeleavveelrsafgeePFsOeSrlaeavdelwvietrhsionfcahechmdaoleagrsoucpr,ebaosteidvwietrhaddossegrrulepv.elsof PFOS
3
`dCeoclnicneedrdutmoaiinaslelry(bge/twmeLe)ndtoaPyEOsSncdondcaeyn2tr.atIinonmoinstvnera(1s9/,8)owrasaspgerceiaftiecrtne|po, he raoftPFoOS
Nodetawascollectedforamy abe anPROS.
APbourghoriwgeorrcoeusfoeqluloawlded,cthroenaeceimseistsuorneosfotdis3dMatEaawvaiscneomtenneaclesLsaarbyocorlulyecStaendadcacorrddOipnegraftoianpglicable
Good Laborty racic.Dtresend eres he ightquality dara vale ise.
ph1ihcasetheestsiongvraesspcoonnsdiubcltyedosfcWoirifnegIesmpapiicoanbsleLGiod.dSLeabotrstrayPrcacCtifchoers.hTmehoeceeondpnurcottootfcoel i
"UThpeoEnnsvpiercoinmmeenntraelcLaebp,re3cMeivcehdai60novfrc,usto8dbyiwla,s4inbliotoedd, nd46serum specimens,fon,on 051959.
U"TphoeEnnsvpiercoiummeenncsleLpatb,re3cMeivcehda50oifvcers,t5od0yw,is5ibflioeodd,.anAdco0psyeorfeascahmfpolemsc,afrnobzeenf, ooun 06in2a9n9. Aactho iseeng.
nemos SST CE RR S EEE
Thereis 2boingimecriteriassidwith hesesplesforLOESMSMSalysis.
{-
TFOals Anais5 E ---- R UEE --E ER'
AnaElTytSi$c4a.l1metEhxocdstioofPossum Perfcroocaneslfcse orOtherFlorcbemsicalCompoundsfom SDeureumtfhoe AssaslivsolUusmiengofHmPaLlCar-EskecsosavpaaiybMles, sstSapndeacrdrcoumrevtesywweirtehprheepfaorleldowiinmgeextcheapntoilonss:tead of Sotudmiems.aAllSansiensd.icAavtaoirloafbglersoasmcprle,vobhuimessweerruemwsoasaeld, c3rewsuaosgnaotkecmoaurgh.sSrioermmaartreiSx ppiekes E`TwSe-rep.r6e0p,arEextdrmacrtaibobnitosfePr.tPFsOSlPortf1o7r1wooacsanuesesdulfroenfaetreoncOetmhaetrelr.orenaormpods rom LiverforAnlysisUsingHPLCElectrosprayMassSpecrometywth he followin exception:
Petals
G0 aL
SMENVIRRONEMEPNTOALRFLABTCOKRHTAOTORO1R.3Y0
Druoem mtahllearsdmalilvlear.moTuwnetlvoef mmaalair spliivkeersawveairbplree,psatraenddfarodmcutrhveemsawlelraerd rvepei,eAdsiadmeestehrabneodl nsttheeadof mieetdhodraelfleereanclemsraerreplortedintesof wgof lyepergamoffiver wetweigh.PFOS ot171was
EUsTiSng8.H5.P1L, CAnEallyesciusoosfprPoatyaMssaisumSpPeecrtfrloumoertoroycansulfoate orOferFucrochericlsinSerumExtracts
ETUSs.in8g.H2P0L,CAnEalylsiesofcPtoMsossussmSpPpeecrrrfooamreoytoycaesufose orOberFsrocheicalinLiverExc
`S`aAmnpalleytperespeaxraatcitoendf--oHm aPsamLplCe a/tEsonwiSptahMiongSpeixMtnraScet:aigoeno abut ammonium hydrogensulfate
(`TOBncAeY)thieannaipoHn.TcBonAtroalliedsenfvoirrmoendm,enhte.nTlheycatsiUonstaegedn steloectciveelyptoalragetrs apniconiscoflvueonrt(oemheemyiecarl.
3
butylter)dried,ad econsiutdinoctane forMSanalysis.
HPLHCPLECS,MaSMalSiquotofexacts nectedsndpasedtrough arevesphaseliquidchromtograptic mocobliulmne,phBaassee,dthoe atmhebtafefinsietyionfetheafonr t8ceharfaocttehreisstaiicaomnoaurnypthoafseiein.thFeocroclacr arlmtnpvaslotatoeeda,rbdid aSnoalultyitoen exPtFraOcStmedafyomchutiate8i0mtiinsuatlesy.sRiestewnetrieomnaitmchsebdeotnweheeHn PsLaCodsaysrtdePmFfOoSsolutwithnio1n%a.ndthe Foolrglaonwiicncg HoPLCmseppairnaoctihoinun,Eg SnhMuoSrdoMcShseprriocv,lisd.esElecatrpoisaprnadys, eacnurneizmaetiaonns eocrhiaqnauleyzsiendgpwriidmearayngfoerof daetectnipornimdoafrmyoolneccrhonas,risageocnfehtaelaey norpaeineessd asttelrieecatceidv.ellyomsiadeesmpcerctureesl.foerMcotolleilsideoncwairuth laonrigezoensdg,as. ersiaigunnGiaqmgumeeseattheiropnroimfsarhyesoenl,ecwtheidcshpaeceieds;etesceeqdu.entcollisionscreatesalesecondary oe Fiosrfreaxgammepnltee,dfortoPoOthSer(oGnsF1Su0c5h)aan8a0laymsiso(cnor9es9poisndsienlgect1eSda0s5)th,e nchdar2a3ct0earismtic(pCrSicOy).onE.Tahchiosifon thmeisghtsehcaovnedtaerysaamgeumcehnartascitserdiistcitc4e9d9anad caprbiemawriyeon0,bdaitfdfirfeernenttPchReOmSifcarlocmomtphoseitcioonmsspnods hat secionofrnagmedntataion ratyer.
Banas
RR
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5.1 Calibration
wFaorsqaunalnytzateidvvedeertyermtiona1t0isoanmsp,laemsid-olmeovenli, clfsramtioen clule v.erifCiacaltbioanti(oCnVcu)rvsetavnerdiaSridciantimoentshaanndolards asesaccnepawdbeireaeifcnreepdmabsleeresponse i lin +. 30% ofthe expectedvale.Inthis dy, llCCV
Quparnetpiatraetdiionnmoefthhaneoalr,gbertacakneatliyntgeseacbhagsreoduopolfisnepr rleg.ressQion aulysiisonf(wceaitcghhatneiadly1tae)iofbttawsooecournvnehse, nspmonese.ofon omore specif daughieros using heTlplerespons toringmodeof he
Peds
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AENRROENPIOERNTTHAOLFLAACBTOTROART1O3R0Y
3aMvailloatbl#e2a1i7heputriitmye8o6f9d%a )coofllPecRtOioSnwasepsaretedfroerscaulsibBraatvieonostabdeaenrdcso.mAescepudr.ty information wissot
52 Blanks Tsawmpolteos.fouBrlaenxtkrsawcteironebalcacnekpsa,bulaiizfiongtwalrgeertaanlsymtoegwaatsedmetaetsite,dwsehroeveexhaecitiedtwoifthdectaecchtbiaonchoroaf specificanalyte.Intis stdy, allblanksweraccepabe
53 Surrogates
`w1a1s,m2o2nTiethronryedctocronofirpm egrrosfinustoamerntoawlfoashcus,tediaf1sencaesseusraruroyga.ltSefwimnooginastaarneasltypsoienss.eSwuaTsoagcacercepsapboflnosere
alanalyses.
5.4 Matrix Spikes
`
Ov0erextcheepctoiuornsseoalfltmheaatnalsypsiisk,eswsehyo-wcegdhactcmepaatblieckoevsewreeseopfregpraerseeditnhatnh5e0c%a.l Oifverftomuarmhtaix.e.With
spFikOesSexrtercaocvteerdoynof947297%9a9,ndtwasoewceornedrseacmovpelreesdhoouwseiddPetEOeSacrcepclovaebrlyeoafn3g2e5o%f.+T-h5e0s%e.ouOtvlyeisnagmrpecloevherdies
`Bweecraeucsoentfhienreedm,abinuitnngc,26vmiaotursixersrpoirkweaswserreeawdiliy dsehnieacdc.eAptnableorrenss,pikoionfgtahremeatcitionvsusspekcetnedfo
aedditxionaphlmeastelrtiwxoasapniokmieaslwineesr. Feixntraalct,edd ctoco0.n3fmiiswcahkautlawtaisonthaoluygnhttohbeedlaotwarreedcuocvteiorny.pUropcoensd,isicgohvtery
oeftxheacalcculwtateiiornneootrn,sestdhe.orginalmat spikeswere confirmed obesccepableand headdine-
BSeicxateuesnemtahreirewsapiskeslwietlreemparlelpaarrdedeirnaavabiiatbsleer,.rAablbiltmeirxwasspiuksesedsh5owesduaocgceapetmablaeeicovtriysofdTy0-.
130%
55 LaboratoryControl Samples
LaboratoryControlSamplesaenot componentofisstudy.
5.6 Sample Related Comments
s`uSbtmuimptsewdewrithntohtisalstyuzdyediflorbaenaynarleysziedasnepoetdeentdiuaplocnwarbitoen roeqtuherstfaonmPtFhOeSs.pOethre.rmIanttiecvsentof
furtheranalysis, 0additonalreportwillbegeocrted.
"E
LOa Der
`AWdidtihtfieowneaxlc,ecpotnisonisd,ePrRigOShleeavveelrsaigetPheFsOeSrleavnedllsiwvietrhsionfetahcehrdaosladgsroiunpc,rbeoatshedvwieth0dodsseegarlov.esof PFOS 2d2eaclrienbeedtdweren2a0-m35b%aeoofwtetehiendsacryla8eavenlldsdolafyP2yO2.SSmeearsluvreeldsoonfdFaOyS8.meLeavseulrseodfPi OanSimianltshsaecrviefricseodofnday aanniimmaallssssaaccrriiffiicceeddoonnddaayy 28.2wee, on verag,30%lowerth tho levelsdetermined i he versof Icnmoostnanimcalisn,efvorena(sgpeu/cgi)faiwcatistmgerpeiaotienrtothhaenn.ratio ofPFOSconcentration sera (sg0nPF)OS.
Petes
GO SG
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7 Daa Quality ObjectivesandDatsIntegr ~~ THT NIE TR
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+ Acceptableprecisionofduplicates - <20%,determinedby MS/MSDanalysis
Acepablerecoversofples 70% 0 130%foser S040 15056foc vr
+ TUascekofcaovnifaibrlmeaatlolrryumateitvheofdos--Gliyvseinst,hecseolecntifviotyorfmtehtebaondalsywteircaelwtoeoldused(HPLC-ESMSMS)and
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+ (Dmeraomtmocnchsaetldalttsoiosnosndooffaspnecfliofyiicisitpyenc~i3Sfp%iec)cpaiafadirctiethynewr.easspondsemoonfstareatsetdbonyecchhraomraatcotgerraspphircocretenotidorn itinvge:
+ Thohmeogceoaeyn,vcasinoootfcntohempleenocnetmhaeterdiaatlet(hFiOsrSe,ploorttw#a17s1e),ewidth,reOsppeceteobpecehra,cisiiztayt,iaonn8d
Complete, copyofteeportwillonl te 3MEnvicamesaLab chives.
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