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Aeven: = FA AR226-C0%0 EN-18 3M Environmental Laboratory- Fluorine Analytical Chemistry Team MDFoeroncegas3r8i1%c Cores om KrisHansen-Sr.AnalytCihecmaislt Screeningof PFOS levelsinEagles and Albatross summy:en pls idses of idse, on vente ld cage1dfe may albatross, wereceived attheEnvironmentLaabl.TheeagleserawascollectedfrombirdsinNorthern MMinniescotha(2i(1ssagammppalleesn)),.tAhlelUfpipveeraPlbeantirnossusslaamopflMeiscwheirgeaon(bt2asianmepdlfersu)m,bainrddtshfeoLuonwdaertPheneiOnfsfuilceasoCflabrplot `onSandITslhaensdewirtashaimntplheesMwiedrweaeyxtArtaocltleidn; tehxternaocrttswhecreentarnaallPyazceidfiqucaOncteiatant.ivelyfor perfinorooctane `sAunlafloyntatied(ePntFiOfSic)abtiyohniwgha-spvreersisfuireedlbiyqcuiodmpcarhisronoomfmaoltecoulgarrioaa-pPhLmCayrse-stsecpnetciiotnretoimcmetetroyfr(EtoPheLseCx-ptErarScMtaSed)y. i sdoeanicsmioaf egde oSanmwpeleseer atmilsoyv0aP Shse Bet pErL (`PaFndOaSn)al;y5t0icPaFlpOaSrwamaestedertseacrteedaitnacthheedatlboatthriossrsaepboorvte.thelimitofquantitation(10ppb). Specificresults techniqu`eThperpovriedseesnacneaodfdiPtFiOoSnialndesgarmepeloesfocefrctaaginlteysteortahweaasnvaelryitfeiieddeuntsiifnicgaHtFioLnCb-yEspSeMciSfMicSa.lTlyhmionsitoring. fragmentsdaughterions(m/z=80,99,130, 180,230) characteristicofthe PFOSprimary ion (m/z =499). ErperioTehaetpmcamsmatroyw vsof ROSA, omnes sb oh `ofthesamop fcalgle eses ra. Samplepreparation: Ion-pairingextraction HPLC: racers renton tne fr 20S In apHcontrolledenvironment,anion-pairingreagent,tetrabutylammoniumsulfate(TBA),is `used 10extract theanalytefrom thematrix.Anioniccompounds, likePFOSand perfluorooctancate - (POAA), areselectivelytargetedbythe cationic reagent.Subsequenttotheformation ofthe TBA-anion. pair,the analyteistransferred to anon-polarorganicsolvent(ethylacetate),dried, andreconstitutedin. `methanolfor HPLC-ESMS analysis. . InHPLC,analiquotoftheextractisinjectedandpassedthrough achromatographiccolumn. `Basedontheaffinityofthe analyteforthestationary-phaseinthe columnrelativetotheliquidmobilephasepassingthroughthecolumn,the analyteisretained for acharacteristicamountoftime. For EHmSAt:RDientecttaionoaTndFmOoSatsoronni,tnFoOfSthe alayeesctoeul1eaornphiab BceatrotsBol e EOS ls Tt= 9nt9 PFOSsolutionandthe analyteextracted fromserainthisanalysiswerematchedto within 1%onthe `amu,correspondingtothemassoftheanionicsurfactant (CoF17SO5-). Thisionwasmonitoredselectively tomaximizesensitivity. Ascanofm/z=100to 1210 (negativeonly)wasalsocollected. 000530 osouss : ESMSMSSe:veCroanlfsirammaptlieosnoinftahniaslsyettewdeernetafncaaltyizoznbyESMSMStoveritythe ideatityofthe PFOSanalyte icoonm.pEoSu-nMdiSdMenStiifsivceartiyosni.mAilsaritnoEESSMSM,,aecxocmepptotuhnatdsipteacdidfsiacniaonddiitsieloencatleddi.meAnfstieornsoeflceertactinhtteysiteoloecnte,d ifornaigmsecnhtarsa,cchtaerraiczteedrfiusrttihceorfbtyhesmmoalsehciunlgei,atarpeacrrtewaietdhahnidgdhe-teencetregdyg.as.As result ofthe smashiniogni,c: . . ionissmFasohreedxianmtpoloet,hfeorriPoFnsOsSuacnahlayssi8s0,aiomnu4(9coirsrseeslpeocntdeidnagstthSeOc)o,mp9o9uanzdnspe(cciofrircepsrpoinmdairnygitoonF.STOh)is, in13t0haemsaump(lcoersr,ecsapcohnodifngttheosCesFe,cSoOnyd)a,ry18f0raagrmaue(ntCsiFs.dSetOe)c,te4da0dt2h3a0daetmect(orC.FS05). ILPisFprOeseSnt QualityDcuonettroolssaummpmlearsiyz:limitations,duplicateextractionandmatrixspike analysiswerenotcarried ionusttoeandtohfesaenseamxplets.rQmauaatcnrtiixttcauetrivodneo.fAsPtRhOeSleexvteralcstwiaosnedfeftieciremnicnyeodfrePlRaOtSiviestuo naksnaonwdna,ntdhselsevreeastuclatrsve sbehfoourledabnedcaofntseirdtehreesdasmpelems.iO-neq25u0-aapnpnbdcotafliisbcrrtaoteaiaointncghqieuacvlkiwteya.sa`zTahlesytzaendadfatnedrcfuirvveeswamapslsensa;lryezceodvtewircye, r`ewqausaircedc,tehpeetxatartabct7ls%em.aMyibneimrae-laqzuaallyziotdy.controlwasassociatedwiththisanalysis. Hfmoreprecisionis . LiofQmuantiitattion Thelowstandardanalyzedwiththesssamples was10ppb;thisis thelimitofquantitation associatedwiththeanalysis. i IHnPsLtrCusmyesntteamlspecifics: `HewlettP`aCcoklaurmdnS:eKreiyessto1n1e0B0eLtiasqiulidCuCshromatograph 2Sp21m0pa0rmtimclesize FSlolovwematteA:: 320.00muMmAnmm.oniumAcetate SSoollvveeaattGBr:adieat:Methanol `4 Hold a5t9%0B1 %iBnfo99.r530m.0 5i0nmsi.s. R`Feotludrantto445 5%B%fBoira31..5m50imnisn.s. IInjnectjioen cv/otslauimmpoel:en:1s014L. Electmrasossspepctrromaetyer Microma`sMsasPslaLtyfnorxm2.I4TSAoPfYtMwaasresSpectrome"Ctheicrk," CMoondee:voellteacgterso:sp6r0avynegative S`oAunralcyezteervmapceurautmuprree.ssures1:105.0C0.0043 mBar,0.000079mBar Lous: 499, 413, 369 Electrode: cross-flow ;' 000531 osiouss 2 Electrospray MSMS `Micromass Quattro IIAPIMassSpectrometer, "Madeline" `Mas3s.1LSoyftnwaxre Canevoltage6s0:v Collgai sensergiy:4o5nV/ Mode: electrospexy negative Sourssperm:+ 113C. + APnalryzierlvomua:c4au9u9mr;p4rye9s8sures:0.000043mBar, 0.000079mBar . loads: Zepray . Daughterions:80, 99,130, 180,230;78 . 0sRs 000532 La Slama Tose > LOCATIONS AND DATA FROM AVIAN BLOOD PLASMA SAMPLES TO: Minn3eaMpoCloirsp,oMriatninoensota BY: JohnP. Giesy and Associates : Hilltop Place - `Will2i3a5ms5tBonr,avMeincdheirgaRnoa4d8895 July 18, 1994 000533 Avian blood plasma samples collected from two species, the bald eagle (Haliacerus leucocephalus)andtheLaysanalbatross (Diomedea immutabilis) were sent to 3M for analysis for CyF,;S0,and CF,,C0;. Additidoatnafaolr these blood samples follows: Laysan albatrosses withinthAeMsiamdpwlaeysoAtfoLlalyisnatnhaelnboarttrho-scseenstwrearlPeaccoilflieccOtecdefanr.omTatbhleOef1fpircoevrisdCelsuabpdlodtiontdSiaantodaIonsnlatanhlde birdssampled: `Tnaubmlbeer1,.anBdadnadtemubmlboeord,wayesacroblilredcwteadsfobran5dLead,ysaagnealabtatcroolslescetsiofnoofmbMliodowdaysaAmtpollel,, bnolrotohd-cseanmtprlael PacificOcean. [soos| poses | om om | | 0 0 |vacowss| isssyiom| |wacosm| mmm | [o[ oossoo | |_twoome rs| | s 8 | | tahoasr |noe | losT.19156 Nootherdata onorganochlorinepesticidesfrom thesebirdsiscurrentlyavailable,however, aseperatesplitsampleofeachhasbeenarchived. Baldeagles two caAchlflrsoammtplheesuopfpbearladnedaglloewsewrepreencionlsluelcatsedowfiMtihcihnitghaenM(iFdiwgeusrte,1w)i. tThaobnleef2rpormoMviindneessaodtdai,toannadl dataonthe birds sampled: 000534 pens ube. Bed meroncoat, egion, ae of odspl collection, x,wight,ade ndysof a wa no esng bdeagesiom 8 | o[rmromgg|fIere [fa oor::e|o_e|ooeem [[ooame[on|a] | eea ooom omao==n[[]=wm==iem[[[fogro=egem[[[rooeomem]|e=e{[[ooneo|||v=|