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am [Lt SUA ARR26 - 3578 awErvIROMMRENTOAL VLwABoEOERoCATtOTtRsY Analyti:cal Report Con, FeCay Definitive Study: Quantitative Screening of Commercial Lots of Human Serum Obtained in 2004 for Endogenous Fluorochemicals Using Solid Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry Laboratory Request Number: E05-0442 Testing Laboratory 3M Environmental Health and Safety Operations 3M Environmental Laboratory 3M Environmental Laboratory MaPrrkojEe.ctElLleeafdson Building 2-3E-09 PO Box 33331 Saint Paul, MN 55133-3331 Phone: 661-778-5405 `TWesitliinBgaumFialKcdi.ilniRgtey2aM-ga3eEnn-,a0g9Pehm.e0.nt PO Box 33331 Saint Paul, MN 55133-3331 Phone: 651-778-6565 = SS UR5a a7gpe:F = - = > Requestor Dale Bacon Building 2-3E-09 PO Box 33331 Saint Paul, MN 55133-3331 Phone: 651-778-4736 Page tof19 ------------------------------------------------------------------------ WMENVIRONMFENRTAOL LNUAOBOER0AC8T0OT0R2Y 3M Environmental Laboratory Analytical Report Project Number: E05-0442 1 Introduction / Summary `The following analytical report prescats data from commercially available normal pooled human serum that were purchased by the 3M Eavironmental Laboratory and. subsequently screened for endogenous fluorochenicals. `Thirty-six separate lotsofpooled normal human serum wee extracted using a solid `lpihqausied ecxhtrroamctaitoongrtaecphhnyi/qtuaenadnedm mscarsesensepdecftorrosmiexttreyen(dLiOfMfSer/nMtSf)l.uorSoecrhuemmicsaalmspluessing were received from various suppliers between 9/9/04 and 12/2/04. Samples were extracted on 5/11/2005 and analyzed 5123/2005. Hoptafluorobutyric acid (PFBA) was included in the original listofsixtoen target analytes. However,duto instabilityin the methanol extract, analyticaldatafor PFBA will not be included in this report. Instead, a separatestudy will be conducted including the re-extractionofthe thirty-six lotsofcommercial serum with acetonitrile and analysis using a newly developed method that provides isomer resolution.Thoseresultswilbereportedin aseparatereport. `Sample results are summarizedinTables 1 and 2. The average values reported represent samples in which there was detectable analyte. Sample values that were less than the limitofquantitation were not included in the average value calculations. Please refer to Section for individual sample results. Page20f19 er------------i ---- ------------------------ wonmosss eonsru i. Serr rorom Fe (oom) (ng) X allaon n on[o om[ol om] [Median |70s [oooes|owe|321 |ozwr|oas |oak[oor| [Wigh Izv[oows[oan|sz ier |ose |ova |aoe | [tow om Jooosss|ooe |03% ooseo |ooze|ooisz|oowe| `Standard Deviation |0378[000622| 0.111|121 ous|o1w |017s|oowa| i moI rs EA CArT [ame [Mean [Megan eSEratersevmottmerTT |won[oor mTn|om[we |eer| [Wen tow Tmt[mt|cmt[en] pots | ges| gens| | wa Toms [oows |28 | ws | we |oo | |W[owe|oown|ass[ws we|ows| [|oommsaa|oowwss|oowoswo[|oemwe||amme| ww0eJ|oowmme]|| NA? =NotApplicablebecausethisanalytewas notdetectedinanyof thesamples. -- sommonsSirsTspoSny 2 ES Reference Substances EE apool E -- Fa EtE [operas|rnecirren||woemeen[ | omrn e |yonero] [omwn ] Treetmoosammiead ||omnoxciraesn|| nowmm ||o roxi mom|e wwamn|| oowm terrence| ons | Site | on | on | om] [re|tcGairneo as |r ouvet rts| rToww ieno|anon] [rbot || | our wien vee re [I -- Fosa | aM em TCR280(99131-038) 98.94% aNone Ee ens Wi mews | Tmae om II | ami |Toranowes aw | om moe mn 5m=]| on ve] a Ferfunroocanon se. Te " ome| =B Tmmmm NMRresultsindicate thatthe PFOSreferencesubstanceconsists of 30.8%branched isomer, and the PFOA reference substance consists of22.1% branched isomer. Thesevalueswereusedforthedeterminationof theisomerratiosintheserum samples (presented in Table 10). I. | SMENIRONMPENRTALOLANJBGOEEROASCToOTuRY? 3 Sample Preparation "The samples for this study were prepared as follows: 1. The serumsampleswereallowedtothawandwarmtoroom temperature. 2. Four milliliters of serum (or water in the case of method blanks) were added to a 15 mL screw-capped polypropylene centrifuge tube. 3.Matrixspikesand methodblankswereprepared by spikingtheserum (or water) with the analytesofinterest. In addition, C PFOAand 0, PFOS `were addedassurrogates to allserum samples, calibrationstandards,matrix. `blanks, andmethodblanksatconceofn 1.0t4ar nd0a.9t 50nig/o mLsners um respectively to evaluate extraction method performance. 4. Ten milliliters ofacetonitrile were added to the serum and the centrifuge ptruebceispiwteartee.capped and vortex mixed, allowing the serum proteins to 5. The tubes were centrifuged at approximately 3500 rpm for 20 minutes to pellet the precipitate. 6. Aferremovalfromthecentrifuge,thesupematantwastransferred tabottle `containing 70 mLof water. 7. The samples were passed througah preconditioned SPE cartridge and eluted `with 2 mL ofmethanol. Quantitation was accomplished using high performance liquid chromatography tandem mass spectrometry. The following parameters were used: Lsyisqtueim.d Chromatograph: Hewleti-Packard Series 1100 Liquid Chromatograph Analytical column: Keystone BetasiTM Cs 2.1x100mm, Sumparticle size CStoolpuTminmtee:mp2e0r.a0tmuirne:ut3e0sC Flow rate: 300 uL/min Tnjection volume: pL. MSooblilveenpAht:as2e.0commMponaemnmtosn:ium acetatein ASTMType I water Solvent B: HPLC Grade Methanol Solvent Gradient: Iomw we axuwe uBoo ssooww awo omwx Page Sof19 eee eee MENROMAFERNUTEACLTLWABEODRSAbTOeReY MSoafstswaSrep:ecAtnraolymsett"er:VeMrDsiXonSc1i.e4xTM API 4000 Q-Trap Mass Spectrometer Detector Tonization Mode: Electrospray Negative . Temperature: 450C Gs: 35 Gs2: 45 Entrance Potential: -10 Analysis Type: Multiple Reaction Monitoring (MRM) Table4. Acquisition Parameters [[NPFRPAAGAAce)|[Tasmoe | | masmom [7 o=w | [DAGAce | ams |wenwanesTw | [[PFOACsAGd) | wae | wmeawovws 45 | [[G CoAfsadd [TsT uwso | | cwemvawemmwsezmens | | wa8 || [Cuts | amo | sermeszes ws | [Cohod | emo | werweesser | ow |} [esaTae 17m Te | [FosATMTas 177s Tw | [ores Tass 1 same | = | [Peis 7 swe | mame [we | [pros | ame | women ~~ ow | [eros 1" ese 7 wsams mw | [_meros | mee [ewe 0 | [[PPrroosAito2gTM [smwwee| TT wwwsw | wwo o]| `When multiple transitions were monitored, the total ion current (TIC) was used to quantify cach analyte, thereby providing greatersensitivitythan individual Q3 ion measurements. 4 Analysis 4.1 Calibration 411 Calibration Curve Anextractedcalibration curvewasformedbyspikingrabbitserumat prescribed. levelsandextractingthecurveinthesamemanner 2thesamples. Stock Solutions wereindividuallyprepared from neat flvorochemicals and diluted in methanol.Sampleswerequantifiedversus a 15-pointextractedcalibration curve. Page of19 WUEVIRONPMREONJTEALCLTAHOB.OR0A5T0O6R4Y2 `Theregressionanalysiswasperformedusing aquadraticcurvefit weighted 1/x. Calibrationstandardswerewithin +25% (230%forthe LowerLimit of cQaluiabnriattiaoinosnta(nLdaLrOdQs)wwhiicthhwaecreonotewiftohiffndeti3e0rm%cinwaeitrieoneno>t0ni.n9ct9l0u.deLdoiwn-tlheev.el calibrationcurve,Calibration standardsthatwerenotgreaterthan2xthemethod. blankswere notincludedinthecalibrationcurve,exceptwherenoted. 412 ContinuingCalibrationVerification (CCV) AContinaingCalibration Verification(CCV)wasrunatleastonceevery 10 samples,bracketingthesampleswiththecalibrationcurve. TheCCVrecovery waswithin25%forallanalytes. 413 SystemSuitability Fivesystemsuitabilitystandardswereanalyzedbeforeth initialcalibration curve andaferthelastCCV. Thesesampleshadareacountswith a%4RSDof<5%and aretention time%RSDof 2%whenevaluatedindependentlyexceptfor the: followinginstances: "Thesystem suitabilitysamplesforeachoftheperfluorinaied acanidFdOSsA. filed.Ineachcasethe%RSDofthe retention timeswaswellwithintolerance limits,butthe areacountsvariedbyasmuchas20.3%.Thefailofuevrerey `perfluorinatedacidtested suggeststhepresenceof systemiceffectonthatclass ofanalytes.Thisshouldbekeptinmindwhen evaluatingthedatapresentedin| hisreport. 414 LowerLimitofQuantita(LtLiOoQn) `TheLLOQforeachanalytewasequaltothe nominalconcentrationofthelowest standardinthecalibrationcurvethatmetaccuracyrequirementsof70% -130% `andthathad a leattwiceasmanyareacountsasthemethodblanks. 42 Blanks 421 Method Blanks Method blanksconsistedofaliquotsofMilli-Qwater extractedinthesame `<m5an0n%eorafstthheeLsLamOpQlefosr.Athleliofrteshpeemcetitvheoadnballyatneksswiintthitshseftouldlyohwaidngarexecaecpotuinotnss: FHA: Twooutofthreemethodblankswasgreaterthan 50%ofthe LLOQ;none wereabovetheLLOQ. C7Acid:Oneofthreemethodblankshadarescountsgreaterthan 50% of theLLOQ;nonewereabovethe LLOQ. C1 Acid:Oneoftreemethodblankshadareacountsgreaterthan 50% oftheLLOQ;nonewereabovetheLLOQ = FOSA: Twooutof throsmethodblanksweregreaterthan50%ofthe LLOQ;nonewereabovetheLLOQ. Page 70119 WENVIRONMFENTRAL LOWAoBOCR0A8TT4O4RY7 PFBS:Twomethod blankshadareacoc greaterthan50% ofthe LLOQ;oneshowedanomalouscontaminationand wasabovetheLLOQ. 422 MatrixBlanks Matrix blanks consistedofaliofbqlanukraobbittsersum extracted in the same `maastnhensameplers.Three matrixblanks werepreparedandanalyzedwiththe samples. Maiix blankscontaining endogenous levels ofanalyto that were above the LLOQ are detailed below. Tabl5e. Endogenous Analyte inRabbitSerum [Sample _TTMTOWRA TGi1ACID|PFBS | THPFOS| THPFDS |Ltoamgmi)| 0.00504|oc0es2 | 000506 |000520 | 0.00803 | [WixBik0505111| ooces | owe | ooest | oom | cous | [MxBlic0505112| oomse | ooss | coors | oomo | oow | [xB 050511:3 | oowz |oowes | ooome | come | oom | [Aveeaerfargotee ee|0onocoe|To owadse[n| oheCoAeRsAT|ohocmoges |Feoo | `Theaverageendogenousvalueswereused ocorrectthematrixspikeresponse. 423 SolventBlanks `Methanolblankswereanalyzedthroughouttheanalytical un.Analyteresponse. waslessthan % theLLOQinal cases. Surrogate PcaFliObArat(i1o,n2s-taCn]daarndds,PmFaOtSrix['b*l0a;n]kws,eraendadmdeetdhaosdsbulrarnokgsatteostevoaallulatseerthuemesxatmrpalcetiso,n `method performance. All PFOA [1,2-"*C] surrogate recoveries were within 30%, `rbeuctotvweoryorftanhgeePtFoO+S.3[4'%*0.y] Srpeeccoivfeirciessurwreorgaeotuertesciodever3y0d%a,taeixstpernedsienngttehdebseulrorwo.gate. Page8of19 e e e ---- i ------ -------------- ------------ SUENVIRONMPENTRALLOANBOOCR0A8TtTOtRYt Table6. Surrogate Recovery EC PRFeOcAo[v1e,r2y-,%C]| | RPeFcOovSer[y",0,] PRFeOcoAv[e1r,y2-,%C]|| RPeFcOovSer[y0,g%] [mmr| von| | wom[wee] [issnosostia| toms | ose | remeom| om || [[(FuicemownosswosstviztT|TM"oaoonn | | Twramm ||||rveoawsweers| |eew| |rwen|| [[CCiosmsomsnestz[[ouow[|oowm ||[| mmweorowos || svenno|w]| [samme[soe[oon | esos[am ren | [roossuss| wm | oom [77vNwow | vexTaw | Msciess | ow | ew || meaewo| eow | mw | [rvnoso1 ow 1 ew TT vases T vee TT em | [vasss|eTe [TT easess ew | ew | [runes Trew Trew ||veasses ee |ew | |e | am om Ll wew m|om [reassessTew [em || eases me ve [owas | Tow | ve |[meas ew | aw | [wages| wwTew |[Teaser we | mw | [maoo | vex | eem TTvNwsms wee | em | [maser [vex aTAZ [wagers |Teen Te | ease [ones Te | vw ow |] measses [owes | ew |om | | mowesss 113%,[om] sx [ew| ox ew| ew |ww | 4.4 Laboratory Control Spikes (LCS) Six Laboratory Control Spikes (LCS) were prepared in rabbit scrum and analyzed with the samples. Results were corrected for endogenous levels ofanalyte in the matrix (where appropriate), and are presented below. Page9of19 envmoENR TALS LAsoRE ATORY Table 7. Matix Spike Recovaries Nominal | overt | [[[siissooossssssvnnisestas|| ooomsseee ||| oooommmey | | rrweoeeom m|] Frmostiss| 300 | 200 ox | . [msosostiisa2| 306 | aus | yum | GEsacmriss || oosms || oomm [|mwwn]] bsososust | sos| aa |wm | r beosesTusa|T 203T |T 21 |. ex | Page 00019 SM ENVIRONM"ENPTARLLNAOOBOER0A5CT0O4TR4Y2 `Table 7. Matrix Spike Recoveries (continued) -- Popes | ww ] om [usososusz| or | ores [usososnss| "oor| ore [ssosostiss| 200 | 2a6 [sosossa | 20r | 280 [wsossriss| aor | 27 + 1 [isossver| oxo | oss [isososusz| oxo | oz [isososso| ooo| om [msosostis | 300 | 204 [osososisa | 300 | 30a [rsososiss| 300 | aos | mm] | am | | ao | | mw | | om | | ow | 1 asx | rw | vow | mm | om | wom | [isossusr| oon | oar x| [isososmsa[oon | om | ws | [CisosostisaTosn | om | ow | [somerset| ast | as | vos | [rsomsusa| ann |ae | wow | [hsoeosties| aur 1 sos 1 osx | remem [sosstss | 03% | om [osx | Cis|o0 ss|uos su s| [usossist| 208 | 201 | orm | [sososvsz| 200 | aes | was | [rsosossa| 200 | ase | vim | 1 % [iso|sooxos| ti onsea [to [ws|o3m0s|ias0s| too [hsosostisz| 300 | ass | vos | Tew -- 1i -- TT TT Page11010 WM EIRONUEL NTAL H LABORe ATORY Table 7. MatrixSpike Recoveries (continued) NominalConc. (ObservedConc. |e[ [Coie seoome sts[ s|| oe oome| | moe oann] || oomm |o|y Ciseostiss| o2m0 |Taona |asxw|| Coseonss| 20 | 5a | vow| ---- [rvT sososussT|T aw |Tr a81| vox | ClseossaTons 1 ow |om | ] 1 20% --Dose-- sToi--1--30--1--ax--| Cocesmon 3001300 oo | Coooomaon| 300 |22 | ax| Page 120619 ENVIRONMFERNOTIACLLTAWBOOER0A5TDOiReYs Table 7. Matrix Spike Recoveries (continued and comected for sndogenous target analytes) Coonnwieo:s oEnvdaoegmetnnou,s|| cEon"roCegaoaannioteuenr|Re Lov vm. | [[Cisegoamgsetriisstz||oosmme||oosses ||oomweenr|| oamw || vieeww || [1sosostss| ase | nsw |oer| os [oss| [wsossvsal soa | are.| ocosr | a7 |om| --r Tr + Irr TT 1 [isossrist| or |oss | oo | ome |wx| crtaci[sores|omr[ooo|oom | om | ees | [sosstisa| 200 | 200 | ooves 27 | rw | [usososusa| eer | 202 | oows am | ee | [wsossuss| 207 |20| oo | 26 | wow| --r 1 1 + 1 Tr [isosostist|ose| wos | oovess wos |assow | [isosostisa|ose|osm | oooers owe | wo | 62% [sososuss| soe | aw |oooers 206 | orm | rr ---- 1-- TT T1 LS 08051151 [isososiisz| os we | ome we | we | TO hsomosusi|s | omse 20 |ew| -- rr -- T=-- -- 11 [isossist|osz os | oose ose osx| : [noose a aoe | oows am | ame | cT--cail~nlavcriaonss.co cl+ined 3 4 leth1e97%confidence velend wbexchded1m1fri1 e NR =Not Reportedbecausemeasableamousof argsanaly werenoobserved Page 3019 --_---- ENVIRONME"NPTARL OLA0JBOER0A8CT4OTR2Y 4.5 Accuracy m`aThteriaxccsupriakceyrfeocroevaerciheasnfaolryttheartepaonarltyetde.waTshcearlecsuullattsaedrbeyptraekisnegnttheiednaTavbeler5o.aftghee Table 8. Method Accuracy for Individual Analytes [LoreTassrc are |asc] o | [NEPA 1 cow | | FesA | ex | [[mPoHrAa | eww|| | wowTT Fosa | ex "Pras[wow | | [ProA | sam |"Peis | en | [conda T sox [[ PrOS[com | [cloaca| ew ||THPFOS| <vaw | [ctiAsa[ax | [7THPFOS| ssw | Lotzase |wenTT--77 1 4.6 Sample Related Comments The extraction and analysis ofthe samples ws performed uiilizinga non-vlidated rmeectohvoedri.eTs,heanmdattrhiexcsalpiibkrearteisounlctusr,vPeFsOhoAul[d1,b2e-c"oCn]siadnedrePdFwOhSe[n*e0v;a]lusautrirnoggatthee accuracy and precisionofthe sample results. 5 Individual Sample Data Tabl9aensd 10summarize individualsampledata. Table 8. Porfiuorinated Acid Resuits | sgn |020 Joouselozoae som |sre |ozs| ose| oom [Asoo|oass [<uoa|<uoa|am |ose|ores | ome |osm| [masses | 151 [<uoa|oorse[osteo|own|oares|oss |ocetz| [Asser |156[oorss|oie|oss|ors |ox0|oar|ocaor | [Ase [oses|ocosss|omar|s72|10|oe |oes|ooose| [aesssTvsToooess| oowes|ae| as | asst |ose | aos | [Aes T vasT<uoalozo | ser|118|oss | oie| oosws | [nAseso[ores Toooes|oes |252| 196 |ota | arse | cosmo } |Tnasoe0[oom|oooses |ozto |201[ott|oxo |oa| oom | | naeos7[o4s0T<uoo|oz |ass|ost|oaw|ote| cows| | asors[osoTocossa| oasa|3c |oo |oer | ara | oom | (CrTnoaeeeoesTosasa Jlosoo(me5|8 ses | W40H2R|rooosv|eos. 0|% ome|ooxes | Page 140119 erp HLEET sn I mm Table 9. Perfluorinated Acid Results (continued) [2 oe ean om ve | ss |sr | [ager | 323 |<iioa|oouz|osss|ooeso| oosrs | come | <uoo| [TNAeos1 | 0327|<uoa]oosss|2 |osm|ow | cores |<uoa| [Theo | 108|<uoa| 023 |33m |ose |ow |ows |oom | |TnAos | 1.75 |oooese|norso|orro |006| oosso |owz|oom | [rxs0%8 [106 [cuca]ores| 200| 141 | oss | oes | oowr | [Aeosr|1:2 [cuca ore| 23s | ter|oa | oss | oows | [ToA7o00 | 108 [cuca ore| see[ort | osm |omz |ooo | [TNA70%8|oss|<uoa|oes |as| cess| oss |oosss | oo | [nasoss|100[<uoa|oars | 436 |120 | oan |ows | ooo| [Nass |oe1s | ooms|oomss |201|100 |ose | 02 | oes | | Aes |"100|cuca|ooeos| aor| te | oss |oa2e|oosr| {Thao | 211 |<uoa|ooms|a0 |ore |ozs |ous |oos| | aeoss| 127 |<uoo|oouz| 308 | 0785| o2es |oorss|ootso| [maeoss| +26 [<uoa|orn |220 |oes| ose |ome | ooo| [Thaeoe |100 |<u0a|<woo|ast|oew | oan |ous| ooss | [Twaeosa | 128 "<uco| 020| 400 |0 | ose | omr |cows| |ThAoss|oes|<uoo2| 81< |ou se o |ona|| ocore [Nasa [ore |<uoa| 01s | 447 |oo | os | ows |oome| [aeorz1110[<uoo|ozs| 319 7st| ozs 0.128 00182. [asore | 136 |<uoo | ooass|ose [oma|ooze |oot | <uoo | [Twaeomi 1[cuca]ozs | 321[oses| oa ose|ooter| [TAGS Toso[<u00|ooss|231 |oss |ore |oosss | <uwoo| [A688 oote '<uoa|oous|1s3|osto | oz |owes |<uoa| [Mean 104+ ;oout|oss | 208 |oma| oom |ows |ocms | [won "2v Too3s |oare|sr2 | 197| oses | [tow oss ooomss ous|osse|00s |oozre |oom|ootos| S eEon moeo]e r om] [oorwms |"3|o | ss |oo|a |3 | ss | 0 | sw envIROMR ENTALRisOERoC AsToOsRYs Tables. Sample Results for Addionai Peefiuorinatad and Highty Fluorinated Analytes [0[ass(goit)T[0i.0a05n01|[0a.0s0s4saT]0o.0m50e8[|s0o.1r58||s0u.1s03|fu.cau0cezao||oo.o0smus|| [[aTaesss TTu<iioo0[[oaeas{[oammees [|otseae[|a22m4 [[ccuuccaa||oorms|| [[reemsss Tu<ouinoon[[oaas|aosoinor| t11ess[|szeso||ccuuccaa||ocooorrs|| [TAs |<cuioo | ors ome |aes |tes [cuca|ose| [[wTesAsst0rTo|ocnuieo0[|oasesss|[ooomwer|aszore ||twoo7|[c<uuicaa [|o"oommes|| [[wThheonisnT|ucoua|oaurs[Tcooomee| ssesrsT|eeoo[|c<uucoao[|oooomws|| [[sTmni e TuwcoooToonws osweioo sieevs[|aiams[|cuwcoao||oooom|| [ [s im e TeeTuu<asuno [T|oaatwase[T[ooomomemn{| aaosmsa||itntese |cucuuocao[||ooooumuen||| [esr c1i0a |om [oom |202 |120 | woo|oun| [[eTsess cwuoooa[|aocuenr[|oosoamma|2t0es |8261s6|T<cuuocaa[|oomuasr || [Tess <uoa[wows|oooses |284 | 140|cca|ows | [eF mThesss i<cio ooq "opoiseer ooommoama [|eaomwT|awmet||m ccauuccaa[Toeouumsr|| [amos cuca{aie |oss| aso |21| uo [our| [{[mA Toee orrsosT[uu<cuoooo|[|ooaiimess|oosomooeemr 3aasz0e |||wase2ss|i|<<cuuuccoooo|[osoceosemts||| [som[won[ouTwos os |ani|cuca|oss| [[ATswaiezm Tucuooo[|aocwes(owooro[|1w5e5 |wszez[|<cuuiccooT|oomseer]] eyie i oesBE me en TT Page 160119 --_--m W TM ENVIROMEPNTRALOLWUAOBOEER0ASCT0O4TR4Y2 ATnaabllyet3e.s S(acomnptlienuRed)esfourAdldittionsal Perfluorinated and Highly Fluorinated FOSA| FBS Coa iy seo [odes oun] oor | a0 |oso ones] Loe Lo LanLoosLoe onoLome| [mon |" wa |omo ootees| 2s | ao| wa |oosez| [Median [wa oto |oowr|285 | was| wa |oows| [Won |oooscz|owe|oom |ae |or| wa |ome| [tow Tocessz| nos |nooss|ose |200| wa |onorm | fromerste] oyLoom ome| so {an| Lom] TT he[nCeooA rfwkmskT Fo(G + oa e 801A0S5o E TalOyRHds sarge[e3 v) [| 4%.| [ | Table 10. isomer Ratios for Individual Samples Samplo ID `Sampo Origin BFraFnOcAhe%d|| BPrFanOcSheWd isomer _| lsomer [mmo[ca[k wow e | s um | [wes TT Wes | wor| a | [mess Poweis |om | ex | [wes | Pome | iow | aes | [ow [7 e Newvas r | [owes [woe | [owes TT Vos |ax | ww | [owes wome [aww |ow | Montreal, Quebec 2m ew [me |w Wowsmows mec | 2% |ew| [wer | wecweos |woe | wm | [owes TT vem | wor | wx | [wewe -- owoms | woo | aw | [wes Gwoma | aw | aw | [mews T camms | em [ow | [wer osm | ax | aw | [owes] [ress [men] [aes [mes Cavtantia mewn mewn aomor |[asoow n| [ax| ee ww | os |om | Page 170619 e eeee eeee ------r-- ENVIRONMEPNTRALOLWVAOBOER0A6CoTOTdRY = owes be TASH Tween | ex | ae] [ vmV [ Tawe ceor [|om easw | TNABS[ T wdToe | ww | [we awed | aw | aes | [ vwemer 1 Massowsew |aoa | sew | [ower TT esses asx | aw | [wee ems [os | aw | owes 7Tem [wow | ww | [owe TT ew [woe [aw | [ rweem TT ew ioe | ww | rr 1 TT hee ame |am | ""ThTeNb-rAaLn6c9h7e7dTanodm~e6s9T7n8 aoeesfvroopmlt|ehwassa<me1ooLt0orfQpooileod senrum. |tT| aww | +*Theaverageandstandarddeviton epeecatanythosesapswithisomervaluessbovethe LLOQ. 6 Data/Sample Retention AElnlvoirriognimneanltraalwLdaabtoaraatnodrty.heTanhaelytetsitcamlarteeprioarltshaanvdebaenaelnytairccahlirveefdearetntcheest3aMndard reservesamples,aswellasthesamplespertainingto thisprojectarearchivedatthe 3M Environmental Laboratory. Reserve samples, digital copiesoforiginal data andal orginal paper data will be: retained in the archives of 3M Environmental Laboratory for aperiodof at least 10 years following report signing. 7 Conclusion Under the conditionsofthe study, endogenous fluorochemicals were found to be `present in all samples. NFPA, PFOA, Cy Acid, Cio Acid, Cy; Acid, FOSA, PFHS, PFOS and THPFDS weredeteincevtereyldotofserum. TO andPH FBSwA ere. detectedinaibutthreesamples,andtheCy Acidwasdetectedin 30of 36samples. Conversely, PFHA was only detected in 9of 36 samples, and FBSA was only detected in 1of36 samples. THPFOS was not detected in anyofthe samples using the present methodology. PFOA [1,2-C] surrogate recoveries were all within 30% `fwohriilendPiFviOdSual['a*n0a,l]ytseusrrroagnagteedrefcroovmer+i/e-s1w%erfeo a+l/l-w2it7h%inwh+ii-lo34o%ve.raMlletmehtohdoadccuracy uncertainty (based on isotopically labeled surrogate recovery) was +/- 34%. Page 180119 -- eee-------- weReRscSREAATLOERY ET WTFLER Trees ToorS Ub)Fei dd ~Ts l s2pforr/ e05" 2-- `Wikiam Reagen, Laboratory Manager /2/63fe Date "The 3MEnvironmental Laboratory's Quality Assurance Unithas auditedthe dataand report for this project. Quality Representative 12-1- 206 Date Page 90019