Document OgO9qX5mrE51nje9Vx05Y6Mv
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STUDY TITLE Extraction of Potassium Perfluorooctanesulfonate from Mallard Serum and Mallard Liver
for Analysis Using HPLC-Electrospray/Mass Spectrometry
DATAREQUIREMENTS
Analytical Method Regirements STUDY DIRECTOR Sean Gallagher
STUDYCOMPLETEDON
September 06, 2001
PERFORMING LABORATORY/ TESTING FACILITY
Centre AnaSlay3tt0ie4ca8CloRlLelaesbgoeera,actPhorAiDer1si6,v8eI0n1c. (Centre) Phone: 814-231-8032
STUDY SPONSOR
3M EnvironmentaBluiTledcihnngo2lo3gEy-0a9nd Safety Services St.Paul, POMBNox 53533133133331 PROJECT
CenCteenPtreotSotcuodlyNNuummbbeerr::0002P3--002832:042 Total Pages: 104
tr
600479
-_-- ConeSey No: 023.042
CPeoavteiroocSutnudaylionNsutmebefrrom M0a2l3a.0n4d2,Seruemtt1nedd Mal"aBdxcLtiivoern foroAfnalysPiostsUssdhunmg
HPLC-Blactrospray/Mass Spectrometry," conducted for 3M Environmental Technology andSafetyServices, wasperformedincompliancewith USEPA TSCAGoodLaboratory PracticeStandards (40CFRPart792)byCentre Analytical Iaboratodes,Inc.
Princ7ip.al avehnovterguir Cenre Analytical LaboratoriIensc,. /
SSA teumdyGDaL lingohrer z Della Wildlte Ineradana, Lic.
-- --R na L C Ta=o dan 3SMpagdEonrviRreopnrmeesoctolunTsecnologyad SueyServices
BuAso)pl BeGliolo Hal
Cot Amat Lorrie Ia.
Panation
600480
_--sy- mm--m
Centre Study No: 023.042
QUALITY ASSURANCE STATEMENT
C0e2n3t.r0e42A,naelnyttiitclaeld,La"bEoxrtartaocrtiieosn' QoufalPiottyaAssssiuurmanPceerfUlruiotroroecvtiaenweesdulfCoennattree Sftruodmy NMaulmlbaerrd SAlelrurmevainedweMdallpahradseLsivweerrfeoriAnnsapleycstiesd UfsoirngcoHnPdLuCc-tElaeccctorrodsipnrgayt/oMaCsesntSrpe.ectArnoamleyttriyc"a.l LLaabboorraattoorriyesP"raScttaincdearSdtaOnpdaerrdast.ingAPllrofciendduirnegss, wtehereStruedpyorPtreodtotcoolt,heanSdtuadlyspDpilrieccatbolreaGnodotdo management.
Puss 1 Poicol Review 2. FEoxritacitficoand,on 3 RawDawReview 4DaRfatvDReipaormtd
Review 5. FRienvaileRweport
IDpaetceed 112000 wom
121200 WB2U0
sr01
Date CReepnotreted to SDtautdey RDeipreocrttoerdatnod Management SponsorManagement
113000
122800
wave
122800
1221/00
12800
32901
Eo
arson
sot
Naomi Lovallo U (aot dont
oDlatoe r
Sr. Quality Assurance Auditor
Centre Analytical Laboratories, Ic.
Page 3of 104
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CentreStudy No.: 023.042
CERTIFQIFCAUATHTENITIOCINTY
"Thisreport, forCentre Study Number023-042, Is atreandcompleterepresentationof `the raw data foc the study.
SPurbimietnadnbvye:ntgur,C5C0oo4nn8tvRe:yeAsenosneeD!avLeibros, In. State College, PA 16801
Seen: (RQ Deke CentreAnalyticalLaboratories,Inc.
A Be uf
: hind, aronC Coatre Analytical Laboratories, Inc.FacilityManagement: CPCroesoiideBnntouin Lore;n, a.
StudyDinca, lite amt:
Aaa b Maen
`RSeaantGaellsagtheor n, Li.
Sponsor sae IM:
eA. WII.
x.ronwsi.i WE
Rs
33 Environmental Phnology andSatery Services
ConesAst Labrie.
6-ge-01 Be
lio {
Date.
fo
ve
0ho4as2
_-- mmm
Centre Study No: 023.042
STUDY IDENTIFICATION
Extraction of PoftoarsAsniaulmysPiesrfUlsuionrgooHcPtLanCe-sEullefcotnraotespfrraoym/MMaaslslaSrpdecSterroummetarnyd Mallard Liver
CENTRE PROTOCOL NUMBER: 00P-023-042
CENTRESTUDY NUMBER: 023-042
TYPE OF STUDY:
Analytical
SAMPLE MATRIX:
Mallard Serum and Mallard Liver
`TEST SUBSTANCE:
Perfluorooctanesulfonate (PFOS)
SPONSOR:
3BuMilEdnivnigr2o-n3m6e-n0t9al Technology and Safety Services PO Box 33331 St. Paul, MN 551333331
STUDY DIRECTOR:
S`WeialndlGifaellIangthemeartional, Ltd. 8Ea5s9t8onC,oMmmDer2c1e60D1rive
SPONSOR REPRESENTATIVE:
`TESTING FACILITY: ANALYTICAL PHASE TIMETABLE:
Rochelle Robideau B3uMilEdnivngir2o.n3mEe-n0t9al Technology and Safety Services PO Box 33331 St. Paul, MN 55133-3331
C3e0n4t8reReAsneaalrytcihcaDrlivLea.boratories, Inc. State College, PA 16801
Study Initiation Date: Experimental Start Date:
11/10/00 1117/00
ESxtpuedryiCmoemnptalletTieornmiDnataet:ion Date:
03/13/01 09/06/01
Centre Analytical Laboratories, Inc.
Page Sof 104
_-- Cente Stuy No 023.012
PROJECT PERSONNEL
The Study Director for this project was Sean Gallgher at Wide Intemational, Lid. Tvahreiofuoslpohwaisnegsoperstohennsetludfyr:om Centre Analytical Laboratories, Inc., were associated with
Name -- Dave Bel Melissa Keanedy Whitel
`Tiffany Proctor
Angela Morgan Michelle Armand Lawrence Ord Rickey Keller
Karen Risha.
Tile Scintis Scientist GroupTeam Leader
`Technician
Technician Techvician Sample Custodian Sample Custodian
Scientist
Centre Analytical Laboratories Ic. :
Pageof 104 00484
---- ---- ------ --------e--e-------------------- CeeStudyNo: 023042
TAOFB CONL TENE TS
Page
GQUOAOLDITLYAABSOSRUARTAONRCYEPSRTAACTTEICMEENCTOMPLIcANCEcSTcATEMENT 2
CERTIFICATION OF AUTHENTICITY ..c.ocomimsssmssssmmmsmsmssmsensmenon
STUDYIDENTIFICATION........ -- mss
-------
LIST OFAPPENDICES...
11
6.0 DESCOR FAI NALP YTIT CAI L ON METHOD....c.ccocmsmsimmsmmmssssssmmssn 14
6.2PreparationofStandardsandFOrfication
SOIUtONS............o 14
6656DQescruiptiaononafdIinEsxtraaummpelntteaCniAdIOCpHoeBrUsOntNi.ng voConditons.res 1163
90 CONCLUSIONS...
10.0 RETENTION OF DATA AND SAMPLES .......ococosmssimssmmemsmmsssssrn 19
CentreAnalyticalLaboratories, Inc.
Pa7 ogf1e04
600485
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`CentreStudyNo: 023.042
LI OF TSABLTES
TableL SummofaPRrOSyinReagent BABS...
Page 2]
Tablel. SummaryofPROS in Mallard Liver
BIAS...
22
Table Il. Summaryof PFOSinMallardSerum
BIRSKS......crcnn22
Table IV. Summaryof PFOSRecoveries in Mallard LIVE...
23
TableV. SummoafPrFOyS RecovienrMaillearsd Serum... 24.
Table VL. TSEuMmnmAaEryioODfP19ROWSEeinkAsd)ultc Liver Samm plaet0s ppo m a. (Tests 25
Table VIL. STuEmDmoDaf6PIrRWOEyOSeikSnN)Adult Liver Samples at 1.8 pprmn ai. (Tn est n 26
Table
VIIL
SummaryofPFOS in Adult TEMD6WeOekN)
Lc iver Sam mpalte6.s2s ppam.
(Test
21
Table IX. TSeurmmmianartyioofn P19FWOeSeikn sAd)ultv Liver Sm ampleast 17.6ppm ai. (Test 28
Table X. TSeurmmmianartyioofnP1R2OWSeeiknsJ)uve.nilve oLivvervSnanmmasptm0lpmpemnacsi.n(nTesst nn 29
Table XI. STeurmmmianartyioofn P1F2OWSeienkJsu)venilec Livero Sampv lesate 1.8pps m ai. (Test 30
Table XIL. STuEmMmBarAyOoNfP1F2OWSEienkSJu)vceonnivle Liver Sampleas 6.2 ppm ai. (Test
Table
XII.
TSeurmmmioafn1ParR2OWtySeiieknosJn)u.v.en.ile
Liver
Samples
at
17.6
ppm
a.. (Test mn
`TableXIV. Summaryof PFOSinControl AdultSerum
Samples.......c..vovven33
`Table XV. STuEmMmRaArIyOoNf P19OWSEEKinSA)dultv Serum Sampr laets0ppmai.s (Test 3
Table XVI. T SummEaryI ofP6FDWOeSeOkin)AN dult Seruc m Samples atv 1.8 ppm a.i. (s Test 35
`Table XVII. Summary of PFOSin Adult Serum Sampalte6.s2ppm i (Test
`TableXVIILTeSrmuimnmaatiroynof19PWFeOeSksi)n Adv ult Serum Sampn les at 17.6ppmc .i. (Test 31
CentreAnalytical LaboratoriIensc,.
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:
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CentrStudy No 023.082
LI
ABLES (Continued)
TableXIX.SSAuDmImaEr)yoc fPFOS in Adult Sero um Sampleast 17.6ppe m a. (6 Week Pa3g8e TableXX. Summary ofPFinOJuveSnile Serum Sample1s0pm a. (Test
`Table XXI. Summary of PFOS in Juvenile SerumSamplesat 1.8 ppm a.. (Test
Table XI Summary ofPFOS in Juvenile Seam Samples at 6.2ppm a. Test Termination 12 Weeks) cecum]
`Table CRRon 12Wegks) ree XXIII. Summaryof PFOSin Juvenile Serum Sampleast 17.6 ppm a.i. (Test A2 Table XXIV. Summary ofPercent Meistures for Mallard Liver Ample v.43
ConveAnyi Laborstorc ne.
Pages 104 650487
_--mm
Centre Study No. 023.042
Figure 1. Figure 2. Figur3e. Figured.
Figure5.
Figure 6.
Figure 7.
Figure 8.
Figure 9.
Figure 10.
LIST OF
s
Typical
Calibration
Curve
fOr
PFOS
....c.coceosrnsncn
Page 46
Chromatogram Representing a 0.1 ng/mL standard for PFOS ..........4T
Chromatogram Representinag 1.0 ng/mL standard for PFOS ........48
RCehargoemnattoBgrlamaAR,neSperkte:se1nt1i2n0g0a04Re)agr ent Blanko for PFOr S (Centres ID dd
0C0h0r3o8m0a3toBglraanmk ARe,pSreets:en1ti1ng2C1ont0ro0lBMa)ll.ar.d .Se.ru.mrfovr PrFrOSr(mCenstrseIrDn: s50
0Ch0r0o3m8a0t4oBglraanmk RAe,pSreets:en1t1i2ng00Co0n8t)rolr Mallard Livev r for PFOS,s (Centre ID: S|
PCPhbroofmaPtFoOgSra(mCReenptrreesIeDn:ti0n0g03C8on0t3roSlpkMaAl,laSretd:
Serum fortified 1121008)...
with
10
52
wCihtrhoPmaFtOoSgr(aCmenRteeprIeDs:en0t0i0n3g8C0o4ntSrpoklAM,alSleatr:d1L1i2ve1r0F0oAr)ti.f.ie.d.a.tc1c0v00crpprbe.n53
C00h0r8o1m4a3t,ogSproanmsRoerpIrDe:se2n3t3i2n,gSJeutv:en1i1l2e7M0al0l)a.r.d.Serum Sample (Centre ID4 :
C00h0r8o1m0a8t,oSgproanmsRoerpIrDe:se2n3t3i7n,gSJeutv:en1il1e2Ma1ll0ar0d LAiv)er.S.amvplrer(CvenetrserIDe: SS
Centre Analytical Laboratories Inc
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Centre Study No: 023-042
LIST OF APPENDICES
Page
Appendix A. SAtudEy PrDotocAoBl 0AM0DPE-VE02I3B-NO0N4.2S(CentrerSrturdy No. 023-042)and
56
Centre Analytical Laboratories, Inc.
Page 110f104
' 600489
_--m
ee
Centre Study No.: 023-042
1.0 SUMMARY
Centre serum
AsnaamlpylteiscalfoLrabtohreatodreiteesr,miInnac.ti(oCnenotfrep)eerxftlruaocrtoeodctmaanlclsaurldfolniavteer
samples (PFOS)
and in
mallard mallard
serum and mallard liver according to protocol 00P-023-042 (Appendix A).
``TThheelLiOmiQtfoofrqeauchamatnritfxowiramsatldleaatredtrlmiiivneerodwianns a1m0eptphboadnvderi1f0icnagt/iomnLsftourdmyaplelrafrodrsmeerduamt.
Centre (Centre Study: from non-quantifiable
l0e2v3e-l0s44()a.peRaekswidausesdoetfecPtFedOaSt
tinhethceormraelslpaornddliinvgeransaalmyptleersetreanntgieodn
time but pg/mL)
twoa2s2.l8esusg/tgh.anTthheeselorweessulttscoanrceenrterpaotritoend
of on
the calibration standards (0.0001 a wet weight basis. PFOS in the
`mallard serum samples ranged from non-quantifiable levels to 218 ug/g.
`T1h2e%a.vTerhaegaevpeerracgeenpterrecceonvterreycoivesrtyand+asrtdanddeavriadtdieovniaftoiroPnfFoOrS PiFn OlSiviernsseamrpulmessawmapsle9s5w%as+ 93% 10%.
2.0 OBJECTIVE s`pTehceiombejencstoivfemoafltlhairsdlsitvuedryawnadsmtaolldaertdersmeirnuemluesvienlsgotfhpeearnfalluyotriocoacltmaentchsuoldfsodneastcer(iPbFeOdSi)n in protocol 00P-023.042.
3.0 INTRODUCTION
`lTihviesrreapnodrmtaldletaaridlssetrhuemr,esuuslitnsgotfhtehaenalayntaliycsailsfmoertthhoedsdeentteirtlmeidn,at"iEoxntorafctPioFnOoSf iPnotmaaslsliaurmd
PUesrifnlguoroHoPcLtCa-nEelsuelcftornoasiperoary/OMtahsesr
Fluorochemical _ Spectrometry"
Compounds From Liver and "Extraction of
for Analysis Potassium
UPesrifnlguoHrPoLoCc-tEanleescutlrfoosnparteayo/rMOatshseSrpeFclturoormoecthreym"i.cal Compounds From Serum for Analysis
The study was initiated on November 10, 2000, protocol number 00P-023-042. The experimental
when the start date
study director was November
signed Centre 17, 2000, and
theexperimental termindaatteiwoans March 13, 2001.
Centre Analytical Laboratories, Inc.
Page 120f 104 6n0490
_--mm--m--m--m----
Centre Study No: 023-042
40 SYSTEM
``TwhaescroencteriovlemdaolnlaMradyli1v8e,ra20n0d0sefrroummuWisleddifioertInhteemmaattiroinxalblLadnk.sEaansdtomna,tMriDx.fTorhtiefciocanttiroonsl `amsaslilganreddltihveerCwenatsreasIsDiognfe0d0t0h3e80C3en.tre IDof0003804 and the control mallard serum was
ASixuty gma1l0ul,a2rs0d0it0v.erThsaemsplaemsplaensdwseixrteysmtaolrleadrfdrsoezreunumnstaimlptlheesywweerreelreocgegievdediantbCyenCternetroen spearmspolnenselanodnfoArutgyumsatlla16r,d 2s0e0r0umasnadmpslteosrewdefrreozreenc.civAend oanddFietbironuaalryt2w4e,nt2y00m1alalnadrdstloirveedr frozen until they were logged in by Centre personnel on March 1, 2001 aSsasmopcilaeteldogw-iitnhatnhdscshtuadiyn. oSftcoursatgoedryecionrfdosrmwaitlilobneckaenptbaet fCoeunntrdeiAnnatlhyetircaawl dLaatbaoraptaocrkiaegse, Inacss.oacinadtedawtirtuhetchiospsytoudfy.thestoragerecordscanbefoundinthe rawdatapackage
5.0 REFERENCE MATERIAL
ETnhveiraonnamleytnitcaall TsetcahnndoalrodgyPaFnOdSSewrvaiscesr.eceived at Centre on June 3, 2000 from 3M `Tmhaeteraivalaiwlaabslestoirnefdorfmraozteino.n for the reference material is listed below. The reference
a
Centre
IR
- fa
PFOS
00-023-042 TCROO0I746 979 0831/01
`The molecular structure ofPFOS is given below.
CPhFeOmiScal Name~~ = Molecular weight =
wIe
Perfluorooctanesulfonate. 499 (CyF11S05)
dNeortiev:edT,hisepnoetuarsasliumm poerlflueoarnocdocstutaannledsauerldfofnaotrem[fCrFo1m7wSh0i5cKh],PFmOolSec(ualnaiornw)eiisght 538.
Centre Analytical Laboratories, Inc.
Page 130f 104
650491
_--_--m--m mm
Centre Study Nos: 023.042
6.0 DESCRIPTION OF ANALYTICAL METHOD
AFnlauloyrtoicchaelmimceatlhoCdosmepnotiutnldeds"EFxrtormactLiiovneorfPfoortaAsnsaliyusmisPeUrsfilnuogroHoPcLtCa-neEsluelcftornoastperoary/OMtahsesr
Spectrometry" Fluorochemical
Canodmpo"uExntdrsactFiroonm
oSferuPnotafosrsiAunmalyPseirsflUusoirnogocHtaPnLeCs-uEllfeocnattreosporray/OMtahsesr
Spectrometry" were used for this study.
61 Extraction Procedure
pAr~oc0e.du5r0e.gAsfatmeprlefoorftlifiivceartaionndofaa1p0pr0opLriaaltieqsuaomtpolefst,htesheesraummpwlaesswuesreedvfoorrttehxeeedxftorarct~io1n5 sweacsonaddsd.edOntoetmhiellsileirtuermosfam0.p5leMs.TTBwAowamsilaldidterds tooft0h.e2l5ivMer ssaomdpiluemscaanrdbo0n.a5temi/lsloidliituemr bsaimcpalrebso.naFtievwemaisllaidlidteedrsotoftMheTBliEvwerassaamdpdleesd1a0nbdot1htmihllilliivteerrawnadsseardudmesdamtopltehse.seEraucmh samimnp.leFwoaurspmillalicleitdeorsnoftrhiset-oarcgtainoinschlaakyeerrfwoars ~ta2k0enmiannd.adnridetdhoenn8ceninttrorgienfeufvagopreo~rdat1o5r aLnCd/MtShe/nMSreecloencsttriotsuptready.with 1 milliliter of methanol. Each sample was analyzed by
62 PreparationofStandards and Fortification Solutions
SAtnaanldyatridalsLoalbuotriaotnosriewse'reproptroecpoalre0d0P-o0n23S-0e4p2t.embAenrin1d8i,vi2du0a0l0staoscksspteacnidfairedd sionlutCieonntroef P(cFoOrrSecwteads fporreppaurreidtaytaancdonscaletntcroanttieonnt)ofin10m0etuhga/nomlL.byFdriosmsolthviisngso1l0utmigon,oftah1e.0stpagnd/amrLd vforotilficuautmpiotneost1a0n0dmarLdwsioltuhtmieotnwhaansoplr.epared by taking 1mLofthe stock and bringing the Afort0i.f1icuatgi/onmlsftoarntdiafridcaatnidonbsrtianngdianrgdwthaesvpolrumee pupbatyorta1ek0i0dnmgL10wmitLh moeftthhaneo1l..0 Aug0i.m01L 1g0/0mmLLstwaintdhamredtwhaansoplr,eparedbytaking 10mLofthe0.1 pg/mLstaannddbraingringtdo
A0.s0e1tpogf/stmaLnsdoalrudtsiocnosntinaitnhiengfoPlFlOowSiwngamsapnrneepra:redbyserialdilutionofthe 0.1pgm.and
Cnitial Conoe.r (ug/ml) Volum5e (mL) Dilute1d0t0o (mL) Final Co0n0e0.5(ug/ml
01 0.1
2
100
1
100
0.002 0.001
001 001
5 2
100 100
0.0005 0.0002
:
of PFOS001
1
100
0.0001
CenteAnalyticalLaboratories,Inc.
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_--mm--m--m----
Centre Study Nos: 023.042
The stock stored in
standard solution and a refrigerator (4 +
all fortification 2C) when not
and in
cusael.ibratDioocnumsteanntdaatridosnolouftiosntsanwdearred
preparation can be found in the raw data associated with this report.
63 Chromatography `tQiumaenotiffiPcFatOiSonwoafsP~F4O.S4 mwians. aPcecaokmsplwiesrheeddebteyctLeOd MinSt/heMSconetlreocltrmoastprriacye.s cTohrererseptoenndtiinogn atlotetrheseavnearlaylteforrettiefnitciaotniontirmee,cobvuertietsheaanmdoutnhetsesdtetewcetreed lweesrsetohnalnytshiegnliofwiecsanttceanlioburgahtitoon standard (0.0001 pg/mL).
64 Instrument Seasitiviey
Tchonecesnmtarlalteiosntosfta0n.d00a0r1d
amount injected pg/mLofPFOS.
during
the
chromatographic
runhad
a
65 Descriptionof Instrument and Operating Conditions Instrument: PE SCIEX API 3000 Biomolecular Mass Analyzer
Interface: SCIEX Turbolon Spray Liquid Introduction Interface
Computer: DellUlraScanP1110
Software: HPLC:
P`WEiSncdioewxsAnNaTl,ysvtervseirosnio4n 1.1
Hewlett Packard HP Quat
P(uHPm)pSeries
1100
HP Vacuum Degasser
HP Autosampler
HP Column Oven
CHoPlLuCmCnolTuemmnp:.Ge3n5esiCs Cs (Jones Chromatography), 2.1 mm x 50 mm, 4 MoIbnjieclteiPonhVaosle.:(A1)0:pL2mMAmmonium AcetateinASTMtype Iwater MFolboiwlReatPeh:ase (B0).:3 mMLe/tmhiann.ol
Centr Analytical LaboratoriIensc,.
Page150f 104
650493
_--
Ti0me %@A %4B
12.00 00 11000
75 40
60
1.0 40
60
Centre Study No.: 023-042.
Tons monitored: PFOS negative
499599
Approximate
20
`PTuanerFialemeters C1So-nltorsoplrsay 'DPF-PD-eFcolcuusstienrignPgotPeontteinatlial
EP-Entrance Potential
DF-Deflector (CE-Collision Energy
(CXP-Collision Cell Exit Potential
CEM-Channel Electron Multiplier
42S0at00 2531000
100
70
30hd00
2800.0
NGebausliFzleorwGsas
s1a2t
CColulritsaiionnGaGse.s TIS Temperature
143 asec
6.6 Quantitation and Example Calculation
`Ten microlitersofsaomrcpaliblrateion standard were injected intothe LC/MS/MS. The
plienaekararrceagrweasssiomne)asbuyreAdnaalnydstthseofsttwaanrdeardusciunrgvesiwxascognecennetrraatteidon(susionfg s1t/axndfairt`dws.eighTtheed `tchoenecqeuntartaitoinosn bfeolrowma.llard liver (ug/g) and mallard serum (g/mL) was determined from Equation 1 calculated the amountofanalyte found (in ng/mL, based on peak area) using
the standard curve (linear regression parameters) generated by the Analyst software
perqougartaimo.nsforTsheernumEaquraetsihoonwn2).calculated the amount of analyte found in pg/mL (the
Centre Analytical Laboratories nc.
Page 160f 104
r04a9q
_--_--
Centre Study No. 023-002
EquatioIn:
Analyte found (ng/mL) =(Peakarea -intercept) slope.
Eq`uAanatliyto2en:found (ug/mL) =(anal,found(ng/mL) x FV (mL) xDF xEV(mL) 1ug
(AV (mL) x sample vol. (mL)
1000 ng
`WhDFerFVe=:= DFiinlaultiVoonlFuacmteor
AEVV ==EAxlitqrucottoVnolVuomleu.me
cForasalmpcltehsupfeolrrtciefanietdtrewcieotvhedrkyn.own amounts of PFOS prior to extraction, Equation 3
Equatio3n:
Recovery (%) = (anal.found (ug/ml) - avg. anal.inctrl (ug/ml) x (1000ng/1 g))
`amount added (ng/mL)
x 100
An exampleof a calculation usainan ctugal sample follows:
nMagl/lmaLrpdweistaehkrPuaFmrOeSsa,amwphleereC:entre
ID
=
0003803 Spk
esse
A
(Set:
112100B), fortified at
10
sinltoeprecept
-- 7sims
dilution factor =
angvgadadmetdin(fcoornttlreovlels) ==
final volume
=
0I(nNgot quaniible)
1mL
extraction volume
- SmL
salaimqpuloet vwoeilguhmte(volume) == 04.1mmL.
From equation 1:
Analyte found (ng/mL) = [6575784-0515]
From equation 2: = OfngmL Analyte found (ug/ml) = (O8n@gmmLlxx0|immlix)xSml)x10L0umgg
Centre Analytica LaboratoriIec=s,. 0.00976 pg/mL.
Page 1707104
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- _-- ----
Centre Study No: 023.042
`From equation 3:
% Recovery =
-
(0.00976ug/m1l0xn=g/0mnLg/mL)x1000) x 100
= 98%
7.0 EXPERIMENTAL DESIGN
tEawcohmastertioxfbslaanmkpslefsort(ilfiiveedr
or at
ksneorwunm)cocnocnesnitsrtaetdioonfs,onaendre~ag2e0ntsabmlpalneks,.
oEnaecmhastarimxplbelawnaks,
extracted using the appropriate method and then analyzed in duplicate.
8.0 RESULTS
`The liver
PFOS blanks
faonudndmailnlatrhde
sreearguemntblbalnaknsksaraergeivleisnteidn
iTnabTlaebsleIT
I.&
TIIh.e
PFOS
in
the
mallard
Individual recoveries for average percent recovery
PFOS in standard
the liver deviation
samples for PFOS
are detailed in in liver samples
Table IV. was 95% +
The 12%,
Individual recoveries for average percent recovery
PFOS in relative
stthaendsaerrdudmevsiaamtipolnesfoarrPe FdOetSaiilnedseirnumTasbalmeplVe.s
The was
93% 10%.
dPeFteOcSteidntathethmealcloarrrdeslpiovnerdisnagmpalnaelsyrteanrgeetedntfiroonmtniomne-qbuuatnwtiafsialbelsse tlhevaenlsth(ealpoewaekstwas rceosnucletnstarraetiloinstoedfitnheTacablliebsraVtIio-nXIsItLa.ndaTrhdes r(e0s.u0l0t0s1arpegr/empoLr)tetdoo2n2.a8wuegt/gw.eiIgnhdtivbiadsuiasl. dPeFtOecSteidnatthethmealcloarrrdesspeornudminsgaamnpalleysterarentgeendtifornotmimnoenb-uqtuawnatsiflieasbslethlaenvetlhse(laopweesatk was r`ecsounlctesntarraetiloinstoefd itnheTcaablliebsraXtiIoVn-XstXaInIdLa,rds (0.0001 g/mL) to 218 ugg. Individual
`The percent moisturesforthe mallard liver samplesare given in Table XXIV.
9.0 CONCLUSION;
t`oThpermotaolcloalrd00lPi-ve0r2a3.n0d4s2e.rum samples were successfully extracted and analyzed according
Centre Analytical Laboratories, Inc.
Page 18.01 104
00496
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CentreStudy No: 023.042
10.0 RETENTION OF DATA. AMPLE! `LWabhoernattohreifsi,naIlnr.epwoirltl ibsceomsphilpepteed,taollthoerisgpinoanlsopra.peTrhidastdaogeesnenroatteidncblyudCeefnatcrieliAtnya-slpyetciicfailc <ruabwmidtaitad.suEcxhacats cionpsitersumoefntalllrogasw, dhaotwa,evaesrweelxlacst acospiigensedofcotpeymopefrtahteurefinlaolgasnawliylticbael Lreapboorrtataonridesal,lIonrci.gianraclhifvaecisfliotryt-shpeecpiefirciordaowftdiatmae, wsipelcibfeierdetiani4ne0dCinFtRhePaCretn7t9r2e.AnRaeltyatiinceadl samplesofreference substances are archived by the sponsor.
Centre Analytical Laboratories, Inc.
Page 1907104
600497
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Centre Study No. 023.062
Centre Analytical Laboratories, In.
Page 200f 104
G20498
-
CentreStudy No.: 023-042
Table]. Sponsor ID
ta na ba ba ma ma ba ba na ma ma na na na ma ma ma ns
Summary of PFOS in Reagent Blanks
Centre D
ResgentBlankA ReagentBlakA ResgenBlnkA ResgentBlankA ResgentBlankA ResgentBlakA ResgentBlankA ResgentBlankA ResgentBlnkA ResgenBlankA ResgentBlankA RegenBlukA ResgemBlnkA ResgentBlankA ResgentBlankA ResgentBlankA RegeuBlukA ReageotBlankA
Set Number 1117004 11I700A 12000A 112000A 1I2100A 1121004 1121008 1121008 12100 12100A 1127008 1127008 O0J070IA 0307014 030701B 030701B 03080IA OBA
Extraction _Date 11/1700 111700 112000 112000 112100 112100 1121/00 121/00 1127/00 112700 112700 112700 3701 3701 3701 3701 3801 YBOL
Analysis Date T1/18-19/00 11718-19700 17202100 1202100 1222300 17223000 1723100 1172300 17282900 17282900 111722990100 3901 39/01 39-1001 309-1001 nol ET AVERAGE: STANDARD DEVIATION:
Asalyte Found (ug/g)
NQ No No Ne Ne No No No No Ne NNoe No No No Ne No Ng NQ NQ
* Duplicate injection
'NQ but
w=aNsoltesQsuatnhtainftihseblleow(eAsptecaoknwceanstrdaettieocntoefdtahtethceacloibrrraetsipononsdtianngdaarndasly(0t.e0r0e0te1nptigo/nmtLi)me
Fsotarnvdaarldu,es0.r0e0c0o1rdged/masLN)Qw,a0s.u0s0e0d05toucga/lgc(uhlaalteftthhee avvaelureaogfetahned sltoawnedsatrcdaldiebvriaattiioonn.
LOQ=0.01 pg/g for liver and 0.01 pg/mL for serum
Centre Analytical Laboratories, Inc.
Page 21 of 104 650499
I Cente Study No: 023-042
Table Il. Summary of PFOS in Mallard Liver Blanks
Spowsor Cenmtre m Ta oo0EsMBaBkEAAt TMMm oc0oEmOMBaBkKAAr MMmm oooWmoBiKBkAA Wmoa Oo0mMmOB4BmKkAAC
NuSmuber ExtDmuceion ADmatyes NDINTTOOOAA TI1V7IT0000 T/IIASG1I990N00 ILNZ0O0OAA 1122000W0 11220022100000 1I2ZI0OAA ZURII 2 122B00 OO00RRIIAA V3O%0LL 3WbooLL
AVERAGE STANDARDDEVIATION:
FouAndmyGig) 00000000235040
NNOQ NNOO NNeo NNOQ.
Table IIL. Sponsor
mwom mMem Wmma mwam 1
SummaryofPFOS in Mallard Serum Blanks
Centre D oGGoBmGkBEAKtA oOWmmB3aBkaAkAt oOoONIDBNaBkUAKAt OommSsBNUBkKAAt oCMOMOMBmBKAA'
Su Number
Eucion Dae
Amik Date
Amie Found Gul)
11221000088 T12200000 11122330000 NNoe
1I22O0OAA L2217000 1122880M
NQ NQ
1MI227700BB 112Z7U0000 11122990000 00N0e1s
OO0I0AIA 3377001 33990011 000000RmS
O00000I8B 33071m 306--100000 000000319S7
AVERAGE: STANDARD DEVIATION:
00.0000233393
* Duplicate injection NbuQt =waNsoltesQsutanhtainftihaeblleow(eAstpecaokncweantsrdaettieocntoefdtahtethcaelciobrrarteisopnosntdainndgaradnsal(y0t.e0r0e0t1enptgio/nmtLi)me
LOQ = 0.01 ggfo liverand0.01 pgforsem rum sFtoarndvaarldu,es0.r0e0c0o1rduegd/amsLN)Qw,a0s.u0s0e0d05togc/almcuLl(ahtaeltfhtehaevevarlaugeeoafntdhsetalnodwaersdt dceavliiabtriaotni.on
Centre Analytical Laboratories, Inc.
Page 2201104
-.
0500
ee
Centre Study No.: 023-042
Table IV. Summary of PFOS Recoveries in Mallard Liver
Sponsor m EY) ma = m na na nm na nm na m na EY ma mm m
Centre. n
Set Extraction Analysis Amt Number Date Date Added (ng/g)
0003804SpkA_1I700AD 1/17/00 11/19/00 0003804SpkA* I1I700AD 111700 111900
10 10
0003804 SpkB 111700A 1/17/00 118-1970 50
0003804 SpkB 11I700A 1/1700 11/18-19/00 0003804 SpkA 112000AR 112000 1122000
50 100
0003804SpkA II2000AR 0003804 SpkB 112000A
112000 112000
1122/00 11202100
100 4000
0004SpkB 112000A 0003804SpkA 112100A
112000 11202100 12100 11222300
4000 1000
0003804SpkA 1121004 II2100 112223000 0003804 SpkB 112100AD 1121/00 1127/00
1000 20000
0003804SpkB* 112100AD 0003804 SpA O3080IA
112100 JBOI
112700 30
20000 20
O003804SpkA* O30S0IA IBOI 3101 0003804 SpkB 03080IAD 801 31-1200
20 200
0003804SpkB_O30801AD _ BOL 311-1201
200 AVERAGE:
STANDARD DEVIATION:
RELATIVESTANDARD DEVIATION:
* Duplicate injection
LOQ= 0.01 g/gforliver and 0.01 pg/mL for serum
% Recovery
9 id 85 " 14 ns 106 107 [3 8 % 8 2 2 107 101 95. 11 12
Centre Analytical Laboratories, Inc.
Page 23 of 104 600501
JE
CentreStudy No.: 023-042
Table V. Summary of PFOS Recoveries in Mallard Serum
Spomsor D
Centre
St Number
Euncion Date
Amps Dae
AddedAmotpml)
Reco%very
mmoe DOOOMMDISSEAAS 112201000088 1122110000 11122330000 1100
%9%
mmoo OO003M0OIISSKKBBe 11122000088 11122110000 111122330000 0000 au
mmoo OOOOMMDSIKSAEA 120000AA 1122770000 11122829S00 1100
aw
Wmme
OGSOIOIISSKKBDS 11227000AA
12700 ZO
111228822990000
10000 10000
9 1
Mmmo CGMOMJIGSESKKAA 112277000088 11122770000 111122990000 550000
99
mwom OOOMMOSBKB 1122/700003 112270000 11229000 110000000000
mmoo OGOOHMGGSSKKAAC OGOOIAA 3370011 3390010 110000
"
mmoo OOXIMSOIKSBK*B OOOT0IAA 33770001 33990001 11000000 FY
mmoo OOONMMOIISSKKAA?Z OO7700 33770011 3395-11000011 110000
%%
m na oom BSKSpEkB22 0000000188 337001 33S8o0n0i1 11000000 uuss
STANDARD DEAVVIEARTAIGOEN:: 9121
* Duplicate nection
RELATIVE STANDARD DEVIATION: 12.
LOQ=0.01 ug/gforliverand 0.01 pgfomrser.um
(Centre Analytical Laboratories, nc.
Page 240f 104
650502
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CentreStudy No. 023-042
Table VI. Spomsor Toe 119966120 19620 1963 19630 1964 19640 15657" 119966560 196% 1967 1 19670 1968 19680 1969 19690 1970 & 19700
Summary of PFOS in Adult Liver Samples at0 ppm a.i. (Test Termination 19 Weeks)
Centre 0008006 00000088000067 0003007 0008008 0800s 0008008 0008005 0008010 o0o0o0s8o0t110 ooosor1 oooson2 oooson2 000013 0008013 000801 0008014 0008015 o00so1s
set Number TOA HHIOTOA0A WIT00A HIT00A MITA WIA NIA HOA IWIITAA WT0A IWIT700AADDDD HIT0AD HI0AD II70AD NI0AD UIT0AD LIT0AD
Eataction Date
Ambys Date
A700 00
1T1I1B8I1990000
1/700 W700
I1V1I1B8I1S90000
IAT00 A700
11V1I8B1A990000
1A00 ATO
1IAABIR90I0
NATO A700
11118s1i990000
11/770000 1I1A8B1S90000
1100 ATWO
112000 112000
WATO0 A700
111900 11900
1AT00 1700
111900 11/1900
11700 W700
11/1900 11/19/00
AVERAGE:
STANDARDDEVIATION:
Amite Found (sg 0000813 00000000756039 0000631 0000537 0000887
000ISS 000iST 000110 000i 00000044362 oss osu 0238 0246 ous 0106 0358 0343 00.241398
* Duplicate injection LO=0Q.01 g/gforliavnde0.r01 g/fomrseL rum
Centre Analytical Laboratories, In.
Page 25 of 104
Gn0503
SE
Centre Study No.: 023-042
Table VIL. Summary of PFOS in Adult Liver Samples at 1.8 ppm a.i. (Test Termination 6 Weeks)
`Sponsor
Centre
D
D
EE0011-00226633:2211006655% #01003108378700
E01-0263:2106/+6 0103871
E0LO263-21066* 0103871
01026321067 0103872
EOL0263:21067 0103872
E01-0263:21068 A' 0103873
EE00LL-0022663321:026180%469
0103873 0103874
E0L026321069% E01-0263:21075 +
0103874 0103880
E0L0263:21075 0103880
E0L026321076 = 0103881
E0L026321076% 0103881
E0L0263:21077 0103882
E0LO26321077% 0103882
E0L-0263:21078 0103883
E0L026321078% E010263:21079
0103883 0103884
E0L0263:21079 0103884
set Number 030801AD 030801AD 030801AD 030801AD 030801AD. 030801AD. 030801AD. 030801AD. 030801AD 030801AD 030801AD. 030801AD. 030801AD. 030801AD 030801AD 030801AD 030801AD. 030801AD 030801AD. 030801AD.
Extraction Analysis
Date
Date
mor 31-200
or anton
wor 3200
wor 31200
wor 3100
yor 311200
wor 311200
mol aol
31200 3200
wor 3nL26l
wor 30
wor Inne
gol 32
wwol L100
Iwol LI20l
ol L101
wor nwo!
amor 320
or 311200
301 3AnViEiRzAoGlE:
STANDARD DEVIATION:
Analyte Fouad (igg)
0359 0350 0647 0631 0386 0880 211 204 022 0232 0317 0326 0219 0230 0194 0197 036 030 0.0893 00888 0.535 0574
* Duplicate injection O=Q 0.01 g/gforliavnde0.r01 pg/fomrseLru.m
CentreAnalyticalLaboratories,Inc.
Page260f 104 650504
ee
Centre Study No.: 023-042
`Table VIIL Summary of PFOS in Adult Liver Samples at 6.2 ppm a.i. (Test Termination 6 Weeks)
`Sponsor D
E0L0263:21070 E01-0263:21070 E0L026321071 E0L0263:21071% EOL0263:21072 E0L0263:21072% EE0OLLO02266332211007733* E01026321004 EOLOZ6321074% E01-0263:21080 E01-0263:21080 EO1-0263:21081 EOL-0263:21081 E0L026321082 EOL0263:21082 EEO0LI0022663:32211008833* | E010263:21084 Eolas zion
Centre D
0103875 0103875 0103876 0103876 0103877 0103877 0103878 0103878 0103879 0103879 0103885 0103885. 0103886 0103886 0103887 0103887 0103888 0103888. 0103889 oioassy
set Number 030801AD. 030801AD 030801AD 030801AD 030801AD 030801AD. 030801AD. 030801AD. 030801AD. 030801AD 030801AD 030801AD. 030801AD. 030801AD. 030801AD. 030801AD 030801AD 030801AD 030801AD 030801AD
Extraction Date
Analysis Date
Auaiyte Found(sg)
301 311200 104
01 31200 101
ol 3nLizon mol 3-200
0963 0507
mol 32 wor 3200
192 181
wor 320 0791
mor 31200 0827
sol Inno 128
wel Iwol
3me0n L200
134 100
ol 3L20n 1.03
01 31200 00614
wor 3nn0l or Intnl
00578 0473
mol 3200 0517
301 31-200 1.66
gol M1200 1.52
01 ViL1200 00862
OL
yil1201 00878 AVERAGE: 0.920
STANDARD DEVIATION: 0576
* Duplicate injection LO=0.Q01pggforliverand0.01 pg/fomrseLru.m
Centre Analytical Laboratories, Inc.
Page 27of 104 650505
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Cente Study No: 023.042
Table IX. Sponsor
1O91T0T 12 020 1393%0 1l0o9s40er 191995s+ 11399960 19097s+ 11099988+1 1939990 . 2a00000.
ee
Summary of PFOS in Adult Liver Samples at 17.6 (Test Termination 19 Weeks)
cerne Gowmee WGoomon GWoolwss oooooosostosis oooooscmz0 proe z oooosoczmz ccaoossoozss Gwoomwas ooonoaocanenss
emSbuer TN0AADDD IN0IAOADDDD T00OAADDD WWoieoAADD WWwIoAADD UWi0wAoDADD WWooooAADD WWiooAADD N0IAWADDDD NLiooaeAdD
EaDmaeon ADmaites WiViK0 11122000m0 IWAATTOO 111122000000 IIVATNNOO 111122000000 nwaimwoo 111919k00 0 00 1111s900 1MA7N0D0 11122000000 1w0o 1199 07000 111119900 WNATTOO 111122000000 ntimoo 1iinsewd STANDARDDEVaIvAeTmIaOeNs:
ppm a. FoAunmdiGeg)
11569 z2s9 626 2rmy 5360 1n2s rses i2n6 115651 ssoin 69s57
* Duplicate injection
LO=0Q.01pg forliverand 0.01 pg/fomrseLru.m
CenteAnalyticalLaboratories, Inc.
-
Page2807 104
G20506
---------------------------------------------- Cente Stay Noi 023.062
TablXe. Summary of PFOS in Juvenile Liver Samples at 0 ppm a.i.
(Test Termination 12 Weeks)
Spar Core
ZDDoooecT wwooownns
noe coms
a23o0e3 00c0o80m8s8
mB20eo5e4 0cw00oe8ms08sw9
2ZZ0oo7n 00ow0w8m0s90
mTBieaerr
woamn wows
NuSmuber BuDnaiion ADmaites roAmmiae)
lmiomonn lmoa
Taawvem nwaomnamn mw mao
NNeo No
loa low noam Ne
med 1120004 l11o20w0e0 loam 1120-21100 NNeQ
1ll1mm2w0ee0d0n4 m1l12o0w0w0 1an12m0-a2m1n10o0 NNNQeo
1ll1m2m0o0sk04 lowe
1al2o0w0w0 mw
1no12ao021mm00 naw
NNNeeo Ne
lmmwwoaa mumme mnaoaamm NNoe
216%
0008093
112000
112000 1120-2100
No
B8i1e77 00c0o80m9e4. D0a2e0 oom 0008095
mwa 1120004 1n12m00e0 pam 11202100 NNoe 1u12m00a0 1u12m00e0 1wA12Vo0E-2nR11Am0G0E NnNoOO
STANDARD DEVIATION: No
+ Dut ston NbuQt.waNsoetsQutahnainfihaeblleow(epstecaoknweaesnrdteocniofdthtethcealciborrarteisopnosnidainndgradnsal(y0t.e0r00t1egiofn i)me
LOQ=0.01 ug/g for liver and 0.01 pg/mL for serum
For values recorded ss NG, 0.00008 g/m.(lfte value ofthe lowest calibration
`standard, 0.0001 pg/mL) was used to calculate the average and standard deviation.
CarreAnalytica Laboratories, nc. -
Page 2907108 650507
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Centre Study No. 123.042
Table XI. SummoafPrFOyS in Juvenile Liver Samples at 1.8 ppm ai. (Test Termination 12 Weeks)
`Sponsor 2522 220 2m 2m3s0 22s6t 2236208 20 230% 2300 am1e 7 2m F 200 ame 30 234 2340
CePnytre 208096. 0008096 0008097 `00000088009978 00000088009998 0000088019090 008100 oousiol ooasior 00000088110022 0008103 0008103 0008104 008104 0008105 0008105
Nusmebter EDxtartacetion AnDaaltyseis FoAunnadly(tuegg
200A U2000A
12000 11202100 12000 11202000
000s 000458
L2000A 12000 11202000 00012
1L22000AA 1122000000 111220022100000 000000112590
DUZ20000A
1122000000 111220022010000
000lst 000236
UU220000AA
1122000000 111220022010000
000245 000167
N2000A L200A
12000 12000
111220022100000
00o00o1l6s5s
200A U20A
12000 1200
12020 120200
0cois2 00009
I000A 12000 1202000 0000763
200A 12000 11202100 0000425
U200A 12000 1202000 0000430
000A 120GO 120200 0000969
JOA 12060 120200 0000966
I2000A 12000 1120200 000386
200A 112000 1202000 0003s
AVERAGE: 000189
STANDARD DEVIATION: 0.0126
* Duplicate nection
LOQ=0.01 g/gforliverand 0.01 pgf/orsmerLum
Centre Analytical Laboratories, Inc.
Page 3007104
650508
Sy
CentreStudy No.:023-042
Table XII. Summaryof PFOS in Juvenile Liver Samples at 6.2 ppm a.i. (Test Termination 12 Weeks)
Sponsor n 2335 7
23350 2336 2336 337 237 238 238 239 23390 241 7 241 na nae 243 2430 24 nur 2346 246
Centre
0008106 0008106 0008107 0008107 0008108 0008108 0008109 0008109 0008110 0008110 0008111 o0os111 0008112 0008112 0008113 0008113 0008114 0008114 o00si1s 0008115
set Number T12100A 121004 1121004 1121004 1121004 1121004 1121004 121004 1121004 1121004 112100A 112100A 120A 1121004 112100A 1121004 1121004 121004 20000 2000AD
Extraction Aualyss
Date
Date
T2100 1122300
12100 11222300
NRO 11222300
HAO 11222300
N20 11222300
NRIN0 11222300
NO 122300
UZI0 1122300
UZI0 1122300
12100 11222300
1200 11222300
H2U00 1222300
H2I00 11222300
N20 12223000
M2100 12223000
N2U0 1222300
1200 222300
12100 11222300
1200 112700
112000 1/2100
AVERAGE:
STANDARD DEVIATION:
Aualyte Found(lg)
0.00197 0.00200 0.00377 0.00378 0.00380 0.00363 0.0055 0.00835 0.00840 0.00518 0.00306 000313 000312 000320 000329 000332 000402 0.00405 00141 00146 0.00482 0.00341
* Duplicate injection LOQ = 0.01 ug/g for liver and 0.01 pg/mL for serum
Centre AnalyticalLaboratorics,Inc.
Pag3e1 of 104 600509
CentreStudy No. 023-042
`Table XIIL Summary of PFOS in Juvenile Liver Samples at 17.6 ppm ai. (Test Termination 12 Weeks)
`Sponsor Centre
D
I"
247 Foose
2470 oootis
2 Foon
240 0008117
88 F 008118
2830 ooos11s
210 ooos1s
21840 oasis
BSN o0omi20
dBsNs cooosio2nl
ase o0os121
sss oon
2s
ooo
zoe oo
2590
0012s
260 ooos2e
2600 o0asi2e
2B630M ooooosB1ia2ss
set Number 21000 121000 121000 I2100AD I210AD 121000 21000 121000 120A 12201000A0 121000 I2100AD 121000 121000 N20AD TAA 200A 1N22110000A0D
Extrction Date 12100 20 UZIBO 120 U2IR0 20 120 U2IO 1210 112200 120 120 12100 1i2100 120 1210 1210 1u2a0e STANDARD
Asi Date __ 12700 112700 112700 112700 112700 112700 112700 112700 12230 112122370000 112700 112000 112700 112700 112700 122300 122300 111122770000 AVERAGE: DEVIATION:
Assiyie Found (up)
00383 oms10 00456 00465 00234 021 oom ois 00110 0000160156 00629 oo17s 001 ool oon 00063 0006s ooooism1 0.0262 0.0168
* Duplicate injection
LOQ=0.01 ug/gforliverand0.01 pg/fomrseLru.m
CentreAnalyticalLaboratories,Inc.
Page 3201104
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------ ----------------
CentreStudyNo: 023-042
`TableXIV.Summary of PFOS in Control Adult Serum Samples
Sponsor D
E0I-026321005 A E01-026321005 EOI-0263-21006 E01-0263:21006 EOL-0263:210077 EE00LI02266332211000078%y E0L-0263:21008 E01-026321000 A E01-026321009% E0I026321025F B010263:21025% E0I026321026 EOI-0263:21026* EO0L0263:210277 E0L0263:21027% E0I026321028 EDI263:21028% E0I026321029F EOLO263:21029
Ceatre m
0103810 0103810 0103811 0103811 0103812 0103812 0103813 0103813 0103814. 0103814 0103830 0103830 0103831 0103831 0103832 0103832 0103833 0103833 0103834. 0103834
set Number 0307014 0307014. 030701A 0307014 0307014 030701A 030701A 030701A 030701A 030701A 0307018 0307018 0307018 0307018 0307018 0307018 0307018 0307018 0307018 0307018
Extraction Analysis Analyte
Date Date Found(sgiml)
301 3901
0.0463
m1 3901
0.0455
m1 3901 0.00828
301 3901 0.00528
3m 3901 0.00984.
nm 3901
00103
nm 3901 sams
301 3m01 0.00452:
301 3901 000423
m1 3901 000616"
or 3s-oo1 0.00285
ol 39-1001 0.00207
nol 38-001
No
or 3s-1001
No
ol 3-001
No
ol 35-1001
NQ
or 39-1001 000428
ol 3so0l 000265
or 39-001 wL___39-1001
NNQo
AVERAGE: 0.00797
STANDARD DEVIATION: 0.0134
* Duplicate injection. 'NQ=NotQuantifiable (Apeakwas detectedatthecorresponding analyteretentiontime `butwas lessthanthelowestconcentrationofthecalibration standards(0.0001 g/mL)
Forvalues recorded as NQ, 0.00005 pg/mL(halfthe valueofthe lowest calibration standard,0.0001pg/mL)wasusedtocalculatetheaverageandstandarddeviation.
LOQ=0.01 ug/gforliavnde0.r01 pgf/orsmerLum
Centre Analytical Laboratories, Inc.
Page330f 104 00511
--_--_--mmmm---
CentreStudyNo: 023-042
Table XV. SummaryofPFOS in Adult Serum Samplesat 0 ppm a.i. (Test Termination 19 Weeks)
`Sponsor D 1961 m
1961+ 1962 F 19620 0 1963
191693640 19640 1965 11996656% 196% 1967 1967 1968 1968 1969 1 11996790 F 19700
Centre m
0008026 0008026. 0008027 0008027 0008028 00000088002289 0008029 0008030 00000088003310 0008031 0008032 0008032 0008033 0008033 0008034 00000088003354 0008035
set Number 1121008 1121008 1121008 1121008 1121008 121008 1121008 1121008 1121008 1121008 1121008 1121008 121080 121008D 121080 1I21008D 121008D 12008D 1200BD 1I21008D
Extraction Date nao UI uz 12100 120 1200 HZU0 1210 Hz nao 120 ZI 12100 12100 L200 12100 12100 L200 12100 12100 STANDARD
Aualysis Date 123000 11723000 1123000 1123000 12300 112300 1172300 1123000 112300 112300 112300 112300 117272800 1127-2800 11272800 1127-2800 1127-2800 1127-2000 1127-2000 1127:2800 AVERAGE: DEVIATION:
Analyte Found (ug/ml)
0.00605 0.00594 0.00494 0.00501 0.00844 000825 0.00798 0.00761 00104 00103 00358 00357 611 602 380 381 0843 os
141 138 122 243
* Duplicate injection
LOQ=0.01 g/gforliverand0.01 pgf/orsmerLum
CentreAnalyticalLaboratories,Inc.
Page 34.0 104 650512
650513
Gn0514
EE
Centre Study No.: 023-042
Table XVIII. Summaryof PFOS in Adult Serum Samples at 17.6ppm ai. (Test Termination 19 Weeks)
SponDsor CaDre NeSstbr BuDunsd ADuubee pomAsme
oe Tm ceowes EE omy
iTawlnon>s mid
Tmaeei hei
Tnaiweeo aww
6ar0
oDeSM oe
wmeosks wows
lucmdd mlwn>
Nm2ao0 210
haaakkwoo
o1s le
oImerF wwoow lw2iodwd m1a2w0o0 haoswoe soamee
1199955nM oo 0008040 11i2o10w0DBD>D ni221100 1ha2w8e0o0 l18m2
r14 5e969+ F
00wo08w0i4e1 woo
1mm1o2e1w0o0DB>D>D izowD>
aw12ai1em0 mai
1ow1aw2n8e0e0 name
a2a1un8 ai
o119n9989F4 00oo08w0o4s3
to
wots
1mm1ii21ww00ooB>>DD 1m1o2o1i/i0e0 umd 1200
1n1na2a8m/w0oe0 hase
11l5ss6 ler
e 20 00 owoutss mGaowpda huoauws doaweew amsm --
+Dts jcion
STANDARDDEVIATION: 650
LLOQ =0.01 pg/gforliavnde0.r01 pgf/ or m serL um
CentreAnalyticalLabrsicrie nc.
Page 7of104
||
600515
--_--_--m ---- -- ----
`CentreStNuo.0d23-y042
`Table
XIX.
SummoafPrFOyS in Adult 2.0. (6 Week Samples)
Serum
Samples
at
17.6
ppm
Sponsor CaIDte NeSmbter
EEOOLLO022663321:022100030 00110033882255 OG3S0O8800I1AADD
E EOLO 2632I102&1 O010I38E26 O000T700IIAADD
EEOLMO26Z322002020mmM 0O1l083277 OG30O70OIADD
EEDOLLR0S2I26I3022130243 0O1I0O3I88 OG007T00IIAADD
EEOOLLO2O663322110204204 001100383299 0G3S0O800IIAADD
EEOULL262362310241000 O0IlO0SSMMSS G03007700I1BBDD
EEOOLLOO2266332210140141= 0011003366 0G3007700I1BBDD
EEDLIOD62I623I201020002
00347 OMT
003007700IIBBDD
EEOOLLO206236231201630*63 00110033488 0G30077001IBBDD
E E0La 0263u2104 o010s38s49 oG3w0m7i01BBDD
----
-
*Duplicatenection
ExDtueon ADmaytss 33770011 n3-t12o0 3370001 snio000t1 33710 annoont a37r0n1 sarnioo0t1 337011 nnttoo 33770011 3nIoo111i0o11 33770011 0011110010 3370011 nee1i1n0 3370011 noet1i0o1n a3/o70r1 o30u-1t01 ST--ANDARDDEVAIVAETRIAOGNE::
LOQ = 0.01 g/gforliverand 0.01 pg/mLforserum
FounAdsaGiyyinet) 11816 11521 115576 113387 9212 Q5l9 9p2y 10578 318s 1"414 76859
J `CentreAnalyticalLaboratories, Inc.
Page 380f104
Gn0516
Centre Study No.: 023-042
Table XX. Summaryof PFOS in Juvenile Serum Samples at0 ppm a.. (Test Termination 12 Weeks)
`Sponsor D 201
2010 B02F 200
220003 205M
208 207 20 208M
208 21M Bur BI6M 23160 BI 217 20 F 2200
Ceatre o
0008126 0008126 0008127 0008127 00000088112288 0008129 0008129 0008130 0008130 0008131 0008131 0008132 0008132 0008133 0008133 0008134 0008134 0008135 0008135
set Number 112700A 1127004 112700A 112700A 1127004 112700A 112700A 1127004 127004 112700A 12700A 112700A 1127004 112700A 1127008 112700A 127004 112700A 112700A 112700A
Extraction Date 112700 1n22m0e0 0200 12700 12700 10200 0200 12700 12700 102700 12700 12700 12700 12700 12700 12700 12700 1200 1127000 STANDARD
Analysis Dats 117282900 11117228822990000 11282900 11282900 11282900 117282900 11282900 11282900 128900 11282900 11282900 11282900 11282900 1282900 1282900 1282900 1282900 1282900 11282900 AVERAGE: DEVIATION:
Aualyte Found (ug/ml)
NQ NNQo 00N0o4S 0.00453 No No 000278 000272 No No No No 0.00381 000379 0.00626 0.00601 0.00141 0.00153 0.00190 0.00022
* Duplicate injction 'NQ =NotQuantifisble (Apeakwasdetectedatthecorrespondinganalyteretention time `butwaslessthanthe lowestconcentrationofthecalibrationstandards(0.0001 pg/mL)
ForvaluesrecaosNrQ,d0.0e00d05pg/mL(halfthevalueof the lowestcalibration standard,0.0001pg/mL)wasusedtocalculatetheaverageandstandarddeviation.
LO=0.Q01 g/gforliverand0.01 pgf/orsmerLum
CentreAnalyticalLaboratories Inc.
Pa39g0f1e04 600517
--------------eeeen.
CentreStudy No. 023-042
Table XXL. Summary ofPFOS in Juvenile Serum Samples at 1.8 ppm a. (Test Termination 12 Weeks)
Sponsor D 22
220 25M 2230 mse mse
2232660 2M 0 200 2300 2m a1 nn ae ZF
230 2213440 M
Centre D
`0008136 oasis ooomis7 o00n137 oon ooosi3s o0o0o0m8i1s399 oso o0osia0 ooostat o00m1a1 ose 00812 0008143 0008143 oon ooostes ooooosontiadss
set Number
ExDtaratcetion AuDaaltyeis FouAnsdsGiyjtmel)
200A 200A
112700 ne
1282900 nos
0046t 0mm
H20A 270A
nT 12700
u2s29M0 zea
0mm oom
200A 270A
L270 D270
128290 12s2900
00497 004s)
2U702A U122700 1122882299000 0000116s0
UD uD
120 uAMO
129300 125300
029 0250
UZOA H200A
AO 12700
12E29M0 1282900
0007 000m7
200A 1270 128290 ool
H270A 120A
12700 1270
1282900 28290
000998 ool
200A UIA
L200 u2M0
128290 I2s290
00110 0039
100A 120A
UZI0 12700
1220 1282900
003 005s
120A 120 1A1V2E8R29A0G0E: 0o.o0s5s0s7
STANDARDDEVIATION: 00701
*Duplicate njction
LO=0Q.01 g/gforliverand0.01 pg/forsmerLum
CentroAnalyticalLaboratories, Inc.
Page 400f 104
00518
----
CentreStudyNo. 023-042
`Table XXII. SummaryofPFOS in Juvenile Serum Samples at 6.2 ppm a.i. (Test Termination 12 Weeks)
`Sponsor D
Contre D
set Extmcton Amys Assiyie Number Date Date Found g/ml)
Ws r ase
000sles o0aslas
27008 n20B
ZIm0 ZI
11250 11290
00159 00162
BF 26
oo0mier 0008147
127000 U20D
u2M0 UZM0
1293080 1293080
ois 012
2p 237+
0008148 oases
12D uD
uAM0 name
230M 2am
01s om
22380A0 0o0a0s81i4s9
1UZ2ODD 21m200 11228S3I0M000
00ss 00592
2PM mee
000m) 000810
120d U200D
120 L200
1293000 11293000
00889 0040
2A ooonist 2410 o0osist
20D uEM0 1293000 00sS6 12D 120 1230W 00sss
22 Bar
Foon ooon1s2
208 uZos
umm amo
112900 11290
00380 00383
26M ons 2430 o00sts3
127000 12700
12700 1293000 2M 230
00700 0077
Bu 2040
oooniss o00s1ss
HID 12D
1200 ua0
129300 1293000
006% oosss
246 23460
ooomiss oasis
UZ 2008
ame 1mm
112sM0 1s
00371 oor
:
AVERAGE: 0.0734
STANDARDDEVIATION: 0.0466
* Duplict njcton
LOQ=0.01 ug/gforliver and0.01 pg/fomrsLeru.m
CentreAnalyticalLaboratories, Inc.
Page41of 104
650519
_--_--nmmm
Centre Study No. 023-042
`Table XXIIL Summary of PFOS in Juvenile Serum Samples at 17.6 ppm ai. (Test Termination 12 Weeks)
`Sponsor D 247
247 248 F
2480 653 F 28530 2354 2840 285M 23850 BM 287 258 F 258 25917 2890 260M
260 26 A 263
Ceatre D
0008156 0008156 0008157 0008157 0008158 0008158 0008159 0008159 0008160 0008160 0008161 0008161 00162 00si62 0008163 0008163 0008164 0008164 0008165 0008165
* Duplicate injection
set Namber 1127000 1127000 1127000 127000 1127000 1127000 1127000 127000 127000 1127000 1127000 NZD 127000 127000 127000 1127000 1127000 1127000 1127000 127000
Extraction Analysis
Date
Date __
12700 11729-3000
102700 11729-3000
1200 11253000
1200 11293000
1200 2M
1129-3000 1129-3000
20 1129-3000
name 11293000
1200 1129-3000
1200 1129-3000
12700 1129-3000
U2 1128-3000
1200 11253000
020 1129-3000
120 11253000
120 1129-3000
270 11293000
nzmo 11253000
120 11293000
12700 11729-3000
AVERAGE:
STANDARDDEVIATION:
Auaiyte. Found (ig/ml)
0490 0496 0.150 0156 0894 008 0591 0621 03% 0384 0347 os47 os12 0517 0402 0404 [2 0514 0439 0434 0.456 0.184
LOQ=0.01 g/gforliavnde0.r01 pg/mLforserum
`CentreAnalyticalLaboratories,Inc.
| Page420f104
600520
--
CenteStayNo 023042
`Table XXIV. Summaryof Percent Moistures for Mallard Liver
SamplesSpoor
CoDur otAvesne
vToe wwonos m68a7
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mmo owosws iiee
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7me0 as
mmn2 oowmse ne
Dmun waowwns aos
ms won 117
CentsAnayaLaboratori ne.
Page 3a104
600521
_--
CentreStudy No: 023-042
`TableXXIV (cont'). SummaryofPercent Moistures for Mallard Liver
Spoor
Samples Care
Aversge
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Ds Masare
mnye wwowm 6677
2239 owoommo e7ss
nnae owmw mm2s
znus owosm m62e
wnso oooommiss 77s
znss owoomm mm23
BBus oooomm eesn
nBmw oowmn2 ums0
BBHe oowosm mesn
loBese oooomos 7Tasn
EBoll2a6mzIe0s6 oOoOSn 82140
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758 m2
EBlleen oowwss
74 71s
BBiIgSs oolwees 71s
EBlmaesl ooums 87277
EBllmearns oowwes T7i1s9
E Bie as oososm 76630
BBLomlee0ns oow0ss mT2e
EElLsIe oolss 786174
Enosioion ows m3
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Figure2. Chromatogram Representing a 0.1 ng/mL standard for
PFOS
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Page 4700104 600525
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BEEEEE. omOW
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