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AR226-194T
STUDY TITLE Exiacion of PoftoarsAsniaulmysPiesfUlsuicnrgoHoPtLaCns.uEfloenaotseprfaoymMMaaslslaSrpdcSceuroummeannd Millard ivr
DATA REQUIREMENTS
Analytical Method Requirements
STUDY DIRECTOR
Sean Gallagher
STUDY COMPLETED ON September 06,2001
PERFORMINGLABORATORY [TESTING FACILITY Centre AnaSlyu3t0ti4ca8CloRlLleaesbgoee,raactPhoAriDer1si6,v8eI0n1c. (Centre) Phone. 614.231.8032
STUDY
SOR
3M EnvironmentaBluiTlecihnngo2l9og6y.0a5nd Safty Services St.PaPulOBMoN 535313359133331
PROJECT
CenCteonPreotSocuoldNNuombmebre:r0002P5--002453.042
Total Pages: 104
CoOiINt
CenSeayNo: 023.062 HCPPeaLcuCmcErloeoccSraotnscypsrlafyoMNnauasmeebreSrpoemctrMo0aml2elt0arr0yd,0"Sceoanendoett1teneddd fMoarll"3aBMrxdwEaLacivtviieorrnoufmoreaoAafnlsTlePycoehuocUslssoiugnmsg
andSafety Services, wasparformedincompliance withUSEPATSCAGoodLaboratory Practice Standards (40CFR Part 79 by 2 Cen) tre Analytical IabaratoreIsnc,.
PCreiinnltcyiepRaA.lsveatyTlpge)kernLoarbratrion, Lc. ;
SA en Gal llgher f Dlg SWtiuldydDlinIcnteomraions Lic
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MEponnvdeirroRuepmreensaelntTa echnoanldSoagftyy Services
Alo, pl Date.
BeGio
Cant Analyte Libros
Pgsaation
0ROAST
_--
CenteStdy No: 023082
QUALITY ASSURANCE STATEMENT
C0Se2en3rt.ur0me42Aa,nnadelnyMttiaitlcllaelad,rLda"bLEoixrvtaertarocrtfioierosn'AnQoauflaylsPiiotstyaUAsssssiiunurgmanHPcPeeLrCfUl-nuEiotkrcorotecrvtoiaesnwpeesrdualyfCMoennaatstrsee S`fpSrteoucdmtyrNoMumaemltblrerydr ALLlaalbboorrraaettovoririeyewsPe"rdaScttpaihncadesaerSsdtaOnwpdeaerrrdeast.iinngsAplPelrcotfceiedndduifnrogers, wtcehoernedSutrcuetdpyorPatrceocdtoortcdooilnt,hgeanStdotualCdleynaDtpiperl.eicctaAobnlrselayGntodioa(dl0 management.
Phase
| Procol Review
2 FEoxritsicftiicaotni,on 5 RawDuaReview 4 RDraafwtDRmepaoratd
Review 5. FRienvaileRweport
Due
Inspected
112000 wave
121200 MSU
sir
Date CReenpteoretdo SDtautdeyDRierpeocrttoerda0nd
Management SponsorManagement
1130100
10800
nav
122800
120100
12800
3900
Ey
aor
01
Naomi Lovallo ULas--i Fenll~ Sr. QualityAssurance Auditor
HDealotre
Centre Ansytca Laboratories, Ic.
Page 3of104 0452
Con Sy No: 28.002
CERTIFOIFCAUATHTENITIOCINTY
"Thsrepo,forCnrSud Number 23.04,1 re en completarepresentationof
the rawdataforthestudy.
Submittedby: 3048 Reearn Dive Centre Analytica! Laboratories, Inc. foray `State College. PA 16801
[----
ScienaR= eel
CentreAnalyticalLaboratories, Inc.
Cone Antica! Laboratories, Ic.Pcl Maoageasas:
J ched,griia
RFreenmieansn wD, Cen AnayaLabortrion, oc.
Study Dirt, Widto vmatona: '
Ae I. Yalan
SWeialdnliGfaellIaagrhmesrtona, Lid.
id
6-JeF 0]
Bw
4llojo \
Date
SponsorRepresentative, IM:
gH 3 Envsonmenial HehnolosysndSater Services ConteAsanLaborato,
E Pagarios
600451
_----
mr -- L
Centre Study No. 023.042.
STUDY IDENTIFICATION
Extraction of PoftoarsAsniaulmysPiesrfUlsuionrgooHcPtLaCne-sEullefcotnraotespfrraoym/MMaaslslaSrpdecSterroummetarnyd Mallard Liver CENTRE PROTOCOL NUMBER: 00P-023-042
CENTRE STUDY NUMBER: 023-042
TYPE OF STUDY:
Analytical
SAMPLE MATRIX:
Mallard Serum and MallardLiver
`TEST SUBSTANCE: SPONSOR:
Perfluorooctanesulfonate (PFOS) 3BuMilEdnivnigr2o-n3mEe-n0t9al Technology and Safety Services PO Box 33331 St. Paul, MN 55133.3331
STUDY DIRECTOR:
SWieladnliGfaellIangthemeartional, Lid. 8598 Commerce Drive Easton, MD 21601
SPONSOR REPRESENTATIVE:
TESTING FACILITY: ANALYTICAL PHASE TIMETABLE:
Rochelle Robideau B3uMilEdnivnigr2o-n3mEe-n0t9al Technology and Safety Services. PO Box 33331 St. Paul, MN 55133-3331
C3e0n4t8reReAsneaalrycthicDarlivLea.boratories, Inc. State College, PA 16801
Study Initiation Date:
11/10/00
EExxppeerriimmeennttaall STtearrmtiDnaattei:on Date:
11/17/00 03/13/01
Study Completion Date:
09/06/01
Centre Analytical Laboratories, Inc.
Page Sof 104 GROAN
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Centre Study No. 023-042
PROJECT PERSONNEL
`The `The
Study Director for folowing personnel
this project from Centre
was Sean Analytical
GLaalbloargahteorriaets,WiInlcd.l,ifweerIentaesmsaotciioantaeld,
Lid. with
various phases of the study:
Name
Emily Stauffer Dave Bell Melissa Kennedy Whitsel Tiffany Proctor Angela Morgan Michelle Arjmand Lawrence Ord Rickey Keller Karen Risha
Title
Scientist Scientist `Group/Team Leader Technician Technician Technician Sample Custodian `Sample Custodian Scientist
Centre Analytical Laboratories, Inc.
Page 6of 104 CROSSES
_--eee Centre Study No. 023.042
TAOFB COL NTEE NTS
Page
GQUOAOLDILTAYBAOSRSAUTROARNYCPERSACTTAITCEEMECNOTMPLIw ANCEeSTAt TEMEn NT..e . ss
SCTEURDTIYFIIDCEANTTIIOFNIOCFATAIUOTNHEc NTICITYc wc... m
PTRAOBJLEECOTFPCEORSNOTNENNETLS c css s s]
LIE ST OF L FIGURES. ccc
10
L1I0STSOUFMAMPAPREYN.D.IC.EScccvrsennenomososeenioeneoeoeons 12
20 3.0
OINBTJREOCDTUICVTEIOcNo.c
cc rmmmmm sssmsosmsmsososonmonereeeeenosssosoo1so2nd2
40 5.0
TREEFSETRSEYNSCTEEMMAcTEoRIvALev rsessel133
6.0 DESCRIPTION OFANALYTICALMETHOD ...ccoovorvroeeerosoeneon 14
6632 PCIrOMeALpOaBTorAfPaShtYtanicdao.rdncs ranrd cForrtinficnatoionsSOslWstinonso..e..o..e...o..e..o...o..e..e..o...s...1..514
66.45DINSeUEUMsIEDEcoSfEIrnsNtirSumIpenVttaYnd.iOp.eor.atvninrg Cronditieons.s..o .....s........o.e.n.e.n......11S5
7.60.6EXQPEuRIaMEnNaTtnAdLiEDXEtMSPIIaGENtCawoli.c.u.olatnion..s.oos
oor oon
16 18
91:00.0CROENTCELNUTSIIOOFNNSDA ANDT SAn MPA LeES r....v.....e....csooov eosin 1198
Centre Analytical Laboratories, Inc.
Page 7of 104
GROAN?
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Centre Study No. 023-042
LI OFTS ABLT ES
Table.
SummoafPrROyS in Reagent BIAIKS.....cccrcnrnn
Page 2]
Table I. SummoafPrFOyS in MalLilveraBANrKS.d..
22
TableI. SummoafPrFOyS in Mallard Serum BIGDKS.......ccccrrnnnn 22
Table IV. Summaryof PFOS Recoveries in Mallard LIVE...
23
Table V. Summary ofPFOS RecoveriiesnMallard Serum .........ooonnrnn 24
Table VI. TSEuMmMmIaDrAyNoONfP19FWOSEEinKASd)ult Liv ver Sampr lesat 0s ppm a. (Tess t mn 2
`Table VII. TSEMuMom UfR6PFm WUOESSOkia SNn)Adv urltLiyver Sampls east1.8ppm a.s (Test 26
Table VILL TSummEaryRofR6PFWeOOeSkisnR)Adulc t Liver Samplesv at 6.2 ppm ai. s (Test 2
`Table IX. TSuEmTmDarRyOoNfP19FOWSEEiKnSA)duc lt Liverr Sampleo s at 17.n 6 ppm.i.(Test 28
Table X. TSeurmmmianartyioofn P12FOWSeeiknsJu)vec nile Liver Sampv lesat 0 ppm as .i. (Test 29
Table XI. TSEummImnaAriyoofn P12FOWSeeiknsJ)uvev nile Lio ver Sar mples ae t 1.8 ps pm .i.e(Tsesst en 30
Table XIL TSruMmImnaRrUyOoNfP1R2OWSeienksJ)uvec nile Liver Sav mples at 6.2s ppm .i. (Tes] t
Table
XIII.
Summary of TTDMON
P12ROWSeeiknSJu)venic le Livee r Samps least 17s .6 ppme ai. (Ts est
32
`TableXIV. SumofPmFOaSinrContyrol Adult Serum Samples........v.vc.ovevn33
Table XV. TSumMmarDy of1ZP9FWOOESEiSnN)AdultcSoervumoSramsplsens astn0 poprmsa..n(nTesstns 3
`Table XVI. TSumEmaMryDof6APFWOOESEKNiSn)AdvultvSerum Samples at 1.8 ppm a.i. (Test 35
`Table XVII. TSuEmmarRyofI6PWeFOeOkSsiR)nAduc lt Serum Samplv es a6t.2ppm .is . (Test 36
Table
XVIIL, SummaryofPFOS in TEMUNRON 19 WEEKS)
Av dult Serumr Samples ats 17.6 ppm a.i.
(Test ose
1
Centre Analytical Laboratories, Inc.
Page Bor 104
60488
_----m 4a mm
Centre Study No. 023.042
LIST OF TABLES (Continued)
`TableXIX.
SSEumPmAar)yofc PFOS o in Adur lt Sers um Sae mplest at 17.6s ppma.ei.s(6sWeereke
Page
38
`TableXX. TSuEmMmUarNyOoNfP12FOWSeienkJsuv)enirle Senrums Samples at ppma.i. (Test 39
Table XXI. TSuEmMmUaNrGyOoNf P12FOWSEiEnSJ)uvc enile Sr erum Saa mples s at 1.8 ps pm ai. (Test 40
`Table XXII.TSEuDAmOmNoaf1P2rFWOEySEiKSn)Jc uveniler Serum So ampless at6.2ps pam.i.e (Test d
Table XXIII.TESuNmSmaOrRyof12PWFOESEiSn )Juvec nile SerumSamv plesat 17.6 ps pm a.i. (Test 42
Table XXIV. SummaryofPercent MoisturesforMalLilveraSarmpldes .............. 43
Centre Analytical Laboratories, Inc
Page 9of 104
GROANS
_--DPmmm
Centre StudyNo.: 023.042
Figure 1. Figur2e. Figur3e. Figure 4.
Figure 5.
Figure 6.
Figure 7.
Figure 8.
Figure 9.
Figure 10.
LI OFFS IGUT RES Typical CalibrationCurvefOr PFOS ccc Page Chromatogram Representai0n.g1 ng/mL standard for PROS... 47 Chromatogram Representinag 1.0 ng/mL standard for PFOS................48 ReCahrgoemnattBogarnakmAR,eSept:r1e12s0e0a0nARt)eaio gnengt Blank for r PROS (Centn re ID dd C00h0r3o8m0a3toBglraanmk RAe,pSreets:en1t1i2n1g00C8o)n.t.r.ol Mallard Serum for PFOS (Centre ID: 50 C00h0r3o8m0a4tBolgarnamk RAe,pSreet:sen1t1in2g0Co0n0trAol)Mar llard Livev r for POS,s (Centre ID: S| pCphbroomfaPtFoOgSra(mCeRnetprreesIeDn:ti0n0g03C8o0nt3roSlpkMaAl,laSredt:S1e1ru2m10fo0rBti)fiecd wcitch 10 52 CWihtrhomPaFtOoSgr(aCmenRterperIeDs:en0t0i0n3g8C0o4ntSrpoklAM,alSleat:rd1L1i2v1er0F0oArt)ifciecd cat 1000pp5b 3 0C0h0r8o1m4a3t,oSgproanmsoRreIpDr:es2e3nt3i2n,gSJeutv:en1il1e 2Ma7ll0ar0d SAe)ru.m .Sa.mprler(cCecntnerIDn: $4 C00h0r8o1m0a8t,ogSproanmsoRreIprDe:se2n3t3i7n,gSJeutv:en1i1l2e10M0al4l)a.r.d. Liver Sample (Centre ID: SS
(Centre Analytical Laboratories, Inc
Page100f104
GRO4D0
_-- --
mm ee
Centre Study No.; 023-042 LIST OF APPENDICES
Page Appendix A AStumdyEPrnotoAcoalMn0dE0DPE-n0V2tI3-B0sO4N2 .(C.e.nt.r.e .St.ucdvy uNov.e0v2s3-s0s42s)samnsdsssnns 56.
Centre Analytical Laboratories, Inc.
Page 11 of 104 G04nL
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Centre Study No.: 023-042
1.0 SUMMARY (Centre Analytical Laboratories, Inc. (Cente) extracted mallard liver samples and mallard sseerruumm asnadmmpallelsarfdorlitvehre adcectoerrdmiinngattoiopnrotoofcopler0f0lPu-o0r2oo3c-t0a4n2es(uAlpfpoenantdeix(AP)F.OS) in mallard
`The limit of quantitation for mallard liver was 10 ppb and 10 ng/mL for mallard serum.
CfTerhnoetmrLenOo(nQC-eqnfutoarrneteiaSftciuhadbyml:atl0re2i3vx-e0lw4a4()sa.pdeeRatekesriwmdaiunseesddeotifencPateFdmOeaStthitonhdethcveoerrmirafelislcpaaotrindodnliinsvgteruadnsyaalmpypetlreefrsoertrmeaenntdgieoadnt `t#migaml/elmarLbdu)tsteworau2sm2.sl8easmgsp/ltgeh.sanrTathnhegeesdelforwreeossumtltnsocnoa-nrqceuearnnetiprioafrtitiaeobdnleoonflevtaehlewsect0alw2ie1bir8gahtgitognb.assitsa.ndaPrFdsOS(0i.n00t0h1e
`The average percent recovery + standard deviation for PFOS in liver samples was 95% + 12%. The average percent recover+y standard deviation for PFOS in serum samples was 93% + 10%.
2.0 OBJECTIVE
`The objectiveofthis study
psrpoetcoicmoeln0s0oPf-m0a2l3l-a0r4d2.liver
was
and
to determine levelso
mallard serum using
fperfluorooctanesulfonate (PFOS)
the analytical methods described in
in
3.0 INTRODUCTIS
`This report details the resultsofthe analysis for the determination of PFOS in mallard
lPievrefrluaonrdoomcatlalnacrsdulsfeornuamt,e Using HPLC-Electospr
ousriOntghtehre ay/Mass
FalnSauploeyrctoitccrhaolemmemitecrtaylh"oCdosamnepndtoiutln"edEd,xst"rFEarxcottrimaocnLtiivoeonrfofforPPooAttnaaasslssyisiuiumsm
PerfluorooctancsulfonateorOther Fluorochemical Compounds From Serum for Analysis
Using HPLC-Electrospray/Mass Spectrometry".
pTrhoetosctouldynuwmabserin0i0tPia-t0e2d3-o0n42N.ovTehmebeerxpe10r,im2e0n0t0a,l wstharetndatthee wsatusdNyodvieremcbteorr s1i7g,n2e0d00C,enatnrde
the experimental termination date was March 13, 2001.
Centre Analytica Laboratories, Inc.
Page 1207104
GROOT
Centre Study No: 023-042
4.0 TEST SYSTEM
mwTaahlselarcreodcntelriiovvleedrmowanlalsMaraadsyslii1gv8ne,er2da0nt0hd0esfCerernoutmmrWeuilsIdeDldiofffeo0rI0nt0th3eem8ma0at4tiroainnxadlbLtlihade.n,kcsoEnaatnsrtdoolnm,maatMlrDlia.xrdfoTrshteierfiuccmoanttwiroaonsls assignedtheCeInDotf 00r038e03.
ASuixgtuystmal10l,ar2d00l0i.veTr hsaemsplaemsplaends swiexrteysmtaolrleadrfdrsoezreunmusntaimlpltehseywewreererelcoegigveedd iant bCyenCternetorne fspreaormzspeolnnensuenlatinlodntfhoeAryutgywuemsratellla1o6rg,dgs2ede0r0iu0nbmaysnCadempnsltteorsreewdpeerfrrseoozrneenn.ceeliovAnendMoaanrddcFihetbi1ro,nua2al0r0yt1w2.4e,nt2y00m1alalnadrdstloirveedr Ina`sScsa.omacpilnaedteldoagwt-iritnuheatcnhoidspcsyhtoaudifyn.tohSfetcosurtsaotgroedarygeecironerfcdosorrmwaditlslicobanenckabenpetbfaeot ufCnoedunntirdne itAnnhatelhyertaircwaawdladLtaatbaaoprpaatacockrkaiaeggsee, associated with this study.
5.0 REFERENCE MATERIA]
ETnhveiraonnamleytnitcaall TsetcahnndoalrodgyPFanOdSSewravsicerseceived at Centre on June 3, 2000 from 3M mTahteeriaavlaiwlaabslestoirnefdorfmroazteino.n for the reference material is listed below. The reference
Compound PFOS
Centre ControlNo.. 0003-082
TCRNo. TCROWI746
Purity (%) 97.9
Expi0r8a3t1io/n01Date
`The molecular structureof PFOS is given below.
CPhFeOmiScal Name = Molecular weight =
wlI--o
Perfluoroocianesulfonate: 499 (CeF1nSOy)
dNeortiev:ed.Thisepnoetuatsrasliummolpeecrufllueoarnoodctsatnaensdualrfdofnoatrem[fCraoFm wShOiKc]h,PFmoOlSec(ualnaironw)eiisght 538.
Centre Analytical Laboratories, nc.
Page 130104
nossa
_--
Centre Study No.: 023.042
6.0 DESCRIPTION OF ANALYTICAL METHOD
FAnlauloyrtoicchaelmimceatlhoCdosmepnotiutnledds"EFxrtormactLiiovneroffoProtAansasliyusmisPeUrsfilnuogroHoPcLtCa-neEsluelcftornoastperoary/OMtahsesr FSlpueocrtorcohmeemtircya"l Canodmpo"uExntdrsactFiroonm SoferuPmotfaosrsiAunmalyPseirsflUusoirnogocHtPanLeCs-uEllfeocntatreosporray/OMtahsesr Spectrometry" were used forths study.
6.1 Extraction Procedure
pAro~ce0d.ur5e0.g sAafmieprlefoorftlifiivceartaionndofaap1p0r0opkrLiaatleiqsuaomtpolfets,hethseesraummplweasswseerdefvoorrttehexeedxftroacr~ti1o5n bwsieaccsaornabddosdn.aetdOen1w0eatmshielalsidlediretuedrmtosofam0tp.hl5eesMl.ivTerTBwAsaomwpmalislelsaildiadtneedrds t1oofmti0hl.el2i5lliivtMeerr sswaoamdspiluaemdsdceaadnrdbot0on.a5ttheme/islsoledlrituuemmr ssaammppllees.waFsivpelamcileldiloitnerwsriosftM-aTctBioEn wsahsakaedrdfeodrt~obo2t0hmtihne.laivnedratnhdensceernutmrisfaumgepdlefso.r E~ac1h5 aminnd. thFeonurremciolnlsitliitteurtsedofwithteh o1rgaminlilcillitaeyrerowfamsetthaakneonl.andEdarcihedsoanmpalenitwraosgenaneavlaypzoerdatboyr LC/MS/MS electrospray.
62 Preparationof Standards and Fortification Solutions
PASntFaaOlnySdtairwcdaalssLpoarlbeuoptraiarotneosdriawetsea"recpornopctreoencptoarlra0et0diPo-no0on2f3-S10e040p2t.g"em/bAmenLr ibn1yd8i,dvii2sdsu0ao0ll0vsitnaogsck1s0sptmeacgnidfoiafertddhseionlsuttCaienodnnatrordef f(ocrotrirfeicctaetdionfosrtapnudrairtdy saonldutisaolntwcaosntpernetp)arinedmbeythtaankoiln.g 1FmrLomofthtihsessotlouctkioann,dabr1i.n0gipngg/mtLh.e volume up t0 100 mL with methanol.
fAort0i.f1icaptgi/onmLstafnodrairfdcaatnidon
bsrtianngdianrgdtwheasvoplruempeareudp
by to
t1a0k0inmgL10wimthLomeftthahneol1,.0
pg/mL. A 0.01
ug/L standard wasprepared 100 mL with methanol.
by
taking
10mL
ofthe
0.1
ug/mL
standard
and
bringing
to
0A.0s1etpogf/smtaLnsdoalrudtsiocnosntnatihneifngolPoRwOiSngwamsanpnreerp:ared by serial dilutionofthe 0.1 pg/mL and
initial Con01c. (ug/ml)
Volume (mL) 5
Diluted to Gm) 100
Final Cone. (ug/ml) 0.005
01 0.1
2 1
100 100
0002 0001
001 001
5 2
100 100
0.0005 0.0002
001
1
100
0.0001
!of PFOS
Centre Analytical Laboratories, Inc.
Page 140f104
[FLERE
Centre Study No: 023-042
The stock stored in
standard solution a refrigerator (4
and +
all fortification 2C) when not
and in
calibration standard solutions were use. Documentation of standard
`preparation can be found in the raw data associated with this report
63 Chromatography
Quantification timeofPFOS
of was
PFOS ~ 4.4
was min.
aPcecaokmsplwiesrheeddebteyctLeCd/iMn Sth/eMcSonetlreocltrmoastprriacye.s
The retention corresponding
a1l0tetrheseavnearlaylteforrettiefnitciaotniontirmee,covbeurtitehseaanmdouthnetsredsettewcetreed wleesrsetohnalnytshiegnliofwiecsanttceanlioburgahtiotno
standard (0.0001 pg/mL).
6.4 Instrument Sensitivity cTohnecenstmraaltlieosntofst0a.n0d0a0r1d pga/momuLnotf PiFnOjeSc.ted during the chromatographic run had a
6.5 DescriptionofInstrument and Operating Conditions Instrument: PE SCIEX API 3000 Biomolecular Mass Analyzer
Interface: SCIEX Turbolon Spray Liquid Introduction Interface
Computer: Dell UltraScan P1110
Software: HPLC:
`PWEinScdioewxsAnNaTl,ysvtervseirosnio4n 1.1 Hewlett Packard (HP) Series 1100
HHPP VQuaactuPumumDpegasser HP Autosampler HP Column Oven
HPLC Column:Genesis Column Temp.: 35C
Cy
(Jones
Chromatography),
2.1
mm
x
50
mm,
4p
MInojbeicltieoPnhVaols.:e (A1)0:pL2.mM Ammonium Acetate in ASTM type I water
Mobile Phase FlowRate:
(B): 0.3
Methanol m/min.
Centre Analytical Laboratories, Inc.
Page 15.0F 104
Coan;
Time 0
%6A
%4B
00 10
70 0 100
75 40 6
no 40 6
Centre Study No.: 023.042
Tons monitored:
Approximate
APmFOiSe neMgoadtieve Transit4i9o9nM5o9n9itored Retention4T2i0me(min)
`Tune File Parameters
ICSo-nltosrporlasy
42S0et00
DP-Declustering Potential
510
FP-Focusing Potential
2300
EP-Entrance Potential
100
CE-Collision Energy
70
CXP-Collision Cell Exit Potential
5
DF-Deflector
3000
CEM-Channel Electron Multiplier
28000
NGebausliFzleorwGsas
s1e2t
Curtain Gas
13
Collision Gas
4
IS Temperature
350C
6.6 Quantitation and Example Calculation
"Ten microlitersofsample or calibration standard were injected into the LCMS/MS. The
peakareawas measuredandthestandardcurvewasgenerated(using 1x.fitweighted
linear regression) by Analyst software using six concentrations of standards. The
concentration the equations
for mallard below.
liver
(g/g)
and
mallard
serum
(g/mL)
was
determined
from
tEhqeuasttiaonnda|rdcalccuurlvaeted(ltihneeaarmroeugnrtesosfioannaplayrtaemfeoteurnsd)(ignennegr/amtLe,d bbaysetdhoenApnealayksatresao)futwsairneg epqruoagtriaomn.s foTrhseenruEmquaraetisohnow2).calculated the amount of analyte found in pg/mL (the
Centre Analytical Laboratories, Inc.
Page 160f 104
CRO5NG
CentreStudy No. 023-042.
Equation 1; Analyte found (ng/mL) =(Paslroeepae inaterckept)
Eq`Aunaatlyito2efnound (ug/L) =(anal. found (ng/mL) xFV(mL)x DF x EV(mL) 1ug
(AV (mL) sample vol. (mL)
1000 ng
`WhFerVe:= Final Volume
DEFV == DEixlturtaicotnioFnacVtoolrume AV = Aliquot Volume
cFoar lsacmpultelhseapfeotrrtceiefnidetdrewciotvherky.nown amounts of PFOS prior to extraction, Equation 3
Recovery (%) = (anal.found (pg/mL) -avg. aamnoiaunnlctta.rdlde(dg/(mnLg)/mLx()1000ng/! pg)) x 100.
AneMxaalmlparldeosferacuamlcsualmaptlieonuCseinntrgeanIaDct0u0a0l3s8a0m3pleSpfkolAlow(sS:et: 1121008), forfied at 10
ng/mL wiptehakPFrOeSa, where: = es
isnltoeprecept
-= sTimso
dilution factor
=
ngadded (fortlevel) =
avg. amt in controls =
1
Ing
0 (Not quantifiable)
final volume
=
1mL
extraction volume
=
SmL
aslaimqpuloet vwoeilguhmte(volume) == 40.mLmL
From eAqnuaaltyitoenf1o:und (ogiml)
= [6558-515
7740
From equation 2:
= 08ng/mL
Anlyte found (ug/ml) = (0.8ng/GmmLLxxOmilmxl1)xSm)1L0u0gg
= 0.00976 pg/mL. Centre Analytical Laboratories, Ic.
Pege 1707104
GO0aN7
ee
AA AAA A
EEE
From e%quaRteicoonve3r:y =
-
(0.00976 ug/ml10xng~i0mnLg/mL) x1000) x 100
= 0%
Cente Study No. 023.042
7.0 EXPERIMENTAL DESIGN
etExwatocrhamcastteertdioxufsbislnaagmntkphsleefsaoprp(tlriiovpfeririaeaotdtreksnmeeortwuhnmo)cdocnaocnnesdnittsrhtaeetndioaonnfsa,loynazeneddre-ia2ng0deunsptalmibcplalateneks.,. oEnaechmastarimxplbelawnaks,
8.0 RESULTS
lTihveerPblFaOnSksfaonudndmailnltrhde sreearguemntblbalnaknsksareargeivliesnteidn TinabTlaebsleII.& TIIhL.e PFOS in the mallard
aInvdeirvaigdeuaplercreecnotvreercioevserfyor+
PFOS in standard
the liver deviation
samples for PFOS
are detailed in in liver samples
Table IV. was 95% +
The 12%.
aIvnedirvaigdeuaplerrceenctovreecrosvefroyr PFreOlSativien stthaendsaerrdudmevsiaamtipolnesfoarrPe RdOetSaiilnedseirnumTasbalmeplVe.s Twhaes
93% + 10%.
dPeFtOecSteid atthethmealcloarrrdesipvonrdisnagmpalneaslyrtanrgeetdenftiroonmtniomne-bquutanwtisflieasbl tlehvaenlsth(ealpoewaekstwas
concentration of the calibration standards (0.0001 pg/mL) t0 22.8 ug/g. Individual results are listed in Tables VI-XIIL. The results are reported on a wet weight basis.
dPeFtOecSteidn atthethmealcloarrrdesspeornudminsgaamnpalleysterarentgeendtifornoimmneonb-uqtuawnatsiflieasbethlaenvetlhse(laopweaskt was concentration ofthe calibration standards (0.0001 g/mL) to 218 ugg. Individual
results are listed in Tables XIV-XXIIL.
The percent moistures for the mallard liver samples are given in Table XXIV.
9.0 CONCLUSION:
"The mallard liver and serum samples were successfully extracted and analyzed according
to protocol 00P-023-042.
Cente Analytical Laboratories Inc.
Page 18.0f 104
C0303
_--
Centre Study No.: 023-042
10.0 RETENTION OF DATAAND SAMPLES
LWahboernattohreiefsi,naIlncr.epwoirltl ibsecosmhpilpepteed,taollthoerisgipnoanlsopra.peTrhdiastadogcesnenroatteidncblyudCeefnatcrielAintay-lsypteciicfaicl
raw data
submitted.
such as
Exact
instrument logs,
copiesofall raw
however exact
data, as well as
copies of temperature logs will be
a signed copyofthe final analytical
report and all original facility-specific raw data, will be retained in the Centre Analytical
Laboratories, Inc. archivesfor the periodoftime specified in 40 CFR Part 792. Retained
`samplesofreference substances are archived by the sponsor.
Centre Analytical Laboratories, Inc.
Page 190f 104
GORD
_-- Centre Study No. 023.042
Centre Analytica Laboratories, Ic.
Page 200104
COLE
_---rmemmm--m--m--m--
Centre Study No.: 023-042
Tablel. Summary of PFOS in Reagent Blanks
Sponsor D m nm na ma ma nm nm Mm ne ne me mm ne na nm ne mm ma
Centre n
ReagemBlukA ReagentBlukA ReagentBlankA ReagemBlankA ReagentBlmkA ReagenBlankA ReagemBlnkA ReagentBlukA ReagentBlakA ResgentBlankA RReeaaggeenmtBBllankkAA ReegemBlankA ResgentBlaukA ReagentBlukA ResgemBlukA ResgemBlnkA ReagentBlakA
Set Number [700A 700A 112004 112000A 11200 112100 [12008 112108 112700A 1127004 127008 1127008 03070IA 030701A 030701B 030701B 00S0IA 03080IA
Extraction Date 11/1700 111700 112000 112000 112100 112100 112100 112100 112700 112700 112700 112700 3701 3/701 3701 3/701 YO ysl
Analysis Date T118-19/00 11718-1900 17202100 112021100 1222300 1222300 172300 11723100 11728:29/00 17282900 1129000 12900 3901 3901 30399--11000011
01 no
AVERAGE: STANDARD DEVIATION:
Avalyte Found (g/g
No No No No No No No Ne NQ No Ne Ne No Ne NNoo No NQ NQ ~~ NQ
* Duplicate injection
N`buQt w=aNsoltesQsuatnhtainftihaeblleow(eAstpecaokncweantsradteitoencotefdtahtetchaelciobrrarteisopnosntdainndgarandasl(y0t.e0r0e0t1engt/iomnLt)i)me For values recorded as NQ, 0.00005 ug/g(halfthe valueofthe lowest calibration standard, 0.0001 pg/mL) was used to calculate the average and standard deviation. LOQ=0.01 pg/g for liver and 0.01 pg/mL for serum
Centre Analytical Laboratories, Inc.
Page 21 of 104 C0050
--YVP A AA__A
Centre Study No.: 023-042
Table IL. Sponsor
iy m Mo nm mo m mo m m
Summary of PFOS in Mallard Liver Blanks
Centre I'y 0003804 BlaAk 00000S3B80l4mBlkmAkA O0000B3O80B4EBlmuAkA 0030SBlakA 0000003380044BBllannkkAA
Set Number
Eutncen Date
Amsyis Anayte Date Found (ugg)
11700A ILT00A
11700 LATO
T8190 LVISI90
0000296 0000300
112000A 100A
12000 1200
11210220020000
NQ NQ
12100A L2IOA
120 L2MO
11222230000
NQ NO
GIOIA 0080IA
IOI 3801
I1vol num
Ne No
STANDARDDEVAIVAETRIAOGNE:: ~~ NNQQ
Table Il. Summary of PFOS in Mallard Serum Blanks
`Sponsor D
Centre 1)
Set Number
Exracton Date
Amslsis Awalyte Date Found (ug/ml)
n no
0003803Blank A 00303BlmkA
1121008 I2IOB
12100 L200
112300 112300
No No
Mo OON0BB00I3BBllmnkkAA 112I2000AA 1Z27U00 111228822990000 NNQQ
mo O0D00B3G8B0U3BmlkmAkAt 111220700088 LL220700 11122990000 00N01Q59
m mo
00B08O0I3BBalkamAkA
G0T0IA 030A
IOI 301
3901 3901
000826 000825
na
O0N03003303BlBaUmkkAA _
0307018 O30701B_
3701 3701
391001 39-1001
000159 000397
To
-
AVERAGE: 0.00239
STANDARD DEVIATION: 000333
* Duplicate injection
`NbuQt w=aNsoltesQsutahnatniftihaeblleow(eAstpecaokncweanstrdaettieocntoefdthaettchaelciobrrarteisopnosntdainndgaradnsal(y0t.e0r0e0t1enptgio/nmtLi)me LOQ = 0.01 ug/g for liver and 0.01 pg/mL for serum
sFtoarndvaarldu,es0.r0e0c0o1rdge/d masLN)Qw,as0.u0s0e0d08topcga/lcmuLl(ahtaeltfhteheavevraalgueeoafntdhestalnodwaersdtdceavliiabtriaotni.on
Centre Analytical Laboratories, Inc.
Page 220 104
CROSBY
_----
-
Cente Study No.: 023.042
Table IV. Summary of PFOS Recoveries in Mallard Liver
Spomsor Cemntre NuSmuber ExrDauceion ADmapes AddeAdmtiog) Reco"very
mTMo To
MWOUMSSKAA ITIITOWAADD 1TAATTOO0D 1T11990000 WONSKB IIA IAW B10
T1o So
3" a
mTMo CCDMMOSSSKABS I1ZIOO000AAR 12A0T0000 I1A12S2I000 10So0 TO OODSOISKAT IZOOAR 12000 12200 100
1"4 1s
mTMo OCNMOOASSSKEBB 120000AA 1122000000 11220022110000 44000000 mo ODMOSSKA 120A LUO 122200 1000
110076
TToo 0COMMMOOSISSKpABT I21A0DA 112200 112227203000 210000000 0is
TMmo DONmOEIMSHSKKBA IG2O0I0AAD Nm2oMlO 1Yi2o0) 20000 2
Tmoo oCOODNMOMISSKKABT GOONMRIIAAD BEOOII M3L10O1 2200 m o0oispkBe osomiaD ymwi uum ae
1207 1
STANDARD DEAVVIEARTAIGOEN:: 9115
RELATIVESTANDARDDEVIATION: 12
*Duplicate jection
LOQ=0.01 g/g for liver and 0.01 pg/mL. for serum
Centre Anatytical Laboratories, nc.
Page 23of 104 CROGHG
EEE
EE
--------
CenteStNous d0230y62
Table V. Summary of PFOS Recoveries in Mallard Serum
Spor CDawumbeSer BuDnuece ADbueb asscAomotpm) ne"ve
mmoo
GCDONSSKEAA' Ii2o00nB ome mee
2Ri0e ake
2Ti0me low
d1o0 sw
0a w
mmoo mo
oowsoSKeA mmoAm OOMBSKA IZA
eewio L270
u1omwe0 1282900
s0w lo
aw u
mmoo mo
OGNGOSSKKED LIMAA OONSKA Zw
1N2o70 ize
1l2o0e29s0m0 190
tloeooo so
a25
mmoo GOSSEKSA wUpR mE SKe me
02200 a0
motw ios
oswwe owe
2a a
nnoo no
oCoOMNmOSSKkAA mGwoowiAA omll ws ooo 00
s3a8r0 eo
1000 0
" "
mmoo CoOmNOeSKrA mDoowwBn mJol 0mo0l mo COMSAT Grom 370i i000
loow 100
5 0
num oGmOssSioRr ocoonmn odole 3310000 0ie0 n1ss
Rr--
RELATIVESSTTAANNDDAARRDDDDEEAVVVIIEAARTTAIIGOOENN::.
3121 13
LOQ= 0.01 ug or liver and 0.01 pgmforserum
Centre Analytica Laboratories, Inc.
Page2401104 Gro:
Centre Study No. 023-042
Table VI. SummaryofPFOS in Adult Liver Samples at 0 ppm a.i. (Test Termination 19 Weeks)
Sponsor D 1961 ~ 19610 1562 19620 1963 ~ 19630 1964 19640
1965" 1965+ 1966 1566+ 1967 11 1967 1968 1968+ 1969" 1969 1970 19700
Centre D
"0008006 0008006 0008007 008007 0008008 0008008 0008005 0008009 0008010 o00so10 ooosont 0008011 0008012 008012 0003013 0008013 0008014 0008014 o00sols o0usors
set Number 700A WIA HOA HOA HOA HOA DIA HOGA HA MOA HIMA UI0A II70ADD MIT00ADD HI700AD UI0AD HIT0AD UI0AD HIT00AD UIT00AD
Extraction Date
AnDalaytseis
TU T/IB1900
IAT IBIS
1700 1S1900
ATWO 181900
A700 181900
A700 11181900
A700 181900
A700 1181900
1700 1181900
100 IISI900
1N700 1ABI900
1700 181900
14700 112000
11700 112000
1700 111900
1700 11900
1700 111900
1700 111900
1700 111900
1700 111900
AVERAGE:
STANDARD DEVIATION:
FoAumnadiy(stpei) 0000813 0000763 0000509 0.000631 0.000957 0.000887 0001S 0001S7 000110 00011 0.0046 0.00432 0662 oss 0238 0246 ois 0106 0358 0343 0.138 0.219
* Duplicate injection
LOQ = 0.01 g/g forliverand 0.01 pg/mL for serum
CentreAnalytical Laboratories, Inc.
Pagoef21054
GOOS0
Centre StudyNo.: 023-042
Table VIL. Summary of PFOS in Adult Liver Samples at 1.8 ppm a.i. (Test Termination 6 Weeks)
`Sponsor
Centre.
m
D
B0I-0263:21065 #1 0103870
E01-0263:21065* 0103870
E01-0263-21066 7 0103871
E01-026321066* 0103871
E01-026321067 1 0103872
EO1-0263:21067* 0103872
E01-0263-21068 4 0103873
E0I-0263210680 0103873
E01-0263-210649 0103874
E01026321069 0103874
E01-026321075 0103880
E01026321075* 0103880
01026321076 = 0103881
E0I-026321076* 0103881
0102632107F7 0103882
E01-026321077 0103882
E0I026321078 0103883
EOLOZ6321078 0103883
E01-026321079 0103884
EO1-0263:21079 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 EET] OL Imon M01 31201 801 mel 301 VA1200 IOI 311200 ILO 31-1200 IOI 3-200 IO 31200 OL I-1200 IROL 31-1200 IOI 31-1200 IOI 3-200 aor 31201 ol Ino 01 31201 IOI 200 IOI 3201 OL 3200 IROL 31-1201
AVERAGE: STANDARD DEVIATION:
Analyte Found (ug/g)
0359 0350 0647 0631 0386 [ 211 204 0222 0232 0317 0326 0219 0230 0.19 0197 0346 030 00893 0.0888 0.535 0.574
* Duplicate injection
LOQ = 0.01 ug/g for liver and 0.01 g/mL for serum
Centre Analytical Laboratories, In.
Page 26 of 104, ROSOS
--------------------_--S----------------
Centre Study No.: 023.042
Table VIIL Summary of PFOS in Adult Liver Samples at 6.2 ppm a.i. (Test Termination 6 Weeks)
Spoor Contre
n
n
Tao | oes
EBoLo2els20e70 o0l1o0x3w8T75s
BL 00s
EEslemne 00003
B Ellsoen 0ol0s
BLE ol0sw
EE0L0026632210000 0ol1o0as3s9s
EE0o2ne6i3o2s0e8r 0l1o0s3s8e8s6
EBLls0e8 Oo1l3s
EE02l632e10m85 00110308838
EEoolLaseis2i2o0n8s || 0ol1o03s3s8s
E01-0263-21084* ' 0103889
Sa Number TO0IAD GGOoOIoAdD GOIAD GoOa0IdAD oGooIADD ood GoO0oIAdD GGOoIaAdD GGoOwOiADD GGoOwiOADD ooomRoIAADD -(030801AD
Eaacion Due IAL m3oD OI BsaOoL 0 a0 yao 3sa0o mOoIr A3Om0L1 3mm0 mOoLl
Amis Due T1120 aMnLoOnl Lol Lmiaonn ynnaazlon maze Lmiaon mM2a0z mdaezl 3d1n2l0o1l aLnoioln
3801 AV1E-R1A2G1E: STANDARD DEVIATION:
Amite Found Gugp
Tod 01916 0907 115912 oomm 128 1Ir 34 odnes o0aasims o1s6i6 01052s 0000878 0576
* Duplicate injection
LOQ=0.01 g/g for liver and 0.01 pg/mL for serum
Centre Analytical Laboratories, Inc.
Page 27. 104 G05
-- ee ------
Centre Study No.: 023-042
Table IX. Summary of PFOS in Adult Liver Samples at 17.6 ppm a.i. (Test Termination 19 Weeks)
Sponnsor 199110 1 1199220 0 1109929+37 199 940 11099955% + 1199996+ 19099770, 119999880 1919990. 22000000,
cenre ooooasusoolrss oooo0osm0orr?r oWoOoRmIiSs ocoansnonryy o0o000s8o0z200 oooooossoo2tn onoooossotzzz2 oooo0osso0z2s3 G0R0E4 aooooossc0z2ss
NuSmbeer. TIII0T0WAADDDD MHIOAADDD 1HTI0O0AADDDD WN0AADD HWIA00DAD UNIIO0AADDDD WOIAADD noaodp II00AADDD nwio00AADD_
EDrucieon ADmuies T11I70O0 T1117220000 0117000 111122000000 A700 120m AnTaOe 11192e00e0 nAmTeO 11199000 T0 eo 111920000 0Ta0me 111290000 AwTaOe 1nissm wNAmTO n112s00w0 An7a0e0 n11a2s00e0 nnmee A1VuEoRmAeGE: STANDARD DEVIATION:
FouAsnsdiyGtuei 116549 nnss e 2Im 299 316302 s1es assmt 313565 p1r61e 69.1604 657
Re --
LOQ= 0.01 g/g for liver and 0.01 pg/mL. for serum
Centre Analytical Laboratories, Inc.
Page 28of 104 600508
Centre Study No. 023-042
Table X. Summary of PROS in Juvenile Liver Samples at 0 ppm a.i. (Test Termination 12 Weeks)
Sponsor D 2T01o0T 02002 2200330 2305 223300570 223008 2208107 B2u31e67 B2i1e7r 7 z2i20 2300
Centee oooosn08es ocoooso0s8?7 o0o0o0s8o0s8s8 000089 00000083005809 00000088005510 o0o0o0s800s912 0000003005823 0000038008943 00000038008554 ooos0ss
Nsumeber EDxtaratcetion AwDaatyes FouAnnadlyGtieg) 01200000A8 1122000000 11112200221100000 NNoo 010000AA 1M22000000 111220022110000 NIQ 220000AA H120R00 1112200221000 NNOQ U20A 12000 1202000 NQ 10200000A4 112200000 1122002210000 NNOQ 122000AA 1B2A00O0 112200220000 NNOQ 110000AA 1H2Z000M00 2w200220u00 NNQQ 220000AA 112200000 111220022100000 NNoO 0W0A0A 122000000 1U122002210000 NNoO 220000AA 1122000M0 11112200221100000 NNoo 200A 12000 1A1V20E2R1A0G00E: NNoQ
STANDARD DEVIATION: NQ
* Duplicate njecion 'NQ = Not Quantifiable (A peak was detected at the corresponding analyte retention time but was less than the lowest concentration ofthe calibration standards (0.0001 pg/mL)
LOQ=0.01 ug/g forliverand 0.01 pg/mL. for serum
For values recorded as NQ, 0.00005 pg/mL(halfthe valueofthe lowest calibration standard, 0.0001 pg/mL) was used to calculate the average and standard deviation.
Centre Analytical Laboratories, Inc.
Page 2907104
600509
Centre Study No.: 023-042
Table XI. Summary of PFOS in Juvenile Liver Samples at 1.8 ppm
a.i. (Test Termination 12 Weeks)
ISpo"nsor CanDre nTurts acSoouuascnese azm pcrooend? zmss ocoaonnsoonsss 3256206 ccoonossoassss aIeo oooooossiioonn 0 00 pooecsetor ameA ooooosiocz amE woonotomn zmam poraoeeios 2mes ooaonosniiooss
MeSmtber BuDnaiteon ADmaites__FouAnmdiGeui) 2T0o0oAn aToomte ITizzoaeio oooonoeksstd HlOAA nnoaotb 2Z00aane0 oooooiodd II0o0nA noaowm tzzooaeie oaooooiisseo o10Aa nnaowm ntzzooaaweo ooouoamees lloowos nnoocw nnmzoaaiweoe oovsies llAA lnoowe ntmaeioee ooooaiosism llAA nlooww nnaavaanl oomaernss lMZMAoA 1A2000000 1122002201000 0o0w0a04s0 0INAA o20o0m0 1112200221000 o0s0o0o0s9e6s9 ilowAa anooee nnmamueeo ooewse
STANDARD DEAVVIEARTAIGOEN:, 00.0010182)6
+ Duplse nection
LOQ = 0.01 gg or liver and 0.01 gL. for serum
Centre AnsytclLaborstris Inc.
Page3007104 Gnosis
_--
Centre Smdy No: 023.042
Table XII Summary of PFOS in Juvenile Liver Samples at 6.2 ppm a.i. (Test Termination 12 Weeks)
Sponsor CIern)tre 2F 50 C0T 008106 22360 coooooss1ioorr zZet ooooossiiooss 0 38 0o0s08i1o0s9 2m33900 peoeslo nBaaes oowmeint z2a0 oooouossiiiz2 223360/0 oooomuisn1s3 24B0f ooomiiiee 223066 oossts
NomSboer MT2G10A8 LMIGAA IIII0AA IW2I0AA 220000AA 1I22I00AA 220000AA M0AAA 220000AA 1122i0000A0D
EDaactieon ADmuees 1N221000 T1272232000 NN2200 1122220000 NN2Z0I N1222000 N2200 m122a25e00 U12R10I0 11222290000 NN2200 122220200 2N200 212220000 NN2200 122220000 N2200 MW2220000 112211000 112200 STANDARD DEAVVIEARTAIGOEN::
FouAnmdiyuisep) ooooolos oooom 0o0o08m0 0ooouosssss 000000810s0 0ooo0xn6 0o0on0 0o0o0m 000000ks2 ooooms 00..0000344817
* Duplcae jecion L0=Q 0.01 ggforliverand 0.01 pg/mL. forserum
Genre Analytical Laborsoie, Ic.
Page 31 of 104
600532
_--_--
Centre Study No.: 023-042
`Table XIII.
Sponmor nTaUeTE DBa OF e25y3 F B2u5r47 D2355sM nz2s5u7r nBsOeC BB3o5o 2600 n23e6r3
Summary of PFOS in Juvenile Liver Samples at ai. (Test Termination 12 Weeks)
Cnanre OweMllEs wwoonm
wos 0008118. 00w0o81u1l9 0o00o81m20
0ow00oo8m1n221 wwnisz aowoonosiszs 0w00o8w12s5
NeSweer iI200AADD I22M00AADD iow 112100AD mio 112100AD l1121A004
U11u22N0100AW0>ADD nwaDa mloAd 208 u11o2i1o0o0wArD
BuDcueks ADmueb Tmaawuo unmmme n2 ame Goammeo n12a1w10e0 nNa2m0o bnaaziwo u12m10m0 n12a1m0e0 u11m22a2m30e0 um12a1o0e0 munaam2mmmeo daowme unmamm m0a2w0o muammme nz mam 11w2a1w0e0 Au1V2Em7R0mA0GE: STANDARD DEVIATION:
17.6 ppm
roAmmigigep) oooom oossse oo 0.0234 c00o1m8s4 o00i11s0 0o0.o00m6s1s6 oooonm oooonm ome 0oo2oo6n2 o0ta
* Duplicate injection
L0Q= 0.01 ug/gfo liver and 0.01 pgm. for serum
CentreAnalytica Laboratories,Inc.
Page 201104 Grose
eee
Centre Study No.: 023-042
Table XIV. Summary of PFOS in Control Adult Serum Samples
Spoor Care BE0o10s2s632201000s5 1 _ o0l1a0s3s8i100 oE0lL02e65a:2t10e06 0o1l003s8E1i1l EELlsss2o0n0n ooizs EEo0LLc2s6a2lio0o0s8s, ooloossis BE0oL0l63e21s0085 0o1i003s8e1e6 EEE016l-0226e30-21m6025YF l0o1o0os3s8o3!0 BBls ascs ooizs Bsr oz EE01l026s3-21a028F 0o10s38s33 EE01-o026i3-2n1029 0o10i38s34
NaSmbter wwooonl cGooolwe CGoonaA GGooooiaA wGoooaA 03G07o01i GGoooon GGouoon 0c30o70i1.
0c30o7o01s8
BxDmucedon ADmuies FouAndsGiuemi)
ovinol 3se0m ooneess
ysoon dsemo ooosm
o3ml sasmoo o0o0m1s0s3
eoll m0oosoom"iss
wmmll swee oooosois"
3300 mol
3398-11000001 soo)
00.000020875 No
m01asos0n00 nIe)
ym aso No
Emdl 3s9-o10n01 0o.o0u04s2s8
EyLm 3sA/Ve-Eo1R0nA0nG1E: G0NN0Oo757 STANDARD DEVIATION: 0.0134
NQ =NotQuantifiable (A peakwas detected atthecorresponding analyteretention time `butwas lessthan the lowestconcentraotfitohnecalibrationstandards (0.0001 pg/mL) For values recordedas NQ, 0.00005 g/mL(halfthe valueofthe lowest calibration standard,0.0001 pg/mL)wasused tocalculatethe averageandstandarddeviation. LOQ = 0.01 g/g for liver and 0.01 pg/mL for serum
CentreAnalytica Labortoies,Ic
Page33of 104 R052
_--
Centre Study No.: 023-042
(TTaebslteTXeVr.minSautimomna1r9yWoefePkFs)OS in Adult Serum Samples at0 ppm a.i.
D `Sponsor
Centre.
1966110 m 0o0o0o8R0t2a6s
wBeRrE. oooon
119066330 ocoooaoczss
1w96e40s 0c0o08o2s9
191665050 0o0oo0s3as0n
191696646 oooooacms1
19a 67 peoeor m
1156688 Coas000t80s33
1916996094 ooo0ososcassse
rwe f ooooooasnsass
* Duplicate jection LOQ= 0.01 ug/g for liver and 0.01
NSumebter 2121B08 2I20I008B m1i2e0s8 1m2i0s8 1u2n1w0s8 nMi2e0s8 INBBDD 1220008D0 nIZ2IB0BDD LunBEDD
ExDtruacetion AnaDlyuseis Tn221w000 nTUaZWe0 D12RWO0 212030 npz2w0o un2eww0e 1nz2w0e 2naMe Dn2aWc0e Lnaavee 0D2020E2 we 2lo0we nnzaawwe 1Tz2e0 uuzzaawweee wmmz nzaraawme0 uuim unmmomme STANDARD DEAVVIEARTAIGOEN::
pgm. for serum
FouAnndaulygtme r) 000o0o60s5 o0o0os0osl oosomes oocosmssr 0o0o10k3 ooeos 6enmn a3mm o0u3s 1La3rs 210232
CentreAnalytica Laboratories, Inc.
Page34of 104 R051
_-_--
Centre Study No 023-042
Table XVI. Summary of PFOS in Adult Serum Samples at 1.8 ppm ai.
(Test Termination 6 Weeks)
Sponnsor Contre BELNQGG2200000 MOoTwss EELlO6m20s0M oOwHlSs mBLoRGa20n2. oOOoRmT BBILQ26622005 4 oomoEeE BEE0L1-Q0l26G3-22o100104C Oo01W0n3E8s1S9 EBLLG2260200I0C OooWpSs BBLLO6O20G2 F 0OGE5E7 EB6L2A0D2E EOBTS BElaLeoOtar 0oopHsy modo omy
NuSmtber oOoAoADD cGooooAdD oGoUpOiAADd oooo0oiiAADD 0oo30Uo7Oo01BiADbD oooooBoD GoUoO0BBDD oooooBmD cooomwmd coop
ExDmactieon ADmuien 3Imeml o310o01 aviieol yyoomo d3o0e1 wvoiooll v3o0l1 3o1o00n0 3am7m0ii1 vo3i1o0e0l1w 3vomlm vviioeideol 3a0o0n0 voiewmer m3o0lm vvioondol wmmml vviieowism am vAiVEeRwAsGE: STANDARDDEVIATION:
FounAdwepnt) 1T1s 021 2z0s 220044 o1100ss6 o6s7s o6u4 oadaes iaes 1i04 815
* Duplicate injection.
LL=O0.Q01 ug/gforliverand 0.01 pgf/orsmerL um
Centre Analytical Laboratories, Inc.
Pa 35g of1e04
6005155
_--
CentrStudy No. 023-042
Table XVIL Summary ofPFOS in Adult Serum Samples at 6.2 ppm a.i. (Test Termination 6 Weeks)
`Sponsor
m Centre.
EBooLmreesa2t0oriss 0l1o03s3s0
B EoLoa26se 2006m ooteo
BE0oL26l32e10s17 71 oolol3sez2
EElsmaa ooolms
BE0L02o63.2m 1019 4 0o10n36o24
EEO0LL062s623021308305 00110033100
EENOLL0O66220100%36067 ooll030ual
BE0aL2s6sa20r7% 0o0o32
EE00622083 l01o0s3s8e4s3
[ E0L0263r 21039 e loa
NuSmebter TGOOADD GwooowlAADD wwooooiAdD wwoooodd 0 GoDD ooiodd owoo0oBdD oGoowBdD oB0BDD GsoOoOmDD
ExDtraatcteion AnaDlyuseis 3abl 33n000o1r oonl 33000m1 aieo o30o0 oonn nnoooonn a37m0l1 3v0o0m wwoor woett e a0ml ewuomm 3 wo oweonnm aIII wMoouml ailo Myooumn STANDARD DEAVVIEARTAIGOEN::
FounAndaglytme ) 1wr w35s5 iusss nus7 238 n3i 228m 3ana e6l0s3 23m6 262 200
* Duplicate injection.
LOQ = 0.01 ug/g forliverand 0.01 pg/mL for serum
Centre Analytical Laboratories, Inc.
Page 360f 104 60525
EEE
----
Centre Study No. 023.042
Table XVIIL Summoaf PrFOyS in Adult Serum Samples at 17.6 ppm a.i. (Test Termination 19 Weeks)
Spomnsor CIe'nStre
1T9o1T M0003M6
1109220 FE 0o0o0o8s03e7s
11099309M 00s3
110994906F oooono0Mso3
1199m5s0 M oGooSsoMdn
191996+F9 peeoorosoat
199770
CoooOsoLn2
1F 0980 oo00n 08s
191999990M4 IooMm
20w0o00 oooooossoosuss
-
* Duplicate injection
NuSmebter
Eatcion Dats
Amis Date
Amite Found gum)
UIZ2II0OBBDDDD | 1T2210M0 111122880000 a0n
11220100880000 11122110000 11112280000 30
1I2Z0I0O8B0D0D 2L2010 111122380000 11598
122000880000 1GI2N0O 111122880000 552309
112210000B8D0D0 212010 111122880000 110
11I22010088000D 1122M100 11122880000 a21n8
I120B08D00 L1221I000 111122380000 220
uI22008B0DDD 1112210M0 1111228w0e00 11556
I121B008D00 112200 111122380000 116516
l122i10000880DDD 11122100000 121w72c8000 2m05
T STANDARD DEAVVIAETRIOANG:E: 615s0
LOQ =0.01 g/gfor livaendr 0.01 pg/mLfor serum
Centre Analytical Laboratories, Ic.
Page 370f 104 6Hos27
_--
Centre Study No.:023-042
Table XIX. SummaryofPFOS in Adult Serum Samples at 17.6 ppm ai. (6 Week Samples)
`SIp"on)sor
CenItDre
EEOOLL26221000000A O01I302JS
EELOOL6O6S322012012&1 0011003382266
EEOOLLOO662I120I202m 00I10033K82277
EEOOLOL226632I1201203%243 O0IIO0S3E2S8
EEOOLLOGZI62I12014*044 OOIIO3GES
EEOOLUL6Z3Z6II0420I%E0 OOll003SMRSS
EEO0L63S22I044F O01I3G6
EEO0LL62I26130201200 00l003S4M77
EE00LL62I623120103043 001503M8
EE00L1O02I623I:02M1Y044 00110033884499
----
MSeemtber OGOOSNIIAADD GGS0O0N0IIAADD GGOO0IIAADD OGOOIADD OGORROOIIAADD OOSXOTNOOIIBBDD G0XOTT00IIBBDD GGS3O0N0OIIBBDD GG33007700I1BBDD G_03300770011BBDD
ExtrDacuteion AnaDlaytseis FounAndaGlyytaen)
30710 I31-122000
1186
3377011 3n1o0o0n1
11521
33777011 3n000011
11557
33770m11 3s0n0o0u1t
e1d8
3m7011 sanntiizoonl
a3921
3377001 3n30o-14110011
a5519
3370011 3I0n-o111m010
0o32
330m1
001-110011
7158
33770011 nsonot
135
33777/0011 3n10o-11m01
1144
STANDARDDEVAIVAETRIAOGNE::~~ 658795
LOQ=0.01 g/g for liver and 0.01 pg/fomrseLru.m
J( CentreAnalyticalLaboratories nc.
Page380f 104
aout
CentreStudy No.: 023-042
Table XX.
SpoDmor oTrOeC BDuoe,e BDoro 0Z5o0sm zBoroA B23o0r8 M BDBiieUreMm iBeore mmi or zr
Summary of PFOS in Juvenile Serum Samples at 0 ppm a.i. (Test Termination 12 Weeks)
caDre ooonesiszs wooonoiznr oooonnszs peoeoerze ooonsatozo
pee0008131 pr0oe0e0wn8e1e3s2 ooooeoizms oooowaiezse peer]
NoSmuber BuDnuteon ADmuiss __FoAudmiiem) TZooAn Tzzmmo mesmatme NNOe ooAA nzmme uummsmmww NNee IIAA 1zZIo00 2n8s0w0 0o0o0ni mooAn unzz uuzssmwm NNeo ooAA nnzz ouossassm oooom
oA 1127004 nz 12700 ssw 1128-2900
NNQe
Wo112O7A0N0A Un127zz00 so117s2a8a-2s9w1m00 0NN0eQ0 OIAA nnzz oossaassmm00 000000s lIAA nUzZ o2ssassmw0o o00o00o1 loon imi uAnVeEaRAsGeE: o00o0n1s5y0
STANDARD DEVIATION: 000222
* Duplicate injection
NQ = NotQuantifible (Apeakwasdetected athecorrespondinganalyteretentiontime
`butwas lessthanthe lowestconcentraotfitohne calibrationstandards (0.0001 pg/mL))
`For values recorded as NQ, 0.00005 pg/mL(halfthe value ofthe lowest calibration standard, 0.0001 pg/mL)wasusedtocalculatetheaverageandstandarddeviation.
LOQ= 0.01 ggforliverand 0.01 pgf/ormserLum
CentreAnalyticalLaboratories, Inc.
Page3907104 600529
--_--_--nPBPBVH--HPHPRPMPA------------,_,--_--
CentreStudy No.: 023-042
Table XXL. Summary ofPFOS in Juvenile Serum Samples at 1.8 ppm a.i. (Test Termination 12 Weeks)
Sponsor Centre
ry
I"
2 `0008136
x20 23
Moo0s081?36
2230 0008137
ms 2250
o0o00o8s1i3n8
226 m6
00139 o0ns135
2M 2280
ooosi0 ooasie0
230 ooos1e
2300 o0aster
2M ome
2310 2m
oo0ooossitea3z
232 o0os1a3
BBE oni
233 o0oses
234M 23340
ooosues oous1es
set Nomber N2I00A 200A M204 270A UM2O0AA IZA NZ0A H200D 127000 290A U200A 120A UMZZ000AA I200A 120A 270A 120A 200A
Extraction Aualysls
Date Date
T2700 T2820
N20 NZ
uZsM0 zs
120 1282900
112200 22889900
12700 12M
1282900 Isa
1AM0 120
11293000 11293000
1200 1282900
12700 12W0
111228822990000
12ZmT000 s112m329o00
URM0 120
11228822990000
N20 282900
020 120
2s2M0 1ps2om0
AVERAGE:
STANDARD DEVIATION:
Auaiyte Found (sgimt)
0046s oom oooom 000044977 00160 001ss 0249 00020570s 0o0o0l7o4l7 0o.o00u9s98 0000x1309 00339 005s 0.o0o5s0s7s 0.0701
* Duplicate jection
LO=0Q.01 ug/gforliavnde0.r01 pgf/orsmerLum
CentreAnalytical Laboratories, Inc.
Page40of 104
R05.49
--------------------------------------------e
CentreStudyNo.: 023-042
`Table XXII. Summaryof PFOS in Juvenile Serum Samplesat6.2 ppm al. (Test Termination 12 Weeks)
Sponsor D 2s350r 26 F 226370 2A 370
23w0a1 2B390A a BF z2a0M 2s30e 2040 23244660 7
Centre D
0c0o8u1s46e. ooosiar oo0o0s8114a7 00000104s8 0o0o0o8s1i4s9o 0c0o0m81s5)0 oooosnisst oooooossitss2s 0o0o0m8i1s5s3 ooomise oooooosm1ssss
set Exacton Amis Assi Number Date Date Found (gmt) mW2200088 u12m70e0 11122s5m000 o0o115692 20D uz es ous u20DD 2uz0I0 etossoe 001s1t Un20DD 1n2e0m 1n2e83s00e0 0o0s5sm UZOD 12M 1283000 00852 UUZZO0DD 1122MM 11122S933000000 0o0o84m0 1200 nie n;sdmeo 00s 1u2Z00B0 N12200 11R1s2309000 00003s8s0E N0ZBD Nn2m0 L1RS2390000 000037803 UNZZIODD NL22I00 11228S33000000 000067776 UZIOD L270 1283000 0068s u11z2I70o0B8 1220700112119209000 007m1m
STANDARDDEAVVIEARTAIGOEN:: 00.0047636
* Duplicate njecion LOQ = 0.01 ug/g forliver and 0.01 pg/mL for serum
Centre Analytical Laboratorcs, Inc.
Page 41 of104 CHOBIT
------,----
CentreStadyNo: 023-042
Table XXIII Summary of PFOS in Juvenile Serum Samples at 17.6 ppm a.i. (Test Termination 12 Weeks)
`Sponsor n 247 2470 BE 2480 255 2530 2354 10
2380 2355 M 23550 2571 21570 BE 258 25917 23590 2360 2600 26M 263
Centre D 0008156 000816 ooomis oasis? o0as1ss ooas1ss 0008159 0008159 o0osic0 ooosico ooosist ooos161 come oasis oases o0asies oases oo0siss 000sl6s ooostes
set Estacion Amsipis Asiyte
Number Date Date Found ug/ml)
12000 HOD
N20 120
1129933000m00
0044%%
12700 N20 293000 01s
12700 H2700D
N20 127M0
29300 1293000
013s 0884
12700 HD
12700 1ATM0
293M0 1293000
oses 0551
H2700D 1270 1293000 021
UD 120 1S30M0 03%
HOD UZ
12M 12700
Nos 1293000
03s 0347
20D 1RM0 1293000 0547
12700 120 129300 0si2
H200D 27000
NANO 02M0
11293000 129300
017 ode
H2700D 120 1293000 040s
20D 20 2M os
UZOD 12M 1S30M0 0Sie
UND UZIOD
120 112700
193000 11793000
0439 0434
AVERAGE: 0.496
STANDARD DEVIATION: 0.184
* Duplicate injection
LOQ = 0.01 gle for liver and 0.01 pg/mL for serum
CentreAnalyticalLaboratories, Inc.
Page4207104
O52
--_--mmme
Centre Study No.: 023-042
Table XXIV. Summary of Percent Moistures for Mallard Liver Samples Spoor Coatre Averge m ID % Mobsters Tevre ooeosm 671 66 oooomoms 679527 s6ess oosool 77590 6wo oosooo; 7704 w6o oowssios m69ss 291 oownls m75s3 199 oososo 771a9 919s oooonm 7is4 w9o9s oooomm2 703s w19o9 oomozmes men0n BBOeL mosws 77636 w2s0 oosws mms1 22008 ooswo 7m2o0 BmiEe wwomn 67s60 0Bo owowwss 7nss mmmm mmsss m7ss mmS6 ocoomms Tms2 220% oomoam emso mm02 wwomm nnga mma3 ocmommoos eens as oom ma
CentreAnalytical Laboratories, Inc.
Pa43g of1e04
60523
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`Table XXIV (cont'). Summary of Percent Moistures for Mallard Liver Samples
Spomor Cae Average ID %Moture
6 wor 7 2nwm owmoem 6e9s7 9Ba wwms m7oss n55e wowmsn mm92 264 coossse 6m29 Bnos wooomnms 703 nnss mosm me2s nnss oommae aess 2u%m wwonms2 mms0 2n6e0 woenss 6ra0l EB0oLLO2e6s3221006656 001100701 $T1i0s ELes2067 o0Nn 824 EEO0LLO02266332211006689 0011003 778528 EL2e200 00s 74 EBLl6a20z0o7n1 0o0o7n6 775s EEOOLLese2sI02T0s 0ol0ess 87217s Enes20s oso 717 EELlese20m%6 oolwees T7i1s9 EBO0LE2S6202% o01l0e38s4 76680 EEOLlOGs20t08 o01s38s86 7726 Bmw ols 767 EEOLLoOe6sI22i1o0n8 0o0w3s8 87134
Centre AnalyticalLaboratoris,Inc.
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Figure 2.
Chromatogram Representing a 0.1 ng/mL standard for PFOS
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Figure3. Chromatogram Representinag 1.0 ng/mL standard for
PFOS
I leA eO neTe
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pe 4
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Figure 4. Chromatogram Representing a Reagent Blank for PROS (Centre ID Reagent Blank A, Set: 1120004)
(Rf
| EET dAh. mo!
)
I[EEEnEe A =
EfElEag18
Ds I
~| -
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*
: wlRArSe T
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Figur5e. Chromatogram Representing Control Mallard Serum for PFOS (Centre ID: 0003803 Blank A, Set: 112100B)
es
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Page 500f 104 GROSa2
CeStudnyNots023.e042
Figure 6. Chromatogram Representing Control Mallard Liver for
PFOS, (Centre ID: 0003804 BlankA, Set: 1120004)
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Page S1of 104
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Figure 7.
Chromatogram Representing Control Mallard Serum fortified with 10 ppbof PFOS
(Centre ID: 0003803 Spk A, Set: 112100B)
[BEETag EE. ==
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CeatreStudy No.:023-042 Figure8. Chromatogram Representing Control Mallard Liver
Fortified at 1000 ppb with PFOS (Centre ID: 0003804 Spk A, Set: 1121004)
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Pages3of 104
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Centre StudyNo.:023-042
Figured. Chromatogram Representing Juvenile Mallard Serum Sample (Centre ID: 0008143, Sponsor ID: 2332,
Set: 112700A)
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Figure 10. Chromatogram Representing Juvenile Mallard Liver Sample (Centre ID: 0008108, Sponsor ID: 2337,
Set: 1121004)
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Study Protocol 00P-023-042
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Amendments and Deviation
Centre Analytica Laboratories,Ic.
PageS6f 104
GRO515
Centre Study No.: 023-042
Cone ProtNo.p2302
STUDY PROTOCOL
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15. REFERENCES
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1 GUoSo.dEinvirbounoenParlrcPirctaecSteiannoAyrge,ncFy.nToRsaie,S40uCFRbPrCsto7a9n3dnAcct(TeSCAs).
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