Document dneL22j9ZyvbeDmn4zZn7Mm89
STUD TITLE ExtractionofPota`AsnsailyusmisPeUrsfilnugorHoPoLcCt-aEnelseucltfroonsaptreafyr/oMmas`sQuSaiplecSterroummetarnyd Quail Liver for
DRAETQAUIREMENTS
Analytical Method Requirements
STUDY DIRECTOR
Sean Gallagher
STUDYCOMPLETEDON
September 06, 2001
PERFORMINGLABORATORY / TESTINGFACILITY. Centre Analy3t0i4ca8lRLeasbeoarractohrDiresi,veInc. (Centre) StPahtoenCeo:ll8e1g4e-,2P31A-410638201 STUDY SPONSOR
3M Environmental Technology and Safty Services St.PaBuuPliO,ldMBinoNgx523-53313E33-310-93331 PROJECT
CenlCreenPtreotSotcuodlyNNuummbbeerr::0002P3-.002431.041
"Total Pages: 102
crozat
CentreStudy No.: 023.041
CFeofmoenomSmuetryatonNtusmbfaom C3r0a8S.en ttshGdul LEvsisaociorn sofUsinPgomams PESlicencit,reoStpSeraamyno/Minastswi4SspepCcPterRotmeetrry.1"5ccoonydouBcptesdsfowrr5 ii3M BaEBv2ior8noTnmSenCtAalcTGeoochnnoloegy 4and
ir
Principal Invesdgator
CentreAnalytical Laboratories, Inc.
'
Ler HAWS
R Soy DiE e Sean Gallagher 1
aa
SR oom Taney nd Stet Seis
Cou AinLeto e.
Bf r y
elo
Date.
Peri
cosan
CentreStudyNo.: 023.041
QUALITY ASSURANCE STATEMENT
C0a2ne3dn-tQ0eu4a1iA,lnaeLlnityivttielcreadlf,oLr"aEAbxnotarrlaaytcsotirisioenUss'oifQnuPgaolHtiPatLsysCi-AuEshlseuPcretarrnfoclseupoUrrnaoioytc/tMraaensvessiueSlwpfeeodcnatCtreeonmtferrteomStQuudaylNuSmebruemr `wOepreeratrienvgiPerwoecdeduforres,cotnhdeucSttudayccPorrodtioncgol,toanCdenatllreapApnlailcyatbilcealGoLoadboLraabtoorrriayet"so'rAylSlPtrapanhcdatasirecdse Standards. All findings were reported to the Study Director and to management.
Phase 1. Protocol Review 2. Extraction 3. RawDa &
Summary Table: Review 4. Raw Data and Draft Report Review S. Final Report Review
Date Inspected 12/19/00 12/1900 2283101
332601
9601
Date Reported Centre
to
`SDtautdey RDierpeocrttoerdatno.d
Management SponsorManagement
122100
1272800
122100
1228000
3901
302301
4901
so
9601
9/601
oe) Naomi Lovallo
doneke
Sr. Quality Assurance Auditor
Dateele
Centre Analytical Laboratories, Inc.
Page 3 of 102 2113
Conestty No mont
`This report, for CentreStudyNumber theraw dataforthe study.
023-041,
is
8 trusand
`complete
representation
of
Suboltadty S3Co0un4et8reCRoeAlslmsarigeehnPDaAriLivae6b0o1rato, nc.
(814) 231-8032
Principal Investigator, Centre:
CSaoenneitAlte! Labor, Tc.
J Bue P
Cen Ande! abortries, oc. Facity Masagement:
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4-0)
PRriidae
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.
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Spons Reeescnaive, 3M: SE
eteeeiia
<F1 Bhviroamental Techology andSafetyServices
Con AyeLberoron,s.
Pasdti2
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Centre Study No. 023.041
STUDY IDENTIFICATION Extraction of PotAanaslsyisuimsPUesriflnugorHoPoLcCt-aEnleescultfroonsaptreafyr/oMmasQsuaSiplecSterroummetarnyd Quail Liver for
CENTRE PROTOCOL NUMBER: 00P-023-041
CENTRESTUDY NUMBER: 023-041
TYPE OF STUDY:
Analytical
SAMPLEMATRIX:
`QuailSearnduQuamil Liver
TEST SUBSTANCE: SPONSOR:
Perfluorooctanesulfonate (PFOS)
3M Environmental Building 2-3E-09
Technology
and
Safety
Services
PO Box 33331
St. Paul, MN 55133-3331
STUDY DIRECTOR:
Sean Gallagher `Wildlife Intemational, Ltd. 8598 Commerce Drive Easton, MD 21601
SPONSOR REPRESENTATIVE:
`TESTING FACILITY: ANALYTICAL PHASE TIMETABLE:
3RoMchEenlvlierRoonbmiednteaalu Technology and Safety Services Building 2-38-09 PO Box 33331 St. Paul, MN 55133-3331
3Ce0n4t8reReAsneaalrytcihcaDlriLvaeboratories, Inc. State College, PA 16801
Study Initiation Date: `Experimental Start Date: ESxtpuedryiCmoemnptalletTieornmiDnataet:ion Date:
12/08/00 12/18/00 03/08/01 09/06/01
Centre Analytical Laboratories, Inc.
Page S of 102
creas
Cone Stuy No: 23.041
PROJECT PERSONNEL
TTvahhreeiofSuotslupldhoyawisDnegsiopeeftrosroenfinoercltyfirsomprCejnettewAansalSyteiacnalGLalalbgohseornast,WIincl.deweIentsempaaticoenasl aLin.
Name
Emily Stuer
Dave Bell
MisaKennedy Whisel ohnFahey TiffanyProctor Angela Morgan Michele Armand LawrenceOra Rickey Keller Shawn Rob Karen Risa
Tide
Scientist
Scientist
Supervisor Operations Manager Technician Technician Technician Sample Custodian Sample Custodian Sample Custodian scent
Cone Ayia Laborsre, ne
Pag or 102 crog
Centre StudyNo.: 023-041
TAOFBCOL NTEE NTS
GQUOAOLDITLYABAOSRSAUTROARNCYEPRSATCATTIE ECMEECNOE TMvPLI.AN.CEcST.ATcEMoENsT csrorePag32e
CSTUEDYRIDTENITIFFOIIFCAACTUIATONTH.E.I.NOTINCITY... PROJECT PERSONNEL...
8
E TLIASBTLOEFOTFACOBNTLENETSS...c.c.c.c.c.cT occmosssmssmmossneeoss
LIST OFAPPENDICES...
11
23.00 OINBTJREOCDUTCITVIEON......coccocccmmmmmmssessoosonrnoes 1122
5600RDEFEERSENCCERMAOITFEPARNITAALLIYTOIC.NA.L.M.E.T.H.O.D....o.ooomoonroro 1413
62 Preparation of Standards and Fortification Solutions...
14
7066.65EDXQ esPcEriRUpItMioEAnNoaTfnIANndLsEtXDrAtEuMmSDeIIniEtGaCNnldoCOv puelrnaatiinog n.c ......Cs o.nd.iioonss.r..e..r........1....1.8..615 91:00.0 RCONECLT USIOEOFNDN SA.T.AT.ANIDSO AMPNLES... ...coooooorsro 1189
CentreAnalytical Laboratories, nc.
Page Tar 102
Cnoany
CentreStudy No 023-041
ISTOF TABLE
TableL Table IL.
SummoafPrFOyS inReagent BIAIKS.....ccvrrossnPa3g1e Summaryof PFOSinQuailLIVE BIADKS ccs22.
Table Il. TableIV.
SSuummmmaarryyooff PPFFOOSSiRenGOQVuEariileSseirnuQmUBIAAIIKLSIVE... ....cccoeo2322.
TableV. Table VL.
SSuummmarmyooaffPPrFFOOySSiRnAeducltOLiviVenrQeSUarialimSepeartlUs.ep.ps.m.a...(.T.es.t..oomeo 24.
TableVIL. TSuEmmMaBryHofO1PN9FOWSECiknSA)dr ult iver Samples s at 1.8ppmai.s (Test 25
Table
VIIL
TEMD6RWEEHKSO) N Summaryof PFinOAduSlt
corres Liver Sampalte6.s2ppma. (Test
26
Table IX. STumEmarNyofD6PFWOOOSKiNSn)Aduo lt Liver Sar mples at 17.e 6 ppmai(Ts est 21
Table X. STuEmMmRaArLyoONfP1F9OWSEiEnKSJ)uvr enileLiverSamplr es at0ppm af, (Tr est 28
Table XI. STuEmMmRaArIyOoNf P12FOWSEEinKJSu)venv ile Liver Samplr east 1.8ppmai. s (Test 29
`Table XII.
TEMRAION 12 WEEKS) rvs SummaryofPFOSinJuvenile Liver Sampalte6.s2 ppam. (Test
30
TableXII. TSuEmmMaIryDofO1PN2FOWSEEinKJSuv)enir le Liverr Samplr east 17.6 ppm a. (Test 3]
TableXIV. TSuOmRmaRrOyoNf1P9FOWSEBiKnSA)dulc tSeruo m Samps lesat 0m ppm a.o i. (Tests 33 `Table XV. SummaryofPFOSinAdultSerumSamplesat 1.8 ppm a, (Test
Table XVI. TSuEmTmoUfa6PDrWFEOyEOSKSiNn)Aduc ltSerr umSamo plesas t 6.2s ppm ae . (Tess t 35 Table XVII. Summary ofPROSin Adult SerumSamplesat 17.6ppm ai. (Test
`TableXVIIL SummaryofPFOS in Juvenile Serum Sampatl0pepsm .i. (Test
`Table XIX. STummEaryR of1P2R FOWSEO iEnSJ)uRvenilec Serum Samplr es at 1.8ppmas .. (Test 38 Table XX. T SummEaryN of1P2OWEFiERKnSJO)uver nSile Serum Samr ples at 6.2 ppmr a. (Test 39
CentreAnalytical Laboratories Inc.
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Centre Study No. 023-041
LIST OF TABLES (continued)
`Table
XXI.
Summaryof TERROR
1P2FWOESEKiSn)Ju.veensielrerSmeerruamrSsasmspslresmnatss1s7.s6spmpsmstas..mn(Tsensstns
Page 4
`Table XXII. SummaryofPercent Moistures for Quail Liver Samples.................41
Centre AnalyticalLaboratories, Inc. :
Page9of 102 n25.49
CentreStudy No.: 023-041
Figure 1. Figure 2. Figure 3. Figure 4.
Figure 5.
Figure 6.
Figure 7.
Figure 8.
Figure 9.
Figure 10.
LIST OF FIGURES
Typical Calibration Curve Or PROS...) Page
Chromatogram Representing a 0.1 ng/mL standard for PFOS............... 44
Chromatogram Representinag 1.0 ng/mL stanfodrPaFOrS.d.............. 45
RCehargoemnattBolgarnakmAR,epSreet:se1nt2i2n0g 0a0Re)agce.n.tvBlcarnskofomrrPeFoOmSs(nCsenotsremIsDosnsnd
OC0hLr1o4m2a4toBglraanmk RAe,prSeets:en1t2i2n0g0C0o8n)trc ol Quo ail Sc erumfo orPFo OS (n Centrs e ID:]
Chromatogram 0007870 Blank
RAe,pSreets:en1t2i1n9g0C0o8n)trcol QeuailcLiveer for
PFOS,
(Centre
ID: A
nCgh/rommLaotfogPrFaOmS R(eCpernetsreenItDi:ng0C0o1n1t4r2ol4 SQupakilA,SeSert:um1F2o2r0t0i0f4i)e.d.w.i.t..h.5.0.0.........49
wCihtrhoPmaFtOoSgr(aCemnRterperIeDs:en0t0i1n1g4C2o3ntSrpoklAQ,uaSeit:Li1v2er18Fo0r0tiAfi)e.d.a.t .10..pp.bo....50
C00h0r7o9m6a5t,oSgproanmsoRrepIrDe:se9n5t4i4n,gSJeutv:e1ni2l2e0Q0u0aiAl)S.e.r.u.mceSacmcprloer(rCeenrterse ID: 51
C00h0r7o9m2a6t,oSgproanmsRoerpIrDe:se9n5t4i4n,gSJeutv:e1ni2l1e80Q0ua8i)l..L.iver Sample (Centre ID: 52.
CentreAnalytica]Laboratories, Inc.
Page 1007102 2150
CentreStNou.: 0d23.y041
STOFAPPEND Page
AppendiAx. SAtumdyMProEtoNco2Gl00dM0DPE-E02NV3-Ot04N1S(Cv entreSte udy No.r 023-v 04a1n)d e $3
Centre Analytical Laboratories, Ine.
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CentreStudy No. 023-041
1.0 SUMMARY
(spCreeorntutomrceolsAa0nm0aplPly-et0si2c3af-lo0r4Lt1ahbe(oAdrpeaptteeonridmcii,nxaIAtn)ic.o.n (oCfepnetrrf)lueoxrtoroaccttaendesquulafiolnaltieve(rPFsaOmSp)leasccaonrddinqgua(i0l Tqwhueaeriellidlmeiitvteeorrfmsqianmepduleinsatrhaenfnmgoeetrtdqhufoaardiolvmtleirnviooefrniwc-anqatuisaonn1ts0itfpuipdbbylee(nCldeenfvteorlresqus(taauidplyesa0ek2r3uw.m0a51s40)d.negt/ePcmFtLOe.dS aTitnhettshoee Wcceaolimigebhrstaptobianosndisis.ntgaRnadenasarilddysutee(s0r.oe0ft0e0Pn1tFiOgonS/tmiinLmte)hebtquouta8wi3la7sseglr/eugsms. tshaTamhnpelsteehserrelasonuwlgetessdtfarcroonmrceep0no.tr0rt0aet2di1o2onnpogaf/wmteLht.e levels 10.263 pg/mL. T19h50e%%av.e1Tr1ah9g%ee.apveercreangtepreercocveenrtyrecsotvaenrdya+rdsdteavnidaatirodndefvoiratPioRnOSfiornPsFeOrSuimnsalmivpelressawmpalses1w0a8s%
2.0 OBJECTIVE
Tshpeecoibmjeencstoivfeqoufatihilsisvteruadnywdqausatioldseetreurmmuisniengltevheelasonaflpyetrifclaulomreotochtoadnsedseulsfcorniabteedi(nPFOS) in protocol 00P-023-041
0 DUCTION TaPhenirdsflrueqopuroaorlotcdtelatinaveiesl,usltfuhosniarntegesuoltrthseoOtfhatneahrlyFatlniucaoalrlyoscimhseefmtoihcotahdlesdCeeotnmetriptmoliuendna,dtis"oEFnxortrofamPctFSiOeoSrnuimonfqfourPaoAltnaasslesyrisuuemm PUUessriilnnlggorHoPoHLcPCtL-aCEn-lcEeslcuctlcrftoorsnoaptsreparyoa/ryM/aOMstashseSsrpeFclStuproeorcmotecrthoremyme"itcwraiylt"hCtohamenpmdoauifn"idEcsxattrFiarocotnimsonlLiisvteeodrfifnorPSeoActntaaislosynisui6.ms tTphrheoeetxospctoeulrndiymuemwnbatesalri0tni0tPei-a0tre2d3m-o0ni4d1Da.netcTeaehwmeatbesexiMrpaeorr8,icnm2he0n08t0,a,2l0w0sh1ta.erntdattheewsatusdyDedcireemcbtoerrs1i8g,n2e0d00C,eantnrde
Centre Analytical Laboratories, ne.
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`CentreStudy No. 023-041
4.0 TESTSYSTEM
Trehceeicvoendtroonl Nquoavielmsbeerrum28a,n2d0l0i0vefrruosmedWiflodrltihfeemIanttrerinxatbiloannaklsLaindd.mEaasrtioxn,foMrDti.fications was sheerumcwonatsroal squasililtighveenrCewenatsrdewIsDiognfe0d01t1h4e2C4e,ntre ID of 0011423 and the control quail pfFeiurfgtsuyos-nstniexl10q,uoan2i0l0A0us.geursuTtmhes1a6sm,apm2lpe0ls0e0sanawdnedrseisxsttotyroqerudeadiflfroolzzievenen.r suanAminlplatedhsdeiywteiwroeneraelreltcowegeignveetddy aiqtnuaCbieylntCsreeenmtaoenn sfraomzpelnesuntainldthtewyewnetryequlaoiglgeidveirn sbyamCpelnetsrewepreresornenceelivoend FoenbrFueabrryua2r6y, 2205,012001 and steveg ISnsaeo.mcpailanetdeldogwii{ntrhiaetnhd<iOscpshytauoidnfyo.tfShteocrussattgooerdrayegceiornrefdocsrowmraidtlsilconbaenckabneepbfaetoufConeundntidrneitAnnhatelhyetairwcaawldLdaaaabtoaprapatacockrkiaaeggse.e associated with tis study.
5.0 REFERENCE MATERIAL
TEhnveiarnoanlmyetnitcaallsTteacnhdnaorldogPyFaOndSSweraviscrese.ceivedatCentre on June3, 2000from 3M mmTaahtteeerriiaaavllaiwwlaaabsslessttioonrrfeeoddrmfaartcoiczooennr.difonSrgttatbohieltihtryeefcwearesnecneotrmaatsetsoreifsasilaendiasflinylistsiihtsiesad cnsbtdeulwadoyaw.bstut Tsetheheed rrpeeffreerrieennoccee expiration. The solubiolfitthye reference materialwas otrelevantothsstudy.
PFOS
00023082 TCROO0I7-46 979
Themolecularstructureof PFOS is given below,
0&1!
PChReOmiScal Name = Molecular weight =
o
we
4P9er9fl(uCoyrFoo1cSt0an3e)sulfonate
dNeortiev:edT,hiesnpeouttarssailummopleercfullueoraonodctsatnacnsdualrfdonfaotrem 538.
from (CaF
wShOicKh],PFmOolSec(ualnaironw)eiisght
`Centre Analytical Laboratories, Inc.
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n2153
Centre Study No 023.041
60 D)
N OF ANALYTI
0D
SEPplaeutcoytrtroioccmhaeeltmrimyce"atlhoaCdnosdmpeno"tuEitxnltdeadsc"tFEixrotonrmacoStfieornuoPmoftPafosorstiaAunsmailuyPsmiesPreUfrsluiunoogrrHoPoLcCi-aEnleescutfroonssperaoOryt/Mhaesrs
SSppeocotrroocmheemtircya"lwiCtohmtpheoumonddisficFartoimonsLilvisetredfborelAouwlwyesriesuUsseidnogHrPodLsrC-seEttluaedyca.ttroespraOyt/Mhaesrs
6.1 Extraction Procedure
seEcro0ncd0sa.inLOnamleiamqbuLeotfooofrflt0f.hc5eaMtsieTornBuomAfaawpnpadrso~apd0rdi.es5dtgt0ostsahamemppllleiev,erotfshaleimsvpaelmrepswlaaessnwdueserde vfoor rtheesexptraocti0o1n
oSncsdheeedtlu1i0mvebrssoatmahplmtehspe.lsaeeTnrwsduomm1mlan.Ldowf0lai.vse2ar5dsdMaempsdlotedosit.uhmesEcaeacrrhubomsnasamatpmelplelsaedsi.uFmibve0o.5mmLuLotfweMsTBi aEddwaesd
ssohavamekpnelreafwnodars~dar2ni0aemdlyizonen.daabnnydtNLh-CeE/nvMcaeSpn/tMarnSidfeultgehecedtnfroorsrepcr~oayn1.s5tmiitt.eFd owuitrhmw1Lismotpf.tohonefgobrgainwirccilsaty-eEarcawtcaiohsn
62 PreparationofStandards and Fortifieation Solutions
oparnonaoytwdicaaslpSLroaelbpioatrroaentdsoarwtieeasrceopnrpocrteeoncptoarlart0ei0doPon-n0o2f3S.1e00p40t1eu.gm/bAmenlr,ibn1yd5i,dvii2sd0suoa0ll0vsianosgcksphecoifwieed isonluCtiaonnoef
L(oetoimfeicctateidonfosrtapnudratryd volume up 100 mL
oalnudtisoalntwcaosntpernetp)ariendmbetyhtaankoiln,g with methanal,
1
`mFrLoomftthye
so1l0utmiogn,oftah1e0stpagn/dmalr,d geek ri. bringing the
Tnfgore/tmif0Li:c1asttiaognnd/asmrtLdawfnoadrastripdfrieacpnaatdiroebndrbisnytgatinandkgairtndhgwea1vs0om plruempoeafrutL ephdeb105y.,11Wt0ak/0inmpge 1w0imnLmoeftthhaneo1l.0 Ag0m.0t1
100 mL with methanol,
standardandbringing to
gAs/emtLofssotlauntidoanrsdisncotnhteafionlilnogwiPnFgOmSanwnaers.prepbaydriluetiodnofthe 0.1 g/mLand 0.01
Initial Cone. gm)! 0[1 00.011 001 001
Centre Analyt!oicfalPLFaOboSratories, Inc.
Volume (ml) 25 51 2 1
Died10t0 (a) 110000 100 110000
Fil Co0m0e0(5ug/L 00.000012 0000000025 00001
Page 140 102
e--
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Centre Study No. 023-041
"The stock standard solution and all fortification and calibration standard solutions were
sptroerpeadraitnionacraenfbriegfeoruatnodrin(4ther+a2wdCa)twaahsesnocinaotteidwnituhsteh.i
Documentofasttaindoarnd report.
63 Chromatography
`Quantification of PFOS was accomplished by LC/MS/MS analysis using electrospray
LC/MS/MS. TheretentiontimeofPFOSwas ~4.4min.Peaksweredetectedinthe
control matrices comresponding to detected were significant enough to
the analyte retention time alter the results reported in
tahnids
sstoudmye.ofthe
amounts
6.4 Instrument Sensitivity "The smallest standard amount injected during the chromatographic run was equivalent to 0.0001 pg/mL ofPFOS.
65 Descriptionof Instrument and Operating Conditions Mass Spec: PE SCIEX API 3000 Biomolecular Mass Analyzer
Interface: SCIEX Turbolon Spray Liquid Introduction Interface. Harvard infusion pump
Computer: Dell UltraScan P1110
Software: HPLC:
PE SciexAnalyst 11 WHeiwnldeottwsPaNcTkard (HP) Series 1100
HHPP VQuaactuPuummDpegasser HP Autosampler HP Column Oven
HPLC Column:Genesis Cs (Jones Chromatography), 2.1 mun x 50 mm, dys CInojlecutminonTVemopl.:; 103p5L.C Mobile Phase (A): 2 mM Ammonium Acetate in ASTM type I water Mobile Phase (B): Methanol FlowRate: 0.3 mLmin.
Centre Analytical Laboratories, Inc.
Page 15 of 102
C72455
(CentreStudyNo: 023-041
Ti0me %6A %4B 0 0 10 7705 60 14000 no 6 4
Ions monitored:
Approximate
APmRiOSe neMgoadieve Transit4io9n9M3o9n9itored Retention44T0ime (min)
`Tune File Parameters
1CSo-nltosrporlasy
42s0et00
DP-Declustering Potential
510
FP-Focusing Potential
2300
EP-Entrance Potential
100
CE-Collision Energy
EY
CXP-Collision Cell Exit Potential
5
`CEM:ChannDeFl-DEelfelcetcrtoonr Multiplier
238000000
NGeabusliFzleorwGsas
S1e2t
CCoulrltisaiionnGGass
1"3
TIS Temperature
350C
6.6 QuantiatnadEtxaimoplne Calculation
p"eTaenkamirccraolwiatesrmseoafssuarmepldeanordtcahleibsrtaatniodnarsdtacnudravredwwaass giennjeecrtaetdend(tuostihnegLOxMfSi/tMwSe.ighTehde linear regression) by Analyst software using six concentrations of standards. The concentration for quail serum and quail liver was determined from the following equations UseEquation 1tocalculatetheamountof analytefound(inng/mL,basedon peakarca)
pursoinggratmh.estTahnednarudsceuErqvuea(tliionnea2r rtoegcraelscsuiloantepahreameatmeorusn)togefnaenraatleydtbeyfotuhendAnianluysgtgs(ofgt/wamrLe
for serum samples).
CentreAnalyticalLaboratories Inc.
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CentreStudyNo: 023-041
Equatio1n: Analyte found (ng/mL) =(Peak salroepae intercept)
`Equati2on: `Anlyte found (ug/g) =(anal.found (og(/AmVL)(xmLF)Vx(msaLm)plxeDwFix.E)V(m)) x1L0u0gmg
Where: FV = Final Volume DEVF == DEixlturtaicotnioFnacVtoolrume AV = Aliquot Volume
ForsamplesfortifiedwithknownamouonfPtFOsSprior toextraucsteEiquoatnio,n 3 to cEaqlucualtatieo3tnh5e percent recovery. Recovery (4) =
(anal.found(ug/g) --avagm.oaunanltyatdeidneedt(rlg(/ugg/)g)| xi1g000ngx100%
Anexampleof acalculationusinganactualsamplefollows:
Quailliversample Centre ID 0007870 Spk A (Set: 1219004), fortified at 1000ng/gwith
PWhFeOrSe.: peak area isnltoeprecept dilution factor
=m e- 4a63m -0
ng/g added (fort level) = avg. amt in controls =
1000 ng/g. 0 (Not quantifiable)
feixnvaal cvtoilounmveolume aslaimqpuloet vwoeliguhmte
== S1mmLL == aosms
From eAqnuaaltyitoenf1o:und (ogiml) =
From eAqnuaaltyitoenf2o:und (ug/6) =
= [14783%-463] 39mngmL (3(.Gm9Lxnm0L5ggx)/10m0xLSmxl) x1L0u00g08
= 0975 pg/mL
CenteAnalyticalLaboratories, Inc.
Page 1706102
cnoasy
_--mmm--m--mm
CentreStudy No. 023-041
From e%quaRteicoonve3r:y = 0.975ug/ml=01u0g0/0mnlg)gx(1000ng/lug) x 100%
= o%
7.0 EXPERIMENTAL DESIGN
Each sctofsamples (liver two matrix blanks fortified
aotrskenrouwmn)ccoonncseinsttraetdioofnso,naendr~ea2ge0ntsambpllaensk.,
oEnaecmhastarimxplbelawnaks,.
extracted using the appropriate method and then analyzed in duplicate.
8.0 RESULTS
`bTlhaenkPsFaOnSdfqouuanildisenrtuhmerbelaangkesntabrleagnikvseanrien TlastbeldeisnIIT&ablIeILI.. The PFOSinthequailliver
Individual recoveries for average percent recovery
PFOS in standard
the liver samples deviation for PFOS
are detailed in in liver samples
Table IV. was 95%
The 119%.
Individual recoveries for average percent recovery
POS in + standard
the serum deviation
samples for PFOS
are detailed in Table in serum samples was
V. The 108% +
10%.
atPtRhOeScinothre qurailelisavneraplsyaotmeprlneetsednrtaiinognentdifgmreobmuntown-aqsulaentsisftihaablnetlheevellosw(eastpceoakncweanstdreatetciotoefdn
`tTheabclaelsiVbrIa-tXiIoInL.staTnhdearrdessu(l0s.0a0r0e1reppgor/tmeLd)ontoa
8.37 wet
peg. weight
Individual besis.
results
are
listed
in
FOS inthe quail serum samples ranged from 0.00212 g/mL. levels to 263 pg/mL. Individual results are listed in Tables XIV-XXI.
`The average percent moisture forthe quail liver samples are given in Table XXII.
20 CLUSION!
"The quail liverandserumsamples weresuccessfullyextracted and analyzed accorditnog protocol 00P-023-041.
CentreAnalytical LaboratoriIensc.,
Page 180f102
Cn2458
_--
Centre Study No; 023-041
10.0 RETENTION OF DATA AND SAMPLES
L`aWbhoernattohreiefsi,naIlncr.epwoirltl ibsecosmhpilpepteed,taollthoerisgpionnalsopra.peTrhdiastdaogeesnenroatteidncblyudCeefnatcrieliAtny-aslpyetciicfailc
raw data such as `submitted. Exact
instrument logs, copies of all raw
however exact data, as well as
copies of temperature logs will be a signed copyofthe final analytical
rLeapboorrtataonridesal,l Ionrci.gianraclhifvaecsifliotryt-hspeecpiefirciordaowftdiatma,ewsiplelcibfeierdetianin4e0dCiFntRhPearCten7t9r2e. AnRaeltyatiinceadl
samplesofreference substances are archived by the sponsor.
CentreAnalyticalLaboratories,Inc.
Page 190f 102 C2159
_-- Centre Study No: 023-041
Centre Analytical Laboratories, Inc.
Page 20 of 102
C2160
_--
`Centre Study No. 023.041
Table I. Summary of PFOS in Reagent Blanks
Sponsor D
Centre I'y
BEo RReesaggeenmcBDllaunkkAA
= TM
RReeaggmeBnitBmlknAkAt
wn mo
RReeasggeenBiBllnakoAkA
mo RReeaggeeBnltBulkuAkA
mmoo RReeggeBmlBalkuAkA
m"o RReeggemnBBulkkAA
mo RReesggaeBnltBmlkuAkA
mn RReegsgeennBiBllnaknAkA _
* Duplicate nection
NeSmebter ExrDaaceton ADmaeb_FouAdus(iyeten
1R220I80000A4 2121108000 11211990000 NNoo
12808 DINB
I121E800
11222000000
NnQo
2L1I0SAA 21211990000 112222110000 NNoo
1220I90000B8 112211990000 11222112220000 NNQQ
2I0Z2000A0A 1122000000 112222220000 00000000220000
1D202000008 12222000000 1D22220A00 NNQQ
CGOONSOIIAA 3ISSO0I1 3366770001 NnDD
0O0G6O0IIAA 33660011 3y7o0n NNgo
STANDARDDEVAIVAETRIAOGNE: ~~
NQ NQ
NbuQt w=aNsoltesQsutahnatniftihseblleow(eAstpecaokncweantsrdaettieocnotfedthatetchaelciborrarteisopnosntdainndgaradnsal(y0t.e0r0e0t1enptgio/nmtLi)me ND = Not Detected
FoForrvvaalluueessrreeccoorrddeeddaass NNDQ,,z0e.r0o0w0a0s5ugse/dmLtoc(ahlaclufltahteetvahleueaovfertahgeealnodwessttacnadlairbdradteivoination. standard, 0.0001 g/mL) wes used to calculate the average and standard deviation.
LOQ= 001 ug/g for liver and 0.01 pg/mL for serum
(Centre Analytical Laboratories nc.
Page21of102
C2162
_--mmmmm--------
Centre Study No 023-041
Table IL. Summary of PFOS in Quail Liver Blanks
`Sponsor m na m Na
ass 4s4 ase 456
Centre D
01423Blk A 0143 BlanAk 011423 BlukA 0011423 Blank A 007SI0BlnkA ONTSTOBlmkA* 00772BlkA 000TST2BlnkA
Set Number 12800A 121800A 1218008 1218008 121900A L2I90A O3060IA 030601A
Extraction Aulysis Date Date 121800 12/1900 121800 1219/00 121800 122000 121800 122000 121900 122100 121900 1221/00 E01 3/701 601 3101 AVERAGE:
STANDARD DEVIATION:
Amalyte Found (uglp)
No No 000113 000109 No No 000120 000110 0.000590 0.000578
Table II. Summary of PFOS in Quail Serum Blanks
`Sponsor D TM ma mn nm nm nm a m
Ceatre D
0011424Black A 0U44BlAk 0U44BlnkA 011424BlrAk 001144Blnk A 0011424 Blank A* 011424BlarAk 01144 BlanAk
* Duplicate injection
Set Number 1219008 1219008 12000A 12000A 1220008 1220008 G30S0IA O30S0IA___
Extraction Amaysis Date Date 121900 12212200 121900 12212200 122000 122200 122000 122200 122000 12222300 122000 12222500 SOL I6TOl 3SOL___ 36701 AVERAGE:
STANDARD DEVIATION:
Amaiyte Found (ig/ml)
00136 00144 00138 00151 00127 00109 0.00885 000.00811559 0.00384
NbuQt w=aNsoltesQsutahnatnitfihaeblloew(eAsptecakowans dectecetoefdntahtettchaelrciborraarteistopnosintdainondgaarnndasly(t0e.r0e0t0e1ntgi/onmtLi)me
For values recorded as NQ, 0.00005 g/g(half standard, 0.0001 pg/mL) was used to calculate
the the
valueofthe average and
lowest calibration standard deviation.
LOQ = 0.01 ug/g forliverand 0.01 pg/mL for serum
Centre Analytical Laboratories, Inc.
Page2207102
24562
_--m-a
CentreStudy No. 023-041
Table IV. Summaryof PFOS Recoveries in Quail Liver
Sponsor D
Ceatre I"
Set Number
Extraction Date
Analysis Date
Amt Added oglg)
Mm mo
MGIOISAKSAKTA L1I2ISM0AA 2211880000 112211990000
0 10
mo mo
OOIISSKBB* LLIINSOAA 112211880000 112211990000
2000 2000
mo mo
OOUIMI3SSKKAAT 1122IIB0KBB 2211880000 112222000000
1000 1000
mo mo
OOOOUISNKSKBB 112200AA 112211880000 1122220022010000
20000 20000
44544 COOOUTBSTIOSOKSAA II2211990000AA 112211990000 11222211//0000 11000000
45 458
OCUOT0BBTTOIOSSKKBB 1I221190000AA 11211990000 11222210000
2200000000
456 456
O0OTTRERSSAKTA
ONG 006A
EOI E01
370 3700
2 I
455 456
o0ouOnMsTTRSspKkmBe 0G300G600I1A
601 digo
3700 3mon
20 20
STANDARD DEAVVIEARTAIGOEN::
RELATIVESTANDARD DEVIATION:
* Duplicate nection
LOQ=0.01 g/gforliavnde0.r01 pg/fomrsLeru.m
Reco%very 02 104 101 103 3 no 0 0 % 103 8u 9 8 = 594 11 12
Centre Analytical Laboratories, Inc.
Page 23 of 102
n2483
_----m--
`Centre Study No: 023.041
Table V. SummaryofPFOS Recoveries in Quail Serum
Spomnsor
Cemntre
NuSmtber
ExDcuieon
AmDbaess
AddedAmotpml)
% Recovery
mmoo OODIIMI4ASSHKHAAT 112211990000B8D0 112V1I990000 1122234200000 550000 mo OIGUSKB RIND 12I900 DE 10000
01036 0
mToo OOUDIAOSAKSBKA 1I22100BAD 11222900000 12122322200000 10000000 mo ODlAMSPKAC 12004 122000 122200 500
1)06 103
mmoo NOONAISSKKBBT I2Z00000AA D122200000 112222220000 10000000000 mo OISKA I200B 12000 m2 S00
1E0l3 108
mmoo OGUIGANASSKKABT 1D2000088 21222000000 D12222223000 10s0w000 mo OIASKBY 1200 122000 1222230 100000
1110 a
mmoo OONIAASSKKAAT OGOOSA uSs0o1 Y36e70w1 mo OUGASKB GO0IA usoL 36701
110000 1000
22 07
nm 0ASKBT G0SOIA uso ver 1000 11s
STANDARD DEAVVIEARTAIGOEN:: 1906
RELATIVE STANDARD DEVIATION: 9
* Duplicate jection
LO=0Q.01 ug/gforliverand0.01 pg/fomrsLeru.m
Centre Analytical Laboratories, Inc.
Page24f 102
2164
--_----ee
Canes No: 23.00
Table VI. Summary of PFOS in Adult Liver Samples at 0 ppm a.i.
(Test Termination 19 Weeks)
-- SpoEnsor GeEazrs NSoo mbrhuemor 0 Soe NTumobnesr DTatae
A"pwee poAmme Ter Date Found (upp)
-a-
Qoommaae
dDniuweeoss maimeeo wlhaelewm
ss hg
ome dod ew lee oe
--~
wwoooivvsee DDdiuweeesrs mmaweemo m ilmoeew eowea ami umd ame am od
pi-d
woomwn
iwwoeorrn lweveme hllaeeeww
em he
r-o~) -
wwQooownss nmdeeuownssd wDwaowee hilaeaenmme seaoomn owe Dawes wm lew bom
--> wWCooowwwss wawemersd Daiawmowo lllaawmwes ooommme
-
BGOorm eeB DierSUTvAEiNsD.eA.RD.DERlVIeATmeION,
ose 3
[--
NQ = Not Qunnifible (A peak ws detected he responding ale rc me
`but was less than the lowestconcentrationofthe calibration standards (0.0001 pg/mL))
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.
a
LC0onQte=t001apgtfor overaondI 0.0 pnfors.erum ge25 1<S1E03492u33Sd3I3]5s=8% S21wEi4g3
"0155
_--_--
Centre Study No.: 023-041
Table VIL.
Summary of PFOS in Adult (Test Termination 6 Weeks)
Liver
Samples
at
1.8
ppm
a.i.
-- E0LS0p2o5n9s2o0r780 C0eI1n0't2Sr59e7 B NGuNsOmu0embIbteeArrD EDDxt3aart0atcee1tione ADSDmaaottyrees FFouoAn0uud3s0(i0uygeg)
EE0OLLOO22sS9S:22007788010 00110022999987 00006001IAADD 331660011 ssootn 0o14m9
EEOLO2oSO2s 0%81 o10e2s9s9s8 E0L2s52072 ol02999
000000IIAADD 3J6e0o1l 00601AD 3601
30a1m sor
00314314 0311
EEO0LL2O2s5552:027078%35 00110033000000 0000600IAAD 3J1e6o0l1 asont o04s2s2
E EoLoo 2se2sons 0o1o0s3o0a1l 00066001IAADD 33660011 smoorr 0o008s4a3s
0E10L0O225555:220077%0 00110033000077 c00o60lIAdD a36n0i1 ssoorn 00221100
EE0Lo0L2s25s2s0709910 100130030088 Gc0o6s0llAADD 360011 soorn 0o19m1
EE0OLL022sS952200779922 00110033000099 G00o0aA s6o0r1 sm0n0 o00o12t4
EE00LLo022ss55:2200779933 0110033001100 0G0O6I01AADD 33106011 ootn 0o0o39t4
EEoolla022sso522007790%4 _ootloossoonnnt 003006600I1AADD 33660011 ssootn 0o0o62n9
To -- -- To STANDAR"DADEVVIEATRIOAN:GE:00.a12m4
* Duplicate nection
LOQ=0.01 ug/gforliverand 0.01 pg/fomrsLer.um
CentreAnalytical LaboratoriIensc,.
Page260f 102
n2156
_--
Centre Study No.: 023-041
`Table VIL Summary of PFOS in Adult Liver Samples at 6.2 ppm a.i. (Test Termination 6 Weeks)
`Sponsor n
E01-0255.20785 E01-0259-20785* ED1-0259-20736 E01-0259-20786* ED1-0259.20787 EE0011--00225599--2200778878% E01-0259-20788" E01-0259.20789 E0E101--00225559..2200778995~ E01-0259-20795* E01-0259-20796 E01-0259-20796* E01-0259.20797 E01-0259-20797* E01-0259-20798. E01-0255.20798+ EE0011-.00225595..2200779999+
Centre D
0103002 0103002 0103003 0103003 0103004 0103004 0103005 0103008 0103006 0103006 oi03012 o103012 0103013 0103013 oio3014 0103014 0103015 0103015 0103016 0103016
set Number 030601AD. 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD
* Duplicate injection LOQ = 0.01 ug/g for liver and 0.01 pg/mL for serum
Extraction Aaalysis
Date. Date
3601 301
3601
01
601 wor
601 mol
3601 mo!
601
01
601 wo
601
01
3501 mol
Jem
01
601 3601
nol 01
601 mor
601 aro
3601 mol
3601 301
601 mo
3/601 mor
601
01
601
01
STANDARD DEAVVIEARTAIGOEN::
Analyte Found (uglg)
115 120 L18 119 143 142 1.60 151 1.06 117 0216 0208 0.115 0.0934 0.0801 00197 0.187 0218 [= 00954 0.715 0.606
Centre Analytical Laboratories, Inc.
Page 27 of 102 noa57
-_--
Centre Study No. 023-041
Table IX.
Summaryof PFOS (Test Termination
in 19
Adult Liver Weeks)
Samples
at
17.6
ppm
a.i.
Sponsor n a8 ane 82 ane a ase a ane
ass asst
486 asst 487 a7 488 ase 489 sgn 90 4500
Ceatre D
0007877 0007877 0007878 0007878 0007879 0007879 0007380 0007580 0007881 0007881 0007882 0007882 0007883 0007883 0007884 0007884 0007885 0007885 0007886 0007386
* Duplicate injection
set Number 121800AD I280AD 120800AD 12100AD I2I80AD 121800AD 121800AD I2I80AD I21800AD I21800AD I2I0AD I2I800AD 121800AD 12100AD I2I80AD 121800AD 12100AD I2I80AD 12180AD 121800AD
Extraction Analysis
Date
Date
121800 122000
121800 122000
121800 122000
121800 122000
121800 121800
122000 122000
121800 122000
121800 121800
122000 122000
121800 122000
121800 121800
122000 122000
121800 122000
121800 122000
121800 122000
121800 122000
121800 122000
121800 121800
122000 122000
121800 127000
STANDARD DEAVVIEARTAIGOEN::
Analyte. Found(ugjg)
1.08 105 4.10 "17 837 830 141 143 154 151 041s 0392 117 Lis sit 0509 242 248 0351 0360 2.13 239
LO=0Q.01 g/gforliverand0.01 pgf/orsmerLum
Centre Analytical Laboratories, Inc.
Page 280f 102 "2108
Centre Study No. 023-041
Table X.
Summary of PFOS in (Test Termination 12
Juvenile Weeks)
Liver
Samples
at
0
ppm
a.i.
Sponsor m
os505305e os9056060
908 o9s5o1s2e ssn o9s5i1s5e sossisze 995522000 sosnn 9525 o9s5a2s6e - 9526" * Duplicat injection
Centre "00000077550077 00000077550088 00000077950099 00077991100 0000007791111 00007991122 00000077991133 0000077991144 0000077991155 000079911s6
set Number 2121188000088 2218000088 21211880088 22188000088 2R1I80S0B8 22118800088 21210880088 122118800088 2R1I0S0B8 DIB 121808
Extraction Date
Aualys Date
Amalie Foun,
21211880000 112202000000 NNoQ
2A810m0 11222000000
No NQ
121880000 112222000000
No No
2211880000 112220000000
No No
211880000 12222000000 0o0000077sss
2201880000 112202000000
No NQ
2211880000 1o2o20o00 0000007ss
2211880000 112222000000 0000000675s6
2E18000 201220000
No No
1A28n10s000 112202000000
N N
STANDARD DEAVVIAETRIOAN:GE:00..000000321561
'bNuQt w=aNsoltesQsuatnhtainftihseblleow(eAsptecaokncweanstrdaettieocntoefdatthtehceacliobrrraetsipononsdtainndgaarndasly(t0e.0r0e0t1engti/omntLi)me sFtoarndvaarldu,es0.r0e0c0o1rdged/masLN)Qw,a0s.u0s0e0d05togc/algc(uhlaaltfetthhee avvaelruaeogeftahned sltoawnedsatrcdaldievbiraattiioonn, LOQ = 0.01 pg for liver and 0.01 pg/mL for serum
Centre Analytical Laboratories, Inc.
Page 29of 102
C23gg
_--m$--s--_e--e----eYYY
Centre Study No.: 023-041
Table XI. Summary of PFOS in Juvenile Liver Samples at 1.8 ppm a.i. (Test Termination 12 Weeks)
Sponsor m 9528
9s 9529 95290 9530 95300 9531 95310 9533 9533 9535 9s3se 9540 9sd0* 9541 9sal 9543 9543+ 9544 sage
Centre D
0007917 0007917 0007918 0007918 0007919 0007915 0007920 0007920 0007921 0007921 007522 0007922 0007923 0007923 0007924 0007924 0007925 0007925 0007926 0007926
* Duplicate injection
set Number 1215008 1215008 1218008 1218008 1218008 1218008 1218008 1215008 1213008 1218008 1213008 1215008 1215008 1218008 1218008 1213008 1218008 1213008 1218008 1215008
Extraction Analysis
Date
Date
121800 122000
121800 122000
121800 122000
121800 122000
121800 122000
121800 122000
121800 122000
121800 122000
121800 121800
122000 122000
21800 122000
121800 122000
121800 122000
12180 122000
121800 122000
1201800 122000
121800 122000
121800 122000
21800 122000
121800 127000
STANDARD DEAVVIEARTAIGOEN::
Analyte Found (ug/g
00130 00128 0.00295 0.00295 000904 0.00876 0.00417 0.00435 ons oon? ons 00114 000635 0.00623 0.00305 000297 00126 00126 000514 000521 0.00792 0.00393
LO=0Q .01 ug/gforliavnde0.r01 pgf/orsmerLum
Centre Analytical LaboratoriIensc,.
Page300f102 n2270
-_--
Centre StudyNo. 023-041
Table XIL. Sa.u.m(mTeasrtyTeorfmPiFnOatSioinnJ1u2veWneielkesL)iver Samples at 6.2 ppm
Sponsor IY sir o9s5a4g9e osisn 9551 a9s5s5i2s 95520
o9s55s5 9559 osson os965611 9562 ose2r 9563 os630 ss9e5a6r4 -- * Dupliat nfcton
Centre 0007927 0000077992287 00000077992289 000077993209 00000077993310 0000077993312 007932 00000077993333 0000077993344 0007935 0000007799335 00936
set Number RIA I21G0AA ZRIINAA ZI0A IIAA Z22IIN000AADD 112211%900A0D0 212II0900AADD Z12I19N0A4 121900AD 2Z1I90N0A0 210A
EDxtaratcetion
Amiyss Date
11900 121900
122100 2210
0 1900
112222110000
1i2s90o0 112222110000
112919000 112221000
21211990000 112222330000
112211990000 11222330000
112211990000 112222330000
1122i199M000 112222110000
121900 122300
12211990000 11223000
121900 120100
STANDARD DEAVVIEARTAIGOEN::
FouAnnadl(yutepp) 000000300s3 0oo0t1o0s0 oo ooizs 0o0o06 0000440180 0000334410 00s ous oooart2s1 00193 c0o01o9s7 o0o0o1082r 0.0186
LOQ= 0.01 gg for liver and 0.01 pg/mL. for serum
Centre AnalyticalLaboratories,Inc.
Page31 of102
-_-- --
Centre Study No. 023-041
Table
XIII
SummaryofPFOS in a. (Test Termination
Juvenile Liver 12 Weeks)
Samples
at
17.6
ppm
`Sponsor ry 9567 oss7e 9570 95700 ss975575% 9579 99557809" ss5t5o1r ose osm 9s5i8z3e osuar 9534 ossuta oss
Centre 'y 0000707995377 00000077993388 00000077993395 o0000a7r54400 0007941 00000077994412 0000077994432 00000077594434 0000077594454 00000077994465. 0007546
set Number IA 210A Z12II0A0ADD Z12IIN00AA I12IV00DAD IZI00AD 11221190000AADD ZIZII0A0ADD Z12I10900AADD ZI00AD I12NI0AAD Z12I19A00DAD _
Extraction Date
Aull Date
11221190000 112222110000
112211990000 112222330000
1212910000 11221000
112211990000 11222330000
121900 121900
122300 122300
1122711990000 112222330000
1219m0 122300
1129190000 112202330000
121900 121900
122300 122300
112211990000 11222330000
1219m0 127300
STANDARD DEAVVIEARTAIGOEN::
Amsiyte Found (pig
000000990142 0000062294 000000882239 0o0o8s9s8o 00461 0oo00s4s1 0000475417 003 0156 012 00.010s1 0000337500 00..00451973
* Duplicate injection
LOQ= 0.01 ug/gforliverand0.01 g/fomrseL rum
Centre Analytical Laboratories, In.
Page 220f 102
ran
Centre Study No: 023-041
`Table XIV. Summary of PFOS in Adult Serum Samples at 0 ppm a.i. (Test Termination 19 Weeks)
`Sponsor n as1 sie 4s2 sae 453
asi ast asin ass asso 4s ase 451 asm ass ass 459 sor
Ceatre iy 0007887 0007887 0007888 0078s 0007885 0007885 0007890 00078%0 0007891 0007891 0007852 0007892 0007893 0007893 0007894 0007894 0007895 0007895
* Duplicate injection
set Number 1219008D 121908D 1215008 1219008 121008D 121900BD 1219008 1219008 1219008 1219008 12090080 121008D 12190BD 12908D 2IS0BD 12190BD 12908D 12090080
Extraction Amaiysls
Date Date
120900 1272324100
121900 122324000
121900 12212200
121900 12212200
121900 121900
122324100 12232400
121900 12212200
2190 1221-2200
121900 121900
12212200 1272122000
121900 12232400
121900 122324100
121900 122324100
121900 1223-24100
121900 1223:2400
121900 1223-2400
121900 122324100
121900 127232400
AVERAGE:
STANDARD DEVIATION:
Analyte Found (ug/ml)
Its is 00102 0.00909 9.04 104 0.00274 000212 00125 00123 632 646 658 635 0.105 0102 875 850 478 "ot
LOQ = 0.01 ug/g for liver and 0.01 pg/mL for serum
Centre Analytical Laboratories, Inc.
Page 33 0f 102 2373
-_--
Cente Stdy No: 023.041
Table XV. S(TuemstmaTerrymionfaPtFiOoSn 6inWeAedkulst) Serum Samples at 1.8 ppm a.i.
SIp"oor cenntre NmSbter Expaatce t AmDauiyess
TE0laE 2so2s ms2e oomloaeses E0L252075 oles
mwoeoid Isseo Tarnaaem Good sol aman
BE0Lo02slo20TSs oolloa29nn Bolossamse owen
wooaoAdD ssooll namaann wosiAD vsol nan
BBooll@assssaa0sssse oozssm EoLmsass oer
GcooswIAADD ssooll aanaanl GosAD Iso aman
EEooLLss9arvsee oolleas Blase olor
GGoowioAdD wood
usoslm 3a7naa)l Isola
EEo0Ls0sa7m6ee oostso EoLsooes olaasg
cwoossiAADD ussool nnaanl GowiAD sol aan
BEoollssss2a0in6esse oolsoaess:i momar olosw:
cLord sol aman oooAD sol aman
T EEo0LsLosa0on2esse ooalsaeys woT oosoAADD_TTTyussooLl sainnanamn e
STANDARDDEVIATION:
* Duplicate njction
FounAndsiyte 91029 s10614 s1s6p0 2331 n1570 sIorl a15s7 o1n84s o10rs om 107
LOQ= 0.01 gg orliverand 0.01 pg/mLforserum
Cente Analytical Laboratories, Inc.
Page 3401102
cnoava
-_--
Cente Study Nos 023.041
Table XVI. Summaryof PFOS in Adult Serum Samples at 6.2 ppm a.i. (Test Termination 6Weeks)
T Spoor Cs oDne mNoeC mbbe a E sDeue RETDruaeo e ro-- maatgen
Bilsaasns oowosd Bsa oows
sceoowwd sold
dvaeeanmn
anraemn sneer
S2ol sar
BBiloomme oowmsy Blase oom
mmoowoiAdd owen
vasso se
naaaen aman
s0i4s "2
mmioasswaevse Basar
aommsm own
Emme osu
sooann wowAd
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naneeew aren
mowiab ven nae
awse i567
EBimamsee oosssm mise ooms
mooowobd emn aarnean coos sn nee
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BBass es oosms BLT ow
mGooooiAAbb wood
vnelm dso
naraeen nae
psra sae
BBioosapmi oosws Enso osm
ooowoiAob sveen rneaeel mosoiab yen ram
253110 in
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Dulce jcion
LO=0Q.01 uggfor liverand0.01 pgomrse.rum
Conte Analytical Laboratoriesnc,
Page350102 n0175
CentreStudy No.: 023-041
Table XVII. Summaryof PFOS in Adult Serum Samples at 17.6 ppm ai. (Test Termination 19 Weeks)
`Spamsor ID as ane 52 ase as aur ass
asse 487 as7e ass ass 489 anv 490 4900
Centre. D
0007896 0007396 0007897 0007897 0007898 0007898 0007899 0007899 0007500 0007900 0007901 0007901 0007902 0007902 0007903 0007903
* Duplicate injection
Nusmebter 1219008D (2190BD 1219008D 12190BD 121900BD 121908D 121908D 129008D 121908D 1219008D 121900BD 12090BD 030501AD 030501AD 1219008D 1219008D
ExDtaratcetion ADnaaltyseis
121900 1223.2410
121900 1223-24100
121900 12232410
121900 1223240
121900 1223-24100
121900 122324100
121900 12232410
121900 121900
1223-24100 122324100
121900 122324100
121900 121900
122324100 1223-24100
3501 3-801
3/501 37801
121900 1223-24100
121900 1223-200
STANDARD DAEVVEIARTAIGOEN::
FounAndal(yutge/m 260 26 al 24 11s 106 5 mn 133 127 158 168 22 28 687 680 122 920
LOQ=0.01 ug/g for liver and 0.01 pg/mL for serum
Centre Analytical Laboratories, Inc.
Page36.0f 102 "2176
Centre Study No.: 023-041
Table XVIII. Summaryof PFOS in Juvenile Serum Samplesat 0 ppm a. (Test Termination 12 Weeks)
`SpoIssor ss5o50a3+
9506 9506 908 o9s5o1s2e o9s5i12sn oosiisse sstr 9520 995522050 ost ss952n6 =
Centre 00000077994477 00000077994488 00000077994459 00000077995500 0000077995511 00000077995522 00000077995533 0007954 0000077995554 -- 0007955=
* Dupliat injection
Nusmebter 12200000A0 020000AA 122020000A4 220000AA 200000AA 102020000A4 220000AA 200A 220000AA 200A
EDxtaratcetion AnDaaltyesis
112220000000 112222220000
11220000000 11222220000
112222000000 112222020000
112200000000 112222220000
112220000000 1p22n2220000
112202000000 112222220000
11222200000 112222220000
120000 122000
122200 122000
112200000000 11o2n2o0m000
STANDARD DEAVVIEARTAIGOEN::
FouAndmite (ugmi) 000000438865. 00000078m4 000000336159 00000043517 0o0o007s829s o00o03o78 000000336975 000000453582 0o0o00338s4s 00.0000144727
LOQ=0.01piglgforliverand 0.01 pg/mLforserum
Centre Analytical LaboratoriIensc,.
Page370f 102
n2a77
CentreSudyNo: 023-041
Table XIX. aS. um(mTeasrtyToefrmPiFnOatSioinnJ1u2veWneielkesS)erum Samples at 1.8 ppm
SIpo"nsor Ice)are MeSmaber Eumpcatiion ADmuiet FounAdnsyie igen)
E s5s5a2g9e caaaorrssssrs 2020000Dr A 2n0o0t0e 112224mm ootoema n
s9s5z3s0n ssx0r
o0o0007795s7s coorssy
220000AA avooowco 11222220m0 oo0oarss moon ot zw oom
s953e1 5533
p00r07e98y5 aworsen
020000AA nnoovvee 112222220000 o00osm 000A 2000 122200 ooss
o95s3e5 sszse
000000765610 worss1
020000AA 2o2o00t0 112222220000 000A 000 122200
o[0rsemnst ro
ssssis 9541
par0oerse2 0007563
220000AA noovvoo 112222mm 000A noc 12200
aooos ous21
ssssate ssn
000007996634 0007s
222000AA 2a0o0c0 112222220000 oo00ommes 200A 20k 122200 00s
sssssn a00000r79966s5 012020000A8 11n200v000 112a20m0 o0o0u1s6ss
TT STANDARDDEVIAaTIOeN: e001e98
Duplicate jection
LO=0Q.01 gg forliverand0.01 pg/fomrsLer.um
Centre Analytical LaboratoriIense,.
.
Page 380102
C2378
CentreStudy No.: 023-041
Table XX. Summaryof PFOS in Juvenile Serum Samplesat6.2 ppm a. (Test Termination 12 Weeks)
`Sponsor. ID 9548 sage o9s5i4s5n s9s55i1 9552 9ss2e 9535 9ssse 9gs5s5o9r 9561 sere 9562 ose 9563 ose 9564 9564"
Centre D
0007966 007966 00000077996677 o0000a7799668s. 0007969 0007969 0007970 0007970 00000077997711 007972 007972 0007973 007973 0007974. 0007974 0007975 o00r97s
* Duplicate injection
set Number 12000 20000 1122000000 1222000000 122008 1220008 2000 12000 122000000 120000 2000 12000 12000 2000 2000 12000 122000
Extraction Date
Amaiysis Date
12000 122000
124m 122400
122000 22000
122000 122400
122000 122000
122400 120400
122000 122000
12222300 12222300
122000 122000
122400 122000
122000 122000
122400 122400
120000 120000
122000 122000
120000 122000
122000 120000
122400 122000
120000 122000
112202000000 112272400000
STANDARD DEAVVIEARTAIGOEN::
Analyte Found (sym)
0137 0160 0382 0390 02 0208 o0se2 000284335 0218 ol61 0o6us8 om oan 0x9 0022559 ooiir 00.2080338
LO=0Q.01 ggforlivaenrd 0.01 pgf/orsmerLum
Centre Analytical Laboratories, Inc.
Page 39 of 102 C2179
_--_--mmmm$----------
CentreStudyNo.: 023-041
Table XXI. Summary of PFOS in Juvenile Serum Samples at 17.6 ppm a.i. (Test Termination 12 Weeks)
Sponsor D
9567 9s67* 9570 9s70% 9575 575 9579 95790 9580 9580" 9581 ssi 9582 ose 9583 oss 9584 sr 9588 osgs*
Ceatre D
0007976 0007976 0007977 0007977 0007978 0007978 0007979 0007979 0007980 0007980 0007981 0007981 0007982 0007982 0007983 0007983 0007984 0007984 0007985 0007985
* Duplicate injection
set Number 1220000 1220000 1220000 1220000 1220000 1220000 1220000 1220000 1220000 1220000 1220000 1220000 1220000 1220000 1220000 1220000 1220000 1220000 1220000 1220000
Extraction Date
Aualyss Date
122000 122400
122000 122400
122000 122400
122000 122400
122000 122000
122400 122400
122000 122400
122000 122400
122000 122400
122000 122000
122400 12240
122000 122400
122000 122000
122000 122400
122000 122400
122000 122400
122000 122400
122000 122400
120000 122400
122000 120400
STANDARD DEAVVIEARTAIGOEN::
FounAdua(lnygt/emL) 0329 0355 0483 os12 0241 0252 0.406 0424 0287 0254 0295 0285 0459 0473 o0s21 0524 0553 0564 0s 0505 0.413 0.114
LO=0Q.01pg/gforliverand0.01 pgf/orsmerLum
Centre Analytical Laboratories, Inc.
Page 40.0f 102 C2480
CentreStudy No.: 023-041
`Table XXII. Summary ofPercent Moistures for Quail Liver Samples
Spo>mor EE
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Centre Analytical Larson, nc.
Page stor 02 crest
CentreStudy No.:023.041
(Centre Analytical Laboratories, In.
Page 4207102
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Em no
EEE |:
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Page 4700102
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Figure 6.
Centre Study No.: 023-041
Chromatogram Representing Control Quail Liver for
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CentreAnalyticalLaboratories, Inc.
Page480f102
Cen Sudy No:023.01
Figure 7.
Chromatogram Representing Control Quail Serum Fortified with 500 ng/mLof PFOS
(Centre ID: 0011424Spk A, Set: 122000)
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PageS00f102 "2190
--_----
Centr Study No: 23.041
Figure9.
Chromatogram Representing Juvenile Quail SerumSample (Centre ID: 0007965, Sponsor ID: 9544, Set: 1220004)
EE = ; EEEE.E EHn[ao
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Contr AntaLaboratori, ic.
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C2192
--_--_--
Centre Study No.: 023-041
APPENDIX A
Study Protocol
00P-023-041 (Centre Study No. 023-041)
and Amendments and Deviations
Centro AnavticlLaboratories, Ine,
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STUDYPROTOCOL
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PROTOCOLIDENTIFICATION NUMBER
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TAOFBCONLTENETS he
TABLE OFCONTENTS
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A PURPOSE Dy
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2 TESTMoAoTERIAIS 3 SPONSOR
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4 TESTINGFACILITYANDPERFORMINGLABORATORY........._.._.4
5 PROPOSEDEXPERIMENTALTOMEFRAME.
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7: SAMPLE PROCESSING, STORAGE ANDIDENTIFICATION......__:..
2 ANALMEYTHOTDe ICAe L r.
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5
10.
EXPERDENIALDESIGNcri10
PROTOCOLAMENDMENTSAND DEVIATIONS.10
RECORDS eerie ee 1)
12. QUALITYASSURANCE creme12
13. DATAANDREPORT
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14. ARCHIVESTATEMENT meee
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TS REFERENCES.
16. PROTOCOLAPPROVAL eee 1.
APPENDDE:ANALYTICALMETHODS.
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FRU TELEPHONE: Tees 651-778-7065
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