Document XRz9vZeOOMb60j8LdXY6onRkR
STUDY TITLE `Extraction of Po`tAansasliyusimsPUesrifnlugoHroPoLcCt:aFnleseucltfoosnpatreeyf/rMoamsRseSdpeBcltoroodmeCterllys and Serum for
DRAETQAUIREMENTS
Analytical Method Requirements
STUDY DIRECTOR Sean Gallagher
ANALYTICAL REPORT DATE
June 2, 2003
PERFORMING LABORATORY/TESTING FACILITY
30E5x8ygReesneRaerscehaDrrcihve SuPthoeneC:ol8l1g4e-,2P72A-110638901
STUDYSPONSOR
3M EnvironmentaBluiTledcihnngo2lo3g5y-a0n9d Safety Services
St.Paul PO MBoNx 5353133331:3331
.
PROJECT
ExygEexnygPernotSotcuodlyNNuumbmebre:r:0012P3--002636-066
Total Pages: 98
Grosaz
pms os
G
LABORATORY PRACTICE COMPLIANCE STATEMENT
e nepEToTm ii tysciLdtemrEuEaSFeELE Safety Services, was performed in compliance with US EPA TSCA Good Laboratory
Ee FA dinl ble
_ofofy
d = \ a
4
.
A
005233
ExygenStudy No 023.066
QUALITY ASSURANCE STATEMENT
Exygen's Quality Assurance Unit reviewed Exygen Study Number 023-066, entitled, "Extraction of Potassium Perfluorooctanesulfonate from Red Blood Cells for Analysis cUosnidnugcHtPaLccCorBdliencgtrtoospErxayyg/eMna'sssSStpaencdtarrodmeOtrpye"r.atiAnlglPrreovcieeduwreeds,phtahseesStwuedrye Pirnostpoeccotle,dafnodr aSltludapypDliirceacbtloerGaonoddtoLmaabnoargaetmoeryntP.ractice Standards. ~All findings were reported to the
Phase 1 Prococol Review 2. FEoxraicitciaotnon
3 RawDaaReview 4 RawDaaReview 5 DReavfiReewport 6 FRnevsileRwepor
Date DateERuepgoernted to SDuadtye RDierpeocrtoerda0nd Inspected Management SponsorManagement
522001 601
ensor
201 eal
son
646801 71301
ono
87.901 82101
oor
1VISIGIONN 120500
one
OUULZUOS 060203
oss
QLuyadliiaty AsSsphuttrerance Auditor
Datoecfozfes
Exygen Research
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Exygen Study No: 023.066
CERTIFICATION OF AUTHENTICITY
"hTehisrraepdoratt, ffoorrEthxeysgeand,Study Number 023-06,
Swmitedby:
3E0xy%geRnesRceasrecahcDhrive St1at9e2C7o2l:le1g0e3,5PA 16801
Principal nvestigator, Bxygen:
re and complet representation of
ScieIntiRst feck Exygen Research
Exygen Facility Management:
Load --
RSicehartd A. EGrins, RAAD.
Exysen Research
Study Director, Wilde Intemational: fl
AtAN.
SWeialndGaellIangehmeratona, Lid.
SponsorRepreseaive,Enix:
Bueez joy
sues Bre
alo
Date
JEnoidm efthea
-
Exygen Research
Dae 6/12/03 Page dots
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Exygen Study No: 023.066
STUDY IDENTIFICATION
Extraction of Potassium Perfluorooctanesulfonate from Red Blood Cells and Serum for `Analysis Using HPLC-Electrospray/Mass Spectrometry
EXYGEN PROTOCOL NUMBER: 01P-023-066
EXYGEN STUDY NUMBER: 023.066
TYPE OF STUDY:
Analytical
SAMPLE MATRIX:
Mallard and Quail Red Blood Cells and Serum
`TEST SUBSTANCE:
Perfluorooctanesulfonate (PFOS)
SPONSOR:
3M Environmental Technology and Safety Services Building 2-38-09 PO Box 33331 St. Paul, MN55133-3331
STUDY DIRECTOR:
Sean Gallagher `Wildlife Intemational, Ltd. 8598 Commerce Drive. Easton, MD 21601
SPONSOR REPRESENTATIVE:
John Newsted `Entrix, Inc. 4295 Okemos Road, Suite 101 Okemos, MI 48864.
`TESTING FACILITY/PRINCIPAL: EmilyR. Decker
INVESTIGATOR
Exygen Research
3058 Research Drive
State College, PA 16801
ANALYTICAL PHASE TIMETABLE:
Study Initiation Date: Experimental Start Date: Experimental Termination Date: Analytical Report Date:
04/23/01 05/18/01 07/28/01 06/02/03
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Exygen Study No. 023-066
PROJECT PERSONNEL
`The Study Director for this project was Scan Gallagher at Wildlife International, Lid `The following personnel from Centre Analytical Laboratories, Inc., were associated with various phases of the study:
Name Emily Decker Dave Bell Karen Risha Ling Ling Liu Marcia Swartzwelder Xiaoming Zhu, Mitra Agjmand Lawrence Ord Ed Cames `Shawn Robb
Title Scientist Scientist Scientist Technician Technician Technician Technician `Sample Custodian Sample Custodian Sample Custodian
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Exygen Study No. 023.066
TAOFBCONLTENETS
Page
GQOUOALDL ITYAA SSURB ANCEO PSRTACATR TIECMEEA NCTOcMPcT L.IANO CESTR ATEMY ENT +... 32
S`TUCDEYIRDTENITIFOFFIICACAUTTAHITEONNIT.I.OC.INTY... III
PRTAOBJLEECTOFPCEORNSTOENNNTESL...
A6
LILISSTT OOFFFTIAGBURLEESS........_.____L_LLLLsooo
8
LIST OFAPPENDICES
coos
11
4300 TIENSTTRSOYDSUTCETMI.O.N.......
BR
IIISyg
65.00 DREFEERESNCECMOAFRTAENRIAILAYLPT.I.CT.ALMIETOHODN ce 318
66..2PrEeXpUarQaCtHioOnPoIOfGSEtAaUnIdEa.rdso andFortifs ication Sos Rtons
oo 114
L 63CHIOMo OBTAPhY. c-- o -- 6.5Descriptionof Instrument and Operating
e CIIS
Conditions. .
13
7.066EQ XPERu IMENTi aAndLEDXEl ASTIplGeNo Calc culn atione eves r
1186
9100.0CR ONCLUESIONTS.O..FEDANTAATNDI SAOMPNLES...
19
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ExygenStudyNo.023-066
Table.
Table Il. TableLl. TableIV. Table V. `Table VL. `Table VIL `Table VIL TableIX. Table X.
LIST OF TABLES
SumofPmFOSainRreagy ent BIAnKS voor
Page 21
SummoafPrFOyS in MallardRedBI00dCell BIANKS..............cccnn. 22.
SummoafPrFOyS in Mallard Serum BIanKS ...c..cvrrren 22.
SummoafPrFOyS in Quail RedBloodCell Blanks ................
23
SummoafPrFOyS in Quail Serum Blanks. S--
--
SummaryofPFOS Recoveries in Mallard Red Blood Cells --
SummaryofPFOS Recoveries in Mallard Serum...
25
SummaryofPFOS Recoveries in Quail Red Blood Celis...
--
Summary ofPFOSRecovineQuraiil Seerusm ...........
smn 2
Summary of PFOS in Mallard Red Blood Cell Samples at 0 ppm a.. for
Table XI. SWEuEKm'SmoafPrFn OyS ins MalReldeBalnoomrdCaedlslsSmasmeantp1--0l--ppe--mas.i. for 29
TableXIL
Summary of PFOS LE --
in
MalRledaBrloodd Cell censor
Samples at 50 a--
ppm
a.i. for --
`Table
XIII.
SummoafPrFOyS in Mallard Red Blood Cell Samples Watkin
at
0
ppm a.i. for --
`Table
XIV.
Summary of PFOS WEEK 10.
in
Mallard
Red Blood
Cell
Samples at sem
10 ppm ai. wns
for
`Table XV.
Summary WR AS
.of PcFOoSoin cMalslarmd RmedmBlmoosd Cemll--Sa--mpl--es
at
0
ppm
a..
for --
`Table
XVI.
Summary of PFOS Week15......
insn Mallard
Red
Blood Cell Samples at 10 ppm a.i. for wrnnermmmonm--
`Table XVII Summaryof PFOS in Mallard Red Blood Cell Samples at50 ppm ai. for
Table XVII Suom fPFOm Sina Mallar rdSey rum Samplesat 0 ppm a.i.forWeek 5 ...34 Table XIX. Summary of PFinO MallSardSerum Samples at 10 ppm a.i. for Week 5..35 `Table XX. SummaryofPOS in Mallard SerumSamplesat50 ppm a. for Week 5....35 `Table XXI. Summary ofPFOS in MallardSerumSamplesat 0 ppm a.i. for Week 10....36
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Exygen Study No: 023.066
`Table XXIL SummofaPrFOyS in Mallard Serum Samples at 10 ppm .i for Week
`Table XXIIL WSEuRmKma1r5y of PFc OS in Male lard Serus m Sampless at 0 ppme a.i. for s38 `Table XXIV. Summery of PFA OS in Mallard Serum Samples at 10ppm a.i. for `Table XXV. Summary of PFOS in MallardSerumSamples at 50 ppm a.i. for
`Table XXVI. SFOuEmWmaErRySKof Pc FOS ino Quail Ro ed Blon od Cell Samplesat 0pp a. 40 `Table XXVILWSEuRmKmSa.r.y.ocf.PcFcOeSrrinrmQuranislsRsesdsBmlmoaomdaCnemlleeSaemepnlaerseastn10 ppmsommaesi. for `Table XXVIL Summary of PFOS in Quail Red Blood Cell Samplesat 50 ppm a.. for
TableXXIX. SummaryofPFOSinQuailRedBloodCellSamapt0lppemasi. for
`TableXXX. SWuEmEmKar1yo0f.P.FOsSsinsQsuasilsRsedsBslosodnCselslmSammpmlesssats10mpnprsma.for3
`Table
XXX.
SWuemmkar1y5of cPFoOSmin sQuail
Red
Blood
Cell
Samplaets0ppm ai. for s--t;
`Table
XXXII.
Summary FOF WEEK
of PFOS 15. .
in
Quail
Red
Blood
Cell
Samples
at
10
ppm
ai.
45
`Table XXXII SummofaPrFOyS in Quail Red Blood Cell Samples at 50 ppm a.
A
`Table XXXIV. SummaryofPROSinQuailSerum Samapt0lppemas. for Week5....46
`Table XXXV. SumofmPFOaSirnQuyail Serum Samples at 10 ppm a.i. forWeck 5..47
`Table XXXVI. Summary of PFOS in Quail Serum Samples at 50 ppm ai. for
`Table XXXVIL. SummoafPrFOyS inQuail Serum Samat0ppplmae..fsor
A"
`Table
XXXVI
WSeeukm1m0o.af.Pr.FOyS
in
Quail
Serum
Sampleast 10 NS
pprm
a.
for --
`Table XXXIX. SummaryofPFOS in Quail Serum Samplaet0s ppm a.i. for Week 15...50
`Table XL. SummoafPrFOyS in Quail SerumSamples at 10 ppm as. forWeck15 .....51
`Table XLL. SumofmPFOaSirnQuyail Serum SamatpSOlppem s.i. for TERM .....5.1
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LIST OF FIGURES
Page
Figur1e. TypicalCalibCruravetfoir on PEOS.......vevoessmomsn 53
Figur2e. ChromatogramRepresenting a0.1 ng/mL standard or POS ............ 54
Figur3e. Chromatogram Representing a 1.0 ng/mLstandardfor PFOS ....... 55
Figured. (ECxhyrgomeantIoDgRreamagReenptreBsleanntkiAna,gSRetea0ge5n1t8B0l1an)k for PcOScc
56
Figure 5. Chromatogram Representing Control Quail Red Blood Cels for POS
(Exygen ID: 0107376Blank A,Set:
051801A)............... -- 51
Figure 6. (CEhxryogmeantIoDg:ra0m10R7e3p7r5esBelnatniknAg ,ConStetr:ol07Qu2a3i0l1CS)erum forvPFOSc , r 58 Figure 7. Cwihtrhom1a0tnogg/rmaLmoRfepPrFeOseSnt(iEnxgygCoenntIrDo:l 0Q1ua0i7l37R6edSpBkloAo,dSeCte:lSl1f8o0rtIiDfiRe)d.....59 Figure 8. Cwihtrhom1a0tnogrgam/oRfePmpFreOLsSent(iCnegntCroenItDr:ol0Q1u0a7i3l75SSerpukmA,forSteitf:ie0d72301D)....... 60 Figur9e. C0hro1mato0Sgproan7msoRre0IprDe:s48e5n4t-i4n1g08Q-u,4ai0l1RWeKdSB,lSoto:dICSe1l8l0SIamDpRl)e (c.Exygen ID:61 Figure 10. CSphornosmoartIoDg:r4am5R4epr-es1en0ti8ng-Q4ua0iSle7tS:-er0Wu7m2K3SL0a1mSDpDl,)e (Ec xygene ID: 0s 107207,62
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Appendix A
LIST OF APPENDICES Page
AStmuednydPmreontotcsolan0d1PD-ev0i2g3ti.o0n6s6...(.E.x.y..g.e.n..Study Now. e02r3-0s66e) asndmmmlh
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Exyeen Sudy No. 023.066
1.0 SUMMARY
sEaxmypgleens Rfeosretahrechde(tEexrymgineant)ieoxntroafcpteedflmuaolrloaorcdtaanndesquufaoilnarteed (bPlRooOdS)ceallcesoarmdpilnegsoanpdrosteorcuolm
O1P-023-066 (Appendix A).
"The limit of quanaion fo mallard red blood cell and serum was 10 ng/mL. The iit mofatqiuaxntwiatsatdieontefromrinqeuadilinraemdebtlhooodd vceelrlisficaantdiosnesrtuumdywpaesrf1o0rmnegd/maLt.CenTthree (LCOeQntefoSr teayc:h
023-065).
pPgO/mSL.in PthFeOmSalilnartdheremdalbllaorodd cseelrlusmamspalmepslersanrgaendgefdrofmronomn-nqonu-adneittefcitaebdelleevells ttoo461685 pg/mL. gP/OmSL.in PtRheOSquaiinltehedqbulaoiodsccreulm ssaammpplleess rraannggeedd ffrroommnnoonn-qquuaannttiiffiiaabbllee lleevveells ttoo 536114 bemL. sTahmeplaevserasngde speerrcuemntsarmepcloveesriweesre+9st0a%nd=ar9d%deavniadti9o9n%for 1P3F%O,Sreinspmecatlilvaerldy.reTdhbeloaovdercalgle spearmcpelnetsrewceorvee1ry00%st2an1d0ar%dadnedvi1at0i2o%n or20P%F,OSresipnecqtuiive]lyr.ed blood cel samples and serum
2.0 OBJECTIVE
"sTpheecoibmjeencstiovfeomafltlhairsdsatnuddyquwaaisl teo ddebtleoromdinceelllesvaemlpsloefspaenrdflsuerrouomctsaanmepsluefsonuastineg(tPheFOSi)n
analytical method described in protocol 01P-023-066.
3.0 INTRODUCTION
""aTnEhdxitsqrruseacpiiooretndodefbtlaPioolotsdatschseelilurmsesaPumelptrlsfelosufoartnohdoecstaeannraelusymusilssfaomfnopalteest,hoerusdOietnthgeerrtmhiFenuaaotnrailooyncthioecfamlsPcmFaeOltShCooidnmpemnoatulilnlaedrdsd, From Serum for Analysis Using HPLC-ElectrosprayMass Spectrometry. epTxrhpoeetorcsiotmluednnytualmwbatesermiiOn1nitPti-ia0to2en3d-d0oa6nt6e.AwparsTilhJeu2le3y,x3p6e2,r0i02m10e,0n1twahlesntatthedatsetuwdaysdiMraecyto1r8,si2g0n0e1d, Eaxnydgtehne
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Exygen Study No. 023.066
4.0 TESTSYSTEM
`"mTahtecicxonftorrotlifmiacaltliaornds awnedrequraeicleirveeddbclhoioldlecdelolsn abnldueseicreumonusMeadyfo1r7t,he20m0a1tcfixrobmlaWniklsdlainfde Intemational Lid.Easton, MD. They were assignedthefollowingExygenID numbers:
QuMaaitlrSiexrum MaQlulaairldBSleoroudm Millard Blood
E0x1y0g73e7n5D 00110077337776 0107378
rSeecveeinvteyd-scehvielnleqduaoinl brleudeblicoeodatceEllxysgaemnpleosn aMnadyse1v7e,nt2y-0s0i1x aqunadillosgegreudm isnambpyleEsxywgeerne speervseonntnye-ltwaondmaplllaacreddsienrfurmozseanmsptloersagwee.reServeecnetiyv-etdhrceheilmlaeldlaorndbrleude bilcoeoadt cEexllygsaemnpolensMaanyd 17,2001 and logged inbyExygen personnel and placed in frozen storage. aSsasmopcliaeteldogw-iitnhatnhdiscshtauidny.ofStcoursatgoedyreicnofrodrsmwaitlilonbecaknepbteatfoEuxnydgeinn atnhedatrarwuedactoappyaocfkatghee storage records can be found inthe raw data package associated with this study.
5.0 REFERENCE MATERIAL
ETnhveiraonnamleytnitcaall TsetcahnndoalrdogPyFaOndSSewraviscesr.eceived at Exygen on June 3, 2000 from 3M mTahteeriaavlaiwlaabslestoirnefdorfmroazteino.n for the reference material is listed below. The reference
CoPmFpOoSund Exyg0e0nC0o2n3tr0o2lNo,TCTRCOR0ONIoT,46 Pur9i7t9y(%)Epira0t83i1o/n0D1ate
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Exygen Study No: 023-066
`The molecular structure of PFOS is given below.
PFOS
Chemical Name Molecular weight
= =
Perfluorooctanesulfonate 499 (CuFy7S0)
crI o {
dNeortiev:ed,Thies pnoetuatsrasliummolpeecruflleuoarnoodcsttaanensdualrfdofnoatrem [fCryoFmiwrShOiscKh]P,FmOolSec(uanliaornw)eiisght 538.
6.0 DESCRIPTION OFANALYTICAL METHOD
FAnlauloyrtoicchaelmimceatlhoCdomepntoiutlnedds"EFxrtroamctSieornuomf fPoortaAsnsailuymsisPerUfsliunogroHoPctLaCnEelseuclftornoastperoary/OMtahsesr Spectrometry" was used for this study.
61 Extraction Procedure
AAft1e0r0fUorLtifailciaqtuiootn oofftahpeprreodprbilaotoedcsealmlpslaesn,dthseersuammpwlaess uwseerdefovrorttheexeexdtrfaocrti~on15prosceecdounrdes.. tAhne saalmipqlueost.oO0f.n5e mmiilllliilliitteerrooff00..255MMtseotdriaubmutcyalrabmomnoantieu/msohdyidurmobgiecnarsbuolnfaattee wwaass aaddddeedd ttoo pthleacseadmpolnesw.risFti-avcetimoinllislhiatekresr offorM~TB20E mwienr.eaandddetdhentoctehnetrsiafmupgleeds.for E~ac1h5 smaimnp.leFwoausr rmeilcloinlsittietrsutoefd wthiethor1gamniilclilliatyeerrowfemreethtaankoeln.anEdacdrhiesdamopnlea wniatsroagneanlyezveadporbaytoLrOaMnSd/tMheSn electrospray.
62 PreparationofStandards and Fortification Solutions
OSItPa-n0d2a3rd.0s6o6l.utioAnsnwienrdeivpirdueaplaresdtoocnk Msatarncdhard14,so2l0u0t1ionasofspePciFfOiSed winasExpyrgeepnarperdotaotcola ws`acalostnccpeonrntetrpeaantrti)eodninobfyme1tt0ah0kaingnogl/.m1 LFmrLboymodfitsthsihsoelsvsoitlnougctki1oan0,nmdagb1r.o0ifnptgghie/nmgsLtt.ahnefdoarvrtoidlf(iuccmaoetrirouencptsettdoanf1doa0rr0pdumrsioLtlyuwtaiintodhn methanol.
fAort0i.f1icpatgi/omnl.stfaonrdtairfdicaatnidon
bsrtianngdianrgdthweasvoplruempeareudp
by to
t1a0k0inmgL10wimthLmoefthatnheol.1.0
pg/mL A 0.01
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.
:
CNO5A5
Exygen Study No. 023.066
m10g0/mmLLswtiatnhdamredtwhaasnoplrepared by taking 10mL of the 0.1 g/mL standard and bringing to
0A.0s1etgo/fmstLansdoalrudtsiocnosntinaitnhiengfoPllFoOwSingwamsanpnreerp:ared by serial ilution ofthe0.1 g/m. and
nial Conc. (ig/ml) 01
Volume (mL) 5
Dilutetod (mL) 100
Final Cone. (imi) 0005
[051
2 1
100 100
0.002 0001
000011
5 2
100 100
0.0005 00002
of PROS001
1
100
0.0001
"The stock stored in
standard solution and a refrigerator (4
all fortification 2C) when not
and in
calibration standard solutions were use. Documentation of standard
preparation can be found in therawdata associated with this report.
63 Chromatography
QtuiamneotiffiPcFatOiSon
of was
PFOS ~ 4.4
was min.
aPcecaokmsplwiesrheeddebtyectLeCd/iMnSt/heMcSonetlreocltrmoastprriacye.s
cTohrreesrpeotnednitinogn.
atlotetrheseavnearlaylteforrettiefnitciaotniontimree,cobvuetritehse
aanmdoutnhetsredsettewcetreed
were less
tohnalnytshiegnliofwiecsantt
enough to calibration
standard (0.0001 pg/mL).
6.4 Instrument Sensitivity Tcohnecenstmraaltlieosntof0s.ta0n0d0a1rdg/ammoLunotf PFiOnjSe,cted during the chromatographic. run had a
6.5 Description of Instrument and Operating Conditions Instrument: PE SCIEX API 3000 Biomolecular Mass Analyzer
Interface: SCIEX Turbolon Spray Liquid Introduction Interface
Computer: Dell UltraScan P1110
Software: HPLC:
Exygen Research
P`WEiSncdioewxsAnNaTl,ysvtervseirosnio4n 1.1
Hewlett Packard HP Quat
P(uHPm)p
Series
1100
HP Vacuum Degasser
Page 15.098
"9516
Exygen Study No. 023.066
HHPP CAoutlousmanmpOlveern
CHoPlLuCmnCoTleummnp::Ge3n5esCis Cs (Jones Chromatography), 2.1 mm x 50 mm, dy. IMnojbeicltieonPhVaols.e (A1)0:pL2 mM Ammonium Acetate in ASTM type water MFolboiwlReaPteh:ase (B0).:3 mMeLtmhiann.ol
Timo e wBA %aB
0000
10 100
n75o 660 440
Tons monitored:
APnaFlOySte
nMeogduieve |Transit4io9n9M5o9n9itored
Approximate Rete4nT2i0tmei(moinn)
TPunaerFialemeters
Controls
se
1S-lospray
4200.0
DPF-PD-eFcolcuusstienrignPgotPeontteinatlial
2-501.00
CXP-CoECPlE-l-ECinostlorlnainsCcieoelnlPoEEtxneientrtigPaoyltential
1000 5
`CEM.ChamDnFe-lDeEfllecetcrtoonr Muliplier
238000000
NGebausliFzleorwGsas
s1e2t
TICSoCluTlreitmsaipionenrGaGatasusre
34 sc
6.6 Quantitation and Example Calculation
pTeeankmiacrreoaliwtaesrsmoefassaumrpeldeoandcatlhiebrsattaionndasrtdancduarrvdewwearse ignejneecrtaetdedint(oustihnegL1IxMSf/itMwSe,ighTthede
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C0317
ExygenStudy No. 023-066 cloinnecaerntrreagtrieosnsiwoans) dbeyterAmnianleydstfrsoomfttwhaereequuastiinognssbiexlocwo.ncentrations of standards. The tEhqeuasttiaonnda|rdcalccuurlvaeted(ltihneeaarmroeugnrtesosfioannaplayrtaemfetoeurnsd)(ignennegr/amtLe,d bbaysetdheonApnealayksatresao)ftuwsairneg epqruoagtriaomn.s foTrhseenruEmquaaretisohnow2n)calculated the amount of analyte found in pg/mL (the
EquatioIn: Analyt found (ng/mL) =(Peakasrloepae-intercept)
EqAunaatlyitoe2n:found (ug/ml) =(anal.found(ng/mL) XFV(mL)xDExEV(mL)x 1sg
Where:
(AV (mL) x sample vol. (mL)
1000ng
DFVF == DFiinlaultiVoonlFuacmteor
AEVV == EAxltirqaucottioVnoVloulmueme
cFaolrcuslaatmepdletshefpoerrtcifeinetdrewciotvherky.nown amounts of PFOS prior to extraction, Equation 3
ReEcqouvaetriyo3(n:%) = ana). found (g/m-aLvg). aanamlo.uinntcatdrded(ug/(mL)n)gjmLx)(1000ng/1 ug) x 100
An eMxalalmaprldeosfearcuamlcuslaamtpiloenCuesnitnrgeanIDact0u0a0l3s8a0m3plSepkfolAlow(sS:et: ng/mL with PFOS, where:
112100B),
forified
at
10
inpteearkcearpeta
== esisss
dsilloutpieon factor ==m0
anvggadadmetdin(ocrotnlieovlels) == 0I(nNgot quantifiable)
efixntaalcvtoiolnumveolume == SammL
salaimqpuloet wveoilguhmte(volume) == 0a.1mmL
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Exygen Study No: 023.066
From eqAnuaaltyitoenf1o:und (ng/mL) = [657578-0515
From equation 2
= osngmL
Analytefound (ig/ml) = (08ng/mLx | mLx1xSmLyxLug
@mLx01ml) 10000g
From equation 3: = 0.00976 pg/mL % Recovery = (0.00976ug/ml1.0xng=/m0L.g/mL)x1000) x 100
= om
7.0 EXPERIMENTAL DESIGN
bElaacnhk,scttwoof smaamtrpilxesb(larndksblfooortdicfieeldlaotrksnerouwmn) ccoonncseinsttreadtioofnos,narnedag~ent20blsaanmkp,loesn.e maEtarcihx sample was extracted usin the appropriate method and then analyzed in duplicate.
8.0 RESULTS
"PTFheOSamionutnhte omfalPlaFrOdSefdoubnldooidnctehlelsraenagdesnterbulmanbklsanakrse aliestgeidviennTianbTlaeblI.esTIhe&amIIoLu.ntThoef `PaTemhaoekusnatmwoeourfnetPdsFetOedScetteiendcttiehndethqweueacriolentrroeondllybmlaostoirdginciceefslilccsaonratrnedesnpsooeunrgduihmnga(tr0oe atglhiteveerannasilenyvteTeraablreltefesonrttIiioVfnic&taitmiVeo.,n craelciobvreartiieosnasntdanadsaradr(e0s.u0lt00a1reprge/pmoLrt)eda.ndTnhoet qrusatntoiffitahbelseamples were less than the lowest
dInedtiivliedduailn rTeacbolveesrieVsI f&orVPIFLOSThien atvheeramgaellpaerrdcernetdrbelcoovoedriceesll+asntdansdearrdumdesviaamtpiloenss afroer
rPeFspOeSctiivnelmya.llaIrnddirveidduballoordecceolvlearnsd fsoerrPumROsSampilnestheweqrueai9l0r%ed b9lo%odancdell99a%nd+se1r3u6m,
dseavmipalteisonsarefodrePtFilOeSd
in in
Tables mallard
rVeIdIIbl&oodIXc.ell
The and
saveerruamgesapmeprlceesntwererceov1e0ri0e%s
+
1st0a%ndaanrdd
102% 20%, respectively.
pPgF/OmSL.inItnhdeivmiadlulaalrdrerseudltbslaoeodlicsetleld sianmpTlaebslersanXg-eXdVIfLr,omPnRonOdSetiencttheedmlaelvlealrsdto4se1r8um
Exygen Research
Page 180198
.
"0349
Exygen Study No:023.066 TsaambplleessXrVaIngIeLdXfXrVo.m non-detected levels 0 685 g/mL. Individual esuls are listed in IPnFdOivSidiuntalhereqsulatislareedlibslteododicneTllabslaemsplXeXsVrIaXngXeXdIfIrLom. nPoFn-OeSticntethde lqeuvaeillss1e0r3u6m1sga/mmplLe.s ranged from non-deteted levels 0 514 pg/mL. Individual resuls are lsted in Tables
XXXIV-XLL
9.0 CONCLUSION: a"TnhaelymzaeldlaarcdcoarnddinqguatiolprreodtobclooloOd1Pce-l0l23a.n0d66s,erum samples were successfully extracted and
10.0 RETENTION OF DATA AND SAMPLES s`hWihpepnedthetofitnhale rseppoonrstoris. comTphliested,oealsl onroitginianlclpuadpeerfadcaitlatyg-esnpeerciaftiecd rbaywExdyagteanswuiclhl base cionpsitersumoenftalllogrsa,whdoawteav,ears ewxealclt acsopaiessigonfedtecmoppeyraotfurtehelofgisnalwilalnalbyetiscaulbmrietpeodrt. anEdxaacltl oaofrricghtiiinvmaeeldsfbapyceictlihtfeyi-essdppoeincnsiof4ri0.c rCaFwRdaPtaar,twi7l9l2.be RreettaaiinneeddisnatmhpeleEsxyogfenreafrecrheinvceessfuobrsttahnecpeesriaorde
Exyaen Research
.
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Exygen Study No.: 023.066
Tablel. SummaryofPFOS in Reagent Blanks
`Sponsor Centre
Set
=IMe Dm ResgIfeDiDB_ln_k_A _NuNOmuSmbISbeOeIrrA
nm RegenBlankA OSISOIA
nm RegenBlnkA2 OSISOIB
ma nm
ReagemBlankA2 RegemBlnkA
0SISOIB 00014
mo ReagenBlnkA 0S40IA
Mm mo
ReageotBhnkA 021018 ResgemBlankA 021018
mM mo
ReageBlakA RegenBlnkA
OS20IA 0S20IA
Mm nm
RegemBlukA 052008 RegenBlakA 052018
mo RegemBlrkA 0S20IC
mo mo
RegemBlukA ReagenBlnkA3
0S20IC OTIS0IA
mo mM
ReagentBlnkA3 ResgentBlukA
O710IA O200IA
mo ResgewBlamkA O700IA
nm ne
RegemBlikA2 020018 RegmBlnkA2 020018
mo mo
RegemBlmkA 0723014 RegeaBlkA 0723014
mm mo
RegenBlnkA2 0723018 ResgenBlankA2 O230IB
mo m_
ResgenBlnkA3 OR30IC ReagenBlak AS OR30IC
Estraction DaDattee S801 S801 5/1801 S/I801 52100 52101 52101 52101 52200 52201 52200 $2201 52201 52201 7/1901 71901 72000 72000 72001 70001 72301 72300 2300 72301 72300 772301
Analysis DDaattee S/18-19/01 sns-1om1 S901 S901 S201 p20! spa! 52201 siso1 S301 s2s01 S301 S301 19S-3200100 119-2001 2100 101 212200 721-2200 1501 125001 401 72401 42501 12425001
AVERAGE: STANDARD DEVIATION:
Analyte FFoouunndd G(uug/mmil))
No No No No No No No No No No No No Ng NNDo ND ND ND No ND Ng No No No No No NQ ~~ NQ
* Duplicate injection
bNuQt w=aNsoltesQsutahnatnitfhiaeblleow(eAstpecaokncweantsrdaettioencotefdthaetchaelicborrarteisopnosntdainndgaradnsal(y0t.e0r0e0t1enptgio/nmtLi)me ND = Not Detected (A peak was not detected at the corresponding analyte retention time) sFtoarndvaarldu,es0.r0e0c0o1rdpegd/amsLN)Qw,a0s.u0s0e0d05topcga/lcmuLla(thealtfhtehaevevraalgueeoafndthsetalnodwaersdt dceavliiabtriaotni,on LOQ = 0.01 pg/mL for red blood cells and serum
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Exygen Study No.: 023.066
Table I. Sponsor
n convol comvol comvol comvol comrol conrol conol __conwol _
Summary of PFOS in Mallard Red Blood Cell Blanks
Centre Dn
OlO7378BlnkA OO7TVEBUnkA OlO7VSBlmkA OlO7VEBlankA* OlOT8BlankA2 010778 Blank AZ OIO778BlankB 007378 Blank B
Set Extraction Analysis
Number ___ Date Date
0520018 OS210B
S2U0I S2uUOI
52200 52200
020A 0S201A
S201 S201
S200 S300
052018 S201 S301
0S201B 52201 S301
0S20IC 052201C
SP201 522001
S301 snyo1
AVERAGE:
STANDARD DEVIATION:
Analyte Found (sgjmL)
No No No No 000224 000184 No NQ 0.000548 0.000927
Table III. Summary of PFOS in Mallard Serum Blanks
`Sponsor ID conwol convol conwol convol convol convol
Centre. ID OIO7377 Blank A OIO73TT Blak A3 OlO7377BlankA OIO7377BlmkA _0_0O7I30777STBIlBnlnkkAA22
* Duplicate nection
Set Number OTIOIA OTI%IA OT001A O72001A 0720018 0720018
Edracion Amlysis
Date Date
9001 7192001
AOL 92001
72001 72101
72001 72001
72001 72001
212201 212201
AVERAGE:
STANDARD DEVIATION:
Analyte Found (ug/ml)
0.00325 000331 000277 000312 000188 000214 0.00275 0.000605
bNuQt w=asNoltesQsutahnatniftihaeblleow(eAstpecaokncwenatsradteitoenctoefd tahtethceacliobrrraetsiopnonsdtainndgaradnsal(y0t.e0r0e0t1enptgio/nmtLi)me LOQ= 0.01 pg/mL for red blood cells and serum
sFtoarndvaarldu,es0.r0e0c0o1rdpegd/amsLN)Qw,a0s.u0s0e0d05topcga/lcmuLl(ahtaelftthehaevevarlaugee aofndthsetalnodwaersdt dceavliiabtriaotni.on
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Exygen Study No. 023.066
Table IV. Sponsor
In conol cool connl cowol cool cowol conol _comol
Summary of PFOS in Quail Red Blood Cell Blanks
Centre ry
Set Number
Extraction Date
Awalyss Analyte Date __Found (ug/ml)
0lO0lTO6TBIl6aBIsnkkAA* |
OSISOIA OSISOIA
SS8A0SO1L | S58U.S1I9O001I
NQ No
OOIIOO7T66BBllnnkkAA2Z* 0O5S1I8SO0I8B
SASOI SA8OI
S901 S901
NQ NQ
OlT6BhakA OTV6BnkA
0R10IA ORU0IA
S2OI S2IOI
spol spol
NQ No
__O0IlT07V3G7B6lBnskkAA __0oSs2200iCc sSpzo2o0n1 ssnpoulm Nxgo
STANDARDDEVAIVAERTAIGOEN::
NQ Ng
Table V. Summary of PFOSin Quail Serum Blanks
Sponsor Centre
ny
ccoonooll OLOOITOVTSSBIlSaBnnkkAA
conrol comol
OOI00TTVVSBSaBrkkAA22
comol comol
_OOWT07V3SSBBhlknkAASY
* Duplicate nection
Set Number
Extraction Date
Amalyls Analyte Date Found (gm)
OO7T2O0IIAADD 7722330011 m72o60l1 | o00o03m09
0O27300I8B
2301 2301
7400 7400
No No
OOTTBIOICC
72301 72301
228822550011
NQ NQ
STANDARD DEAVVIEARTAIGOEN::
0.00100 0.00148
bIuNtQw=aNsoltesQsutahnainiftihaeblleow(eAstpecaokncwenatsrdaettieocntoefdtahtetchaelciborrarteisopnosntdainndgaradnsal(y0t.e0r0e0t1engti/omn Lti)me LO=0Q.01 pg/mLforred bloodcells andserum
Fstoarndvaarldu,es0.r0e0c0o1rdge/d masLN)Qw,as0.u0s0e0d05topcga/lcmuLla(thealtfhethaevevraalguee aofndthsetalnodwaersdtdceavliiabtriaotni.on
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Table VI. Sponsor m onl cool comol cowol cool cool conol conrol comrol ccoommool cool comol cool
Summary of PFOS Recoveries in Mallard Red Blood Cells
Centre IY
Set Number
Extraction Date
Analysis Date
Amt Added ogiml)
= Recovery
Ol0TTSSpA OW0TISSpkA*
020018 O2001B
S2101 S2U0I
52201 S201
0 10
ss a
OTVESKB OITNSSpkB
020018 O2001B
S201 S2UDI
52200 $2201
50000 50000
ot 95
OITNSSpA OIOTMSSpk AT
O201A 02014
S201 52201
52301 2301
10 10
8 2
OTMSSKB OIOTMSSpBY
020A OS20IA
52201 $2201
52301 52301
50000 50000
5 2
OI07V8SpA2 OO7TESpkA2
052018 022008
S201 S201
2300 SRL
10 10
5 76
OIOTSSpkB2 OITNSSpkB2+
O0S201B 02018
S201 52201
sol $2301
50000 50000
101 105
OTVSSKB 0107378 Spk Be
0S201C 052201C
52201 5201
S301 spon
50000 50000
102 101
AVERAGE: 90
RELATIVESSTTAANNDDAARRDD DDEEVVIIAATTIIOONN::
9 11
* Duplicate injection LOQ:= 0.01 pg/mL for red blood cells and serum
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`Table VIL. Summaryof PFOS Recoveries in Mallard Serum
`Sponsor iD control convol comvol comrol comrol comrol conwol convol contol convol comrol comrol
Centre nD
007377 SpkA3 0107377 SpkA3* OIOT3VTSkB3 OlO77TSpKB3*
OOTITSpkA OIOT37TSpkAT OI0TITISpkB 007377 Spk Be OIOT3I7SpkA2 0IO7377SpkA2 O07377SpkB2 _0I07377SpkB2
Set Number O71901A O7190IA 701A O7I90IA 02001A OROOIA 072001A 072001A OT200IB 072001B 0720018 0720018
Extraction Analysis Amt
Date Date Added (ng/ml)
719001 7192001 10
71901 7192001 10
T1901 7192001 500000
F901 192000 72001 721/01
500000 10
2001 72101 72001 72100
10 500000
72001 72100 500000
72001 77212201 10
72001 772122001 10
72001 7212201 500000
720001 721.2200 500000
AVERAGE:
RELATIVESSTTAANNDDAARRDD DDEEVVIIAATTIIOONN::
* Duplicate injection
% Recovery
% 8 un m2 7% 2 uw 9 107 110 2 2 99 13 13.
LOQ=0.01 pg/mLforredbloodcellsandserum
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Engen Sudy No: 02.066
`Table VIIL Summary of PFOS Recoveries in Quail Red Blood Cells
Sofmyer Cone
CoDme ubSee OTs SA OIo0IR
Buurceion Jer
ADmues TR
astA1om0 n)
eo" s ox
Gnoolll OOOOWOITeGoSsSAKuADEC OHDSWHOIOODDIDRRR SSSa0mwIi samamaiizaoo0li lo in5nt
oGGoownll OoOweSeSsKkSEA oOOSSSHHHOOODDDRRR 0 wweell Swaaeiiilll 010 ii1ino
GoCoulll OOOOe0TsSSSSEKkAAeC oGoSnHOiOoADnR 0 uSonil assnmmeei 1100 ov5s
ooouuolll OoOOOemTseGSSkKxEDA ooomswienc sssoaolmlnt aasoeolll ssww10ee
0
cool
owvesa_smoc
smo
SsTAmNeDARD DEEVIRiAoATIGONE:
0on0 10
RELATIVESTANDARDDEVIATION, 10
upc in LOQ= 0.01 pg/mL forredblo clls adserum
Bugg Reseach
Page250198 (9357
Exygen Study Nos 023.066
Table IX. Summary of PFOS Recoveries in Quail Serum
Simnor CoIDre NmSbaer DuDrueon ADmaties AddedAgmmt) Bers
cCoonioll ool
OGIOTTSSISpSAAT MOTOILOIAARR Z12o30r1 OWSSIB ON0WR 230
772a5s0o1r sel
100 swe
@w jos
oonoll nol
OOOWTITSSSSKKDAT2 OWSAZ
OOROOWDR Tu2wl0L ODODE
Rmeeall Remel
Stoaweried lo wm
coommo ool
OWoTSISsSkHXBBeZ 0O0DmO OOTISSIAS OmOD
mmyeel 2301
nnwoell 620
ssweloeo
iae 106
ooooll cool
OOWTISSSABAS oOmOoiDc 0WIISspEY ODOC
a23u0l1 mu
7R2622900 1measnl
swIoe Sooo
l0eso toy
RELATIVESSTTAANNDDAARRDDDDEEAVVVIIEAARTTAIIGOOENN,:.
12002 20
[--
LOQ=001 pg/mL for red blood cells and serum
ExygenResearch
Pugs270108
(9558
Exygen Study No: 023.066
Table X. Summary of PFOS in Mallard Red Blood Cell Samples at0 ppm ai. for Week 5
`Sponsor i
Centre m
Set Number
Exraction Date
ADvaatieyss
FouAnndaluyptiemi)
44SSELII0D2OAWWESST 001007223300 00220100185 sSa2w0o0r 5p2a20m0 ASGI9SIWES 010731 02008 S201 spa
NQ 00N01Q97
4SSELIIG0RLDWWESS
010731 01022
0B 02108
sol sao
seal span
BLORIWESS 0022 0208 20 2200
000167 NNgo
ASSLEIDGIIRWIEST 00110022333 002210088 sSa2uo0l spp2oo0n
NQ No
AASSLHIIOIDSSEEWWEKSS 00017034 O02RU0OB sS2au0rL sspeaann
~Q No
AASSLLIIBOISSWWIISST 000073355 00210008 sSa2u0l1 ssppaann 00N01o43
AA5SLLIIOOIDCCWWESS_ 0010032366 002210088 ssaouuorl
sao ___snain
NQ NQ.
STANDARD DEAVVIEARTAIGOEN:: 00.000000470016
* Duplicate injection
NbuQt w=aNsoltesQsutahnatniftihaeblleow(eAstpecaokncweantsrdaettioenctoefdtahtetchaelciborrarteisopnosntdainndgaradnsal(y0t.e0r0e0t1engti/omn Lti)me LOQ:= 0.01pg/mLforredbloodcealndslersum sFtoarndvaarldu,es0.r0e0c0o1rdpegd/amsLN)Qw,as0.u0s0e0d05topcga/lcmuLla(thealtfhethaevevraalgueeoafndthsetalnodwaersdt dceavliiabtriaotni.on
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Page 28 of95
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Table XI.
Summaryof PFOS in 10 ppm a.i. for Week
Mallard
Red
Blood
Cell
Samples
at
-- 4S41S0po9In2s8o0r.WKS C0e1n0n7t2r3e7 N0uNSum2Sm0beb0teeBrrD . BDxDaSa2actuti0eeLon AD5nDaa2alt3tysee0is FFoouunnAdnd2a(4lr4ygtieml)
4ASSELIIOORR0HWEWSS 0011007223378
00221I00IBBDD
S201 sauor
ssoouul
7 n2
A4LSHIII0TIDDLOWWESS 0011007223389 0022100BBDD Ss2a0uo1l Ss3oy0o0n ASEIGIDLWKS 00239 020BD S201 S230
100 1s 23
SAESICOIWTWEKSS
007240 010740
0S0BD 0SI0IBD
201 s2u01
seul soa
151 131
SASLEIIONNTWESS 001002724411 00SU10BDD Ss2zu1o0l sspaaon
01 08
S4SE4II9DD4EWENS 00100722422 00RSA00IBBDD 2s1zu0o1l 5s2p3a0m0
as 395
4SSELII09VVSSWWEESS 0010077224403 0ORSU0OIBBDD
S2uol S2i01
s52p3a0m0
189 188
4A5S41L0I9392T966.WWEisS 0011007024444 00SS2U0001BBDD __sszpuuo0ln ssosunl
264 285
I
AVERAGE: 173
STANDARD DEVIATION: 880
* Duplicate injection LOQ =0.01 pg/mLforred blood cells and serum
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Table XII. S50umpmpamray..offoPrFWOeSekin5Mallard Red Blood Cell Samples at
B Spoor CoInDtT re NeSwter ExpmceT on ADmaa tesa our Asmie
SSLEIIOOSITBOIWSS 0000742665 0os2m0oi1cDD S2222001 SIOITOWS 010246 020i smn
332440m1 suo
am2n 13
ee STANDARD DEVIATION: 33
`Table XIIL Summary of PFOS in Mallard Red Blood Cell Samples at 0
ppm a.i. for Week 10
SpoInsor CeInrstre SSHEODDOWOA OOTED SSIHOODOWOKWOI Ol0m0SR1S SSIHOODDSSLIWWNAKOD oOlmmsz SSHOORDWWOK 0O0T25S3 SSHHOOURDWSKWO O0o0mmsss SBUHODOSEWNO O0lT0mSSS SSHHOOTDSSWWKAO 0O0o2m%s S SIOO DCWE IO 010002T5S7T L--
NuSmbter Erpuitoe n AmDaabesi
0Gs0zoMlA Ssammi Fsaavsoer
o0s0ma s22a0o1 ssomuall
0o0maa ssaawm ssvmeonl
0os2m0oAa sS2a0m1 ssvotl
osmmaa ssaaom ssaavne
oosomA ssoaom ssmmvaoll
oomoam s22a0mi 0smaA spol
ssmoyyl mvol
__osmoiTa T soo spa
STANDARD DEVIATION:
FouAnsnse NNoo xNoo xxoo xxoo NNoo Nxo Nxoo
o0Nmposs --0.000--600 --
N=QNot Quantifiable (A peak was detected athe coresponding analyte retention ime
but was less than the lowest concentrationofthe calibration standards. (0.0001 pg/mL)
LOQ=0.01 g/m.forred blood cels and serum sFtoarndvaarldu,es00re0c0o1rdpegd/amsLN)Qw,as0.u0s0e0d05togc/almcuLla(thetahfetahveevraalgueeoafntdhestalnodwaersdt dceavliiabtriaotni.on
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Table XIV. Summaryof PFOS in Mallard Red Blood Cell Samples at 10 ppm a.i. for Week 10
`Sponsor iL) SSHIIM-WKIO AS-I9WO-WKIO ASEI0WKIO A5I09200-WKIO AASSEEIIDOIIVVLLWWKKIIOO SSHI022WKI0 ASHI022WKIO SSEIORVIWKIO 4541093293WKI0H ASEI00304WKI0 ASEI9304-WKIO SSEUIVSWKIO 4S4109320SWKIOH ASEI0IV6WKIO 454109306:WKIO
Centre in 007258 0107258 007259 0107259 007260 0107260 0107261 0IOT261 010762 010262 0107263 0I07263 007264 0107264 0107265 0107265
* Duplicate injection
Set Number 02201AD 0S201AD 052201AD 05201AD 02201AD 0S20AD OS20IAD 05201AD 0S201AD 0201AD 0S201AD 0S201AD 0S201AD OS0IAD 0S201AD 052201AD
Extraction Analysis
Date Date
sp201 Sm
Sm32amn smal
S201 sp32emn
Sm201 sp3am
Sm201 S201
sp32am sma
S201 sp3.2401
Sm201 spam
52201 sp324010
Smal spam
S201 sma
sami sm3aaol
Sm201 spat
S221 span
S201 sp3.2401
520001 ___s3.2a01
AVERAGE:
STANDARD DEVIATION:
Analyte Found (ug/ml
193 196 204 202 161 169 613 660 3s 42 08 569 161 160 1s 17 303 207
LOQ=0.01 pg/mL for red blood cells and serum
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Table XV.
Summaryof PFOS in ppm a.i. for Week 15.
Mallard
Red
Blood
Cell
Samples
at
0
`Sponsor ny
Centre n
AASSEEIIDONDOAOWWKKISS 001100206666
ASSSEHIIOORR0SOWWKKIISST
00261 00267
ASLEIUBSSI
006s 010268
AASSLEIIO0RRSWWKKIISST 0010022660
AASELOIDDWI KS 001002200
ASSSELIIOORDSSEEWWKKIISST 007071
AAESRCIOTS
0102 010272
ASSSEEIIOOR6SCNWKKIISS 0011007227733
SAI1V0W6KWIEISS 001100727784
0
* Duplicate njcton
Set Number 00522200088 0s20i ooss2200i88 0022008 0os220088 0208 00s2200i8B 0s2u0o 00s2200i88 ooszs20oi8
Extraction Date
Analysis Date
557222200010 s3aa0n1!
span sa01
sns01 sn3o1
200 spr
ssna3a0m11
2s2p0a0m
sa301 301
5S22200000 ssnn330011
ssppaamn ssan30r1
s22a0n0 sns3a0l1
ssmaamm snnyoon1
ssapnat ssnp3o0l1
STANDARD DEAVVIEARTAIGOEN::
FounAndalaygtien) NO NQ No
[Neoy oo0iss No No No ~Q ND ND NNQo No No No 0000.0002064133
NbNuQDt w==aNsNooltepsQseuatakhnaidniefttiehacebtlleeodw(eAstpecaonkcwenatsradteitoenctoefdtahtetchaelciborrarteisopnosntdainndgaradnsal(y0t.e0r0e0t1engti/omn Ltime )
LOQ:= 0.01 pg/mL for red blood cells and serum
sdFetovarinadvtaairlodnu,,es0.r0e0c0o1rduegd/amsLN)Qa,nd0.f0o0r0N0D5,pzge/rmoLw(ahsalufstehde tvoaclaulecuolfatthetehleowaevsetrcaagleibarnadtisotnandard
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Exygen Sudy No: 023.066
`Table XVI. S10umpmpamray.i.offoPrFWOeSekin1M5allard Red Blood Cell Samples at
Spomnsor SSmIaODMWS SSHIODO0NWASS SSIEIOODDIILLWWAASS SSLHIOODIMDWWKSS SSLUIOODDDWNAWSS SSLIHOSODAWWKISSS SSSIHOOVIBSSWWAASS SSLHOOTWSS
CeInrt)re G00o275s O00m7e6 0000227 OOT0I7S 00007299 OOT0E0 0010072881 0000T2E8
NeSmbter e02ionmsd 00ss2200mBDD oo0oBdD oossmao0BBDD 0ossmTOOBBDDRR 00s2200BBDDRR o0sSm0oBmODRR 05o2s02108B0D
BuDatceo AnDuaeis FounAdnayte
Im220o1 S smiaue nt r2e
3322001 3Sm3a4av0e1l a24s4m
s37m2a0 msmsssagnl wosa
332220010 3smzasaawvoorr ass
Ssm2a0l ssmmuo)
1m1s
0 S200 aovurr
fryr
SS220011 sapmaann
s65o6
s32m0n0 ssppsaasvuell 0o5a0ns
STANDARDDEVIATION: 3+95
`Table
XVIL Summary 50 ppm a..
of PFOS in for TERM
Mallard
Red
Blood
Cell
Samples
at
Sponsor Centre SER own
NuSmbter once
BuDaceo AwDaatyes FouAnndaiyepms mera a
SSSILOISDOOMLTTEERRMMY LIOR
0O00788 oosmoomhDR _0l0m8s_osoimbr
s2m0a1l 32201
ssamawoorl sur
0ms as
Tee STANDARDDEVIAT. ION. 30
Duplicate infection
LOQ= 0.01 g/mLforred blood cells and serum
Exygen Research
Page 330198
70564
Exygen Sy Nos 023.065
`Table XVIIL Summoa fPr FOyS in Mallard Serum Samples at 0 ppm a.i. for Wee5k
Sow CaD_r_e TEs Gone
Nesmaber one
BuDnuieon ADmaiek Toe Tae
roAmwe pe
SSHEOORRSEWWSS 00m0m0 SBS on
oomoan omen
0000 00
omveel vel
asesesn ose
sSeHoOuRImNwGe SHORES
oonosm 0005
ooomna omen
0000 2000
amveel mm
sgeeeen oe
SSUODORRSSWWSS seu
00007005 0nw
ommowliaa own
T7200000 Toon
i moeel
SHORSWS Ones amin 2000 Tae
eeeesn seeee
SSLeOmWS selonsews:
o0o0n9 00
onmwean enon
70000 mon
amieel __oaim
egeeee gee
To Dipl json
aaSTAn NDARDDEL VIATION: e o0otey
LOQ=001 gmfored loo cells ndserum
Exgen Research
Page 34ot + gnOSE5
Exygen Study No. 023.066
Table
XIX.
Summaryof PFOS ai. for Week 5
in
Mallard
Serum
Samples
at
10
ppm
Sponsor n
Centee I"
A4S5E10I9G2T8B.WWEK5S 00100B3I100
AASSEEIIIOIVTOOWWKKSSS
0B OIOBIL
ASSSEEIIGOIZWILLWWEKSS 00008112
GASSIOHRODRWEES
00513 0I0BI3
SSEIORIWES SEIN
OTIS 00D
ASEIDTLWKS SEI09WKST
0031S 0I0BIS
4SSSEEII0O9R3I2SW9Wi5sS- 0010073M16
Set Number 020000I1AADD 007220000I1AADD 002200000AADD 02001AD 0O70000AADD OORD0IOIAADD 0200700IIAADD 072001AD
Extraction Analysis
Date Date
07200011 772223000007
M2000011 77222200010
0700011 77222200000
72001 2001
02001 72201
72000 M00
200 22001
001 70001
722000 72201
772000010173T0200010
STANDARDDEVAIVAETRIAOGNE::
Analyte Found (gmt)
28 120 96 952 108 110 84 55 94 766 06 515 733 769. $6.4 222
`Table XX. Sau.mfmorarWyeoefkP5FOS in Mallard Serum Samples at 50 ppm
Sponsor n
Centre 'y
44SS4EII0O9I3RVOWWKKSST
O01 01087
45S6S1E0I9O3I3T0OWWKKSS 0010073S18
* Duplicate injection
Set Number OR00IAD 07001AD 00722000I1AADD
EBuraction Analysis
Date Date
72001 7001
712200 722001
7T2200010172270220010
STANDARD DEAVVIEARTAIGOEN::
Analyte Found (imi)
376 "0 20 2 347 0
LOQ= 0.01 pgfor/ redblmoodcL ells and serum
Exygen Research
Page 35098
19866
Exygen Study No: 023.066
`Table XXI.fSourmWmeaerky1o0f PFOS in Mallard Serum Samples at 0 ppm a.i.
Sponnsyor Centee
Tee ASEIORAWKOT
oo 01072
SSLIORSOWKIO ASLISIOWKI
0023 007323
ASSSEEIOI9DSIISSLIWKKIIOO
00724 010724
ASSSLHIISOIRWWKKIIOO 0010077255
ABSUEIIIORRIIWKIIKOOT 0011007732266
SEIORWNKO ASEIOEWKO
0037 00727
AASSLHIISOWSAWIKIOOT 0011007732288
ASSSEEIIOODSSECWWKKIIO: 0011007732299
EE
* Duplicate injection
NuSmebter amen O0T2O0O0I1B8 002200008B O02M0O0O1I8B 0022000108 OoNOoOIlB 02008 0O2P0I0SB 00n00001I8B
ExrDaacteton AnDaaltyseis
moo 001
Tarp Im2200
2001 R001
2201 A200
001 001
212200 22200
72000010 1122220000
702000011 72122220000
moon 001
2721122020010
70000011 212220010
M20001 01m22m00
STANDARD DEAVVIEARTAIGOEN::
FounAdn.alyte 0o0o0os 00o000esss o0on0ssss ooaosips oNoDo ND 000000s 0ooooosdsse 00.0000246766
NNbuDQt w==aNNsooltepsQseuatakhnatdneitfteahcebtlleeodw(eAstpecaonkcwenatsradteitoencotfedtaht tchaelciborrarteisopnosntdainndgaradnsal(y0t.e0r0e0t1enptgio/nmtLi)me LOQ= 0.01 pg/mL for red blood cells and serum Fsdetovarinadvtaairlodun,,es0.r0e0c0o1rdge/d masLN)Qa.nd0.f0o0r0N0D5,g/zemrLo.w(ahsalufstehdetvoaclaulecoulfattheetlheowaevsetracagleibarnadtisotnandard
Exygen Research
Page 36of98
GCNOSE7
Exygen Study No.: 023-066 `Table XXII. Summaryof PFOS in Mallard Serum Samples at 10ppm
ad. for Week 10
Sponsor i)
S-I98.WKIO AS-109.3289-WKIO 4SI9390-WKIO 4SH1093290-WKIO AA5S4E1I0093ODLLWWKKIIOO ASHIOIOLWKIO 4S-1093292WKIO ASLI09IWKIO 4541003203-WKIO ASHIO0EWKIO ASE109096WKIOT ASLIOIBSWKIO ASI9395WKIO 4A5S41E0I03O2V066-WWkKII0O_
Centre nD
0107330 0107330 007331 007331 010732 010732 0107333 007333 007334 0107334 007335 0107335 0107336 0107336 00737 0107337
* Duplicate injection
set Number. 07001BD 07200BD 0720008D 07T200BD 0T00IBD 0720008D 0720018D 07T00BD 0T00BD 072001BD 072001BD 0T00IBD 072001BD 0T2001BD 072001BD 072001BD
Extraction Analysis
Date Date
70001 722010
72000 72201
2001 722001
72001 72201
2001 2001
722m1 722001
2001 722001
72001 70201
72001 72m)
72001 72001
22001 722001
72001 72201
72001 722000
72001 72201
2001 J2201
720000720001
AVERAGE:
STANDARD DEVIATION:
LOQ=0.01 pg/mL for redbloodcells and serum
Analyte Found (g/ml)
145 147 27 325 95 102 107 nm 132 136 853 864 123 120 14 2 105 3s
Exygen Research
Page 370798 n9568
Exygen Study No. 023.066
`Table XXIII. Summary of PFOS in Mallard Serum Samples at 0 ppm a. for Week 15
Sponnsor Core NuSmbter ExDaactteon AnDauleyt
SSEOaVOmWKe IS GOoTInS SHBUOWKS 00D
GIA OIA T9e0o1 T71e92001 010A W010
SSHHOODZOOWWKKSS 00000D SLSRSOWKS 007H0
GoIuA 011A
o9o0 7T952000011 Tom T9200)
SSIIOOTDSSILLWWKKSS O000TM1I SLOWS 0032
0O1N0OA ON0IA
TTooooll 751290200011 onl T9001
SSIHOEDRSIWWKKSS 0000332 OGNI0IAA ASIOLSWKS 00 ona
TToooml 179922000001 gol T9200
SSLHBROSEWWKISS 0O0T4 SSHIDSSWKIS oles
OTNI0NIAA om0lA
9o0m 77119920000011 moni msa0m
D ASSSHIIIOOORSBSNEWWASSS 00OE I1000MTMsSS OG1I5MO0IIAAA M9mi9090l
7T1992300001 719001
STANDARDDEVIATION:
* Duplicate injection
poAsnsite oNoDo 00x1o0s oNspo o1om 00N0D0s oNoDr ooNmDs oogveee ND 0.00616
NNbuQDt w==aNNsooltepQseuahaknatdniefttiehscebtlleeodw(eAstpecaokncwenatsradteitoencotfedtahtethcalciborrarteisopnosnadnidngaradnsal(y0t.e0r0e0t1enptiyomnLiyme LO= 0Q01 g/mforLredbloodcellsandserum Fsdetovarinadvtaairlodun,,es0.r0e0c0o1rdpegd/amsLN)Qa,nd0.f0o0r0N0D5,gz/moLw(ahsalufstehd tvoaclauleocuflattheetlheowaevsetrcaagleibarnadtisotnandard
Bxygen Research
Page 380198
n0869
Exygen Study No: 023.066
Table
XXIV.
Summaryof PFOS ai. for Week 15
in
Mallard
Serum
Samples
at
10
ppm
Sponsor I
AASSEEIIDRIB2BWWKKIISS SAHSIH0IIBIO0WWKIKSSH ASSSLEIISOIIBBLLWWKKIISSS AASSIHOIIDRTNNWWKKIISSS ASSEEII0DIRBWIIWWKKIISSS AASSEEIIIOTTWIWKKIISSS ASSSEEIISOINWSSWWKKIISSS 4A5S4E10I9O3T2V966WWKIISS
Ceatre
0011007734477 0010077488 0010077M3)5 007350 0OII00TBISS0I 0O0O3BSSI2 0O0OSD 00007733S5)4 007334
Set Number
Extraction Date
Analysis Date __
OG7TI00IIAADD T9I0O1N 772200221110017
OOTTI00IIAADD
Mom 01
220022110011
OTTOI0AIADD 990m 27022012010011
OM0IAD O710IAD
90 901
7202001 7202000
OOTTI00IIAADD
901 M901
77220022110011
O7O1T9I00IIAADD M9O0L1 77220022010011
0ONT0OIIAADD
om M901
77220022100011
O07T1I900I1AADD 9901172027300201011
STANDARDDEAVVIEARTAIGOEN::
Analyte Found (apni)
i22 162 101 875 152 2 21 1s 128 2 6a753 wr 116. 952 113 735 7.3
Table
XXYV.
Summary of PFOS ai. for TERM
in
Mallard
Serum
Samples
at
50 ppm
Sponsor hy
Centre D
A4S54L1I0O93R299I7TTEERRMM 0011007733555
ASS140190O29ETTEERRMM: 0011007733566
I
* Duplicate injection
Set Number 007720000I1AADD _0_R07W200I0iAADD
Extraction Date
Amalysis Date
7T220000010 7773202010
77220000011 7T722230000
STANDARD DEAVVIEATRIAOGNE:
Analyte Found (ugimt)
685 1 664 sor 638 a
LOQ=0.01 pg/mL.forred blood cells and serum
Exygen Research
Page 390f98
68870
Exygen Study No. 023.066
`Table XXVL. Spupmmmaa.ryfoorfWPeFeOkSin Quail Red Blood Cell Samples at 0
Sponsor D
Centre I.
ASSSLHIIOBBHILLWWESST
010707 0007
ASSHCISBIIOQWWISS 000000788
ASSSHHOILSIIOEWWIEST 0000700709
SSSSLCIIBOILGIAEWWIISST 000077008800
ASSECIISBIISSWWEISS 0000008811
ASSCLIIBBIISWEEWSS 0000008822
ASSSLHIIBOIBSKWEIWSSt 001007700883
NuSmbter ExnDaatceion ADmaityess FouAnndai(yuigiemt)
GSISOIA 0SISOIA
SA80l Sasol
SeionT si901
No No
0GsISO0I1AA ssungwooll ssnss.iioooln NNoo
OOSsIs0iIeA sS1isg0eL ssnsnioonl Nnoe
OOSSIIIOOIIAA SS8A0M1O Ssn8s.91o0ml Nxo
0OSSIISOOIIAA sSaumsDo1 sss.s1osm1 NNoo
OOSIAA SS1a0wl sSnnss11990011
000202 000264
0G51S80I14 ssussowl __s_assntsosnoln Nnoo
STANDARD DEAVVIEARTAIGOEN:: 00..000000949830
* Duplicate nection
bNuQt w=aNsoltesQsutahnainiftihaeblleow(eAstpecaokncwenatsradteitoenctoefdtahtetchaelicborrarteisopnosntdainndgaradnsal(y0t.e0r0e0t1enmtioLn t)ime LOQ = 0.01 ug/Lforred bloodcels and serum sFtoarndvaarldu,es0.r0e0c0o1rdpegd/amsLN)Qw,as0.u0s0e0d05togc/almcuLla(thealtfhthaevevraalgueeofantdhestalnodwaersdt dceavliiabtriaotni.on
Exygen Research
Page 400198
619571
Exygen Study No. 023.066
`Table XXVII. S10umpmpamray.io.ffoPrFWOeSekin`Quail Red Blood Cell Samples at
Sponnsor TSHIeOBAr OLWIeS SSHHIBIALRWWESS SSHLOIWMS SSULIIGHOOLLWWIISS SSLHIIGOOLISSWNEISS' SSELIIB00EEWWIISS SSLSIIBOAL0LMNWIISS SS4HIOBM0OBLWWISS
Centre NuSmbter BaDtaeon AwDaaties
o0l0o7r0a8 sOtSIOsIDRoln18ao0e1n 00085 OSIOIDRD sso
F31a5r0m1 smo
001007008%5 GOSSISIOBIDDRRD 1188001 00086 GSISODR 51801
s3a13a0011 smiaa01
0000008 OOSSIISBOODDRR iSISB0O1 OOS OSHOIDRD 101
ssiigsaanl smn
001000700885 O0SSIISSOOIIDDRRDD s51a8m0o1 asvaenr
O0L0S0 OOSSIHHOOIIDDRRDD SS810011 000% OSIODRD 5180
3$2300011 3nv01
00100009011 O0SSIIO0IIDDRRDD S51S8D0I1 3322000m1
STANDARDaDEmVIAeTIOsN:
FoAnstyeum) 30 130515 2094 2a5s3 1w0r50 100s0 ssosui wae1 324
"Duplicse injection LOQ:=0.01 pgm for redblood cellsandserum
Bxygen Research
Page al or98
Coa57R
Exygen Study No. 023066
`Table XXVIIL Summaryof PFOS in Quail Red Blood Cell Samples at
50 ppm a.i. for Week 5
m TSaors oe Coome wesmmsobaiecro r BuDurem ADmuebe souAsmie
Sseewass seman ws:
oooon oom
oo0zicoh ooo
asmno smo
svasue sper
o&s I
a STANDARDDEVIATION. 054 --
`Table XXIX.. SummaryofPFOS in `Quail Red Blood Cell Samples at 0 ppm a.i. for Week 10
T Sor CoDreumba eSar h bDuuem ADmueb romAsmie
SSLHGILEWWGI00 SHOEWGe
TooiT0ol o0m0l
osisoun ssaeteol osion swe
isgoonrs sion
JIo Na
SSHHOSOEWE0 oooonnmm SEOWI0 00m
oouuonm wsaen oom sel
aoiiee sn
SHOWN oun om se
xroo No
SSOLOBISSWWKOO SHOEWN0
OOn0TnI6 ows
oosistools ssavt0ell oso ae
gsemr isgeor
Nxoa NNoo
S SSHOEOOWWOA
oowsnss ois
oowonm Osiom
osenl vive
asmoem ae
SLOW Ol oD vise
r~o No
T e SLo OVO 00710 e sii sve e ime Ne
[--
STANDARDDEVIATION. NG
bNut=waNsoItsQsutahnatnifhieableow(eAstpecaokncwenatsradteitoenctoedtahe tchalcibormaetsiopnosntdainndgaradnsal(yt0e0r0e)ctpioanmi)me LO=0Q.01 pg/mL forerblood cels and serum sFtoarndvaarldu,es0.e0c0a0r1dged/amsLN)Qw,a0s.u0s0e0d050gca/lmcuLla(teatfhtehaevevraalguee osfntdhie leowesst ecalaibrartion
Exygen Research
Page 20098
-
20573
Exygen Study No. 023.066
`Table XXX.Summaryof PFOS in Quail ppm ai. for Week 10
Red Blood Cell Samples at
10
`Sponsor In 454-108401-WKIO 454108401-WKID 454108402WKIO 4A5S4L1I088440023-WWKKIIOO 445S4HII008844030-4WWKKIIOO 4SSS4I10088440045WWKKIIOO 454I08405-WKI 445S1E10088440066WWKKIIOO AASSHEII00B84400-7WWKKIIOO SH108408WKIO ASC108408-WKIO
Centre.
0107108 007108 007109 0107109 OIOTLIO 0107110 OIO7LLL OLO7III OI07U2 007112 010713 OIOTII3 0107114 00711S 00711S 0107115
* Duplicate infection
Set Nomber GSISOIDRD OSISOIDRD OSISOIDRD OSISOIDRD OSISOIDR OSISOIDR OSISOIDR OSIOIDR OSISOIDR OSISOIDR OOSSIISSOOIIDDRR OSISOIDR OSISOIDR OSISOIDR OSISOIDR
Extraction Analysis
Date Date
18001 S722001
s/101 S01
S/180L S220
18/01 SASL
S201 s212200
ASO 5212200
sAROL S180
5212200 S121
ASO sasOL
s212200 s212200
sAmOL S180L
5s2p1i.22u20000
SASL SASOL
s;12200 sr212200
SASOL 5212200
1301 spiaoo
STANDARD DEAVVIEARTIAOGNE::
Analyte Found (pg/mL)
2 on 203 190 50 207 190 22 180 200 489 505. 28 23 04 302 129 20
LO=0Q.01 pg/mLforredbloodcells and serum
Exygen Research "
Page 43098 no374
Bayan Suty Nos 023.066
`Table XXXI. Summary of PFOS in Quail Red Blood Cell Samples at 0
ppm a.i. for Week 15
Sew>er CoDm_e SHOWS 00
mSbee Dubmscein oT mlon T oun
Abmerb eaae
pomAsme
SSSHHHIOOIOGGGWWWSSS OOONOOSM SHIGE OU
ooommooienn 020
somouw se ssemmee
Nnxooo aes
ou mee
SSSUHHMOKSOSGWWWINSSS Oo00Ii0Ds SOSSWAS O00
ooomlaman nSmiaiml an ou
nasammeee) me
earenos ee
SSSHHHWOBINIOWGNWIGSSS 0Oo0wm2Eiz1n CHEWS OZ
boommlaonnn oSSwualnm oma 0
vaweivaee de
oNNeaos oe
SSSHOBOSISSWWWISS 00o0Ommm sme oon
opmmolannn onion
mSsiuoon se
smavmeee, sme
aINc)oe
Te STANDARDDEVIATION. oats
"Duplin
BNIuNDtQ w==aNNsooltepsQseuahaknaidnfeiteahcebieledow(estpckoncwenitsradteitocntoefdtathtchealcoirrraeosnpoandnindgaarnt(3e0r00tponmtime
LOQ =0.01 pg/mLforred blood cells and serum
dFSeolvrnidavtaailrou,nes0.r0e0c0o1rdgedmas aNQ,n0.f0o0r0N0D5,psge/rmoLw(shalfstheetovahlueuolflthetlhoewmesetrcaalibmradtisonandr
Eugen Research
Page ator 670575
Exygen Study No. 023.066
`Table XXXIL S10upmmpamray.o.ffoPrFWOeSekin1Q5uail Red Blood Cell Samples at
Sponsor
centre
NuSmbter Bupceo AwDuaeys FounAdnayie
SSEIIBSORLWWKKSSST 0000M5 T O0S00AADD SS220011 HSIARWKS 006
armsrge0rn Smaayer
236
SSHHOINWSS 00001227 SHIOLOANS 008
GR21A0ADD Ssa2te0l 002010A1ADD sao
ssmmssaavweer smsaum
2L1e2s 188
ASSHHOISOAMOSLWWAISS 000701298 ASEIOASWAS 09
002200IAADD 020AD
Ssm2iUm0 sSamm0ll
ssmmsaaavvegrl sssave
2130 158
GSEHIILSOOOWNKAISS 0000700 SSHILOIWAS 00731
OGUU00IAADD SS22001 02001AD 210
sammszagvuegrn asmsaa
3n6s1 an
SSIHBIASTMEWWKSS O00O12 SHOALNKS 0012
2Os0mINcDD ssmaoo 02010 S201
osasmagver seen
s1w3 124
a SSHIISGILUWGES 0OIN0NLB 200s1A0ADD sMuo0) smaaggaan
s16575 sit
STANDARDDEVIATION:-- 243
`Table XXXIIL5S0upmpmmaray.io.ffoPrFTOESRiMn Quail Red Blood Cel Samples at
P SpIon"sor Crna e NuSmbter ExtDrr aatcteion AnDaatyess FounAdnayiegmt)
ASSUIIMLPOTTEERRNMS SEISHOTERM
001007M35 0107135
0ossziocD om0icD
s322m00 ilesmyn 37301 spam
T3E56 S 1I0m6
Te o a STANDARD DEVIATION:
e14e4
* Duplicate injection
LOQ= 0.01 g/mL. for red blood cells and serum
Exygen Research ------
Page asofsg 10576
Exygen Study No: 023-066
Table
XXXIV.
Summary of for Week
PFOS
in
Quail
Serum
Samples
at
0
ppm
a.i.
Spomnsor 45108361 WES
Centre 0107154
NuSmebter 07301AR
EurDaactteion 72300
Analysis Date Trasior
FouAnndal(yyteim)
ASEHIOSSIILWQIWSST O00077I1S5E O02700IAARR ALUSIQWST 0071S OZ0IAR
m3u0l1 01
sasil
om 000012459
ASSSLHIIBBIIGGWWIESST 0O0I0771ISSS O0OI0ARR
32300
72800 772950010
SSEIOSIAWS 0071 O0IAR
00134 o0o011s6s6
ABLEISOISAGWWISS 0O00T7I1S9T 0O020ALRR
203100 v0
a7s2is 72300
ASEUBIGWIS 010719 OZ0IAR
c00o0s5a1s0 ous
A[SSLHII0BOIB6IASWIWSS' 00017017600 O03M0A1ARR
mTo30ll 72301
sT2i30r1 72500
0oo0i1s2s0 oois6
* Duplicate injection
STANDARDDEVAIVAETRIAOGNE:: 00.000175466
LOQ = 0.01 pg/mL for red blood cells and serum
Exygen Research
.
-
--------------------------------------
Page 46 or95
Coa577
Exygen Study No: 023.066
`Table XXXV. Summary of PFOS in Quail Serum Samples at 10 ppm ai. for Week 5
Spoor ID
SAESEII00S8440022WWEsST ASLIS4OLWES AASSHLLI00BS400LLWWEASST ASLI0840LWEST A4SSELIIB04S040SSWWKESS 4SSLLI10088440066-WWKEsSe ASSSLLIISG4O0I-WWEESS SS4A5CS1IL0BI80A4B004S80WWiIKsSSe:
Centre Py
007162 O0TI 01071 007063 0O0l701TI664H OOIIOOTTIIGSSS OLOTIGS OOII0OT7IIEGT6 0107167 001O1I0O77T1I16G86S 8
Set Number 0O7Z2X001IAADD O0IAD OOMXO0IIAADD OMNIAD OOZIB00IIAADD 0730IAD 0O2M3F00IIAADD OAD O0M7O2X030I0I1AAADD
Extraction Amalysic
Date Date
72301 R30
72600 T2601
R30 72600
30L 2301
72601 72600
2301 70601
T2301 301
72601 70601
T2301 72601
22330011 7722660011
2R0300 7722660001
0233000172AV60E0R6A10G1E:
STANDARD DEVIATION:
Analyte Found qugimt)
58 56 us 8 10s 983 18 1s 106 a1047 6363 g$se9i8as 350
`Table XXXVI. Summary of PFOS in Quail Serum Samples at 50 ppm a. for Week 5
Sponsor
ASUIBMLWKS S4LSCII004844412WWEKSS ASSS10C8I44I2.WWIiSSe * Duplicate injection
Centee 007092 00110077009923 00110700993)
Set Number O72301AD OOZ00IIAADD U0R001IAADD
Extraction Avalysis Analyte
Date Date Found (gmt)
2301 72600 2300 72600
S51 52
R3OL 7722330000
772226600610 0s;s52209
STANDARDDEVAIVAETRIAOGNE::
541 194
LOQ= 0.01 pg/mLforred blood cells and serum
Exygen Research
Page 47 of 98
nas78
Exygen Study No:023.066
Table XXXVIL
Summary of ai. for Week
PFOS 10
in
Quail
Serum
Samplesat
0
ppm
Sponsor CoIDre SSIHSI06LL3W6KIOW0T O00TUTT SHS0H3IGBWIQKWOKTO 00007S8 SSH4BII0GGWWK0O 0000D ASSHHBIBIIAAWWKKOOT 00001810 SSSIH0ISB3SSWWKKOOT O0T0TSE SS4IIB0683W6K6WOKT0 OOITEE SS4O10L30.IWKT0 O0N0SS SSSSSCSIILOISLBMIOEWWWIKK0OO OI0O0I0OlTISsSSt *Duplcste njcion
NeSwaer EwDcaieon Abmaiies FounAdmiemi) O0HBO aR3v01 7722440011 00000408s3 0omBB TR2v300l0 7722440001 0000009s5 0ooBm 2v3o0l1 2T0040001 0o0o0s4a617 momoom TTy3o 0424001 ooooos oO7m0 T723m01 a724l00 oooozne OomToBm T22330010 47204011 00000082397 ooom T723I01 d24l00 oooo0ssiezs 0oOmr7o0 mpTyRvIeO n7p4u0ol1i ooooooousssayss
STANDARDDEVAIVAETRIAOGNE:: 000000180350
LOQ=001 pg/mL forred blood celsandserum
Exygen Research
Page agofos 69579
ExStyudyNgos0e23.n066
`Table XXXVIIL Summary of PFOS in Quail Serum Samples at 10 ppm ai.for Wee1k0
Sor CoDmeumbSa: BuDmucieon Aumei.s romAsmie
T smsosWoL) waA 0 oonneessT oommooniiiobnppe T 7mmee0lr T O mmaammeeaO sp ee
Slseaiosmswoao oowonl SUOABW0 oe
oomwooinodD omobp
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mmaamwe mame
ag
U SUONO WKO OoOiSs seoswa0 ome
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mmaann maw
2l0os 19
sseeooeswwaa00 ooowne seo oo
ommoobnop omoib>
waell Tel
mmaas mas
llogs lio
SsSeLiIo0sSwLaW00_O0oIiosL _ oorwzooDibd o20w1l mmmraasael oorso
STANDARDDEVAIVAETRIAOGNE. 613144
Dipceineion
LO=0Q.01 pgmfored blood els and serum
Engen Research
Pugs 49.019 6n0s580
Exygen Study No.: 023.066
`Table XXXIX. Summaryof PFOS in Quail Serum Samples at0 ppm a.i. for Week 15
`Sponsor i)
4SEI08361-WKIS 45410836LWKIS 44SSLHII0B8332IWQKWIKISSS 4S4I0BIGIWKIS A4SSHII0B83I6AAWWKKIISSS 454108364WKISS 4S-I0836SWKIS 4SCI0836SWKISS 4SI08366WKIS 4SLIBICWKIS 4SEI083I6IWKIS 4SLIBITWKIST 4S4I0B3GBWKIS 4SI0836BWKISS SSEIBIBWKIS 4541083WKIST
Centre m
0107192 010712 010793 0107193 OI07IS6 007194 OIO7I9S OIO7I9S 0107196 007196 0107197 007197 OI07I98 OIOTI98 0107199 0107199 007200 0107200
* Duplicate injection
set Extraction Analysis
Number. Date Date
O7230IC 72301 n42500
O730IC T2301 04201
O730IC ORC
301 242500 2301 7242500
30IC IIL 242500
ORC OM30IC
2301 242500 2301 2425001
O730IC O230IC
2301 2425001 2301 42501
0720C 0301 7242500
O230IC OI30IC
2301 0242500 2301 2425001
O70 ORC
II 1242500 2301 242501
070 O230IC
301 242500 2301 242500
ORICON 242500
072301C 3017425001
AVERAGE:
STANDARD DEVIATION:
Analyte Found (ug/ml)
NQ No No No 000154 0.00160 No NQ No No Ne No 000227 0.00249 000253 0.00255 00162 000160 0.000928 0.00105
bNuQt w=aNsoltesQsutahnatniftihaeblleow(eAstpecaokncwenatsradteitoenctoefdatthetchaelciborrarteisopnosntdainndgaradnsal(y0t.e0r0e0t1enptgio/nmtLi)me LOQ = 0.01 pg/mL for red blood cells and serum
sFtoarndvaarldu,es0.r0e0c0o1rdpegd/amsLN)Qa,nd0.f0o0r0N0D5,pzge/rmoLwa(hsalufstehdetvoaclaulecuolfattheetlhoewaevsetrcaagleibarnadtisotnandard deviation.
Exygen Research
Page 500f 98 79581
Exygen Study No: 023.066
`Table XL. Summaryof PFOS in Quail Serum Samples at 10 ppm a.i. for Week 15
`Sponsor Centre
D
n
445S1A0088440011-LWWKKIISS
007201 0107201
4455110088440022WWKKISS 00100702022
44SSLLII08B44O0LNWWKKIISS
007203 0107203
4SGIS404WKIS 0107204
44SS4411008844004SWWKKIISS 0011007220065
44S544110048040S6WWKKIISS 0010027200S6
445S140180480460-7WWKKIISS LO0I00T076
44SSE41-0I804840078--WWKKIISST 0000720078
4S5SLL1I804L0I8IWWKKIISS 00110077220098
A4SSLL1I0S8I38I3WWKISST 00110072090
Se Number O07T203I0IDDDD 0O2300DDD OOT3300IDDDD OM3OIDD OO7T203I0DDDD 0O772T33001IDDDD 02O3T001IDDDD 0077223300IIDDDD 0O2T3300IIDDDD 00273203I0D0D
Extraction Auaiysis
Date Date
72301 2301
772277..22880001
7722330011 772277.22880000
72301 2301
772277.22880010
301 72301
727-2800 7272801
72301 727.0800
72301 72301
772277.22880011
72301 72301
772277..22880011
72301 2301
772277.22880000
72301 R30
772277.-22880000
3203011 jA7mV2E7i.Ra2Am8Go0E1l:
STANDARD DEVIATION:
Analyte Found (gm)
181 150 5s2a1s 26 29 1 107 11 156 704 698 107 ue 102 891 BL i91e5403 86:6
`Table XL1. Summaryof PFOS in Quail Serum Samples at 50 ppm a.i. for TERM
Sponsor ID
Centre Se n Number
AS4SC5C1II0OO8AS4I410OI-0TTTEEERRMM::_00001710027722111111 000077223300D11D0D0
* Duplicate injection
Extraction Date
Analysis Date
72301 030011
m771m22r702.o08m800o11l
STANDARD DEAVVIEARTAIGOEN::
FouAnndal(yutgemt) 6 S4s9iu5a. 269
LOQ= 0.01 pg/mLforred blood cells and serum
Exygen Research
Page 51of98
C2582
Exygen Study No: 023.066
Exygen Research
Page 520198
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Exygen Study No: 023.066
Figure 1. Typical Calibration Curve for PFOS 8 SHIB(PROOS)1:"UnAear Rape(1swsehoingn): TEZ267x + 1176.240989188)
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Exygen Research
m`ConB ceniton inw t. w IR Page 53 of 98
[LLERES
Beppe Sy No: 022068
Figure 2.
Chromatogram Representing a 0.1 ng/mL standard for PFOS
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Chromatogram Representing Control Quail Red Blood Cells fortified with 10 ngo/fm PFL OS (Exygen ID: 0107376 Spk A, Set: 051801DR)
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Figure 8.
Chromatogram Representing Control Quail Serum fortified with 10 ng/mL of PFOS
(Exygen ID: 0107375 Spk A, Set:072301D)
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ExygenSudy No: 023.066
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Chromatogram Representing Quail Red Blood Cell Sample
(Exygen ID: 0107084, Sponsor ID: 454-108-401 `WKS, Set:
051801DR)
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Exygen Research
Page 620198 50393
APPENDIX A
Study Protocol 01P-023-066
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Amendments and Deviations
Exygen Research
Pugs 018 anos
Exygen Study Nos 023.066
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