Document DG6Z7VwV4xrgDk28VqByxrLM
A--
AR236- (544
STUDYTITLE
Extactonof Psassum Perflcrocuncslfose fom gg Membrane, Albumen, and `Yolk for Analysis Using HPLC-Electrospray/Mass Spectrometry
DATAREQUIREMENTS
Analytical Method Requirements
STUDYDIRECTOR
-
Sean Gallagher
STUDYCOMPLETEDON
Sepimber 06,2001
=
PERFORMINGLABORATORY/ TESTINGFACILITY
Conte Ans0o48nRLebsoearrscrhireis,veIn. Cone)
State College, PA 16801
Phone: 814-231-8032
STUDY SPONSOR
3M Boiling 236.05 Environmental Technology and Safety Services SLPaoPlOMBoNx 5353133331.3351
PROJECT
CenCtoenPtreotSoceolyNNumobmeer::0002P5-.002633063 Toul Page: 102
GRO
ContrStNuos0d23.y063
GL OODABO PRAR CTICA ECOMT PLIAO NCESTR ATEMY ENT
Cente Study Number 023.063, emtiled `Buiaction of Potssiom Perflucfr romoBgo gMc embt rana e, An lbusmes n,au ndYlolf kfoo r Ann alya sist Usis ng.
following exceptions. HPLC-Electrospray/Mass Spectrometry," conducted for IM Environmental Technology
andSafetyServices, wasperformedincompliance withUS EPA TSCAGoodLaboratory Practica Standards (40 CFRPart 792)byCentreAnalyticalLaboratories, Inc withthe
1. p7i9s2c.e6f3o.rtMhueibnetasdnaennotsearnudtCdalitbrhaeticoxnaocfiEoqnuiepmhen8t. of. No equipment SOPwasin
PrincipRal vestigaior
CentreAnalytical Laboratories, Inc.
r
A Smmaaan BD Wilt Ttematonal, Lid
fel--t
Bue4 ls t |
GeneAnatylesLabora,bo.
|
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--------------------------eeeeeeeeeeeeeeeeeeeren Centre Study No. 023063
A
NCE STATE
C0Me2en3mt-br0re6a3An,nea,leynttiiAtcllabeldu,Lmaebn"o,Erxattroaarncidteiso'nYQoulaoklfitPyfooAtrsassuAsrniaaunlmcyseiPsUenriftUlusroiernvogiocetwaHenPdeLsCCue-lnEftolrneeactStetruodsfyprroNamuymMEbagesgsr
Spectrometry". All examined phases were reviewed for conduct according to Centre
Analytical Laboratories' Standard Operating Procedures, the Study Protocol, and all
applicable Good Laboratory Practice Standards. All findings were reported to the Study Director and to management
TM 1ProocolReview 2. EFoxrttmicftiicaotni,on 3 RawDuaReview 4 DRnatwDRempaormtd
Review 5. FRienvaileRweport
lDopaetceted 330001 001
45901 44801
aso
Date Reported to Date Reported to
MaCneangtermeent SpSotnusdoyrDMiarencatgoermaenndt
amor
smo
01
son
41801
sm
42601
son
ais0r
aso
`Ange Morgan
Quality Assurance itor
efor Date
Centre Analytical Laboratories, loc.
Page3of 102 60057
_--
Contr Sindy No:023063
CERTIFOIFCAUATHTENITIOCIN TY
"Thinrasepi,ffoorCheiasseyStyNumber 73.063, tre 1 complta geesuaionof Subminodby, CentoAnalytLabor,nc.
S3t0a4t8eRCesoealrclhPDeArgi1v6ee80,1
(814)231-8032
`Principal Investigator, Centre:
B CSoenceoa Annat ya Lae borsts, Jc.
Cen AmtytcnLavoro,Ic,FctltyMing:
RichGarduA. d.
=
PCroneeiAsmaytea Laboatn c.
Study Dict
Ll / Nadler
SWeianlGeallTaeghmeartion,Li.
SponsorReproseaive
seJ b
-
Bu9e
p01 Fa
aio]
Dus
SE " ContesAnalyte) LabrieLc.
Pract iz
C0055
------
Centre Study No.: 023.063
STUDY IDENTIFICATION
"ExtractionYooflkPoftorasAsniaulmysPiesrfUlsuionrgooHcPtLaCn-esEallefcotnraotsepfrraoym/MEagsgsMSepemcbtrraonmeet,rAy,l"bumen, and CENTRE PROTOCOL NUMBER: 00P-023-063
CENTRESTUDY NUMBER: 023.063
TYPE OF STUDY:
Analytical
SAMPLE MATRIX:
MaYlollkardandQuailEgg Membrane, Albumeann,d
TEST SUBSTANCE:
Perfluorooctanesulfonate (PFOS)
SPONSOR:
3M Environmental Technology and Safety Services Building 2-3E-09 PO Box 33331 St Paul, MN 55133-3331
STUDY DIRECTOR:
`SWeialndliGfaellIangthemeartional, Lid. 8598 Commerce Drive: Easton, MD 21601
`TESTING FACILITY:
Centre Analytical Laboratories, Inc. 3048 Research Drive State College, PA 16801
ANALYTICAL PHASE TIMETABLE:
Study Initiation Date:
0326/01
EExxppeerriimmeennttaall TStearrmtiDnaattei:on Date: 0043/2062//0011
Study Completion Date:
09/06/01
Centre Analytical Laboratories, Inc.
Page Sof 102
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--_-- Centre Study No: 023.063
PROJECTPERSONNEL
``TThhee fSotluldoywiDnigrepcetrosronfnoerltfhirsomprCoejnecttrewAansalSyetiacnalGaLlalbaorgahteorriaets,WiIlndc.i,ifweerIentaesmsaotciioantaeld, wLiitdh. various phasesofthe study:
Name Emily Decker Dave Bell Mitra Armand Ling Ling Liu YuQiong Tan Xiaoming Zhu Lawrence Ord Rickey Keller Shawn Robb
Tite Scientist Scientist Technician Technician Technician Technician Sample Custodian Sample Custodian `Sample Custodian
CentreAnalyticalLaboratories, nc.
Page 6of 102
GRO%LT
_----mmmmem
CentreStudy No: 023-063
TAOFBCOL NTEE NTS
RY Pag|e
(QGUOAOLDILTAYBAOSRSAUTROARNYCEPSRTAACTTEIMCEENCTOMP.L.I.AocNvCsEunSeTsAseTnEeMsEs NT ...e .........m ...ooo 2
SCTEUDRY ITDEINTFIFOIIFCACATUITAOHNETN.TII.COcIoTNYrrcsoscssesnsmsssmsssssssissmsssmessssntonnens
fe
LT ISTA OFOTFB ACBOLNEL STEc NE TSo ...s ..ct cnsme nmss smsmsssssissmsssssn81
LI OFFS IGUT RES... LIST OFAPPENDICES.
11 12
20 OBJECTIVE... 3.0 INTRODUCTION c.stsssnsssssssssssssrs
13 13
5.0 REFERENCE MATERIALwc. 6.0 DESCRIPTION OF ANALYTICAL METHOD.
14 1S
6.2 PreparationofStandards and Fortification SONGONS................covmerrrne 15
6:4 6.5
INSUUMENL SENSIIVILY corns, Description ofInstrumentand Operating CONItONS.............owurroens
16 17
7.06.E6XQPEuRIaMEnNaTtnAdLEiXDaEtmSpIlaGeCNta.l.ci.u.lo.a.tcniooono.e.v.smssssmssssssssnsno1ns819
8.0 RESULTS... 90 CONCLUSIONS o.com
20 20
10.0 RETENTIONOF DATA ANDSAMPLES......c..covvummsmnnnnssssirmnsns 21
CentreAnalytical LaboratorieInsc,.
Page 7of 102 CRORE
eee. Centre Study No: 023-063
LIST OF TABLES
Table Summary of PROS in Reagent BIANKS ......vvovssPa2g3e Table Il. Summary of PFOS in Mallard Membrane BIAAKS ver 24 Table IL Summary of PFOS in Mallard AIDUMEN BIATKS......r.roeorrrrsrrrs 24 Table IV. Summaryof PROS it Mallard YOIK BIAUKS crores 24 Table V. SummaryofPROS Recoveries in Mallard MEMbIANC......ccrvcr 25 Table VI. SummaryofPFOS Recoveries in Mallard AIBUMEN.......coccervcone 25 Table VIL SummaryofPFOS Recoveries in Mallard Yolk.. S-- Table VILL Summary ofPOSforWeek 1 Mallard Membrane Control Samples........ 26 Table IX. SummaryofPFOS for Week 1 Mallard Membrane Samples at
Table X. SummaryofPROS for Week | Mallard Membrane Samples at
Table XI. SummaryofPROS for Week | Mallard Albumen Control Samples......... 28 `Table XIL. Summary of PFOS for Week | Mallard Albumen Samples at 6.2 ppm ai. 28
`Table XIII SummaryofPFOS for Week | Mallard Albumen Samples at 17.6 ppm i ..29 `Table XIV. Summary of PFOS for Week | Mallard Yolk Control Samples..............29
`Table XV. Summary of PFOS for Week | Mallard Yolk Samples at 6.2 ppm i ........30 Table XVI. Summary of PFOS for Weck | Mallard Yolk Samples at 17.6 ppm ai ... 30 Table XVIL SummaryofPFOS for Week 6 Mallard Membrane Control Samplcs....... 31
Table XVII. Summary of POS for Week 6 Mallard Membrane Samples at SZE Bussmmamimssmsmsmmi----l
`Table XIX. Summary of PFOS for Week 6 Mallard Membrane Samples at
Table XX. Summary of PFOS for Week 6 Mallard Albumen Control Samples.......... 32
"Table XXI. Summary of PFOS for Week 6 Mallard Albumen Samples at 6.2 ppm si... 33
Table XXL SummaryofPFOS for Week 6 Mallard Albumen Samples at 17.6 ppm ai 33
Table XXIIL SummoafPrROyS for Week 6 Mallard Yolk Control Samples ........34
Table XXIV. SummoafPrFOyS for Week 6 Mallard Yolk Samplesat 6.2 ppm ai ..34
Centre Analytical Laboratories, Inc.
Page 807102
GORE
reese,
Centre Study No. 023.063
Table XXV. Summary of POS for Week 6 Mallard Yolk Samples at 17.6 ppm ai ... 35
Table XVI SummaryofPFOS in Quail Membrane BIoOKS ccc 35
Table XXVIL Summary of PFOS in Quail Albumen BIGTKS .......cccrcror 35
`Table XXVIIL Summary of PFOS in Qual Yolk BARKS ......v.cccrcrcenrcsns 36
`Table XXIX. Summary of PROS Recoveries in Quail MEDIAN...
36
`Table XXX. Summary of PFOS Recoveries in Quail AIUD ...vvecrvcrsnne 31
`Table X31. Summary of PFOS Recoveries in Quail YOK.....rocsrvvvcnsens 31
`Table XJ. SummaryofPOS for Week 1 Quail Membrane Control Samples... 38
Table
XOOKIL. SummaryofPFOS STROM Rs
for
Week
1
Quail
Membrane Samples at ----
`Table
XXXIV.
Summary of FLEUR
n PFOS fa or Weem k 1 Qui ail Men mbrane
Samples
at
`Table XXXV. Summary of PROS for Week 1 Quail Albumen Control Samples ........ 39 `TableXXXVI. SumofmPOSaforrWeyek 1 QuailAlbumen Samplesat 6.2ppm ai...40 `Table XXXVIL TSumEmaEryRofm PROS fom r Weekm 1 Quail Albumen Samples at
`Table XXXVI. SummaryofPFOS for Week 1 Quail Yolk Control Samples...........41
`Table XXXIX. Summary of PFOS for Week 1 Quail Yolk Samples ot 6.2 ppm gi ..... 41 Table XL. Summary of PFOS for Week 1 Quail Yolk Samples at 17.6 ppm si..........42
`Table XL Summary of PFOS for Week 6 Quail Membrane Control S&mpes...........42 `Table XLIL Summary of PFOS for Week 6 Quail Membrane Samples a 6.2 ppm ai...43 `Table XLII. SummoafPrFOyS for Week 6QuailMembrane Samples at 17.6 ppm i..43
Table XLIV. SummaryofPFOS for Week 6 Quail Albumen Control Samples........... 44
Table XLV. Summary of PFOS for Week 6 Quail Albumen Samples at 6.2 ppm i ..... 44.
`Table XLVI. SummaryofPFOS for Week 6 Qual Albumen Samples at 17.6 ppm si.... 45
Table XLVIL SummaryofPFOS for Week 6 Quail Yolk Control Samples ............ 45
`Table XLVIIL SummaryofPFOS for Week 6 Quail Yolk Samples at 6.2 ppm i .......46.
Table IL. Summary of PFOSforWeek 6 Quail Yolk Samples at 17.6 ppm s........... 46
Table L. Summaryof Moisture Determinations for Mallard Membrane Samples..... 47
Table LL Summary of Moisture Determinations for Mallard Albumen Samples.......48
Centre AnalyticalLaboratories,Inc
Page9of 102
chav
eee.
Centre Study No. 023-063 Table LIL. Summaryof Moisture Determinations for Mallard Yolk Samples.....49 Table LIN. Summary of Moisture Determinations for Quail Membrane Samples ...... 50 `Table LIV. Summary of Moisture DeterminationsforQual Albumen Samples......... 51 Table LV. Summary of Moisture Determinations for Quail Yolk Samples.............52
`CentreAnalyticalLaboratories, nc
Page 100f 102 6n0vL
eee.
`Centre Study No: 023-063
Figure 1. Figure 2. Figure 3. Figure 4.
Figure 5.
Figure 6.
Figure 7.
LI OF FS IGUT RES
Rage Typical Calibration Curve fOr PROS ...vvvvovrcerssnsesssnsos 54 Chromatogram Representing a 0.1 ng/mL standard for PFOS .............55 Chromatogram Representing a 1.0 ng/mL. standard for BOS... 56. Chromatogram Representing a Reagent Blank for PFOS (Centre ID Reagent Blank A, Set: 032601A)..rorvvovnrvsvevesinn ST CIDh:ro0m0a0t3o8g02raBmlRaenpkrAe,seSnetti:n0g3C2o6nt0r1oCl)Mallarrd Mrembrrane for PFOS (Centre58 CPPhbroomfaPtFoOgSr,am(CReenptrreeseInDt:i0n0g0C3o8n0t2roSlpMkalAlaDrudp.MeImnjb,rSaent:e0Fo3r2ti6fi0e1dCwi)thcc..1.0 59 Cath6r.o2mpatpomgria(mER0e1p-r0e2s6e3n-t2i0n8g2M5a)ll(aCrendtMreemIDb:ra01n0e3S09a2m,plSeetf:r0o3m26W0e1Ce)k..1.....60
`Centre Analytical Laboratories, Inc.
||
Page 11of102
GaCED
--_--------
Centre StadyNo:023-063 LAISPTPOFENDICES
Page AppendiAx StudyProtocol 00P-023-063 (Centre Study No. 023-063) and
Centre Analytical Laboratories, oc.
Page 1201102 CRORES
_--_-- Centre Study No: 023.063
1.0 SUMMARY
CaelnbturmeenAnaalnydticyaollkLasbaormaptloersiesfo,rIntch.e(dCeetnetrrem)ineaxttiroanctoefd mpaelrfllaurodroaoncdtaqnueasiullfeogngatme.em(bPrFaOnSe), according to protocol 00P-023-063 (Appendix A)
`dTehteerlmiimintedofinquaanmiettahtoidonvafloirdeataicohn msatturdiyxpwearsfor1m0epdpbat. CeTnhtereL(OCQentfroer Setaucdhy:ma0t2r3i-x02w7a).s
PFOS ranged concentration
fofrotmhenolno-wqeusatntciafliiabbrlateio(nwhsetraendnaornd-q(u0.a1ntnfgia/bmlLe)isledveeflisnetdo
as less than 434 nglg in
the the
`amlablulamrednmseammbprleasn,easnadmpflreosm, nforno-qmuannotni-fqiuaabnliefileavbelles lteove6l3s,5t0o03n5g5/0g ninegtheinmatlhelamradlyloalrkd
samples. membrane
POS ranged samples, from
fnroonm-qunaonnt-ifqiuaabnlteifliebvleels
letvoel9s3.t9o
n2e0g.90i0n
tnhge/gquianil
tahelbquumaeinl
soafmtphleesse,reasnudltfsarroemrneonp-qouaonrtnitafaewbeldet
level (0 65,500 weight basis.
ng/g
in
the
quail
yolk
samples.
All
The average albumen, and
percent recoveries yolk samples were
+ standard deviations for 91% 6%, 91% + 16%,
PFOS in and 93%
mallard membrane, 13%, respectively.
Talhbeumaevne,raagned ypeorlckseantmprleecsovweerirees 1+0s2ta%nd1ar1d%,d8evi5at%ion5s%,foarndP9FOS6+i7n%%q,uarielspmecetmibvrelayn.e,
2.0 OBJECTIVE
`The objective of this analyticalphaseofthe studywastodeterminelevelsof paelrbfulmueonr,ooacntdanyeosluklfuosniantget(hPeFaOnSal)ytiincsalpemceitmheondstoiftlmead,ll"aDredtearnmdinqauatiilonegogf membrane, Perfluorooctanesulfonate in Egg Membrane, Ablumen and Yolk by LC/MS/MS".
ODUCTION
`This report details the results of the analysis for the determination of PFOS in mallard and quail egg membrane, albumen, and yolk using the analytical method entitled, "Determination of Pefluorooctanesulfonate in Egg Membrane, Ablumen and Yolk by LC/MS/MS".
`This analytical portion of the study was initiated on March 26, 2001, when the study
d`iMraerccthor26s,ig2n0e0d1,Caenntdrtehepreoxtpoecroilmennutmabletrer0m0iPn-a0t2i3on-0d6a3t.e
The experimental was April 2, 2001
start
date
was
Centre Analytical Laboratories, nc.
Page 130f102 CORT
Centre Study No: 023.063
4.0 TESTSYSTEM
bTlhaenkcsontarnodl mmaaltlrairxd afonrdtiqfiucaaltioengsgwmeermebrraencee,iveadlbuomnenM,aaynd 1y8o,lk20u0se0d ffroromtheWimladtirfixe
IwnetreemaatsisoinganledLitdo.,thEeadsitfofne,reMntDmatarnidcesst:ored frozen at Centre. The following Centre ID's
MallaMradtMreimxbrane
Co00n03e8I02D
Mallard Albumen
0003800
Mallard Yolk
0003799
Quail Membrane
0003798
Quail Albumen
0003796
Quail Yolk
0003795
On February 23, frozen until they
2001, were
308 quil logged in
egg samples were received. The by Centre personnel on February
samples 26, 2001
were and
stored stored
fwreorzeens.torOend fFreobzreunaruynti2l4,th2e0y01w,ere19l4ogmgaeldlairndbeyggCesnatmrpelpeesrswoenrneelreocneiMvaedr.chT1h,e20s0a1mplaensd
sshteolrle.d fEraoczehn.coEmapcohncegngt soafmtphleeergegcewiavsedgwiavsendiaviudneidquientCoemnetmrberIaDnea,t atlhbeutmiemne,oyfollko,gainnd.
sAltphouogwhenralelesoxftrotahcetreedggansdamapnalleyszewde.re received at Centre, only those designated by the
aSsasmopcliaeteldogw-iitnhatnhdiscshtauidyn.ofStcoursatgoedryecionrfdosrmwaitlilobneckaenptbaet fCeonutnrdeiAnnatlhyetircaawl dLaabtoaraptaocrkiaegs,e
Inc. and a associated
true copyofthestoragerecords with this study.
canbefound
intherawdatapackage
5.0 REFERENCEMATERIAL
TheanalyticalstandardPFOSwasreceivedat Centre on June 3, 2000from 3M Environmental Technology and Services Stability was not assessiend this study butthereference material was stored according to trheefecreerntcieficmaatteoerfiaanlalwyassisn(otfrorzeelne)vaanntd twoasthiussesdtpurdyi.ortToheexpaivraaitiloanb.le Tihnefosromlautbiiolnityofofrtthhee reference material i listed below.
CPomFpOoSund ~~ Cent0re0C0o2n3v0ol2No. TCRTOC0R0NIoT.46 Pur9i7t9y(%) Expir0a8t3i1o/n0D1ate
Centre Analytical Laboratories. Ic.
Page 14of 102 CRORES
BE
`The molecular structureofPFOS is given below.
CPhFeOmSical Name ~~ = Molecular weight =
wt--o
Perfluorooctanesulfonate 499 (CiFinSO)
Centre Study No. 023-063
oNbottaei:neTd,heisnpeouttaraslsimuomlepceurlfleuaonrodoscttaanndeasrudlffornoatmew[hCiacFhirtSheOsPKF]O,Smo(laenciuolna)risweight 538.
6.0 DESCRIPTION OF ANALYTICAL METHOD
MAneamlbyrtiacnael, Ambeltuhmoedn aenntdiYtloeldk b"yDeLtCe/rmMiSn/atMiSo"n waosf usPeedrfflourotrhoiosctstaundcys.ulfonste in Egg 6.1 Extraction Procedure
Egg membrane
`Aad0d.e1d tgostahmepslaempwlaes aulsoendgfwoirththtehreexetrsatcatiinolnespsrsotceeedlurbeea.ds.OneThmeilslialmiptelreowfamsetthheannopllawcaesd `omninai-bceeantdribfeuagteerats~et2a0t0p0osriptmifonor7 ~fo2r m$inmuitneust.es.EacThhesasmapmlpelweawsafsilttheernedcaenntdrainfaulgyezdeodnbya LC/MS/MS electrospray.
Egg albumen and yolk
A 10 g `methanol
sample was used were added to the
for the sample.
extraction The sample
procedure. was placed
Twenty-five milliliters on & wrist-action shaker
of for
o1f5 tmhienustaemsplaendwtahsentackeenntrainfudge0d.a5tg~o2f0c0a0rbropnm wfaos~rad1d0edm.inuTthese. saAmpfliveewmailslislihtaekreanlitqhueont
allowed t0it. Each sample was filtered and analyzed by LC/MS/MS electrospray.
6.2 Preparation of Standards and Fortification Solutions
Standard solutions were prepared on March 14, 2001 as specified in Centre Analytical
Laboratories" protocol 00P-023-027. An individual stock standard soluotfiPFoOnS was
prepared at a concentration of 100 g/mL by dissolving 10 mgofthe standard (corrected
for purity and salt content) in methanol. From this solution, a 1.0 pg/mL fortification
s1t0a0ndmaLrdwsiotlhutmieotnhawnaosl.prepared by taking 1 mL of the stock and bringing the volume upto
Centre Analytical Laboratories, Ic.
Page 15 of 102
COREY
_--
Centre Study No. 023.063
fTohretif0i.c1atgio/n mstLanfdoarrtidfiacnadtiobnrisntgainndgartdhewavsolpurmeeparuepdtboy1t0a0kimngL1w0itmhLmeotfhtahneol1..0 Ag/0.m0L1 g10/0mmLLswtiatnhdamredtwhaansolp.reparedbytaking 10mL ofthe0.1 pg/mLstandardandbringing to
nAgs/emtoLfssotluatnidoanrsdsinctohnetfaoilnlionwgiPngFOmaSnnwears.prepared by dilution of the 0.1 pg/mL and 0.01
Initial Cone. (ug/ml) 01 01 0.1 001 001 o0f0P1FOS
Volume (mL) 5 2 1 5 2 1
Diluted to (mL) 100 100 100 110000 100
Final Cons. (ug/L) 0.005 0002 0.001 00..00000025 0.0001
s`Tthoeresdtoicnk astarenfdrairgdersaotlourti(o4naCnd 2allCf)ortwifhiecnationnotanidn cuaslei.bratDioocnusmteanntdaatridosnoloutfiosntsanwdearred preparation can be found in the raw data associated with this report.
63 Chromatography tQuiamneotiffiPcFatOiSonWoafsP~F4O.S4 mwians. aPcecaokmsplwiesrheeddebtyectLeCd/iMnSt/heMcSonetlreocltrmoastprriacye.s cTohrreesrpeotnednitnigo,n a1l0tetrhethaenraelsyutletsreitnesnetvieornaltiomfe,thbeutretchoevearimeosunrtepsordteetdecatnedd twheerreesotnwleyrseiglneissfitchaantn ethneoulogwhestto calibration standard (0.0001 pg/mL).
64 Instrument Sensitivity cTohnecenstmraaltlieosntofs0t.a0n0d0ar1dg/ammoLuonftPFiOnjSe.cted during the chromatographic run had a
Centre AnalyticalLaboratories,Inc.
Pa16gof1e02 COPD
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Centre Study No. 023.063
65 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:
PESciexAnalyst version 1.1 `Windows NT, version 4 Hewlett Packard (HP) Series 1100
HP Quat Pump HP Vacuum Degasser HP Autosampler HP Column Oven
HPLCColumn:Genesis Cs (Jones Chromatography), 2.1 mm x 50 mm, 4 Column Temp. 35C. Injection Vol.: 10 uL `MMoobbiillee PPhhaassee ((BA)):: M2emthManAolmmonium Acetate in ASTM typeI water FlowRate: 0.3 mUmin.
Ti0me %6A0 %4B 00 0 100 79 0 10 n75o 660 4400
Tons monitored:
Approximate
APnRgOSe neMgoadtieve Transi4ti9o9nM3o9n9itored Retention4T4i0me(min)
TPuanerFialme eters
1CS-olnotsrporlasy 'D`PF-PD-eFcolcusutseirnignPgotPeontteinatlial ECPE-CEontlriasnicoenPoEtneenrtigayl CXP-Collision Cell Exit Potential Centre AnalyticalLaboratories,lnc
42S0et00 2531000 1EO0)0
5 Page 1701102
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e-- r ----------------------------------------
Centre Study No. 023.063
`CEM.ChanDnFe-lDEelfelcctrtoonrMultiplier
238000000
NeGbausliFzleorwGass
s1a2t
CColulritsiinonGGaass
14 4
IS Temperature
asc
66 QuantiatnadEtxaimoplne Calculation
p`Teeankmairceroalwitaesrsmeofassuarmepdleanodr tcahleisbrtaatnidoanrdstcaunrdvaerdwawsergeeninejreactteedd(iunstiontghe1/LxCw/eMiSgh/tMeSd.liTnehaer croengcreesnstiroant)iobnys fAonralmyasltlasrodftawanrdequusaiilngegatg lmeaesmtbrfiavnee,conaclebnutmreant,ionasndofyosltaknd(anrgd/sg,) wTehree determined from the equations below. `tEhqeuasttiaonnda1rdcalccuurlvaeted(ltihneeaarmroeugnrtesosfioannaplayrteamfeotuenrd)(ignennegr/amtLe,dbabsyetdhoenApneaalyksatresso)futswianrge program.ThenEquation 2 calculatedtheamooufannalyt found in ng/g.
Equatio1n;
Analyte found (ng/mL) = (Pareae.-inatrcekps)
slope.
`Equatio2n: Analyte found (ng/g) =anal.foundsa(mnpgl/emwLi). X(F)V(mL)xDE
WheFrVe:= Final Volume DF = Dilution Factor
cFaolrcuslaamtpedletshefpoerricfeinetdrewciotvherkyn.own amouns of PFOS prior to extraction, Equation 3
Equatio3n;
Recovery (%)= (anal. Found`(angm/ogu)nt- aadved.edan(anlg./ign)cir (ng/gx) 100
`An MeaxlalmaprldeoaflbaucmaelnculsaatmipolnesCienngtraen IacDtu0a0l0s3a8m0p0leSpfoklAlows(:Set: 0326014), fortified at 10 Pbb with POS, where:
CenireAnalytical Laboratories, Ic.
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Cao
--_--_----
`Centre Study No: 023-063
peak area intercept
= =
slope. dilution factor
= FE
nagv/ggaamdtdiendc(ofnotrtrollevsel)
= =
final volme sample weight
= =
3 on 600 10nglg 0s(Nmot quantifiable) lomsg
Note: (No.1t qnugamnLti)f.iable is defined as less thantheconcentrationofthe lowest standard
From equation 1: Analyte found (ogfml)
= [3369-971] 6700
From equation 2:
= 036ngmL
Analyte found (ng/g) = (0n.3g61.0/038m(g)LxmL2x15)
From equation 3: % Recovery
= 897ngmL = (89170nnggllgex=0ngipx) 100
Note:Thisexample
= calculation
90% was doneusing
rounded
numbers,
and
thereforemaybe:
slightlydifferentfromthe values shown in the RAW DATA.
7.0 EXPERIMENTAL DESIGN Efoarcthifiseedt aotfksnamopwlnescocnocnesnitsrtaetdioofnso,naendre~age2n0tsbalmapnlke,s.oneEamacthrisxambpllanek,watswoexmtartarcitxedbluasniknsg tbhleanakppwraosprainaatleyzmeedt.hod and then analyzed in duplicate. Also, in each set, a Type I HzO
CentreAnalyticalLaboratories, Inc.
Page 1901 102 CRO%ET
--_--_--m-mm-----
Centre Study No. 023.063
8.0 RESULTS
PFOS found in the `membrane, albumen,
reagent blanks are and yolk blanks are
listed given
in in
Table Tables
I The I-IV.
PFOS in The PFOS
the mallard in the quail
d`emteemcbtreadnei,n saelvbeuramleonf,tahnedcyoonltkrolblmaantkrsicaerse, ghiovweenveinrTfaebwlewserXeXsVigIn-ifXiXcaVnItIeLnouPgFhOtSo awltaesr
the recoveries reported.
dIentdaiivlieddualinreTcaobvleerisesVf-oVrIPLFOSThien athveermaaglelapredrcmeenmtbrraecnoev,erailebsu+mens,taannddarydoldkevsiaamtpiolness faroer
PFOS in mallard membrane, albumen, and yolk samples were 91% + 6%, 91% + 16%,
aalnbdu9me3n%, an1d3%yo,lkresspaemcptliveeslya.reIdnedtiaviildeudalinreTcoavbelreiesXXfIorX-PXFXOXSI.in Tthheeqauavielramgeembperracneen,t
recoveries + samples were
1st0a2n%da+rd11d%ev,ia8t5i%ons+
5f%or,
aPnFdO9S6%in+q7u%ai,lremsepmecbtriavenley,.
albumen,
and
yolk
cPoFncOeSntrraantgioend
froofm
ntohne-qualnotwiefsitableca(lwihberrateionnon-qsutaanntdiafridable(0i.s1
defined as ng/mL)
less then levels
the to
4th3e4mnagl/lgarind tahlebmuamlelnarsdammpelmebsr,aannedsafmrpolmesn,onf-rqoumanntoinf-iqaubalnetilfeivsebllsetloev6e3ls,5t0o03n5g5/0gnign/gthien
mallard yolk samples. These results are reported on a wet weight basis. Individual
rseosmueltofartehelismtaeldlainrdTaebglgesmeVmIbIrIa-nXeXYa.nd Seogmgealobfutmheen hsiaghmplleevselcsooufldPFbeOSfrroempoprotsesdibfloer
contamination from the egg yolk or outer shell.
PfrFoOmSnroann-qgueadntfirfoimabnloen-lqeuvaelnstitfoab9l3e.9lenvge/lgs tion 2t0h,e9q0u0ainlg/aglibnutmheenqsuaaimlplmeesm,barnadnefrsoammpnloens-, a`quwaentiiwfieaibglhetlebavseilss.toI6n5di,v5i0d0uanlg/rgesiunlttshearqeualiilstyedolikn sTaambplleess. XXTXhIeLs-eIrLe.sultSsoamreeorfetpohretehdiognh levels of POS reported for some of the quail egg membrane and egg albumen samples could be from possible contamination from the egg yolk or outer shell. The Sponsor Representative also informed Centre that the quail outer shells were not washed prior to sepasation of the intemal components.
`Theaverage percent moisturesforthe mallard and quail egg membrane, albumen, and yolk samples are given in Tables L-LV.
9.0 CONCLUSIONS
`The mallard and quail egg membrane, albumen, and yolk samples were successfully extracted and analyzed according to protocol 00P-023-063,
Centre Analytical Laboratories, Inc.
Page20of 102
nov
eee e------------------------ Centre Study No. 023.063
10.0 RETENTION OF DAT SAMPLI
L`aWbhoernattohreiefsi,naIlncr.epwoirltlibsecosmhpilpepteed,taol thoerisgpionanlsopr.apeTrhdiastadogeesnenroatteidncblyudCeenfatcrieliAtnya-slpyetciicfailc
raw data such as submitted. Exact
instrument logs, copies of all raw
however exact data, as well as
acospiigensedofcotpeympoeftrahteurfeinlaolgsanawliyltlicbael
Lraebpoorrtataonridesal,lIonrci.gainraclhifvaecslfiotyr-tshpeecipfeirciordawofdtaitam,ewsiplelcibfeierdetiani4ne0dCinFRthePaCretn7t9r2e. AnRaeltyatiinceald
samples of reference substances are archived by the sponsor.
`CentreAnalytical Laboratoriensc,.
Pa21gof1e02 GOR
_-- Cente Sudy Nos 023.063
Contre Anaya Laboratories
Page 2201102 Cans
Centre Study No: 023.063
Table. Summary of PFOS in Reagent Blanks
Spowor Centre
D
mmm RRaegngiBBllkkAA
m RegmBlwkA
nmm RRaeggneBBalokkAAt
mm RRaeggennBBnlkukAAt
mmo RReeggmmBBllnukkAAt
mnmo RReaggeenmBlBankkAA*
mwm RRaeggmebmBllmukkAAt
wm RegiBlnkAt
mwm RReaggeemmBlBwnkkAAt
wmm RReeggeemmBlBmlkkAAt
nm RegmBlukA
nmma RReegaegnwBBllankkAAr
nMmm RReeggnwBBllmnkkAA
mnoo RReeggnwBBilnnkkAAt
na RemenBlmkA
* Duplicate injection
St Number
Exmcon Dae
ADmuies
FoAunmdigtpeh
0O2O6IAA
660011
w62001 M6201
NQ NQ
ORGIB 32601 32701 NQ
OORR6GIIBC 332660011 3M2200010 NNQe
OOR0I4C M3206011 3322080010 NNoo
0O2008A 332270011 W38282000 NNOo
02708 3201 3282900 NQ
OOR200ICC 3M2270011 3322990011 NNoo
OORIMIAA 3322880011 3355000011 NNoo
OORRMIBB 3322880011 3355000011 NNoo
OORRSS00IIAA 33990011 356110001 NNQQ
GOD9SO0IB W32990011 5A4I0L0 NNQQ
OOSSXXOOIIAA 33000011 44110011 NNeo
0OB0O8E 0300011 44220000 NNoo
OGSB00CIC O33D00I1 4a2n0no0 xNoo
STANDARDDEVAIVAETRIAOGNE:: NNOQ
NQ =Not Quantifiable (les than the concentrationofthe lowest standard (0.1 ng/mL) LOQ=10ppb
CentreAnalytical LaboratorieIsc,.
Page23of 102 Coz
_--_--mmYe------------------ ------,----
Centre Study No. 023.063
Table IL. Sponmsor
wWow wWmw
Summary of PFOS in Mallard Membrane Blanks
Cenmtre CGNOMRRBWDEAAT oommsMwRpuBkuAAr
NuSmtber BuDnacieon AmDaitnee FoAumdit(peb) 0O2R0OIICC 820600 vveo7mnl xNeo 0ow2oi0c zzml n3o9om NNoo
STANDARDDEVAIVAETRIAOGNE:: NNQQ
Table III. Sponnsor
wm TM mwoo nm
Summaryof PFOS in Mallard Albumen Blanks
Centre NuSmbter CCNOMWOOBBMMkKAAT| OOINIAA COOM0ONBOMBkKAAT 0ORXOI0B 0OBMWmOkBAMtKA_ 0OBN0WIICC
BuDraceion ADuues W36600I1 Sa220 I3O0I Mm2a9l0 3300000,1 n42o0l0 STANDARDDEAVVIEARTAIGOEN::
FoAumnidytGeop) NNQQ NNGQ 665093 22692
Table IV. Summary of PFOS in Mallard Yolk Blanks
Sponsor Cone NuSmaber ExDmactieon ADmaice FoAunmdiptpeb) mwom CGXOMTOOBBkUAAT 002R6GO0I8B a3a2e800l 3um2l7 NNoo nnmo oMmOveBomMmKkAAr _ o0w2wo0iAA v2z eomeim 505510 STANDARDDEAVVIEARTAIGOEN:: 455478
--
1N0QQ==N1o0tpQpuabntifiable (ess than the concentrationof th lowest standard (0.1 ng/mL)
wFoarsruesseidduteoscraelccourladteedtahseNaQve,rhaaglefoafndtshetacnodnacredntdreavtiiatoinoon.f the lowest standard (1.25 ppb)
CentreAnalyticalLaboratories Inc.
Page2601 102
610703
eeeen
Table V. Spmoor mmoo mwom mmoo mnom
CentreStudy Nos:023-063
SummaryofPFOS Recoveriesin Mallard Membrane
CeIntDre NeSmbter BnDcaieon ADmuies AlAdmta) Reco=very
NGBOQMSRKSAAT O02RIRC 3s6n0l1 7w271ml 1100
0o
NGNMQRSSKKBB R02e0IcC 6asmol z32o7n1 1100
oa
cKoNMBRRSSkKAAr oowoCIC vooll 3399001 110
94
oowwmMwQsSiKbBe oowiwoic owlm 3no0n0i Fi0l
osss
STANDARDDEAVVIEARTIAOGNE:: 561
RELATIVESTANDARDDEVIATION: 7
Table VL. Summary ofPFOS Recoveries in Mallard Albumen
Spowor ICe"n)tre NuSmtber BrDcaiteon AwDbastels AddeAdmppb) Recovery
wmmo CGOOOBMOOSSEKKAA ORR6ROOIIAA 2I66001I a 626 01 1100
1w
mmoo CONNNNOOSSKKBB OO0RRKGOOIIAA MMeeoo aassmm 999%
524
wwoo NGWOOWSOSKKAAT OORROO oOlL m m2 l 1100
0105
wmoo oGONWWOOSSAKBBe OGwIiOOB 3o2l0 mMm0m 999
101
mmoo OCNOOOSSAAT oONmOIcC 330000011 a4n2o0n1 1100
aFl
mm o oCo OMBs OS OOIOBOICC 33050000 4a2000 sseeanmss F5Y
STANDARDDEAVVIEARTAIGOEN:: 5116
RELATIVESTANDARDDEVIATION: 17
*Duplicate nection
L0Q=10ppb
CentreAnalytical Laboratories, nc.
Page25of 102 a0%3T
-- _--_--_-- AmoemAM-- Ammm ------ ------ ------
Centre Study No.: 023-063
`Table VIL. Summaryof PFOS Recoveries in Mallard Yolk
Spoor CeDn___re NuSmtber ExDuoen ADsuiee AdieAdmtopt) Recovery
NNae oOo0e7O0SSEAAc GommeOeInB 332ao600l 323020l0 T1o0
1o0r4
NNoo ooomSmOoSSkKBBe oOm6en0s s6u0i1 33277000 9%%
9%
NNoe Co0mMsOeSSKKAAT GOXOIAA a3o0l 3w2a80r1 100
nn
NNee oOooMwSosKihe o0wmoAiA_ a3v0e0 3w2w0e0 95
558
STANDARDDEAVVIEARTIAOGNE:: 1933
RELATIVESTANDARD DEVIATION: 14
Table VILL Summary of PFOS for Week 1 Mallard Membrane Control Samples
SpIon"sor CIen"t)re REoiLmmeeesss o00o2m0O0 BEolLemEaess oonos EEollmelmaosose 0o0w0s8 EEllecom 0o0o0 EEOlLGmG0MoS Oonsess
* Duplicate Injection
NuSmtber EDaatrtceion ADmupes FoAunmdigep) oonweilcc saswo ammm0o NNoo oonneilcC daassoe 33aam NNoo oonneoollcC adsaeoo 33a0m Nxoo moneicc veeoo 3ve0e1l NNoo 0onweeliCc swoeln 3s7m0n1 NNoo
STANDARDDEAVVIEARTAIGOEN:: ~~ NNQo
NQ = Not Quantifiable (less than the concentration of the lowest standard (0.1 ng/mL)) LOQ = 10 ppb.
CentreAnalyticalLaboratories,Ic.
Page2601 102 Crave
--_--_--mnmm
Centre Sendy No. 023.063
Table IX.
SummaryofPFOS at6.2 ppmai
for
Week
1
Mallard
Membrane
Samples
Sponsor Centre BBlomeawmss oowws EEllGeed20s8e6 OOTSSS EEllmmewesrz 0os3o0 EEOlL6m208s7 0o0w3s0 EElLCmss oodwss
NeSmtber BxDmucieon ADmatiek o0wneeo0licc | wwaee0r 3320000 mopeeloiec wwesno z327o0 omneelcC eweon mya0m 0onneiNcC dmeemwi 3m0n0 oownec waesno 3s2m0i0
TTSTANDARD DEaVvIAeTmIOeNs:
FoAunmdioept T1e6t3e0r "562s m712 5219 sEns a11.2 r
Table X. SummaryofPFOS for Week 1 Mallard Membrane Samples at 17.6 ppm ai
Sponsor CentDre NuSmbter EatDraatcedon ADmubea FoAuamdigeph) EBOiLmewasssee ooi0mes 0RoewOollcc awseo 3m27000 2260a00 BElmleamssse ooosn oonmeiolcc awessow 322000 2255 EEoLLo2s0a8osssTr ooomm oommce ovsomr vvemer 5wo BELlGE0a6SsI 0o6s o0nneilcC smuelw 3372001 2217m0 EBmleeal 0o0w2s4 oommeidcc wdeaenw 3wamm s201 TT STANDARDaDEmVIAeTIOsN: a2m31 + Duplcte njecion
LOQ = 10 ppb
R+eprPeossesinbtlaeticvoentreaqmuiensattiwoenrebynoytolukseodr 0outcearlcsuhlealtlectohmepaovneernatgeofansdamsptlaendaanrdd daesvipaetrioSnp,onsor
CenireAnalytical Laboratoriensc.,
Page270f 102
R07
_--
Centre Study No. 023.063
Table XI.
Summary Samples
of
PFOS
for
Week
1
Mallard
Albumen
Control
SIpo"nsor
Centre n
EE IGG EN 0o0oml
EEOlLmmeieaseasSyS oOsOsS
BElOLmaezmosfssee o0Io0Nm0D
BEimmeeaNssee ooisee
EEllGmese ooisse
St Number
Barton Date
Amis Due
Amie Found Gp)
RGeIlAA weessowl wmeeamn NNQG
momeelNaA wwsew veeamm NNGQ
oORnGDeIA saswo e326m70 NNgo
0GReO0lAA wssw e3a2mm NNQG
omeula wwsednl emeaomw NnGo
STANDARDDEAVIVAETRIAOGNE:: NNaQ
`Table XII.
Summaryof PFOS at 6.2 ppm ai
for Week 1MallardAlbumen Samples
Sponsor
CIe"nt)re
EEOLlwae0s Oosw
EElLmeMwsSe 0o0oMm
l Eleesm 0o0n2a1
EElLmCs OolONSISSl
EELLeGoeo0Muss OolSoviSss
[L----
NSuembter ExDtaratcetion AnaDlyuseis FoAnualytGep) oRmeelnA wWees0wr vaeem 2278s o0n2co0lAn sdowe0 es2a0m0 71680 0ooAl seoo eveaaml ssemr 0mReAOlA ssoll wseaamli s5s6 moemlaa sweooii enaema e59x5
STANDARDDEAVVIEARTAIGOEN:: 51.860
NQ = Not Quantifiable
LOQ=10ppb
(less
than
the
concentration
of
the
lowest
standard
(0.1
ng/mL)
Centre Analytics Laboratories, Inc.
Page 280 102 [re
-_--
mM
Centre Study No. 023-063
Table
XIII.
Summaryof PFOS at 17.6 ppm ai
for
Week
1
Mallard
Albumen
Samples
Sponmsor EEODLLOO322S0088SS66 EELOLOOG6aS20088SS6e EEOOLLOO6SB20088S506 EEODLLO26G3220088S507 EEOOLLOOGSS220068S5T1e EEODLLOOGASS20088SSIST EDLOJGI06SE
Cenmtre 0O0I20R0I77 0o10l1o7rDep 010012003T1D3ip 0O10I32D21 O0IIO03SN2S1T OoIlONoIaSsT loss
NumSbeer EDxactieon ADuateb OOD TM6R01 E osTmTR oomn0iIcC 33a00001l maomlr 00m3O0O0IICC 0300011 a4nmoml OomReOOlA daee0wl seaammi GGmOeOAlA daeo0l mweeaann OOMRGIOIAA 33660011 eenmool eommelaA eneowi azwseavamml
TTTSTANDT ARD De EVIATe ION:
FouAnmd,iye s1i3s8gge 1a3as6e5s0 e24e7 2z3ss T2o33e g1ar7e a 1g 220
`Table
XIV.
Summary Samples
of
PFOS
for
Week
1
Mallard
Yolk
Control
Spomor Centre EEOLOL NIZ0E6S: 0Ol0os9io8E EEDoLLoOeSzoBtSsIs o00Ri02 EEOOLLOONGSIa20088SS4 OOllm03o0s6 EEDOLLOO2S620S8026 OOINES EEOLLOOGNMS008b3I oodviee *Duplicte nection
NuSmbeer. OOumeoelnB o0wneosB G0e600l8B 0RnOaBB ea2emOlB
EDxtartacetion AnDaatley emoeoni ammlon vdaassool 3ammomr e3aoenm aymm adaosonl 33ammm) emoenm ysomm STANDARD DEAVVIEARTAIGOEN::
FoAunnadlyte NNoo NNoo NNQo NNoo NNoe NNQQ
L'N0QQ==N1o0tpQpuabntifisble (Jess than the concentration of the lowest standard (0.1 ng/mL)
CRe+en*ptPrroeesssAeninabtllayetticivoceanltrLaeamqbuioenrsaatttiowroeinreesb,ynIoycto.luksoerdotuotcearlcsuhlealtlectohmepaovneernatgeofansdamsptalnedaanrdd daPesapvigeaerti2So9np0,o1ns1o02r
aon
---
Cente Study No. 023.063
Table XV. Summary of PFOS for Week 1 Mallard Yolk Samples at 6.2 ppmai
Sponsor m
TEoolorceizeoensst EEOlL2mo0Mss EEllmseoem BEOLLGO2E6322008M4T7 EBollmaeoMms
Centre ID
0O0N0S OONN OOOUSS OOB7S8 OoNoS
St Becton Asis Nember Due Due
Amie Fou ey)
GGR266O0IDD 3a2e600l1 33221122880010 2257800
OORRGIDD 3606001 332712288000 11510000
OOIRDD 36ze0o 3372sa w38o9w0
0OR6MIDD 33600011 33221022880000 1101510000
OomReDn 2v6e0m 3y2n1o28s0o1 112211000
STANDARDDEAVVIEARTAIGOEN:: 8435000
`Table XVI. Summary of PFOS for Week 1 Mallard Yolk Samples at 17.6 ppm ai
Spoor m
Centre St n Nomber
FTOoLrmceoasmssse| 0000M1l4| 00RNMG0OIIDD
EEDlLOm26e3s20s65r0 OONN 0GR260DID
BEooleliausssT oloOowwilss O0NN6OOIIDD
EBLoDlEeSsT oOldIs o0nNc6oIiDp
EEolmLeeE sit 0o0Nw2 oOmRMeInD
Extraction Auaiys Dae Due 3S2O60L1 3327722880001 3a2o60r1 3321722880000 3a0n0i1 732212880m0 a3aee00lr 332a122880000 s30o60i1 3m2a72s80s1 STANDARDDEAVVIEARTAIGOEN::
FoAuswd e(opt) 330030000 000000 Sse26000 S53117000 62100000 4182500000
+ Duplicate nection
LOQ= 10 ppb.
CentreAnalytical Laboratories, Ic.
Page300f 102 Ca0Z
eee,
Cente Study No. 023.063
Table XVIL Summaryof PFOS for Week 6 Mallard Membrane Control Samples
Spoor n
Cenntre
TEooLOm26e32m09e93 0o10s37e64
E Elmmss 0oll0SeT6ss
E ELmsews es oollss
EElmmeerrs o0s0es?
EB msL 09 o_oilsnsso
NuSmbter EDxtruacetion ADmuien FoAuwndyigep) oozco wamoon a3so0 xNoo oazroo vwoo oomm xxoo oozzoo wwmo 3wosm NNoo oomiic omonn n39s0o1 xxoe owrcoc vomn 3_s9no0m Nxoo
STANDARDDEVAIVAETRIAOGNE: ~~ NNQQ
Table XVIIL Summary of PFOS for Week 6 Mallard Membrane Samples at 6.2 ppmai
Sponsor D
Centre m
EToLOo63m200e79% 00100s37T0s8
BEoOLLOo2s63s221i00010 00110033779966
EEolmmezeosnse 001l003S7T4
BBOLoOl62s09a71 0010036k76
EoOlLeCs60280s8 0010033774488
Dupe jction
Sa Number
Exncin Date
Amis Dute
Amie Found (pt)
oGaooic aomnon a39n0s1
08 6
Gozzoocc wwom waoonn 555533
Gazmocc mwoonn saos 508577
oomooc waomn ewoow 1m
oommooicc wsmmn _3_9sn0se1n 268
STANDARDDEAVVIEARTAIGOEN:: 711730
'NQ = Not Quantifiable (less thanthe concentrationofthe lowest standard (0.1 ng/mL)
LOQ= 10 ppb.
R+epProessseinbtlaeticvoentraemquiensattiwoenrbeynoytolukseodr tooutcearlcsuhlelaltectohmepaovneernatgeofansdamsptlaendaanrdddaesvipaetrioSnp.onsor
CentreAnalytical Laboratoriensc.,
Pa31g0f1e02 GRO%7S
---
Centre Study No: 023.063
`Table XIX. Summary of PFOS for Week 6 Mallard Membrane Samples at 17.6 ppm ai
Sponsor D
EELOoL02266332200099911 EOL2620%0 E EDLU6IL 21002 EE0OLLOO2266332211000032 EOLEI2I005 EEoOLLoO226633221100040
Centre
001100337T3S66 003752 0O1l003m6s020 00110033880004 0103804 _0_1o0l3os8a0o8s
Numseb.er o icDh Gzocp oooidd ooioeo oo ooioeo
EDxturacetion AuDaalytseis zsezn 33ss sae 391 woeln 33ss wwoon 33ss we 3s sImo n3osm STANDARD DEAVVIEARTAIGOEN::
FoAumnadli(pepb) -Fn 36 330170 33096 07 22091 64122
Table XX. Summary of PFOS for Week 6 Mallard Albumen Control
Samples
Sponsor. Centre
m
I"
EELOL02652200909933 O0l1o033TTeess
EOL2620094 EOLOGI20994
0103769 0103769
EEoOLLoO2I32200099955e 00110033733
EoLoes2097s 0103653
EEOOLLO6G3R2200999775 001I0O336T98L3
EoLo26s 20007 ola
* Duplicate Injection
set Number Gaol oowos oooo oooomm ocoool oom
Ecracton Amis Date Date 01 moni mzlm s 0 O smoi 3s282O900 vmonn s328a29o01 0 wn 3 329m00 soo ass STANDARDDEVAIVAETRIAOGNE::
Awalyte Found (op)
Ne NNQQ NNQo NNoo NNeo No NNGG
NQ = Not Qunifiable (less than the concentrationofthe lowest standard (0.1 ng/mL) LOQ=10ppb
Centre Analytical Laboratories, Inc.
Page 320f 102
GROZ YG
_
Centre Study No: 023-063
`Table XXI. SummaryofPFOSfor Week 6 Mallard Albumen Samples at 6.2 ppm ai
Sposor
Ceatre
mn
D
EOLO632007 0103709
EOLO6320979 0103709
EOL26321000 0103797
E0LO263210000 0103797
EDLO26320988 0103745
EOLO26320988 0103745
EOLD6R2ST 0103677
E0LO26320971 010367)
EOL26320989 0103749
E0L0263209850 0103749
set Extraction Analyses Number Date Date 0208 3201 3282900 ol 30 3282910 om sam 008 3201 3282900 ool 201 3282001 0327018 amon ase 02708 amo ans2em O20 a0 sam 0708 amon ans2em0 008 am mse
AVERAGE: STANDARD DEVIATION:
Asalyte __Found (ppb)
58 62 192 804 636 625 10 681 sm 83 7.15 0987
`Table XXII. SummaryofPFOS for Week 6 Mallard Albumen Samples at 17.6 ppm ai
`Spowsor mn
EE0OLL0O226632302909911 EOL06320990 E0LO263209900 EOLD632002 EEO0LLO266232211000023 EDLO632I003* EE0OLL0O226633221100008+ * Duplicate Infection
Centre n
00110033775577 010353 0103753 0103801 00110033880015 0103805 00110033880099
set Number ool 0B ool oom oo oozzoo oo ool oO
Extraction Analyss Amite
Date Date Found(ppb)
aml sasasml 253
U0 Ies2901 | 249
201 3282900 11
aon 3ns20m0 17
20 382900 197
waneol 3308822000000 21964
al smn 31 3282901
240 191
301 3nsaom 172
AVERAGE: 202
STANDARDDEVIATION: 412
LOQ=10ppb
CentreAnalyticalLaboratories,Inc.
Page 330f102
GROR TY
----
Centre Study No. 023-063
`Table XXIIL Summary of PFOS for Week 6 Mallard Yolk Control
Samples
`Sponsor
Centre n
EOL620%95 0l0vTer
E EOLOL 26320E994
Ol03TE 0103766
EEOOLL00266332200999945
0103766 0IO3TIO
EEOOLL2O6236.322009997550
0103TI0 0103690
EOLO63209750 0103650
EEO0LLQO663I22000909770
010378 0103778
set Number oot ozolA oziolA ool ooooll ozo ozoiA ool ool
Extraction Analysls Analyte
Date Date Found (pb)
el wen
aso! esol
No No
wel aon
aol seen
No NQ
aeoonn eessoo NNog
ao we
esol nso!
No No
oon ower
son nwo
NQ NO
AVERAGE: NQ
STANDARD DEVIATION: ~~ NQ
`Table XXIV. Summary of PFOS for Week 6 Mallard Yolk Samples at 6.2 ppm ai
`Sponsor
EEOOLLM066332200997799 EEOOLLOO266I3Z21I0000010 EE OLO6L320E 9880 EEDOLLOQ2E6332200997711 EE0OLL0026633.2200998899 * Duplicate Injection
Centre
0103706 0103706 010379 0103794 0l03%4 001100373462 0103674 0103746 0103746
set Nomber IAD o0200ADD o201AD oD oooopd 00D 001A o0AD
Extraction Analysls
Date Date
san 301
3901 32900
301 mon
390L 391
mon mon
3mL 32901
dol 30L
3901 39L
32701 3mm0L
3291 309ml
AVERAGE:
STANDARD DEVIATION:
Analyte Found (pb)
16100 15700 9860 10400 11200 1160860000 16900 200 26600 16100 6330
'NQ = Not Quantifiable (less than the concentration of the lowest standard (0.1 ng/mL) LOQ= 10 ppb
CentreAnalyticalLaboratories,Inc.
Pa34gof1e02 [De]
--
Centre Study No. 023.063
Table XV. Summaryof PFOS for Week 6 Mallard Yolk Samples at 17.6 ppm ai
SponDsor CenDtre BTiomsea 0O03Os EBLloeeaae0r OOOFSS EBlmaiiln oolwoewsss EBLmee20l0 oOlIs03:E LEBellnmoes o010w30s6
MeSmaber GTzOoAaDp GROOIAADD OoWNO0IIAADD GGzroosAp> owwriooiadD
ExDnatceon ADmuiiss FoAumdiGep aammnl wweell a41o0 Z32O0 WSIELR 660 OONLL Sp0L1 SSITSOO mmeml wweel 66100 omnm mwsmm d46o6e0 STANDARD DeEVIAaTIOeN: s857o0
Table XXVI. Summaryof PFOS in Quail Membrane Blanks
Sponsor m
Cente D
MeSmaber BxDcatteon ADmueb FoAumdi(eph)
Bm oOmssOBuS kAAr mOmEOIoA S9m W361L00 NNQo
WTMm coooMssoBlsnkA oOmNoGnDsBRR 3300001 442a0m0 Nxo
STANDARD DEAVVIEARTAIGOEN:: ~~ NNQO
Table XXVIIL Summaryof PFOS in Quail Albumen Blanks
Spioynsor Wmm mLE)
Cenntre oSoowTeGsBBuRkmAAT o00w0v37o9s6mBwlawnkAAr
Dulce icion
NuSmbter OOEDBIB 0o33m00e1n4
DaDnucein ADmateb 38208I0 30000010 y33o00m1 AaVanEnoRonAGE STANDARDDEVIATION:
FoAunmdioept) xNoo NNNoQQ NQ
NQ = Not Quantifiable (less than the concentrationofthe lowest standard (0.1 ng/mL))
LOQ= 10 ppb.
Cente Analytical Laborateris, Ic.
Page 3501102
C0709
_-_
Centre Study No: 023-063
`Table XXVIIL Summaryof PFOS in Quail Yolk Blanks
`Sponsor Cenmtre
NuSmbter ExtDraactteion ADmaties FoAunnadlyt(pept)
- COOITOSBlakA| O3280IA 32801 33001 i)
mo OONSSBlmkA* OIA EOI 33001 No
om 003795BimkA O90 32901 AWOL ND
ms ONMGSBnkA* 030008 3901 3BL410L ND
AVERAGE: NQ
STANDARDDEVIATION: NQ
`Table XXIX. Summaryof PFOS Recoveries in Quail Membrane
Sponsor Centre Set Extraction Analyse Amt
%
Nomber Date Date Added (ppb) Recovery
wm OTBSRKA GR0IA 32901 36100
10
102
mo OOIESpkA OR0IA 32901 IBID
10
106
no ONNSESGKB ON0IA 32901 30IDL 986
8
mo 00NOESKBe ORSIA 32901 3BIDL 96
8
ma ONIESkA OBOIBR 33001 4200
10
14
m O0NESpkA OBOOIBR 35001 4201
10
16
m OOISESKB O300IB 35001 4201 9%
108
ma O0IOESkBe 03018 33001 anol
9
101
AVERAGE: 102
STANDARDDEVIATION: 11
RELATIVESTANDARDDEVIATION: 11
* Duplicate Infection
NQ = Not Quantifiable (ess than the concentrationofthe lowest standard (0.1 ng/mL)) ND = No peak detected. LOQ= 10 ppb
CentreAnalyticalLaboratories,Inc.
Page 3606102
CRO7.80
_--
Centre Study No: 023-063
`Table XXX. SummaryofPFOS Recoveries in Quail Albumen
`Sponsor m hs m m na mo mo mo m
Centre n
Set Extraction Analyse Number Date Date
Amt Added (ppb)
% Recovery
OOIO6SPKA 02801 32801 33001
10
O06SpkA ORMIB 30801 33001
10
ONISpkB ORMIB 30801 33001 9963
0
OOI6SHkBe O2M0IB 280 35001 9963
8
ONSSKA 030A 3800 411
10
2
OOI6SKA ON0OIA 330OL LOL
10
8
OONUESHKB O00IA A001 41
%
9
o0msespkBe ON00A 300i ion 9%
9
AVERAGE: 85
RELATIVSETSTAANNDDAARRDDDDEEVVIIAATTIIOONN::
~~
6
`Table XXXI. Summary of PFOS Recoveries in Quail Yolk
Sponsor D
Centre D
Set Extraction Analyse Number _ Date Date
Amt Added (ppb)
Recovery
me mo
ONIOSSpA ONGSSpkAS
ORMIA ORMIA
32801 30801
35001 35001
10 10
102 104
mo OOSSSKB ORMIA 30801 33001 9623
9%
m OOISSKBe ORMIA 32801 38001 9623
101
Mm OOIISSpA ONSOIB 3901 IBL4IOL 10
"
Mm OOISSkA ONSOIB 3901 IAAL 10
Mm OOMSSSpKB ONSOID ISmI 4200 omen
04
m o0NSSSKBe ONSOID nomi nam oss
9
AVERAGE: 96
RELATIVSESTTAANNDDAARRDDDDEEVVIIAATTIIOONN::
7 7
* Duplicate Injection
L0Q=10ppb
Centre Analytical Laboratories, Inc
Page 37 of 102
G0z5L
-----
Centre Study No.: 023063
`Table XXXII Summaryof PFOS for Week 1 Quail Membrane Control
Samples Sponsor Centre
se
Bxraction Aualyls Asaire
I"
"3 Number
Tormsezoe| O09m| ORS0IA
Due 31
Date Found (ppb) anil S20
EEO0LLo02sSo92-02s005067e O010I19F91 oONSmOIaA o39mmL A3W0 sNso
EEOLLoOsS5O2200S2007 0012010961 OoNSoOIlA o3o9MIBuNl Nxoo
EELoLsopa2ss0a2os0 OOI0GG ORORSSOOIIAA d39v0b1 3WBOII xxoo
EEoOLLmossssz2o0nsise 0O0l10%g OON0SIOAA 3a9m0l1 3AI0L NNoo
Eolmsoason oli Guo wom AaVEiRoAGE: NNoQ
STANDARD DEVIATION: NQ
Table XXXIIL SummaryofPFOS for Week 1 Quail Membrane Samples at 6.2 ppm ai
`SIp'oSnsor B T0 oa 6 EEoolloosassszao0ssiieer EEool0L2ss99:2200552277% EEooLloassssazoossilsse EoOrLoO2NssSa200s22E Se + Duplicte nection
Centre oOlwo0ee O0000199 00110022007711 0o0l2a3 O010O20S78
NSuemtber EDxtartacetion AnDaalytseis FoAunnadly(tpped) GHEOOIDD SS0N1L l4aaum 1m800 OONRSSOIIAA 3D9I0 3WBIWOLL 21 oomoal swoon uwom 1re6 OGNSOOAIA 939b01 W301L00 m1mn OcNuSOsIpD 3s9mmn eannooln ln1sso0oer
STANDa ARD DEVIw ATION: e w25w3
INQ = Not Quantifiable (less than the concentration of the lowest standard (0.1 ng/mL)
L0Q= 10 ppb w+asPonsostibwlaeschoendtaprmiionrattoiosnepbayraytoiloknoorfoiuntteerrnsahlelclomcpoomnpeonntesn.tAofsspaemrpSlpeosnisnocre outer shell `dReeviparteisoenn.tative request these values were not used to calculate the average and standard
wFoarsruesseidduteoscraelccoulradteedtahseNaQve,rhagaefaonfdtshetacnodnacredntdreavitaitoinono.f the lowest standard (0.5 ppb)
CentreAnalyticalLaboratories, Inc.
Page3801102
CROAT
Centre Study No.: 023-063
Table XXXIV. Summary of PFOS for Week 1 Quail Membrane Samples at 17.6 ppm ai
Sponsor Ceure
n
Eolas OI
EELlmSsI O00S79
BOLOSOZ0SH OI0ET
EElLsmss 0ol9s
EEiLmmssowossiisss oolamss
BEoOLLOOsSSo0zS0Ss3e OOSloS5s
Sa Exmcn Amis Amie Number Date Due Fou gph) 00D 01 4na0n 2000 o0NoSIdD u0s1o annaaom 21100k000 ORSOD W901 4n2ml 11100 0G0ODD uwsoon aannnai 113%0000 oonmooD aOs0o1 a1n0o0n 1122560000 o03nSOsD w9o0m1 a4nn2amml 90%
STANDARD DEAVVIEARTAIGOEN:: 143113000
Table XXXV. Summary ofPFOS for Week 1 Quail Albumen Control Samples
n `Sponsor
CenI"t)re
EEmosIwGoassot0sse| OOI0OI8SE
BEoOLLoOaSsOs2a00550077 OOllOII%S22
E EOLm OSS2s00 Oo2s0
EEOBLoOiSms0oSn2iC oOwnIs
ELH 0
ELSooo
Duplicate nection
NSuemtb.er O0N0SIIBB OGR:EsOOIIBB Oo0sBo ooosm 0B Guan
ExtrDaactteion AnaDlaytseis FoAunsadlygtpeh) 33220810 3360000000 NNoo a38s0m1 3300aH Nxoo 3o8w0 336000010 xNoo azsaol 3350000000 NNoo 3240 35000 No vom sm NO STANDARDDEAVVIEARTAIGOEN:: ~~ NNoQ
N10QQ==N1o0tpQpuabntifiable (less than the concentration of the lowest standard (0.1 ng/mL))
CentreAnalyticalLaboratories, Inc.
Pa 39g of1e 02
6007.4
------------------------------------
Cente Study No. 023.063
`Table XXXVI. Summary of PFOS for Week 1 Quail Albumen Samples at 6.2 ppmai
Spoor
Care
NeSmiber
ETorlmsmomose | OOWpIs OORSBIB
RBoollsooaossilee OOlalm0 OOMmSsOIBB
EEllmss oolia OONRSRIIBB
FEoollgmsosaasoislsse oOlogams OORMSSIIBB
EBooimlsoaosss Oolwass OommssoIlBn
A
BxmDcuiion ADmaites FoAunmdipeb) IEZDwLo 3A00I3MdL 6S6A R3208011 3A033M0 22748 SJOawLO M0I0N3Im 23944 E300011 3A0003310 S68018 wpuloi 53R0033uomL_ 999397% STANDARDDEeVIAeTIOsN: a16w1
Table XXXVIL SummaryofPFOS for Week 1 Quail Albumen Samples at 17.6 ppm ai
SpIon"sor CeIn"t)re NuSmtber PToerlmoas oOllase) oOwwSsOoIlB FToolrmmssooaa0ssssiie oOlscosss oonwss BBoolmmssooasoise oOlacs oonwsosB PToorlmaso0ssisi oowllls oORMn0IsB EBoorlmmssoaooosssss Ooloams oowsolIsB A Duplicate nection
EDxmuceion ADmupes FouAnmdi(eap) JSaOwL dA000a3iMdLl 111739 mpsli 3A0033m0l 91507S apsaoo o30a30n1 110170 aROoL 360330L 2Si3S w3%eR0lL ao0o0di3o0i_L_ 9100)d STANDARv DDEVeIATIeON: 168302
1L0Q=10ppb
CenteAnalytical Laboratoriensc.,
Page400 102
007
-
CentreStudy No. 023.063
Table XXXVIIL SummaryofPFOS for Week 1 Quail Yolk Control Samples
SponIsor Contre
ToLmsoas0s | 0I0I98S
EEorLsos0ss0s lool0iissE
EEoLlomasssHa00ss0r0e oOIl0ISsEY
EoLOsp205200 EOLOSS021
001l002200441S
EEoLosasssaoesze 00il0012909d7S
EoLoso 0505 otoissn
NuSmeber EDxaitmceton mGassollA wsoanw ocsaosloa wdaemonn oooss00llaa ssoammoo oomosoll nawwoe oomss0lnamaaweol
ADmuies 33000000 330000001 3300000011 330000011 3o3o00n0 AVERAGE:
STANDARD DEVIATION:
FoAunndatapet) NNoo NNoe NNoo NNoo NNoo NO
Ne
Table XXXIX. SummaryofPFOS for Week 1 Quail Yolk Samples at 6.2
ppmai
Sponsor
Centre
Boiss EOLOSO0S26*
0O1l02a06s5
EBooLLoO2aSssSas0I5el4* 001l002200177
Es EOLOSO20527%
0o10l20e69
BEomLsmssoiossiss ooloaa!
EBooLmLsso0ossasse oolloorr
* Duplicate nction
St Nomber
Extraction Due
Amys Date
ToosnIAsD ewsoorl WwoeLl
oomus00iAADD mmo0l 3O0L
oouz0oAADD ams0oL aWmOon
GcozsoiiapD oassoor 3w8o10n0
coos0olADopassoi ssuwo
AVERAGE:
STANDARD DEVIATION:
FoAunudb(epb) 17500 185s300 112010 113230000 113080 11206000 3150
L'O=QN=N1Q o0tpQpuabntifiable (less thantheconcentrationofthe lowest standard (0.1 ng/mL))
Centre Analytical Laboratories, Ic.
Page lof 102 6075
eee EEE eee
Centre Study No: 023-063
Table XL. SummaryofPFOS
ppm ai
`Sponsor
Centre
D
I"
E0LO2s920525 0102077
EEOOLLOO22SSSO22050391
0102077 010208S
EEO0LLOOSSOO2200SS3R12*
010208S 0102089
EEODlL22sso0.220055182
0102089 0102033
EEOOLLOO2SSOS2200SS3138
0102033 0102083
EOLO2s9205330 0102093
for Week set Number 2801AD 028010 o2AD ons0iAD os0AD oA onsoiAD ona ons0IAD oti
1 Quail Yolk Samples at 17.6
Extraction Amalyss
Date Date
32801 38101
3om01 3am
38101 3BI0L
3zam 3om01
Imo 3BIOL
osm samo
38100 3nwoL
3as0L 32801
3BwOL 3BW0L
nso wo
STANDARDDEAVVIEARTAIGOEN::
Analyte Found (ppb)
2500 41200 3200 3100 37400 3890 38100 38300 a0 B60 38700 4130
`Table XLI Summary of PFOS for Week 6 Quail Membrane Control
Samples
Sponsor
Centre
D
n
EEDoLLOoS2Oso220077I3Sse
0102903 0102903
EEDOLLO2SSO2027T3I6E
0102907 0102907
EEOOLLOSSSO220077T7Y
0l09L1 002911
EEO0LLOOS2OS2200T200C
0102843 0102843
EEO0LLOO22SSSO2200773388
0102915 0102915
* Duplicate Injection
set Number Osos ool oso ooo ons 030018 0330018 oooso o0B
Extraction Date
AuDaaltyess
FoAunnadly(taep)
Aol eo aol a2
NO NQ
won soo
4200 az;
ossee 93
soon aor
anon ann
156m 164ve
wool ano 21800
oeool aannoir 2s4e40e0
wo
AVaEnRoAlGE:
6300 NQ
STANDARDDEVIATION: ~~ NQ
NQ= Not Quantifisble (less than the concentrationofthe lowest standard (0.1 ng/mL) LOQ= 10 ppb
*+ Possible contamination by yolkorouter shell componentof sample since outer shell Rweapsrensoetnwtaatsihveedrperqiuoersttothseespearvaatliuoensowfeirnetenmoatlucsoemdptoonceanltcsu.latAestpheeravSeproangseoarnd standard deviation.
CentreAnalytical Laboratories, Inc.
Page 420f102
GONZL
-
Cre Study Nos 023063
`Table XLIL Summary of PFOS for Week 6 Quail Membrane Samples at 62 ppmai
n Tosa
I" os
BBrlaossssoammse 00100933s
LBoolosasssaemess oOiSs
BBLooslsasonsas O010S29H43
EBoroaslsasease 00100994473
Lose ose
GNoamobenr 0Du0e 4D2a0te0 Fowd12a0pt)
Goaoomn owoooll 440200 2913
GGaaoonn nnoomo 4422000 208
moooomn 0wo0o aea0m 1106
Goaoomn wooool a4m2 oom noo ean
114s 14
STANDARDDEAVIVAETRIAOGNE: 31894
Table XLIIL. Summaryof PFOS for Week 6 Quail Membrane Samples at 17.6 ppm ai
Sponnsor Cire MeSmber BuDnuieon ADmaties FoAwmdioept)
BBoirsoassooanm oOlsast) oioseas olomsss
TGxoomD> 300001 442a0n0i CAOBD lool 4201
w3s8 as
BEoswsead oomssss Bossa Ooms
OGRNOONBBDD 0so0l 44220000 GHOED 300i 4a
4a"n
EBolLoossosoorsmosr O01I0zsEen Bolasoarsi 00967
oonoom wnoooo 4a0o0 mo 00 40
p25s0 186
A Eovopsoanrsie__oiazser ooo STvAiNvDoARDDEeVIaAeoTeIOsN: 81a65m56
+ Duplcecion
LOQ=10ppb.
CentreAnalyticalLaboratories, nc.
Paged3of 102 Ga0zE?
-
Centre Study No.: 023-063
Table XLIV. SummaryofPFOS for Week 6 Quail Albumen Control
Samples
`Sponnsor
CenDtre
BEooLol2sm5s20T73s5 0011002290088
EEOoLLOOSSs2o0270I66 00110022590088
B BoLlsTa o0s1i2z
E ElmLsaT mo oollss
EEnlmmsmss 0o9sise
NSuemtber EDxturacetion AnDaluyesis FoAuvnadlygtpeh) o0xoAA awsoouo aanioorn xNoo mGiooiaa w0o0o aannoonn Nxoo oGuooloaa wwoooo aanm Nxoo ooxoollA 0000011 aanoo NNoo oooollA n0o0o1 aannoon NNoo
STANDARDDEVAIVAETRIAOGNE:: ~~ NNQQ
`Table XLV. SummaryofPFOS for Week 6 Quail Albumen Samples at 62 ppmai
Spoor Cenre
Su Exmcion Amis Amiyie
B Tomson on NGeObArD D30a00 D4a10w1 FewEdnpy
sE olosr a0Taz RloTs moaooloA o0o0r aanooln 651995
BBOoLlOSmOs20TMsA 0o10l29s40 oGoolla 0do0m 4an1o0n o69n1
B BoimLsmaM ons o01i04e0 oooon wdoomo aannoo 5826
EEDOLLOO2SSSO2T0ATSSS 0O1l0O2R9S4as8 oovoo d36o00o1 aaiimo 3s3i6s
Foss oioasas oon nwo AVwEoRrAGE: 5e6y3
* Duplicate nection
STANDARDDEVIATION: 112
'NQ = Not Quantifiabe (ess than the concentration of the lowest standard (0.1 ng/L) L0Q=10ppb
Cente Analyical Laboratories nc.
Page dd of 102
C0788
Centre Study No.: 023-063
`Table XLVI. SummaryofPFOS
17.6 ppm ai
Spomor
Centre
I'S
I'S
EEoLLoo22ss5o2200778477 0o1l0o229s5s22
EOLOSO20T 0102956
EEOOLLO2OSSOS22070448 00110022996506
EOLOSO2074S 0102960
EEO0LLO22sSS9220075500 00110022996644
EE0oLOL22SsO2o027051n%s_L__ 00110022996688
for Week6 Quail Albumen Samples at Su Extraction Asalyds Awayte Number Date Date Found (ph)
GcOoLlAa 3o0o00l1 4a1n0o1n o58s1 cola wool anol 152 GcoOlAa 0so0l aaiioo 11416 cola wool an 12 ccoollaa o0o0l awioon 116637 G0olAa 0so0m waoon 115564
STANDARD DEAVVIEARTAIGOEN:: 214349
Table XLVIL Summaryof PFOS for Week 6 Quail Yolk Control
Samples
SIpon"sor Centre EooLaO2sso2e07s3s 00110022990011 E0L2so2076 0102905 EE0OLLOO2SSOO220077SST6 00110022990095 EEOoLLOoS2Ss2s0oT0SmT0S 0o1l0o2z5s0al9 EBOLoOSlO2s0a70 00110022894113 EOLO2SS20738 _oloos13 * Duplicate nection
NuSmtber EDxtartacetion ADmaties__ FoAuwnadiy(tpepb)
O0s0o8s ssooln awisaiwmal NNQO
oo son wlawml NO
0onsBolB osoonl BwAaLl SisNQ
0o0o8p ssoonn aailawanml SNuios
Oo0w8s ssmmnn awilawaoml NNQD
on%0B
sm
aAVlEuRmAGiE:
ND NQ
STANDARD DEVIATION: NQ
NQ = Not Quantifiabe (less than the concentrationofthe lowest standard (0.1 ng/mL) ND = No peak detected L0Q= 10 ppb
`+w*aPsohsesdipbrlieorcoontsaempianraattiioonn obfyionutteemraslheclolmcpoomnpenotnse.ntAosfpsearmSpploenssionrceRoepurteesresnhtealtlivwea.s not request these values were not used to calculate the average and standard deviation.
entreAnalytical LaboratoriIensc.,
Padsgof1e02
0007.59
_----
Centre Study No. 023063
`Table XLVITL. Summary ofPFOS for Week 6 Quail Yolk Samples at 62 ppmai
Sponsor Centre
m
I'S
BBLoOOmTMe 001020929
EBmolaon ooloems
BEoOLLoOsNszO00u7eMr 00110022993377
EEDLO0LOTSAO0S%SS 001l002z994H1L
EEO0LO0NS9O046 o01100a2s9a6s5
Se Number oGoon
sosoonD
oosoopD ooownn oooon
Exacton Assis Date Date ave wiami uwsoem wsaam
ange anam
awmol ew2i0m0 nsoom me2a0m0 nooomm awonma STANDARDDEAVVIEARTAIGOEN::
Amine Found Gp)
390, s3s0o
3610"
2ne6o0 ssooosno,' aosseeoon.r 37161000
Table IL. Summaryof PFOS for Week 6 Quail Yolk Samples at 17.6
ppm ai
Sponsor
n Centre.
BBooosao 0o10l29e89
B Eo ss m oolsss
BEoslpomrsus ooulmss7
EEOiLmGsSmSwTrSs0oT Oollom2sse6ll
EBomLsosoa7ssiis_ o0ula0onssess
+ Duplicte nection
NSuemtb.er ExtDraatcteion AnaDleyiseis. FoAunnadlyt(epb) oTsooni noonmri naonoano ssswo 0am0oDn 0 nom Mwo2o0l eeses oGoonD woonmi n4a2m0 ddsesooo) ocmoonn nwoowm awonm aesesen, oooonp nnoomm nwoamm ssmenm
STANDARD DEAVVIEARTAIGOEN:: 566551000
NQ= Not Quantifiable (less thantheconcentrationofthe loweststandard (0.1 ng/mL))
CentreAnalyticalLaboratories, Inc.
Pad6gof1e02
Co0ran
Centre Sudy Nos: 023-063
Table L. Summary of Moisture DeterminationsforMallard Membrane Samples
Sponsor D
E0EL001206236.52200885532 EE00L1G22s6332200884524 EoEL0c12062633..2200882453 EEOOLL0226633.2200884362
E01 026320047 EOB0OLL00226633..2200084586 EBOoL 0226633.2200885570 EEO0L10206236.32.200885518 EO10263.20093 EE0O11..00226633..2200009954 EEO01102062633..2200907957 EBO1o0l26s3a.2201007019 EE0oLL02266332200557818 EEooLr206a3623020958991 E0EL00L2c6236.32201009002 E0E012c82633.2211000034
Centre m
00110033220004 oot0033126008 oomsiess 0ow731620 ow1s0 owo2ni16 oo0w3s2i2s0z o0mn o03764 oou0s37m6s oowse0 o0u03s96 0ou003364746 oorlousnss o01w0m38s020 oo1100m3ss0084
Aversge Motsture wsso0 70500 1000 71500 0 w75o0 s8a500 885500 50 0in0 000 0750 0750 0500 00 7050
CentreAnalyticalLaboratories, nc.
Paged7of 102 R07
Centre Study No.: 023-063
Table LL. Summaryof Moisture Determinations for Mallard Albumen Samples
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Centre Study No.: 023-063
`Table LIIL Summary of Moisture Determinations for Quail Membrane Samples
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CentreStudy No.: 023-063
APPENDIX A
Study Protocol
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Amendments and Deviations
Centre Analytical Labortris Ic.
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irirte pmsoeoyi.Ciose.ili fy edoS 16 REFERENCES
1 Uo S. EvinPrPi irSonaAsg,ryF.tToor seeS 4CERt FoClo3m5eeAct(s TSCA).
Cote inLiar. Centre AnsytcalLaborsores,Inc.
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