Document km4JY4LOdZ37a1qodZaRyDB3n
Northwest Biossalyt0ial 226-172 9
ReSgtoryt NNoo,,NNWWBBRS0O0L..009615
Quantitative Determination of PFOS and Related Compounds in Human Serum and Plasma by LC/MS/MS
Sample Analysis Report for Protocol EPL0012
NortAhwDeisvtisBiioonanoaflNytWicTalI(ncN.WB)
Sal1t12L1akEeasCtit3y9,00UTSo8u4t1h24
PREPARED FOR:
3M Company
Epidemiology, Medical Department
2203W-05 StPaul, MN 55144
2=
EEZR on
= ue
2
AUTHOR: Oinie J Dbl Connie O. Sakashita, B.S,NW Project Manager
APPROVED FOR RELEASE BY:
eS
RbligeLr. Foltz, Ph. NWBTechnDiircecatolr
DATE: 41-20-07
DATE: 1-21-41
Paget
Northwest Bioanalytical
QUALITY ASSURANCE STATEMENT
Study No. NWBS00-091 Report No. NWBRO1-065
LABORATORY:
ANorDitvhiwseisotnBoifoaNnWalTytIincca.l (NWB) S1a1l2t1LaEaksetC3i9ty0,0USTout84h124.
SPONSOR:
3EpMidCeomimoplaongyy, Medical Department 220.3W.05 St. Paul, MN 55144
COMPOUNDS):
PFOS and Related Compounds
NWBSTUDYNUMBER: NWBS00.091
SPONSOR STUDYNUMBER: EPL0012
NWB STUDY TITLE:
``CQouamnptoituantdivseiDneHtuermmainnaSteiornuomfaP ndPlFaasnmdO aRbeylaSLteCdMS/MS
r"Tehgeulcaltienidcnalosnctluidnyidceaslcsrtiubdey.diHnotwiesvreerp,oNrtoirstnhowteisntcBliuodaenadlwyittihcianltchoenddeufcitnsitalilonsotufdiaesGwLiPthin the gSutiuddeileisn(eTsoitfeth2e1 UC.FSR.FPDarAtG5o8)o,dtheLaObEorCaDtoPrryiPnrcaicptliecsoe fRGegouoladtiLoanbsorfaortoNroyncPlriancitciacle aLanbdotrhae.tory JStaupdaineesseonMtHheWSaGfeotoyodfLaDbrourgasto(rOyrPdriancatniccee NSot.an2d1a,rdPAOrBdiNnoatinfciecfaotrioNnoNnoc.lin4i24c.a)l LTahbeorfaotlolroywing inspwereepecrfotrmeidbyothenNWsB QAUperSOP.
Inspection and Reporting Statement. DoafIntspece tion PhoafSstuedy
Date Report Sento Date Report Sent to NWBProject Manager NWBManagemen
1167-O2c3t02c0t020000 An`aSlaymtpilceaAlnPallyasnis
214600661122000000
2239ONcotv-200011Nov2001
FiRnaleReDprap ofrttanod Rr awDtata
01Nov2001 23 Now 2001
310612000 3031N0ocvt22000011 30Nov2001
*Reparts to NWB Management ae issued monthly.
Ainscocrapnorraetaesdonianbtloythbies efsitnaalblriesphoerdt,atchceumraettehloydrsefalnecdtptrhoecerdauwrdeastad.escribed and the results
5N3W%B) LQyfnuality AsChsainu, raBnAc.e Compliance Auditor
Dat(e 23-20 (
Page2
Sones ssid
ReSpouu NNoe. NWEERDSY0T65
COMPLIANCE STATEMENT
"The clinical study des
regulated nonclinical
cribed
study.
in this report
However, to
is not included within
the bestofour knowle
the definition
dge, this proje
ofa GLP
ct was.
RceognudluacttieodnisnfaorccNoorndcalnicneicwailtLhatbhoeragutiodreylSitnuedsoifest(hTeitUl.eS.21FCDFARGPoarotd5L8a)baonrdataocrcyoPrrdaicntgicteo
the metanhdprooceddurses described within this report. In addition, the study followed.
the guidelines ofthe OECD Principles ofGood Laboratory Practice and theJapanese
'MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies
on the SafetyofDrugs (Ordinance No. 21, PAB Notification No. 424)
`This report contains serum sample results. As reported in NWB report NWBR00-122 [5.3], serum sample results obtained using plasma curves for PFOSA, PFOSAA, POAA,
PFHS, M556 and M570 did not meet NWB SOP requirements for validation.
raw data. Anyknowncircumstancesthatmay have affectedthequalityor integrityoftheprojector
`reporteddataare discussedwithin thereport.Thisreportrepresentsan accuraterecordof
loinc 0 udoaril CNoWnnBiePrOo.jeScatkaMsahniatag,eBr.S.
! 7 F<
er L. Foltz, Ph.D. NWB Technical Director
sr20-0/
Date
[1-21-0)
Date.
rages
Norihwest Bioanalytical
TABLE OF CONTENTS
ReSptourdtyNNoo.. NNWWBBRSO010-009615
SIGNATURE PAGE sss |
QUALITY ASSURANCE STATEMERT commons 2
COMPLIANCE STATEMENT css:
TABLE OFCONTENTS comms
LI OFTS ABLT ES .......
rn
LOIRESIT B wassnmmansmsmmsnsmmmsmsmmsmsmmessamnsnd
br DTORODUCTION mmm
8
2. METHODOLOGY.
:
rnd
3. SAMPLEANALYSIS o.oo 12
4. PEBOLIE SD DISCUSSION mmission 18
5. REFERENCES. --
S--3
6. DATARETENTION .....ocomsrmsmsmsssmmsssssssmsmssssmmsssssssssssssassnn 16
LIST OF TABLES
`Table 1. Calibration CUrVe SUIIFMOFAPTFOYS vrei 1
Table 2. CaliCurbverSWMaMAtTYiOron PFOA.
18
Tabl3e. CaliCUbVerSUMaMAtYfiOrPoEHnS .......c.cvvvvorvenrssninsrenen 19
`Table 4. Calibration Curve SUMfMorPAROrSAYA....cvvsvrsvosssssssssesen: 20
Table 5. Calibration Curve Summary for PFOSA
2
`Table 6. Calibration CUrve SUMIMOrAMTSSY6 verses 2.
Table 7. CaliCurbverSUaRAtT fioron MS70.....c.evcvornsnerisens 23
`Table 8. Back-Calculated ConcentrationsofCalibration StandfoarrPdFOsS....vuvor 24
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Table 9. Back-Calculated ConcentrationsofCalibration Standards for PFOA... 25
Table 10. Back-Calculated Concentrationsof Calibration Standardsfor PFHS vv: 26
Table 11. Back-Calculated ConcentrationsofCalibration Standards for PROSAA........... 27
Table 12. Back-Calculated ConcentrationsofCalibration Standards for PFOSA..............28
Table 13. Back-Calculated ConcentrationsofCalibration Standards for MSS6.
29
Table 14.Back-Calculated ConcentrationsofCalibration StanfdoarMr7d0.s..
31
Table 15. AnaQlCSyUmMtAIiYfocr al POS...
3
Table 16. AnalQCySumtmairycforal PFOA..
mm
J2
----
`Table 18. AnalQyCtSuimmcarayflorPFOSAA.
smmsm--30
Table 19. AnaQlCSyumtmariyfcorPaEOlSA
vos
37
Table 20. AnalyQCtSiUcMMaAlY fOr MSS...
38.
Table21. AnalyQCtSiumcmaarly for M570...
39
Table 22. Serum Study Sample CONCENTAONS.........vcrrevrvrsrssesrnssrne 40
Table 23. Plasma Study Sample CONGENTBHONS vv
"
48
Table 24. RepeatAnalysis Teble for PFinOUMSD SEQUIM...
55
Table 25.RepeatAnalysis Table forPFinOHumAan Serum...
wn BS
Table 26. RepeatAnalysisTable for PFinHHumSan SEQUIM...
56
Table 27.RepeatAnalysisTable for PEOSAA in HUMAN SEM...
56
Table 28.RepeatAnalysisTable for PFOSA in Human Serum
mss)
Table 29.Repeat AnalysisTable for MSinSHUM6aD SERUM crv
ST
`Table 30.RepeatAnalysisTable for M570 in Human Serum
msm
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LIST OF FIGURES
cI
--
59
Figure 2. Representative Calibration Curve or PFOA ..vvuvunonresnnssnssnnson: 59
Figure 3. Representative CalibrationCUFVe for PFS...
60
Figure 4. Representative Calibration Curve for PFOSAA cc.
A.
Figure5. Representative Calibration Curve for PEOSA cvs 61
Figure 6. Representative CalibrationCurve for MSS6.....c.uvccrnsasernsnne 6
Figure 7. Representative CalibrationCurve for MS70.......c..
mmmm---_%
Figur8e. Human PlasmaBlank for PFOS
--------
6
Figur9e. Human PlBa lanksformPFOaA .............
sm--
Figure 10. Human PlasmaBIank for PFHS ......ccccccounorarons
sens
Figure 11. Human PlasmaBlank for PFOSAA. ..
mmmmmm----"
Figure 12. Human Plasma BlfoarPRnOSkA..c.c.ccvvvv
67
Figure 13. Human PlasmaBlankfor MS6....
ARR--
Figure 14. Human Plasma Bankfor MS70 cca
samt
Figure 15. Human Plasma Blank with Interal Standard (QfCor 0PFO)S ccc
10
Figure 16. HumanPlasmaBlank with Internal Standard (QC0)for PFOA ...ccvcrvrenn 71
Figure 17. HumanPlasmaBlank with Internal Standard (QC0) for PFHS c.ccvcrnnnn 12
Figure 18. Human Plesma Blank with Internal Standard (QCO) for PFOSAA. snsennes TS
Figure 19. Human Plasma Blank with Internal Standard (QC0) for PFOSA...ccvccnrer7:4
Figure 20. Human Plasma Blank with Intemal Standard (QC0) for MSS6............. 7
Figure 21. Human PlasmaBlankwith Internal Standard (QC0) for MST0...ccvcrvvvvovvvs 76
Figure 22. Low Standard for PFOS
sm--
wonnsT
Figure 23.LowStanfodraPFrOAd corn
ssn 78
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Figure 24. Low Standardfor PFHS crore
snd
Figure 25. Low Standard for PROSAA revs
--
Figure26. LowStanfodrPaFOrSAd......... FIGUTe 27. LOW SIANAAIA FO S56...
ssnss----_1 82
Figure 28. Low Standard for MS70-........cc... smash
Figure 29. HighStandardfor PFOS.... mns------"--
Figure 30. High Standard for PFOA ...evcurnvosrsrnsssnsn
---
Figure 31. HighStanfdoraPFrHSd ......... ------ smn 36
Figure 32. High StandardforPROSAA wrens
81
Figure 33. High StafnordPRaOSrAd ..c.cccourrnsnrsnssssossssne8:8
Figure 34. High Standard for MSS6 .....ovvurveninscsssnssnsnsssninens 89
Figure 35. High SAAT FOF M570...
%
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Quantitative Determination of PFOS and Related Compounds in Human Serum and Plasma by LC/MS/MS
Sample Analysis Report for Protocol EPI-0012
1. INTRODUCTION "This report summarizes the analytical results from the quaniitationof PFOS, PFOA, PFHS, PFOSAA, PFOSA, M556, and M570 in human serum and plasma samples for 3M `Company (3M) in supportofProtocol EPL0012 [5.1]. The LC/MS/MS method for the analytes has a targeted calibration curve range of 1.00 to 500 ppb (except for M356 which has a LLOQ of 2.50 ppb). The actual calibration curve range for cach analyte varies based upon the persistent levelsofthe analyte in the matrix. For this studs, the assay exhibited the following LLOQ and ULOQ values
APmFiOSte PFOA PEHS PFOSAA PFOSA Mss6 M70
0 3L9l40ppQb 1.92ppb 1.36 ppb 1.60 ppb 1.00 ppb 2.50 ppb 1.00 ppb
u"ao pp 481 ppb 523 ppb 501 ppb 500 ppb 500 ppb 500 ppb
`The sponsor was 3M Company (Epidemiology, Medical Department, 220-3W-05, St. Paul, MN 55144), and the Study Director was Jeffrey H. Mandel, M.D, MP.H. The Study Contact at 3M was Jean Burris. James K. Lundberg was the technical contact at 3M. The following is lst ofNWB supervisory personnel involved in the completion of this work: Connie O, Sakashita, B.S. (NWB Project Manager); Patrick Bennett, M.S., M.B.A. (NWB Laboratory Director); Rodger L. Foltz, Ph.D. (NWB Technical Director). Laboratory personnel involved in the completionofthis study included Suzanne
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Newman, B.S. (NWB Research Scientist); Emily Yardimei, B.S. (NWB Associate Research Scientist).
NWB SOPs and guidelines were used in the conductofthis study and were available to study personnel in electronic and/or hard copy formas.
Date Study Initiated: 24-Sep-2000_ Date Analyses Completed: _07-Apr-2001 `The clinical study described in his report is not included within the definition ofa GLP regulated nonclinical study. However, Northwest Bioanalytical conducts all studies `within the guidelinesofthe U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58), the OECD PrinciplesofGood Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard OrdinanceforNonclinical Laboratory Studies on the Safetyof Drugs (Ordinance No. 21, PAB Notification No. 424). Any changes to or deviations from the original protocol (Analytical Plan) were documented through approved protocol amendments or deviation memos and are retained within the raw data.
2. METHODOLOGY
`The assay used for this study is reported in Northwest Bioanalytical reports NWBRO0108 (5.2)andNWBR00-122 [5.3]. Chinese human plasma was used for the calibration curves and quality control samples. Serum sample results obtained using plasma curves are discussed in NWBROO-122. `Samples for this study were received at NW on the following dates:
Receipt Date
25-Jul-2000 26-Jul-2000
NumberofSamples Received
243 is1
Storage Condition (except during analysis)
20C 20C
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Reference Material
Analyte PFOS. PFOA PHS PFOSAA PFOSA
Lot Number 193 245
SE036 617 214
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Purity Expiration Date _ Source _ 100% 31Dec:2010 3M 100% 31Dec200 3M 911% 0lJan2010 3M 538% 31-Dec200 3M 100% 31-Dec2010 3M
"Stored dry
Storage Conditions Room temperature* Room temperature
20C Room temperature Roomtemperature
Analyte
MSS6 MST0 THPFOS
Lot Number Purity Expiration Date _ Source _ Storage Conditions
NBII3047-8D 99.89% 31-Dec2010 11850626 99.75% 31-Dec-2010
3M Room temperature 3M Roomtemperature
59909 90% 31-Dec2010 3M Room temperature
`The reference material purity for PFOS, PFOSA, PFHS, and PFOA was not available: prior to the conductofths study. Therefore, the reference material purity was assumed to be 100%.
3M contracted with Centre Analytical Laboratories, Inc., in State College, Pennsylvania to determine the absolute concentrationofPFOS, PFOA, and PFHS in NW stock Solutions used to prepare the analytical standards and controls used for this studies. All amangements for purity determinations and the transfer of NWB solutions to Centre: Analytical Laboratories, Inc., were performed by 3M. Based on Centre Analytical Laboratories" results, the concentrationsofplasma calibrator and quality control samples
were corrected using the following factors:
Analyte PFOS PFOA PFHS
Correction Facior 0821 0.961 1.043
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Eight or more calibration standards were prepared on the dayofeach run by adding
100 uLof blank Chinese human plasma and 400kLof 50mM ammonium acetate in water (unadjusted pH ~6.9) to 13 x 100 mm polypropylene tubes. After abriefvortex
`mixing, 10.0 iLofthe appropriate spiking solution was added. The final calibration
standard concentrations in human plasma for each analyte are listed below:
`Analyte
Calibration Standard Concentrations*
PFOS
394,517, 113,23.6, 44.2, 85.4, 209, 332 and 414ppb.
PFOA
192,336, 10.6,25.0,49.0,97.1, 241, 385 and 481 ppb
PFHS
1.36,292,10.7,26.5, 52.6, 104,262, 418and 523 ppb
PFOSAA
1.60,3.10, 10.6,25.6,50.6,101,251, 401and 501 ppb
PFOSA
1.00,2.50, 10.0, 25.0, 50.0, 100, 250, 400 and 500 ppb
M36
2530.,2100,100,.275,205,.75,0.500,.71,001,0215,02,514,004a01ndan5d0050p1ppbp(bu(nrsun1 1-8)17)
Ms70 1.010.,920.,530.,401,0.100,92,5.205,.95,0.500,.91,001,012,502,514,0040a1ndan5d0050p1ppbp(bru(nrsun1 1-8)17)
E*aTchheatnaarlgyettechaalsibradtiifofnerceunrtvfeinraalncguersve1r0a0ngpepbbas(0ed50u0popnbth(eepxecrespitstMenStSl6evwehlsicohfthhaesaanaLlLytOeQnotfh 2h.5u0mpab)n.
pmlaaslmea uscd. Run 18 for MSS6 and MS70 used new pool ofplasma with diferent persis levels of
In addition, blank human plasma samples, both with and without internal standard (designated as QCUs and Blanks, respectively), were assayed in cach analytical run.
Analytical QCs were prepared in Chinese human plasma on October 6, 2000, October 11, 2000, October 27, 2000 and March 8, 2001 and stored in a -20 C freezer. For each run, analytical QC levels were assayed in duplicate.
QC Concentrations (ppb)*
Analyte
Low
Medium
High
PFOS
640
126
332
PFOA
481
145
385
PFHS
448
156
an
PFOSAA
460
151
401
PFOSA
4.00
150
400
MsS6
400
150
400
M70
400
150
400
c"oTnhceentrragtionQsCbcaosendcuepnotnrtahetipseorrnes4ss.e0n0tpepvb,el1o5f0 tphpebaanndal4y00nptphbe.uEmacah apnlaalsmyahsaesddifferentQC.
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The intemal standard (THPFOS) was added to all serum samples (except Blanks) fora final concentrationofapproximately 200 ppb. The analytical method consisted ofa liquid-liquid extraction procedure followed by evaporation and reconstitutionofthe extract residue with 20 mM ammonium acetate in water: 20 mM ammonium acetate in methanol (30:70 v/v). The samples were analyzed by liquid chromatography/tandem mass spectrometry using an API 3000. The instrument was operated in the multiple reaction monitoring (MRM) mode under optimized conditions for PFOS, PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 detectionofthe negative ions formed by TurbolonSprayTM ionization. 3. SAMPLE ANALYSIS PFOS, PFOA, PFHS, PFOSAA, PFOSA, M556, M570, and THPFOS chromatographic peaks were integrated using the MacQuan software (version 1.6) with a smooth factor of one. Quantitation was based upon quadratic regression analysisofweighted (1/x') calibration curves using area ratio vs. concentration utilizing Watson DMLIMS software (version 6.1.1.04). The samples were injected in a systematic order. 31. Acceptance Criteria
For an analytical run to be accepted, it must have met the acceptance criteria listed below which are consistent with regulatory and industry recommendations. Calibration Curve Each run will include in duplicate calibration standards at six or more concentrations covering the lower to upper limitofquantitation. For all analytes except PFOSA and PFOSAA, at least three-fourthsof the calibration standards back-calculated concentrations must be within 15% (+ 20% for LLOQ)ofther individual target concentrations. For PFOSA and PFOSAA, at least three-fourthsofthe calibration standards back-calculated concentrations must be within + 20% (+ 25% for LLOQ)
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oftheir individual target concentrations. A calibration standard will be considered an outlierifitis greater than two times the acceptance criteia for that standard.
Lower Limit of Quantitation
`The back-calculated concentrationsofat least oneofthe duplicate lowest points in the calibration curve must be within 25%ofthe target concentration for PFOSA and. PFOSAA to qualify as the LLOQ and within 20%ofthe target concenration to qualify as the LLOQ for all other analytes. Ifthis criterion is not met, the next level is subjected to the same test and the LLOQ raised accordingly.
Quality Control Samples
Each analytical run wil include low, medium and high QC samples in duplicate. The `measured concentrationsofat least two-thirdsofall analytical QCs must be within 20%oftheir target concentrations ( 25% for PFOSA and PFOSAAY), and no two QCs at the same concentration can be outside the limit. If study samples require: dilution, a dilution QC will be analyzed in triplicate for cach dilution level (except for PFOSA and PFOSAA which should not be diluted with control matrix). At least two dilution QCs at each level must be within 20%ofits target concentrations in order to accept diluted study samples at that level. The dilution QC acceptance is independentofthe undiluted analytical QC acceptance.
4. RESULTS AND DISCUSSION
Serum sample results obtained using plasma curves for PFOA, PFHS, PFOSAA, PFOSA, M56, and M570 did not meet NWB SOP requirements for validation. Results may vary on average up to 26% from results obtained using human serum calibration curves at some concentration levels for PFOA, PFHS, PFOSAA, M556, and M570. For PFOSA, results may vary on average up 10 43% from results obtained using human serum calibration curves. This data is reported in Assay Revalidation Addendum Report NWBR00-122 [5.3]. However, in order to obtain the lower limitofquantitationofless than 5 ppb required by the sponsor, it was necessary to use plasma calibration curves.
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Nemes Bai
uty awursos
Thm RToRuS Rweoir hEemm RwooR Comm Each accepted run met the acceptance criteria set for the calibration curve|`points, for the lower limitof quantitation (LLOQ) and for the analytical quality control (QC) samples.
32 AAned AAwooelt AMcctp AAvceiedd 5 Ahecetl AAoald AAcerdetAcoeed 76 ANtA Aegmetd AcNceal nAcaoped OSAA cel hAecoemedd AAccpepeedt psersetd w1o0 Apt Ac: e An: d Aoed BBOONNAA NNAA NNAA NNAA 5BNApe Aocmt Acwoaed Aard 16 Ried Reed Reed Reed w7 nAacer Awcat Acnaid Apwned EE
Besnteynbonevinin
Rmsteyconetn Roeomedte,ten Watson DMLIMS system (no met Rrepdcu--suntp
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Run PFOSA Result
m
T Accepted
2 Accepted
3 Accepted
4 Accepted
5 Accepted
6
NA
7 Accepted
8 Accepted
9 Accepted
10 Accepted
n
-
2 NA
1 NA
14
NA
15 Accepted
16 Rejected
17 Accepted
18 NA
MsS6 Result Accepted Accepted Accepted Accepted Accepted
NA Rejected Rejected Accepted Accepted
-
MS70 Result "Accepted Accepted Accepted Accepted Accepted
NA Rejected Accepted Accepted Accepted
-
Accepted Rejected
Accepted NA
Accepted Rejected
NA Accepted Accepted Rejected
Rejected Rejected
Accepted Accepted N/A = ot analyzed
Comments Pre-study assay evaluation.
aQnaClytfeasi.led for rejected rCaelcitbreadtiaonnalcyutrev.e failed for `RWuantsmoinstDaMkeLnIlyMcSresaytsetdeimn(no data collected). Rfaeiilneedcftoirorneojfecutend a7.nalQyCtess Reinjectionofrun 8. pRreejpeacrtaetdiodnueemtoors.ample Qs filed for rected analytes.
Oneofthe medium QC replicates in Run 17 gave very high PFOSA and PFOSAA. results. These results appear to be outliers which skew the overall study statistics. Without inclusionofthis QC result, the medium QC statistics are as follows:
PFOSAA_PFOSA Men 162 153 sp. 18s 177 cv 10 16 SiTheoretical 1073 1020 wins 73 20
N19 19
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Any known circumstances that may have affected the quality or integrityofthe data are included in this report.
5. REFERENCES
5.1. 3M Company Protocol EPI-0012. "Serum fluorochemical trendsof out-of-country residents in CLUE I (1974) and CLUE I (1989) epidemiologic investigations."
52. C.Sakashita. "Quantitative Determinationof PFOS, PFOSA, PFOSAA, POAA, PFHS, M556 and M570 in Human Serum by LC/MS/MS." Assay Revalidation Report. NWB Study NWBS00-040. NWB Report NWBROO-108. January 24, 2001.
53. C.Sakashita. "Quantitative DeterminationofPFOS, PFOSA, PFOSAA, POAA, PFHS, M556 and M570 in Human Serum by LC/MS/MS." Assay Revalidation Addendum Report. NWB Study NWBS00-040. NWB Report NWBROO-122. November 20, 2001,
6. DATARETENTION
`The raw data and final report for this study will be stored in the NWB Archives, 1121 East 3900 South, Salt Lake City, UT 84124 per regulations and contract agreement. After submissionofthe final report to the Sponsor, remaining study samples will be stored `under required conditions until confirmationof Sample Disposition/Retum Authorization is received from the Sponsor. 3M Company will be notified concerning final disposition ofrecords at completionofcontract obligations.
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Sere Quadratic xweighted 1x". All concentrations are Trsmalioa expresasspepbd. 00
oun|9 |-oomons [oosme[ooomoo |oasmm [|ssot ||oirre]| s00uszom||7v[|oomwoowmss [omen|comrs|ooosos |a5s5e0|awee||
BE RE Cvo e T[ewrLlawe[[ me [w os [o ||]
[------
RStuedyNNopo..NNWoWBBSRr0O01.00t6951
Table 2. Calibration Curve Summary for PFOA Quad weighed 14. All concentrations se expressed sp.
NRuumbner A
[RSquarea[ LLOQ
15002000 | 6 | 0.000002| 0.022043| 0.000611|0.9 |19 92|8482 1|
ou | 5 [oom [aorsma|ooo | ass |192 sr | 16:0612000
0.000000| 0.013756|0.007270|09|9 1928 |as2 1|
18002000 |4| -0.000001 [0.015425|0002433| 09964 |19 |482 1|
20-00-2000
0.000000| 0.014501| 0003931|09|9 1927 | 49 81|
[50am] 0 aowonr oor | oars | ose|132 | an | [e3s1v00t2w0o00r||1 1s| a0o.0m0o00n0r1{s[0o01o87s50[|os00o0r1r2o4s4||_0 aosea9 ||119 922|| a7 sss || C so JoC onfaves Eovoomne ) |RwCom ||| me [aesm [ame| oao |||
AB, and Care coeficents sed to define ts calibration cure
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"Table 3. Calibration Curve Summary for PFHS
Quadratic weighed 1, Al concenaions sr expreassspebd.
NuRmubner
C [RSquarea| LLOGQ[ ULOQ
v13e0o0a2m0o0n0 ||3 1 [|-o0.w00n00s10[| a00o3n0430[|s0o00m07o81||o0m997e3 ||1 1343 || 56 213||
[vion50c||a5 +000|[-ooot0o0m0o0rsf[o002r661e8|oov0ournsesrs|| sooowmses ||11363|| 556 223|| 2[0-0i61:2o000|u+ ao [0.-0a0m0o0m0s6| [0.o02m7o61m4| 0.003405|09|9 1364 | 59 23|
31:0t2000|15| 0.000009 [0.031737| 0.006465| 09976 |13 | 56 23 |
SCso
Taow0on JovToYm [ose |oCveEn |||
ALB, 40d Car cosfciets wed to defn th clbratin cure
Pare 19
NorthwestBiosralyica
ReSptourdty NNoo. NNWWEBSRO010.009615
"Table 4. Calibration Curve Summary for POSAA
Quadraticweighed 114. Allconcenstrerexaprtesiidospnrs
Run A
c [RSquarea[LLOC[ULOQ
Number
reoumon|5 fowomos [ooamzssresss[|oowonze|| oo05m900 | 10| or|
oso [oazson [somes|om |160|a so]
[[118-500c0t2200000][5 4 | w0o.0w0o00r0e1 |o0w.0a363s55[|o0.a01r17s81 ||oo0.r9936 ||110.||6ss0o01||
20002000 [8| 0.000005 [0035370| 0003269|09|9 1601 |s2 o1|
roam| 15 |-osomor |oozae |-somom | avez| a0| sor]
7) er T[ esp oooo00T3 o[0n080[s|eoommses[|eowooor || [||
AB, 404 Car cosfciets wet defn th calibration curve
Page 20
Northwest Biosralyica
ReSptourdtyNNoo.. NNWWBBRSO00L009615
`Table 5. Calibration Curve Summary for PROSA
[T++ ] onder Quadraicweighed 15.Allconcenatrerexaprtessiedoanpbs.
[i1e3o00m2a00m0o||1 som| 0o.000s005oo[0u0n59e58e5|o0a01r35s19|"a0s59s1o4||1vs00 || 250 0000|]
icvomomn||s mooro mam n[aso oorme|o atmrom e|oonr||1ev0s00||so0w0|]
Fsa1r9o0ru0a2um0o0m|0
|
|
s79os|o0so0o00m00r0||aa0.ov0su36n29c7||oo0vn.0o1em16es0r7|||
a0oo.s9w8en9s1
|||1a0000 |||sss0 0oo0|]]
[Ssroouwamno||1150 [atooomms aos oossso|amo |100| 0|
23 Mar2001
0000002| 0034802| 0.013699| 0.9847 |100| 500|
JE EC RT
[ws e p[wooooo00s [woonaias[6|wo0oesear[|ooososo |||||
AB, 230 Car osfets ved to defn th calbration curv
Paget
Northwest Bioanalyics!
ReSptourdtyNNoo.. NNWWBBSR0O0L.006915
"Table 6. Calibration Curve Summary for M556
Quadraic weighed 15. All concenaioanres expressed a pb.
Run
A
C [RSquarea|LLOQ[ ULOQ
[amo|Num|ber ooor [ous ows| oom |zw | |
0.000000| 0.025056| 0.002464| 09875 |2.|55000|
wt16oo-uo0rw1aa-wm20oo0|n0|+ + 0oo.ov0mo0o0w0mo0os2[|c0.a01r98e22| 0s.0o0r47s05||0 ooon9 os ||9 222.5003 || 5s1 o00||
[Eorownaemo| 10
0.000006| 0.029287| 0.003549| 09936
omoms omssr | omer| osm |20 | 0|
[o3p1ea0tocr |t|12105s00| 0o.v0o0t00w0r1| 0.018373| 0.001923| 0.9972 |25 |s0 00|
So oowonr soonoso | oor|||
SE TN ) TI
A,B, 0d Car coeffcints wed to define the calibration curve
Page
Northwest Biosralyica
ReSptourdtyNNoo. NNWWBBSR0O0L.006915
Table 7. Calibration Curve Summary for MS70
Quai weighted 14, All concetionsare expresspepdb
me|,| 2]2] [reece] 13-002000| 1 | -0.000004| 0.044503 [0006965|09|9 1.001 | 58 00|
io14w00m2o00o0||s3om| -o0.00s0007|[0o0o5m5032|[o0.o00m8m87s9|| 0o9o88m4 ||1 10 0||ss00 0o0||
Farieas| > u+e[Toaavmowomorr o[[oom|ses[[aasmasr ||oovss ||110a ||s0o]|
[vouramo| 1a oom [own[outs |oom |10 |so| [3o10r61a-2p0w00|v o0m.00o00m06|[0o.w03e85s61[|w00o12r04m0||0oo. mss9 [|1139 .000|2 | s5o04r0||
CSoT] TNoEonsfooown20s [omm0ess CsomTe ||] TwTo wlw 1]
AB.and Car cooficents ved to define the calbration cre.
ren
--
x-- e See
`Table 8. Back-Calculated Concentrations of Calibration Standards for PFOS
0 dd ddd Quadratic weighted 11x". All concentrations are expressed as ppb.
gem| +[Doow 5s0|w2|ea[fe7[[rsoee[o9m [[oore[5] [osm |5Tooos[aow[[aiss[[ooeesrffaons[[r0s3[[a0s[[oese[one]
odo| 5[Taom[ssaez[uuso[[oomaa[Jwiaar[[aowo[o0v[o|e| [wae|+s[weo[sno [[awsa[lzmor[[seae mwos[as[[oeul[m|]
[swam |5amwl[s9w2[[wwoe[laur[f0e5 mwa|m20[woww[a]v| [0m0| 7 Toamo[saan[[mwao[[awurr [[wwaall7w0e[aon[[oww|l|] [smo|v oonm[l4emw[[1u5s[[moo2r[owr]o moo7[aaow[oowwf[ror]] [oem| 0T[oonw[[assos[[9uss[[2o0w7s[[wwoawres[worz[[oooor[[aoorn]] [row | 15 T[eeso[50[w1r0| f[assso[]uwsa[wmso[ouw[awr]] [wCarT |7 e won[sml [06s m200[[rae asm[sw]ls 2w2m[w2] l[]|
I | ESoI w[5m[H 1s| [we H 0[a] seor] Towrw[[o5ur[fsoos[|ie[ooarrlsu[[u5a[[meoo]]msso]] Twwwlulown lo[leow[loou[alr]sl[en01l3s] 0]0]
res is
rsa msn
Table 9. Back-Calculated Concentrations of Calibration Standards for PFOA
Quadratic weighted 1/x". All concentrations are expressed as ppb.
[[e2ammT|>--r|[2or[3250[w[os[25[[50=7 [J ova 30[] oo[7] Doma |5[[1m9os[o50n[noem|s25s6[|dwor9[froae[20|awwe[f1] [eww|5T1w[[ooonr[[uooa[[s7s[|s0va[[owuas[[aso0|maor[[on|] [om |Teow[[oaos[[owwsn[[a5s7i[o0r[[rouss[[ooaLoaon[o|r] [Soman| 52Ta0w[an[[woos s|mo5|[oe[[oave[aams [oono[omr| [mowam|77 Ten[oorn[[wooe|m5s5[[sseo[f2on7e[[o2m[fe1o [oomm| [mow | +T{o1om[o2w2[[w07r[|amrv[[samro[[oousr[[2a0w|wf[ or [Samo| Tawor[a om[wos[n 51 [ovooe [|wwor[1msw mono[o]e| [r[ eam | 5 T ior[oonw[[oowro [[2r0o0a[w2o[[uwmw a[20o[u0[f4o0r]| [Evwam | T[vws[Daww[nrs[moeaw0s2[[omn[aasne oom][wom]| C T hwTwT T e ]wrT[wTslwTdmTlm1]]
vsenll {owoue[[ooaarr[[womsg 135504||2 [[oa|r[3a|[wa[m0] mal To2r[[52s[[owro[[e2ra[oaa[aes[[weoa]ea]oa]s] i Iwlwlwlvlwlalolnln]
ons
nW ate dP uno
dP do dl ll ld Quadratic weighted 1/x". All concentrations are expressed as ppb. --. [isouzon||Tovssr[5oa[[onr[eoo{aone[[owrr|lm[oee n]| [wows |5T[vooer[2a9w5{[m0a6[|os0[[saae [oousr|aasne[[oanw[s0v] [iowa]5[1v56s[2e9w[o0o7[a2es5[[sotro[[o|earw [[aanwf[asns]] [wowzow|5Trisoa[2n9[o0a6[a0oef[roe[[oonof|3a 0[sn[e| [ouzom |TTvooo[aw9{|ivs[[2o0e0[[o5t8T[vooro|nr[[eannJsau| [C svowzaT o|7T[ovloaarns[w1i0[ws0|]oses> 0ow2 [[amonar0]] [ivouton|5Tovelr[a0n[w1as|[aovoe[[osio [[1o0r2l[209 [eown[o7]] [Eowzon| [isoel|azon[1w07 e0a[oees[io[loe[eema[r|] [C sowsT |i [ve 0[sol r[1 [e 200[m9n 70[o07a [w0w[a] 0m]0] [C zwzonT | [Toa[a5n0|[w0e6[aoens |[osans[[oves[aamn[[owmsom]] r elTTowT [awT or[T 7 [sTwT[ 1| 1 [ sol TT ous[o7a2[[o0uro [[w0o[|200s[[775a5s [[15023[[a10a3as]] C [ oTwolae [w0l7w[0l0w[i26v[o0laT n[alona5l]u1l2 nos]]
A
wipe msn
`Table 11. Back-Calculated Concentrations of Calibration Standards for PROSAA. Quadratic weighted 1'. All concentrations ae expressesd ppb.
[[oFowreme]|ia+.||2vsr[|250[wwee |[3a07 J[ooorTsorrwe[F3anoomr|
[www] 5 [|ivoer[[s2sa[[1n00a|m20i2[[awsao[oanse|oamr[[oem[sor]] [ieoazio| 5 [[vsssso|sssos[[i1o0[[r0r[[ssrooo[womra[2om[[oosn[ar|] [wowamo]+ive[aaeos[[a0o [[ovv1a[[oaao[ass][2amw[[oowm osmr]] [oC wsT |--oT|1n5[e2 [rosnl|mi7[asar[woa mzw[[oan w] [vowel7T"wior[oaw[[uwse|auvf[ases[waa[ono [oass[soie]] [C evoazoT n|v [T1o72n|esasa[o07s|[2m0so[o9s1lmverl[oorn[[weocm]| [owe] ouTrw[aomw[[uoow[aeesr[faass [ownro[]iamw [[osew[[eaw] [sC ows | 15[var|[aasee[0w7w s|aw0[wni[oova[oawr[foas ar|] [ston] 17T7ie6[[aoree[[0o6o amsooeLfaosns[[oowes[aoorr[[ooasr[[aors]]
T1wT[oT o[oT m[sol [T zn[o1w]] e sol Termn s[[saswe[owwesawto[[owvv oo e7ars[303[[ornto[ema] [[e is[[zsea[Tvoev o[[oara[[aino[]5e7sr ][36r[raoa5r4]] aTwlwlwlo wlalnln]s]
rons ri
wise msn
`Table 12. Back-Calculated Concentrationsof Calibration Standards for PROSA
[o[reoT|1o i [[m a2r][2 Treo so[na on[oT er
iwowatmo[5Jos |aan r[103e58T[uosas[oens |[2ao|r[fo]s| [ieouzow|5T[s106a[3o0[[owns[[2o0vsrf|eaao[osvoas [2m[[aas[[|| [vows | +T[1o0m7[aawre[v12a6]]a2s05a[[ssnso[onvaa[[asTso[omo[[oars|] ivouzo1w|5J[oiss [a20ns[[oam m20o0[[5w2s[mosn[z2w[[oomu[oe|| Cavour T|7TJoommo[|a2ax[ovor]m1[[awsa]ma me[onno[looe]| [ovowma| 5TJsos|[o2am1[[oasls|mosr[[sooi[swosx|[omf|ors[[oomr] [ouzow1| 6T[oowis|[o21s9[[wose[[2a07[[wsoo] 0os1[12s[[oae[7]| stows1 | TJwoo[2za[l96u]s257[[soowrl[mosvo[oomn|[5]m0|
vursto1r| 17TJoooew|[aoowe[[o5w6 m2i05[[wwra ww02[m0a| ]0 [ rr o am [ww s]1T 0[wsT ]iws [T 30[on] [aw] e sol Joun [[o2m[r1o0rs ||3a0m5 [[sssoo s[]eoree [35[[aamo[ov|e [w vom] e Tora[[5or2[[w1os 0o]w20o[[1o0s|[oea]w [o1as][o7s2[[o3r]] I TNEN ECEDEE ENEN
EE i
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FiH E[ =LLLLLLE L IR LR I Pe ARE 1S2VE L E t L T L Ae e A T ee l, ala | V1EL [l2 eR[Elaaalales[leleleElEEs] 4 V1ie1r [2 alae aa Ee eeae] 3 { 12 [eE efalel eees ed eea] e] 4 +3[E2[LelLa lelele]ale = ae ae azz e]s]
BJs JeleeleeeelEeealEeaee2)
:
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ilaEE Table JRA 15. Analytical QC Summary for PFOS
Crom 7Teown[|Twwm [|wwso| (6.40 ppb) (126 ppb) | (332 ppb) CT rem 7Te oT n wwms |wwe| [rC oman 7T|oeT o[ww e[ow w]| T remoT | T | se a [w wo[|wwme|] CT rem[5To oT n |oww o |] wo] [C am| 7Te wT eew | s[] | [oT ma |vT|seT w[Tmww[|womr]| [C EomT | 0T|o ea[www w|] C Gr&o T|em enT w | mowo[|w| wm | [vT am 7TeeeT w [[ems[ow w
om 1 Tw[T wm [T ow sell Teeew [ [eas[[wwer]] CToaersee] T| e 97[w ws |w ns] C oeTrTf r[mws Tw]
"Table 16. Analytical QC Summary for PFOA
[em Teje gog i [| (481 ppb)| (145 ppb) | (385 ppb) [eos [3[sos| ws [| wi] [s1 ul mw [wm | [ona [| [ass [| wn | wo| [Te [ wm m [om | [oom | 5[sm| we |om| [Ts[wT om] [oowao[4[asTw | ww ] [es[wr[ams | [oeao[5Tew[im | wo|
[sw wsTm| [aonawo[7 |wm| so | ei]
[ LC Tewm s Tm] [Rosa [| &[am| i; |wes|
[Te [mew | we| [Zowao[w0 [snTm | es |
1 [sws wT] m| [awTwTw|
[veo[1m [am[we | en] [C Tas w T Tw| 1-- 7 1 [ve TamJuss | we| [so Tow ws |as|
[w T oome ee |] a1| [Cimmeosica] | 08| tose |1034| [mal Toa] eo |]a| CoTol = [=]
`Table 17. Analytical QC Summary for PFHS
[ee Tee i [| (@48ppb)| (156ppb) | (417 ppb) [oom [7[aa | wo[om| [Te ws [=m] [oma | 5[aw| use [am | [Tew w 1] a] [oowaon[5[sas | io [an | [Tes ws [] sw] [eowam[aTes [we [wo |
Tew [wm [as| [oman |[ass[wo [ ws|
[Tes mw [] wo| [ows | 7 [ase| ww [ws|
[ LC Tee w [l Ww] [ova [8 [ase | ww [ wo |
[TT [sa] om [ ow | [Zona | 10 [ast[mm [ ws|
Tes [wm Tw| [rowan [15 [ass| 0[aw |
[Tea wm [] we| [Bveaoo[7m [am[us [as| [Tew wm [] aw] TT 1 1 [v Tee e Twl [a] [soTow ws [] ao| [w Tae | l es [ ss | Coimmeoeical [iat[hoz [92 | [ome Tar as Tor| Co To[=]
res ic
neIdTeer
Table I 18. AnalyticQaCl Summary for PFOSAA ns [mma Tro
T emo +[sns [[wwmm | woer| iC mo[5T[eowT w[[wwme | wase [T eam[5[ToeT ww[[ooew[|wwes | C remo| +T[oowT n[| ww| e| [rC amm [5TeoT ow[wwmm | oewn| [oC mn| 7 [TewT w|woww[ewe] C remo 7T[aenT [wwmonen| T emT0Too n[wwm [|oww | DC ream| 5T[eowT o[w 0 w | | EC m]TTe eT [emw [wee] TT a el T we[woaT [o] e [ewmT[m owo[[m awowr[|] eaz| CdI =[=]
a
miatse woenn
Table J 19. Analytical QC Summary for PFOSA.
[mmm Trro e en tm |]| ome 7Jo[ (4.00 ppb)| ow(150 ppb) | ow | | (400 ppb)
CremT|T5T[oonw[owwe [|wa| eo1 n[5T [ow|o[w | own| CT rem| T[owT w[ [wew[om o]| rC oma| 5T[oawT w[moww[|owwo| oom1 w| 7T[eoen[[o0m [[ooww | [C em| +T[eoT we[[wosw [|owwr| T ema| 0T[awsT [wew [wr|| [rC eamT | 5T [oo w|w w[|ow] C Emo| 7T[eoT en[ [w we w r C TT eT nTTow [ar
[mmera|| woveo[[| owoesr [|oovio |] [Coom I Taw0[w0u [5] 0|
zie
S FT I
ld AE Table 20. Analytical QC tos Summary for M556
(T Gow T | 7TJsa e|w w [|wewm | (4.00 ppb)| (150 ppb) | (400 ppb) [T roomT |5T [one[wwm |[aw@ | [T emo| 5T[ewwT w| a iw [|wwm | T sew | TwT [e wwee [|Cwwn] [oF ma |5T[eowsT w | wew|] wr| [aC ww| 5T[sw eT |w ow [a a]| ET om|w Tew sT [wwmme a |ow | EC omT | 0T [awe|w wr[|owe | GT ramm| T[swoT [w wow n| [FanT|TwoTens [w mw w|] rr
immeol] Tows[w iose [on] s| e Tvw e emTm w w [Taw]]
ress
SHI)
[omeBe Table 21. mts Analytical QC Summary for M570
T Comm | 7T|ewT e|[www |a]| (4.00 ppb)| (150 ppb) (400 ppb) MT eow|5T[awnT |wwe w |] m| CT eo T | 5T [soo|w oe |oowm]] [EC om | +T[aaT n|[wmo5 [|oomw]] T om| 5e [ow|m w w ae | [rC eam| T[oevT [[wows [|om]| ET omTwo e [w o|w wmm]] MC omo| 7T[oawT a|wwwm [w] m] CT rowe| 5T[oawT n|wae m|a]n | [TaranT|[ T [ow n|w [|w=s]| T mlT [owT [w Ta] ] e ol l om[wm ere | wuaw]] [itovmeeall Tsso[|5_w| o|| deT m aTo]
res sti
Sayuo mnsyn `Table 22. ---------- Serum Study Sample Concentrations
[[iiooww[1366|[ 29 2 [am00050 |6w]o0u10 s2_0[wo0a1 0u0m0[oso9 eas [|s-6 rurooaanunoo)] [[ioom [[m1603[|313 |Jat_000|0]w1w95w [ooauatnm[[sooecsa -|-uoaaanoo)) [[oorrse 11029[[aLto00000933 100000050tooeas00 0000000[[101000500|-ttii0aaun0] [owe[we] 20 |1% [arouse <oonon[wooasn] 122| [[oowws[rs3[]56 [|00s0o0[]oauonace0]a0o0a0u0m0|[-iuo00aass0[|-utiooaanuo0o]] [[oTows[sossa|[astonmasm|| 1366|| nsoor [[a=ucov0ouaoumm[-uuoonoaassno)[s-uooanaoo]) [[oosm [mosa||50 [|ww00a0e56)|| i16osw[)oooaumm[uoosoeassnn|[[--uuooaannoo)] [[ooomoTTowra[]5s5w | swuo |[s1e [|isoauuomwooos|e<o|-nuooeaaasrmo|]) [[oooen [owss|[a5m3 ||3sn [|isoow][c=woooonse[sioonoeassn]swiooaaenon)| [[ow astT[a5s[]3479 || 1v7o5[[tvoomu0]0u0o0o0ne[o0|0waov[w-eoisoeansn|)o [[eommo[[sooo]eses||3to5[|i-u0i0o0w woo0u00|[suo0v0eassn0|[-otiaorasn)o [IoC n[5EC34|RaEse |3 ET | E1EmT |EoeLouo)n[EsuToasEo[sTiFoauio [CeosmosTTaoor]2sw || i2ws ||-w1io0ano[[u-poownm ociouoasso|wmooamoooo]) se TT(eimEbeeetamntsotasgstwoSpeeemlecsetsedredefr LOECEmEiEtT
SeOTTHOSAT--N aid et msc
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Tobe. SoroA sShadt ySneolo ecCoonsrs sttaotins Contd)
[[eSeen[oroosr][raown avm0|[ov3os0an[Toomems [J osae[[uwsww | [wsws [[22x3[[satsoooouaosmn[to1o5ns| 1r5o7 [[swooauumro wouooaaassoo|-ciooouuosn]] [[oirons[[ass]] ao3r[isoours[]oa15n |swuoouunm|w-ouaieoseos|n[-csioownoons]
ChioosseTTor|| ssoor [aswor |[2215 [[rrooaun ||--swio0oeess0o[[-suooonons| [[ooems[saea][aarvr [ieovnr s]ioo0vim[roooamm woonoeesso[[--uuoooauuocno]) [[oonmsaTJeso[]s3woon] 2so0r [[teonn [rwoouam oooouaso|--ucooaonuooon)] [ColownTssro]] a2307 | r3o0 [[suatooooa][sroowaunso|-ioo0easn[|-ouooonooo) CE ions[Ema]Ee30)[R30E[EoEu] ioIu)s]EwoEoeEsn[Eoeon)] Dio Taro8E ] 11 [ Tw [0ET00 Y oI omFwo0ees0E[-uE000)00| [[oonms[[vasve[]to97u[1| 3 [0030 [swooanotno wwooo0aessn0|[--ocoo0uuo0o0]| [[aorms[a1e[]mo1at[]2109 |[iotnor@[Swiooouum[arioo0oeessno[|--wwioouuoono]] [[iims[[ve|[ar2oo0us[n]c15w[Jiwi0o0000e [[soworumnm[rrooaaeassoo||cwwoouounoooo]] [EvEer[ston _E10I|29 2[roanI)|F-wo0easn[Eaoay| [irTfhaatT]eepsaasror[natt oA r rb[euoee00rstonN ursduOCootaseo[i-uo2o0on]
Sms ROLHLSRO E--n Te gs
[r |ve Too e ae | o oe| ov --
R--ig--i
Table 2. SeruP m Study SA ample Co. nentrnons Canines)
[eCorm [[mm0o|[usounsn[|w1oa0se[] zari|0<uaoui0on|[wiu|ooaeeosn|[orroooaanmm||
[ss 1[sous] 196 [ro0a0@| 0000[00a [0am|
C[iown[[o0s|| 2a3s[|13s6[|0|0u0ocu00o00n0 |uwduep[reooaaausm]| [[iioos [[515579| [19[[aaww0o0u0n5e0]1oan0_[<ioraoausmo[o0e0as ||--ui0oaannm0o] [IEwCo[aos[RaE3 |N0Es|ET3E5)[P<oaIum oes |-usToaEno) [[hiems[3oe s2w6 |[i3 o005a|] >in[|o<uooomum|aauooees|[w-iwooaaummo))]] [[iCrmome[[517[]o5nams[m [-9cto00[50o] u1i [tvooaauanm[uooeaessn[[-ouaoanuo [[sioosn[[oou>s[[a3r9 ||-wao00[0rooaan]] ooaotm0[0on0eas[[-ouwaoanuo) [[iCiss [1o0oo>|[<iou099|000[50r| ooaa1n0] ooaan0[o0n0ess[[-ouaoanno) [Ciosmm[[ooos[] 53m[|01 000|]ao1ust [woiaono[u0m0a|u[[o-uuionoauenms [CCooost[oosre[2e3n || o33n0[|o>ma[iooaaumu[moe|sio[[-ou0saoeanns [[wios[woeas[| i2s0e[|mo1n97a[]awoamn0s[o oooanmauwooceessn[|osasn|] [[oomn[[ai7so]]a3s0 |[-otoousa|]3is9s[|o<iooomum|ouoecess|[--uuooaamu)o]) [Raore.mhp [m3e5]r m5eE 9ei ch|i n2 an e [wpmoeecwt ooioen nm aC QCoeee [iona2200n4]
ST meePOPROSE A PR--SOSMSsdTtied nepmcsa
ie
i ----
`Table 22. PU Serum Study Sample Concentrations (Continued)
[E or[0T ]on | ior[l ion [l iow woael oa] [[ooomrTTionro]] 2sn8[io1u7sJ]o5u [souanoouaisoaoa[s i[wrozooacauanosn]] [[oooommTDsoelam |[iotoeuss|o[sirown [uoooaunso[iiooaaaemso[riooo0uussoo]] [[oooomm T[ionee]] 32m[[i2o0us[]to1n7 [ooaauusso]oi]oa-ewsoo]aGarexoosoouuossoo])] [BwEsENTEsE ]E3T |72 [BsEioEn roranr]rreoaym]rtrocra] [[oowoemr[[a7+e[]mosamn[a 1oan|]svwer[[osaoonn]iiooaaeesso]]itooucsa]] [[oowwToaorr| aoon[|io_us|] s1os [[oaiaoannm] ioooaamso]]iioo0uumsm]] [oEoE[E7N]os|EsEn)|EsT w [sEiToaumEioEe]ErToaEm)] EIENEEN ET BE ET TE EyME
[Sm[9s]so[21 [aiow0m sian]woes]aioaim] BE [EsEoNlE3E9T |E1E IE)|ETis[sEioTnEs EioE eas]ErToaEm)] [[oomw [[03s+[[0-0m0o9a0a[|i1o0u[s o| user[owaoanus]orwoaaea ] 1100000000)) [[oowm[[i3e1s 1[00so0r9s[[sii0on0s0[[ssooano ooaats][trooa a]Ttroo0auumm))
D GoSsPh re os tfebicpnnMN mes on ESECS PoMSE STdi scl
J.
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Report No. NWBRO1-065
`Table 22. Rar Serum Study Sample Concentrations (Continued)
[EoomS[ae a[2 ounnl[so0 a ni |ioel0 l]amoanlm)l] [[oowm[wwar[]m2o3o|n 3st[[swovos[[siooncoinu[aaiocaesn][waizoooonuomn]) [[roio TToou]s]01[910[[iwoooor[oonuiim iwoaoaoss[a[zoooonnon]] [ECTaEw[E0N[5E9T |7ao | EiSm JEeToOn)[E-weoceem|Eazrocaem) [EvE 0EE[EoEna C00T050|EoEat)1E00y00|Et1r60ee3[Erir000 [[iosn[517[]5zi1e || swos [[oiauoauonm|[[aauttoocoeessscs[[aaooteoouomun)o]) [[soonr w9a4|]s2e6 ||aow00n05|0| ooaw r[ooontm[[wiooees[oox0m|] [[sonsTaoos]]_sz6o[|osnn |[aaro00m[sooum[[ioocaas [[iooooaos)]] [[ssosn oTooror[]saawc [|aai0o|]S3io0a [soooomn[[-ouceoassn||iouaum|)] [[soesee[sosro|[ssor|| 1000 [[aio0au0) o0na0n[[--0uuccaaee0ssnn[[-0wioou0sooo) [[ssmssJJre[[<etoiaoaatssnn|| 1ress [| a00r0[oo0u0o0n[[--uuiccaaeessnn[[-0io0aasom) [[sossoe[[5s0r+|[eo_aus2n[1372s|_o[at[-oanonavon[[ou-uooaaaeessnnn[-6uso00a0sodo))] [[sisoss[0970| 51956 [|-uso1a9u5[0|oruoai oonnoon[[0100aa[[600000000)] [[iioonssT|1o2[ [ro0asm 0[-wo0ause7] o3u91s6[o-n0a50n0[[01io6n0a16s9n[[5 t1o1o0a00 s0o)0] E Tp eshet be es r nrCun 20
Smme OFTOSAFErO sMt To ps cle
--
a-- e me!
`Table 22. PA Serum Study Sample Concentrations (Continued)
[[Soivger[ [ro]|rox[romnsn[[rSoosu [rroosasm[w00eamJ]io00e0]] [Cooow[[5352][smo3o0om[51575 [Jawuoou0]neo|auusooa| ntiom0e-io11a000a000s090])) [Ceoonss[|1o5es]"i5tovnus0[10105056|| otao ||<ioonaaum][sooane][-iiroo0ano])]
[[oopomr[[xm0e|]wi20106099[[w0i000003300[[SS0o00u] ooaa [0i0oaaes| 1100000090)) [[womr[[w7a]] =n[s5o5 [[Sauuoo0000@@]ircoaann]ioo00aasm]| 110000000000)] [[oCowonn [ooeri[]o_1n5as n[[2to0us[]i00+1[]ooaanmoaudoceems[[a11oo0oaumm)])
CCoooms[[o5r||0 ow[m5[|i030500[]uooooumm [soucoceessmm[[aaisoocoaamm))]] [Ceow0[910[o5a0 n|[0v0056[aii0o00]<rwooaauumooaeessn[[a4i1o000a0m))]] [[oTarsos[[5032[| 220 |[u0104003[6i0100000.0[orooanm[[-01000aa5[[1r0o00a.m0]] [[mome[7s0ts]]33055| 19 JJaatioonw@ oouuii]iaiooee]] rrooacusam]]
[oss[1] soe| 210[rou ono[00a tioauo)]
[[oowsr5s57|| s2s0 [1[u0u000005506|[t0vo0a1u 0] o0n0a0m[[000000500[[TT1100000000)) [[oenvn[r|es ioaa59[[11000756[|atuooao00 t0o0oaom][0wo0oaas [[1o1a00u0m0])
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Ss TON PESPOSAA FT--OOMet me ht gr
lal llMlRl Table 22. Serum Study Sample Concentrations (Continued)
"0 |163|00093 [000036
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Table 23. oreoset, Plasma Study Sample Concentrations
[m[iro[e25]| rsoar[[rmmann[ ]3[r oa [ e ou| s|e wieoaeus]| [or sto| a7 [tons[ sw |awoouon[<troauso[oats [[riRonsa[Tiaseors||[semwse [ [[ s3n| |s av w [|[auiioooor aauuuommn[[[sswwuiowouaoaasss oo[|]otawotio_so|) [[[aiisora rsws|[| sesswmr[Jta[sooun|s]]31o7n[|rvoroouaannnon[[tooouaas]]wtozoaocctsa]| [iESmEo[ErCa| eer [zCwT | sCTo EmoEuoEn|ETso |<tiEoaTum] [[sioin[1066|| sase [[attoooo] 3113ss[r|wooaunnon[[-ooaeaimo]| t1ome] [a5t0oEaN|EsTs Jasons]EsCe[rEoaEn Eorues]EiEoc] [EzE oEoT|EeEs [Izw|EET)[oEonEon[EoCeEs[EoEaTt [[[sanonow[esraess||] oaesne[[|tatooou3nssso|]] s3336s[[[owoaooanuumo[[zooueauassso]]csiooconas|]| [[sraasra||sswrrsw 3 sw |[uaowuoauuomn[[=trioosaasonwoooao)| [[iiss Taaoisr|[as2r[zoos][ 2yu[|raowaoonnon[[ooaan]]<izoaatcan]| [[sssoom[sv[]m ss |3_||31%0[|rroouaumm oounsan[[wwoooss]] [[assira s57] seos [ioaanns[a]52%0 ||TSsooaunmm[[ucioounss [[wwiooanwoo])]
ee nTienrgaeedeonwtraee enr tprorn ee rbCmf2 J
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Table25. PemraeStsudoy Snupt Contcsnta,tos Continued)
[[swraesr][rmorr[[mmaensa[]roewe[ouetss[| oioewa[ewno]o [[srmes[assa || eens | s23w ||3om[[osuoon [wrooan soexm|] [[sasson|[wmsr|[ie2ss0 [[w7o[[swuooaoumm| ioouasaso[|i1o0us_]| [a2se [EaoEr|CeE [3EmE|E3CaT [EauoE 0um[Eioauyso[sono] [[sissian[osnesx[|7v6[imoaena]]1 [[arrooaaunosoo[[-otarosasssoo]] ooccm|| EEEYEEN EEETI ECTEO ECCEN E EE EEEryeEBEET [[sisesno[[siaos[[asmw [i1oou|] 2i0[raoroaunnoo[[rrooaanm]] saiee|] [[iissoms[3903| [32e[[ammoooouuss0e]] +337 [[rrooaann [wooaasso[]wiooaoism|| [[esssaeswa[eeno[enaw [|Soeos |saswooaouummwooaosn[1i6]] [sEeTe EssNo[aEsI E1E 7E2T EwFon[Eoeues oETem| [[saswaemo2[ |so |is v||asm3 [[t wwooaaauom[[-rwoooam aso|swiicocaanon] [nosre[[sooe|| eear [[awsor ||sewe[w[aowaoauumm[[swwoooeasso]o1osn|) [oronn[raoea[|sr|2ro[a39n0 [awwooa0n0omn[[wriooaaasno]] oaort || [[aariirs[eaosss|| soarre1s0s | ssswo[[wwooaonosn[]vosuxs |oioxo|| [EarEsTEoCsa[asCEe [3EEmT |Y7%I[rEoaen Eiecee)mEanT]
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Table 2. Plasema SotudynSampsleaConncetntoratsions Continued)
[[grsessa[rosr][ [rsorw[arme|[o rieee[[[rrooesamm[[a voevea[[nio| uws]
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`Table 23. PI, Plasma Study Sample Concentrations (Continued)
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"Table 23. BT Plasma Study Sample Concentrations (Continued)
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`Table 23. Plasmaamnion oe Study Sample cots Concentrations (Continued)
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Figure 1. Representative Calibration Curve for PFOS
ce RYaRTA
ol
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Figure. Representative Calibration Carve for PFOA -- srs ---- oo ---
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`Figure 3. Representative Calibration Curve for PFHS
! | F T SER t --
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Figure 4. Representative Calibration Curve for PROSAA
I SREET ER !
iI
|
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ReSptourdtyNNoo.. NNWWBBRSO010.009615
Figure 5. Representative Calibration Curve for PFOSA
otp tta E50E CiSt OE 0) >--
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Figure 6. Representative Calibration Curve for M556
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Figure 7. Representative Calibration Curve for MS70
LS Cr
Page 62
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Figure 8. HumanPlasmaBlank for PFOS
Ba =m EE m=n S T] Rn lEn3
al
ea: ww ec [e 20] @
lt
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Figur9e.Human Plasma Blank for PFOA
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= Z=Sere.
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RStuedyNNoop..NNWoWBBRSOr0L0--00t9615
Figure 11. Human Plasma Blank for PFOSAA
pr ros e ee jr
m r w oe oww m r n 10
sme =ess
= m f i---- r a -- Eoo sE -- -- Em]
ee] E ------m a | emn E be fort ax w wv av--ee e 3 r 3
a -- ]
a
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Page 66
Northwest Bioanalytical
RStuedyNNopo..NNoWWBBSRr0O0L.00t6951
Figure 12. Human Plasma Blank for PFOSA
wrerre97n05 bone
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Page 67
NorwestBioanalytical Figure 13. Human Plasma Blank for M556 RStuedyNNopo..NNWoWBBRSOr010..00t9615
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a = wrn 2m5] ffoarrgevdi=ne
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Page68
Norwest Bosnia!
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Figure 14. Homan Plasma Blank for MST0
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Figure 16. Human Plasma Blank with Internal Standard (QCO) for PFOA
en BE------ me EE men miRmE
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Figure 17. Human Plasma Blank with Internal Standard (QC) for PFHS
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Figure 18. Human Plasma Blank with Internal Standard (QC0) for PROSAA
iporosayan mE
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Figure 19. Human Plasma Blank with Internal Standard (QC) for PFOSA
e rFl fem rrornJE wF = imeenE E =dt ry mE =
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Figure 20. Human Plasma Blank with Internal Standard (QO) for M556
-- res
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ReSptourdtyNNoo.. NNWWBBRSO010..009615
Figure 21. Human Plasma Blank with Internal Standard (QC0) for MS70
jE nr e E apnri=m =
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7
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Page 76
Notessic Figure 22. Low Standard for PROS Ew BE eenaliS= a BEEEE. REES =
Rechuotttsa)l
E a Ee rE ] ] = ee
= = J
o
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Br TORneeem=]
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=
3
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m TeE m|= rEE r ee : Sr 2 = wwnae] ]
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Figure 24. Low Standard for PFHS
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m mS eem E y 5 e 23
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i
:
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Northwest Biossayial Figure 26. Low Standard for PFOSA RepSoturdtyNNoo.. NNWWBBSR0O01.009615 E -- emsstarE e em) en = w nnee m T 2RS5 freepn w m= ie nes a38
=
qe
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[US
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fm]
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Figure 27. Low Standard for M556
wrmasais oS [J intae
= Emmewseh vve ee =] mew e 8 m%
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Figure 28. Low Standard for M570
BEs 5E--e-- Emn-- S-- Sa a SET= ErEERoPnEEEEEk , XT4 = ik: EoE = Eeeagmt r] th ===
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Figure 29. High Standard for PFOS
FrrFsi m-- ame on
s= hee b 8 o m weE m m S82
RStuedyNNopo..NNoWWBBSRr0001-0t09615
| Soli
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----
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Norwest Bioanalytical Figure 30. High Standard for PFOA
= r--n-- s= m av=e ed SEcoEnn w ah= nao nb8a]}5
ReSptourdtyNNoo.. NNWWBBRSO0L0..009615
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4
fa m oer -- 0 o-- ] ]
;
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GEE BH
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45
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Northwest Bioanalytical
Figure 31. High Standard for PFHS
Esmsnas oon p-- eie e--
= Eee2 wwaeewvenevn 8 24 e4%%
re
ReSptourdtyNNoo.. NNWWBBRSO0I0..009615
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=i
mmra-- a a3
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ff m a =i ]
= Zi ----]|
%
Page 86
Nebo ene5. ig si frPROSAA e -- m
EE.
= am z
2a2bHe J --
E E = S=hE r = es
ea G0 bts
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= z2l08 a Ew--lrye3
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== = E E r= F r E y||
a0 Rey
TRE
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Nochves Bosmyical Figure 33. High Standard for PFOSA
B re E Pme em
mP i 0 T m= ee
Ee i
RSeptoyrtNeo NNWwBBRSO0I0009615
E E fme na a e--]
rar !
= = --=-- ] |
kbdSuit
--
ve EE s
wuE seani= mmms.l [b1ee07
10
o
= = = -- B------ = -- | [il pagent
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Figure 34. High Standard for M556
S me feseereme TT Sm E ERTEEEREe mEEEEER)>4
sRtaeys ansorto4n
E = a _=--e e ==|
[ E ---- E EsEaEe -- EEEEER{
= E-- e i --
!
E==--d
EEE SA
ess
Northwes: Bioanalytical Figure 35. High Standard for MS70 RStuedyNNopo..NNWoWBBRSOr010-.00t6951.
EEmE pe rov e
| m eve eE m em%m
nario me
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pve
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ges FT|
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=
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oh
e-- -- i i r ---- -- ----|
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