Document GmXg0zjRR0QqMxGwE99Mq3md4

Northwest Bioanalytical ARQAG -- 113 SStuudyeNo. mNWBsS0e0-1s45 Quantitative Determination of PFOS and Related Compounds in Human Serum by LC/MS/MS Sample Analysis Report for Protocol EPI-0016 Northwest Bioanalytical (NWB) A1D1i2v1iEsaisont o3f9N00WSTouItnhc. Salt Lake City,UT84124 ) PREPARED FOR: 3M Company Corporate Occupational Medicine, Medical Department 220.3W-05 St. Paul, MN 55144 = =5 BS=E Zz 5 = 8 AUTHOR: Lonwee Zedl7" Connie O. Sakashitz, B.S, NWB Project Manager APPROVED FOR SE BY: fger L. Foltz, Ph.D., NWB Technical Director ) Page 1 DATE: /-/0- 02. DATE: _/=/0-0 CONTA NO CRI 000599 Northwest Bioanalytical RSetpuordty NNoo.. NNWWBBRSOO0I--114555 LABORATORY: SPONSOR: QUALITY ASSURANCE STATEMENT Northwest A Division Bioanalytical ofNWT Inc. (NWB) S1a1l2t1LaEaksetC3i9ty0,0USTout8h4124 C3oMrpCooramtpeaOncycupational Medicine, Medical Department 220-3W-05 St. Paul, MN 55144. COMPOUND(S): PFOS and Related Compounds NWB STUDY NUMBER: NWBS00-145 SPONSOR STUDY NUMBER:~~ EPI-0016 NWB STUDY TITLE: QCuoamnptiotuantidvse iDneHteurmmainnatSieornuomfbPyFLOOSMaSn/dMRSe,lated J r`Tehgeulcaltiendicnalonsctluidnyicdaelssctruidbye.d iHnotwheivserre,poNrotritshnwoetsitnBcilouadneadlywtiitchailnctohnedduecftisniatlilosntoudfiaesGwLiPthin the guidelines ofthe U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory JStaupdaineesse(TMitHleW21GCoFoRd LPaarbtor5a8t),ortyhePrOaEctCicDe SPrtianncdiaprldesOrofdiGnoaondceLafobrorNaotnocrliynPircaacltiLcaeboarnadtothre.y iSntsupdeicetsioonnstwheerSeafpeetryfoofrmDerdugbsy(tOherdNinWaBnceQNAo.U 2p1e,rPSOAPB.Notification No. 424.) The following Inspection and Reporting Statement. DateofInspection ~~ PhoafSstuedy 22:23 0ct 2001 2224:O2c3t02c0t021001 15-16 Nov 2001 07-09 Jan 2002 10 Jan 2002 Standards Preparation AQnCalyPtriecpaalraPtliaonn Sample Analysis FRienpaolrtReDproarftURaw Data Date Report Sent to NWPProjectManager 230ct 2001 2234 0Occtt22000011 16 Nov 2001 09 Jan 2002 10 Jan 2002 Date Report Sent to NWBManagement* 31 0c2001 331100cett 22000011 30 Nov 2001 31 Jan 2002 ~ 31 Jan 2002 "Reports to NWB Management are issued monthly. As can reasonably be incorporated into this established, final report atchceurmaettehloydrsefalnecdt ptrhoecreaduwrdeastad.escribed and the results ) cy Lfin Chain, B.A. NWB Quality Assurance Compliance Auditor Date 01-10-02 000600 Page2 Northwest Bioanalytical ReSptourdtyNNoo.. NNWWBBRSOOL0--115455 COMPLIANCE STATEMENT "rTehgeulcaltiendicanlonsctluidnyicdaelssctruidbye.d iHnowtehiverre,potrot tihsenobtesitnocflouuderdkwniotwhliendtghee,dtehfiisniptrioojnecotfawaGsLP cReognudluacttieodnsinfaorccNoorndcalninciecwailtLhatbhoeragtuiodreylSitneusdioefts h(TeitUl.eS.21FCDFARGPoarotd5L8a)baonrdataocrcyoPrrdaicntgicteo ttMhheeHmgWueitdGheoolodinsdeasLnaodbfoptrrhaoetcoOerdEyuPCrreaDsctPdireciesnccSriitpbalenedsdaworiftdGhiOonroddtihniLsaanrbecoperoarftto.orrNyIonnPrcaadlcdiitntiiiccoeanla,nLtdahbetohsretauJtdaoyprayfnoSeltslueodwieeds oiinnnccitldhueedneStdasfitenhtatythoimsfarDyerpohuragtvs.e(TaOhfrifdseicnrteaepndoctretheNroeq.pura2el1si,etnyPtosAraBinnNtaoectgciruifrtiaycotafettirohenecoNrpodr.ooj4fe2c4tth.oe) rAarnewpyodarkttnae.odwdnata is [CoonnniecOe. SaOkashitfs, Bl.Soats NWB Project Manager ) ReffaerTeLc_hFnoilciazl, DPihr.eDc.tor D/a-e10-02 -- /=1o--03 Date 000601 Puge3 Northwest Bioanalytical TABLE OF CONTENTS RSeptourdtyNNoo.. NNWWBBRSO0I0.-115455 SIGNATURE PAGE... QUALITY ASSURANCE STATEMENT ccs COMPLIANCE STATEMENT ccs d TABLE OF CONTENTS rns LIST OF TABLES oss LIST OF FIGURES... 1. INTRODUCTION. 2. METHODOLOGY conn) 3. SAMPLE ANALYSIS ccc 12 ) 4 RESULTS AND DISCUSSION wo |3 5. REFERENCES ovis 14 6. DATA RETENTION consists13 LIST OF TABLES Table 1. Calibration Curve Summary for PROS... 16 Table 2. Calibration Curve SUMmMAry for PFOA ccs 1 Table 3. Calibration Curve Summary for PHS... 18 Table 4. Calibration Curve Summary fr PROSAA csr 19 Table 5. Calibration Curve Summary for PROSA ......rrrmsssssns20 Table 6. Calibration Curve SUMMArY fOr MSS6.......cvmmssissnssnn2] Table 7. Calibration Curve SUMMATY for M570... 22. ) Table. Back-Calculated ConcentrationsofCalibration Standards for PFOS nnn 23 000602 Pages Northwest Bioanalytical ReSptourdtyNNoo.. NNWWBBRSO0I0--115455 Table 9. Back-Caleulated Concentrations of Calibration Standards for PFOA ...............24 Table 10. Back-Calculated ConcentorfaCatliibroatniosn Standards for PFHS ..................25 Table 11. Back-Calculated ConcentrationsofCalibration Standards for PEOSAA................26 `Table 12. Back-Calculated ConcentrationsofCalibration Standards for PFOSA..........27 Table 13. Back-Calculated Concentrationsof Calibration Standards for MSS6 ...................28 Table 14. Back-Calculated ConcentrationsofCalibration Standards for M570 ...................29 `Table 15. Analytical QC SUMMATY fOr PROS... 30 Table 16. Analytical QC Summaryfor PFOA o.com 31 Table 17. Analytical QC SUMMATY f0 PFHS ccc 32 `Table 18. Analytical QC Summary fr PROSAA rcs 33 Table 19. Analytical QC SUmmMAry fOr PPOSA .vrcorcssssssnssnsnnrsonnn34. y Teble20. Analytical QC SUMMAY or MSS6.covsmsn 35 Table21. Analytical QC SUMMARY fOr MST0..ccvrcmssssssnsnrnesenn36 `Table 22. Serum Study Sample CONGENLTAONS. rcs 37 LIST OF FIGURES Figure |. Representative Calibration Curve for PROS .....corunccrronsnsnmsnrmnnn 45 Figure 2. Representative Calibration Curve fOr PFOA... dS Figure 3. Representative Calibration Curve for PFHS ......ccccsrsmmmsnsd Figure 4. Representative Calibration Curve for PROSAA cvs Figure 5. Representative Calibration Curve for PROSA. cvs dT Figure 6. Representative Calibration Curve fr M536 .....uncuscrccorrsnsssnn41 Figure7. Representative Calibration Curve fOr M570... d8 J) Figure S. Human Plasma BIank for PFOS ...omreccssnssssssnsndd 000603 Pages Northwest Bioanalytical ReSptourdtyNNoo. NNWWBBRSO0I0--115455 Figure9. Human Plasma BIAnk fOr PFOA wc... 50 Figure 10. Human Plasma BIankforPHS... 1 Figure 11. Human Plasma Blank for PFOSAA weenie 52 Figure 12. Human Plasma BInk for PFOSA ccs 53 Figure 13. HumanPIasmaBIaK for MSG... 54 Figure 14. Human Plasma BIankfor M570... sms SS. Figure 15. Human Plasma Blank with Intemal Standard (QO) for PFOS ........cov.omron 56 Figure 16. Human Plasma Blank with Internal Standard (QC) for PFOA... ST Figure 17. Human PlasmaBlank with Internal Standard (QO) for PFHS oon58. Figure 18. Human Plasma Blank with Intermal Standard (QO) for PFOSAA.......ccrr 59 Figure 19. Human Plasma Blank with Internal Standard (QO) for PFOSA cc... 60 Figure 20. Human Plasma Blank with Internal Standard (QC0) for M56... 6] ' Figure 21. Human Plasma Blank with Intemal Standard (QO) for M570... 62. Figure 22. Low Standard for PROS. 63 Figure 23. Low Standard for PROA corners sss 64 Figure 24. Low Standard fr PFHS.ccvvonssssssssossssmsmmsn6S Figure 25. Low Standard for PROSAA vrsG6. Figure 26. Low Standard for PFOSA .vvcrsmnssssssnsnsonsomsnn1 Figure 27. LOW StanfdOraM5r56d... Figure 28. Low Standard for MST0.cnnsntssssssnsssssioens69 Figure 29. High StanfdoraPrFdOS.ccvurmamscssnsnsnsnsmsnssnn 10 Figure 30. High StafonrPFdOAav rdests 1 Figure 31. High Standard for PHS... 12 "Figure 32. High Standard for PEOSAA rer ssm--r8 Pages 000664 NorthwestBioanalytical Study No. NWBS00-145 Report No. NWBROI-155 Figure33. High SIAdard fOr PFOSA crosses 74 Figure 34. High SUNard fOr MSS6..orsssseses oon 75 Figure35. High Standard 07MST0.crcrrvrcmsessssensosmsmsesseeesonos 76 ) 000605 Page? Northwest Bioanalytical ReSptourdtyNNoo.. NNWWBBRSO0I0--115455 Quantitative Determination of PFOS and Related Compounds in Human Serum by LC/MS/MS Sample Analysis Report for Protocol EPI-0016 1. INTRODUCTION `This report summarizes the analytical results from the quantitation of POS, PFOA, PFHS, PFOSAA, PFOSA, M556, and MS70 in human serum samples for 3M Company (3M) in support of Protocol EPL-0016 [5.1]. The LC/MS/MS method for the analytes has a targeted calibration curve range of 1.00 to 500 ppb (except for M556 which has a LLOQ 0F2.50 ppb). The actual calibration curve range for each analyte varies based upon the persistent levelsofthe analyte in the matrix. For this study, the assay exhibited the following LLOQ and ULOQ values: ) -- -_-- -- oAn-- walye te ILlLOeQ 0 uUoLOQQ PFOS 337 ppb 413 ppb PFOA 1.44 ppb 481 ppb : PFHS 1.36 ppb 522 ppb PFOSAA 1.50 ppb 501 ppb PFOSA 1.00 ppb 500 ppb Mss 2.50 ppb 500 ppb --0 Ms70 101.0p0 ppbb = s50000pppbb The sponsor was 3M Company (Corporate Occupational Medicine, Medical Department, 220-3W-05, St. Paul, MN 55144), and the Study Director was JeffreHy. Mandel, M.D., M.P.H. The Study Contact at 3M was Jean M. Burris. James K. Lundberg was the technical contact at 3M. The following is a list of NWB supervisory personnel involved in the completionofthis 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 000606 Pages Northwest Bioanalytical ReSptourdty NNoo.. NNWWBBRSO0L0--115455 study included Suzanne Newman, B.S. (NWB Research Scientist); Laura Struhs, B.S. (NWB Scientist) and Anna Akrami, B.S. (NWB Associate ResearchScientist). NWB SOPs and guidelines were used in the conduct of this studyand were available to study personnel in electronic and/or hard copy formats. Date Study Initiated: _23-Oct-2001 Date Analyses Completed: 16-Nov-2001 `The clinical study described in this 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 Principles ofGood Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the SafetyofDrugs (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 NWBROO108 [5.2] and NWBR00-122 [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 NWBR00-122. Samples for this study were received at NWB on the following date: TT RReeecepipit DDaatee MNeummbbeerrof Samples Received Storage Condition _-- (e(xexecpepttdduuirignagnaanahlyssiisy) _-- 23-Oct-2001 = 262 w-20c C ) 000607 Pages Northwest Bioanalytical Reference Material ReSptourdtyNNoo.. NNWWBBRSOOL0--115455 Analyte PROS Lot Number Purity Expiration Date Source Storage Conditions 193 100% 31-Dec2010 3M Room temperature PFOA 25 100% 31-Dec2010 3M Room temperature PFHS SE036 100% 01-Jan-2010 3M 20C PFOSAA PFOSA 617 538% 31-Dec2010 3M Room temperature 214 100% 31-Dec-2010 3M Room temperature MSS6 NBII3047-8D 99.89% 31-Dec-2010 3M Room temperature Ms70 11850626 99.75% 31-Dec-2010 3M Room temperature T THPFOS 59909 90%me31-aT Decs-20l0 3M Room temperature `The reference material purity for PFOS, PFOSA, PFHS, and PFOA was not available prior to the conductof this 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 NWB stock solutions used to prepare the analytical standards and controls used for this studies. All amangements for purity determinations and the transfer ofNWA 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 Factor 0.821 0.961 1.043 Eight or more calibration standards were prepared on the day of each run by adding ) 100 uLofblank Chinese human plasma and 400 uLof 50 mM ammonium acetate in Page 10 000608 Northwest Bioanalytical ReSptourdtyNNoo.. NNWWBBRSO0L0--115455 `water (unadjusted pH ~6.9) to 13 x 100 mm polypropylene tubes. After abrief vortex mixing, 10.0 kLof the appropriate spiking solution was added. The final calibration : standard concentrations in human plasma for each analyte are listed below: --AAnnaalbyttee PFOS CaClailibbrraattiioonnSSttaannddaarrddCCoonncceennttrraattiioonnss** 3.37,4.60, 10.8, 23.1, 43.6, 84.6, 208, 331 and 413 ppb PFOA 1.44,2.88, 10.1, 24.5, 48.5, 97.1, 241, 385 and 481ppb PFHS 1.36,2.92, 10.7, 26.4, 52.5, 104, 261, 417 and 522ppb PFOSAA 1.50,3.00, 10.5, 25.5, 50.5, 101, 251, 401 and 501 ppb PFOSA 1.00, 2.50, 10.0, 25.0, 50.0, 100, 250, 400 and 500 ppb M556 2.50, 10.0, 25.0, 50.0, 100, 250, 400 and 500 ppb. --1 +2 TheMt0 50 ar7ge0t c_ 0 alibr_ at, ion cur2 ve r1a.n0g05 e, i2s.51.00 0,0 1p0p.b0, ,(02550.001 ,p55p00.e00x0 ,,c1e1p00t000 ,M,S22S55600,,, wh44i00c00haha2 nansddaS5L005 L00pOpQppbbo0 f 2.50 , pp), pEloacshmaanawleydt.e has diffrent inal curve ange based upon the persistent levelsofthe anal i the un, In addition, blank human plasma samples, both with and without internal standard (designataesd QC0s and Blanks, respectively), were assayed in each analytical run. ) Analytical QCs were prepared in Chinese human plasma on November 5, 2001 and stored - ina -20 C freezer. For each run, analytical QC levels were. assayed in duplicate. QC Concentrations (ppb)* 0 Analyte Low. Medium High PFOS 5.83 126 331 PFOA 4.32 144 384 PFHS 448 156 417 PFOSAA 4.50 151 401 PFOSA 4.00 150 400 M556 --MM570 0 4.00 440.000 150 400 s15o0 440000 c*oTncheenttraargteitonQsCbacsoendceunptroantitohnesperresis4t.e0n0tplpevbe,ls1o5f0tphebaannaldy4te00inphpbe. hEuamcahnapnlaalystmeahsaesddiffrent QC The internal standard (THPFOS) was added to all serum samples (except Blanks) for a final concentration of approximately 200 ppb. 000609 Page 11 Northwest Bioanalytical ReSptourdty NNoo.. NNWWBBRSO0I0--14555 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 turboionspray 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. J 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 limit of quantitation. For all analytes except PFOSA and PFOSAA, at least three-fourthsofthe calibration standard's back-calculated concentrations must be within 15% (+ 20% for LLOQ) of their individual target concentrations. For PFOSA and PFOSAA, at least three-fourths of the calibration standards back-calculated concentrations must be within + 20% (+ 25% for LLOQ) oftheir individual target concentrations. A calibration standard will be considered an outlier ifitis greater than two times the acceptance criteria for that standard. ) 000610 Page 12 Northwest Biounalyical Lower Limit of Quantitation RepSoturdty NNoo..NNWWBBSR0O0I-115455 The back-calculated concentrations ofat least oneof the duplicate lowest points in the calibration curve must be within 25% of the target concentration for PFOSA and. PFOSAA to qualify as the LLOQ and within + 20%of the target concentration to qualifyas the LLOQ for all other analytes. Ifthis criterion is not met, the next level is subjected to the same test and the LLOQ raisedaccordingly. Quality Control Samples Each analytical run will include low, medium and high QC samples in duplicate. The `measured concentrations ofat least two-thirdsofall analytical QCs must be within 20%of their target concentrations(+ 25% for PFOSA and PFOSAA), and no two QCs at the same concentration can be outside the limit. Ifstudy samples require dilution, a dilution QC will be analyzed in triplicate for each 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%ofts target concentrations in order to accept diluted study samples at that level. The dilution QC acceptance is independent of the undiluted analytical QCacceptance. 4. RESULTS AND DISCUSSION Serum sample results obtained using plasma curves for PFOA, PFHS, PFOSAA, PFOSA, M556, 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 to 43% from results obtained using human serum calibration curves. These data are reported in Assay Revalidation AddendumReport NWBRO0-122 [5.3]. However, in order to obtain the lower limitof quantitation of less than $ ppb required by the sponsor, it was necessary to use plasma calibration curves. ) Percent theoretical and percent bias are separate calculations determined from the`mean. Therefore, due to rounding, percent theoretical plus percent bias may not equal 100.0%. Pages 000611 Northwest Bioanalytical ReSptourdtyNNoo., NNWWBBSROODL--114555 Each accepted run met the acceptance criteria set fo the calibration curve points, for the lower limitof quantitation (LLOQ) and for the analytical qualitycontrol (QC) samples. "RIuDn PRResOulSt PFResOulAt PRResEuSlt FFROesSulAt A| Commem Accepted Accepted Accepted Accepted 2 Accepted Accepted Accepted Accepted 3 Accepled Accepted Accepted Accepted 4 5 NA Accepted NA Accepted NA Accepted NA Accepted Runssabmploeprerpartatioen rdor 6 Accepied Accepted Accepted Accepted 7 Accepled Accepted Accepted Accepted 8 Accepied Accepted Accepted Accepted NIA= notapplicale RIuDn PRFeOsStA ReMssulst RMess7ul0t Comments U Accepted Accepted Accepted ) 2 Accepted Accepted Accepted 3 Accepied Accepted Accepted 4 5 NA Accepted NA Accepted NA Runaborted, sample preparateironr Accepted 6 Accepied Accepted Accepted 7 Accepted Accepted Accepted 8 Accepied Accepied Accepted NA =notapplicable Any known circumstances that may have affected the quality or integrityof the data are. included in this report. 5. REFERENCES 5.1. 3M Company Protocol EPL-0016. "Identificationof Fluorochemicals in Serum from and Elderly Population in the Seattle, Washington Metropolitan Area." Page 14 000612 Northwest Bioanalytical RepSoturdtyNNoo.. NNWWBBRSO0I0--115455 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 NWBRO010-8. January 24, 2001 $3. C.Sakashita. "Quantitative Determinationof PFOS, PFOSA, PFOSAA, POAA, PFHS, M556 2nd M570 in Human Serum by LC/MS/MS." Assay Revalidation Addendum Report. NWB Study NWBS00-040. NWB Report NWBR00-122. 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 confirmation of Sample Disposition/Retum Authorization is received from the Sponsor. 3M Company will be notified concerning final disposition } ofrecords at completionofcontract obligations. Page 15 000613 a es Table I. Calibration Curve Summary for PFOS Quadratic weighted 1/x'. All concentrationsareexpressed as ppb. Run A c LLOQ |[ULOQ [[5i3oewrsts01|[e5 TToomoon[[oowwwss osoo m||oomaenes||55n5577|]s aa11|] [63a|sooomon [ous owoms omer|557|a1] [I so] ToCsowror[coomoews]seorns[EoEm || S e ATIeT [wwA e|| ! `A, B, and Care coefficients used to define the calibration curve. 000614 Table 2. Calibration Curve Summary for PFOA wT Quadratic weighted I/x%. All c concentrations are expresseads ppb, Toa oro [N[[iosvorvaatetoo||n[6 55ovTToooowwaotounnotstr [[[oooovouoosras[[aoomsomsse|ooowmoeemrn|||rrreesavs | svvi1t]]| [[ii6soovvaattoess||57 JJoovoomon[Toorwna[a-omzoomrsee[|oomra ||reevs| oarr]] [esmn]] Jooomwoono[voonwsse oammoomrse[|o-omseorrs | |] ] C welR 1 C TTwo osy [owr [I ea T |] ] 000615 Table 3. Calibration Curve Summary for PFHS `Quadratic weighted 1x All concentrations ar expressedasppb. al II I PP [[[ie1eo%svoont|||33Toooomoomnrnf[Jooosmoossnoes[oamosamurse||a_asssmreosr ||v11s3365e||5||| [[r1s5woovvzzooto||7sooooonoosmoer [aomaasrees |oasssm||11556]55|| CSCisseoel]t mTToJowuoom[mo[fwooomws[ s osT oawra s]asvorum s ||o]| 000616 Table d. Calibration Curve. Summary for PFOSAA aTe r Quadratic weighted 1x'. All c concentarrae texiproesnsesdas Tio ppb. Tog [issorz|oomommo]r [aousss fieso|rzm osomts ([vseoml] TJoowowwonr [oToomommes[[ aomeeo]oosom s|| | m] a , C rev] PoToo o[--o-- rr{oraws-- [r os--T |T | i 000617 es Sy Table 5. Calibration Curve Summary for PFOSA Quadratic weighted 1/x". All concentrations are.expressed as ppb. [osRNuonvaDaitoer| hR1uen [oweAn [cams omc |ows|L1L6O6Q| U5L0O7Q] [[N[11oe5N%voevaraattsnoosr||]csooTmoomoonno |oooooomrorasTTToooomsnisa||oaosmsmre|||111600000 5s0o]] so] [o(va1te6| 3T2ooowv0ore2[[00o0v10e16nTooaomvmeo|oos m|| 110e0005rs0o]] [S[imsso] we TTToaosvowwwooonrr[TowwooomirenrTo[omoomwrmmms[[[aaoamsms| ||||| ] , CAFTTT----T ------T Page 20 000618 SR Rvetsnges Table 6. Calibration Curve Summary for M556 Quadratic weighted 1/x'. All concentrations are. expressed as ppb. A c R- LLOQ [ULOQ [[i1o3r3i[|5sooosonmor||coommrsrees [i5ovator 5 osomor| some ascmee|aosmmer || 223500]| 55005 ] [i6%ovato |5 osowor|woviss[aonisesors |230 |si] [vesmo]l oToowotior| coovnvee[[moommma[]aamss | || | C [rer] T TtCwoeT e| wieT aoem [Toso | T Poget 000{1619 Table 7. Calibration Curve Summary for M570 = Quadratic weighted 1/x'. All : concentrations are `expressed as ppb. Toe oro [oreN+umbver| oom Towne| sonar|ase|i or] f[iioenoeovvaonrror||5eT|oovmoomesTTooourrsmn|onooorse||aagsesso|| s11o0o | 30010]] [[iivveerv3oir]0+|7 oooomtomJToomoanra|ovoomimrs||aassssme||"sa1o0||s5r01]] 7 I so ToCmTom Toemey0s oomA eers[Eoorn |] , CoJrT11s--1 -- 1 000620 =I Tee wo ww so Table 8. Back-Calculated Concentrationsof Calibration Standards for PFOS Quadratic weighted 1/x'. All concentrations are. `expressed as ppb. [CC oomamtaT [| 3Tse5aaee[lwwoearv[[|wuoooa[|aowoJT|asosv[owossn[|aanvTTooaear[|oonm]]| [s[ si [5TooT rw[eTaloows[[iosx[[aooo seT|ooewirseT[[oonasses[w a|TTooonrr||o3sro]]] [Ct[ ostsrmssaoI r[|e5TTeasoenr[[saoaom[f[iooonnnJ[oar[aaann[[oawsnsas||aamo|Tono| aari|] a| [[ irs1|7TTeo5e0n[saasont [Ttiooor4[[[oo1no[[soaiswzT[omoeasr[[aaonTnisonu sarr| ao] ) [eC m1 TTasT erTfeoanfTT usef[oov[[wooreT[T oassT|aoT weTToaT nn|aar]] [wesaoll [ol TToaa[[[vuswaw[[uowwnT[wwooew[[a5or[[T5a0os[oooanTF[ooooo[ara]]] [C oo lT ToaTwTooe [oaT[awrTTaao e 5Toart[aar] 000621 Table 9. Back-Caleulated ConcentrationsofCalibration Standards for PFOA `Quadratic weighted 1/x". All concentrationsareexpressaeds ppb. (TowRsonior| I {var seonl[oi[woas|r os| Tis[om Jose [oo[mn[wor a aor[ne]| [[v[ eoretim||5+1T i0u|aasmos|o oowmwoa[|omassei[[|osoo onruToousr as n oo7wn[|aonine]]] [verti |5TTowvoar[[[wowiawrT[[oo5nm[[ovao5oaoT|oosoeerr[[oooevrre[[ao0mw|o0r[|aari]]] [[v[ seoriaw[| 57T 1|vvsatr[|[aaos0wo[[|o ooormm[[2sa0ss7o||oows nsoo [T|owuos [a0o6e [[oosnsT|[ao]rr]] C [[ SmI s Ton w [om[eoo m[T aaossoT[oaoarT[ooomsees [[Taaann[|| T9a[aor]n]] [[ C sol Tv ei [TT ooww[e oaT smm[wvT ro1[[raon rr[[sT or[eoT wt |[aeT [[o|r] C [[oewi l TTToeornf[[aasrel[[w ssaa[[owor[[oow ns[[awwalaTawrow l[[w55l[[aa5nr]]] tt 000622 Table 10. Back-Calculated Concentrations of Calibration Standards for PFHS ntt d a Quadratic weighted 1/x". All concentrations are. `expressed as ppb. [[C oommnaenT s]5|TorlJJaeooon]|wu0a5[|w0s7[|voo[r[iomnn[|amnw [[wwaoe5r]]] [C C imoT ]5o T Joos[l e tor [wsaosrn [[ooe 5nr[|imomo a[[[aoomns T[oor anroor]]| [[[ eevveon]]e sT n w[[waonr[e uwaos[[Jmvwoeso|[soa rira[T[oamsrJ[aoawml T[ooen]]| [mC ori1 ]7T[eowfT[eoannJ[[wworen[[aamoosrT[[ooovroe[[omweno[[oawmw[oooono[o]e|] DC [eI van]+TraT e[e50TTwvoT sTJT e20e7 foovs[Tior me[|aaow[aaaor]| [ [wsea]l Toe us [TTasownos[[eooween[[|a or5ass [[Joaionre[[aonae[[r wsso[[asor aose|| Cead l T Tworl[waeo r lowsJlower [liwol[awvlaurl[oaalawr]] 000623 Table 11. Back-QuCaadlractuilcawteeidghCeodnc1ex.ntrAlaltcioonncsentorfatCiaolniabrreaetxiproenssSetdaandpaprb.ds for PEOSAA CEevsoEio R[tEoJEw|Ros[Ewn{Eov|R[Roe|E|E] [C C ovomoT T[3T1wwaoiTlaeew[[[ooosos[[ao3o0rss[[[ow1tro [ownroros|Taoeoo oaow|Tora]] a [oi] [Csivssooritoor[[55 |ivaaeorJJasaornmo[[[arnsoasm[[|o0v0o6[|[ooonosrnJoimioo[[[aoerms[oaess|||rr]|] [tC CwoT T | TovooJesonuoJ[[ooovuw[[oo0oesr[[owoson[|[moiwiwn[[|aaoa[onoarT|onrr]]] [em FC istoT r[7 ovaanr[[asan0we[[Tvwaoa[oosneio [[oooeJ[onswaT[aoosmaooer|] orn|] C CvT e vT eeT [waT [[wT merT [easTe owTwa1eoaTa]] sol Tom oan[oem[a9[onJem[aio mo |oir| Ceo al TowrT[oooT[anrT[owrT]w owTw ie] Pages 000624 "Table 12. Back-Caleulated Concentrations of Calibration Standards for PFOSA Quadratic weighted 1/5'. All concentrations are. expressed as ppb. [(e[C eeroonT|dgT,Tf[eooonson|Twovoa [[TTevawaTsamrvsoT|oiaoosrTooar[TToaaaTTTTooonoToaor]]] [[eormi]n 55TTeoiwooTe losw[Teuoowle|TTeosef|rsaearo Toao||TaoooriTTTeeoaaaae]]]] [CEnT|eTTeeveso[lvean Tiawmia[omrsolaror ow oonTaoaTaoa ]] [[oormn]|v7TooidoTaoweTToonn o sao|r aDaoorrr|TooareTTTaotorarr]]] ) few we e aie a aTaEe e ae a C meel TTwolw asT T eTo w ewa Tareo TtoaTTs aae]] om Page 27 000625 Se Table 13. Back-Calculated Concentrations of Calibration Standards for M556 Quadratic weighted 1x'. Al concentrations are expressed as ppb. [C E eveT s| +Jaal[oww[w weE [w0|o0[w EwE woo[w]r] [v[C oivenT || 3[Taoossee[[Touoanr[Toa2sie[||o90was|T|ownars[[|aowone[owoooo|owre]]] [mC C moT|5 ooe wn[[awm [[ooswe[o [swoon|[[wn0[mool w[[oawmro[oo0]]] [[vC vemmT|| 7Joa eos [T[owomor[T[a2as0e0T[[o0suss |onwwaeo[[|ooanww [[ooaomr|[os]iws]] [T oemT[3eeaanw T[owwo[[[aweoose[[[wosaiua[woworr[a w an aoowr[[or||] --svT o]eT Te owT JooonsT [ [uwTTr |T aor[iaes [e T iwse [air|] I e ol TeESTTosCoeO [[0wIe6o [T oeonT[C wo[oaI[ [5TIo[Ta |O ee Et Page 2s 000628 re ass Table 14. Back-Calculated Concentrations of Calibration Standards for M570 Quadratic weighted 1/x". All concentrationsareexpresseads ppb. [L i oveT n|=+T|elvmw [[d wear[[ooaw [|omoro[[Noolar[|Eom[E o5i8 [EorR|asnr]] [[[ oovmeen1 n||53 J|| vvooasn m[aaaes[|osooure[[[owmnoiao {|oosursee[||oiiooro[[aoaw [nan|erarr||] [i[ [ to |5T ast[[oT o 0nT|ossosr[[[ovw 00o[|omovano [[ow r oermor[[[oooisn[[[a o3on|n0o]]] [ mreevai 1 n||7Taevssoom[[aaaw[[[5oo0mi[[awosonot[[[oaaas||iowmn[[[oo3on[[[oa3mnm |ossrii]|] D)T [ [TT wT [aeamsn[[h ooernr[[aoo oosr[[|nora oe[oommooT[|ow snaor T[aanwn aosnr|]] [C se ollTo oonT e[]ewueT ss[[oownT n[[1wT 5eT[3er[T oseoTomT r[s1 s | I oswelF {Twro[[aos[I sarl[O 5oae [TE ooo[s aoETnT[saIa oiTsOaIa]Tr] ; 000627 a TET Tar]wr Table J 15. Analytical QC Summary for PFOS [rC oermmetmonote[] TT| Gsv5s.o83vopzpoT b| T n |Goow1v26irpepbT T r | Gpo3w 3v1opp]rb.r| E [C ooEm [e 5[eoET |m mT T] I CT C ees[5T[sews 1 w |wwmw T T] e ] E [tC eE mo [R 7T[sesT w N| T TwI] ] CC eremo [3T[ee aarT Ta w mT T Tw ] ] T esol TewsT |a eeT] i [He erwaetl] T [oo a s T |oaao TrasT]] CTTT] 000628 `Table 16. Analytical QC Summary for PFOA [C C eam [2TT[ooawnwT T w w |ww ww ] ] (tI am [5T[owe |n3 wm w | ]| (C evo |&T[oonT T|wm|iwe]] sm|7T[oeo T0w | 30] [eC ves [5TToonT T |mmn] mn] I sol oI w [NaTw as] [e[ miealw Ta om [|wawerw a ] | e]r] ; --_-- 000629 Table 17. Analytical QC Summary for PFHS - Run LowQC |Medium QC High QC C1Tow wo] TeeTwTw C TwT ww] C ToI TwTw C TeI Tw er ' CTTow[wr] C ToT [ww] ml Tw ew] [mem all T Tiw w00e [a aans[ea] ai]] Page 32 0010630 NorthwestBioanalytical Study No. NWBS0014-5 ReportNo. NWBROI155 "Table 18. Analytical QC Summary for PROSAA All concentetions are expressed as ppb. me Lo] as [ae] Number| 450ppb | 1Sippb | 401ppb [Prepasion ate] [05-Nov-2001 05Nev2001[05-2001 [osvovaoor[1[sot[si [7] [[Te [ww [s ew | [odorant[2[506 | wo [wo| [[omevmo[5[eonor[|Tiww T|aaw|] CF omo | 5T[oosT |ww| ] wm | MC oma| 6T|eosnT w |[a a] ] CT ove | 7Tw osT T [wwom w] ) MT orea [5ToenT T| mm0 [Tonw]] C TeT ww r rr 1 r --T [v T ase s [| ww [l wr | [s [omo [ oo[f 20| [wo | ws[es | ss| [[oem | woisr | ior4c|awo] rs| [weal [1T 26 [| L [wwo [wT ww] +> 25% deviation fom theoretical ) 0008631 Page 33 Se os Table 19. Analytical QC Summary for PFOSA [(CoFtrosorvmamosn T[ aNmummbeer||7 s4.0i0psspb|[r|0 i1v150mvppb][|0 i5v40e00sp5p]b|1 CT EE CTe EweR a] C CaoT[TT 5To0e T waar]] ww ECT eCeE [ReEe oEnT w I |Trea|] CC C ivevmor|7TTooswweT T Tw owrT i] Cr oI mer |Ta 1 r w E1 OIa 5] vseol el TTTowwm[w ws Tw 0] [C ComeaellT T Ts n[wosa ot5T ] wi] J 000632 =TE [Es[ne | Table 20. sions Analytical emt QC Summary for M556 C[oFmomponmTioTntTu5e4.0]00p--pb|[Goo1so500nwppsb.o|Grtw4o0n0 eprpb]]| [oon 7Teoww w wo a e ] TenTe a] C E T T ERTo NoEwT [ TNww Ta wNe] Te [ovveemn[|7eTw o0o [|w wae a s] ] ] [T omare |v e ao |w ww e] ] T oe T Te oT |Tw Tw 1 ww ] ] [wsm eol]w eow0e [s es nn w] ] mo] C we oTrewmT T[awo T5w] ] 000633 `Table 21. Analytical QC Summaryfor M570 EE er Ey [{oPsrespoartiaoonoD l[71Tu aNowr200[1 o 05 ww00[ 1[s 5o| v201| [L oon[72T[essesT | aeee| [wawn|| [No[ vator [T 37T220a 5T | w ia w |aas] i] [T [Te wTw | [[ snow[T 76 Taoe | [hwim [e |wao2 || [s[ vozoor [77T Tem | hww ww [|sao] ' [r[ odovzoor[T 7s[7ae [[iwem | a |5any || [ [T 1 e [w7 e[e oi] [ [we TTs oeweT [ sw o n | mw0n|] [m[swme T Tir[[oos esr | wo|| L [m T7w 2o a T [asw l | ] 50 | 000634 Northwest Bioanalytical ReSptourdtyNNoo.. NNWWBBRSOOI0--115455 II al ol Mal al Wall `Table 22. Serum Study Sample Concentrations All concentrations are expressed 2s ppb. Name [[iisossT [anr s TT<eLii0o0o((10o0n)[S0t0sU| S| 4e 73 | |<rwosqase[<<ottoo@o@ms]n ios wsTatoo [ssIme Teroq oo] sn te | als | a0 ||<5io9oig[lm<iooooaessnn]] ll iar] 3a] ra [Ise [ass [is[7558 T<L00 (100[<LLoQ(sh <1060 100[LLOQ 50 295 336 | 267 | 323 T[ettttoqoo(2a.5m0 l[400r6a(1s63]) [sss[32 [se T7523 <irro0oq((0o0o[<<ttiroououssnn|| 46 | in 467| 3a [<mooes] [<iioq@so] im im | [isso[74 FIs [553 T<Ll00(,00)[ aoa(0) 241 [396 150 | 394 | |<i7t005(1[36t) <oLLooo(@5s0n)[[<<Et0o000 5%] on] [ise [oa 11343 Teri00 0] 150 [ae | saw] am [aa [see eis [[iiibsiss [[ssaess TTa<t1teo00o(o00o[s10s7 [|73ise T<1100 1.00)[SII0Q SH _466 | | | sn soo 152 |sor [aa] [eiioo@m] as Jettoo@sn iis j J [ [H8E[5ie7s TJce0oq0u(1o0n0)|ia0e00|] sei 284 [iss [aes Tarioo(100)[<L00s0| 42 ||<isi0w0 38I]<oLoooeason]| | 177 [<io0eso| i| Ta] is | [[i[issssst[The1 si TTe eeiio07 aq(tLoo0o< o0)])<"L1 a20Qsn1t | 503|_0 3_231s760|<|1<tsII06a00((13366[)<<<rLLLiL0oo0ao(3s20o:5)[)[<Li0t6o30a55o00n1]] [[Bisse[[iassTT1<1ti0000(01.,0000) 350 488 | | 12s soi ||<iti0s0(s36[<<Ltrroo0osasoo| [ise[507 [<1L60(100)[SOQUSO 949 | za [<itou@so 241] is] 12] FisTies [is[252 T[e<i0t10o0q(1000)][<02Q0 S[04109 | | 210 10> |[<e1r1t0o0o2@s5o0/0o0 r03]] [ise[er Temoqao] 15 | 63 ||<8r5o0es0]|<toooo)] [[Fsies steTTs iiemzs TJee+tr1r0oo0oq(qq1.oo00n) ]<I1T0eQ7z(1| | 30121a56s87s_| _||<3t1o6o9qsn||]<LaL20s0s (25| 0]) <LiLi0Qes(10]]0)] [ses [eo [ose Tio Tetoqoo] Tetiooqo 550 | iss | sas | 2a eis | 213 [<iooase] sie [atooas] am] L166| 96 Tetoquon] 16 | si | wa l<iooase] as NOTE: Ti(nhde2iv5mi%edutfaholordrPeasFucOlcteSpmAtaaaynncedexPcceFreOidScAtihAes)QaotCfeastchtcheeaptttatrahgneectmeecoacnsrciuetrneetrdriaactoinocne.ntTrhateisotnatfiosrteicaaclheQroCrmaasssotcibaetewditwhiitnhan2y0% |cSucrrvuesm msaamyplvearryefsruosmftoersuPlFisOoAb,taPiFnHedS,usPinFgOsSeArAu,m PcaFlOibSrAa,tioMn3c5u6rvaensd(sMec7R0esoulbtssiannedd uDissicnugspaliaosnmsaecctailiobnr.ation Page37 000635 Nosthwes Boas! RSeupodNioo MNWWOBSROG0L-113535 Table 22. A eh Serum Study Sample Concentrations (Continued) [FoNoere[57 [[sssos1 1a7 [Ss1i2oe0o0oa.ao0mo0|l[w<s0ae0oa0o1ut5is0oo)][<L0000(1| 3%)<Ti 00 038]|<-LLio0e(a3m0[-arisoaatisg] [[E ForTEonm[[aessT[<oioooGnoono[T E ]Saoses(3E 0 as2Y5ne7rO[T|iiiams) [a0i[Jia7aoi7ioc.moo1atenm)]]--Ttaoon ]] [[[rFolTosEmreTTTiaelo si TE<<<rttiioooe0o0Gqamoomnn 4S1IE10oYe30(803:00|7]NEi3e5Esw2C{T|sa7ioosET)||E<s<i1ctiii7ooo10qo(c0taa)unm[i <i5 iiooasu] ran] [rToEm ns E siooC aon] E2Ea ewTTsNJ7 aootXem i]| [[3FasseT176209.6 [Fmms 65510 I|<<<Ci1ro00o00.0a0..m0000a]<tL0o100a00(t(53m00])7]_2es91o7s Termooasn] 16 [5m |||it30s309s4"30J|]a<[t1i0o00a(tG3a3n0015ot0oe8afrroaa]] | is Tart [[) [u8ism8es TTZo5i0se2sTe[io<irrod000on0.o0o]0[[<<1s200i0(z1.[500)]sa4m2ss |a5s 3J4a0io[<<oriaitooaa0(anaanlnmsa[i!rt3aees4eeen4am]]) [sI sws TTes sT TToerooonaS ]ml2inss ||Y osomrTi3Y e6 JTaixlmso0tmanmilitioseua]] [[ForFosisstT[ois1 sse T[T<~<ririiooo0o0(uaoomon[l[<r<coioooootssnnn]]] iassss | aisns a0 Tiss [os TesTuocuml 20 [oT 3a [J|<isiiiooooagtaaeammnlamTiaaars]] Taiocon] s [[[oBlssrsTTe2i7sTTs<euirioooooodaaoomoo]]<tsisoieossm|] sesosx T || si 4as TTdaiiiiiocogaenennn]|atireoeahet]]] [[Bli1ss3%oT[202s1y7TT00r1o000o(0n00]0010020a3103|]052s0ss0o Clio TsTertooaoo sa [sm |<Ioi0or30T]i<liooe [elton(36 og anatooaatio]n] tat] 1si Tatiostoam NOTE: TSh2em5e5thlordPsRcOsSpocaend RriOe aSeosfAhae rheenmeesesncsocemTrnioonfmoc,h QCotkb as] wiibn22200% individual result may exceed the QC acceptance criteria. J * CesSerum vary om sample results ess obedience for PFOA, PFHS, PFOSAA, PFOSA, MSS6 and RoM570 `obtained nl ol using plasma calibration Page 33 000636 Table 22. Serum Study Sample Concentrations(Continued) [il1i1e4[0s2 TStasrT[asutcoouo]<a0os| n 663575| | issuo Fee[204 TeLt00(100)[S00(30)] Temooass| Termooasn| my] sor] TO EE 299341 {Toe [dos_[<L10Q(1.60) S100(50) 336 | ws [<tio0aso]<LL0Q (1.00) 7-5) | <tioa a 0) ireair] Filsor 06 [tos [0 T<i1i0000(1000)]<tr2o0a6us| n 375070 I YE eT)BE | 700 ass Termooso] tor] <troo(eso[ron am] [si EaN s <tT oo(oY n[333 ST 71.Y0E))RYrTE | |<itoo em] im [<roosn]<LL0Q (160) [iz [iat [ila 32a6sTT1010010(010)0[[SSLTL000Q M5S0D]] 314 444 | | 57 a0 <tiooeso ast [auto(50 [S0013)] 0T2000(1.00[S00U0) 344 | 63 [[aissT2e1a T<1r 000o (1.00o [S0m 0(3| 0)] 29458T[e <i0n0 3J0[]ae<tciiooeaataesnsn[]<<cri1ooah atits]n]] EE EEE ET)7 ES YY NE EX [iissT7263 Tatoo] 2m | as 17.3) | issJaEtiXc .)RT :[Flilaa[r77e57s2 1T1et1t6o0oa01o,0o0[l St0o0s0|] 227 676 | | 200 697 oasnl Th] [<iioacaso[ iss] fatoaaso] 3a] 637) Fis1 313 EEE 1142[5 IST [T<<LI1000qY((11.U0000)))[N<SLE I000QT ((is5n]] 43.9403| Y |<I50Q5(1136)[E <<LLiLX 0000 3)5[9000100]| F[haareT [i 2s 0 TT<eitiooq0(1o0o0)[[ssooeoissn]] 260 | 6:2 89% a6 (250) S08150] [eioa@snl ads] Jaioo so en] EEE [iki [297T0600(1000))[SEOYQTH3D]E atB | [Is0[4111100(100)[<LL0Q150) 405 | sJ rs [<7tioXo ) so[1a]| 215 [3 EE 6 TTaY too(Loo)[<LLo0U0) 256 [170 [<tt00250 [sion(roo) [<tiooaso agi I JTX) EK [sor Teimoeaoo] EETCET 1s | 6% | am Fis ae Te0i0] 314|37Tis <LLOQ (230) Taiooes] 615 iis] [ite[196 T40001.00)[<I0Q(130) 282 [<itoo |<0100(39) <LLo so [00(10 30/1100 1.00] Page39 000637 Table 22. Serum Study Sample Concentrations(Continued) l i l Wl ilWl [sFrEToers [[00o0a.t00]<05Q950|] 3a66 [ows[100000 ss | 556 <i60036]aoa ||<isiomo30][<aLriooea(a5sm] oa] 1s FI ise FlinT7203 <LL00(Lon [<00 G50] T<10000.00[<L00Q 50] 358 | 205 430215 [<tioaas0n)]<iiibeassio]] [<rioaeso]<roatas] [iss a2 EY e00e0(C1.00[N<L1E00(50)| 1st - | 265 [<itoq so]<riogian] 17) [ites m2 Fs[117 T<0000 4100 ((11.0000[<<LE000Q(SSO 012833 | |<LL50701(136 <LLoq [<Ito0 (2.50) (250) <CE0a <LLoq 155] (Lod [Firssser [ [02 4 <<i1i1o0o0((11.0000[[<<LLrL000Qu505)0]) [lies| 154 T<L00(100[<EL0Q 50) 345 295 278 |[<i73030(13[0<<tLiLooQo(@2s50m)]<<LrLoogg(aLasos) ] [<it00(36<Lto0asm] ii [s Pisos [|65687 TT2e1w0o0o(1o00n)]L0570s0[]503.s8| |i 269 |atooesn] J=rroqaio] ] za | ast] [[sHiz st[559008 <20111000001(1.0000)[[<<LL00QQ(15500)|[428.475 [rssT7506 Tetoo(oo ass [as | 130 |<LE00(130 [<rLo0(s.50)] <Lo0 (2.30) C00 (00 <LLOQ (100) | wo [<moo@sn]<ioo on] ; [[iSisss[0 6TTa<itioooo(oo ain te | ais 24s I|<<iiitoooo(w3e8<tLooaoeo]<Liioad1s00]] [lisse 1ios [liast [7b [[e<00t0000(1.1000 0224001| | 134123 [|<<Lt1t0o0o(1u5s6)e|<LLz0Qe(2.5|) <LCi00 (m1d]) [[liasses[[4o6o1 T/<<tLi0o000((10.000[<CLi0sQT30|), 376 481 ||<ii5o25o00|[<<titoo00(@2.i5m0 ]E00s(s100]] EO EET EYCeYYBEYY TS NC TYEXY 7TEX) TI | F[[liT ie ssee [[77216s7"0 11e210000((11.0000[) 5 CO214Q56U5S| O| 30e0 3a2ss | | | za1s7mo00 J|[eeatrirrooooqG@sssooo] ror] ie in] [lise [irs [lise [7556 TT4<2LL0000((11.0000[<E2E00Q0(3| 0) 424909 ||<it040(136)] <[Latrot0oao@ssoo | zw] 17s [iE sa [E eerSTele t000.Y0S0277 ES | 6s | 1J 5 [onaYsEo|)sYmT ] [lise asi Fito[320 TT0e20000((10600)[[<1LE70Q7(150|) 396 181 ||<L7C001(136) <<LtLtoo0o((22..500)[<Cit0000 ((116000| Li Tey T1200(100)[E00 501] +22 | 356 [elo(50)C00 (1707) individual result may exceedtheQC acceptance criteria. ! * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration _m 000635 Northwest Biosnalyical ReSptourdtyNNoo., NNWWBBRSO0I0--115455 Table 22. Serum Study Sample Concentrations(Continued) Al concenttion ae expressed5 pb, [rann| Tss al <[ti<ooqL.0L0[O<uiQoe(5L0]OO5s6[o0<| |LL3e O66QJ|(<<tLLiioSoa00G@as|m0| 3i3er [iFiss 7e[136r5aTe0t000q0((110000[[<<LiL00Q0((510.50332519 | 5m Iettoosm | oy] |<Ii00(139 |<Lioq 2.50) roaiam] [isn[ns Files[asa T<tiooaon 1a | ev | 5p T<L00Q(100) [<CE00(50 sat | 650 Jaiosesy] i1p34 ] [=iio0aso] ism F[iossms [[a2e6s0 TT<00000Q0(1000) [<06I0Q9(| 30477262| | e ie Taiooasol isi] <miooasm ino] [luss[zT1o57aTTa<r10o0o(1a0o0n)[<112050(015[0|es3.i15 __|[<L0006(136[|<<iLtIo00o2a5s0n)]S1 LOG(]| Filsss[7725 [sssT7506 Teitoouon| 766 | [1100100[S00 (30 | 720 421 [<tioousal aw [im] |57m [<oo@se] ior] [Lsl8a6r| [7557138 T [11S 00O (100)] [<LL304001| 50] 366605 | 155 3a ]<IL00 (2.50 [<T60 (0) [<iiooGsn| 3m [iss [52 [1158 [214 J<trooon| 1s | se T<1L00(1.00) |<LL0QUS] 301 | 5m |<0100 [<ooesy] re] (136]<LL0Q (50) far )[10[06 [is ois Tattoouon| T<ttooon| 261 | as as |_tos [<ioouaesoso] | sam [toes] 3s] iso] [2 502 Fie Tas [<t100(100[<0Q 30416 T<tioouon|12[ans [5.2 120 [cioq@so)] [eiooaso] Ler] 1s] [ss m0 [riesTse T<tiouon| J<tioouon| ax |_ses |e aiooesn] is | sm 1515 [<oo@s] zm] iar] Fs[775 [ior 1764 0000] 1s | 1100 (100) [<SLL0Q(50 se | 550 895 | 227 |<1100(250)[<LL0Q aH] [<Lioq aso] ia 1498 [5a2 1499 [570 ISLLoquon| 251 |3m <LL0Q(o0)| ssi | sis | 27 106 [<ooeso] [<tiooesy] ies] im | F[s11o50r0T17210752 1[1<011000Q((11..0000)) [|<LLLLO0QQ((115300))|__2|2__3196 |<I100 (136) <LLo0 250) 160 <L100(136)[<LL0G (2.50)|E00 (L651 [se 77561 so [505 Tetoouon]" 1st | [<0t00 (Loo) [<L0Q(50) 6s 352 | sos | 35r [<itocasn] I<lt000s0] 6s] Tio fisos [ios <ti00100 [soe "a0 Teitouon] 229 210 [ai [35 | 30 |e; Jettoqasn| [<itoapsn] zor ise] [sor 752. [68 [263 T<it00100| 231 |_38 T1000 (100) [<LL0Q(L501 257 | zai J<tioq sn [<ii00 36 <Ltoqa0) ion tas] NOTE: T(h4e25m%etfhoordPaFcOcSepAtaanncdePcrOitSerAiaAs)aotefstthheattatrhgeetmecaonscuernetdractoinocne.ntTrahtisotnaftoistiecaalcherQoCr amsussotcibaetewditwhiitnh2a2ny0% individual result may exceed the QC acceptance criteria. ! * cSuerrvuems msaamyplvearryesfurlotsm froersuPlFsOoAb,taPiFnHedS,usPinFgOsSeArAu,m PcaFlOibSrAa,tioMn5c5u6rvaensd(sMeSe7R0esoubltsaiannedd Duissicnugspsliaosnmsaecctailoinb,ration Faget 000639 Table 22. Serum Study Sample Concentrations(Continued) [ [ [s SSI wl To ay 6 TT[4<a0Lw00o00e((ti1oo900n[]E105059G9A| D|] 516e622 | | | sn3[5 ai<torooonasmowetgas]] Fist [ses HEBTis TTeetmio0o0 a(1o0n0[S05000W[D]as507 ser | 30 | sw [<tio0oon]amon mm] [aro0ean ser] emooasn] 130] [ [isIt T [03645T<T1a1t0o0o1o.0n0[|<Ci00sQ(s30| Fists[576 T<0Lo0(100[<it00050] 212 297 585 [eiiooqag)[]trogen | ass [<tioa@sn] | a3 286 | 154] [HET 62 [Isis 850 [<iioo(00[<o0aso] Tlboo(100[00150] 9s 157 | 25 | 37 [ettoa@sn| Tas] |<oaasn| 14] <LL00('s0 [E00 (1a5] [is Tos Flo a aT<oiieoot(ooon[<L1r:ou2s0| )] s2e10 | 335 eiiooasn] |<iooqael<toaesn| 1a 2m] Fis [lisa es T7562 TT0e0i0o000(10.000[E0i00s(5165a3a6 ||<00n(i 36 <<LrLi0o0(o2:w50n[[<iLLo0Q(s108]) ETE [sae T7301 <000C 0(1.Y 00[<C00QN (303E 48 |A Fis [5T<ii00(100[<r00u50)] 361 | J 1TEX YR 17 [<Looaso) 131 ETH oad] ) [lise [isa eos 184 T[e+1u0t00o(o1o.0o0[|S0200m15| 0] 2s4s2i| [<01e 00(36T[e<<ulLiLL0oooa((2:ss5o0n[[[L<T6r00o00g116a00n)]] Fliszs [50114200(100[<LL00150 4 | 5 [atoacsnl a5 | [iiss HSL] 2i0o23 T[1<200000(L(0100)0[[<LLoL0oQ(U5S0O) 348 299 |[<I2T7001(38[[<<iitooq0ps300]00214500]| [lise[oe [Hiss[355 Tao00o0 te [a T1400(100)[<L0QSD| 188 | | 21s 14s [aoa] asm] |<Lto0 (2.50)[<E00(10) [F[liiiissses[[smiss2eTTT11022000000((101.0000])[[<EE0100s0(U03)|0| 262456352| | |<isi10e0(p13[9[<aLt0o0(a2.50][<0110505100|] [i538[354 [lisse[525 T<LL0Q(L00)[<LL0 150] 238 TL00 (100[<L0Q(50440 |<1L00(136) <<LLLL00G0(22.3500)[<L1T605(1]% | 23 [<I100@30 <LL00[100] [listo T7157 Fler [ae T042100000((11..0000[[<<tLLLo00Q(1550)0326265 ||<012010(313[9<t1t0o0o(i25o0)l<L0d6o(100)| ls | [HIZS (mils 409 62 T<[L<00I(1000[0<tLQo00s0o [5L57o79q|1(5sae0 0s ]Je[r<tioooa@csso]n| 200 zn 52 Teroquon| tes | as |<iioouseler | oaoes]m ! * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obiained: using plasma calibration pagei2 000640 Table 22. Serum Study Sample Concentrations(Continued) CT TE EEE YET YO EE EN E EENEYTE EE GH112[ 83] 2 Jsoeuo<tioqin] 3s | is Teioons Ee i | [CHE] [RET 4[4LoQUo0 520 Teuwoe on] 50 im | | 369Tim [<ito0(sonl<Ch2osi5am]] ass |<iooazal<tio tan] ast [GIIz] CE [CRD] 05 [<1400(100)[<L0QUF 741 |inn YJ YT [<7ttXoa5s)n Riro] a7 T0000 525 | ls [i000(39 |<tLo0 (250 [CHa CTE Tatoo is TY |4sTei Jatoousol[Sotneatm]] NSNS 7:10) ME [Ghz] [Giz [GHtIaos] ost 20; 163 <tioqion] 506 | T<1000(100[ST00SD] aor 559 ||5i100m(38][<<ttotqo(o:as5o0[Traoeo(tiad]) T<1000(1.00[<EL00(50)<LL00(LH 753 Jetioqcs [[ouStiHasIs]T2510.04TTe<rLitoooa(oLoo"oams| 1 s9a6e[[<3I00m0136e]<mLic00a(e25s0o[] L1o00mr1]]] C[CEHIE]E 154 C |<L10q) (100[<CL0Q(50) ) [SHIG0] 52 Tattoo(oo 177 | 2.55 eas |<ITY00(J136)E | <LLoX 0 (2.500) RE A | E00 1557]| ws Jatoensol : [SHIDO [Gutisoa] 21 157 Te<0tLi0o0a((1l.0o0o) [SE2L06Q(5181] ess |3s Jaticoqsn] tar 26] 3.17 <T00(136) <L000(250[<L0017] C[TCEHITT 505C [00) 100E Li | 37Y 3 J<ii00(36)]<LLoYaX0)[R <Lr06C 1100] [SHLBOS 117 TeL0Q(100 22s | 344 |<iioo(39) <rtoqsn| 1a] [SoHuitors|]5se7l T[a<LtLo0oQ((LoODo)[lSLL2O0QsUS| ) 339a2 | [<11i6s0(136)Te<LiLoOo0 Go5s0)o| 140] as [[CGHaIBoI]]s2s127T1110000(1.000[]C1EQ63| 6] 335040 [GBI]100 T<10000.0076 | 150 | | 1s 30 sm [<LLoa(250 [0611] TTeeirotooaossoo|[ iar QB Bd [CHIBI774 T<[100< 0(1.I 00[L00Q 0(500( ]) L 430487.||0 <L3L00 Q7(136) )T]e<[ LiLt0oG< a(2s.5o0)ELLa0 OQnm(Q T0]]5] [[CCHHIIBLI]] 5216a0 TT1<0100000 (11..0000[[SLtLLO0Q015500]] [SHI].T<1L00 1.00[StL0010] 439 | 275 3481 | 211 386 Tas T[e<tiitoooo(ssoo[]rosamia]] [<tiooaso 18 (SHIT"572 Tetloo(Loo) as | 3.56 [<00(30) <LL00250 [S000(iam) feats 000641 Northwest Bioanalytical ReSptourdty NNoo.. NNWWBBSROO0L-115455 lal ilt l Wi Table 22. Serum Study Sample Concentrations (Continued) Al concentsionsaerxpressed a pp. Name GHUSI] 31|<LL0Q(100)|LLOQ U0) 42% 255 [<o0asn] 15| [cGiGliHH a]II a 123111 2.0s 6423[|2 <<TLarLiO0 o0Qq(0u1] e.[ 0o(0lo])o) |5<L6L8 O6Q 1(1T .| 50|) s5e 6os"U | |5a25m m7 [<ii00 aso) | <Li0q (oo) <tooas [te] CRIS] 109[<0Q [GHIIs2276a][<100Q oo 294 | 212 (1[ .00) 26 Tass |<i100 | 5% 4| 36) <LaT005[33 t<Ie03s(15] 5) [aiooasn] 3 | [GH17Z 7 CRIS] 456 1100 (1.00) [<LLouon <1 L001(30)|25 96||<EeL0o0 (136 <LL00 ([ 50) ts] [<ioosn[20] [GHiGaT] 66 [GHIIs28] 564 [<10Q(o0| [<100Q (1.00) 231 | 838 | a3 [<LL0Q (130) 335 |<IL00 (138) [<iroo@sn <LLOQ (2.50) [amon (100) [<LLOQ (100) (G[ HII330|G2172H 83 [2[1Z <0LL000Q (1.(01.00)0)[|<LLLLOOQQ(1(.L5500))]322|<LLOQ (136) <LLO@[ 50G) is] <LLOQ (2.50) |<LLOQ(1.00) ) NOTE: T(h2e25m%etfhoordPaRcOcSepAtaanncdePcrRitOeSriAaAt)atoefstthhaattrhegmecoanscuernetdractoinonc.eniTrhaeiosintifsotriecaslcherQrC amsussoteibaecewditwhiitnh2a2ny0% individual result may exceed the QCacceptance criteria, / * rSeureusm msaamyplvearryesrulotms froersuPltFsOoAb,aPinFeHdS,usPinFgOsSeArAu,m PcaFlOibSrAa,tioMnScSu6rvaensd(Mse57R0esoulbttsaiannedd Dusiisnugapiloansmsaecailnib)ration Page ds 000642 Northwest Bioanalytical ReSptourdtyNNoo.. NNWWBBRSOOI0--115455 Figure 1. Representative Calibration Curve for PFOS AnisReRparmasison heozdon15Q:2UQA0D0RaA1TIiCC l-mWeoign3hi0Sn0gnForr = 1FvOoS3 5) 2s g20 2 Bs fu Sos 00 0 0 we mm me mw am Nomis Cone. Figure 2. Representative Calibration Curve for PFOA ) AaRReogrmas snionl! eaioodn~15Q-XUNAovD2R0A)TCIaCl-bWreiiognhSinugndFaar o=or1P7FO1A (5) Qusdric Linit= 4270 3s gs3s0 SB2s0 fo os 00 Rw ww mwme wwme Nomi Cons. Pages 000643 Northwest Bioanalytical RepSoturdtyNNoo. NNWWBBRSOOI0--115455 Figure 3. Representative Calibration Curve for PHS AostaReRpnrasieon tlhydan=1Q5-UNQAouvDa-d2R0rA0i1TeCIaiCisWtme=iio3ghin0iS0ngaFdorrf-or1PXH0S3pp) 2s b5 5s0 50 bBios 0s ao 0 P) x0 0 " Nina Con, Figure 4. Representative Calibration Curve for PFOSAA ) AntRRumepi6rssiyconeedsons15NQoUwA2D0R0A1TCIalCib.raWtieonSnagFsosror P1R0O1S3AA (5) Qed Limi 38 s i5 k oo " P 0 "wo 10 wo Nominal Coe. 000644 Pages Northwest Bioanalytical ReSptourdtyNNoo.. NNWWBBRSOOID--115455 Figure 5. Representative Calibration Curve for PFOSA AostaRReagninolnyMhodn 1=5Q-UNQAoDvuR20Ae0TICLCilmiewteai2gnh1tS8in0gaFanefrrdP1EOs8SA (pb) ' E8 . : 2:b ' 0 mw wm 2% wm Nomina Cone: am we a me Figure 6. Representative Calibration Curve for M556 ) AvayaRRegnrsiaolnyMzeethdoodn=15Q-UNQoAvD-u2R0A01aTCLIiCl-dmiWtaering2h3aiS1n0ig Fdrarfo 1M-SS36 (5h) 2s 20 I bs fo Szos o ww mo mm x ww mm Nomins Cons. Page 7 000645 Northwest Bioanalytical ReSptourdty NNoo.. NNWWBBRSO0I0--115455 Figure 7. Representative Calibration Curve for M570 Asc!ReRgurmsisonaMadaon=1Q5bUNQuAodwDoe2Rt0AieT1dILCCimoibtWae=ii1g2nh5i0Sn8gaFsoorJSoTrOy ot) ' 3i. b * | 21 | 0 ow wm Ww mw me wm Nomina Cons. ) Pagaes 000646 Nordwest Biosys ReSptodrtyNNoo.. NNWWBBRSODLO--115455 Figure 8. Human Plasma Blank for PFOS FEE HH [pErS-- = on Emil EE EE i Eon Jaa : ei BEE Ey ! 3I fm es J---- a-- Ea iia oa mii BE PA - BERANE SUE Sr Pages 0006437 Northves Biomalyics ReSpaorytNNoo NNWVBBRSOOL0--115455 Figure 9. Human Plasma Blank for PFOA - Sn = PE E m = -- PHY B = = Lb il neTh Ee wot =Ai = iT 110 Iitr Fi EE a ARRAN ERNY Sy 3 Ta e rosS PrEr e an E be E =d3 re -- === CEE ; i : * a ta dn Th ON Ta 0 Te bs Pages 000648 [---- Figure 10. Human Plasma Blank for PFHS RStuedyNNoop..NNWoWBBRSOr0L0--1t15455 pB n toeeeE nei) s ima neEdf .= wn = oe mm---- . Em] Te a : + J: iE fae RRA ELAR Sy \ = Ee) 3. -- mmEEEy=2 mere E-- =e]. His ol TT : = | ey SALLE ARARE RL Fagest 000649 Northwest Bioanalytical ReSptourdtyNNoo., NNWWBBRSOOL0--115455 Figure 11. Human Plasma Blank for PFOSAA = eS wo ee ) . m 3 zn d 3 SIT aEnN=EE ae ma racememe eR f pB= tE eem amrm )o Ea El JHlaeeleas obienas|| e ena 0 s agx HEE i opin pin Rome ERR RRR Cer a ear coro tem ill fee efe eaml ie] Ties 6 Jia 4 i 5 ; 5 - EEER EEEE E 000650 Page 2 Northwest Bioanalytical RepSoturdtyNNoo..NNWWBBRSOOL0--115455 Figure 12. Human Plasma Blank for PFOSA poE i ro es m m) m= Sa adh3 frail Sa=mII EE -- en -- ER te Emmy [igenteens anee m r BEEEwo h] TRE HE RR RS i -- maan So = Znmo felb=.2 mm Sa ffaaa]eal [onc= en] - EEE EERE 000651 Pages: Northwest Bioanalytical RepSotrudtyNNoo.. NNWWBBRSO0L0--115455 Figure 13. Human Plasma Blankfor M556 mo oenmenr tos = oar Sm apSEenssl rr rmvente ee oB -- r ea fare im TEEl nl Tia aCnla eeeEisn | fo Ze M1 ar siLm E :JAIEHiSARHTl ORII BL | SEEN ERA er ) ft --e ----n noa a EaunuE yre3ls240 FR Fr-- a =--] " isol | ited |= 2 SELL GA EG ) 000652 Pagess Norwest Boni Figure 14. Human Plasma Blank for M570 RSeupodNNoo., NNWWOBSROO0L--15855 = takDIOL TH= Gerad 1d 10 e ErlEee3y ---- -- atic Le) i wf olBN mi d ARAMA L RC ) = ELE we NEES hr meme Boh fio ome sone] . 3) % fem --ea [anc - HERR ER RANE Ser ) Fagess 000653 Northwest Biosnalytal ReSptoryt NNoo.. NNWWBBSOR0O.1L54-55 Figure 15. Human Plasma Blank with Internal Standard (QC0) for PFOS PEs Ss 5 -- ET eenedr on T. eiiaetl a : l:e TERRYEr ) T= e ro S er on wBeEsEt2 PEE F-- a B e= n ; Tia olf THRGER EERE 000654 Page 56 Northwest Bioanalytical ReSpotrdt NNoo.. NNWWBBSRDOOL-115453 Figure 16. Human Plasma Blank with Internal Standard (QCO) for PFOA e [----r -- e = sm ov8 ate 0 ~ 0en Eatmc aFedn Hr tn % a CHER RR EEE A er ) [T-- mE e mi Frm eefeme = ws= : eT rn |E =fooc=_a Fn | THGR DEE RAE J) Page 57 000855 Northwest Biosnayticl RStuedyNNopo.. NNoWWBRBrOIS-Ot1154-55 Figure 17. Human Plasma Blank with Internal Standard (QC0) for PFHS = --a em m H SoH drE e m_-- n ImeE= E l mr corms mee ~ on E= S E r EE ai Re el TR IR 1 ema Rl 7DL FB A SCA RET E AELE Ser ) = iH --_-- mma] 4 Ammen [eoEes--aer] ] ( onp c m gn) 2 eE TEAL ER BASE Er ) Pagess 000656 Northwest Bioanalytical ReSptourdtyNNoo., NNWWBBS0R0O-1I54.55 Ee =E=se= f teem Figure 18. Human Plasma Blank with Internal Standard (QC0) for PFOSAA -- eee nT ESEN=EE=n3 EE Eamelel s 3 CEE ao me a ) = pots fsI -- SEES --_-- eed mse amon ~ ren EEEE-- E u. n . Ere s | ; : fre CREE RAGA Pages 000657 NorwestBismit Sui No.Nwasoo.145 Figure 19. Human Plasma Blank with Internal Standard (QC) for PFOSA _ P= ==--=--tEo2eo--hEt==sE:k: To BB) 3H EEE ol AA i ! dl,i TOLfNY: TklHEAL Che NRE er ) = == c5 a 5 mm -- Ee= ooc=| SEES SER Se J. 000658 Notte Bioanalytical ReSptourdtyNNoo., NNWWBBSROODI-115455 Figure 20. Human Plasma Blank withInternal Standard (QCO) for M556 eg eeeseeeeeeseesmn. Ee 3 --_--wom orem meee en HH lL El Emel | wm wil wTs m Fo Tol il | il | bl i fil i CER ELSE RARE ! I T= Ta nEeEdE _ oan an = enaa3 oa r-- : Biees=] REET LA ay Paget 000659 Northwest Boma ReSptoryt NNoo.NNWWBBSROO0L-114555 0 Figure 21. Human Plasma Blank with Internal Standard (QCO) for M570 p------= -- Ewell 0 fe ET [emi] A Spi2s i mmm EGER E-- LS-- E S--r . ) =5 -- Tn egy -- == 3 foe m a] [anc Jn] ie TRERREEL Bh J Fages2 000660 Northwest Bioaralyccal Figure 22. Low Standard for PFOS i--_--d a oEmenm Eeeo=n Zioa, _-- WRe EI RdrEo aw ReSptourdtyNNoo.. NNWWBBRSO0I0--115455 a Eee = iesa So L Ee |B , P-- P=] = -- SHEER-- ENT ey _ ms are momen " rn E rE-- a 2 iy = [eoc=- Fil ERRATA Ry Page6s 000661 Norwest Boma Figure 23. Low Standard for PFOA = oEfee . Seen Zu me= RSteyNNoop.,NNWoWBDRSDrOL0--1t15455 =a a Brisa ) E ==E =a Sa e RE REReA -- EE Ei E== R Eo -- ge i fT == Clie 0 So te i Th Th er hess 000662 Nore Biss ReipoyrtoN.o NWWWBBRSOITO.11913 = = Figure 24. Low Standard for PFHS Ease Ey --_-- _-- BE pe EE] fens 5]| si) i& senassiEes fac ; Fae ) _ T= -- EEsEE -- AR er e -- EEOe EE=ERk r EBEeEtE e aSer EEE el SEER RRR NS er , rots 000663 Notts iol RSeoprroo NNBaRst11455 Figure 25. Low Standard for PFOSAA _ mE= FEnmeB n,) Sr5 SooEeIieEd E--_--mr eee= orn CfEeEmmGfe LORi i= Eh ENE E Shr J == Em E =E= EE =e Yne -- e Emme4 y Et. [ooc=-3:r] oe 3 te dh i BSR er 000664 ros [ST -- RepSotrudtyNNoo.. NNWWBBRSOOL0--115455 Figure 26. Low Standard for PFOSA J me l pm orn e e om emnTatedel} J en==hi T rar ar1meen Ty Emi er ---- Tie veils Ean fIEe Yimeat A Et Fa i =5 _ Pe R l EEy L Eis B E= E Ties 6 Ea HE : EERE EEE Pages? 000665 NorthwestBioanalytical ReSptuodryt NNoo..NNWWBBRSOOI0.-115455 Figure 27. Low Standard for M556 pe oemE-- E e Saen y m m movoaHdh JE ne wmaon=ee3 x PR -- FS-- Emit ie 6 salad HE 3 : :Z SORA RR er )y [a =me -- m 5 EEE = _oo-- sd=4 y mer ver moore . -- Ee == Cli dl | 3 ! TREE R EG AR Pages 000666 NorthwestBioanalytical ReSptourdtyNNoo.. NNWWBBRSOOI0--115455 Figure 28. Low Standard for Ms70 Er ri p = d reesei ma ----Er PnmnoedEee 2 Pa E --==: yo BE == i FUL A ), --_-- AEE RANE ey TT E --a ] EEF JE weSmmne e= Tm rn Em mike oe Fe--r 3 = EEm El ERE og 000667 Page 9 Northwest Bioanalyicsl Figure 29. High Standard for PFOS. I Tr menrte Earls --_-- "et PS ------ LG RStudeyNNoop..NNWoWBBRSOrOI0--1t15455 E fma eC=i=s--=oly| Hi afaS r E a WET r 1 = entef a=m Cn CSnmoalEne _ 3 pp -- Tn = 3 feea m] CELA ELA BR ) Page 0 oboces NorthwestBioanalytical RepSoturdtyNNoo.. NNWWBBRSO0I0--114555 Figure 30. High Standard for PFOA = =" Ti ES y emm-- Ee SE =ternemenE t =d: P_--I ty = mn Ei Eoac se fo Tn : : EEE EY ) -= I _ o= fS v-- wRa Emaf= 2e -- PTTim==e " ~ mn -- Ea :: E Ea u AR LAN ERA EG Paget 000669 Nose Bris PSeivn tsisnot Figure 31. High Standard for PFHS -- = e - E= Teoe= e El-E= r ---- eet E = sl h Bo E [a=na : ) = = An hd TERT er s Emmeer EE 2 GEREN ENR Ser J rer2 000670 Nochwest Bioanalytical Figure 32. High Standard for PFOSAA RepSoturdtyNNoo..NNWWBBRSO00L--114555 [r=nes-- tre] eeaH tma eeH fd _ mn fmo-- e= e lL y Soman vor cee -- EE GTi E mem s ] ra ae RE Sh 5 Co Ei of | sled CARE RE ESR er ) rm al JE I Iy J = i 6 ARERR RANG Ser ) Pages 000671 Northwest Bioanalytical RepSoturdtyNNoo..NNWWBBRSOOI0--115455 Figure 33. High Standard for PFOSA [--] =. SE -- mlaeannee owi ondveed 13 _ ePeg s5 * y an tr meen en Em soil Ee : Ve m Got | fo 2 1 LERNER EEL Sr ) [E S-- e m m = E mew 3 TR fooee yd=) =: re nm ere ---- a-- el Ei erieEl] 3 &a ae EH oF AERA ERAT fey Pages 000872 [---- Figure 34. High Standard for M556 RStuedyNNoop,.NNWoWBBRSOrOL0--1t18455 Sa E S r r s p5 2mrte d=IH5m e S_--ree SSEEE=R y = ET -- -- fe dw] BI ES 5 pias fed a LAL LEL RGSAe ; E mR = = e - -- PR SSEuE=le5C:2 Em mr -- = re = Cie ol | REAL BALE ) Pages 000673 Northwest Bioanalytical Figure 35. High Standard for M570 Try HH sn so--nm--re en ReSptourdty NNoo..NNWWBBRSOO0I--114555 =ii = iesel |. SeSlhpman aSaE Sihiasa Sarea AE RETA ey ) 5 ome y = ar wSR S=E 3 PR % wre F-- =[cu=]:n] = 2 : BRE EAS ha ) Page 76 000674