Document xjxJb88oRm9K4z1O51V1gm0QQ

STUDY TITLE Extraction of Potassium Perfluorooctanesulfonate from Quail Serum and Quail Liver for `Analysis Using HPLC-Electrospray/Mass Spectrometry DATA REQUIREMENTS Analytical Method Requirements STUDYDIRECTOR Sean Gallagher UDY COMPLETED. September 06, 2001 PERFORMING LABORATORY / TESTING FACILITY Centre Analytical Laboratories, Inc. (Centre) 3048 Research Drive State College, PA 16801 Phone: 814-231-8032 STUDYSPONSOR 3M Environmental Technology and Safety Services Building 2-3E-09 PO Box 33331 St. Paul, MN 55133-3331 PROJECT CentCreentPrreotSotcuodlyNNuummbbeerr:: 0002P3--002431-041 "Total Pages: 102 60013 _--- Cent SadyNo 073.081 `L GOODABO PRAR CTICA ECOMT PLIAO NCESR TATEY MENT CFPleoerncfieuoosrporoSacuyuinaeysssufSoNnputomecbofemrreotmsQ.0u"a2i3lc0o4Sn1ed,rucutmedacnofdodrQeud3aMl LEi"nvEveixertfoocnrdmeAonnntaalylsiTosefcUhsnionPlgoougAysPsLauCom.d `SParatcteiceSeSrtvaincedsa,rdwa(s40pCeFfRorPmaerdt7i9n2)cobmypCleinstnrceeAwniahlyUtSeELPabAorTaStCoAriGIeocso.,d Laboratory Principe [DIencvkeesrdpaor enueAnalysen Laborsore, Tc. ' 7 SSteuadyGDailrleacgthoerr Wide ermaonal Lid. es i= 3SoEnpvirRoenpmreensteanlaTiyechnonldSoagftyy Services CreAsyaLaborato bc. Y Be ul Bae elof Pan 20t102 NOL Centre Study No: 023-041 QUALITY ASSURANCE STATEMENT : Centre Analytical Laboratories' Quality Assurance Unit reviewed Centre Study Number 0a2n3d-Q04u1a,leLntiivtelredf,or"EAxntarlaycstiisonUsoifnPgoHtPaLsCsi-uEmlePcetrrfolsuporroaoyc/tMaansessuSlpfeocntartoemeftrroym".QuaAilll pShearsuems were reviewed for conduct according to Centre Analytical Laboratories Standard Operating Procedures, the Study Protocol, and all applicable Good Laboratory Practice Standards. All findings were reported o the Study Director and to management. Phase. L Potcol Review 2. Exaction 3 RSuammwarDyaaTable Review 4 RDraafwtDRueapoarntd Review 5. FRienvaileRweport Date Inspected 121900 200 msm DateCReepnorreted to SDtautdey RDeipreocrttoerdatnod Management SponsorManagement 1222100 122800 122100 122800 om 301 32601 4901 son sion os01 ors01 doe) denedtm Naomi Lovallo Sr. Quality Assurance Auditor Date90s Centre Analytical Laboratories, Inc. Page 3of 102 no1-t _-- [------ CERTIFOIPCAUATHTENTIICOITNY Tehiswreper, ffor oCentre Study Number 023-041, is 3 tusandcomplete representation of Sobmitedty: SSCoecenktReoeAlsmeissy,eeDAarlivL1ea6b0o1rstre, oc. ravey Picpel Iver, Cons SCoemnei*Aayfoar Laborde, Ic. Cente Anyi Libraa,,Facilty Management NFenran7dtA.)aril B5. CentsAonLaborato, Io. Sey Dicer, Wilde ermal M, b nl W`SaeaintGasllmagahetron, id. t Bae fa Be4s oo Date Sponsor Representative, 3: ------ oeidan oleRoldoat <A Bhviroamental Techliology and Safety Services Cone Anyi Leben, B fel Feder 60016 Cente Study No. 023041 STUDY IDENTIFICATION Extraction of Potassium Perfluorooctanesulfonate from Quail Serum and Quail Liver for `Analysis Using HPLC-Electrospray/Mass Spectrometry CENTRE PROTOCOL NUMBER: CENTRESTUDY NUMBER: TYPE OF STUDY: SAMPLE MATRIX `TEST SUBSTANCE: SPONSOR: STUDY DIRECTOR: 00P-023-041 023-041 Analytical Quail Serum and Qual Liver Perfluorooctanesulfonate (PFOS) 3M Environmental Technology and Safety Services BPuOilBdoinxg323333.109 St. Paul, MN 55133-3331 Sean Gallagher Wildlife International, Lid. 8598 Commerce Drive Easton, MD 21601 SPONSOR REPRESENTATIVE: `TESTING FACILITY: ANALYTICAL PHASE TIMETABLE: R3oMchEenlvlierRoonbmiendteaaluTechnology and Safety Services. Building 2-38-09 PStO.PBaoulx,3M33N3155133-3331 Centre Analytical Laboratories, Inc. 3048 Research Drive State College, PA 16801 Study Initiation Date: 1208/00 Experimental Start Date: 1201800 ExSptuedryimCeonmtpalletTieornmiDnaattei:onDate: 0039//0086//0011 Centre Analytical Laboratories, In. Page 5of 102 017 Centre Study No.: 023.041 PROJECT PERSONNEL `The Study Director for this project was Sean Gallagher at Wildlife Intemational, Lid. "vTahreiofuoslplohwaisnegs opefrtshoennsetuldyf:rom Centre Analytical Laboratories, Inc., were associated with Name Emily Stauffer Dave Bell Melissa Kennedy Whitsel John Fishery Tiffany Proctor Angela Morgan Michelle Afjmand Lawrence Ord Rickey Keller `Shawn Robb Karen isha Title Scientist Scientist Supervisor Operations Manager Technician Technician Technician Sample Custodian Sample Custodian Sample Custodian Scientist `Centre Analytical Laboratories. Inc. Page 6of 102 "01-8 Cente Study No: 023.041 `TOAFCBONTLENETS Page `GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT ...ooccoumnmmimrnrinn SQCEUTRAUTLDIIYFTIIYCDAAETNSITSOIUNFRIOACFNATACIUEOTNSHTEc ANTTEIMCEIs NTTY.......s .ooovrcrrsssssssssssssssssssssssssoe d3 TABLE OF CONTENTS eosin] 21..00 SOBUJMEMCTAIRVYE cns eem s LIST OF APPENDICES ...o..cocosersrssesssmsssensssmsssssssmsssesssssssesssssssssssssasssseessosssee 1|21 12 43.00 TIENSTTRSOYDSUTCTEIMO.N..ccoromeroeinimossoonessossesomsssIoIoIe 12 56.00 RDEESFCERRIEPNTCIEONMAOTFEARNIAALLYTv ICAL Mo ETHr OD ce ocos on 1134 6.2 Preparation ofStandardsand Fortification Solutions.............. - wrens 14 66..54 DAeSscIriEpNti!onSoEfTInSsHtIrVuImYent and Operating Condiiconos.o..s..oorrwrrrrrror11S3 7.066EQXuPanEtiRtIatMiEonNaTnAdLEDxaEmSpIlGeCNalculc ation si 1168 9100.0 RCEOTNECNLTUISOINONOSF.D.A..T..A AND SAMPLES ....cooormmnrm |19 Contre Analytica Laborstorie, Inc. Page of 102 n0L2 CentreStudy Nos: 023-041 LI OFTS ABLT ES Table SummoafPrFOyS in Reagent BIAS... Pa2g1e Table Il. SumofmPFaOSirnQuyailLiver BIAnKS rovers 22 Table IL. SummoafPrFOyS in Quail Serum BANKS vn 2. Table IV. Summaryof PFOS Recoveries in Quail LIVE... 23 Table V. SummaryofPFOS RecoveirniQueasl SEMI .....c.cvr.rvvvsovvnen 28 Table VI. Summaryof PFOS in Adult Liver Samples at ppm ai. (Test TETMInAUOn 19 Weeks) vss 25 Table VIL. Summaryof PFOS in Adult Liver Samples at 1.8ppm a. (Test TrMI6AWEEOKS)N vrs 26 Table VIIL SummaryofPFOS in Adult Liver Samples at 6.2 ppma.. (Test FE -- Table IX. Summary ofPFOS in Adult Liver Samples at 17.6 ppm ai. (Test Termination 19 Weeks) .rurvvovrrosoesssssossssnnssn 28 Table X. Summaryof PFOS in Juvenile Liver Samples at 0 ppma.i. (Test BE ---- Table XI. Summary of PFOS in Juvenile Liver Samplesat 1.8 ppm a.i. (Test Torastion 12 Wek nemo Table XIL. SummaryofPFOS in Juvenile LiverSamplesat 6.2 ppm a. (Test Termination 12 Weeks) sess 31 "Table XIII TSeuTmnmAatriyoOnfP1F2OWSeeikn sJu)vev nile Liver Samplc esat 17.6 ppmas i. (Test 32 `Table XIV. Summaryof PFOS in Adult Serum Samples at ppm a.i. (Test BL J ---- "Table XV. STuEmTmRaArHyOoNf P6FWOESEKiSn)Acdruvlt Serum Samples at 1.8 ppm aii. (Test 34 Table XVI. TSuemrmmariyonfa6PtWFeiOeSoksinn)Adulvt Seo rum Suamspalte6.s2 ppm ar.. (mTestm--% Table XVII. f SummaryoT f PFOS in Adult SerumSamplesat 17.6 ppm a.. (Test -------- Table XVIIL.TeSrummimnaartyio1ofn2PWFeOeSksi)n Juvenivlve Serum Sampatl0pepmsm ma.i (mTes--t gr Table XIX. SummaryofPFOS in Juvenile Serum Samples Termination 12 Weeks) vrais at 1.8 ppm a.i. (Test wmmnnaldh Table XX. TSuemrmmairnyaotfi1oPn2FOWSeeiknsJ)uvvenilce Serrum Samples at 6.2 ppmeampi. (Test Centre Analytical Laboratories, Inc. Page 80 102 0150 FRr -- t -------------- Centre Study No.: 023-041 LIST OF TABLES (continued) Table XX. Summaryof PFOS in Juvenile Serum Samples at 17.6 ppm a.i. (Test Page TErmMnAtion 12 Weeks) resin -- Table XXII. Summaryof Percent Moistures for Quail Liver Samples... 41 Centre Analytical Laboratories, Inc. Page 9 of 102 n0i=L eeee eeeeee------------------------ CentreStudyNo.; 023-041 LIST OF FIGURES Figure 1. Figure 2. Figure 3. Figure 4. Figure 5. Figure 6. Figure 7. Figure 8. Typical Calibration Curve for PFOS Page ........ourorsnnmussmnssnd Chromatogram Representing a 0.1 ng/mL standard for PFOS vu. 44 Chromatogram Representing a 1.0 ng/mL. standard for PFOS................45 Chromatogram Representing a Reagent Blank for PFOS (Centre ID Reagent Blank A, Set: 1220004) c..vvovvsvssvssssnnrssnnd Chromatogram Representing Control Quail Serum for PFOS (Centre ID: 0011424 Blank A, Set: 1220008) .c.cvvvvvvnsinmnsnmsssmnn 0C0h0r7o8m7a0toBglraanmk RAe,pSreets:en1t2i1n9g0C0oAn)trol.Q.uoaivlcLricveerrfrorsPnFsOmS,rs(CnesntsrieoIrD:oncd Chromatogram ngimL ofPFOS Representing Control Quail Serum Fortified with (Centre ID:0011424Sp A,Set: 1220004) 500. crn dd `CwhirthoPmaFtOoSgr(aCemnRterperIeDs:en0t0i1n1g4C2o3ntSrpokl AQ,uaSielt:Li1v2e1r8F0o0r4t)if.i.e.d at 10 ppb 50 Figure 9. Chromatogram Representing Juvenile Quail Serum Sample (Centre ID: 0007965, Sponsor ID: 9544, Set: 122000)... ners 51 Figure 10. 0C0h0r7o9m2a6t,ogSproanmsRoerpIrDe:se9n5t4i4n,gSJeutv:e1ni2l1e8Q0ua0iBl).Li.v.e.rcScacmoplveur(eCevnstirenrIDr:irnsS2 Centre Analytics] Laboratories, Inc. Page 100f 102 GNOL5T eee------ CentreStudyNo: 023-041 LIST OF APPENDICES Page Appendix A Study Protocol 00P-023-041 (Centre Study No. 023-041)and AMENA2AMDEEVNIBSHONS.....corsnsssnsns 5 Centre Analytical Laboratories, Inc. Page 11 of 102 Cnn3zEy Centre Study No.: 023-041 1.0 SUMMARY Centre Analytical Laboratories, Inc. (Centre) extracted quail liver samples and quail psreortuomcolsa0m0pPl-e0s23f-o0r4t1he(AdpepteenrdmiinxaAt)i.on of perfluorooctanesulfonate (PFOS) according to "The limitof quantation for quail liver was 10 ppb and for quail serum 10 ng/mL. These were determined in the method verification study (Centre study 023-054). PFOS in the quail liver samples ranged from non-quanifiable levels (a peak was detected at the corresponding analyte retention time but was less than the lowest concentration of the calibration standards (0.0001 g/mL) to 8.37 ug/g. These results are reported on a wet weight basis. Residues of PFOS in the quail serum samples rangedfrom0.00212 pg/mL. Tevels 10 263 pg/mL. `The average percent recovery + standard deviation for PFOS in serum samples was 108% + 10%. The average percent reco+vsteanrdaryd deviation for PFOS in liversampleswas 95% 11%, 2.0 OBJECTIVE `The objectiveofthis study was to determine levelsofperfluorooctanesulfonate (PFOS) in specimensof qual liver and quail serum using the analytical methods described in protocol 00P-023-041. 3.0 INTRODUCTION "This report details the results ofthe analysis for the determinationof PFOS in quail serum Paenrdl_uqouraoiolctalinveesru,lfuosniantge otrheOthaenarlyFtliucoarlocmheetmhiocadls Ceonmtiptoleudn,ds"EFxrtroamctSieornumofforPoAtnaaslsyisiusm Using HPLC-Electrospray/Mass Spectrometry" and "Extraction of Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds From Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry" with the modifications listed in Section 6. The study was initiated on December 8, 2000, when the study director signed Centre protocol number 00P-023-041. The experimental start date was December 18, 2000, and the experimental termination date was March 8, 2001. Centre Analytical Laboratories, Inc. Page 120f102 GN0L54 Centre Study No.: 023-041 4.0 TEST SYSTEM "The control qual serum and liver used for the matrixblanksand matrix fortifications was received on November 28, 2000 from Wildlife Intemational Lid., Easton, MD. The control quail liver was assigned the Centre serum was assigned the Centre IDof 0011424. IDof 0011423 and the control quail Fifty-six quail serum samples and sixty quail liver samples were received at Centre on August 10, 2000. The samples were stored frozen until they were logged in by Centre p`searmspolnenselanodntAwuengtuystqua1i6l, 2000 liver and stored frozen. An additional samples were received on February twenty quail 23, 2001 and serum stored frozen untiltheywere logged in by Centre personnel on February 26, 2001. aSsasmopcliaeteldogwiinthanthdiscshtauidny.ofStcoursatgoedyreicnofrodrsmwaitlilonbeckaenptbeatfCoeunntdreiAnnatlhyetircaawl dLaatbaorpaatcokraig,e Inc. and a true copyofthe storage records can be found in therawdata package associated with this study. 5.0 REFERENCE MATERIAL The analytical standard PFOS was received Environmental Technology and Services at Centre on June 3, 2000 from 3M The available information for the reference material is listed below. The reference material was stored frozen. Stability was not assessed in this study but the reference material was stored according to the certificate of analysis and was used prior to expiration. The solubilityofthe reference material was not relevant to this study. Compound Centre ControlNo, _ TCRNo. Purity (%) Expiration Date PFOS 0002-02 TCRO00I746 97.9 08/31/01 `The molecular structureof PFOS is given below. PChReOmiScal Name ~~ = Molecular weight = o we Perfluorooctanesulfonate 499 (CFinSOy) Note: "The neutral molecule and standard form from which PFOS (anion) is derived, is potassium perfluorooctanesulfonate [CyFisSOSK], molecular weight 538. Centre Analytical Laboratories, nc. Page 13 of 102 @nn1Es Centre Study No. 023-041 6.0 DESCRIPTION OF ANALYTICAL METHOD AFnlauloyrtoicchaelmimceatlhoCdosmepnotiutnldeds"FExrtormactSieornuomffPoortAansasliyusmisPeUrsfliunogroHoPcLtCa-neEsluelcftornoastperoary/OMtahsesr Spectrometry" and "Extraction of Potassium _Perfluorooctanesulfonate or Other Fluorochemical Compounds From Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry" with the modifications listedbelow were used for this study. 6.1 Extraction Procedure A 100 L aliquot of the serum and ~ 0.50 g sampleofliver was used for the extraction procedure. After fortificationofappropriate samples, the samples were vortexed fo~r 15 seconds. OnemLof0.5 M TBA was adtodtheelidversamplesand 0.5mLwas added to the serum samples. Two mLof 0.25 M sodium carbonate/sodium bicarbonate was added 10the liversamplaensd 1mLwasaddedtotheserumsamples. FivemLofMTBwaEs added 10 both the serum and liver samples. Each sample was placed on wrist-action shfaor~k20emirn. and then centrifuged fo~r 15 min.FourmLoftheorganic layerwes taken and dried on an N-Evap and then reconstituted with 1 mL of methanol. Each sample was analyzed by LC/MS/MS electrospray. 62 Preparationof Standards and Fortification Solutions Standard solutions were prepared on September 18, 2000 as specified in Centre Analytical Laboratories' protocol 00P-023-041." An individual stock standard solution of PFOS was prepared ata concentration of 100 pg/mL. by dissolving 10 mg ofthestandard (corrected for purity and salt content) in methanol. From this solution, a 1.0 pg/mL. fvoorltiufmiecautipontost1a0n0damrLd swoiltuhtimoenthwaansolp.repared by taking 1mLof the stock and bringing the The 0.1 pg/mL forification standard was prepared by taking 10 mLofthe 1.0 pg/mL fortification standard and bringing the volume up to 100 mL with methanol. A 0.01 `1g00/mmLLswtiatndhamredtwhaansoplr.epared by taking 10 mLofthe 0.1 pg/mL. standard and bringing to A set of standards containing PFOS was prepared by dilutionofthe 0.1 pg/mL and 0.01 g/m solutions inthe following manner. Initial Cone. (g/mL) 0[31 0.1 001 001 001 of PROS. (Centre Analytical Laboratories, Inc. Volume (mL) 25 1 5 2 1 Diluted to (mL) 110000 100 100 100 100 _FinalCone.(ug/ml) 00..000052 0.001 0.0005 0.0002 0.0001 Page 140102 GROL56 Centre Study No.: 023-041 `The stock standard solution and all fortification and calibration standard solutions were stored ina refrigerator (4 + 2C) when not in use. Documentation of standard preparation can be found in the raw data associated with this report. 63 Chromatography Quanification of PFOS was accomplished by LC/MS/MS analysis using electrospray LC/MS/MS. The retention time of PFOS was ~ 4.4 min. Peaks were detected in the control matrices corresponding to the analyte retention time and some of the amounts detected were significant enough to alter the results reported in this study. 6.4 Instrument Seasitivity 0`T.h0e00s1mapllge/smtLostfanPdFarOdS.amount injected during the chromatographic run was equivalent to 6.5 Descriptionof Instrument and Operating Conditions Mass Spec: PE SCIEX API 3000 Biomolecular Mass Analyzer Interface: SCIEX Turbolon Spray Liquid Introduction Interface Harvard infusion pump. Computer: Dell UltraScan P1110 Software: HPLC: PE SciexAnalyst 1.1 HWeiwnldeottwsPaNcTkard (HP) Series 1100 HHPP VQuaactuPumumDpegasser HP Autosampler HP Column Oven HPLC Column:Genesis Cs (Jones Chromatography), 2.1 mm x 50 mm, 44 Column Temp.: 35C IMnojbeicltieonPhVaosle:(1A0):aL2 mM Ammonium Acetate in ASTM typeI water Mobile Phase (B): Methanol FlowRate: 0.3 mLmin. Centre Analytical Laboratories, Inc. Page 15 0f 102 Canis? Centre Study No.: 023-041 Time %A %B 0 60 40 1.0 [J 100 n7750o 660 144000 Tons monitored: Amite Mode TransitionMonitored PFOS negative 49> 99 `Tune File Parameters RetenAtpipornoxTiimmaete(min) 4.40 Controls IS-lospray DP-Declustering Potential FP-Focusing Potential [EP-Entrance Potential CE-Collision Energy CXP-CollDiFs-iDoenfCleelcltEoxrit Potential (CEM-Channel Electron Multiplier NeGbausliFzleorwGsas ColCluirtsaiionnGGaass TIS Temperature 66 Quanitation and Example Calculation Set 4200.0 -51.0 230.0 10.0 70 30-500 2800.0 S1e2t 143 350C "Ten microliters of sample or calibration standard was injected into the LC/MS/MS. The peak area was measured and the standard curve was generated (using 1/x fit weighted linear regression) by Analyst software using six concentrations of standards. The ceqounacteinotnrsa:tion for quail serum and quail liver was determined from the following Use Equation | to calculate the amount of analyte found (in ng/mL, based on peak area) using the standard curve (linear regression parameters) generated by the Analyst software pfrorogsrearmu.m sTahmeplnesu)s.e Equation 2 to calculate the amount of analyte found in pg/g (g/mL Centre Ansytca Laboratories, Inc. Page 1601102 600155 CentreStudy No.: 023-041 Equatio1n: Analyte found (ng/mL=)(Peakaslroepae - intercept) Equation 2: `Analyte found (ug/g) =(anal.found(ng(/AmVL)(xmLF)Vx(smaLm)pxDlwFte.x2E)V(mL) x10L0ug0n.g Where: FV = Final Volume DF = Dilution Factor EAVV ==EAxltirqaucottioVnoVloulmueme. For samples fortified with known amounts of PFOS prior oextraction,use Equation 3 to calculate the percent recovery. Equatio3n: Recovery (%)= (anal.found(ug/g)-avga.maonuanltytaedidnecdt(rln(/u9g/)g)| igx1000ngx100% An exampleof a calculation using an actual sample follows: P`QFuOaiSl.liver sample Centre ID 0007870 SpkA (Set: 121900), fortified at 1000 ng/g with Where: peak area = um intercept = a6 siope = am dnigl/ugtiaodndfeadct(ofrort level) == 1100000 nglg avg. amtincontrols =O (Not quantifiable) feixntarlacvtoilounmveolume ~~ == S1mmL aliquot volume = am sample weight = 05g From equation 1: Analyte found (ng/ml) = [11483 463] 2% From equation 2: = 39mgmL Analyte found (ug/g) = (3@9mxLxn|m05Lggx)10/0xmSmlL)x1L00u0gng = 0975 pgmL Centre Analytical Laboratories, Inc. Page 1706102 00159 --_---- Centre Study No.: 023-041 From equation 3: % Recovery = (0.975ug/ml --01p0g0/0mnLg)/gx(1000ng/1ug) x 100% = 98% 7.0 EXPERIMENTAL DESIGN Etawcohmastertioxfbslaamnkpslefsort(ilfiiveedr aotrksneorwunm)cocnocnesnitsrtaetdioonfs,onaendre~ag2e0ntsabmlpalneks,. oEnaecmhastarimxplbelawnaks, extracted using the appropriate method and then analyzed in duplicate. 8.0 RESULTS `bTlhaenkPsFaOnSd qfuoauinldsienrtuhmebrleaangkesntarbelganikvsenairne TiasbeldesinITT&abIIlLIe. The PFOS inthequail liver Individual recoveries for PFOS in the liver samples are detailed in Table IV. The average percent recovery standard deviation for PFOS in liver samples was 95% 11%. Individual recoveries for PFOS in the serum samples are detailed in Table V. The average percent recovery 10% standard deviation for PFOS in serum samples was 108% + PatFtOhSe cionrtrheespquoanidlinlgivearnaslaymtpelreesternatnigoendtfirmeombuntonw-aqusanletsisfitahbalnetlheevellosw(eastpecaokncweanstrdaettieocnteodf the calibration standards (0.0001 pg/mL) to 8.37 pee. Individual results are listed in Tables VI-XIIL. The results are reported on a wet weight basis. PFOS in the quail serum samples ranged from 0.00212 pg/mL levels t0 263 pg/mL. Individual results are listed in Tables XIV-XXI. The average percent moistures for the quail liver samples are given in Table XXII. 9.0 CONCLUSIONS "The quail liver and serum samples were successfully extracted and analyzed according to protocol 00P-023-041 Centre Analytical Laboratories, Inc. Page 18 of 102 C0350 EE -- Centre Study No.: 023-041 10.0 RETENTION OF DATAAND SAMPLES L`aWbhoernattohreiefsi,naIlnr.epvoirltl ibsecosmhpilpepteed, taollthoerisgpionanlsopra.peTrhidastadogeesnenroatteidncblyudCeefnatcrieliAtyn-aslpyetciicfaicl raw data submitted. such as Exact instrument logs, copiesofall raw however exact data, as well as acospiigensedofcotpeymopefrtahteurefinlaolgasnawliyltlicbael Lreapboorrtataonrdieasl, Ionrci.gainraclhifvaecsifliotryt-hspeepciefriicordaowfdtaitma,e wsiplelcibfeierdetiani4ne0dCinFRthePaCretn7t9r2e.AnRaeltyatiinceadl samplesofreference substances are archived by the sponsor. Centre Analytical Laboratories, Inc. Page 190f 102 n0L8T --_--_-- Centre Study No.: 023-041 Centre Analytical Laboratories, Inc. Page 200f 102 CNL _--nmmm--m--------,,,------ Centre Study No.: 023-041 Tablel. Summary of PFOS in Reagent Blanks Sponsor. Centre Se Number Eatcion Date Aulyis Amlyte Date Found gag) rmyo RReeaggmemBBwlkakAAt 212818000AA 112211880000 112211990000 NNoo n mo ReagenBlokA RegmBlkAt 1218008 DOB 121800 122000 121800 122000 No No nm no ResgeniBlaokA RemBmkAt 1219004 121900 122100 210A D900 122100 Q No n mo ReageniBlnkA RegmiBlkA* 122110900088 112/1990000 112222112220000 NNQO "no RReeapgeenmtBBllaknkAA* 122020000AA 112222000000 11222220000 00.000000220000 m"o RReeaggemntBBllkkAA 11222000060 112222000000 1(222222200000 NNQO mmo RReeggemniBBwlkukAAt GO00S00IIAA S30O1 33/66770000 NNDo m Mm RagemBlnkA RegenBlkA _ 03G00G600IIAA 33660011 330001 NNeo * Duplicate jection STANDARD DEAVVIEARTAIGOEN:: NNQQ INQ = Not Quantifiable (A peak was detected at the corresponding analyte retention time but was less than the lowest concentrationofthe calibration standards (0.0001 pg/mL) ND = Not Detected Forvaluesrecorded as ND,zerowasusedtocalctuhleavaertagee and standard deviation. sFtoarndvaarldu,es0.r0e0c0o1rdged/masLN)Qw,a0s.u0s0e0d05togc/almcuLl(ahtealtfhteheavevraalgueeoafndthsetalnodwaersdt dceavliiabtriaotni.on LOQ= 0.01 g/g or iver and 0.01 pg/mL. for serum Centre Analytical Laboratories, Inc. Page 21 of 102 GO35L _-_-- Centre Study No.; 023-041 Table IL. Sponsor I mnao Nmoo 46 4456 45% Summary of PFOS in Quail Liver Blanks Centre m Set Eximcton Aus Number Dae Due OGUO3NIBBkKAAT| LL220B0000AA 8R80000 11221199/0000 OCOOUI4MNBBlmkkAA 211210803B 1A28080000 112222000000 OOTEIOBlakA o0WOBlkAC 12I00A LIGA 112210990000 11222211/0000 0O00WWTRRBBlkkAAt OOM0IEIAA 6360011 307011 STANDARD DEAVVIEARTAIGOEN:: Ausiyte Foud yp) NNoQ 00000011039 nxNo o0o0o0i1t2o0 00..000000887580 Table III. Summary of PFOS in Quail Serum Blanks Sponsor Centre St Bairacion Amis Amiyie D Number Due Date__ Found (agin) na na GONCABWKA ODIABKA* 11220900B 211990000 11222201122220000 0000114346 mnoo OIMNMBBKWAK*A 1I2Z020000O4A 21222000000 21222220000 0000is3l8 rnaa OONOAN4MB4BKKAAT 11220000088 11222000000 11222222220000 0000110297 mmn 0ll0244BBlkaAkTA GO0SSOAIA VISONIL 366770011 _0_000ou5s5s5o STANDARD DEAVVIEARTAIGOEN:. 0o.o00n3i8s4 * Duplicate injection 'NQ =Not Quantifiable (A peak was detested at the corresponding analyte retention time but was less than the lowest concentrationofthe calibration standards (0.0001 pg/mL) For values recorded as NQ, 0.00005 g/g(halfthe valueofthe lowest calibration standard, 0.0001 pg/mL) was used to caulate the average and standard deviation. LO= 0Q.01 py/gforliverand0.01 pgf/orsmerLum Centre Analytical Laboratories, Inc. Page 220f 102 Ca0Lst _--mm Centre StNou. 0d23-y041 Table IV. Summary of PFOS Recoveries in Quail Liver Spioor CIoDe NeSheer uDcuei ADmupes AddeAdlmagg) Re"cor mmeo COOlNSDKSAESA ZDHIGGOOAA T218t0w0 112211990000 T1o0 110028 wmmo OONOISSKKBD DDiimeonn wiww Diamwo 220000 01013 mWow GOSSKKAA DmUSMWB DD1w0 D22o06w0 llooww In wmmo OOlIISSKKEB DDIOAA MIVWIL 2[202202000000 220000000 05 4SSS WGUOEEOOSSKKAAS RROIAA 2i1990000 22201000 l0o0o0 0 i4 WGOUESOKSBAD iDIAA 11990000 0D2211000) 2200000000 5s 66 ooommmmsSAKrA Gmouoonn Jveeoo 3300 w0 56 Gs6s oowmnmmsSiKeBe mowusoina Jveeoml 3o70l1 E2y0 05 STANDARDDEAVVIEARTAIGOEN:: 9114 RELATIVESTANDARD DEVIATION: 13 + Duplicateineton LOQ =0.01 pg/g for liver and 0.01 pg/mLfor serum Centre AnaytcalLaborstorie, Inc. Pagof1e02 600s -- Centre Study No.: 023.041 Table V. Summary of PFOS Recoveries in Quail Serum Sponsor Centre m D m mo 0004424S4pkAAT m Ma OOI02I44SMPSKKBB mmoo 000OIIAMMASSKKAA mo mo 0OII4AMASSKKBB mo mo U0M0ASMKSAKTA mo 0OUASKB mo mo OOINAAMMSSKKBA mmoo OUMASSKAB mm olapaspkBe * Duplicate injection Set Number 12090080 I2I00BD I2IS00BD 12I900BD 1[2200000A4 1220004 120000 120008 122008 1220008 1220008 ONSOIA OGN0SSOIIAA eosolA Extraction Avalyss Amt % Date Date Added opm) Recovery 121900 DINO 1122223322440000 00 S00 103 106 121900 121900 1122223322440000 100000 100000 0 0 112222000000 112222220000 550000 110036 D20K0 1200 12200 1200 100000 100000 9 103 D200 12000 22200 1222300 S00 S00 108 1o 122000 12222300 122000 1222000 100000 100000 3 9% SOI USOI 360 U6ON 100 100 Je SOL ysor Y6701 vero 1000 1000 0 us STANDARD DEAVVIEARTAIGOEN:: 1906 RELATIVE STANDARD DEVIATION: ~~ 9 LOQ= 0.01 ug/g for iver and 0.01 pgm.forserum Centre Analytical Laboratories, Inc. Page 2407102 a01356 _--m Centr Study No. 023041 Table VI. Summary of PFOS in Adult Liver Samples at 0 ppm a.i. (Test Termination 19 Weeks) Sponsor care assen wouorsm aPe waorrssese aisse owosm ssaer pwrars prses apeon pusos wwoorrnn as2e) wwoons ast aatoomsn aPsr wwoowwss a"awno wwooss Dipl ction NuSmtber EDxuec ADmuies FoAuwneda mAoDw iiswe 1T2a0o00s0 00221ss mLIAA aaww i1219o00 xNoe AmoDd DDaawwee 2omw 00330 a Lion iiswe 1129190000 xNoo Z2iIoAADD iissm Lbooookb ooille pFirn awe 1r220o00 No 2R0INADD awwee apookve ooours LZiAon eawwe iGmook ocoololr missooAaDD wDiwww a20v% oodss pRiAe iiww ii ow oossoloty STANDARDDEVAIVAETRIAOGNE: 000191533 NQ = Not Quantifible (A pes was detected at he corresponding analy retention time `but was less than the lowest concentrationofthe calibration standards (0.0001 pg/mL)) For values recorded as NQ, 0.00005 ug/g(halfthe valueofthe lowest calibration `standard, 0.0001 pg/mL) was used to calculate the average and standard deviation. LO=0Q.01 pglgforliverand 0.01pg/mLforserum x ,3ie 255=32gR5YSa E9%3 T<S28aa3u8i38d3ixd Centre Analytical Laboratories, Inc. Page 25 of 102 00137 _--_--mm Centre Study No. 023-041 Table VIL. Summary of PFOS in Adult Liver Samples at 1.8 ppm a.i. (Test Termination 6 Weeks) `Sponsor n E01-0259-20780 E01-0259-20780 E01-0259-20781 E01-0259-20781* E01-0259-20782 E01-0259-20782* E01-0259-20783 E01-0259-20783 E0I-0259-20784 E01-0259-20784 E01-0259-20790 E01-0259-20790 E01-0259-20791 E01-0259-20791% E01-0259-20792 E01-0259-20792 E01-0259-20793 EO01-0259-20793% E01-0259-20794 EO1-0259-20794 Centre. nD 0102997 0102997 0102998 0102998 0102999 0102999 0103000 0103000 0103001 0103001 0103007 0103007 0103008 0103008 0103009 0103009 0103010 0103010 0103011 0103011 * Duplicate injection set Number 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 0306014 0306014 030601AD 030601AD 030601AD 030601AD Extraction Analysis Date Date 3601 301 3/601 801 3601 801 3601 801 601 3801 3/601 01 601 3801 3601 01 3/601 301 601 mor 601 01 601 301 3/6/01 801 601 301 601 301 601 301 3/601 01 3/601 01 601 mol 601 301 AVERAGE: STANDARD DEVIATION: Analyte Found (ug/g) 0800 om 0149 [x 0341 0311 0.55 0422 00988 0.0843 0210 0210 orm 0191 00124 00121 00381 0.0394 00629 00720 027 0224 LO=Q 0.01 g/g forliverand 0.01 pgf/orsmerLum Centre Analytical Laboratories, Inc. Page 26 of 102 09158) _-- Centre Study No.: 023-041 `Table VIIL Summary of PFOS in Adult Liver Samples at 6.2 ppm a.i. (Test Termination 6 Weeks) Spoasor Cenre I" Ir) EE EEoollomassssarmssss oololsosn2 EOLs9206 0103003 E E0D20S8 00110033000044 EE0l2s5e0 o01l0o30o0s8 EE0nozmsos2r08e9 0o1l0o3x0o0a6s EoLo2ssa079s ol030i2 BEoozss0ms9 oolioir Bsns olson BEOLOz0s529 097* o0l1o0s3o0l1s4 EEnosesn oolwoslolss EEDL0o25ss00999_ o0n10s3o0t1s6 + Duplicate jection Sa Nomber Deb Gooo0oilAdD Good G00o0IDAD oGoodD oGoooApD oloAd oowaoAdD GOOD oo0o60dAD oGooodd GGooDD Exmcion Aus Due Duie 3601 wor 33660011 3m8o0r1 360 mor 636001 m001 u6s0o mamoor u36s0o1 ammool so mol vveoo aao0l 3601 mol v36e0o1 wvoorn vweoor wwoorr 36600 wwoon STANDARD DEAVVIEARTAIGOEN:: Aste Found gig) 11s 112s0 hn 1124 1is6t0 1i0y6 0216 ooizs 00934 oooorr 0012817 ooosm 00.16056 LOQ = 0.01 pg/g for liver and 0.01 pg/mL for serum Centre Analytical Laboratories, Inc. Page 27 of 102 6no1sn _-- ee _-- Centre Study No. 023-041 Table IX. SummaryofPFOS in Adult Liver Samples at 17.6 ppm a.i. (Test Termination 19 Weeks) `Sponsor I Centre m set Extraction Amslpis Awsiyte Number Date Date Found (ugg) ar wr 007877 00777 T2800AD 121800AD 121800 121800 122000 122000 105 105 wn ane 0007878 007878 12100AD 2ISOAD 121800 121800 122000 122000 410 an a ae 0007879 0007879 12180AD 121800 122000 12I80AD 21800 122000 837 830 aw ar 00780 007880 2I80AD 21800 122000 12IS0AD 2/1800 122000 141 143 ass ase 0007381 0007881 1221108000A4D0 112211880000 112222000000 115314 ats aor 007882 0078s 1218040 121800 122000 2ISOAD 121800 122000 oars 032 wr ar 0007883 12180AD 121800 122000 7 0007883 121800AD 121800 122000 Lis a ae 007884 007884 12IS00AD 280 122000 1IS00AD 121800 122000 ost 0309 a aor 007885 o0argss IAD 11800 122000 121800AD 121800 122000 20 248 90 aor 0007836 000786 121800AD 121800 122000 1218040 12nmo0 120000 0351 0360 AVERAGE: 2.13 STANDARD DEVIATION: 239 * Duplicate injection LOQ = 0.01 ug/gforliveanrd 0.01 pg/mL for serum Centre Analytical Laboratories, Inc. Page 280f 102 O Centre Study No.: 023-041 Table X. Sponsor sSs5030+7 959500660 ssssunn ssssiziez ssssiisse sssisis s0sa520 oosstm e9s5s2se s9s522e60 Summary ofPFOS in Juvenile Liver Samples at 0 ppm a.i. (Test Termination 12 Weeks) caBDre cGaooornse0rr cooouorrsoss oaoouurrsseess auawororssiioo pornoeroit aannoorrssiizz aacarosroiis3 aacnarssties ccaoorosiss ooouorssiiss MeSmtber BxDnucieon ADmaiek__ i piss sRiwse 122a00m0 pFises isn 200 J pie oa aww ppiises paawsee paaow niiomn awwww aaww noiins wawww 2222000000 pLiissoss Diaww apaww LniIsOwRs iiWs aDww pJ isws Das 02000 ppiissss apiwsw 2pa0o0 STANDARD DEAVVIEATRIAOGNE: poAunmdigei) x0o xo xNoo xxoo ooxwnoss owxons oNros ooowwneins ooxmsss xx 000N0g351 0006316 * Duplicate injection NQ = Not Quantifsble (A peak was detesteda he corresponding analyte retention time `but was less than the lowest concentration of the calibration standards (0.0001 pg/mL)) For values recorded as NQ, 0.00005 ug/g (halfthe valueofthe lowest calibration `standard, 0.0001 pg/mL) was used to calculate the average and standard deviation. LOQ = 0.01 pg/g for liver and 0.01 pg/mL for serum CentreAnalytical LaboratorieIsnc,. Page 290f102 [TERY _--m-- Centre Study No: 023-041 Table XI. Summary of PFOS in Juvenile Liver Samples at 1.8 ppm a. (Test Termination 12 Weeks) `Sponsor mn 528 sage 9529 5290 9530 95300 9531 os31+ 9533 sae 9535 osase 9540 95400 9541 osal 9543 ssa 9544 osaar Centre I' 007917 007917 007918 007918 007919 0007919 0007920 00000077992210 0007921 00922 00922 000923 000923 0007924 0007924 007925 0007925 007926 0007926 set Extction Amlis Number Date Date 21808 121800 122000 2is0B 21800 122000 121808 121800 122000 121808 121800 122000 1218008 121800 122000 21808 121800 122000 218008 121800 122000 2I180s08 112211880000 112202000000 21808 121800 122000 2is0B 21800 122000 121808 121800 120000 121808 121800 122000 2I80B 21800 22000 11808 121800 122000 21808 121800 122000 IB0B 121800 122000 121808 21808 121800 121800 112202000000 218081201800 120000 AVERAGE: STANDARD DEVIATION: Amaiyte Found (igi) 00130 00128 000295 000295 000904 000876 000417 0o00o43n5. oon oon oon 000635 000623 000305 000297 00126 00000182164 000521 0.00792 0.00393 * Duplicate injection LOQ = 0.01 g/g for liver and 0.01 pg/ml. for serum Centre Analytical Laboratories, Inc. Page 300f102 CooL _--_--mmm Centre Study No. 023-041 Table XII. Summary of PFOS in Juvenile Liver Samples at 6.2 ppm a.. (Test Termination 12 Weeks) `Sponsor n 954s sage 9549 osisn 9551 assis 9552 oss 9555 oss 9559 oss5n 9561 ose 9562 9562+ 9563 sexe 9564 ose Centre I' 0001927 001927 007928 007928 0007929 0007929 0007930 0007930 0007931 0007931 007932 0007932 0007933 0007933 0007934 0007934 0007935 0007935 0007936 0007936 set Number RIA DIA 210A 21004 100A 2I90A 1219004 219004 121900AD 121900AD 12I00AD IAD 2I90AD 121900AD RI0A 210A 12I900AD 12I900AD 210A 21004 Extraction Analysis Date Date 121900 122100 121900 122100 21900 122100 11900 12000 121900 122000 121900 122100 121900 122100 121900 122100 121900 122300 121900 122300 121900 122300 121900 122300 12100 122300 121900 122300 121900 122100 21900 122100 121900 122300 121900 122300 121900 122100 121900 12210 AVERAGE: STANDARD DEVIATION: Analyte Found (uf) 000303 0003S 00100 0010s 00123 oonzs 000316 000302 ogo 00408 00340 00341 004s 004s. 00116 oon21 00193 00197 000i 00001 00182 0.0156 * Duplicate injection LOQ = 0.01 g/g for liver and 0.01 pg/mL for serum Centre Analytical Laboratories, In. Page 31 of 102 0172 -_-- Centre Study No. 023-041 `Table XIII. Summary of PFOS in Juvenile Liver Samples at 17.6 ppm a.i. (Test Termination 12 Weeks) Sponsor Crne NeSmtber ExDmucieen ADmries FouAnmdignei So5s6e7 aG0o0r7e9s57 PWIIA iTsoom aT21o00 o00im s5s5n70e ooaoo0rrs9a3s8 RRIIAADD i21s90o0 a12030 o0o0ha9 s5s5n75se oo0000rrssssso LRIIAA i i900 0 221000 ooooo s9s5t7o9r aaunoorrssaaon L2I9N0DA ii990000 aawwee ooosmo sssstio0r aa00007r9s4a1r 2RI0ADD 22990000 1a3w0e ooookk ssssuaiie awaoarrsseezz RRIIAADD 9i90000 20 30 oouosmt sssisiz poeourses DRiI%oAAD> i21v90e0 p1a2m0 oooomm s5si563 oonnoorrssesss RROIAADD 2129109000 DDawae oosme osu)ar oo0n0orrsseess LLOIADD ii9g0o0 naammee oodoomr osoistsr prtiaosne]s RRIIAADD 1229190000 112733000 o0oxm0 STANDARD DEAVVIEARTAIGOEN:: 000050973 * Duplicate injection. L0= 0Q.01 ugforliverand 0.01 pg/mLforserum Centre Analytical Laboratories, nc. Page 320102 61037 --_--mnm---m---m-m-m-- CentreSedy No. 023-041 Table XIV. Summary of PFOS in Adult Serum Samples at 0 ppm a.i. (Test Termination 19 Weeks) SponDsor Centre NuSmeber EDxantceion ADuates FouAnmdiy(igem) asi1 Go0o07s8e87 LT2IlSsO00BsDD 112211990000 1122223322440000 1Tiss aspoey oovooon7ssssss LSi0s8 ii990000 222211220000 00000150029 as43 0o0o0o7r8s8s5s 2D0I0S000B0D 112210990000 1122223322440000 91004 aassta 0000007788500 D21I90BB 2i1990000 112222102220000 o0o0oe2im2 asases 0000007789911 iSBB 12211990000 11222211220000 0000112ss a4s5t6 ooc0o7oss92 112211990000B8D0 112211990000 11222233:22440000 66426 as5m1 a0o00778es9s DDiiss0ossDD 112211990000 1122223322000000 66355s aasse a0o0o0n7a89s4s DDIISSOBBDD 112211990000 212223322000000 00110025 as45o9 ooo0r0a7g85s5 D1i2S0008B0D 112201990000 112222532.02000 aas7 STANDARDDEVAIVAETRIAOGNE:: 446748 * Duplicte nection LOQ= 0.01 gg for liver and 0.01 pg/mL. for serum Centre Analytica Laboratories, nc. Page 3307102 ROL EEE -- entre Study No.: 023-041 Table XV. Summary of PFOS in Adult Serum Samples at 1.8 ppm a.i. (Test Termination 6 Weeks) Sponor Centre EEoLLoS2s2o007725 o01l002z9s6e9 EEoLmOsso20r7Ss3* oolegam9n EEolLssaTss o01l0e9n7 EEnoslsaasss olwoezn EBloolsLszas07rssse ool0ola02s9nm E BMs E 000029a9 EE00LL02258992200776653% 001l0022558800 EEoOLLa22ssos2a0t06rsse 0oloazsmsl EEnnLsosssa0esss ooolzeess EEo0LLOsSOo-020%76666 0011002299883 NuSmuber GWoOaOdD oGoosoaAdD oo0oss0oimAADD GGooaDd GGOoOoIAdD ooooooAADD wooosooiAADD Go0so0AdD oooossooiAaDD oGoos0aAdD ExnDceion ADmuyes uassoo 3377aam uussoo arann suoslo annaool u3ssool aroann ussmo amnoall uussoo annaam suoslo snaann IuSsOo 3am7aan uussoo anaamn iussoo aanrta STANDARD DEAVVIEATRIAOGNE: FowAdnsgiymtet) 110099 s0512 116604 3518 7203 11590 asosus 118547 aanins s10ms 110172 * Duplicate injection LOQ = 0.01 uy for liver and 0.01 pg/mL. for serum Centre Analytical Laboratories, Inc. Page 34 of 102 600176 EEE EEE A EES. Centre StudyNo. 023-081 Table XVI. Summary of PFOS in Adult Serum (Test Termination 6 Weeks) Samples at 6.2 ppm a.i. Spoinsor Genre EELoSnsT OoIn BEOlLsa00sTSsE o010s297 BELLgSSwTs o0m9e% EEOLLSS920T0 o009l7 EGLoSlsT 0 oo E ELSm20s 6 a0m9% EElosse ooslss BElLaSsTe 0os9s% EEOLLSS9T20O7N0 o0llNs8 EEsLa S oossss MeSmbter 0D0SS0IAADD Gooso0IdD D00Si0IbAD 0GN0SIIAADD 0000ss0IAADD 0oloAdD GGooss00IIAADD oONoSIoAD 000NISAADD oowwsowimAsD ExDnucieon ADmubess ssoolr mnsore ssoerl amannanm uIssoo a3mmaa0nn suoslo aanmoann Iussoo mameanno ssmei ammoann ssool asmoonn uIsSoO 3m7a0n1 suoslo mamoamnn vusseo nmaanot STANDARDDEVAIVAETRIAOGNE:: FounAdmgime ) 52621 50427 w0s4 @6s2 5s6a7s iasotr 2w6n0 asnn fae 21100 30937 * Duplicate injection. L0=0Q.01 wy fo liverand 0.01 pg/fomrsLeru.m Centre Analytica Laboratories, Inc. Page 351102 n01L77 _--_-- --_--_---- _--_----_----_--_--_ _ Centre Study No.: 023-041 `Table XVIL Summary of PFOS in Adult Serum Samples at 17.6 ppm a.i. (Test Termination 19 Weeks) Sponsor Ceatre D ny set Number Extraction Avalyss Date Date Analyte Found (gm) ar wr 0007856 0007896 12190080 2I900BD 121900 12232400 12100 1223:2400 260 263 we 0007897 007897 12190080 1219008D 121900 12232400 121900 1223:2400 a1 24 a ane 0007808 0007808 1219008D 1219008D 11900 121900 11222233::22400000 118 106 a5 ase 0007899 0007899 2I00BD 12190080 121900 12232400 121900 12232400 I m a ar 0007900 0007900 1219000 1219008D 121900 1223.2400 121900 1223:2400 133 m a8 ane 0007501 0007901 1219008D 1219008D 11900 1223.2400 121900 12232000 158 168 a ase 0007902 007902 00501AD 0001AD IsOI 37am Iso1 37801 2 2 90 0 007503 0007903 12190080 1219008D 121900 1223-2400 12/1900 1223-2000 681 630 STANDARD DAEVVEIRAATIGOEN:: 12 530 * Duplicate injection LOQ = 0.01 ng/g for liver and 0.01 pg/mL. for serum Centre Analytical Laboratories, Inc. Page 3607102 n017s _--mhm--mmmm--m--ee ee ee Centre Study No.: 023-041 Table XVIII. Summary of PFOS in Juvenile Serum Samples at 0 ppm a.i. (Test Termination 12 Weeks) Spoor cawne s5so0 Swooras s5s506 wcoooss s55s08 siz owosrsee oomo ssss1sn ooosmto sssiisst wwoosm s5s5i20 ssn wwooss cows ss95s25 wcoowmss s5s526 oocorrsesss Nseem EuDmucieon ADmaeb voAwmieel) m00o0n8 Tp2a00o0 DTaamsoo moon paso pam oooaouds ooo mmeooaA apcaoo ommme mon aco mmm oonws oom mmooaa aaokeo paawwo mon ako mee ooeoso owns wmoenk aamcoo mmamme oomwann mmoonn moa ppaacce aoe mmamm omeo oowonn owes mmoooan aaooee aawwee mon abo mee oowosn owns moon ioe AyVuEmReAGE otauinn STANDARD DEVIATION: tos Dupe ction LOQ=0.01 pg/g for liver and 0.01 pg/mL for serum Cente Analytical Laboratories, In. Pag3e706 102 no17e _--_--mm---m-- -------- Centre Study No. 023-081 Table XIX. Summary of PFOS in Juvenile Serum Samples at 1.8 ppm a.i. (Test Termination 12 Weeks) SIpronssor cenre sSs5a2ae1 au0o9rs5s%s 595522090 oonwoorreossn7 ss553n0 poorunessds s5sa521 oo0o0unrssssso s9s5a33 o0u0r0s560 s9s5a3sse oonuoorrsssstt ssssaoor poorre ssssaat oooourrsseess sossie3 oooooorrssssss o9s5a6s4r oonnuorrsseess NoSmtber BxDnactieon ADmaiek FounAdmGime ) 2m0o0o0n0 T122000000 112222000000 uaroes 2m0o0oAn Dpaa0ww 2a220000 00mamm 0200AA ppaaoww aanwo0 oooonm 0oAA ppaawm 1z222e00 0o0o6m mooAa apoacw 212202000 oooor mmooaa aaoocc 112222220000 ooo0istt3e 0o0o0nA pDaavvewe a1220200 ooouoss mmooonn ppoaww 212270000 o002o1 000000AA 22000000 aaw0e oosomm mmoooonn a120m00 rraanzameo o0o0isse STANDARDDEAVVIEARTIAOGNE: 00001n5d8 Duplicate injection L0=0Q.01 ugfo liverand 0.01 pg/mL forserum Centre Analytical Laboratories, Inc. Page 38 of 102 0001S0 _--mm--mm Centre Study No.: 023-041 Table XX. Summary of PFOS in Juvenile Serum Samples at 6.2 ppm a.i. (Test Termination 12 Weeks) `Sponsor Centre set Extraction Analysis Analy I m Number Date Date Found (gm) E 0007966 1220000 122000 122400 0137 osase 9549 0007966 0007967 122000 20000 122000 122000 112222400000 00136m0 osa9 007967 20D 122000 120000 0390 9551 ossie 0007968 0007968 1220000 1220000 122000 122000 120400 120400 022 0208 9552 os52e 0007965 0007965 1220008 1220008 120000 12222300 120000 12222300 00s o0s3s 9555 0007970 122000 120000 122000 0243 ossse 00970 220000 122000 122000 021s 9559 007971 2000 122000 120400 061 9559 0007971 220000 122000 120400 0.168 9561 0007972 20D 122000 120000 oss os61* 9562 oar 0007973 1220000 1220000 120000 120000 112202440000 o02m31 os62 007973 22000 120000 122000 029 9563 0007974 22000 120000 122000 0259 95630 0007974 2000 120000 122400 0254 9564 0007975 2000 122000 122400 om ose 0001975 12000 120000 120s ums STANDARD DEAVVIEARTAIGOEN:: 000.80338 * Duplicate injection LOQ= 0.01 g/gfor iverand0.01 pgf/ormserLum Centre Analytical Laboratories, Inc. Page 39.07 102 ONLsL _--_--nmmm Centre Study No. 023.041 Table XXI. Sponsor aSs5e67 s9s5n7ur0 s9s5n7s5e s9s577o9n ssssaa0r sasss sssstze oosstt asssaser sousatss Summary of PFOS in Juvenile Serum Samples at 17.6 ppm a.i. (Test Termination 12 Weeks) cenre 0o0r0s97 o0o009779777 wwoorse c0o07n9s75 00000077598800 owooorrs9se1 owroresse 000000758833 o0c0o07rsseass o00000n799s8s NomSbaer 21202000000 0000D> 00 00 m0o0pD 220000000 2D000000 w20o0o0d0 02000000 020000000 222000000 EDxantceion ADuues 21220000 T12229400 2222000000 112222440000 pzaoce 1r2a220e0000 apaonc 112222440000 2222000000 11222240000 a20o0e0 112222440000 aD2e00 1n2a4s0e 12222000000 112222640000 p22a00o0 rraaee p22a0v0e0 11222244000 STANDARD DEAVVIEARTAIGOEN:: FowAdnaGiyynet) 00332s9s o04s5i32 00220s0 0I2rs 00228s7 o0a2t9ss o0a4rss o05s2s1 oossss) o0s st 00.11134 * Duplicate injection LOQ = 0.01 g/g forliveanrd 0.01 pg. for serum Centre Analytical Laboratories, Inc. Page d00f 102 n0352 Centre Study No.: 023-041 `Table XXII. Summary of Percent Moistures for Quail Liver Samples SpoinDsor CeInDtre Mesure Sponsor Centre ID Moisture ast 0007867 667 9559 0007932 73 a2 007868 644 9s61 0007933 806 453 0007865 84 9562 0007934 578 asa 0007870 66 | oss 0007935 4 ass 0007871 61 956 0007936 346 56 0007872 ns 9570 0007938 852 as 0007873 95 9579 0007940 87 ass 007874 12 sas 0007945 96 "60 007876 0 oss 0007946 652 007878 sso 1025920780 0102997 03 a 007880 606 [EDl02s920781 0102998 518 a6 00882 75 [E0ssa0m 0102999 706 a 007884 615 [E01025920783 0103000 10 90 0007886 651 feia2s020784 0103001 7 9506 0007908 707 [EDl025020785 0103002 645 9508 0007908 721 [Ela2se20786 0103003 3 osiz 007910 4 [E0025920087 0103004 16 oss 0007912 732 [E010250.20788 0103008 60 9520 0007913 75 [E00259.20789 0103006 60 on 0007914 63 [E0I0259.20790 0103007 3 9526 07916 615 [E010259.20791 0103008 08 9530 07915 0 [E0I025920792 0103009 610 9540 0007923 667 [E010250:20793 0103010 3 9563 0007925 S11 [E0la2s020794 0103011 us 9544 0007926 558 E0lozse205 0103012 657 9548 0007927 S04 E0L0259.20796 0103013 na 9551 0007929 813 E010259.20797 010301 78 9552 0007930 $35 [E01025920798 0103015 73 9555 0007931 650 |E01oaso20m99 0103016 721 Centre Analytical Laboratories, Inc. Page 41 of 102 GN01L53 ---- ---------------------- ee -- E-- H -- ------ ------ -- Centre StudyNo.: 023-041 Centre Analytical Laboratories, Inc. Page 4201102 aos Contre SayNo:23001 Figure 1. Typical CalibrationCurvefor PFOS ~ : i ' 4 i | \ 7 H| ): i| is $ . be! 5 IM 5 a : | [at ay 22 [lef 5i le | = o ty | lai 9 3 B8 RrriiogiSrnEREERE" CentreAnalytical Laboratories, Inc. || Pa43g of1e 02 COOL: Centre StudyNo.:023-041 Figure 2. Chromatogram Representing a 0.1 ng/mL standard for PFOS EEEELEEEaInQ jae mE i ' omsp, dsm A eS Eee CentreAnalytical Laboratories, In. Pagoddof 02 GROL3G Contr Study No: 023041 Figure3. Chromatogram Representing a 1.0 ng/mL standard for PFOS RRREa FN Centre Asset Laborstres | | I Pa45gof1e02 | j | GROLH7 --e---------------------------------------------- Centre Study No.: 023-041 Figure 4. Chromatogram Representing a Reagent Blank for PFOS (Centre ID Reagent Blank A, Set: 122000A) Efe I EEL HTL Bie WE : aman Centre Analytical Laboratories, Inc. = [Page 46 of 102 C0153 --_--_-- 88 r- -- CentreStudyNo: 023.041 Figure 5. Chromatogram Representing Control Quail Serum for PFOS (Centre ID: 0011424 Blank A, Set:1220004) Ee HE | | I Centre AnalyticalLaboratories Ic. Page 4701102 CONLRS ------ CentreStudy Nos023.041 Figure 6. Chromatogram Representing Control Quail Liver for PFOS, (Centre ID: 0007870 Bla A,nSek t: 121900A) E [ERa EEL HT HEHE 1. P ErEETE CentreAnalyticalLaboratories,Inc. Pa48gof 1e02 GROLH0 _--_--m CentrStudyNo: 023041 Figure 7. Chromatogram Representing Control Quail Serum Fortified with 500 ng/mL of PFOS (Centre ID: 0011424 Spk A, Set: 122000A) EE ak. EXE Ef. i T aEE pe mse Centre Analytical Laboratories, Inc. Pa 49g of1e 02 nLol _---- Ceatre Study No.: 023-041 Figure8. Chromatogram Representing Control Quail Liver Fortified at 10 ppb with PFOS. (Centre ID: 0011423SpkA, Set: 121800A) fe ConeAki rti . || | ---- G001T Centre Study No.: 023-041 Figure 9. Chromatogram Representing Juvenile Quail Serum Sample (Centre ID: 0007965, Sponsor ID: 9544, Set: 1220004) EE = . . = SEE Fo CentreAnlytcalLaboratories Ic Pagoef10s2 GROLDET Contre Sudy No: 025.41 Figure 10. Chromatogram Representing Juvenile Quail Liver Sample (Centre ID: 0007926, Sponsor ID: 9544, Set: 121800B) EEE. OH B (EEmRE ho| . EEEEEL HE a[m- :: Contre Anaya! Laborstrs, ns. Page 200102 0n0194 CentreStudyNo 023.041 Study Protocol 00P-023-041 (Centre Study No. 023-041) and Amendments and Deviations CentreAnalytical Laboratories, Inc. Page 53of 102 NHI; CtrStady Nos023041 : CoonProoptzso01 STUDY PROTOCOL spy EXTRQAUCATIISONEORFAFAORTASSSSQUIPAUAIMLAPLVEIMRVAFESRLSFSUOPORERCAOTNORACOLMTYEASTNEREDYSSIUHLGEHPOLNFRAOTME seonsor SMEnvisnmerBlurTleaohgls1o3ga2y0t5dSutey Seis c : Scr . . .: DATAREQUREMENTS . AMy obo Ree ine TESTING LABORATORY ConeAnsiaoeCrRlLeasembioDrr1.6i3e01 (Goi 2 SRA PROTOCOLIDENTIFICATION NUMBER : weason ComAoi Liss. CeatreAnalytica Laboratories,nc. [ Pa4gofe02 600105 -------------------------------------------------------------- + Conte Study No: 23-081 '' Ceatre ProtocolNo. 00P-023-041 TE BRRGOAAATLALASoS SAESATVA ASs SEM - `TABLEOF CONTENTS we } TAOFBCONLTENETS 2 3 + FURIE memoior mgs | TESTMATERIALS remem : 3.7 SPONSORcrepes 4 TESTING FACILITY ANDPERFORMINGLABORATORY ..--.c4 - 5. PROPOSEDEXPERIMENTALTIME-FRAME cocoons. : : - : . 6. JUSTIFICATIONFORTHESELECTIONOFTHETEST SYSTEM ......ocv 87... ANALYTICALMETHOD cece SAMPLE PROCESSING, STORAGE ANDIDENTIFICATION .ccvunine 5. EXPERDENTALDESIGNcornice10 10. BROTOCOLAMENDMENTSANDDEVIATIONS cr 10 1AL. RQUEACLOIRTDYSAw SSURAe NCE r ln oe rr em 1I : 1W3e. ADRACTHAIAVNEDSTREAPTOERMTENT ceiverreceme mrrrecrmn 12 reeree EE -- 16 PROTOCOLAPPROVAL ce APPENDANALYTICALMETHODS cere 1S CenteAssy!Lorain,Ine. CentreAnalyticalLaboratories,Inc. Page20f43 Pa 55g of e 102 600197 | `CentreStudy Nos: 023-041 : Contr PrNoo.0cPZo3l061 Sud Tite: : } A SCRTARCQUFURAALYLRIAVESRSSFPOERSCTARLOMEESTRLYAGHBL : 1 PURPOSE TsiahmenpplucerpfioosreeOoffduFti oosfudpnycPile10essrlooyoreqonuiaolos(ncePreOuamSOs)nraumsOcpiblneegusmrealtPnhedoordqusuntanelaislilisveeedr, SCopmepcoiunmdesn"Fr(GoMmmeStehroudmumberETS.3-4.)1d5 H"EPxtLraCctEilonccOrfopsoaysasss AEsPTseSry-ls8ui.o6sr0sU)sawicinatgnheHtnhPleoLmnoCdsicEfOiicrcaoOtsibopnersraFyoMeradoscnshSeSerpcieccotanrlo8.mCeotmryp"ouGnMdsmeFrtohmodLivuemrbFeorr "sTthudyQfuoacyoAmspsulriaencsewUinhitEoPfA.enTSCAAnGoaoydLaaLboarbaoerryePrrsacItnc.swnildlaurittst4h0e CFR P20). . 2 TESTMATERALS - Th followinsate andar wllbowc: [Fevers]Totus|ry|Erp | . . [r[ os rco|w won |s ow6 t | `Chemicalnem and trctre ofthecompound is presentedbelow. Cormriocsal Name: Pecoroacasesaifonsc TUPACNume: hepad1calOoor cpwoiseds1i1n22l3it34fASSo66TnTTe8e88 MoClAeScuNluamrbWeeright: 479995(3C93SOT) i : : erp N : NIostpe:fTohreaotunrelsmuofloencsue 1podstsadiaraldtf[rCmOtFhSaOtSPKE],OmSo(leecounlewiedieghvtsS38f.rom Cen AsyaLarsen, Pests CentreAnalyticalLabortories,Inc. Pa$6gof1e02 620195 Centre StudyNo.: 023-041 CP o rNo.ce p 3001. :; Aofra"eccuomrednoiiflntlgecsbtheainmderefafcenruenodcdeysu8bxsCtdaoncnperpeicAnegip,ntm,isot,ortagLefcoaonbdiotcirionn,sg,abnofde.tahreFecoorsd. substanceswillbe includedsspartoftherawdatapackage. Alqseaanetasstbseatnocnes ndneyopepcrdtsFleronmtbee deetn,iwitha `HAZARDINFORMATION ) eAcngueeMlSyDSfortechica) ed isy illbo indat he : 3 sono - | FBuOilBding 33809 3MEnvironmentalTechnologyandSafetyServices Shaamssmam . . . . . SRTFTAUEoXDEoNYPkDRRUIOaRMREiCsTeB6eO5rR1E:e78R4n1e:7s6 .: : 4 TESTING FACILITYANDPERFORMINGLABORATORY Genre AriaLabrieI,c. Ct) 3So0t4a8RCeosleeargch7Dariv1e6101 (Ce . . : : TEEERLXANOTENSEEa.Rt sCHtoaome1-r0B32 + 5 PROPOSEDEXPERIMENTALTIMEFRAME Reports Dex 30.2000 . `ExperimentalStartDate: Experimental Termination Date Dee. 11,2000 Dec. 15,2000 6 QJuisUumSsmTiFOIiRdTiHvFESEImLpElCTcCIlONoOAFbTTyHWEiTIfESeTOSeYSmTNiEM it. . Foldonstaadetet y EP soo risesdy.c"isQe uSra n dydewt illbk laboratoryenvironment. Quail habitatsincludebushypastures,grassyroadsides, ------ fo CntreAnalytica LaborstoiIen,c. Page S70f102 600129 BR Centre Study No.: 023-041 Go Pres Noc3op00 . . - (fanbrdmesiamnatdsiianonfsdoah piennwoyoldlsanwdis,sw1ne0dstG(hoeAyraPireSnco.nsFiEdeOrSedwliandgpraazierds.T1hehuesveoefr 1NsAoc.C 4om1p0s4o Gtshpsiost nspoofdntsoeo r'wesispeyin nsetsm1io.nn4wiptSrh a4olnlOo.f MeIiNfSepUaRPrteAeeSsk % SAMPLEFROCESSING,STORAGEANDIDENTIFICATION = Noprceningwllrie oesr spe.Duefothe llmount TiR`oonfswaegmpnlethaveayilbawybilbel,ltdhelbbioverrresarmpilnesdwbillnoitnbgehomogepniieszeodpsrioor ttomeaxttriacctiaoond; VBAahciehhswiuiaelewenilsdlbofompsiginnga ondurseesdanfmcpilrem,emonfifcnhaeeisodnumeam.b1e0TreCa:,Ccpeile,t hmepncreimlolvebdfgo hictionhnd skayinsndceeGsnt nrahgeP. end Toe SGiuomvspanesrcs ALenldosrpasenspg1e4cntsiyoben1iS2necosdaeomonipcsnciiointngswitwlhlicslbeyrwiioelnldbe oe ote cn. 8 ANALYTICALMETHOD : : CTohmspcuiaemsssOFpfrfoemowuiSlnelbue.PaFiolrsysnAoccsaucsesantiunoUas1ii,nsgOHrmPLOlCrlnecBmroeoocshpaoaedynuhiieoadds + SF ecoiuve aiciym CoromioedO1can mOaahrcFoEarTiSo-oha +de4n1S)ii1n oelh"CeEoxcermoapcniaoisnnFOtmfnPLgiovaeesriaomlr EATnSi4s0iTngofHlPoLwCiBng meofecsiohnswiSllpomescpieis' aOtMh.mmhd:mas . So1.cTkoesrewniillosne,5ndsbtoipsnsasnad nweewili heexpnictnidontporno:ce. The . P`rSuteyopckseSoluati1a6aoc0nksdl(icoso:roefedboFOtSpIc1t010uu0gd..rblyowvmeeiegtthipinyga,cktA1S00dumposof orikmsatmpuenoo1f35m-mo.nLsDPrEombohreet)einof8perepirnion.210 Cfro Po CoonAnn Latour, Peso CentreAnalyticalLaboratories, nc. Page Stof 102 000200 --_--mnm----m---me CT . CentreStNou.;0d23-y041 CirProoclNoz.sr04p1. . .- . ! Rr i : : : + elLa0tuiy/onnli.ntFooi8fc1a0i0omnLSvooolnum-eptertaiesck1.0mBLionfguhpet1o00Ygofr.uswmoicteks methanol. ab. foLriufiianio.nFsoosilfuiicesnioinS.oo10n0-.Pkviolpuemse1tr0i0cmLs.koaftdhberi1n0gopfe1d0 . .0fv0or1uoucgafilwnoilntuh.Foocrmhtaiafineoca!tiiionoSo+lut1i0o0n: -Pviapueme1t0i0cfmLkosfotdheb0i.n1gvpgp/m6L. deaSfteoirgeoefanlpirofeorpratxriaf2ticiaotni.toonst6a%ndaforrds&omlaaxoinmsumiae1r2o5d-omfLL6DmPonEtbhestfeso)minhe8. . CalPbrreeap0ta.ir1oenspSgitixamLnLCdaaMnrdSdItshMe S0.c0a1tpe/nminfosrainfdicaadtsiionnsmoleucihnsa.n va ionof + Trheidsei. typial example;adorn]concentrationsmaybeprepared 5 . TolCooer. gel) Volume3(6) Dvdwbooy FoilCosme Gal). - 0a1 L2i 1100 ooon o0o0l1 001 o 52 11000 000002s 100 ost Sdtaoferioegeflnptlrocerapi8ab2rrinioCo.nfo a6ndfaodrs8lDoaoinms Gnp1e2o5mo.fL6DoP nboisru)nfnhe 2. ThhieelmflibveereusaasSmhepotlcdoeosnnwhil1l2sn2ootr0b1e2cpd.r1ob2yc.beDsaonuddetpotroimiumfkoieetehdxeshcaomimplo.egaeviladbelsec,rsiabmepdliens 3. Tshicleulsmbuenwig0ll5wboemi1gl0h0tfaIon.dlTtihvheeerwamimloouubnnet0t.of3of00.350(M2+T50M.B0.A9asaoncdditeuem tscauemoplneeavrionhlousmdpeifolonc a2b3c0o0in0sphcamk.eabTrhefeorrrsabma2dp0dloeeidnw.inillllabolelevy1te.bl0em1e0i0.edrSeatdmhwpiltechsew0n.i2ilplutgbeepnyllafoocnede=onh15 fiwlies0e: . Cnt AneelLaborer x. Pesotes CentreAnalyticalLaboratories, nc. Page s90f 102 Gozo (CentreStudyNo.: 023-041 Cntr Proce No.023p.041. Bs sm ecorb y.focSbaa tmphlresir weisl.lbe econutiviedin +iavolumeof 1mLof 4. The samplerwillbesyeduncerheflowsconditions: : LCMSIMSSyrem ndOpiratiogConditions Turbolonspray) MassSpc: PESCTEXAPI3000BiowelMaesscAmulylzeee | Inetice: HSaCrIaEXnTnubfoslioonnpSpapyLiquidIneodcionInce - | : Computer, PowerMinchG3 : Sova: WiPnEdSocwescNhTmiy1a1 . HAC: HovletHPkQauratGPIu)pSees 1100 Lo J BEPPAVuaocswmmplDeerguer BPColumnOven " HCPolLuCmCnToemupr:3s5eCsC4 onesChromatography),2. nx 0mm,4 : InjectionVol: 10BL. MoMobbiilleePPhhaassee((3A)): M2emthManAolco AcesinAST type Lwees : Flowhas: 03nllmin. .| T0w m 0Aw2Ww2 w is o0 m@ Ho 0. imnasyebetpeecfsosaanrayce0. dCosotitnesHwPiLthCgOfrfeiretdfdniomdee s1(io0po8,in2ns1e Bemtna3].3C0umaic))c4a0dnbceowueds,fporomvdidiefdferqeunitvmalaenntcuhfomrust(oKgerphiyoinss obuinet. I ConeAnica Labs, x. CenteAnayaLborsoisIc Petes Page 00102 600202 --_--_-- _ CentreStudyNo: 023.041 : GurProto.cps01 ; ATuOSe gMoet Toiieo9nM3o0niordi RehcoEupTeiiinneois) Oonnbadcahonfdmyoblush,aheeretinims ayvary ilyv epeniogan EiTxhnaemnfpoelleorwTiuonngeiFneiesP.aerrampAertloe,vreshdsesVnicleaTmaye,beACctai:n)dvfeo adyvveyifeom ener apni fo re in. . cTlohimeomeanrso)fpthce1s0oLksisnoilso0onn4eidn0w1t2inrgl0i.n5sTprheoml.oiPfRomOonbSislelpoansce,dpcGeoonagsrtsnagvTiof T{u0sn%emdoarh hme pi0e de0d%pp e2teMerassodr oafvoord1hea erewose,n cTIooc,.TOsnhcs ae eesmoilers uidmeeynn 0ecddio nogpri onimmisyo.. Teoni process oybe pen ess . IES Lc CSohnsnaltsy aisaoo . ; QR@RQoeuaiqFooRcdodROinetgmt - ao0g 55 ROQI QTeuaalgbRaiodd2Ofnfie 50503 . R20032S. QQTuuSinirmvaoiordfee 1i60o0 . CEDMFCCoaaMlDBeefcroenMailie w 3000 o. .i : PGGroareiinmnGsa snBa IlS Tiemoprnne - as` c [oIr--Ctansterempe rvolumMeesOFvDint 1001L0C2M0SpILASo,f xhcanon | Con yi Lebron Centre)Analytica Laborstrie, ns. Petar ) Pag1e of 02}| GOZO Centre StNou.0d23-y081 tt . . . t . ( Com PYo.pt 00. Bb sUaiannegtdienodeec,puUrxpvewareriegohgseopedfsrwraderiedasftyocneva.csAfsortyqbcyuhnlitoasre.spLdienaees obnfeicxnlgloodotednicosma3n0ed%l,sabatsailedoatnny cbieuscce.cHeodwdevoecrkoocnetoocrsd,nme0osr%t of elsomberofstandard fie. Tlhsiestc,5one2nn0i5a5o2np5cr(oo42fn05fs8p5ee(Is)fhc foourdcbalobueisbnolnboscaurrjlvloestigieetoreendt operon,nd herelevant of pes tbeena: SIoanfmecpatlcehhseAusnmaapm,ivfsoaliewne,d fco onhe,calbriaiotn hsaLnCdMeSrIsV(Sv.Eexsc.h1e0l10e201i1s)t [Se oy inSucnoddadriiacomsyponcding ot Js six coment be iinnfecccttonandnaisrtsbetoafpcseiracsiendddbysho(ainS)derythe5b1ieo0gnsisn.pineg o.ftAhllraspainde e. 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PROTOCOLAMENDANMDDEEVNIATTISONS, . bAendyodcvuimneinotnesd fdroepthoe prprcoplyfromheheSedlyyDiisncmoa,tPoan8apovcihdanegtewsil0l indsp`rsoptporcoovleodrbythheenPlryincipalbIvdesiwgiulilboemaanddeth wSitundyDitnssceoo.diAenyt faomernpd.s cedvinionswillbe appended(oisprosacl0dnudais he ConsAaya Labour, Pei0otes Centre AnalyticalLaboratories, Inc. Pa3gof1e02 GROEOs5 Fm | { : Lo ; : . -- CentreStNuos d023-y041 Cone Prepat s01 1. 1dBhorcherilneia,nabedyni dosnaism nPeassoep di chlianAa tglmeystedoedccehieosbwptelolrcbheoae npggr,rtd n!dcdhau. ildnbbooyr tehenPti0caquaIlivteyss acnidsSusyDien, opeofsentswilloe 2. Pdheerviountsrroifmntnehee:GpPorvroitntoocn,o,lhdpoletevbaedsa,ocwmfhecisicehad mcpsoactoyen.tsrneodsrnspylnanoengdt : Po icoracvoese n rsv endS.eyoDticctGeovdiaovniewsedptydGA1D.ddd vy 1. Recors : Records 0becoun. lodebot41 ot Bed he [llowig (5 32.0SS"SemFpl kaammprplyleeeandleikeeipcassdeisoe,n)tofasgdaiy(,iackd,hfroicotfiosni,ody:brn) 54AI Denstciipcis aocnouafssusym olcme,abefne chicott oeickogsnhasd . 75&.SAAecmloprmlopex lmemapatoitna iosfosdwndynsn poedels, cogntpiiosnsod ils ' 1101..ACny hbe darppeco ensaaynoofesccyooncosrpaipoonnnecs dy Al chromogrbae nolliowinng: b.SAnudleie,niaad,ejfonettena,riodanust,wsioolawocphoroodoeetnerioifendodriicngfuc.isotnionfletveelaorefateof Acimvieoe.lnscuengd.aerbd fnS,rpeomlsnoFgniFs,owilnadiiondly: incude te pEoaucrdhuyetceannh,sreusswwsii,llnlcoaoonebtiesn npeorrrnemeatonn,ohnnedtTeoemtprheorsso,pfmelowica.uTshg,ecCooeinnlrey miarn ConeAst Labor. Centre AnalyticalLaboratories,Inc. Pgennan Page64.ori! ONPG er--------------------. GeatreStudyNo 023041 :: CT oo TT ComteProtocol No.009-023-041. ir 12. QUALITYASSURANCE . Cocecnutmste QtAiUoarnsc(aawbcilie rlentgioo.wCtohienptere1oQchsB,UosneptYroipstyrtcoemeytaosdtGeUE . SoietPiopslevcoemprli,eCsoonGLMIa,r10anil,roege SondiDngsotf soi 1. DAANDTREPOART 1.oAfflrceretTihdlrtyhadcnah,le,iitpiloelytwhregksrisadonhitr,aocmosclotdwoiolnelbpe,anip,trixteneeldnooegvssesohdnmay,s . nnytyoleTpok psndor rimon.ilawooc t idwi bs : 2.DiAiincleci10oidokiwtililnliedbee,aordbbyoConnte,10sEpErAo.vTeesneipoi ecboysmSstlys { 21.AOnjcytivsssoddfpaasttsmsehdf heproc .. - 345..TSTNieaslemtemsaontc feariptaliesnio edendtllifdipyn ednabtyy nlag meddy,ali0ot,tUpourlnity,wandrcootehmerpchtoarkacteristics. - &5Acov mpte LiangofsCoorp stnytprsoisons pCe otneiwilvliet ondcotcmoopayao,offtChiendStAdrneDygiir1tiheThSe CtyosDnissQtArn,siwdehoiwlbilcioarss ScSoimmpkllaireosf.AtTehteemfednntaoefp eAmLonkp1b0aodcpaipnfvol 3b$ynssehmSoyaofDcOiLrycoapomidpoOoLtsoB ie tad on dlp . o oyaconi oeatfiboyn nshoocdwdpeitseathvotetsn h1efianTeoSooa nciha1lm lbehinlo che fyortKm: eonofr0y v comion e dThaesSmctae yinDeintchtallbesdsnd du bth Pops CoteAnte Liston CentreAnalyticalLaborsiorie, ne. Feds Pa5gof1e02 0007 3 CeatreStNuo.0d23-y041 i Con ProNotcoep zcs0t41 ! REPOOrRigTiDnI:STSRtIudByUDTIsOiNo:r . Copy: CenteAvives " 14. ARCHIVESTATEMENT Sotwuddyatc,oorbdsservbateiomnasnraeiconrdde:dRdeucroirndgshoebceomnadiunctaoifntehdefosrtyh,sucdoyriunmcelnutdaetaoln,l c"hcTahhrirascoemciaiztdaotegisroan1,dsdaepstecrcoiipmdtieonnntyoasfcikpqipnuigneignnrfeotcrowmradetsdisohd,aalralibnnedg trhedetcyiornne.dlautcetd ocf otmeesspuodnd.eAclel: . `adDomoccuaumnmeendntatac,ihisvnedes:tIeUpftionoaceocmppeolsenydao1nnodfabmrheensdtmdeync,tostphsyehaolrdlbayerrericeoiarndlse,prreaoctaoh,e wa3inMld.l - "ofbetcheofimnaelr1ep4r:aexdactecwopcy.cCpeanctkaegwei.ll eanfib elatedongnls.snd copy - 15. REFERENCES . : 1 GUoSo.dELaavbiorraatmoernyPalaPcreotSuonndaArgcs.yF.ialToRaskee,S40uCFbR sPCaontn1t9ra2olnActc(TeSCAs).r ! ConeAnseLabor a. CentreAnalyticalLaboratories, In. Pg ote Pa66gof1e02 Contr StayNo23061 : Ceatre Protocol No.00P-023-041 1 rRorocoLArROvAL : This protwlocol `was auditedbbyyththee Quilty Assurance Unit ofConeAnalytical QualityAssuranceReviewer, Centre Tempteatte `Quality Assurance Auditor Pinca avo,ete like Ehpane i - (iy Managmeennet ple . QEVilarnolee, . : Nlii)fA do=z arte : 0-E0z-e0 . `StudyDirector, 3M : ConsAniies ConsAnalyticalLabor, nian Pugs e10t102 --_--_--m CentreStudy No.: 023-041 !: ! Centre ProsocolNo.00P-023-041 * APPEA.N"CDoBImxXpc:oiAuoNnnAdsLoFfYrPTo IuCSAseLuuMEPorTAeHnOaDyeS rUsoingoBcLEtaBsxOctnthrsspFrfaoyorhincsessse Speco 8. "`SCEopxmiepccoiuoonndsoFfroPmotLaisvieosfPorAenaloysrisoUsincgHaEPlLnsCsaegamOtalyPfhoiooraacsshseirsieal . . ( i . . Coe iL CentreAnalytica Laboratories, oc. - estrus Pa68gof1e02i Co0wLe BESTCOPY AVAILABLE Centre Study No.:023-041 ste? sespmmrenr lei : "a gm re em ConteBROOPO 023N 0... : e RE e SRI oy ; na 0 ha Cen en QUTORY ee oT : BoS Gee miec iioso.m CeemERET ea Ra LD. CF an vim CO; i METNEALyhf abe EE Ta R=. ) ey Cu12 me Ar inp.Mend IT ts otBidoes BOr. " .: CE To . SR a Cos A aii. mL mite CentreAnalyticalLaboratories,Inc. Page 690f 102 GnOwtA _-- BESTCOPY AVAILABLE Co ee -- Centr StudyNo.:023-041 aPractNaOPO Or - . : : CL SEER i =i meve icee 7006}FSA PROBA BROS mPe ROa SE iREESE eee e RE C Ee Da ros el Dorn rein md pode CEO] LIST eniCe iL a mrss ESE Sh 0 |, TROSEAFpaimaceSH SY S CENCE Els pom57" c SeemimtnI ian h LE I . . wi ta FRO RS Ctaae SmtHS es so SE CDE ior ton ans me A NE TER NER CODSCe T mV ip onni veeies FieEd T TE } O er spades Cae FL R i shLeaE E r e mnT e ieASNlR eNnRRERE Ceotre AsalyticalLaboratories,Inc. I - ! Page 170143 Cone nay Labor, nc. Page 0oti02 CORA --- GEST COPY AVAILABLE Centre StNuo.0d23-y041 . SE HE em sei ConteProceso.00.00 BeS DeE R eBE ER DS eEASRRR ae roZt or EERR Ee a PS RS LE rlSDET C a a niga Siasms eni HEiL SR SEEERER TE C Es E Om RSnE L a . . 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