Document ByyGj1264RjEjyaGmNZNJqM6k

A R 1 U -0 1 5 I Laboratory Report Interim Report of Preliminary Data for 26 Week Capsule Toxicology Study with PFOS in Cynomolgus Monkeys Laboratory Report No. FACT-TOX-030 Covance 6329-223 Testing Laboratory 3M Environmental Technology & Safety Services 3M Environmental Laboratory Fluorine Analytical Chemistry Team (FACT) 2-3E-09 935 Bush Avenue, St. Paul, M N 55106 Laboratory Contact Kris Hansen, Ph.D. Bldg. 2-3E-09 P.O.Box 3331 St. Paul, M N 55133-3331 Phone: (651)778-6018 FAX: (651)778-7176 Requester Andrew Seacat and Marv Case 3M Company Toxicology Services 220-2E-02 St. Paul, M N 003677 PAGE 10F 5 3MENVIRREOPNOMRETNNTOA.LFLAACBTO-TROAXTO-0R3Y0 1 Introduction eTfhfeisctsstuodbysewrvaesddiensiCgnyendomtooelsgtuasbmlisohnakPeyFsO. TSedsiteatanriymianl-stawkeerleedvoelseadt wdahiilcyhbtyheorrealagreavnaogoebwseirthvavbalreioaudsverse aa2nm6i-mowuaenlestk.s osStfuePdraFyO.saSSmeipnralelsasacwmtoepsreleewscocitlohlelilcnetceatdegdferlfoarmotimnacltalhpteessautnleaim.niTmalhsaelwrseeawrte1es1reedntithftfroeeretehdneotEstienmvgeirropouonpimnsteasnnotdavloeLrnatehbgearconouduparsnoeaflcoyofzntehtdreol quantitatively for perfluorooctane sulfonate (PFOS). bam(SHnieneaLrtdlaayPebszCraoemm/ldEitapeuSilssnMeitisnasSwgidnMheeeritdSgee)rbh,emy-axpinFtrnredAaescdesCtvubeTadryel.uuilnaTsiqitshnepudegeidcpvatrcenieohrsisnroeuo.nnsmc-apeanatooierrgxinartabrgapsecehxtnyetc/dreaeclceoutcifrotvkrnoen.spoprwAoracnnyeafdtllauyunotriedrc.oeaTmcl hdhemeemteaaxiislcstsarsaalpcrceetoscnawtvtraoaemmirleaienbqtarluyenatinsntaitthnadetivsetulydy In all dose groups, PFOS levels generally increased through the 26-week time point A relatively dramatic itrnaccrkeeadsefoaicrclyurcrleodsebleytwthereonugthheowutetehke 2stuadnyd.thAelwl meeaktr4ixssapmikpelisnagminptleersvwalerMe waliethainndthfeemQaClegPuFidOelSinleevseplescified by the method RfGcohiolgaloonodwgroeLeu.dasbDiqonaurttaaahtloeiptryrpyercsePoeprnnaattrcreaotditlcihoemensregeaanusisidudrtaeehnlseianahlenyisgsd.ihs3TeoMshfteqsEsauenmarvlepiitrslyouensldt,msaatsecahncaootvaurladlLdiilnaabgbbelotecoroaaanttopstrhpiydilisecSrtaietmabdnleepd.rmaerldeimtOhoipndeasrrayetsiatnangbdPliasrrohecesedudabucjrececostrwdtoienrge to 2 SampleReceipt rSeeproarst,awmeprleesrewceeriveesdhbipeptwedeteonth10e/E6/n9v8iraonndm3e/2n/t9al9L. aEbnbvyiroCnomvaennctaelLLaabbopraetrosroyn.neSlaimniptilaetseidnaclcuhdaeidn-ionft-hciusstody upon receipt of the samples. 3 Holding Times There is no holding time criteria associated with these samples for LC/ESMSMS analysis. 003678 PAGE2 OFS 3MENVIRREOPNOMRETNNTOA.LFLAACBTO-TROAXTO-0R3Y0 4 Methods - Analytical and Preparatory AnFFFFfSraAAAAuolrymCCCCftaiTTTTcSc--t-a-eaMMMMlrnum--t--ms1243e..f..00t1o1rho,,,,rEEomAAOdxxnnltstthaairrvallaeyyccressttFriiiissoolfunnoiofirfdooPFAfffolPPountarooaosttAlrsaayoissnsucssiamhsiiluueyUmmmPssiesiiPPncrUfeeaglirlusfsHfiollnuiuPrngoooLrLooHoCccioPvtt/aaEceLnntrSaCeeEMnss-uexuESsltllffrueoaolccnfntotaranoUtleesasptooiernrraogOOyr/HttMOhhPeetahLrrseFACsrlS-unFEpioloulerenooccictrctrorhooFcemshlmpueeroimtacrryyaoicl/cMaohlneaCmsSsoeimcSraupplmeocuotrnrodOms tehteryr Fluid Using HPLC-Electrospray/Mass Spectrometry SaAmnpalleytperiespeaxrtaraticotend-fraoqmueaosuasmsapmle pmleastr,iHx wPLithCi/oEnSpMaiSriMngSr:eiaogne-npta[itreitnragbeuxtytrlaacmtimononium hydrogen sulfate O(TnBcAe t)h] einanaipoHn--TcBonAtroplaleirdisenfovrimroendm, tehnetaTnahleytceaitsiotnraicnsrefeargreendtinsetoleactnivoenly-ptoalragreotsrgaannioicnsicolfvlueonrto(cmhedmhyicl-atlesr.t- butyl ether), dried, and reconstituted in methanol for MS analysis. HPaIcmsnoonLollaHCuublymtPi/ilEtoeLennS.CpeMPhx,BFatarSasOnaeMsceS,atdtleShimdq:oeuanffarooyontrthemaoedlluyfeagtettfeerxafoiatiinurslteainr8tdcdye.t0twqoaismiuafnitatneeihnlrdjieeutiafcnatoettnestirhav.daleiysaRcwtnaheednoatfearropnalkraytciststohseisneeridwtssitttmeiahcrtreeiaoosmmunbgaoeahrtutywcanhpetreheeodanvfsoetaeinrmssietntehap.etnhhdFHeaaosPcrredoLellPCuixqFmausmOyindSsprtcleesehmlo,arlitounitvmotaieowastntotoiataghtnnhridadneaptlr1hhid%qiecu.id ForoglalonwicincgomHpPoLuCndsse,pianrcaltuiodnin,gESflMuoSroMchSepmroicvaildse. sEalercatpriodspanradya,cacnuiroanteizmateioannstefcohrnainqauleyzuisnegdapwrimidaerrialyngfoerof dasunebtdescaetqipourniemnotafcrmyolioloilsneic,oucnlhsaarcrriaoecanttese,riisssmtigcaelonlefertrhasleelcyaononapdleyartraeyt,eiiodsnasietclreferclataegtdimv. eeTlnyhtsmisuinilodiqntueisme btpooemtrhabetuaprrerdisme.daMwryoitilhoecnhu,iglwehsh-eaicnrheeraigoryenigzaesd;, detected. Ftmihsoeifrgsraehegxtsmhaemacevonpentledethd,aefrioynsrtaforPmaFogetOmhcSeheran(irQtoasncFitssensdrSuiescQttehiccOat4es9ad8n9a0aanlamydmscuisua,pn(ircoibmonerra4uer9ssye9pdiooisntnods,edibnliuegfcftettdoeriedfSnfaeQtsiraeOttnhe,tePaccnFhhdeOam2rSa3iccf0rateoalrmmcisoutomict(hppCeorris^mcitSoiaomOrnyps^ioao.unnndE. daTschthhisoatifon secondary ion fragmentation patterns. S Analysis 5.1 Calibration iAnsmtruidm-leenvteall, dexritfrat cCteadlimbraattriioxnccahliebcrkatsiotanncdhaerdcskasrteancdoamrdpliisaanntaiflyinzestdruemveernyta5l-r1e0spsaomnspeleisswtoitmhionn+it/o-r30% of the expected value. QtrweusopaoenxntitstraeatciootfenodonmfetaohtrerimtxaorcgrueervtseapsneacbliryfaitcceksdeaistuinbggahsteeeadrcihoonngsrLouinusepinarogrfetshgaermemspsulieolstni.palQenaurleaysnsptiiostan(twsieoe-nmigohoftneeiadtocr1hi/nxag,niamflyaoptdepeirsoopbf rtahisaeeted)ionfthe instrum ent 003679 PAGE 3 OF S 3MENVIRREOPNOMRETNNTOA.LFLAACBTO-TROAXT-O0R30Y 5.2 Blanks TAwddoiteixotnraalclyti,otnwbolasnakms,puletsiliozfinbglawnkatmeraatrsixsu, rursoegdafteormthaetriexx,tararecteexdtrcaaclitbedrawtioitnhceuarcvhesb,aatcreheoxftsraamctepdleasl.ong with each batch of samples and curves. Blanks are compliant if no targetanalyte is detected above the limit of detection for a specific analyte. In this study, all blanks were compliant. 5.3 Surrogates Tetra-hydro perfluorooctane sulfonate is used as a surrogate in this analysis. Surrogate response is monitored to confirm gross instrumental failure, if necessary. 5.4 Matrix Spikes Duplicate matrix spike analyses utilizing all target analytes were prepared and analyzed for one control tahniismraaLngFe omrasyerbaearnea-leyvsaislu, aretecdo.veries were within the acceptable range o f70-130%. Recoveries outside 5.5 Laboratory Control Samples Laboratory Control Samples are not a componentofthis study. 5.6 Sample Related Comments oEtxhterarcmteedtatbisosluiteessawmepreledsewteecrteeds.crIefenneecdefsosarroyt,heexrtkrnacotws mn mayebtaebsocliatnesneodfEfot-rFcOurSrEen-OtlyHuannchdafroarcPteOriAzeAd. No metabolites using a time-of-flight tandem mass spectrometer. 6 Bata Summary In all dose groups, PFOS levels generally increased through the 26-week time point A relatively dramatic btirnyacctrhkeaeesdmefoaeictrhclyoudrcrleoAdsebfleuytlwlthtearoebnulegthoheof ruwetestuehklets2stiusadnaydtt.athcAheelwldm.eeaktr4ixssapmikpelisnagminptleersvwael reMwaliethainndthfeemQaClegPuFidOelSinleevseplescified This report reflects the most accurate data available at this time. However, all numbers should be considered to be preliminary and are subject to change. 7 Data/Sam ple Retention Samples and extracts will be retained for future evaluation, if necessary. 8 Attachments 8.1 A ttachm ent A: Graphical and numeric summary of average PFOS levels in sera 8.2 A ttachm ent B: Full table of results for PFOS levels in sera 0036S0 PAGE4 OFS 9 Signatures Lisa Cdemeyn, AnAalytical Chemist Kris Hansen, Ph.D., Study Director 3MENVIRREOPNOMRETNNTOA.LFLAACBTO-TROAXTO-0R3Y0 l l r t H 1) Date Date 0036S1 PAGES OF S 300 00 r -- - -................ Covane 29-223 Monkey Serum 6329-223 250 00 200 00 PFOS ug/mL(ppm) 150 00 ---------------------------------------------- 100 00 M 0 0 --------- 000 Group 1M, 0.0mg/kg/day Group 1F, O.Omg/kg/day 0.0G2rmougp/k2gMld,ay Group 2F, 0.02m#1cg/d*y Group 3M, 0.5mg/kg/day Groiqj 3Ft 0.5mg/kg/dy Group 4M, 2mg/kg/day Group 4F, 2mg/k^day Dose Level t Series 1 = Baseline aSeries 2 =Week 1 Seres 3 = Week 2 Seres 4 = Week 4 Seres 5 = Week 6 Seres 6 = Week 8 EExTcSe-l8V-5o0sion 7 0 Seres 7 = Week 12 HSeres 8 =Week 16 Seres 9 = Week 20 Seres 10 = Week 24 Seres 11 = Week 26 ser223xJs SSSSeeeernnriieeee34!2 Serie5 S SSSeeerrinieeesss6S? SS3eeenneeessi9i10I 3/29/99 ZS3C00 Srudy Hi.dud Nutnber(Test Substance) Matrix C 'o v an cr 26 Week Capeuk Toxicity Study with PFUS in Cynomolgus Monkeys T-6295 (PFUS) Monkey Sen IW U Sample DaU Monkey Serum Croup Dose Method Blk Method Blk Matrix Blk Matrix Blk QT-250 ppb (lump 1M, 0 Omy/Vg/dey Group 1F, 0 Omg/kg>day Group 2M, 0 02mg/kf/day Group 2F, 0 02mg/k|/day Group 3M, 0 5m#if/day Group 3F, 0 5mg'kg/day GGrroouupp 44MF,, 22mmgg//kkgf//ddaayy 02/09/99 RWW 02/05/99 SAH 02/09/99 JCP 03/02/99 3AH/RWW 03/10/99 SAH 03/03/99 RWW/JCP 01/03/99 RWW/JCP ________ Baseline_________________________Week! ________________ Week2_________________ W eek4____________________ W eek6_______________ Week ________________Week 12__________ Sample* Average pros ug/mL S35 Std. Dev. Average pros ug/mL RSD Std. Dev. Average upgr/mo sL JtSD Average Std. Dev. p r o s mg/lmL ta b Std. Dev. Average n os WmL J a b Average Std. Dev. p ro s ug/mL rsd Std. Dev. Average ------W D p r o s Std. Dev. ug/mL 1120 b K-1 RabHb2itUSBenBcB-2lk-1 vMOL MDL <MDL MDL <MDL <MDL MDL <MDL <MDL <MDL MDL MOL MOL *MOL Rabbi) Sen Blk-2 1MDL <MDL <MDL <MDL <MDL <MDL <MOL 101% % <UDL 103% MDL 4% MDL 79% -MDL 10% -MW. 79% -M10%W 117% 5% 123% 0% 120% 2% 96% 3% 98% 2% 77% 11% 77% 11% MDI. MDL -MDL <MDL ckmL <MOt <MDL <MDL <MDL <MDL MDL -LOQ LOQ <L6q <UJQ <MDL <MDL <m d L <MDL " <<ULUGQL'" MDL LOQ 003)3 0 00409 LOQ LOQ <MDL <MDL <MDL 108 <MDL U S O il) 0137 l1.i3i7 0.104 0.120 399 425 00.)32603 d.io 4.63 o W 3 0.520 638 0 56 892 0 766 0 75 842 0945 H3I5I! <MDL <MDL <MDL <kibL i u T 5 7 3 25 MDL 4 63 0.568 6.73 <MbL i d i IW 33.6 <MDL 255 3.38 275 l Id 2 2 i 1.16 20.6 4.41 119 4.05 116 22.3104 tfi 49.4 U .i 23.5 lit 112 i.od 268 io i 888 iid 30.0 lii 133 iii 382 hi 14.8 44 0 34 7 4W97 lii 14) !?? 146 Sample DaU 3/12/99 SAH/RWW 3/15/99 JCP/SAH 3/16/99 RWW/SAH 3/16/99 RWW/SAH Monkey Serum Group Dot* ____________________________ Week 16_____________________ Week 20___________________ Week 24________________ Week 26__________ Sample N Average R sb Average b s b A n n g t -- Average ------RSD pros Std. Dev. p ro s Std. Dev. n o s Sid. Dot. p r o s Std. Dot. ug/mL ug/mL ug/mL ug/mL MMeetthhoodd BBllkk IRo b H 1120 Blk-2 MDL <MDL MDL <MDL <MDL <MDL MDL <MDL Matrix Blk Matrix Blk QC *250 ppb Rabbit Sen Blk-1 Rabbit Sen Blk-2 MDL 99% 106% <MDL MDL MDL <MDL <MDL MDL <MDL 4% 89% 16% 78% 121%% 89% 90% 8% 2% 85% 86% 17% 1% Group 1M, 0 Onif/kg/day Group 1F, 0 Ontf/kg'day LOUKQ) <Lo q LOQ 0 0551 00690 0000106625 0000651424 o00o0i8o4i 0000672239 0.0143 0.0158 Group 2M, 0 02mg/kg/day Group 2F. 0 02mg/kg'day Group 3M, 0$mg/kg/day Group 3F, 0 5mg/kg/day Group 4M. 2mg/kg/day Group 4F, 2mg/kg/day 140 13 1 701 52 6 30i 2 37 7 29 5 04 1)3 1)3 Hi 72 5 2I 2734 JJf 184 181 l3 0i 8i 4i 2 h i did 73 4 9.04 lii 16.4 idi 833 11..7776 ili 133 235 202 214981 179 194 13 7 27.2 221678 ill" 26.0 Id 214 4 ii 17.7 eot&0Co84 EETxcSe-l8V-5e0rsion 7 () Mfi223.xls 3/26/99 CFovAaCncTeT#O63X2-90-32023 Snidy: Product NumbcrCTeat Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Sofiware/Version: Filename: R-Squared Value: Slope: Y-Intercept: Date of Extraction/Analyst: Date of Analysis/Analyst: Date of Data Reduction/Analyst: BASELINE MONKEY SERA GDroosuep Sample # Method Blk H20 Blk-1 Method Blk H 20 Blk-2 Matrix Blk Rabbit Sera Blk-1 Matrix Blk Rabbit Sera BIk-2 QC - 250 ppb MKS02059-MS MKS02059-MSD Croup 1 I05508M Control 0.0 mg/kg/day 105S17M I05519M I05520M I05526M I05J27M 105529F I05S30F I05531F I05535F I05544F 105549F Group 2 105513M Low-Dose 105514M 0.02 mg/kg/day I05515M I055I6M I05521M 105525M I05537F 105541F I05S43F I05546F I05547F I05550F Group 3 105S05M Mid-Dose I05510M 0.5 mg/kg/day I05518M I05523M I05524M 105528M I05532F I05538F 105539F 105545F I05548F I05552F Group 4 105506M High-Dose I05507M 2.0 mg/kg/day 105509M 105511M 105512M I05522M I05533F 105534F I05536F 105540F I05542F 10555 IF Limit of Quantitation (LOQ): 25 ng/mL Method Detection Limit (MDL): 12 ng/mL 26 Week Capsule Toxicity Study with PFOS in Cynomolgus Monkeys TM-o6n2kUey(PSPerQaST ------- T ' t * r c lS . ' ) / { , - . ; FACT-M-3.J & FACT-M-4.1 Soup 020199 MassLynx 3.1 See Attachments See Attachments See Attachments See Attachments 02/09/99 RWW 02/13/99 MEE 02/15/99 KJH Sample Data PFOS PFOS Cone. Reported na/mL ui/mL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL 298 120% 283 114% 1.64 <MDL 1.68 <MDL 3.42 <MDL 1.81 <MDL 1.97 <MDL 1.83 <MDL 2.59 1.50 <<MMDDLL 2.07 <MDL 1.82 <MDL 1.95 <MDL 5.57 <MDL Z93 <MDL 1.94 <MDL 0.94 <MDL 2.94 <MDL Z06 <MDL 2.23 <MDL 1.68 <MDL 2.54 <MDL 2.83 <MDL 2.80 <MDL 21..0835 <MDL <MDL 31..4410 <MDL <MDL 1.86 <MDL 1.31 <MDL 2.15 <MDL 2.98 <MDL 3.40 <MDL 2.57 <MDL 2.47 <MDL 3.53 <MDL 3.85 <MDL 2.35 <MDL 2.50 3.07 <MDL <MDL 2.38 <MDL 2.98 <MDL 2.93 <MDL 3.02 <MDL 2.35 <MDL 2.83 <MDL 3.13 <MDL 3.70 <MDL 2.27 <MDL 3 77 <MDL Dale Entered/By: 02/17/99 LAC Date Verified/By: 03/23/99 GML Average PFOS iig/mL <MDL <MDL 117% <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL RSD Std. Dev. <MDL <MDL 5% <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL PFOS * Perfluorooclanesulfonate FACT-M-4.1 Excel Version 7.0 seru223 xls i/ 003684 3/26/99 CFovAaCnTceT#O63X2-90-32023 Study: Product NumbertTest Substance): MMaettrhioxd: /Revision: Analytical Equipment System Number: Instrument Software/Version: Filename: R-Squared Value: Slope: Y-Intercept: Dale of Extraction/Analyst: Date of Analysis/Analyst: Date of Data Reduction/Analyst: WEEK 1 MONKEY SERA Group Sample # Dose Method Blk Method Blk H20 Bile-1 H20 Blk-2 Matrix Blk Rabbit Sera Blk-1 Matrix Blk QC - 250 ppb Rabbit Sera B)k-2 MKS02059-MS MKS02059-MSD Group 1 Control I05508M 105517M 0.0 mg/kg/day I05519M I05520M I05526M I05527M I05529F I05530F 10553 IF I05535F I05544F I05549F Group 2 Low-Dose 105514M 105515M -o<.hcOlZmg/kg/day IOSS16M 105521M 105537F I05541F I05547F I05550F Group 3 I05505M Mid-Dose I05510M -O ri mg/kg/day 105518M I05523M 105524M I05528M 105532F I05538F I05539F 105545F I05548F I05552F Group 4 I05506M High-Dose I05507M -*0 mg/kg/day Ito05s5s0i9IMM 105512M I05522M I05533F I05534F 105536F I0554OF I05542F 10555 IF Limit of Quanutauon (LOQ): 25 ng/mL Method Detection Limit (MDL): !2ng/mL 26 Week Capsule Toxicity Study with PFOS in Cynomolgus Monkeys T-6295 (PFOS) Monkey Sera FACT-M-3.1 A FACT-M-4.1 Madeline 041098 4 Amelia 062498 MassLynx 3.1 See Attachments See Attachments See Attachments See Attachments 02/05/99 SAH 02/08/9,02/10/99.02/12/99,02/17/99 HOJ/DRB 02/10/99,02/16/99,02/26/99 HOJ/DRB Sample Data PFOS PFOS Average Cone. nt/mL Ruexp/omrtLed uPgF/OmSL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL 305 123 304 123% 123% 0.00 <MDL 0.00 <MDL 0.00 <MDL 0.00 <MDL 0.00 <MDL 0.00 <MDL <MDL 0.00 <MDL 0.00 <MDL 0.00 0.00 <<MMDDLL 0.00 <MDL 0.00 <MDL <MDL 495 0.990 383 0.957 519 1.04 677 1.35 1.08 684 1.37 464 1.16 581 519 1.16 1.04 1.18 287 5.74 209 5.23 342 221 6.84 4.41 318 413 5.30 689 5.74 161 5.38 257 5.15 248 4.13 184 4.61 232 465 195 3.90 4.63 665 411 26.6 27.4 351 482 23.4 24.1 711 28.5 539 26.9 26.2 564 28.2 451 22.6 393 26.2 419 209 749 29.9 377 25.1 255 Date Entered/By: 02/10/99.03/02/99 LAC Date Verified/By: 03/23/99 GML RSD Std. Dev. <MDL <MDL 0 <MDL <MDL 16.9 0.183 11.6 0.137 17.0 0.976 12.3 0.57 7.49 1.96 13.3 3 38 PFOS * Perfluorooctanesulfonate FACT-M-4 1 Excel Version 7 0 sera22.1xls 003685 3/26/W CFovAaCncTeT#O63X2-90*32023 Study: Product NumberfTest Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Filename: R-Squared Value: Slope: Y-Intercept: Date of Extnction/Analyst: Date of Analysis/Analyst: Date of Data Reduction/Analyst: WEEK 2 MONKEY SERA Group Sample # Dose Method Blk Method Blk H 20 BUc-1 H20 Blk-2 Matrix Blk Rabbit Sera Blk-1 Matrix Blk Rabbit Sera BUt-2 QC - 250 ppb MMKKSS0022005599--MMSSD Group 1 I05508M Control I05517M 0.0 mg/kg/day I05519M I05520M I05526M I05527M I05529F I05530F 10553 IF I05535F I05544F I05549F Group 2 105514M Low-Dose 105515M 0.02 mg/kg/day 105516M 105521M I05537F 105541F I05547F I05550F MGirdo-uDpos3e I05505M I05510M 0.5 mg/kg/day 105518M I05523M 105524M I05528M I05532F 105538F I05539F I05545F I05548F I05552F Group 4 I05506M High-Dose I05507M 2.0 mg/kg/day I05509M 105511M 105512M I05522M I05533F I05534F I05536F I05540F 105542F 10555 IF Limit of Quantitation (LOQ): 25 ng/mL Method Detection Limit (MDL): !2ng/mL 26 Week Capsule Toxicity Study with PFOS in Cynomolgus Monkeys T-6295 (PFOS) Monkey Sera FACT-M-3.1 4FACT-M-4.I Madeline 041098 li Amelia 062498 MassLynx 3.1 See Attachments See Attachments See Attachments See Attachments 02/09/99 JCP 02/15/99,02/22/99 HOJ 02/19/99,02/25/99 HOJ Sample Data PFOS PFOS Average nCgo/mneL. Reported ug/mL PFOS ug/mL cMDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL 293 300 118 121% 120% 4.09 <MDL 3.07 <MDL 4.53 <MDL 2.08 <MDL 2.02 <MDL 1.89 <MDL <MDL 0.520 <MDL 1.02 <MDL 1.90 <MDL 3.12 <MDL 0.380 <MDL 0.810 <MDL <MDL 575 1.28 513 1.28 492 1.49 425 1.42 1.37 446 1.49 722 1.44 527 550 1.32 1.22 1.37 227 7.58 301 6.01 350 8.75 285 5.69 195 7.78 384 7.68 7.25 173 5.75 416 8.33 232 5.80 329 6.59 320 8.01 295 5.90 673 747 37.3 626 31.3 746 299 706 28.2 976 39.1 899 35.9 33.6 778 31.1 650 588 3229..54 546 24.3 372 24.8 568 22.7 27.5 Date Entered/By: 02/22/99.03/02/99 LAC Date Verified/ By: 03/23/99 GML RSD Std. Dev. <MDL <MDL 2% <MDL <MDL 7.63 0.104 8.79 0.120 16.1 1.16 17.2 1.16 13.1 4.41 14.8 4 05 PFOS * Perfluorooctanesulfonate FACT-M-4.1 Excel Version 7 0 sera223.xls 003686 3/26/99 CFovAaCnTceT# O63X2-90-32023 Study: Product NumberfTesl Substance): Matrix: Melhod/Revision: Analytical Equipment System Number: 26 Week Capsule Toxicity Study with PFOS in Cynomolgus Monkeys T-6295 (PFOS) Monkey Sera ETS-8-4.0 and ETS-8-5.0 Madeline 041098. Amelia 062498, & Soup 020199 Instrument Softwate/Version: Filename: MassLynx 3.1and 3.2 See Attachments R-Squared Value: Slope: Y-Intercept: Date of Extraction/Analyst: Date of Analysis/Analyst: See Attachments See Attachments See Attachments 03/02/99 SAH/RWW 03/05/99,03/08/99.03/25/99 HOJ/MEE/DRB Date of Data Reduction/Analyst: 03/08/99,03/26/99 KJH/DRB Sample Data WEEK 4 MONKEY SERA Group Dose S am ple# PFOS Cone. PFOS Reported Average PFOS RSD Std. Dev. ng/mL ut/mL ug/mL Method Blk Method Blk H20 Blk-1 H20 Blk-2 0 0 <MDL <MDL <MDL <MDL Matrix Blk Rabbit Sera Blk-I 0 <MDL Matrix Blk Rabbit Sera Blk-2 0 <MDL <MDL <MDL Matrix Blk Matrix Blk Matrix Blk Monkey Sera Blk-1 Monkey Sera Blk-2 Monkey Sen Blk-3 7.21 7.17 7.26 <LOQ <LOQ <LOQ <LOQ <LOQ Matrix Blk Monkey Sera Blk-4 6.32 <LOQ <LOQ <LOQ QC - 250 ppb MKS03029-MS-1 253 102 MKS03029-MSD-1 250 101 101 1% QC - 250 ppb MKS03029-MS-2 242 98% MKS03029-MSD-2 235 95* 96 3* Group 1 I05508M 5.43 <LOQ Control I05517M 6.76 <LOQ 0.0 mg/kg/day 105519M 7.91 <LOQ I05520M 6.11 <LOQ I05526M 6.73 <LOQ I05527M I05529F 1.98 6.63 <<LLOOQO <LOO <LOQ I05530F 6.11 <LOQ I05531F 9.19 <LOQ I05535F 8.17 <LOQ I05544F 9.% <LOQ I05549F 8.74 <LOQ <LOQ <LOQ Group 2 105514M 108 3.58 Low-Dose 0.02 mg/kg/day 10S515M 105S16M 172 3.43 196 3.91 18.1 I05S21M 101 5.03 3.99 0.720 I05537F 186 4.65 I05541F 153 3.83 I05547F I05550F 221 163 4.43 4.08 8.53 4.25 0.363 Group 3 I05505M 63.7 21.2 Mid-Dose 105510M 64.6 21.5 0.5 mg/kg/day 105518M 101 25.2 I05523M I05524M I05528M 110 22.0 96.3 95.7 19.3 23.9 9.47 22.2 2.10 I05532F 41.4 20.7 I05538F 117 23.3 I05539F 35.8 17.9 I05545F 46.7 23.4 I05548F I0S552F 78.3 55.9 196 18.6 114 20.6 2.34 Group 4 I05506M 118 295 High-Dose 2.0 mg/kg/day I05507M I05509M 10551IM 105512M I05522M 27.2 27.3 24.2 29.0 30.8 90.6 68.4 60.5 96.6 103 73.8 119 87 8 I05533F 35.2 176 I05534F 36.3 181 I05536F I05540F I05542F 10555 IF 24.0 80.0 834 83.4 29 4 15.0 97.8 75.2 42.7 116 49 4 Limit of Quantitation (LOQ): PFOS 15.2 ng/mL Method Detection Limit (MDL): PFOS 4.76 ng/mL Date Entered/By: 03/08/99,03/26/99 LAC Date Verified/ By: 03/23/99 GML PFOS = Perfluorooctanesulfonate 003637 ETS-8-5.0 Excel Version 7.0 sera223.xls 3/26/09 CFoAvaCnTceT#O63X2-90-32023 Study: 26 Week Capsule Toxicity Study with PFOS in Cynomolgus Monkeys Product NumberfTest Substance): T-6295 (PFOS) Matrix: Monkey Sera Method/Revision: ETS-8-4.0 and ETS-8-5.0 Analytical Equipment System Number: Madeline 041098. Amelia 062498, & Soup 020199 Instrument Softwtue/Version: MassLynx 3.1 and 3.2 Filename: See Attachments R-Squarcd Value: See Attachments Slope: See Attachments Y-Intercepl: Date of Extraction/Analyst: See Attachments 03/10(99 SAH Date of Analysis/Analyst: 03/12/99,03821/99 MEE/DRB Date of Data Reduction/Analyst: 03//18/99,03/24/99 LAC/DRB Sample Data WEEK 6 MONKEY SERA Group Dote Semple # PFOS Cone. PFOS Reported Average PFOS RSD Std. Dev. ng/mL ug/mL ug/mL Method Blk H20Blk-l 0.00 <10 ppb Method Blk Matrix Blk Matrix Blk H20 Blk-2 Rabbit Sera BUt-1 Rabbit Sera Blk-2 7.74 0.00 4.19 <10 ppb <10 ppb <10 ppb <10 ppb <10 ppb <10 ppb <10 ppb Matrix Blk Monkey Sera Blk-1 2.56 <10 ppb Monkey Sera Blk-2 2.55 <10 ppb Monkey Sera Blk-3 1.93 <I0ppb Monkey Sera Blk-4 0.5 <10 ppb <10 ppb <10 ppb QC - 250 ppb MKS03109-MS-1 264 106 MKS03109-MSD-1 253 101* 103* 4% QC - 250 ppb MKS03109-MS-2 243 97% MKS03109-MSD-2 249 100* 98* 2 Group 1 I05S08M 0.00 <MDL Control I055I7M 0.00 <MDL 0.0 mg/kg/day I05519M 0.00 <MDL I05520M 1.60 <MDL I05526M 0.61 <MDL I05527M 9.49 <MDL <MDL <MDL 105529F 1.56 <MDL I05530F 3.38 <MDL 10553IF 4.24 <MDL 105535F 0.00 <MDL I05544F I05549F 0.00 <MDL 3.54 <MDL <MDL <MDL Group 2 105514M 36.6 4.58 Low-Dose 105515M 33.1 4.13 0.02 mg/kg/day 105516M 32.5 4.06 11.9 I0SS21M 41.8 5.23 4.50 0.537 I05537F 42.7 5.34 105541F 45.7 4.57 I05547F I05550F 36.4 4.55 11.2 32.7 4.08 4.63 0.520 Group 3 I05505M 87.4 26.2 Mid-Dose 105510M 56.1 28.1 0.5 mg/kg/day 105518M I05523M 105524M 66.9 25.1 61.9 23.2 72.7 27.2 8.09 I05528M 61.6 23.1 25.5 2.06 105532F 61.2 23.0 I05538F 94.5 23.6 I05539F 61.4 23.0 I05545F I05548F 94.5 28.4 61.3 23.0 11.4 (OJ5J2F 67.0 20.1 23.5 2.68 Group 4 I05506M 182 114 High-Dose 2.0 mg/kg/day I05507M I05509M 105511M 105512M 105522M 165 230 234 211 203 103 115 117 132 8.54 127 118 10.1 I05533F 232 116 I05534F 166 104 I05536F 179 112 I05540F 105542F 10555 IF 227 203 205 113 127 102 112 78..8980 Limit of Quantitation (LOQ): 25 ng/mL Date Enlered/By: 03/19/99,03/24/99 LAC Method Detection Limit (MDL): 12 ng/mL Date Verified/By: 0 PFOS Perfluoroocianesulfonate irrs-H-5 o Excel Version 7 0 sera223.xls 0036S8 3/26/99 CFovAaCncTeT#O63X2-90-32023 Study: 26 Week Capsule Toxicity Study with PFOS in Cynomolgus Monkeys Product NumberfTest Substance): Matrix: TM-o6n2k9e5y(PSFerOaS) Method/Revision: Analytical Equipment System Number: Instrument Softwarc/Version: Filename: R-Squared Value: Slope: ETS-8-4.0 and ETS-8-5.0 Soup 020199 MassLynx 3.1and 3.2 See Attachments See Attachments See Attachments Y-Intercepl: See Attachments Date of Extraction/Analyst: 03/03/99 RWW/JCP Date of Analysis/Analyst: Date of Data Reduction/Analyst: 03/05/99,030999,03/25/99 HOJ/MEE/DRB 03/08/99,03/15/99,03/26W DRB Sample Data WEEK 8 MONKEY SERA Group Sample # Dace prosCone. ng/mL RPepFoOrtSed ug/mL Average PFOS ug/mL RSD Std. Dev. Method Blk H20 Blk-I 0.00 <MDL Method Blk H20 Blk-2 0.00 <MDL <MDL <MDL Matrix Blk Rabbit Sera BIk-1 0.00 <MDL Matrix Blk Rabbit Sera Blk-2 0.00 <MDL <MDL <MDL Matrix Blk Monkey Sera Blk-1 0.00 <MDL Matrix Blk Monkey Sera BIk-2 0.00 <MDL <MDL <MDL QC - 250 ppb MKS03039-MS-1 174 70* QC 250 ppb MKS03039-MSD-1 MKS03039-MS-2 191 205 77* 73* 9* 83* Q C -250 ppb MKS03039-MSD-2 MKS03039-MS-3 MKS03039-MSD-3 185 181 203 75* 79* 10* 7832** 77* 11% Group 1 I05508M 9.43 <MDL Control I05517M 7.68 <MDL 0.0 mg/kg/day I0S519M 12.0 <MDL I05520M 9.03 <MDL I0S526M 11.0 <MDL I05527M 28.8 0.0480 <MDL <MDL I05529F 16.0 <LOQ I05530F 18.3 <LOQ 10553IF 18.0 <LOQ I05535F 14.5 <LOQ I05544F 9.46 <MDL Group 2 I05549F 105514M 15.0 37.2 <6L.2O0Q <LOQ <LOQ Low-Dose I055I5M 33.8 5.63 0.02 mg/kg/day 10S516M 47.1 6.73 8.88 105521M I05537F 34.4 49.2 6.88 7.03 6.36 0.565 105541F 39.0 6.51 I05547F 40.1 6.68 11.8 I05550F 37.1 5.30 6.38 0.752 Group 3 I05505M 122 34.8 Mid-Dose 0.5 mg/kg/day 105510M I05518M 9842..19 27.6 31.4 I05S23M 91.6 30.5 I05524M 118 39.4 12.7 I05S28M 107 30.7 32.4 4.12 I05532F 86.1 34.5 I05538F 106 30.3 I05539F 82.6 33.1 105545F 122 30.5 I05548F 694 27.8 12.7 I05552F 59.5 23.8 30.0 3.82 Group 4 High-Dose I0SS06M I05507M 122 157 83.8 107 2.0 mg/kg/day I05S09M 117 128 105511M 89.8 115 I055I2M IIS 147 16.7 I05522M 127 163 136 22.8 I05533F 107 138 I05534F 98.1 151 I05536F 100 128 I05540F 102 131 I05542F 10555 IF 113 99.2 114059 11.1 133 14.8 Limit of Quantitation (LOQ): 25 ng/mL Date Entered/By: 03/08/99,03/24/99,03/26/99 LAC Method Detection Limit (MDL): 12 ng/mL Date Verified/By: 0 PFOS Perfluorooctanesulfonaie ETS-8-5.0 Excel Version 7.0 sera223 xls 003689 3/26/99 CFovAaCnTceT#O63X2-90-32023 Study: 26 Week Cipiule Toxicity Study with PFOS in Cynomoigui Monkeys Product Number(Test Substance): T-629S (PFOS) Matrix: Monkey Sera Method/Revision: ETS-8-4.0 and ETS-8-5.0 Analytical Equipment System Number Soup 020199 Instrument Software/Version: Filename: MassLynx 3.2 See Attachments R-Squared Value: See Attachments Slope: See Attachments Y-Intercept: Date of Extraction/Analyst: See Attachments 03/03/99 RWW/JCP Date of Analysis/Analyst: Date of Data Reduction/Aoalyst: 3/09/99.03/10/99.03/25/99 DRB 03/15/99,03/24/99,03/26/99 DRB Sample Data WEEK 12 MONKEY SERA Group Dose S am p le# PFOS Cone. ng/mL PFOS Reported ug/mL Average PFOS ug/mL RSD Std. Dev. Method Blk Method Blk Matrix Blk H20 Blk-1 H20 Blk-2 Rabbit Sera Blk-1 0.00 0.00 0.00 <<MMDDLL <MDL <MDL <MDL Matrix Blk Rabbit Sen Blk-2 0.00 <MDL <MDL <MDL Matrix Blk Matrix Blk Monkey Sen Blk-1 Monkey Sen Blk-2 0.00 0.00 <MDL <MDL <MDL <MDL QC - 250 ppb MKS03039-MS-1 174 70 MKS03039-MSD-I 191 77 73* 9* QC - 250 ppb MKS03039-MS-2 MKS03039-MSD-2 205 185 83% 75 79* 10* Q C -250 ppb MKS03039-MS-3 MKS03039-MSD-3 181 203 73* 82* 77* 11* Group 1 Control 0.0 mg/kg/day I05508M I05517M I05519M I05520M 30.9 0.0476 26.9 0.0537 32.8 0.0547 12.7 <LOQ I05526M 21.3 <LOQ 7.67 I05527M 32.6 0.0572 0.0533 0.00409 I05529F 13.2 <LOQ I05530F 18.4 <LOQ 10553 IF 21.1 <LOQ I05535F 11.2 <MDL I05544F 20.2 <LOQ I05549F 25.6 0.0433 <LOQ <LOQ Group 2 105514M 44.7 8.278 Low-Dose 0.02 mg/kg/day I0S515M IOS5I6M 47.5 8.636 50.6 8.72 8.59 I05521M 48.1 100 8.92 0.766 I05537F 61.3 9.02 I05541F I05547F 105550F 3379..56 52.0 7.49 9.43 7.76 8.42 01.914.25 Group 3 Mid-Dose 0.5 mg/kg/day I05505M I05510M 105518M 143 50.0 135 49.0 133 42.1 I05523M I05524M 88.0 44.0 118 47.1 15.3 I05528M 79.2 31.7 44.0 6.73 I05532F 86.9 32.2 I05538F I05539F 94.2 101 41.0 34.7 I05545F II0055554582FF 109 40.2 7779..46 28.9 14.3 30.9 34.7 4.97 Group 4 High-Dose 2.0 mg/kg/day I05506M I05507M I05509M 105511M 103 144 86.4 133 116 154 83.9 124 105512M I05522M 149 88.0 209 19.6 150 152 299 I05533F I05i34F 109 100 IS8 143 I05536F I05540F I05542F 10555 IF 63.6 80.0 122 140 128 114 164 100 146 145 14.6 Limit of Quantitation (LOQ): 25 ng/mL Date Entered/By: 03/08/99,03/24/99,03/26/99 LAC Method Detection Limit (MDL): 12 ng/mL Date Verified/By: 0 PFOS Perfluorooctanesulfonate [rrs-8-5.0 Excel Version 7 0 sera223.xls 003690 3/26/99 CFovAaCncTeT#O63X2-90-32023 Study: Product Number(Tesl Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Venion: Filename: R-Squared Value: Slope: Y-Intercept: Date of Extraction/Analyst: Date of Analysis/Analyst: Date of Data Reduction/Analyst: 26 Week Capsule Toxicity Study with PFOS in Cynomolgus Monkeys T-6295 (PFOS) Monkey Sera ETS-8-4.0 and ETS-8-5.0 Soup 020199 MassLynx 3.2 See Attachments See Attachments See Attachments See Attachments 3/12/99 SAH/RWW 03/13/99,03/19/99 DRB 03/16/99.03/24/99 DRB Sample Data WEEK 16 MONKEY SERA CDroosuep Sample # PFOS Cone PFOS Reported Average PFOS RSD Std. Dev. ng/mL ug/mL ug/mL Method Blk Method Blk Matrix Blk Matrix Blk H20 Blk-1 H20 Blk-2 Rabbit Sera Blk-1 Rabbit Sera Blk-2 0.00 0.00 0.00 0.00 <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL Matrix Blk Matrix BUc Monkey S en Blk-1 Monkey Sen Blk-2 36.21 21.43 0.03621 0.02143 0.0288 0 QC - 250 ppb M K S 0 3 129-M S -1 MKS03129-MSD-1 280 269 101% 97% 99% 4% QC - 230 ppb MKS03129-MS-2 269 97% MKS03129-MSD-2 316 116% 106% 16% Group 1 Control 0.0 mg/kg/day I05508M I05517M I035I9M I05J20M 21.5 <LOQ 20.4 <LOQ 21.1 <LOQ 20.7 <LOQ I03326M I05327M 3189..49 <LOQ 0.0767 <LOO <LOO I03329F I05330F 35.5 0.0546 25.7 <LOQ 10553 IF I05535F 21.5 <LOQ 9.57 <LOQ I05544F 11.6 <LOQ I05549F 28.9 0.0577 <LOQ <LOQ Group 2 Low-Dose 0.02 mg/kg/day 105514M I055I5M I0S516M I05521M 77.7 13.0 47.3 11.8 81.7 12.6 21.9 83.1 18.5 140 3.05 I05537F 10554 IF I05547F I05550F 76.4 13.9 69.2 15.4 66.8 13.4 18.1 53.9 980 13.1 2.37 Group 3 Mid-Dose 0.3 mg/kg/day I05505M I055I0M 105518M 222 74.1 330 66.1 379 75.7 I05523M I05524M 326 65.2 475 79.2 10.4 I05528M 362 60.3 70.1 7.29 I05532F 252 50.4 I05538F 279 46.5 I05539F 347 57.8 I05545F I05548F I05552F 323 538 324213 58.7 9.59 48.2 52.6 5.04 Croup 4 High-Dose 2.0 mg/kg/day I05506M I05507M I05509M 273 228 257 214 296 246 105511M 105512M I05522M I05533F 268 223 296 270 8.42 254 231 235 19.8 245 204 I05534F I05536F 196 196 184 229 I05540F I05542F 105551F 258 231 191 215 210 159 11.9 202 24.1 Limit of Quantitation (LOQ): 25 ng/mL Dale Entered/By: 03/08/99,03/17/99,03/24/99 LAC Method Detection Limit (MDL1: )2ng/mL Date Verified/By: 0 PFOS = Perfluorooctanesulfonale ETS-8-5 0 Excel Version 7 0 sera22.Vx)s 003691 3/26/99 CFovAaCnTceT#O63X2-90-32023 Study: 26 Week Capsule Toxicily Study with PFOS in Cynomolgus Monkeys Product NumberCTest Substance): T-6295 (PFOS) Matrix: Monkey Sera Method/Revision: ETS-8-4.0 and ETS-8-5.0 Analytical Equipment System Number: Soup 020199 Instrument Soflware/Venion: MassLynx 3.1 Filename: See Attachments R-Squared Value: See Attachments Slope: Y-Intercept: Date of Extraction/Analyst: Date of Atialysis/Analyst: Date of Data Reducdon/Analyst: See Attachments See Attachments 3/15/99 JCP/SAH 03/16/99 DRB 03/17/99 DRB Sample Data WEEK 20 MONKEY SERA Croup Dose Sample # PFOS PFOS Average RSD Cone. ng/mL Ruegp/omrtLed PFOS Std. Dev. ug/mL Method Blk Method Blk Matrix Blk Matrix Blk Matrix Blk Matrix Blk QC - 250 ppb H20 Blk-I H20 Blk-2 Rabbit Sen Blk-1 Rabbit Sen Blk-2 Monkey Sen Blk-I Monkev Sen Blk-2 RBS03159-MS-1 RBS03159-MSD-1 0.00 0.00 0.00 0.00 0.00 0.00 232 208 <<MMDDLL <MDL <MDL <MDL <MDL <MDL <MDL NA NA NA NA 94% 84% 89% 11% QC - 250 ppb RBS03159-MS-2 RBS03159-MSD-2 191 195 77% 79% 78% 2% Group 1 Control I05508M I05517M 30.4 0.0434 31.4 0.0523 0.0 mg/kg/day I0S519M I05520M 19.3 <LOQ 23.2 <LOQ I05526M I05527M 30.0 31.5 0.0461 0.0788 0.0551 29.4 0.0162 I05529F 51.6 0.0770 I05530F 38.3 0.0722 10553 I F 105535F I05544F I05549F 28.3 0.061J 19.4 <LOQ 29.6 39.1 0.0630 0.0711 9.5 0.0690 0.0065 Group 2 Low-Dose 0.02 mg/kg/day I05514M I05515M I05516M 10552IM I05537F I05541F 105547F I05550F 88.6 15.5 86.7 13.3 101 98.3 14.9 17.6 11.4 15.3 1.74 70.2 73.2 96.6 359 13.8 14.4 17.9 51.3 14.6 15.3 2.23 74.4 24.3 IS.I Group 3 Mid-Dose I05505M 105510M 237 77.8 253 79.0 0.5 mg/kg/day 1055 IBM I05523M I05524M I05528M I05532F 248 78.8 319 220 223 93.8 79.9 67.6 10.5 79.5 8.37 255 86.4 I05538F 201 59.1 I05539F 105545F I05548F I05552F 210 97.6 171 204 154 57.0 81.5 53.3 25.4 72.5 184 Group 4 I05506M 381 197 High-Dose 2.0 mg/kg/day I05507M 105509M 105511M 105512M I05522M I05533F 282 173 315 189 352 309 302 158 178 ISI 7.62 179 13.7 393 210 I05534F I05536F 303 178 274 182 I05540F I05542F 10555 IF 441 302 330 241 189 140 165 194 27.2 Limit of Quantitation (LOQ): 25 ng/mL Date Entered/By: 03/08/99,03/17/99 LAC Method Detection Limit (MDL): !2ng/mL Dale Verified/By: 0 PFOS = Perfluorooctanesulfonate * Calculated without sample I05J50F. ETS-8-5 0 Excel Version 7 0 sera223 xls 003692 3/26/99 CFovAaCncTeT#O63X2-90-32023 Study: Product NumbcrCTesl Substance): Matrix: Method/Revision: Analytical Equipment System Number: Instrument Software/Version: Filename: R-Squared Value: Slope: Y-Intercept: Date of Extraction/Analyst: Date of Analysis/Analyst: Date of Data Reduction/Analyst: 26 Week Capsule Toxicity Study with PFOS in Cynomolgus Monkeys T-6295 (PFOS) Monkey Sera ETS-8-4.0 and ETS-8-5.0 Amelia 062498 & Soup 020199 MassLynx 3.1 See Attachments See Attachments See Attachments See Attachments 3/16/99 RWW/SAH 03/17/99,03/23/99 DRB 03/23/99,03/24/99 DRB S am p le Data WEEK 24 MONKEY SERA Group Dose S am ple# PFOS PFOS Avenge RSD nCgo/mneL Reported ug/mL PFOS Std. Dev. ug/mL Method Blk Method Blk Matrix Blk Matrix Blk Matrix Blk Matrix Blk QC - 250 ppb H20 Blk-1 H20 Blk-2 Rabbit Sera Blk-1 Rabbit Sera Blk-2 Monkey Sera Blk-1 Monkey Sera Blk-2 RBS03169-MS-1 RBS03169-MSD-1 0.00 0.00 0.00 0.00 0.00 0.00 218 236 <MDL <MDL <MDL <MDL <MDL <MNADL <MDL <MDL NA NA NA 88% 95% 92% 8% QC - 250 ppb RBS03169-MS-2 RBS03169-MSD-2 231 213 93% 86% 89% 8% Q C -250 ppb RBS03169-MS-3 RBS03169-MSD-3 224 220 90% 89% 90% 2% Group 1 Control 0.0 mg/kg/day I05508M I05517M I055I9M I05520M I05526M I05527M I05529F 36.4 0.0560 30.3 0.0606 25.8 0.0517 19.4 <LOQ 24.8 <LOQ 17.7 36.7 0.0765 0.0612 0.0109 40.4 0.06 I05530F 10553IF I0553SF I05544F I05549F 24.2 <LOQ 25.9 0.05 8.36 16.2 33.4 <LOQ <LOQ 15.4 0.06 00544 0.0084 Group 2 Low-Dose 0.02 mg/kg/day 105514M I05515M I055I6M 105521M 105537F 115 18.3 85 13.6 132 17.6 21 141 22.9 18.12 3.815 134 16.7 I05541F I05547F I05550F 133 85 108 17.1 15.9 15.2 16.25 0.8542 Group 3 Mid-Dose 0.5 mg/kg/day 105505M I05510M I0S518M I05523M I05524M I05528M 105532F I05538F 251 96.6 186 81.4 191 73.4 164 74.4 201 155 86.8 10 80.9 82.26 8.58 145 78.7 153 60.6 I05539F 105545F I05548F I05552F 142 86.8 168 79.3 196 139 7707.01 7541 91.024 Group 4 High-Dose 2.0 mg/kg/day I0S506M I055O7M I05509M 110055551121MM 105522M 287 247.1 234 234.4 MM 258 257.9 309 233 329018..46 11.61 267.86 31.1 I05533F I05534F I05536F I05540F I05542F 10555 IF 280 225 225307..16 207 210.8 218 187.8 240 226.5 12.0 131 187.1 216.64 26.0 Limit of Quantitation (LOQ): 25 ng/mL Date Entered/By: 03/24/99 LAC Method Detection Limit (MDL): 12 ng/mL Date Verified/By: 0 PFOS Perfluorooctanesulfonate CTS-K-5.0 Excel Version 7.0 sera223.xls 003693 3/26/99 CFoAvaCnTceT#O63X2-90-32023 Study: Product NumberfTest Substance): Matrix: Method/Revision: Analytical Equipment System Number: 26 Week Capsule Toxicity Study with PFOS in Cynomolgus Monkeys T-6295 (PFOS) Monkey Sera ETS-8-4.0 and ETS-8-5.0 Amelia 062498. Soup 020199 Instrument Software/Version: Filename: R-Squared Value: Slope: Y-Intercept: Date of Extraction/Analyst: MassLynx 3.1 See Attachments See Attachments See Attachments See Attachments 3/16/99 RWW/SAH Date of Analysis/Analyst: Date of Data Reduction/Analyst: 03/17/99,03/21/99 DRB/MEE 03/23/99.03/22/99 DRB/MEE Sample Data WEEK 26 MONKEY SERA Group S am ple# PFOS PFOS Average RSD Dose nCeo/mneL. Reported ut/m L PFOS Std. Dev. ug/rnL Method Blk Method Blk H20 Blk-1 H20 Blk-2 0.00 <MDL 0.00 <MDL <MDL <MDL Matrix Blk Matrix Blk Rabbit Sera Blk-1 Rabbit Sera Blk-2 0.00 0.00 <MDL <MDL <MDL <MDL Matrix Blk Monkey Sera Blk-1 0.00 <MDL M anx Blk Monkey Sera Blk-2 0.00 <MDL <MDL <MDL QC - 250 ppb RBS03169-MS-I 210 85 RBS03169-MSD-l 232 94 89* 10 QC - 250 ppb RBS03169-MS-2 RBS03169-MSD-2 229 193 7982** 85* 17* QC - 250 ppb RBS03169-MS-3 RBS03I69-MSD-3 211 213 85* 86* 86* 1* Group 1 105508M 30.9 0.0619 Control I05517M 31.0 0.0673 0.0 mg/kg/day 105519M I05520M I05526M 27.1 0.0521 16.8 <LOQ 26.7 0.0469 22.9 I05527M 41.7 00835 0.0623 0.0143 I05529F 48.22 0.0765 I05530F 59.68 0.0918 10553IF 30.12 0.0538 I05535F 16.61 <LOQ I05544F 105549F 21.61 <LOQ 21.7 34.69 0.0694 0.0729 0.0158 Group 2 Low-Dose 0.02 mg/kg/day I0S514M 105515M 105516M 151 20.2 143 20.6 131 17.2 8.91 105521M 105537F 112 21.1 19.8 1.76 101 16.8 I0554IF 105547F I05550F 113 18.5 140 85 16.2 14.2 10.8 16.4 1.77 Group 3 105505M 255 116 Mid-Dose 0.5 mg/kg/day 105510M I0S518M I05523M 105524M I05S28M 149 162 142 86.7 176 89.9 160 86.7 30.4 156 77.8 103 31.4 I05532F 209 79.2 105538F 150 73.6 I05539F 216 90.1 I05545F I05548F 105552F 269 107 145 80.6 16.3 142 69.4 83.3 13.5 Group 4 I05506M M M High-Dose I05507M 213 227 2.0 mg/kg/day 105509M 105511M MM 248 177 105512M I05522M 285 298 18S 276 216 2451..50 I05533F 340 253 105534F I05536F 308 233 155 193 105540F I05542F 10555 IF 278 221 206 163 210767 13.0 214 27.7 Limit of Quantitation (LOQ): 25 ng/mL Date Entered/By: 03/23/99 LAC M Moribund Method Detection Limit (MDL): 12 ng/mL Date Verified/By: 0 PFOS Perfluorooctanesulfonate ETS-8-5 0 Excel Version 7.0 sera223.xls 003S94 3/26/99