Document vV7rZyqQBdvD373wmoG1XrEqY

E err1~ESEARCH AR226-1864 OccupatIonal andEnvironmental Health Analysts of perftuorooctenotCAcId (PFOA) In Human Serum Samples \ E~cygenReport No. L0003C)0O \ Testing Laboratory ~ Exggen Research 3058 Research Drive `State College, PA 18801 Requester Dr. Marsha Bailey Occupalkn4alRaocsOl EmraMrCrolnn~,Ieental t'fealth Padcershu~,WV2. 6101. (304)-7~7-0270 Recieved OPPT NCIC 2004 SEPT- 30 PAGE? ~4 E1087140'1 USA T: 8~L281~1302919 I hiIo4~cO-. ~ Results are reported for the ana~sat pefkiorooctanolc add (PFOA) h htznan serum samples received at E.iojgen from Dr. Mar&sa Baley at Occupational and Evlronrnentei Health. The E~enprolect number assigned tothe samples Is P959. ~: ~ A tolal at twelve samples were received at Ex~~gefnt 5 mL screw~capvials labeled with pemoanentrnaslcer. A copy cial sample log-I' kdovmatlcn Is presented ft Attachment A The tesive samples were received ~1 07123it)4. The samples were shipped frozen on cky Ice vi~FedEx. Tne samples were stored frozen from ~e ci eceiptudlanalysis. - 3.1 Sample Preparation Thesamples were extracted ~id analyzed acccrc5ig to thedurient revIsion atmethod ExM-0OB- 211. FIfty niiorolitaes at sample was used for the oxfractlcn pracedLre. tio~gthe Mt~iprobe epperelus, 500 pL ci acet~nlt~iwIeas eddad to the sample end then passed thrcu~a protein -- co~ret 3.2 Sample Analysts by LCIMS and LC/M~M$ In Hl~Presa'.A Uqtid CfvcmalograplW Q1FLC)~an aLk~ioot fextract Is kijec$ed and passed through a a~d.phast.hrcmatogrepl~$cccltsnn. Based on the atl~iIcyi the enaI~,tefor the phees ~ ~e ~ re1~to the ~C~imdob~1ephase. th. aflaMe ~ re*afted ftc a d~actWIS*W~TIO(Id Of *1* 31OM~gHFLC seperatlon, mass spacimmetry provides a rapid and acnaate meerer for analy*'g a wide range at organb conipoirids. Molecijea am Ionized, fragmented, and detected. The bis at and q~teted dracted5tafldafdL rIstf~ci the comporrirle are observed M HPI100s~etamftteilaced ft a FE Sciex APi 4000 s~stern~s usedtoanalyze the sample aodracte. A gracMi* ekxton through a Jones Chromatography Genesis C-8 50x2.1 mmx4mcoWeSUsadfOr$eParatiorL Moble PhaseCA): Mobda Phase (B) 2mMAmrnor'ksn Acetate ft Type S Water Methanol PAGE2eF4 E1D871 402 1kfl2 0.0 40 3.0 40 3.5 0 3.7 0 7.0 0 7.5 40 Flow Rate (rnUnlrt~ 60 50 100 0.3 100 0.5 100 0.5 60 0.5 9.0 40 60 0.5 9.5 40 60 0.3 12.0 40 60 0.3 The fc~Nftgparameters wa'e used foroperation Of the mass specfrometer ~erametv Ionization Mode ~GaLs TMemopner~atuerde Dr~,ingGas(N2) $e~ Electrospray 350"C ~ 7.OLM'ln 415-~.37O(`~C-PFOA) 4.1 C~1lbrat1on A 6.polt~,tce~xatlcncurve was analyzed throughoi.t the anaMical sequence for the Ittiorocompouncle. The calballon poftta were prepared ~t.0.5, 1, ~ 10, 20, Sc) ngknl for PFOA. The hsttrwnt miporsse versus theccncerdralioh was plattedfor each point. Using ~iearregression weti 1/x weighIkig. tie elope, y.lnteccapt and coefllolent ci deteimination 9~ were deteiynteed. A calibration cuve Is acceptable ~rz ~0.985. .For.thexes~.repodedhare..Caft~1OflCrtIedaware-met~ 4.2 Surrogates Starogata s~sws arenctapartol tile anelysIe~ 4.3 Laboratory Control Spikes labocoi*ol spdeie ft tile anaS~4IsaIset wareprepared byadckig a Imovai concentration at the enaMelto codmi htanan aertrn. accuracy. The Isborato~ycontrol spdes mLuabstersathciy~creocnotrvoelrsieps&beestwareeenus8e0d4t2o0a%ss~esslmeveetlhsOadt the 100 end 65-115% for levels greater then the 100 or the data Is re4actad. For the results reported hem, the*S wor*wthft the acceptable ~ 4.4 MatrIx Spikes Two matrix spIkes Ii the analytIcal setwere prepared byadc~ga Io'~ownconcentrationOf the tot~anaI~4atoseparate Iunai sen.rn samples. Maflt)c 5p~5are'~~ assess method accuracyft the mabt~The matrixspIkes shouldShowrecoveries ~ween 85~5%.~ reaubs reported here, the matrix spIkeswere WIthft the acceptable ra~ - E1D871403 4,5 Sample Redated Comments Three samples ft the analytical sat were extracted and analyzed rt di.pticate. iD~licate sample results axe reported alongwiththp sample resuttaft Attachment B. ~$.~ Please see Attachment B for a detailed listing of the analytical results. Results are reported ft paris per billion (rig/mI) forthe analytaeon an as-recet,ed basIs. Samples are deposed of one month after the report is issued Lrdess otherwise specliled. At electronic data Is archived on retrievable media and haid copy reports are stored In data folders ,naiotakied by Ex~jQen.Haropydata Is stored for a mlnbm.mi of flvu years. o~i~j~i~~4 En*cnmental Health wili be notliled 30 days prior to the disposal ci hwdeopyda~ :~ ~ 7.1 AltachmentAtCiki dCussxly 7.2 AztachmentB Analytical Results a gn~Iw~u E10871404 3058 Research Drive State College, PA 16801 Phone: 814.272-1039 Fax: 814.231-1580 Login # ProJect Company Name Submitted By-. Login Type: Started'. Date Stait Due ttate Received Date Received By Spread Sample: 3110 P0000959 DuPont do Nemours & Cc, Inc. Charles R. Powley Immediate Receipt of Samples I 07/23/2004 0W06/2004 07/23/2004 Arnmerrnan, Mark Cpnfoml COC Sample: True Conform CCC: True Conform Sample: True Conform Request True SD/Fl: Decker, Emily ProJect TitJeIrype: Analysis for PFOA In Human Serum Samples by IC/MS/MS / ROUTINE Login Notes: Conform Notes: p~k~ PK0005722 Packaclee / Contalner~ MIS ~ i c~n~mon Sl~..I ID Twro~ControUTemo. 7123134 338:30PM P~cig.& Contanti UncQmprcnhISId FasEX 5455 SOS34885 O~yIc. 0.0 OJrecllon/ ~IndIId av RECEIVED A~m.jm.n,Mwk Coab~erN cooroeze C004082* C0040829 C0040831 C0040534 C0040835 .c004Q88~. C0040841 C0040643 00040544 00040545 C0040541 Gross Weicht 4.009 - 4.40g 470g 4.lOg 4.80g 4.30g .4.60g. 4.6O~ tOOg 4.109 5.309 4.009 QgntillnerTvD. Smls.tumtub 5 ri4 sann~tul* Smllilmit'Jb 5 ml WWI* IUbC 5 ml i.nim tue. .5 sp!~U~D.. 1mm tubs S ml swat tubs 5 nit UflIfl bed 5 mlunm tubs 5ndsm,mtubs Pcewvath,. NONE NONE NONE NONE NONE NONE NONE NONE NONE t'$ONE NONE NONE Mfo. Lot 7/29/04 Logini~I Report Vemien Jul 142004 11:35AM Pa~.1o2f E1D871405 lnstance:~- R0113316 Simob ID t~0030OO-0O0t Contaw C004O8~ Fra~ ~ LIQUID Human SRJUJn 13000-0002 10003000.0003 0004082$ C00.4C825 LIQUID . LIQUID Human Sscum Human Swum . 10003000-0004 C0040831 UQUID HlsT.36 ~wa 10003000.0005 10003000-0006 C0040834 C0040835 LIQUID Human Smnan LIQUID Human Simm . L0003000.000? 10003000.0008 10003000.0005 C0040839 00040841 C0040843 UQUlO Human $8/urn UOUID HumanSimm LiQUID Hwnan Serum ~a L0003000-OOtO 10003000.0011 ~u LIQUID Human Srrum ~. UQUID Human Swim - 10003000.0012 ~48 liQUID Human Sinai Samples Dais Samoled Di1~RiceIved 07/22/2004 07123/2004 05/06~2304 CONFIDENTIAL IOR1s'L~flON 07/22/2004 07/22/2004 07/23/2004 07123/2004 08/06/23Q4 06106/2004 REDACTED 07/22/2004 07123/2004 08/06/2004 07/22/2004 07123/2004 08/0612004 07/2212004 07/23/2004 060612004 07/2212004 07/23/2004 08(0812004 07/22/2004 07/23/2004 08/06/2004 07/22/2004 07/23/2004 08/08/200 07/2212004 07123/2004 08/0812004 07122/2004 07/23/2004 0606/2004 07)22/2004 01123/2004 08(06/2004 7129/04 Login.rpt Repott Version: Jul 14200411:3MM _______ Page2 of 2 E1D871406 Instance:. ROl 13316 CHAIN OF CUSTODY Exygen Research Sample ReceIving 3048 Research 1~814.231.0032 www~exygenreseaich.com OilFy.A XS:li8t.1C4ol.l2eg3e,1P.A115688001 -- C~ollectlof~Sli~te (~name & addc.ss)~ ~ .~ ?~crm r C)1~r r$rr~-urg ~/ ~ C)! ih~iertn~ H~&~DaIe -P~hone: - `75~7~ c j~1d~fo~n~~-I ~i/i/Cite Fax:________________ ~ Email: fAtY~IeLJr~PhtO~Zny~n~F ~ who enters Information on this form must add th&name, signature,inWals,arid date above~Lineout unused prompts. SpecifyAMor PM fortme enbies. lnckidemonth, da~and yearfcirda1e~Contents of package mustbe verified by someone other than the packager; attest to the verification byinitialingand dating the prompt.C~Thorough'y documentthe reason for any time gap beteieen thetime the serum preparation is completed andthe time packaged by addinga footnote to the bottom ofthe page. CONFIDThTL&l~m(FORMATION- REDACT ED . ` . . ~ 1:35:, n I ~i5~ :s~ `-7.~e1 3~~- -~. ~O4 i I, . ~OCs.. `7-~:,Z~-~Y~~I17 ~ 7c~(W .i~:L,5~ 7.~OLI I ~ TI r~ `7~~f~1i~a~r Lfl p S~~l~~-O5~p~ ~ i~t45p 7. ~)4~L1 ~ ~5 *7 ~ ~p ~ ~ ~~~~:1-j 1)Db43.4 -~ 7. 0,d-I ~iO~w - i~ci-i:~~ ~rfl 7.~J../J~'Jjj PtEASE FAX THECOMPLEF~F) ORM ~ G~ p~bitg~mplec Ssmple Re08~g L Cooler ConinteintItas I~p1il~edaftleed II TLT ~7 r#~ --~*r~ ~ThE PIPICC YandinctidetheothvbNOwEhsample ~ment Cooler 10 R4mm~-- lii.i ~ iExy~nSOP V40j C~i*acAt ~vdS~arnp~Hatd4) Page ~03 E10871407  I~itii~1 ~ it ~ $~I~~IN5I~1 i1IIi Ii iO11~t~IH' b~WhE~DV!~h~ . __ ___ ____ ___ - I~'t tf(r i4(u) ~(L~1 ~~`~aD ~is~fl ip~ siaa ~ ~ II"iMufl ~. ~ -- . .~1-- ~ ~ct4)Jwz~~co~ :-~ ~Dr~&1 t+u Q.,J.~uJi~k; --. _____ - I'IV"3llUI'4 a !~tW~~~ r Lu ~AW~~L3fd~U k.~ ~L! a~.oD ~ . - _________ a __1___i___~'ic~Acr,~ - ~()i~)~c~j ~ a l1*t~ . &*(Q~4I~ ~ci~IAL&~l~ ~~ h~ tt~ap o~- ~ 4 ~p~y~5~ _____ it ~_I)Q'CCi~ 5 ~ ~v v n-I ~ 0 -4 0 H Summery of Residue Found (nghnL) for PFOA In Human Sanim Samples CONFIDENTIAL INFORMATION REDACFED . PFOA (ppb) ~1O3 103 65.0 15.7 61.3 90.4 00.4 00.8 40.1 128 81.2 83.1 73.7 10.5 42.8 E1D871409 us& `~T:814.VL1039 ~P814231j58o e~n H Sponsor Summary of Rcov.rt.a(%} for PFOA in Human Serum Samples PFOA Amount Fotlifled CONFIDENTIAL U~4FORMATION 16.2 1040 REDACTED 109* 4590 Summary ot~FOA(nghnL) in Human Serum Control Samples Sponsor ID - Control A \ PFOA (nglmL) 5.41 10 107 1000 103 1000 99 6000 90 AVERAGE: 100 STDDEV: 6.4 % RSD: 8.4 \ E1D871410 USA T: 114.2711039 F-814.231.1560