Document EvB48q7k4ByKmDwz5jam07mNx
AR226-1864
it
RESEARCH *, Proven Results.
\ \ *\.\
\
Analytical Report
Occupational and Environmental Health
Analysis of Perfiuorooetanole Acid (PFOA) in Human Serum Samples
\ Exygen Report No, LQ00300Q
_______ ________
\ Testing Laboratory
\ Exygen Research \ 3058 Research Drive State College, PA 16801
\% ______
_______ ____,______________
\ Requester
Dr.Marsha Bailey Occupational arid Environmental Health
4 RoeemarCircle Parkersbu^ WV 28101
(304J-757-027
\
Recieved OPPT NCIC 2004 SEPT- 30
PAGE1OF4
EID871401
x t s g m f f1i6801, USA
T: 8002813219 F: 814372.1019
i in tro d u ctio n
R asuls are reported for the analysis of pefkiorooctanofc add (PFQA) In human serum samples received at Exygen tram Dr. Marsha Bafey at Occupational and Evironmentai Health. The Exygen preset numberassignedto the samplesis PS59.
A total of twelve samples were received at Exygen in 5 mL screvwcap vials labeled wtti permanentmarker. A copyofa l sample tog-lninformation Is presented in AttachmentA
The twelve samples were received on 07/23/04. The samples were shipped frozen on dry Ice via FedEx. The samples were stored frozen from timeat receiptunt analysis.
3 3.1 Sample Preparation
The samples were extracted Old analysed according to thedarent revision ofmethod ExM-008< 211. Fitly mfcrofitere of sample was used for the extraction procedure. Using the Multiprobe apparatus, 00 pL of acetoniltia was added to the sample arid then passed through a protein
precipitation column.
3.2 Sample Analysis by LCIMS and LC/MS/MS
In High Pressure UqUd Chromatography (HPLC), an aliquotof extract is injected and passed through a IqukFptase chromatographic column. Based on the affiniy of the analyte for the stationary phase in the cokim relative to the Iquid mobile phase, toe analyte is retained tor a charactertste amount of Urna. Fotowtog HPLC separation, mass spectrometry provides a rapid and accurate means lor analyzing a wide range of ornante compounds. Molecules are Ionized, fragmented, and detectad. The ions characteristic of the compounds are observed andquantitated againstextractedstandards.
An HP1100 system Interlaced to a P E SctatAPf 4000system was usedto analyze the sample extracts. A grades* eMion through a Jones Chromatography Genesis C-8
SOx 2.1 mmx 4pm coiurm was used forseparation.
The Wowing gradar*was performed:
Moble Phase (AJ: Moble Phase (B ):
2rnMAmmonfurn Acetate in Type I Water Methanol
PAGC20F4
EID871402
Time
%A
%a
Flow Bate ftnU nhl
0.0 40 60 -------- 05-- ----
ao 40 60
0.3
a s 0 100
0.3
a 7 0 100
05
7.0 0 100
05
75 40 60
05
9.0 40 60
05
9 5 40 60
05
ia o 40
60
05
The following parameterswere used foroperationofthe mass spectrometer
Param eter
Ionization Mode Poiarfty Transitions Monitored G as Temperature Drvirto Gas (N2)
Setttna
Bactrospray
Negative 413->369 (PFO A),415-5370 (" C-PFOA) 350C 7.0U nin
4.1 Calibration
A 6-pofnt calibration curve was analyzed throughout the analytical sequence for tha Ouorocompounds. The calibration points wen prepared a t0 5 , 1, 5, 10, 20, SO ng/htL for PPOA. The hslrutnentrwiponaa versus theconcentration was plottedfar each point Usirra near regression with ite weighting, * s!ope, y+ttercept and coefficient of determination (r ) were determined. A calibrationcurve is acoeptobfeif ^ > 0585.
Forthereeub repottediurerCsJbstiancrterbw eram et
4.2 Surrogates Surrogate spftes were notapartoffob analysis.
4.3 Laboratory Control Spikes Laboratorycontrolsp fas in Ihe analyticalsetwere prepared by acting a known concentration of tlteanteyta to controlhumanserum. Laboratorycontrol spOcesam used to assess method accuracy. The laboratorycontrolspflces mustshow recoveries between 80-120% for lew is at the LOQ and 85-115% (or levels greaterthan the tjOQ or tha data is rejected. Fbr the results reportedhere,the sptoeswerewShtothe acceptable range.
4.4 Matrix Spikes Two matrix spaces in theanalyticalsetware prepared byacting a knownconcentrationc<the targetanalyteto separate humanserun samples. Matrixspices are used to assess method accuracy In thematrix; The matrixsp&as shouldstow recoveries between 85-115%. Forthe resufis reported here,thematrixspateswere within the acceptable range. "
W M iOrA
EID871403
4.5 Sample Related Comments Three samples h the analytical set were extracted and analyzed in dupfcate. OupGcats sample results are repotted alongwiththe sample results in Attachment B .
5 D a t& S q n vm {g ptoese see Attachment B tor a dataBed Isting ofthe analytical resutts. Resists are reported in parts per bflSon (ng/rnL) forthe analytes on an as-received basis.
Samples are deposed of one month after the report is issued unless otherwise specified. A l electronic data Is archived on retrievable media and hard copy reports are stored in data folders maintained by Bogan. Hardcopy data is stored ter a minimum of five yearn. Occupational and Environmental Health wit be notified 30 days prior to the dbposal of hardcopydate.
7.1 AttachmentA ChatoofCustody 72. Attachmenta Analytical Beaute
ft Stg a n h if^ s
PJtGt40f'4
EID871404
3058 Research Drive
State College, PA 16801
research
Phone: 814-272-1039 Fax: 814-231-1580
Lodin
Login Groupi LOOQ3GGO
Login#: Project
3110 P0000959
Company Name: DuPont da Nemours & Co, Ina Submitted By. Chartes R . Pawley
Conform COC Sam ple: True
Conform CO C:
True
Conform Sam ple:
True
Conform Request
True
Login Type:
Immediate Receipt of Samples
Started: Date Start Due Date:
Received Date: Received By:
T 07/23/2004 08/06/2004
07/23/2004 Ammerman, Mark
Spread Sample:
f=xygen SD/PI: Decker, Em ily Project Titte/Type: Analysis for PFOA in Human Serum Samples by LC/MS/MS / ROUTINE
Login Notes:
Conform Notes:
E a s la a t PK0003722
C inon
Packages / Containers
M itt.BM t/C fllW Iftm
SM bn art ID
7/23/04 3:38:30PM Package a c o n ta r e s Uncompromisad
n ao 8488 8093 4889
Tamp, ControUTomo.
Dry lea 0.0
Olfaction /HandladBu
RECEIVED A m rw m ai. Mark
C o n ta in e r#
C0Q40828 C0040828 C0040829 C0G40831 C0040834 C0040B38
.C0PKM2. C0040841 C0040S43 C0OUS44 C004C84S C004Q848
Staw vytfflbl 4.00 g 4.40 g 4.70g 4.80 g 4.80 g 4.10 s
4 4 0 .0 4.80g 5.00 g
440 g 5.10 g 4 .0 0 9
'
s il
S sflta tn o f.T B M 5 mi ann tuba Sm l sanan tube 5 mi sanan tuba 5 mi san an tuba 5 mi sanan tuba 5 mi sanan tuba SflfM nsntu ba S mi sanan tuba Sm l sanan tuba 5 m tsan an tuba
S m i sanan tuba S m l sanan tuba
E aM oatiy NONE NONE NONE NONE NONE NONE NONE NONE NONE NONE NOtC NONE
Mfa ID
7/29/04 Logirupt
Report Version: Jul 14200411:35AM . Pag* 1of2
EID871405
Instance:'-
R0113316
IfflU iB SS ilS SI
S vm .lP
10003000*001
feataintr.
C0Q40826
Matrix UQUID
Samles
Fraetion Sm ele Human Setum '
P aie-Sam Blrt Date ecaivea DateOuq 07/22/2004 07123/2004 08/06/2004
LXJ03OO-OOO2
C040B26
UQUID Human Saturo
C O N FID EN TIA L
07/22/2004 07/23/2004
06/06/2004
L0003000-0003
C004O829
UQUID Human Sarum .
IN FO R M A TIO N 07/22/2004 07/23/2004 08/06/2004
L C 003000*004
C0040031
UQUID Human Sanan
R ED A C TED
07/22/2004 07/23/2004 08*6/2004
L0003000*005
C0040834
uomo Human Serum
07/22/2004 07/23/2004 06/06/2004
L0003000-0006
00040036
uomo Human Serum .
07/22/2004 07/23/2004 06/06/2004
L0003QOO-0007
C0040839
uomo Human Sanan
07/22/2004 07/23/2004 08/06/2004
L0003000-0008
C0040841
uomo Human Sanan
07/22/2004 07/23/2004 08/06/2004
10003000-0009
C0040343
uomo Human Sanan
07/22/2004 07/23/2004 0006/2004
10003000-0010
C0040644
uomo Human Serum
07/22/2004 07/23/2004 06/06/2004
100030004011
C004064S
UQUID Human Sanan
07/22/2004 07/23/2004 08/06/2004
L0003000-0012
C004084
UQUID Human Sanan
07/22/2004 07/23/2004 06/06/2004
7 /2 9 /0 4 Login,rpt
Report Version: JU 14 20041 t:3SAM
p3e2of2
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Instance: '.
R0113316
iSIflfiBBBBEB
en
RESEARCH
CHAIN OF CUSTODY
Exygen Research Sample Receiving * 3048 Research Drive State College, PA 16801
814.231.8032 www.exygenresearch.com
F A X : 8 1 4 .2 3 1 .1 5 8 0
CO LLECTIO N SITE INFORMATION Collection Site (name & address):
S:`p VJ TPhYrf^tchna nI br ariii)rcgu ,,> r f t T S b u r c ] 1.U ) '/ ^ L A C lL .
STAFF INVOLVED IN SAM PLE SHIPMENT L in tfr
aT X l J x a 2 . T p r r i tA I t o m i n
r f t f f T-SQ /V i
mhiilVDate
Phone: Fax:
' - Q C O n _____ - O l r f t ____________
(Mntwl Mame)
iU jm u L L i c r n -Q Q t
InitJi/Ot
Em ail: (Y \ h A i t t t j r v h v g n y O J l f t f r
gndura'
InlUth/CaHT
IMPORTCATANNTZE Each person who enters inform ation on this form mustadd theirnam e,sign;ature, in itia ls,and date
above Line out unused prompts. SpecifyAM or PM fortimeentries. Includemonth,day{anayei arfordales. Contents of
packages mustlbiee verified by someone other than the packager; attest to the verification by initialing and dating the
documentthe reason for any time gap between the tim e the serum preparation is completed
by adding a footnote to the bottom of the page,
,
Sample Identification
r
CONFIDENTIAL INFORMATION-
l
Serem SampIs Prep. Completed . ' Date &T<me
p .ffia n r- 3P CH H S & p n
REDACTED
T Z & M >r . Q Q f t r > n ^
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"V JO C H i;3 g p m
PLEASEFAX THE COM PLET FORM to&ygenSimpleRccewng Cooler Contents Verified ;
priertoh^ppi-igamples
InitialA Date*
KEffTW EPINKCOPyandhdudelhe ftertwowBhampleshipment Cooler 1D/P:
'Relinquished b y
T L X 7 fc |a v
Note:WhensvnpfesuriteatBvhKrf-aafc!eypnxsdusWkxv>qoew SPVWlToctractResaich SampleHandfcgT Page I oRf&1.1U
EID871407
E1D8714Q8
Summary of Residue Found {ngAnL)fo r PFOA in Human Serum Samples
\ Sponsor
_\____________ 0 \
CONFIDENTIAL INFORMATION
REDACTED
PFOA
-JPpfa)
103 103 68.0
15.7 81.3 904 804 50 401 128 61.2 83.1 73.7 70S 42.8
\
\
\ \
EID871409
exygeftxom
EW gen
w L. Precise Research. ' Proven Results.
Ill
Summary of Racovtrlu (%} for PFOA In Human Swum Samples
\ Sponsor \ ID
CONFIDENTIAL INFORMATION REDACTED
\,
PFOA
____________ fa * ) S.10 1&2 1040 1090 <590
Summary of PFOA (nfl/mL)
in Human Sorura Control Sample*
\
Sponsor
\
PFOA
________ ID__________ \_______ (ngftnL)
_______ . Control A
\ __________ SA 7
\\
Amount Fortified
(ppb> 5.0 10 1000 1000 8000 AVERAGE:
STD DEV: %RSD:
Racovsry
-.........<*>.......... 102 107 103 89 90 " 100 BA 6A
'\ \i\
\
E1D871410
PDMrive6801, USA
,TF:t-8.x81y1Ag42.a27i32a1.1m.1053890
