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Precise Research. Proven Results.
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Analytical Report
3M Environmental Technology and Safety Services Analysis of Perfluorooctanesulfonate in Mallard and Quail Egg Yolk
Exygen Report No. 023-070
Testing Laboratory
Exygen Research 3058 Research Drive State College, PA 16801
Requester
William K. Reagen, Ph.D. 3M Environmental Technology and Safety Services
Building 2-3E-09 PO Box 33331
St. Paul, MN 55133-3331
PAGE 10F 5
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Introductiot inf
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Results are reported for the analysis of total perfluorooctanesulfonate (PFOS) in mallard and quail egg yolk samples. Also reported is the PFOS contained in each of the three fractions of egg yolk: very low density lipoprotein (VLDL), phosvitin, and lipovitellin. This study was conducted in accordance with the analytical phase protocol given in Attachment E.
2 Sum
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The samples were submitted in plastic bags, labeled with magic marker and typed print A copy of all sample log-in information is presented in Attachment A
Twelve mallard egg yolk samples and twelve quail egg yolk samples were received on 06/01/02. The samples were shipped frozen on dry ice via Federal Express (FedEx). The twelve mallard yolk samples were combined and homogenized into one sample. The same was done for the twelve quail yolk samples. The samples were stored frozen from lime of receipt until analysis. Four mallard albumen and shell membrane samples and four quail albumen and shell membrane samples were also received on 06/01/02. These samples were not analyzed as part of this study.
3.1 Sample Preparation
3.1.1 Total PFO S Content
A 1.0 g sample was used for the extraction procedure. Twenty-five milliliters of methanol were added to the sample. The sample was placed on a wrist-action shaker for 15 minutes and then centrifuged at - 2000 rpm for ~ 10 minutes. A five milliliter aliquot of the sample was taken and 0.5 g of carbon was added. The sample was shaken then allowed to sit. Each sample was filtered and analyzed by LG/MS/MS electrospray.
3.1.2 PFOS Content in Yolk Fractions
A 5.0 g sample was used for the fractionation. Ten milliliters of a solution containing 0.67 M M gS04, 1 mM phenylmethanesulfonylfluoride (PMSF), and 2 pM leupeptin were added to the sample. The sample was shaken for - 2 minutes and then the suspension was transferred to a centrifuge tube. The sample was centrifuged at 200,000 x g at 4C for 24 hours. The sample was then separated into 2 segments: the very low density lipoprotein (VLDL) and the high density fraction (HDF).
The VLDL was dissolved in a solution containing 20 mM Tris-HCI, 1150 mM NaCI, 0.2 mM EDTA, 1 mM PMSF, and 5 pM leupeptin. The HDF was resuspended in a solution containing 0.45 M M gS04, 1 mM PMSF, and 2 pM leupeptin. Both VLDL and HDF tractions were centrifuged at 200,000 x g at 4C for 16 hours. The VLDL was then dissolved in a solution containing 20 mM Tris-HCI, 150 mM NaCI, 0.2 mM EDTA, 1 mM PMSF, and 5 pM leupeptin and stored at 4C. The HDF was dissolved in a solution containing 0.45 M MgSO,i, 1 mM PMSF, and 2 pM
PAGE2 OF5
leupeptin and then two volumes of cold water was added dropwise and then stored overnight at 4C.
The HDF supernatant (iipovitellin) was decanted and diluted with cold water and stored overnight at 4C. The HDF precipitate (phosvitin) was dissolved in a solution containing 0.4 M M gS04, 1 mM PMSF, and 2 pM leupeptin and then diluted with cold water and stored overnight at 4C. The Iipovitellin and phosvitin were then recovered by centrifugation at 106,000 x g at 4C for 1 hour and dissolved in a solution containing 1 M NaCI, 5 mM Tris-HCI, 1 mM PMSF, and 2 pM leupeptin.
All of the resulting precipitates (-1 .0 g) from each fraction were used for the extraction procedure. Twenty-five milliliters of methanol were added to the sample. The sample was placed on a wrist-action shaker for 15 minutes and then centrifuged at - 2000 rpm for - 10 minutes. A five milliliter aliquot of the sample was taken and 0.5 g of carbon was added. The sample was shaken then allowed to sit. Each sample was filtered and analyzed by LC/MS/MS electrospray
Sample Analysis by LC/MS/MS
In High Pressure Liquid Chromatography (HPLC), an aliquot of extract is injected and passed through a liquid-phase chromatographic column. Based on the affinity of the analyte for the stationary phase in the column relative to the liquid mobile phase, the analyte is retained for a characteristic amount of time. Following HPLC separation, mass spectrometry provides a rapid and accurate means for analyzing a wide range of organic compounds. Molecules are ionized, fragmented, and detected. The ions characteristic of the compound is observed and quantitated against standards. Each sample was analyzed in duplicate.
An HP1000 system interfaced to a Micromass Quattro Ultima system was used to analyze the sample extracts. A gradient elution through a Jones Chromatography Genesis C-8 50 x 2.1 mm x 4pm column was used for separation.
The following gradient was performed:
Mobile Phase (A): Mobile Phase (B):
2mM Ammonium Acetate in Type I Water Methanol
Tim e 0.0 0.4 1.0 7.0 7.5 9.0 9.5 14.0
%A 60 60 10 10 0 0 60 60
%B 40 40 90 90 100 100 40 40
The following parameters were used for operation of the mass spectrometer:
P aram eter Ionization Mode Polarity Transitions Monitored
Setting Electrospray Negative 499->99
PACE3 OF5
o 00093
Gas Temperature Drying Gas (N2)
350C 7.0 L/min
m '-4 .4
m 4.1 Calibration
A 6-point calibration curve was analyzed at the beginning, throughout, and at the end of the analytical sequence for PFOS. The calibration points were prepared for PFOS at 0.1,0.2, 0.5, m 1.0, 2.0, and 5.0 ng/mL. The instrument response versus the concentration was plotted for each point Using linear regression with 1/x weighting, the slope, y-intercept and coefficient of determination (r2) were determined. A calibration curve is acceptable if r2 > 0.990. 0 For the results reported here,'calibration criteria were met. The calibration curves are included in the raw data in Attachment C.
m 4.2 Surrogates
Surrogate spikes are not a component of the analytical method.
m 4.3 Laboratory Control Spikes
Laboratory control spikes in the analytical set were prepared by adding a known concentration m of the analytes to control egg yolk samples. Laboratory control spikes are used to assess
method accuracy. The laboratory control spikes must show recoveries between 70-130% or the data is rejected. For the results reported here, the spikes were within the acceptable range. m
4.4 Matrix Spikes
Matrix spikes were not included with this study.
m
4.5 Sample Related Comments
Duplicate injections were performed for all sample analyses.
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* Please see Attachment B for a detailed listing of the analytical results. Results are reported in parts per billion (ng/g) for PFOS.
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t Samples are disposed of one month after the report is issued unless otherwise specified. All electronic data is archived on retrievable media and hard copy reports are stored in data folders maintained by Exygen. Hardcopy data is stored for a minimum of five years. 3M
"M Environmental will be notified 30 days prior to the disposal of hardcopy data.
m PAGE 4 OF5 C0 0 9 3 3
7.1 Attachment A: Chain of Custody 7.2 Attachment B: Analytical Results 7.3 Attachment C: Raw Analytical Data 7.4 Attachment D: Study Personnel 7.5 Attachment E: Analytical Phase Protocol
8 Signatures
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5/31/2002
Project: E01-1379
3M ENVIRONMENTAL LABORATORY CONTRACT LABORATORY WORK ORDER BY SAMPLE
Contract Lab{s): EXYGEN
1 of 2
Requester: Robideau, Rochelle R (0002-03E-09)
Department: 502180 Site Source: Project Num ber Date Received: 10/4/2001 Project Description: N . Bobwhite Reproduction (Eggs)
ship Dtte:
Zs fh fo --------
Completion Date: Project Lead: Rochelle R. Robideau Phone Number: 651-778-7065 Email Address: rrrobideau@ininm.coni
Comments: NOTE: M1SC SERV " Protein separation to be conducted by Exygen Research.
3M Sam ple
E01-1379-31882 Analysis Code MISC_SERV
Sampled Date Sam ple Description
6/13/2001
10 nom a.i. 230 H Yolk
Analytical Method
' Components
Mise. Services
Mise. Services
Annlyyii P hiJPwti 6/30/2002
E01-1379-31883 aato ptte MISC_SERV
6/13/2001
10 nom a.i. 232 H Yolk
Analytical Method
CTBaasaS
Mise. Services
Mise. Services
Analysis Due Date 6/30/2002
E01-1379-31884 Analwis Code MISC_SERV
6/13/2001
10 unm a.i. 234 H Yolk
Analytical Method
ompopenh
M ise. Services
Mise. Services
Analvsis Due Date 6/30/2002
E 01-1379-31885 Analysis Code MISC_SERV
6/13/2001
10 nom a.i. 236 H Yolk
Analytical Method
Components
M ise. Services
Mise. Services
Analvsis Due Date 6/30/2002
E01-1379-31895 Analvsis Code M1SC_SERV
E01-1379-31896 Analvsis Code MISC_SERV
6/13/2001
10 ppm a.i. 229 I Yolk
Analytical Method
Components
Mise. Services
Mise. Services
6/13/2001
10 nom a.i. 2 3 1 1 Yolk
Analytical Method
Comoonenls
Mise. Services
Mise. Services
Analyaif-Pue Pte 6/30/2002
y'
Analvsis Due Date 6/30/2002
E01-1379-31897 Analysis Code MISC_SERV
6/13/2001
10 nom a.i. 233 I Yolk
Analytical Method
Conino nen ta
Mise. Services
M ise. Services
Analvsis Due Date 6/30/2002
E 01-1379-31898 Analysis Code MISC_SERV
6/13/2001
10 nom a.i. 2 3 5 1 Yolk
Analytical Method
Components
Mise. Services
Mise. Services
Analvsis Due Date 6/30/2002
E01-1379-31939 Analvsis Code MISC_SERV
6/21/2001
10 nom a.i. 226 J Yolk
Analytical Method
Components
Mise. Services
Mise. Services
A nalvsis D ue D ate
6/30/2002
600939
5/31/2002
3M ENVIRONMENTAL LABORATORY CONTRACT LABORATORY WORK ORDER BY SAMPLE
2 of 2
Project: E01-1379 (cont)
Contract Lab(s): EXYGEN
3M Sam ple
Sampled Date Sam ple Description
s'
EO1 - 1 3 7 9 - 3 1 9 4 0 Analysis Code MISC_SERV
6/21/2001
10 ppm a.i. 226 J Albumen
Analytical Method
Comesfleuti
Mise. Services
Mise. Services
Analysis Due Date 6/30/2002
EOI-1379-31942 Analvsis Code MISC_SERV
6/21/2001
10 ppm a.i. 226 J Shell Membrane
Analytical Method
Components
Mise. Services
Mise. Services
Analysis Due Date 6/30/2002
E01-1379-31943 Analysis Code M1SC_SERV
6/21/2001
10 ppm a.i. 230 J Yolk
Analytical Method
exponents
Mise. Services
Mise. Services
Analysis Due Date 6/30/2002
E 0 1 -1379-31944 MISC_SERV
6/21/2001
10 ppm a.i. 230 J Albumen
Analytical Method
omppqenb
Mise. Services
Mise. Services
Analysis Due Date 6/30/2002
E 0 1 -1379-31946 Analysis Code MISC_SERV
6/21/2001
10 pom a.i. 230 J Shell Membrane
Analytical Method
omponents
Mise. Services
Mise. Services
Analysis Due Date 6/30/2002
EOI-1379-31947 Analysis Code PFOS
6/21/2001
10 oom a.i. 232 J Yolk
Analytical Method
nmpon^ft
PFOS by ESMS
PFOS
Analysis Due Date 6/30/2002
E01-1379-31948 Analysis Code PFOS
6/21/2001
10 ppm a.i. 232 J Albumen
Analytical Method
fiM U M ififc
PFOS by ESMS
PFOS
Analysis Due Date 6/30/2002
E01-1379-31950 Analysis Code PFOS
6/21/2001
10 ppm a.i. 232 J Shell Membrane
Analytical Method
Component
PFOS by ESMS
PFOS
Analysis Due Date 6 / 3 0 / 2 02
EOI-1379-31951 Analysis Code PFOS
6/21/2001
10p om a.i. 234 J Yolk
Analytical Method
pipOTnnt?
PFOS by ESMS
PFOS
Analysis P u ; Daft 6/30/2002
E01-1379-31952 Analysis Code PFOS
6/21/2001
10 ppm a.i. 234 J Albumen
Analytical Method
Components
PFOS by ESMS
PFOS
Analysis Due Date 6/30/2002
EO 1 - 1 3 7 9 - 3 1 9 5 4 Analysis Code PFOS
6/21/2001
10 ppm a.i. 234 J Shell Membrane
Analytical Method
Components
PFOS by ESMS
PFOS
Analysis Due Date 6/30/2002
C0 0 9 4 0
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1. 10 ppm a.i. 230 H Y olk
2 10 ppm a.i. 232 H Yolk
3M UMS#
31638
31639
Date Sampled
5/13/01
5/13/01
Time Sampled
Matrix/ Media Enterthenumberofcontawofeach
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3. 10 ppm a.i. 234 H Y olk
31640 5/13/01
4. 10 ppm a.i. 236 H Y olk
31641 5/13/01
5. 10 ppm a.i. 229 I Y olk
31654 5/13/01
6. 10 ppm a.i. 2 3 1 1 Y olk
31655 5/13/01
7. 10 ppm a.i. 233 I Y olk
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Sample "Condition Upon Receipt" Form
Protocol#
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0 3 3 - 0 70
Date & Tim e Received 6>- / - Jt / / / S '
Condition o f Samples
D r u ic .* - r t
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W a y b ill# .73 Y3 /Q M i __ f r t d .7 ).
Comments:
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Sample Login Report
Study Number: Protocol:
023-070 NA
Page 1 of 1
6V600
V erified By/Date:
Printed 6/5/2002
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000974
Centre M ethod No: OOM-023-015
4.4,2. Example Tune File Parameters
The follow ing values are provided as an exam ple. Actual values may vary from instrum ent to instrum ent. A lso, these values m ay be ehngrd from tim e to tim e in order to optim ize for greatest'sensitivity.
The mass spectrom eter is tuned using a 0.5pg/m L PFOS solution, prepared via
dilution o f the stock solution in m ethanol. The solution is infttsed (using a "T" connector) at 10 pL/m in into a 0 .2 mL/min stream o f m obile phase consisting o f 40% m ethanol and 60% 2 mM ammonium acetate. The analytes are initially tuned for the parent ion and then tuned for the product ion. Once the instrument is tuned, the optim ized parameters are saved as a "tune file ". T his tune file is then used during routine analysis. Th tuning procedure may be repeated as necessary to ensure optim al sensitivity.
C ontrols IS-Iospray OR-O rifice RNG-Focus R ing QO-Quad 0 Rod O ffset IQ 1- Inter quad 1 lens S T rS tu b b ies' R O l-Q uadl Rod O ffset
IQ2-Inter quad 2 lens R 02-Q uad 2 rod offset S T 3 -S tu b b ies R 03-.Q uad 3 rod offset DF-CEM D eflection Plate CEM -Channel Electron M ultiplier
Set -4000.0
-6 1 .0 -270.0
1 0 .0 9.3
* 15.0 9 .3
2 0 .0 84.0 10.0 8 6 .0 3 0 0 .0 2 4 0 0 .0
G as F low s
N ebulizer Gas * Curtain Gas
C ollision Gas T B Temperature
Set -12 13
4 350C
4.4.2. CalibrationProcdures
a. Inject the same volum e (between 10 to 20 pL ) 6 f each calibration standard (prepared in M eOH) into the LC/M S/M S.
b. U se linear, I/x w eighted standard curves for quantification. U near standard curves arc generated for each set by linear regression using the
Centre Analytical Laboratories, Inc. Study # 023-015
Page 13
Research
Page
Ko:Centre M ethod OOM-023-015
appropriate software system . A ny calibration standards failing outside
30% . based on its calculated concentration, must be excluded from the
calibration curve. H ow ever, the total number o f calibration standards that
m ay be excluded must not exceed 30% o f the total number o f standards
injected.
a
c. The correlation coefficient (r) for calibration curves generated must be
0 .9925 (r'fW S i). I f caUbaaion. results fall outside these lim its then
appropriate steps should be taken to adjust instrument operation, and the
relevant set o f sam ples m ust be reanalyzed.
> '(
4.4.4. SampleAnalysis
'
a. Inject the same volum e used for the calibration standards {between io to
25 pL) o f each sam ple, fortification, control, etc. into the LO M S/M S.
b. Standards corresponding to at least six concentrations must be included in an analytical se t
j
I { \
c . Inject an entire set o f standards (six) at the beginning o f the run and inject standards interspersed about every >5-10 sam ples. A ll sam ple injections m ust be bracketed by standard injections (see Section 4.5).
'
d. Each set o f sam ples analyzed (not to exceed 25) must include at least one reagent control (m ethod blank), one A STM Type I water blank, at least one matrix control, and tw o matrix control sam ples fortified at known concentrations and carried through the procedure to verify recovery.
( :
e. A ll sam ples must be analyzed w ith duplicate injections.
!j
Note: The analysis performed -during method development included
f
fortifications at 1 0 ,5 0 and 250 ng/g (ppb) for the analyte.
1|
*. f. T he concentration o f each sam ple, fortification, control, etc. is determined
* t
from the-standard curve based on the peak area o f the analyte in all
standards injected during a .se t The standard responses must bracket
responses o f the residue found in the sam ple s e t If necessary, dilute the
sam ples and re-analyze to give a response within the standard curve range.
!
g. Fortifications that bracket the highest residue expected in each treated sam ple w ill be included w ith each sam ple set. If residues are found outside these lim its, additional fortifications w ill be included in a subsequent sample set to establish that m ethod recoveries are available for the .analyte o f interest at concentrations exceeding those in treated sam ples.
i
Centre Analytical Laboratories, Inc. Study #023-015
Page 14
i
Exygen Research
. Page 22 of 39
000976
m
m
m
*
I
i I I I i
1 Centre M ethod No: OOM-023-015
h. F ortification recoveries w ithin 60 to 130% are acceptable for fortifications at d ie LOQ lev el. R ecoveries betw een 7 0 to 120% are acceptable for
fortification s at lev els grtater than tiie LOQ. Failure to m eet these criteria ' requires an investigation o f cause and a fu ll reanalysis o f the affected sam ples.
l. Sam ples in w hich no peaks are detected at the corresponding analyte retention tim es w ill be reported as N D (not detected). Sam ples in w hich peaks are detected at the corresponding analyte retention tim es but are less , than the low est standard w ill be reported as N Q (not quantifiable).
j . 'B ackground lev els o f analyte found in controVblank sam ples that
correspond to values below the LOQ, but are still quantifiable, wiU be
u sed to correct fortification recoveries.
.
j . I f sam ples are not loaded on the instrument to b e analyzed the day they are extracted, sam ples "must be stored.refiigerated at approxim ately 2C to 6C u n til analysis and analyzed preferably w ithin a w eek.
R ecoveries from m ethod developm ent for all m atrices can be found in T ab les I-V I.
4 .5 . P e r fo r m a n c e C r it er ia
-/
i. !
f
!
f ! j !
j.
The follow in g tw o criteria m ust be m et before the in itial analysis o f sam ples,
esp ecially when using different instrumentation set-u p s than those cited in this
m ethod.
*
r - j.
F ig t C riterion - Inject a standard solution on the LC/M S/M S corresponding to the
estim ated LOQ (1 0 ppb LOQ is-equivalent to a standard solution o f 0 .2 ng/m L) and obtain a signal to noise ratio of at least 9:1 relative 'to the reagent blank. If
this criterion cannot be met,- optim ize and- change .instrum ent operating
param eters.
*
' I
Second Criterion - Inject a set o f standards ranging from at or below the LOQ. up to the highest concentration level. Generate a calibration curve for th e analyte and obtain a linear regression with a C oefficient o f determ ination (i3) o f at least 0.985 for the analyte. Once this criterion has been dem onstrated, sam ple may be analyzed w ith standards interspersed.
I ] r
*
j
*
Centre Analytical L aboratories, Inc. Study # 023-015
Exygen Research
Page 15
Page 23 o f 39
000977
Il
M
m
m
i
m
i
i
C entre M ethod N o: OOM-023-O15
4 .6 . T im e R eq u ir ed fo r A n a l y sis
A set o f 14 sam ples can be taken through the extraction procedure in approximately three hours by one person. The LC/MS/MS analysis (8-10 standards and 14 sam ples) w ill take approximately 6 hours.
5. CALCULATIONS 5.1 Analyte Found:
Calculate the amount o f analyte found (in ng/m L, based on peak area) using the standard curve generated by the MacQuan software program using Equation 1. E quation 1:
Anaiyte found (ng/mL) = foeak area - intercept! slope-
5 2 Component Residue Concentration
Determine the component residue concentration using Equation 2
E quation 2: .
f a t t i e r W g) -
sample w eight (g)
Where DF = dilution factor and FV * final volum e tiQte: ng/g = ppb
5.3 Percent Recovery
Calculate the percent recovery for sam ples fortified with known amounts of analytes prior to extraction, from Equation 3.
Equation 3:
Recovery (%) =
(ng/g found - average ng/g found in control)
ng/g added
xlOO
Centre Analytical Laboratories, Inc. Study # 023-015
Page 16
Exygen Research
Page 24 o f 39
000978
C en tn M ethod No: 00M -023-0151
6. SA FETY
*j
There are no unusual hazards associated with this m ethod. The analyst should read the m aterial safety data sheets for all reagents before performing this m ethod Norm al laboratory precautions should be taken.
I I
*(
Centre Analytical Laboratories. Inc. Study # 023-015
Exygen Research
ri t
Page 17
Page 25 of 39
000979
Centre M ethod No: OOM-023-015
r
I
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TABLES
:
i.
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.
i \f
C entre Analytical Laboratories, Inc. Study # 011-015
Exygen Research
Page 18 Page 26 of 39 C R O SSO
Centre M ethod No: OOM-O23-015
Table I: Summary o f Recoveries for PFOS in Quail Egg Membrane
Sam ple
F o rt Level'
_ (PPb)
0003798 M atrix B lank A
0
0003798 M atrix B lank B
0
0003798 M atrix B lank C 0003798 Spk A 0003798 SpkB 0003798 Spk C 0003798 Spk D 0003798 Spk E 0003798 Spk F 0003798 Spk O 0003798 Spk H 0003798 Spk I
0 10 10 10 50 50 50 250 250 250
AVERAGE:
STANDARD DEVIATION:
RELA TIV E STANDARD DEVIATION:
% Recovery
NA NA NA 88 95 92 92 95 W 93 95 93 93
2 3
* .
1
.1
I
f
i
1
i
Table II: Summary of Recoveries for PFOS in Mallard Egg Membrane
S am ple
F o rt Level
0003802 M atrix B lank A 0003802 M atrix B lank B 0003802 M atrix B lank C '
0003802 Spk A 0003802SpkB 0003802 Spk C
0003802 SpkD
0003802 Spk E 0003802 Spk F 0003802 Spk G 0003802 Spk H
0003802 Sok I
___________Se e ^ _____________________ 0 0 0 10 10 10 50 50 50 250 250 250 AVERAGE;
STANDARD DEVIATION:
RELA TIVE STANDARD DEVIATION:
% Recovery
NA ' NA
NA
106
122 106 96 96 90 93. 92 93 99 10 10
N A = N ot A pplicable
* > f
!
1
Centre Analytical Laboratories, Inc. Study # 023-015
Exygen Research
Page 19
Page 27 of 39
Centre Method No: OOM-023-015
Table.HI: Summary of Recoveries for PFOS in Quail Egg Yolk
Sam ple
0003793 M atrix Blank A 0003795 M atrix Bionic B 0003795 M atrix Blank C
0003795 Spk A 0003795 SpkB 0003795 Spk C 0003795 Spk D 0003795 Spk E 0003795 Spk F 0003795 Spk 0003795 Spk H 0003795 Spk I
*
F o rt Level in*/*)
0 0 0 10 10 10
: 50 , 50
50 , 250
250 250
AVERAGE: ^STANDARD DEVIATION: RELA TIVE STANDARD DEVIATION:
% Recovery
NA NA NA 69.
68,
70 72 80 83 85 89 88 78
9
11
Tabl IV: Summary of Recoveries for PFOS In M allard Egg Yolk
S am ple
0003799 M atrix Blank A 0003799 M atrix Blank B 0003799 M atrix B lank C
0003799 Spk-A 0003799 SpkB 0003799 Spk C 0003799 Spk D 0003799 Spk E
0003799 SpkF
0003799 Spk G 0003799 Spk H 0003799 Spk I
F b rt Level
la i/x ) 0 0 0 10 10 10 50 50 50
250 250 250
AVERAGE: STANDARD DEVIATION: RELATIVE STANDARD DEVIATION:
% Recovery
NA NA . NA 83
82 ` 10Q '8 5 88- .
90
8785 88 88 5 *6 .
N A = N ot A pplicable
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Centre Analytical Laboretories, Inc. Study # 023-015
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C009S
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C entre M ethod No: OOM-023-015
. Table Vi Summary of Recoveries for PFOS in Quail Egg Albumen
1 Sim ple 1
,1 000379 M atrix B lank A 000379 M atrix B lank B 000379 M atrix B lank C
0003796 Spk A Cp03796SpkB 000379 Spk C 0003796 Spk D 0003796 Spk E 0003796 Spk F 0003796 Spk G 0003796 Spk H 0003796 SokI
Fort. Level
(ppb) 0 0 0 10 10 . 10 50 50 50 250 250 250 AVERAGE;
STANDARD DEVIATION: RELATIVE STANDARD DEVIATION:
% R ecovery
NA NA NA 79 93 88 96 95 90 97 102 102 94
7 7
Table VI: Summary of Recoveries for PFOS in M allard Egg Albumen
S am ple
: 0003800 M atrix B lank A 0003800 M atrix B lank B 0003800M atrix B lankC 0003800 Spk A . . 0003800 Spk B 0003800 Spk C 0003800 Spk D 0003800 Spk B OQ3800SpkF 0003800 Spk G 0003800SpkH 0003800 Spk I
F o rt Level
(PPb)' '__________________ 0 0.
o 10 ! 10 10 50 50 50 . 250 250 250
AVERAGE: STANDARD DEVIATION: RELATIVE STANDARD DEVIATION:
% Recovery
NA NA NA 93 85 85 96 100 100 98 102 101
96 7 7
N A = N ot A pplicable
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C entre Analytical Laboratories, Inc. Study # 023-015
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Exygen Research
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Centre Method Nos 0OM-013-015
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FIGURES
Centre Analytical Laboratories. Inc. Study # 023-015
Exygeri Research
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Centre M ethod Nos 00M-Q23-Q15
Figure 1: Representative Chromatogram of a Quail Egg Membrane Control
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Figure 2: Representative Chromatogram of a M allard Egg Membrane Control
e n tre A nalytical L aboratories, Inc. Study # 023-0 IS
Exygen Research
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Centre M ethod No: OOM-023-015
- Figure 3: Representative Chromatogram o f a Quail Egg ,Yolk Control
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' Figure 4: Representative Chromatogram of a Mallard Egg Yolk Control i .
Centre Analytical Laboratories, In c Study # 023-015
Exygen Research
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C entre M ethod No: 00M-023-15 Figure 5: Representative Chromatogram of a Quail Egg Albumen Cohtrol
Figure 6: Representative Chromatogram of a Mallard Egg Albumen Control
Centre Analytical Laboratories, Inc. Study # 023-015
Exygen Research
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Page 33 of 39
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Centre M ethod No: 00M -023-015
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Figur 7: Representative Chromatogram of a Quail Egg,Membrane Control
Fortified at 10 ng/g (p p b ),
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Figure 8: Representative Chromatogram o f a Mallard Egg Membrane C ontrol' Fortified at 10.0 ng/g (ppb)
Centre Analytical Laboratories, Inc. Study # 023-015
Exygen Research
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III C entre M ethod No: 00M -023-015 ! Figure 9: Representative Chromatogram o f a Quail Egg Yolk Control Fortified at 10.0 ng/g (ppb)
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Figure 10: Representative Chromatogram of a M allard Egg Yolk Control Fortified at 10.0 ng/g (ppb)
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Centre Analytical Laboratories, Inc. Study # 023-015
Exygen Research
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