Document bBmmyK9RrLr0dGVXoRLZDjMyO

STUDY TITLE Extraction o f Potassium Perfluorooctanesulfonate from Quail Serum and Quail Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry DATA REQUIREM ENTS Analytical Method Requirements STUDY DIRECTOR Sean Gallagher STUDY COM PLETED ON September 06, 2001 PERFORM ING LABORATORY / TESTING FACILITY Centre Analytical Laboratories, Inc. (Centre) 3048 Research Drive State College, PA 16801 Phone: 814-231-8032 STUDY SPONSOR 3M Environmental Technology and Safety Services Building 2-3E-09 PO Box 33331 St. Paul, M N 55133-3331 P R O JE C T Centre Protocol Number: 00P-023-041 Centre Study Number: 023-041 Total Pages: 102 C99141 Centi Study No.: 023*041 ROOD LABORATORY PRACTICE COMPLIANCE STATEMENT Centre Study Number 023*041, entitled "Extraction of Potassium Perfluoroocmesulionate from Quail Serum and Quail Liver for Analysis Using HFLCEleetrospray/Mass Spectrometry," conducted for 3M Environmental Technology and Safety Services, was performed in compliance with US EPA TSCA Good Laboratory Practice Standards (40 CFR Part 792) by Centre Analytical Laboratories, btc. ''f f - T k e L * / ____________________ Tmily Hj Decker Principal Investigator Centre Analytical Laboratories, Inc. _ S ju ai Date Study Director Wildlife international. Ltd. Date 3M Environmental Technology and Safety Services Centre Analytical Laboratories, Inc. Page 2 of 102 Centre Study No.: 023-041 QUALITY ASSURANCE STATEMENT Centre Analytical Laboratories' Quality Assurance Unit reviewed Centre Study Number 023-041, entitled, "Extraction of Potassium Perfluorooctanesulfonate from Quail Serum and Quail Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry". All phases 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 to the Study Director and to management. Phase 1. Protocol Review 2. Extraction 3. Raw Data & Summary Table Review 4. Raw Data and Draft Report Review 5. Final Report Review Date Inspected Date Reported to Date Reported to Centre Study Director and Manaeement Sponsor Management 12/19/00 12/21/00 12/28/00 12/19/00 12/21/00 12/28/00 2/28,3/1/01 3/19/01 3/23/01 3/23-26/01 4/9/01 5/7/01 9/6/01 9/6/01 9/6/01 Naomi Lovallo Sr. Quality Assurance Auditor ____V<k/ /. Date Centre Analytical Laboratories, Inc. Page 3 of 102 Centre Study No-: 023-041 CERTIFICATION OP AUTHENTICITY This report, for Centre Study Number 023-041, is a true and complete representation of the raw data for the study. Submitted by: Centre Analytical Laboratories, Inc. 3048 Research Drive State College, PA 16801 (814)231-8032 Principal Investigator, Centre: f =j L'Jkik _ _ *.. . Centre Analytical Laboratories, Inc. Centre Analytical Laboratories, Inc, Study Director, Wildlife International: Sean Gallagher Wildlife International, Ltd. 1 Sponsor Representative, 3M: Centre Analytical Laboratories, Inc. Date Page 4 of 102 CCOl-'A Centre Study No.: 023-041 STUDY IDENTIFICATION Extraction of Potassium Perfluorooctanesulfonate from Quail Serum and Quail Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry CENTRE PROTOCOL NUMBER: 00P-023-041 CENTRE STUDY NUMBER: 023-041 TYPE OF STUDY: Analytical SAMPLE MATRIX: Quail Serum and Quail Liver TEST SUBSTANCE: Perfluorooctanesulfonate (PFOS) SPONSOR: 3M Environmental Technology and Safety Services Building 2-3E-09 PO B ox 33331 St. Paul, MN 55133-3331 STUDY DIRECTOR: Sean Gallagher Wildlife International, Ltd. 8598 Commerce Drive Easton, MD 21601 SPONSOR REPRESENTATIVE: Rochelle Robideau 3M Environm ental Technology and Safety Services Building 2-3E-09 PO B ox 33331 St. Paul, MN 55133-3331 TESTING FACILITY: Centre Analytical Laboratories, Inc. 3048 Research Drive State College, PA 16801 ANALYTICAL PHASE TIMETABLE: Study Initiation Date: Experimental Start Date: Experimental Termination Date: Study Completion Date: 12/08/00 12/18/00 03/08/01 09/06/01 Centre Analytical Laboratories, Inc. Page 5 of 102 C C O I -1.5 Centre Study No.: 023-041 PROJECT PERSONNEL The Study Director for this project was Sean Gallagher at W ildlife International, Ltd. The following personnel from Centre Analytical Laboratories, Inc., were associated with various phases of the study: Name Emily Stauffer Dave Bell Melissa Kennedy Whitsel John Flaherty Tiffany Proctor Angela Morgan Michelle Arjmand Lawrence Ord Rickey Keller Shawn Robb Karen Risha Title Scientist Scientist Supervisor Operations Manager Technician Technician Technician Sample Custodian Sample Custodian Sam ple C ustodian Scientist Centre Analytical Laboratories, Inc. Page 6 of 102 C C O l'i.S Centre Study No.: 023-041 TABLE OF CONTENTS Page TITLE P A G E ....................................................................................................................................... 1 GOOD LA BORATO RY PRACTICE COM PLIANCE STA TEM EN T..................................2 QUALITY A SSU R A N CE ST A T E M E N T ....................................................................................3 CERTIFICATION OF A U TH E N TIC ITY .....................................................................................4 STUDY IDEN TIFICATION.............................................................................................................5 PRO JECT PER SO N N EL.................................................................................................................. 6 TABLE OF C O N TE N TS.................................................................................................................. 7 LIST OF T A B L E S ..............................................................................................................................8 LIST OF FIG U RES...........................................................................................................................10 LIST OF A PPE N D IC E S..................................................................................................................11 1.0 SU M M A R Y ............................................................................................................................... 12 2.0 O B JE C T IV E .............................................................................................................................. 12 3.0 INTRODU CTIO N..................................................................................................................... 12 4.0 TEST SY S T E M .........................................................................................................................13 5.0 REFERENCE M A T E R IA L ....................................................................................................13 6.0 D ESCRIPTIO N O F ANALYTICAL M E T H O D ................................................................14 6.1 Extraction P ro ced u re.............................................................................................................14 6.2 Preparation o f Standards and Fortification Solutions..................................................... 14 6.3 C hrom atography..................................................................................................................... 15 6.4 Instrum ent Sensitivity............................................................................................................ 15 6.5 D escription o f Instrum ent and Operating C onditions..................................................... 15 6.6 Q uantitation and Exam ple Calculation.............................................................................. 16 7.0 EX PERIM ENTAL D E S IG N ..................................................................................................18 8.0 R E S U L T S ...................................................................................................................................18 9.0 CO N C LU SIO N S....................................................................................................................18 10.0 RETENTIO N O F D A TA AND S A M P L E S ..................................................................... 19 Centre Analytical Laboratories, Inc. Page 7 of 102 Centre Study No.: 023-041 LIST OF TABLES Table I. Page Sum m aiy o f PFOS in Reagent B lanks....................................................................21 Table II. Sum mary o f PFOS in Q uail Liver B la n k s.............................................................22 Table III. Summary o f PFOS in Quail Serum B la n k s.......................................................... 22 Table IV. Summary o f PFOS Recoveries in Quail Liver......................................................23 Table V. Sum mary o f PFOS Recoveries in Quail Serum ................................................... 24 Table VI. Summary o f PFOS in Adult Liver Samples at 0 ppm a.i. (Test Termination 19 W eek s).............................................................................................25 Table VII. Summary o f PFOS in Adult Liver Samples at 1.8 ppm a.i. (Test Termination 6 W e ek s)............................................................................................... 26 Table VIII. Summary o f PFOS in Adult Liver Samples at 6.2 ppm a.i. (Test Term ination 6 W eek s)............................................................................................... 27 Table IX. Summary o f PFOS in A dult Liver Samples at 17.6 ppm a.i. (Test Term ination 19 W e e k s).............................................................................................28 Table X. Summary o f PFOS in Juvenile Liver Samples at 0 ppm a.i. (Test Term ination 12 W e ek s).............................................................................................29 Table XI. Sum mary o f PFOS in Juvenile Liver Samples at 1.8 ppm a.i. (Test Term ination 12 W eek s)............................................................................................. 30 Table XII. Summary o f PFOS in Juvenile Liver Samples at 6.2 ppm a.i. (Test Term ination 12 W eek s).............................................................................................31 Table XIII. Summary o f PFOS in Juvenile Liver Samples at 17.6 ppm a.i. (Test Term ination 12 W e e k s).............................................................................................32 Table XTV. Sum mary o f PFOS in A dult Serum Sam ples at 0 ppm a.i. (Test Term ination 19 W e ek s).............................................................................................33 Table XV. Summary o f PFOS in Adult Serum Sam ples at 1.8 ppm a.i. (Test Term ination 6 W eek s)............................................................................................... 34 Table XVI. Summary o f PFOS in Adult Serum Samples at 6.2 ppm a.i. (Test Term ination 6 W eek s)............................................................................................... 35 Table XVII. Summary o f PFOS in Adult Serum Samples at 17.6 ppm a.i. (Test Term ination 19 W e ek s).............................................................................................36 Table XVIII. Summary o f PFOS in Juvenile Serum Samples at 0 ppm a.i. (Test Term ination 12 W e ek s).............................................................................................37 Table XEX. Summary o f PFOS in Juvenile Serum Sam ples at 1.8 ppm a.i. (Test Term ination 12 W eek s).............................................................................................38 Table XX. Summaiy o f PFOS in Juvenile Serum Samples at 6.2 ppm a.i. (Test Term ination 12 W eek s)............................................................................................. 39 Centre Analytical Laboratories, Inc. Page 8 o f 102 c n o i* s Centre Study No.: 023-041 LIST OF TABLES (continued) Page Table XXI. Summary o f PFOS in Juvenile Serum Samples at 17.6 ppm a.i. (Test Termination 12 W e ek s)........................................................................................... 40 Table XXII. Summary o f Percent M oistures for Quail Liver Sam ples............................... 41 Centre Analytical Laboratories, Inc. Page 9 o f 102 Centre Study No.: 023-041 Figure 1. LIST OF FIGURES Page Typical Calibration Curve for P F O S ..................................................................... 43 Figure 2. Chrom atogram Representing a 0.1 ng/m L standard for P F O S ........................ 44 Figure 3. Chrom atogram Representing a 1.0 ng/m L standard for P F O S ........................ 45 Figure 4. Chromatogram Representing a Reagent Blank for PFOS (Centre ID Reagent B lank A, Set: 122000A ) .......................................................................... 46 Figure 5. Chromatogram Representing Control Quail Serum for PFOS (Centre ID: 0011424 Blank A, Set: 122000A )..........................................................................47 Figure 6. Chromatogram Representing Control Quail Liver for PFOS, (Centre ID: 0007870 Blank A, Set: 121900A ).......................................................................... 48 Figure 7. Chromatogram Representing Control Quail Serum Fortified with 500 ng/mL o f PFOS (Centre ID: 0011424 Spk A, Set: 122000A ).......................... 49 Figure 8. Chromatogram Representing Control Quail Liver Fortified at 10 ppb w ith PFOS (Centre ID: 0011423 Spk A, Set: 121800A)................................... 50 Figure 9. Chromatogram Representing Juvenile Quail Serum Sample (Centre ID: 0007965, Sponsor ID: 9544, Set: 122000A).........................................................51 Figure 10. Chrom atogram Representing Juvenile Quail Liver Sample (Centre ID: 0007926, Sponsor ID: 9544, Set: 121800B)......................................................... 52 Centre Analytical Laboratories, Inc. Page 10 o f 102 Centre Study No.: 023-041 LIST OF APPENDICES Page A ppendix A Study Protocol 00P-023-041 (Centre Study No. 023-041) and Amendments and D eviations............................................................................ 53 Centre Analytical Laboratories, Inc. Page 11 of 102 C H O IS I Centre Study No.: 023-041 1.0 SUMMARY Centre Analytical Laboratories, Inc. (Centre) extracted quail liver samples and quail serum samples for the determination o f perfluorooctanesulfonate (PFOS) according to protocol 00P-023-041 (Appendix A). The lim it o f 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-quantifiable levels (a peak was detected at the corresponding analyte retention time but was less than the lowest concentration o f the calibration standards (0.0001 pg/mL)) to 8.37 pg/g. These results are reported on a wet weight basis. Residues o f PFOS in die quail serum samples ranged from 0.00212 pg/mL levels to 263 pg/mL. The average percent recovery standard deviation for PFOS in serum samples was 108% 10%. The average percent recovery standard deviation for PFOS in liver samples was 95% 11%. 2.0 OBJECTIVE The objective o f this study was to determine levels o f perfluorooctanesulfonate (PFOS) in specimens o f quail liver and quail serum using the analytical methods described in protocol 00P-023-041. 3.0 INTRODUCTION This report details the results o f the analysis for the determination o f PFOS in quail serum and quail liver, using the analytical methods entitled, "Extraction o f Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds From Serum for Analysis Using HPLC-Electrospray/Mass Spectrometry" and "Extraction o f Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds From Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry" with the m odifications 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 12 o f 102 Cn 9 1 S 2 Centre Study No.: 023-041 4.0 TEST SYSTEM The control quail serum and liver used for the matrix blanks and matrix fortifications was received on November 28,2000 from Wildlife International Ltd., Easton, MD. The control quail liver was assigned the Centre ID o f 0011423 and the control quail serum was assigned the Centre ID o f 0011424. 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 personnel on August 16, 2000 and stored frozen. A n additional twenty quail serum samples and twenty quail liver samples were received on February 23, 2001 and stored frozen until they were logged in by Centre personnel on February 26,2001. Sample login and chain o f custody information can be found in the raw data package associated with this study. Storage records will be kept at Centre Analytical Laboratories, Inc. and a true copy o f the storage records can be found in the raw data package associated with this study. 5.0 REFERENCE MATERIAL The analytical standard PFOS was received at Centre on June 3, 2000 from 3M Environmental Technology and Services. 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 o f analysis and was used prior to expiration. The solubility o f the reference material was not relevant to this study. Compound PFOS Centre Control No. TCR No. Purity (%) Expiration Date 00-023-042 TCR 00017-46 97.9 08/31/01 The molecular structure o f PFOS is given below. PFOS Chemical Name Molecular weight = = Perfluorooctanesulfonate 499 (CgFnSOa-) O HC8F17I -- O* N ote: The neutral molecule and standard form from which PFOS (anion) is derived, is potassium perfluorooctanesulfonate [CgFnSOsK], molecular weight 538. Centre Analytical Laboratories, Inc. Page 13 o f 102 CO9153 Centre Study No.: 023-041 6.0 DESCRIPTION OF ANALYTICAL METHOD Analytical methods entitled "Extraction o f Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds From Serum for Analysis Using HPLC-Electrospray/Mass Spectrometry" and "Extraction o f Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds From Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry" with the modifications listed below were used for this study. 6.1 Extraction Procedure A 100 pL aliquot o f the serum and ~ 0.50 g sample o f liver was used for the extraction procedure. A fter fortification o f appropriate sam ples, the sam ples w ere vortexed for - 15 seconds. One mL o f 0.5 M TBA was added to the liver samples and 0.5 mL was added to the serum samples. Two mL o f 0.25 M sodium carbonate/sodium bicarbonate was added to the liver samples and 1 mL was added to the serum samples. Five mL o f MTBE was added to both the serum and liver samples. Each sample was placed on wrist-action shaker for ~ 20 min. and then centrifuged for - 15 min. Four m L o f the organic layer was taken and dried on an N-Evap and then reconstituted with 1 m L o f methanol. Each sample was analyzed by LC/MS/MS electrospray. 6.2 Preparation of 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 at a concentration o f 100 pg/mL by dissolving 10 m g o f the standard (corrected for purity and salt content) in methanol. From this solution, a 1.0 pg/mL fortification standard solution was prepared by taking 1 mL o f the stock and bringing the volume up to 100 mL with methanol. The 0.1 pg/mL fortification standard was prepared by taking 10 mL o f the 1.0 pg/mL fortification standard and bringing the volum e up to 100 m L w ith m ethanol. A 0.01 pg/m L standard was prepared by taking 10 m L o f the 0.1 pg/m L standard and bringing to 100 mL with methanol. A set o f standards containing PFO S was prepared by dilution o f the 0.1 pg/m L and 0.01 pg/mL solutions in the following manner. Initial Cone. (pg/mL)1 0.1 0.1 0.1 0.01 0.01 0.01 1of PFOS Centre Analytical Laboratories, Inc. Volume (mL) 5 2 1 5 2 1 Diluted to (mL) 100 100 100 100 100 100 Final Cone. (pg/mL) 0.005 0.002 0.001 0.0005 0.0002 0.0001 Page 14 of 102 CC0154 Centre Study No.: 023-041 The stock standard solution and all fortification and calibration standard solutions were stored in a refrigerator (4 2C) when not in use. Documentation o f standard preparation can be found in the raw data associated with this report. 6.3 Chromatography Quantification o f PFOS was accomplished by LC/MS/MS analysis using electrospray LC/MS/MS. The retention time o f PFOS was ~ 4.4 min. Peaks were detected in the control matrices corresponding to the analyte retention time and some o f the amounts detected were significant enough to alter the results reported in this study. 6.4 Instrument Sensitivity The smallest standard amount injected during the chromatographic run was equivalent to 0.0001 pg/mL o f PFOS. 6.5 Description of Instrument and Operating Conditions Mass Spec: PE SCIEX API 3000 Biomolecular M ass Analyzer Interface: SCIEX Turboion Spray Liquid Introduction Interface Harvard infusion pump Computer: Dell UltraScan P I 110 Software: HPLC: PE SciexAnalyst 1.1 Windows NT Hewlett Packard (HP) Series 1100 HP Quat Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column:Genesis Cg (Jones Chrom atography), 2.1 m m x 50 m m, 4p Column Temp.: 35 C Injection Voi.: 10 pL Mobile Phase (A): 2 mM Ammonium Acetate in ASTM type I water Mobile Phase (B): Methanol Flow Rate: 0.3 mL/min. Centre Analytical Laboratories, Inc. Page 15 of 102 c r: m Or*vi>r Centre Study No.: 023-041 Time % A % B 0 60 40 1.0 0 100 7.0 0 100 7.5 60 40 11.0 60 40 Ions monitored: Analvte PFOS Mode Transition Monitored negative 499 99 Approximate Retention Time (mini 4.40 Tune File Parameters Controls IS-Iospray DP-Declustering Potential FP-Focusing Potential EP-Entrance Potential CE-Collision Energy CXP-Collision Cell Exit Potential DF-Deflector CEM-Channel Electron Multiplier Set -4200.0 -51.0 -230.0 10.0 -70 -5 300.0 2800.0 Gas Flow? Nebulizer Gas Curtain Gas Collision Gas TIS Temperature 6.6 Quantitation and Example Calculation Set 12 13 4 350C Ten microliters o f 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 o f standards. The concentration for quail serum and quail liver was determined from the following equations: Use Equation 1 to calculate the amount o f analyte found (in ng/mL, based on peak area) using the standard curve (linear regression parameters) generated by the Analyst software program. Then use Equation 2 to calculate the amount o f analyte found in pg/g (pg/mL for serum samples). Centre Analytical Laboratories, Inc. Page 16 o f 102 Cr*a-! r-jQ Centre Study No.: 023-041 Equation 1: Analyte found (ng/mL) = (Peak area - intercept) slope Equation 2: Analyte found (pg/g) = (anal, found (ng/mL) x FV (mL) x DF x EV (mL)) x 1 ug (AV (mL) x sample wt. (g)) 1000 ng Where: FV = Final Volume DF = Dilution Factor EV = Extraction Volume AV = Aliquot Volume For samples fortified with known amounts o f PFOS prior to extraction, use Equation 3 to calculate the percent recovery. Equation 3: Recovery (%) = (anal, found (ue/e) - avg. analvte in Ctrl (ue/g)) x 1000 ne x 100% amount added (ng/g) x 1 pg An example o f a calculation using an actual sample follows: Quail liver sample Centre ID 0007870 Spk A (Set: 121900A), fortified at 1000 ng/g with PFOS. Where: peak area = 11483 intercept = 463 slope = 2790 dilution factor = 100 ng/g added (fort level) = 1000 ng/g avg. amt in controls = 0 (Not quantifiable) final volume 1 mL extraction volume = 5 mL aliquot volume = 4 mL sample weight = 0.5 g From equation 1: Analyte found (ng/mL) = fl 1483- 4631 2790 From equation 2: Analyte found (pg/g) 3.9 ng/mL (3.9 ne/mL x 1 mL x 100 x 5 mLI x 1 ug (4 mL x 0.5 g) 1000 ng = 0.975 pg/mL Centre Analytical Laboratories, Inc. Page 17 of 102 Centre Study No.: 023-041 From equation 3: %Recovery = (0.975 ue/m L - 0 u g/m D x HOOP ng/1 no) x 100% 1000 ng/g = 98% 7.0 EXPERIMENTAL DESIGN Each set o f samples (liver or serum) consisted of one reagent blank, one matrix blank, two matrix blanks fortified at known concentrations, and ~ 20 samples. Each sample was extracted using the appropriate method and then analyzed in duplicate. 8.0 RESULTS The PFOS found in the reagent blanks are listed in T able I. The PFOS in the quail liver blanks and quail serum blanks are given in Tables II &III. Individual recoveries for PFOS in the liver samples are detailed in T able 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 T able V. The average percent recovery standard deviation for PFOS in serum samples was 108% 10% . PFOS in the quail liver samples ranged from non-quantifiable levels (a peak was detected at the corresponding analyte retention time but was less than the lowest concentration o f the calibration standards (0.0001 pg/mL)) to 8.37 pg/g. Individual results are listed in Tables V I-X III. The results are reported on a wet weight basis. PFOS in the quail serum samples ranged from 0.00212 pg/mL levels to 263 pg/mL. Individual results are listed in Tables XIV-XXI. The average percent moistures for the quail liver samples are given in T able XX II. 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 o f 102 C99158 Centre Study No.: 023-041 10.0 RETENTION OF DATA AND SAMPLES When the final report is complete, all original paper data generated by Centre Analytical Laboratories, Inc. will be shipped to the sponsor. This does not include facility-specific raw data such as instrument logs, however exact copies o f temperature logs will be submitted. Exact copies o f all raw data, as well as a signed copy o f the final analytical report and all original facility-specific raw data, will be retained in the Centre Analytical Laboratories, Inc. archives for the period o f time specified in 40 CFR Part 792. Retained samples o f reference substances are archived by the sponsor. Centre Analytical Laboratories, Inc. Page 19 o f 102 c ro is a Centre Study No.: 023-041 TABLES Centre Analytical Laboratories, Inc. Page 20 of 102 CC0160 Centre Study No.: 023-041 Table I. Summary o f PFOS in Reagent Blanks Sponsor ID na na na na na na na na na na na na na na na na Centre ID Reagent Blank A Reagent Blank A* Reagent Blank A Reagent Blank A* Reagent Blank A Reagent Blank A* Reagent Blank A Reagent Blank A* Reagent Blank A Reagent Blank A* Reagent Blank A Reagent Blank A* Reagent Blank A Reagent Blank A* Reagent Blank A Reagent Blank A* * Duplicate injection Set Number 121800A 121800A 121800B 121800B 121900A 121900A 121900B 121900B 122000A 122000A 122000B 122000B 030501A 030501A 030601A 030601A Extraction Analysis Analyte Date Date Found Ing/mL) 12/18/00 12/18/00 12/18/00 12/18/00 12/19/00 12/19/00 12/20/00 12/20/00 NQ NQ NQ NQ 12/19/00 12/21/00 NQ 12/19/00 12/21/00 NQ 12/19/00 12/21-22/00 12/19/00 12/21-22/00 NQ NQ 12/20/00 12/20/00 12/20/00 12/20/00 3/5/01 12/22/00 12/22/00 12/22-23/00 12/22-23/00 3/6-7/01 0.000200 0.000200 NQ NQ ND 3/5/01 3/6-7/01 ND 3/6/01 3/7/01 NQ 3/6/01 3/7/01 NQ AVERAGE: NQ STANDARD DEVIATION: NQ NQ = Not Quantifiable (A peak was detected at the corresponding analyte retention time but was less than the lowest concentration o f the calibration standards (0.0001 pg/mL)) ND = Not Detected For values recorded as ND,zero was used to calculate the average and standard deviation. For values recorded as NQ, 0.00005 pg/mL (half the value o f the 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 Centre Analytical Laboratories, Inc. Page 21 o f 102 Centre Study No.: 023-041 Table II. Summary of PFOS in Quail Liver Blanks Sponsor ID na na na Na 454 454 456 456 Centre ID 0011423 Blank A 0011423 Blank A* 0011423 Blank A 0011423 Blank A* 0007870 Blank A 0007870 Blank A* 0007872 Blank A 0007872 Blank A* Set Number 121800A 121800A I21800B 121800B 121900A 121900A 030601A 030601A Extraction Analysis Date Date 12/18/00 12/18/00 12/18/00 12/18/00 12/19/00 12/19/00 12/20/00 12/20/00 12/19/00 12/21/00 12/19/00 12/21/00 3/6/01 3/7/01 3/6/01 3/7/01 AVERAGE: STANDARD DEVIATION: Analyte Found (pg/g) NQ NQ 0.00113 0.00109 NQ NQ 0.00120 0.00110 0.000590 0.000578 Table III. Summary o f PFOS in Quail Serum Blanks Sponsor ID na na na na na na na na Centre ID 0011424 Blank A 0011424 Blank A* 0011424 Blank A 0011424 Blank A* 0011424 Blank A 0011424 Blank A* 0011424 Blank A 0011424 Blank A* Set Number 121900B 121900B 122000A 122000A 122000B 122000B 030501A 030501A Extraction Analysis Analyte Date Date Found (ue/mL) 12/19/00 12/21-22/00 0.0136 12/19/00 12/21-22/00 0.0144 12/20/00 12/22/00 0.0138 12/20/00 12/22/00 0.0151 12/20/00 12/22-23/00 0.0127 12/20/00 12/22-23/00 0.0109 3/5/01 3/6-7/01 0.00555 3/5/01 3/6-7/01 AVERAGE: 0.00559 0.0115 STANDARD DEVIATION: 0.00384 * Duplicate injection NQ = N ot Quantifiable (A peak was detected at the corresponding analyte retention time but was less than the lowest concentration o f the calibration standards (0.0001 pg/mL)) For values recorded as NQ, 0.00005 pg/g (half the value o f the 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/m L for serum Centre Analytical Laboratories, Inc. Page 22 of 102 Centre Study No.: 023-041 Table IV. Summary o f PFOS Recoveries in Quail Liver Sponsor ID na na na na na na na na 454 454 454 454 456 456 456 456 Centre ID 0011423 Spk A 0011423 Spk A* 0011423 Spk B 0011423 SpkB* 0011423 Spk A 0011423 Spk A* 0011423 Spk B 0011423 SpkB* 0007870 Spk A 0007870 Spk A* 0007870 SpkB 0007870 SpkB* 0007872 Spk A 0007872 Spk A* 0007872 Spk B 0007872 SpkB* Set Number 121800A 121800A 121800A 121800A 121800B 121800B 121900A 121900A 121900A 121900A 121900A 121900A 030601A 030601A 030601A 030601A Extraction Analysis Date Date Amt Added fng/g) 12/18/00 12/18/00 12/18/00 12/18/00 12/18/00 12/18/00 12/18/00 12/18/00 12/19/00 12/19/00 12/19/00 12/19/00 3/6/01 3/6/01 3/6/01 3/6/01 12/19/00 12/19/00 12/19/00 12/19/00 12/20/00 12/20/00 12/20-21/00 12/20-21/00 12/21/00 12/21/00 12/21/00 12/21/00 3/7/01 3/7/01 3/7/01 3/7/01 10 10 2000 2000 1000 1000 20000 20000 1000 1000 20000 20000 20 20 200 200 AVERAGE: STANDARD DEVIATION: RELATIVE STANDARD DEVIATION: % Recovery 102 104 101 103 113 110 80 80 99 103 85 84 93 86 82 84 94 11 12 * Duplicate injection LOQ = 0.01 ng/g for liver and 0.01 ng/mL for serum Centre Analytical Laboratories, Inc. Page 23 of 102 c c o ln a Centre Study No.: 023-041 Table V. Summary of PFOS Recoveries in Quail Serum Sponsor ID na na na na na na na na na na na na na na na na Centre ID 0011424 SpieA 0011424 Spk A* 0011424 SpkB 0011424 SpkB* 0011424 Spk A 0011424 Spk A* 0011424 SpkB 0011424 SpkB* 0011424 Spk A 0011424 Spk A* 0011424 SpkB 0011424 SpkB* 0011424 Spk A 0011424 Spk A* 0011424 SpkB 0011424 SpkB* Set Number 121900BD 121900BD 121900BD 121900BD 122000A 122000A 122000A 1220DOA 122000B 122000B 122000B 122000B 030501A 030501A 030501A 030501A Extraction Analysis Amt Date Date Added (ne/mLl 12/19/00 12/23-24/00 500 12/19/00 12/23-24/00 500 12/19/00 12/23-24/00 100000 12/19/00 12/23-24/00 100000 12/20/00 12/22/00 500 12/20/00 12/22/00 500 12/20/00 12/22/00 100000 12/20/00 12/22/00 100000 12/20/00 12/22-23/00 500 12/20/00 12/22-23/00 500 12/20/00 12/22-23/00 100000 12/20/00 12/22-23/00 100000 3/5/01 3/6-7/01 100 3/5/01 3/6-7/01 100 3/5/01 3/6-7/01 1000 3/5/01 3/6-7/01 1000 AVERAGE: STANDARD DEVIATION: RELATIVE STANDARD DEVIATION: % Recovery 103 106 90 93 106 103 97 103 108 110 113 98 122 122 107 115 106 9 9 * Duplicate injection LOQ = 0.01 |ig/g for liver and 0.01 |ig/m L for serum Centre Analytical Laboratories, Inc. Page 24 of 102 OC 0 1 .6 4 Centre Study No.: 023-041 Table VI. Summary of PFOS in Adult Liver Samples at 0 ppm a.i. (Test Termination 19 Weeks) Sponsor ID 451 451* 452 452* 453 453* 454 454* 455 455* 456 456* 457 457* 458 458* 459 459* 460 460* Centre ID 0007867 0007867 0007868 0007868 0007869 0007869 0007870 0007870 0007871 0007871 0007872 0007872 0007873 0007873 0007874 0007874 0007875 0007875 0007876 0007876 Set Number 121800AD 121800AD 121800A 121800A 121800AD 121800AD 121800A 121800A 121800AD 121800AD 121800A 121800A 121800AD 121800AD 121800A 121800A 121800AD 121800AD 121800A 121800A Extraction Analysis Date Date 12/18/00 12/18/00 12/20/00 12/20/00 12/18/00 12/18/00 12/18/00 12/18/00 12/18/00 12/18/00 12/18/00 12/18/00 12/18/00 12/18/00 12/18/00 12/18/00 12/18/00 12/18/00 12/18/00 12/18/00 12/18/00 12/18/00 12/19/00 12/19/00 12/20/00 12/20/00 12/19/00 12/19/00 12/20/00 12/20/00 12/19/00 12/20/00 12/20/00 12/20/00 12/19/00 12/19/00 12/20/00 12/20/00 12/19/00 12/19/00 AVERAGE: STANDARD DEVIATION: Analyte Found (ue/e) 0.215 0.215 NQ NQ 0.303 0.304 NQ NQ 0.114 0.111 NQ NQ 0.0762 0.0739 0.0103 0.0104 0.236 0.235 0.00117 0.00117 0.0953 0.113 * Duplicate injection NQ = Not Quantifiable (A peak was detected at the corresponding analyte retention time but was less than the lowest concentration o f the calibration standards (0.0001 pg/mL)) For values recorded as NQ, 0.00005 pg/g (half the value o f the 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/m L for serum Centre Analytical Laboratories, Inc. Page 25 of 102 G 0 0 G 5 Centre Study No.: 023-041 Table VII. Summary of PFOS in Adult Liver Samples at 1.8 ppm a.i. (Test Termination 6 Weeks) Sponsor ID E01-0259-20780 E01-0259-20780* E01-0259-20781 EOI-0259-20781* E01-0259-20782 EOI-0259-20782* EOI-0259-20783 EOl-0259-20783* EOl-0259-20784 E01-0259-20784* E01-0259-20790 E01-0259-20790* EOI-0259-20791 EOI-0259-20791* EOI-0259-20792 EOl-0259-20792* EOI-0259-20793 E01-0259-20793* EOI-0259-20794 EOI-0259-20794* Centre ID 0102997 0102997 0102998 0102998 0102999 0102999 0103000 0103000 0103001 0103001 0103007 0103007 0103008 0103008 0103009 0103009 0103010 0103010 0103011 0103011 Set Number 030601AD 030601AD 030601 AD 030601AD 030601AD 030601 AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601A 030601A 030601AD 030601AD 030601AD 030601AD Extraction Analysis Date Date 3/6/01 3/6/01 3/8/01 3/8/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/7/01 3/7/01 3/8/01 3/8/01 3/8/01 3/8/01 AVERAGE: STANDARD DEVIATION: Analyte Found Cig/g) 0.800 0.722 0.149 0.134 0.341 0.311 0.455 0.422 0.0988 0.0843 0.210 0.210 0.177 0.191 0.0124 0.0121 0.0381 0.0394 0.0629 0.0720 0.227 0.224 * Duplicate injection LOQ = 0.01 pg/g for liver and 0.01 fjg/mL for serum Centre Analytical Laboratories, Inc. Page 26 o f 102 CCOl f ^ G Centre Study No.: 023-041 Table V ffl. Summary of PFOS in Adult Liver Samples at 6.2 ppm a.i. (Test Termination 6 Weeks) Sponsor ID EOI-0259-20785 E01-0259-20785* E01-0259-20786 E01-0259-20786* E01-0259-20787 EOI-0259-20787* EO1-0259-20788 E01-0259-20788* E01-0259-20789 EOI-0259-20789* EOl-0259-20795 E01-0259-20795* E01-0259-20796 EOI-0259-20796* EOl-0259-20797 E01-0259-20797* EOI-0259-20798 EOl-0259-20798* EOI-0259-20799 EOI-0259-20799* Duplicate injection Centre ID 0103002 0103002 0103003 0103003 0103004 0103004 0103005 0103005 0103006 0103006 0103012 0103012 0103013 0103013 0103014 0103014 0103015 0103015 0103016 0103016 Set Number 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601 AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD 030601AD Extraction Date Analysis Date 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/6/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 3/6/01 3/8/01 AVERAGE: STANDARD DEVIATION: Analyte Found (he/e) 1.15 1.20 1.18 1.19 1.43 1.42 1.60 1.51 1.06 1.17 0.216 0.208 0.115 0.0934 0.0801 0.0797 0.187 0.218 0.0901 0.0954 0.715 0.606 LOQ = 0.01 jrg/g for liver and 0.01 ng/m L for serum Centre Analytical Laboratories, Inc. Page 27 o f 102 c Centre Study No.: 023-041 Table IX. Summary o f PFOS in Adult Liver Samples at 17.6 ppm a.i. (Test Termination 19 Weeks) Sponsor ID 481 481* 482 482* 483 483* 484 484* 485 485* 486 486* 487 487* 488 488* 489 489* 490 490* Centre ID 0007877 0007877 0007878 0007878 0007879 0007879 0007880 0007880 0007881 0007881 0007882 0007882 0007883 0007883 0007884 0007884 0007885 0007885 0007886 0007886 Set Number 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD 121800AD Extraction Analysis Date Date 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 AVERAGE: STANDARD DEVIATION: Analyte Found (pg/g) 1.05 1.05 4.10 4.17 8.37 8.30 1.41 1.43 1.54 1.51 0.415 0.392 1.17 1.15 0.511 0.509 2.42 2.48 0.351 0.360 2.13 2.39 * Duplicate injection LOQ = 0.01 jig/g for liver and 0.01 pg/mL for serum Centre Analytical Laboratories, Inc. Page 28 of 102 Centre Study No.: 023-041 Table X. Summary of PFOS in Juvenile Liver Samples at 0 ppm a.i. (Test Termination 12 Weeks) Sponsor ID 9503 9503* 9506 9506* 9508 9508* 9512 9512* 9515 9515* 9518 9518* 9520 9520* 9522 9522* 9525 9525* 9526 9526* Centre ID 0007907 0007907 0007908 0007908 0007909 0007909 0007910 0007910 0007911 0007911 0007912 0007912 0007913 0007913 0007914 0007914 0007915 0007915 0007916 0007916 Set Number 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B Extraction Analysis Date Date 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 AVERAGE: STANDARD DEVIATION: Analyte Found (ng/g) NQ NQ NQ NQ NQ NQ NQ NQ 0.000785 0.000755 NQ NQ 0.000734 0.000672 0.000718 0.000656 NQ NQ NQ NQ 0.000251 0.000316 * Duplicate injection NQ = Not Quantifiable (A peak was detected at the corresponding analyte retention time but was less than the lowest concentration o f the calibration standards (0.0001 pg/mL)) For values recorded as NQ, 0.00005 pg/g (half the value o f the 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 Centre Analytical Laboratories, Inc. Page 29 of 102 Centre Study No.: 023-041 Table XI. Summary of PFOS in Juvenile Liver Samples at 1.8 ppm a.i. (Test Termination 12 Weeks) Sponsor ID 9528 9528* 9529 9529* 9530 9530* 9531 9531* 9533 9533* 9535 9535* 9540 9540* 9541 9541* 9543 9543* 9544 9544* Centre ID 0007917 0007917 0007918 0007918 0007919 0007919 0007920 0007920 0007921 0007921 0007922 0007922 0007923 0007923 0007924 0007924 0007925 0007925 0007926 0007926 Set Number 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B 121800B Extraction Analysis Date Date 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/18/00 12/18/00 12/20/00 12/20/00 12/20/00 12/18/00 12/20/00 12/18/00 12/18/00 12/18/00 12/20/00 12/20/00 12/20/00 12/18/00 12/20/00 12/18/00 12/20/00 12/18/00 12/18/00 12/20/00 12/20/00 12/18/00 12/18/00 12/20/00 12/20/00 12/18/00 12/18/00 12/20/00 12/20/00 AVERAGE: STANDARD DEVIATION: Analyte Found (ug/g) 0.0130 0.0128 0.00295 0.00295 0.00904 0.00876 0.00417 0.00435 0.0119 0.0117 0.0113 0.0114 0.00635 0.00623 0.00305 0.00297 0.0126 0.0126 0.00514 0.00521 0.00792 0.00393 * Duplicate injection LOQ = 0.01 ng/g for liver and 0.01 pg/mL for serum Centre Analytical Laboratories, Inc. Page 30 o f 102 Centre Study No.: 023-041 Table XII. Summary o f PFOS in Juvenile Liver Samples at 6.2 ppm a.i. (Test Termination 12 Weeks) Sponsor ID 9548 9548* 9549 9549* 9551 9551* 9552 9552* 9555 9555* 9559 9559* 9561 9561* 9562 9562* 9563 9563* 9564 9564* Centre ID 0007927 0007927 0007928 0007928 0007929 0007929 0007930 0007930 0007931 0007931 0007932 0007932 0007933 0007933 0007934 0007934 0007935 0007935 0007936 0007936 Set Number 121900A 121900A 121900A 121900A 121900A 121900A 121900A 121900A 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD 121900A 121900A 121900AD 121900AD 121900A 121900A Extraction Analysis Date Date 12/19/00 12/19/00 12/21/00 12/21/00 12/19/00 12/21/00 12/19/00 12/21/00 12/19/00 12/19/00 12/21/00 12/21/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/21/00 12/21/00 12/23/00 12/23/00 12/23/00 12/23/00 12/19/00 12/23/00 12/19/00 12/23/00 12/19/00 12/21/00 12/19/00 12/19/00 12/21/00 12/23/00 12/19/00 12/23/00 12/19/00 12/21/00 12/19/00 12/21/00 AVERAGE: STANDARD DEVIATION: Analyte Found Oig/g) 0.00303 0.00305 0.0100 0.0105 0.0123 0.0125 0.00316 0.00302 0.0410 0.0408 0.0340 0.0341 0.0446 0.0445 0.0116 0.0121 0.0193 0.0197 0.00184 0.00201 0.0182 0.0156 * Duplicate injection LOQ = 0.01 (Jig/g for liver and 0.01 ng/mL for serum Centre Analytical Laboratories, Inc. Page 31 o f 102 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 ID 9567 9567* 9570 9570* 9575 9575* 9579 9579* 9580 9580* 9581 9581* 9582 9582* 9583 9583* 9584 9584* 9588 9588* Centre ID 0007937 0007937 0007938 0007938 0007939 0007939 0007940 0007940 0007941 0007941 0007942 0007942 0007943 0007943 0007944 0007944 0007945 0007945 0007946 0007946 Set Number 121900A 121900A 121900AD 121900AD 121900A 121900A 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD 121900AD Extraction Analysis Date Date 12/19/00 12/21/00 12/19/00 12/21/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/23/00 12/23/00 12/21/00 12/21/00 12/23/00 12/23/00 12/23/00 12/23/00 12/23/00 12/23/00 12/23/00 12/23/00 12/23/00 12/23/00 12/23/00 12/23/00 12/19/00 12/23/00 12/19/00 12/23/00 AVERAGE: STANDARD DEVIATION: Analyte Found (ug/g) 0.00904 0.00912 0.0424 0.0429 0.00629 0.00623 0.0880 0.0898 0.0461 0.0441 0.0492 0.0451 0.0747 0.0733 0.156 0.132 0.0983 0.101 0.0350 0.0370 0.0593 0.0417 * Duplicate injection LOQ = 0.01 ng/g for liver and 0.01 pg/mL for serum Centre Analytical Laboratories, Inc. Page 32 o f 102 Centre Study No.: 023-041 Table XTV. Summary of PFOS in Adult Serum Samples at 0 ppm a.i. (Test Termination 19 Weeks) Sponsor ID 451 451* 452 452* 453 453* 454 454* 455 455* 456 456* 457 457* 458 458* 459 459* Centre ID 0007887 0007887 0007888 0007888 0007889 0007889 0007890 0007890 0007891 0007891 0007892 0007892 0007893 0007893 0007894 0007894 0007895 0007895 Set Number 121900BD 121900BD 121900B 121900B 121900BD 121900BD 121900B 121900B 121900B 121900B 121900BD 121900BD 121900BD 121900BD 121900BD 121900BD 121900BD 121900BD Extraction Analysis Date Date 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/19/00 12/23-24/00 12/23-24/00 12/21-22/00 12/21-22/00 12/23-24/00 12/23-24/00 12/21-22/00 12/21-22/00 12/21-22/00 12/21-22/00 12/23-24/00 12/23-24/00 12/23-24/00 12/23-24/00 12/23-24/00 12/23-24/00 12/23-24/00 12/23-24/00 AVERAGE: STANDARD DEVIATION: Analyte Found (ua/mL) 11.6 11.8 0.0102 0.00909 9.04 10.4 0.00274 0.00212 0.0125 0.0123 6.32 6.46 6.58 6.35 0.105 0.102 8.75 8.50 4.78 4.64 * Duplicate injection LOQ = 0.01 ng/g for liver and 0.01 ng/m L for serum Centre Analytical Laboratories, Inc. Page 33 o f 102 ;0 0 1 7 3 Centre Study No.: 023-041 Table XV. Sum m ary o f PFOS in A dult Serum Sam ples at 1.8 ppm a.i. (Test Term ination 6 W eeks) Sponsor ID E01-0259-20752 EOI-0259-20752* EOI-0259-20753 EOl-0259-20753* EOI-0259-20754 EOI-0259-20754* EOI-0259-20755 EOI-0259-20755* EOI-0259-20756 EOI-0259-20756* EOI-0259-20762 E01-0259-20762* EOI-0259-20763 EOI-0259-20763* E01-0259-20764 EOI-0259-20764* EOI-0259-20765 E01-0259-20765* EOI-0259-20766 E01-0259-20766* Centre ID 0102969 0102969 0102970 0102970 0102971 0102971 0102972 0102972 0102973 0102973 0102979 0102979 0102980 0102980 0102981 0102981 0102982 0102982 0102983 0102983 Set Number 03050IAD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD Extraction Analysis Date Date 3/5/01 3/5/01 3/5/01 3/7-8/01 3/7-8/01 3/7-8/01 3/5/01 3/5/01 3/5/01 3/5/01 3/5/01 3/5/01 3/5/01 3/5/01 3/5/01 3/5/01 3/5/01 3/5/01 3/7-8/01 3/7-8/01 3/7-8/01 3/7-8/01 3/7-8/01 3/7-8/01 3/7-8/01 3/7-8/01 3/7-8/01 3/7-8/01 3/7-8/01 3/7-8/01 3/5/01 3/5/01 3/5/01 3/5/01 3/7-8/01 3/7-8/01 3/7-8/01 3/7-8/01 3/5/01 3/7-8/01 AVERAGE: STANDARD DEVIATION: Analyte Found (mt/mL) 10.9 10.9 7.92 8.01 16.4 16.0 35.8 33.1 24.3 23.7 1.50 1.89 5.01 4.98 1.57 1.84 0.134 0.117 10.5 9.79 11.2 10.7 * Duplicate injection LOQ = 0.01 jxg/g for liver and 0.01 ng/mL for serum Centre Analytical Laboratories, Inc. Page 34 o f 102 Centre Study No.: 023-041 Table XVI. Summary of PFOS in Adult Serum Samples at 6.2 ppm a.i. (Test Termination 6 Weeks) Sponsor ID E01-0259-20757 EOI-0259-20757* EOI-0259-20758 EOl-0259-20758* EOl-0259-20759 EOI-0259-20759* EOI-0259-20760 EOI-0259-20760* EOl-0259-20761 EOI-0259-20761* EOI-0259-20767 E01-0259-20767* E01-0259-20768 EOI-0259-20768* E01-0259-20769 E01-0259-20769* E01-0259-20770 E01-0259-20770* E01-0259-20771 EOI-0259-20771* Centre ID 0102974 0102974 0102975 0102975 0102976 0102976 0102977 0102977 0102978 0102978 0102984 0102984 0102985 0102985 0102986 0102986 0102987 0102987 0102988 0102988 Set Number 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501 AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501AD 030501 AD 030501AD 030501AD 030501 AD 030501AD 030501AD Extraction Analysis Date Date 3/5/01 3/5/01 3/7-8/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/5/01 3/7-8/01 3/7-8/01 3/5/01 3/5/01 3/5/01 3/5/01 3/5/01 3/5/01 3/7-8/01 3/7-8/01 3/7-8/01 3/7-8/01 3/7-8/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/5/01 3/5/01 3/7-8/01 3/7-8/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 3/5/01 3/7-8/01 AVERAGE: STANDARD DEVIATION: Analyte Found (ue/m h) 52.2 56.1 102 94.7 80.4 84.6 69.2 62.9 84.6 86.7 4.57 4.07 2.72 2.61 4.02 3.87 3.24 3.31 2.10 1.70 40.3 39.7 * Duplicate injection LOQ = 0.01 ng/g for liver and 0.01 (ig/mL for serum Centre Analytical Laboratories, Inc. Page 35 o f 102 Centre Study No.: 023-041 Table XVQ. Summary of PFOS in Adult Serum Samples at 17.6 ppm a.i. (Test Termination 19 Weeks) Sponsor ID 481 481* 482 482* 484 484* 485 485* 487 487* 488 488* 489 489* 490 490* Centre ID 0007896 0007896 0007897 0007897 0007898 0007898 0007899 0007899 0007900 0007900 0007901 0007901 0007902 0007902 0007903 0007903 Set Number 121900BD 121900BD 121900BD 121900BD 121900BD 121900BD 121900BD 121900BD I21900BD 121900BD 121900BD 121900BD 030501AD 030501AD 121900BD 121900BD Extraction Analysis Date Date 12/19/00 12/23-24/00 12/19/00 12/23-24/00 12/19/00 12/23-24/00 12/19/00 12/23-24/00 12/19/00 12/19/00 12/23-24/00 12/23-24/00 12/19/00 12/19/00 12/19/00 12/23-24/00 12/23-24/00 12/23-24/00 12/19/00 12/19/00 12/19/00 12/23-24/00 12/23-24/00 12/23-24/00 3/5/01 3/7-8/01 3/5/01 3/7-8/01 12/19/00 12/23-24/00 12/19/00 12/23-24/00 AVERAGE: STANDARD DEVIATION: Analyte Found (ue/mL) 260 263 43.1 42.4 118 106 179 172 133 127 15.8 16.8 232 228 6.87 6.80 122 93.0 * Duplicate injection LOQ = 0.01 iig/gfor liver and 0.01 ng/m L for serum Centre Analytical Laboratories, Inc. Page 36 o f 102 Centre Study No.: 023-041 Table XVIII. Summary of PFOS in Juvenile Serum Samples at 0 ppm a.i. (Test Termination 12 Weeks) Sponsor ID 9503 9503* 9506 9506* 9508 9508* 9512 9512* 9515 9515* 9518 9518* 9520 9520* 9525 9525* 9526 9526* Centre ID 0007947 0007947 0007948 0007948 0007949 0007949 0007950 0007950 0007951 0007951 0007952 0007952 0007953 0007953 0007954 0007954 0007955 0007955 Set Number 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A Extraction Analysis Date Date 12/20/00 12/22/00 12/20/00 12/20/00 12/20/00 12/22/00 12/22/00 12/22/00 12/20/00 12/20/00 12/22/00 12/22/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/22/00 12/22/00 12/22/00 12/22/00 12/22/00 12/22/00 12/20/00 12/20/00 12/20/00 12/22/00 12/22/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 AVERAGE: STANDARD DEVIATION: Analyte Found (ue/mL) 0.00486 0.00385 0.00718 0.00754 0.00365 0.00319 0.00431 0.00457 0.00789 0.00528 0.00378 0.00481 0.00367 0.00395 0.00552 0.00438 0.00354 0.00388 0.00477 0.00142 * Duplicate injection LOQ ==0.01 |tg /g fo r liver and 0.01 ng/m L for serum Centre Analytical Laboratories, Inc. Page 37 o f 102 C7 Centre Study No.: 023-041 Table XIX. Summary of PFOS in Juvenile Serum Samples at 1.8 ppm a.i. (Test Termination 12 Weeks) Sponsor ID 9528 9528* 9529 9529* 9530 9530* 9531 9531* 9533 9533* 9535 9535* 9540 9540* 9541 9541* 9543 9543* 9544 9544* Centre ID 0007956 0007956 0007957 0007957 0007958 0007958 0007959 0007959 0007960 0007960 0007961 0007961 0007962 0007962 0007963 0007963 0007964 0007964 0007965 0007965 Set Number 122000D 122000D 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A 122000A Extraction Date Analysis Date 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 12/20/00 12/22/00 AVERAGE: STANDARD DEVIATION: Analyte Found (ue/mL) 0.0762 0.0670 0.0273 0.0284 0.00785 0.00824 0.0480 0.0476 0.0488 0.0494 0.0416 0.0413 0.0192 0.0189 0.0321 0.0334 0.00969 0.00983 0.0158 0.0166 0.0324 0.0198 * Duplicate injection LOQ = 0.01 fig/g for liver and 0.01 pg/mL for serum Centre Analytical Laboratories, Inc. Page 38 o f 102 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 ID 9548 9548* 9549 9549* 9551 9551* 9552 9552* 9555 9555* 9559 9559* 9561 9561* 9562 9562* 9563 9563* 9564 9564* Centre ID 0007966 0007966 0007967 0007967 0007968 0007968 0007969 0007969 0007970 0007970 0007971 0007971 0007972 0007972 0007973 0007973 0007974 0007974 0007975 0007975 Set Number 122000D 122000D 122000D I22000D 122000D I22000D 122000B 122000B 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D Extraction Date Analysis Date 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/20/00 12/24/00 12/24/00 12/24/00 12/24/00 12/24/00 12/24/00 12/22-23/00 12/22-23/00 12/24/00 12/24/00 12/24/00 12/24/00 12/24/00 12/24/00 12/24/00 12/24/00 12/24/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 AVERAGE: STANDARD DEVIATION: Analyte Found Oie/mL) 0.137 0.160 0.382 0.390 0.222 0.208 0.0542 0.0535 0.243 0.218 0.161 0.168 0.185 0.171 0.231 0.229 0.259 0.254 0.171 0.173 0.203 0.0838 * Duplicate injection LOQ = 0.01 ng/g for liver and 0.01 |ag/mL for serum Centre Analytical Laboratories, Inc. Page 39 of 102 Centre Study No.: 023-041 Table XXI. Summary of PFOS in Juvenile Serum Samples at 17.6 ppm a.i. (Test Termination 12 Weeks) Sponsor ID 9567 9567* 9570 9570* 9575 9575* 9579 9579* 9580 9580* 9581 9581* 9582 9582* 9583 9583* 9584 9584* 9588 9588* Centre ID 0007976 0007976 0007977 0007977 0007978 0007978 0007979 0007979 0007980 0007980 0007981 0007981 0007982 0007982 0007983 0007983 0007984 0007984 0007985 0007985 Set Number 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D 122000D Extraction Date Analysis Date 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 12/20/00 12/24/00 AVERAGE: STANDARD DEVIATION: Analyte Found Oig/mL) 0.329 0.355 0.483 0.512 0.241 0.252 0.406 0.424 0.287 0.254 0.295 0.285 0.459 0.473 0.521 0.524 0.553 0.564 0.532 0.509 0.413 0.114 * Duplicate injection LOQ = 0.01 ng/g for liver and 0.01 ng/mL for serum Centre Analytical Laboratories, Inc. Page 40 o f 102 C " 0 5 .8 0 Centre Study No.: 023-041 Table XXII. Summary o f Percent M oistures for Q uail L iver Sam ples Sponsor ID 451 452 453 454 455 456 457 458 460 482 484 486 488 490 9506 9508 9512 9518 9520 9522 9526 9530 9540 9543 9544 9548 9551 9552 9555 Centre ID 0007867 0007868 0007869 0007870 0007871 0007872 0007873 0007874 0007876 0007878 0007880 0007882 0007884 0007886 0007908 0007909 0007910 0007912 0007913 0007914 0007916 0007919 0007923 0007925 0007926 0007927 0007929 0007930 0007931 % Moisture Sponsor ID 66.7 9559 64.4 9561 68.4 9562 65.6 9563 64.1 9564 71.8 9570 59.5 9579 71.2 9584 69.0 9588 55.0 E01-0259-20780 60.6 E01-0259-20781 72.5 E01-0259-20782 61.5 E01-0259-20783 65.1 EO1-0259-20784 70.7 E01-0259-20785 72.1 E01-0259-20786 67.4 E01-0259-20787 73.2 E01-0259-20788 73.5 E01-0259-20789 68.3 E01-0259-20790 67.9 E01-0259-20791 70.0 E01-0259-20792 66.7 E01-0259-20793 57.1 E01-0259-20794 55.8 E01-0259-20795 59.4 EO1-0259-20796 81.3 EO1-0259-20797 53.5 EO1-0259-20798 65.0 EO1-0259-20799 Centre ID 0007932 0007933 0007934 0007935 0007936 0007938 0007940 0007945 0007946 0102997 0102998 0102999 0103000 0103001 0103002 0103003 0103004 0103005 0103006 0103007 0103008 0103009 0103010 0103011 0103012 0103013 0103014 0103015 0103016 % Moisture 78.3 80.6 57.8 63.4 34.6 85.2 88.7 59.6 65.2 70.3 57.8 70.6 67.0 67.7 64.5 72.3 67.6 68.0 68.0 69.3 70.9 67.0 65.3 74.5 65.7 71.7 72.8 71.3 72.1 Centre Analytical Laboratories, Inc. Page 41 o f 102 Centre Study No.: 023-041 FIGURES Centre Analytical Laboratories, Inc. Page 42 o f 102 C C 01S2 A Area, couras gg 01 0< 0( ot 05 p i -r* .-r-r* r fi b b b b o 'o b 'o - * * * -^ * | SJ o 4- j ; 1 ! M: ES Cs. tar la m rs '2 ce r*j i 1 l' cd] ! bl o m _; S ] .? 01J ^ 1 ; j . wJ ! ,,i ! '\ ! 1 ! 1 4k 1 * i *1 i .1 ! * ! i N : V \ \- >; i - : E8 f? M : tS E t& 13 I m m -m m m m fc m m BE SS K? t j \ / a u ----- j f ------------ ^ ------y r -------- i n - - - ------UU ----------- O L i ru i<wv - 'iv'r*"u ------r ------ Centre Study No.: 023-041 Figure 2. Chromatogram Representing a 0.1 ng/mL standard for PFOS tu * laden: 1 Saaplc Type: ' C oeeeatsatlen: kcq. D ate: : I c q . "timi 1 oc 0.100 12/22/60 10:37:10 Mt ! M U IM i 1 O M eU tf faeces: n oise Tfcsesbold: 1 Area Tftceabeid: ! M a . SoooOts: RT Nindo: - C apaetef *T: : Sep. ttiddi: ' s e p . Melo b e: 1 Sap* Seek R atio : : cap. M j. Reclot 1 Cap. Vai. Ratio; ; Ose R e la tiv e RT: !.. i l.N .99 1 30.0 4.i t 0.20 o.ot 9.00 4.00 3.00 Ne see in s a r g i a . ; P -.1..::..; . J 233 . 220 J 1 200. i 100; 1 iso i i ,, 140, * * 120 f f J 100 lac. type: ReCeeeiea f is : 1 Aseet , neiRbet S ta rt Tlsw: 1 Bed T la e t Manual 4.49 ! 1033,0 e o a au 2.1Se*002 cps 4.40 ala 4.9 1 j 40 4 j ^ _*_* 0 * 1.0 t J 10 ' ' !.. I 1 . I f'js %rv**'^w * 2.1 3.0 W 4.0 4. 3 0 Tima, min ,v . IN 9 3 0.0 0.3 7tJ J..J ' A 7.0 " f.V " "" Centre Analytical Laboratories, Inc. .................................................... - ....... .... . - ...- Page 44 o f 102 Centre Study No.: 023-041 Figure 3. Chromatogram Representing a 1.0 ng/mL standard for PFOS ||||S S S 5 i 8 aw w in taaaaiiit Scapi ladiici pi Typ*: Co*c*Atracle: t o |. OtU: 1 Ae*. Tiara; Standard 1.000 12/22/00 1 1 :1 3 : AN ; M odiri*' 1 Im ehinv Factor: 1 Soia* TMc*alioid; ' Afa Tbcaahold: dea. saoocha: : OT NLadow: ` xp*ctd a i: 1 Sop. Miotot ( Sop. teitficr Cxp, H i k Macia B*p. AdJ. t a t l s : Cip. Val. R itte: Qm t e l a ti KT: Ua 1 1.S1 *.33 1 20.0 4.31 0.20 0.01 9.00 4.0 t3e.00 > Ine. Typa: 1 te concio* timi > Ara*: \ folpbt: i S ta r t TIm i j te d Tiara; M utui 4.50 aia 4000.C 1.13#*00) 4.40 a la 4.41 a ia mi Itoo- I 400 400- 1 200 too t.O 1.0 2.0 * 0-0 J - * 4.0 4.J 9.0 9.0 4.0 f.S t.0 t.| Centre Analytical Laboratories, Inc. Page 45 o f 102 o.^ Centre Study No.: 023-041 Figure 4. Chromatogram Representing a R eagent Blank for PFOS (Centre ID Reagent Blank A, Set: 122000A) : iM pU Index: ! ta a U tjp: 1 Coaeentcatiee: I Acq. Oien: , Aeq. Tine: Aleak 0.000 12/22/00 12:04:41 M 1 Nedified: Tee I d tA ia t Faecox: 1 i Hola* Threshold: U l ; Aren Threshold: .44 Run. Soooths: 1 ' RT Window: - 30.0 aec ; Expected a ft 4.51 U lo p . Width! 0.20 ! sop. height: . b p . fw k Ratio; 0.01 $.00 1 . Exp. Adi. Ratio: Exp, Val. Ratlor 4.00 3.00 ti Uaa R elativ a Rt: Bo 1 ' Xnt. Typet : Retention Tine: 1 Atoa: H eig h t: ! S ta rt Tina: End Tino: naatwl 4.50 nia z :. cooats 4.40r*0tf cpe 4.3 n ia 4.07 nia 4M | 4M 3M m. 200 IM 100 50 0 .48> J-W 5 M . ^ U 4.0 4.* 4 0 4 4 Tbnet artn IHMI 7.51 7.71 Centre Analytical Laboratories, Inc. Page 46 o f 102 Centre Study No.: 023-041 Figure 5. Chromatogram Representing Control Quail Serum for PFOS (Centre ID: 0011424 Blank A, Set: 122000A) Saxple Xadax: flawple Type) C o eeeetx atlo e: Acq. Dace: Acq. Tine: To p0.l0a0n0k 12/22/00 12:21:80 M ; Modified: 1Benchlaq fac to r: | Poiee T hm keldi I k m Thseafcold: i Iff Window: expected iff: , Sep. Width: Sep. Heiqht: Sxp. Soak R atio : Exp. Adj. R etie: Rxp. V ai. R e tie : Uee R e la tiv e Iff: 1Tea 11..001 30.0 4.SI 0.20 05..0001 4.00 3.00 a< m I In c. Type: ! R eteetlon Tine: i Acta: j Naifkt: I Scare Tine: : End T ine: Heeeal 4.SO a la 4710.0 ceenta l.03e+003 4.30 4.83 Centre Analytical Laboratories, Inc, Page 47 o f 102 C r 'll. 8 Centre Study No.: 023-041 Figure 6. Chromatogram Representing Control Q uail Liver for PFOS, (Centre ID: 0007870 Blank A Set: 121900A) j M aple tadtxi | Staple type; lank 12/21/00 Concentration: | Ac*. Date: 0.000 Ac*. Tlae: 11:20:14 AN J NodMled: i Ranching Factor: Noise fbteahoid: Y1i.ena I Area TBhoreosthho:ld: l . ; RT window: : expected nr: ; Sep. Width: 30.0 IM 4 .SI a il 0.20 I Sep. Reipht: 0.01 ! Cxp. Seek R atio: 3.00 j exp. Ad). Ratio: , Exp. V al. R atio: ' Ooe R e la tiv e W ; 4.00 3.00 NO { l u t . Type: Retention tin e : Acea: | height: ! S tart Tice: Cnd T im : 4.41 412.0 1.01et002 q 4.37 Bin 4 . SI oin "! "1 033 0* j 1A -.'..ii. \* v V I Centre Analytical Laboratories, Inc. Page 48 o f 102 Centre Study No.: 023-041 Figure 7. Chromatogram Representing Control Q uail Serum Fortified with 500 ng/m L o f PFOS (Centre ID: 0011424 Spk A , Set: 122000A) ;SupU lad u i 'tM pi np*> ! ConcMCracioai IAc*, ta c it ; Aeq. T1m : 12 oe 2.004 12/22/00 12iirl7 m : M odifiai: vnehino F ie te n :Mol* T lin s k e ld i Ac* Thxatold: Nua. Saeecfta: RT Nlndowr U p M ttd RT: Sp. Width; Sp. Exp. Nk b c i e : Cap. Ad}. U t i o i . Cap. Vi. M c io : Oea M la tlv * RT: y l t.5n5 1 30.0 4. SI 0.20 0.01 1.00 4.00 3.00 do l t . Typ*: R eten tio n Tint: Ax: HaiqhC: S care T1m : . CM fi} Manual 4.4 TSTO.O l.?*003 4.40 in 4.02 in i i j 1 1100 ' 1 100 | 1200 j t : 2001 1j 0- l.S 1.0 l.s 4.0 4.1 M Tiww.hUw 1.1 1.0 1.1 T.a T.l ___________ Centre Analytical Laboratories, b e. Page 49 o f 102 Centre Study No.: 023-041 Figure 8. Chromatogram Representing Control Q uail Liver Fortified at 10 ppb with PFOS (Centre ID: 0011423 Spk A, Set: 121800A) U4/.1PVMM I l i t l l M Ml >nurtitn rtctMs IIU IMMMm u iI M l* TktMlwUr liM ltX t: il, nat il.tl 1i1.1 * . l 1M l * tap. N a iuiui 1 ta. M ). U t t ii t Cap. W . M U V M IMUfKN BTs M tM UM flM I *cet N al*i t u n tiaai Cut tuai ml 1 l.lt aui I 14. IN M lI 44..141J H> IM I MS __4_.9___4L. . . 7J - M Centre Analytical Laboratories, Inc, Page 50 o f 102 Centre Study No.: 023-041 Figure 9. Chromatogram R epresenting Juvenile Q uail Serum Sample (Centre ID: 0007965, Sponsor ID: 9544, Set: 122000A) Centre Analytical Laboratories, Inc, Page SI o f 102 C' CT 9:192 Centre Study No.: 023-041 APPENDIX A Study Protocol 00P-023-041 (Centre Study No. 023-041) and Amendments and Deviations Centre Analytical Laboratories, Inc. Page 53 o f 102 C~ ? 93 Centre Study No.: 023-041 r Centre Protocol No. OOP-023-041 STUDY PROTOCOL STUDY TITLE EXTRACTIONOF POTASSIUMPERFLUOROOCTANESULFONATEFROM QUAIL SERUM AND QUAILLIVER FOR ANALYSIS USING HPLC- ' ELECTROSFRAY/MASS SPECTROMETRY . SPONSOR 3M Environmental Technology and Safety Services Building 2-3E-09 PO Box 33331 St. Paul, MN 55133-3331 DATA REQUIREMENTS - Analytical Method Requirements TESTING LABORATORY Centre A nalytical Laboratories, Inc. (Centre) 3048 Research Drive State College. PA 16801 Phone 814-231-8032 PROTOCOL IDENTIFICATION NUMBER : 00P-023-041 Centre Analytical Laboretories, Inc. Centre Analytical Laboratories, Inc. Page l o f 43 Page 54 o f 102 C C 0194 Centre Study No.: 023-041 Centre Protocol No. OOP-023-041 Title: EXTRACTION OF POTASSIUMPERFLUOROOCTANESULFONATEFROM QUAIL SERUM AND QUAILLIVERFOR ANALYSIS USING HPLC. . ELECTROSPRAY/MASS SPECTROMETRY - TABLE OF CONTENTS TABLEOF CONTENTS. Page 1. PURPOSE. ! **M la .3 TEST MATERIALS ; 3. SPONSOR.. 4. TESTING FACILITYAND PERFORMINGLABORATORY________ ; 4 5. PROPOSED EXPERIMENTALTIME-FRAME_____ ______ 4 6. JUSTIFICATION FORTHE SELECTION OF THE TEST SYSTEM_______ 4 7. . SAMPLE PROCESSINO, STORAGE ANDIDENTIFICATION-----________5 8. ANALYTICAL METHOD........................................ 5 9. EXPERIMENTALDESIGN.........- ---- --------------- :---- -------------------- 10 10. PROTOCOLAMENDMENTS ANDDEVIATIONS-------------.'._________10 11. RECORDS______ !___ ______________ _________ ____________ ....... 11 12. QUALITYASSURANCE......... 12 13. DATA AND REPORT-- ----- :..... 14. ARCHIVE STATEM ENT........... 12 13 15. REFERENCES__ 13 16. PROTOCOL APPROVAI_____ .14 APPENDIX: ANALYTICALMETHODS... .15 Centre A nalytical Laboratories, Inc. Centre Analytical Laboratories, Inc. Page2of43 Page 55 o f 102 --lT Centre Study No.: 023-041 Centre Protocol No. OOP-023-041 SSrtyTitle; ! EXTRACTION OF POTASSIUM PERFLUOROOCTANESULFONATE FROM QUAIL SERUM AND QUAIL LIVER FOR ANALYSIS USING HFLC- ELECTROSPRAY/MSS SPECTROMETRY 1. PURPOSE The purpose of this study is to snalyze quail serum samples and quail Ever samples for residues of perfluorooctanesulfonate (PFOS) using methods entitled, "Extraction Of Potassium Perfluorooctanesulfonate Or Other Fluorochemical Compounds From- Senim For Analysis Using HPLC-Electrospray/Masi Spectrometry" (3M method number ETS-8-4.1) and "Extraction Of Potassium Perfluorooctanesulfonate Or Other Fluorochemical Compounds From Liver For Analysis Using HPLC-Electrospray/Mass Spectrometry" (3M method number ETS-S-6.0) with the modifications fisted in Section 8. The QualityAssurance Unit of Centre Analytical Laboratories, Inc., will audit the study for compliance with EPA TSCA Good Laboratory Practice standards 40 CFRPart 792(1). 2. TEST MATERIALS The following analytical standards will be used: Test Material PFOS ' TCR Number TCR00017-46 Purity(%). 97.9 Expiration Date 08/31/01 Chemical name and structure of die compound is presented below. PFOS Chemical Name: IUPAC Name: ' Perfluorooctanesulfonate 1-Octanesulfonic acid.l.1.2,23.3.4,433.6,6.7,7,8,8.8hcptadccafluoro-, potassium salt CASNumber. 2795-39-3 MolecularWeight: 499 (CjFitSOj- ) O II CaFnjS-- o* 0 Note: The neutral molecule and standard form that PFOS (anion) is derived from ' is perfluorooctanesulfonate potassium salt [CiFnSOjK], molecular weight 538. Centre Analytical Laboratories, b e . Page 3 o f 43 Centre Analytical Laboratories, Inc. Page 56 o f 102 Centre Study No.: 023-041 CentreProtocol No.00P-Q23-041 A record of test and reference substance receipt, storage conditions, and a record of use win be maintained at Centre Analytical Laboratories, Inc. Forms documenting chaln-of-custody and shipping records for tracking of the test substances wiUbe included as part ofthe raw data package. AH standards/test substances and any prepared solutions must be identified with a unique label or number on the container or cross-referenced to the container. HAZARDDSfORMATION A current MSDS for the chemical(s) used in this study wiU be maintained at the testing facility. 3. SPONSOR 3M Environmental Technology and Safety Sendees Building 2-3E-09 PO Box 33331 ' S t Paul, MN 55133-3331 STUDY DffilCTOR: Rochelle Robideau TELEPHONE- 651-778-7065 FAX NUMBER: 651-778-6176 - - 4. TESTING FACILITY AND PERFORMING LABORATORY Centre Analytical Laboratories, Inc. (Centre) 3048 Research Drive State College, PA 16801 PRINCIPAL INVESTIGATOR; Emily R. Stauffer, Centre TELEPHONE: 814-231-8032 FAX NUMBER: 814-231-1580 5. PROPOSED EXPERIMENTAL TIME-FRAME Experimental Start Date Experimental Termination Date Report Issued Dec. 11,2000 Dec. 15,2000 Dec. 30.2000 6. JUSTIFICATION FOR THE SELECTION OF THE TEST SYSTEM : Quail serum samples and liver samples collected by Wildlife International, Ltd. will be used as the test systems for this study. ' Quails .-represent wild bird populations and they are an EPA recommended species because they do well in a laboratory environment Quail habitats include bushy pastures, grassy roadsides. Centre Analytical Laboratories, Inc. Page 4 o f 43 Centre Analytical Laboratories, Inc. Page 57 o f 102 C O'197 Centre Study No.: 023-041 CentreProtocol No. 00P-023-041 farmlandsand open woodlands, and they are considered land grazers. The use of these matrices for the study was to determine if PFOS was deposited in the liver and serum of mating adults that were fed PFOS. A complete description of the test system along with all of foe in-life parameters is documented in foe sponsor's protocot no. 454A)1060Q/QP/SUB454, Project No. 454-104 that is associated with this analytical protocol. SAMPLE PROCESSING,STORAGE AND IDENTIFICATION No processing will be required for the serum samples. Due to foe small amount of sample available, foe liver samples will not be homogenized prior to extraction: however, they will be homogenized by laying the samples on a flat surface and mashing them by hand as best as possible. Each sample will be assigned a unique sample identification number at Centre, which will be used for tracking and identification of foe samples. The samples will be stored in a temperature-monitored freezer, maintained at < -10* C, except when removed for extraction and analysis as described in the method. The samples will be keptisolated from the test substanceduring storage. Sample receipt and storage location and conditions during the tudy will be documented.' All samples and any resulting sample extracts will be identified with a unique label or-sample number. Such identification will be either oh the container or cross-referenced to the container. ANALYTICAL METHOD The serum samples will be analyzed according to,the analytical method titled "Extraction Of Potassium Perfluorooctanesulfonate Or Other Buorochemical Compounds *Pram Serum For Analysis Using HPLC-Electrospray/Masa Spectrometry" (3M method'number ETS-8-4.1) and the control liver samples will be analyzed eecordinf to the m ethod titled "E xtraction Of P o tau iu m Perfluorooctanesulfonate Or. Other.Huorochcmicsl Compounds Pnom liver For Analysis Using HPLC-Electrospray/Mass Spectrometry" (3M method number ETS-8-6.0). The followingmodifications will be applied to each method: I. There will be no surrogate standard used in the extraction procedure. The stock, fortificattion, and calibration standards will be prepared as follows: Stock Solution Prepare s stock solution of PFOS at 100 pg/mL by weighing out 10.0 mg of analytical standard (corrected forpercent salt and percent purity). Adjust final volume to 100 mL with methanol in a 100-mL volumetric flask. Store this C C 9 1 .H S Centre Study No.: 023-041 Centre Protocol No. OOP-023-041 F o rtificatio n S olutions a. 1.0 ug/mL Fortification Solution - Pipette.1.0 mL of the 100 pg/ml. stock solution into a 100 mL volumetric flask. Bring up to volume with methanol. b. 0,l ,m taL ,Ftifiqtion Solution - Pipette lO.O mL of the 1.0 pgfml fortification solution into a 100-mL volumetric flask and bring up to r voaanrw ith ffietitanor r " 7" ` c. 0.01 ug/mL Fortification Solution - Pipette 10.0 mL of the 0.1 pg/mL fortification solution into a 100-mL volumetric flask and bring up to volume with methanol Store all fortification standard solutions (in 125-mL LDPE bottles) in a refrigerator at 2C to 6C for a maximum period of 6 months from the date of preparation. C alib ratio n S tan d ard s Prepare six LC/MS/MS calibration standards in methanol via dilution of the 0.1 pgfmL and the 0.01 pg/mL fortification solutions. This is a typical example; additional concentrations may be prepared as needed. Initial Cone. (pgftriL) 0.1 0.1 0.1 0.01 0.01 0.01 Volume (mL) 5 -2 1 5 2 1 M uted to (mL) 100 100 100 100 100 100 Final Cone. (pg/mL) 0.005 0.002 . 0.001 0.0005 0.0002 0.0001 Store all calibration standard solutions (in 125-mL LD PE bottles) in a refrigerator at 2C to 6C for a maximum period of 6 months from the date of preparation. 2. The liver samples will not be processed to make the homogenate described in the method Section 1Z2 to 12.12. Due to limited sample available, samples will be mashedon a flat surface by handprior to extraction. i 3. The sample weight for'liver will be 0.50 g ( 0.05) and the aample volume for serum will be iOOpL The amount of 03 M TBA added to the serum sample will be 0J mL and the amount of 0.25 M sodium carixmate/sodium bicarbonate buffer added will be 1.0 mL Samples will be placed on a wristaction shaker for -2 0 min. at level 10 and then centrifuged for - 15 min ' -3000 rpm. The samples will only be filtered with 0.2 pm nylon mesh filter if- Centre A nalytical Laboratories, Inc. Page 6 o f 43 Centre Analytical Laboratories, Inc. Page 59 o f 102 C99200 C^ Vt' f* ^ ^ L-fc. c r ' ?//-0 2 Cn 0 2 0 3 OCO& 04 CO0205 C ~006 09207 C C 0208 C99209  ^ a.*?-1* Q b e s t c o p y a v a ila b le C entre Study N o.: 023-041 Ccnac-PrBKeeH*for(Xff-02?-041 rrv . . 2JL 8 g rru E iA im M A T n iita^K T ^i:-- 1- T O ^ te isiw e ^ te ^ - '. <> -' .S C : ' > -i- -I--- *Uj*M.*i*,<38 QxfodI [OlOlllL;*^V-Vv.v.'f >.-* *r,`* i l i i i L t o O ) i L' ; vK >. ; . `- V .. u U J N . % 4 .j ; > . 7 ; - P - - . - 1.: . _ . 1* *i .*.*..* *" * (f , * >1n d 3 t e a with ' 3rin*e4om 3.' i . ` n ttuytnnnw B ran^ equmieai a -. /:.. ; m seoB e ^jjijcaS . *` J S o& n W c a ih ^ $ M ^ ,J X k a or qinla*, *; \' *-S Metfc^T-Batyl E lba;'C ^n^lr.'gijm 'distiiied orHPtC ends * _ **. , . . , - i .*,**;. . t :. V%. y ^ ' *? j i ? ! ' ----- ^ *-7 Medunol, OomioW,gb* da W orHPLC grade '- ' ':YX': $f" ' S.S Scnm orU god^ftom firnvplicr .' . M TiierochemkalitimUrdi o tS.X FFOS(3MSpieUltyQ>cmicdDiYioc),inotecal*rwtight53S *3. PFOSAPM Specialty Chntiictl DhdtiooX'iBotaettiweight- 499 . hfiJtru .*;* CentreAnalytic*!Laboratories,Inc. Centre Analytical Laboratories, Inc. Page 18 of43 Page 71 o f 102 C C 0 P .1 1 B E S T COPYA V A I L A B L E ,Cntre Study N o.: 023-041 G flBPW Col No.1M P4>234m- M UVJ. *. <I *Sfj'4l ,gj SJOj'lN .y-'L i/m W i .mlLNiIgcnbcttU. .. . IQOn^Tolniairiefbikindiffl^tovtiW .^ ^ - 'L N algroe bottle. `.'S - `. i * ..** ; - ~ i oTTBAinto 1Lwb 10ring V . ; : NaOH,addstowtjr st&p&fmn&t lonpOT)..ixnt.tQvotassewftfa 8-i(U 035 M ipdiam ciri>oo*laliodnBilcj rti^ it^ . %f fffbiim^y g*f ftffi __ V -bigrtioiMtB (NiHCOJ fata a l tfnbnlmcrE&&brio*knrohimewb bib- K*'**!a .1 O * " laaaina I m L * ! ! I f a la a M ImiM a J J 'OE r . j -*>*.*. . . . . ***** o l3Jbqpam eberA K >ctarieaIataqdB d<ai> fvrairt*.'lfi .... - '. aooreditoilealitMjdjrdiiroiopttoCfcrBampK coevsTOijBB, ! ;VtokakmconUmmg 1-OOppcnPFOS, lJSp^PFO SA , &5*7ppjn pgr ; < .^ U O f^ W O S M B ) >V-: '.i'. t.11J Wagh epproaimiidy 100mgofFOS into * top ml.votaaettie f l i ^ w ^ ! M IA Bring to Tohmttwith methanolJbra.itoek itaadod ofqiprsm utd^ 1000pr <` . : (jagtaL). . ; " ' ' " " S SJL 5 DiUiwthe atockbaton with methslfi>ra W ring aondifd 1 bttouof rfm tmtftty 5ftppm, U U Dih#e working djrdl with methanol tor a workingaandari 2 lotion of : p|w .j.oppin. : '. . ' . , C entn A nalytical Laboratories, Inc. Centre Analytical Laboratories, Inc. Page 19 of43 Page 72 o f 102 r* rt *~i * o J. . i . w BESTCOPYA V A t t A B f e f r Centre Study No.: 023-041 CentrePretocoWarflQp 023 041_____ . . -Jv. -vr"i -- SSipetrte bbuaS G *..1m0JJt j^nLitiqnbtib *30 ; ' ` iiiV< fl*.y; fr.-?Tl ^ - . y ;*ml, tod^ji{D^- ** 4}Julifc.'.` . . 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Centre Analytical Laboratories, Inc. Page27 of43 Page 80 o f 102 C9 9 2 2 0 B ES T C Q FIfAM A1LA r Centre Study N o.: 023-041 ' --Ceiiae-PratiMnUJ^ 001*4)73,041_ W*fcSeren )-UXca ?-r '` ,vXSKtrcaosvssy-!, .* `I l* ' . 'v itK WT"I?' *t*r V.**# / filM .V Cio.I-112' towQn;* *S5 (. v . wc t V ;.. f5$ KaUritScran fttpeednat; LatinoVL nMGQIBj 4 offtdnliY ;k b s s $ * j& fin*)0ui - c.* ffofaL) ? <dR!.;55 WIIUbi , au-jw ;i V'llriq* . r.aofflT. LmrCw,^ :'cn-n4*;' -Ttoo-ioj.; Hi|fcam7 V r tlA .m p , J74-7< ' -L;si-m wc ;I>*=.: ?`njsj .j7i !.. .7-W 'J ... .1. . 47Wi ' 1 n..*' *, U.;" v : o . k U. ' \ . ,t * * \ V- *v A u d i a n i ft*Lflv ftr*\111')''- ^ V . . ( V .,, ...........,{ CJentre Analytical laboratories, lac. Centre Analytical Laboratories, Inc. ............. " * Page 28 of43Page 81 o f 102 C '"v n * 7 <r> * V *> a**. t BESTCOPYA V A I L A B L E r Centre Study No.: 023-041 7 Cwu-nnwocat.MQ_nni>^?,_ ^ ;___ i f L.V CentreAnalytic*!Laboratories, Inc. Centre Analytical Laboratories, Inc. Page 29 of43 Page 82 o f 102 Cv ' - t - f .-a* d ES TC O P YA V / Centre Study No.: 023-041 C enm Protocol-N e. 00P-O23-O4J- r. c Centr Analytic*! Laboratories, Inc. Centre Analytical Laboratories, Inc. Page 30 of43 Page 83 o f 102' B E S T COPYA V A I L A B L E Centre Study No.: 023-041 ^elieAeteed.N&4*42M*L. VW' . '. r***^ o-j -?:< > 1 ioi ~*_ ^ |LS ', . ' -* * P w w i y j " TW :*`r ` /- >- - : : .;.... ,M p f l^ ^ S ^ ^ ( i& k m (ifpDtaiiDBmalt) CjFnSO, - ' -. . H, ' :o^yi' rth"w?ji&BivjfhfwMHmp'f^-t :\''vr-"`!-i-n ~r r-j ;. ':.' 1 '. ...... ;}:,, ^3-3 . 3.4 BPflRR/Tg :. " ~. r``* ' ' '" !-V. . . ; 7 ; Somjpts standard: lH-lH-ZEMH p etfn o w tq '*. . .... , > t 4 ' V > 1 . , ' . .-Vi*, i ; ^ . 1 . ;44 "' ^ ,^ A^ ` .": j ~ . ------------ WS | B*' v '. ^ * ? & '%x *Z.^^^^u^JBi: '<:?'*?' 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' " i ~-' stan d a n h .`tt d tir t a 13-fl I n e a lm l a tc a g t ! cm c g ilratinns o f CTOS ^ e a B ^ ^ ' -' . 11?!;ToeachVwdciieiiniliiri ppgpf f i fr e W rf O ' .. % '. . ?* - *' ' .f/.B* M* Ur .Yl iy*--.; i ; *1 fe-'-'J !'<'.>'*' ' -WSitf' ; Mh.-i>".Va''( W.'u-.C/%3; . ;. t -. S- J Centre Analytical Laboratories, Ine. Centre Analytical Laboratories, Inc. * ' : . Page 35 o f 43 Page 88 o f 102 000228 BEST C O P Y A V A I L A B L E Centre Study No.: 023-041 --Came ProtocolNot-0QP-02J-04l- ApproximateSpikingAnioamOI(^lJbratlaB Staadirdi' 'B.WQQQBKSWIIMIMHa' JL: PFOS mfiwr iteXttiAstSlifVKIv i- i->.-Blank xazofimi t y >; V-..7V. Ar.v ODOSppm -^O JO b n B v V rrt. *-: 4 fl* 'V V 'M h B bJI'* .'.. 1 0 - . : 20 ./.J V ii'- 0.010 ppm C ' - .; 0.02Sppa. . .'-.0 .0 5 0 ppm.- - % 0 3 0 - .J # ? \.< *.*o <vi 0.100 ppm \ V* S.0 A 10*. 0350 ppm J3 p fr.Kidi / - ' V i . 0300 ppm . :- U l ^ - -*-.0.750 ppm - JO ppeiV -r";- - ^ " 130 ppm':-' , v- ;124 O bliti (Ijilli i n i lllijplji . s l'?;.- .. 1X2 Cat ppnuiimtely I gofllTerain^d^r^ 5 f e d |^|^BrtrfaM pn>cdiiwbeit ' ' -V.?' .If-' li'T: . .* -`113 Wedicghhthe'unmmnpbbdditiirecitlfyr in^tiota ardeod lpalattticema nip^uelevvi2wT^r_v; ' " '\ -. -.1 1 i L_ a_ * . . . . *a ___ *. -*v * * * . .-y\\ \ I l io Cip (heampia I vlte Sir IS tecondt. label the mpoi vialUi fee ttady number, eight. BrerID,data*1maty*initial*,'- 'i o *. * ' Centre Analytical Laboratories be. C oltre Analytical Laboratories, Inc. Page 36 of 43 Page 89 o f 102 B ES T C O P Y A V A ILA B LE Centre Study No.: 023-041 *Centre!ProtocoH4or<)8P>023-Q41------- - *. WPIMrommtttBJBMIOIII M . -. -ultfSfrlftriI ' * * * '.** '* * v< " Y ` ; U J MlTBonPttroM>WCT :. . i^.Ccowfti&iBt o i Cflei r ` ' ' MA3 CoPMimiIHintion Ttrificatio o a mpletedctanaectheamfigucSv; = '-ffff 'jj?- lAff f O U J m o H r n T m ^ i m V ^ 'M M M S t M m r ~ v`; - >&?*''. ".- 15.1 Samplewat dupoted in biohnird containch, flm nabh olvcntwi* e iifdipd in ' MghBTUcontamcn-ndmed Ira pipefla waste a dispoecdinbrolcen'ilm fivrf.^^ : O locatedkibebtantaiy.' : ., '. ', . ( ; *|'.. *' ", x*t`** *. . Centre Analytical Laboratories. Inc. Centre Analytical Laboratories, Lie. Page 37 of43 000230 BEST COr Y AVAILABLE c oe study no .: 023-0 ~6eutic, PnXixolWoreP-0a3-04j------ ~ ' i S S 5 2 S $ t i 3 ^ 12.11.......... .. :1: ~ S O ? iiS f < * V :. ?z*'.'Uf-"%';.? .' - 1^1: i ^ ; : ll^ P i^ a n p la n (ht naiytial mlro|en eviK aSrua^to.' appcoximiielYi 2 hoorr^ *-- >>*, .*; :. " t to o d t alrij^ ~ ljeiB |t 1135,V ota an fi30:ioe n ^ '^ t* i-'':.: '' .r^ < V T \^ r ... . ''"Av".' - IK Attacka<X2~fiat'ivtam ^/O tvitoa 3 esytinvabdisfir jBnaf^.to amfen. * ... f \ ``\ 12 ^UbriihBat0Tb1 withthaSidy mmber. ~.* ^naroi'flwd obfmt,akbmc^ akd*,nd mlyl(i)pribriaiaitiwaxtracSoa: T ~v . 1Q 8 CapMditewrttd<matiamtralnreor*tpprmnmtely4*C m tS l5 !3 fa ? \ (^ lieltih B b ad m w d cri^ .titM M tolh tsd D ew ^ W i^ itai^ o^ S S r ^ . VoririciAinjtni^biDdr/M^ptriile. " " :' ; ' S>. . : :. * ^ v * .** - *c -t*.. '.;.v : av :*"... :** ' Ns o . ' < ; & : ? 4/ : .CentreAnalytic!Laboratories, toc.. Centre Analytical Laboratories, Inc. Page 38 of43 Page 91 o f 102 000231 BESTCOPYAVAILABtE- Centre Study No.: 023-041 -i 'CnftTrofoct No. OOP-023-041- : Liver ftr orOthttAaioiiieFluofOcbeaktlSui&clmtsftom Spectramehjr ^ . ' lltt A racTO D oni^^ 1 '' ' ' 1^.1 ETS-S-7.0, `Aodyss otU nc' S it Sped i-aeteiHPT^Elcetroi|nt> 2M JtEfflStfi Revieion ` yJw.l ' > t r . & . i y j y .^ y '. PtfiFnrf vsSs* b .' '. . . , v Y -^y ;Q Centre AnalyticalLaboratories, be. Centre Analytical Laboratories, Inc. Pege 39 of43 Page 92 o f 102 000232 BEST COPY AVAILABLE Centre Study No.: 023-041 ----- CentreProtocol No. 0QF4&-G4J- flJ yi v w i .M M k* S on op ttS td F C M h S td i ;;r c M i* std ; a r t a l ^ p p w s S S S S f ^flCwfli - . p p m - .40>" l ' ' r p p m C. lW Dty .p V sfe.V iV .: **.< ; ; ' v : v */ ^ S M W i i U *<?}&: & > * > r < i . ' * v ? ..- - i ' . i l l W i . t r : - * ..*f *. **..- rjrV .Tfe v : V,->r iV: * a-4. --- - - f - -- --- " r.- J r ^7r*''*<'*-*, . r: * , . I.,:|~ aTj" f ;--..V- ie*i - i >** > *. .. *:* w * . . , tret *.- . -aer* " 'III* 1 * 1 " * **>"' ^ a r - : r , w - A '*: * V'Wv * .J ,V * . T4*#,k *. * . rf * . . v ; %*!** ' * . . * jpL% * * * '* c ; r . ,. i-> . .J. . 4*. . .. . ... f * .-- fff, '- >rA* W* K . -.A w ii' . t t V T . .- J ttlA **. "aS * ->j.* r.'- StrS.t.-iW jr.*.. /< * V* . . i.. *. ^ -.w 2 & n K W i **\ v '* * fc% P i , - ; 4 *> v : a*. . .. 7 w 5 $ 7 S s S 5 ^ < a r iV -< :* - r * r - - 'K: ts.* ,, , .. i-.-M iw v w iw k ii #:>*ry -' ' - ^ - jdlUk. %K-> flri'm i f f ' V- % " . *1 -, i*a*'Ci*V->V'vC r ^ .'N le R r ' a***..* *> --r .l > **; *i . ". A'i* -,.V 3*U a.* A - *- -1 u a u t e M w a . e ^ v r . . . U -- K g . * , - f - . ' .......................... <.<>>,- / * *,* H -Sn. V ^ * l? .-. i .... 11.................- i . .... " `. v . V 1 i f f . l7 " rr i|IIIII J ^ r f 3 L h A H in B S OE -- iB g g M jW t f M ^ W 4 ^ t H a f c r . ... .. k^ ^ B S L . - * * * ...... . .v .^ T T W * ^ ! _ _ _ ! _______ <> ?.. W n M C liM M M m i m R S K R OE j ..J a S B L -- -- T * * = *\ * ~ .. A a c h m ftMDULOQ V * .'- 1. - . .'s ft A EancdaaofPPOS4 liwr . . I . CentreAnalyticalbpntorie. Inc. Centre Analytical Laboratories, Inc. Page 40of43 Page 93 o f 102 000233 COPbest v / S V A l l - A B t6fir-- Centre Study No.: 023-041 CentreProtocol No.00P-023-041- -- C w npo iiK l vM D L ** T 5 5 " v ,v 7 -- < p ^ ) A p p ra rin a te c w m t n t lo a s ta be e n d Ib r p n p a rio t the 4W*4 tt S t a d ^ l i b r a U o i C in r 7 > ; V i-.? '? -: .. r e o s . - ^ . . - . 45. ' . 2 9 .i 30p j * . - 1200p p b v - . w ..-, > -. Pf o s a x / 336 t l l . K U ppb'-M O O ppb - , , ... - p O s A A i - ; ~34.fi..': " 7 1 3 - .30p p b - t 200ppb > - - . P C K T O W | j p S T T 345? fi0 i ^ - 900p ^ - , r . " ^ . " - - M 3J o H r .* y , i2fi2; f iO p p b r l W p p b - , . ' .' 7 - , -a. :------- PPoSB*ir] ilO fi.' 30p p b il300ppb % .:. ` f : ' %-.-, : . , v miiir? " ril* * 1tnrarm to ' iqulvaS-i.V............. h ^ W m c tto r lirgggTwereegniktoto . * L _ _L L n ' r - A .s s s s :s 5 S ? P B B a s s s S !f f ^ s 5 ? f ^ ^ .... >.. . 'U w r ;- a i d f , matrix - .M M U ttt 119-1237 -12M MS Umir wefrf hapand : !"n * p iir -M ta iU b t* ;- 4 4 9 - 1 0 7 . .;.* * * C . > m tv J^ta StigA sL - 'a r e .* ____ 1 ^ 1 p iS | Lm r N b Babbit kapaiad a of. JM M U 114-102 V 4 .f i l i a t e la * aid ''f& fe n S . M l M taU rM K lH lU U -" O Awiftm u.wfcMDU;LOQ. :Vila ,. . a' wI et, :eIrTfSm*aUtaU iw __ i r " "V Centre Analytical Laboratories Inc. Centre Analytical Laboratories, Inc. :- ;.r..V>;.vv!v. ^ .* Page41 of43 Page 94 o f 102 000234 BST -COPY AVAILABLE Centre Study No.; 023-041 CaaticProttxoJN iW M O S M i- : y f4 -5 i ' 4 1 'VOS 41,X |i * r , C ^ t a a .. 1 ilT L .- n ( > y t> 4 n a n * > * low a d t& riff*; ' a m '" . ' . ' . m . ' i : ^' i* WQ* .lKjc SBK 'an a .*- am n w i >m o fl 3J-I0# vhw . v C anrooB : " - v . W - ; : a u rix '. S R laM ii' - b > l - /S B w I& i '. v : X S S i & t! i * n 1* ' t S E S H e S B $ > * p v $ Kw a ;''. ________ .." y - g i g - i - . ^ . .N i.'-v'-*--' V.- -vt/ > V,.- '. j vyav/- sT * W . -r i- v. Q EIM40 ,Emrina of OS flwdiLiwt CentreAnalytical Laboratories, toe Centre Analytical Laboratories, Inc. **11*14 Pige 42of43 Page 95 o f 102 000235 MWfPg BEST iOPY A V A I L A B L E Centre Study No.: 023-041 CentreProtocol Na (XJP-023-H1 ' t r t tw t: M e*ae: 'M a i mJL,T S- g g .; 'ia U 3 ' U O O ; '. TB T A l osoo 0300 0J 0 A ttO .' 0 5 0 0 SCO SCO 5 jP 0 -. - SCO SjOO SCO 300 .s e c OlSOO osoo 0 3 0 0 '. io o SCOSCO SOC - g a r r ro s iA M eo w ' M o m 'M e o w ' row io s o o a 0 J0 0 OJOOS' <<0300 0300 0300 OlSOO y USO O b J U o jo o ' 0 3 0 0 '. k'OSOO LM V ^C O ^I rs c T T U n - S r JJ6. - io o - . io * i X . s e c 's '. js s p r b ; - -r -i Al L U Oj004 " o o te 0020 S3SS-- O 0 I0 .D cw jq r C ttf H i t "' 0107 " o io i ' 0107 T io J - 0C30 0107 ' "T ra n 0107 Ti5C w THWitU praar T O X I B S riiilcew* vriwi.-j V IM ; < H i d ^ . SCO * ->i*>f?r - "~eow ' ''eft-' rt COM *; ft m : 39 SCO - se* s e i - . Q C UC . 7110 v fcL* no 110 M e ' J : '-Mi- T S T " S i .. J P Me M i 7 s*e soe .593 soe - S T " ISO "'~ i W .. 130 120 iaa S O M ~ n a r r . 29* ": ..m W " " S " B T T *90 59* . 599 54j9W9j-- .'*** - M 599 : ** l l M " ' Jl**~ 119* 119 1191 not - M *0 Sample "TT" ; Metis Aart ' ' !** . vfao afc' - aL r IB-- " W " ' TST'. K23 .A. ret - tjyrrliti *2i ij.-mML*k -i rm y r ^ -m '1 w s r i ' w * -racr ffOSIA U*** m a TS-r a Eai-- SlT.etlltlniw" ETS444 E sncta afWOSte a Um r>ii Hfu CentreAnalytkaJ Laboratories,Inc. Centre Analytical Laboratories, Inc. Page43 of43 Page 96 o f 102 000236 SEP. 6.2001 11:39AM ENVIRONMENTAL LAB 2 3E 09 C entre Study N o.: 023-041 NO. 5647 P. 2 3041BaorchD rir, Stab CoO<tiPA UML PhoMi (04)2314(02,V toW lti (114)23MM3 PROTOCOL AMENDMENT Page l o f i AmendmentNumber 1 EffectiveDote: 12/18 CentreStudyNumber:003-041 CentreProtocolNumber OOP-023-041 DESQPT1QNOFA? 1. $ 9: Experimental Dsiign SECTION AMSNPSDIQ 1. Change the last paragraph to n a d i* M ow : Moisture determination will be performedon all liver aamplei according to AOAC Officii] Method 950.46 Section B. (a), with the followingmodification!: 1. The lunple weight will be - 0.5 g. 2. The drying tin will be -12-14 hour. RATIONALE 1. At the request of the iponior, moifturn determination! will be donefor every liver sample. Due to limited samplesize, the sample weight used will be -0.5 g initead of -2 g. The drying time required far such a small sample size does nothave to be 16-18 hours, to the Mtmplet will be dried for -1 2 -1 4 hours IMPACT ONTHE SmCX 1. No negative impact on the study. Date * 1 Date Cent QAUReview Fabnarr 12.1998/1 RECEIVED TIME SEP. 6. X: 32PM Centre Analytical Laboratories, Inc. Page 97 o f 102 000237 SEP. 6.2001 II:39AM ENVIRONMENTAL LAB 2 3E 09 Centre Study No.: 023-041 NO. 5647 P. 5 CauxeStody Number Q22iL PROTOCOLAMENDMENT AnwndmwnNumber 2 BflbctlveDatr Q3/2MD1 CeaBe Protocol Nanbcr P*|Olof 1 1. | S: Staple Aaafyii* (0 2. |9 : ExperimentalDesign 3. { 1: LC/MS/M5Syitomaad OperatingConditionsCTurboIbtuprty) AMBWPBPTO 1. Chug* dielist sentencetoread theMowing: Staples Inwhichpeaks ire detected *tthe correspondingsaalyts retentiontime*hot arele u due Chelowedconcentrationof diecalibration standards (0.0001 jigfaL) willbereportedas NQCnotqusndiUble). 2. Addthefollowing: Thefollowingequations will be used far qusatitiiion ofthe samples: l.AnilytBPound(ngfthL) (peakteat - intercept)/ dope AV(mL)x samplewt(g)xl0G0ng WhetFV flnil volume,DF* dilutionfactor, BV* extraction volume.AV -aliquot Vftlumw 3Jeew w v /^ Caul, famedftiefaJJ- tv r aaalvtBtn ctri ftiaftriLn t in m nf inn anomt added(ng/mL)x 1|ig 3.Cbtnge diecomputerlilted toDellUUraSctaPI110 r a t io n a l e 1-3. Clarifybowthesamplesarequantitated andrepostedandtheinstrumentsused to acquire data. 1-3. NdnegativeImpactoa tha study. taipdiW ktatorS(u(an RECEIVED H I SEP. 6^ 1:32PM Centre Analytical Laboratories, Inc. d* Centre OAU Review kr Ot~ lila ftf **age 1 000238 C entre Study N o.: 023-041 3048 R m ard i D rin , Stato CaU*, FA U M l. FW (114)131-8031, Faohafl (114)231-1133 Centre Study N um ber 023-041 PROTOCOL AMENDMENT Amendment N um ber 2 Date o f Occurrence: 08/24/01 Page 1 o f 1 Centre Protocol N um ber OQP-023-041 DESCRIPTION OF AMENDED SECTION 1. $ 3 : SPONSOR AMENDED TO 1. Change the study director from Rochelle Robideau at 3M Environmental Technology and Safety Services to Sean Gallagher at Wildlife International, LIT}, 8S98 Commerce Drive, Eastern, MD 21601, phone: 410-822-8600, fine: 410-822-0632. 2. Change Rochelle Robideau to the Sponsor Representative. RATIONALE 1-2. By request o f Rochelle Robideau (fax dated 08/24/01 included in correspondence section o f the raw data associated with this study) IMPACT ON THE STUDY 1-2. No negative impact on the study. tb>Ui Date Incomliintig SC htuudliyf TDTitrMeActtonar CStiguna fahtuirwe * T l0\ D ate C entreQ A U Review 6 fe lC - f r i v o l Febnary 12,1998/1 Centre Analytical Laboratories, Inc. Page 99 o f 102 000239 SEP. 6. 2001 11:40AM EHV1R0JMEHTAL LAB Z 3E 09 Centre Study No.: 023-041 HO. 5647 P. 8 urn i -- iUm h si*cunep.rAmax. nau< 9U)2114032,ita u ie joi-m i 1 PROTOCOL DEVIATION DeviationNumber: 1 Dateof Occurrence: (1) 12/21/00 Cento StudyNumber 023-041 ContreProtocol Number 00P-023-O41 DESOUPTKWOFDEVIATION 1- I Amendment!: Didnotpetfaaamoiinmdetenitinatioa antiie followingeeapto became there wu no templeavailablea te extoetion: ti CsnB sJhnddlD Q ta B hbsjSu b IsJD fflw m 0007*75 459 0007920 9531 0007*79 413 0007921 9533 ! 00078*1 4*5 0007922 9535 I 0007**3 0007*15 417 - 4(9 0007924 000792* 9541 954 0007907 9503 0007937 9S7 0007911 9515 0007941 95*0 0007915 9525 0007942 ' 95*1 0007917 932* 0007943 95*2 0007911 9529 0007944 95*3 ACTIONSTAKEN sneTwhhi.! 1. Protocol deviationtoned. Recorded By/Date: IMPACTONTHBSTUDY 1. Noremit*forthemotennodetermination willbe availablefortheeeample*. ! CAL QAU Review kfu. RECEIVED TlfE SEP. 6. 1:32PM Centre Analytical Laboratories, Inc. ftbraw U .199tfl Page 100 o f 102 000240 SEP. 6.2001 11:40AM EP1R0M HTAL LAB 2 3E 09 Centre Study No.: 023-041 HO. 5647 P . 7 304SSaNarcbDrtM ,3lataCa0t|*PAlfM l. f t * 914} 231-M32,Fiwm to (114)231-1253 PROTOCOL DEVIATION Dcviitioo Number 2 DataflfOceuRCacR (1)12/21/00 Centre Stody N um ber 023-041 Cantia Protocol Number 00M23-O41 DESCRIPTIONOPDEVIATION I. 6Amendment(91* Weighedtan than- 03 gfortot moiian datemriaationon thefollowing amplebecameIt wu all ofthe taispla availablealterextraction: 0007913 0007S67 0007MO 0007927 000793 000793 CHaatIP 9520 451 4M 9 sa - 9564 9970 S a iib lil 034 030 033 &32 03 037 1. Protocol deviationlasu^d. ACTIONSTAKEN ' SOfrcritisn. 16.1 Raconfad By/Ttat- iSjl IMPACTONTHESTUDY 1. No nagativa impact became mourara wm till calculated ad the reaula did not vary Ignlflcantly bomtoe moUtnmmoltt for lanplei dutweighed-Oig. RECEIVED TI SEP. S. l:32PTI Centre Analytical Laboratories, Inc. tebemy IX tto lfl Page 101 o f 102 000241 SEP. 6.2001 11:40AM ENVIRONMENTAL LAB 2 3E 09 Centre Study No.: 023-041 NO. 5647 P . 6 SMSSMetttiSifa. State CehatPAUNL PbMM(114)231-MU,ie o fa fle 14)231.12 P R O T O C O L D E V IA T IO N Deviation Number 3 D ateof Occmrence: (1) 12/21/00, (2) 12/21/00 and 3/12/01 . Centre Study N um ber 023-041 Ceom Protocol N um ber 00P-023-O41 DESCRIPTION OPDEVIATION t. I Amendment*1; Did ra t perform m obtore detenninatioe on the M ow ing urapict becauie cbae w u no u m ple reliable after extraction: C ttttjSlB B feJD 0007177 0007939 0011423 CBb o JC 411 9373 nt 1 f Amendment#1: The ovra cem peritureftethexraiim m ddem iinatiani wa* 110*C ACTONS TABU 1-1 Protocol d e v iid o a iiiq p d r-\ Recorded Bv/D etg 3 _________________________ _ ^ IMPACT ONTHE STUDY 1. No nealt fo r the moUunc determination will be evaflablete there rem plei. 2. No negitive im pact fc i^ I^ tig a io rS i,n a ru re Date E S t e r n e i*gief/Sponeor Renw ientitiv Sunam ta Date ' ' CAL QAU Review-----------------V K - _ 000242