Document 4aEjb7kE3jDjJ2xk2yQnY0G0V

Northwest Bioanalytical _ Study No. biWBS00-145 Report No. NWBR01-155 Quantitative Determination of PFOS and Related Compounds Serum by LC/MS/MS in Human Sample Analysis Report for Protocol EPI-0016 Northwest Bioanalytical (NWB) A Division of NWT Inc. 1121 East 3900 South Salt Lake City, UT 84124 PREPARED FOR: 3M Company Corporate Occupational Medicine, Medical Department 220-3W-05 St. Paul, MN 55144 AUTHOR: Connie O. Sakashita, B.S., NWB Project Manager l_ger v L. Foltz, Ph.D., I_B Technical Director DATE: / _ / o - C) "2-- Page 1 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR01-155 QUALITY ASSURANCE STATEMENT LABORATORY: SPONSOR: Northwest Bioanalytical (NWB) A Division of NWT Inc. 1121 East 3900 South Salt Lake City, UT 84124 3M Company Corporate Occupational 220-3W-05 St. Paul, MN 55144 Medicine, Medical Department COMPOUND(S): NWB STUDY NUMBER: SPONSOR STUDY NUMBER: PFOS and Related Compounds NWBS00-145 EPI-0016 NWB STUDY TITLE: Quantitative Determination of PFOS and Related Compounds in Human Serum by LC/MS/MS The clinical study described in this report is not included within the definition of a GLP regulated nonclinical study. However, Northwest Bioanalytical conducts all studies within the guidelines of the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58), the OECD Principles of Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety of Drugs (Ordinance No. 21, PAB Notification No. 424.) The following inspections were performed by the NWB QAU per SOP. Inspection and Reporting Statement. Date of Inspection Phase of Study Date Report Sent to NW-B Proiect Manager Date Report Sent to NWB Management* 22-23 Oct 2001 22-23 Oct 2001 24 Oct 2001 15-16 Nov 2001 07-09 Jan 2002 10 Jan 2002 Standards Preparation QC Preparation Analytical Plan Sample Analysis Report Draft/Raw Data Final Report 23 Oct 2001 23 Oct 2001 24 Oct 2001 16 Nov 2001 09 Jan 2002 10 Jan 2002 31 Oct 2001 31 Oct 2001 31 Oct 2001 30 Nov 2001 .... 31 Jan 2002 31 Jan 2002 *Reports to NWB Management are issued monthly. As can reasonably be established, the methods and procedures described and the results incorporated into this final report accurately reflect the raw data. _cy L_an C'hain_B.A. Date NWB Quality Assurance Compliance Auditor Page 2 NorthwestBioanalytical COMPLIANCE STATEMENT StudyNo. NWBS00-145 ReportNo. NWBR01-155 The clinical study described in this report is not included within the definition ofa GLP regulated nonclinical study. However, to the best of our knowledge, this project was conducted in accordance with the guidelines of the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58) and according to the methods and procedures described within this report. In addition, the study followed the guidelines of the OECD Principles of Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety of Drugs (Ordinance No. 21, PAB Notification No. 424.) Any known incidents that may have affected the quality or integrity of the project or reported data is included in this report. This report represents an accurate record of the raw data. Connie O. Sakashita, B.S. Date NW'B Project Manager ) R gerL cFl.m_lcPtaDZh;rDtor Date Page 3 Northwest Bioanalytical TABLE OF CONTENTS Study No. NWBS00- !45 Report No. NWBR01-155 SIGNATURE PAGE ........................................................................................................................ 1 QUALITY ASSURANCE STATEMENT ...................................................................................... 2 COMPLIANCE STATEMENT ....................................................................................................... 3 TABLE OF CONTENTS ................................................................................................................. 4 LIST OF TABLES ........................................................................................................................... 4 LIST OF FIGURES .......................................................................................................................... 5 1. INTRODUCTION .................................................................................................................... 8 2. METHODOLOGY ............................................................................................... .................... 9 3. SAMPLE ANALYSIS ........................................................................................................... 12 4. RESULTS AND DISCUSSION ............................................................................................ 13 5. REFERENCES ...................................................................................................................... 14 6. DATA RETENTION ............................................................................................................. 15 LIST OF TABLES Table 1. Calibration Curve Summary for PFOS ........................................................................... 16 Table 2. Calibration Curve Summary for PFOA ........................................................ ,................. 17 Table 3. Calibration Curve Summary for PFHS ........................................................................... 18 Table 4. Calibration Curve Summary for PFOSAA ..................................................................... 19 Table 5. Calibration Curve Summary for PFOSA ........................................................................ 20 Table 6. Calibration Curve Summary for M556 ........................................................................... 21 Table 7. Calibration Curve Summary for M570 ........................................................................... 22 Table 8. Back-Calculated Concentrations of Calibration Standards for PFOS ........... ................. 23 Page 4 Noah,vest B ioanalytical Study No. NWBS00-145 Report No. NWBR01-155 Table 9. Back-Calculated Concentrations of Calibration Standards for PFOA ............................ 24 Table 10. Back-Calculated Concentrations of Calibration Standards for PFHS ................ i......... 25 Table 1l. Back-Calculated Concentrations of Calibration Standards for PFOSAA ..................... 26 Table 12. Back-Calculated Concentrations of Calibration Standards for PFOSA ........................ 27 Table 13. Back-Calculated Concentrations of Calibration Standards for M556 .......................... 28 Table 14. Back-Calculated Concentrations of Calibration Standards for M570 .......................... 29 Table 15. Analytical QC Summary for PFOS ............................................................................... 30 Table 16. Analytical QC Summary for PFOA ................................................. ............................. 31 Table 17. Analytical QC Summary for PFHS ............................................................................... 32 Table 18. Analytical QC Summary for PFOSAA ......................................................................... 33 Table 19. Analytical QC Summary for PFOSA ................... ......................................................... 34 Table 20. Analytical QC Summary for M556 ............................................................................... 35 Table 21. Analytical QC Summary for M570 .......... .i................................................................... 36 Table 22. Serum Study Sample Concentrations .................................................... ........................ 37 LIST OF FIGURES Figure 1. Representative Calibration Curve for PFOS ................................................................. 45 Figure 2. Representative Calibration Curve for PFOA ................... .............................................. 45 Figure 3. Representative Calibration Curve for PFHS ................................................................. 46 Figure 4. Representative Calibration Curve for PFOSAA ............................................................ 46 Figure 5. Representative Calibration Curve for PFOSA ............................................................... 47 Figure 6. Representative Calibration Curve for M556 ................................................................. 47 Figure 7. Representative Calibration Curve for M570 ................................................................. 48 ) Figure 8. Human Plasma Blank for PFOS .................................................................................... 49 Page 5 Northwest Bioanalytical Study No. NWBSO0-145 Report No. NWBR01-155 Figure 9. Human Plasma Blank [br PFOA ................................................................................... 50 Figure 10. Human Plasma Blank for PFHS .................................................................................. 51 Figure 11. Human Plasma Blank for PFOSAA ............................................................................ 52 Figure 12. Human Plasma Blank for PFOSA ............................................................................... 53 Figure 13. Human Plasma Blank for M556 .................................................................................. 54 Figure 14. Human Plasma Blank forM570 ........................................................... i...................... 55 Figure 15. Human Plasma Blank with Internal Standard (QC0) for PFOS .................................. 56 Figure 16. Human Plasma Blank with Internal Standard (QC0) for PFOA .................................. 57 Figure 17. Human Plasma Blank with Intemal Standard (QC0) for PFHS .................................. 58 Figure 18. Human Plasma Blank with Internal Standard (QC0) for PFOSAA ............................. 59 Figure 19. Human Plasma Blank with Internal Standard (QCO) for PFOSA ............................... 60 Figure 20. Human Plasma Blank with Internal Standard (QC0) for M556 .................................. 61 ) Figure 21. Human Plasma Blank with Internal Standard (QC0) for M570 .................................. 62 Figure 22. Low Standard for PFOS ............................................................................................... 63 Figure 23. Low Standard for PFOA .............................................................................................. 64 Figure 24. Low Standard for PFHS ............................................................................................... 65 Figure 25. Low Standard for PFOSAA ......................................................................................... 66 Figure 26. Low Standard for PFOSA ...... ...................................................................................... 67 Figure 27. Low Standard for M556 ............................................................................................... 68 Figure 28. Low Standard for M570 .......................... ............................................................... . ..... 69 Figure 29. High Standard for PFOS .............................................................................................. 70 Figure 30. High Standard for PFOA ............................................................................................. 71 Figure 31. High Standard for PFHS .............................................................................................. 72 i J Figure 32. High Standard for PFOSAA ........................................................................................ 73 Page 6 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR01-155 Figure 33. High Standard for PFOSA ........................................................................................... 74 Figure 34. High Standard for M556 .............................................................................................. 75 Figure 35. High Standard for M570 .............................................................................................. 76 ) Page 7 NorthwestBioanalytical StudyNo. NWBS00-145 ReportNo. NWBR01-155 Quantitative Determination of PFOS and Related Serum by LC/MS/MS Compounds in Human Sample Analysis Report for Protocol EPI-0016 1. INTRODUCTION This report summarizes the analytical results from the quantitation ofPFOS, PFOA, PFHS, PFOSAA, PFOSA, M556, and M570 in human serum samples for 3M Company (3M) in support of Protocol EPI-0016 [5.1 ]. The LC/MS/MS method for the analytes has a targeted calibration curve range of 1.00 to 500 ppb (except for M556 which has a LLOQ of 2.50 ppb). The actual calibration curve range for each analyte varies based upon the persistent levels of the analyte in the matrix. For this study, the assay exhibited the following LLOQ and ULOQ values: ) Analyte LLOQ ULOQ PFOS 3.37 ppb 413 ppb PFOA 1.44 ppb 481 ppb PFHS 1.36 ppb 522 ppb PFOSAA PFOSA 1.50 ppb 1.00 ppb 501 ppb 500 ppb M556 2.50 ppb 500 ppb M570 1.00 ppb 500 ppb The sponsor was 3M Company (Corporate Occupational Medicine, Medical Department, 220-3W-05, St. Paul, MN 55144), and the Study Director was Jeffrey H. Mandel, M.D., M.P.H. The Study Contact at 3M was Jean M. Burris. James K. Lundberg was the technical contact at 3M. The following is a list of NWB supervisory personnel involved in the completion of this work: Connie O. Sakashita, B.S. (NWB Project Manager); Patrick Bennett, M.S., M.B.A. (NWB Laboratory Director); Rodger L. Foltz, Ph.D. (NWB Technical Director). Laboratory personnel involved in the completion of this ) Page8 Northwest Bioanalytical Study No. NW13S00-145 Report No. NWBR01-155 study included Suzanne Newman, B.S. (NWB Research Scientist); Laura Stmhs, B.S. (NWB Scientist) and Anna Akrami, B.S. (NWB Associate Research Scientist). NWB SOPs and guidelines were used in the conduct of this study and were available to study personnel in electronic and/or hard copy formats. Date Study Initiated: 23-Oct-2001 Date Analyses Completed: 16-Nov-2001 The clinical study described in this report is not included within the definition of a GLP regulated nonclinical study. However, Northwest Bioanalytical conducts all studies within the guidelines of the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58), the OECD Principles of Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety of Drags (Ordinance No. 21, PAB Notification No. 424). Any changes to or deviations from the original protocol (Analytical Plan) were documented through approved protocol amendments or deviation ) memos and are retained within the raw data. 2. METFIODOLOGY The assay used for this study is reported in Northwest Bioanalytical reports NWBR00- 108 [5.2] and NWBR00-122 [5.3]. Chinese human plasma was used for the calibration curves and quality control samples. are discussed in NWBR00-122. Serum sample results obtained using plasma curves Samples for this study were received at NWB on the following date: Receipt Date 23-Oct-2001 Number of Samples Received 262 Storage Condition (except during analysis) -20 C Page 9 NorthwestBioanalytical Reference Material StudyNo. NWBS00-145 ReportNo. NWBR01-155 Analyte PFOS PFOA PFHS PFOSAA PFOSA M556 M570 THPFOS Lot Number 193 245 SE-036 617 214 NBlI3047-SD 118506-26 59909 Puri.tv Expiration Date 100% 3 l-Dec-2010 100% 100% 3 l-Dec-2010 01-Jan-2010 53.8% 31-Dec-2010 100% 31-Dec-2010 99.89% 31-Dec-2010 99.75% 31-Dec-2010 90% 31-Dec-2010 *Storeddry Source 3M 3M 3M 3M 3M 3M 3M 3M Storage Conditions Room temperature* Room temperature* -20 C Room temperature Room temperature Room temperature Room temperature Room temperature The reference material purity for PFOS, PFOSA, PFHS, and PFOA was not available prior to the conduct of this study. Therefore, the reference material purity was assumed to be 100%. 3M contracted with Centre Analytical Laboratories, Inc., in State College, Pennsylvania to determine the absolute concentration of PFOS, PFOA, and PFHS in NWB stock solutions used to prepare the analytical standards and controls used for this studies. All arrangements for purity determinations and the transfer of NWB solutions to Centre Analytical Laboratories, Inc., were performed by 3M. Based on Centre Analytical Laboratories' results, the concentrations of plasma calibrator and quality control samples were corrected using the following factors: Analyte PFOS PFOA PFHS Correction Factor 0.821 0.961 1.043 Eight or more calibration standards were prepared on the day of each run by adding I00 I.tLof blank Chinese human plasma and 400 _L of 50 mM ammonium acetate in Page 10 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR01-155 water (unadjusted pH -6.9) to 13 x 100 mm polypropylene tubes. After a brief vortex mixing, 10.0 _L of the appropriate spiking solution was added. The final calibration standard concentrations in human plasma for each analyte are listed below: Analyte PFOS PFOA PFHS PFOSAA PFOSA M556 M570 Calibration Standard Concentrations* 3.37, 4.60, 10.8, 23.1, 43.6, 84.6, 208, 331 and 413 ppb 1.44, 2.88, 10.1, 24.5, 48.5, 97.1,241,385 and 481 ppb 1.36, 2.92, 10.7, 26.4, 52.5, 104, 261,417 and 522 ppb 1.50, 3.00, 10.5, 25.5, 50.5, 101,251,401 and 501 ppb 1.00, 2.50, 10.0, 25.0, 50.0, 100, 250, 400 and 500 ppb 2.50, 10.0, 25.0, 50.0, 100, 250, 400 and 500 ppb 1.00, 2.50, 10.0, 25.0, 50.0, 100, 250, 400 and 500 ppb * The target calibration curve range is 1.00 ppb to 500 ppb (except M556 which has a LLOQ of 2.50 ppb). Each analyte has a different final curve range based upon the persistent levels of the analyte in the human plasma used. In addition, blank human plasma samples, both with and without internal standard (designated as QC0s and Blanks, respectively), were assayed in each analytical run. Analytical QCs were prepared in Chinese human plasma on November 5, 2001 and stored in a -20 C freezer. For each run, analytical QC levels were assayed in duplicate. Analyte PFOS PFOA PFHS PFOSA.A PFOSA M556 M570 QC Concentrations (ppb)* Low Medium High 5.83 126 331 4.32 144 384 4.48 156 417 4.50 151 401 4.00 150 400 4.00 150 400 4.00 150 400 * The target QC concentrations are 4.00 ppb, 150 ppb and 400 ppb. Each analyte has different QC concentrations based upon the persistent levels of the analyte in the human plasma used. The internal standard (THPFOS) was added to all serum samples (except Blanks) for a final concentration of approximately 200 ppb. Page 11 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWB R01-155 The analytical method consisted of a liquid:liquid extraction procedure followed by evaporation and reconstitution of the extract residue with 20 mM ammonium acetate in water: 20 mM ammonium acetate in methanol (30:70 v/v). The samples were analyzed by liquid chromatography/tandem mass spectrometry using an AP13000. The instrument was operated in the multiple reaction monitoring (MRM) mode under optimized conditions for PFOS, PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 detection of the negative ions formed by turboionspray ionization. 3. SAMPLE ANALYSIS PFOS, PFOA, PFHS, PFOSAA, PFOSA, M556, M570, and THPFOS chromatographic peaks were integrated using the MacQuan software (version 1.6) with a smooth factor of one. Quantitation was based upon quadratic regression analysis of weighted (1/x 2) calibration curves using area ratio vs. concentration utilizing Watson DMLIMS software (version 6.1.1.04). The samples were injected in a systematic order. 3.1. Acceptance Criteria For an analytical run to be accepted, it must have met the acceptance criteria listed below which are consistent with regulatory and industry recommendations. Calibration Curve Each run will include in duplicate calibration standards at six or more concentrations covering the lower to upper limit of quantitation. For all analytes except PFOSA and PFOSA.A, at least three-fourths of the calibration standard's back-calculated concentrations must be within + 15% (+ 20% for LLOQ) of their individual target concentrations. For PFOSA and PFOSAA, at least three-fourths of the calibration standard's back-calculated concentrations must be within + 20% (_+25% for LLOQ) of their individual target concentrations. A calibration standard will be considered an outlier if it is greater than two times the acceptance criteria for that standard. Page 12 Northwest Bioanalytical Lower Lhnit of Quantitation Study No. NWBSO0-145 Report No. NWB R0 l- 15.5 The back-calculated concentrations of at least one of the duplicate lowest points in the calibration curve must be within + 25% of the target concentration for PFOSA and PFOSAA to qualify as the LLOQ and within + 20% of the target concentration to qualify as the LLOQ for all other analytes. If this criterion is not met, the next level is subjected to the same test and the LLOQ raised accordingly. Quality Control Samples Each analytical run will include low, medium and high QC samples in duplicate. The measured concentrations of at least two-thirds of all analytical QCs must be within + 20% of their target concentrations (+ 25% for PFOSA and PFOSAA), and no two QCs at the same concentration can be outside the limit. If study samples require dilution, a dilution QC will be analyzed in triplicate for each dilution level (except for PFOSA and PFOSAA which should not be diluted with control matrix). At least two : dilution QCs at each level must be within + 20% of its target concentrations in order to accept diluted study samples at that level. The dilution QC acceptance is independent of the undiluted analytical QC acceptance. 4. RESULTS AND DISCUSSION Serum sample results obtained using plasma curves for PFOA, PFHS, PFOSAA, PFOSA, M556, and M570 did not meet NWB SOP requirements for validation. Results may vary on average up to 26% from results obtained using human serum calibration curves at some concentration levels for PFOA, PFHS, PFOSAA, M556, and M570. For PFOSA, results may vary on average up to 43% from results obtained using human serum calibration curves. These data are reported in Assay Revalidation Addendum Report NWBR00-122 1"5.3]. However, in order to obtain the lower limit of quantitation of less than 5 ppb required by the sponsor, it was necessary to use plasma calibration curves. Percent theoretical and percent bias are separate calculations determined from the mean. Therefore, due to rounding, percent theoretical plus percent bias may not equal 100.0%. Page 13 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR0I- 155 Each accepted run met the acceptance criteria set for the calibration curve points, for the lower limit ofquantitation (LLOQ) and tbr the analytical quality control (QC) samples. Run PFOS ID Result PFOA Result PFHS Result PFOSAA Result Comments 1 Accepted Accepted Accepted Accepted 2 Accepted Accepted Accepted Accepted 3 Accepted Accepted Accepted Accepted 4 N/A N/A N/A N/A Run aborted, sample preparation error 5 Accepted Accepted Accepted Accepted 6 Accepted Accepted Accepted Accepted 7 Accepted Accepted Accepted Accepted 8 Accepted Accepted Accepted Accepted N/A = not applicable Run PFOSA ID Result 1 Accepted 2 Accepted 3 Accepted 4 N/A 5 Accepted 6 Accepted 7 Accepted 8 Accepted M556 Result Accepted Accepted Accepted N/A Accepted Accepted Accepted Accepted M570 Result Accepted Accepted Accepted N/A Accepted Accepted Accepted Accepted Comments Run aborted, sample preparation error Any known circumstances N/A = not applicable that may have affected the quality or integrity of the data are included in this report. REFERENCES 3M Company Protocol EPI-O016. "Identification of Fluorochemicals in Serum from and Elderly Population in the Seattle, Washington Metropolitan Area." Page 14 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR0[-155 5.2. C. Sakashita. "Quantitative Determination of PFOS, PFOSA, PFOSAA, POAA, PFHS, M556 and M570 in Human Serum by LC/MS/MS." Assay Revalidation Report. NWB Study NWBS00-040. NWB Report NWBR00-108. January24, 2001. 5.3. C. Sakashita. "Quantitative Determination ofPFOS, PFOSA, PFOSAA, POAA, PFHS, M556 and M570 in Human Serum by LC/MS/MS." Assay Revalidation Addendum Report. NWB Study NWBS00-040. NWB Report NWBR00-122. November 20, 2001. 6. DATA RETENTION The raw data and final report for this study will be stored in the NWB Archives, 1121 East 3900 South, Salt Lake City, UT 84124 per regulations'and contract agreement. After submission of the final report to the Sponsor, remaining study samples will be stored under required conditions until confirmatiov of Sample Disposition/Return Authofizatioq is received from the Sponsor. 3M Company will be notified concerning final disposition of records at completion of contract obligations. Page 15 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR01-155 Table 1. Calibration Curve Summary for PFOS Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date 08-Nov-2001 09-Nov-2001 13-Nov-2001 14-Nov-2001 15-Nov-2001 15-Nov-2001 16-Nov-2001 Run Number 1 2 3 5 6 7 8 A 0.000000 0.000000 -0.000001 0.000000 -0.000001 -0.000001 0.000000 B 0.004611 0.004551 0.004805 0.005168 0.004975 0.004756 0.005736 C 0.001070 -0.000952 0.001604 0.001523 -0.001202 -0.001763 -0.000223 RSquared 0.9984 0.9958 0.9974 0.9917 0.9985 0.9956 0.9964 LLOQ 3.37 3.37 3.37 3.37 3.37 3.37 3.37 ULOQ 413 413 413 413 413 413 413 Mean S.D. %CV n 0.000000 0.000001 7 0.004943 0.000408 8.3 7 0.000008 0.001387 17337.5 7 0.9963 0.0023 0.2 7 A, B, and C are coefficients used to define the calibration curve. Page 16 Northwest Bioarmiytical Study No. NWBS00-145 Report No. NWBR0 l- 155 Table 2. Calibration Curve Summary for PFOA Quadratic weighted l/x_. All concentrations are expressed as ppb. Run Date 08-Nov-2001 09-Nov-2001 13-Nov-2001 14-Nov-200I 15-Nov-2001 15-Nov-2001 16-Nov-2001 Run Number 1 2 3 5 6 7 8 A 0.000001 0.000001 0.000000 -0.000001 0.000001 0.000001 0.000000 B 0.006091 0.005194 0.005054 0.005711 0.006132 0.006102 0.006771 C 0.001738 0.000808 0.000831 0.000382 -0.000212 0.000361 -0.000296 RSquared 0.9965 0.9931 0.9960 0.9966 0.9961 0.9977 0.9970 LLOQ ULO(_ 1.44 481 1.44 481 1.44 481 1.44 481 1.44 481 1.44 481 1.44 481 Mean S.D. %CV n 0.000000 0.000001 7 0.005865 0.000596 10.2 7 0.000516 0.000696 134.9 7 0.9961 0.0015 0.2 7 A, B, and C are coefficients used to define the calibration curve. Page i 7 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR01-155 Table 3. Calibration Curve Summary for PFHS Quadratic weighted l/x_. All concentrations are expressed as ppb. Run Date 08-Nov-2001 =, 09-Nov-2001 Run Number 1 2 A -0.000002 -0.000002 B 0.007829 0.008314 C R- Squared 0.000656 0.9971 ,, ,, -0.001142 0.9969 LLOQ ULOQ 1.36 522 1.36 522 13-Nov-2001 3 -0.000001 0.005315 0.000115 0.9972 1.36 522 14-Nov-2001 I i 15-Nov-2001 5 43.000001 0.006211 -0.000433 0.9960 1.36 522 6 -0.000002 0.006849 -0.001305 0.9977 1.36 522 .. ., . 15-Nov-2001 7 43.000002 0.006791 -0.000751 0.9978 1.36 522 .... | ....... " 16-Nov-2001 8 -0.000002 0.006953 0.000081 0.9986 1.36 522 Mean S.D. %CV -0.000002 0.000000 0.0 0.006895 0.000989 14.3 -0.000397 0.000719 -181.1 0.9973 0.0008 0.1 ) n 7 7 7 7 A, B, and C are coefficients used to define the calibration curve. Page 18 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR01-155 Table 4. Calibration Curve Summary for PFOSAA Quadratic weighted l/x". All concentrations are expressed as ppb. Run Date 08-Nov-2001 09-Nov-2001 ,, 13-Nov-2001 14-Nov-2001 15-Nov-200I 15-Nov-2001 16-Nov-2001 Run Number 1 2 3 5 6 7 8 A 0.000002 0.000001 -0.000001 -0.000001 0.000001 0.000002 0.000003 B C 0.004883 0.002297 0.005152 0.000251 0.010855 i-0.001647 0.010710 -0.000618 0.008626 -0.000767 0.007392 -0.001672 0.011058 -0.000963 RSquared 0.9868 0.9916 0.9963 0.9811 0.9955 0.9905 0.9960 LLOQ 1.50 1.50 1.50 1.50 1.50 1.50 1.50 ULOQ ... 501 501 501 501 501 501 501 . .... i Mean 0.000001 0.008382 -0.000446 0.9911 S.D. 0.000002 0.002659 0.001376 0.0056 %CV 200.0 31.7 -308.5 0.6 ) n 7 7 7 7 A, B, and C are coefficients used to define the calibration curve. ) Page 19 Northwest Bioanalytical Study No. NWBS00-I45 Report No. NWBR01-155 Table 5. Calibration Curve Summary for PFOSA Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date 08-Nov-2001 09-Nov-2001 13-Nov-2001 14-Nov-2001 15-Nov-2001 15-Nov-2001 16-Nov-2001 Run Number 1 2 3 5 6 7 8 A B 0.000001 0.000001 -0.000002 -0.00000l 0.000002 0.000002 0.000004 0.005637 0.005563 0.014503 0.013789 0.010415 0.010693 0.0 [4421 C 0.000591 0.001213 0.002158 0.002219 0.000499 0.000700 0.003092 RSquared 0.9955 0.9908 0.9896 0.9880 0.9971 0.9940 0.9962 LLOQ 1.00 1.00 1.00 1.00 1.00 1.00 1.00 ULOQ 500 500 500 500 500 500 500 Mean S.D. %CV 0.000001 0.000002 200.0 0.010717 0.003872 36.1 0.001496 0.001003 67.0 0.9930 0.0036 0.4 n 7 7 7 7 A, B, and C _e coefficients used to define _e calibration curve. Page 20 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR0 I- 155 Table 6. Calibration Curve Summary for M556 Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date 08-Nov-2001 09-Nov-2001 13-Nov-2001 14-Nov-2001 15-Nov-2001 15-Nov-2001 16-Nov-2001 Run Number I 2 3 5 6 7 8 A 0.000001 0.000001 0.000000 0.000000 0.000001 0.000002 0.000001 B 0.006345 0.00689/ 0.004174 ,m 0.003962 0.003844 0.003291 0.004646 C -0.000642 -0.001177 -0.002780 0.001886 -0.002125 -0.000626 -0.001463 RSquared 0.9952 0.9950 0.9942 0.9844 0.9986 0.9947 0.9970 LLOQ ULOQ 2.50 500 2.50 500 2.50 500 2.50 500 2.50 500 2.50 500 2.50 500 Mean S.D. %CV ,w 0.000001 0.000001 100.0 0.004736 0.001356 28.6 -0.000990 0.001488 -150.3 0.9942 0.0046 0.5 n 7 7 7 7 ] ,,- A, B, and C are coefficients used to def'me the calibration curve. Page 21 Northwest Bioanalytical Study No. NWBS00-| 45 Report No. NWBR.01-155 Table 7. Calibration Curve Summary for M570 Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date 08-Nov-2001 09-Nov-2001 13-Nov-2001 14-Nov-2001 15-Nov-2001 15-Nov-2001 16-Nov-2001 Run Number l 2 3 5 6 7 8 A , ,_ 0.000001 0.000001 -0.000003 -0.000002 0.000001 0.000001 0.000001 B C ,, ..... 0.007316 0.000681 0.007844 0.00 [ 194 0.015001 0.000743 0.014938 0.013060 0.001637 0.001232 0.011552 0.000705 0.016317 0.002517 RSquared 0.9969 0.9924 0.9964 0.9922 0.9940 0.9936 0.9979 LLOQ 1.00 1.00 1.00 1.00 1.00 1.00 1.00 ULOQ 500 500 500 500 500 500 500 Mean 0.000000 0.012290 0.001244 0.9948 S.D. , %CV: , n , ...... ....... 0.000002 _ 7 0.003564) 0.000663 [ 29.0 53.3 7 7 0.0023 0.2 7 ...... A, B, and C are coefficients used to define the calibration curve. Page22 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR01-155 Table 8. Back-Calculated Concentrations of Calibration Standards for PFOS Quadratic weighted l/x". All concentrations are expressed as ppb. Run Date Run 3.37 4.60 10.8 23.1 43.6 84.6 208 331 413 Number 08-Nov-200 | 1 3.44 4.54 10.9 23.0 43.8 84.8 212 326 424 3.42 4.37 10.9 24.4 43.3 77.8 213 342 393 09-Nov-2001 u 2 3.58 4.49 11.1 22.9 42.2 87.3 219 336 373 ,= 3.37 4.39 10.4 21.7 41.9 85.6 238 335 403 13-Nov-2001 3 3.57 4.80 10.8 24.9 44.1 84.8 220 338 399 3.16 4.50 10.3 22.4 41.6 81.8 215 324 410 14-Nov-2001 5 3.07 5.33 10.1 23.8 43.6 82.5 213 317 412 2.97 5.41 10.2 22.7 42.8 83.6 217 334 416 15-Nov,2001 6 3.46 4.77 10.8 24.1 40.7 85.5 208 338 426 3.24 4.51 10.7 24.1 42.0 86.3 205 325 402 15-Nov-2001 7 3.06 4.58 10.4 23.1 41.5 77.2 209 314 443 3.43 5.09 10.9 24.8 45.4 83.7 217 323 407 16-Nov-2001 8 3.63 4.32 11.6 23.8 40.6 80.8 209 328 403 t .... 3.21 4.41 11.4 24.2 44.7 78.3 206 342 425 L Mean S.D. %CV %Bias n .... 3.33 4.68 10.8 23.6 42.7 82.9 214 330 410 0.211 0.357 0.440 0.947 1.47 3.27 8.28 8.98 17.0 6.3 7.6 4.1 4.0 3.4 3.9 - 1,2 1.7 0.0 2.2 -2. I -2.0 3.9 2.7 4.1 2.9 -0.3 -0.7 14 14 14 14 14 14 14 14 14 Page 23 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR0 i- 155 Table 9. Back-Calculated Concentrations of Calibration Standards for PFOA Quadratic weighted l/x 2. All concentrations are expressed as ppb. Run Date Run 1.44 2.88 10.1 2d.5 48.5 97.1 241 385 481 Number 08-Nov-2001 1 1.56 3.08 10.1 24.5 49.1 92.3 248 373 470 09-Nov-2001 2 13-Nov-2001 3 14-Nov-2001 5 15-Nov-2001 6 15-Nov-2001 7 16-blov-2001 8 t .... 11..3711 22..7733 91.05.62 ..22..65..21 4590..44 8190.37 225551 430838 447464 1.26 2.73 9.55 22.5 47.2 97.5 266 390 472 1.60 2.90 9.74 23.8 47.7 91.7 245 377 443 1.27 2.95 9.74 26.2 50. I 96.7 252 414 488 1.44 *4.47 9.53 27.5 48.7 99.6 229 380 484 1.47 *5.21 8.81 24.9 49.4 95.7 250 401 465 1.36 2.58 9.29 24.7 43.9 101 244 375 481 1.56 2.97 11.1 25.5 48.3 99.0 247 391 475 1.58 2.90 9.72 25.0 48.9 91.9 246 385 489 1.33 2.77 9.74 26.1 50.8 95.6 238 389 470 1.54 3.12 9.94 25.5 49.2 93.0 233 390 459 '" 1.30 2.80 9.91 25.5 48.5 93.5 233 408 496 Mean S.D. %CV %Bias n 1.45 2.86 9.78 25.2 48.7 95.7 246 0.145 0.160 0.513 1.19 1.69 3.94 9.83 10.0 5.6 5.2 4.7 - 3.5 4.1 4.0 0.7 -0.7 -3.2 2.9 0.4 - 1,4 2.1 14 12 14 I4 14 14 14 I * Sample deactivated as an outlier (not included in summary statistics) 390 472 12.4 15.7 3.2 3.3 1.3 - 1.9 14 14 ,,. Page 24 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR01-155 Table I0. Back-Calculated Concentrations of Calibration Standards for PFHS Quadratic weighted l/x 2. All concentrations are expressed as ppb. Run Date 08-Nov-2001 Run Number 1 09-Nov-2001 2 ,_ 13-Nov-2001 3 14-Nov-2001 5 15-Nov-2001 6 .... 15-Nov-2001 7 1.36 2.92 1.44 1.3 ! 1.43 1.33 1.40 1.31 1.39 1.33 1.28 1.46 1.39 1.42 2.94 2.72 2.97 2.74 2.95 2.97 *4.07 *4.42 2.93 2.78 2.76 2.71 10.7 26.4 11.5 10.3 11.2 10.2 I0.1 10.6 10.6 11.I 11.2 11.4 10.1 10.7 29.2 26.6 27.3 25.2 30.1 25.5 28.5 26.6 26.9 26.1 26.3 28.5 52.5 104 261 53.3 99.8 264 49.3 99.4 260 53.6 111 282 49.8 98.2 271 51.5 100 262 50.9 103 278 51.2 93.9 304 49.7 100 262 52.7 105 263 48.9 99.0 259 ] 52.4 106 253 55.7 104 265 417 522 412 540 420 515 448 499 398 498 ] 420 509 401 536 408 521 398 523 436 533 409 507 394 516 428 538 16-Nov-2001 8 1.36 3.03 10.6 26.7 49.8 103 264 421 508 ) 1.34 2.85 i0.9 28.6 51.9 97.8 258 426 532 Mean S.D. %CV %Bias n 1.37 2.86 10.8 27.3 51.5 I01 268 416 520 0.0557 0.115 0.477 1.46 1.94 4.24 13.0 15.7 14.4 4.1 4.0 4.4 5.3 3.8 4.2 4.9 3.8 2.8 0.7 -2. I 0.9 3.4 - 1.9 -2.9 2.7 -0.2 -0.4 14 12 14 14 14 14 14 14 14 * Sample deactivated as an outlier (not included in summary statistics) -) Page 25 Northwest Bioanalytical Study No. NWBS00-145 Report No. NW/3R01-155 Table 11. Back-Calculated Concentrations of Calibration Standards Quadratic weighted l/x 2. All concentrations are expressed as ppb. for PFOSAA Run Date Run 1.50 3.00 10.5 25.5 50.5 101 251 "401 501 Number 08-Nov-2001 I 1.23 2.63 10.3 25.2 52.8 111 276 428 509 1.90 2.87 10.3 26.5 51.0 86.7 251 399 448 09-Nov-2001 2 1.62 2.88 10.8 26.6 53.8 105 266 405 451 1.51 2.63 9.67 23.7 46.8 98.0 300 416 473 13-Nov-2001 3 1.61 3.00 11.0 24.9 54.1 106 266 435 457 1.41 2.94 9.72 24.7 49.7 95.7 243 415 488 14-Nov-2001 5 1.40 *4.70 8.98 27.6 48.3 102 207 386 515 1.38 4.10 8.98 26.7 52.3 99.2 269 442 489 15-Nov-2001 6 1.49 3.11 10.4 28.9 42.5 103 261 411 525 1.49 2.95 10.6 26.8 48.9 98.9 235 401 477 15-Nov-2001 7 1.49 2.67 9.62 24.0 48.9 93.3 245 361 564 1.48 3.52 10.4 27.7 53.6 108 275 376 482 16-Nov-2001 8 1.53 2.76 10.6 28.1 53.5 101 255 411 506 1.62 2.61 10.2 25.8 52.3 91.9 251 398 488 Mean S.D. %CV %Bias n 1.51 2.97 10.1 26.2 50.6 0.153 0.420 0.629 1.57 3.31 I0.I 14.1 6.2 6.0 6.5 0.7 -1.0 -3.8 2.7 0.2 14 13 14 14 14 100 257 6.63 21.9 6.6 8.5 -1.0 2.4 14 14 406 491 22.0 31.4 5.4 6.4 1.2 -2.0 14 14 * Sample deactivated as an oudier (not included in summary statistics) Page 26 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR0 l- 155 Table 12, Back-Calculated Concentrations of Calibration Standards for PFOSA Quadratic weighted fir,". All concentrations are expressed as ppb. Run Date Run 1.00 2.50 10.0 25.0 50.0 100 250 400 500 Number 08-Nov-2001 1 0.955 2.45 9.66 23.7 51.9 100 266 396 51 l 0.992 2.91 10.0 26.0 48.4 87.5 253 413 472 09-Nov-2001 2 0.831 2.61 9.84 25.5 51.9 100 263 376 487 1.19 2.33 9.56 23.1 48.6 98.4 298 403 479 13-Nov-2001 3 1.09 2.89 10.6 25.0 56.8 108 258 446 462 0.875 2.37 8.69 23.2 46.8 91.4 231 423 480 14-Nov-2001 5 1.00 *4.45 ' 8.89 27.4 48.0 98,3 208 395 496 0.919 3.12 8.63 26.8 52.2 94.6 268 436 502 15-Nov-2001 6 1.09 2.66 10.2 25.7 49.2 100 256 400 525 0.919 2.27 10.2 25.9 47.4 100 236 406 477 15-Nov-2001 7 1.04 2.45 8.98 25.0 50.5 89.4 236 423 527 0.934 2.79 9.85 27.1 54.0 94.2 272 385 466 16-Nov-2001 8 1.10 2.66 9.95 27.6 50.7 94.7 249 397 510 0.915 2.24 9.88 25.7 51,1 94.1 237 418 494 Mean _ S.D. %CV /oBias n 0.989 2.60 9.64 25.6 50.5 96.5 252 0.101 0.274 0.610 1.45 2.75 5.29 22.0 10.2 10.5 6,3 5.7 5.4 5.5 8.7 -l.l 4.0 -3.6 2.4 1.0 -3.5 0.8 14 13 14 14 14 14 14 * Sample deactivated as an outlier (not included in summary statistics) 408 492 19.4 20.9 4.8 4.2 2.0 -1.6 14 14 Page 27 Northwest Bioanalytical Study No. NWBSO0-145 P..eport No. NWB R0 l- 155 Table 13. Back-Calculated Concentrations of Calibration Standards for M556 Quadratic weighted l/x 2. All concentrations are expressed as ppb. i Run Date Run 2.50 10.0 25.0 50.0 100 250 400 500 Number 08-Nov-2001 1 2.26 9.38 23.4 51.9 103 259 410 507 2.75 10.3 27.3 50.5 87.1 255 405 472 09-Nov-2001 2 2.65 10.1 25.8 50.2 99.3 261 389 456 2.36 9.91 23.1 46.8 97.5 291 416 494 13-Nov-2001 3 2.59 11.1 25.2 53.6 102 276 430 476 2.43 8.53 24.1 49.7 92.5 238 404 479 14-Nov-2001 5 *4.38 8.25 30.4 51.8 107 224 396 490 2.70 7.51 23.5 54.9 101 268 431 476 15-Nov-2001 6 2.48 10.I 24.7 45.5 100 257 407 515 2.52 10.0 25.1 51.0 106 252 387 480 15-Nov-2001 7 2.31 9.28 25.4 50.5 88.4 251 390 539 2.72 10.0 24.8 54.2 103 268 388 467 16-Nov-2001 '8 2.61 9.97 26.5 46.2 102 245 401 496 ) 2.34 10.5 26.9 45.1 97.5 252 421 490 Mean S.D. %CV %Bias n 2.52 9.64 25.4 50.1 99.0 257 0.167 0.964 1.92 3.18 - 6.01 16.3 6.6 10.0 7.6 6_3 6.1 6.3 0.8 -3.6 1.6 0.2 - 1.0 2.8 13 14 14 14 14 14 * Sample deactivated as an outlier (not included in summary statistics) 405 488 14.9 21.4 3.7 4.4 1.3 -2.4 14 14 Page 28 Northwest B ioanalytical Study No. NWB S00-145 Report No. NWBRO !- 155 Table 14. Back-Calculated Concentrations of Calibration Standards for M570 Quadratic weighted i/x _. All concentrations are expressed as ppb, Run Date Run 1.00 2.50 10. 0 25.0 50.0 100 250 400 500 Number 08-Nov-200 J 1 1.03 2.47 9.84 23.1 50.9 108 263 417 511 0.987 2.42 10.2 26.3 50,2 89.3 254 397 462 09-Nov-2001 2 1.11 2.52 10.1 25.9 51.4 104 264 403 443 0,925 2,27 9.96 23.2 45,4 95.9 299 411 487 13-Nov-2001 3 1.08 2.64 10.0 24.1 52.3 102 264 421 450 0.896 2.58 9.38 24.0 49.6 96.1 255 425 484 14-Nov-2001 5 0.985 *4.20 9.07 28.9 47.3 103 212 399 506 1.03 *3.85 8.56 27.0 52.2 99.8 275 424 479 15-Nov-2001 6 1.10 2.64 9.91 27.3 41.3 100 271 408 514 0.906 2.32 10.1 26.8 48.2 102 243 394 475 15-Nov-2001 7 0.930 2,33 9.10 25.1 49.4 90.7 239 373 561 1.07 2.72 9.95 26.7 52.6 105 276 382 470 16-Nov-2001 8 1.06 2.57 9.97 26.8 49.7 98.8 250 409 506 0.963 2.28 10.1 25.3 51.9 92.0 244 406 489 Mean S.D. %CV %Bias n 1.01 2.48 9.73 25.8 49.5 99.0 258 0.0736 0.155 0.499 1.69 3.13 5.60 20.7 7.3 6.3 5.1 6.6 6.3 5.7 8.0 1.0 -0.8 -2.7 3.2 -1.0 -1.0 3.2 14 12 14 14 14 14 14 * Sample deactivated as an outlier (not included in summary statistics) 405 488 15.2 30.3 3.8 6.2 1.3 -2.4 14 14 Page 29 Northwest Bioanalytical Study No. NWI3SO0.145 Report No. NWBR0t- 155 Table 15. Analytical QC Summary for PFOS All concentrations are expressed as ppb. Run Date Run Number Low QC 5.83 ppb Medium QC 126 ppb High QC 331 ppb Preparation Date 08-Nov-2001 1 05-Nov-2001 5.89 05-Nov-2001 121 05-Nov-2001 336 5.75 127 349 09-Nov-2001 2 6.63 120 338 6.50 121 333 13-Nov-2001 3 6.21 134 363 m.. 6.28 118 335 14-Nov-2001 5 5.48 108 303 5.95 114 322 15-Nov-2001 6 6.16 128 338 6.20 I 18 347 15-Nov-2001 7 5.56 114 323 / 6.11 117 355 16-Nov-2001 8 6.21 124 330 .= 6.17 120 323 Mean S.D. %CV .. %Theoretical %Bias n 6.08 0.325 5.3 104.3 4.3 .= 14 120 6.56 5.5 " 95.2 -4.8 14 335 15.3 4.6 101.2 1.2 14 Page 30 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR01-155 Table 16. Analytical QC Summary for PFOA All concentrations are expressed as ppb. Run Date Preparation Date 08-Nov-2001 Run Number 1 09-Nov-2001 2 13-Nov-2001 3 14-Nov-2001 5 15-Nov-2001 6 15-Nov-2001 7 16-Nov-2001 8 Low QC 4.32 ppb 05-Nov-2001 4.04 3.80 4.25 3.78 4.03 4.46 4.16 4.63 4.30 4.30 4.25 4.65 4.30 4.33 Medil, m QC 144 ppb 05-Nov-2001 138 141 137 138 156 141 132 135 139 136 140 139 142 131 tligh QC 384 ppb 05-Nov-2001 384 395 391 382 436 430 351 391 394 396 379 399 383 374 Mean S.D. %CV %Theoretical %Bias n 4.23 139 392 0.261 5.89 21.3 6.2 4.2 5.4 97.9 96.5 102.1 -2.1 -3.5 2.1 14 14 14 Page 31 / Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR0 I- 155 Table 17. Analytical QC Summary for PFHS All concentrations are expressed as ppb. Run Date Run Number Preparation Date 08-Nov-2001 1 09-Nov-2001 2 13-Nov-2001 3 14-Nov-2001 5 15-Nov-2001 6 15-Nov-2001 7 16-Nov-2001 8 Low QC 4.48 ppb 05-Nov-2001 4.50 4.13 4.55 4.61 *6.27 4.42 4.82 4.15 4.58 4.27 4.24 4.51 4.49 4.39 Medium QC 156 ppb 05-Nov-2001 140 146 140 142 176 144 131 143 144 129 143 149 141 144 High QC 417 ppb 05-Nov-2001 404 409 401 389 443 433 358 385 397 408 407 415 407 392 Mean S.D. %CV %Theoretical %Bias n 4.57 144 0.526 10.7 11.5 7.4 102.0 92.3 2.0 -7.7 14 14 * > +_20%deviation from theoretical 403 20.5 5.1 96.6 --, q -3.4 14 Page 32 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR01-155 Table 18. Analytical QC Summary for PFOSAA All concentrations are expressed as ppb. Run Date Run Number Low QC 4.50 ppb Medium QC 151 ppb High QC 401 ppb Preparation Date 08-Nov-2001 05-Nov-2001 05-Nov-200 I. 05-Nov-2001 1 5.01 151 392 4.35 149 419 09-Nov-2001 2 5.06 149 400 13-Nov-2001 .... 3 4.31 "3.34 145 -- .. . _ 401 150 446 4.79 149 453 14-Nov-2001 5 3.95 139 399 4.75 148 421 15-Nov-2001 6 5.03 159 443 4.32 149 398 15-Nov-2001 7 4.75 139 353 !) ....... 4.60 I29 395 .,, 16-Nov-2001 8 4.74 150 390 4.89 146 387 Mean S.D. %CV %Theoretical %Bias n 4.56 147 0.478 7.07 10.5 4.8 I01.3 97.4 1.3 -2.6 14 14 ..... I * > +_.25%deviation from theoretical 407 '1 27.0 6.6 !01.5 1.5 14 .=, Page 33 Northwest Bioanalytical Study No. NWBS00-145 geport_No. NWBR0l- 155 Table 19. Analytical QC Summary for PFOSA All concentrationsare expressedas ppb. Run Date Run Number Low QC 4.00 ppb Medium QC 150 ppb High QC 400 ppb Preparation Date _ 08-Nov-2001 1 05-Nov-200 ! 05-Nov-200 ] 05-Nov-2001 3.84 149 398 4.16 149 424 09-Nov-2001 2 4.17 3.67 133 393 133 404 13-Nov-2001 3 3.09 159 446 4.22 153 427 14-Nov-2001 5 3.37 4.42 140 411 139 443 15-Nov-2001 6 4.73 3.80 151 412 142 395 15-Nov-2001 7 3.82 ,.. 3.80 131 346 121 399 16-Nov-2001 8 4.15 3.77 142 347 135 359 Mean' S.D. %CV %Theoretical %Bias n 3.93 0.420 10.7 98.3 -1.8 14 141 400 10.3 31.7 7.3 7.9 94.0 100.0 -6.0 0.0 14 14 Page 34 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR01-155 Table 20. Analytical QC Summary for M556 All concentrations are expressed as ppb. Run Date Run Number Loiv QC 4.00 ppb Medium QC 150 ppb High QC 400 ppb Preparation Date 08-Nov-200 [ 05-Nov-2001 05-Nov-2001 05-Nov-2001 1 3.80 140 396 4.02 145 432 09-Nov-2001 2 4.58 145 408 4.18 I43 414 13-Nov-2001 3 *3.07 151 470 i.. 3.41 146 436 14-Nov-2001 5 3.43 148 383 3.38 143 419 15-Nov-2001 6 *5.10 157 414 3.95 148 416 15-Nov-2001 7 3.91 148 .387 ) 4.16 138 419 16-Nov-2001 8 4.53 145 404 4.53 143 387 Mean S.D. %CV %Theoretical %Bias n 4.00 146 0.564 4.70 14.1 3.2 100.0 97.3 0.0 -2.7 14 14 *> +_20%deviation from theoretical 413 23.0 5.6 103.3 3.3 14 Page 35 Northwest Bioanalytical , Study No. NWBS00-145 Report No. NWBR01-155 Table 21. Analytical QC Summary for M570 All concentrations are expressed as ppb. , ) Run Date Preparation Date 08-Nov-2001 Run Number 1 09-Nov-2001 2 13-Nov-2001 3 14-Nov-2001 5 15-Nov-2001 6 15-Nov-2001 7 16-Nov-2001 8 Low QC 4.00 ppb 05-Nov-2001 4.07 3.86 4.55 4.20 *2.95 4.32 3.83 4.49 4.49 3.74 ' 4.02 ....... 4.22 4.25 4.32 Medium QC 150 ppb 05-Nov-2001 149 146 146 140 143 149 142 146 153 147 141 132 149 144 High QC 400 ppb 05-Nov-2001 397 433 405 404 451 455 388 429 432 411 367 399 403 391 Mean S.D. %CV %Theoretical %Bias n 4.09 145 0.415 5.13 10.1 3.5 102.3 96.7 2.3 -3.3 14 14 *> +_20*/d,eviation from theoretical 412 25.0 6.1 103.0 3.0 14 Page 36 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR01-155 Table 22. Serum Study Sample Concentrations All concentrations are expressed as ppb. Sample Name 11331 11332 11333 11334 11335 11336 1!337 11338 11339 11340 11341 11342 11343 11344 11345 11346 11347 11348 11349 11350 11351 113.52 11353 11354 11355 11356 11357 11358 11359 11360 11361 11362 11363 11364 11365 11366 PFOS 33.7 28.8 44.8 1 PFOSA* II PFOSAA* I<LLOQ (1.00) 1.96 <LLOQ (l.O0) <LLOQ (1.50) <LLOQ (l.00) 3.33 PFOA* 6.20 4.73 6.16 PFHS* M556" <LLOQ (1.36) 4.50 3.99 <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) 5'I570" 1.30 1.37 2.22 12.4 .._ <LLOQ (1.00.). 1.64 2.47 <.LLOQ (1.36) <L.LOQ (2.50) 1.82 18.5 <LLOQ (1.00) <LLOQ (1.50) <LLOQ (1.44) <LLOQ (1.36) <LLOQ (2.50) <LLOQ (1.00) 25.4 .... <LLOQ (l.O0) <LLOQ (1.50) .. 2.93 29.8 <LLOQ (1.00) <LLOQ (1.50) 3.56 33.2 ..... <LLOQ (I.00!. <LLOQ (1.50) 4.03 32.3 _. <LLOQ (I.00! <LLOQ (1.50) 4.67 37.4 .., <LLOQ (l.O0) 2.41 3.96 35.3 _. <LLOQ (1.O0). 1.50 2.94 83.2 <LLOQ (1.O0) 19.0 4.69 30.8 . <LLOQ (1.oo.)<LLOQ (1.50) . 3.78 61.9 <LLOQ (1.O0) 10.7 7.35 2.67 3.23 _ 1.73 2.48 <LLOQ (1.36) 7.19 3.20 2.00 3.35 <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) 4.79 <LLOQ (2.50) 3.04 1.36 <LL()Q (1.00) 1.72 1.29 <LLOQ (1.00) <LLOQ (1.00) 3.25 <LLOQ (1.00) 2.68 54.9 <LLOQ (1.00.) 1.68 11.4 34.6 <LLOQ (1.00) <LLOQ (1.50) 4.66 5.00 <LL.OQ (2.50) 2.50 1.92 <LLOQ (2.50) 1.18 58.9 _ <LLOQ (1.00) 5.43 7.52 7.78 <LLOQ (2.50) <LL0, Q (I.00) 57.7 <LLOQ (1.00) 2.44 5.01 5.80 <LLOQ (2.50) 1.18 14.5 ... <LLOQ (I.00)_ <LLOQ (1.50) 2.84 <LLOQ (1.36) <LLOQ (2.50) 1.43 24.5 <LLOQ (1.00) <LLOQ (1.50) 4.12 1.77 <LLOQ (2.50) !.38 14.7 <LLOQ (I.00) <LLOQ (1.50) 10.6 <LLOQ (1.36) <LLOQ (2.50) 3.55 13.5 ! <LLOQ (I.00) 4.73 2.37 22.1 <LLOQ (1.00) 2.48 3.75 71.3 -' <LLOQ (1.00) I 3.80 1 12.5 48.3 <LLOQ (I.00) } 4.88 _. 4.01 59.7 <LLOQ (1.00) <LLOQ (1.50) 9.19 18.8 <LLOQ (I.00) 2.01 4.03 <.L.LOQ (1.36) :<LLOQ (2.50) 5.26 <LLOQ (2.50) 15.9 <LLOQ (1.36) 2.40 <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) 2.10 <LLOQ (2.50) <LLOQ (1.00) <LLO.Q (1.00) 2=47 1.13 1.26 1.08 25.2 <LLOQ (1.00) <LLOQ (1.50) 49.7 <LLOQ (1.00) 1.93 19.0 <LLOQ (1.00) 4.58 16.3 , <LLOQ (I.00).. <LLOQ (1.50) 95.2 <LLOQ (1.00! 17.7 133 ' <LLOQ (1.00! 16.2 49.1 <LLOQ (I.00), 5.30 104 <LLOQ (1.00) 1.95 i 39.6 <LLOQ (1.00)- / 1.63 t 1.94 6.32 4.27 2.58 8.56 16.7 5.24 9.16 5.i3 10.3 8.53 1.99 1.69 3.29 <LLOQ (1.36) .... 2.48 2.13 "" 4.42 <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) ...2.80 2.89 ] <LLoQ (2.50) <LLOQ (2.50) ,,, I<LLOQ (2.50) <LLOQ (1.00) <LLOQ (1.00) <LLOQ (1.00) [ <LLO.Q_ (1.00)_ 1.82 i149 3.76 2.74 2.97 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within +_20% (+_25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with arty individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSA.A, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 37 Northwest B ioanalytical Study No. NWBS00-145 Report No. NWBR01-155 Table 22. Serum Study Sample Concentrations All concentrations are expressed as ppb. (Continued) S:,mple Name 11367 .. 11368 11369 11370 11371 11372 11373 11374 11375 11376" 11377 11378 11379 11380 11381 _.11382 11383 11384 11385 ...1. 1386 11387 11388 ,..11389 11390 11391 11392 "I 1393 11394 11395 11396 11397 11398 11399 11400 I1401 PFOS PFOSA* PFOSAA* PFOA* PFHS* M556" _I570" 13.7 10.7 31.7 30.1 22.9 27.8 18.1 40.0 18.5 21.1 71.8 35.3 11.2 60.1 29.6 35.9 26.1 19.3 30.2 47.2 53.5 28.9 38.3 31.618.6 37.1 25.6 43.2 24.2 73.7 41.7 45.7 10.7 22.1 44.5 <LLOQ (1.00) <LLOQ (1.00) <LLOQ (1.00) <LLoQ (1.00) <LLOQ (1.00) <LLOQ (1.00) <LLOQ (I.00) <LLOQ (1.00) <LLOQ (1'.50) <LLOQ (1..50) <LLOQ (1.50) 2.13 2.25 <LLOQ (1.50) 2.19 13.8 -" 2.2"{) <LLOQ (1.44) 2.37 3.64 2.75 3.42 2.35 6.85 2.31 <LLOQ (1.36) 1.63 1.45 1.79 1.84 <LLOQ (1.36) 2.98 <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (1.00 i <LLO.Q (1.00) 2.80 1.05 1.09 1.13 1.18 3.25 <LLOQ (1.00) <LLOQ (1.00) <LLOQ (1.00) <LLOQ (1:50) <LLOQ (1.50) 2.22 <LLOQ (1.00) 3.55 <LLOQ (1.00) 1.69 <LLOQ (1.00) <LLOQ (1.50) <LLOQ (1.00) <LLOQ (1.50) <LLOQ (1.00) <LLOQ (1.50) <LLOQ (1.00) 1.81 <LLOQ (I.00) ] <LLOQ (i.50) <LLOQ (1.00) <LLOQ (1.50) <LLOQ (1.00) 8.12 <LLOQ (1.00) 2.28 <LLOQ (Ii00) 14.6 3.32 1.81 6.34 6.19 2.89 4.18 2.47 5.08 3.70 2.90 ._. 4.24 . 5.17 5.04 ..... 4.65 3.04 1.36 17.5 2.21 <LLOQ (1.36) 2.39 <LLOQ (1.36) 1.58 1.59 1.96 2.49 2.57 2.65 3.95 <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) 2.67 <LLOQ (1.00) 1.48 1.77 2.45 1.00 <LLOQ (1.00) <LLOQ (1.00) <LLOQ (1.00) 3.01 2146 <LLOQ (1.00) <LLO..Q (1.00) <LLOQ (1.00) 2.06 .... <LLOQ (1.00) <LLOQ (1.00) <LLOQ (1.00) <LLOQ (1.00) <LLOQ (I.00) <LLOQ (1.00) <LLOQ (1.00) 1.73 / -- 1.64 t <LLOQ (1.50) <LLOQ (1.5.9) <LLOQ (1.50) 2.62 5.16 " 3.82 3.44 1.86 2.45 3.20" 3.98 3.47 2.40 <LLOQ (2.50) .!.49 1.90 ,<LLOQ (2.50) <LLOQ (1.00) 2.72 <LLOQ (2.50) 1.27 1.88 <LLOQ (2.50) 1.84 1.5S <LLOQ (2.50) <LL0."(_ (I.00 i 3.63 <LLOQ (2.50) 5.69 1.87 <LLOQ (2.50) <LLOQ (l.00i _ <LLOQ (1.00) 5.62 <LLOQ (1.00) : <LLOQ (1.50) <LLOQ (1.00) 2.27 .... 6.92 4.30 5.50 8.28 <LLOQ (2.50) <LLOQ (1.00) 2.48 <LLOQ (2.50) 1.02 1.94 <LLOQ (2.50) <LLOQ (1.00) !<LLOQ (1.00) <LLOQ (i.00) <LLOQ (I.00) <LLOQ (1.50) <LLOQ (1.50) 3.24 . 2.44 3.00 5.03 <LLOQ (1.36) <LLOQ (1.36) 5.12 <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (1.00) 1.31 <LLO'Q'(t.00i" NOTE: The method acceptance criteria states that the measured concentration for each QC must be within +_20% (+_25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSA.A, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 38 Northwest Bioanalytical Study No. NWBS00-145 Report No. N_VBR0 I- 155 Table 22. Serum Study Sample Concentrations All concentrations are expressed as ppb. (Continued) 11402 11403 11404 11405 11406 11407 11408 11409 11410 11411 11412 11413 11414. 11415 11416 11417 " 11418 11419 11420 11421 .... 11422 11423. 11424 ]1425 11426 11427 11428 _. 11429 11430 11431 11432 11433 1.1434 11435 11436 .os 51.5 <LLOQ (1.00) <LLOQ (1.50) I ,,,,s. I M ,0. 6-135 9.74 <[LOQ (2.50) " t.39 2"i.7 <LLOQ (1.00) 2.94"" 4157" 1.80' <LLOQ (2.50) 2.08 29.4"" 22.3 40.6 40.6 27.0 13.8 104 25.1 .... 26.5 34.1 ....... 18.0 61.3 r<LI-OQ (1.00) !<I._LO_Q(1.50) <LLOQ (1.00) 1.74 <LLO.Q" (1.00) <LLoQ (1.50) <LLOQ (1.00) <LLOQ (1.50) <LLOQ (!.00) 2.06 <LLOQ (1.00) <L.LO.Q 0.50) <LLOQ ' (1.00) 2.57 <LLO Q (I.00.) 3.33 <LLOQ (1.00) <L_OQ.' (!.50) <LLOQ (1.00) <LLOQ (1.50) I ............. <LLOQ. (1..00), <LLOQ (1.50) <LLOQ. (!..00) 3.79 ' 2J99' 2:19 . 3:56 7.00 ,L 3"57.., 4.17 10.2 <LLO(_ (i.44) 3.14 4.44 3:84 7.53 3.42 1.43 4.57 7.00 2.46 2.22 2.33 1.7[ .8.74 1.40 6.32. 6.43 <LLOQ (2.50) <.LLOQ!I.00) <..LLOQ (2.50) 2.13 ' <LL,.O.,.Q.(2.50) <LL'(DQ (L00) <LLOQ (2.50) 1.01 <LLOQ (2.50) <LLOQ (1100) <LLO..Q (2.50) 1.13 <LLOQ (2.50) 4.05 <LL_OQ (2.50) <LLOQ (1.00) <LLOQ (2.50) 2.71 <LLOQ (2.50) <.L.LOQ,(I.00) <LLOQ (2.50) <LLOQ,(1.00) <LLOQ (2.50) <LLOQ (I.00) 22.1 .... 58.9 25.6 26.3 " <LLOQ <LLOQ <LLOQ <LLOQ (1.00) (1.00) (I.00) (1.00) <LLOQ (1.50) <LLOQ (1.50) 2.43 2.23 2.28 5.67 4.69 " 4"30' ' <LLOQ.(1:36) 17.1 2.78 1.5+ " <LLOQ (2.50) <LLOQ (2.50) _<LLOQ (2.50) )<LLOQ (2.50) 1.44 i.83 1.14 1.62 27.2 <LLOQ (I.00) <LLOQ (!.50) i " 2_'27" ' 2.02 .... <LLOQ (2.50) - ']'.95 6!.3 , <LLOQ (3.37) <LLOQ (1..00) ' 10.5 [ 8.76 .... 6.97 <LLOQ (2.50) 3.31 <LLOQ (1.00) <LLOQ (1.50) <LLOQ (1.44) <LLOQ (1.36) <LLOQ (2.50) <LLOQ (1.00) 37.3 i <LLOQ (1.00) <LLOQ(I.50) 4.90 25.4 <LLOQ (1.00) 5.31 6.62 3.52 <LLOQ (2.50) ' <LLOQ (i.00) 1.92 <LLOQ (2.50) 4.74 15.1., 25.8 41.6 29.3 29.7 <LLO(_'(I.00)'! <LLo(_(I'.'50)' 3.43 <LLOQ (1.00)_ <LLOQ (1.50) 2.64 <LLOQ (1.00)<LLOQ(I:5_0 ) .... 8.98 <LLOQ (1.00) 2.9_4 ...... 5.90 <LLOQ (1.00) <LLOQ (1.50) 4.44 <LLOQ (1.36) 6.22 2.66 1.68 4.74 <LLOQ !2.50) <LLO Q (,2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (I..00) 3.48 6.30 3.51 1.63 41.1 <LLOQ : I i00) <LLOQI(iI50) ! 4.08 2.15 <LLO =Q(2.50) <L.LOQ (I.00) 26.3 _ <LLOQ (1.00) <LLOQ (I.50) 2.56 . 1.70 <LLOQ (2.50) 3.71 114 [ <LLOQ (I.0'0) 4.6"3 ! 14.4 2.32 <LLOQ (2.50)) 3.03 48.8 l<LLOQ(I.00)'<LLOQ-(IIS0) 9.17 7..42 <LLOQ(2..5Oj) 6.i5" 30.7 <LLOQ (I.00) 24.3 <LLOQ (1.00) 1.87 .... 6.89 3.14 3.72 2.22 ..... <LLOQ (2.50) 1.16 1.59 <LLOQ (2.50) <I_LOQ (1.00) 14.6 <LLOQ (I.00) I<LLbQ (1:.5.0) 2.82 "" <LLOQ (1.36) <LLO.Q.(2.50) <LLOQ (I.00) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within +_20% (+_25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 39 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR01-155 Table 22. Serum Study Sample Concentrations All concentrations are expressed as ppb. (Continued) Sample Name PFOS 11437 11438 .[ 20.2 32.8 11439 49.9 11440 11441 11442 11443 11,_4"4 ... 11445 .....11446 11447 . ! 1448 114.4..9.... 11450 15.4 20.3 12.2 34.6 ..17.2 _/1.7 29.2 20.4 .13.4. 36.7 36.8 11451 11452 11453 11454 50.8.... 39.0 34.3 29.0 11455 27.6 __! 1456 ..11457 11458 11459 11460 16.4 138 19.0 46.1 51.6 11461 42.9 11462 175 11463 .., 9.06 11464 26.7 11465 11466 "11467 ...... 1.7.5.... 33.6 32.6 11468 11469 11470 11471 64.7 28.1 ' '"2.0 61.4 11472 28.3 PFOSA* PFOS,Uk* - <t.[OQ[([.9o) 5.89 <LLOQ (1.00) <LLOQ (1.50) <LLOQ(1.00) 8.95 <LLOQ (1.00) <LLOQ (1.50) I <LLOQ (1.00) I <LLOQ (l.50) <LLOQ (1.00)) <LLOQ (1.50) <LLOQ (1.00) 2.26 <LLOQ (1.00) <LLOQ (1.50) <LLO Q (1.00) <LLOQ (1.50) <LLOQ (1.00) <LLOQ (1.50) <LLOQ (1.00) <LLOQ (1.50) <LLOQ (1.00) <LLOQ (1.50) <LLOQ.(1.O0) 3.76 <LLOQ (I.00) <LLOQ (1.50) <L.L.OQ (1.00) <LLOQ (1.00) <L.LOQ (1.00) <LLOQ (1.00) <LLOQ (i.50) <LLOQ (1.50) 2.86 2.18 <LLOQ_(1.0_0) 1.62 <LLOQ (I.00) 2.40 <LLOQ (1.00) 21.1 <LLOQ (1.00) 1.57 <LLOQ (1.00) <LLOQ (1.50) <LLOQ(1.00) 2.81 <LLOQ <LLOQ <LLOQ <LLOQ (1.00) (1.00) !1.00) (1.00) 1.60 2.46 1.79 <LLOQ (1.50) <LLOQ (1.00) 2.00 <LLOQ (1.00) <LLOQ (1.50) <LLOQ(1.00) t.78 <LLOQ (I.00) <LLOQ (1.00) <LLOQ (1.00) <LLOQ (I.00) 2.77 1.77 <I,LOQ (1.50) 6.75 '_:LLOQ (1.00) I <LLOQ (1.50) PFOA* PFHS* M556" M570" 2.63 6.47 5.96 3.33 4.30 1.84 4.54 2.33 1.87 3.45 2.99 2.78 4.05 3.18 4.87 2.85 4.44 4.19 2.48 3.42 11.3 2.76 4.81 6.17 2.21 9.25 4.35 3.02 2.99 4.40 5.4 l 6.84 3.96 1.81 9.95 4.22 <LLOQ (1.36) <LLOQ (2150) : <LLOQ (1.00 3.22 <LLOQ (2.50) 1.55 <LLOQ'ii.36) <LLOQ(2.,5O)<LLOQ(I.00 2.05., _ <LLOQ (2.50) 1.28 2.15 <LLO.Q. (2.50) <LLOQ (!.00) 2.65 <LLOQ (2.50) .<LLOQ (1.00) 4.25 <LLOQ (2.50) 1.70 <LLOQ (1.36) <LLOQ (2.50) <LLOQ (1.00) 3.7.! ' <.LLOQ (2.50) <LLOQ (.1.00) 2.30 <LLOQ (2:.50).._.<LLOQ (1.00) <LLOQ (.1.36) <LLOQ (2.50) .<LLOQ (I.00) <LLOQ (1.36) <LLOQ (2:50) 1.18 2.69 <LLOQ (2.50) 2.86 1.72 <LLOQ (2.50) 2.58 1.80 <LLOQ (1.36) 1.47. <LLOQ (1.36) <LLO_Q..(2.50) _<.LLOQ('1.00) <LLOQ (2.50) <LLOQ (I.00) <LLOQ (2..50)...<LLOQ (1.00) <LLOQ (2.50) <LLOQ (1.00) <LLOQ (1.36) <LLOQ (2.50) 1.16 <LLOQ (1.36)i <LLOQ (1.36). <LLOQ (1.36) 5.25 1.58 <LLOQ. (2.50) <LLOQ (i'.00) 2..82 . 1.22 <LLOQ (2.50) .... 2.86 <LLOQ (2.50) <LLOQ (!.00) <LLoQ'(2.50) 1.52 5.44 <LLOQ.(2.50) 4.94 17.0 <LLOQ (2.50) 1.01. 4.90 <LLOQ (2.50) 1.02 2.74 <LLOQ (2.50) 1.71 <LLOQ (1.36i <LLOQ.(2.50) 2.00 4.23 <LLOQ (2.50) 1.75 4.0() <LLOQ (2.50) 2.81 1.59 2.16 <LLOQ (i.36) 1.64 <LLOQ (2.50) ! <LLOQ (2.5.0) <LLOQ (2.50) <LLOQ (2.50) 4.23 _..<LLCS(Q1.00) <LLOQ (1.00) 2.87 3.56 <LLOQ (2.50) <LLOQ (i.00) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within :/:20% (+_25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 40 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBRO I- 155 Table 22. Serum Study Sample Concentrations All concentrations are expressed as ppb. (Continued) S N__.m'1ne_ pie 11473 11474 11475 11476 11477 11478 11479 11480 11481 11482 11483 11484 11485 11486 11487 11488 11489 11490 11491 11492 11493 11494 11495" 11496 11497 11498 11499 11500 11501 11502 11503 11504 11505 11506 11507 11508 PFOS 32.1 27.9 27.4 18.9 38.1 47.5 28.4 48_4 26.0 . 19_7 4712 72.5 _. 3316 31.8 3713 25.2 .. 2114 2916 91.5 50.2 24.4 47.0 48.6 47.3 76.4 34.2 57.0 20.5 17.2 42.2 56. i 30.5 .... 104 44.0 .... 32.1 24.3 i PFOSt'" P FOSA._," <LL3Q (1.00) <LLOQ (1.00) <LLOQ (1.00) <LLOQ (l.00) <LLOQ (i.50) <LLOQ (1.50) <LLOQ (1.50) <LLOQ (1.50) <LLOQ (1.00) 1.96 <LLOQ (1.00) 1.61 <LLOQ (1.00) <LLOQ (i.50i" <LL0..Q (i.00) 6.49 <LLOQ (1.00) <LLOQ (i.50) <LLOQ (l.00) <LLOQ (1.00) _<LLOQ (1.00) <LLOQ (1.50) 2.50 7.66 <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ <LLOQ (1.00) (1.00) (1.00) (1.00) (1.00) (1.00) (1.00) <LLOQ (!.;50) <LLOQ (1.50) 3.40 1.68 <LLOQ (1.50) 2.67 1.85 <LLOQ (1.00) <LLOQ. (1.00) <LLOQ (1.00) <LLOQ (1.00) <LLOQ (1.50) 1.82 4.38 1.53 <LLOQ (1.00) 1.82 <LLOQ (1.0.0) <LLoQ (1:50) <LLOQ (1.00) L57 <LLOQ_ (1.00) 5.54 <LLOQ (I.00) <LLOQ (i.50) <LLOQ (1.00) <LLOQ (1.50) <LLOQ (1.00) <LLOQ (l.50) <LLOQ (1.00) 1.58 <LLOQ (l.00) <LLOQ (1.50) <LLOQ (1.0.0) 2.29 <LLO.Q. (l.00) 2. I0 <LLOQ (1.00) 2.31 <LLOQ (I.00) <LLOQ (1.50) PF O_," P F_IS" I _$56" 1_I570" 3.60 6.01 3.59 3.21 ' 2.67 3.66 5.79 <LLoQ (1.36) <LL..OQ. (2150) <LLOQ (2.50) <LLOQ (2.50) <LL'O-Q (2.'50) i.67 2.38 1.09 <LLOQ (I.00) 6.16 2.38 <LLOQ (2:50) 1.84 6.97 3.19 <LLOQ (2.50) 1.52 4.44 6.50 <LLOQ (2.50) 1.99 7.22 ..... 1.69 <LLOQ (2..50) 1.54 4.74 3.64 <LLOQ (2.50) 1.70 3.15 <LLOQ (1.36) <LLOQ (2.50) <LLOQ (1.00) 6.41 2.06 <LLOQ (2.50) 1.43 7.20 <LLOQ (1.36) 4.09 1.82 4.21 . 3.72 <LLOQ (2.50) 1.08 3.69 1.95 <LLOQ (2.50) <LLOQ (I.00) 6.65 3.21 <LLOQ (2..50) 3.39 5.40 3.78 <LL.O...Q(2.50) 1.43 3.01 <LLOQ (1.36) <LLO.Q (2.50) 1.41 7.23 <LLOQ (1.36) <LLOQ (2.50) 3.44 10.5 5.42 <LLOQ (2.50) 1.50 4.16 3.12 <LLOQ (2.50) 1.67 4.75 2.47 <LLOQ (2.50) 1.53 5.95 2.62 <LLOQ (2.50) 2.23 7.78 3.15 <LLOQ (2.50) 1.48 4.62 5.50 <LLO.Q (2.50) <LLOQ (I.00) 8.95 2.27 <LLOQ (2.50) 1.44 3.72 2.77 <LL0 .Q (2.5.0) 1.45 5.38 10.6 <LLOQ (2.50) 1.78 3.96 <I_LOQ.(1.36 ) <LLOQ (2.50) 1.60 2.21 <LLOQ (1.36) <LLOQ (2.50) <LLOQ (1.00) 7.45 2.55 <LLO...Q(2.50) 1.97 6.90 40.3 <LLOQ (2.50) 6.56 3.52 3.94 <LLOQ (2.50) 1.I0 7.81 3.85 <LLOQ (2.50) 2.08 8.07 6.92 <LLOQ (2.50) 1.90 3.89 2.21 <LLOQ (2.50) 1.01 2.57 <LLOQ.!l.36) <LLOQ (2.50) 1.49 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within +_20% (+_25% for PFOSA and PFOSA.A) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary fi'om results obtained using serum calibration curves (see Results and Discussion section). Page 41 Northwest Bioanalytical Study No. NW[3S00-145 Report No. NWBROI-155 Table 22. Serum Study Sample Concentrations All concentrations are expressed as ppb. (Continued) Sample Name 11509 .....11510 11511 11512 11513 ... 11514 11515 .... 11516 11517 11518 11519 11520 11521 11522 11523 11524 11525 11526 11527 11528 PFOS 22.9 46.7 161 54.4 14.5 20.4 26.5 37.6 49.2 8.50 19.5 25.3 18.6 35.2 28.7 20.1 23.9 49.8 15.4 31.1 11529 11530 11531 11532 [5.6 19.3 21.2 40.4 11533 25.5 11534 20.5 11535 23.2 11536 38.6 11537 11538 11539 15.4 .. 33.4 32.9 11540 15.7 I i541 24.4 11542 40.9 GHi1281 36.2 GHt 1282 18.2 PFOSA* PFOSAA* PFOA* <LLOQ (l.00) 1.59' I<LLOQ (1.00) <LLOQ...(I.00) <LLOQ(I.00) <LLOQ".(.'.I..5. 0) 5.99 <LLOQ (1.50).. <LLOQ (l.00) <LLOQ.(I,00) <LLOQ (1.00) <LLOQ (1.00) <LLOQ (1.00) 3.03 1.58 <LLOQ (i.50) <LLOQ (!:50) <LLOQ (1.50) <'I_LOQ (1.00) <LLOQ (1.50) <LLOQ (1.00) <LLOQ (1.50) <LLOQ (I.00) 1.92.. <LLOQ (t.00) 1.83 <LLOQ(1.00)<LLOQ (1.50) <LLOQ (I.00) 1.80 <LLOQ (1.00) <LLOQ (1.50) <LLOQ (1.00) <LLOQ (1.50) <LLOQ (I.00) 2.30 <LLOQ (1.00) <LLOQ (1.50) <LLoQ (1 .00) <LLOQ (1.50) '<LLOQ.I(I.O)d <LLOQ (i[50)" <LLOQ (I.00) <LLOQ (1.50) <LLOQ (1.00) <LLOQ (1.50) <LLOQ (1.00) 1.62 <LL.OQ (1.00) <LLOQ (1.00) <LLOQ (1.00) <LLOQ .(I.00) <LLOQ (1.50) <LLOQ (1.50)' <LLOQ (1.50) 1.86 , <LLOQ (1,00) <I_L_Q (I.00) <LLOQ (1.00) <LLOQ (1.50) <LLOQ (1.50) <LLOQ (1.50) <LLOQ (I.00.) <LLOQ (1.50) <LLOQ (1.00) <LLOQ (1.50) <LLOQ (1.00! <LLOQ (1.50) <LLOQ (I.00) <LLOQ (1.50) <LLOQ (1.00) 1.68 5.53 6.62 14.2 5.07 4.58 2,12 2.97 5.83 9.56 1.57 2.10 3.63 2.48 5.36 4.73 3.48 3.61 5.51 2.82 ...4....43 2.15 3.18 2.99 4.76 1.88 2.20 2.62 6.95 2.43 2.38 4.40 2.25 3.69 3.77 5.91 2.58 PFHS* M556" _I570" 2.23 <LLOQ (2.5'0) ' <LLOQ (1.00 5.35 <LLOQ (2.50) 1.13 4.61 <LLOQ (2.50) <LLOQ..(!.00 ) 3.30 <LLO.Q. (2.50) 2.87 8.03 . <LLOQ (2.50) 1.20 <LLOQ (1,36)_<_L_LOQ (2.50) 2.86 4.86 <LLOQ (2.50) 1.54 4.35 <LLOQ (2.50) 1.05 2.03 <LLOQ (2.50) 2.48 3.72 <LLOQ (2.50) <LLOQ (I,00) 2.35 <LLOQ (1.36) 1.71 <LLQQ (2.50) 1.53 <LLOQ...(2.5.0) 2.70 <LLO.Q..(2.50) <LLOQ (1.00) <LLOQ (1.36)<LLOQ (2.50) 2.39 <.I_LOQ (2.50) .. 1.37 <LLOQ (2.50) 1.38 <LLOQ(2.50) 6.41 <LLOQ (2.50) <LLOQ (1.36) <LLOQ (2.50) 3.99 <LLOQ (2.50) <LLOQ.!I.00) 1.21 <LLOQ (1.00) <LLOQ (1.00) <LLOQ (!.00) <LLOQ (1.00) 2.05 <LLOQ (1.36)<LLOQ._(2.50)<LLOQ ii'.O0) 2.71 <LLOQ (2.50) <LLOQ (1.00) <LLOQ (1.36) <LLOQ (2.50) 2.46 2.16 <LLOQ (2.50) 2.57 1.46 1.38 ... 1.49 9..60 <LLOQ.(2.50) <LLOQ (2.50) <LLOQ_(2.50) <LL.OQ..(2.50) <LLOQ (1.00) <LLOQ..(.1..00). <LLOQ (1.00) 1.26 <LLOQ (1,36) <LLOQ (1.36) 2,28 <LLOQ (2,50) <LL0(_"(2.50) <LLOQ (2.50) 1,45 ._ <LLOQ..(.!.00).. <LLOQ (1.00) <LLOQ (1.36) <LLOQ (2..50) <LLOQ (1.00) 21.8 <LLOQ (2.50) 3.10 2.68 <.LLOQ..(2.50) 2.00 3.10 <LLOQ (2.50) <LLOQ (1.36) I <LLOQ..(2.50) 2.13 . .. 2.49 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within +9_0% (+_25% tbr PFOSA and PFOSA.A) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 42 Northwest B ioanalytical Study No. NWBS00-145 Report No. NWBR01-155 Table 22. Serum Study Sample Concentrations All concentrations are expressed as ppb. (Continued) Sample Name GH11283 GH11284 GH11285 GH11286 r"GH11287 GH11288_ GH11289 GH11290 GH11291 GH11292 GH11293 GH11294 GH11295 GH11296 GHl1297 GH11298 GH11299 GH11300 GH11301 GHI1302 GH11303 "GHl1304 GH11305 GHl1306 GHI!307 GH11308 GH11309 GH11310 GH11311 GH11312 GHII313 GH11314 GHII315 GH11316 GHII317 GH11318 PFOS PFOSA* PFOSAA* PFOA* PFHS* M556" IVI570" 13.8' <LLOQ (1.00) <LLOQ (1.50) 2,29 3.37 <LLOQ (2.50) <LLOQ (i'.O0 18.7 21.1 29.4 52.0 40.5 37.7 22.7 41.3 62.6 <LLOQ (I.00) .<LLOQ (l.00) <LLOQ (1.00) .<LLOQ (1.00) <LLOQ (1.00) :<LLOQ (1.00) <.LL.O(QI.00) <LLOQ (1.00) <LLOQ (1.00) .<LLOQ (!..50) <LLO.Q (1.50) 3.09 1.74 <LLOQ (I.50) 1.81 3.25 1.54 2.09 3.60 3.82 3.69 4.55 7.41 6169 4.13 4.53 6.56 5.20 1.96 1.83 <LLOQ (1.36) 1.78 2.94 <LLOQ (1.36) 8.76 5.25 <LLOQ (2.50) 1.13 <LLOQ (2.30) 2.52,, <LLOQ (2.50) <LLOQ (1.00) <LL.0.Q (2.50) 4.24 <LLOQ (2.50) 1.78 <LLOQ (2.50) i:62 <LLOQ (2.50) <LLOQ (1.00i <LLOQ (2.50) 1.04 <LLOQ (2.50) 3.48 9.58 20.3 16.3 30.0 21.8 - <LLOQ (1.00) <LLOQ (1.00) <LLOQ (1.00) <LLOQ (1.00) <LLOQ (1.00) 5.06 <LLOQ (1.50) <LLOQ (1.50) 4.29 1.531...... 2.04 5.59 <LLOQ (1:44) 5.24 3.96 <LLOQ (1.36) 1.70 7.23 3108 <LLOQ (1.36) <LLOQ (2:50) <LLO.Q (2.50) <LLOQ (2:50) <LLOQ (2.50) <.LLOQ (2.50) <LLOQ (I.00) 1.61 2.82 1.91 <LLOQ (1.00) 54.3 <LLOQ (1.00) 1.68 6.52 2.84 <LLOQ (2.50) 4111 15.4 - '<LLOQ (I.00) <LLO_Q (i'1'50) 2.55 <LLOQ (1.36) <LLOQ (2.50) <LLOQ (I.00) 27.2 <.LLOQ(I.00) 1.77 4.28 1.85 <..LLO.(Q2.50) 1.02 27.1 <LLOQ (1.00) 2.61 6.88 3.t8 <LLOQ (2.50) 2.09 15.7 <LLOQ (1.00) <LLOQ (1..50) 3.17 <LLOQ (1.36) <LLOQ (2.50) <LLO_ (I.00) 30.5 <LLQ.Q (1.00) 1.61 3.73 <LLOQ (1.36) I<..LLOQ(2.50) <LLOQ. (1.00) 16.2 <LL..O..Q(i..00) 3..75 ..... 1.79 2.03 <LLOQ (2.50) 1.49 11.7 <LLOQ (1.00) 2.24 3.44 ..<LLOQ (1.36) <LLOQ. (2.50) 1.43 21.2 <LLOQ (1.00) <LLOQ (1.50) 3.22 <LLOQ (1.36) <LLOQ (2.50) 2.37 36.I <LLOQ (1.00) <LLOQ (1.50) 3.92 <LLOQ (1.36) <LLOQ (2.50) 1.40 35.7 <LLQ.Q. (I.00) 2.05 3.34 1.90 <.LLOQ (2.50) 2.52 21.2 .. 44.8 <LLOQ (1.00) <LLO.Q (1.50) <LLOQ (1_00) 1.64 3.04 .... 10.6 <LLOQ (2.5.0) <LLOQ (1.00) 3.50 2.01 <LLOQ (2.50) 1.77 103 <LLOQ (1.00) 7.65 13.4 <LLOQ (1.00) <LLOQ (1.50) 15.0 6.84 <.LLOQ (2:.5_0) 2.79 3.47 <LLOQ (1.36) <LLOQ (2.50) <LLOQ (1.00) 27.4 <LLOQ (1.00) <LLOQ (1...50) 4.08 26.0 <LLOQ (1.00) <LLOQ (1.50) 4.59 31.8 <LLOQ(I.00) <LLOQ(I.50) 3.81 27.1 <LLOQ (1.00) <LLOQ (1.50) 3.86 39.7 i <LLOQ (1.00) 2.06 5.33 37.2 t <LLOQ (1.00) 1.66 ..... _ 3.56 2.74 2.75 2.1i 2.78 3.90 <LLOQ (1.36) <LLO..Q.(2.50) <LLOQ (2.50) <LLOQ(2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2150) 2.12 5.07 <LLOQ(1.00) 1.59 1.75 <LLOQ (I.00) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within +_20% (+95% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sampte results for PFOA, PFHS, PFOSA.A, PFOSA,/VI556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 43 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR01-155 Table 22, Serum Study Sample Concentrations All concentrations are expressed as ppb. (Continued) Sample Name GH11319 GH11320 GH11321 GH11322 GH11323 GH11324 'GH11325 GH11326 GH11327 GH11328 GH11329 GH11330 PFOS 34.1 21.6 43.5 104 10.9 27.6 _ 17.7 45.6 69.6 36.4 12.8 27.3 PFOSA* PFOSAA* " PFOA* PFHS* 5'I556" M570" <LLOQ (1.00) <LLOQ (1.50) 4.24 <LLOQ (I.00) <LLOQ (1.50) ...... 3.91 <LLoQ (1.00) 6.67 6.96 <LLOQ (1.00) 9.85 15.4 <LLOQ (1.00) 2.94 2.!2 <LLOQ (1.00) 2.69 4.55 <LLOQ (1.00) <LLOQ (1.50) 2.96 <LLOQ (I.00) 11.1 5.89 <LLOQ (1.00) 2.37 8.38 !<LLOQ (1.00) <LLOQ (1.50) .. 3.35 <LLOQ (1.00) <LLOQ (1.50) 3.22 <LLOQ (1.00) <LLOQ (1.50) 3,03 2.55 .2.97 2.19 3.73 <LLOQ (1.36) 3.58 <LLOQ (1.36) 6.02 2.39 .. <LLOQ (1.36) <LLOQ (l.36) .1..92 <Li..OQ (2.50) <LLOQ (2.50) <LLOQ (2.50) 2.75 <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLO Q (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLOQ (2.50) <LLO Q (2.50) 1.29 <LLOQ !1.00) 1.04 1.06 <LLOQ (1.00) 1.30 1.16 2.06 <LLOQ (1.00) <LLOQ (1.00) 1.53 <LLOQ (1.00) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within _+20% (+_25%for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. ) * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 44 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWB R01-15 5 Figure 1. Representative Calibration Curve for PFOS Analytical Run 6 analyzed on 15-Nov-2001 Calibration Standards forPFOS (ppb) Regression Method = QUADRATIC - Weighting Factor = I/X**2 Quadratic Limit = 4300 2.5 E 1.0 2 _0.5 -o= 1.5 0.0 _ I 0 50 1 _ I I t I t 100 150 200 250 300 350 400 450 Nominal Cone. 3.5 3_.20.s _2.0 _1.5 _1.0 --0.5 0.0 0 Figure 2. Representative Calibration Curve for PFOA Analytical Run 6 analyzed on 15-Nov-2001 Calibration Standards forPFOA (ppb) Regression Method -- QUADRATIC - Weighting Factor ---I/X**2 Quadratic Limit = -4270 , _ I 50 100 150 200 250 300 350 400 450 500 Nominal Cone. Page 45 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR01-155 Figure 3. Representative Calibration Curve for PFHS 3.5 3.0 _2.5 ,_2.o _1.5 Analytical Run 6 analyzed on 15-Nov-2001 Calibration Standards for PFHS (ppb) Regression IVlethod = QUADRATIC - Weighting Factor = I/X**2 Quadratic Limit = 2200 0.0 0 T I I I I 100 200 300 400 500 600 Nominal Cone. Figure 4. Representative Calibration Curve for PFOSAA Analytical Run 6 analyzed on ! 5-Nov-2001 Calibration Standards for FFOSAA (ppb) Regression Method = QUADRATIC - Weighting Factor = I/X**2 Quadratic Limit = -3640 5 24 o 0 1O0 200 300 400 500 600 Nominal Cone. Page 46 Northwest Bioanalytical Study No. NWBSO0-145 Report No. NWBR01- | 55 Figure 5. Representative Calibration Curve for PFOSA Analytical Run6 analyzed on 15-Nov-2001 Calibration Standards forPFOSA(ppb) Regression Method = QUADRATIC - Weighting Factor = I/X**2 Quadratic Limit = -2180 7 0 1 _= I/ 1 i 0_ 0 50 i I i I I i i i 100 150 200 250 300 350 400 450 500 Nominal Cone. Figure 6. Representative Calibration Curve for M556 J Analytical Run6 analyzed on 15-Nov-2001 Calibration Standards for M556 (ppb) Regression Method = QUADRATIC - Weighting Factor = I/X**2 Quadratic Limit -- -23 I0 2.5 l 1.5 _0.5 0.0 _ J J i t I 1 i ; _ 0 50 1O0 150 200 250 300 350 400 450 500 Nominal Cone. Page 47 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR01-155 Figure 7. Representative Calibration Curve for M570 Analytical Run 6 analyzed on 15-Nov-2001 Calibration Standards for/Vl570 (ppb) Regression Method = QUADRATIC - Weighting Factor = I/X**2 Quadratic Limit = -I 2500 7 _k 6 g5 24 e.. _3 N 1 0_ I I I t I I l I I 0 50 100 i50 200 250 300 350 400 450 500 NominalCone. Page 48 Northwest Bioanalytical Figure 8. Human Plasma Blank for PFOS i_os I Inlem,d _l.14_l,2td]:'l-lJt_:{2_ USeAm._ C_rmm _.Lelhad N_ _,Lq _.ol 4.0 Qu4_4 Thr_ 1.0 Min. WIWIdl SI $ EAxbisstoelduteRRTeJenl$lc:0m6Time 8M_uel.l. _lWid I0200 RTWlnS'm_ 20I SGQI45010_7 t O]TSOOI4SCONTROL_BLANlff_loCommera Study No. NWBS00-145 Report No. NWBR01-155 +,.a., 3.9 Area 13561 Heir! Ilt9 .... _+./: ::?:' +: .: -._...:-'...::: :i i::._+:, :"i?+"};': ,- _o ...!i.i-.:,._:i::::_;:..!.::__:.i.::.i:2,.1:.:", ::+-:!_..:,:#i:,:;::i:;_!!fili::_;_i-'_!_i_i:ii_i2. Ime_ralio_ ',Nid_h (_32.8 Retemio_ Time 5:01 !:.:-.:i-:i:.i: 6|'_._!::I21: .. 191.;:-124,1 .301:..3611::_+421_:':._,i481 !:_i;_,4l.:_.:-EOt::_::_mn-i_ IT_PFOs use _s InternalSl_d_d ExpecledRT 4:31 Current/_th_xl J ,'_c+s+"rhre_ =o.0 Quam Thre_ 4.0 Min. W'_I.__ $ Base.Wid 100 RTWin. 25 Mull _ 10 Smo_q,_..__,_ I $0014501037 ! 037S_014$ CONTROL BLANl_oCommenl _ila,n_T,,imeo End Time 8:$9 in I _od _00,0 70 _:::..:':-i:+:::_r:ii:?!;:.!!:".i_:.:i;i:.:..:!.ii_;:i_?:_::;i!;:.':!+:.i_!:ii_;;i:i:i+__i:::iy_::_._F+i::._+:..':_ 0:00.0 I._]!l." "::' "'"..i_+";._r..!..!..:_,.. ::;. ." . "+".i'_" .::.::":: . +.. _'!,':..:_-;k._!_".:;":.".._:.;'_;::.....: -.+Tim. _.o _i ?_.,i.'_ _7! ,o ,+ ,,, +lJl + :+:,_i _ i _!+i!.:il : +,,,+ J Page 49 Northwest Bioanalytical Figure 9. Human Plasma Blank for PFOA Study No. NWBS00-145 Report No. NWBR0 I- 155 61 121 le: :41 _Ot _*1. ,121 ,4Sl _,_,l 601 .Sc_r-- 0:'_1 1:42 2:_2 3 '-_ 4:13 _,'03 5:54 6:44 7:3_ e_-"5 Page 50 Northwest Bioanalytical Figure 10. Human Plasma Blank for PFHS Study No. NWBS00-145 Report No. NWBR01-155 Page 5 [ Northwest Bioanalytical Figure 11. Human Plasma Blank for PFOSAA Study No. NWBS00-145 Report No. NWBR01-155 Page 52 Northwest Bioanalytica[ Figure 12. Human Plasma Blank for PFOSA Study No. NWBS00-145 Report No. NWBR0 I- 155 0:.(30.0 0:00.0 0:00,0 Page 53 Northwest B ioanalytical Figure 13. Human Plasma Blank for M556 Study No. NWBS00-145 Report No. NWBR01-155 Page 54 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWB R01 - 155 Figure 14. Human Plasma Blank for lVI570 pi5,"o I JnletnalSI._dald: fl4PF{_ U_ Area A_tae Relemiunlime Expe'aed RT 5:$4 C_mnl Kteth_l N,,_,_,d'_ 5.0 _uanl I_le_ 1.0 ,MMuilW.nl...__W._idWid 20S RT Win. 20 9..','.e.:_,_dl I00I _O14501037 1 037 $00_4$ CONTROL BtANl@4oCommem . _ . ,.. : .... :rI, N_'9,20013:IIAM ". :" . 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Human Plasma Blank with Internal Standard (QC0) for PFOSA Page 60 Northwest Bioanalytical Study No. NWBS00- !45 Report No. NWBR01-155 Figure 20. Human Plasma Blank with Internal Standard (QC0) for M556 Page 61 Northwest Bioanalytical Study No. NWBS00-145 Report No. NWBR0 L-155 Figure 21. Human Plasma Blank with Internal Standard (QC0) for 5'I570 Page 62 Northwest Bioanalytical Figure 22. Low Standard for PFOS Study No. NWBS00-145 Report No. NWBR0 I- 155 Page 63 Northwest Bioanalytical Figure 23. Low Standard for PFOA Study No. NWBS00-145 Report No. NWBR0 I- 155 .) , Page64 Northwest Bioanalytical Figure 24. Low Standard for PFHS Study No. NWBS00-J45 Report No. NWBR01-155 Page 65 Northwest Bioanalytical Figure 25. Low Standard for PFOSAA Study No. NWBS00-145 Report No. NWB R0 L-155 Page 66 Northwest Bioanalytical Figure 26. Low Standard for PFOSA Study No. NWBSO0-145 Report No. NWB R01-155 Page 67 Northwest Bioanalytical Figure 27. 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High Standard for PFOSA Study No. NWBS00-145 Report No. NWBR01-155 Page 74 Northwest Bioanalytical Figure 34. High Standard for M556 Study No. NWBS00-145 Report No. NWBR01-155 Page 7.5 Northwest Bioanalytical Figure 35. High Standard for 5'I570 Study No. NWBS00-145 Report No. NWB R0 l- 155 ) / Page 76