Document 2jODejYJJrZEqZ827nL93pDLp

Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Quantitative Determination of PFOS and Related Compounds in Human Serum by LC/MS/MS Sample Analysis Report for Protocol EPI-0013 Northwest Bioanalytical (NWB) A Division of NWT Ine. 1121 East 3900 South Salt Lake City, UT 84124 PREPARED FOR: 3M Company Coiporate Occupational Medicine, Medical Department 220-3W-05 St. Paul, MN 55144 AUTHOR /C -U Connie O. Sakashita, B.S., NWB Project Manager APPROVED FOR RELEASE BY: Rodger L. Foltz, Ph.D., NWM Technical Director DATE: / - 9 - 2 - DATE: /- Page 1 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 QUALITY ASSURANCE STATEMENT LABORATORY: Northwest Bioanalytical (NWB) A Division of NWT, [nc. 1121 East 3900 South Salt Lake City, UT 84124 ' SPONSOR: 3M Company Corporate Occupational Medicine, Medical Department 220-3 W-05 St. Paul, MN 55144 COMPOUND(S): PFOS, PFOA (POAA), PFHS, PFOSA, PFOSAA, M556, M570 NWB STUDY NUMBER: NWBSOO-128 SPONSOR STUDY NUMBER: EPI-0013 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 projects in accordance with 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. Inspection Date 28 Nov 2000 20-23 Mar 2001 05-06 Apr 2001 02-04 May 2001 31 Dec 2001 - 0 7 Jan 2002 09 Jan 2002 Phase of Study Analytical Plan Sample Analysis Sample Receipt QC Preparation Report Draft/ Raw Data Final Report Date Inspection Report Issued To NWB Project Manager 'NWB Manaeement 28 Nov 2000 30 Nov 2000 23 Mar 2001 31 Mar 2001 06 Apr 2001 30 Apr 2001 04 May 2001 31 May 2001 07 Jan 2002 31 Jan 2002 09 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. Sheryl A. Mathews, A.K.S. NWB QAU Compliance Auditor Jd. Date Page 2 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 COMPLIANCE STATEMENT The clinical study described in this report is not included within the definition o f a GLP regulated nonclinical study. However, to the best o f our knowledge, this project was conducted in accordance with the guidelines o f 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 o f the OECD Principles o f Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety o f Drugs (Ordinance No. 21, PAB Notification No. 424.) Any known incidents that may have affected the quality or integrity o f the project or reported data is included in this report. This report represents an accurate record o f the raw data. & 7U C U Connie O. Sakashita, B.S. NWB Project Manager / - 9- VZ-' Date NWB Technical Director Page 3 Northwest Bioanalytical TABLE OF CONTENTS Study No. NWBS00-I28 Report No. NWBRO1-066 SIGNATURE PAGE................................................................................................................................... 1 QUALITY ASSURANCE STA TEM EN T............................................................................................. 2 COMPLIANCE STATEM ENT................................................................................................................ 3 TABLE OF CONTENTS...........................................................................................................................4 LIST OF TA BLES......................................................................................................................................4 LIST OF FIGURES.....................................................................................................................................5 1. INTRODUCTION.............................................................................................................................. 8 2. METHODOLOGY.................................................................................................................. 9 3. SAMPLE A N A LY SIS.................................................................................................................... 11 4. RESULTS AND DISCUSSION.....................................................................................................13 5. REFEREN CES.................................................................................................................................19 6. DATA RETEN TIO N ...................................................................................................................... 20 LIST OF TABLES Table 1. Calibration Curve Summary for PFO S............................................... ................................. 21 Table 2. Calibration Curve Summary for PFH S........................................... -..................................... 22 Table 3. Calibration Curve Summary for P F O A ............................................................................... 23 Table 4. Calibration Curve Summary for PFO SA A ..........................................................................24 Table 5. Calibration Curve Summary for PFO SA ............................................................................. 25 Table 6. Calibration Curve Summary for M 556.................................................................................26 Table 7. Calibration Curve Summary for M 570.................................................................................27 Table 8. Back-Calculated Concentrations o f Calibration Standards for P F O S ............................ 28 Page 4 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 9. Back-Calculated Concentrations o f Calibration Standards for P F H S ..............................30 Table 10. Back-Calculated Concentrations o f Calibration Standards for PFOA............................32 Table 11. Back-Calculated Concentrations o f Calibration Standards for PFOSAA...................... 36 Table 12. Back-Calculated Concentrations o f Calibration Standards for PFOSA..........................39 Table 13. Back-Calculated Concentrations o f Calibration Standards for M 5 5 6 ............................41 Table 14. Back-Calculated Concentrations o f Calibration Standards for M 5 7 0 ............................43 Table 15. Analytical QC Summary for PFO S......................................................................................45 Table 16. Analytical QC Summary for PFH S......................................................................................48 Table 17. Analytical QC Summary for PF O A .....................................................................................51 Table 18. Analytical QC Summary for PFO SA A ............................................................................... 54 Table 19. Analytical QC Summary for PFO SA .................................................................................. 57 Table 20. Analytical QC Summary for M 556.............. 60 Table 21. Analytical QC Summary for M 570......................................................................................62 Table 22. Study Sample Concentrations............................................................................................... 65 Table 23. Repeat Analysis Table for PF O S .......................................................................................104 LIST OF FIGURES Figure 1. Representative Calibration Curve for P F O S ...................................... 105 Figure 2. Representative Calibration Curve for P F H S .....................................................................105 Figure 3. Representative Calibration Curve for PFO A .....................................................................106 Figure 4. Representative Calibration Curve for PFOSAA............................................................... 106 Figure 5. Representative Calibration Curve for PFOSA.................................................................. 107 Figure 6. Representative Calibration Curve for M556 .....................................................................107 Figure 7. Representative Calibration Curve for M 5 7 0 .....................................................................108 Page 5 Northwest Bioanalytieal Study No. NWBSOO-128 Report No. NWBROl-066 Figure 8. Human Plasma Blank for PFO S..........................................................................................109 Figure 9. Human Plasma Blank for PFH S..........................................................................................110 Figure 10. Human Plasma Blank for P F O A ..................................................................................... 111 Figure 11. Human Plasm a Blank for PFO SA A ............................................................................... 112 Figure 12. Human Plasm a Blank for PFO SA ...................................................................................113 Figure 13. Human Plasma Blank for M 556...................................................................................... 114 Figure 14. Human Plasma Blank for M 570...................................................................................... 113 Figure 15. Human Plasm a Blank with Internal Standard (QCO) for P F O S ................................ 116 Figure 16. Human Plasma Blank with Internal Standard (QCO) for P F H S ................................ 117 Figure 17. Human Plasma Blank with Internal Standard (QCO) for PFOA................................ 118 Figure 18. Human Plasm a Blank with Internal Standard (QCO) for PFOSAA...........................119 Figure 19.Human Plasm a Blank with Internal Standard (QCO) for PFO SA ..................................120 Figure 20. Human Plasm a Blank with Internal Standard (QCO) for M 5 5 6 ................................ 121 Figure 21. Human Plasm a Blank with Internal Standard (QCO) for M 5 7 0................................ 122 Figure 22. Low Standard for PFOS.................................................................................................... 123 Figure 23. Low Standard for PFHS.................................................................................................... 124 Figure 24. Low Standard for PFO A...................................................................................................123 Figure 25. Low Standard for PFOSAA..............................................................................................123 Figure 26. Low Standard for PFOSA................................................................................................. 122 Figure 27. Low Standard for M556.................................................................................................... 128 Figure 28. Low Standard for M570......................................................... 129 Figure 29. High Standard for PFOS................................................................................................... I 30 Figure 30. High Standard for PFHS................................................................................................... 121 Figure 3 1. High Standard for PF O A ..................................................................................................122 Page 6 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Figure 32. High Standardfor PFOSAA.............................................................................................. 133 Figure 33. High StandardforPFO SA ................................................................................................. 134 Figure 34. High StandardforM 556.................................................................................................... 135 Figure 35. High StandardforM 570.................................................................................................... 136 Page 7 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Quantitative Determination ofPFOS and Related Compounds in Human Serum by LC/MS/MS Sample Analysis for Protocol EPI-0013 1. IN TR O D U C TIO N This report summarizes the analytical results from the quantitation ofPFO S, PFHS, PFOA, PFOSAA, PFOSA, M556, and M570 in human serum samples for 3M Company in support o f Protocol EPI-0013 [5.1]. The LC/MS/MS method for the analytes exhibited a quadratic response and had target LLOQ and ULOQ values o f 1.00 ppb (2.50 ppb for M556) and 500 ppb for the analytes. The testing facility 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. The Study Contacts at 3M Company were Jean Burris, M.P.H, R.N., and James Lundberg, Ph.D. The following is a list o f NWB supervisory personnel involved in the completion o f this work: Connie O. Sakashita, B.S. (NWB Project Manager); Tonya Felix, M.A. (NWB Acting 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 o f this study included Suzanne Newman, B.S. (NWB Research Scientist), Toni Peacock, B.S. (NWB Assistant Scientist) and Emily Yardimci, B.S. (NWB Associate Research Scientist). NWB SOPs and guidelines were used in the conduct o f this study and were available to study personnel in electronic and hard copy formats. Date Study Initiated: 15-Nov-2000 Date Analyses Completed: 11-May-2001 The clinical study described in this report is not included within the definition o f a GLP regulated nonclinical study. However, Northwest Bioanalytical conducts all studies within the guidelines o f the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58), the OECD Principles o f Good Page 8 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety o f Drugs (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. METHODOLOGY The assay used for this study is reported in Northwest Bioanalytical reports NWBR00108 [5.2] and NWBR00-122 [5.3]. Chinese human plasma was used for the calibration curves and quality control samples. Serum sample results obtained using plasma curves are discussed in NWBR00-122. Samples for this study were received at NWB on the following dates: Receipt Date 22-NOV-2000 21-Feb-2001 06-Mar-2001 15-Mar-2001 05-Apr-2001 Number o fSamples Received 100 . 108 330 16 125 Storage Condition (except during analysis) -20 C -20 C -20 C -20 C -20 C Reference Material Analyte Lot Number Purity Expiration Source Storage Conditions Date PFOS (FC-95) 193 100% 31-Dec-2010 3M_ Room temperature* PFHS SE-036 100% 01-Jan-2010 3M -20 C PFOA (FC-143) 245 100% 31-Dec-2010 3M Room temperature* PFOSAA (FC-129) 617 53.8% 31-Dec-2010 3M Room temperature PFOSA 214 100% 31-Dec-2010 3M Room temperature M556 NB113047-8D 99.89% 31-Dec-2010 3M Room temperature M570 118506-26 99.75% 31-Dec-2010 3M Room temperature THPFOS 59909 90.0% 31-Dec-2010 3M Room temperature *Stored dry Page 9 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Eight or more calibration standards were prepared on the day o f each run by adding 100 pL o f blank human plasma and 400 pL o f 50 mM ammonium acetate in water (unadjusted pH ~6.9) to 13 x 100 mm polypropylene tubes. After a brief vortex mixing, 10.0 pL o f the appropriate spiking solution was added. The absolute purity o f PFOS, PFOSA, PFOA, and PFHS reference material was not available prior to the conduct o f 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 o f PFOS, PFHS, and PFOA in NW B stock solutions used to prepare the analytical standards and controls used for this studies. All arrangements for purity determinations and the transfer o f NWB solutions to Centre Analytical Laboratories, Inc., were performed by 3M. Based on Centre Analytical Laboratories' results, the concentrations o f plasma calibrator and quality control samples were corrected using the following factors: Analyte PFOS PFHS PFOA Correction Factor 0.836 0.909 0.855 The final calibration standard concentrations in human plasma for each analyte can be found in Tables 8 - 1 4 . NOTE: Due to the use o f different matrix pools with different persistent levels, there are several standard concentrations in these tables. However, only eight (for M556) or nine (all other analytes) standards are used for a single curve. The target calibration curve range is 1.00 ppb (2.50 ppb M556) to 500 ppb prior to correction for purity. In addition, blank plasma samples, both with and without internal standard (designated as QCOs and Blanks, respectively), were assayed in each analytical run. Analytical QCs were prepared in human plasma on October 27, 2000, March 8, 2001, April 5, 2001 and May 2, 2001 and frozen in a -20 C freezer. For each run, analytical QC levels were assayed in duplicate. In addition, for each dilution level, dilution QCs Page 10 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 were run in triplicate in any analytical run that contained diluted subject samples. The QC concentrations are shown below: Analyte PFOS PFHS PFOA PFOSAA PFOSA M556 M570 Low QC Concentrations* All concentrations are expressed as ppb. M edium High 5.75, 6.40 4.48 4.32, 4.81 4.30, 4.60 4.00 4.00 4.00 126 156,157 145 150,151 150 150 150 331,332 417,418 385 400, 401 400 400 400 Dilution DF=5 348 * The target QC concentrations are 4.00 ppb, 150 ppb and 400 ppb prior to correction for purity. Each analyte has different QC concentrations based upon the persistent levels o f the analyte in the human plasma used. The internal standard (THPFOS) was added to all plasma and serum samples (except Blanks) for a final concentration o f approximately 200 ppb. The analytical method consisted o f a liquiddiquid 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 API 3000. The instrument was operated in the multiple reaction monitoring (MRM) mode under optimized conditions for PFOS, PFHS, PFOA, PFOSAA, PFOSA, M556 and M570 detection o f the negative ions formed by TurboIonSprayTM ionization. 3. SAMPLE ANALYSIS PFOS, PFHS, PFOA, PFOSAA, PFOSA, M556, M570, and THPFOS chromatographic peaks were integrated using the MacQuan software (version 1.6) with a smooth factor o f one. Quantitation was based upon quadratic regression analysis o f weighted (1/x2) calibration curves using area ratio vs. concentration utilizing Watson DMLIMS software (version 6.1.1.04). The samples were injected in a systematic order. Page 11 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBROI-066 For sample 11689, the measured concentration o f PFOS was corrected for the persistent level o f analyte present in the dilution matrix. The concentration is reported as a whole number and has not been rounded to 3 significant figures. 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 calibration standards in duplicate at six or more concentrations covering the lower to upper limit o f quantitation. For all analytes except PFOSA and PFOSAA, at least three-fourths o f the calibration standard's back-calculated concentrations must be within 15% ( 20% for LLOQ) o f their individual target concentrations. For PFOSA and PFOSAA, at least three-fourths o f the calibration standard's back-calculated concentrations must be within 20% ( 25% for LLOQ) o f 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. Lower Limit o f Quantitation The back-calculated concentrations o f at least one o f the duplicate lowest points in the calibration curve must be within 25% o f the target concentration for PFOSA and PFOSAA to qualify as the LLOQ and within 20% o f 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 o f at least two-thirds o f all analytical QCs must be within 20% o f 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 Page 12 Northwest Bioanaiytical Study No. NWBSOO-128 Report No. NWBRO1-066 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% o f its target concentrations in order to accept diluted study samples at that level. The dilution QC acceptance is independent o f the undiluted analytical QC acceptance. 4. RESULTS AND DISCUSSION Serum sample results obtained using plasma curves for PFHS, PFOA, 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 PFHS, PFOA, 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 [5.3]. However, in order to obtain the lower limit o f quantitation o f less than 5 ppb required by the sponsor, it was necessary to use plasma calibration curves. Each accepted run met the acceptance criteria set for the calibration curve points, for the lower limit o f quantitation (LLOQ) and for the analytical quality control (QC) samples. Run Analyte Regression Extraction No. Status Date Assay Date LLOQ ULOQ 1 PFOS Accepted 27-NOV-2000 27-NOV-2000 3.94 414 1 PFOSA Accepted 27-NOV-2000 27-NOV-2000 1.00 500 1 PFOSAA Accepted 27-NOV-2000 27-NOV-2000 1.60 501 1 PFOA Accepted 27-NOV-2000 27-NOV-2000 1.92 481 1 PFHS Accepted 27-NOV-2000 27-NOV-2000 1.36 523 1 M 5 5 6 Accepted 27-NOV-2000 27-NOV-2000 2.50 500 1 M 5 7 0 Accepted 27-NOV-2000 27-NOV-2000 1.00 500 2 PFOS Accepted 27-NOV-2000 28-Nov-2000 3.94 414 2 PFOSA Accepted 27-NOV-2000 28-Nov-2000 1.00 500 2 PFOSAA Accepted 27-NOV-2000 28-Nov-2000 1.60 501 2 PFOA Accepted 27-NOV-2000 28-Nov-2000 1.92 481 2 PFHS Accepted 27-NOV-2000 28-Nov-2000 1.36 523 Comment Page 13 Northwest Bioanalytieal Study No. NWBS00-128 Report No. NW BR0I-066 Run Analyte Regression Extraction No. Status Date Assay Date LLOQ ULOQ Comment 2 M556 Accepted 27-NOV-2000 28-NOV-2000 2.50 500 2 M570 Accepted 27-NOV-2000 28-NOV-2000 1.00 500 3 PFOS - - - Run aborted due to power outage (repeated in run 6) 3 PFOSA - - - Run aborted due to power outage (repeated in run 6) 3 PFOSAA - - - Run aborted due to power outage (repeated in run 6) 3 PFOA - - - Run aborted due to power outage (repeated in run 6) 3 PFHS - - - Run aborted due to power outage (repeated in run 6) 3 M556 - - - Run aborted due to power outage (repeated in run 6) 3 M570 - - - Run aborted due to power outage (repeated in run 6) 4 PFOS Accepted 21-Mar-2001 23-Mar-2001 3.94 4 PFOSA Accepted 21-Mar-2001 23-Mar-2001 .1.00 4 PFOSAA Accepted 21-Mar-2001 23-Mar-2001 1.60 4 PFOA Accepted 21-Mar-2001 23-Mar-2001 1.92 4 PFHS Accepted 21-Mar-2001 23-Mar-2001 1.36 4 M556 Rejected 21-Mar-2001 23-Mar-2001 2.50 4 M570 Rejected 21-Mar-2001 23-Mar-2001 1.00 5 PFOS Accepted 22-Mar-2001 24-Mar-2001 3.94 5 PFOSA Accepted 22-Mar-2001 24-Mar-2001 1.00 5 PFOSAA Accepted 22-Mar-2001 24-Mar-2001 1.60 5 PFOA Accepted 22-Mar-2001 24-Mar-2001 1.92 5 PFHS Accepted 22-Mar-2001 24-Mar-2001 1.36 5 M556 Accepted 22-Mar-2001 24-Mar-2001 2.50 5 M570 Accepted 22-Mar-2001 24-Mar-2001 1.00 6 PFOS Accepted 26-Mar-2001 26-Mar-2001 4.27 6 PFOSA Accepted 26-Mar-2001 26-Mar-2001 1.40 6 PFOSAA Accepted 26-Mar-2001 26-Mar-2001 2.80 6 PFOA Accepted 26-Mar-2001 26-Mar-2001 2.11 6 PFHS Accepted 26-Mar-2001 26-Mar-2001 2.09 414 500 501 481 523 500 QCs failed 500 QCs failed 414 500 501 481 523 500 500 414 500 502 482 523 Page 14 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Run Analyte Regression No. Status 6 M556 Accepted 6 M570 Accepted 7 PFOS Accepted 7 PFOSA Accepted 7 PFOSAA Accepted 7 PFOA Accepted 7 PFHS Accepted 7 M556 Accepted 7 M570 Accepted 8 PFOS Accepted 8 PFOSA Accepted 8 PFOSAA Accepted 8 PFOA Accepted 8 PFHS Accepted 8 M556 Accepted 8 M570 Accepted 9 PFOS Accepted 9 PFOSA Accepted 9 PFOSAA Accepted 9 PFOA Accepted 9 PFHS Accepted 9 M556 Rejected 9 M570 Rejected 10 PFOS. Accepted 10 PFOSA Accepted 10 PFOSAA Accepted 10 PFOA Accepted 10 PFHS Accepted 10 M556 Accepted 10 M570 Accepted 11 PFOS Accepted 11 PFOSA Accepted 11 PFOSAA Rejected Extraction Date 26-Mar-2001 26-Mar-2001 26-Mar-200I 26-Mar-2001 26-Mar-2001 26-Mar-2001 26-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 2 8-Mar-2001 28-Mar-2001 28-Mar-2001 28-Mar-2001 28-Mar-2001 28-Mar-2001 28-Mar-2001 28-Mar-2001 28-Mar-2001 28-Mar-2001 28-Mar-2001 28-Mar-2001 30-Mar-2001 30-Mar-2001 30-Mar-2001 30-Mar-2001 30-Mar-2001 30-Mar-2001 30-Mar-2001 30-Mar-2001 30-Mar-2001 30-Mar-2001 Assay Date LLOQ ULOQ Comment 26-Mar-200l 26-Mar-2001 26-Mar-2001 26-Mar-2001 26-Mar-2001 26-Mar-2001 26-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 28-Mar-2001 28-Mar-2001 28-Mar-2001 28-Mar-2001 28-Mar-2001 28-Mar-200i 28-Mar-2001 28-Mar-2001 28-Mar-2001 28-Mar-2001 28-Mar-2001 28-Mar-2001 30-Mar-2001 30-Mar-2001 30-Mar-2001 30-Mar-200l 30-Mar-2001 30-Mar-2001 30-Mar-2001 30-Mar-2001 30-Mar-2001 30-Mar-200l 3.20 1.80 4.27 1.40 2.80 2.11 2.09 3.20 1.80 4.27 1.40 2.80 2.11 2.09 3.20 1.80 4.27 1.40 2.80 2.11 2.09 3.20 1.80 4.27 1.40 2.80 2.11 2.09 3.20 1.80 4.27 1.40 2.80 501 501 414 500 502 482 523 501 501 414 500 502 482 523 501 501 414 500 502 482 523 501 Low QCs failed 501 Curve and QC fail 414 500 502 482 523 501 501 414 500 502 Curve fails Page 15 Northwest Bioanalytical Study No. NWBS00-12S Report No. NWBRO1-066 Run Analyte Regression Extraction No. Status Date 11 PFOA Rejected 30-Mar-200l 11 PFHS Accepted 30-Mar-200l 11 M556 Accepted 30-Mar-200l 11 M570 Rejected 30-Mar-2001 12 M556 Accepted 28-Mar-2001 Assay Date LLOQ ULOQ Comment 30-Mar-2001 30-Mar-2001 30-Mar-2001 30-Mar-2001 01-Apr-2001 2.11 2.09 3.20 1.80 3.20 482 Curve fails 523 501 501 Curve fails 501 Run 12 was a reinjection o f run 9 for M556 and M570 only 12 M570 Accepted 28-Mar-2001 01-Apr-2001 1.80 501 Run 12 was a reinjection o f run 9 for M556 and M570 only 13 PFOS Accepted 13 PFOSA Accepted 13 PFOSAA Accepted 13 PFOA Accepted 13 PFHS Accepted 13 M556 Rejected 13 M570 Accepted 14 PFOS Accepted 14 PFOSA Accepted 14 PFOSAA Accepted 14 PFOA Accepted 14 PFHS Accepted 14 M556 Accepted 14 M570 Accepted 15 PFOS Accepted 15 PFOSA Accepted 15 PFOSAA Accepted 15 PFOA Accepted 15 PFHS Accepted 15 M556 Accepted 15 M570 Accepted 16 PFOS Accepted 16 PFOSA Accepted 16 PFOSAA Rejected 02-Apr-2001 02-Apr-2001 02-Apr-2001 02-Apr-2001 02-Apr-2001 02-Apr-2001 02-Apr-2001 04-Apr-2001 04-Apr-2001 04-Apr-2001 04-Apr-2001 04-Apr-2001 04-Apr-2001 04-Apr-2001 06-Apr-2001 06-Apr-2001 06-Apr-2001 06-Apr-2001 06-Apr-2001 06-Apr-2001 06-Apr-2001 09-Apr-2001 09-Apr-2001 09-Apr-2001 02-Apr-2001 02-Apr-2001 02-Apr-2001 02-Apr-2001 02-Apr-2001 02-Apr-2001 02-Apr-2001 07-Apr-2001 07-Apr-2001 07-Apr-2001 07-Apr-2001 07-Apr-2001 07-Apr-2001 07-Apr-2001 09-Apr-2001 09-Apr-2001 09-Apr-2001 09-Apr-2001 09-Apr-2001 09-Apr-2001 09-Apr-2001 11-Apr-2001 11-Apr-2001 11-Apr-2001 4.27 1.40 2.80 2.11 2.09 3.20 1.80 4.27 1.40 2.80 2.11 2.09 3.20 1.80 4.27 1.40 2.80 2.11 2.09 3.20 1.80 4.27 1.40 2.80 414 500 502 482 523 501 Low QCs failed 501 414 500 502 482 523 501 501 414 500 502 482 523 501 501 414 500 502 Curve fails Page 16 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Run Analyte Regression Extraction No. Status Date 16 PFOA Rejected 09-Apr-2001 16 PFHS Accepted 09-Apr-2001 16 M556 Rejected 09-Apr-2001 16 M570 Rejected 09-Apr-2001 17 PFOS Accepted 10-Apr-2001 17 PFOSA Accepted 10-Apr-2001 17 PFOSAA Accepted 10-Apr-2001 17 PFOA Accepted 10-Apr-2001 17 PFHS Accepted 10-Apr-2001 17 M556 Accepted 10-Apr-2001 17 M570 Accepted 10-Apr-2001 18 PFOS Accepted 19-Apr-2001 18 PFOSA Accepted 19-Apr-2001 18 PFOSAA Accepted 19-Apr-2001 18 PFOA Accepted 19-Apr-2001 18 PFHS Accepted 19-Apr-2001 18 M556 Accepted 19-Apr-2001 18 M570 Rejected 19-Apr-2001 19 PFOS Rejected 09-Apr-2001 19 PFOSA Rejected 09-Apr-2001 19 PFOSAA Accepted 19 PFOA Accepted 19 PFHS Rejected 09-Apr-2001 09-Apr-2001 09-Apr-2001 19 M556 Accepted 09-Apr-2001 19 M570 Accepted 09-Apr-2001 20 PFOS Accepted 06-Apr-2001 20 PFOSA Accepted 06-Apr-2001 Assay Date 11-Apr-2001 11-Apr-2001 11-Apr-2001 11-Apr-2001 12-Apr-2001 12-Apr-2001 12-Apr-2001 12-Apr-2001 12-Apr-2001 12-Apr-2001 12-Apr-2001 23-Apr-2001 23-Apr-2001 23-Apr-2001 23-Apr-2001 23-Apr-2001 23-Apr-2001 23-Apr-2001 14-Apr-2001 14-Apr-2001 14-Apr-2001 14-Apr-2001 14-Apr-2001 14-Apr-2001 14-Apr-2001 13-Apr-2001 13-Apr-2001 LLOQ ULOQ Comment 2.11 482 Curve fails 2.09 523 3.20 501 Curve fails 1.80 501 Curve fails 4.27 414 1.40 500 2.80 502 2.11 482 2.09 523 3.20 501 1.80 501 4.27 414 1.40 500 2.80 502 2.11 482 2.09 523 3.20 501 1.80 501 Curve and Low QC failed 4.02 414 Reinjection of run 16: Analyte results not needed 1.30 500 Reinjection of run 16: Analyte results not needed 2.80 502 Reinjection of run 16 2.11 482 Reinjection of run 16 2.09 523 Reinjection of run 16: Analyte results not needed 3.20 501 Reinjection of run 16 1.80 501 Reinjection of run 16 4.27 414 Pre-study assay evaluation (new Chinese plasma pool and QCs) 1.40 500 Pre-study assay evaluation (new Chinese plasma pool and QCs) Page 17 Northwest Bioanalytical Study No. NWBS00-I28 Report No. NWBRO1-066 Run Analyte Regression Extraction No. Status Date Assay Date LLOQ ULOQ Comment 20 PFOSAA Accepted 06-Apr-2001 13-Apr-2001 2.80 502 Pre-study assay evaluation (new Chinese plasma pool and QCs) 20 PFOA Accepted 06-Apr-2001 13-Apr-2001 2.10 482 Pre-study assay evaluation (new Chinese plasma pool and QCs) 20 PFHS Accepted 06-Apr-2001 13-Apr-200l 2.09 523 Pre-study assay evaluation (new Chinese plasma pool and QCs) 20 M556 Rejected 06-Apr-2001 13-Apr-2001 1.60 501 Pre-study assay evaluation (new Chinese plasma pool and QCs); Low QC fail. 20 M570 Accepted 06-Apr-2001 13-Apr-2001 1.90 501 Pre-study assay evaluation (new Chinese plasma pool and QCs) 21 PFOSAA Accepted 17-Apr-2001 22-Apr-2001 2.80 502 Run was analyzed for PFOSAA, PFOA and M570 only 21 PFOA Accepted 17-Apr-2001 22-Apr-2001 2.11 482 Run was analyzed for PFOSAA, PFOA and M570 only 21 M570 Accepted 17-Apr-2001 22-Apr-2001 1.80 501 Run was analyzed for PFOSAA, PFOA and M570 only 22 M570 Accepted 19-Apr-2001 24-Apr-2001 1.80 501 Reinjection o f run 18 for M570 only 23 PFOS Accepted 02-May-2001 05-May-2001 3.86 414 Pre-study assay evaluation of new low QC 23 PFOSA Accepted 02-May-2001 05-May-2001 1.50 501 Pre-study assay evaluation o f new low QC 23 PFOSAA Accepted 02-May-2001 05-May-2001 2.40 501 Pre-study assay evaluation o f new low QC 23 PFOA Accepted 02-May-2001 05-May-2001 2.31 482 Pre-study assay evaluation o f new low QC 23 PFHS Accepted 02-May-2001 05-May-2001 2.50 523 Pre-study assay evaluation o f new low QC 23 M556 Accepted 02-May-2001 05-May-2001 3.80 501 Pre-study assay evaluation of new low QC 23 M570 Accepted 02-May-2001 05-May-2001 2.30 501 Pre-study assay evaluation o f new low QC 24 PFOSAA Rejected 10-May-2001 10-May-2001 1.50 501 Sample preparation error 24 PFOA Rejected 10-May-2001 10-May-2001 25.4 482 Sample preparation error Page 18 Northwest Bioanalytical Study No. NWBS00-I28 Report No. NWBRO1-066 Run Analyte Regression Extraction No. Status Date 24 PFHS Rejected 10-May-2001 24 M570 Rejected 10-May-200l 25 PFOSAA Accepted 11-May-2001 25 PFOA Accepted 11-May-2001 25 PFHS Rejected 11-May-2001 25 M570 Accepted 11-May-2001 Assay Date LLOQ ULOQ Comment [0-May-200l 10-May-2001 11-May-2001 11-May-2001 1l-May-2001 11-May-2001 2.50 2.30 1.30 1.44 1.36 1.00 523 Sample preparation error 501 Sample preparation error 500 481 522 Analyte results not needed 500 In run 4 for PFOSA and PFOSAA, one of the medium QC samples gave extremely high results. These results appear to skew the overall statistics for these analytes. Without this "outlier", the overall %CV was 9.2% for PFOSA and 12.3% for PFOSAA. The overall %Bias was 2.0% for PFOSA and 5.3% for PFOSAA. In run 8 for PFOA, one o f the low QC samples gave an extremely low result o f 0.161 ppb. This result appears to skew the overall statistics for the analyte. Without this "outlier", the overall %CV was 14.1% and the %Bias was -10.0% / Any known circumstances that may have affected the quality or integrity of the data are included in this report. 5. REFERENCES 5.1. 3M Company Protocol EPI-0013. "Identification o f Fluorochemicals in Sera o f American Red Cross Blood Donors in the United States." September 29, 2000. 5.2. C. Sakashita. "Quantitative Determination o f PFOS, PFOSA, PFOSAA, POAA, PFHS, M556 and M570 in Human Serum by LC/MS/MS." Assay Revalidation Report. NWB Study NWBS00-040. NWB Report NW BR00-108. January 24, 2001. 5.3. C. Sakashita. "Quantitative Determination o f PFOS, PFOSA, PFOSAA, POAA, PFHS, M556 and M570 in Human Serum by LC/MS/MS." Assay Revalidation Addendum Report. NWB Study NWBS00-040. NWB Report NW BR00-122. November 20, 2001. Page 19 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBROI -066 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 o f the final report to the Sponsor, remaining study samples will be stored under required conditions until confirmation o f Sample Disposition/Retum Authorization is received from the Sponsor. 3M Company will be notified concerning final disposition o f records at completion o f contract obligations. Page 20 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 1. Calibration Curve Summary for PFOS Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date 27-NOV-2000 28-NOV-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 30-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 11-Apr-2001 12-Apr-2001 23-Apr-2001 Run Number 1 2 4 5 6 7 8 9 10 11 13 14 15 16 17 18 A -0.000031 -0.000027 0.000002 -0.000002 -0.000001 0.000003 0.000000 0.000000 0.000000 0.000001 -0.000003 -0.000010 0.000004 -0.000006 -0.000009 -0.000002 B 0.052622 0.049661 0.039134 0.009354 0.010776 0.035721 0.037629 0.010093 0.011733 0.047343 0.045861 0.039827 0.045781 0.058787 0.055527 0.017703 C R-Squared LLOQ ITLOQ 0.012630 0.017690 0.020796 0.001128 -0.003903 0.024340 0.025011 0.007090 0.002809 0.024473 0.035036 0.014677 0.046887 -0.001384 0.020155 0.000222 0.9958 0.9926 0.9869 0.9985 0.9867 0.9943 0.9931 0.9895 0.9947 0.9733 0.9973 0.9925 0.9919 0.9942 0.9976 0.9935 3.94 414 3.94 414 3.94 414 3.94 414 4.27 414 4.27 414 4.27 414 4.27 414 4.27 414 4.27 414 4.27 414 4.27 414 4.27 414 4.27 414 4.27 414 4.27 414 Mean S.D. %cv n -0.000005 0.000010 -200.0 16 0.035472 0.017605 49.6 16 0.015479 0.014172 91.6 16 0.9920 0.0060 0.6 16 A, B, and C are coefficients used to define the calibration curve. Page 2 1 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 2. Calibration Curve Summary for PFHS Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date 27-Nov-2000 28-NOV-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 30-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 11-Apr-2001 12-Apr-2001 23-Apr-2001 Run Number 1 2 4 5 6 7 8 9 10 11 13 14 15 16 17 18 A B C R-Squared LLOQ ULOQ -0.000013 -0.000013 -0.000002 -0.000002 -0.000002 -0.000004 -0.000003 -0.000002 -0.000001 0.000000 -0.000004 -0.000006 -0.000002 -0.000007 -0.000007 -0.000004 0.030678 0.031308 0.021861 0.007620 0.008120 0.023053 0.025470 0.008701 0.008569 0.028707 0.021870 0.021837 0.022158 0.029426 0.026000 0.011306 0.025452 0.026252 0.020425 0.006999 -0.002637 0.006759 0.002418 0.002381 0.003686 0.027904 0.016367 0.012060 0.030931 0.013375 0.009029 0.008022 0.9949 0.9950 0.9959 0.9966 0.9953 0.9902 0.9892 0.9972 0.9836 0.9813 0.9858 0.9915 0.9901 0.9881 0.9970 0.9875 1.36 523 1.36 523 1.36 523 1.36 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 Mean S.D. %cv n -0.000004 0.000004 -100.0 16 0.020418 0.008650 42.4 16 0.013089 0.010370 79.2 16 0.9912 0.0050 0.5 16 A, B, and C are coefficients used to define the calibration curve. Page 22 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBROt-066 Table 3. Calibration Curve Summary for PFOA Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 27-Nov-2000 28-NOV-2000 23-Mar-200l 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 12-Apr-2001 14-Apr-2001 22-Apr-2001 23-Apr-2001 11-May-2001 Run Number l 2 4 5 6 7 8 9 10 13 14 15 17 19 21 18 25 A B C R-Squared LLOQ ULOQ -0.000001 -0.000002 0.000001 -0.000001 0.000000 0.000003 0.000002 0.000000 0.000000 -0.000001 -0.000003 0.000002 0.000000 -0.000001 0.000000 -0.000002 -0.000001 0.015479 0.016334 0.008393 0.007290 0.007392 0.008327 0.008675 0.007316 0.007744 0.008171 0.009779 0.007753 0.007833 0.007768 0.015981 0.016857 0.012990 0.005741 0.015052 0.007706 0.002187 -0.000487 0.004956 0.015973 0.005861 0.003135 0.003088 0.000405 0.019137 0.004324 0.001433 -0.001298 0.000933 -0.002765 0.9933 0.9877 0.9842 0.9979 0.9898 0.9865 0.9825 0.9940 0.9964 0.9901 0.9926 0.9872 0.9945 0.9954 0.9878 0.9905 0.9962 1.92 481 1.92 481 1.92 481 1.92 481 2.11 482 2.11 482 2.11 482 2.11 482 2.11 482 2.11 482 2.11 482 2.11 482 2.11 482 2.11 482 2.11 482 2.11 482 1.44 481 Mean S.D. %CV n 0.000000 0.000002 NCL 17 0.010240 0.003645 35.6 17 0.005022 0.006254 124.5 17 0.9910 0.0045 0.5 17 A, B, and C are coefficients used to define the calibration curve. NCL = not calculable Page 23 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 4. Calibration Curve Summary for PFOSAA Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 27-NOV-2000 28-NOV-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 30-Mar-2001 02-Apr-200l 07-Apr-2001 09-Apr-2001 12-Apr-2001 14-Apr-2001 22-Apr-2001 23-Apr-2001 11-May-2001 Run Number 1 2 4 5 6 7 8 9 10 13 14 15 17 19 21 18 25 AB C R-Squared LLOQ ULOQ 0.000000 0.013246 0.007247 0.9804 1.60 501 0.000005 0.012198 0.010441 0.9797 1.60 501 0.000001 0.007894 0.004964 0.9685 1.60 501 0.000001 0.006730 0.010546 0.9935 1.60 501 0.000002 0.008322 -0.001161 0.9836 2.80 502 0.000001 0.007111 -0.001354 0.9760 2.80 502 0.000001 0.005138 -0.004421 0.9798 2.80 502 0.000002 0.006742 0.011207 0.9666 2.80 502 0.000003 0.007717 0.008093 0.9848 2.80 502 0.000008 0.024032 0.015403 0.9884 2.80 502 0.000001 0.033688 0.011384 0.9867 2.80 502 0.000014 0.029651 0.017800 0.9846 2.80 502 0.000006 0.025674 0.007502 0.9944 2.80 502 0.000012 0.026710 -0.009422 0.9813 2.80 502 0.000004 0.007075 -0.004642 0.9735 2.80 502 0.000004 0.007908 0.000878 0.9744 2.80 502 0.000002 0.012005 0.000362 0.9937 1.30 500 Mean S.D. %CV n 0.000004 0.000004 100.0 17 0.014226 0.009564 67.2 17 0.004990 0.007661 153.5 17 0.9818 0.0083 0.8 17 A, B, and C are coefficients used to define the calibration curve. Page 24 Northwest Bioanalytical Study No. NWBSOO-123 Report No. NWBRO1-066 Table 5. Calibration Curve Summary for PFOSA Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 27-NOV-2000 28-NOV-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 30-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 11-Apr-2001 12-Apr-2001 23-Apr-2001 Run Number 1 2 4 5 6 7 8 9 10 11 13 14 15 16 17 18 A B C R-Squared LLOQ ULOQ -0.000041 -0.000025 0.000002 -0.000002 -0.000001 -0.000002 0.000001 0.000000 -0.000003 0.000018 -0.000008 -0.000011 -0.000006 0.000034 -0.000010 0.000007 0.096146 0.087183 0.034802 0.018868 0.023192 0.034174 0.032420 0.022395 0.023907 0.108434 0.108295 0.097511 0.119455 0.124021 0.129002 0.040292 0.018081 0.015131 0.013699 0.003711 -0.012070 0.000108 0.015115 0.000709 0.000482 0.040511 0.054874 0.020730 0.031195 -0.030446 0.003170 0.010493 0.9920 0.9931 0.9847 0.9985 0.9931 0.9956 0.9965 0.9848 0.9934 0.9882 0.9885 0.9819 0.9923 0.9870 0.9944 0.9936 1.00 500 1.00 500 1.00 500 1.00 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 Mean S.D. %CV n -0.000003 0.000016 -533.3 16 0.068756 0.042828 62.3 16 0.011593 0.020139 173.7 16 0.9911 0.0047 0.5 16 A, B, and C are coefficients used to define the calibration curve. Page 25 Northwest Bioanalytical Study No. NWBSOO-123 Report No. NWBRO1-066 Table 6. Calibration Curve Summary for M556 Quadratic weighted l/.x\ All concentrations are expressed as ppb. Run Date 27-NOV-2000 28-NOV-2000 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 30-Mar-2001 30-Mar-2001 01-Apr-2001 07-Apr-2001 09-Apr-2001 12-Apr-2001 14-Apr-2001 23-Apr-2001 Run Number 1 2 5 6 7 8 10 11 12 14 15 17 19 18 AB C R-Squared LLOQ ULOQ 0.000001 0.008245 0.002637 0.9851 2.50 500 0.000003 0.007109 0.006480 0.9931 2.50 500 0.000001 0.002937 0.003249 0.9943 2.50 500 0.000001 0.003973 -0.002024 0.9809 3.20 501 0.000001 0.006232 -0.005748 0.9928 3.20 501 0.000001 0.004865 -0.004285 0.9923 3.20 501 0.000001 0.002628 0.000476 0.9939 3.20 501 0.000003 0.004105 0.002505 0.9789 3.20 501 0.000001 0.002392 0.001473 0.9825 3.20 501 0.000001 0.007457 0.002028 0.9924 3.20 501 0.000003 0.006599 0.008776 0.9891 3.20 501 0.000002 0.006819 -0.003271 0.9913 3.20 501 0.000003 0.006308 -0.001438 0.9886 3.20 501 0.000002 0.003128 0.001358 0.9870 3.20 501 Mean S.D. %CV n 0.000002 0.000001 50.0 14 0.005200 0.001993 38.3 14 0.000873 0.004007 459.0 14 0.9887 0.0051 0.5 14 A, B, and C are coefficients used to define the calibration curve. Page 26 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 7. Calibration Curve Summary for M570 Quadratic weighted I/x\ All concentrations are expressed as ppb. Run Date 27-NOV-2000 28-NOV-2000 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 30-Mar-2001 01-Apr-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 12-Apr-2001 14-Apr-2001 22-Apr-2001 24-Apr-2001 11-May-2001 Run Number 1 2 5 6 7 8 10 12 13 14 15 17 19 21 22 25 A B C R-Squared LLOQ ULOQ -0.000003 0.000002 0.000000 0.000002 0.000001 0.000002 0.000001 0.000001 0.000007 -0.000001 0.000011 0.000004 0.000009 0.000001 0.000018 0.000000 0.022236 0.021764 0.003326 0.003649 0.017625 0.013605 0.003548 0.003371 0.027857 0.034478 0.032868 0.030324 0.030213 0.003114 0.038537 0.004063 0.026662 0.021002 0.003631 -0.000239 0.009909 0.006783 0.001744 0.002595 0.035353 0.018645 0.046246 0.016921 0.008691 -0.002037 0.040536 -0.001174 0.9910 0.9902 0.9937 0.9851 0.9880 0.9911 0.9859 0.9779 0.9890 0.9854 0.9863 0.9936 0.9817 0.9880 0.9873 0.9955 1.00 500 1.00 500 1.00 500 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.00 500 Mean S.D. %CV n 0.000003 0.000005 166.7 16 0.018161 0.013225 72.8 16 0.014704 0.015506 105.5 16 0.9881 0.0045 0.5 16 A, B, and C are coefficients used to define the calibration curve. Page 27 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 8. Back-Calculated Concentrations of Calibration Standards for PFOS Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 27-NOV-2000 Run Number 1 28-NOV-2000 2 23-Mar-2001 4 24-Mar-2001 5 26-Mar-2001 6 26-Mar-2001 7 28-Mar-2001 8 28-Mar-2001 9 30-Mar-2001 10 3.94 4.27 5.17 5.50 11.3 11.7 23.6 24.0 44.2 44.5 85.4 85.5 209 332 414 4.04 5.05 11.1 24.1 48.3 80.9 234 307 432 3.98 5.02 11.4 *44.7 **18.9 77.2 209 321 417 4.05 4.91 10.9 25.4 49.5 84.5 234 299 450 4.00 5.24 10.6 *42.1 **18.1 74.2 204 319 416 4.01 5.70 10.6 26.0 41.2 81.4 232 293 419 3.42 5.60 11.3 20.3 48.5 89.2 186 380 399 3.99 5.05 11.6 23.2 46.8 82.0 209 351 421 3.94 5.07 11.6 24.2 44.0 81.3 205 314 415 4.13 4.95 11.4 22.1 42.0 73.8 191 319 419 4.46 5.64 13.7 23.7 53.9 81.8 223 368 399 4.75 5.64 11.4 25.7 46.6 80.7 214 365 392 3.85 5.34 11.4 23.8 41.9 86.0 218 304 422 4.25 5.23 12.4 24.8 52.8 86.1 203 332 437 4.54 5.26 11.0 24.3 40.5 80.3 190 340 406 5.01 5.55 11.3 26.7 49.0 89.0 207 335 415 4.07 4.86 10.0 23.0 46.2 76.3 224 314 415 4.55 4.89 13.0 24.7 45.4 81.5 199 345 391 4.54 5.10 10.8 23.8 44.1 86.6 221 342 413 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to preparation error Page 28 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 8. Back-Calculated Concentrations of Calibration Standards for PFOS (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 11-Apr-2001 12-Apr-2001 23-Apr-2001 Run Number 11 13 14 15 16 17 18 3.94 4.27 5.17 5.50 11.3 11.7 23.6 24.0 44.2 44.5 85.4 85.5 209 332 414 5.45 3.63 4.16 4.59 4.24 4.47 5.00 4.03 4.66 3.92 4.45 ***2.26 4.61 4.33 4.97 5.49 5.28 5.54 5.75 4.96 5.11 5.46 5.37 5.69 5.20 5.38 5.25 5.25 10.6 20.5 11.1 24.2 11.1 24.8 11.5 22.9 12.2 26.9 11.2 21.3 10.5 25.9 10.5 23.5 11.1 22.8 11.6 24.5 11.3 25.4 12.5 23.3 11.2 25.3 11.3 22.9 44.9 81.5 204 311 397 52.8 106 169 381 428 44.9 85.4 213 351 426 46.0 86.2 208 337 374 46.3 88.3 225 373 409 42.0 81.9 195 329 380 47.1 90.8 223 359 407 45.0 80.4 206 320 394 47.4 72.9 224 328 395 47.7 87.9 209 342 417 44.2 86.4 196 328 435 45.9 82.6 207 341 405 44.9 76.0 201 314 377 48.1 90.0 230 364 426 Mean S.D. %CV %Bias n 3.93 0.208 5.3 -0.3 8 4.42 0.411 9.3 3.5 23 5.21 5.30 11.1 11.4 23.9 24.0 46.4 46.2 81.3 84.1 210 335 411 0.290 0.263 0.407 0.830 2.01 1.57 3.18 3.39 4.48 6.80 15.1 23.8 17.8 5.6 5.0 3.7 7.3 8.4 6.5 6.9 7.3 5.5 8.1 7.2 7.1 4.3 0.8 -3.6 -1.8 -2.6 1.3 0.0 5.0 3.8 -4.8 -1.6 0.5 0.9 -0.7 8 24 8 24 6 24 6 24 8 24 32 32 32 *** Sample deactivated due to unacceptable internal standard response Page 29 Northwest Bioanalytical Study No. N W B S00-128 Report No. NWBRO1-066 Table 9. Back-Calculated Concentrations of Calibration Standards for PFHS Run Date 27-NOV-2000 Run Number 1 28-NOV-2000 2 23-Mar-2001 4 24-Mar-2001 5 26-Mar-2001 6 1.36 1.39 1.46 1.42 1.42 1.41 1.31 1.33 1.48 26-Mar-2001 7 28-Mar-2001 8 28-Mar-2001 9 30-Mar-2001 10 Quadratic weighted 1/x2. All concentrations are expressed as ppb. 2.09 2.92 3.65 10.7 11.5 26.5 27.1 52.6 53.2 104 105 262 418 523 2.66 10.8 27.4 54.5 2.54 11.4 *54.5 **26.8 2.78 10.7 28.0 57.6 2.46 10.9 *50.7 **25.0 3.13 10.6 28.1 52.5 2.71 10.8 28.5 48.1 2.76 11.1 26.5 55.2 2.58 11.3 27.3 53.8 2.08 3.70 11.0 26.9 2.12 3.64 10.7 28.7 50.8 62.9 2.42 3.23 11.6 27.3 1.94 3.39 12.4 29.4 52.6 54.0 2.20 2.96 12.3 30.9 60.1 2.30 3.21 11.3 27.6 2.22 3.66 11.6 26.4 1.99 3.49 12.0 28.8 2.11 2.83 13.2 31.4 2.27 3.71 10.3 28.8 52.9 52.3 55.5 51.1 58.8 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to preparation error 98.9 278 373 508 106 271 415 564 101 274 386 536 102 257 421 534 98.5 283 405 527 104 237 449 512 99.5 261 432 528 101 255 389 545 98.2 247 409 525 102 271 441 516 90.7 242 398 472 108 294 418 594 94.6 236 437 533 104 243 415 545 105 255 455 496 96.2 254 412 544 107 223 465 550 91.3 239 374 565 Page 30 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 9. Back-Calculated Concentrations of Calibration Standards for PFHS (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date Run 1.36 Number 2.09 2.92 3.65 10.7 11.5 26.5 27.1 52.6 53.2 104 105 262 418 523 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 11-Apr-2001 12-Apr-2001 23-Apr-2001 11 13 14 15 16 17 18 2.62 2.90 12.0 24.6 1.89 3.36 11.1 28.0 1.77 2.88 10.9 27.4 2.68 3.61 11.7 27.2 1.97 2.94 11.4 26.7 2.43 3.59 11.9 30.9 2.60 3.30 11.0 28.0 1.75 3.56 10.7 27.2 2.28 2.97 11.3 26.6 2.23 3.20 12.7 29.3 2.12 3.87 10.9 28.5 ***1.93 3.29 12.0 28.3 2.54 3.15 10.7 27.1 1.94 3.33 11.0 26.4 53.2 99.0 249 406 502 66.3 114 230 468 537 52.9 107 255 439 506 57.4 108 266 445 485 51.5 98.0 270 431 497 54.6 103 268 422 523 56.4 110 264 449 514 55.9 99.4 263 411 498 53.8 85.9 251 433 482 58.5 106 288 445 514 53.0 103 248 419 552 55.8 98.0 253 425 519 50.2 114 251 427 502 63.9 107 282 398 522 Mean S.D. %CV %Bias n 1.40 0.0585 4.2 2.9 8 2.19 2.70 3.32 11.0 11.5 27.6 28.0 53.6 55.6 0.266 0.205 0.305 0.288 0.717 0.715 1.60 3.19 4.29 12.1 7.6 9.2 2.6 6.2 2.6 5.7 6.0 7.7 4.8 -7.5 -9.0 2.8 0.0 4.2 3.3 1.9 4.5 23 8 24 8 24 6 24 6 24 *** Sample deactivated due to unacceptable internal standard response 101 102 258 422 523 2.59 7.17 17.1 24.2 26.4 2.6 7.0 6.6 5.7 5.0 -2.9 -2.9 -1.5 1.0 0.0 8 24 32 32 32 Page 31 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 10. Back-Calculated Concentrations of Calibration Standards for PFOA Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date Run 1.92 3.36 10.6 25.0 49.0 97.1 241 385 481 Number 27-NOV-2000 28-NOV-2000 23-Mar-2001 24-Mar-2001 1 1.88 3.04 9.65 25.3 51.6 87.9 252 356 457 2.13 3.14 11.5 *53.4 **22.5 103 261 387 503 2 1.77 2.97 10.2 28.0 52.8 93.6 244 390 478 2.37 2.78 10.9 *46.6 **19.9 94.2 247 372 483 4 1.54 2.87 12.5 27.4 50.2 90.7 256 383 492 2.40 3.40 10.7 20.7 48.5 99.6 222 400 465 5 1.89 3.05 10.4 24.4 51.5 92.7 243 399 477 2.05 3.38 10.6 26.2 51.4 94.9 236 380 480 Mean S.D. %CV %Bias n 2.00 3.08 10.8 25.3 51.0 94.6 245 384 480 0.295 0.222 0.869 2.63 1.48 4.79 14.1 14.4 12.9 14.8 7.2 8.0 10.4 2.9 5.1 5.8 3.8 2.7 4.2 -8.3 1.9 1.2 4.1 -2.6 1.7 -0.3 -0.2 8 8 8 6 6 8 34 10 10 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to sample preparation error Page 32 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 10. Back-Calculated Concentrations of Calibration Standards for PFOA (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 26-Mar-2001 Run Number 6 26-Mar-2001 . 7 28-Mar-2001 8 28-Mar-2001 9 30-Mar-2001 10 02-Apr-2001 13 07-Apr-2001 09-Apr-2001 14 15 12-Apr-2001 17 2.11 3.56 10.8 25.2 49.2 97.3 241 386 482 2.49 3.57 9.76 24.0 49.0 92.5 244 355 501 1.87 3.25 10.3 26.8 59.1 93.8 255 396 466 *4.06 3.37 11.5 23.1 46.7 87.7 234 387 440 2.45 2.72 10.2 29.1 52.2 103 275 385 501 2.06 *1.68 7.94 27.8 55.8 90.6 249 372 477 2.44 2.73 13.2 26.0 46.7 93.2 245 400 480 2.40 3.26 11.4 25.5 48.8 99.5 242 392 465 2.09 3.07 10.0 23.9 55.2 96.2 251 392 470 2.03 3.10 11.4 25.7 52.4 95.3 236 389 474 2.30 3.69 10.1 24.8 49.1 94.9 256 386 479 1.83 3.48 10.2 25.1 49.5 95.0 250 419 489 *3.48 4.55 10.5 23.8 50.1 94.9 238 390 437 2.06 3.54 10.4 25.1 45.5 85.6 240 390 459 *4.56 *5.97 13.2 23.9 52.7 95.5 238 408 498 1.84 *0.842 7.81 25.3 45.7 98.2 228 389 431 2.30 4.05 10.9 27.1 53.9 101 261 407 498 2.13 2.95 11.0 26.1 47.2 102 225 380 489 ***1 13 4.03 11.3 24.6 49.9 91.7 246 408 472 * Sample deactivated as an outlier (not included in summary statistics) *** Sample deactivated due to unacceptable internal standard response Page 33 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 10. Back-Calculated Concentrations of Calibration Standards for PFOA (Continued) Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date 14-Apr-2001 Run Number 19 22-Apr-2001 21 23-Apr-2001 18 2.11 2.13 *6.30 1.71 2.62 2.40 1.85 3.56 10.8 25.2 49.2 97.3 241 386 482 3.41 *6.57 3.35 3.45 3.82 3.21 10.4 26.2 47.9 94.7 225 382 506 12.2 23.8 49.9 93.1 275 364 474 10.4 24.8 51.8 95.2 226 384 466 10.7 28.4 48.9 99.2 213 435 489 10.7 27.5 49.8 80.4 262 388 483 10.9 23.4 54.2 92.6 255 381 465 Mean S.D. %CV %Bias n 2.16 0.266 12.3 2.4 19 3.43 0.449 13.1 -3.7 20 10.7 25.5 50.5 94.4 245 1.24 1.64 3.42 5.09 14.1 11.6 6.4 6.8 5.4 5.8 -0.9 1.2 2.6 -3.0 1.7 24 24 24 24 34 * Sample deactivated as an outlier (not included in summary statistics) 391 475 16.8 20.1 4.3 4.2 1.3 -1.5 24 24 Page 34 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 10. Back-Calculated Concentrations of Calibration Standards for PFOA (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 11-May-2001 Run Number 25 1.44 2.88 10.1 24.5 48.5 96.6 241 385 481 1.46 2.95 9.39 25.2 45.5 90.0 245 399 482 1.33 3.14 11.0 26.3 45.6 94.6 242 371 487 Mean S.D. %CV %Bias n 1.40 3.05 10.2 25.8 45.6 92.3 245 384 480 ISD ISD ISD ISD ISD ISD 14.1 14.4 12.9 ISD ISD ISD ISD ISD ISD 5.8 3.8 2.7 -2.8 5.9 1.0 5.3 -6.0 -4.5 1.7 -0.3 -0.2 2 2 2 2 2 2 34 10 10 ISD = insufficient data points for statistical calculations Page 35 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 11. Back-Calculated Concentrations of Calibration Standards for PFOSAA Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date Run 1.60 3.10 10.6 25.6 50.6 101 251 401 501 Number 27-NOV-2000 1 1.81 3.48 10.3 26.6 61.0 97.6 303 395 538 28-NOV-2000 2 1.39 2.80 9.64 *50.8 **17.1 77.2 252 369 467 1.45 2.36 8.59 24.5 51.0 92.0 282 364 491 1.77 3.84 12.0 *58.2 **22.6 101 293 399 491 23-Mar-2001 4 *7.76 4.18 10.6 24.9 46.5 94.5 301 321 525 1.32 3.23 10.3 17.3 59.0 108 243 459 460 24-Mar-2001 5 1.62 2.75 11.0 25.6 55.3 103 272 413 511 1.80 2.59 10.3 26.8 49.2 97.0 255 369 484 Mean S.D. %CV %Bias n 1.59 3.15 10.3 24.3 53.7 96.3 275 386 496 0.207 0.641 0.987 3.54 5.72 9.20 23.3 40.7 27.2 13.0 20.3 9.6 14.6 10.7 9.6 8.5 10.5 5.5 -0.6 1.6 -2.8 -5.1 6.1 -4.7 9.6 -3.7 - 1.0 7886 6 8 8 8 8 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to sample preparation error Page 36 Northwest Bioanalytical Study No. NWBS00-128 Report No. NVVBRO1-066 Table 11. Back-Calculated Concentrations of Calibration Standards for PFOSAA (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 26-Mar-2001 Run Number 6 26-Mar-2001 7 28-Mar-2001 8 28-Mar-2001 9 30-Mar-2001 10 02-Apr-2001 13 07-Apr-2001 09-Apr-2001 14 15 12-Apr-2001 17 1.30 2.80 4.30 10.3 11.8 25.3 26.8 50.3 51.8 100 102 250 252 2.68 2.99 3.63 2.44 3.28 3.05 3.68 2.43 2.98 3.21 2.32 3.13 2.68 3.29 2.87 3.18 3.20 ***0.932 3.87 4.57 4.22 3.48 2.92 3.75 4.64 3.02 3.21 3.82 5.07 4.16 3.97 3.72 3.34 4.62 3.67 3.88 12.0 23.8 48.1 86.7 *19.7 26.7 65.1 99.3 11.3 28.1 59.3 90.3 10.4 26.7 45.8 108 10.6 24.9 58.9 97.5 14.6 27.2 51.7 101 11.8 33.2 59.2 110 9.06 21.9 52.8 88.1 14.6 28.0 48.4 103 10.6 25.9 47.1 111 11.0 27.2 54.9 101 10.7 24.3 54.1 97.1 12.1 29.8 49.7 107 12.1 20.8 54.2 107 9.14 26.5 49.8 107 10.8 26.9 56.0 111 11.9 29.5 50.8 102 12.0 26.8 51.6 ' 105 * Sample deactivated as an outlier (not included in summary statistics) *** Sample deactivated due to unacceptable internal standard response 250 287 292 282 242 269 257 302 253 271 280 262 266 244 268 286 240 254 400 402 358 461 463 380 378 439 380 386 417 419 433 388 422 451 410 421 381 420 500 502 505 463 446 459 503 481 516 473 459 495 513 443 454 468 435 490 503 510 Page 37 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 11. Back-Calculated Concentrations of Calibration Standards for PFOSAA (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 14-Apr-2001 Run Number 19 1.30 22-Apr-2001 21 23-Apr-2001 18 11-May-2001 25 1.45 1.24 2.80 2.32 3.30 2.32 3.73 3.26 3.18 2.84 2.33 4.30 10.3 11.8 25.3 26.8 50.3 51.8 100 102 250 252 400 402 500 502 4.35 10.7 25.5 54.0 113 254 425 510 4.45 11.3 23.9 57.1 87.2 310 340 478 2.75 10.1 26.7 55.7 103 217 393 492 4.79 13.0 26.5 54.8 112 238 453 500 3.04 12.7 31.8 53.2 99.2 289 413 467 3.81 8.77 22.2 51.4 110 290 403 459 10.6 28.3 52.3 102 266 428 495 10.3 23.2 48.1 94.5 257 386 472 Mean S.D. %CV %Bias n 1.35 2.97 3.88 10.5 11.4 25.8 26.5 50.2 53.5 98.3 102 262 267 407 410 484 480 ISD 0.437 0.634 ISD 1.50 ISD 2.90 ISD 4.48 ISD 8.01 ISD 22.9 ISD 32.1 ISD 24.6 ISD 14.7 16.3 ISD 13.2 ISD 10.9 ISD 8.4 ISD 7.9 ISD 8.6 ISD 7.8 ISD 5.1 3.8 6.1 -9.8 1.9 -3.4 2.0 -1.1 -0.2 3.3 -1.7 0.0 4.8 6.0 1.8 2.0 -3.2 -4.4 2 25 24 2 23 2 24 2 24 2 24 2 24 2 24 2 24 ISD --insufficient data points for statistical calculations Page 38 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 12. Back-Calculated Concentrations of Calibration Standards for PFOSA Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 27-NOV-2000 Run Number 1 28-NOV-2000 2 23-Mar-2001 4 24-Mar-2001 5 26-Mar-2001 6 26-Mar-2001 7 28-Mar-2001 8 28-Mar-2001 9 30-Mar-2001 10 30-Mar-2001 11 1.00 1.40 2.50 2.90 10.0 10.4 25.0 25.4 50.0 50.4 100 250 400 500 1.10 0.893 1.08 0.906 0.984 0.906 0.935 1.08 1.38 1.38 *2.12 1.41 *0.353 1.36 1.53 1.25 1.39 1.51 *2.96 1.39 2.57 9.38 27.4 52.7 97.7 287 378 569 2.46 10.0 *46.1 **18.1 87.8 242 349 497 2.40 9.06 26.8 50.2 97.9 283 354 560 2.70 10.2 *48.6 **19.1 93.3 256 377 480 2.94 9.66 26.3 50.7 93.2 285 370 522 2.80 10.6 17.0 49.6 106 240 431 458 2.47 10.1 24.6 51.2 98.1 255 406 517 2.40 10.1 26.3 49.2 98.4 247 382 497 2.93 9.65 24.1 43.9 94.7 245 382 491 3.10 *16.2 26.6 58.7 101 260 453 471 3.01 10.3 26.6 50.7 88.9 251 423 461 2.79 10.0 26.1 46.4 110 273 377 518 3.21 11.1 25.2 54.8 99.8 240 409 527 2.74 10.1 25.5 45.6 96.8 247 401 479 3.37 10.2 30.2 51.2 106 254 388 500 2.65 8.72 21.7 49.8 89.4 304 387 471 2.47 12.1 27.1 48.9 92.0 238 409 488 2.83 9.54 26.4 48.9 104 261 416 492 2.91 11.1 23.8 50.3 99.9 259 383 448 2.95 9.56 24.4 58.4 *154 203 476 524 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to sample preparation error Page 39 Northwest Bioanalytical Study No. NW BS0-128 Report No. NWBRO1-066 Table 12. Back-Calculated Concentrations of Calibration Standards for PFOSA (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date Run Number 1.00 1.40 2.50 2.90 10.0 10.4 25.0 25.4 50.0 50.4 100 250 400 500 02-Apr-2001 07-Apr-2001 09-Apr-2001 11-Apr-2001 12-Apr-2001 23-Apr-2001 13 14 15 16 17 18 1.06 1.66 1.14 1.66 *2.32 1.40 1.59 1.23 1.47 ***0.557 1.44 1.33 2.93 10.2 26.1 52.2 99.3 262 429 517 3.32 9.31 24.0 51.2 97.3 249 393 452 3.23 10.9 29.4 52.0 109 285 426 502 2.58 10.1 18.9 48.0 97.7 227 399 457 2.77 9.77 28.9 51.8 112 281 429 518 3.11 9.74 23.9 46.7 92.5 232 364 472 2.67 9.79 22.9 55.6 88.9 285 346 473 3.16 9.03 26.6 54.6 111 241 416 533 2.55 10.5 29.5 47.5 103 223 386 536 2.86 11.0 25.2 47.4 102 247 403 501 3.00 9.87 28.1 49.5 83.9 256 405 481 3.01 9.81 23.4 50.8 115 269 389 503 Mean S.D. %CV %Bias n 0.986 0.0884 9.0 -1.4 8 1.40 0.158 11.3 0.0 19 2.59 2.92 9.89 10.1 24.7 25.6 0.201 0.244 0.493 0.758 3.90 2.63 7.8 8.4 5.0 7.5 15.8 10.3 3.6 0.7 -1.1 -2.9 -1.2 0.8 8 24 8 23 6 24 50.6 1.26 2.5 1.2 6 * Sample deactivated as an outlier (not included in summary statistics) *** Sample deactivated due to unacceptable internal standard response 50.6 98.9 256 398 497 3.78 7.71 21.8 29.0 30.3 7.5 7.8 8.5 7.3 6.1 0.4 -1.1 2.4 -0.5 -0.6 24 31 32 32 32 Page 40 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 13. Back-Calculated Concentrations of Calibration Standards for M556 Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 27-NOV-2000 Run Number 1 28-NOV-2000 2 24-Mar-2001 26-Mar-2001 5 6 2.50 2.81 2.23 2.20 2.83 2.05 2.98 26-Mar-2001 7 28-Mar-2001 8 30-Mar-2001 10 30-Mar-2001 11 01-Apr-2001 12 3.20 10.0 10.7 25.0 25.7 50.0 50.7 100 101 250 251 400 401 500 501 3.16 3.08 3.15 3.15 3.13 *4.76 2.75 3.55 3.36 3.00 3.90 2.63 10.2 27.5 56.0 98.1 287 421 555 8.65 *45.7 **17.3 84.1 235 360 451 9.06 24.5 48.3 91.1 269 378 499 10.7 *53.6 **21.2 106 274 404 486 9.42 24.5 52.5 104 256 407 504 10.0 24.7 49.8 99.5 248 384 499 9.86 23.1 43.9 86.7 234 361 497 13.9 25.7 60.8 97.4 271 460 496 10.5 25.7 55.1 85.8 258 445 468 12.1 26.0 45.1 101 263 381 506 9.57 29.3 53.8 91.5 234 373 508 12.2 25.6 47.5 96.3 255 440 504 12.4 27.1 49.3 96.9 245 407 485 10.4 24.0 47.4 101 265 416 496 12.2 23.8 52.0 102 247 364 445 10.2 23.2 58.2 *145 209 487 538 10.7 29.4 56.4 102 263 398 498 8.84 23.4 52.9 80.0 289 383 490 * Sample deactivated as an outlier (not included in summary statistics) * * Sample deactivated due to sample preparation error Page 41 Northwest Bioanalytical Study No. N W B S00-128 Repon No. NWBRO J-066 Table 13. Back-Calculated Concentrations of Calibration Standards for M556 (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date Run 2.50 Number 3.20 10.0 10.7 25.0 25.7 50.0 50.7 100 101 250 251 400 401 500 SOI 07-Apr-2001 14 09-Apr-2001 15 12-Apr-2001 17 14-Apr-2001 19 23-Apr-2001 18 3.47 9.97 28.4 49.5 99.9 258 425 478 2.95 11.4 20.9 54.3 104 239 427 477 2.68 8.84 27.5 49.7 108 254 421 459 3.93 9.80 24.8 52.2 103 266 416 489 2.67 10.5 25.8 46.2 97.3 226 368 490 3.68 11.4 26.2 54.6 105 255 441 523 3.21 9.15 25.9 51.3 106 225 408 530 3.30 11.0 23.8 55.8 96.2 303 348 488 2.89 10.2 25.8 51.1 81.9 253 402 461 3.65 9.66 23.7 53.8 115 295 419 488 Mean S.D. %CV %Bias n 2.52 3.20 9.67 10.7 25.3 25.4 51.7 51.9 97.1 97.9 262 255 392 409 499 492 0.400 0.387 0.765 1.29 1.47 2.12 3.38 4.29 8.23 8.74 18.9 22.7 22.3 34.9 33.6 22.4 15.9 12.1 7.9 12.1 5.8 8.3 6.5 8.3 8.5 8.9 7.2 8.9 5.7 8.5 6.7 4.6 0.8 0.0 -3.3 0.0 1.2 -1.2 3.4 2.4 -2.9 -3.1 4.8 1.6 -2.0 2.0 -0.2 -1.8 6 21 6 22 4 22 4 22 6 21 6 22 6 22 6 22 Page 42 Northwest Bioanalytical Study No. NWBSOO-128 Repon No. NWBRO1-066 Table 14. Back-Calculated Concentrations of Calibration Standards for M570 Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 27-NOV-2000 Run Number 1 28-NOV-2000 2 24-Mar-2001 5 26-Mar-2001 6 26-Mar-2001 7 28-Mar-2001 8 30-Mar-2001 10 01-Apr-2001 12 02-Apr-2001 13 1.00 1.05 1.01 0.991 1.56 0.927 1.15 1.80 2.50 3.30 10.0 10.8 25.0 25.8 50.0 50.8 100 101 250 251 400 401 500 501 2.47 9.76 26.4 58.7 94.4 275 390 530 2.09 10.1 *50.6 **18.6 87.5 266 374 472 2.16 8.82 23.2 52.0 88.8 269 374 480 2.90 11.4 *58.7 **21.2 101 274 407 507 2.07 10.3 26.0 55.4 96.9 263 414 507 2.40 9.59 26.1 50.6 97.2 241 382 492 1.60 2.96 10.5 24.6 48.6 90.0 238 354 489 2.08 3.37 18.0 28.3 *69.4 108 296 461 474 2.04 3.40 9.97 25.7 56.3 89.3 274 462 464 1.49 3.55 10.2 27.4 44.2 105 262 385 469 1.89 3.04 9.96 25.8 60.0 101 228 405 503 1.90 2.84 12.3 25.4 48.3 94.2 262 435 473 1.87 2.55 12.8 28.6 48.7 98.3 234 413 468 2.08 2.73 9.87 26.2 47.6 109 279 410 500 2.15 3.70 10.3 32.2 56.2 103 254 387 508 1.60 2.53 8.98 22.4 53.2 86.3 297 370 496 1.53 2.87 10.3 27.1 54.5 98.1 258 426 522 2.25 ' 3.19 10.3 24.4 54.2 101 266 382 450 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to sample preparation error Page 43 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 14. Back-Calculated Concentrations of Calibration Standards for M570 (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 07-Apr-2001 Run Number 14 09-Apr-2001 15 12-Apr-2001 14-Apr-2001 22-Apr-2001 17 19 21 24-Apr-2001 22 11-May-2001 25 1.00 1.80 2.50 3.30 10.0 10.8 25.0 25.8 50.0 50.8 100 101 250 251 400 401 500 501 1.65 3.24 2.11 2.80 1.98 2.39 1.86 3.60 2.03 2.78 ***0.564 2.92 1.46 3.44 2.18 3.19 1.94 2.56 *3.02 3.40 1.68 3.12 2.15 2.76 1.03 2.64 10.3 1.01 2.12 9.85 10.9 30.4 10.8 19.4 8.68 26.3 10.1 27.6 11.5 28.1 11.3 24.7 9.54 25.8 10.2 24.0 10.9 25.2 12.4 27.2 10.1 22.5 10.4 29.0 26.8 50.8 24.6 46.9 52.3 109 263 436 475 52.0 102 231 426 466 48.4 107 255 403 448 54.8 107 279 424 491 50.5 103 229 387 517 51.2 104 248 416 501 52.4 112 240 418 521 56.6 88.5 310 340 477 54.0 106 214 395 502 48.9 101 214 448 518 53.7 119 268 390 508 52.8 86.3 263 406 470 99.5 257 435 466 98.6 267 370 508 Mean S.D. %CV %Bias n 1.02 0.0677 6.6 2.0 7 1.89 0.246 13.0 5.0 22 2.36 3.04 10.0 10.5 25.5 26.2 52.4 0.302 0.371 0.736 1.01 1.36 2.72 4.12 12.8 12.2 7.4 9.6 5.3 10.4 7.9 -5.6 -7.9 0.0 -2.8 2.0 1.6 4.8 8 24 8 23 6 24 6 52.1 95.5 101 264 257 393 407 495 488 3.64 4.94 8.50 10.9 25.4 23.2 30.6 21.7 22.4 7.0 5.2 8.4 4.1 9.9 5.9 7.5 4.4 4.6 2.6 -4.5 0.0 5.6 2.4 -1.8 1.5 - 1.0 -2.6 23 8 24 8 24 8 24 8 24 * Sample deactivated as an outlier (not included in summary statistics) * * * Sample deactivated due unacceptable internal standard response Page 44 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 15. Analytical QC Summary for PFOS All concentrations are expressed as ppb. Run Date Run Number Low QC 6.40 ppb Low QC 5.75 ppb Preparation 27-Oct-2000 05-Apr-2001 Date 27-NOV-2000 1 5.91 28-Nov-2000 2 6.13 6.49 23-Mar-2001 4 5.82 *4.60 24-Mar-2001 5 6.50 6.36 26-Mar-2001 6 6.49 5.88 26-Mar-2001 7 6.49 6.70 28-Mar-2001 8 5.88 5.58 28-Mar-2001 9 6.29 5.65 5.14 Medium QC 126 ppb 27-Oct-2000 121 127 121 125 135 *192 134 131 **74.2 119 139 123 117 133 141 140 Medium QC 126 ppb 05-Apr-2001 High QC 332 ppb 27-Oct-2000 High QC 332 ppb 08-Mar-2001 High QC 331 ppb High QC 348 ppb DF=5 05-Apr-2001 08-Mar-2001 320 372 347 351 354 333 343 362 304 344 326 323 348 323 357 344 * >20% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response Page 45 Northwest Bioanalytical Study No. N W B S00-128 Report No. NWBRO1-066 Table 15. Analytical QC Summary for PFOS (Continued) All concentrations are expressed as ppb. Run Date Run Number Low QC 6.40 ppb Low QC 5.75 ppb Preparation 27-Oct-2000 05-Apr-2001 Date 30-Mar-2001 10 6.08 30-Mar-2001 11 5.74 6.60 5.82 02-Apr-2001 13 6.47 07-Apr-2001 14 6.65 6.21 09-Apr-2001 15 6.22 5.78 11-Apr-2001 16 5.84 6.99 12-Apr-2001 17 6.51 6.25 6.20 Medium QC 126 ppb 27-Oct-2000 127 138 126 118 130 137 123 125 132 135 130 122 137 141 Medium QC 126 ppb 05-Apr-2001 High QC 332 ppb High QC 332 ppb 27-Oct-2000 08-Mar-2001 324 332 328 **149 346 330 373 330 332 357 339 345 357 352 High QC 331 ppb 05-Apr-2001 High QC 348 ppb DF=5 08-Mar-2001 353 357 365 ** Sample deactivated due to unacceptable internal standard response Page 46 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 15. Analytical QC Summary for PFOS (Continued) All concentrations are expressed as ppb. Run Date 23-Apr-2001 Run Number Low QC 6.40 ppb Low QC 5.75 ppb Preparation 27-Oct-2000 05-Apr-2001 Date 18 6.57 6.84 Medium QC 126 ppb 27-Oct-2000 Medium QC 126 ppb 05-Apr-2001 138 130 High QC 332 ppb High QC 332 ppb High QC 331 ppb 27-Oct-2000 08-Mar-2001 05-Apr-2001 296 330 High QC 348 ppb DF=5 08-Mar-2001 Mean S.D. %CV %Theoretical %Bias n 6.11 6.71 132 134 348 339 313 358 0.492 ISD 13.7 ISD 16.3 15.8 ISD 6.11 8.1 ISD 10.4 ISD 4.7 4.7 ISD 1.7 95.5 116.7 104.8 106.3 104.8 102.1 94.6 102.9 -4.5 16.7 4.8 6.3 4.8 2.1 -5.4 2.9 30 2 29 2 8 21 2 3 ISD - insufficient data points for statistical calculation Page 47 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 16. Analytical QC Summary for PFHS All concentrations are expressed as ppb. Run Date 27-NOV-2000 28-NOV-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 Run Number Preparation Date 1 2 4 5 6 7 8 9 Low QC 4.48 ppb 27-Oct-2000 Low QC 4.48 ppb 05-Apr-2001 Medium QC 156 ppb 27-Oct-2000 Medium QC 157 ppb 05-Apr-2001 High QC 417 ppb 27-Oct-2000 3.61 161 4.28 148 3.70 157 3.86 153 4.29 155 4.06 171 3.96 164 4.02 161 4.85 **128 5.07 157 4.71 157 4.95 135 5.31 158 4.35 158 4.32 158 3.92 158 382 443 411 445 428 406 414 460 ** Sample deactivated due to unacceptable internal standard response High QC 417 ppb 08-Mar-2001 373 396 411 407 420 383 392 415 High QC 418 ppb 05-Apr-2001 Page 48 Northwest Bioanalytical Run Date 30-Mar-2001 Run Number Preparation Date 10 30-Mar-2001 02-Apr-2001 11 13 07-Apr-2001 14 09-Apr-2001 15 11-Apr-2001 12-Apr-2001 16 17 Table 16. Analytical QC Summary for PFHS (Continued) All concentrations are expressed as ppb. Low QC 4.48 ppb 27-Oct-2000 Low QC 4.48 ppb 05-Apr-2001 Medium QC 156 ppb 27-Oct-2000 Medium QC 157 ppb 05-Apr-2001 High QC 417 ppb 27-Oct-2000 *3.48 4.29 4.08 4.06 4.20 4.38 4.87 4.25 3.92 3.68 4.85 3.62 4.14 4.43 136 146 151 154 158 158 153 149 156 152 155 155 157 153 * >20% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response Study No. NWBS00-128 Report No. NWBRO1-066 High QC 417 ppb 08-Mar-2001 High QC 418 ppb 05-Apr-2001 413 345 391 **200 428 436 408 378 444 401 387 383 397 404 Page 49 Northwest Bioanalytical Run Date 23-Apr-2001 Run Number Preparation Date 18 Table 16. Analytical QC Summary for PFHS (Continued) All concentrations are expressed as ppb. Low QC 4.48 ppb 27-Oct-2000 Low QC 4.48 ppb 05-Apr-2001 Medium QC 156 ppb 27-Oct-2000 Medium QC 157 ppb 05-Apr-2001 High QC 417 ppb 27-Oct-2000 3.87 166 4.05 145 Study No. NWBS00-128 Report No. NWBRO1-066 High QC 417 ppb 08-Mar-2001 High QC 418 ppb 05-Apr-200l 397 389 Mean S.D. %CV %Theoretical %Bias n 4.25 0.467 11.0 94.9 -5.1 30 3.96 ISD ISD 88.4 -11.6 2 155 7.17 4.6 99.4 -0.6 29 156 ISD ISD 99.4 -0.6 2 ISD - insufficient data points for statistical calculation 424 25.3 6.0 101.7 1.7 8 401 22.6 5.6 96.2 -3.8 21 393 ISD ISD 94.0 -6.0 2 Page 50 Northwest Bioanalytical Study No. NW BS00-128 Report No. NW BR01-066 Table 17. Analytical QC Summary for PFOA All concentrations are expressed as ppb. Run Date Run Number Preparation Date Low QC 4.81 ppb Low QC 4.32 ppb 27-Oct-2000 05-Apr-2001 Low QC 4.32 ppb 02-May-2001 Medium QC Medium QC High QC 145 ppb 145 ppb 385 ppb 27-Oct-2000 05-Apr-2001 27-Oct-2000 High QC 385 ppb 08-Mar-2001 High QC 385 ppb 05-Apr-2001 27-NOV-2000 28-NOV-2000 23-Mar-2001 24~Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 1 2 4 5 6 7 8 9 4.55 4.30 4.35 3.92 *2.72 4.85 4.09 *3.69 4.12 4.81 5.47 4.93 4.63 *0.161 4.33 3.89 154 160 151 162 159 152 143 151 **124 152 146 140 151 156 158 157 403 429 416 439 412 381 390 377 393 395 348 384 404 375 404 433 * >20% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response Page 51 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NVVBRO1-066 Table 17. Analytical QC Summary for PFOA (Continued) All concentrations are expressed as ppb. Run Date Run Number Preparation Date Low QC 4.81 ppb Low QC 4.32 ppb 27-Oct-2000 05-Apr-2001 Low QC 4.32 ppb 02-May-2001 Medium QC Medium QC High QC 145 ppb 145 ppb 385 ppb 27-Oct-2000 05-Apr-2001 27-Oct-2000 High QC 385 ppb 08-Mar-2001 High QC 385 ppb 05-Apr-2001 30-Mar-2001 10 02-Apr-2001 13 07-Apr-2001 14 09-Apr-2001 15 12-Apr-2001 17 14-Apr-2001 19 22-Apr-2001 21 23-Apr-2001 18 4.29 4.14 4.56 4.15 *5.97 4.77 4.45 *3.61 4.17 4.07 *3.79 5.04 4.03 3.90 3.82 4.67 151 155 145 139 145 136 159 147 151 158 131 *109 143 170 141 151 393 382 381 336 381 361 406 351 372 375 377 401 401 361 370 414 * >20% deviation from theoretical Page 52 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 17. Analytical QC Summary for PFOA (Continued) All concentrations are expressed as ppb. Run Date Run Number Low QC 4.81 ppb Low QC 4.32 ppb Low QC Medium QC Medium QC High QC 4.32 ppb 145 ppb 145 ppb 385 ppb High QC 385 ppb High QC 385 ppb Preparation 27-Oct-2000 05-Apr-200l 02-May-2001 27-Oct-2000 05-Apr-2001 27-Oct-2000 08-Mar-2001 05-Apr-2001 Date 11-May-2001 25 4.16 150 386 4.65 148 398 Mean S.D. %CV %Theoretical %Bias n 4.19 0.970 23.2 87.1 -12.9 30 4.25 4.41 149 148 ISD ISD 11.5 4.51 ISD ISD 7.7 3.0 98.4 102.1 102.8 102.1 -1.6 2.1 2.8 2.1 2 2 29 4 ISD = insufficient data points for statistical calculation * 406 22.3 5.5 105.5 5.5 8 382 22.5 5.9 99.2 -0.8 22 392 18.6 4.7 101.8 1.8 4 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 18. Analytical QC Summary for PFOSAA All concentrations are expressed as ppb. Run Date Run Number Low QC 4.60 ppb Preparation 27-Oct-2000 Date Low QC 4.30 ppb 05-Apr-2001 Low QC 4.30 ppb 02-May-2001 Medium QC 151 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 High QC 401 ppb 27-Oct-2000 High QC 401 ppb 08-Mar-2001 High QC 400 ppb 05-Apr-2001 27-NOV-2000 1 4.22 141 398 28-NOV-2000 23-Mar-2001 2 4 *3.38 4.50 3.66 *2.38 167 425 150 378 165 368 172 463 24-Mar-2001 5 26-Mar-2001 6 26-Mar-2001 7 28-Mar-2001 8 28-Mar-2001 9 4.11 4.22 4.11 4.55 4.98 4.85 4.26 *6.56 4.31 4.16 4.41 *374 157 157 **71.5 130 146 135 145 142 . 183 175 456 1. 422 389 348 445 365 384 415 383 440 415 * >25% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response Page 54 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 18. Analytical QC Summary for PFOSAA (Continued) All concentrations are expressed as ppb. Run Date Run Number Low QC 4.60 ppb Preparation 27-Oct-2000 Date Low QC 4.30 ppb 05-Apr-2001 Low QC 4.30 ppb 02-May-2001 Medium QC 151 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 High QC 401 ppb 27-Oct-2000 High QC 401 ppb 08-Mar-2001 High QC 400 ppb 05-Apr-2001 30-Mar-2001 10 02-Apr-2001 13 07-Apr-2001 14 09-Apr-2001 15 12-Apr-2001 17 14-Apr-2001 19 22-Apr-2001 21 23-Apr-2001 18 5.47 4.96 *6.00 5.38 5.41 4.70 4.61 3.71 5.23 5.04 4.60 5.43 *6.60 4.64 4.41 5.33 149 170 154 153 166 154 170 165 178 *189 160 123 149 *218 167 169 380 376 412 360 452 439 426 380 465 448 420 429 432 413 398 427 * >25% deviation from theoretical Page 55 Northwest Bioanalytical Study No. N W B S00-128 Report No. NWBRO1-066 Table 18. Analytical QC Summary for PFOSAA (Continued) All concentrations are expressed as ppb. Run Date 11-May-2001 Run Number Low QC 4.60 ppb Preparation 27-Oct-2000 Date 25 Low QC 4.30 ppb 05-Apr-2001 Low QC 4.30 ppb 02-May-2001 4.34 3.95 Medium QC 151 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 143 145 High QC 401 ppb 27-Oct-2000 High QC 401 ppb High QC 400 ppb 08-Mar-2001 05-Apr-2001 424 407 Mean S.D. %CV %Theoretical %Bias n 4.68 0.882 18.8 101.7 1-7 30 4.87 4.15 167 156 ISD ISD 44.2 13.9 ISD ISD 26.5 8.9 113.3 96.5 110.6 104.0 13.3 -3.5 10.6 4.0 2 2 29 4 ISD - insufficient data points for statistical calculations 412 35.1 8.5 102.7 2.7 8 410 33.2 8.1 102.2 2.2 22 414 13.8 3.3 103.5 3.5 4 Page 56 Northwest Bioanalytical Table 19. Analytical QC Summary for PFOSA All concentrations are expressed as ppb. Run Date 27-NOV-2000 28-NOV-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 Run Number Preparation Date 1 2 4 5 6 7 8 9 Low QC 4.00 ppb 27-Oct-2000 4.39 4.12 4.86 3.97 *2.33 4.47 3.94 4.21 3.85 3.85 4.80 3.98 4.16 3.58 3.84 3.82 Low QC 4.00 ppb 05-Apr-2001 Medium QC 150 ppb 27-Oct-2000 147 162 146 158 180 *328 156 158 **72.6 133 141 133 146 155 173 157 Medium QC 150 ppb 05-Apr-2001 High QC 400 ppb 27-Oct-2000 399 466 416 386 434 417 423 399 * >25% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response Study No. NWBS00-128 Report No. NWBRO1-066 High QC 400 ppb 08-Mar-2001 High QC 400 ppb 05-Apr-2001 311 457 369 396 431 406 447 408 Page 57 Northwest Bioanalytical Table 19. Analytical QC Summary for PFOSA (Continued) All concentrations are expressed as ppb. Run Date 30-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 11-Apr-2001 12-Apr-2001 Run Number Preparation Date 10 11 13 14 15 16 17 Low QC 4.00 ppb 27-Oct-2000 4.16 3.96 *5.14 4.08 4.21 4.39 4.79 4.46 4.19 3.92 *5.84 4.95 4.53 4.38 Low QC 4.00 ppb 05-Apr-2001 Medium QC 150 ppb 27-Oct-2000 144 161 138 124 148 159 150 147 157 157 165 127 155 170 Medium QC 150 ppb 05-Apr-2001 High QC 400 ppb 27-Oct-2000 * >25% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response Study No. NWBSOO-128 Report No. NVVBRO1-066 High QC 400 ppb 08-Mar-200l High QC 400 ppb 05-Apr-2001 400 368 392 **170 431 361 456 424 423 422 404 425 437 403 Page 58 Northwest Bioanalytical Table 19. Analytical QC Summary for PFOSA (Continued) All concentrations are expressed as ppb. Run Date 23-Apr-2001 Run Number Preparation Date 18 Low QC 4.00 ppb 27-Oct-2000 Low QC 4.00 ppb 05-Apr-2001 4.95 4.73 Medium QC 150 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 178 170 High QC 400 ppb 27-Oct-2000 Study No. NW BS00-128 Report No. NWBRO1-066 High QC 400 ppb 08-Mar-2001 High QC 400 ppb 05-Apr-2001 392 436 Mean S.D. %CV "/Theoretical %Bias n 4.24 0.596 14.1 106.0 6.0 30 4.84 ISD ISD 121.0 21.0 2 158 35.3 22.3 105.3 5.3 29 174 ISD ISD 116.0 16.0 2 418 24.9 6.0 104.5 4.5 8 ISD --insufficient data points for statistical calculations 408 34.9 8.6 102.0 2.0 21 414 ISD ISD 103.5 3.5 2 Page 59 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 20. Analytical QC Summary for M556 All concentrations are expressed as ppb. Run Date 27-NOV-2000 28-NOV-2000 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 30-Mar-2001 30-Mar-2001 01-Apr-2001 Run Number Preparation Date 1 2 5 6 7 8 10 11 12 Low QC 4.00 ppb Low QC 4.00 ppb 27-Oct-2000 05-Apr-2001 4.09 3.23 4.52 3.60 4.77 3.60 3.52 4.07 4.45 *2.73 *6.68 4.15 *4.85 4.06 ***7.47 4.28 *5.69 4.35 Medium QC ISO ppb 27-Oct-2000 133 161 144 166 160 156 **79.4 137 137 124 164 166 149 171 146 126 162 158 Medium QC 150 ppb 05-Apr-2001 High QC 400 ppb 27-Oct-2000 423 439 393 389 High QC 400 ppb 08-Mar-2001 402 401 367 428 354 404 426 388 382 385 369 **173 396 388 High QC 400 ppb 05-Apr-2001 * >20% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response *** Sample deactivated due to carryover Page 60 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Table 20. Analytical QC Summary for MS56 (Continued) All concentrations are expressed as ppb. Run Date Run Number Preparation Date Low QC 4.00 ppb Low QC 4.00 ppb 27-Oct-2000 05-Apr-2001 Medium QC 150 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 High QC 400 ppb 27-Oct-2000 High QC 400 ppb High QC 400 ppb 08-Mar-2001 05-Apr-2001 07-Apr-2001 14 4.73 152 407 3.51 145 387 09-Apr-2001 15 4.02 171 434 12-Apr-2001 17 *3.14 4.40 164 164 395 395 14-Apr-2001 19 4.29 3.75 162 155 387 396 4.71 *115 23-Apr-2001 18 4.51 180 406 381 4.11 160 395 Mean S.D. %CV %Theoretical %Bias n 4.21 0.818 19.4 105.3 5.3 25 4.31 ISD ISD 107.8 7.8 2 152 15.5 10.2 101.3 1.3 25 170 ISD ISD 113.3 13.3 2 406 21.0 5.2 101.5 1.5 6 * >20% deviation from theoretical ISD = insufficient data points for statistical calculations 395 20.3 5.1 98.8 -1.3 19 388 ISD ISD 97.0 -3.0 2 Page 61 Northwest Bioanalytical Study No. N W B S00-128 Report No. NWBRO1-066 Table 21. Analytical QC Summary for M570 All concentrations are expressed as ppb. Run Date Run Number Low QC 4.00 ppb Preparation 27-Oct-2000 Date Low QC 4.00 ppb 05-Apr-2001 Low QC 4.00 ppb 02-May-2001 Medium QC 150 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 High QC 400 ppb 27-Oct-2000 High QC 400 ppb 08-Mar-2001 High QC 400 ppb 05-Apr-2001 27-NOV-2000 1 28-NOV-2000 2 24-Mar-2001 5 26-Mar-2001 6 26-Mar-2001 7 28-Mar-2001 8 30-Mar-2001 10 01-Apr-2001 12 3.61 *3.07 4.10 3.59 3.81 3.89 3.63 4.00 4.75 3.26 *5.01 3.25 4.64 3.54 3.78 3.60 # 149 163 151 169 168 165 **74.2 140 150 133 156 161 150 180 166 169 388 451 383 394 415 412 338 447 344 403 433 396 359 379 411 364 * >20% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response Page 62 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 21. Analytical QC Summary for M570 (Continued) AH concentrations are expressed as ppb. Run Date Run Number Preparation Date Low QC 4.00 ppb 27-Oct-2000 Low QC 4.00 ppb 05-Apr-2001 Low QC 4.00 ppb 02-May-2001 Medium QC 150 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 High QC 400 ppb 27-Oct-2000 High QC 400 ppb 08-Mar-2001 High QC 400 ppb 05-Apr-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 12-Apr-2001 14-Apr-2001 22-Apr-2001 24-Apr-2001 13 14 15 17 19 21 22 4.55 3.99 4.80 4.37 3.91 *2.69 4.38 4.28 4.17 4.26 *5.54 3.89 ' *3.11 4.18 156 162 159 156 168 163 172 *185 158 120 146 *207 178 168 405 362 446 423 380 375 447 446 413 423 . 447 413 373 393 * >20% deviation from theoretical Page 63 Northwest Bioanalytical Study No. NW BS0-128 Report No. NWBRO1-066 Table 21. Analytical QC Summary for M570 (Continued) All concentrations are expressed as ppb. Run Date 11-May-2001 Run Number Preparation Date 25 Low QC 4.00 ppb 27-Oct-2000 Low QC 4.00 ppb 05-Apr-2001 Low QC 4.00 ppb 02-May-2001 4.51 2.83 Medium QC 150 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 143 149 High QC 400 ppb 27-Oct-2000 High QC 400 ppb 08-Mar-2001 High QC 400 ppb 05-Apr-2001 417 408 Mean S.D. %CV %Theoretical %Bias n 4.01 0.621 15.5 100.3 0.3 28 3.65 3.67 160 160 ISD ISD 16.6 16.3 ISD ISD 10.4 10.2 91.3 91.8 106.7 106.7 -8.8 -8.3 6.7 6.7 2 2 27 4 * >20% deviation from theoretical ISD = insufficient data points for statistical calculations 407 25.0 6.1 101.8 1.8 6 402 35.4 8.8 100.5 0.5 22 398 19.2 4.8 99.5 -0.5 4 Page 64 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations All concentrations are expressed as ppb. Sample ID 10956 PFOS Concentration (PPb) 54.1 10957 51.3 10958 80.5 10959 69.3 10960 37.3 10961 48.4 10962 55.7 10963 42.0 10964 114 10965 45.0 10966 29.2 10967 31.7 10968 42.8 10969 37.9 10970 46.7 10971 13.4 10972 24.0 10973 34.1 PFHS* Concentration (PPb) 3.10 5.45 12.4 3.01 2.95 2.79 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 8.00 <LLOQ(2.09) <LLOQ(2.09) 9.26 2.96 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 3.68 PFOA* Concentration (ppb) 3.95 6.64 22.2 13.9 5.13 2.77 4.44 6.58 7.07 3.90 <LLOQ(2.11) <LLOQ(2.11) 5.17 <LLOQ(2.11) 3.35 <LLOQ(2.11) <LLOQ(2.11) 5.11 PFOSAA* Concentration (ppb) 3.68 <LLOQ(2.80) 7.59 4.13 <LLOQ(2.80) <LLOQ(2.80) 4.21 3.55 9.05 <LLOQ(2.80) 2.81 4.58 <LLOQ(2.80) 4.23 3.08 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) <LLOQ(1.80) 3.10 <LLOQ(1.80) 2.26 <LLOQ(1.80) 6.18 <LLOQ(1.80) <LLOQ(1.80) 4.97 2.55 <LLOQ(1.80) <LLOQ(1.80) 4.72 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 65 Northwest Bioanalytical Study No. N W B S00-128 Repon No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID PFOS Concentration (PPb) 10974 51.8 10975 35.8 10976 44.0 10977 99.7 10978 48.7 10979 44.2 10980 . 57.7 10981 25.8 10982 46.4 10983 38.6 10984 75.1 10985 41.9 10986 57.7 10987 14.0 10988 39.2 10989 68.9 10990 38.6 10991 36.6 PFHS* . Concentration (Ppb) <LLOQ(2.09) 5.73 2.62 5.98 <LLOQ(2.09) <LLOQ(2.09) 3.66 4.98 7.28 <LLOQ(2.09) <LLOQ(2.09) 6.97 3.26 <LLOQ(2.09) 2.17 2.53 <LLOQ(2.09) 2.11 PFOA* Concentration (PPb) 3.37 3.04 7.32 6.94 3.23 3.16 4.86 2.59 2.20 <LLOQ(2.11) 17.4 2.22 5.04 <LLOQ(2.11) <LLOQ(2.11) 5.28 4.42 <LLOQ(2.11) PFOSAA* Concentration (PPb) 3.46 3.43 3.43 8.67 4.47 <LLOQ(2.80) 4.33 <LLOQ(2.80) <LLOQ(2.80) 3.90 3.44 <LLOQ(2.80) 5.09 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.45 PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) <LLOQ(1.80) 2.03 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 5.13 <LLOQ(1.80) <LLOQ(1.80) 2.86 <LLOQ(1.80) 3.31 <LLOQ(1.80) 3.16 <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 66 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 10992 PFOS Concentration (ppb) 19.4 10993 18.9 10994 44.6 10995 61.6 10996 39.2 10997 25.6 10998 70.6 10999 101 11000 42.3 11001 16.3 11002 127 11003 65.2 11004 40.1 11005 25.8 11006 39.1 11007 36.8 11008 26.2 11009 19.5 PFHS* Concentration (ppb) <LLOQ(2.09) <LLOQ(2.09) 2.18 2.26 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 8.84 <LLOQ(2.09) <LLOQ(2.09) 3.45 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.17 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (PPb) <LLOQ(2.11) 2.29 2.51 4.38 3.69 <LLOQ(2.11) 6.92 8.54 <LLOQ(2.11) <LLOQ(2.11) 9.90 2.84 3.43 <LLOQ(2.11) <LLOQ(2.11) 9.12 4.76 <LLOQ(2.11) PFOSAA* Concentration (ppb) <LLOQ(2.80) 3.62 <LLOQ(2.80) 4.11 5.76 <LLOQ(2.80) 5.16 4.69 <LLOQ(2.80) <LLOQ(2.80) 6.22 3.69 3.63 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.01 PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1,40) MS56* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 5.11 <LLOQ(1.80) 2.99 16.4 <LLOQ(1.80) <LLOQ(1.80) 3.99 <LLOQ(1.80) <LLOQ(1.80) 2.17 2.58 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 vaiy from results obtained using serum calibration curves (see Results and Discussion section). Page 67 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 11010 PFOS Concentration (PPb) 40.9 non 33.6 11012 23.0 11013 47.8 11014 38.7 11015 105 11016 42.2 11017 27.7 11018 19.0 11019 84.9 11020 33.3 11021 19.4 11022 15.1 11023 50.3 11024 57.5 11025 57.5 11026 48.8 11027 48.7 PFHS* Concentration (PPb) 2.18 <LLOQ(2.09) 2.26 7.39 <LLOQ(2.09) 2.29 8.70 <LLOQ(2.09) 2.20 2.67 2.59 <LLOQ(2.09) 3.58 3.59 <LLOQ(2.09) <LLOQ(2.09) 2.74 5.70 PFOA* Concentration (ppb) 2.78 5.50 3.73 8.05 4.25 10.2 7.65 3.55 3.75 17.0 3.80 2.47 <LLOQ(2.11) 3.83 5.91 7.68 3.97 6.74 PFOSAA* Concentration (PPb) 3.95 6.00 <LLOQ(2.80) 4.93 6.10 6.49 4.12 3.34 <LLOQ(2.80) 3.96 4.63 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 7.77 7.48 3.49 4.95 PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) <LLOQ(3.20) 12.7 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) <LLOQ(1.80) 5.18 5.33 1.88 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.00 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.53 2.45 <LLOQ(1.80) 2.20 2.26 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 68 Northwest Bioanalytical Study No. N W B S00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 11028 PFOS Concentration (PPb) 45.2 11029 21.9 11030 36.7 11031 54.5 11032 39.8 11033 63.2 11034 26.4 11035 38.6 11036 26.4 11037 17.3 11038 41.1 11039 60.7 11040 44.7 11041 42.8 11042 11043 55.7 27.1 11044 34.2 11045 49.0 PFHS* Concentration (PPb) 2.13 <LLOQ(2.09) <LLOQ(2.09) 8.04 <LLOQ(2.09) 4.36 9.84 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.23 2.85 <LLOQ(2.09) 3.07 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.16 PFOA* Concentration (PPb) 6.43 3.61 6.17 4.69 3.95 6.34 4.68 9.98 2.95 <LLOQ(2.11) 3 -17 7.45 4.35 ' 10.1 3.84 2.39 5.38 6.15 PFOSAA* Concentration (PPb) <LLOQ(2.80) <LLOQ(2.80) 3.00 <LLOQ(2.80) 3.25 3.25 4.83 <LLOQ(2.80) <LLOQ(2.80) 4.44 7.37 <LLOQ(2.80) <LLOQ(2.80) 3.19 3.85 <LLOQ(2.80) 2.84 <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (Ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M57* Concentration (ppb) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 5.51 <LLOQ(1.80) <LLOQ(1.80) 1.84 2.57 <LLOQ(1.80) 5.93 <LLOQ(1.80) <LLOQ(1.80) 2.04 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of die 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 69 Northwest Bioanalytical Study No. NW BS0-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 11046 PFOS Concentration (PPb) 56.9 11047 73.8 11048 70.8 11049 33.5 11050 40.4 11051 26.7 11052 44.3 11053 44.8 11054 49.6 11055 27.5 11056 27.0 11057 51.9 11058 53.2 11059 48.7 11060 36.4 11061 18.3 11062 58.1 11063 25.8 PFHS* Concentration (ppb) 2.11 3.75 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 3.03 2.39 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (ppb) 5.98 7.45 8.77 4.71 4.11 <LLOQ(2.11) 3.41 8.70 5.27 3.32 6.01 7.40 5.78 6.82 4.67 2.34 20.2 5.08 PFOSAA* Concentration (PPb) 4.34 3.84 27.6 <LLOQ(2.80) 6.39 3.11 8.78 <LLOQ(2.80) 2.99 3.13 <LLOQ(2.80) <LLOQ(2.80) 6.47 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) 5.88 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) <LLOQ(1.80) <LLOQ(1.80) 7.82 <LLOQ(1.80) <LLOQ(1.80) 2.51 <LLOQ(1.80) 2.96 2.02 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 5.38 4.14 <LLOQ(1.80) 1.93 <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 70 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID PFOS Concentration (PPb) 11064 56.0 11065 56.5 11066 30.1 11067 31.5 11068 6.63 11069 27.6 11070 205 11071 27.6 11072 . 49.4 11073 47.6 11074 29.7 11075 69.7 11076 27.4 11077 42.6 11078 46.9 11079 32.3 11080 43.4 10556 14.1 PFHS* Concentration (PPb) 2.96 2.91 2.27 8.26 <LLOQ(2.09) <LLOQ(2.09) 2.63 2.73 3.74 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.42 <LLOQ(2.09) 5.27 <LLOQ(2.09) 3.88 PFOA* Concentration (ppb) 9.41 3.86 3.69 8.37 <LLOQ(2.11) 5.53 34.1 4.60 14.1 4.78 3.59 6.18 4.63 6.26 6.02 5.79 8.73 4.18 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.23 <LLOQ(2.80) 5.28 <LLOQ(2.80) <LLOQ(2.80) 3.35 3.67 5.54 <LLOQ(2.80) 4.38 3.88 3.44 <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) 5.29 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.89 <LLOQ(1.80) 2.13 3.35 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.89 <LLOQ(1.80) 3.46 2.01 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 71 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ED 10557 PFOS Concentration (ppb) 22.5 10558 33.1 10559 35.4 10560 16.9 10561 40.0 10562 25.3 10563 56.0 10564 18.1 10565 47.2 10566 29.5 10567 23.3 10568 13.6 10569 18.5 10570 19.9 10571 20.7 10572 26.0 10573 30.6 10574 21.1 PFHS* Concentration (PPb) 2.42 PFOA* Concentration (PPb) 5.84 10.4 8.55 12.6 3.55 <LLOQ(2.09) 3.37 2.38 10.5 2.09 ' 4.54 3.49 7.83 <LLOQ(2.09) 5.37 6.23 8.44 3.55 10.0 2.37 6.88 <LLOQ(2.09) 2.21 2.41 3.43 <LLOQ(2.09) 3.53 2.81 3.77 5.16 4.30 2.10 6.29 <LLOQ(2.09) 3.19 PFOSAA* Concentration (ppb) 2.81 3.51 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.48 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 4.07 <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) <LLOQ(1.80) 4.26 <LLOQ(1.80) 2.47 2.40 2.60 <LLOQ(1.80) <LLOQ(1.80) 2.57 2.64 5.88 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.31 <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 72 Northwest Bioanalytical Sample ID 10575 PFOS Concentration (PPb) <LLOQ(4.27) 10576 20.3 10577 23.6 10578 63.7 10579 37.4 10580 44.1 10581 9.83 10582 25.7 10583 39.2 10584 13.5 10585 37.6 10586 32.1 10587 11.0 10588 18.1 10589 37.2 10590 52.6 10591 38.2 10592 51.7 Study No. N W B S00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (PPb) <LLOQ(2.09) 3.13 2.54 5.97 2.28 <LLOQ(2.09) <LLOQ(2.09) 2.10 2.56 <LLOQ(2.09) 3.67 2.71 8.05 <LLOQ(2.09) 4.96 8.80 4.18 11.2 PFOA* Concentration (ppb) <LLOQ(2.11) 4.17 4.60 9.31 7.36 6.25 5.84 4.11 9.18 ' 4.81 7.23 3.87 3.50 6.97 6.73 .11.8 6.75 13.6 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) 2.92 5.14 <LLOQ(2.80) 3.24 2.92 <LLOQ(2.80) 3.26 <LLOQ(2.80) 4.84 <LLOQ(2.80) <LLOQ(2.80) 3.10 4.40 <LLOQ(2.80) 3.29 2.98 PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.37 3.16 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 3.19 <LLOQ(1.80) 1.89 <LLOQ(1.80) 3.41 <LLOQ(1.80) 5.84 4.29 19.0 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 73 Northwest Bioanalytical Sample ID PFOS Concentration (PPb) 10593 30.9 10594 74.2 10595 37.1 10596 21.8 10597 14.3 10598 29.9 10599 18.0 10600 47.7 10601 43.5 10602 20.8 10603 23.5 10604 10.2 10605 25.2 10606 27.6 10607 36.7 10608 30.8 10609 29.7 10610 65.8 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Study No. NWBSOO-128 Report No. NWBRO1-066 PFHS* Concentration (PPb) 6.75 10.2 2.56 2.39 <LLOQ(2.09) 2.89 2.51 3.16 <LLOQ(2.09) 3.20 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(1.36) 3.62 1.72 2.76 1.87 PFOA* Concentration (ppb) 6.20 13.9 4.59 3.91 3.36 9.69 4.10 7.19 3.04 5.09 5.23 2.67 3.49 7.16 7.89 8.13 6.53 13.7 PFOSAA* Concentration (ppb) <LLOQ(2.80) 6.71 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.58 3.13 <LLOQ(2.80) 3.35 3.24 3.01 <LLOQ(1.60) <LLOQ( 1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) <LLOQ(1.80) 2.11 <LLOQ(1.80) 2.40 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 3.78 2.05 1.93 <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 serum calibration curves (see Results and Discussion section). and M570 obtained using plasma calibration curves may vary from results obtained using Page 74 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 10611 PFOS Concentration (ppb) 22.2 10612 32.0 10613 67.6 10614 57.6 10615 36.0 10616 27.7 10617 25.8 10619 22.7 10620 54.3 10621 14.0 10622 35.5 10623 11.7 10624 25.3 10625 35.2 10626 41.7 10627 31.8 10628 25.4 10629 36.3 PFHS* Concentration (PPb) <LLOQ(1.36) 11.4 1.49 5.36 <LLOQ(1.36) <LLOQ(1.36) 3.31 2.16 6.80 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) 3.70 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) 2.84 <LLOQ(1.36) PFOA* Concentration (PPb) 5.82 7.23 10.7 10.1 4.01 5.76 5.24 4.40 9.52 2.47 6.63 4.13 5.89 4.17 7.28 6.28 6.87 4.55 PFOSAA* Concentration (PPb) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 2.42 <LLOQ(1.60) 2.59 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) PFOSA* Concentration (PPb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556* Concentration (ppb) M570* Concentration (ppb) <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) 3.92 <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) 13.0 <LLOQ(3.20) . <LLOQ(1.80) <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) 2.39 <LLOQ(3.20) 3.36 <LLOQ(3.20) 1.88 <LLOQ(3.20) 4.42 <LLOQ(3.20) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Seram 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 75 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) AH concentrations are expressed as ppb. Sample ID 10630 PFOS Concentration (PPb) 30.3 10631 54.1 10632 41.4 10633 87.2 10634 10635 30.6 36.8 10636 26.3 10637 10638 12.7 45.2 10639 44.7 10640 19.3 10641 19.8 10642 80.9 10643 10644 40.5 23.9 10645 26.5 10646 48.7 10647 26.7 PFHS* Concentration (ppb) 1.99 1.51 1.47 <LLOQ(1.36) <LLOQ(1.36) 1.79 1.84 <LLOQ(1.36) 2.80 <LLOQ(1.36) 2.36 <LLOQ(1.36) 2.08 2.29 3.45 <LLOQ(1.36) 1.60 1.40 PFOA* Concentration (PPb) 4.65 8.91 5.23 5.48 7.36 5.27 3.48 3.52 8.02 9.13 4.73 3.07 5.93 7.21 7.29 5.04 10.5 7.51 PFOSAA* Concentration (PPb) <LLOQ(1.60) 2.28 <LLOQ(1.60) 2.35 <LLOQ(1.60) <LLOQ(1.60) 3.32 1.61 1.62 4.68 <LLOQ(2.80) 1.78 2.99 2.45 <LLOQ(1.60) <LLOQ(1.60) 3.00 3.34 PFOSA* Concentration (PPb) <LLOQ(1.0Q) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.40) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) <LLOQ(1.80) <LLOQ(1.80) 3.03 2.65 <LLOQ(1.80) <LLOQ(1.80) 2.67 <LLOQ(1.80) <LLOQ(1.80) 2.12 <LLOQ(1.80) 1.83 3.65 <LLOQ(1.80) 2.41 <LLOQ(1.80) 3.48 6.35 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 76 Northwest Bioanalytical Sample ID PFOS Concentration (PPb) 10648 16.7 10649 39.0 10650 14.3 10651 28.6 10652 32.7 10653 11.7 10654 28.5 10655 15.9 10656 33.9 10657 48.1 10658 45.7 10659 18.7 10660 26.1 10661 28.6 10662 44.5 10663 26.9 10664 31.4 10665 44.9 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Study No. NWBS00-128 Report No. NWBRO1-066 PFHS* Concentration (PPb) <LLOQ(1.36) 1.58 <LLOQ(1.36) 1.36 2.12 <LLOQ(1.36) 2.19 2.64 2.23 3.02 3.79 2.94 6.70 2.68 <LLOQ(2.09) 2.85 <LLOQ(2.09) 2.57 PFOA* Concentration (ppb) 3.49 10.1 2.86 5.69 11.4 2.13 11.4 4.26 2.14 . 3.46 5.80 4.57 4.58 5.56 6.28 2.80 3.28 5.48 PFOSAA* Concentration (ppb) 4.28 4.64 <LLOQ(1.60) <LLOQ(1.60) 2.81 <LLOQ(1.60) 2.43 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 5.09 <LLOQ(2.80) 4.40 PFOSA* Concentration (ppb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) 2.95 <LLOQ(1.80) 1.84 <LLOQ(1.80) 2.51 9.66 2.83 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 4.30 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f die 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 serum calibration curves (see Results and Discussion section) Page 77 Northwest Bioanalytical Study No. N W B S00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 10666 PFOS Concentration (ppb) 29.9 10667 40.8 10668 19.8 10328 24.3 10329 50.6 10330 47.7 10331 31.7 10332 30.8 10333 31.9 10334 24.6 10335 19.3 10336 42.5 10337 32.1 10338 19.3 10339 28.4 10340 39.2 10341 14.8 10342 23.1 PFHS* Concentration (PPb) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(1.36) 3.86 3.50 8.44 5.15 1.65 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) 1.52 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) 4.89 . PFOA* Concentration (PPb) 4.65 4.41 4.30 4.90 7.92 18.7 5.39 4.08 4.05 3.23 3.20 3.62 5.76 2.46 4.59 5.02 3.84 8.59 PFOSAA* Concentration (PPb) 4.52 <LLOQ(2.80) <LLOQ(2.80) 2.59 4.83 5.56 <LLOQ(1.60) 1.87 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 2.22 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 4.66 <LLOQ(1.60) 2.17 PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <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) <LLOQ(2.50) <LLOQ(2.50) M570* Concentration (Ppb) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.00) 1.95 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 1.76 <LLOQ( 1.00) <LLOQ(1.00) 1.21 6.28 3.92 <LLOQ( 1.00) 1.35 <LLOQ(1.00) <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) o f 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 78 Northwest BioanalyticaJ Sample PFOS ID Concentration (ppb) 10343 29.6 10344 44.9 10345 45.6 10346 39.8 10347 14.7 10348 17.7 10349 33.0 10350 30.5 10351 34.8 10352 18.0 10353 23.8 10354 31.6 10355 95.7 10356 26.5 10357 22.0 10358 43.5 10359 71.0 10360 17.0 Study No. N W B S00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) <LLOQ(1.36) <LLOQ(1.36) 2.07 2.44 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) 2.58 6.40 <LLOQ(2.09) 2.02 3.17 1.43 <LLOQ(1.36) <LLOQ(1.36) 4.08 1.37 <LLOQ(1.36) PFOA* Concentration (ppb) 6.45 3.03 5.74 4.38 2.28 3.58 4.94 2.35 3.95 <LLOQ(2.11) 6.55 4.74 10.7 3.80 4.05 4.92 5.30 4.90 PFOSAA* Concentration (ppb) 3.42 4.92 <LLOQ(1.60) 1.83 <LLOQ(1.60) <LLOQ(1.60) 2.05 4.32 <LLOQ(1.60) <LLOQ(2.80) <LLOQ(1.60) <LLOQ(1.60) 2.38 <LLOQ(1.60) 1.84 3.40 1.96 1.79 PFOSA* Concentration (PPb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.40) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556* Concentration (PPb) <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(3.20) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570* Concentration (ppb) 1.50 2.51 <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) 2.83 1.39 5.37 3.17 <LLOQ(1.80) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ( 1.00) <LLOQ( 1.00) <LLOQ(1.00) 1.51 1.03 1.28 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 79 Northwest Bioanalytical Sample ID 10361 PFOS Concentration (Ppb) 7.70 10362 41.7 10363 34.7 10364 22.8 10365 22.6 10366 21.9 10367 17.7 10368 74.3 10369 18.1 10370 24.7 10371 71.8 10372 59.5 10373 52.8 10374 ' 29.7 10375 49.2 10376 21.1 10377 88.4 10378 100 Study No. N W B S00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (PPb) <LLOQ(1.36) 3.02 1.41 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) <LLOQ(2.09) <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) 7.12 12.0 3.87 <LLOQ(1.36) 10.8 <LLOQ(1.36) 6.67 1.37 PFOA* Concentration (PPb) 2.53 5.90 4.93 3.92 3.07 4.96 <LLOQ(2.11) 9.98 3.53 3.98 7.18 5.03 20.0 4.85 4.40 3.54 15.8 5.57 PFOSAA* Concentration (PPb) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 1.83 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(2.80) 10.3 <LLOQ(1.60) 2.75 5.41 <LLOQ(1.60) 1.79 1.94 <LLOQ(1.60) <LLOQ(1.60) 7.53 4.93 PFOSA* Concentration (Ppb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.40) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.-00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556* Concentration (PPb) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(3.20) <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) M570* Concentration (PPb) <LLOQ(1.00) 3.01 1.59 <LLOQ(1.00) 1.85 <LLOQ(1.00) <LLOQ(1.80) <LLOQ(1.00) 3.02 <LLOQ(1.00) 3.89 2.62 10.6 <LLOQ(1.00) 2.20 1.62 2.31 1.52 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 80 Northwest Bioanalytical Sample ID PFOS Concentration (ppb) 10379 54.6 10380 31.3 10381 34.8 10382 35.8 10383 15.6 10384 24.7 10385 28.3 10386 41.4 10387 11.7 10388 79.1 10389 28.4 10390 15.8 10391 48.4 10392 55.5 10393 20.9 10394 21.7 10395 40.0 10396 36.3 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Study No. NWBSOO-128 Report No. NWBRO1-066 PFHS* Concentration (PPb) <LLOQ(1.36) 1.49 <LLOQ(1.36) 1.72 <LLOQ(1.36) <LLOQ(1.36) 2.03 5.75 <LLOQ(1.36) <LLOQ(2.09) 1.60 <LLOQ(1.36) 2.45 1.61 1.41 1.65 4.73 1.81 PFOA* Concentration (PPb) 3.88 4.22 3.92 2.81 2.80 2.56 4.89 3.30 2.43 5.93 4.29 3.09 7.41 5.34 2.91 2.18 4.92 5.66 PFOSAA* Concentration (PPb) 3.27 <LLOQ(1.60) 2.56 <LLOQ(1.60) <LLOQ(1.60) 2.34 <LLOQ(1.60) 8.31 <LLOQ(1.60) 4.38 <LLOQ(1.60) <LLOQ(1.60) 3.27 2.54 1.98 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) PFOSA* Concentration (ppb) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.40) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556* Concentration (ppb) <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(3.20) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570* Concentration (ppb) <LLOQ(1.00) 1.72 1.69 1.70 2.84 <LLOQ( 1.00) 1.40 1.33 <LLOQ(1.00) <LLOQ(1.80) 1.29 2.42 3.07 4.03 3.12 <LLOQ(1.00) 1.41 2.32 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 cutwes may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 81 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID PFOS Concentration (PPb) 10397 28.2 10398 36.9 10399 38.9 10400 27.5 10401 32.0 10402 25.2 ' 10403 34.3 10404 30.6 10405 36.5 10406 24.1 10407 27.0 10408 80.4 10409 28.8 10410 88.8 10411 32.3 10412 53.5 10413 16.8 10414 27.0 PFHS* Concentration (ppb) 6.51 5.10 5.63 <LLOQ(1.36) 2.79 <LLOQ(1.36) 3.92 3.56 1.69 6.87 <LLOQ(1.36) 1.90 1.61 15.2 <LLOQ(1.36) 1.87 <LLOQ(1.36) <LLOQ(1.36) PFOA* Concentration (ppb) 4.57 5.59 3.38 4.57 5.63 <LLOQ(1.92) 2.97 2.78 7.05 6.27 4.62 10.6 3.49 13.8 3.26 8.98 2.53 3.17 PFOSAA* Concentration (PPb) <LLOQ(1.60) <LLOQ(1.60) 2.00 1.72 <LLOQ(2.80) 2.12 <LLOQ(1.60) 4.71 <LLOQ(1.60) 1.78 2.44 2.83 1.75 3.43 1.68 7.34 <LLOQ(1.60) 2.57 PFOSA* Concentration (ppb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.40) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556* Concentration (PPb) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(3.20) <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) M570* Concentration (ppb) 1.62 4.39 <LLOQ(1.00) 1.34 <LLOQ(1.80) 4.05 <LLOQ(1.00) 1.34 <LLOQ(1.00) 2.03 6.76 1.81 <LLOQ(1.00) 4.60 <LLOQ(1.00) 3.45 <LLOQ(1.00) 1.42 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 82 Northwest Bioanalytical Study No. N W B S00-128 Repon No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 10415 PFOS Concentration (ppb) 207 10416 17.2 10417 37.7 10418 29.1 10419 30.6 10420 56.6 10421 33.6 10422 14.4 10423 36.7 10424 38.8 10425 30.8 10426 115 10427 57.7 11883 17.8 11884 26.1 11885 26.5 11886 26.6 11887 60.1 PFHS* Concentration (ppb) 2.09 <LLOQ(1.36) 4.54 <LLOQ(1.36) <LLOQ(1.36) 2.70 1.83 <LLOQ(1.36) <LLOQ(1.36) 1.39 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (ppb) 14.9 <LLOQ(1.92) 4.28 4.43 2.82 11.5 4.61 2.40 5.76 3.38 3.59 10.3 5.95 2.40 <LLOQ(2.11) 6.13 4.07 26.7 PFOSAA* Concentration (PPb) 7.76 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 2.58 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 12.9 1.91 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (PPb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) <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) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 5.07 1.63 1.78 <LLOQ(1.00) 3.20 7.63 <LLOQ(1.00) 2.21 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.93 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 83 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBR01-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 11888 PFOS Concentration (PPb) 91.8 11889 33.8 11890 23.2 11891 71.3 11892 30.2 11893 35.0 11894 22.0 11895 12.5 11896 34.2 10756 166 10757 77.9 10758 133 10759 160 10760 38.1 10761 90.5 10762 41.7 10763 36.4 10764 30.3 PFHS* Concentration (ppb) 7.34 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 3.60 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 4.51 4.27 11.6 2.78 1.71 1.50 <LLOQ( 1.36) <LLOQ(1.36) <LLOQ(1.36) PFOA* Concentration (ppb) 10.1 5.85 3.64 6.40 7.40 4.90 4.55 4.48 4.71 29.0 11.7 6.25 15.3 5.39 8.54 6.09 6.25 3.29 PFOSAA* Concentration (ppb) 3.64 3.43 <LLOQ(2.80) 4.04 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 60.1 52.9 7.18 8.11 <LLOQ(1.60) 12.2 1.80 <LLOQ(1.60) <LLOQ(1.60) PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) 12.9 9.21 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570* Concentration (PPb) 13.3 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.90 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 3.75 <LLOQ(1.00) 5.21 1.28 1.55 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <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) o f 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 vaiy from results obtained using serum calibration curves (see Results and Discussion section). Page 84 Northwest Bioanalytical Study No. N W B S00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 10765 PFOS Concentration (ppb) 96.1 10766 40.7 10767 34.1 10768 28.1 10769 54.7 10770 42.7 10771 26.8 10772 36.1 10773 66.6 10774 77.2 10775 46.8 10776 159 10777 49.1 10778 31.0 10779 22.7 10780 10781 57.3 43.9 10782 79.0 PFHS* Concentration (PPb) 3.73 7.70 <LLOQ(1.36) 4.56 4.64 <LLOQ(1.36) 1.57 2.00 15.6 2.25 <LLOQ(1.36) 4.24 2.76 <LLOQ(1.36) <LLOQ(1.36) 3.76 2.78 4.71 PFOA* Concentration (PPb) 11.7 6.54 6.81 5.96 6.69 4.14 4.70 4.34 5.78 8.75 9.30 29.8 6.08 2.21 5.12 7.72 6.04 9.85 PFOSAA* Concentration (PPb) 1.75 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 2.19 <LLOQ(1.60) <LLOQ(1.60) 3.44 2.89 8.08 8.98 56.6 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 3.56 1.68 3.38 PFOSA* Concentration (PPb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556* Concentration (ppb) <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) 12.2 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570* Concentration (PPb) 2.82 <LLOQ(1.00) 1.65 <LLOQ(1.00) 1.18 1.59 4.22 <LLOQ(1.00) 2.77 1.86 <LLOQ(1.00) 2.45 <LLOQ(1.00) 2.07 <LLOQ( 1.00) 1.73 <LLOQ(1.00) <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) o f 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 85 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 10783 PFOS Concentration (PPb) 54.2 10784 37.3 10785 31.6 10786 38.9 10787 73.0 10788 33.8 10789 49.3 10790 55.2 10791 69.8 10792 22.0 10793 31.1 10794 74.2 10795 105 10796 40.2 10797 52.5 10798 58.2 10799 117 10800 75.1 PFHS* Concentration (ppb) 1.78 2.12 1.91 5.22 6.27 2.19 2.00 <LLOQ(1.36) 2.67 1.38 1.64 3.86 2.09 19.8 4.12 4.96 1.70 3.15 PFOA* Concentration (ppb) 7.46 5.89 4.88 4.79 18.2 5.34 7.30 6.45 7.16 4.02 5.08 10.6 5.51 8.76 4.32 7.87 13.1 8.95 PFOSAA* Concentration (PPb) 4.60 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 2.28 <LLOQ(1.60) 1.95 4.51 2.36 <LLOQ(1.60) 2.31 13.7 1.96 2.09 1.76 1.81 5.44 8.62 PFOSA* Concentration (ppb) <LLOQ(1.00) <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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556* Concentration (ppb) <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) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570* Concentration (ppb) 2.05 <LLOQ(1.00) <LLOQ( 1.00) 1.98 2.16 <LLOQ(1.00) 1.61 <LLOQ(1.00) 1.57 1.21 <LLOQ(1.00) <LLOQ(1.00) 2.67 <LLOQ(1.00) 4.69 1.97 1.27 2.97 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 86 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID PFOS Concentration (pph) 10801 48.7 10802 33.3 10803 32.6 10804 68.5 10805 45.5 10806 110 10807 33.9 10808 40.3 10809 29.8 10810 42.9 10811 32.6 10812 69.9 10813 27.4 10814 38.4 10815 55.1 10816 50.1 10817 106 10818 67.6 PFHS* Concentration (ppb) 2.48 <LLOQ(1.36) 8.59 <LLOQ(1.36) 4.35 11.5 3.52 1.86 1.79 <LLOQ(2.09) <LLOQ(2.09) 3.77 <LLOQ(2.09) 2.82 <LLOQ(2.09) 4.39 4.58 9.17 PFOA* Concentration (PPb) 6.21 4.47 4.31 17.8 6.93 21.8 7.08 2.70 4.72 3.54 4.45 7.50 2.85 6.57 8.35 2.60 7.17 11.4 PFOSAA* Concentration (Ppb) <LLOQ(1.60) 6.91 <LLOQ(1.60) 3.71 <LLOQ(1.60) 3.35 <LLOQ(1.60) <LLOQ(1.60) 3.58 3.58 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 6.45 4.05 3.04 3.25 <LLOQ(2.80) PFOSA* Concentration (PPb) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) M570* Concentration (PPb) <LLOQ(2.50) 1.22 <LLOQ(2.50) 2.16 <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) 3.03 <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) 5.59 <LLOQ(2.50) 1.68 <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) 2.99 <LLOQ(3.20) 2.46 <LLOQ(3.20) 1.95 <LLOQ(3.20) 3.66 <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) , 5.68 <LLOQ(3.20) <LLOQ(1.80) <LLOQ(3.20) 5.34 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 87 Northwest Bioanalytical Study No. N W B S00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 10819 PFOS Concentration (PPb) 37.1 10820 71.0 10821 45.3 10822 54.4 10823 35.9 10824 109 10825 72.7 10826 30.6 10827 59.4 10828 143 10829 Not Received 10830 34.3 10831 75.8 10832 44.5 10833 68.9 10834 10835 49.8 71.3 10836 35.5 PFHS* Concentration (ppb) <LLOQ(2.09) 2.96 <LLOQ(2.09) 10.7 <LLOQ(2.09) <LLOQ(2.09) 14.1 2.47 5.37 3.33 Not Received 4.97 9.32 4.10 3.29 5.53 4.02 3.82 PFOA* Concentration (ppb) 4.65 3.88 4.17 7.46 7.14 6.50 6.90 3.42 8.35 13.4 Not Received 5.75 13.5 4.87 10.7 3.62 10.7 4.66 PFOSAA* Concentration (ppb) 3.21 4.70 <LLOQ(2.80) 15.1 <LLOQ(2.80) 9.12 <LLOQ(2.80) 3.76 6.62 8.59 Not Received <LLOQ(2.80) 4.28 <LLOQ(2.80) 3.51 5.10 <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) Not Received <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) 3.91 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) Not Received <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (Ppb) <LLOQ(1.80) 2.09 <LLOQ(1.80) 4.37 5.51 4.18 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 4.03 Not Received 8.31 5.26 <LLOQ(1.80) 10.8 <LLOQ(1.80) 4.47 <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 88 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample . PFOS ID Concentration (PPb) 10837 Not Received 10838 36.5 10839 Not Received 10840 34.1 10841 68.2 10842 154 10843 41.8 10844 70.7 10845 Not Received 10846 65.8 10847 92.4 10848 44.2 10849 51.5 10850 10851 40.7 70.5 10852 19.3 10853 31.7 10854 50.5 PFHS* Concentration (PPb) Not Received 7.12 Not Received 2.50 22.4 12.1 2.34 9.59 Not Received 18.7 12.9 <LLOQ(2.09) 2.98 <LLOQ(2.09) 4.00 <LLOQ(2.09) <LLOQ(2.09) 2.46 PFOA* Concentration (PPb) Not Received 8.60 Not Received 6.97 5.68 18.2 4.37 14.9 Not Received 13.3 9.46 3.27 7.02 <LLOQ(2.11) 6.49 2.95 4.70 3.97 PFOSAA* Concentration (ppb) Not Received <LLOQ(2.80) Not Received <LLOQ(2.80) 4.33 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) Not Received 2.85 4.10 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.65 PFOSA* Concentration (PPb) Not Received <LLOQ(1.40) Not Received <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) Not Received <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (Ppb) Not Received <LLOQ(3.20) Not Received <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) Not Received <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) Not Received 5.75 Not Received 2.83 <LLOQ(1.80) <LLOQ(1.80) 8.20 6.61 Not Received 2.83 3.57 <LLOQ(1.80) 1.99 <LLOQ(1.80) 2.11 <LLOQ(1.80) 3.44 <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 89 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) ' A ll concentrations are expressed as ppb. Sample ID 10855 PFOS Concentration (ppb) 18.5 10856 36.3 10857 81.9 10858 54.7 10859 19.5 10860 Not Received 10861 39.9 10862 37.8 10863 70.6 10864 58.3 10865 56.8 10866 24.0 10867 57.4 10868 22.9 11649 17.6 11650 28.3 11651 48.8 11652 23.5 PFHS* Concentration (ppb) <LLOQ(2.09) 7.00 2.48 <LLOQ(2.09) <LLOQ(2.09) Not Received 2.57 4.03 <LLOQ(2.09) 2.34 6.25 <LLOQ(2.09) 2.28 4.80 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (PPb) 2.16 4.66 12.0 4.82 <LLOQ(2.11) Not Received 3.35 4.23 4.20 3.80 3.85 3.03 5.32 3.46 3.96 3.49 4.07 2.71 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) Not Received 5.15 <LLOQ(2.80) 3.11 <LLOQ(2.80) 24.7 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.20 3.24 25.1 <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) Not Received <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ( 1.4.0) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) Not Received <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) 3.88 <LLOQ(3.20) 5.12 <LLOQ(3.20) M570* Concentration (PPb) 2.53 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) Not Received 3.21 2.23 3.10 <LLOQ(1.80) <LLOQ(1.80) 2.35 3.95 2.79 <LLOQ(1.80) 2.06 <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 90 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID PFOS Concentration (ppb) 11653 25.2 11654 329 11655 31.2 11656 31.5 11657 70.3 11658 27.4 11659 43.9 11660 17.7 11661 46.4 11662 44.6 11663 14.0 11664 64.1 11665 45.0 11666 37.7 11667 9.45 11668 29.9 11669 31.9 11670 28.3 PFHS* Concentration (PPb) <LLOQ(2.09) 6.91 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.54 11.8 <LLOQ(2.09) <LLOQ(2.09) 10.9 <LLOQ(2.09) 2.48 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (PPb) 4.76 16.7 3.77 3.13 6.63 2.94 3.61 3.13 3.91 4.92 3.77 6.96 4.49 5.07 <LLOQ(2.11) 3.81 6.28 4.08 PFOSAA* Concentration (PPb) 3.89 36.9 <LLOQ(2.80) <LLOQ(2.80) 13.3 <LLOQ(2.80) <LLOQ(2.80) 3.42 4.90 2.82 4.98 9.91 5.04 2.83 <LLOQ(2.80) 5.86 3.77 2.92 PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I,40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) 12.2 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) 4.21 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.96 <LLOQ(1.80) <LLOQ(1.80) 2.43 <LLOQ(1.80) 2.63 2.06 <LLOQ(1.80) 2.03 <LLOQ(1.80) 2.86 <LLOQ(1.80) 1.82 <LLOQ(1.80) 3.64 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 91 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID PFOS Concentration (PPb) 11671 37.7 11672 30.7 11673 36.2 11674 37.5 11675 14.2 11676 12.0 11677 43.4 11678 32.2 11679 17.0 11680 44.5 11681 15.8 11682 9.20 11683 40.3 11684 42.3 11685 24.4 11686 14.6 11687 36.1 11688 17.2 PFHS* Concentration (ppb) 2.16 <LLQQ(2.09) <LLOQ(2.09) 3.91 3.99 <LLOQ(2.09) 3.22 3.83 <LLOQ(2.09) 7.24 <LLOQ(2.09) <LLOQ(2.09) 8.61 <LLOQ(2.09) <LLOQ(2.09) 4.12 2.11 <LLOQ(2.09) PFOA* Concentration (ppb) 4.44 5.43 2.68 4.44 3.22 2.33 3.60 3.57 2.56 6.79 5.41 <LLOQ(2.11) 6.21 4.48 2.34 5.38 4.10 <LLOQ(2.11) PFOSAA* Concentration (PPb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.39 2.96 <LLOQ(2.80) 5.66 <LLOQ(2.80) <LLOQ(2.80) 4.72 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 4.43 PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) <LLOQ(1.80) 2.37 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.65 <LLOQ(1.80) 2.62 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 92 Northwest Bioanalytical Study No. N W B S00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID PFOS Concentration (ppb) 11689 1656** 11690 25.6 11691 24.4 11692 14.2 11693 27.1 11694 33.4 11695 20.8 11696 14.5 11697 108 11698 124 11699 22.9 11700 25.5 11701 14.1 11702 39.0 11703 12.0 11704 78.7 11705 12.0 PFHS* Concentration (ppb) 9.87 <LLOQ(2.09) 2.59 <LLOQ(2.09) 2.58 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.28 <LLOQ(2.09) <LLOQ(2.09) 3.27 <LLOQ(2.09) 6.54 <LLOQ(2.09) PFOA* Concentration (ppb) 4.32 2.92 3.13 2.71 3.91 <LLOQ(2.11) 3.04 <LLOQ(2.11) 12.2 12.0 4.24 3.48 3.11 5.61 <LLOQ(2.11) 12.9 3.09 PFOSAA* Concentration (PPb) <LLOQ(2.80) <LLOQ(2.80) 3.88 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.03 13.0 9.58 <LLOQ(2.80) 5.45 <LLOQ(2.80) 6.74 2.97 15.6 <LLOQ(2.80) PFOSA* Concentration (Ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) 3.58 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) ** Concentration corrected for amount o f persistent PFOS in dilution matrix. M570* Concentration (PPb) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.14 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.07 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(l .80) <LLOQ(1.80) 3.70 <LLOQ(1.80) 3.68 <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 93 Northwest Bioanalytical Sample ID 11706 PFOS Concentration (PPb) 22.3 11707 17.5 11708 14.5 11709 43.5 11710 35.9 11711 30.3 11712 11.1 11713 50.8 11714 18.4 11715 36.8 11716 12.6 11717 13.2 11718 17.6 11719 16.1 11720 25.2 11721 37.4 11722 8.26 11723 30.2 Study No. N W B S00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (PPb) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 3.37 <LLOQ(2.09) <LLOQ(2.09) 3.76 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.25 <LLOQ(2.09) <LLOQ(2.09) 2.26 <LLOQ(2.09) 5.64 PFOA* Concentration (ppb) 3.35 3.87 2.43 5.13 2.90 3.45 3.39 11.2 3.80 4.04 <LLOQ(2.11) <LLOQ(2.11) 5.15 3.22 2.11 4.13 2.53 4.19 PFOSAA* Concentration (PPb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.48 <LLOQ(2.80) 20.6 6.13 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 2.63 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.21 PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ'(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) 1.96 <LLOQ(1.80) 4.82 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 5.27 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.55 5.50 <LLOQ(1.80) <LLOQ(1.80) 1.95 <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 M 570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 94 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) AH concentrations are expressed as ppb. Sample ID PFOS Concentration (ppb) 11725 16.6 11726 20.2 11727 25.7 11729 21.6 11731 63.4 11732 30.3 11735 20.5 11739 54.6 11745 26.9 11746 24.6 11748 31.1 11749 17.6 11750 20.8 11751 6.60 11752 45.3 11753 29,2 11754 37.8 11756 36.4 y PFHS* Concentration (PPb) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 4.77 <LLOQ(2.09) <LLOQ(2.09) 9.42 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 5.48 <LLOQ(2.09) <LLOQ(2.09) 3.61 <LLOQ(2.09) 4.53 PFOA* Concentration (PPb) <LLOQ(2.11) 2.78 8.48 4.08 10.2 4.07 3.05 5.41 4.97 3.76 3.31 4.36 4.37 <LLOQ(2.11) 4.09 2.28 3.66 8.37 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) 2.90 7.58 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 5.86 4.48 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 2.95 7.38 3.59 PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) <LLOQ(1.80) 2.68 <LLOQ(1.80) 3.10 2.85 <LLOQ(1.80) <LLOQ(1.80) 2.06 <LLOQ(1.80) <LLOQ(1.80) 1.94 <LLOQ(1.80) 1.85 2.05 <LLOQ(1.80) <LLOQ(1.80) 6.89 NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 95 Northwest Bioanalytical Study No. N W B S00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID PFOS Concentration (Ppb) 11757 34.1 11758 24.8 11759 17.9 11761 17.2 11762 20.0 11763 28.3 11765 22.3 11766 49.1 11767 16.6 11768 14.8 11769 26.0 11771 6.03 11772 40.4 11773 9.26 11156 44.3 11157 28.0 11158 21.5 11159 40.0 PFHS* Concentration (Ppb) 6.63 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 4.13 <LLOQ(2.09) <LLOQ(2.09) 2.16 4.10 3.04 PFOA* Concentration (PPb) 3.58 4.65 4.20 <LLOQ(2.11) 2.82 6.68 2.62 4.74 2.97 2.52 4.17 2.76 7.03 <LLOQ(2.11) 6.33 3.28 4.16 4.72 PFOSAA* Concentration (Ppb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.20 3.55 4.33 <LLOQ(2.80) 7.58 <LLOQ(2.80) 3.18 3.25 2.81 <LLOQ(2.80) 2.87 3.11 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) 6.60 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) 2.02 2.22 <LLOQ(1.80) 2.59 2.85 2.94 4.62 2.93 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.93 <LLOQ(1.80) 3.84 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 96 Northwest Bioanalytical Study No. NW BS00-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample 11) 11160 PFOS Concentration (ppb) 31.5 11161 20.7 11162 30.9 11163 56.8 11164 76.4 11165 93.3 11166 17.7 11167 11.1 11168 48.1 1.1169 36.6 11170 41.4 11171 48.1 11172 50.3 11173 42.7 11174 65.4 11175 52.6 11176 24.3 11177 30.8 PFHS* Concentration (PPb) <LLOQ(2.09) <LLOQ(2.09) 3.08 2.40 4.42 13.7 3.64 <LLOQ(2.09) 3.33 3.51 <LLOQ(2.09) 5.19 15.3 <LLOQ(2.09) 3.24 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (ppb) 2.74 3.03 6.16 4.63 9.41 5.53 <LLOQ(2.11) <LLOQ(2.11) 4.69 5.19 8.30 4.74 5.31 4.77 6.58 5.50 <LLOQ(2.11) 3.33 PFOSAA* Concentration (PPb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.14 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) MS56* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) <LLOQ(1.80) <LLOQ(1.80) 2.04 <LLOQ(1.80) 4.60 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.97 1.96 <LLOQ(1.80) 3.96 3.37 <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 97 Northwest Bioanalytical Study No. NW BS0-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample PFOS ID Concentration (ppb) 11178 41.0 11179 35.2 11180 28.3 11181 92.8 11182 50.0 11183 37.4 11184 48.8 11185 71.6 11186 21.7 11187 15.1 11188 23.2 11189 52.6 11190 81.9 11191 24.3 11192 27.1 11193 34.3 11194 17.1 11195 45.6 PFHS* Concentration (PPb) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 12.4 25.7 5.94 9.40 4.31 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (ppb) 9.73 3.68 3.44 4.16 14.2 <LLOQ(2.11) 5.68 9.01 4.50 <LLOQ(2.11) <LLOQ(2.11) 13.2 6.91 - 3.26 5.59 7.09 <LLOQ(2.11) 7.49 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 9.91 <LLOQ(2.80) <LLOQ(2.80) 2.92 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) 3.84 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) 2.88 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.97 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 7.86 3.99 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 98 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID PFOS Concentration (ppb) 11196 18.2 11197 21.4 11198 38.2 11199 28.8 11200 26.2 11201 24.1 11202 42.1 11203 25.2 11204 31.1 11205 12.8 11206 24.3 11207 44.2 11208 15.9 11209 25.7 11210 29.3 11211 47.5 11212 69.6 11213 51.9 PFHS* Concentration (PPb) <LLOQ(2.09) <LLOQ(2.09) 11.1 <LLOQ(2.09) <LLOQ(2.09) 4.20 10.7 2.79 3.27 2.26 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 4.41 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (PPb) 4.69 3.76 3.02 <LLOQ(2.11) 2.87 3.00 6.93 3.45 5.55 2.47 6.67 5.25 3.61 4.69 4.32 2.81 7.25 5.10 PFOSAA* Concentration (PPb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 4.64 . <LLOQ(2.80) 3.34 3.98 PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(l .40) <LLOQ(1.40) <LLOQ(1.40) 2.09 <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (Ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (PPb) <LLOQ(1.80) 2.07 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.96 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 3.30 2.10 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 99 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 11214 PFOS Concentration (PPb) 36.4 11215 122 11216 42.5 11217 41.4 11218 57.9 11219 19.4 11220 29.8 11221 46.0 11222 26.5 11223 41.5 11224 64.9 11225 29.9 11226 18.7 11227 23.1 11228 41.4 11229 45.9 11230 85.2 11231 62.9 PFHS* Concentration (PPb) 6.25 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.91 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 19.2 5.21 66.3 <LLOQ(2.09) <LLOQ(2.09) 2.33 <LLOQ(2.09) 3.22 2.45 2.51 PFOA* Concentration (ppb) 3.57 5.93 5.22 6.32 6.89 <LLOQ(2.11) 2.94 6.44 2.73 5.80 4.30 4.50 5.01 4.61 6.50 5.43 7.01 3.53 PFOSAA* Concentration (ppb) 4.34 3.21 2.98 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 4.60 6.36 PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 3.01 <LLOQ(1.80) 3.12 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 4.02 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.07 2.57 <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 100 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID PFOS Concentration (ppb) 11232 21.6 11233 30.0 11234 39.0 11235 22.0 11236 26.7 11237 80.0 11238 37.8 11239 24.7 11240 37.2 11241 139 11242 65.9 11243 27.0 11244 64.9 11245 29.7 11246 28.2 11247 19.0 11248 36.2 11249 36.3 PFHS* Concentration (PPb) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.23 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.64 <LLOQ(2.09) 5.3 9.47 <LLOQ(2.09) 3.73 2.22 <LLOQ(2.09) <LLOQ(2.09) 5.00 <LLOQ(2.09) PFOA* Concentration (PPb) 4.87 3.10 4.81 3.39 4.13 9.10 4.97 4.41 3.29 20.6 6.87 3.01 8.74 5.21 2.44 3.14 5.70 5.58 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.18 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.83 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.26 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (PPb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) 4.44 2.15 2.58 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 6.15 2.56 1.88 <LLOQ(1.80) <LLOQ(1.80) 2.49 <LLOQ(1.80) <LLOQ(1.80) 2.17 <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f die 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 101 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBR01-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample ID 11250 PFOS Concentration (ppb) 26.1 11251 34.6 11252 13.1 11253 11254 56.8 50.8 11256 47.8 11257 33.8 11258 23.1 11259 7.63 11260 34.7 11261 12.6 11262 11263 17.7 226 11264 42.2 11265 24.7 11266 11267 27.2 36.8 11268 39.7 PFHS* Concentration (PPb) 4.07 2.19 <LLOQ(2.09) 4.36 <LLOQ(2.09) 7.07 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 4.14 3.80 <LLOQ(2.09) <LLOQ(2.09) 5.11 2.45 <LLOQ(2.09) 11.3 <LLOQ(2.09) PFOA* Concentration (PPb) 2.32 5.07 <LLOQ(2.11) 7.39 4.81 2.64 5.55 4.33 <LLOQ(2.11) 5.12 2.53 4.07 52.3 3.54 5.69 3.47 2.84 2.47 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 21.2 3.65 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 7.22 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556* Concentration (PPb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.87 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 1.86 <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 102 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample PFOS ID Concentration (ppb) 11269 25.2 PFHS* Concentration (ppb) 3.67 PFOA* Concentration (ppb) 2.54 PFOSAA* Concentration (PPb) <LLOQ(2.80) PFOSA* Concentration (PPb) <LLOQ(1.40) M556* Concentration (ppb) <LLOQ(3.20) M570* Concentration (ppb) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f 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 103 Northwest Bioanalytical Table 23. Repeat Analysis Table for PFOS Study No. NW BS00-128 Report No. NWBRO1-066 Sample ED 11689 Original Cone. ppb >ULOQ(414) Original Run Number 10 Reason for Reassay 1 Reassay Cone. Reassay Run ppb Number 1670 17 Reported Cone, ppb 1656* * Concentration corrected for amount o f persistent PFOS in dilution matrix. Reason for Reported Cone. 1 REASONS FOR REASSAY: 1). Greater than the ULOQ. REASONS FOR REPORTED CONC: 1). Original result outside o f quantitation range. Reassay results reported. Page 104 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Figure 1. Representative Calibration Curve for PFOS Analytical Run t analyzed on 27-Nov-2000 Calibration Standards for PFOS (ppb) Regression Method QUADRATIC Weighting Factor l/X**2 Quadratic Limit * S49 InanimaRp Figure 2. Representative Calibration Curve for PFHS Analytical Run 1 analyzed on 27-Nov-2000 Calibration Standards for PFHS (ppb) Regression Method QUADRATIC-Weighting Factor !/X**2 Quadratic Limit 1190 faanm.atR'voa Page 105 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Figure 3. Representative Calibration Curve for PFOA Analytical Run l analyzed on 27-Nov*2000 Calibration Standards for PFOA (ppb) Regression Method * QUADRATIC Weighting Factor * l/X**2 Quadratic Limit * 10400 Figure 4. Representative Calibration Curve for PFOSAA Analytical Run I analyzed on 27-Nov-2000 Calibration Standards for PFOSAA (ppb) Regression Method ~ QUADRATIC - Weighting Factor " l/X**2 Quadratic Limit -1 11000 Page 106 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Figure 5. Representative Calibration Curve for PFOSA Analytical Run I analyzed on 27-Nov-200Q Calibration Standards for PFOSA (ppb) Regression Method QUADRATIC Weighting Factor - l/X**2 Quadratic Limit * 1160 Figure 6. Representative Calibration Curve for M556 Analytical Run 1 analyzed on 27-Nov-2000 Calibration Standards for MS56 (ppb) Regression Method " QUADRATIC - Weighting Factor 1/X**2 Quadratic Limit * <5890 Page 107 Northwest Bioanalytical Study No. NWBS00-I28 Report No. NW BR0I-066 Figure 7. Representative Calibration Curve for M570 Analytical Run I analyzed on 27-Nov-2000 Calibration Standards for M57 (ppb) Regression Method - QUADRATIC *Weighting Factor " l/X**2 Quadratic Limit * 3420 la struma it Response Page 108 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Figure 8. Human Plasma Blank for PFOS IPFOS Internal Standard: FHPfOS Use Area Absolute Retention Time Expected RT 5.31 I Current Method Noise Hires. 5.0 5.0 Quant Hires. 0.2 0.2 Min. Width 33 Mult. Width 12 12 8ase. Width 150 ISO T Win. (secs) 20 20 Smooth J1 ITHPFOS use as Internal Standard Expected RT 4.63 Current Method 3 Noise ~Tnres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 ISO RT Win. (secs) 20 20 Smooth 11 Page 109 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Figure 9. Human Plasma Blank for PFHS [Pf H S Internal Standard: THPFOS Use Aree Absolute Retention fime Expected RT 4.00 Current Method I Noise Hues. 3 0 3.0 Quant Hires. 0.5 0.5 Min. Width 44 Mult. Width 12 12 Base. Width 150 ISO RT Win. (secs! 20 20 Smooth 11 $0012301-011 1 O H S00128 CO N TRO LJH AN K 1 M on. N ov 27. 2000 7:20 PM 8.98 in 1 period 1: 8.98 M R M , 571 scans 399.1V > 8 0 .0 Area 11S9 Start Time End Time Inteeration Width Retention Time Inteeration Tvoe It 14W H S 3.77 4.03 0.27 3.92 A -B B SS .intensity: I1 eps-> iT H P fQ S" use as Internal Standard Expected RT Noise Thres. Quant Thres. Min. Width Mult. Width 8ase. Width RT Win. (secs) Smooth Method 10.0 10.0 0.2 0.2 ____3 _10_ 3 10 150 150 ____20. 1 20 1 $0012B01-011 on1 500128 C 0N TR01.8LA N K 1 M o a N ov 27. 2000 7:20 PM 8.98 in 1 period Ott* N o Comment 285 intensity : 23 cps:_ !: 8.98 M R M . 571 scans 427.(V> 407.0 Area 0 Helht 0 Starr Time End Time Inteeration Width Retention Time inteeration Tvoe ItliH H M ffil 0.00 0.00 0.00 0.00 SB -80 70 ;60 30 40 30- 'so 356 120 ...210 260 422 - 304 10 0 101 201 301 401 :: 301 1.59 3.17 4.74; 6.32, 7.90 Page 110 Northwest Btoanalytical Study No. NWBSOO-128 Report No. NWB RO1-066 Figure 10. Human Plasma Blank for PFOA IP O A A Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 4.59 Current Method I Noise rhres. t o 1.0 Quant Thres. 0.9 0.9 Min. Width 3 3 Mult. Width to 10 Base. Width ISO ISO T win. (secs) 20 20 Smooth 1 1 1 011 SO O I28 C O N TRC X.81 A N K 1 Mon. N ov 27. 2000 7:20 PM 8.98 in 1 period t: 8.98 M R M . 571 scam 413.0*> 169.0 Area 1104 Heieht 147 Start Time End Time Imeeration Width Retention Time Imeeration Tvoe 4.44 4.74 0.30 4.60 A -88 Intensity : 166 cps IT H P fO S use as Internal Standard Expected RT 4.63 Current Method I Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 1S0 ISO T Win. (secs) 20 20 Smooth 11 Page 111 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 FigOure 11. Human Plasma Blank for PFOSAA IT H P fO S use as Internal Standard Expected RT 4.53 Current Method I Noise Three. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 ISO tTW in. (secs) 20 20 Smooth 1 1 t 011 $00128 CON TRO LJ L A N K 1 Mon, N ov 27, 2000 7:20 PM B.98 in 1 period 1: 8.98 M R M , 571 scans 427.0> 407.0 Area 0 Heiehr 0 Start Time End Time Inteeration Width Retention Time Intesration Tvoe Itl+MMOl 0.00 0.00 0.00 0.00 HQ intensity : 23 cps L Page 112 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Figure 1' 2. Human Plasma Blank for PFOSA IPfOSA Internal Standard: fHPfOS Use v e a Absolute Retention Time Expected RT S.70 I Current Method Noise fhres. 2.0 5.0 Quant Thtes. Min. Widlh t o 1.0 Ss Mull. Width 10 10 Base. Width ISO ISO T Win. (sea) 20 20 Smooth t1 $0012001*011 1 011 S00128 C O NTRO t.BLANK 1 M on, N ov 27, 2000 7:20 PM 0.90 in l period 100 1: 0.90 M R M , 571 scans 90 490.O-> 70.0 80- Area 2097 Heiehr 140 Start Time End Time Intecration Width Retention Time Imperation Tvoe S.56 6.07 0.50 S.B0 A * 8B 70. 66 60- 1 X * -* 4- IH Q N o Comment 270 323 207 . t . 5 3.17 4.74 Page 113 Northwest Bioanalytical Study No. NWBS00-I28 Report No. NWBRO1-066 Figure 13. Human Plasma Blank for M556 IM556 Internal Standard: IH P fO S Use Area Absolute Retention Time Expected RT S.37 Current Method Noise Thres. 0.4 0.4 Quant Thres. O.t 0.1 Min. Width 3 3 Mult. Width it 11 8ase. Width 150 ISO RT Win. (sees! 20 20 Smooth 1 ft t O il SCOI2 9 CONTROL BLANK I IT H P fO S u m as Internal Standard Expected RT 4. S3 Current Method I Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width ISO 150 T Win. (secs) 20 20 Smooth 1 1 Page 114 Northwest Bioanalytical Study No. NWBS00-I28 Report No. NWBRO1-066 Figure 14. Human Plasma Blank for M570 IM S7 0 Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5.63 Noise Thres. Quant Thres. Min. Width Mult. Width Base. Width RT Win. (secs) Smooth Method 30 3.0 0.S 0.5 __s. S is IS ISO 150 20 20 1 IT H P fO S use as Internai Standard Expected RT 4.63 Current Method I Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 10 base. Width 150 ISO T Win. (secs) 20 20 Smooth 11 Page 115 Northwest Bioanalytioal Study No. NWBS00-128 Report No. NWBRO1-066 Figure 15. Human Plasma Blank with Internal Standard (QCO) for PFOS IPFOS Internal Standard: THPfOS Use Area Absolute Retention Time Expected RT 5.31 Current Method I Noise Thres. S.O 5.0 Quant Thres, 0.2 0.2 Min. Width 3 3 Mult. Width 12 12 Base. Width 150 150 T Win. (secs) Smooth 20 20 1I IT H P fO S use as Internal Standard Expected RT 4.63 Current Method I Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 150 IT Win. (secs) 20 20 Smooth 1 ! Page 116 Northwest Bioanalytieal Study No. NWBSOO-128 Report No. NWBRO1-066 Figure 16. Human Plasma Blank with Internal Standard (QCO) for PFHS IPFHS Internal Standard: THPfOS Use Area Absolute Retention Time Expected RT 4.00 C urrent Method I Noise rhres. 3.0 Quant Then. 0.5 Min. Width Mult. Width 4 12 Base. Width ISO RT Win. (sea) Smooth 20 1 *0012301-012 1 012S00128QCO t Mon, N o v 27. 2000 7:32 PM 8.99 in 1 period 1: 8.98 M RM , S71 scans 399.0->80.0 1 1 ! Area 11 SS Height 162 Stan Time End Time Integration Width Retention Time 3.73 4.05 0.32 3.91 A -80 E0 N o Comment \ intensity : 17 eps ITHPFOS use as Internal Standard Expected RT 4.63 Current Method I Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 10 Base. Width 150 ISO IT Win. (sea) 20 20 Smooth 11 Page 117 Northwest Bioanalytioal Study No. NWBSO-128 Report No. NWBRO1-066 Figure 17. Human Plasma Blank with Internal Standard (QCO) for PFOA IPOA.< Internal Standard: THPF05 Use Area Absolute Retention Time Expected RT 4.59 Current Method I Noise Thres. 1.0 10 Quant Hires. 0.9 0.9 Min. Width 33 Mult. Width 10 10 Base. Width 150 ISO RT Win. (secs) 20 20 Smooth 11 1THPFOS use as Internal Standard Expected RT 4.63 Noise Thres. Quant Thres. Min. Width Mult. Width Base. Width RT Win. (sea) Smooth 10.0 ' 0.2 3 10 150 20 1 10.0 0.2 3 10 150 20 1 1 012 500123 QCO 1 Mon. N ov 27. 2000 7 J 2 PM S.98 in 1 period 100-1 - 286 1: 8.98 M R M . 571 scans 90- 427.0- >4 07 .0 80 :iS s i i i Area 1B5736 Heieht 27311 Start Time End Time Integration Width Retention Time Integration Tvoe ItU M H S 4.30 4.84 0.54 4.51 A BB MM 70 H 60 H .50\. 40 H .!^ 30 H HP 20- intensity : 27311 cps to 54 103 101 ! .59 181 201 3.17 301 4.74 394 401 . 6,32 316 sot 7.90 s i r Page 118 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBR01-066 Figure 18. Human Plasma Blank with Internal Standard (QCO) for PFOSAA IPPOSAA Internal Standard: THPfO S U m Area Absolute Retention Time Expected RT 5.93 ~~~1 Current Noise Thres. Quant Thres. Min. Wldih Mult. Width Base. Width RT Win. (secsl Smooth Method 4.0 t.S 3 13 ISO 20 1 Page 119 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBRO1-066 Figure 19. Human Plasma Blank with Internal Standard (QCO) for PFOSA IPFOSA Internal Standaid: THPFOS Use Area Expected RT S.70 Noise Thres. Quant Thres. Min. Width Mult. Width Base Width RT Win. (secs) Smooth 3.0 1.0 S 10 ISO 20 1 3.0 1.0 s 10 ISO 20 1 IT H P fO S us as Internal Standard Expected RT 4.63 Current Method I Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 10 Base. Width ISO 150 IT Win. (secs) 20 20 Smooth 11 Page 120 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 FigOure 20. Human Plasma Blank with Internal Standard (QCO) for M556 iM SSi internal Standard: fHPPOS Use Area Absolute Retention Time Expected RT SJ7 Current Method 1 Noise fives. 0.4 0.4 Quant fives. 0.1 0.1 Min. Width 3 Mult. Width 11 11 Base. Width 150 150 T Win. (secs) 20 20 Smooth 1 1 I 012 S00128 QCO 1 ITHPFOS use as Internal Standard Expected RT 4.63 Current Method I Noise fives. 10.0 10.0 Quant fives. 0.2 0.2 Min. Width 3 3 M u lt Width 10 10 Base. Width 150 150 T Win. (secs) 20 20 Smooth 1 1 Page 121 Northwest Bioanalytieal Study No. NWBSOO-128 Report No. NWB RO1-066 Figure 21. Human Plasma Blank with Internal Standard (QCO) for M570 IM S70 Internai Standard: THPfO S Use Area Absolute Retention Time Expected RT 5.63 I Current Method Noise Hues. 3.0 Quant Thres. 0.5 Min. Width 5 Mult. Width 15 Base. Width ISO RT Win. (seal Smooth 20 I $0012801-012 1 012 S00128 QCO 1 N o Comment IT H P fO S use as Internal Standard Expeaed RT 4.63 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mull. Width 10 10 Base. Width 150 150 T Win. (sea) 20 20 Smooth 11 $0012801-012 1 012 $00128 QCO 1 N o Comment Page 122 Northwest Bioanalytical Figure 22. Low Standard for PFOS Study No. NWBS00-128 Report No. NWBRO1-066 IREOS Internal Standard: THP fO S Ute Are Absolute Retention Tme Expected RT SJl I Current Method Noise Thres. S.O S.O Quant Thres. 0.2 0.2 Min. Width 3 3 Mull. Width 12 12 Base. Width ISO 150 T Win. (sea) 20 20 Smooth 11 $00) 26 01<002 I 002 S00128 Stdl 1 I N o Comment IT H R fO S use as Internal Standard Expected RT 4.63 iaoI Current Method Noise Thres. 10.0 Quant Thres. Min. Width 0.2 ____ 3 0.2 3 Mult. Width Base. Width _____10 1S0 10 150 RTWin. (seal Smooth ____ 20 1 20 1 1 002 $00128 Stdl 1 1 Page 123 Northwest Bioanalytical Figure 23. Low Standard for PFHS Study No. NWBSOO-128 Report No. NWBRO1-066 IPFHS Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 4.00 Current Method I Noise Thres. 3.0 3.0 Quant Thres. 0.5 0.S Min. Width 44 Mult. Width 12 12 Base. Width 150 150 T Win. (secs) 20 20 Smooth 11 I 002S00128Std1 1 1 Mon. N ov 27, 2000 5 J 6 PM 8.98 in 1 period 1: fl.9flM RM .571 scans 399.0->80.0 NoC Height End Time Integration Width Retention Time Integration Type i+i4i<w H h intensity : 1493 cps ITHPFOS use as Internal Standard Expected RT 4.63 Current Method I Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 150 T Win. (sea) 20 20 Smooth 11 Page 124 Northwest Bioanalytical Figure 24. Low Standard for PFOA Study No. NWBSOO-128 Report No. NWBRO1-066 IPOAA Internai Standard: THPfO S Use Area Absolute Retention Time Expected RT 4.S9 3 N Ih Current Method 1.0 1.0 Quant Thres. 0.9 0.9 Min. Width 3 3 Mult. Width 10 10 Base. Width ISO ISO RT Win. (sea) 20 20 Smooth 11 0012601-002 1 002 $00128 Sldl 1 1 Mon. N ov 27, 2000 5:36 P M 6.98 in I period _ 1: 8.98 m RM, S71 scans 4 l3 .0 -> 169.0 Area 6248 Heieht 669 Start Time End Time Integration Width Retention Time Integration Tvoe ItU M M B l 4.2S 4.77 0.52 4.54 A -88 HQ N o Comment ;.: intensity : 684 eps ITHPFOS us as Internai Standard Expeaed RT Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 8ase. Width 150 150 RT Win. (sea) 20 20 Page 125 Northwest Bioanalytical Figure 25. Low Standard for PFOSAA Study No. NWBS00-I28 Report No. NWBRO1-066 IPfOSAA Internai Standard: rHPFOS Use Area Absolute Retention Time Expected RT 5.93 I Current Method Noise Hires. 4.0 4.0 Quant Thres. 1.5 1.5 Min. Width 33 Mull. Width 13 13 Base. Width 150 150 T Win. (sea) 20 20 Smooth 11 $0012801-002 I 002 $00128 Stdl I 1 N o Comment IT H P fO S use as internal Standard Expected RT 4.63 1 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 150 RT Win. (sea) 20 20 Smooth 11 $0012801-002 1 002 SO128 Stdl 1 1 No Comment Page 126 Northwest Bioanalytieal Figure 26. Low Standard for PFOSA Study No. NWBSOO-128 Report No. NWBRO1-066 Ip f o sa Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5.70 I Current Method Noise fhres. 3.0 3.0 Quant Hires. 1.0 1.0 Min. Width 55 Mult. Width 10 10 Base. Width ISO ISO T Win. (secs! 20 20 Smooth 11 S0OI28OI-0O2 I 002 S0012A Sidl 1 1 No Comment ITHPfOS use es Interrai Standard Expected RT 4.63 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 10 Base. Width 150 1S0 T Win. (seat 20 20 Smooth 11 $0012801*002 1 002 SOCI 28 Sidl 1 I N o Comment Page 127 Northwest Bioanalytical Figure 27. Low Standard for M556 Study No. NWBSOO-128 Report No. NWBRO1-066 IM S 56 Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5.37 1 Current Method Noise Hues. 0.4 0.4 Quant Thres. 0.1 0.1 Min. Width 3 3 MulL Width 11 11 Base. Width ISO ISO RT Win. (secs) 20 20 Smooth I 1 $0012801-00} 1 0 03 $00128 Std2 1 Mon. N o v 27. 2000 5:47 PM 8.98 in 1 period too- 1: 8.98 M R M . 571 scans 90- 556.0 > 498.0 :so- Area 4630 Heieht 686 Start Time End Tme Inteerahon Width Retention Time Intesation Tvoe 70- 5.25 5.72 0.47 5.55 A - 38 SB bO- 30' - 4C- ||3CT: intensity : 687 cp* 332 24 t * 13 3 1 0 6 . 6 9 101 201 - '3 0 1 401' 1.59 4 74 32 SOt :;: 7.90 s s r Page 128 Northwest Bioanalytical Figure 28. Low Standard for M570 Study No. NWBS00-128 Report No. NWBRO1-066 IM S 70 Internai Standard: THPFOS U s e -Vea Absolute Retention Time Expected RT S.63 . Current Method Noise Dues. 3.0 3.0 Quant Thres. 0.5 0.5 Min. Width 5 5 Mult. Width IS 15 Base. Width ISO 150 R f Win. (secs) 20 20 Smooth 11 1 002 500128 Sedi 1 ! ITHPfO S use as Internal Standard Expected RT 4.63 Current Method \ Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 150 tr Win. (secs) 20 20 Smooth 1 1 Page 129 Northwest Bioanalytieal Figure 29. High Standard for PFOS Study No. NWBSOO-128 Report No. NWBR01-066 IPFOS Internal Standard: H-IPFOS Use Area Absolute Retention Time Expected RT 5J1 1 Current Method Noise Otres. 5 0 5.0 Quant Hues. 0.2 0.2 Min. Width 33 Mull. Width 12 12 Base. Width tso ISO RT Win. (secs) 20 20 Smooth 11 $0012801-080 1 080S0128 Sid9 2 1 N o Comment ITH PFOS use as Internal Standard Expected RT 4.63 Current Method 1 Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 10 Base. Width 1S0 150 TW in. (secs) 20 20 Smooth 11 Page 130 Northwest Bioanalytical Figure 30. High Standard for PFHS Study No. NWBSOO-128 Report No. NWBRO1-066 IPFHS Internal Standard: fH P fO S Use Area Absolute Retention Time Expected RT 4.00 ] Current Method Noise Thres. J.Q 3.0 Quant Dues. O.S 0.S Min. Width 4 4 Mult. Width 12 12 Base. Width ISO 150 RT Win. (sea) 20 20 Smooth 1 1 IT H P fO S use as Internal Standard Expected RT 4.63 Current Method I Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 1 3 Muh. Width 10 10 Base. Width ISO ISO RT Win. (secs) 20 20 Smooth 1 1 Page 131 Northwest Bioanalytical Figure 31. High Standard for PFOA Study No. NWBSOO-128 Report No. NWBRO1-066 IPOAA Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 4.59 ] Current Method Noise ihres. 1.0 1.0 Quant ihres. 0.9 0.9 Min. Width 33 Mult. Width 10 10 8ase. Width 50 ISO RT Win. (sees! 20 20 Smooth 11 0012801-080 1 080 S00128 Std9 2 1 N o Comment IT H P fQ S use es Internal Standard Expected RT 4.63 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 10 Base. Width 150 150 T Win. (sea) 20 20 Smooth 11 1 080S00128 Std9 2 1 Page 132 Northwest Bioanalytical Study No. NWBSOO-128 Report No. NWBRO1-066 Figure 32. High Standard for PFOSAA IP fO SA A Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5.93 I Current Method Noise Thres. 4.0 4.0 Quant Thres. t.S 1.5 Min. Width 33 Mult. Width 13 13 Base. Width ISO 150 T Win. (secs) 20 20 Smooth 11 $0012801-060 1 080S00l28Std9 2 1 N o Comment IT H P fO S use as Internal Standard Expected RT 4.63 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 10 Bate. Width 150 150 IT Win. (secs) 20 20 Smooth 11 1 060 S00126 Std9 2 1 Page 133 Northwest Bioanaiytical Figure 33. High Standard for PFOSA Study No. NWBSOO-128 Report No. NWBRO1-066 IPfOSA internet Standard: fHPfOS Use Afea I Current Method Noise Hues. 3.0 3.0 Quant Thres. 1.0 1.0 Min. Width Ss Absolute Retention firne Mull. Width 10 10 Expected XT S.70 8ase. Width T Win. (seal ISO ISO 20 20 Smooth 11 $0012801-060 9t 060SOOI26 Sid 2 1 No Comme ITHPFOS use as Internal Standard Expected XT 4.63 Current Method 10.0Noise Thres. to.o Quant Thres. 0.2 0.2 Min. Width Mult. Width Base. Width XT Win. (secs) Smooth 33 10 10 1S0 ISO 20 20 11 Page 134 Northwest Bioaiialytical Figure 34. High Standard for VI556 Study No. NWBS00-128 Report No. NWBR01-066 |MSS(. Internal Standard: THPfO S Use Area Absolute Retention Time Expected RT 5.37 I Current Method Noise Thres. 0.4 Quant rhres. M Min. Width 3 Mult. Width It It Base. Width 150 150 RT win. (secs) Smooth 20 I t OSO S00128 Sid9 2 I ITHPFOS use as Internal Standard ~ 1 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 M u lt Width 10 10 Expected RT 4.63 Base. Width T Win. (secs) 150 150 20 20 Smooth 11 $0012801-080 1 080 S00128 Std9 2 1 Tue, N ov 2B, 2000 8:39 A M 8.98 in 1 period 1: 8.98 M R M , 571 scans 427.0>>407.Q Area 160597 Heisht 18653 Start Time End Time Imeeration Width Retention Time tnteeration Type 4.27 4.73 0.46 4.51 A -B B ItU k H S P l i m N o Comment inteniittj : 18653 eps Page 135 Northwest Bioarialytical Figure 35. High Standard for VI570 Study No. NWBS00-128 Report No. NWBRO1-066 |m S 70 ' ~~1 Current M ethod Internai Standard: THPfO S Use Area Noise Thres. 3.0 3.0 Quant Thres. 0.5 0.5 Min. Width 5 5 Absolute Retention Time Mult. Width IS 15 Expected RT 5.63 Base. Width ISO 150 RT Win. (sect) 20 20 Smooth 11 $0012801-060 1 060 S00128 Sld9 2 1 N o Comment ITHPfOS use as Internal Standard Expected RT 4.63 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 150 IT Win. (secs) 20 20 Smooth 11 $0012801-060 1 060 S00128 Std9 2 1 Tue, N ov 26. 2000 8:39 A M 8.98 in 1 period 1: 8.98 M R M , 571 scans . 427.0->407.0 Area 160597 Heieht 18653 Start Time End Time Intesration Width Retention Time Integration Type 4.27 4.73 0.46 4.51 A 88 EQ! N o Comment Page 136