Document MM3vDd5na2Mdw2e1nRGgM7k3j

j NorthwestBioanalytical f RSetpuodryt NNoo..NNWWB'BRS0010--006951 Quantitative Determination of PFOS and Related Compounds Serum and Plasma by LC/MS/MS in Human Sample Analysis Report EPI-0012 for Protocol Northwest Bioanalytical (NWB) A Division of NWT Inc. 1121 East 3900 South Salt Lake City, UT 84124 PREPARED FOR: 3M Company Epidemiology, Medical Department 220-3W-05 St. Paul, MN 55144 AUTHOR: _gb, Cz_" Jff_" Connie O. Sakashita, B.S., NWB Project Manager APPRDVED FOR RELEASE BY: //"_"=-_, "_'Jo'-_' "" R__GC_geLr. Foltz, -P-h.Di-.j,- NW- B Technical Director DATE: //-_O-c9 / DATE: ]/-2[-,1 Page 1 Northwest Bioanalytical QUALITY ASSURANCE STATEMENT Study No. NWBS00-091 Report No. NWBR01-065 LABORATORY: Northwest Bioanalytical (NWB) A Division of NWT Inc. 1121 East 3900 South Salt Lake City, UT 84124 SPONSOR: 3M Company Epidemiology, 220-3W-05 St. Paul, MN Medical 55144 Department COMPOUND(S): NWB STUDY NUMBER: SPONSOR STUDY NUMBER: PFOS and Related Compounds NWBS00-091 EPI-0012 NWB STUDY TITLE: Quantitative Determination of PFOS and Related Compounds in Human Serum and Plasma by LC/MS/MS The clinical study described in this report is not included within the definition of a GLP regulated nonclinical study. However, Northwest Bioanalytical conducts all studies within the guidelines of the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Tire 21 CFR Part 58), the OECD Principles of Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety of Drugs (Ordinance No. 21, PAB Notification No. 424.) The following inspections were performed by the NWB QAU per SOP. Inspection and Reporting Statement. Date of/nspection Phase of Study Date Report Sent to NWB Proiect Manager Date Report Sent to NWB Management* 16 Oct 2000 17-23 Oct 2000 29 Oct- 01 Nov 2001 23 Nov 2001 Analytical Plan Sample Analysis Report Draft and Raw Data Final Report 16 Oct 2000 24 Oct 2000 01 Nov 2001 23 Nov 2001 31 Oct 2000 31 Oct 2001 30 Nov 2001 30 Nov 2001 *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. S_ Lyl_ Chain, B.A. - - Date NWB Quality Assurance Compliance Auditor Page 2 NorthwestBioanalytical StudyNo. NWBS00-091 ReportNo. NWBR01-065 COMPLIANCE STATEMENT The clinicasltudydescribeidnthisreportisnotincludedwithinthedefinitioofna GLP regulatendonclinicasltudy.However,tothebestofourknowledge,thisprojecwtas conductedinaccordancewiththeguidelineosftheU.S.FDA Good LaboratorPyractice RegulationfsorNonclinicaLlaboratorSytudies(Titl2e1 CFR Part58)andaccordingto the methods and procedures described within this report. In addition, the study followed the guidelines of the OECD Principles of Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety of Drugs (Ordinance No. 21, PAB Notification No. 424.) This report contains serum sample results. As reported in NWB report NWBR00-122 [5.3], serum sample results obtained using plasma curves for PFOSA, PFOSAA, POAA, PFHS, M556 and M570 did not meet NWB SOP requirements for validation. Any known circumstances that may have affected the quality or integrity of the project or reported data are discussed within the report. This report represents an accurate record of the raw data. Connie O. Sakashita, B.S. NWB Project Manager erL.Foltz,Ph.D.0 NWB TechnicaDlirector Date Date Page 3 NorthwestBioanalytical TABLE OF CONTENTS StudyNo. NWBS00-091 ReportNo. NWBR01-065 SIGNATURE PAGE ....................................................................................................................... 1 QUALITY ASSURANCE STATEMENT ...................................................................................... 2 COMPLIANCE STATEMENT ...................................................................................................... 3 TABLE OF CONTENTS ................................................................................................................ 4 LIST OF TABLES .......................................................................................................................... 4 LIST OF FIGURES ......................................................................................................................... 6 1. INTRODUCTION ................................................................................................................... 8 2. METHODOLOGY .................................................................................................................. 9 3. SAMPLE ANALYSIS ........................................................................................................... 12 4. RESULTS AND DISCUSSION ............................................................................................ 13 5. REFERENCES ...................................................................................................................... 16 6. DATA RETENTION ............................................................................................................ 16 LIST OF TABLES Table 1. Calibration Curve Summary for PFOS ................. ......................................................... 17 Table 2. Calibration Curve Summary for PFOA .......................................................................... 18 Table 3. Calibration Curve Summary for PFHS .......................................................................... 19 Table 4. Calibration Curve Summary for PFOSAA ..................................................................... 20 Table 5. Calibration Curve Summary for PFOSA ....................................................................... 21 Table 6. Calibration Curve Summary for M556 .......................................................................... 22 Table 7. Calibration Curve Summary for M570 .......................................................................... 23 Table 8. Back-Calculated Concentrations of Calibration Standards for PFOS ............................ 24 Page4 NorthwestBioanalytical StudyNo. NWBS00-091 ReportNo. NWBR01-065 Table 9. Back-Calculated Concentrations of Calibration Standards for PFOA ........................... 25 Table 10. Back-Calculated Concentrations of Calibration Standards for PFHS .......................... 26 Table 11. Back-Calculated Concentrations of Calibration Standards for PFOSAA .................... 27 Table 12. Back-Calculated Concentrations of Calibration Standards for PFOSA ....................... 28 Table 13. Back-Calculated Concentrations of Calibration Standards for M556 .......................... 29 Table 14. Back-Calculated Concentrations of Calibration Standards for M570 .......................... 31 Table 15. Analytical QC Summary for PFOS .............................................................................. 33 Table 16. Analytical QC Summary for PFOA ............................................................................. 34 Table 17. Analytical QC Summary for PFHS .............................................................................. 35 Table 18. Analytical QC Summary for PFOSAA ........................................................................ 36 Table 19. Analytical QC Summary for PFOSA ........................................................................... 37 Table 20. Analytical QC Summary for M556 .............................................................................. 38 Table 21. Analytical QC Summary for M570 .............................................................................. 39 Table 22. Serum Study Sample Concentrations ........................................................................... 40 Table 23. Plasma Study Sample Concentrations .......................................................................... 48 Table 24. Repeat Analysis Table for PFOS in Human Serum ..................................................... 55 Table 25. Repeat Analysis Table for PFOA in Human Serum ..................................................... 55 Table 26. Repeat Analysis Table for PFHS in Human Serum ..................................................... 56 Table 27. Repeat Analysis Table for PFOSAA in Human Serum ............................................... 56 Table 28. Repeat Analysis Table for PFOSA in Human Serum .................................................. 57 Table 29. Repeat Analysis Table for M556 in Human Serum ..................................................... 57 Table 30. Repeat Analys!s Table for M570 in Human Serum ..................................................... 58 Page5 NorthwestBioanalytical LIST OF FIGURES StudyNo. NWBS00-091 ReportNo. NWBR01-065 Figure 1. Representative Calibration Curve for PFOS ............................................................ ..... 59 Figure 2. Representative Calibration Curve for PFOA ................................................................ 59 Figure 3. Representative Calibration Curve for PFHS ................................................................. 60 Figure 4. Representative Calibration Curve for PFOSAA ............................................................ 60 Figure 5. Representative Calibration Curve for PFOSA .............................................................. 61 Figure 6. Representative Calibration Curve for M556 ................................................................. 61 Figure 7. Representative Calibration Curve for M570 ................................................................. 62 Figure 8. Human Plasma Blank for PFOS ................................................................................... 63 Figure 9. Human Plasma Blank for PFOA ................................................................................... 64 Figure 10. Human Plasma Blank for PFHS ................................................................................. 65 Figure 11. Human Plasma Blank for PFOSAA ............................................................................ 66 Figure 12. Human Plasma Blank for PFOSA ............................................................................... 67 Figure 13. Human Plasma Blank for M556 ................................................................................. 68 Figure 14. Human Plasma Blank for M570 ................................................................................. 69 Figure 15. Human Plasma Blank with Internal Standard (QC0) for PFOS .................................. 70 Figure 16. Human Plasma Blank with Internal Standard (QC0) for PFOA ................................. 71 Figure 17. Human Plasma Blank with Intemal Standard (QC0) for PFHS .................................. 72 Figure 18. Human Plasma Blank with Internal Standard (QC0) for PFOSAA ............................ 73 Figure 19. Human Plasma Blank with Internal Standard (QC0) for PFOSA ............................... 74 Figure 20. Human Plasma Blank with Internal Standard (QC0) for M556 .................................. 75 Figure 21. Human Plasma Blank with Internal Standard (QC0) for M570 .................................. 76 Figure 22. Low Standard for PFOS .............................................................................................. 77 Figure 23. Low Standard for PFOA ............................................................................................. 78 Page 6 NorthwestBioanalytical StudyNo. NWBS00-091 ReportNo. NWBR01-065 Figure 24. Low Standard for PFHS .............................................................................................. 79 Figure 25. Low Standard for PFOSAA ........................................................................................ 80 Figure 26. Low Standard for PFOSA ........................................................................................... 81 Figure 27. Low Standard for M556 .............................................................................................. 82 Figure 28. Low Standard for M570 .............................................................................................. 83 Figure 29. High Standard for PFOS ............................................................................................. 84 Figure 30. High Standard for PFOA ............................................................................................ 85 Figure 31. High Standard for PFHS ............................................................................................. 86 Figure 32. High Standard for PFOSAA ....................................................................................... 87 Figure 33. High Standard for PFOSA .......................................................................................... 88 Figure 34. High Standard for M556 ............................................................................................. 89 Figure 35. High Standard for M570 ............................................................................................. 90 Page 7 NorthwestBioanalytical StudyNo. NWBS00-091 ReportNo. NWBR01-065 Quantitative Determination of PFOS and Related Compounds Serum and Plasma by LC/MS/MS in Human Sample Analysis Report for Protocol EPI-0012 1. INTRODUCTION This report summarizes the analytical results from the quantitation of PFOS, PFOA, PFHS, PFOSAA, PFOSA, M556, and M570 in human serum and plasma samples for 3M Company (3M) in support of Protocol EPI-0012 [5.1]. The LC/MS/MS method for the analytes has a targeted calibration curve range of 1.00 to 500 ppb (except for M556 which has a LLOQ of 2.50 ppb). The actual calibration curve range for each analyte varies based upon the persistent levels of the analyte in the matrix. For this study, the assay exhibited the following LLOQ and ULOQ values: Analyte PFOS PFOA PFHS PFOSAA PFOSA M556 M570 LLOQ 3.94 ppb 1.92 ppb 1.36 ppb 1.60 ppb 1.00 ppb 2.50 ppb 1.00 ppb ULOQ 414 ppb 481 ppb 523 ppb 501 ppb 500 ppb 500 ppb 500 ppb The sponsor was 3M Company (Epidemiology, Medical Department, 220-3W-05, St. Paul, MN 55144), and the Study Director was Jeffrey H. Mandel, M.D., M.P.H. The Study Contact at 3M was Jean Burris. James K. Lundberg was the technical contact at 3M. The following is a list of NWB supervisory personnel involved in the completion of this work: Connie O. Sakashita, B.S. (NWB Project Manager); Patrick Bennett, M.S., M.B.A. (NWB Laboratory Director); Rodger L. Foltz, Ph.D. (NWB Technical Director). Laboratory personnel involved in the completion of this study included Suzanne Page 8 NorthwestBioanalytical StudyNo. NWBS00-091 ReportNo. NWBR01-065 Newman, B.S. (NWB Research Scientist); Emily Yardimci, B.S. (NWB Associate Research Scientist). NWB SOPs and guidelines were used in the conduct of this study and were available to study personnel in electronic and/or hard copy formats. Date Study Initiated: 24-Sep-2000 Date Analyses Completed: 07-Apr-2001 The clinical study described in this report is not included within the definition of a GLP regulated nonclinical study. However, Northwest Bioanalytical conducts all studies within the guidelines of the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58), the OECD Principles of Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety of 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 NWBR00- 108 [5.2] and NWBR00-122 [5.3]. Chinese human plasma was used for the calibration curves and quality control samples. are discussed in NWBR00-122. Serum sample results obtained using plasma curves Samples for this study were received at NWB on the following dates: Receipt Date 25-Jul-2000 26-Jul-2000 Number of Samples Received 243 151 Storage Condition (except during analysis) -20 C -20 C Page 9 NorthwestBioanalytical Reference Material StudyNo. NWBS00-091 ReportNo. NWBR01-065 Analyte PFOS PFOA PFHS PFOSAA PFOSA Lot Number 193 245 SE-036 617 214 Purity 100% 100% 91.1% Expiration Date 31 -Dec-2010 31-Dec-2010 01-Jan-2010 53.8% 31-Dec-2010 100% 31-Dec-2010 *Storeddry Source 3M 3M 3M 3M 3M Storage Conditions Room temperature* Room temperature* -20 C Room temperature Room temperature Analyte M556 M570 THPFOS Lot Number NB113047-8D 118506-26 59909 Purity Expiration Date 99.89% 31-Dec-2010 99.75% 31-Dec-2010 90% 31-Dec-2010 Source 3M 3M 3M Storage Conditions Room temperature Room temperature Room temperature The reference material purity for PFOS, PFOSA, PFHS, and PFOA was not available prior to the conduct of this study. Therefore, the reference material purity was assumed to be 100%. 3M contracted with Centre Analytical Laboratories, Inc., in State College, Pennsylvania to determine the absolute concentration ofPFOS, PFOA, and PFHS in NWB stock solutions used to prepare the analytical standards and controls used for this studies. All arrangements for purity determinations and the transfer of NWB solutions to Centre Analytical Laboratories, Inc., were performed by 3M. Based on Centre Analytical Laboratories' results, the concentrations of plasma calibrator and quality control samples were corrected using the following factors: Analyte PFOS PFOA PFHS Correction Factor 0.821 0.961 1.043 Page I0 NorthwestBioanalytical StudyNo. NWBS00-091 ReportNo. NWBR01-065 Eight or more calibration standards were prepared on the day of each run by adding 100 _tL of blank Chinese human plasma and 400 ].tL of 50 mM ammonium acetate in water (unadjusted pH -6.9) to 13 x 100 mm polypropylene tubes. After a brief vortex mixing, 10.0 ].tL of the appropriate spiking solution was added. The final calibration standard concentrations in human plasma for each analyte are listed below: Analyte PFOS PFOA PFHS PFOSAA PFOSA M556 M570 Calibration Standard Concentrations* 3.94, 5.17, 11.3, 23.6, 44.2, 85.4, 209, 332 and 414ppb 1.92, 3.36, 10.6, 25.0, 49.0, 97.1,241,385 and 481 ppb 1.36, 2.92, 10.7, 26.5, 52.6, 104, 262,418 and 523 ppb 1.60, 3.10, 10.6, 25.6, 50.6, 101,251,401 and 501 ppb 1.00, 2.50, 10.0, 25.0, 50.0, 100, 250, 400 and 500 ppb 2.50, 10.0, 25.0, 50.0, 100, 250, 400 and 500 ppb (runs 1 - 17) 3.20, 10.7, 25.7, 50.7, 101,251,401 and 501 ppb (run 18) 1.00, 2.50, 10.0, 25.0, 50.0, 100, 250, 400 and 500 ppb (runs 1 - 17) 1.90, 3.40, 10.9, 25.9, 50.9, 101,251,401 and 501 ppb (run 18) * The target calibrationcurverange is 1.00ppb to 500 ppb (exceptM556 whichhas a LLOQ of 2.50 ppb). Each analyte has a differentfinal curverangebased upon the persistentlevels ofthe analyte in thehuman plasmaused. Run 18 for M556 and M570 used a new pool of plasmawith differentpersistentlevelsof analyte. In addition, blank human plasma samples, both with and without internal standard (designated as QC0s and Blanks, respectively), were assayed in each analytical run. Analytical QCs were prepared in Chinese human plasma on October 6, 2000, October 11, 2000, October 27, 2000 and March 8, 2001 and stored in a -20 C freezer. For each run, analytical QC levels were assayed in duplicate. Analyte PFOS PFOA PFHS PFOSAA PFOSA M556 M570 QC Concentrations (ppb)* Low Medium High 6.40 126 332 4.81 145 385 4.48 156 417 4.60 151 401 4.00 150 400 4.00 150 400 4.00 150 400 *The target QC concentrationsare4.00 ppb, 150ppb and 400 ppb. Each analytehas differentQC concentrationsbased uponthe persistentlevels of the analyte in thehumanplasmaused. Page 11 NorthwestBioanalytical StudyNo. NlXq,3S00-091 ReportNo. NWBR01-065 The internal standard (THPFOS) was added to all serum samples (except Blanks) for a final concentration of approximately 200 ppb. The analytical method consisted of a liquid:liquid extraction procedure followed by evaporation and reconstitution of the extract residue with 20 mM ammonium acetate in water: 20 mM ammonium acetate in methanol (30:70 v/v). The samples were analyzed by liquid chromatography/tandem mass spectrometry using an API 3000. The instrument was operated in the multiple reaction monitoring (MRM) mode under optimized conditions for PFOS, PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 detection of the negative ions formed by TurboIonSpray TM ionization. 3. SAMPLE ANALYSIS PFOS, PFOA, PFHS, PFOSAA, PFOSA, M556, M570, and THPFOS chromatographic peaks were integrated using the MacQuan software (version 1.6) with a smooth factor of one. Quantitation was based upon quadratic regression analysis of weighted (1/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. 3.1. Acceptance Criteria For an analytical run to be accepted, it must have met the acceptance criteria listed below which are consistent with regulatory and industry recommendations. Calibration Curve Each run will include in duplicate calibration standards at six or more concentrations covering the lower to upper limit of quantitation. For all analytes except PFOSA and PFOSAA, at least three-fourths of the calibration standard's back-calculated concentrations must be within + 15% (+ 20% for LLOQ) of their individual target concentrations. For PFOSA and PFOSAA, at least three-fourths of the calibration standard's back-calculated concentrations must be within _+20% (+ 25% for LLOQ) Page 12 NorthwestBioanalytical StudyNo. NWBS00-091 ReportNo. NWBR01-065 of their individual target concentrations. A calibration standard will be considered an outlier if it is greater than two times the acceptance criteria for that standard. Lower Limit of Quantitation The back-calculated concentrations of at least one of the duplicate lowest points in the calibration curve must be within + 25% of the target concentration for PFOSA and PFOSAA to qualify as the LLOQ and within + 20% of the target concentration to qualify as the LLOQ for all other analytes. If this criterion is not met, the next level is subjected to the same test and the LLOQ raised accordingly. Quality Control Samples Each analytical run will include low, medium and high QC samples in duplicate. The measured concentrations of at least two-thirds of all analytical QCs must be within + 20% of their target concentrations (+ 25% for PFOSA and PFOSAA), and no two QCs at the same concentration can be outside the limit. If study samples require dilution, a dilution QC will be analyzed in triplicate for each dilution level (except for PFOSA and PFOSAA which should not be diluted with control matrix). At least two dilution QCs at each level must be within + 20% of its target concentrations in order to accept diluted study samples at that level. The dilution QC acceptance is independent of the undiluted analytical QC acceptance. 4. RESULTS AND DISCUSSION Serum sample results obtained using plasma curves for PFOA, PFHS, PFOSAA, PFOSA, M556, and M570 did not meet NWB SOP requirements for validation. Results may vary on average up to 26% from results obtained using human serum calibration curves at some concentration levels for PFOA, PFHS, PFOSAA, M556, and M570. For PFOSA, results may vary on average up to 43% from results obtained using human serum calibration curves. This data is reported in Assay Revalidation Addendum Report NWBR00-122 [5.3]. However, in order to obtain the lower limit of quantitation of less than 5 ppb required by the sponsor, it was necessary to use plasma calibration curves. Page 13 Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Each accepted run met the acceptance criteria set for the calibration curve points, for the lower limit of quantitation (LLOQ) and for the analytical quality control (QC) samples. Run PFOS ID Result 1 Accepted 2 Accepted 3 Accepted 4 Accepted 5 Accepted 6 N/A 7 Accepted 8 Accepted 9 Accepted 10 Accepted 11 .... 12 N/A 13 N/A 14 N/A 15 Accepted 16 Rejected 17 Accepted 18 N/A PFOA Result Rejected Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted N/A N/A N/A Accepted Rejected Accepted N/A PFHS Result Accepted Accepted Accepted Accepted Accepted N/A Accepted Accepted Accepted Accepted PFOSAA Result Accepted Accepted Accepted Accepted Accepted N/A Accepted Accepted Accepted Accepted N/A N/A N/A Accepted Rejected N/A N/A N/A Accepted Rejected Accepted N/A Accepted N/A N/A = not analyzed Comments Calibration curve failed for rejected analyte. Pre-study assay evaluation. Run mistakenly created in Watson DMLIMS .system (no data collected). Reinj ection of run 7. Reinjection of run 8. Rejected due to sample preparation error. Page 14 Bioanalytical Run PFOSA Result ID 1 Accepted 2 Accepted 3 Accepted 4 Accepted 5 Accepted 6 N/A 7 Accepted 8 Accepted 9 Accepted 10 Accepted 11 - 12 N/A 13 N/A 14 N/A 15 Accepted 16 Rejected 17 Accepted 18 N/A M556 Result M570 Result Study No. NWBS00-091 Report No. NWBR01-065 Comments Accepted Accepted Accepted Accepted Accepted N/A Rejected Rejected Accepted Accepted Accepted Accepted Accepted Accepted Accepted N/A Rejected Accepted Accepted Accepted Accepted Rejected Accepted N/A Accepted Rejected N/A Accepted Accepted Rejected Rejected Rejected Accepted Accepted N/A = not analyzed Pre-study assay evaluation. QCs failed for rejected analytes. Calibration curve failed for rejected analyte. Run mistakenly created in Watson DMLIMS system (no data collected). Reinjection of run 7. QCs failed for rejected analytes. Reinjection of run 8. Rejected due to sample preparation error. QCs failed for rejected analytes. One of the medium QC replicates in Run 17 gave very high PFOSA and PFOSAA results. These results appear to be outliers which skew the overall study statistics. Without inclusion of this QC result, the medium QC statistics are as follows: Mean S.D. %CV %Theoretical %Bias N PFOSAA 162 18.5 11.0 107.3 7.3 19 PFOSA 153 17.7 11.6 102.0 2.0 19 Page 15 NorthwestBioanalytical StudyNo. NWBS00-091 ReportNo. NWBR01-065 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-0012. "Serum fluorochemical trends of out-of-country residents in CLUE I (1974) and CLUE II (1989) epidemiologic investigations." 5.2. C. Sakashita. "Quantitative Determination of PFOS, PFOSA, PFOSAA, POAA, PFHS, M556 and M570 in Human Serum by LC/MS/MS." Assay Revalidation Report. NWB Study NWBS00-040. NWB Report NWBR00-108. January 24, 2001. 5.3. C. Sakashita. "Quantitative Determination ofPFOS, PFOSA, PFOSAA, POAA, PFHS, M556 and M570 in Human Serum by LC/MS/MS." Assay Revalidation Addendum Report. NWB Study NWBS00-040. November 20, 2001. NWB Report NWBR00-122. 6. DATA RETENTION The raw data and final report for this study will be stored in the NWB Archives, 1121 East 3900 South, Salt Lake City, UT 84124 per regulations and contract agreement. After submission of the final report to the Sponsor, remaining study samples will be stored under required conditions until confirmation of Sample Disposition/Return Authorization is received from the Sponsor. 3M Company will be notified concerning final disposition of records at completion of contract obligations. Page 16 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 1. Calibration Curve Summary for PFOS Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 13-Oct-2000 14-Oct-2000 16-Oct-2000 18-Oct-2000 19-Oct-2000 20-Oct-2000 20-Oct-2000 23-Oct-2000 31-Oct-2000 23-Mar-2001 Run Number 1 3 5 4 9 7 8 10 15 17 A B C R-Squared LLOQ ULOQ -0.000005 -0.000007 -0.000007 -0.000010 -0.000002 -0.000008 -0.000009 -0.000010 -0.000005 0.000002 0.029065 0.030835 0.024230 0.028656 0.020051 0.021563 0.021893 0.022789 0.027791 0.039134 0.003518 -0.004262 -0.022998 0.010100 0.008280 0.013487 0.002918 0.007538 0.010909 0.020796 0.9970 0.9967 0.9930 0.9911 0.9944 0.9881 0.9922 0.9836 0.9956 0.9869 3.94 414 3.94 414 3.94 414 3.94 414 3.94 414 3.94 414 3.94 414 3.94 414 3.94 414 3.94 414 Mean S.D. %CV n -0.000006 0.000004 -66.7 10 0.026601 0.005748 21.6 10 0.005029 0.011906 236.7 10 0.9919 0.0045 0.5 10 A,B, and C arecoefficientsusedtodefinethecalibrationcu_e. Page 17 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 2. Calibration Curve Summary for PFOA Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 14-Oct-2000 15-Oct-2000 16-Oct-2000 18-Oct-2000 19-Oct-2000 20-Oct-2000 20-Oct-2000 23-Oct-2000 31-Oct-2000 23-Mar-2001 Run Number 3 6 5 4 9 7 8 10 15 17 A B C R-Squared LLOQ ULOQ 0.000000 0.000002 0.000000 -0.000001 0.000004 0.000000 0.000001 0.000001 0.000001 0.000001 0.021802 0.022043 0.013756 0.015425 0.015292 0.014501 0.013316 0.013509 0.018750 0.008393 -0.010687 -0.000611 -0.007270 -0.002433 0.002113 -0.003931 -0.003358 0.001640 0.001244 0.007706 0.9983 0.9982 0.9982 0.9964 0.9875 0.9979 0.9964 0.9856 0.9967 0.9842 1.92 481 1.92 481 1.92 481 1.92 481 1.92 481 1.92 481 1.92 481 1.92 481 1.92 481 1.92 481 Mean S.D. %CV n 0.000001 0.000001 100.0 10 0.015679 0.004165 26.6 10 -0.001559 0.005206 -333.9 10 0.9939 0.0057 0.6 10 A,B, and C arecoefficientsusedtodefinethecalibrationcu_e. Page 18 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 3. Calibration Curve Summary for PFHS Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 13-Oct-2000 14-Oct-2000 16-Oct-2000 18-Oct-2000 19-Oct-2000 20-Oct-2000 20-Oct-2000 23-Oct-2000 31-Oct-2000 23-Mar-200! Run Number 1 3 5 4 9 7 8 10 15 17 A B C R-Squared LLOQ ULOQ -0.000010 -0.000010 -0.000009 -0.000007 -0.000005 -0.000006 -0.000005 -0.000004 -0.000009 -0.000002 0.030430 0.031509 0.027185 0.026276 0.026618 0.027614 0.024990 0.024289 0.031737 0.021861 0.000781 0.004692 -0.000974 0.001867 0.007959 0.003405 0.005704 0.010779 0.006465 0.020425 0.9973 0.9958 0.9926 0.9986 0.9895 0.9949 0.9975 0.9948 0.9976 0.9959 1.36 523 1.36 523 1.36 523 1.36 523 1.36 523 1.36 523 1.36 523 1.36 523 1.36 523 1.36 523 Mean S.D. %CV n -0.000007 0.000003 -42.9 10 0.027251 0.003211 11.8 10 0.006110 0.006113 100.0 10 0.9955 0.0027 0.3 10 A,B, and C arecoefficientsusedtodefine _ecalibrationcu_e. Page 19 NorthwestBioanalytical StudyNo. NWBS00-091 ReportNo. NWBR01-065 Table 4. Calibration Curve Summary for PFOSAA Quadraticweighted 1/xz. All concentrationsare expressedas ppb. Run Date 13-Oct-2000 14-Oct-2000 16-Oct-2000 18-Oct-2000 19-0ct-2000 20-0ct-2000 20-0ct-2000 23-0ct-2000 31-0ct-2000 23-Mar-2001 Run Number 1 3 5 4 9 7 8 10 15 17 A B C R-Squared LLOQ ULOQ 0.000005 0.000004 0.000000 0.000001 0.000002 -0.000004 -0.000005 -0.000003 -0.000001 0.000001 0.026658 0.033575 0.025009 0.036355 0.021746 0.030680 0.035370 0.025921 0.023946 0.007894 0.002620 -0.001462 -0.008698 -0.011781 0.017518 0.001307 -0.003269 0.008516 -0.003099 0.004964 0.9900 0.9859 0.9925 0.9936 0.9772 0.9809 0.9912 0.9750 0.9952 0.9685 1.60 501 1.60 501 1.60 501 1.60 501 1.60 501 1.60 501 1.60 501 1.60 501 1.60 501 1.60 501 Mean S.D. %CV n 0.000000 0.000003 10 0.026715 0.008305 31.1 l0 0.000662 0.008466 1278.9 10 0.9850 0.0091 0.9 10 A,B, and Carecoefficientsusedtodefinethecalibrationcu_e. Page 20 NorthwestBioanalytical StudyNo. NWBS00-091 ReportNo. NWBR0t-065 Table 5. Calibration Curve Summary for PFOSA Quadraticweighted1/x2. All concentrationsareexpressedas ppb. Run Date 13-Oct-2000 14-Oct-2000 16-Oct-2000 18-Oct-2000 19-Oct-2000 20-Oct-2000 20-Oct-2000 23-Oct-2000 31-Oct-2000 23-Mar-2001 Run Number 1 3 5 4 9 7 8 10 15 17 A B C R-Squared LLOQ ULOQ -0.000005 -0.000005 -0.000004 -0.000010 0.000000 -0.000007 -0.000010 -0.000013 -0.000013 0.000002 0.059585 0.060205 0.047126 0.071207 0.036297 0.041996 0.046357 0.044171 0.052859 0.034802 0.013519 0.017572 -0.000891 0.006196 0.011607 0.014850 0.008887 0.009049 0.003517 0.013699 0.9914 0.9940 0.9938 0.9853 0.9891 0.9813 0.9868 0.9824 0.9949 0.9847 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 Mean S.D. %CV n -0.000006 0.000005 -83.3 10 0.049461 0.011496 23.2 10 0.009801 0.005641 57.6 10 0.9884 0.0050 0.5 10 A,B, andC arecoe_ciemsusedtodefine _ecalibrationcu_e. Page 21 NorthwestBioanalytical StudyNo. NWBS00-091 Repo_ No. NWBR01-065 Table 6. Calibration Curve Summary for M556 Quadraticweighted l/x2. All concentrationsare expressedas ppb. Run Date 13-Oct-2000 14-Oct-2000 16-Oct-2000 18-Oct-2000 19-Oct-2000 21-Oct-2000 22-Oct-2000 23-Oct-2000 31-Oct-2000 07-Apr-2001 Run Number 1 3 5 4 9 13 12 10 15 18 A B C R-Squared LLOQ ULOQ 0.000002 0.000000 -0.000002 -0.000004 0.000000 -0.000006 -0.000006 -0.000009 -0.000001 0.000001 0.018046 0.025056 0.019822 0.027460 0.021846 0.029287 0.026339 0.025551 0.018373 0.007457 0.011395 0.002464 -0.004705 -0.000627 0.010790 0.003549 0.005660 -0.002177 0.001923 0.002028 0.9826 0.9875 0.9931 0.9882 0.9800 0.9936 0.9846 0.9893 0.9972 0.9924 2.50 500 2.50 500 2.50 500 2.50 500 2.50 500 2.50 500 2.50 500 2.50 500 2.50 500 3.20 501 Mean S.D. %CV n -0.000002 0.000004 -200.0 I0 0.021924 0.006400 29.2 10 0.003030 0.005167 170.5 10 0.9889 0.0054 0.5 10 A, B, and C are coe_cients used to define the calibrationcu_e. Page 22 NorthwestBioanalytical StudyNo. NWBS00-091 ReportNo. NWBR01-065 Table 7. Calibration Curve Summary for M570 Quadraticweighted 1/x_. All concentrationsare expressedas ppb. Run Date 13-Oct-2000 14-Oct-2000 16-Oct-2000 18-Oct-2000 19-Oct-2000 20-Oct-2000 23-Oct-2000 30-Oct-2000 31-Oct-2000 07-Apr-2001 Run Number 1 3 5 4 9 8 10 14 15 18 A B C R-Squared LLOQ ULOQ -0.000004 -0.000007 -0.000008 -0.000012 0.000001 -0.000017 -0.000006 -0.000004 -0.000006 -0.000001 0.044503 0.055032 0.039426 0.056127 0.035531 0.055069 0.040644 0.033297 0.038561 0.034524 0.006965 0.008879 0.001905 0.004675 0.023102 0.020659 0.023177 0.021686 0.012040 0.014973 0.9918 0.9884 0.9946 0.9929 0.9784 0.9948 0.9892 0.9878 0.9924 0.9858 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.90 501 Mean S.D. %CV n -0.000006 0.000005 -83.3 10 0.043271 0.008970 20.7 10 0.013806 0.008054 58.3 10 0.9896 0.0049 0.5 10 A, B, andC are coefficientsused to define _e cali_ation curve. Page23 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 8. Back-Calculated Concentrations of Calibration Standards Quadratic weighted 1/x2. All concentrations are expressed as ppb. for PFOS Run Date 13-Oct-2000 14-Oct-2000 16-Oct-2000 18-Oct-2000 19-Oct-2000 20-Oct-2000 20-Oct-2000 23-Oct-2000 31-Oct-2000 23-Mar-2001 Run Number 1 3 5 4 9 7 8 10 15 17 3.94 5.17 11.3 23.6 44.2 85.4 209 332 414 3.81 5.60 3.81 5.08 3.83 4.87 *7.35 5.33 4.08 5.12 3.65 5.16 4.30 5.63 3.54 4.72 4.30 4.92 3.80 5.23 3.32 4.82 4.67 5.42 3.76 4.79 3.73 6.03 3.80 4.56 4.28 5.50 3.65 5.67 4.10 4.90 4.01 5.70 3.42 5.60 12.2 24.2 43.7 86.4 209 331 415 11.2 22.1 45.1 77.4 220 336 406 11.6 24.1 43.1 83.3 203 336 428 12.5 24.9 42.5 77.5 215 325 414 11.3 23.1 42.6 71.2 201 324 406 12.9 24.6 45.8 90.2 200 363 427 12.5 26.1 46.6 85.9 218 350 442 10.2 22.3 42.3 78.6 199 316 392 10.3 24.1 50.5 78.2 213 342 410 10.8 24.2 46.3 78.8 212 336 403 10.0 21.7 44.2 77.9 212 322 395 12.1 24.7 49.8 85.4 219 334 430 11.3 23.2 41.8 76.7 200 327 431 11.8 26.1 47.7 80.9 204 333 434 9.95 20.7 53.2 77.5 "122 307 371 12.5 *3.05 44.9 89.6 197 365 464 12.0 23.4 45.0 84.2 224 347 424 10.7 23.3 42.3 84.5 203 345 368 10.6 26.0 41.2 81.4 232 293 419 11.3 20.3 48.5 89.2 186 380 399 Mean S.D. %CV %Bias n 3.89 0.337 8.7 -1.3 19 5.23 0.401 7.7 1.2 20 11.4 0.913 8.0 0.9 20 23.6 45.4 81.7 209 336 414 1.68 3.24 5.11 11.1 20.0 23.0 7.1 7.1 6.3 5.3 6.0 5.6 0.0 2.7 -4.3 0.0 1.2 0.0 19 20 20 19 20 20 * Sample deactivated as an outlier (not included in summary statistics) Page 24 NorthwestBioanalytical StudyNo. NWBS00-091 ReportNo. NWBR01-065 Table 9. Back-Calculated Concentrations of Calibration Standards for PFOA Quadraticweighted 1/x2. All concentrationsare expressedasppb. Run Date 14-Oct-2000 Run Number 3 15-Oct-2000 6 16-Oct-2000 5 18-Oct-2000 4 19-Oct-2000 9 20-Oct-2000 7 20-Oct-2000 8 23-Oct-2000 10 31-Oct-2000 15 23-Mar-2001 17 1.92 3.36 10.6 25.0 49.0 97.1 241 385 481 1.97 3.36 *7.07 3.12 1.95 3.43 1.89 3.34 1.99 3.33 1.85 3.33 1.74 3.25 2.16 3.32 2.02 2.83 2.12 3.08 1.77 3.52 2.05 3.28 1.99 2.92 1.88 3.62 2.04 3.22 2.00 2.81 1.94 3.49 1.88 3.36 1.54 2.87 2.40 3.40 10.5 25.3 50.2 94.4 240 388 470 11.4 25.9 46.4 92.6 248 396 480 9.83 25.6 46.9 97.3 245 380 461 10.4 26.5 50.2 92.8 256 396 480 10.9 25.7 48.8 89.6 241 402 483 10.5 26.1 50.7 92.5 233 402 461 9.97 25.7 47.0 93.5 236 403 466 10.5 25.9 52.6 97.4 249 386 475 8.96 23.9 53.8 81.6 244 371 454 10.4 28.5 55.4 98.6 270 403 478 9.98 25.5 50.0 92.7 243 371 478 10.7 24.7 52.0 95.1 244 384 497 10.7 25.8 48.1 94.6 243 392 493 I 1.0 26.7 50.0 88.7 226 382 485 10.9 25.1 *69.9 110 173 408 476 10.8 "10.2 48.9 108 225 414 493 9.80 24.9 47.2 89.3 250 383 470 10.7 26.6 49.5 99.2 247 427 443 12.5 27.4 50.2 90.7 256 383 492 10.7 20.7 48.5 99.6 222 400 465 Mean S.D. %CV %Bias n 1.96 3.24 10.6 25.6 0.178 0.234 0.705 1.56 9.1 7.2 6.7 6.1 2.1 -3.6 0.0 2.4 19 20 20 19 49.8 94.9 240 394 475 2.39 6.41 19.3 14.3 14.0 4.8 6.8 8.0 3.6 2.9 1.6 -2.3 -0.4 2.3 -1.2 19 20 20 20 20 * Sampledeactivatedas an outlier(not includedin summarystatistics) Page25 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 10. Back-Calculated Concentrations of Calibration Standards for PFHS Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 13-Oct-2000 Run Number 1 14-Oct-2000 3 16-Oct-2000 5 18-Oct-2000 4 19-Oct-2000 9 20-Oct-2000 7 20-Oct-2000 8 23-Oct-2000 10 31-Oct-2000 15 23-Mar-2001 17 1.36 2.92 10.7 26.5 52.6 104 262 418 523 1.25 3.25 1.37 3.03 1.41 2.95 "7.41 2.56 1.56 2.99 1.15 2.86 1.38 2.93 *25.7 2.81 1.39 2.93 1.23 3.45 1.21 2.75 1.59 2.72 1.41 2.90 1.31 2.90 1.34 2.68 1.47 2.76 1.30 3.01 1.42 2.77 1.41 3.13 1.31 2.71 10.7 25.9 11.1 26.2 51.1 101 248 52.6 99.7 272 398 528 431 543 10.6 27.9 12.2 26.6 52.6 104 251 52.2 94.7 254 418 540 418 539 10.7 27.5 10.9 26.5 51.0 92.8 257 50.7 120 245 413 528 439 524 10.6 29.0 51.6 109 252 426 537 10.4 26.0 53.2 101 257 411 522 8.79 25.0 11.5 27.8 55.8 84.1 255 56.1 106 278 430 511 421 524 11.0 27.8 56.3 101 269 408 510 10.1 26.5 53.5 101 264 423 531 11.4 28.6 52.9 102 259 429 557 10.4 26.9 53.1 93.1 248 411 516 10.7 27.9 *74.5 115 "176 432 502 I0.1 *8.57 52.1 110 231 431 531 11.2 26.0 49.7 98.7 268 419 530 11.2 27.4 52.0 102 266 455 478 10.6 28.1 10.8 28.5 52.5 98.5 283 48.1 104 237 405 527 449 512 Mean S.D. %CV %Bias n 1.36 2.90 10.7 27.2 52.5 102 258 423 525 0.114 0.208 0.677 1.09 2.06 7.95 13.3 14.3 16.9 8.4 7.2 6.3 4.0 3.9 7.8 5.2 3.4 3.2 0.0 -0.7 0.0 2.6 -0.2 -1.9 -1.5 1.2 0.4 18 20 20 19 19 20 19 20 20 * Sample deactivated as an outlier (not included in summary statistics) Page 26 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 11. Back-Calculated Concentrations of Calibration Standards Quadratic weighted l/x 2. All concentrations are expressed as ppb. for PFOSAA Run Date 13-Oct-2000 Run Number 1 14-Oct-2000 3 16-Oct-2000 5 18-Oct-2000 4 19-Oct-2000 9 20-Oct-2000 7 20-Oct-2000 8 23-Oct-2000 10 31-Oct-2000 15 23-Mar-2001 17 1.60 3.10 10.6 25.6 50.6 101 251 401 501 1.54 3.29 10.4 24.7 45.5 91.3 236 383 472 1.50 3.50 11.2 25.1 54.2 92.6 308 425 502 1.61 2.40 10.9 24.2 45.0 93.4 237 388 494 *5.30 3.55 12.9 27.7 46.9 98.3 292 405 506 1.84 3.05 11.0 28.0 52.0 89.1 263 428 484 1.42 2.85 10.9 24.4 50.8 95.8 247 440 457 1.45 2.81 10.1 23.1 49.2 93.8 250 384 472 1.73 3.49 10.6 26.1 53.7 110 269 424 506 1.58 2.29 7.91 23.7 52.4 89.8 248 371 450 1.74 3.61 10.4 29.1 62.5 100 287 435 516 1.31 4.10 10.5 24.8 57.6 99.0 *373 425 514 1.71 2.84 10.4 22.0 51.5 87.6 275 380 472 1.72 3.26 10.7 26.6 53.1 102 291 424 536 1.40 3.34 9.16 26.8 46.5 94.0 237 356 469 1.91 2.72 10.9 24.5 68.5 104 179 424 502 1.52 2.56 10.6 "1.44 49.1 102 238 409 540 1.41 3.26 10.7 24.0 48.1 94.6 271 394 487 1.68 3.36 10.9 25.4 48.1 106 261 433 467 *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 Mean S.D. %CV %Bias n 1.58 3.18 10.6 24.9 52.0 97.3 260 405 492 0.176 0.504 0.916 2.54 6.06 6.42 30.3 33.1 26.6 11.1 15.8 8.6 10.2 11.7 6.6 11.7 8.2 5.4 -1.3 2.6 0.0 -2.7 2.8 -3.7 3.6 1.0 -1.8 18 20 20 19 20 20 19 20 20 * Sample deactivated as an outlier (not included in summary statistics) Page 27 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 12. Back-Calculated Concentrations of Calibration Standards Quadratic weighted 1/x2. All concentrations are expressed as ppb. for PFOSA Run Date 13-Oct-2000 14-Oct-2000 16-Oct-2000 18-Oct-2000 19-Oct-2000 20-Oct-2000 20-Oct-2000 23-Oct-2000 31-Oct-2000 23-Mar-2001 Run Number 1 3 5 4 9 7 8 10 15 17 1.00 2.50 10.0 25.0 50.0 100 250 400 500 1.01 2.84 10.6 25.8 46.6 93.0 249 390 510 0.864 2.91 10.2 22.4 49.3 87.2 275 408 493 0.980 2.21 10.3 25.8 45.8 98.5 242 375 513 *2.36 2.87 10.3 27.1 46.0 94.0 277 395 510 1.06 2.43 9.13 24.5 48.3 86.9 249 394 472 0.924 2.66 11.2 25.6 54.0 97.1 255 458 485 1.07 2.76 12.6 26.3 54.4 98.8 285 417 508 0.936 2.17 8.44 21.9 46.6 89.8 246 386 469 1.15 2.36 8.79 25.8 59.2 83.0 268 399 496 0.882 2.52 9.47 27.1 53.8 89.7 260 410 480 0.760 2.34 8.72 23.1 48.2 90.2 247 371 456 1.24 2.70 11.4 22.8 59.1 105 281 405 541 0.851 2.21 9.55 22.1 44.0 90.8 256 391 479 1.11 3.05 10.3 29.2 50.9 106 259 396 528 0.939 2.19 9.62 22.7 55.0 99.1 168 392 477 1.08 2.60 11.5 *1.08 55.8 102 227 474 573 0.930 2.62 9.96 25.7 52.8 101 289 438 529 1.06 2.48 9.45 24.1 47.2 100 229 362 453 0.984 2.94 9.66 26.3 50.7 93.2 285 370 522 0.906 2.80 10.6 17.0 49.6 106 240 431 458 Mean S.D. %CV %Bias n 0.986 2.58 10.1 24.5 50.9 95.6 254 403 498 0.117 0.276 1.04 2.70 4.46 6.76 27.5 28.9 31.4 11.9 10.7 10.3 11.0 8.8 7.1 10.8 7.2 6.3 -1.4 3.2 1.0 -2.0 1.8 -4.4 1.6 0.8 -0.4 19 20 20 19 20 20 20 20 20 * Sample deactivated as an outlier (not included in summary statistics) Page 28 5i ErEEE EEE BHEEEEEEEEEE 22 CTT Wo [eee eeos e] ERT iV [2 Ellee s 5] alr[e sr as ela els] 2 L1[2 E ele[E efelef=eallLeal=Ell5=]Elc e8] | El Oy E$o2hero[2[3l3[al3) =la[z alaeal; e ale A= Ed $1[2[elofele[alele]elo[ee alee 4 Ea [2[e[ale[zlalxle[]e[z]z]]s[ae]) po THHHEHEHEELEE : & 13] |g] 13] || (2 [3] |2 z =s222aa| 8 [TTR EERE i& [[aaJ|ef[oe[s]][Jeef[aa[fealfee][] 21$f [offs] JeEEl] Ela EfalLa [L|JeE lslaslRel] |y E2110 1% eelTelefe] [EIR Ielefalal| 533i 1 EEE 3 . SA FNNEENECEERR: : Ex3[f a LEa E|eepaa eel] 1 $1 [a|[Ts ofElee [ele] #2 P [a [R le eE lefele] EH] Z B _o o o o o o o, o o Riis: = Ba [[CTTaEl fAEN g E[LELRTEFOEORREER 1$ [leaa slalael a Eele eefalaelel 4 {1 EER 3A1 EEREIERNEalEaEeEEE ) {2 3=EE LT= EREE ERE 323z i $HE fJ[EINRENENEEHeAEeRE: Fla] [slgfals[ 4 pi] i g Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 15. Analytieal QC Summary for PFOS All concentrations are expressed as ppb. Run Date 13-Oct-2000 Run Number 1 14-Oct-2000 3 16-Oct-2000 5 18-Oct-2000 ,4 19-Oct-2000 9 20-Oct-2000 7 20-Oct-2000 8 23-Oet-2000 10 31-Oct-2000 15 23-Mar-2001 17 Low QC (6.40 ppb) 6.41 6.14 6.48 6.80 7.41 "7.81 5.61 5.31 6.77 6.94 *4.41 6.34 5.88 6.28 6.61 5.83 6.62 6.18 *4.60 6.50 Medium QC (126 ppb) 132 127 132 126 109 130 120 107 130 131 131 137 125 139 139 130 129 135 135 "192 High QC (332 ppb) 330 355 339 348 353 309 266 302 340 343 323 375 377 352 359 338 323 322 354 333 Mean S.D. %CV %Theoretical %Bias n 6.25 0.826 13.2 97.7 -2.3 20 132 16.5 12.5 104.8 4.8 20 * > +20% deviation from theoretical 337 25.7 7.6 101.5 1.5 20 Page 33 Northwest Bioanalyticat Study No. NWBS00-091 Report No. NWBR01-065 Table 16. Analytical QC Summary for PFOA All concentrations are expressed as ppb. Run Date 14-0ct-2000 15-0ct-2000 16-0ct-2000 18-0ct-2000 19-0ct-2000 20-0ct-2000 20-0ct-2000 23-0ct-2000 31 -Oct-2000 23-Mar-2001 Run Number 3 6 5 4 9 7 8 10 15 17 Low QC (4.81 ppb) 5.08 5.18 Medium QC (145 ppb) 146 149 4.45 147 4.72 143 5.77 142 5.53 151 4.57 147 4.64 157 4.68 152 5.47 155 *3.70 150 4.84 172 4.83 152 4.87 "181 5.13 171 5.28 167 4.87 156 4.90 ] 147 *2.72 159 4.85 152 High QC (385 ppb) 391 393 359 377 384 374 399 388 390 422 414 398 *466 386 425 431 399 380 412 381 Mean S.D. %CV %Theoretical %Bias n 4.80 0.660 13.8 99.8 -0.2 20 155 10.5 6.8 106.9 6.9 20 * > _+20%deviation from theoretical 398 24.3 6.1 103.4 3.4 20 Page 34 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 17. Analytical QC Summary for PFHS All concentrations are expressed as ppb. Run Date 13-Ot-2000 14-0ct-2000 16-0ct-2000 18-0ct-2000 19-0ct-2000 20-0ct-2000 20-0ct-2000 23-0ct-2000 31-Oct-2000 23-Mar-2001 Run Number 1 3 5 4 9 7 8 10 15 17 Low QC (4.48 ppb) 4.24 4.43 4.60 4.69 5.35 4.81 4.50 4.08 4.66 4.83 4.84 5.12 4.36 5.21 4.64 4.66 4.35 4.60 4.29 4.06 Medium QC (156 ppb) 149 139 154 153 159 156 160 161 159 155 163 167 157 * 188 172 178 160 151 155 171 High QC (417 ppb) 373 421 392 410 441 386 400 408 415 419 406 387 469 440 425 442 403 400 428 406 Mean S.D. %CV %Theoretical %Bias n 4.62 160 414 0.349 10.8 22.9 7.6 6.8 5.5 103.1 102.6 99.3 3.1 2.6 -0.7 20 20 20 * > +20% deviation from theoretical Page 35 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 18. Analytical QC Summary for PFOSAA All concentrations are expressed as ppb. Run Date 13-Oct-2000 14-Oct-2000 16-Oct-2000 18-Oct-2000 19-Oct-2000 20-Oct-2000 20-Oct-2000 23-Oct-2000 31 -Oct-2000 23-Mar-2001 Run Number 1 3 5 4 9 7 8 10 15 17 Low QC (4.60 ppb) 5.10 5.08 4.46 4.85 "5.86 5.14 4.08 3.98 *3.38 4.43 "3.10 4.26 4.73 3.91 4.24 4.29 4.43 4.03 *2.38 4.11 Medium QC (151 ppb) 162 152 176 148 136 156 136 152 150 152 183 * 194 184 "201 160 143 160 157 172 *374 High QC (401 ppb) 411 456 425 456 395 372 379 346 401 426 462 450 *538 377 459 458 393 394 463 456 Mean S.D. 4.29 172 426 0.772 50.8 45.0 %CV %Theoretical %Bias n 18.0 29.5t 10.6 93.3 113.9] 106.2 -6.7 13.9]" 6.2 20 20 20 * > +_25%deviation from theoretical t See comments in Section 4, Results and Discussion Page 36 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 19. Analytical QC Summary for PFOSA All concentrations are expressed as ppb. Run Date 13-Oct-2000 14-Oct-2000 16-Oct-2000 18-Oct-2000 19-Oct-2000 20-Oct-2000 20-Oct-2000 23-Oct-2000 31-Oct-2000 23-Mar-2001 Run Number 1 3 5 4 9 7 8 10 15 17 Low QC (4.00 ppb) 4.37 3.84 3.72 4.21 4.55 4.68 3.29 3.20 4.59 4.65 "2.21 4.14 3.64 4.08 4.58 4.07 3.74 4.10 "2.33 4.47 Medium QC (150 ppb) 148 143 166 148 125 160 127 * 109 170 171 150 158 155 163 175 146 154 158 180 *328 High QC (400 ppb) 392 426 420 449 418 375 *280 334 440 432 368 467 467 350 "483 450 423 412 434 417 Mean S.D. %CV %Theoretical %Bias n 3.92 0.712 18.2 98.0 -2.0 20 162 42.9 26.5? 108.018.0 20 412 49.8 12.1 103.0 3.0 20 * > +25% deviation from theoretical -_See comments in Section 4, Results and Discussion Page 37 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 20. Analytical QC Summary for M556 All concentrations are expressed as ppb. Run Date 13-Oct-2000 14-Oct-2000 16-Oct-2000 18-Oct-2000 19-Oct-2000 21-Oct-2000 22-Oct-2000 23-Oct-2000 31 -Oct-2000 07-Apr-2001 Run Number 1 3 5 4 9 13 12 10 15 18 Low QC (4.00 ppb) 3.65 4.28 3.93 4.30 *5.47 4.68 3.81 3.96 4.10 4.45 3.64 4.14 *2.62 3.33 4.60 4.32 3.95 3.93 4.73 3.51 Medium QC (150 ppb) 149 155 150 156 143 162 140 157 146 147 145 167 * 194 177 157 140 161 149 152 145 High QC (400 ppb) 398 459 452 444 395 378 407 395 387 457 426 411 432 401 443 439 417 406 407 387 Mean S.D. %CV %Theoretical Bias n 4.07 0.599 14.7 101.8 1.8 20 155 13.1 8.5 103.3 3.3 20 * > +20% deviation from theoretical 417 25.2 6.0 104.3 4.3 20 Page 38 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 21. Analytical QC Summary for M570 All concentrations are expressed as ppb. Run Date 13-0ct-2000 14-Oct-2000 16-Oct-2000 18-Oct-2000 19-Oct-2000 20-Oct-2000 23-Oct-2000 30-Oct-2000 31-Oct-2000 07-Apr-2001 Run Number 1 3 5 4 9 8 10 14 15 18 Low QC (4.00 ppb) 4.60 4.46 4.13 4.47 "5.02 4.75 3.58 * 3.51 Medium QC (150 ppb) 157 148 166 150 134 159 135 150 3.85 151 4.84 157 4.37 175 3.68 *207 4.20 167 4.43 148 3.21 159 3.86 159 3.70 164 3.99 160 *4.90 159 4.47 156 High QC (400 ppb) 408 454 432 459 392 375 384 352 400 434 *561 372 468 473 402 413 410 416 446 423 Mean S.D. %CV %Theoretical %Bias l n! 4.20 158 0.512 15.2 12.2 9.6 105.0 5.0 105.3 5.3 20 20 * > +20% deviation from theoretical 424 46.2 10.9 106.0 6.0 20 Page 39 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 22. Serum Study Sample Concentrations All concentrations are expressed as ppb. Sample No. 00223 00461 00660 00759 01339 01346 01485 01696 01739 01816 01997 02005 02393 03257 03423 03450 03482 04063 04627 04789 04854 05250 05325 05333 05370 05447 05456 05570 PFOS PFOA* PFHS* PFOSAA* PFOSA* 23.9 [<LLOQ(I.92) 1.54 <LLOQ(1.60) <LLOQ(1.00) 16.6 2.47 1.96 <LLOQ(1.60) <LLOQ(1.00) 13.8 2.52 <LLOQ(1.36) 3.12 <LLOQ(1.00) 23.0 1.96 <LLOQ(1.36) 1.95 <LLOQ(I.00) 16.3 2.79 1.38 <LLOQ(I.60) <LLOQ(1.00) 10.9 <LLOQ(1.92) <LLOQ(1 36) <LLOQ(I.60) <LLOQ(1.00) 13.2 <LLOQ(1.92)<LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.00) 18.6 2.43 1.36 <LLOQ(1.60) <LLOQ(1.00) 15.7 <LLOQ(1.92)'<LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.00) 22.3 2.23 <LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.00) 67.8 2.65 3.63 <LLOQ(1.60) <LLOQ(1.00) 55.4 3.02 1.66 12.9 <LLOQ(1.00) 25.8 <LLOQ(1.92) 2.36 2.01 <LLOQ(1.00) 41.4 2.13 1.46 1.65 <LLOQ(1.00) 23.6 3.10 <LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.00) 60.1 3.57 3.11 1.86 <LLOQ(1.00) 80.2 3.30 4.59 1.79 <LLOQ(1.00) 32.8 3.31 3.18 <LLOQ(1.60) <LLOQ(1.00) 44.6 2.98 3.33 3.67 <LLOQ(1.00) 25.5 4.53 1.65 <LLOQ(1.60) <LLOQ(1.00) 20.9 2.17 38.9 3.66 1.75 <LLOQ(1.60) <LLOQ(I.00) 2.05 ]<LLOQ(1.60) <LLOQ(1.00) 56.0 6.57 4.49 <LLOQ(1.60) <LLOQ(1.00) 37.5 2.58 2.97 <LLOQ(1.60) <LLOQ(1.00) 49.0 2.87 2.41 3.78 <LLOQ(1.00) 32.4 3.86 2.54 1.71 <LLOQ(1.00) 61.9 3.42 2.55 <LLOQ(I.60) <LLOQ(1.00) 50.4 2.50 1.87 1.67 <LLOQ(1.00) M556" <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) <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" <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 1.22 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.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) <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/'0 (+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 Kesults and Discussion section). Page 40 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 22. Serum Study Sample Concentrations All concentrations are expressed as ppb. (Continued) Sample No. 05573 05842 05843 10277 10525 10526 10637 10664 10726 10736 10773 10837 10873 10881 10885 10891 10899 10910 10960 10991 11174 11214 11260 12651 13214 13225 13421 13592 PFOS PFOA* 52.1 2.81 24.3 <LLOQ(1.92) 26.3 <LLOQ(1.92) 27.8 2.01 34.9 2.36 112 3.01 38.7 2.61 54.3 4.11 21.4 2.17 82.0 2.54 42.3 <LLOQ(I.92) 52.7 2.07 35.0 2.31 30.6 <LLOQ(1.92) 29.3 2.49 15.6 <LLOQ(1.92) 24.0 3.11 23.5 <LLOQ(1.92) 34.6 1.97 26.1 <LLOQ(1.92) 24.6 2.59 37.6 <LLOQ(1.92) 139 2.44 19.5 <LLOQ(1.92) 22.7 <LLOQ(1.92) 19.2 1.98 20.0 <LLOQ(1.92) 41.4 4.21 PFHS* 2.00 <LLOQ(1.36) 1.58 <LLOQ(1.36) 3.01 8.41 2.87 6.17 <LLOQ(1.36) 2.61 4.05 3.49 1.93 1.96 3.69 1.42 1.88 1.36 2.71 1.50 2.06 1.52 6.09 <LLOQ(1.36) 1.63 1.50 1.57 2.51 PFOSAA* PFOSA* M556" M570" 2.14 1.67 1.87 2.23 <LLOQ(1.60) 2.14 2.15 <LLOQ(1.60) 2.38 6.96 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 2.34 <LLOQ(1.60) 1.83 <LLOQ(1.60) <LLOQ(I.60) 2.44 2.58 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(I.60) [<LLOQ(I.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00)I<LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <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(I.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(I.00) <LLOQ(1.00 ) <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) 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 41 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 22. Serum Study Sample Concentrations All concentrations are expressed as ppb. (Continued) Sample No. 13657 13738 13911 14068 14071 14089 14091 14338 14357 14363 14679 14726 14863 14993 15016 15317 15508 15744 15750 15756 20198 20219 20554 21040 21476 23023 23704 23724 PFOS PFOA* 21.3 <LLOQ(1.92) 20.0 3.48 8.76 <LLOQ(1.92) 29.1 <LLOQ(1.92) 11.6 <LLOQ(I.92) 30.8 2.15 26.0 2.34 33.7 1.93 15.9 2.39 46.8 2.34 25.5 2.75 35.8 2.43 22.3 2.06 25.1 <LLOQ(1.92) 15.7 3.20 24.3 2.17 34.6 2.87 36.3 2.84 14.9 <LLOQ(l.92) 16.9 2.73 33.6 3.19 57.4 6.19 35.7 2.36 40.2 1.96 24.5 2.09 68.7 4.55 15.0 2.10 23.3 2.59 PFtIS* PFOSAA* PFOSA* M556" M570" <LLOQ(1.36) 1.67 <LLOQ(I.36) 1.96 <LLOQ(1.36) 1.45 2.55 <LLOQ(1.36) <LLOQ(1.36) 3.06 1.92 2.25 <LLOQ(1.36) <LLOQ(1.36) 2.39 <LLOQ(1.36) 3.24 2.93 <LLOQ(1.36) <LLOQ(1.36) 1.52 6.33 2.28 1.92 <LLOQ(1.36) 4.04 <LLOQ(1.36) 2.26 2.52 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 1.74 <LLOQ(1.60) <LLOQ(1.60) 1.83 2.45 <LLOQ(1.60) 1.81 3.28 1.83 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 1.64 I 3.78 ]<LLOQ(1.60) <LLOQ(I.60) 2.00 2.52 1.88 i<LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00):<LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) 1.12 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50)I<LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) 1.84 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within +_20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 42 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 22. Serum Study Sample Concentrations All concentrations are expressed as ppb. (Continued) Sample No. 23957 24003 24020 24022 24077 24138 24206 24363 24413 24421 24958 24959 24963 24968 30612 30713 31297 31432 31652 32126 32535 32704 33007 33292 33340 33341 33787 33788 PFOS PFOA* PFHS* PFOSAA* PFOSA* M556" M570" 32.0 3.83 4.08 18.0 2.43 1.72 32.7 2.28 <LLOQ(I.36) 31.4 2.70 1.65 21.5 2.00 <LLOQ(1.36) 36.4 2.29 2.45 18.4 2.48 <LLOQ(1.36) 35.9 2.11 <LLOQ(1.36) 45.6 3.75 2.29 7.14 I<LLOQ(1.92) <LLOQ(1.36) 41.4 3.28 1.69 36.8 2.91 <LLOQ(1.36) 46.8 6.11 4.57 51.7 6.36 4.42 20.1 1.94 <LLOQ(1.36) 38.1 2.60 1.57 36.4 2.52 1.54 35.3 3.28 2.00 27.1 <LLOQ(1.92) <LLOQ(I.36) 39.6 3.09 2.16 13.3 <LLOQ(1.92) 1.75 25.1 2.34 <LLOQ(1.36) 45.0 2.97 1.43 23.3 <LLOQ(I.92) <LLOQ(1.36) 25.1 <LLOQ(1.92) <LLOQ(1.36) 20.3 <LLOQ(1.92) 1.43 15.8 <LLOQ(1.92)<LLOQ(1.36) 27.1 3.01 <LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.O0) <LLOQ(2.50) <LLOQ(1.O0) <LLOQ(1.60) <LLOQ(1.O0) <LLOQ(2.50) <LLOQ(1.O0) 5.29 <LLOQ(1.O0) <LLOQ(2.50) <LLOQ(1.O0) 1.86 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.O0) <LLOQ(I.60)_<LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(I.60) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 1.77 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 2.38 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 8.21 <LLOQ(t.00) <LLOQ(2.50) <LLOQ(1.00) 2.06 <LLOQ(1.O0) <LLOQ(2.50) <LLOQ(1.00) 1.97 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(I.00) 3.01 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 3.06 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50)[<LLOQ(1.00) <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) 3.92 <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(I.60) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.60) <LLOQ(I.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(I.60) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 1.94 <LLOQ(1.O0) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 5.68 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(I.00) <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within +20% (+_25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 43 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 22. Serum Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. PFOS PFOA* PFHS* PFOSAA* PFOSA* M556" M570" 33793 33897 33914 33958 34087 34117 34119 34222 34279 34307 34549 34917 35082 35084 35174 35253 35318 35332 35346 35576 35599 35935 35946 35950 35956 40106 40388 40734 32.4 2.61 68.2 2.32 147 <LLOQ(1.92) 36.4 1.97 42.0 2.54 54.8 4.09 141 3.97 134 3.25 14.3 <LLOQ(1.92) 31.7 2.46 178 3.51 68.2 3.45 29.4 2.09 18.3 <LLOQ(1.92) 21.9 2.69 67.6 2.47 36.1 3.46 36.7 2.33 45.0 3.57 33.1 8.03 34.6 <LLOQ(1.92) 34.7 <LLOQ(1.92) 35.7 <LLOQ(1.92) 30.4 2.25 29.0 1.96 59.7 3.99 14.2 <LLOQ(1.92) 25.2 <LLOQ(1.92) 1.40 2.54 3.11 1.69 1.86 <LLOQ(1.36) 2.91 5.17 <LLOQ(1.36) 3.67 10.6 3.12 <LLOQ(1.36) <LLOQ(1.36) 1.81 5.72 <LLOQ(1.36) 2.00 2.00 1.70 1.44 1.64 1.72 <LLOQ(1.36) <LLOQ(1.36) 5.19 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.60) 3.17 <LLOQ(1.60) <LLOQ(1.60) 2.76 1.77 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 3.06 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 2.00 <LLOQ(1.60) 2.50 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 227 2.72 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(I.60) <LLOQ(1.60) 2.16 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) [<LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) 4.40 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1,00) <LLOQ(1.00) <LLOQ(2.50) 3.44 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50)!<LLOQ(I,00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50)_<LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1,00) <LLOQ(2.50)_<LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50)<LLOQ(1.00) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 44 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 22. Serum Study Sample Concentrations All concentrations are expressed as ppb. (Continued) Sample No. 40790 40867 40868 40881 40916 40955 40991 40993 41000 41002 41003 41012 41014 41020 41067 41499 41508 41509 41516 41523 41551 41559 41566 41569 41605 41611 41613 41620 PFOS PFOA* PFHS* PFOSAA* PFOSA* M556" M570" 32.5 2.44 <LLOQ(1.36) I<LLOQ(1.60) <LLOQ(I.00) <LLOQ(2.50) <LLOQ(1.00) 26.2 <LLOQ(1.92) 1.75 <LLOQ(1.60) <LLOQ(I.00) <LLOQ(2.50) <LLOQ(1.00) 57.9 2.39 3.57 <LLOQ(1.60) <LLOQ(1.O0) <LLOQ(2.50) <LLOQ(1.O0) 29.6 3.47 1.53 1.65 <LLOQ(1.O0) <LLOQ(2.50) <LLOQ(1.O0) 15.6 <LLOQ(1.92) <LLOQ(1.36) <LLOQ(1.60)I<LLOQ(1.O0) <LLOQ(2.50) <LLOQ(1.O0) 9.52 <LLOQ(I.92) <LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.O0) <LLOQ(2.50) <LLOQ(1.O0) 20.4 2.16 <LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.O0) <LLOQ(2.50) <LLOQ(1.O0) 24.8 <LLOQ(1.92) <LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.O0) <LLOQ(2.50) <LLOQ(1.00) 43.2 2.11 2.08 <LLOQ(1.60) <LLOQ(1.O0) <LLOQ(2.50) <LLOQ(1.O0) 49.7 4.76 3.32 <LLOQ(1.60) <LLOQ(1.O0) <LLOQ(2.50) <LLOQ(1.O0) 34.7 <LLOQ(1.92) <LLOQ(1.36) 2.34 <LLOQ(1.O0) <LLOQ(2.50) <LLOQ(1.O0) 29.1 1.95 2.19 <LLOQ(1.60) <LLOQ(I.O0) <LLOQ(2.50) <LLOQ(1.O0) 41.3 2.80 3.90 <LLOQ(1.60) <LLOQ(1.O0) <LLOQ(2.50) <LLOQ(1.O0) 42.1 2.96 2.31 2.50 <LLOQ(1.O0) <LLOQ(2.50) I<LLOQ(1.O0) 32.0 3.03 1.89 <LLOQ(1.60) <LLOQ(1.O0) <LLOQ(2.50) <LLOQ(1.O0) 18.5 <LLOQ(1.92) <LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.O0) <LLOQ(2.50) <LLOQ(1.O0) 20.2 2.64 <LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50)<LLOQ(1.00) 25.3 2.67 1.40 <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 54.6 3.05 2.30 <LLOQ(1.60) <LLOQ(I.00) <LLOQ(2.50)I<LLOQ(1.00) 27.8 3.23 1.92 <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 21.9 <LLOQ(1.92) <LLOQ(1.36) 1.72 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 55.2 3.06 2.16 <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50)<LLOQ(1.00) 37.5 2.78 <LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50)]<LLOQ(I.00) 23.5 5.96 <LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 35.7 2.08 <LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 14.6 <LLOQ(1.92) <LLOQ(1.36) <LLOQ(1.60) <LLOQ(I.00) <LLOQ(2.50) <LLOQ(1.00) 32.3 1.98 1.57 <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 22.4 6.13 <LLOQ(1.36) <LLOQ(1.60)' <LLOQ(I.00) <LLOQ(2.50) <LLOQ(1.00) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within +20% (+_25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 45 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 22. Serum Study Sample Concentrations All concentrations are expressed as ppb. (Continued) Sample No. 41621 41623 41626 41633 41650 41665 41784 41859 42174 42524 42579 42621 42671 42818 43095 43146 43246 43310 43484 43519 43520 43542 43864 43882 44145 44391 44448 45329 PFOS PFOA* PFHS* PFOSAA* PFOSA* M556" M570" 11.8 <LLOQ(1.92) 20.3 2.39 18.1 <LLOQ(1.92) 20.0 <LLOQ(1.92) 25.2 <LLOQ(1.92) 25.2 2.42 28.6 <LLOQ(1.92) 18.4 <LLOQ(I.92) 42.8 2.65 32.1 5.78 39.0 3.49 40.5 2.32 21.1 <LLOQ(1.92) 19.5 3.06 34.5 2.13 49.0 3.86 50.3 2.76 52.2 2.91 22.4 <LLOQ(1.92) 12.4 <LLOQ(1.92) 38.2 <LLOQ(1.92) 12.5 2.39 28.4 2.23 18.6 2.20 34.4 <LLOQ(1.92) 20.5 <LLOQ(1.92) 38.3 2.16 17.0 <LLOQ(1.92) <LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.36) 1.60 <LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.36) 1.99 1.86 2.24 1.63 I<LLOQ(1.60) 1.76 <LLOQ(1.60) 1.50 2.79 2.68 <LLOQ(1.60) 2.16 <LLOQ(1.60) <LLOQ(1.36) 2.95 <LLOQ(1.36) <LLOQ(1.60) 2.95 <LLOQ(1.60) 5.05 <LLOQ(1.60) 2.72 <LLOQ(1.60) 3.76 <LLOQ(1.60) <LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.36) 6.73 4.15 <LLOQ(1.60) 2.58 1.96 <LLOQ(I.36) <LLOQ(1.60) <LLOQ(1.36) 2.94 <LLOQ(1.36) <LLOQ(1.60) <LLOQ(1.36) <LLOQ(1.60) 2.60 2.42 <LLOQ(1.36) 4.31 <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) <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) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(3.20) <LLOQ(1.90) <LLOQ(2.50) <LLOQ(I.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(I.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) 1.21 <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(I.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50)'<LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) <LLOQ(2.50) 2.83 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 46 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 22. Serum Study Sample Concentrations All concentrations are expressed as ppb. (Continued) Sample No. 45330 PFOS PFOA* 16.3 <LLOQ(I.92) PFHS* <LLOQ(1.36) PFOSAA* 4.61 PFOSA* M556" <LLOQ(1.00) <LLOQ(2.50) M570" 2.67 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 47 Northwest Bioanalytical Table 23. Plasma Study Sample Concentrations All concentrations are expressed as ppb. Study No. NWBS00-091 Report No. NWBR01-065 Sample No. A-0150 A-0277 A-0334 A-0790 A-1093 A-1211 A-1212 A-1242 A-1332 A-1335 A-1880 A-1929 A-2007 A-2159 A-2527 A-2542 A-2759 A-2760 A-2919 A-3003 A-3133 A-3142 A-3151 A-3169 A-3234 A-3260 A-3297 A-3322 A-3327 PFOS 22.9 31.9 61.8 33.3 16.7 29.3 41.3 18.5 13.1 89.6 41.2 16.6 27.0 28.2 20.1 29.0 36.9 27.5 29.6 64.8 42.9 40.7 10.5 21.7 17.3 69.1 33.4 23.7 41.9 PFOA 3.23 2.75 7.68 12.8 5.06 4.84 6.05 2.00 3.02 6.46 6.47 2.64 6.52 5.83 2.96 4.43 4.36 4.56 4.76 5.34 3.39 9.49 2.12 3.17 3.15 5.57 4.09 4.04 5.34 PFHS PFOSAA PFOSA M556 M570 <LLOQ(1.36) <LLOQ(1.36) 7.91 2.32 2.31 1.91 2.71 <LLOQ(1.36) <LLOQ(1.36) 6.88 2.74 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) 3.07 1.47 2.32 <LLOQ(I.36) <LLOQ(1.36) 2.55 2.30 1.42 <LLOQ(1.36) 1.39 <LLOQ(1.36) 2.35 3.45 <LLOQ(1.36) 2.57 3.29 5.18 3.78 2.85 2.87 2.50 2.59 3.08 1.77 6.07 4.09 3.15 4.25 2.64 2.96 <LLOQ(1.60) 1.83 3.33 3.65 2.44 3.88 8.80 2.47 3.12 3.95 2.50 1.90 2.63 3.50 <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(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) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <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) 5.61 <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) <LLOQ(1.00) <LLOQ(1.00) 2.42 1.80 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) 1.24 <LLOQ(1.00) 1.04 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 2.09 <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) 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. Page 48 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 23. Plasma Study Sample Concentrations All concentrations are expressed as ppb. (Continued) Sample PFOS No. A-3354 23.3 A-3355 70.3 A-3380 29.0 A-3410 69.3 A-3439 61.7 A-3442 27.3 A-3447 40.7 A-3461 43.5 A-3532 56.8 A-3534 40.4 A-3600 38.6 A-3630 32.3 A-3631 17.9 A-3683 33.0 A-3796 19.2 A-3797 62.5 A-3834 48.6 A-3844 33.0 A-3869 58.0 A-3954 29.2 A-3955 22.9 A-3956 38.6 A-4060 45.0 A-4078 41.5 A-4097 19.6 A-4115 45.8 A-4173 60.5 A-4979 55.3 A-6362 30.9 PFOA 18.9 4.73 6.40 71.7 10.8 6.42 6.77 5.76 3.39 4.31 5.43 5.74 4.90 3.29 7.14 6.79 6.50 6.32 5.33 3.58 3.67 5.31 5.92 7.90 5.51 6.98 9.61 5.94 4.54 PFHS PFOSAA PFOSA M556 M570 <LLOQ(1.36) 3.09 2.38 16.5 2.40 2.15 2.23 11.4 <LLOQ(1.36) 4.55 3.14 1.79 <LLOQ(1.36) <LLOQ(I.36) <LLOQ(1.36) 4.65 4.31 1.77 2.59 1.48 1.94 2.54 14.1 2.97 1.64 14.5 1.45 3.22 2.35 6.10 5.72 3.99 28.7 3.86 2.96 3.41 3.83 13.3 5.22 3.93 2.93 2.60 4.19 2.27 <LLOQ(1.60) 2.66 2.87 3.42 4.23 2.02 3.60 7.14 3.50 2.11 4.56 5.15. 3.76 1.60 <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) <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(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) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 3.34 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(1.00) 2.26 <LLOQ(1.00) 1.10 <LLOQ(1.00) 1.07 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 3.15 <LLOQ(1.00) 2.14 3.64 <LLOQ(1.00) <LLOQ(1.00) 1.11 1.63 <LLOQ(1.00) 5.69 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 1.43 1.01 <LLOQ(1.00) <LLOQ(1.00) 1.35 <LLOQ(I.00) <LLOQ(I.00) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within +_20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Page 49 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 23. Plasma Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. A-6657 A-7535 A-7826 A-8008 A-8013 A-8028 A-8115 B-0585 B-1082 B-1112 B-1394 B-1739 B-1740 B-1783 B-2127 B-2170 B-2171 B-2199 B-2228 B-2584 B-2924 B-2938 B-3110 B-3114 B-3163 B-3169 B-3170 B-3171 B-3172 PFOS 32.8 45.5 12.1 28.4 27.2 53.6 54.8 35.2 36.9 20.8 34.8 12.2 28.4 50.1 65.5 33.4 56.4 40.3 38.7 58.6 52.5 45.8 41.0 31.8 65.7 59.1 52.8 50.0 28.9 PFOA 6.70 5.59 2.05 5.39 5.58 5.63 5.99 3.51 5.62 2.95 5.23 3.03 4.51 6.40 6.14 4.39 7.78 5.33 5.55 6.42 10.9 7.32 5.26 3.99 8.58 5.85 5.77 5.19 5.50 PFHS 2.27 2.84 <LLOQ(1.36) 3.15 3.11 1.44 1.60 1.55 1.94 1.56 2.87 7.17 6.51 2.21 4.24 1.98 4.22 3.01 1.45 2.34 2.56 3.97 11.3 1.41 2.63 2.32 3.82 2.29 <LLOQ(1.36) PFOSAA 2.50 3.64 4.30 1.96 2.36 4.40 4.91 1.79 5.25 2.26 2.59 4.05 1.97 29.5 5.42 2.38 3.34 2.24 5.42 5.24 28.0 4.06 2.57 3.90 5.39 2.83 3.42 4.39 4.07 PFOSA M556 M570 <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) <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) <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) 5.19 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 6.63 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 1.29 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 1.32 1.17 1.04 1.77 <LLOQ(1.00) <LLOQ(I.00) 1.69 1.80 <LLOQ(1.00) 1.71 2.86 4.46 1.11 <LLOQ(1.00) 1.11 1.84 1.61 <LLOQ(1.00) <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) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Page 50 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 23. Plasma Study Sample Concentrations All concentrations are expressed as ppb. (Continued) Sample No. B-3195 B-3197 B-3198 B-3206 B-3211 B-3212 B-3225 B-3241 B-3242 B-3265 B-3266 B-3276 B-3282 B-3290 B-3292 B-3402 B-3563 B-3575 B-3844 B-3852 B-3948 B-3952 B-3955 B-3960 B-3978 B-4054 B-4258 B-4259 B-4887 PFOS PFOA 24.2 4.56 48.2 6.97 43.7 6.66 6.50 <LLOQ(1.92) 39.7 5.41 38.6 6.46 40.7 6.76 20.7 3.05 22.7 2.66 59.0 6.93 22.4 3.76 32.9 5.69 44.1 4.89 35.7 7.32 25.9 5.39 32.5 6.35 33.6 5.01 13.6 4.49 18.1 4.57 36.1_ 6.43 41.0 5.54 38.7 7.77 12.9 10.5 18.1 2.91 31.6 8.01 11.6 3.32 25.0 4.32 34.6 4.40 12.9 3.13 PFHS 1.87 3.63 4.87 <LLOQ(1.36) 4.37 2.96 15.2 <LLOQ(1.36) <LLOQ(1.36) 4.95 2.14 2.18 4.05 2.63 2.37 3.89 1.57 1.57 2.24 3.43 2.64 4.31 4.39 3.09 2.57 1.60 3.01 1.56 <LLOQ(1.36) PFOSAA 2.90 5.91 <LLOQ(1.60) 2.71 <LLOQ(1.60) <LLOQ(1.60) 2.30 2.08 2.45 4.76 3.78 3.65 6.60 2.79 5.17 4.50 2.78 2.20 2.08 4.31 5.16 2.56 <LLOQ(1.60) <LLOQ(1.60) 3.39 4.71 3.86 3.22 2.44 PFOSA M556 M570 <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) <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(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) <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) 1.27 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 1.04 1.38 1.44 4.37 <LLOQ(1.00) 1.25 <LLOQ(1.00) <LLOQ(1.00) 5.46 1.33 <LLOQ(1.00) <LLOQ(I.00) 1.63 <LLOQ(1.00) <LLOQ(I.00) 1.65 <LLOQ(1.00) 1.01 <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 1.51 1.57 <LLOQ(1.00) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within +20% (+25% for PFOSA and PFOSA.A) of the target concentration. individual result may exceed the QC acceptance criteria. The statistical error associated with any Page 51 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 23. Plasma Study Sample Concentrations All concentrations are expressed as ppb. (Continued) Sample No. PFOS B-5109 19.2 B-5434 29.5 B-5521 20.7 B-5548 37.5 B-5549 44.0 B-5966 32.1 B-6165 57.3 B-6201 16.5 B-6396 123 B-6397 23.0 B-6649 37.5 B-6883 34.9 B-7259 21.8 B-7512 24.8 B-7926 36.5 B-7936 36.3 B-7957 25.8 B-7962 24.2 F-0494 59.6 F-1385 25.3 F-2872 53.0 F-3028 18.2 F-3029 27.5 F-3118 41.4 F-3233 39.7 F-3367 51.1 F-3368 42.3 F--4089 51.0 F.d,166 41.1 PFOA 5.51 6.21 2.77 6.21 6.05 8.38 12.5 4.14 11.0 4.43 22.0 5.95 6.52 6.37 14.8 13.5 4.53 3.89 19.0 4.43 7.27 6.00 3.33 5.73 5.69 6.57 5.86 9.63 6.71 PFHS PFOSAA PFOSA M556 M570 1.92 3.40 9.89 4.18 3.34 8.98 30.3 2.47 5.86 1.67 65.4 9.16 2.10 2.62 2.38 1.95 18.6 16.2 48.1 <LLOQ(1.36) 3.23 <LLOQ(t.36) 1.83 2.15 13.3 3.22 2.79 11.3 3.13 3.67 3.71 <LLOQ(1.60) 3.09 6.65 2.47 <LLOQ(1.60) <LLOQ(1.60) 127 3.00 2.58 4.98 2.36 2.27 7.36 7.61 3.47 3.56 5.02 5.57 3.30 3.00 2.25 12.4 2.42 40.9 10.1 8.91 4.04 <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(I.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) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(3.20) <LLOQ(2.50) 4.32 <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) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(1.00) 3.74 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.90) <LLOQ(1.00) 1.27 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 1.05 <LLOQ(1.00) 2.64 2.65 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 1.34 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) t.37 <LLOQ(I.00) <LLOQ(1.00) 2.18 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. Page 52 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 23. Plasma Study Sample Concentrations All concentrations are expressed as ppb. (Continued) Sample No. F-4441 F-4456 F-4516 F-4995 F-5050 F-5112 F-5156 F-5289 F-6133 F-6202 F-6610 F-6614 F-6715 F-6716 L-0840 L-0866 L-0868 L-0948 L-1484 L-3082 L-4078 L-4134 L-4535 L-4553 L-4637 L-4731 L-4845 L-5881 L-5945 PFOS I 25.7 48.2 40.9 27.8 38.0 33.2 21.7 28.2 31.7 39.5 25.8 29.2 39.1 37.3 63.4 24.5 48.2 48.1 10.3 35,6 58.1 23,6 16.6 40.2 61.1 33.0 27.5 22.8 18.4 PFOA 5.32 6.96 6.05 5.68 4.85 5.15 3.41 4.06 3.91 4.97 3.74 3.67 9.65 10.2 7.00 8.86 11.7 6.53 2,23 6,68 10.4 4.13 3.81 7.49 9.10 5.62 8.63 3.18 4.00 PFHS PFOSAA PFOSA M556 51570 3.08 2.59 1.56 5.17 6.65 2.46 <LLOQ(1.36) 1.82 3.82 1.78 3.02 3.98 5.50 5.13 3.42 5.54 7.39 4.15 <LLOQ(1.36) 2.07 2.27 1.64 <LLOQ(1.36) 6.57 2,28 <LLOQ(1.36) 40.3 <LLOQ(1.36) 1.59 <LLOQ(1.60) 3.16 2.69 2.00 3.07 3.42 <LLOQ(I.60) 1.82 4.62 12.4 9,23 9.72 2.06 1.97 11.5 2.22 1.97 3,68 2.55 3,23 4.86 3.10 1.85 2.79 86.0 40.8 3.42 3.39 <LLOQ(1.60) <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(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) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 2.70 <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) <LLOQ(2.50) 1.39 1.33 1.20 <LLOQ(1.00) <LLOQ(1.00) 2.06 <LLOQ(1.00) 1.06 <LLOQ(1.00) <LLOQ(1.00) 1.16 1.22 1.02 <LLOQ(1.00) 5.22 <LLOQ(1.00) 1.89 1.37 <LLOQ(1.00) 1.34 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 1.91 1.14 <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) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Page 53 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Table 23. Plasma Study Sample Concentrations All concentrations are expressed as ppb. (Continued) Sample No. PFOS L-7039 32.7 L-7225 32.1 L-7415 35.7 L-7472 30.0 L-7703 49.8 L-7709 43.7 L-7726 25.4 L-7728 31.9 M-0106 52.3 M-0160 25.9 M-0424 67.6 M-0474 37.1 M-2136 41.3 M-2213 42.4 M-2214 40.1 M-2228 32.2 M-2233 54.4 M-2247 33.3 M-3719 20.7 M-4002 78.8 M-4294 37.0 M-4726 26.1 M-4732 25.3 PFOA 5.60 4.54 7.22 4.84 6.26 5.87 4.41, 5.82 5.91 5.86 8.85 7.45 6.34 4.89 6.85 6.40 12.5 7.51 3.07 8.22 5.99 3.60 3.23 PFHS 3.25 4.69 2.69 2.65 1.89 1.84 6.44 8.25 3.55 1.61 6.08 1.86 1.51 2.03 <LLOQ(1.36) 5.29 20.6 <LLOQ(1.36) <LLOQ(1.36) 9.63 8.73 <LLOQ(1.36) <LLOQ(1.36) PFOSAA PFOSA M556 M570 2.48 <LLOQ(1.00) <LLOQ(2.50) 2.22 2.43 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(I.00) 8.00 <LLOQ(1.00) 2.60 1.92 3.73 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 4.28 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(I.00) 3.66 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 5.88 <LLOQ(1.00) <LLOQ(2.50) 1.36 7.98 <LLOQ(1.00) <LLOQ(2.50) 1.65 4.40 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 7.19 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 3.66 <LLOQ(1.00) <LLOQ(2.50) 1.17 10.5 <LLOQ(1.00) <LLOQ(2.50) 2.44 4.90 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 2.89 <LLOQ(1.00) <LLOQ(2.50) 1.09 4.69 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 5.04 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(I.00) 7.07 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 4.81 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 2.49 . <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 14.4 <LLOQ(1.00) <LLOQ(2.50) _2.36 2.90 <LLOQ(1.00) <LLOQ(2.50) 3.25 7.44 <LLOQ(1.00) <LLOQ(2.50) 2.18 7.00 <LLOQ(1.00) <LLOQ(2.50) 2.06 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. Page 54 gH s E{ EH 3 i2s 2ifg zHE 2 8 2H8E siiy g :i 83 E 2% g: 7HEa &: Ss: |S i i= |g 3 z R|Ev] 23 $ (5 Z gfl|Eysd(= 3 |Z]. z BEERS 5 53s EREEIE g2 Z3 EE =-- gZf3 || F= lz|& S2ESg = EE a35 88Ed2 F FE|R RSE2E|EE3 g2FfH z s5g s89SA gE=f]H 2 287% 2 1lz |( 28 3 e 3g g2i% Fg|R2 EE= 2g3f 5 5, 2 3 22 < 15% 3F5E32E3 23Il5e3,s Y. 2 |5% 3:lds gq 2 : S(t EHEPS{R 5 2 5B%225 5 I Ssl- 3 23zi SiFH F81H8 i 2 |= 2% 2 L2 2i3L3 iz 1 3 55 |% i 8E3E gZ f zi 2: 2 3Ss 228Z%Z% iz2 5 3, iii: 252i8s 3 E$Is. 2: Egio 2FiE i : B32 E|5 : |v oif 3[2F|E $ if 7 iIEC BoEufoil JE 4g 3; |5:4x|= REEEL23 2 A 3% F |gs5R8|= 2i 3EEE i[=5228 gti $TE2Ell 1g6 2(133 5 cEoEfNzrPo2oE&lE|%fE2 |=|3|3] |Y iE:sgfz; 5.3 2S1SESls] 22i 22E5 ||gg 4i:f 3 232 1028 813 3 8i 3z% 02 |5g u 7 Iglzz iIl;e, Z i(22 =5[S28x 3i 31 : ls fli: 5E4E2 E5EE 3 4 3% EE |o " =IE 2 ly %5 33 i itA] 28 2E:S ||Aa| 824 : S$ gf $ gt 3 zs1 3= ii: ;z #= bi 2 i: Ez, 4 HH2 [E355ES|- HS i [ra : iz, 4 sif : =i= i: Fg BRE: = 03, 2 138] 3Eo 2 |[88| @ LEP ZF 3:Z liz. ss =33 2:El5z525 32 22%225 of3 EFR|EEE%2 gf3 = 3 5S%&F:z 2 FgEk 2Ele |g|) 8E2 FE E eElz E8|31| 8iu: E$21E9 [O55]E zz8iz 2f1F3E |[|55F] :% :i 3 12 8S3| &#2= iBz E go3lg 2&z ZZ3fHe:i1Ez5% E s2g(lxE[5is3f15 g 2 gi E LAE S5T5%H%: TE5FI5=sF%2E 1 (3% 57 it 3 35 sg2 [8] 35% F5e: ||3S| 23% i 53 5: S$ zi 2 32 i 5i32 &|3g: 4: 2i (3 i H Z S_|13 i 32 [5 E EI37 S 3iEi : i $P s 2 |[F3e22 i%l|=2 SI3i 3 HH 3Elz g|3l| 8E F$(SFE|%| zd $iEl2s 8[[383 sEsc e2= i ' ggs le[= x ME $42 EL, ; i 552 5 3 13 g 3 Fg |= i 2 3 FH i 3%: Northwest Bioanalytical Study No. NWB S00-091 Report No. NWBR01-065 Figure 1. Representative Calibration Curve for PFOS 12 , Analytical Run 3 analyzed on ]4-Oct-2000 Calibration Standards for PFOS (ppb) Regression Method - QUADRATIC - Weighting Factor = l/X*'2 QuadraticLimit_ 2200 g _4 0_ I I I P I I i 0 50 100 150 200 250 300 350 400 450 Nominal Cone. Figure 2. Representative Calibration Curve for PFOA Analytical Run 3 analyzed on 14-Oct-2000 Calibration Standards for POAA Regression Method ffiQUADRATIC - Weighting Factor = If X**2 Quadratic Limit ffi571000 (ppb) 12 10 4 2 0 50 ] 00 ] 50 200 250 300 350 400 450 500 Nominal Cone. Page 59 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Figure 3. Representative Calibration Curve for PFHS 16 14 12 o Analytical Run 3 analyzed gegrassion Method on 14-Oct-2000 Calibration Standards for PFHS = QUADRATIC - Weighting Factor = 1/X*'2 Quadratic Limit = 1600 (ppb) 0 100 200 300 400 500 600 Nominal Cone. Figure 4. Representative Calibration Curve for PFOSAA Analytical Run 3 analyzed on 14-Oct-2000 Calibration Standards Regression Method = QUADRATIC - Weighting Factor Quadratic Limit = -4280 for PFOSAA = I/X**2 (ppb) 16 12 _lO 6 4 0 i i 0 I00 200 300 400 500 600 Nominal Cone. Page 60 Northwest Bioanalytical Figure 5. Representative Study No. NWBS00-091 Report No. NWBR01-065 Calibration Curve for PFOSA Analytical Run 3 analyzedon 14-Oct-2000 Calibration Standardsfor PFOSA (ppb) Regression Method = QUADRATIC - Weighting Factor = lfX'*2 QuadraticLimit = 5900 30 25 _ 20-_ 0' : ! I I ! i 'I I 0 50 100 150 200 250 300 350 400 450 500 Nominal Cone. Figure 6. Representative Calibration Curve for M556 Analytical Run 3 analyzed on 14-Oct-2000 Calibration Standards for M556 (ppb) RegressiMocnthod= QUADRATIC -WeightinFgacto=rI/X*=2 Quadratic Limit = 108000 10 g, 4 2 0 _ 0 50 100 150 200 250 300 350 400 450 500 Nominal Conc. Page 61 Northwest Bioanalytical Figure 7. Representative Calibration Study No. NWBS00-091 Report No. NWBR01-065 Curve for M570 30 ] i I Analytical Run 3 analyzed Regression Method on 14-OcI-2000 Calibration Standards for M570 = QUADRATIC - Weighting Factor = 1/X'*2 Quadratic Limit = 3820 (ppb) 201 0 m'i_ I 0 50 I I I I 100 150 200 250 300 350 400 450 500 Nominal Cone. Page 62 Northwest Bioanalytical Figure 8. Human Plasma Blank for PFOS Study No. NWBS00-091 Report No. NWBR01-065 [PFOS Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 4.96 Current Method [ Noise Thres. _ 5.0 Quant Thres. _ 0.2 Min. Width 131 3 Mult. Width 1121 12 Base. Width _ 100 RT Win. (seca) _ 20 Smooth Ill 1 s009105011 5 011 S00091 CONTROL BLANK 1 Mon, Oct 16, 2000 9:25 PM 8.98 in 1 pedod 1:8.98 MRM, 571 scans 499.0->80.0 Area 8448 558 4.54 5.17 0.63 4.77 A- BB NOComment ITHPFOS use as internal Standard Expected RT 4.32 I Noise Thres. Current _ Method 10.0 Quant Thres. _ Min. Width _ Mult. Width _ Base. Width _ RT Win. (secs) _ Smooth I 1.0 3 5 100 20 11 1 s009105011 5 0q 1 BG'0091 CONTROL BLANK 1 No Comment _,_on.Oct 16. 2000 9:25 PM 8,98 in 1 period 1:8.98 MRM, 571 scans 427.0->407.0 Area 0 Height 0 Start Time End Time Int_ration Width Retention "rime Integration Type 0.00 O.00 0.00 0.0O __ _#_ ................. !_?_i _,_ _ _ _;: N_x4_ Page 63 Northwest Bioanalytical Figure 9. Human Plasma Blank for PFOA Study No. NWB S00-09 l Report No. NWBR01-065 Current Method Use Area Absolute Retention Time Expected RT 4.41 IPOAAIntSetrannadl ard: THPFOS Quant Thres. 0.51 0.5 Min. Width .--q 3 Muir, Width _t i 8 Base. Width _ 100 RT Win. (secs) _ 20 I NoiseTShmreoso.th I _1"0"--'_ 1.01 s009105011 5 0!1 S00091 CONTROL BLANK 1 No Comment Mon, Oct 16. 2000 9:25 PM _'_ ,_%_::%_ 1:8.98 MRM. 571 scans 413.0->169.0 _'!_ _: AHreeigaht 75783 Start'rime End Time Inte.c/retionWidth Retention Time Inte_retion T,pe 4.14 4.49 0.36 4.37 A-BB _,._ _ _i!;_ _,,__; _ _: i_ ....................... _ _ ; ;;1:__ _ _,_7 Page 64 Northwest Bioanalytical Figure 10. Human Plasma Blank for PFHS Study No. NWB S00-09 l Report No. NWBR01-065 [PFHB ] Currant Method Noise Thnes. _ 3.0 Internal Standard: THPFOS Quant Thras. _ 0.5 Use Area Min. Width _ 4 Abso4ute Retention Time Mult. Width _ 10 Expected RT 3.62 Base. Width _ 100 RT Win. (secs) _ Smooth I 20 1] 1 s009105011 5 011 S00091 CONTROL BLANK 1 vton, Oct 16, 20009:25 PM 8,_ioI_iod 1:8.98 MRM, 571 scans 399.0>80.0 Area 1008 Height 125 Start Time End Time Inte,(Iration Width Retention Time Integration Type 3.64 3.96 0.32 3.73 A - BB No Comment __!_!_; _ i _._, _ ................ _>96_, [THPFOS use as Intemal Standard Expected RT 4.32 I _Current Method Noise Thras. 1P1--0--,0--1---I 10.0 Quant Thres, [1.0[ 1.0 Min. Width I 31 3 Mult. Width I 5J 5 Base. Width _ RT Win. (secs) _ Smooth 1 100 20 II 1 S009105011 5 011 $0009! CONTROL BLANK 1 Mon, Oct 16, 2000 0:25 PM 0.98 in 1 period 1:8.98 MRM, 571 scans 427.00>407.0 NO Comment Area 0 Height 0 Start Time 0.00 End Time 0,00 Integration Width 0,00 Retention Time 0.00 Integration Type Ifl4,l'_'lNl_l Page 65 Northwest Bioanalytical Study No. NWB S00-091 Report No. NWBR01-065 Figure 11. Human Plasma Blank for PFOSAA [PFOSAA Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 6.05 I Current Method Noise Thres. _ 4.0 Quant Thres. _ Min. Wadth _ Muir W}dth _ Base. Width _ RT Win. (seas) _ Smooth [ 1.0 3 12 100 20 1[ 1 s009105011 5 011 S00091 CONTROL BLANK 1 16, 2000 9:25 PM No Comment 2759 340 5.67 6.10 0.43 5.91 A - BB [THPFOS use as Internal Standard Expected RT 4.32 ] Current Method Noise Thres. [_ 10.0 Quant Thras. _ 1.0 Min. Width _ 3 MulL Width _ 5 Base. W_lth _ 100 RT Win, (secs) _ Smooth _ 20 1I 1 s009105011 5 011 S00091 CONTROL BLANK 1 Non, Oct 16, 2000 9:25 PM 0.96 in 1 _riod I_ _ _ I_ NO Comment 1:8.98 MRM, 671 scans 427.0->407.0 Ar_, 0 i Height 0 Start Time 0.00 End 13me 0.00 IRnetete_nratitoi0nnTWimideth 00..0000 Inte_lration Type I_ _i :_ _,:_ _ i__!i__ :_I0_ { ;i_i_ ................. _i_ _ _-_,_ _ Page 66 Northwest Bioanalytieal Figure 12. Human Plasma Blank for PFOSA Study No. NWBS00-091 Report No. NWBR01-065 Current Method Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5.59 IPFOSA Quant Thres, Min. Width Muff. Width Base. Wktth RT Win. (seca) ] NoiseSTmhoreosth. _ 0.1 5 10 100 20 3.01 s009105011 5 011 S00091 CONTROL BLANK 1 18, 2000 9:25 PM No Comment 965 108 5.48 5.78 0.30 A-W [THPFOS use as Internal Standard Expected RT 4.32 [ _Current Method Noise Thres. 110.01 10.0 Quant Thres. _ Min. Width I MulL Width I Base. Width _ RT Win. (secs) _ Smooth Ill 1.0 31 3 51 5 100 20 1 s00910501 i 5 011 S00091 CONTROL BLANK 1 Mon, Oct 16, 2000 9:25 PM 8.98 in 1 period 1:8.98 MRM, 571 scans No Comment .... Area 0 Height 0 Start Time 0.00 End Time 0,00 Inte_jrationWidth 0.00 Retention Time 0.00 Integration T)'pe :..y:_. ::: ......=..=,.,=, = Page 67 Northwest Bioanalytical Figure 13. Human Plasma Blank for M556 Study No. NWB S00-091 Report No. NWBR01-065 IMS_ Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5.36 = Current Method I Noise Thins. _ _ 1.0 Quant Thins. _ Min. Width _ Mull Width 1181 Base. Width _ RT Win. (secs) _ Smooth _ 0.1 3 18 200 20 1 sG_09105011 5011 S0009! CONTROL BLANK 1 Mon. Oct 16, 2000 9:25 PM 8.98 in 1 period 1: 8.98 MRM, 571 tD01 556.0->498.0 No Comment Area 905 Height 138 Start Time End Time Integretion Width Retention Time Integration Type 5.23 5.52 0.28 5.39 A - BB : _0_ I THPFOS use as Intamal Standard Expected RT 4.32 I Noise Thres. _1C10u.r0r1ent Meth1o0d.0 Quant Thres. _1_ 1.0 Min. width 131 3 Mult. Width 151 5 Base. Width _ 100 RT Win. (secs) _ 20 Smooth Ill 1 s009105011 5 011 S00091 CONTROL BLANK 1 Mon, Oct 16, 2000 9:25 PM 8.98 in 1 I_riod 1:8.98 MRM, 571 scans 427.0->407.0 No Comment Araa 0 Height 0 Start Time End Time 0.00 0.00 Integration Width 0.00 Retention T]me 0.00 Integration Type II'I_,I_I,-,IPI__I Page 68 Northwest Bioanalytical Figure 14_ Human Plasma Blank for M570 Study No. NWBS00-091 Report No, NWBR01-065 [M570 Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5.89 _ Current Method Noise Thres. [_ 30 Quant Thres. _ 0.2 Min. Width _ 5 Mult. Width _ 15 Base. Width _ RT Win. (secs) _ Smooth _ 100 20 1I 1 s009105011 5 011 300091 CONTROL BLANK 1 Mon, Oct, 16, 20009:25 PM 8.98 in 1 period 1:8.98 MRM, 571 scans 90: 570.0->419.1 NO Comment Area 1408 Height 202 Start Time 5.47 End Time 5.86 Inte_lr,ation Width Retention Time Integretion Type 0.39 5.67 I I A - BB [ I_I_'I"'IMI_I [THPFOS [ use as Internal Standard " Current Noise Thres. _ Quant Thres. 11OI Method 10.0 1.0 Min. Width [ 31 3 Expected RT 4.32 Muir. Width _ Base. Width _ RT Win. (secs) _ Smooth _ 5 100 20 1I 1 s0091050!1 5011 SC009! CONTROL BLANK 1 Mon, Oct 16, 2000 9:25 PM 8.98 in 1 pened 1:8.98 MRM, 571 scans 427.0->407.0 NoComment Area 0 Height 0 Start Time End Time 0.00 0.00 Integration Width 0.00 Retention Time O.OO I Integration Type 1t'14,1...tM1_1 Page 69 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Figure 15. Human Plasma Blank with Internal Standard (QC0) for PFOS [PFOS Current Method I Noise Thres. _ 5.0 Use Area Absolute Retention Time Expected RT 4.96 tntemal Standard: THPFOS Min. Width Mult. W_dth Base. Width RT Win. (seca) Quant STmhoreoeth. _ sGV09105001 5 001 $_q091 QC 0 1 _,'lon,Oct 16, 2000 7:28 PM 8.98 in 1 period 1:8.98 MRM, 571 scans 499.0->80.0 No Comment Area 8316 Height 638 Start Time End Time Inter.retion Width Retention Time Integration Type 4.55 5.12 0.57 4.79 A - BB 3 12 100 20 0.2t I THPFOS Current Method I Noise Three. _ 10.0 Expected RT 4,32 use as Intamal Standard Min, Width 3 Mull Width 5 Base. Width 100 RT Win. (secs) 20 QuantSTmhoroesth, _ 1.01 s009105001 5 001 S00091 QC 0 1 IMon, Oct 16, 2000 7:28 PM 8.98 in 1 period 1:8.98 MRM, 571 scans 427.0->407.0 Area 118018 Height Start Time End Time 17845 Integration Width Retention Time Integration Type 4.19 4.57 0.38 4.38 A * BB No Comment Page 70 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Figure 16. Human Plasma Blank with Internal Standard (QC0) for PFOA ipoA A ] Noise Thres. _1C1,u9r1rent Metho1d.0 internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 4.41 Quant Thres. I-'---_--IL Min. Width _1 3J Muir Width 181 Base. Width _ RT Win. (secs) _ Smooth J 'lJ 0.S 3 8 100 20 1 s009105001 5 001 SC_q01QC 0 1 No Comment Mort. Oct 16, 2000 7:28 PM 8.98 in 1 perio(l 1:8.98 MRM, 571 scans !i 413.0->169.0 Area 1050 104 4.14 4.55 0.41 A- BB use as Internal Standard Expected RT 4.32 ITHPFOS Current Method Quant Thres. Min. Width Muir Width Base. Width RT Win. (secs) _ Noise S"mDloroethS,_ 1.0 3 5 100 20 10.01 sC-09105001 5 001 S00091 QC 0 1 Mon, Oct 16, 2000 7:28 PM 8.98 in 1 period 1:8.98 MRM, 571 scans 427.0->407.0 Area 118018 Height 17845 Start Time Width 4.19 4.57 0.38 4.38 A - BB No Comment Page 71 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Figure 17. Human Plasma Blank with Internal Standard (QC0) for PFHS IPFHS Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 3.62 I _Current Method Noise Thres. _ 3.0 Quant Thres. _ 0.5 Min. Width _ 4 MulL Width 1101 10 Base. Width _ 100 RTWin. (secs) _ 20 Smooth _ 1 sOOt05001 5 001 S0009_ QC 0 1 Mon, Oc_ I_, 2900 ?:28 PM 698 in 1 period 1:8.98 MRM, 571 scans 399.0->80.0 No Comment Area 879 Height 95 Start Time 3.51 End Time 3.83 Inte(,{r,etion Width 0.32 Retention Time 3.77 Inte_lretionType A - BB I'_1_I'_IMI_I I TuHsePaFsOSInternal Standard Expected RT 4.32 Current Method I Noise Thres. _ 10.0 Quant Thres. 1.0 Min. Width 3 Mult. Width 5 Base. Width 100 RT Win. (secs) 20 Smooth 1 s009105001 " 5 001 S00091 QC 0 Moo, Oct 16, 2000 7:28 PM 8.98 in 1 period 1:8.98 MRM, 571 scans 427.0->407.0 Area 118018 Heiqht Start Time End Time 17845 IntecdrationWidth Retention Time Integration Type 4.19 4.57 0.38 4.38 A - BB No Comment Page 72 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Figure 18. Human Plasma Blank with Internal Standard (QC0) for PFOSAA ipFos_ Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 6.05 = Current Method I Noise Thres. 14,01 4,0 Qusnt Thtes. t--------t_ 1.0 Min. Width [31 3 Mull Width 1121 12 Base. Width _ 100 RT Win. (secs) _ 20 Smooth Ill 1 sO09105001 5 001 S00091 QC 0 1 Mon, Oct, 16. 2000 7:28 PM 8.98 in 1 period 1:6.88MRM57,1.... 584.1->419.1 Area 1124 Height 193 Start Time End Time Integration Width Retention Time Integmtioo Type 5,72 6.02 0.30 5.89 A - BB No Comment iTHPFOS use as Intamal Standard Expected RT 4.32 I _Current Method Noise Thres. 110.01 10.0 Quant Thres. _ 1,0 Min. width 131 3 Mull width 151 5 Base. Width _ RT win. (seca) _ Smooth I 100 20 1} 1 s009105001 5 001 SC<)091QC 0 1 Mon, Oct 16, 2000 7:28 PM 6.98 in 1 period 1:8.98 MRM, 571 .scans 427.0->407.0 No Comment Area 118018 Hei,qht Start Time End Time 17845 Integration Width Retention Time Integration T),pe 4.19 4.57 0.38 4.38 A - BB Page 73 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Figure 19. Human Plasma Blank with Internal Standard (QC0) for PFOSA IPFOSA Internal Standard: THPFO$ Use Area Absolute Retenl_onTime Expected RT 5.59 I Current i Noise Thres. Method 3.0 Quant Thres. i.-Min. Width =,--- Muft. Width _ Base. Width E.-RT Win. (secs) _-- Smooth _ 0.1 5 10 100 20 1 s009105001 5 001 S0009_ QC 0 1 Oct 1_, 2000 7;28 PM No Comment 0 o.oo 0.00 N'_ i?r _ _,_ _..,.____,i_::::_:_3 Page 74 Northwest Bioanalytical Figure 20. Human Plasma Blank with Internal Standard Study No. N'vVBS00-091 Report No. NWBR01-065 (QC0) for M556 I M556 internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5.36 I Current Method Noise Thres. _] 1.0 Quant Thres. _ 0.1 Min. Width _ 3 Mult. Width _ 18 Base. Width _ 200 RT Win. (secs) _ 20 Smooth [1[ 1 s009105001 5 001 $00001 QC 0 1 Mon, Oct 16, 2000 7:28 PM 8.98 in '1period 1:8.98 MRM. 571 scans 556.0->498.0 No Comment Area 0 0 .... width [THPFOS use as Internal Standard Expected RT 4.32 [ Current Method Noise Three. I_ _ 10.0 Quant Three. [1.0[ 1.0 Min. width 131 3 Mull width J 51 5 Base. W'Klth_ RT Win. (sacs) _ Smooth I 100 20 11 1 s009105001 5 001 $00091 QC 0 1 Vlon, Oct 16, 2000 7:28 PM _! 8.98 in 1 period 1:8.98 MRM, 571 scans 427.0->407.0 Area 118018 Hei,qht Start Time End Time 17845 IntecJrationWid_ Retention Time Inte(jration Type 4.19 4.57 0.38 4.38 A - BB No Comment Page 75 Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Figure 21. Human Plasma Blank with Internal Standard (QC0) for M570 [meT0 Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 8.89 Current Method J Noise Thres. _ 3.0 Quant Thres. _ 0.2 Min, Width 151 5 Mull Width 115] 15 Base. Width _ RT Win. (secs) _ Smooth Ill 100 20 1 sOOg105001 5 001 S00091 QC O 1 lg. 2000 7:28 PM No Comment 0 0 0.00 0.00 n Width 0.00 0.00 I THPFOS use as Internal Standard Expected RT 4.32 Current Method I Noise Three. [_ 10.0 Quant Three, _ Min. Width [ 1.0 3J 3 Mult, Width 151 5 Base. Wclth _ RT Win. (secs) _ Smooth I 100 20 lJ 1 s009105001 5 001 800091 QC 0 1 k,lon, Oct 16, 20007:28 PM 8.98 in 1 period 1:8.98 MRM, 571 scans 427.0->407.0 No Comment Area 118018 Hei,qht Stad Time End Time 17845 Inte<jrationWidth Retention Time Integration Type 4.19 4.57 0.38 4,38 A * BB Page 76 Northwest Bioanalytical Figure 22. Low Standard for PFOS Current Method [PFOS [ Internal Standard: THPFOS Use Area Absolute Retention Time Noise Thres. _ 5.0 Quent Thres. _ Min. Width i 0.2 3i 3 MulL Width 1121 12 Expected RT 4.96 Base. width _ RT win. (secs) _ Smooth _ 100 20 1 s_09105002 5 002 S0009i Stdl 1 1 Mort, Oct 16, 2000 7:40 PM 8.96 in 1 period 1:8.98 MRM, 571 scans 499.0->80,0 Area 11564 Height 741 ;tam Time End Time Inte_retion Width Retention Time Intecjretion T_c_e 4.52 5.15 0.63 4.98 A - BB No Comment Study No. NWBS00-091 Report No. NWBR01-065 [THPFOS use as Internal Standard Expected RT 4.32 Current Method ] Noise Thres. _ Quant Thres. _ Min. width I Mull Width _ Base. Width _ RT Win. (secs) _ Smooth I 10.0 1.0 31 3 5 100 20 11 1 s009105002" 5 002 S00091 Stdl 1 1 iMon, Oct 16, 2000 7:40 PM 8.g8 in 1 period 1: 8.98MRM, 571 scans 427.0->407.0 152577 22509 4.t9 4.60 0.41 4.38 A - BB I_1_I**IMI_I No Comment Page 77 Northwest Bioanalytical Figure 23. Low Standard for PFOA Internal S_ndard: THPFOS Use Area Absolute Reten_on Time Expected RT 4.41 I Currant Method I i Noise _s. 11.01 1.0 Quant _res. _ Min. Width 131 MulL Width 181 Base. Width _ RT Win. (sacs) _ Smooth [11 0.5 3 8 100 20 1 sC_9105002 5 002 SC_091 Stdl I 1 No Comment Mon. Oct 16. 2000 7:40 PM 8.98 n t period : 1:8.98 MRM, 571 scans _0 413.0->169.0 30,o H_ght 329 S_d Time End Time Inter,ration Width Retention Time Integration Type 4.07 4.55 0.49 4.40 A- BB _Qi i_ :il : i,i,'__ _ _:_ Study No. NWBS00-091 Report No. NWBR01-065 ITHPFOS use as Internal Standard Expected RT 4.32 I Current Method I m Noise Thres. 110.01 10,0 Quant Thres. _ Min. Width 131 Mult. Width 151 Base. Width _ RT Win. (sect) _ Smooth Ill 1,0 3 5 100 20 1 s009105002 5 002 S00091 Stdl 1 1 Vlon, Oc_ 16, 2000 7:40 PM 8.98 in 1 period 1:8.98 MRM, 571 scans 427.0->407.0 No Comment Area 152577 22509 Start Time End Time Retention Time 4,19 4,60 0.41 4.38 A - BB Page 78 Northwest Bioanalytical Figure 24. Low Standard for PFHS iPFH S ] Current Method Noise Thres. _ 3.0 Internal Standard: THPFOS Quant Thres. _ 0.5 Use Area Min. Width _ 4 Absolute Retention Time Muir. Width _ 10 Expected RT 3.62 Base. Width _ 100 RT Win. (sacs) _ 20 Smooth _ 1 SC,.._9106002 5 002 S._091 Stdl 1 1 Mor_,Oct 16, 2000 7:40 PM 8.98 in 1 period _|0_ 1:8.9M6 RM57, 1a=ns 399._-80.0 A_a 633e Hsetigaht_T7im05 , End Time Int_. ration Width Retention Time Integration Type 339 !i::_ 3.94 0.55 _( 3.73 _i_i A - BB _'_ No Comment ii!i!ii_iii_!i Study No. NWBS00-091 Report No. NWBR01-065 I THPFOS use as Intemal Standard Expected RT 4.32 I t"-'--'----tCurMreentht od Noise Threa. _ 10.0 Quant Thres. 11.01 1.0 Min. Width I 3_ 3 Mull Width 151 5 Base. W'idth _ RT Win. (sacs) _ Smooth _ 100 20 11 1 s009105002 5 002 S00091 Stdl 1 1 Mon, Oct 16, 2000 7:40 PM 8.98 in 1 period 1:8.98 MRM, 571 scans 427.0->407.0 Area 152577 225O9 No Comment 0.41 4.38 A - BB Page 79 Northwest Bioanalytical Figure 25. Low Standard for PFOSAA Study No. NWBS00-091 Report No. NWBR01-065 [PFOSAA ] _Current Methoci Noise Thres. 14.01 4.0 Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 6.05 Quant Thres. _ 1.0 Min. Width _ 3 Mult. Width 1121 12 Base. Width _ 100 RT Win. (secs) _ 20 SmOoth I1] 1 s009105002 5 002 S000g! Stdl 1 1 MortO. _16,20007:40PM 8.98 in 1 period 1:8.96 MRM, 571 scans 584.%>419.1 No Comment Area 5691 725 5.61 6.11 =Width 0.50 A- BB _--_' ITHPFOB use as Internal Standard Expected RT 4.32 j Current Method Noise Thres. _] 10.0 Quant Thres. _ 1.0 Min. Width 131 3 MulL W'Klth 151 5 Base. WKIth _ 100 RTWin. [secs) _ 20 Smt_oth Ilt 1 sO09105002 5 002 S00091 Btdl 1 1 Mon, Oct t6, 20007:40 PM 8.98 in 1 pedod 1:8.98 MRM, 571 scans 427.0->407.0 Area 152577 Hei,qht 22509 Start Time End Time Integration Width Retention Time Integration Type 4.19 4.60 0.41 4.36 A - BB NN No Comment Page 80 Northwest Bioanalytical Figure 26. Low Standard for PFOSA Study No. NWBS00-091 Report No. NWBR01-065 IPFOSA Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5.59 i Cun_nt Method I Noise Thres. I 3.0_ 3.0 Ouant Thres. _ Min. Width [5] MulL Width [101 Base. Width _ RT Win. (secs) _ Smooth _ 0.t 5 10 100 20 1I 1 s009105002 5 002 S00091 Std! 1 1 k_on, Oct 16, 2000 7:40 PM 8,98 in 1 period 1:8.98 MRM, 571 scans 498.0->78,0 Area 7479 Hei_]ht 934 Start Time End Time Integration Width Retention Time Integration Type 5.26 5.86 0.60 5.67 A - BB No Comment I THPFOS use as Internal Standard Expected RT 4.32 I Current Method Noise Thres. [_ 10.0 Quant Thres. _ 1.0 Min. W_dth _ 3 Mull W=dth _ 5 Base. Width _ 100 RT Win. (secs) _ 20 Smooth Ill 1 s009105002 5 002 800091 Bid1 1 1 16, 2000 7:40 PM No Comment 152577 22509 Page 81 Northwest Bioanalytical Figure 27. Low Standard for M556 [M556 Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5.36 ] _Current Method No_seThres. _ Quant Thres. 10.11 1.0 0.1 Min. Width _ 3 Mull Width [18[ 18 Base. Width _ RT Win. (secs) _ Smooth _ 200 20 1I 1 sC_9105003 5 003 S0009"_ S[d2 1 1 Mon, Oct 16, 2000 7:52 PM 6.96 in 1 period 1: 8.98 MRM, 571 scans 556.0->496.0 No Comment Area 6787 Height 907 Start Time 5.12 End Time 5.58 Inte_retion Width 0.46 Retention Time Integration T),pe 5.42 A - B8 1_'1,1,1,..t_ Study No. NWB S00-091 Report No. NWBR01-065 [THPFOS use as Internal Standard Expected RT 4.32 ] Current Method Noise Thins. [_ 10.0 Quant Three. _ 1.0 Min. Width _ 3 Mutt. Width _ 5 Base. Width _ 100 RT Win. (secs) _ Smooth I 20 1_ 1 s009105003 . 5 003 S00091 Std2 1 1 Mon, Oct 16. 2000 7:52 PM 8.98 in I period _i_(3 1:8.98 MRM. 571 scans ,_)_ No Comment 427.0->407.0 ii _ Area HSteairqthTt ime End Time 149502 22420 |nt_retion Width Retention Time _ 4.22 4.63 _ 0.41 _ 4.38 Integration Tit_oe A - BB _ Page 82 Northwest Bioanalytical Figure 28. Low Standard for M570 Current Method IM570 ] Internal Standard: THPFOS Use Area Absolute Retention Time Noise Thres. Quant Thres. Min. Wid_ Muff- Wtd_ _ _ 151 115] Expen_ed RT 5.89 Base, Width _ RT Win. {sees) _ Smooth Ill 3.0 0.2 5 15 100 20 1 s009105_02 5 002 S0009_ S_dl 1 No Comment 5.98 in 1 period !; 1:8.98 MRM. 571 scans 570.0->419.1 Area 7142 Hei,_]ht 1105 Start Time End lqme Integration Width Retention Time Integration Type 5.44 5.68 0.44 5.69 A - BB _;/'Oq ': Study No. NWBS00-091 Report No. NWBR01-065 ITHPFOS use as InternalStandard Expected RT 4.32 I N_==Thr1esI.0.01lO.O Quant Thre=. _ Mth. Width _ MutL Width _ Base. Width _ R'r Win. (sees) _ Smooth [11 1.0 3 5 100 20 1 S009105002 5 002 S00091 Sldl 1 1 Mon, Oct 16, 2000 7:40 PM !_: I 8.96 in 1 period _ 1:8.98 MRM, 571 scans 427,0->407.0 _ Area 152577 _.._ No Comment i StarI'Pane End Time Integration Width Retention Time Integration Type 4.19 4.60 0.41 4.38 A - BB "_=Q _*_ _ Page 83 Northwest Bioanalytical Figure 29. High Standard for PFOS I PFOS Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 4.96 J _Current Method Noise Thres. _ 5.0 Quent Thres. 10.21 0.2 Min. Width _ Mull Width _ Base. Width _ RT Win, (sect) _ Smooth J 3 12 100 20 11 1 s009105010 5 010 S00091 Std9 1 1 Non, Oct 16, 2000 9:13 PM I::! 8.98 in 1 period 1:8.98 MRM, 571 scans 499.0->80.0 lg Ama 1221800 Height Start Time 12O59O ! End Time i Int_, ration Width Retention Time Inta_ratJon Type 4.41 5.47 1.06 4.98 A - BV No Comment Study No. NWBS00-091 Report No. NWBR01-065 JTHPFOS use as Intamal Standard Expected RT 4.32 j Current Method Noise Three. [_ 10.0 Quant Thrse. _ 1.0 Min. Width _ 3 Muir W'KU_ _ 5 Base. Width _ 100 RTWin. (secs) _ 20 Smooth J lJ 1 s009105010 5 010 S00091 Std9 1 1 Mort, Oct 16, 2000 9:13 PM 8g8inI pe,od _ 1:8.98 MRM, 571 scans 4270-,4o7o Area 141962 Heiflht Start Time 20849 End Time Integration Width Retantion Time Inteprat on Type 4.21 4.59 0.38 4.38 A - BB _;Sfl _ _ii_ _ No Comment iii3i;O_ Page 84 Northwest Bioanalytical Figure 30. High Standard for PFOA Study No. NWBS00-09I Report No. NWBR01-065 [POA.A Internal Standard: THPFO$ Use Area Absolute Retention Time Expected RT 4.41 I _Current Method Noise Thres. 1.0 Quant Thnss. 10.51 0.5 Min. Width _ Mull Width _ Base. Width _ RT Win. (seca) _ SmooIth 3 8 100 20 11 1 s009105010 5 010 S00091 Sld9 1 1 Mon. Oct 16, 2000 9:13 PM 8,98 in 1 period 1:8.98 MRM, 571 scans 413.0->169.0 NOComment Area 951504 Height 100477 ; Start Time 3.94 End Time 4.82 Intefl,ration Width Retention Time Intagmtion Type 0.88 4.43 A - BV JTHPFOS use as Intamal Standard Expected RT 4.32 [ _Current Method Noise Thins, _ 10.0 Min. Width 3 Mull Wlclth 5 Base. W'_th 100 RT Win. (seca) 20 QuantSTmhoreo=th. _ 1.01 S009105010 5 010 S00091 Std9 1 1 Mon, Oct 16, 2000 :13 P_.t _i! 8.98 in 1 period 1:8,98 MRM, 571 scans 427.0->407.0 Area 141962 Hei,qht Start Tone End Time 20849 Integration Width Retention Time Integ._tion Type 4.21 4.59 0.38 4.38 A - BB No Comment Page 85 Northwest Bioanalytical Figure 31. High Standard for PFHS IPFHS I Internal Standard: THPFOS Noise Thres. Quant Thres, _Current Method 3.0 I 0.SJ 0.5 Use Area Absoluta Retention Time Expected RT 3.62 Min. Width _ 4 Muir. Width _ 10 Base. Width [1001 100 RT Win. (secs) _ Smooth _ 20 lJ 1 s009105010 5 010 $000e_IStd9 1 1 Mon. Oct 16, 2000 9:13 PM 5.98 in 1 period |QO 1:8.98 MRM, 571 scans 399.0->80.0 No Comment Area 1677751 Height 191933 Start Time End Time Integration Width Retention Time Integration Type 3.28 4.29 1.01 3.75 A - BV Study No. NWBS00-091 Report No. NWBR01-065 iTHPFOS use as Intamal Standard Expected RT 432 I Current Method Noise Thins. [_ Quant Thres. _ 10.0 1.0 Min. Width _ 3 Muir. Width _ Base. Width _ RT Win. (secs) _ Smooth Ill 5 100 20 1 S009105010 5 010 800091 Stdg 1 1 NO Comment Mon, Oct 16, 2000 9:13 PM 8.98 in1 period 1:8.9_8.., 5,1.... ] ,._,:._, '!_@_ 427.0->407.0 Area 141962 Hei.qht 20849 Start Time End Time Integration W'KI_ 4.21 4.59 0.38 _ _'; i_ _ i _ii RinetetegnratitoionnTTimypee A4-.3B8B li_ ] Page 86 Northwest Bioanalytical Figure 32. High Standard for PFOSAA Study No. N_VB S00-091 Report No. NWBR01-065 [PFOSAA Intamai Standard: THPFOS Use Area Absolute Retention Time Expected RT 6.05 I _Current Method Noise Thres. 4.0 Quant Thres. [ 1.0J 1.0 Min. Width _3J 3 MulL Widt_ _ 12 Base. Width I 1001 100 RT Win. (secs) _ 20 Smooth _ 1 s009105010 5 010 SD009"_ Std9 1 1 Mon, Oct 16, 2000 9:13 PM 8.96 in 1 period 1:8.98 MRM, 571 scans 584.1->419.1 Area 1725312 Height Start Time End Time 222064 Integration Width Retention Time Integration Type 5.44 6.60 1.17 5.91 A - BV No Comment ITHPFOS use as Internal Standard Expected RT 4.32 Current Method J No_se Thres. _ 10.0 Quent Thres. 1.0 Min. Width 3 Mull Width 5 Base. Width 100 RT Win. (seca) 20 Smooth 1 s009105010 - 5 010 S00091 Std9 1 1 Mon, Oct 16, 2000 9:13 PM 8.98 in 1 period 1:8.98 MRM, 571 scans 427.0->407.0 !Area 141962 He_,qht 20849 Start Time 4.21 End Time 4.59 Integration Wid_ 0.38 Retention Time 4.38 Intaration Type A - BB Ifl,l,l'.'lMl_l No Comment Page 87 # Northwest Bioanalytical Study No. NWBS00-091 Report No. NWBR01-065 Figure 33. High Standard for PFOSA ]PFOSA I _Current Method Noise Thres. 13.01 3.0 Internal Stanaard: THPFOS Use Area Absolute RetenUoo Time Expected RT 5.59 Quant Thras. _ Min. Width _ Mull Width _ Base. Width _ RT Win. (secs) _ Smooth Ill 0.1 5 10 100 20 1 s009105010 5010 S00091 Sid9 1 1 Mort. Oct 16. 2000 9:13 PM 8,98 in 1 period 1:8.98 MRM, 571 scans 498.0->78.0 Area 3016013 Height 331247 Start Time End Time Integration Width Retention 33me Integration Type 5.20 6.87 1.67 5.67 A - BB NO Comment ! I THPFOS USeas Internal Standard Expected RT 4.32 I Current Method Noise Thras. _ 10.0 Quant Thras. _ 1.0 Min. Width _ 3 Mull Width _ 5 Base. Width _ 100 RT Win. (secs) _ Smooth I 20 11 1 s009105010 5 010 S00091 Std9 1 1 Mon, Oct 16, 20009:13 PM 8.9s In 1 period t_ 1:8.98 MRM, 571 scans !"_ 427.0->407.0 ;_ No Comment" Area 141962 Hei,qht 20849 Start Time End Time Integration Width Retention Time Integration Type 4.21 4.59 0.38 4.38 A - BB 1_14,1"'1_1__1 , _i ii_..i.!. _:_ _0 i_! ........ Page 88 Northwest Bioanalytical Figure 34. High Standard for M556 Study No. NWBS00-09] Report No. NWBR01-065 Page 89 Northwest Bioanalytical Figure 35. High Standard for M570 Study No. NWB S00-091 Report No. NWBR01-065 tM570 internal Standard: THPFOS Use Area AbsOlute Retention Time Expected RT 5.89 I _Current Method Noise Thres, 13.01 3.0 Quant Thres. _ Min. Width _ Mutt. Width 1151 Base. Width _ RT Win. (sees) _ Smooth Ill 0.2 5 15 100 20 1 S00910'_310 5010 S000gl Std9 1 1 Mort, Oct 16, 2000 9:13 PM 6.98 in 1 period 1:8.98 MRM, 571 scans 570.0->419.1 Area 2436405 326724 5.33 6.38 1.06 5.70 A - BV No Comment 3_'_'_"_ ,p$ ITHPFOS use as thtemal Standard Expected RT 4.32 I r'-------tCurrMenet hod Noise Thins. _ 10.0 Quant "l_res. 11.01 1.0 Min. Width 131 3 Mult. Width 151 5 Base. Width _ 100 RT Win. (secs) _ 20 Smooth Ill 1 s009105010 5 0'_0 S00091 Std9 1 1 Mon. Oci 16, 2000 9:13 PM 8.98 in 1 pedod 1:8.98 MRM. 571 scans 427.0->407.0 Area 141962 HeiRht Start Time End Time 20849 Intagmtion Width Retention Time Intecjration Type 4.21 4.59 0.38 4.38 A - BB No Comment Page 90