Document aBMDoYEjMZVXORYObrORom769

/,i'qorthwest Bioanaiytical Study No. NWBS00-088 Report No. NWBR01-001 Quantitative Determination of PFOS and Related Compounds in Human Serum by LC/MS/MS Sample Analysis Report for Protocol EPI-0011 Northwest Bioanalytical (NWB) A Division of NWT Inc. 1121 East 3900 South Salt Lake City, UT 84124 PREPARED FOR: 3M Company Corporate Occupational Medicine, Medical Department 220-3W-05 St. Paul, MN 55144 AUTHOR: Connie O. Sakashita, B.S., NWB Project Manager APPROVED FOR RELEASE By: Rodger L. Foltz, Ph.D., N'_B Technical Director Page 1 Northwest BioanaLytical Study No. NWBS00-088 Report No. NWBR01-001 QUALITY ASSURANCE STATEMENT LABORATORY: Northwest BioanalyticaI (NWB) A Division of NWT Inc. 1121 East 3900 South Salt Lake City, UT 84124 SPONSOR: 3M Company Corporate Occupational 220-3W-05 St. Paul, MN 55144 Medicine, Medical Department COMPOUND(S): NWB STUDY NUMBER: SPONSOR STUDY NUMBER: PFOS and Related Compounds NWBS00-088 EPI-0011 NWB STUDY TITLE: Quantitative Determination of PFOS and Related Compounds in Human Serum by LC/MS/MS The clinical study described in this report is not included within the definition of a GLP regulated nonclinical study. However, Northwest Bioanalyticat conducts all studies within the guidelines of the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58), the OECD Principles of Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety of Drugs (Ordinance No. 21, PAB Notification No. 424.) The following inspections were performed by the NWB QAU per SOP. Inspection and Reporting Statement. Date of Inspection Phase of Study Date Report Sent to N'WB Project Manager Date Report Sent to NWB Management* 22-25 Sep 2000 16 Oct 2000 07-13 Nov 2000 20-25 Oct 2001 27 Nov 2001 03 Dec 2001 Sample Receipt Analytical Plan Sample Analysis Report Draft/Raw Data 2'_ Report Draft/Raw Data Final Report 25 Sep 2000 16 Oct 2000 14 Nov 2000 25 Oct 200 l 27 Nov 2001 03 Dec 2001 29 Sep 2000 31 Oct 2000 30 Nov 2000 31 Oct 2001 30 Nov 2001 31 Dec 200l *Reports to NWB Management are issued monthly. As can reasonably be established, the methods and procedures described incorporated into this final report accurately reflect the raw data. 4L,-JJ.. S_cy Lynn Chain, B.A.- Date NWB Quality Assurance Compliance Auditor and the results Page 2 Northwest Bioanalytical COMPLIANCE STATEMENT Study No. NWBS00-088 Report No. NWBR01-001 The clinical study described in this report is not included within the definition ofa GLP regulated nonclinical study. However, to the best ofour knowledge, this project was conducted in accordance with the guidelines of the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58) and according to the methods and procedures described within this report. In addition, the study followed the guidelines of the OECD Principles of Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety of Drugs (Ordinance No. 21, PAB Notification No. 424.) Any known incidents that may have affected the quality or integrity of the project or reported data is included in this report. This report represents an accurate record of the raw data. Connie O. Sakashita, B.S. Date NWB Project Manager R z, P Date NWB Technical Director Page 3 NorthwestBioanalytical TABLE OF CONTENTS StudyNo. NWBSO0-088 Report No. NWBR01-001 SIGNATURE PAGE ....................................................................................................................... I QUALITY ASSURANCE STATEMENT ...................................................................................... 2 COMPLIANCE STATEMENT ....................................................................................................... 3 TABLE OF CONTENTS ................................................................................................................. 4 LIST OF TABLES ........................................................................................................................... 4 LIST OF FIGURES. ........................... i............................................................................................ 5 1. INTRODUCTION .............................................. . .................................................................... 8 2. METHODOLOGY .................................................................................................................. 9 3. SAMPLE ANALYSIS ........................................................................................................... 12 4. RESULTS AND DISCUSSION ............................................................................................ 13 5. REFERENCES ...................................................................................................................... 17 6. DATA RETENTION ............................................................................................................. 17 LIST OF TABLES Table 1. Calibration Curve Summary for PFOS ........................................................................... 18 Table 2. Calibration Curve Summary for PFOA .......................................................................... 19 Table 3. Calibration Curve Summary for PFHS ........................................................................... 20 Table 4. Calibration Curve Summary for PFOSAA. ..................................................................... 21 Table 5. Calibration Curve Summary for PFOSA .......................... .............................................. 22 Table 6. Calibration Curve Summary for M556 ........................................................................... 23 Table 7. Calibration Curve Summary for M570 ........................................................................... 24 Table 8. Back-Calculated Concentrations of Calibration Standards for PFOS ............................ 25 Page4 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 9. Back-Calculated Concentrations of Calibration Standards tbr PFOA ............................ 27 Table 10. Back-Calculated Concentrations of Calibration Standards for PFHS ............ :............. 29 Table I 1. Back-Calculated Concentrations of Calibration Standards for PFOSA.A ..................... 31 Table 12. Back-Calculated Concentrations of Calibration Standards for PFOSA ....................... 33 Table 13. Back-Calculated Concentrations of Calibration Standards for M556 .......................... 35 Table 14. Back-Calculated Concentrations of Calibration Standards for M570 .......................... 37 Table 15. Analytical QC Summary for PFOS .............................................................................. 39 Table 16. Analytical QC Summary for PFOA .............................................................................. 41 Table 17. Analytical QC Summary for PFHS .............................................................................. 43 Table 18. Analytical QC Summary for PFOSA.A ......................................................................... 45 Table 19. Analytical QC Summary for PFOSA ............................................................................ 47 Table 20. Analytical QC Summary for M556 ..... i........................................................................ 49 Table 21. Analytical QC Summary for M570 .............................................................................. 51 Table 22. Study Sample Concentrations ....................................................................................... 53 Table 23. Repeat Analysis Table for PFOS .................................................................. ................ 92 Table 24. Repeat Analysis Table for PFI--IS.................................................................................. 92 LIST OF FIGURES Figure 1. Representative Calibration Curve for PFOS ................................................................. 93 Figure 2. Representative Calibration Curve for PFOA ................................................................. 93 Figure 3. Representative Calibration Curve for PFHS ................................................................. 94 Figure 4. Representative Calibration Curve for PFOSA.A ............................................................ 94 Figure 5. Representative Calibration Curve for PFOSA .............................................................. 95 Figure 6. Representative Calibration Curve for M556 ................................................................. 95 Page 5 NorthwestBioanalytical StudyNo. NWBS00-088 Report No. NWBR01-00l Figure 7. Represerttative Calibration Curve tbr M570 ............... .................................. i............... 96 Figure 8. Human Serum Btank for PFOS ....................................................................... .............. 97 Figure 9. Human Serum Blank for PFOA .................................................................................... 98 Figure 10. Human Serum Blank for PFHS ................................................................................... 99 Figure 11. Human Serum Blank for PFOSAA ........................................................................... 100 Figure 12. Human Serum Blank for PFOSA .............................................................................. 101 Figure 13. Human Serum Blank for M556 ................................................................................. 102 Figure 14. Human Serum Blank for M570 ................................................................................. 103 Figure 15. Human Serum Blank with Internal Standard (QC0) for PFOS .................................. 104 Figure 16. Human Serum Blank with Internal Standard (QC0) for PFOA ................................. 105 Figure 17. Human Serum Blank with Internal Standard (QC0) for PFHS ................................. 106 Figure 18. Human Serum Blank with Internal Standard (QC0) for PFOSA.A ........................... 107 Figure 19. Human Serum Blank with Internal Standard (QC0) for PFOSA .............................. 108 Figure 20. Human Serum Blank with Internal Standard (QC0) for M556 ................................. 109 Figure 21. Human Serum Blank with Internal Standard (QC0) for M570 ................................. 110 Figure 22. Low Standard (3.94 ppb) for PFOS ........................................................................... 111 Figure 23. Low Standard (1.92 ppb) for PFOA .......................................................................... 112 Figure 24. Low Standard (1.36 ppb) for PFHS ........................................................................... 113 Figure 25. Low Standard (1.60 ppb) for PFOSA.A ..................................................................... 114 Figure 26. Low Standard (1.00 ppb) for PFOSA ........................................................................ 115 Figure 27. Low Standard (2.50 ppb) for M556 ........................................................................... 116 Figure 28. Low Standard (1.00 ppb) for M570 ........................................................................... 117 Figure 29. High Standard (414 ppb) for PFOS ........................................................................... 118 Page6 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-00 t Figure 30. High Standard (48l ppb) for PFOA .......................................................................... 1 t9 Figure 31. High Standard (523 ppb) for PFHS ................................................................ '........... t20 Figure 32. High Standard (501 ppb) for PFOSA.A ..................................................................... 121 Figure 33. High Standard (500 ppb) for PFOSA ........................................................................ 122 Figure 34. High Standard (500 ppb) for M556 .................................................................... . ...... 123 Figure 35. High Standard (500 ppb) for M570 ........................................................................... 124 Page 7 NorthwestBioanalytical Study No.NWBS00-088 Report No. NWBI_01-001 Quantitative Determination of PFOS and Related in Human Serum by LC/MS/MS Compounds Sample Analysis Report for Protocol EPI-0011 1. INTRODUCTION This report summarizes the analytical results from the quantitation of PFOS, PFOA, PFHS, PFOSAA, PFOSA, M556, and M570 in human serum samples for 3M Company in support of Protocol EPI-0011 [5.1]. The LC/MS/MS method for the analytes exhibited a quadratic response for 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 testing facility was 3M Company (Corporate Occupational Medicine, Medical Department, 220-3W-05, St. Paul, MN 55144), and the Study Director was Jeffrey H. Mandel, M.D., M.P.H. James K. Lundberg served as 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 Newman, B.S. (NWB Research Scientist); Emily Yardimci, B.S. (NWB 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. Page8 NorthwestBioanalytical StudyNo. NWBS00-088 Report No.NWBR01-001 Date Study Initiated: 22-Sep-2000 Date Analyses Completed: 25-Mar-2001 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 NWBR00108 [5.2] and NW'BR00-122 [5.3]. Chinese human plasma was used for the calibration curves and quality control samples. Serum sample results obtained using plasma curves are discussed in NWBR00-122. Samples for this study were received at NWB on the following dates: Receipt Date 21-Sep-2000 22-Sep-2000 21-Feb-2001 Number of Samples Received 526 73 62 Storage Condition (except during analysis) -20 C -20 C -20 C Page9 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Reference Material Analyte PFOS PFOA PFHS PFOSA.A PFOSA M556 M570 THPFOS Lot Number Purity Expiration Date 193 100% 3 l-Dec-2010 245 SE-036 100% 100% 31-Dec-2010 01-Jan-2010 617 53.8% 31-Dec-2010 214 100% 31-Dec-2010 NBl13047-SD 99.89% 31-Dec-2010 118506-26 59909 99.75% 90% 31-Dec-2010 31-Dec-2010 Source 3M 3M 3M 3M 3M 3M 3M 3M Storage Conditions Room temperature* Room temperature* -20"C Room temperature Room temperature Room temperature Room temperatttre Room temperature *Stored dry The reference material purity for PFOS, PFOSA, PFHS, and PFOA was not available prior to the conduct of this study. Therefore, the referencematerial 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 Eight or more calibration standards were prepared on the day of each run by adding 100 I-tLof blank human Chinese plasma and 400 I-tLof 50 mM ammonium acetate in Page 10 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-00I water (unadjusted pH -6.9) to 13 x 100 mm polypropylene tubes. After a brief vortex mixing, 10.0 I.tL of the appropriate spiking solution was added.The final calibration standard concentrations in human Chinese 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 414 ppb 1.92, 3.36, 10.6, 25.0, 49.0, 97.1, 24l, 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 1.00, 2.50, 10.0, 25.0, 50.0, 100, 250, 400, and 500 ppb * The target calibration curve range is 1.00 ppb to 500 ppb (except for M556 which has a LLOQ of 2.50 ppb). Each analyte has a different final curve range based upon the persistent levels of the analyte in the human Chinese plasma used. In addition, blank plasma samples, both with and without internal standard (desig-nated as QC0s and Blanks, respectively), were assayed in each analytical run. Analytical QCs were prepared in human Chinese plasma on October 6, 2000, October 11, 2000, and October 27, 2000"and stored in a -20 C freezer. For each run, analytical QC levels were assayed in duplicate. In addition, for each dilution level, dilution QCs were run in triplicate in any analytical run that contained diluted subject samples. The QC concentration levels are shown in the following table. Analyte PFOS PFOA PFHS PFOSAA PFOSA M556 M570 QC Concentrations All concentrations are expressed as ppb. Low Medium High High, DF = 2 6.40 126 332 335 4.81 145 385 386 4.48 156 417 418 4.60 151 401 401 4.00 150 400 400 4.00 150 400 400 4.00 150 400 400 Page 11 Northwest Bioanalytieal Study No. NWBS00-088 Report No. NWBR0!-001 The internal standard (THPFOS) was added to all plasma and 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 a PE Sciex 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 PE Sciex MacQuan software (version 1.6) with a smooth factor of one. Quantitation was based upon quadratic regression analysis of weighted (1/x 2) calibration curves using area ratio vs. concentration utilizing Watson DMLIMS software (version 6.1.1.04). The samples were injected in a systematic order. 3.1. Acceptance Criteria For an analytical run to be accepted, it must have met the acceptance criteria listed below which are consistent with regulatory and industry recommendations. Calibration Curve ,,_k,. 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 Page 12 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-00 ! standard's back-calculated concentrations must be within + 20% (+ 25% for LLOQ) of their individual target concentrations. A calibration standard will be considered an outlier if it is greater than two times the acceptance criteria tbr 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 PFOSA.A 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 cart 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 Page 13 Bioanalytical Study No. NWBSO0-088 Report No. NWBR01-00 [ calibration curves. However, in order to obtain the lower limit ofquantitation required by the Sponsor, it was necessary to use plasma curves. less than 5 Each accepted run met the acceptance criteria set for the calibration curve points, for the lower limit ofquantitation (LLOQ) and for the analytical quality control (QC) samples. Run ID I PFOS Result Rejected 2 Accepted 3 Accepted 4 Accepted 5 Accepted 6 Accepted 7 Accepted 8 Accepted 9 Accepted 10 Accepted 11 Accepted 12 Accepted 13 Accepted 14 Accepted 15 N/A 16 N/A 17 Accepted PFOA Result Rejected PFHS Result Rejected PFOSAA Result Rejected Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Rejected N/A N/A N/A N/A Accepted N/A Accepted Accepted Accepted N/A = not analyzed Comments All analytes rejected due to sample preparation error LLOQ raised for PFOS Low QCs failed for PFOSAA. Run ID 1 2 3 4 5 PFOSA Result Rejected Accepted Accepted Accepted Accepted M556 Result Rejected Accepted Accepted Accepted Accepted M570 Result Rejected Accepted Accepted Accepted Accepted Comments All analytes rejected due to sample preparation error Page 14 Northwest Bioanalytical Run ID 6 7 8 9 10 lt PFOSA Result Accepted Accepted Accepted Accepted Accepted Rejected 12 Accepted 13 Accepted 14 Accepted 15 Rejected 16 N/A 17 Accepted Study No. NWBS00-088 Report No. NWBR0i-001 M556 Result M570 Result Comments Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted N/A N/A Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Rejected N/A Accepted Accepted Standard curve tailed t'or PFOSA. Reinjection of Run 11 for PFOSAA only. Low QCs failed for M570 Standard curve failed for PFOSA N/A = not analyzed Because of the limited sample volume available, several samples in this study were l: analyzed at a dilution factor of 2. High QC samples, diluted at a factor of 2, were also analyzed in triplicate. METH00040 did not meet the validation acceptance criteria for analysis of QC samples containing PFOSA or PFOSAA at concentrations above the ULOQ (analyzed after dilution). Samples containing PFOSA or PFOSA.A at concentrations less than the ULOQ and analyzed after diluting with control matrix were not evaluated for accuracy and precision during method validation. PFOSA and PFOSAA accuracy and precision for the diluted high QC samples from 3 separate runs was determined to assess the validity of diluting samples with Chinese plasma when samples have PFOSA or PFOSAA concentrations less than the ULOQ. (Refer to PFOSA.A results in Runs 12, 13, and 16 and PFOSA results in Runs 12, 13, and l 4.) Both intra- and inter-assay precision were <15% and intra- and inter-assay accuracy deviated <15% from target (data not shown). Therefore, the accuracy and precision _ obtained after diluting samples with Chinese plasma when samples have PFOSA or Page 15 NorthwestBioanalytical Study No.NWBS00-088 ReportNo. NWBR01-001 PFOSAA concentrations less than the ULOQ is acceptable and PFOSA and PFOSAA results frorn diluted samples will be reported. The lack of dilution data prior to analysis of diluted of high QC samples did not affect the quality of the assay or integrity of the PFOSA and PFOSAA datal Sample 230 was analyzed on Run 1 which had to be rejected for all analytes due to sample preparation error. There is insufficient sample for reanalysis. SOP Deviations Samples 2193 to 2363 and 2366 to 2500 were analyzed for PFOSA in Run 11 and Run 15. The standard curves did not meet the acceptance criteria in either run and therefore, PFOSA results were rejected. There was insufficient sample to reanalyze. Since the runs failed, no standard or QC data from the runs is included in this report. All subject PFOSA sample results obtained in Runs 11 and 15 were less than the LLOQ. The standard curve failed due to scatter and less than three-fourths of the standards were within the acceptance criteria. However, the mean of the low QC results in the two runs ranged from 109.8 to 114.3% of target and the LLOQ samples for run 15 deviated less than w+ 5% of target. Since there is insufficient sample volume to repeat the analyses, the client has requested that the <LLOQ results be reported as conditional information. The criteria specified in the analytical plan for rejection of calibration standards was not followed for the M570 curve in run 12. Standard 1, replicate 1 was deactivated as an outlier even though the % deviation from target was less than 2 times the acceptance criteria for that standard prior to deactivation. As a general practice, both LLOQs are deactivated if both LLOQ results are outside of the specified acceptance criteria. For this run, when both LLOQs were deactivated, the calculated concentration of Std I, replicate 1, deviated 61% from target and replicate 2 was 1l% from target. This indicated that Std I, repl 1 was a true outlier and Std 1, repl 2 was originally not fitting the curve because Std I, repl 1 was skewing the curve. When Page 16 NorthwestBioanalytical StudyNo. NWBS00-088 R.cportNo. NWBR01-001 Std 1, repl 2 is reactivated, it has a deviation of 2% from target. Therefore, the regression will be accepted with only Std 1, repl I deactivated as an outlier. Since the regression is scientifically sound and acceptance criteria for the run are met, this deviation does not effect the quality of the data or integrity of the study. 5. REFERENCES 5. I. 3M Company Protocol EP[-0011. "Identification of Fluorochemicals in Sera of Children in the United States." March 16, 2000. 5.2. C. Sakashita. "Quantitative Determination ofPFOS, 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. NWB Report NWBR00-122. November 20, 2001. 6. DATA RETENTION The raw data and final report for this study will be stored in the NWB Archives, 1121 East 3900 South, Salt Lake City, UT 84124 per regulations and contract agreement. After submission of the final report to the Sponsor, remaining study samples will be stored under required conditions until 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 17 NurthwestBioanalytical Study No.NWBS00-088 ReportNo. NWBR01-001 Table 1. Calibration Curve Summary Mr PFOS Quadratieweightedl/x:. All concentrationsare expressedas ppb. Run Date Run A Number B C R-Squared LLOQ ULOQ 31-Oct-2000 2 -0.000005 0.027791 0.010909 0.9956 3.94 414 01-Nov-2000 3 -0.000005 0.027419 0.006602 0.9990 3.94 414 04-Nov-2000 4 -0.000007 0.030558 0.012087 0.996i 3.94 414 06-Nov-2000 5 -0.000017 0.038499 0.015935 0.9953 3.94 414 08-Nov-2000 6 -0.000011 0.035306 0.007489 0.9960 3.94 414 09-Nov-2000 7 -0.000010 0.039703 0.010533 0.9894 3.94 414 10-Nov-2000 8 -0.000008 0.035218 0.033595 0.9921 3.94 414 12-Nov-2000 9 -0.000003 0.020611 0.020473 0.9912 3.94 414 13-Nov-2000 10 -0.000007 0.029955 0.022348 0.9918 3.94 414 14-Nov-2000 11 0.000005 0.026248 0.022175 0.9791 3.94 414 15-Nov-2000 12 -0.000005 0.041499 0.007161 0.9829 5.17 414 ( 16-Nov-2000 13 -0.000003 0.036442 0.026638 0.9820 3.94 414 18-Nov-2000 14 -0.000006 0.034381 0.024135 0.9970 3.94 414 25-Mar-2001 17 -0.000001 0.008025 0.004145 0.9969 3.94 414 Mean S.D. %CV n -0.000006 0.000005 -83.3 14 0.030833 0.008779 28.5 14 0.016016 0.008935 55.8 14 0.9917 0.0063 0.6 14 A, B, and C an coe_cien_ usedto define thecalibrationcurve. Page 18 Northwest Biounalytical Study No. NWBS00-088 Report No. NWB R01-001 Table 2. Calibration Curve Summary for PFOA Quadratic weighted l/x". All concentrations are expressed as ppb. Run Date 31-Oct-2000 0t-Nov-2000 04-Nov-2000 06-Nov-2000 08-Nov-2000 09-Nov-2000 lO-Nov-2000 12-Nov-2000 13-Nov-2000 14-Nov-2000 15-Nov-2000 16-Nov-2000 18-Nov-2000 25-Mar-2001 Run Number 2 3 4 5 6 7 8 9 10 11 12 13 14 17 A B C R-Squared LLOQ ULOQ 0.000001 0.000002 0.000001 0.000000 -0.000001 -0.000002 0.000001 0.000001 0.000001 0.000008 0.000002 -0.000001 0.000000 0.000000 0.018750 0.018998 0.014032 0.014340 0.014866 0.014932 0.015103 0.010333 0.015660 0.013586 0.015457 0.017638 0.020492 0.006597 0.001244 0.000186 0.001606 0.002050 0.000095 0.002985 0.009536 0.003017 0.002794 0.006940 0.005125 0.007935 0.010441 0.002091 0.9967 0.9980 0.9945 0.9941 0.9971 0.9961 0.9941 0.9961 0.9936 0.9842 0.9903 0.9922 0.9921 0.9921 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 1.92 481 1.92 481 1.92 481 1.92 481 Mean S.D. %CV n 0.000001 0.000002 200.0 14 0.015056 0.003547 23.6 14 0.004003 0.003414 85.3 14 0.9937 0.0035 0.4 14 A, B, and C are coefficients used to define the calibration curve. Page 19 NorthwestBioanalytical StudyNo. NWBS00-088 ReportNo. NWBR01-001 Table 3. Calibration Curve Summary Mr PFHS Quadraticweightedl/x2. Allconcentrationsareexpressedas ppb. Run Date 31-Oct-2000 01-Nov-2000 04-Nov-2000 06-Nov-2000 08-Nov-2000 09-Nov-2000 lO-Nov-2000 12-Nov-2000 13-Nov-2000 14-Nov-2000 15-Nov-2000 16-Nov-2000 18-Nov-2000 25-Mar-2001 Run Number 2 3 4 5 6 7 8 9 10 11 12 13 14 17 A B C R-Squared LLOQ ULOQ -0.000009 -0.000010 -0.000008 -0.000015 -0.000015 -0.000011 -0.000008 -0.000006 -0.000008 -0.000006 -0.000008 -0.000007 -0.000008 -0.000002 0.031737 0.032478 0.031233 0.034135 0.035218 0.030154 0.028971 0.020349 0.030472 0.032776 0.030669 0.028744 0.032203 0.007658 0.006465 0.009418 0.014139 0.015590 0.009051 0.011565 0.027667 0.010603 0.025208 0.025491 0.025839 0.027330 0.024941 0.007909 0.9976 0.9979 0.9965 0.9952 0.9964 0.9977 0.9946 0.9983 0.9979 0.9964 0.9887 0.9930 0.9922 0.9937 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 1.36 523 1.36 523 1.36 523 1.36 523 Mean S.D. %CV n -0.000009 0.000003 -33.3 14 0.029057 0.007075 24.3 14 0.017230 0.008299 48.2 14 0.9954 0.0028 0.3 14 A, B, and C are coefficien_usedto definethe calibrationculwe. Page 20 Northwest Bioanalytica! Study No. NWBS00-088 Report No. NWBR01-00I Table 4. Calibration Curve Summary for PFOSAA Quadratic weighted l/x". All concentrations are expressed as ppb. Run Date 31-Oct-2000 01-Nov-2000 04-Nov-2000 06-Nov-2000 08-Nov-2000 09-Nov-2000 10-Nov-2000 12-Nov-2000 13-Nov-2000 14-Nov-2000 15-Nov-2000 16-Nov-2000 20-Nov-2000 25-Mar-2001 Run Number 2 3 4 5 6 7 8 9 10 11 12 13 16 17 A B C R-Squared LLOQ ULOQ -0.000001 0.023946 -0.003099 0.9952 1.60 501 0.000002 0.022379 0.004347 0.9940 1.60 501 0.000000 0.016980 0.005491 0.9840 1.60 501 0.000000 0.016621 0.003312 0.9827 1.60 501 0.000000 0.018859 0.003795 0.9939 1.60 501 0.000002 0.014599 0.003438 0.9901 1.60 501 0.000004 0.017031 0.025660 0.9812 1.60 501 0.000001 0.011371 0.000468 0.9982 1.60 501 0.000004 0.019123 0.007920 0.9937 1.60 501 0.000016 0.014974 0.016220 0.9802 1.60 501 0.000004 0.012533 0.009564 0.9810 1.60 501 0.000004 0.014478 0.010593 0.9859 1.60 501 0.000003 0.020670 0.021239 0.9927 1.60 501 0.000001 0.005029 0.010607 0.9928 1.60 501 Mean S.D. %CV n 0.000003 0.000004 133.3 14 0.016328 0.004833 29.6 14 0.008540 0.007974 93.4 14 0.9890 0.0062 0.6 14 A, B, and C are coefficients used to define the cal_ration cu_e. Page 21 NurthwestBioanatyticat Study No.NWBS00-088 ReportNo. NWBR01-001 Table 5. Calibration Curve Summary for PFOSA Quadraticweightedl/x2. All concentrationsare expressedas ppb. Run Date 3l-Oct-2000 01-Nov-2000 04-Nov-2000 06-Nov-2000 08-Nov-2000 09-Nov-2000 10-Nov-2000 12-Nov-2000 13-Nov-2000 15-Nov-2000 16-Nov-2000 18-Nov-2000 25-Mar-2001 Run Number 2 3 4 5 6 7 8 9 l0 12 13 14 17 A B C R-Squared LLOQ ULOQ -0.000013 -0.000003 -0.000012 -0.000018 -0.000015 -0.000013 -0.000011 -0.000007 -0.000005 -0.000009 -0.000007 -0.000010 0.000000 0.052859 0.046250 0.054175 0.069706 0.060806 0.072938 0.067435 0.036838 0.051854 0.077880 0.069240 0.064050 0.015780 0.003517 0.010476 0.011593 0.019030 0.009414 0.011198 0.045288 0.013009 0.018661 0.003529 0.029141 0.019102 0.005386 0.9949 0.9961 0.9918 0.9964 0.9958 0.9921 0.9914 0.9930 0.9911 0.9855 0.9812 0.9945 0.9945 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 1.00 500 1.00 500 1.00 500 Mean S.D. %CV n -0.000009 0.000005 -55.6 13 0.056909 0.016948 29.8 13 0.015334 0.011547 75.3 13 0.9922 0.0044 0.4 13 A, B, and C are coe_cients usedto definethe calibrationcurve_ Page22 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-00 l Table 6. Calibration Curve Summary Mr M556 Quadratic weighted l/x:. All concentrations are expressed _ ppb. Run Date Run A B C R-Squared LLOQ ULOQ Number 31-0ct-2000 2 -0.000001 0.018373 0.001923 0.9972 2.50 500 01-Nov-2000 3 0.000002 0.017583 0.005331 0.9972 2.50 500 04-Nov-2000 4 0.000002 0.007944 0.003887 0.9903 2.50 500 06-Nov-2000 5 0.000001 0.007717 0.004452 0.9822 2.50 500 08-Nov-2000 6 0.000002 0.009283 0.002596 0.9949 2.50 500 09-Nov-2000 7 0.000002 0.007610 0.002860 0.9985 2.50 500 10-Nov-2000 8 0.000002 0.008464 0.004466 0.9975 2.50 500 12-Nov-2000 9 0.000002 0.006106 0.003591 0.9968 2.50 500 13-Nov-2000 10 0.000003 0.008526 0.004733 0.9962 2.50 500 14-Nov-2000 11 0.000007 0.007051 0.006423 0.9867 2.50 500 15-Nov-2000 12 0.000003 0.006747 0.003029 0.9911 2.50 500 i 16-Nov-2000 13 0.000002 0.006485 0.002510 0.9936 2.50 500 18-Nov-2000 14 0.000002 0.008566 0.004178 0.9942 2.50 500 25-Mar-2001 17 0.000001 0.002650 0.001081 0.9955 2.50 500 Mean S.D. %CV n 0.000002 0.000002 100.0 14 0.008793 0.004209 47.9 14 0.003647 0.001423 39.0 14 0.9937 0.0047 0.5 14 A, B, and C arc coefficients used to define the calibration cu_e. Page 23 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 7. Calibration Curve Summary Mr M570 Quadratic weighted l/x:. All concentrations are expressed as ppb. Run Date 31-Oct-2000 01-Nov-2000 04-Nov-2000 06-Nov-2000 08-Nov-2000 09-Nov-2000 10-Nov-2000 12-Nov-2000 13-Nov-2000 14-Nov-2000 15-Nov-2000 16-Nov-2000 20-Nov-2000 25-Mar-2001 Run Number 2 3 4 5 6 7 8 9 10 11 12 13 16 17 A B C R-Squared LLOQ ULOQ -0.000006 -0.000001 -0.000002 -0.000002 0.000000 0.000001 0.000002 -0.000002 0.000002 0.000020 0.000003 0.000006 0.000000 0.000000 0.038561 0.036248 0.027976 0.026862 0.030532 0.024223 0.028172 0.018677 0.030589 0.025065 0.021180 0.022590 0.033466 0.002606 0.012040 0.019154 0.012726 0.016535 0.016991 0.014409 0.063424 0.009480 0.027413 0.030430 0.014447 0.034515 0.044312 0.003896 0.9924 0.9952 0.9860 0.9908 0.9961 0.9863 0.9950 0.9951 0.9938 0.9807 0.9847 0.9802 0.9914 0.9929 1.00 500 _.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 1.00 500 1.00 500 1.00 500 Mean S.D. %CV n 0.000002 0.000006 300.0 14 0.026196 0.008809 33.6 14 0.022841 0.015953 69.8 14 0.9900 0.0055 0.6 t4 A, B, and C are coefficients used to define the calibration cu_e. Page 24 Norttlwest Bioartaiytical Study No. NWBS00-088 Report No. NWBR01-00 l Table 8. Back-Calculated Concentrations of Calibration Standards Quadratic weighted l/x2. All concentrations are expressed as ppb. for PFOS Run Date 31-Oct-2000 Run Number 2 01-Nov-2000 3 04-Nov-2000 4 06-Nov-2000 5 08-Nov-2000 6 09-Nov-2000 7 10-Nov-2000 8 12-Nov-2000 9 13-Nov-2000 10 14-Nov-2000 11 15-Nov-2000 12 16-Nov-2000 13 3.94 5.17 1.1.3 23.6 44.2 85.4 209 332 414 3.65 5.67 12.0 23.4 45.0 84.2 224 347 424 4.10 4.90 10.7 23.3 42.3 84.5 203 345 368 4.00 5.15 11.4 23.7 46.7 84.5 198 329 422 3.94 5.04 l 1.4 23.9 43.4 83.6 207 351 405 4.16 5.31 10.5 21.2 44.9 83.7 205 340 411 3.70 5.05 12.6 24.1 45.7 86.9 213 332 409 3.97 5.37 12.4 25.7 45.3 82.8 203 352 428 3.83 4.96 10.7 23.2 43.5 77.3 *116 * 399 3.96 5.74 11.1 25.6 44.5 87.0 215 350 436 3.69 5.02 11.3 22.8 42.9 81.8 193 333 386 4.26 5.56 12.2 26.7 46.7 89.3 227 357 433 3.56 4.85 10.3 22.2 40.9 77.1 184 338 376 4.57 4.83 11.9 24.8 47.0 86.6 212 *7.53 4.35 I1.0 22.5 41.1 87.8 207 353 418 325 390 3.67 5.25 12.0 25.1 49.0 89.1 220 339 443 4.53 4.57 10.2 23.0 42.0 79.6 195 321 392 3.84 6.11 12.3 24.2 45.l 85.5 222 344 401 3.76 4.53 11.3 24.0 40.4 75.9 208 332 413 4.56 5.74 11.8 26.3 50.7 90.5 **95.5 354 401 3.26 4.83 9.79 21.9 **28.5 64.6 210 354 391 "['4.93 5.81 10.8 25.9 47.0 96.6 245 374 456 "['3.23 4.86 I0.1 20.9 43.6 77.6 184 294 354 3.31 4.34 10.3 22.6 43.8 75.1 201 313 391 4.83 5.52 12.0 26.2 50.4 79.5 233 330 452 Sample deactivated due to preparation error * Sample deactivated as an outlier I"LLOQ failed Page 25 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-00I "Fable 8. Back-Calculated Concentrations of Calibration Standards for PFOS (Continued) Quadratic weighted l/x-'. All concentrations are expressed as ppb. Run Date 18-Nov-2000 Run Number I4 25-Mar-2001 17 3.94 5.17 11.3 23.6 44.2 85.4 209 332 414 3.88 5.45 11.0 23.1 44.6 83.3 206 357 388 4.03 4.71 12.3 24.2 42.4 85.9 208 333 422 3.98 4.71 11.1 25.5 44.7 81.6 211 344 423 4.26 4.93 11.4 24.0 44.7 82.6 202 344 390 Mean S.D. %CV %Bias n 3.97 0.383 9.6 0.8 25 5.11 11.3 23.9 44.8 83.0 0.461 0.784 1.55 2.63 6.03 9.0 6.9 6.5 5.9 7.3 -1.2 0.0 1.3 1.4 -2.8 28 28 28 27 28 209 340 408 13.9 16.0 24.6 6.7 4.7 6.0 0.0 2.4 -1.4 26 27 28 Page 26 Northwest Bioanatytical Table 9. Back-Calculated Concentrations of Calibration Study N_ NWBS00-088 Report No. NWI3ROI-OOI Standards for PFOA Quadratic weighted I/xz. All concentrations are expressed as ppb. Run Date iRun Number 1.92 3.36 10.6 25.0 49.0 97.1 241 385 481 31-Oct-2000 0l-Nov-2000 04-Nov-2000 06-Nov-2000 08-Nov-2000 09-Nov-2000 I0-Nov-2000 12-Nov-2000 13-Nov-2000 14-Nov-2000 15-Nov-2000 16-Nov-2000 2 1.94 3.49 9.80 24.9 47.2 89.3 250 383 470 1.88 3.36 10.7 26.6 49.5 99.2 247 427 443 3 1.85 3.30 10.0 24.0 51.6 98.9 227 38l 472 1.94 3.64 10.5 25.7 48.7 95.3 249 406 478 4 2.05 3.27 9.53 21.4 49.2 90.5 245 385 456 1.80 3.49 11.0 27.9 51.0 102 253 398 478 5 1.89 3.14 10.6 25.0 47.0 84.0 234 374 482 1.92 3.63 10.5 27.3 55.5 92.8 "164 * 509 6 2.03 3.22 9.85 27.5 49.6 97.8 253 382 48 l 1.98 3.03 10.3 25.1 50.8 95.0 237 387 471 7 2.17 3.06 10.4 25.8 49.2 92.7 244 394 501 1.77 3.34 10.8 25.6 50.2 95.0 243 399 437 8 2.17 2.75 9.73 26.1 49.5 95.4 238 386 484 "6.15 3.22 11.2 24.5 50.9 103 255 378 467 9 2.02 3.53 11.0 23.9 51.0 94.5 235 365 477 *3.54 2.92 10.0 24.3 52.3 99.6 251 416 467 10 2.22 3.19 10.8 26.1 52.2 93.0 249 412 463 1.77 2.97 10.6 27.2 47.1 87.0 242 386 473 11 2.30 3.92 10.6 27.2 53.6 96.8 **57.3 381 445 1.59 2.72 9.75 24.0 *'15.4 83.8 258 418 482 12 2.28 3.16 9.24 25.1 49.5 90.5 233 339 494 1.70 3.22 10.7 25.3 56.9 102 246 415 480 13 1.82 3.28 t 0.4 27.0 51.3 96.7 233 372 466 2.22 2.81 10.3 26.0 52.9 86.4 253 369 523 Sample deactivated due to preparation error , ** Sample deactivated as an outlier Page 27 Northwest Bioanalytical Study No, NWBS00-088 Report No. NWBR01-001 Table 9. Back-Calculated Concentrations of Calibration Standards for PFOA (Continued) Quadratic weighted l/x:. All concentrations are expressed as ppb. Run Date 18-Nov-2000 Run Number 14 25-Mar-200t 17 1.92 3.36 10.6 25.0 49.0 97.1 241 385 481 1.77 3.29 9.90 25. I 48.7 96.5 243 404 441 2.20 2.90 12.5 25.6 46.1 93.9 248 398 486 1.85 2.67 10.4 27.l 49.4 95.5 234 395 474 2.26 3.15 10.9 25.9 50.4 94.2 241 416 455 Mean S.D. %CV %Bias n 1.98 3.20 10.4 25.6 50.4 0.199 0.298 0.634 1.40 2.47 10.1 9.3 6.1 5.5 4.9 3.1 -4.8 -1.9 2.4 2.9 26 28 28 28 27 94.3 244 5.07 8.09 5.4 3.3 -2.9 1.2 28 26 391 473 19.6 19.7 5.0 4.2 1.6 -1.7 27 28 Page 28 Northwest Bioaua[ytical Table 10. Back-Calculated Concentrations Study No. NWBS00-088 Report No. NWBR01-001 of Calibration Standards for PFHS Run Date Quadratic weighted L/x". AI[ concentrations are expressed as ppb. Run Number 1.36 2.92 10.7 26.5 52.6 104 262 418 523 31-Oct-2000 2 0t-Nov-2000 3 04-Nov-2000 4 06-Nov-2000 ., 5 .. 1.30 3.01 11.2 26.0 49.7 98.7 268 1.42 2.77 11.2 27.4 52.0 102 266 1.36 2.73 11.2 25.8 5I.I m ,. 1.35 3.12 10.6 27. l 55.7 104 238 100 268 1.43 3.08 9.86 28.5 51.2 96.4 247 1.31 2.67 10.7 28.7 53.1 106 271 1.40 2.86 11.0 26.6 51.5 87.1 252 , .... 1.36 2.72 11.5 28.8 55.5 102 "167 4t9 530 455 478 417 513 442 532 432 513 424 524 431 515 * 554 08-N..o..v..-.2000 09-Nov-2000 10-Nov-2000 12-Nov-2000 I .... 13-Nov-2000 14-Nov-2000.] 15-Nov-2000 [6-Nov-2000 6 11..4244 23..8156 1110..41 2285..37 5523..48 9160.13 226407 442350 554176 7 1.44 2.80 11.2 26.8 51.9 101 256 409 518 1.26 3.05 11.0 26.4 52.3 101 251 468 [515 r 8 1.51 2.37 10.9 26.4 53.1 103 250 413 537 *5.46 2.69 II.I 28.1 54.0 107 272 413 515 9 1.35 2.88 10.6 25.4 51.4 96.8 256 391 529 *3.07 2.97 10.9 28.3 55.3 103 270 439 530 10 1.35 2.85 11.1 26.4 52.5 102 262 432 520 1.41 2.73 11.3 27.9 48.8 99.6 273 434 492 11 1.45 2.61 I0.7 27.4 50.4 104 *'79.3, 416 488 1.32 2.95 10.8 28.0 **23.7 101 269 469 503 m, 12 1.55 2.74 11.4 29.4 55.4 120 276 475 56l 1.30 2.47 10.2 25.4 51.9 91.9 237 370 482 13 1.23 2.66 11.2 27.3 55.1 104 270 407 521 1.59 2.64 10.8 27.3 56.3 89.6 255 420 542 Sample deactivated due to preparation error * Sample deactivated as art outlier Page 29 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 10. Back-Calculated Concentrations of Calibration Standards (Continued) Quadratic weighted l/x2. All concentrations are expressed as ppb. for PFHS Run Date 18-Nov-2000 Run Number 14 25-Mar-2001 17 1.36 2.92 10.7 26.5 52.6 104 262 418 523 1.26 2.98 10.l 26.3 53.8 97.8 264 428 534 1.48 2.6 l 13.3 26.6 50.3 99.7 253 407 534 1.39 2.46 10.4 28.0 55.4 103 277 440 521 1.52 2.52 I0.6 27.5 55.3 103 258 427 474 Mean S.D. %CV %Bias n 1.39 2.78 10.9 27.2 52.9 101 260 427 519 0.0963 0.208 0.631 1.09 2.07 5.94 11.2 22.9 21.7 6.9 7.5 5.8 4.0 3.9 5.9 4.3 5.4 4.2 2.2 -4.8 1.9 2.6 0.6 -2.9 -0.8 2.2 -0.8 26 28 28 28 27 28 26 27 28 Page 30 Northwest BioanalyticaI Study No. NWBS00-088 Report No. NWBR01-001 Table 1I. Back-Calculated Concentrations of Calibration Standards for PFOSAA Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date Run Number 1.60 3.10 10.6 25.6 50.6 101 251 401 501 31-Oct-2000 01-Nov-2000 04-Nov-2000 06-Nov-2000 08-Nov-2000 09-Nov-2000 10-Nov-2000 12-Nov-2000 13-Nov-2000 14-Nov-2000 15-Nov-2000 16-Nov-2000 20-Nov-2000 2 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 3 1.66 2.85 9.40 25.l 55.4 97.5 248 375 495 1.54 3.50 9.99 26.9 48.8 107 261 443 481 4 1.58 3.53 8.37 19.1 50.2 94.5 243 392 461 1.56 3.00 12.0 28.9 54.9 107 285 429 496 5 1.24 2.77 10.1 23.3 45.8 95.8 242 379 494 1.94 3.56 10.4 27.7 55.2 115 "186 * 532 6 1.52 2.88 8.73 26.6 47.4 96.4 257 432 501 1.72 3.23 11.7 26.7 51.7 106 255 392 468 7 1.46 2.84 9.64 24.8 45.8 90.1 260 389 449 1.71 3.48 11.5 27.8 53.0 102 253 472 495 8 1.98 2.13 9.82 25.8 54.7 98.0 253 403 463 *8.58 2.70 10.6 24.6 50.3 122 289 396 489 9 1.6l 3.09 10.1 24.6 50.3 99.6 250 376 487 *2.67 3.15 10.2 27.0 51.5 104 269 420 504 10 1.59 3.22 11.1 24.2 50.2 98.0 275 402 424 1.60 2.96 11.2 26.3 44.9 99.5 264 403 549 11 1.54 3.40 9.75 28.5 59.2 105 *'138 391 445 1.53 3.39 9.65 26.4 37.1 82.5 284 447 507 12 1.85 2.88 7.98 22.3 44.4 99.5 270 364 465 1.40 3.33 10.9 25.3 62.0 I13 284 437 483 13 1.72 2.88 11.9 28.4 56.9 93.4 282 419 502 *5.99 2.81. 9.59 25.7 48.4 80.6 281 336 506 16 1.52 3.14 9.31 23.8 47.1 98.1 253 413 447 1.72 2.88 12.4 27.4 48.8 107 267 407 520 Sample deactivated due to preparation error * Sample deactivated as an outlier Page 31 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 11. Back-Calculated Concentrations of Calibration Standards for PFOSAA (Continued) Quadratic weighted l/x:. All concentrations are expressed as ppb. Run Date 25-Mar-2001 Run Number 17 1.60 3.10 10.6 25.6 50.6 101 251 401 501 1.67 2.93 10.8 29.8 52.5 103 255 420 500 1.71 2.54 10.5 24.2 49.1 94.5 249 429 456 Mean S.D. %CV %Bias n 1.62 0.164 10.1 1.3 25 3.06 10.3 25.7 50.4 100 264 407 485 0.333 1.08 2.24 5.03 8.84 14.0 29.0 27.9 10.9 10.5 8.7 10.0 8.8 5.3 7.1 5.8 -1.3 -2.8 0.4 -0.4 -1.0 5.2 28 28 28 28 28 26 1.5 -3.2 27 28 Page 32 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 12. Back-Calculated Concentrations of Calibration Standards Quadratic weighted l/x'-. All concentrations are expressed as ppb. for PFOSA Run Date Run Number 1.00 2.50 10.0 25.0 50.0 100 250 400 500 3I-Oct-2000 01-Nov-2000 04-Nov-2000 06-Nov-2000 08-Nov-2000 09-Nov-2000 10-Nov-2000 12-Nov-2000 13-Nov-2000 15-Nov-2000 16-Nov-2000 18-Nov-2000 2 0.930 2.62 9.96 25.7 52.8 101 289 438 529 1.06 2.48 9.45 24.1 47.2 I00 229 362 453 3 0.913 2.40 8.86 25.1 52.l 99.1 238 380 497 1.10 2.56 9.78 26.7 50.4 104 255 432 491 4 1.00 2.64 9.23 19.1 51.8 101 248 386 494 0.998 2.33 11.5 26.1 53.7 105 24l 399 525 5 0.934 2.63 10.I 26.9 48.7 104 248 395 521 1.03 2.60 9.67 25.7 48.4 86.1 "138 * 499 6 0.992 2.63 8.92 28.0 49.4 104 261 413 545 0.985 2.57 9.69 26.0 46.9 97.0 235 368 482 7 1.04 2.71 10.4 28.9 50.5 105 271 444 521 0.945 2.38 8.88 24.5 47.2 91.4 215 394 461 8 1.12 2.15 10.7 27.9 52.5 103 259 424 522 "1.67 2.04 10.I 23.6 47.1 105 252 366 467 9 0.979 2.58 11.4 25.8 56.6 107 251 422 541 1.00 2.53 9.14 22.1 45.8 91.7 232 385 473 10 1.12 2.81 10.8 26.6 53.1 98.2 258 426 477 0.850 2.32 9.74 25.9 43.7 85.7 245 390 521 12 *'1.61 3.03 8.79 26.1 50.1 114 294 416 544 0.921 2.62 8.99 21.3 52.4 91.2 232 388 422 13 0.788 2.06 8.94 24.4 47.6 86.3 234 385 479 1.22 2.85 10.8 29.0 54.2 95.7 286 382 547 14 0.965 2.39 I0.0 24.9 47.2 102 240 466 438 1.04 2.59 10.2 27.5 45.2 95.6 276 392 495 ,.,I Sample deactivated due to preparation error * Sample deactivated as an outlier Page 33 Northwest Bit)analytical Study No. NWBS00-088 Report No. NWBR01-001 Table 12. Back-Calculated Concentrations of Calibration Standards (Continued) Quadratic weighted l/xz. All concentrations are expressed as ppb. for PFOSA Run Date Run Number 1.00 2.50 10.0 25.0 50.0 100 250 400 500 25-Mar-2001 17 0.900 2.36 10.3 28.0 48.3 101 236 410 505 1.14 2.30 10.3 25.8 48.4 95.1 241 432 479 Mean S.D. %CV %Bias n 0.999 2.51 9.87 25.6 49.7 98.8 25l 404 497 0.0978 0.232 0.781 2.28 3.14 7.01 20.0 26.7 33.7 9.8 9.2 7.9 8.9 6.3 7.1 8.0 6.6 6.8 -0.1 0.4 -1.3 2.4 -0.6 -1.2 0.4 1.0 -0.6 24 26 26 26 26 26 25 25 26 Page 34 Northwest Bioanalytical Table 13. Back-Calculated Concentrations of Calibration Study No. NWBS00-088 Report No. NWBR01-001 Standards for [_1556 Run Date Quadratic weighted l/x_'. All concentrations are expressed as ppb. Run Number 2.50 10.0 25.0 50.0 100 250 400 500 31-Oct-2000 2 0 l-Nov-2000 3 04-Nov-2000 4 06-Nov-2000 5 08-Nov-2000 6 09-Nov-2000 7 10-Nov-2000 8 12-Nov-2000 9 13-Nov-2000 10 14-Nov-2000 11 IS-Nov-2000 16-Nov-2000 12 m,, 13 18-Nov-2000 14 2.33 9.67 24.3 51.9 2.70 9.81 25.8 49.3 2.55 9.86 25.9 55.5 2.48 9.52 23.6 47.4 2.38 8.49 19.4 53.2 2.63 11.8 26.4 52.2 2.02 8.91 22.7 46.0 2.98 10.7 28.8 58.2 2.28 8.40 26.1 46.3 2.75 11.0 25.7 51.4 2.51 9.73 25.7 49.3 2.50 9.91 25.5 51.8 2.37 9.94 23.7 47.6 2.63 10.3 24.0 50.9 2.61 9.22 23.4 50.6 2.43 9.95 26.7 51.0 2.52 10.3 25.5 52.3 2.43 10.4 26.0 46.8 2.77 9.58 27.2 57.3 2.33 8.48 24.2 *'33.4 2.46 8.06 22.9 46.3 , ,, 2.66 10.1 23.9 57.7 ,, 2.70 10.0 27.2 53.3 2.32 9.10 25.3 52.2 2.69 9.91 23.3 48.0 2.25 11.4 26.6 48. I 95.2 255 104 249 107 246 96.2 241 96.1 248 104 263 86.0 235 107 *200 98.1 255 102 250 95.5 253 100 238 97.9 244 109 271 97.8 233 107 264 96.5 261 88.5 248 103 *'127 81.4 272 105 276 104 260 92.8 _ 255 87.3 271 96.4 242 .)7.0 256 388 499 438 470 403 505 421 478 388 485 416 500 385 49,2 * 538 413 494 409 481 400 488 432 490 402 487 394 500 376 499 421 502 429 458 403 516 392 453 439 505 388 483 42"7 464 m 414 499 359 513 434 454 420 503 _'Sample deactivated due to preparation error * Sample deactivated as an outlier Page 35 Northwest Bioanatytical Study No. NWBS00-088 Report No. NWBR0 t-001 Table 13. Back-Calculated Concentrations of Calibration Standards for M556 (Continued) Quadratic weighted t/x". All concentrations are expressed as ppb. Run Date Run Number 2.50 10.0 25.0 50.0 100 250 400 500 25-Mar-200 t 17 2.71 10.1 27.4 51.0 99.1 247 420 507 2.26 10.4 23.7 47.9 94.0 240 431 460 Mean S.D. %CV %Bias n 2.51 9.82 25.0 50.9 98.1 253 409 490 0.205 0.872 1.90 3.49 6.83 11.9 20.5 20.2 8.2 8.9 7.6 6.9 7.0 4.7 5.0 4. I 0.4 -1.8 0.0 28 28 28 1.8 -1.9 1.2 2.3 -2.0 27 28 26 27 28 Page 36 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR0|-00 [ Table 14. Back-Calculated Concentrations of Calibration Standards for M570 " Quadratic weighted l/x 2. All concentrations are expressed as ppb. Run Date Run Number 1.00 2.50 10.0 25.0 50.0 100 250 400 500 31-Oct-2000 0l-Nov-2000 04-Nov-2000 06-Nov-2000 08-Nov-2000 09-Nov-2000 10-Nov-2000 12-Nov-2000 13-Nov-2000 14-Nov-2000 15-Nov-2000 16-Nov-2000 20-Nov-2000 2 0_828 2.29 10.I 23.6 48.1 93.7 262 392 486 1.18 2.66 9.94 25.9 50.6 109 252 431 475 3 1.07 2.22 9.01 25.2 54.1 100 239 383 485 0.992 2.43 9.48 27.2 50.1 106 259 441 482 4 0.974 2.74 8.15 18.7 49.4 96.4 239 389 466 1.02 2.29 11.8 28.0 55.0 105 269 427 506 5 0.930 2.09 9.52 23.9 44.9 97.3 234 384 486 1.10 2.75 10.3 26.6 56.0 110 "183 * 538 6 0.952 2.50 8.31 25.8 49.0 I00 251 404 496 1.08 2.35 10.6 25.7 51.9 107 249 404 488 7 0.805 2.08 9.40 24.8 45.9 94.4 247 392 452 1.23 2.66 10.6 27.0 53.8 105 246 463 499 8 1.01 **0.653 9.16 24.3 52.0 98.0 240 403 468 "6.51 *'1.29 9.43 23.5 50.3 118 276 402 498 9 0.964 2.40 9.29 23.1 48.8 96.7 235 375 482 "1.93 2.89 9.84 25.7 53.4 105 264 432 510 10 1.05 2.33 10.7 24.0 50.3 100 258 407 437 1.03 2.13 10.9 27.1 45.7 98.2 258 401 543 11 1.I0 2.78 9.29 26.7 57.0 104 *'133 399 440 0.813 2.87 9.1l 25.9 37.9 81.5 276 444 508 12 *'1.53 2.39 7.28 22.l 45.2 101 259 369 457 1.02 2.62 i0.3 25.2 62.8 112 269 439 495 13 1.16 1.93 10.8 28.4 57.9 I00 276 422 497 1.03 1.83 9.[9 26.1 52.0 83.4 275 340 495 16 0.933 2.6l 9.04 24.! 46.9 96.9 241 423 449 1.10 2.13 12.0 26.t 48.4 107 260 404 523 Sample deactivated due to preparation error * Sample deactivated as an outlier Page 37 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 14. Back-Calculated Concentrations of Calibration Standards for M570 Quadratic weighted l/x:. All concentrationsare expressed as ppb. (Continued) Run Date Run Number 1.00 2.50 25-Mar-2001 17 1.03 1.98 1.05 *'1.64 I0.0 25.0 50.0 100 250 9.84 29.0 52.3 102 252 10.0 24.8 50.4 90.5 241 400 500 424 508 419 458 Mean S.D. %CV: %Bias n 1.02 0.106 10.4 2.0 25 2.40 0.304 12.7 -4.0 25 9.76 25.3 50.7 101 255 408 487 1.03 I'2.09 4.84 7.92 13.4 26.4 26.9 10.6 8.3 9.5 7.8 5.3 6.5 5.5 -2.4 1.2 1.4 1,0 2.0 2.0 -2.6 28 28 28 28 26 27 28 Page 38 NorthwestBioanalytical StudyNo. NW13S00-088 ReportNo. NWBR01-00l Table 15. Analytical QC Summary for PFOS All concentrationsare expressedas ppb. Run Date Run Number 3 l-Oct-2000 2 01-Nov-2000 3 04-Nov-2000 4 06-Nov-2000 5 08-Nov-2000 6 09-Nov-2000 7 ..... i 10-Nov-2000 8 .,, 12-Nov-2000 9 13-Nov-2000 10 14-Nov-2000 11 15-Nov-2000 12 Low QC 6.40 ppb 6.62 6.18 6.79 7.16 6.57 6.63 6.03 5.30 6.70 5.98 6.00 5.96 6.36 6.38 6.18 6.31 6.71 6.38 5.31 6.73 6.50 5.84 Medium QC 126 ppb 129 1.35 125 124 131 130 105 122 147 128 137 108 136 134 132 127 139 136 136 133 14l 1.03 High QC 332 ppb 323 322 369 354 314 322 291 283 343 320 302 293 323 318 299 304 327 312 322 294 319 330 Dilution QC 335 ppb DF=2 320 323 350 Page39 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR0 [-00 l Table 15. Analytical QC Summary for PFOS (Continued) All concentrations are expressed as ppb. Run Date Run Number 16-Nov-2000 l3 18-Nov-2000 14 25-Mar-2001 17 m, Low QC 6.40 ppb 6.65 5.98 5.87 6.06 6.26 5.95 Medium QC 126 ppb 126 129 130 126 137 135 High QC 332 ppb 297 319 338 336 367 349 Dilution QC 335 ppb DF=2 307 312 359 335 342 345 335 338 471 Mean .., S.D. %CV %Theoretical %Bias n 6.26 129 321 345 0.430 10.1 22.1 42.6 6.9 7.8 6.9 12.3 97.8 102.4 96.7 103.0 -2.2 2.4 -3.3 3.0 28 28 28 12 Page 40 NorthwestBioanalytical Study No.NWBS00-088 Report No. NWBR01-001 Table 16. Analytical QC Summary for PFOA All concentrationsareexpressedas ppb. Run Date Run Number 31-Oct-2000 2 0l-Nov-2000 3 04-Nov-2000 4 06-Nov-2000 5 08-Nov-2000 6 09-Nov-2000 7 10-Nov-2000 8 12-Nov-2000 9 13-Nov-2000 10 14-Nov-2000 11 15-Nov-2000 12 16-Nov-2000 13 Low QC 4.81 ppb 4.87 4.90 4.78 4.68 5.51 5.09 4.45 5.10 4.81 4.18 4.22 4.15 4.23 4.66 4.72 5.45 5.05 4.80 4.19 4.67 4.09 4.50 4.43 4.65 lVledium QC 145 ppb t56 147 144 144 149 159 140 147 154 159 147 130 154 160 151 150 159 158 153 155 158 127 143 160 High QC 385 ppb 399 380 396 408 384 383 342 368 423 388 369 356 375 385 382 353 391 353 371 371 419 422 420 421 Dilution QC 386 ppb DF=2 396 425 406 388 391 402 Page41 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 16. Analytical QC Summary for PFOA (Continued) All concentrations are expressed as ppb. Run Date Run Number 18-Nov-2000 14 25-Mar-2001 17 LowQC 4.81 ppb 3.92 3.90 4.28 4.06 Medium QC 145 ppb 147 151 163 159 High QC 385ppb 386 394 412 422 Dilution QC 386ppb DF=2 392 416 381 404 401 449 Mean S.D. %CV %Theoretical %Bias n 4.58 0.432 9.4 95.2 -4.8 28 151 8.80 5.8 104.1 4.1 28 388 23.6 6. I 100.8 0.8 28 404 18.6 4.6 104.7 4.7 12 Page 42 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-00I Table 17. Analytical QC Summary ibr PFHS All concentrations are expressed as ppb. Run Date Run Number 31-Oct-2000 2 01-Nov-2000 3 04-Nov-2000 4 06-Nov-2000 5 08-Nov-2000 6 09-Nov-2000 7 10-Nov-2000 8 12-Nov-2000 9 13-Nov-2000 10 14-Nov-2000 11 15-Nov-2000 12 16-Nov-2000 13 LowQC 4.48 ppb 4.35 4.60 4.34 4.44 4.37 4.40 4.10 4.14 3.99 3.89 4.09 4.67 3.76 4.00 3.99 4.57 4.32 4.15 4.08 3.80 4.06 3.84 3.63 4.12 Medium QC 156 ppb 160 151 144 146 163 160 144 150 157 157 154 134 162 158 154 166 171 158 167 155 164 150 146 167 High QC 417 ppb 403 400 420 432 404 409 364 386 404 413 371 397 408 404 391 410 404 435 385 396 373 400 401 396 Dilution QC 418 ppb DF=2 367 365 378 418 43l 401 Page 43 NorthwestBioanaiytical StudyNo. NWBS00-088 R.eportNo. NWBR01-001 Table 17. Analytical QC Summary for PFHS (Continued) Allconcentrationsare expressedas ppb. Run Date Run Number 18-Nov-2000 14 25-Mar-2001 17 Low QC IMedium QC 4.48 ppb 156 ppb 3.74 155 3.85 148 3.85 153 3.72 153 High QC 417 ppb 454 397 448 427 Dilution QC 418 ppb DF=2 39l 401 414 .. 390 403 449 Mean S.D. %CV %Theoretical %Bias n 4.10 155 405 401 0.287 8.40 21.0 25.0 7.0 5.4 5.2 6.2 91.5 99.4 97.1 95.9 -8.5 -0.6 -2.9 -4. t 28 28 28 12 Page44 NorthwestBiuanatytical Study No. NWBS00-088 ReportNo. NWBR01-00l Table 18. Analytical QC Summary lbr PFOSAA Allconcentrationsare expressedas ppb. Run Date Run Number Low QC 4.60 ppb Medium QC 151 ppb High QC 401 ppb Dilution QC 401 ppb DF=2 31-Oct-2000 2 4.43 160 393 4.03 157 394 01-Nov-2000 3 *5.84 150 485 5.21 172 488 04-Nov-2000 4 4.26 151 391 4.10 162 388 06-Nov-2000 5 3.77 136 366 4.18 138 356 08-Nov-2000 6 5.22 176 443 4.35 I57 434 09-Nov-2000 7 3.50 ,m, 3.93 153 359 128 409 10-Nov-2000 8 4.23 163 415 4155 181 430 12-Nov-2000 9 4.15 153 380 , 5.55 172. 389 13-Nov-2000 10 5.24 151 415 5.06 172 323 14-Nov-2000 11 3.71 168 399 4.52 150 371 15-Nov-2000 12 *3.39 158 451 4t9 3.70 116 427 491 422 [6-Nov-2000 13 4.10 137 419 401 4.15 157 412 399 424 *>e 25%deviationfromtheoretical Page45 t Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-00 I Table 18. Analytical QC Summary for PFOSAA (Continued) All concentrations are expressed as ppb. Run Date Run Number 20-Nov-2000 16 25-Mar-2001 17 Low QC 4.60 ppb 3.81 *3.24 4.86 3.72 Medium QC 151 ppb High QC 401 ppb 164 361 155 472 173 429 173 420 Dilution QC 401 ppb DF=2 411 414 397 426 422 *634 Mean S.D. %CV %Theoretical %]3ias n 4.31 0.667 15.5 93.7 -6.3 28 157 15.3 9.7 104.0 4.0 28 I 408 39.4 9.7 101.7 1.7 28 * >-a:25% deviation from theoretical 438 66.3 15.1 109.2 9.2 12 Page 46 Northwest 13ioatxalytical Study No. NWBS00-088 Report No. NWBR0 [-001 Table 19. Analytical QC Summary for PFOSA All concentrations are expressed as ppb. Run Date Run Number 31 -Oct-2000 2 01-Nov-2000 3 04-Nov-2000 4 06-Nov-2000 5 08-Nov-2000 6 09-Nov-2000 7 10-Nov-2000 8 12-Nov-2000 9 13-Nov-2000 10 l 5-Nov-2000 12 16-Nov-2000 13 Low QC 4.00 ppb 3.74 4.10 4.72 *5.03 4.16 4.04 3.66 3.49 4.75 4.15 4.05 3.70 4.38 4.58 4.65 4.20 4.76 4.74 4.27 3.88 4.54 3.72 Medium QC 150 ppb 154 158 151 161 147 158 127 155 183 145 164 126 166 164 163 153 172 172 171 *111 150 149 High QC 400 ppb 423 412 488 471 401 433 357 342 462 423 371 350 419 412 363 363 422 357 432 443 369 391 Dilution QC 400 ppb DF=2 421 455 475 350 360 453 * _ 25% deviation from theoretical Page 47 NorthwestBioanalytical Study No. NWBS00-088 ReportNo. NWBR01-001 Table 19. Analytical QC Summary for PFOSA (Continued) Allconcentrationsare expressedasppb. Run Date Run Numberl 18-Nov-2000 14 25-Mar-2001 17 Low QC 4.00 ppb 4.28 4.23 4.50 4.07 Medium QC 150 ppb 156 147 180 180 High QC 400 ppb 385 417 450 444 Dilution QC 400 ppb DF=2 428 423 397 437 438 *552 Mean S.D. %CV %Theoretical %Bias n 4.24 0.399 9.4 106.0 6.0 26 156 16.6 10.6 104.0 4.0 26 407 39.4 9.7 I 01.8 1.8 26 * >-_25%deviationfromtheoretical 430 51.3 11.9 107.5 7.5 I 12 Page48 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-00 I 'Table 20. Analytical QC Summary for M556 All concentrations are expressed as ppb. Run Date Run Number 31-Oct-2000 2 0l-Nov-2000 3 04-Nov-2000 4 06-Nov-2000 5 08-Nov-2000 6 09-Nov-2000 7 10-Nov-2000 8 12-Nov-2000 9 13-Nov-2000 10 14-Nov-2000 11 15-Nov-2000 12 16-Nov-2000 13 Low QC 4.00 ppb Medium QC 150 ppb 3.95 3.93 "4.81 4.62 4.08 3.70 3.57 3.30 4.74 3.63 3.63 4.11 4.25 4.18 3.56 4.00 4.49 4.29 3.36 4.51 "3.14 3.56 16l 149 163 171 156 163 141 146 172 160 155 132 161 "182 158 176 164 175 163 157 156 * 112 3.98 139 3.81 154 High QC 400 ppb 417 406 449 *492 397 393 373 383 444 431 367 398 417 423 384 404 421 357 394 384 427 420 416 407 Dilution QC 400 ppb DF=2 402 464 416 397 385 427 >-a2: 0% deviation from theoretical Page 49 NorthwestBioanalytical Study No. NWBSO0-088 ReportNo. NWBROt-O0I Table 20. Analytical QC Summary for lV1556(Continued) Allconcentrationsare expressedas ppb. Run Date Run Number 18-Nov-2000 14 25-Mar-2001 17 LowQC 4.00 ppb Medium QC 150 ppb 3.87 150 3.69 157 4.09 168 3.52 162 High QC 400 ppb 382 424 455 434 Dilution QC 400 ppb DF=2 416 419 406 403 392 *627 Mean S.D. %CV %Theoretical %Bias i1 3.94 0.437 11.1 98.5 -1.5 157 14.3 9.1 104.7 4.7 411 29.3 7.1 102.8 2.8 430 65.5 15.2 107.5 7.5 28 28 28 I 12 * _ 20%deviationfromtheoretical Page50 NorthwestBioanalytical Study No.NWBS00-088 ReportNo. NWBR01-001 Table 21. Analytical QC Summary _r M570 Allconcen_ationsare expressedas ppb. Run Date Run Numberl 31-Oct-2000 2 01-Nov-2000 3 04-Nov-2000 4 06-Nov-2000 5 08-Nov-2000 6 09-Nov-2000 7 10-Nov-2000 8 12-Nov-2000 9 13-Nov-2000 10 14-Nov-2000 11 15-Nov-2000 12 16-Nov-2000 13 Low QC 4.00ppb 3.70 3.99 4.52 5.13 3.68 4.06 "3.10 3.60 4.48 3.85 "3.13 3.51 *2.97 3.37 3.94 4.30 4.12 4.85 3.43 4.32 3.29 3.64 3.25 3.65 Medium QC 150ppb 164 160 152 178 147 165 133 146 *182 161 154 131 165 "184 154 173 158 176 166 154 155 "114 14l 161 High QC 400ppb 410 416 476 "491 400 385 362 379 446 422 364 409 421 427 384 397 420 326 408 383 452 429 423 415 Dilution QC 400ppb DF=2 414 *490 424 413 399 435 >-J:20%deviationffomtheoreticaI Page51 Northwest Bioanalytical Study No. NWBS00-088 Repo,'t No. NWBROL-001 Table 21. Analytical QC Summary for M570 (Continued) All concentrations are expressed as ppb. Run Date Run Number 20-Nov-2000 16 25-Mar-2001 17 Low QC 4.00 ppb *2.76 3.33 3.20 *2.89 Mediu.m QC 150 ppb 169 151 165 159 High QC 400 ppb 372 *484 461 4l i Dilution QC 400 ppb D'F=2 415 421 391 383 400 *648 Mean S.D. %CV %Theoretical %Bias n 3.72 0.596 16.0 93.0 -7.0 28 158 15.6 9.9 105.3 5.3 28 413 38.1 9.2 103.3 .d 3.3 28 * >-a:20% deviation from theoretical 436 72.1 16.5 109.0 9.0 12 Page 52 Northwest Bioanalytical Study No. NV_rBS00-088 Report No. NWBR01-001 Table 22. Study Sample Concentrations All concentrations are expressed as ppb. Sample No. 0021 0056 0087 0104 0109 0122 0123 0126 0127 0128 0131 0133 0136 0149 0151 0167 0174 PFOS Concentration 11.1 27.1 18.1 67.3 19.4 36.8 29.0 39.6 42.8 81.2 68.0 65.2 83.8 .... 39.3 29.8 77.6 36.1 PFOA Concentration* 2.13 5.79 3.95 6.14 2.65 3.35 3.37 3.77 <LLOQ(2.88) 5.60 4.68 6.91 8.65 I .... 2.94 5.00 7.70 3.85 PFHS Concentration* <LLOQ(1.36) 3.72 1.99 3.82 6.12 4.28 <LLOQ(I.36) 10.4 <LLOQ(2.41) 21.2 28.1 21.6 180 25.7 11.0 1.81 7.09 PFOSA_A Concentration* <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 4.54 3.03 <LLOQ(1.60) <LLOQ(2.60) 5.50 5.45 2.11 <LLOQ(1.60) 2.33 3.11 6.32 4.06 PFOSA Concentration* <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(2.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 2.7. 4.62 <LLOQ(2.50) <LLOQ(5.00) 7.33 6.1 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) lV1570 Concentration* <LLOQ(I.00) <LLOQ(1.00) 5.15 3.28 6.55 <LLOQ(I.00) 2.37 1.74 <LLOQ(2.00) 4.81 1.53 <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 1.91 Serum sample results obtained using plasma curves may vary fiom results obtained fi'om serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been con'ected for the persistent level of analyte ill the dilution matrix. The method acceptance criteria states the concentration for each QC must be within :1:20%(+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 53 Northwest Bioanalytical Study No. NW'BS00-088 Report No. NWBR01-001 Table 22. Study Sample Concentrations (Continued) All concentl'ations are expressed as ppb. Sample No. 0187 0192 0193 0194 0196 0197 0198 0199 0210 0216 0217 0228 0229 0230 0231 PFOS Concentration PFOA Concentration* PFHS Concentration* PFOSAA Concentration* 31.1 3.56 <LLOQ(1.36) 3.69 35.7 6.93 6.05 6.66 90.2 6.41 71.3 3.14 24.5 4.44 1.41 <LLOQ(1.60) 11.6 1.95 <LLOQ(I.36) 1.64 38.9 5.46 <LLOQ(1.36) 4.95 71.9 7.43 <LLOQ(1.36) 4.12 54.8 7.37 30.0 <LLOQ(2.60) 33.9 5.44 4.14 4.76 38.2 4.79 3.12 2.42 43.6 5.16 6.86 5.34 16.6 3.89 6.83 <LLOQ(1.60) 122 10.4 145 4.93 No result No result No result ](Insufficient sample (Insufficient sample i(Insufficient sample volume) volume) volume) No result (Insufficient sample volume) 93.9 7.8 17.8 6.07 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) No result (Insufficient sample volume) <LLOQ(1.00) M556 Concentration* <LLOQ(2.50) <LLOQ(2.50) 3.58 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 5.94 <LLOQ(5.00) 7.16 <LLOQ(2.50) 5.59 <LLOQ(2.50) 4.35 No result (Insufficient sample volume) 8.55 M570 Concentration* 2.04 <LLOQ(1.00) <LLOQ(I.O0) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) 7.26 2.42 5.03 <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(I.00) No result (Insufficient sample volume) 23 Serum sample results obtained using plasma curves may vary from results obtained fi'om serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 54 Northwest Bioanalytical Study No. NWBS00-088 Reporf No. NW-BR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0247 0250 0251 0259 0269 0270 0290 0296 0308 0315 0329 0341 0342 0344 0356 0358 0365 PFOS Concentration 42.4 37.7 51.3 38.3 92.3 25.7 28.7 23.3 23.7 94.2 29.6 53.0 38.3 31.1 45.8 30.0 26.8 _ PFOA Concentration* 2.92 6.11 4.32 5.07 8.71 5.09 4.08 4.28 3.56 4.74 2.66 4.89 5.88 3.26 7.85 .4.32 <LLOQ(2.88) PFHS Concentration* 11.4 2.51 16.1 11.3 75.4 <LLOQ(I.36) 3.23 <LLOQ(1.36) <LLOQ(1.36) 11.2 4.60 2.33 <LLOQ(I.36) <LLOQ(2.41) 1.50 2.27 <LLOQ(2.41) PFOSAA Concentration* 3.19 <LLOQ(I.60) 3.11 2.04 15.3 4.54 <LLOQ(I.60) 2.62 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 6.61 1.98 <LLOQ(2.60) 4.37 3.53 <LLOQ(2.60) PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(2.00) <LLOQ( 1.00) <LLOQ(I.00) <LLOQ(2.00) M556 Concentration* 2.88 <LLOQ(2.50) 4.94 5.88 8.4 4.42 <LLOQ(2.50) <LLOQ(2.50) 3.54 <LLOQ(2.50) 3.21 3.77 , <LLOQ(2.50) <LLOQ(5.00) 9.71 <LLOQ(2.50) <LLOQ(5.00) M570 Concentration* 1.06 2.67 3.11 <LLOQ(I.00) 5.16 1 2.53 <LLOQ(1.00) 1.36 2.15 2 2.59 1.28 <LLOQ(2.00) 26.6 1.3 <LLOQ(2.00) Senlm sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected nm (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC nmst be within +20% (+_25% for PFOSA and PFOSA.A) of the target concentration. The statistical elTor of any individual result may exceed the QC acceptance criteria. Page 55 Northwest Bioanalytical Study No. Na,VBS00-088 Report No. N_VBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0366 0367 0370 0385 0386 0387 0388 0398 0404 0405 0407 0410 0411 0415 0420 0421 0423 PFOS Concentration 41.5 67.7 87.4 50.2 96.5 56.5 24.2 31.4 69.1 77.2 17.8 49.3 106 53.2 35.7 65.9 184 PFOA Concentration* 4.88 7.21 9.35 9.02 6.85 6.83 3.46 2.61 4.27 6.62 2.46 4.94 5.78 5.21 5.49 5.63 9.20 PFHS Concentration* <LLOQ(1.36) 4.78 37.4 7.08 74.1 35.3 1.94 4.32 49.3 24.3 <LLOQ(1.36) 2.54 33.9 41.3 2.61 2.20 89.3 PFOSAA Concentration* 3.94 4.85 7.33 1.97 3.24 3.28 2.09 3.20 5.10 4.54 3.79 8.78 8.72 4.39 3.26 9.82 6.71 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00)<LLOQ(1.00) M556 Concentration* <LLOQ(2.50) <LLOQ(2.50) 3.82 <LLOQ(2.50) 3.35 2.56 <LLOQ(2.50) <LLOQ(2.50) 2.61 3.29 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570 Concentration* 1.48 1.49 6.63 3.74 8.3 1.47 3.69 <LLOQ(1.00) 1.17 1o. 1 <LLOQ(1.00) 2.48 3.19 4.12 1.74 4.25 3.29 Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected, for the persistent level of analyte in the dilution man'ix. The method acceptance criteria state_ the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 56 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0425 0432 0456 0463 0465 0466 0470 0476 0478 0493 0495 0498 0499 0500 0521 0524 0526 PFOS Concentration 31.9 46.1 34.4 34.7 42.5 21"/.3 34.4 124 56.7 106 52.0 63.4 27.6 59.9 31.9 59.5 46.9 PFOA Concentration* i, 6.79 7.06 8.30 3.97 6.90 4.03 4.39 14.6 9.05 7.56 6.14 5.19 5.28 4.72 11.0 7.20 4.29 PFHS Concentration* 5.36 3.05 3.69 7.64 6.2t 6.75 3.21 7.36 34.8 50.5 3.11 18.1 2.98 21.2 6.52 37.5 2.07 PFOSAA Concentration* 4.17 4.62 3.01 3.61 3.28 3.56 3.54 11.3 5.59 8.83 3.50 4.17 4.52 8.94 5.31 3.44 11.2 PFOSA Concentration* <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(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) M556 Concentration* 3.21 3.82 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 2.58 <LLOQ(2.50) 9.59 3.46 9.45 <LLOQ(2.50) 3.83 2.74 5.88 <LLOQ(2.50) 3.26 8.22 M570 Concentration* 4.8 1.78 3.09 3.42 4.35 4.73 2.28 31 19.7 1.84 2.83 2.71 2.27 2 3.01 4.14 6.39 Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have boen corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical en'or of any individual result may exceed the QC acceptance criteria. Page 57 Northwest Bioanalytical Study No. N_rBs00-088 Report No. N-WBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0527 0528 0530 0531 0532 0534 0541 0542 0545 0548 0572 0578 0583 0585 0586 0587 0588 PFOS Concentration 15.4 30.3 98.1 97.9 38.1 34.6 54.0 29.5 36.9 75.7 20.4 77.6 70.1 64.8 39.5 58.2 46.0 PFOA Concentration* 2.52 5.10 8.12 6.43 6.81 4.39 6.88 5.18 8.01 9.00 3.00 7.66 5.54 6.25 5.73 7.36 5.77 PFHS Concentration* 4.78 17.0 150 72.0 11.0 5.63 1.70 .<LLOQ(1.36) 7.32 52.0 <LLOQ(1.36) 80.6 14.6 34.5 20.5 22.0 11.6 PFOSAA Concentration* 4.18 2.09 11.5 10.3 1.84 2.59 5.55 5.11 ' 2.68 3.98 8.92 4.48 12.9 4.82 1.82 9.06 3.59 PFOSA Concentration* <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.O0) <LLOQ(I.O0) <LLOQ(1.O0) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) M556 Coneentration* <LLOQ(2.50) 2.66 5.91 3.67 <LLOQ(2.50) 2.8 3.24 3.15 2.79 <LLOQ(2.50) 3.25 5.4 6.81 2.82 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570 Concentration* 3.38 4.46 1.62 1.71 1.02 1.66 5.05 4.13 3.66 2.13 1.75 1.27 5.09 4.5 3 6.77 1.7 Serum sample results obtained using plasma curves may vary fi'om results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (-1-25%for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 58 Northwest Bioanalytical t Study No. NW13S00-088 ' Report No. NWBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0589 0590 0592 0593 0598 0599 0604 0606 0607 0608 PFOS Concentration 31.0 33.4 35.1 165 25.6 77.1 18.0 37.6 48.2 52.3 PFOA Concentration* 7.57 6.37 3.15 7.94 5.40 7.44 3.54 5.71 5.72 8.01 PFHS Concentration* 3.71 8.80 1.75 129 1.91 21.8 2.85 2.84 2.55 1.82 PFOSAA Concentration* 2.84 9.81 2.99 2.40 2.56 6.25 <LLOQ(1.60) 4.69 10.3 8.98 PFOSA Concentration* <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) M556 Concentration* <LLOQ(2.50) 9.8 <LLOQ(2.50) <LLOQ(2.50) 4.05 4.42 <LLOQ(2.50) 4.11 7 3.42 M570 Concentration* <LLOQ(I.00) 4.02 2.22 <LLOQL 1.00) 4.75 5.91 1.5 7.17 2.82 3.57 0610 29.0 0611 20.3 0621 23.2 0627 72.7 0628 29.8 0629 37.6 0631 54.5 5.36 7.30 2.19 <LLOQ(1.36) 4.57 3.13 4.65 20.0 2.64 <LLOQ(I.36) 4.86 <LLOQ(1.36) 7.68 11.4 4.23 ] <LLOQ(I.00) 3.38 11.8 3.66 <LLOQ(1.00) <LLOQ(2.50) <LLOQ(1.00) 3.95 <LLOQ(1.00) <LLOQ(2.50) 2.12 5.02 <LLOQ(1.00) <LLOQ(2.50) 1.51 6.26 <LLOQ(I.00) 2.64 3.60 8.71 <LLOQ(1.00) 2.55 <LLOQ( 1.00) 6.72 <LLOQ(1.00) 4.63 <LLOQ(I.00) Serum sample results obtained using plasma curves may va_, from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC mnst be within -l-20% (+25% for PFOSA and PFOSAA) of the target concennation. The statistical error of any individual result may exceed the QC acceptance criteria. Page 59 Northwest Bioanalytical Study No. N-WBS00-088 Report No. N_VBR01-001 Table 22. Study Sample Concentrations (Continued) All concenta'ations are expressed as ppb. Sample No. 0649 0657 0658 0664 0665 0666 0667 0673 0676 0678 0679 / 0680 068 | 0689 0695 0697 0700 PFOS Concentration 28.8 27.4 19.7 55.1 31.9 16.3 57.8 34.3 25.6 50.0 30.2 44.6 31.9 40_1 28.1 27.8 17.8 PFOA Concentration* <LLOQ(2.88) 5.90 2.91 3.80 4.96 3.17 7.41 4.21 4.91 7.09 3.16 5.80 4.81 5.35 4.08 4.29 3.90 PFHS Concentration* <LLOQ(2.41) 6.25 <LLOQ(I.36) 3.80 4.68 <LLOQ( 1.36) 37.1 1.38 1.64 7.21 <LLOQ(1.36) 2.35 5.19 <LLOQ(1.36) 2.65 1.56 1.83 PFOSA.A Concentration* <LLOQ(2.60) 3.71 2.34 4.67 3.36 3.19 3.95. 8.58 4.54 11.2 5.15 9.12 4.18 3.97 5.70 3.65 <LLOQ(I.60) PFOSA Concentration* <LLOQ(2.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.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) M556 Concentration* <LLOQ(5.00) 3.25 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 3.4 <LLOQ(2.50) 3.7 <LLOQ(2.50) 4.86 <LLOQ(2.50) 2.91 3.46 <LLOQ(2.50) <LLOQ(2.50) M570 Concentration* <LLOQ(2.00) 3.78 <LLOQ(I.00) 1.26 2.14 <LLOQ( 1.00) 6.96 5.39 3.56 7.87 <LLOQ(1.00) 2.92 2.06 6.03 <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) Sert, m sample restdts obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion ). Results are fiom a rejected rtm (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution roanix. The method acceptance criteria states the concentration for each QC must be within _+20%(_+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 60 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 22. Study Sample Concentrations (Continued) Ali concentrations are expressed as ppb. Sampie No. 0711 0712 0713 0714 0719 0720 0721 0723 0725 0741 0748 0752 0753 0754 0763 0769 077 ! PFOS Concentration 8.76 19.5 32.4 23.3 34.8 42.7 37.8 32.2 26.9 33.3 22.0 16.7 37.1 33.6 35.7 19.5 8 ! .0 PFOA Concentration* 2.02 2.54 4.34 2.78 3.82 5.26 4.97 4.87 5.17 4.36 6.00 2.46 4.67 5.63 5.05 3.40 4.88 PFHS Concentration* <LLOQ(1.36) <LLOQ(1.36) <LLOQ(I.36) 1.96 1.82 4.88 8.24 9.44 1.42 1.85 5.04 <LLOQ(1.36) 1.38 <LLOQ( 1.36) 7.10 4.87 2.43 PFOSAA Concentration* 2.23 3.76 2.71 <LLOQ(1.60) 4.90 3.05 5.34 4.95 8.99 3.66 3.67 3.52 2.96 5.97 4.60 <LLOQ(1.60) 3.34 PFOSA Concentration* <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(I.00) <LLOQ( 1.00) M556 Concentration* 3.63 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 8.87 <LLOQ(2:50) 5.36 2.66 2.95 3.76 <LLOQ(2.50) <LLOQ(2.50) 5.12 <LLOQ(2.50) <LLOQ(2.50) 3.38 M570 Concentration* <LLOQ(I.00) 2.93 <LLOQ(1.00) 1.61 <LLOQ(I.00) 4.44 1.19 <LLOQ( 1.00) <LL.OQ(1.00) 2.51 1.81 1.34 5.36 <LLOQ( 1.00) 1.13 <LLOQ(1.00) 14.2 Serum sample results obtained using plasma curves may vary fi'om results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 61 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 22. Study Sample Concentrations (Continued) ': All concentrations are expressed as ppb. Sample No. 0774 0775 0779 0783 0784 0785 0788 0792 0795 0796 0798 0799 0800 0813 0814 0823 0829 PFOS Concentration 27.9 41.4 27.9 28.8 39.1 70.6 51.1 54.2 32.3 17.6 40.2 54.4 34.1 12.2 40.7 56.3 41.8 PFOA Concentration* 2.49 9.11 4.44 7.14 5.65 6.97 7.34 5.54 5.70 4.61 4.33 3.54 5.98 3.84 5.47 6.59 4.36 PFHS Concentration* 3.65 8.85 8.86 3.50 9.21 41.3 36.4 4.68 9.86 3.11 2.55 3.60 <LLOQ(1.36) 4.31 2.39 1.70 13.2 PFOSAA Concentration* 5.19 5.06 2.04 5.92 3.27 1.71 3.87 3.18 2.05 <LLOQ(1.60) 7.35 4.12 6.89 2.20 5.76 3.78 5.30 PFOSA Concentration* <LLOQ(I.00) <LLOQ( 1.00) <LLOQ(I.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(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) M556 Concentration* <LLOQ(2.50) 7.2 2.87 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 3.1 <LLOQ(2.50) 4.47 3.93 4.28 3.21 2.7 <LLOQ(2.50) 4.44 6.58 3.15 M570 Concentration* 3.25 14.3 1.3 4.58 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) 3.73 1.59 1.42 <LLOQ(I.00) 8.16 <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) 8.26 1.83 Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concenu'ation. The statistical error of any individual result may exceed the QC acceptance criteria. Page 62 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0830 0840 0841 0845 0846 0848 0849 0859 0864 0866 0867 0869 0872 0876 0880 0881 0883 PFOS Concentration 32.0 49.7 33.1 67.7 39,3 27.2 33.4 59.5 74.3 43.8 26.7 31.7 58.1 50.1 71.7 45.7 42.8 PFOA Concentration* 6.12 5.70 5.68 5.77 4,44 3.26 3.76 8.31 4.23 9.42 3.86 6.81 6.46 6.10 8.95 3.92 5.09 PFHS Concentration* 3.80 2.71 19.5 5.21 2.04 2.77 3.24 12.6 13.0 18.5 8.01 <LLOQ(1.36) 3.48 6.68 5.35 <LLOQ(1.36) 18.4 PFOSAA Concentration* 10.3 2.96 6.56 20.7 7.87 4.27 3.86 6.56 2.25 2.10 2.01 4.79 I 9.96 3.75 5.84 6.01 6.14 PFOSA Concentration* <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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) M556 Concentration* 5.92 3.55 2.82 15.5 5,82 2.91 2.75 4.46 4.02 <LLOQ(2.50) <LLOQ(2.50) 6.17 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 4.09 <LLOQ(2.50) M570 Concentration* 18.4 5.64 3.54 4.44 <LLOQ(I,00) 1.7 1.55 3.22 9. g 1 3.24 1.98 <LLOQ(I.00) 7.85 1.42 26.7 <LLOQ(1.00) 2.93 Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (:t:25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 63 Northwest Bioanalytical Study No. NWBS00-088 Report No. N_VBR01-001 Table 22. Study Sample Concentrations (Continued) All concenta'ations are expressed as ppb. Sample No. 0890 0906 0907 0909 0910 0916 0922 0928 0937 0938 0950 0953 0956 0970 0971 0986 0987 PFOS Concentration 17.3 36.3 59.4 36.8 24.4 17.6 40.7 74.6 39.3 43.9 24.8 30.3 27.5 40.4 11.4 20. ! 58.2 PFOA Concentration* 3.80 4.47 6.43 4.09 3.13 2.85 8.18 6.55 3.61 7.20 4.90 8.51 3.62 6.62 2.62 2.57 4.35 PFHS Concentration* 3.91 <LLOQ(I.36) 7.14 <LLOQ(1.36) 1.87 <LLOQ(1.36) <LLOQ( 1.36) 43.2 2.69 1.67 5.34 1.47 <LLOQ(1.36) 6.18 <LLOQ(1.36) <LLOQ(1.36) 3.94' PFOSAA Concentration* 2.69 21.7 4.84 4.41 7.23 2.11 8.51 3.86 6.95 4.06 " 5.12 5.69 2.24 9.69 <LLOQ(1.60) 2.46 16.2 PFOSA Concentration* <LLOQ(I.00) <LLOQ(1.00) <I_LOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.O0) <LLOQ( 1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ( 1.00) M556 Concentration* <LLOQ(2.50) 3.81 10.5 <LLOQ(2.50) 6.52 <LLOQ(2.50) 3.6 <LLOQ(2.50) 3.65 5.07 4.11 4.28 <LLOQ(2.50) 2.66 <LLOQ(2.50) <LLOQ(2.50) 3.42 M570 Concentration* 1 1.55 9.95 1.11 <LLOQ( 1.00) 1.08 1.7 4.28 2.91 1.54 1.31 3.79 1.8 2.95 <LLOQ(1.00) 1.51 9105 Senml sample results obtained using plasma curves may val 7 from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). Tile concentrations of any diluted samples have been corrected for the persistent level ofanalyte in the dilution matt-ix. The method acceptance criteria states the concentxation for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentaation. The statistical error of any individual result may exceed the QC acceptance criteria. Page 64 Nolahwest Bioanalytical Study No. Na,VBS00-088 Report No. N_rBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1001 1003 1005 1012 1013 1017 1019 1021 1023 1029 1030 1039 1042 1044 1048 1053 1057 PFOS Concentration 21.7 18.0 26.8 27.4 I 38.0 16.8 39.9 25.6 28.9 86.4 23.8 325 50.7 81.4 25.1 66.6 62.8 PFOA Concentration* 3.25 3.52 5.39 2.47 5.45 3.46 7.16 9.81 3.01 6.18 3.89 56.1 5.06 8.05 6.33 4.25 8.62 PFHS Concentration* <LLOQ(1.36) 2.18 <LLOQ(I.36) 1.44 3.46 <LLOQ(1.36) 2.54 5.11 <LLOQ(I.36) 74.2 <LLOQ(1.36) 416 39.6 51.9 2.94 35.7 6.40 PFOSAA Concentration* 1.64 <LLOQ(1.60) <LLOQ(I.60) 4.07 3.90 7.37 5.58 <LLOQ(1.60) 6.14 3.18 5.10 3.62 3.21 5.79 2.94 3.45 7.90 PFOSA Concentration* <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(I.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) M556 Concentration* <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 3.14 <LLOQ(2.50) <LLOQ(2.50) 2.54 <LLOQ(2.50) 2.68 4.01 <LLOQ(2.50) 4.25 <LLOQ(2.50) <LLOQ(2.50) 4.05 M570 Concentration* 2.32 <LLOQ(1.00) 4.31 <LLOQ(I.00) 2.6 2.29 7.97 3.71 3.03 2.1 1.51 7.76 3.6 1.92 4.21 2.45 17.8 Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been conected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSA.A) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 65 Northwest Bioanalytical Study No. NWBS00-088 Repot1 No. NqVBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1059 1067 1068 1070 1072 1073 1082 1085 1088 1090 1101 1104 1113 1115 1117 1121 1122 PFOS Concentration 27.9 45.1 19.5 22.4 43.2 33.6 48.2 38.2 31.3 50.9 32.8 62.6 20.2 40.4 46.5 48.7 36.5 PFOA Concentration* 4.09 5.32 3.11 3.57 6.22 2.64 4.66 3.43 6.98 5.85 2.90 5.63 3.08 5.04 3.09 5.60 5.40 PFHS Concentration* <LLOQ(1.36) 10.4 <LLOQ(1.36) 9.07 1.92 2.19 7.91 1.59 1.77 12.4 9.41 13.3 <LLOQ(1.36) 36.2 <LLOQ(1.36) 2.60 11.9 PFOSAA Concentration* 7.44 3.17 <LLOQ(1.60) 2.72 6.89 7.83 4.62 2.98 2.16 4.99 1.73 6.31 <LLOQ(1.60) 1.74 6.89 5.10 2.96 PFOSA Concentration* <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ( 1.00) <LLOQ(I.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(I.00) M556 Concentration* 5.33 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 5.99 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 2.97 5.8 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) ,4.01 <LLOQ(2.50) M570 Concentration* <LLOQ(1.00) 1.01 1.58 <LLOQ(I.00) <LLOQ(1.00) 3.69 3.6 1.83 <LLOQ(1.00) 6.28 5.83 2.25 <LLOQ(1.00) 1.4 1.91 4.77 2.5 Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected rtm (see Results and Discussioni_ The concentrations of any diluted samples have been corrected for the persistent level ofanalyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 66 Northwest Bioanalytical Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Study No. NWBS00-088 Report No. NWBR01-001 Sample No. 1124 1126 1129 1133 1136 1144 1147 1152 1153 1154 1155 1157 1166 1168 1171 1172 1173 PFOS Concentration 20.7 33.1 52.0 26.7 27.1 30.1 30.1 17.7 31.3 22.5 31.7 53.0 34.8 53.7 55.2 118 43.4 PFOA ConcentratiOn* 4.35 4.90 6.85 4.15 4.21 4.59 5.51 4.33 4.28 3.61 3.71 4.38 5.80 5.22 5.21 11.9 11.0 PFHS Concentration* 4.70 10.4 4.55 20.3 2.00 3.47 2.39 3.25 8.63 2.44 <LLOQ( 1.36) 11.5 10.5 2.86 2.57 4.07 9.77 PFOSAA Concentration* 2.13 5.66 4.24 1.79 6.23 5.01 7.87 <LLOQ(I.60) 2.27 4.08 5.29 2.51 5.60 3.61 9.22 5.94 4.22 PFOSA Concentration* <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.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(I.00) <LLOQ(1.00) M556 Concentration* <LLOQ(2.50) 2.5 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 3.29 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 4.01 <LLOQ(2.50) <LLOQ(2.50) 4.33 6.36 14.9 <LLOQ(2.50) M570 Concentration* 3.15 4.22 5.69 <LLOQ(1.00) .<LLOQ( 1.00) 1.88 2.15 1.56 <LLOQ(I.00) 2.31 1.69 3.28 <LLOQ(1.00) 12.5 17 48 6.27 Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 67 Northwest Bioanalytical Study No. 1',O,VBS00-088 Report No. NWBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as pph. Sample No. 1174 1175 I 177 1178 1179 11797 11798 11799 11800 11801 11802 11803 11804 11805 11806 11807 11808 PFOS Concentration 39.6 28.6 73.8 51.5 49.0 27.9 69.7 142 131 42.9 647 110 120 90.2 98.9 66.6 54. I PFOA Concentration* 5.35 3.95 9.51 4.87 6.85 3.37 9.74 22.1 7.13 6.52 23.3 8.61 9.03 9.64 7.51 5.74 5.57 PFHS Concentration* 17.2 <LLOQ(1.36) 14.3 1.74 18.3 8.71 58.2 268 82.9 10.4 873 80.8 181 65.5 44.7 44.3 21.8 PFOSAA Concentration* 8.52 3.23 3.66 17.0 6.21 <LLOQ(2.60) <LLOQ(2.60) 6.31 5.26 <LLOQ(2.60) 3.02 15.4 2.90 3.51 <LLOQ(2.60) <LLOQ(2.60) 3.76 PFOSA Concentration* <LLOQ( 1.00) <LLOQ(1.O0) <LLOQ( 1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) M556 Concentration* 4.4 <LLOQ(2.50) 4.76 6.17 5.77 <LLOQ(5.00) <LLOQ(5.00) 11.9 <LLOQ(5.00) <LLOQ(5.00) 13.7 6.01 <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) M570 Concentration* 1.97 1.01 13.4 3.45 7.04 <LLOQ(2.00) <LLOQ(2.00) 16.9 10.8 <LLOQ(2.00) 4.4 2.92 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) Set_m sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). Tile concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be witlfin :1:20%(+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 68 Nollhwest Bioanalytical ,_ Study No. NWBS00-088 Report No. N-_,VBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 11809 11810 11811 11812 11813 11814 11815 11816 11817 11818 11819 1182 11820 11821 11822 11823 11824 PFOS Concentration 418 21.8 90.9 199 39.7 419 47.3 88.5 81.5 143 68.9 38.1 118 26.0 52.5 28.8 52.6 PFOA Concentration* 70.0 3.56 6.70 11.4 5.69 65.6 7.47 19.5 6.05 10.2 7.35 4.26 9.34 <LLOQ(2.88) 5.09 <LLOQ(2.88) 6.65 PFHS Concentration* 484 5.99 136 109 12.5 469 8.13 _ 19.3 142 105 5.17 13.0 167 6.77 19.9 <LLOQ(2.41) <LI.OQ(2.41 ) PFOSAA Concentration* <LLOQ(2.60) <LLOQ(2.60) 7.90 2.98 2.72 <LLOQ(2.60) 10.0 6.18 5.47 <LLOQ(2.60) <LLOQ(2.60) 5.36 3.00 <LLOQ(2.60) 4.90 3.24 3.83 PFOSA Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) M556 Concentration* <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) 7.38 <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) M570 Concentration* 5.52 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 6.64 <LLOQ(2.00) 35.1 <LLOQ(2.00) <LLOQ(2.00) 10.9 2 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LI.OQ(2.00) Sermn sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are fiom a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of ally individual result may exceed the QC acceptance criteria. Page 69 Northwest Bioanalytical Study No. NWBS00-088 Report No. Na,VBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 11825 11826 11827 11828 11829 1183 11830 11831 11832 11833 11834 11835 11836 11837 11838 ! 1839 1184 PFOS Concentration 92.1 46.1 131 164 83.9 57.7 34.7 28.1 32.0 188 76.6 685 55.9 160 17.6 101 37. ! PFOA Concentration* 20.54 5.32 8.71 7.63 6.91 11.6 4.13 3.05 3.19 18.5 5.97 23.0 6.43 7.44 3.40 25.9 5.07 PFHS Concentration* 20.9 <LLOQ(2.41) 101 132 24.1 21.8 5.53 6.04 7.86 228 7.85 933 <LLOQ(2.41) 135 <LLOQ(2.41) 20.2 1.44 PFOSAA Concentration* 7.02 <LLOQ(2.60) 15.7 <LLOQ(2.60) 5.09 2.39 4.52 <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) 3.23 2.65 3.55 <LLOQ(2.60) <LLOQ(2.60) 8.27 1.70 PFOSA Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(1.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(1.00) M556 Concentration* 8.74 <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(2.50) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) 13.5 13.8 <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) 9.47 <LLOQ(2.50) M570 Concentration* 35.6 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 2.4 <LLOQ(1.00) 3.32 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 9.14 6.01 11.3 <LI_OQ(2.00) <LLOQ(2.00) 45.4 2.63 Senlm sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are fiom a rejected run (see Results and Discussion). The concentrations of any diluted samples have been con'ected for the persistent level of analyte in the dilution matrix. The naethod acceptance criteria states tl_econcentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 70 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-00 ! Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 11840 11841 11842 11843 11844 11845 11846 11847 11848 11849 i 1850 11851 11852 11853 11854 11855 11856 PFOS Concentration 42.2 127 74.8 146 29.7 i 96 88.0 14.9 162 145 613 54.1 170 431 93.1 103 20.3 PFOA Concentration* 8.99 9.54 5.40 10.8 3.47 20.2 6.77 <LLOQ(2.88) 21.9 13.6 22.5 4.76 7.44 6712 15.9 19.6 <LLOQ(2.88) PFHS Concentration* 2.56 171 <LLOQ(2.41 ) 108 <LLOQ(2.41) 235 141 <LLOQ(2.41) 274 64.0 864 12.9 135 490 10.5 20.8 <LLOQ(2.41) PFOSAA Concentration* 3.58 <LLOQ(2.60) 8.33 <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) 7.35 <LLOQ(2.60) 7.77 19.7 <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) 8.05 <LLOQ(2.60) PFOSA Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) M556 Concentration* <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) 16 15.4 13 <LLOQ(5.00 ) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) 9.46 <LLOQ(5.00) M570 Concentration* <LLOQ(2.00) <LLOQ(2.00) 2.17 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 21.9 3.76 4.31 29.9 <LLOQ(2.00) 7.19 2.17 <LLOQ(2.00) <LLOQ(2.00) Serum sample results obtained using plasma curves may vary from results obtah_ed from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The metlaod acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 71 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 11857 11858 1186 1199 1214, 1217 1229 1232 1239 1240 1248 1254 1255 1261 1264 1269 1273 PFOS Concentration 199 144 39.3 62.2 44.2 70.7 37.7 53.5 37.5 I 67.6 42.7 35.4 97.9 47.5 51.5 78.1 72. I PFOA Concentration* 20.0 20.8 10.2 8.64 5.55 6.72 3.05 6.70 3.46 10.3 4.40 5.44 9.80 6.27 8.51 16.4 7.52 PFHS Concentration* PFOSAA Concentration* 241 <LLOQ(2.60) 257 4.69 1.89 6.23 3.15 6.64 33.9 2.93 42.4 <LLOQ( 1.36) 2.97 6.45 ..... 3.47 2.83 1,38 61.4 2.50 9.61 76.5 4.53 18.2 6.98 5.56 14.3 4.44 3.26 2.97 2.09 4.71 3.62 4. I0 11.6 PFOSA Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I. 00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ C1.00) M556 Concentration* <LLOQ(5.00) 12.1 2.79 5.76 2.61 <LLOQ(2.50) 6.33 4.46 <LLOQ(2.50) 4.12 3.09 <LLOQ(2.50) 3.24 3.59 5.35 3.34 4.91 M570 Concentration* <LLOQ(2.00) 18.7 I. ! 4 9.65 4.3 <LLOQ(I.00) 1.56 13.8 4.45 6.12 1,77 1.81 3.22 3.44 6.9 2.48 5.23 Serum sample results obtained using plasma curves may vary from results obtained fi'om serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been con'ected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states tile concentration for each QC must be within _+20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical en'or of any individual result may exceed the QC acceptance criteria. Page 72 Northwest Bioanalytical Study No. NW13S00-088 Report No. NWBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1291 1294 1296 1299 1311 1314 1323 1337 1339 1356 1358 1364 1368 1372 1387 1393 1395 PFOS Concentration 37.9 119 39.9 27.7 36.0 51.7 95.4 65.4 27.8 24.3 37.1 33.3 61.7 34.8 35.0 134 110 PFOA Concentration* 6.74 17.5 4.74 6.57 6.05 5.35 15.1 6.41 7.17 3.15 3.96 5.10 13.3 5.88 6.76 7.71 I 1.6 PFHS Concentration* 2.52 220 9.16 <LLOQ(I.36) 3.67 18.1 10.5 5.46 <LLOQ(1.36) 1.58 1.60 3.19 8.18 <LLOQ(1.36) 3.26 88.2 129 PFOSAA Concentration* 6.93 6.71 18.7 <LLOQ(1.60) 5.39 7.14 5.54 9.47 2.26 3.27 9.17 6.95 3.93 6.66 4.53 7.42 9.89 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.O0) <LLOQ(1.00) <LLOQ(1.O0) <LLOQ(1.O0) <LLOQ(I.O0) <LLOQ( 1.00) <LLOQ( 1.00) <LLOQ(I.O0) <LLOQ(1.O0) <LLOQ( 1.00) <LLOQ(I.00) M556 Concentration* <LLOQ(2.50) 13.1 6.84 <LLOQ(2.50) <LLOQ(2.50) ,5.59 <LLOQ(2.50) 5.09 <LLOQ(2.50) <LLOQ(2.50) 6.09 5.4 5.84 <LLOQ(2.50) 2.96 4.44 2.6 M570 Concentration* 3.56 16.3 7.38 1.9 1.12 1.05 5.85 3.93 <LLOQ(I,O0) <LLOQ(1.O0) !.31 <LLOQ( 1.00) 19.6 <LLOQ(1.00) 3.67 2.52 <LLOQ(i.00) Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected nm (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concennation. Tile statistical error of any individual result may exceed the QC acceptance criteria. Page 73 Northwest Bioanalytical Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Study No. NWBS00-088 Report No. NWBR01-001 Sample No. 1398 1400 1407 1408 1409 1410 1411 1412 1418 1420 1423 1424 1427 1431 1433 1435 1438 PFOS Concentration 37.6 32.5 24.3 34.7 34.0 21.3 31.5 35.1 36.2 34.5 22.7 29.3 17.6 27.6 20.3 19.0 56.9 PFOA Concentration* 8.55 5.00 2.84 3.96 3.92 3.41 4.76 4.58 6.24 4.71 5.08 2.69 3.34 5.68 2.88 3.48 5.83 PFHS Concentration* 4.44 1.49 2.57 4.19 1.58 <LLOQ(1.36) 2.52 7.03 <LLOQ(1.36) 6.13 5.63 1.47 <LLOQ(I.36) 5.81 <LLOQ(1.36) 4.19 22.4 PFOSAA Concentration* 5.02 3.17 5.69 .4.69 3.88 3.40 4.26 14.1 10.4 5.18 1.82 2.47 4.95 4.45 1.89 2.60 2.91 PFOSA Concentration* <LLOQ(I.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(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ( 1.00) M556 Concentration* <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 2.73 3.48 2.74 <LLOQ(2.50) 5.44 5.77 2.77 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 4.54 <LLOQ(2.50) <LLOQ(2.50) 2.72 M570 Concentration* 3.69 1.25 1.54 1.84 1.06 1.42 3.85 . 4.53 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) 1.52 1.98 1.42 1.24 1.72 2.46 Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 74 Northwest Bioanalytical Study No. NWBS00-088 Report No. NrWBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1439 1448 1455 1461 1467 1468 1470 1472 1482 1483 1491 1493 1494 1496 1498 1503 1510 PFOS Concentration PFOA Concentration* 20.1 .......... 64.8 4.77 5.35 16.7 3.23 41.3 6.21 18.2 3.30 16.6 2.66 36.2 8.05 32.4 5.55 i 59.4 4.88 54.6 5.24 26.2 3.36 37.6 4.49 16.8 3.01 54.9 4.53 41.7 4.42 24.6 2.40 32.5 3.21 PFHS Concentration* 9.34 21.8 <LLOQ(1.36) 19.2 5.74 3.46 5.69 1.77 17.2 8.66 3.73 10.6 <LLOQ(1.36) 38.3 <LLOQ(1.36) 2.73 13.7 PFOSAA Concentration* 3.57 9.13 <LLOQ(I.60) 2.71 <LLOQ(I.60) <LLOQ(1.60) 4.97 1_71 ,i ', 18.3 23.8 2.62 <LLOQ(1.60) 2.77 1.95 5.31 2.39 <LLOQ(1.60) PFOSA Concentration* <LLOQ(I.00) i <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* 5.46 4.43 <LLOQ(2.50) 3.34 <LLOQ(2.50) <LLOQ(2.50) 4.3 2.88 .i 6.53 12 <LLOQ(2.50) 4.27 2.79 4.95 3.7 <LLOQ(2.50) 3.24 M570 Concentration* 2.87 <LLOQ(I.00) <LLOQ(1.00) 2.98 <LLOQ(I.00) <LLOQ(1.00) 4.88 1.23 3.52 4.1 <LLOQ(I.00) 22.7 2.28 <LLOQ(I.00) !. 13 1.68 17.1 Serum sample results obtained using plasma curves may vary fi'om results obtained from sel_Jm curves (see Results and Discussion). , Results are from a rejected n,n (see Results and Discussion). Tile concentrations of any diluted samples have been cmxected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within -1-20%(+25% for PFOSA and PFOSAA) of file target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 75 Northwest Bioanalytical Study No. Na,VBS00-088 Report No. N_VBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1512 1513 1517 1524 1529 1537 1538 1542 1545 1558 1559 1574 1582 1590 1597 1603 16 ! I PFOS Concentration 26.4 34.1 62.8 28.9 26.5 10.4 35.9 17.2 28.9 50.8 61.0 25.0 26.0 39.3 31.5 25.4 37.3 PFOA Concentration* 2.63 4.37 5.76 4.82 4.56 <LLOQ(1.92) 2.36 2.14 3.89 7.92 10.5 4.75 3.20 6.61 9.93 5.53 13.0 PFHS Coneentration* 12.1 5.13 58.8 4.30 2.73 <LLOQ(1.36) 11.2 <LLOQ(1.36) 2.28 13.8 14.2 6.47 <LLOQ( 1.36) 4.27 3.34 <LLOQ(1.36) 1.52 PFOSAA Coneentration* 1.73 3.27 <LLOQ(1.60) 1.66 3.83 <LLOQ(1.60) 4.33 <LLOQ(1.60) 6.05 10.4 8.56 2.17 1.89 5.56 2.8 5.99 6.68 PFOSA Concentration* <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.O0) <LLOQ( 1.00) <LLOQ(I.00) <LLOQ(I.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(I.00) <LLOQ( 1.00) M556 Concentration* <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 6.23 6.06 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 2.5 4.44 6.92 <LLOQ(2.50) 3.07 8.75 2.74 <LLOQ(2.50) 5.62 M570 Concentration* 4.33 1.9 <LLOQ(I.00) 15.2 <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 1.61 2 <LLOQ(1.00) <LLOQ( 1.00) 1.49 <LLOQ(I.00) 5.75 Sermn sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 76 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Sample No. 1616 1618 1620 1624 1626 1630 1634 1637 1640 1643 1646 1647 1652 1653 1663 1665 1668 PFOS Concentration 30.0 26.1 21.8 45.4 25.0 13.6 22.7 35.7 11_9 17.5 15.8 18.8 34.7 44.2 1!.5 15.0 20.5 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFOA Concentration* 4.67 3.08 3.19 5.54 3.15 3.13 2.56 3.08 2.46 2.33 2.34 3.79 6.21 7.80 2.15 <LLOQ(1.92) 2.9 PFHS Concentration* 3.79 5.35 1.87 41.5 1.55 <LLOQ(1.36) 7.25 23.3 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) 5.59 4.54 <LLOQ(I.36) <LLOQ(1.36) 2.29 PFOSAA Concentration* <LLOQ(1.60) 4.69 <LLOQ(1.60) 1.60 <LLOQ(1.60) <LLOQ(1.60) 1.73 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 2.26 2.81 5.50 7.02 <LLOQ(I.60) 6.09 2.15 PFOSA Concentration* <LLOQ(E00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) M556 Concentration* <LLOQ(2.50) 2.77 <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) 3.75 4.14 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) , M570 Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) ,:LLOQ(1.00) <LLOQ(1.00) <LI, OQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ( 1.00) 3.91 <LLOQtl.00) <LLOQ(I.00) <LLOQ(1.00) Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 77 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1669 1677 1678 1679 1680 1690 1692 1700 1707 1709 1716 1719 1721 1722 1735 1748 1766 PFOS Concentration 33.9 27.6 15.9 28.1 23.0 38.1 42.6 22.4 42.4 42.5 33.3 21.2 26.1 28.6 27.5 27.2 43.6 PFOA Concentration* 6.64 2.58 2.46 4.27 2.69 4.97 8.11 2.14 3.56 4.74 4.57 4.55 4.96 3.25 5.88 3.44 5.28 PFHS Concentration* 3.25 3.31 <LLOQ(1.36) 3.52 <LLOQ(1.36) <LLOQ(I.36) 8.96 <LLOQ(1.36) 4.17 38.5 <LLOQ(I.36) 2.25 1.93 <LLOQ(1.36) 1.97 3.14 7.07 PFOSAA Concentration* 6.72 2.38 3.13 2.39 3.74 12.8 11.2 6.01 5.07 3.71 6.99 1.93 1.67 <LLOQ(1.60) 7.19 2.25 5.68 PFOSA Concentration* <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ( 1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) M556 Concentration* 2.87 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 5_.49 <LLOQ(2.50) 4.96 4.06 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 3.66 <LLOQ(2.50) <LLOQ(2.50) M570 Concentration* 2.33 1.32 1.74 2.39 6.08 1.01 1.57 <LLOQ( 1.001 3.77 " 3.43 3.47 1.21 <LLOQ(1.00) 2.82 2.74 2.65 2.97 Sel_mi sample resuhs obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within _+20%(+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 78 Northwest Bioanalytical Study No. NWBS00-088 Report No. N\VBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1778 1781 1788 1806 1809 1816 1817 1819 1822 1825 1830 1834 1837 1842 1857 1875 1876 PFOS Concentration 25.3 32.4 49.7 67.7 12.7 33.9 29.3 29.3 48.8 20.5 19.9 28.7 71.8 32.2 21.3 28.3 25.0 PFOA Concentration* 5.66 4.02 5.74 7.17 1.95 5.93 4.40 4.12 6.01 4.76 4.29 5.75 8.95 5.37 5.70 4.91 5.60 PFHS Concentration* 1.65 1.67 19.6 94.2 <LLOQ(I.36) <LLOQ( 1.36) 12.4 7.59 17.8 2.65 2.79 15.7 4.69 9.45 <LLOQ( 1.36) 1.58 8.53 PFOSAA Concentration* 1.70 3.58 5.97 4.75 <LLOQ(1.60) 11.6 3.54 2.90 9.63 2.44 1.62 3.68 12.9 1.69 5.07 2.18 2.24 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) i <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(I.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(I.00) M556 Concentration* 2.62 <LLOQ(2.50) 5.25 <LLOQ(2.50) <LLOQ(2.50) 9.82 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 2.78 9.88 <LLOQ(2.50) 19.1 7.29 4.54 <LLOQ(2.50) 2.79 M570 Concentration* 6.74 6.82 1.12 <LLOQ_ 1.00) <LLOQ(I.00) <LLOQ( 1.00) 1.56 2.62 2.01 2.04 2.47 3.06 38.1 3.89 <LLOQ( 1.00) 1.88 1.72 Scrim1 sample results oblained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 79 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-00 ! Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1886 1887 1888 1898 1909 1911 1912 1913 1934 1942 1953 1954 1956 1959 1961 1962 1965 PFOS Concentration 52.6 16.9 40.5 18.3 149 35.3 46.2 43.9 51.2 50.1 74.3 55.5 30.6 23.8 31.0 16.2 75.2 PFOA Concentration* 9.49 3.22 8.11 5.26 16.1 6.28 7.32 9.06 6.99 8.54 7.94 5.09 5.05 4.26 5.54 4.12 6.65 PFHS Concentration* 2.01 <LLOQ(I.36) 2.39 3.40 170 2.44 3.17 " ........ 3.52 4.44 4.83 18.9 1.64 10.7 3.42 12.3 <LLOQ(1.36) 87.9 PFOSAA Concentration* 19.6 4.81 5.31 2.22 3.81 2.40 6.16 " 2.93 4.90 3.22 5.18 6.62 3.20 3.87 2.95 <LLOQ(1.60) 5.62 PFOSA Concentration* <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ( 1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) M556 Concentration* 9.53 <LLOQ(2.50) 6.41 <LLOQ(2.50) 2.76 4.56 2.65 | <LLOQ(2.50) <LLOQ(2.50) 3.02 2.76 4.45 <LLOQ(2.50) <LLOQ(2.50) 3.06 <LLOQ(2.50) 4.22 M570 Concentration* <LLOQ(1.00) 1.38 1.22 1.03 1.28 1.15 1.58 ,., 5.23 13.1 1.95 4.27 3.76 4.77 2.37 2.27 <LLOQ(I.00) 2.13 Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for tile persistent level of analyte in the dilution matrix. Tile method acceptance criteria states tile concentration for each QC must be within +20% (-I-25%for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 80 Northwest Bioanalytical Study No. NWBS00-088 Report No. NrWBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1982 1996 2000 2002 2003 2022 2038 2041 2050 2052 2054 2056 2074 2075 2076 2078 2079 PFOS Concentration 18.2 27.1, 93.7 96.8 52.2 34.7 70.4 22.8 41.5 25.8 20.7 45.6 48.5 38.8 39.4 86.8 59.9 PFOA Concentration* 4.15 3.82 10.1 7.17 4.87 3.94 8.89 5.69 4.61 <LLOQ(2.88) 3.06 4.31 5.54 5.30 6.65 19.5 6.63 PFHS Concentration* 1.51 2.43 7.12 90.8 3.72 4.98 15.8 7.12 2.83 <LLOQ(2.41) 2.36 15.4 2.21 3.75 8.06 20.4 4.84 PFOSA.A Concentration* 3.93 3.43 8.19 2.93 8.86 1.80 2.35 1.88 2.64 <LLOQ(2.60) 3.50 5.44 4.60 2.19 6.49 8.81 2.40 PFOSA Concentration* <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(2.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) M556 Concentration* <LLOQ(2.50) <LLOQ(2.50) 9.14 <LLOQ(2.50) 3.48 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 3.28 <LLOQ(5.00) 2.84 <LLOQ(2.50) 2.77 2.93 3.48 10.2 5.37 M570 Concentration* 2.25 <LLOQ( 1.00) 17.9 2.45 3.08 2.63 5.81 <LLOQ(1.00) 8.4 <LLOQ(2.00) <LLOQ(1.00) 1.49 3.03 5.4 4.24 42.5 14.8 Serum sample results obtained using plasma curves may vary fi'om results obtained from serum curves (see Results and Discussion). Results are fi-om a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within -t-20% (+25% for PFOSA and PFOSAA) of the target concennation. The statistical error of any individual result may exceed the QC acceptance criteria. Page 81 Northwest Bioanalytical Table 22. Study Sample Coneentrations (Continued) All concentrations are expressed as ppb. Study No. N_VBS00-088 Report No. N-WBR01-001 Sample No. 2082 2087 2089 2099 2104 2112 2114 2115 2121 2124 2127 2140 2141 2144 2150 2151 2156 PFOS Concentration 86.6 34.4 21.0 47.1 55.3 80.5 42.8 28.0 55.1 42.5 62.1 26.1 29.7 37.0 39.2 23.9 46.6 PFOA Concentration* 6.87 8.42 4.61 5.29 6.83 10.7 4.48 5.83 4.10 6.95 8.96 3.67 6.77 4.06 4.24 3.37 7.95 PFHS Concentration* 84.1 1.55 2.16 4.23 47.6 62.2 3.39 5.04 19.2 15.9 27.9 2.81 <LLOQ(I.36) 2.65 9.88 1.64 13.6 PFOSAA Concentration* 9.70 7.75 4.61 5.82 <LLOQ(1.60) 5.79 4.62 5.3 4.52 4.33 3.43 2.28 <LLOQ(1.60) 6.25 6.59 <LLOQ(1.60) 3.94 PFOSA Concentration* <LLOQ(I.00) <LLOQ(I.00) <LLOQ( 1.00) <LLOQ(I.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(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) M556 Concentration* <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) ' 3.32 <LLOQ(2.50) 2.75 3.38 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 6.14 9.89 <LLOQ(2.50) <LLOQ(2.50) M570 Concentration* 1.97 <LLOQ(1.00) <LLOQ( 1.00) 2.09 1.36 1.64 3.76 4.04 9.68 4.14 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 1.1 2.36 <LLOQ(1.00) 3.82 Scrim1 sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of ally diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 82 Northwest Bioanalyticai Study No. N_VBS00-088 Report No. NW'BR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 2 158 2162 2164 2168 2171 2173 2174 2176 2179 2181 2184 2186 2191 2193 2200 2220 2227 PFOS Concentration 36.4 48.1 36.2 515 65.5 49.5 63.5 73.2 123 116 53.3 50.2 40.2 40.1 41.5 42.4 69.9 PFOA Concentration* 6.93 5.10 5.08 20.2 7.09 5.23 14.0 8.55 9.96 11.5 10.5 8.36 4.52 6.62 5.66 5.61 7.47 PFHS Concentration* 6.10 14.1 4.51 712 37.3 18.2 5.92 59.2 107 55.4 5.07 3.11 <LLOQ(1.36) 31.9 12.1 8.01 104 PFOSAA Concentration* 4.02 1.81 2.58 4.04 5.69 4.68 5.23 2.68 7.47 18.1 3.94 7.97 3.37 6.45 4.73 7.73 <LLOQ(I.60) PFOSA Concentration* <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LEOQ( 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(I.00)** <LLOQ(I.00)** M556 Concentration* 2.55 <LLOQ(2.50) <LLOQ(2.50) 16.4 <LLOQ(2.50) 5.08 3.92 3.49 4.01 13.4 6.68 3.88 2.97 4.54 <LLOQ(2.50) <LLOQ(2.50) 5.59 M570 Concentration* 2.48 2.12 3.35 7 2.8 8.34 17.7 3.47 9.76 4.82 7.53 5.6 1.08 6.58 1.42 6.69 6.75 Scrim1 sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical en'or of any individual result may exceed the QC acceptance criteria. Page 83 Northwest Bioanalytical Study No. Na,VBS00-088 Report No. N'x\rBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 2230 2234 2236 2239 2244 2246 2248 2260 2265 2273 2298 2307 2323 2327 2335 2341 2348 PFOS Concentration 66.6 36.1 39.8 17.2 26.2 34.7 60.8 6.67 44.8 28.3 17.7 43.9 25.5 24.3 26.5 43.4 34.7 PFOA Concentration* 7.92 5.77 5.97 2.77 2.91 5.06 6.72 <LLOQ(I.92) 5.09 3.45 2.22 5.52 3.65 5.47 3.18 7.21 4.45 PFHS Concentration* 84.2 14.8 25.4 12.5 3.44 4.20 29.6 <LLOQ(1.36) 10.4 1.79 <LLOQ(I.36) 4.73 <LLOQ(1.36) 3.79 3.79 2.25 <LLOQ(l.36) PFOSAA Concentration* <LLOQ(1.60) 2.95 2.92 <LLOQ(I.60) 3.69 2.96 3.21 <LLOQ(1.60) 4.18 <LLOQ(I.60) 3.16 8.03 <LLOQ(1.60) 2.22 <LLOQ(1.60) 5.43 5.20 PFOSA Concentration* <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(I.00)** <LLOQ(I.00)** <LLOQ(1.00)** <LLOQ(I.00)** <LLOQ(1.00)** <LLOQ(I.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(I.00)** <LLOQ(I.00)** <LLOQ(I.00)** <LLOQ(1.00)** <LLOQ(I.00)** <LLOQ( 1.00)** <LLOQ(I.00)** M556 Concentration* <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 2.94 <LLOQ(2.50) 5.33 <LLOQ(2.50) 4.53 7.59 M570 Concentration* 1,36 2.32 2.93 <LLOQ(1.00) <LLOQ(I.00) 1.85 2.55 <LLOQ(1.00) 1.29 3.59 2.48 1.2 4.55 <LLOQ(1.00) <LLOQ(1.00) 10.6 6.4 Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC nmst be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical elTor of any individual result may exceed the QC acceptance criteria. Page 84 Northwest Bioanalytical Study No. N_VBS00-088 Report No. NWBR01-00 ! Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 2349 2350 2351 2353 2355 2358 2360 2363 2365 2366 2368 2376 2386 2395 2397 2400 2406 PFOS Concentration 40.8 76.4 36.9 34.0 36.2 61.8 29.9 29.7 42.4 65.7 42.8 43.2 11.2 61.8 77.2 62.4 29.1 PFOA Concentration* 3.86 8.86 3.79 3.86 4.72 10.3 7.43 3.52 3.56 5.24 5.39 4.20 <LLOQ(I.92) 4.45 7.81 7.37 3.76 PFHS Concentration* 4.49 20.3 1.76 4.51 1.62 1.79 <LLOQ(1.36) 2.65 7.62 7.92 10.5 4.50 <LLOQ(I.36) 4.20 27.2 10.5 <LLOQ(I.36) PFOSAA Concentration* <LLOQ(I.60) 13.1 <LLOQ(1.60) 2.19 <LLOQ(I.60) 2.93 5.02 6.43 <LLOQ(I.60) 4.39 2.50 3.41 5.19 10.3 7.78 3.39 <LLOQ(1.60) PFOSA Concentration* <LLOQ(I.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(I.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(I.00)** <LLOQ(I.00)** <LLOQ(I.00) <LLOQ(I.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(I.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(I.00)** <LLOQ(I.00)** M556 Concentration* <LLOQ(2.50) 6.83 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 4.72 4.53 3.67 <LLOQ(2.50) <LLOQ(2.50) 3.77 <LLOQ(2.50) <LLOQ(2.50) 13.4 5.09 2.55 3.62 M570 Concentration* 5.22 16.8 <LLOQ(1.00) 1.45 1.33 13.4 1.05 3.12 3.33 4.88 3.54 4.58 <LLOQ(1.00) 19.5 2.89 10.4 3.5 Senmi sample results obtained using plasma curves may vary fiom results obtained from sel'um curves (see Results and Discussion). Results are from a rejected _un (see Results and Discussion). Tiie concentrations of any diluted samples have been con'ected for the persistent level ofanalyte iz(the dilution matrix. The method acceptance criteria states the coneentTation for each QC must be within +20% (-1-25%for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 85 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 2431 2433 2436 2438 2440 2474 2491 2493 2495 2496 2499 2500 2514 2516 25 ! 7 2522 2524 PFOS Concentration 50.6 27.7 33.0 61.9 23.6 42.9 40.1 34.4 20.8 28.0 28.0 26.3 36.9 54. i 51.6 30.2 3g.6 PFOA . Concentration* 4.80 5.50 9.32 _ 7.05 6.95 3.60 5.82 7.11 3.08 5.40 2.42 3.02 4.05 6.95 11.3 3.27 3.68 PFHS Concentration* 5.57 2.93 3.45 3.34 1.66 1.79 10.3 5.99 2.53 6.77 73.9 10.2 4.29 2.08 73.4 1.39 2.02 PFOSAA Concentration* 2.82 5.46 2.95 11.2 <LLOQ(I.60) 9.55 2.44 6.14 <LLOQ(1.60) 5.36 <LLOQ(1.60) <LLOQ(1.60) 4.66 10.1 3.02 <LLOQ(1.60) 4.65 PFOSA Concentration* <LLOQ(I.00)** <LLOQ(I.00)** <LLOQ(I.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLO Q( 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(I.00) M556 Concentration* 9.74 3.47 4.67 4.89 <LLOQ(2.50) 3.25 <LLOQ(2.50) 4.34 2.58 3.15 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 3.68 4.49 <LLOQ(2.50) 4.69 M570 Concentration* 9.19 <LLOQ(1.00) 2.8 l 7.48 <LLOQ(1.00) 1.35 1.49 2 8.11 5.24 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 2.41 <LLOQ(1.00) <LLOQ(I.00) 3.9 Sermn sample results oblained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 86 Northwest Bioanalytical Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Study No. NWBS00-088 Report No. N_VB R01-001 Sample No. 2526 2528 2531 2567 2570 2575 2577 2584 2585 2590 2593 2597 9433 9434 9435 9436 0437 PFOS Concentration 37.0 122 27.3 29.0 42.7 52.1 21.6 217 58.5 45.0 32.9 43.8 38.2 45.7 35.7 35.1 14.7 PFOA Concentration* 4.49 5.87 2.75 4.44 3.71 5.92 <LLOQ(I.92) 34.2 6.27 5.52 6.98 5.67 9.14 4.55 6.29 6.78 <LLOQ(2.88) PFHS Concentration* 3.65 2.90 1.99 <LLOQ(I.36) <LLOQ(I.36) 32.6 2.17 497 1.66 2.12 <LLOQ(1.36) 15.2 4.97 11.7 25.5 <LLOQ(2.41) <LLOQ(2.41) PFOSAA Concentration* 4.26 4.63 1.96 2.21 3.73 8.19 <LLOQ(1.60) 8.82 9.68 2.13 2.10 3.85 5.78 3.71 <LLOQ(2.60) : 4.01 <LLOQ(2.60) PFOSA Concentration* <LLOQ(I.00) <LLOQ( .1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(2.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ( 1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) M556 Concentration* <LLOQ(2.50) 12.3 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 7.53 <LLOQ(2.50) 6.27 10.9 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 5.43 <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) M570 Concentration* <LLOQ(! .00) 34.4 4.19 <LLOQ(I.00) <LLOQ(I.00) <LLOQ(2.00) <LLOQ(I.00) 2.92 22.2 10.8 <LLOQ(I.00) 3.16 <LLOQ(2.00) 2.23 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within -1-20%(+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 87 Northwest Bioanalyticai Study No. NWBS00-088 Report No. N_rBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 9438 9439 9440 9441 9442 9443 9444 9445 9446 9447 9448 9449 9450 9451 9452 9453 9454 PFOS Concentration 47.7 40.5 ! 5.0 48.0 32.3 51.6 42.1 98.9 25.2 39.8 20.4 45.1 29.8 40.1 43.5 30.5 40.2 PFOA Concentration* 8.15 6.54 <LLOQ(2.88) 5.05 4.41 7.49 6.64 6.35 3.73 <LLOQ(2.88) 3.31 5.66 3.18 3.69 4.96 3.54 3.95 PFHS Concentration* 5.81 6.65 <LLOQ(2.41) <LLOQ(2.41) 4.22 <LLOQ(2.4 I) 9.06 88.7 <LLOQ(2.41) 33.0 <LLOQ(2.41) <LLOQ(2.41) <LLOQ(2.41) <LLOQ(2.41) 22.3 4.48 <LLOQ(2.41) PFOSAA Concentration* <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) 4.23 <LLOQ(2.60) 7.41 <LLOQ(2.60) 3.61 <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) 4.60 <LLOQ(2.60) 5.18 <LLOQ(2.60) <LLOQ(2.60i 4.8 i PFOSA Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) M556 Concentration* <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) M570 Concentration* <LLOQ(2.00) 10.3 <LLOQ(2.00) 2.37 <LLOQ(2.00) <LLOQ(2.00) 5.59 4.88 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 6.54 4.1 <LLOQ(2.00) 2.95 <LLOQ(2.00) <LLOQ(2.00) Senmi sample resulls obl_lined using p}asma curves may vary fiom results obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for-the persistent level of analyte irathe dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 88 Nmahwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 9455 9456 9457' 9458 9459 9460 9461 9462 9463 9464 9465 9466 9467 9468 9469 9470 9471 PFOS Concentration 25.8 66.1 35.8 31.6 62.8 18.8 29.2 40.9 28.0 17.2 16.5 50.0 49.7 49.1 80.5 28.9 55.6 PFOA Concentration* 4.74 14.94 <LLOQ(2.88) 3.39 6.12 4.09 4.08 <LLOQ(2.88) 3.71 <LLOQ(2.88) <LLOQ(2.88) 7.50 5.98 7.10 18.64 5.32 11.5 PFHS Concentration* 3.84 20.5 2.49 3.58 3.35 17.1 <LLOQ(2.41) 23.0 3.4 2.98 <LLOQ(2.41) <LLOQ(2.41) <LLOQ(2.41) <LLOQ(2.41) 38.1 7.78 40.2 PFOSAA Concentration* 15.8 5.70 5.49 <LLOQ(2.60) 3.32 <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) 2.71 4.24 10.5 <LLOQ(2.60) 10.8 PFOSA Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) M556 Concentration* <LLOQ(5.00) 7.24 <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) .<LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) M570 Concentration* <LLOQ(2.00) 7.38 <LLOQ(2:00) 5.13 2.08 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 3.67 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) Sertnn sample results obtained using plasma curves may vary from resulls obtained from serum curves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been con'ected for the persistent level of analyte in the dilution man'ix. The method acceptance criteria states the concentration for each QC nmst be within :t:20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 89 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 9472 9473 9474 9475 9476 9477 9478 9479 9480 9481 9482 9483 9484 9485 9486 9487 9488 PFOS Concentration 54.9 34.7 43.3 57.2 40.0 22.4 33.6 14.1 42.2 33.8 33.9 " 24.7 10.2 37.4 32.7 46.7 22.0 PFOA Concentration* 3.93 4.96 4.95 7.03 <LLOQ(2.88) 2.97 5.15 <LLOQ(2.88) 5.99 5.37 <LLOQ(2.88) <LLOQ(2.88) <LLOQ(2.88) 4.45 4.23 6.81 4.36 PFHS Concentration* 9.60 12.2 6.56 4.70 10.2 <LLOQ(2.41) <LLOQ(2.41) <LLOQ(2.41) 2.58 <LLOQ(2.41) 12.39 <LLOQ(2.41) <LLOQ(2.41), 6.54 <LLOQ(2.41) 6.40 <LLOQ(2.41) PFOSAA Concentration* 3.56 <LLOQ(2.60) 2.74 <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) 3.89 <LLOQ(2.60) <LLOQ(2.60) 6.08 <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) 4.76 4.41 3.59 <LLOQ(2.60) PFOSA Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) M556 Concentration* <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) 5.26 <LLOQ(5.00) M570 Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 2.79 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 3.12 <LLOQ(2.00) Seruln sample results obtained using plasma curves may vary from results obtained from senma craves (see Results and Discussion). Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 90 Northwest Bioanalytical Sample No. 9489 9490 9491 9492 9493 9494 9495 9496 9497 9498 9499 9500 9501 9502 9503 9504 9505 PFOS Concentration 27.0 21.2 60.9 30.3 31.6 20.3 41.4 33.1 97.9 49.7 29.3 30.3 35.6 17.8 29.3 34.3 27.0 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFOA Concentration* 3.04 3.88 6.41 <LLOQ(2.88) 5.43 <LLOQ(2.88) 7.57 4.76 14.64 2.93 3.76 <LLOQ(2.88) 4.70 <LLOQ(2.88) 3.22 ' 5.14 4.75 PFHS Concentration* <LLOQ(2.41) 12.2 37.6 <LLOQ(2.41) <LLOQ(2.41) <LLOQ(2.41) 4.56 3.10 114 67.3 8.67 <LLOQ(2.41) <LLOQ(2.41) <LLOQ(2.41) <LLOQ(2.41) 10.4 4.54 PFOSAA Concentration* 6.87 <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) 3.83 <LLOQ(2.60) 9.31 3.04 <LLOQ(2.60) <LLOQ(2.60) 2.61 <LLOQ(2.60) 5.47 2.74 <LLOQ(2.60) <LLOQ(2.60) 5.37 PFOSA Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) Study No. N\VBS00-088 Report No. N_VBRO 1-001 M556 Concentration* <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) M570 Concentration* 11.3 <LLOQ(2.00) 2.45 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 8.68 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 3.02 <LLOQ(2.00) <LLOQ(2.00) 2.62 <LLOQ(2.00) Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). Results are from a rejected run(see Results and Discussion). The concentrations of any diluted samples have been con'ected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 91 Northwest Bioanalyticai Sample No. 2168 Table 23. Repeat Analysis Table for PFOS Study No. NWBS00-088 Report No. NWBR01-001 Treatment Ped Time Oh Original Cone. ppb >ULOQ(414) Original Run Number 10 Reason for Reassay 1 Reassay Cone. ppb 515 Reassay, Run Number 14 Reported Cone. ppb 515 Reason for Reported Conc. 1 Sample No. 2168 Table 24. Repeat Analysis Table for PFHS Treatment Ped Time Oh Original Cone. ppb >ULOQ(523) Original Run Number 10 Reason for Reassay 1 Reassay Cone. ppb 712 Reassay Run Number 14 Reported Cone. ppb 712 Reason for Reported Cone. 1 REASONS FOR REASSAY: 1). Greater than tile ULOQ. REASONS FOR REPORTED CONC: 1). Original result outside of quantitation Page 92 range. Reassay results reported. Northwest Bioana|ytical Figure I. Representative Saldy No. NWBS00-088 Repor_ No. NWBR01-001 Calibration Curve for PFOS A.alytical Run 7 analyzed on 09-Nov-2000 Calibration S|andards ['orPFOS Regression MeUiod = QUADRATIC - Weighting Factor - I/X'2 Quadratic Limit _ 20130 (ng/mL) 16A, 14. A 12 i lO '0 50 I00 150 200 250 300 350 400 4.50 Nominal Cone. (ng/mL) Figure 2. Representative Calibration Curve for PFOA Analytical Run 7 analyzed on 09-Nov-2000 Calibration Standards for PFOA (nWm.L) P,.cSre_ioe Method - QUADP,.ATIC - Weighting Factor = IlX**2 Quadratic Limit - 3190 7 6 5 2 I 0 0 ! , , $0 100 I $0 20Q 250 300 350 400 450 500 Nominal Cone. (ng/mL) Page 93 Northwest Bioanalytical Study No. NWBS00-088 , Report No. NWBR01-001 Figure 3. Representative Calibration Curve for PFHS Aaaiytical Run7 analyzedon 09-Nov-2000CaiibralionStandards[br PFHS(nghuL) RegressionMethod- QUADRATIC WeightingFactor= I/X"2 QuadraticLintit - 1410 14 12 10 _8 I" 4 2 0 0 100 200 300 400 J00 600 Nominal Cone. (ng/mL) Figure 4. Representative Calibration Curve for PFOSAA Analytical Run 7 analyzed on 09-Nov-2000 CalibrationStandards for PFOSAA {ng/mL) Regression Method - QUADRATIC - Weighting Factor- I/X**2 QuadraticLimit= -4160 8 7 6 i' 2 I 0 100 200 300 400 $00 600 Nominal Conc.(n .WmL) Page 94 Northwest Bioanalytica[ Study No. NWBS00-088 Report No. NWBR01-001 Figure 5. Representative Calibration Curve for PFOSA A,aly6cal Run 7 a,alyzcd on 09-Nov-2000 CalibrationStandards['orPFOSA (nghuL) Rcgre_sio, Method = QUADRATIC - Weighting FaL:Ior- I/X'2 Quadratic I.hlliI = 2830 3S 30 25 i2o i 10 $ 0 t I . 50 100 150 200 250 300 350 400 450 500 Nominal Cone. (n_mL) 4.$ 4..0 3.5 3.0 _2J Figure 6. Representative Calibration Curve for M556 Analytical Run7 analyzed on 09-Nov-2000 Calibration Standardsfor M556 (ng/mL) Regression Method - QUADRATIC - Weighting Factor= l/X*"2 Quadratic Limit - -1620 1.5 1.0 03 8 2.0 0.0 f _ 0 50 _ I 1 _ t I I 100 150 200 250 300 350 400 450 :TOO NominalCone.(n ,g,'ml) Page 95 Northwest Bioanalytical Figure 7. Representative Study No. NWBS00-088 Report No. NWI3R01-00 i Calibration Curve for 5'I570 Analytical Run 7 analy'tcd on 09-Nov-_.OQO Calibration Standards Re,.dression Method = QUADRATIC- Weighting Factor- Quadratic Limit = -23900 for M570 (ng/vuL) I/X'*2 14 ,5 IO i, i 4 2 0 -- , 50 [ , , 100 I $0 200 250 300 350 Nominal Cone, (ng/mL) 400 4.$0 500 Page 96 Northwest Bioaualytical Figure 8. Human Serum Blank for PFOS Study No. NWBS00-088 Report No. NWBR01-001 iPFos Internal Slandard: THPFO$ Use Area Absolute Retention 13me Expected RT 4:54 I NO_ l_res. i Cu/fsfll Memod F 5.01 5.0 Quanl Thins. _'_P--"---'--I MIn. Wld/_ _ Mull. Wldgl _ Base. wiath _ RT win, (secs) _ smco_l 11 0.2 3 12 150 20 1 s0008807.012 7 012 S00088 CONTROL_BLANK t No Cornme_ I'hu. NOv 9. 2000 9:08 PM ]:06 8:59 in I peaod 100 I: 8:5g MRM, 571 scans -cO 499.0->80.0 Area 26722 He_lnt Start Time End Time 1744 Inte(:Jr_UonV_dth Retention 73me Inte(Jr"atlonType [_.L,H"'I"I_ 4:30 5:17 0:46.3 4:49 A - BV I_1--_ 00 70 60 50 40 3:0 20. tO' 301 f:3_ 3:10 4:45 intensity : 1746 cps 40 t 6 :I"_ 501 7;54 Scar, Tin'_e_ ITHPFOS I Cun'enl Noise Thins. 110.01 Me61od 10.0 use as fnmmal Stan(mrd Quant Thins. P"--'-'f_ 0.2 :' MIn. Wldm _ 3 Expected RT 4:15 MulL Width _ 10 Base. Widtll _ 150 RT Win. (secs) _ Smoom I 20 II 1 s0008807-012 7 012 S00088 CONTROLBLANK 1 NO Comment Thu, Nov 9, 2000 9:05 PM 207 intensit,j : 25 ps 1:B:59 MRM, 571 scans Area 0 427.0->407.0 HSteai_rtlhTf_me 0 Retention Time Intecjrat;on Type 97 BTCt !_ 0:00.0 50 1: ] 0:O0.0 30 367 436 ,I.80 l0 0 ...... 101 _-"01 3()t I :._5 5:10 4:45 i 41_1 501 So;,n 6:1'9 7:_4 Time ..r Page 97 Northwest Bioanalytical Figure 9. Human Serum Blank for PFOA Study No. NWBS00-088 Report No. NWBR01-001 Cun'ao_ M_l_xl Iltl_lrlil S(a_clal_l:rHPFOS Quanl Tme_, 0.9 Use Area Min, W_ 3 AOsok=aRemnaon T_ne MuR. Wl_tll 9 Ex0eCll_ RT 4:27 8ass. Wilm 150 RT Win. (saa) 20 iv;-,:,'^ Smo_lt ] Noise r_e_ _ I.O1 $OOOBEk]T1,.2O T 012 _ Thu. NOv 9. 20(_ 9:08 PM 8:59 in I _ t: 8:59 MRM. 5;'1 _ 4t3.0_ 19,0 CONTROL BLANK t OO .QO' _0' NOC,omm_ 281 Area 2655 HIi_gl( 2t3 Start T, ne End T'Jell Ima_qIion Wi(fln Time 4:13 4:46 9:32.1 4:26 _,0" 50" 40- ' 30- _tt_|ttJ : 227 cps 36m3 42g 503 .101 I :_5 201 3:10 _.CII 401 4:4_ 6:19 501 .Sc,mr--'- 7:54 T_L!!.': ITHPFOS use as Internal Stan0am Expected RT 4:15 I Current Method No_se "_res. I lo.o l _o.0 Quant Thins. __ Mia. W10ttt _ MutL W_:lth _ Base. Wlclt_ _ RT Win. (sees) _ Smooth I 0.2 3 10 150 20 1] I s0008807-012 7 012 $00088 CONTROLBLANK I NO Comment Thu. Nov 9. 2000 9:08 PM 2B7 8:5g in 1 pedod 100 1:8:59 MRM. 571 scans 427'.0->407.0 int_sit_ : 25 l)s Area 0 He_l_t 0 70 97 E.0, 3'617 438 480 ;lart Time !ndTime 0:0O.0 0:00.0 _0. 3 69 __o Retention 13me Inm_ratJon Type 0:00.0 50' " = I- I il 5 10" 0 , 101 :3_ 164 1ttJ, , 2L31 301 401 3:10 4:45 6 : 19 gO1 ' _.<_,n 7 :_4 Tim_._l_. Page 98 Northwest Bioanalytical Figure 10. Human Serum Blank for PFHS Study No. NWBS00-088 Report No. NWBR01-00 [ ip_Hs I Noise Thres. C[3u.r0re1nt Metho3d.0 Internal Slandard: THPFOS Use Area Absolule Relentlon T_me Quant Thtes. _ 0.5 Mill. Wiath 141 4 Mull. WiGth f t2t 12 Ex!sected RT 3:37 Base. Wk:lth _ RT Wtn. (see,=) _ Smooth I 150 20 11 1 S0008807-012 7 012 B00088 CONTROL_BLANK 1 NO Comment Thu. NOV g. 2000 9:00 PM 239 8:5gin 1 period ; IOl0 1:8:59 MRM. 571 scans 399.0>80.0 intensity : 1_3 l>S Helcjnt 126 AStraerat Time 1410 60 3:29 70 t In lejt-attonWIWI1 Retention Time Intecjration Type 0:30.3 3:46 A- as 409 53') Iil I 348 t 4581. II 1Ol 201 I :35 3:t0 3;01 4:45 401 6;19 501 Scar, t--- 7:54 Time]; 5 I THPFOS use as Internal Standard Expected RT 4:15 I Current Method No/se Thres. I_ttttt_ 10.0 Quant Thres. _ 0.2 Min. W1dtll _ 3 Mull. Wlclth _ 10 Base. Width _ 150 RT Win. (sees) _ 20 smoothl 11 1 s0008807-012 7 012 S00088 CONTROL_BLANK 1 No Comment Thu, NOV g, 2000 9:08 PM 28'7 8:59 in 1 period 1130- 1:8:59 MRM. 871 scans 90- 427.0>407.0 !JO" Area 0 He_ht o Stab Time End Time 0:00.0 0:00.0 70- 97 60- 50- ] 69 164 Jntensi_ : "5 ps 36/7 438 4.80 / Retenlion Time Inlecjralion Type I_ I"'IM_ 0:00.0 _0- r_ll_=i] 11301 101 :35 .... 201 E.:I0 l _01 401 4:45 6:19 501 7:54 _,,_an Tin',e F Page 99 Northwest Bioanalytical Figure 11. Human Serum Blank for PFOSAA Study No. NWBS00-088 Report No. NWBRO 1-001 IPFOSAA Internal Standard: THPFOS Use Area Absolute Retention 1line ExpeCted RT 5;56 I Current NOiSe Thres. [ _ Method 4.0 Quant Thins. _ 1.5 MIn. Width _ 3 Mull. Wldlh 1131 13 Base. Wid#l _ RT Win. (SacS) _ SmOOth I 150 20 II 1 S0008807-012 7 012 S00088 CONTROL_BLANK 1 NO Comment Thu. NOVg. 2000 9:08 PM 8:59 in 1 _ I: 8:5g MRM. 571 scans 100] / 901 int_si_ : t 62 cps 379 A5r8e4a.1->419.11020 HeicJhi 129 End Time 6:06 7_1_I 60 ] Retention Time 5:58 Ime(:dmtion Type A - BB _ It'1,1,1'.'1_1_1 []1-i-i-i_ r2Oot I 519 , 101 I :3._ 241 31 =, [ 201 301 , 4.01 ,J 501 , $_, 3:10 ,'1:45 6:1'9 7:_4 Tfmel;-: ITHPFOS use aS Internal Standard Expected RT 4:15 I Cu_f No_a Thres. [ 10_ Method 10.0 Quant Thins. _ Min.Width _ Mull Width _ Base. Wloti1 _ RT Win. (secs) _ Smooth I 0.2 3 10 150 20 1I 1 0008807-012 7 012 $00088 CONTROLBIANK Thu. NOv g, 2000 9:08 PM 8:59 in 1 pedod 100 I NO Comment 287 intensittJ : 25 cps 1:B:59 MRM. 571 scans 90 427.0->4070 Area 0 Height 0 ;taft Time End Time -Retention Time Inteqmtion Type _0 70 97 367 433 480 60 0:00,0 50 0:00.0 3 69 164 ooo11(I 0:00.0 _0" I 1o. 0 .... fl ' ,1 I 01 Zl_lI _,0t 401 501 Seat, f--.- 1::35 Z.:IO 4:45 6:19 7:_4 Tirc,_t ; Page 100 Northwest Bioanalytical Study No. NWB$00-088 Report No. NWBR01-001 Figure 12. Human Serum Blank for PFOSA [PFOSA Inlemal Standard: THPFOS Use Area AbsokJle Relention T.'me Expecmd RT 5:35 I Current Method Noise Thres. [ 3.0| 3.0 Ouant Three. _ Mbl, Width _ Mull. WIdlh _ Base, W*dth _ RT Win, (secs) _ s,noo_ 0.3 5 10 150 20 1[ t s0008807-012 ? 012 S00088 CONTROL_BlANK 1 No Comment rhu. Nov 9, 2000 9:08 PM 362 8:59in 1 period 100. 1:8:59 MRM, 571 scans c'J'0' 498.0->78.0 Area 3039 ,Hexjht 202 Start Time 3070- 60- 5:11 50" Inte(jration Width Retention Time ,Integration Type 0:38.8 5:42 A- W 40-0. 32 7t 145 2 !2I33 Jntensib.J : 209 Cps 495 [ I01 201 301 401 501 Se.aw, I :35 3:10 4:45 6:19 7:54 Timely< (THPFOS use as Internal Standard Expected RT 4:15 Cucrent Method I Noise Thres. [_ 10.0 Quanl Thins. _ 0.2 Mhl. Wide1 _ 3 Mult, Width _ 10 Base. W'_dthj 1...5.50..] 150 RT WI_. (secs) _ 20 smooIth 11 1 s0008807-O12 7 012 S00088 CONTROLBLANK 1 NOCommenl Thu, Nov 9, 2000 9:08 PM 287 8:5g in I penod [00 1:8:59 MRM, 571 scans 90 427.0->407.0 BO Area 0 Hecjnl 0 ;tart Time End Time 0:00,0 0:00.0 70 97 60 5O 0 69 164 intensity : 25 CpS 36.7 438 480 Relentioct Time Intejration Type 0:0O.0 ,_0 I0" 0 ,, 1:35 _.:10 4:4_, 6:19 7:54 Tin',e ..'_-- Page 101 Northwest Bioanalytical Figure 13. Human Serum Blank for M556 Study No. NWBS00-088 Report No. NWBR01-00 [ p,ts5,3 Internal Standard: THPFOS Use Area A0_lule Reten_ Time Expected RT 5:25 I Cu_ni I Noise Thres. [_ Method 0.4 Quant Thres. _ Min. Width I 3[ MulL _th 1101 0.1 3 10 Base. _dth _ RT Wln. (seca) _ Smooth I 1 20 II 1 s0008807-012 7 0t2 500088 CONTROL_BLANK 1 NOComment Thu, Nov 9, 2000 9:08 PM 8:59 in 1 period I: 8:59 MRM. 571 scans 550.0->4_.0 Area 155 H_ht 55 S=n Time End Time 5:20 5:27 fRneI_tet_ntion T_imdteh 05::2057.6 00 c'JO '_" 70' 60" _0J 44 344 250 29_ _bmsit 9 : 57 cps ldl 201 301 4dl 5_t Saair,,-,,-- 1:35 3:10 ,1:45 6:IS 7:54 Timet:_ ITHPFOS use as Int_al $mn_=_ _p_ RT 4:15 I Noise _re=. i Current _0_ Method 10.0 Quan! _. _ _.__ Mull. _dth _ Base. _th _ RT Win. {secs) _ Smooth I 0.2 3 10 150 20 II 1 s_08807_12 7 012 $0_88 CO_ROL B_NK 1 No Comment Thu. NOV 9. 2000 9:0B PM 287 8:59 In I period 100 t: 8:59M_. 571 scans 90 427.0->_7.0 _10 Area 0 70 97 tnten=i_ : 25 cps . 36/ 7 438480 $E1n=d_ TTimimee Retention Time Inter,ration Type 00::0_0.0.0 50 69 164 0:00.0 _0 HIee,lh$i1*Ho_l_ r__f_=] 6zoo_oI ,_t , I01 _01 :35 _ :10 - i 1i , 1 = IL, 30| 40I _Ol 4:45 6 :19 7 :$4 Scan Tin',e ..F Page 102 Northwest Bi.oatmlytical Figure 14. Human Serum Blank for [V!570 Study No. NWBS00-088 Report No. NWBR01-001 [MSr0 Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5:38 I Currant Memod NO_reives[. 3.o_ a.o Quant Thins. _ Mln. VVialh _ Mull. Width _ Base, Width _ RT Win. (secs) _ Smooth I 0.$ 5 15 150 20 1I 1 s0008807,.012 7 012 S00088 CONTROLBLANK 1 No Commefll rhu, NOV g, 2000 9:08 PM 8:59 in I penod 1: 8:59MRM. 571 scans 570.O- >41 g. 1 Area H_jht 1074 144 100 :30' 70' 60- End Time In te(:jralion Width 5:55 0:18.9 40- Retention Time 5:44 .77-,0- Inte,cjraiJon Type A - BB 191 Start Time 5:37 :SO- intcctsit 9 : l_[l ps 364 4 _! ,I ]5 101 I :3,_ .201 3:10 301 4:45 401 6:19 501 7:=,,4 S,:;.,trr,.rTimel, ,, ITHPFOS I mCurrent Method NO_e Three. i IO.0_ 10.0 use as Internal StandaKl Ouant Thres. _ 0.2 I Mkt. Width _ 3 MuIL VV'idth _ 10 Expected RT 4:15 Base Width __._.1_50._ 150 RT Win, (sen=) _ 20 SmooI th _ 1 sO008807-O12 7 012 SOOOB8 CONTROLBLANK t ThU, NOV9. 2000 9:08 PM 5:59 in I !oenod 100 NO Comment 287 inten_bj : 25 p* 1:8:59 MRM, 571 scans 427.0->407.0 8121 Area O 70 97 367 438 480 ,_,, o to I Star Time 0:00.0 50 _wo_oojj:11 EndTime Retention Time Inteqmtion Type 0:000 0 69 164 0:000 _,O ' J ,, olh l0 tO I 201 [ _;131 4131 5U I Sear, :35 _.:10 .4:4_ 6:19 7:54. T irne..r...'-. Page 103 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR.0 [-001 Figure 15. Human Serum Blank with Internal Standard (QC0) for PFOS IPFOS I i Cun'en I MeUlod NO_e Thres. [ S.O_ 5.0 internal Slandard: THPFO-_ USe Area Absolute Retlmtlon Time Expected RT 4:54 Quanl Titres. __ MIn. Wldftl 131 Mull. Width _ Base. 'MOth _ RT W_fl.(secB) _ smootth 0.2 3 12 150 20 11 1 s0008807-001 7 001 S00088 CCO I No Comment rhu, Nov g, 2000 7:00 PM 8:59 in 1 period 100 1:6:59 MRM, 571 scans 499.0->60.0 813 70 Area 39395 He_nt 2605 60 Start Time End T_me 4:34 50 5:32 Intecd_tion Wldtll Retenuon Time Intacj_llon Type 0:57.7 40, 4:50 30 A - 8V l,_l_,l"*iI__-l'_:I20I.r_ I0, 0 "i - , " t ' I01 201 1:3._ 3:10 intensity : 2606 cps 307 L_ ," , , 301 4:4:5 ", "-"'_'* 401 6:1'9 [ -_iOl 7.'_4 ,'" S,_i', r,r-Timel_ ITHPFOS use as Internal Standard Expected RT 4:15 I iCurrent Method NOiSe Thins. F I0.0] m.0 Qu,_t Thins. _._ Min. Wk3m 131 MulL Width 1101 Base. Wtdth _ Rr_n. (sees) _ Smooth t 11 0.2 3 10 150 Zo I s0008807-001 7 001 SO0006 QCO I No Comment Thu. NOv 9, 2000 7:00 PM 281 6:59 in I period 100' 1:8:50 MRM. 571 scans ojQ. 427.0->407.0 _JO" Area 273196 He_ht Statl Time End Time 35433 4:12 4:48 IntecFaUon W'_th Retention Time 0:33.1 4:26 Intonation Type A - BB [._1_,1'_1_!__1ti_ 6O50" 40" 30- _o- 10- . k., I :35 _:10 4:4_ int_sib_l : 3_434 c:ps t--- 6:19 7:._4 TimeI.: Page 104 Northwest Bioanalytical i Figure 16. Human Serum Blank with Internal Standard Study No. NWBS00-088 Report No. NWBR01-00 I (QC0) for PFOA Cun'e_ MetPl_ Intema_ Standa;(l:THpFOS Use Area Absetule RetewmonTime Exoected RT 4;27 1P+PU+ QuaintThes. Min,WiGU1 MtaL Wk:lth Base. Wk_lh RT win. (sees) Smoom I Noise Thres. _ sO008807-O01 7 001 _CI088 QC0 1 Thu, NOv 9. 2000 7;00 PM 8:59in I period IOQ 1: 8:59MRM. 571 sc3wts 413.0-_ 18g.0 80 Arel 3134 Hq.gr_ 227 Start Time EncITime tmegfauon Wiam Retention Time Integration Type 70 60 4:12 4:45 ,_0 0:33.; 4:29 A- BV 30 NOCommenl 0.9 3 9 150 20 1 1.0 2S5 _ntensitq : 241 cps i I 380 423 486 Q , i, , , " i , "1' , 1, 101 201 301 401 -_01 $_m p.... 1:35 3:10 '_ :'{'5 E,:I9 7::54 Time_;_ LTHPFOS use as Internal Stano'afd Expected RT 4:15 I _Current Method Noise Three. 110.01 10.0 Quan[ Thfes._ My,_.,',e_, Mull, Width _ Base, WkttB I.__._.. _ RT Win. (=e_) _ Smooth I 1I 0.2 3 10 150 20 1 S0008807-001 7 001 S000B80C0 1 No Commetll Thu, NOv 0, 2000 7:00 PM 28_ 8:59 in 1 pedod I O0 1:8:59 MRM. 571 scans 427.0->407.0 70 Area 273106 Height 35433 Staa Tlme End _me In tecJrationWidth 60' 4:12 _0" 4:48 0:33.1 40. Relention T'tme 4:2iB _0' !nteqraUon Type A - fiB I0. o, 1_I * :61 '" ._0' t I :3.'_ 3:10 4:4_; intensittJ : 35434 cps ,wJ I 6:1"9 5o I 7:_4 $c_n Time ,.r_ Page 105 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWB R01-001 Figure 17. Human Serum Blank with Internal Standard (QC0) for PFHS JPF:HS Current Method J Noise Thres. _ 3.0 Use Area Min. Width 4 Absolute Retentmn Time Mull _ 12 Ex_.cted RT 3:37 Ba_e. Width 150 RT Win. {secs) 20 Interna_ $lanaatd: THPFOS QuanlS"mrhoreosm. _ 0.51 s{llJO8807-OO! 7 001 SOOOS8QC0 1 NOComment Thu, NOv 9, 2000 7:Q0PM 243 8:59 in I period ,00 1: &SgMRM. 57; =can= 399.0->80.0 Area 1769 Heitjhl 193 Time End Time IntecJrationW'_th Retention Time 80' 70' 60" 3:39 50" 3:59 0_19.8 d_" 3:50 7,0. int_msi_ : 200 ps 412 o , i , Jt I 01 201 1 :_,5 5:10 J ," [ I i , 30 t 401 501 $_n tr'- 4:45 6:19 7:54 Time[i_: irHP_os use as Internal Standard Expected RT 4:15 I Noise l_res. Current Ilo.o7 Method lO.O Quant Thres. __ M_. Width _ Mull Width _ Base. Width _ RT Win, (sacs) _ SmoothJ 0.2 3 10 150 20 1I ! 80008807-001 7 001 500088 QC0 1 NO Comment Thu, Nov 9, 2000 7:Q0 PM 8:59 in I period 100 1: 8:5g MRM, 571 scans 427.0->407.0 Area 273196 He,hi Start Time End Time 35433 4:12 4:48 Inteqmgon Wiclth Reten_on Time 0:33.1 4:28 Intecjration Type A - BB It'1_,1"'1"1__1] 80 70 60 40 2o. 10 0 It_l 2t3! 1:35 ]:10 inUmsit U : 35434 cps 281 d_ 301 4:45 .... 401 6:19 501 7;54 Sc._n Tim_. Page 106 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Figure 18. Human Serum Blank with Internal Standard (QC0) for PFOSAA [PFOSAA Internal SlandaKl: THPFOS Use Area Absolute Relenfion Time Expected RT 5:56 I Current Method Noise Thres. I 4,0_ 4.0 Quanl Titres. _ MIO. Width _ Mull. Width _ Base. Width _ RT Win. (sees) _ Smml 1.5 3 13 150 20 _I 1 0008807-001 7 001 S00088 QC0 1 NO Comment rnu, Nov 9. 2000 7:00 PM 8:59in 1:8:59 1 period MRM, 571 scans 584.1 ->419,1 100C-'O. 30 70- intensit9:92 ps 382 / 4_7 1 429 327 513 Hei(jhl 0 Start "l_me End Time 60 - 0:00.0 50" 0:00.0 268 I 219 I RInetete<njrtaiotinon TTimyepe Inlel:dmtion V_dth Area 0 0:00.0 0:00.0 30- 49 I00 40- 171_I tllJ{ tO# 1:35 20! 3:10 I !i 301 4:4_ ' ,l.Ot 6:19 51_I 7:54 Scar, Time _F ITHPFOS use as Internal SlandaKI Expected RT 4:15 I N_se_re_.[ ICurrent Me01od lo.ol lo.o Quant Thins. _' _' 0.2 u_..w_th_ 3 Mull WIdU1 _ 10 Base. Width _ 150 RT Win. (Boca) _ smooI_ 20 II i s0008807-001 7 001 S00088 QC0 1 NO Comment Thu, NOV9, 20007:00 PM _"_l 8:59 in 1 period I00 I: 8:59 MRM. 571 scans 90 427.0>407.0 70 Area 273198 Heicjht 35433 60' Start Time End Time 4:12 50 4:48 Intonation Width Retention Time Intecjration Type 0:33.1 40' 4:26 30. A - BB tO" ! L_ o laz _, ' A36, I :35 ._.:10 4:43 inten>dbj : 3_4_4 p$ 46, '_L_, S,'_,r, 6.19 7:54, Tin,el-, Page 107 Northwest Bioanalytica[ ' Study No. NWBS00-088 Report No. NWBR.01-00 l Figure 19. Human Serum Blank with Internal Standard (QC0) for PFOSA IPFOSA Internal StanOarU: THPFC$ Use Area Absomte Retention Time Ex0ected RT 5:35 ] Nome Thres. _I Curre3n.t01 Memo3d.0 Quan! Thres. 10.3[ 0.3 Min. Width _ 5 Mult. Wtclth [10[ 10 Base. Width _ RT_. (_cs) _ Sincere I 150 20 tI I s0008807-00 t 7 001 $00088 QC0 1 Thu, Nov 9, 2000 7:00 PM No Comment 8:59intperiorJ 498.0->7B.0 Area . He_ht 0 Start Time End Time tntecjration Width 1_2 ] BO 70 0:00.0 0:000 0:00.0 , 40-[26 It 124 tB4 , i |--257 intensity : 59 op$ :361 525! II Ji I I|[_ 4t_.[44l I_, 101 .201 30t 40t 501 _ .r_"- I :7_$ _:10 4:45 6:19 7:$4 Time IT_PFOS use as Internal Standard Expected RT 4:15 t Current No_e Thfes, _ Method 10.0 Quant Thres. P------.--I_ 0.2 Mkt.V_dth [31 3 MulL Wk:l_ [10] 10 Base. Width _ RT Writ. (secs) _ Smooth I 150 20 1] 1 s0008807-001 7 0,1 _00088 QC0 1 No Comment Thu, Nov 9, 2000 7:00 PM 28! .:Sg in 1 pe_lo_ 100 1:8:59 MRM, 571 scans 90 427.Q->407.0 Area 273196 HeiJht 35433 Start Time End 13me Inte_ralJoWnklth Retention 'i3me Inm_mtion Type 4:12 4:48 0:33.1 4.:26 A" BB BO 70' (JO" 40' _a3. tO" 0 I i31 2131 _0 t 1:3_ _,:_0 4.45 intensit_ : 354:34 eps 4,:11 _:19 _01 7:$4. So.an TJn',_J .: Page 108 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Figure 20. Human Serum Blank with Internal Standard (QC0) for M556 IM556 ] Currenl Methoa Noise Thins. _ 0.4 Internal Standard: THPFOS use Area Ouant Trims. _ Min, Width _ 0.1 3 Absolute Retention T_me Muir, Wlath _ 10 Expected RT 5:25 Base. Wk:lth_ 150 RT Win, (sac=) _ S._otIh 20 11 1 0008807-001 7 001 S00088 Q_ t NO Comment l'hu. NOv 9, 2000 7:00 PM 2"_8 8:59 in I pedoa IOLI I intens|tIi : 17 eps 1: 8:59MRM, 556.0->498,0 571 scans He_Jl_l 0 oStarl Time End 13me Inte(jratlon Wldt_ Retention Time InteBmlJon Type 0:00.0 0:00.0 O:00.0 0:00.0 NEi 90 30 70 7'9 6,0 _:] 40 `30 2o lO o II 209 3_1 416 161 ' z61 1:35 `3 : I 0 ill 361 " 4oi 561 3e;,o , 4:45 6.: 19 7 :_4 Time_ ITHPFO$ use as Internal Standa_l Expected RT 4:15 I ICulrrent Method _e _res. _ 10,0 Quant Thres. P--------I_ MIn. Width 131 MulL I^Idth I I01 Base. W1:1_1..._.1_ RT W'm. {secs) _ SmOIOth 11 0.2 3 10 150 20 1 s0008807-001 7 001 B00088 QCO 1 No Comment Thu, NOV9, 2000 7:00 PM 281 8:5g in 1 period 100 1:8:59 MRM, 571 scans '90 427.0->407 0 .90 70 Area 273198 Height 35433 60 Start Time End Time 4:12 50 4:46 Inteji'ation Width 0:33.1 40 Retention Time Inte_ration Type 4:28 30 A - BB _tensity : 354,34 p$ .- t0 o 1,Jl zdl '_z,_ol 4dr 5dl s_ai--.'- I :_ ._:10 4:45 _1:19 7:_,4 Tin',el, ,: Page [09 Northwest Bioanalytica[ Study No. NWBS00-088 Report No. NWBR01-001 Figure 21. Human Serum Blank with Internal Standard (QCO) for M570 I_lsTo I Cuffent Noise Thres. F3.0_ Method 3.0 Internal Standard: THPFOS Use Area At)solute Retentiofl Time Expm:ted RT 5:38 Quant Thins. _ Mia. Wl(lth 151 Mull, Width _ Base. Wklth _ RT Win. (=ecs) _ smooIm 0.5 5 15 150 20 1[ 1 0008807-001 7 001 500088 QC0 I No Comment Thu, Nov 9. 2000 7:00 PM 3_,3 8:59in 1 pe_od IOO] 1: 8:5g MRM, 571 scans _J Area 0 H5e7_0J.0h-!>419.1 0 8it intensit_ : 71 ps 493 tntecjmtion Type REnetdenTtimolinoelnTteim(_era 1 0:00.00:00"0 $040:1,!,,[ 1,_, it_,,18_7 I01 201 I :3-_ 3:10 25|rh__,t 301 4:43 401 6:19 L 501 7:'34 So_n . TimeI?. ITHPFOS use as Internal Standard Expecte0 RT 4:15 I i Current Noise Thres. FI0.0_ Method 10.0 Quant Three. __ 0.2 Min. Wk:Ith 131 3 MUR.Width _ 10 Base. Width _ 150 RT Wln, (sac=) _ 20 smoothl I [ 0008807-001 7 QOl S00088 QC0 1 NO Commenl Thu. NovB, 2000 7:00 PM 2'81 8:59 in I pedod OO' 1: 8:5g MRM, 571 scans 90. 427.0->407.0 Area 273198 HeKJht Start "Nine En_ Ttme 35433 Inte(JratJonVVirlth Retention Time tntecj_tlon Type 4:12 4:46 0:33. I 4:26 A - BB 80' 70, 60 50" 4030- 2. 10- CI 1151 ' "261 ' _1 ! :3_ c'.:l 0 4;_._ intensit 9 : 354:34 ps 461 6:1'_ .'_OI ' aO,_t_t.=l- 7:_4 Time_ _. Page II0 Northwest Bioanaiytical Study No. NWBS00-088 Report No. NWBR01-001 Figure 22. Low Standard (3.94 ppb) for PFOS IPFOS I mCurrent Method Noise Thres. r 5_ 5.0 Inmmal Standard: THPFOS Use Area Absolum Retention _me Expected RT 4:54 Quant Thres. _ Min. Width _ Mull. WIdlh _ Base. Width _ RT Win. (sacs) _ smonm I 0.2 3 12 150 20 II I s000800T-002 7 002 500088 $ldl 1 1 No Commenl rhu. Nov9. 2000 7:11 PM 318 8:5g in I gedod [00 1: 8:5g MRM, 571 scans 90 49g.0->80.0 Area 4851 g Hei(Jht 3423 Start Time End Time Inte(jration Width Relention Time Inte(jration Type _0' 70 60 4:31 50 5:28 0:56.7" 40- 5:01 $0- A - BV tntensi_ : 3;425 Cps IO- 0 ---. - ; , -r- - T ,'_ 101 ,?.01 301 401 I :35 3:lO 4:45 6:r9 :501 7:54 Sc_r, Time :.'_ [THPFOS use as Internal Slandard Expected RT 4:15 Current Method l Noise Thres. _ 10.0 Quant Thins, _ Min. Width _ MulL Width _ Base. Wld_ _ RT Win. (lecs) _ sm_l 0.2 3 10 150 20 _1 1 s0008807-002 7 002 $00088 Stdl 1 1 No Comment Thu. Nov g, 2000 7:11 PM 8:59 in 1 petlocl 1: 8:5g MRM, 571 scans 427.0->407.0 Area 270289 He_hl tart Time End Time 38113 , InleJralion Width Retention Time ,)ntecjration Type 4:12 4:47 0:35.0 4:25 A BB N[] 100 90 eO 70 60 50 40 b'O so, 10. 0 Idl 1:35 2dl ..T:.I 0 2_30 "J _ _ol 4:45 intensity : 36114 cps ,, 4OT 6:19 , sdl 7:,54 Sc-_n Tir_e ,._- Page l l I Northwest Bioanalytica[ Study No. NWBSO0-088 Report No. NWBR.O I.-O01 Figure 23. Low Standard (1.92 ppb) for PFOA Cutmnt MeUlotl IneernalStandard: THPFOS [_-uA UseArea AbsOluteRetention T_-ie Ex0eaed RT 4:27 Qua_ Thces, ] No,,e "l'htes. _ Min.Width ]3] MtJ_.WldU1 _ 0ale. Width _ RTWln. (see.s) I 201 s,_o.I, '_ s_0880_-002 70o2 500088 S_1 1 1 Thu. Nov g. 2000 7:11 PM 8:S9 in I _mol 0O I1 8:SOMRM. 571 scans r.aO, 413.0-> 18g.0 I:_0' Aria g563 Helgtl 722 St;In Time En(:lTime Integration Wi(Ith Re_enbonTime Inle(jration Type 4:02 4:55 0:52.9 4:28 A - 08 70" q_..O" $0" 40 _0" NOCommont 0.9 1.0 3 9 150 20 1 293 10- 101 21:11 _:01 1:35 3:10 4:45 inkensibj : 734 ps 4(]I 6:19 -_01 7:54 SC._ Time! .>_ ITHPFOS use as Internal Standa_ Expectel RT 4:15 I iCurrent MeUlod Noise Thins.110.0] 10.0 Quant Ti_, _ 0.2 MIn. Width [31 3 Mull Width 1101 10 Base. W10th_ 150 RTw_.=ec_a) 20 Smooml 11 I S0008807-002 7 002 S00088 Stdl 1 1 NO Comment ! :Thu, Nov9. 2000 ?':11 PM .280 8:Sg in 1 period I 0(] 1:8:59 MRM, 571 scans 427.0->407.0 Area 270289 Hecj#It Start Time End Time 38113 Intecjtall_Olndth Retention Tlme Inee_lration T_/pe - 4:12 4:47 0:35.0 4:25 A - 08 70 60 50 40' "7-O IO- l '_ ' ,dl ' z_v ' _ol I :35 -3:IQ 4:45 inten_;it_ : 3611 4 eps ,_dl 6:19 561 7:54 s_r,.-- Tirnel.< Page 112 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Figure 24. Low Standard (1.36 ppb) for PFHS IPFHS Lnternal Standard:. THPFOS Use Area Absolute Retention Time Expected RT 3:37 I Currenl Noise Thres. _P--------d MethocI 3.0 Quart! Thros. I 0.51 0.5 Mth. W_lth 141_ 4 Muir. Width 112} !2 Base. Wfdll__ 150 RT Win. (secs) _ Smooth I 20 It 1 s0008807-002 7 002 500088 $1dl 1 1 NO Comment Thu, NOV 9, 20Q0 7: I t PM 239 8:5g in 1 per_:l 100 1:8:59 MRM, =;71 scans ,"0' 39g.0->80.0 80" 70- Area 14877 HeicJht 1486 60- , Start Time ' End Time 3:25 S0- 4:01 Intecjration Width 0:35.9 40- Retention Time 3:48 50- Intecjration T_oe A - 88 lo 101 201 1:35 3:10 301 4:4S intensibj : 1492 ops 401 6:19 S01 Sc.._r, .... 7:54 Timel_ I "rHPFOS use as Interne6 $tandart:l Expectecl RT 4:15 I Current Method Noise Thres. _ 10.0 Quant Thres. _ 0.2 Min. Width _ 3 Muir. Wtdth _ 10 Base. Width _ 150 RT Win. (sere). _ 20 SmooI th 11 1 s0008807-002 7 002 500088 Stdl I 1 No Comment ;TIlu. Nov g, 2000 7:! 1 PM 8:5g in 1 period 1:8:59 MRM. 571 scans 427.0->407.0 Area 270289 He_jh I Start Time End Time 36113 Inle(Jration Width Retention Time Integration T)tpe 4:12 4:47 0:35.0 4:25 A - 8B N[] 100 90 _JO 70 50 40 50 2o 10" o .... ICII 2.01 I :.35 5:10 intensit U : 36114 tiPS 2gO I Lr, , _.01 4_11 4:45 6:19 501 _.,c.>,t_ 7:$4 7 rr,e .,F Page 113 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-00 l Figure 25. Low Standard (1.60 ppb) for PFOSAA IP_OSAA Internal Standard: THPFO$ Use Area Absolute Retemk_rl Time Ex0acted RT 5:56 I Cutren! Method Noise Thtes. [ 4.01 4.0 Quant Thres. l----'m--''t_ 1.5 Min. Width _ 3 Mull wk:lth [ 131 13 Base. Width _ 150 RT _. (sa_) _ 20 SmooIth _I 1 s0008807-002 i IThu. Nov 9, 2000 8:59 in I period 7 002 S00088 7:11 PM Stdl 1 1 I00 1:8:59 MRM, 571 scans 584.1->419.1 80 7O Area 6584 Hel(jh! 727 Start Time End T_Tle 60 5:37 50 6:07 Inte<jration W_Oth 0:30.3 40 Retention Time 5:58 30 tntecjraton T_'pe A - BB No Comment intensit,,i : 750 ps 376 10, 101 I :35 201 3:10 301 401 4:45 6:19 501 S"c._, r--- 7:_4 Tim e[:_ irH_,_os use as Internal Standard Expected RT 4:15 I i Current Noise Thres. 110.0] Method 10.0 Quant T11ttm. _ Mth. Wldtll 131 Muir. Wk:lth 1101 Base. Width _ RT Win. (sees) _ smthl 0.2 3 10 150 20 _1 i S0008807-002 7 002 $00088 Stdl I I No Comment Thu. Nov 9, 2000 7:11 PM 280 8:59 in I period 00. 1:8:59 MRM. 571 scans 427.O->40?.0 Area 270289 He_il! $1art Time End Time 30113 :Inte,<lralton Width Retention 13me Intej_tion T_/pe 4:12 4:47 0:35.0 4:25 A - BB 90' _JO" 70- 6050" 4030- 10- o 16z _6, ' sdl I :3_ 3:10 4;4_ intensit U : 36114 ps 46, 6 ;1'_" _dl 7:._4 s_, Tiff,4 : Page 114 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Figure 26. Low Standard (1.00 ppb) for PFOSA IPFOSA I mCurrent Method Noise Thins. I_ 3.0 Internal Standard: THPFOS Use Area Absolute Relent_n Time Expected RT 5:35 Ouant Thres. _ 0.3 MIn. Width _ 5 MUlL Wld_ _ 10 Base. WlOth_ " 150 RT Win. (seca) _ 20 smoothl i I i s0008807-002 7 002 S00088 Sial1 1 I No Comment Thu. NOV 9, 2000 7:t I PM 361 8:59 in t period 1130' 1: 8:59MRM, 57t scans -cd0' 498.0->78,0 Area 23812 HeKjhl 2540 Start Time , End Time , In le_Farion Width Retention Time Intecjralion Type I+t,H"'IMI_ 80" 70, 5:18 5:55 0:39.7 5:41 A - BB 6050" 4030; _-]_=J 2010- k_tensRV : 2543 cp$ 101 2OI 301 4=31 301 Sc-_n I :_5 3:10 4:45 6:19 7:54 Time_ ITHPFOS use as tnte#nal $landa_ Expected RT 4:15 I _re i Current Method | 10.0_ 10.0 Quant Thins. _ Mm. Wldm I MulL Width _ Base. _::lth _ RT Win. (sees) _ Smoom I 0.2 3J 3 10 150 20 11 1 s0008807-002 7 002 S00088 Stdl I 1 rhu, Novg. 2000 7:11 PM 8:50 in t period I: 8:59 MRM, 571 scans 427.0->407.0 Area 270289 Hei(Jht 38113 Start Time End Time Inte(jta lion width Retentio_ Time Intecjmtion Type 1+14,1"IvM, l_ 4:12 4:47 0:35.0 4:25 A * 8B []1-i'i_ 10090_JO" 70- _" 50- 403;0" __oo2_ i 0! No Comment II_I 1:3_ 201 _.:I0 _0 _4'r' ' _01 4:45 intensit_ : 361 t 4 ps .... 401 6:1"_ 501 7:'_4 Sear, Timel : Page 115 Northwest Bioanaiytical Study No. NWBS00-088 Report No. NWBR01-001 Figure 27. Low Standard (2.50 ppb) for t_1556 IMSScl ] Internal Standard: THPFO q Use Area Absolute Retention Time ExpecteO RT 5.42 Current Method Noise Tnres. _ Quant Thres. _ Min. VVk:lth_ Mull. Wioth _ Base. Wldm _ RT Wln. (secs) _ smooI= 0.4 0.1 3 10 150 20 11 1 S0005807-003 7 003 S00088 $t02 1 1 iThu, NOv 9. 2000 7:23 PM 8.98 in 1 penod t 00 I: 8.98 MRM. 571 scans 90 559.0->498.0 =30 Area 5991 70 Hei(Jhl 789 Start Time End Time 5.15 60 5.63 In te_mtion V_CI_ Retention Time 0.47 50 5.4.4 Inte_lra_on Type A - B9 40 I1`1+1'*t_l_ _ 3o 20. 10. NO Comment intensRy : 769 ops 345 0 _. t., , 4. u ioI :61 1.59 3.17 . L ,_ j ,= z6i 46, ' _o2 So_. 4.74 6.32 7.90 Tim_ ITHPFOS use as Internal Standard Exaected RT 4.25 I _Current Me(hod Noise Thins. 110.01 19.0 Quant Thres. _ Min. V_lth _ Mull. Width _ Base. Width _ RTWtn. (sec$) _ smoothl 0.2 3 I0 150 20 11 I ,0008807-003 7 003 S00088 $td2 1 1 NO Comment rhu, NOV9. 2000 7:23 PM 280 8.98 _11 period 0O 1: 9.9B MRM, 571 scans 90 427.0->407,9 ;a0 Alea 272919 70 Heiqht 35852 ;_lrt Time 4.19 60 End Time 4.77 Inlec_raion Width 0.58 _0 Retention Time 4.41 Integration Type A - BB 40 It'1_,1'_'1_ _ zo fntensft_ : 3,_53"3 ops tO, o J. 161 261 ml 461 ' _6, 's.... Page 116 Northwest Bioanalytical Figure 28. Low Standard Study No. NWBS00-088 Report No. NWBR01-001 (1.00 ppb) for M570 [PA570 j Internal Slandard: THPFOS Use Area Absolute Relenbon Time Expected RT 5;38 _Currenl Memod Noise Thres. 13.01 30 Quanl Three, _ Min. Wktth I 0.5 5l 5 Mull Width 1151 15 Base wldm _ RT Win. (secs) _ Smooth I 150 20 1I l s0008807-002 7 002 S00088 SIal I 1 NO Comment TllU, NOv 9, 2000 7:11 PM 363 8:59 in 1 0ertod 00 1:8:59 MRM, 571 scans 90 570.0->419.1 Area 9166 Hei(Jht Staa Time End Time 1236 Intecjration Width Retention Time Intecjralion Type 5:28 5:58 0:27.4 5:43 A - BB N[] _0. "tO 60 50. 40.T-O" 510- intensity : 124_ _ps 101 I :32 201 3:10 301 401 ,1:45 6:19 501 7:54 S ",r-i.t.im. Timel $ IY_'PFOS use as Internal Standard Expected RT 4:15 I Curre_l Method No__s,e'es1.1o.ol lO.0 Quanl Three. P--------I_ 0.2 Min. Width _ 3 Mull. Width _ 10 Base. Width _ 150 RT Win. (sees) _ 20 smootIh 1 I I s0008807-002 7 002 S00088 S_I 1 1 Thu, NOV9, 2000 7:11 PM 8:59 in 1 period 1:8:59 MRM. 571 scans 4 100] 90 427.0->407.0 Area 270289 Height Start Time Ena Time 381 t3 lnte,qr,ation Width Retenlion Time lnteclration Type B0 70 4:12 4:47 0:35.0 4:25 A - BB _0 50 4,0 II 30 J 1,1'I+1"'I__Ii_-I=_1zo 10 c NOCommenl -->80 d ?. tB, :z6, _oT 1:35 _.:10 4;4_ intensity : SSI 14 ,._pS _dl 561 s_,..r-- 6;19 7:54 Tin',+i _. Page 117 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Figure 29. High Standard (414 ppb) for PFOS IPFOS I Cun'en t Method Noise Thres. [ 5.o_ 5.0 Internal Standard: THPFOS Use Area Absokule Retention Time Expected RT 4:54 Ouant Thres. __ 0,2 Min. Width 131 3 Muir., WIoth _ Base. WidU1_ RT Wln, (secs) _ Smooth I 12 150 20 1I 0008807-010 7 010 500088 $109 1 1 NO Comment 1"hu,NOV 9. 2000 8:45 PM 318 8:SBin 1 pedod I00 1:8:59 MRM. 571 scans 499.0->80.0 80 70 Area 345341'5 He, tit 285223 60 Start Time 4:22 50 End Time 8:04 lnte(j ration Width 1:42 40 Retention Time 5:01 Inte(ji-ation Type A - BV intensitq : 285227 cos 10. o 161' 2di "3l oi' ' _1 s6t s_,._ I :35 5:10 4:_5 6:19 7:54 Timei_ irHPFOS use as Internal Standard Expected RT 4:15 I Current NOise Threi. _ Method 10.0 Quant Thins. _ Min. Width ] Mull Width I Base. Width _ RT Win. (secs) _ $_Oth I 0.2 31 3 101 10 150 20 1J 1 S0008807-010 7 010 S00088 Stab I I NO Comment Thu. NOV 9. 2000 8:45 PM 8:59 in I period 00, I: 8:59 MRM. 571 scans 90 427.0->407,0 _0, 70. Area 225323 He_ht 28708 60" Start l_me End Time 4:12 50' 4:48 Int_lJon Wid_ Retsnllon Time Inle<dratlon Type 0:34.0 40- 4:28 30- A - B8 2_11 intens'it_ : 2_710 cps 10- o _6J ,'dl' _61 ' 4dr s61 s-_i-n--- 1:35 _:I0 ,I. :4.._ 6:19 7:34 Tin',eI: < Page 118 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-00 [ Figure 30. High Standard (481 ppb) for PFOA I_'_UA C_rent MeU1od I Noise Thins. I_ 1.0 Use Area Mitt. WkJth 3 AOso6t_eRet(zfllionTime Mu_. Wio_l 9 Ex_eaed RT 4:27 Base. Wk_rl 150 RT win, (sees) 20 Intem_ St_ClaKl: THPFOS Qua_ STmhroeoem. _ 0,91 soo088o7-0t0 7 01o 500088 S_ ! I No Commm Thu. NOV9, 2000 8:4'; PM *I: 8:59MRM, STI _ Area 1553455 Ht, gi_ 145923 Start Time 3:$5 E_ r_e 4:50 2_3 i1 50"t Retenzion Time Integrabon Tyge 4:28 _. A RV intensity : 145935 cpS O! ..... !01 1:3:_; " ,'2 ..... 201 301 401 3:10 4:45 6:19 501 :-_;an 7:54 T me!_ ITHPFOS use as Internal Stan0aKI Expected RT 4:15 Current MethOd ] Noise Thins. [_ 10.0 Quant Thres. _ 0.2 MIn. Wldm _ 3 Mull Wl_th _ 10 Base. Width _ 150 RT Win. (sees) _ 20 SmooI th I I I S0008807,'010 7 010 $00088 Sto"9 1 1 rhu, Nov 9. 2000 8:45 PM 8:59 in I Deriod i00 h 8:59 MRM. 571 scans 427.0->407 0 Area 225323 He_t_t 28708 Start T_le End T_ma Inteqtation ta_<ltll Retention Time Inte(jr'Jtion T_/pe If l,l,l"'l_t_l _0 70 E,0 4:12 ._0" 4:48 0:34.0 40' 4:26 _,0' A - BEI 20" I'_i-1-_ I0, o NOConrwnenl 281 inteesit U : 28710 cp_ t,51 I :3_ r- 1 , zrjl ' 3oI ,;61 5& 3:1 r'J 4:45 6:19 7:_4 _,_, Tirne _'_. Page I19 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Figure 31. High Standard (523 ppb) tbr PFHS IPFHS Internal Slanctar(l: THPFO$ Use Area Absolute REHenhon Time F.xDecte(I RT 3:37 Cun'en! Meli'lod '1 No_se Thins. _ Quanl Thres. _ Min. W'KIth 141 Mull _,Mdth 1121 Base. Width _ RT _In. (secs) _ SmooIth I I 3.0 0.5 4 12 150 20 1 S0008807-010 7 010 S00088 $1dg I I Thu, NOv 9, 2000 8:45 PM 8:59 in I period ]013 I: 8:59 MRM. 571 scans 90 399.0->80.0 Area 287g0g0 He_dht Sta_ Time End T'_ne 274134 Int_. ration Width Retention Time tnteqnatJon TyPe 3:20 4:46 1:25 3:48 A BV 80 70' 60, 50. 40/ r.T..0" . H'I4,I'v,IMI_ _111_ zo10- o NO Comment 24f intensity : 274143 cpS 161 1:35 26T 3:10 im , z6t 4at 4:45 6:19 5_1 7:54 s_, T_ne[:i" IrHPFOS use as Intema_ S_r_,rd Expected R'I" 4:11_ I Current Method Noise Thres. I 10.0 J 18.0 Quant Thres. _ 0.2 Min. Width 13[ 3 Mull. W_Ith _ 10 _]aee. vv'Rfm_._ 150 RTW_(s. ee_s) 20 Smooth I II I s0008807-010 7 010 $OOO88 Stag I 1 No Comment Thu. NOv 9, 2000 8:45 PM 281 8:5g in 1 perJoa 100" 1: 8:5g MRM, 871 scans 90. 427.0->407,0 Area 225323 He_ht 28708 SPa_ Time En(_ Time In !e_ratJon Width Retention Time Intecj_tion Type 8CI. 70. 4:12 4:46 0:34.0 4:26 A 8B .. 6050- 40,._O- intenstt_t : 28710 cps 0 161 2dl ' Z01 4dl _dl S_nr-- I :.35 5:10 4:4_ 6:1'9 7:54. Time] .: Page 120 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-00 l Figure 32. High Standard (501 ppb) for PFOSAA Currenl Method {PFOSAAISntIaenmdaalrO: THPFOS I Noise Thres. _ 4.0 Quanl l"hms. J 1.5] 1.5 Use Area AbsokJte RelentJon Time Min. W_th _ 3 MulL Width _ 13 Expected RT 5:58 Base. W_th _._ 150 RT Win. (secs) _ 20 Smoom[ I I s0008807-010 7 010 $00088 Std9 1 1 No Comment The. Nov 9, 2000 8:45 PM 8:59 in 1 period " 1: B:Sg MRM, 571 tJcans 584.1->419.1 Area 1550445 He_/lt tan Time nd Time 174924 Inte<jratlon Width Retention Time Inte<J_UOn Type 5:29 8:52 1:23 5:58 A - BV Nm OO 90 _0' 70 F_,0. 50. 4030. 2 0. I01 201 301 1 :_,5 3 :t 0 4:45 intensity : 174951 rps 377' 401 501 Se:,r, 6 : 19 7:54 Timel_ Cun'en I Method [THPFOS _ No_se Thres. _ 10.0 use as Internal Standard Quant Thins. _ 0.2 ;.. Min. WIO_ _ 3 Mull Width _ 10 Expected RT 4:15 Base. W'K:lth_ 150 RT Win. (secs) _ 20 smooml 11 1 s0008807-0 t0 7 010 500088 Sldg 1 I No Comment Thu. NOv 9, 2000 8:45 PM 8:5g in I pedod 10Q' 2`31 1:8:59 MRM. 571 scans 90. 427.0->407.0 Area 225323 _He_Jht '28708 Start Time End "nine Inte_raUon Width Retention Time fnte<3raion T_ , _JO" 70" . 60- 4:12 50" 4:46 0:34,0 40- 4:25 A. BB ,_.0" I l_l_,l"'I_Ii__lII-i-2io-.i-i-i-i-i-i-_ 10- k_tensit 9 : 2"3710 ps t :3_ ,_.: I0 4:4_ 6:19 7:-.%4 Ti;',er_ Page 121 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-00 [ Figure 33. High Standard (500 ppb) for PFOSA fl IPFOSA Interne| Standard: THPFOS Use Area Abso_le Retention Time ExpeCll_t RT 5;35 I ICurmn! MeU1od Noise ThtH. F "l.0 ] 3.0 Ouant Three. _ a.:1 Min. W1dtff _ 5 Mull W_UI _ 10 Base. Widlh _ 150 RT Win. {sacs} _ 20 smootth II i s0008807-010 ? 010 S00088 $1d9 1 1 NOComment rhu. Nov g. 2000 8:45 PM 8:59 in I period 1: 8:5g MRM. 57t scans 498.0->78.0 Area 7778824 Height Start Time Ead T/me 882348 Inte_lration Width Retenlion Time Intejralton Type 5:12 8:3g 1:27 5:41 A - BV 10O ;3CI 70 60 .50 40, _0' intensitq : 68"2470 p$ 361 10' J m, _ , 0 16! 261 361 461 501 Sc_n I :35 5:10 4:4.5 6:19 7:54 Timel_ ITHPFOS use as Internal Standard Expected RT 4:15 I ICurrent Method Ne_ Thre_. J _.01 10.0 Quant Throe. P-----'-H_ 0.2 MIn. v_ctm 131 3 MulL W'K:IIh1101 10 Base. Width _ 150 RT W_. (sacs) _ 20 Smaou_l 11 I S0008807-010 7 010 S00088 SMg 1 I NO Comment Thu. Nov 9. 2000 8:45 PM 281 8:59 in 1 pedod I O0 1:8:59 MRM. 571 scans 90 427.o->4o7'.o _0 70. Area 225323 Heicjl_t 28708 60. Start "nine End Time 4:12 50' 4:48 lnta<jrat_on Widffl Retention Time Inte<_ration Type 0:34.0 40' 4:28 30" A 8B intensitQ : 28710 cps 10- o ,61 :61 ' zgl ' .5_ ' 56, so_ir.,-.,- 1:35 _:10 4:45 6:1"!* 7:54 T ir.',@l,. Page 122 Northwest Bioanaiytica[ Study No. NWBS00-088 Report No. NWBR0 [-001 Figure 34. High Standard (500 ppb) for M556 IM556 Inlema! Standard: THPFO$ Use Area AbsokJte Reterltlon Time Expected RT 5:25 I Current i No_se Thins. [ _ Method 0.4 Ouanl Thins: _ MIn. Width _ Mult. Width L_J01 Base. WIdU1_ RT w_. {sees) _ SmoOthf 1] 0.1 3 10 B 150 Zo I 50008807-010 7 010 500088 Std9 1 I No Comment Thu. NOVg. 2000 6:45 PM 345 8:59 in I period I O0 I: 6:59 MRM, 571 scans cjQ 558.0->498.0 80 7O Area 964595 Hek:Jht 111295 60' Start Time End Time 4:55 50 6:04 Int_ji'afJon V_l_ Retention Time Inte_t3tJon Type 1:09 40, 5:26 _O, A. BV intensity : ! 112<36 cps to. r j! L M , o IdT N1 ' 3dl 4,_I 561 s_.,,'.,-...- I :35 3:10 4:45 6:t9 7:$4 rim,q,_ ITHPFOB use as tntemat Standard Expected RT 4:15 Current MeUlod I No_e'_,,e__ _oo Quant ThroB. _ 0.2 Min. Wk:lB1_ 3 Mull Width _ 10 Base. Width _ 150 RTWm. (secs) _ s,.oo_I 26 11 1 ;0008607-010 7 010 B00086 $td9 1 1 NO Comment Thu. NOv g, 2000 8:45 PM 281 8:5g in I period 00 1: 8:5Q MRM, 571 scans 90 427.0o_4Q7.0 Area 225323 HeKJht Start Time _:ncl Time 26708 Integration Width Retention Time intecj_tion Type 4:12 4:48 0:34.0 4:28 A - 6B _' 70' 60' 50, 40. .,_0" tO- _ntensit_ : 28710 cps t :35 .T:,I 0 4:4_ 6:19 7:$4 Tin',e -.['_- Page 123 1,11, Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Figure 35. High Standard (500 ppb) for M570 I.ST0 Internal Stendard: THPFO$ Use Area AbsOlule Retention Time Expected RT 5:38 I Cuffent Method N_se Thres. _ 3.0 _ 3.0 Quant Thres. __ Min. _th _ Mull. Wklth _ Base. Width _ RT Win. (sec=) _ Smoothl 0.5 5 15 150 20 It I ;0008807-010 7 010 $00088 Bid9 1 I Thu. Nov 9,, 2000 0:4.5 PM 8:5g in i period 00 1: 8:5g MRM. 571 scans 90 570.0-_'419.1 80 70 Area 2494791 He, hi 303847 Start Time End Time 5:21 50 5:46 Inte,qr,ation Width 1:24 40 Retention Time Integration Type 5:43 30 A - BV NO Comment i_tensit_ : 30T_5 pS 363 10 t .%..m o ,I :6351 _3:I10 34:o45h .6:_19oI _7:o54, rir. :., ._ ITHPFO $ use as Internal Standard Expected RT 4:15 "j Noise Thres. _I Curlure.unt IMorn1e0d.0 Quant Thins. _ M_. Wldth _ Mull W'_lth _ Base. Wldm _ RT _. (secs) _ Smooth I 0.2 3 10 150 20 iI 1 =0008807-010 7 010 $00085 Bid91 I NOComment Thu. Nov9. 2000 5:45 PM 2gt 5:5o_.', I period _00 1:8:59 MRM. 571 scans 90 427.O->407.0 _O 70 Area 225323 Height 28708 60 Staa Time End Time 4:12 _0 4.:46 inte_dration Width 0:34.0 40 Retention Time Integration Type 4:25 50 A BB intensity : _3710 ps r , o ' ,6z ' :_I ' 50, ' _, _6, _._ I :._5 3:10 '.1.:45 6:19 7:54 Tin',_ -: Page 124