Document qo8EDOvNKyp5490QLXRXvnvG

. iNorthwest Bioanalytical Study No. NWBS00-08S Report No. NWBRO1-001 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 APPP Y: Rodgt chnical Director DATE: // - 3 - 0 / Page 1 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 QUALITY ASSURANCE STATEMENT LABORATORY: Northwest Bioanalytical (NWB) A Division of NWT Ine. 1121 East 3900 South Salt Lake City, UT 84124 SPONSOR: 3M Company Corporate Occupational Medicine, Medical Department 220-3W-05 St. Paul, MN 55144 COMPOUND(S): PFOS and Related Compounds NWB STUDY NUMBER: NWBS00-088 SPONSOR STUDY NUMBER: 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 Bioanalytical conducts all studies within the guidelines of the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58), the OECD Principles of Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety of Drugs (Ordinance No. 21, PAB Notification No. 424.) The following inspections were performed by the NWB QAU per SOP. Inspection and Reporting Statement. Date o f Inspection Phase o f Study Date Report Sent to Date Report Sent to NWB Project Manager NW B 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 2ndReport Draft/Raw Data Final Report 25 Sep 2000 16 Oct 2000 14 Nov 2000 25 Oct 2001 27 Nov 2001 03 Dec 2001 29 Sep 2000 31 Oct 2000 30 Nov 2000 31 Oct 2001 30 Nov 2001 31 Dec 2001 "Reports to NWB Management are issued monthly. As can reasonably be established, the methods and procedures described and the results incorporated into this final report accurately reflect the raw data. NWB Quality Assurance Compliance Auditor Date Page 2 Northwest Bioanulytieal Study No. NVVS00-088 Report No. NVVBRO1-001 COMPLIANCE STATEMENT The clinical study described in this report is not included within the definition o f a GLP regulated nonclinical study. However, to the best o f our knowledge, this project was conducted in accordance with the guidelines o f the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58) and according to the methods and procedures described within this report. In addition, the study followed the guidelines o f the OECD Principles o f Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety o f Drugs (Ordinance No. 21, PAB Notification No. 424.) Any known incidents that may have affected the quality or integrity o f the project or reported data is included in this report. This report represents an accurate record o f the raw data. Connie O. Sakashita, B.S. NWB Project Manager NWB Technical Director //-! Date Date Page 3 Northwest Bioanalytieul TABLE OF CONTENTS Study No. NWBSOO-088 Report No. NWBRO1-001 SIGNATURE P A G E ................................................................................................................................... 1 QUALITY ASSURANCE STATEM ENT..............................................................................................2 COMPLIANCE STATEM ENT.................................................................................................................3 TABLE OF CO NTEN TS............................................................................................................................4 LIST OF TA B LES.......................................................................................................................................4 LIST OF FIG U R E S.............................. 5 1. IN TR O D U C TIO N .................................................. 8 2. M ETH O D O LO G Y .............................................................................................................................9 3. SAMPLE A N A LY SIS.......................................................................................................................12 4. RESULTS AND DISCUSSION.....................................................................................................13 5. R EFE R EN C ES..................................................................................................................................17 6. DATA R ETEN TIO N ....................................................................................................................... 17 LIST OF TABLES Table 1. Calibration Curve Summary for PF O S .................................................................................. 18 Table 2. Calibration Curve Summary for P F O A ................................................................................. 19 Table 3. Calibration Curve Summary for P F H S ..................................................................................20 Table 4. Calibration Curve Summary for PFO SA A ........................................................................... 21 Table 5. Calibration Curve Summary for PFO SA ............................ 22 Table 6. Calibration Curve Summary for M 556..................................................................................23 Table 7. Calibration Curve Summary for M 570..................................................................................24 Table 8. Back-Calculated Concentrations o f Calibration Standards for P F O S .............................25 Page 4 Northwest Biuanalytical Study No. NWBS00-088 Report No. NW BR0I-00I Table 9. Back-Calculated Concentrations o f Calibration Standards for PFOA..............................27 Table 10. Back-Calculated Concentrations o f Calibration Standards for PF H S ............ :.............. 29 Table 11. Back-Calculated Concentrations o f Calibration Standards for PFOSAA..............31 Table 12. Back-Calculated Concentrations o f Calibration Standards for P F O S A ................33 Table 13. Back-Calculated Concentrations o f Calibration Standards for M556 ................... 35 Table 14. Back-Calculated Concentrations o f Calibration Standards for M 5 7 0 ................... 37 Table 15. Analytical QC Summary for P F O S ..................................................................................... 39 Table 16. Analytical QC Summary for PFO A ..................................................................................... 41 Table 17. Analytical QC Summary for P F H S ..................................................................................... 43 Table 18. Analytical QC Summary for PFO SA A ................................................................................45 Table 19. Analytical QC Summary for PFOSA................................................................................... 47 Table 20. Analytical QC Summary for M556 ..................................................................................... 49 Table 21. Analytical QC Summary forM 570 .................................................................................... 51 Table 22. Study Sample Concentrations.............................................................................................. 53 Table 23. Repeat Analysis Table for PF O S....................................................................... 92 Table 24. Repeat Analysis Table for PF H S ........................................................................................ 92 LIST OF FIGURES Figure 1. Representative Calibration Curve for P F O S ......................................................................93 Figure 2. Representative Calibration Curve for PFO A ..................................................................... 93 Figure 3. Representative Calibration Curve for P F H S ..................................................................... 94 Figure 4. Representative Calibration Curve for PFOSAA................................................................94 Figure 5. Representative Calibration Curve for P F O S A .................................................................. 95 Figure 6. Representative Calibration Curve for M 5 5 6 ......................................................................95 Page 5 Northwest Biounalytieiil Study No. NWBSOO-088 Report No. NW BR0I-00I Figure 7. Representative Calibration Curve for M 5 7 0 ............... .......................................................96 Figure 8. Human Serum Blank for PFO S............................................................................. :..............97 Figure 9. Human Serum Blank for P F O A ............................................................................................98 Figure 10. Human Serum Blank for PF H S........................................................................................... 99 Figure 11. Human Serum Blank for PF O SA A .................................................................................. 100 Figure 12. Human Serum Blank for PF O S A ......................................................................................101 Figure 13. Human Serum Blank for M 556......................................................................................... 102 Figure 14. Human Serum Blank for M 570......................................................................................... 103 Figure 15. Human Serum Blank with Internal Standard (QC0) for P F O S ............................. 104 Figure 16. Human Serum Blank with Internal Standard (QC0) for PFOA...................................105 Figure 17. Human Serum Blank with Internal Standard (QC0) for P F H S ...................................06 Figure 18. Human Serum Blank with Internal Standard (QC0) for PF O SA A ............................ 107 Figure 19. Human Serum Blank with Internal Standard (QC0) for P F O SA ............................... 108 Figure 20. Human Serum Blank with Internal Standard (QC0) for M 5 5 6 ...................................109 Figure21. Human Serum Blank with Internal Standard (QC0) fo rM 5 7 0 ................................... 110 Figure 22. Low Standard (3.94 ppb) for PFO S.................................................................................. 111 Figure 23. Low Standard (1.92 ppb) for P F O A ................................................................................. 112 Figure 24. Low Standard (1.36 ppb) for PFH S.................................................................................. 113 Figure 25. Low Standard (1.60 ppb) for PFO SA A ............................................................................114 Figure 26. Low Standard (1.00 ppb) for PFO SA ............................................................................... 115 Figure 27. Low Standard (2.50 ppb) forM 556.................................................................................. 116 Figure 28. Low Standard (1.00 ppb) forM 570.................................................................................. 117 Figure 29. High Standard (414 ppb) for PF O S.................................................................................. 118 Page 6 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Figure 30. High Standard (481 ppb) for P F O A ................................................................................ 119 Figure 31. High Standard (523 ppb) for PF H S ..................................................................... '............120 Figure 32. High Standard (501 ppb) for PFO SA A ............................................................................121 Figure 33. High Standard (500 ppb) for PF O SA ............................................................................... 122 Figure 34. High Standard (500 ppb) fo rM 5 5 6 .......................................................................... 123 Figure 35. High Standard (500 ppb) for M 570.................................................................................. 124 ( Page 7 Northwest Bioanalytieal Study No. NWBSOO-088 Report No. NVVBRO1-001 Quantitative Determination of PFOS and Related Compounds in Human Serum by LC/MS/MS Sample Analysis Report for Protocol EPI-0011 1. INTRODUCTION This report summarizes the analytical results from the quantitation o f PFOS, PFOA, PFHS, PFOSAA, PFOSA, M556, and M570 in human serum samples for 3M Company in support o f Protocol EPI-0011 [5.1]. The LC/MS/MS method for the analytes exhibited a quadratic response for the following LLOQ and ULOQ values: A n aly te 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, 220-3 W-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 o f NWB supervisory personnel involved in the completion o f 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 o f 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 o f this study and were available to study personnel in electronic and/or hard copy formats. Page 8 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Date Study Initiated: 22-Sep-2000 Date Analyses Completed: 25-Mar-2001 However, Northwest Bioanalytical conducts all studies within the guidelines o f the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58), the OECD Principles o f Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety o f Drugs (Ordinance No. 21, PAB Notification No. 424). Any changes to or deviations from the original protocol (Analytical Plan) were documented through approved protocol amendments or deviation memos and are retained within the raw data. 2. M ETHODOLOGY 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 o f Samples Received 526 73 62 iOK0> o Storage Condition (except during analysis) -20 C -20 C Page 9 Northwest Bioanalytieal Study No. NVVBSOO-088 Report No. NVVBRO1-001 Reference Material Analyte PFOS PFOA PFHS PFOSAA PFOSA M556 M570 THPFOS Lot Number Purity Expiration Date Source 193 100% 3l-Dec-2010 3M 245 100% 31-Dec-2010 3M SE-036 100% 01-Jan-2010 3M 617 53.8% 31-Dec-2010 3M 214 100% 31-Dec-2010 3M NB113047-8D 99.89% 31-Dec-2010 3M 118506-26 99.75% 31-Dec-2010 3M 59909 90% 31-Dec-2010 3M U O O 1 Storage Conditions Room temperature* Room temperature* Room temperature Room temperature Room temperature Room temperature Room temperature Stored dry The reference material purity for PFOS, PFOSA, PFHS, and PFOA was not available prior to the conduct o f this study. Therefore, the reference material purity was assumed to be 100%. 3M contracted with Centre Analytical Laboratories, Inc., in State College, Pennsylvania to determine the absolute concentration o f PFOS, 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 o f NWB solutions to Centre A nalytical Laboratories, Inc., w ere perform ed b y 3M . B ased on Centre A nalytical Laboratories' results, the concentrations o f 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 pL o f blank human Chinese plasma and 400 pL o f 50 mM ammonium acetate in Page 10 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 water (unadjusted pH -6.9) to 13 x 100 mm polypropylene tubes. After a brief vortex mixing, 10.0 jllL o f the appropriate spiking solution was added.The final calibration standard concentrations in human Chinese plasma for each analyte are listed below: A nalyte 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, 241, 385, and 481 ppb 1.36, 2.92, 10.7, 26.5, 52.6, 104, 262, 418, and 523 ppb 1.60, 3.10, 10.6, 25.6, 50.6, 101, 251, 401, and 501 ppb 1.00, 2.50, 10.0, 25.0, 50.0, 100, 250, 400, and 500 ppb 2.50, 10.0, 25.0, 50.0, 100, 250, 400, and 500 ppb 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 (designated as QCOs 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. A nalyte PFOS PFOA PFHS PFOSAA PFOSA M556 M570 Low 6.40 4.81 4.48 4.60 4.00 4.00 4.00 QC Concentrations All concentrations are expressed as ppb. M edium High High, DF = 2 126 332 335 145 385 386 156 417 418 151 401 401 150 400 400 150 400 400 150 400 400 Page 11 Northwest Bioanalytieal Study No. NWBS00-088 Report No. NWBR01-001 The internal standard (THPFOS) was added to all plasma and serum samples (except Blanks) for a final concentration o f approximately 200 ppb. The analytical method consisted o f a liquid: liquid extraction procedure followed by evaporation and reconstitution o f 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 o f the negative ions formed by TurboIonSprayTM 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 o f one. Quantitation was based upon quadratic regression analysis o f weighted (1/x2) calibration curves using area ratio vs. concentration utilizing Watson DMLIMS software (version 6.1.1.04). The samples were injected in a systematic order. 3.1. Acceptance Criteria For an analytical run to be accepted, it must have met the acceptance criteria listed below which are consistent with regulatory and industry recommendations. Calibration Curve Each run will include in duplicate calibration standards at six or more concentrations covering the lower to upper limit o f quantitation. For all analytes except PFOSA and PFOSAA, at least three-fourths o f the calibration standard's back-calculated concentrations must be within 15% ( 20% for LLOQ) o f their individual target concentrations. For PFOSA and PFOSAA, at least three-fourths o f the calibration Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBRO1-001 standard's back-calculated concentrations must be within 20% ( 25% for LLOQ) of their individual target concentrations. A calibration standard will be considered an outlier if it is greater than two times the acceptance criteria for that standard. Lower Limit o f Quantitation The back-calculated concentrations o f at least one o f the duplicate lowest points in the calibration curve must be within 25% of the target concentration for PFOSA and PFOSAA to qualify as the LLOQ and within 20% o f the target concentration to qualify as the LLOQ for ail 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 o f all analytical QCs must be within 20% o f their target concentrations ( 25% for PFOSA and PFOSAA), and no two QCs at the same concentration can be outside the limit. If study samples require dilution, a dilution QC will be analyzed in triplicate for each dilution level (except for PFOSA and PFOSAA which should not be diluted with control matrix). At least two dilution QCs at each level must be within 20% o f its target concentrations in order to accept diluted study samples at that level. The dilution QC acceptance is independent o f the undiluted analytical QC acceptance. 4, RESULTS AND DISCUSSION Serum sample results obtained using plasma curves for 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 Northwest Bioanalytical Study No. NW BS00-088 Report No. NWBR01-001 calibration curves. However, in order to obtain the lower limit o f quantitation less than 5 ppb required by the Sponsor, it was necessary to use plasma curves. Each accepted run met the acceptance criteria set for the calibration curve points, for the lower limit o f quantitation (LLOQ) and for the analytical quality control (QC) samples. Run ID 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 PFOS R esu lt Rejected Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted N /A N /A Accepted PFOA Result Rejected Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted N/A N/A Accepted PFHS R esu lt Rejected Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted N /A N /A Accepted PFOSAA Result C om m ents Rejected All analytes rejected due to sample preparation error Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted LLOQ raised for PFOS Accepted Rejected Low QCs failed for PFOSAA. N/A Accepted Accepted N/A = not analyzed Run ID 1 PFOSA R esu lt Rejected 2 Accepted 3 Accepted 4 Accepted 5 Accepted M556 Result Rejected Accepted Accepted Accepted Accepted M570 Result Rejected Accepted Accepted Accepted Accepted C om m ents All analytes rejected due to sample preparation error Page 14 Northwest Bioanalytieal Study No. NWBSQ0-088 Report No. NWBR01-001 Run ID 6 7 8 9 10 11 12 13 14 15 16 17 PFOSA R esu lt Accepted Accepted Accepted Accepted Accepted Rejected Accepted Accepted Accepted Rejected N /A Accepted M556 Result Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted N/A N/A Accepted M570 Result Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Rejected N/A Accepted Accepted C om m ents Standard curve failed for PFOSA. Reinjection o f Run 11 for PFOSAA only. Low QCs failed for M 570 Standard curve failed for PFOSA N/A = not analyzed Because o f the limited sample volume available, several samples in this study were analyzed at a dilution factor o f 2. High QC samples, diluted at a factor o f 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 PFOSAA 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 o f diluting samples with Chinese plasma when samples have PFOSA or PFOSAA concentrations less than the ULOQ. (Refer to PFOSAA results in Runs 12, 13, and 16 and PFOSA results in Runs 12, 13, and 14.) 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 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBR01-001 PFOSAA concentrations less than the ULOQ is acceptable and PFOSA and PFOSAA results from diluted samples will be reported. . The lack o f dilution data prior to analysis o f diluted o f high QC samples did not affect the quality o f the assay or integrity o f the PFOSA and PFOSAA data. 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 o f the standards were within the acceptance criteria. However, the mean o f 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 + 5% o f 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 o f 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 o f the specified acceptance criteria. For this run, when both LLOQs were deactivated, the calculated concentration ofS td 1, replicate 1, deviated 61% from target and replicate 2 was 11% from target. This indicated that Std 1, repl 1 was a true outlier and Std 1, repl 2 was originally not fitting the curve because Std 1, repl 1 was skewing the curve. When Page 16 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Std l, repl 2 is reactivated, it has a deviation o f 2% from target. Therefore, the regression will be accepted with only Std 1, repl 1 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 o f the data or integrity o f the study. 5. REFERENCES 5.1. 3M Company Protocol EPI-0011. "Identification o f Fluorochemicals in Sera o f Children in the United States." March 16, 2000. 5.2. C. Sakashita. "Quantitative Determination o f PFOS, PFOSA, PFOSAA, POAA, PFHS, M556 and M570 in Human Serum by LC/MS/MS." Assay Revalidation Report. NWB Study NWBS00-040. NWB Report NW BR00-108. January 24, 2001. 5.3. C. Sakashita. "Quantitative Determination o f PFOS, PFOSA, PFOSAA, POAA, PFHS, M556 and M570 in Human Serum by LC/MS/MS." Assay Revalidation Addendum Report. NWB Study NWBS00-040. NWB Report NW BR00-122. November 20, 2001. 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, U T 84124 per regulations and contract agreement. After submission o f the final report to the Sponsor, remaining study samples will be stored under required conditions until confirmation of Sample Disposition/Retum Authorization is received from the Sponsor. 3M Company will be notified concerning final disposition o f records at completion o f contract obligations. Page 17 Northwest Bioanalytieal Study No. NWBSOO-088 Report No. NWBROl-OOl Table 1. Calibration Curve Summary for PFOS Quadratic weighted l/x \ All concentrations are expressed as ppb. Run Date 31 -Oct-2000 01-Nov-2000 04-NOV-2000 O-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 18-NOV-2000 25-Mar-2001 Run Number 2 .> 4 5 6 7 8 9 10 11 12 13 14 17 A B C R-Squared LLOQ ULOQ -0.000005 0.027791 0.010909 0.9956 3.94 414 -0.000005 0.027419 0.006602 0.9990 3.94 414 -0.000007 0.030558 0.012087 0.9961 3.94 414 -0.000017 0.038499 0.015935 0.9953 3.94 414 -0.000011 0.035306 0.007489 0.9960 3.94 414 -0.000010 0.039703 0.010533 0.9894 3.94 414 -0.000008 0.035218 0.033595 0.9921 3.94 414 -0.000003 0.020611 0.020473 0.9912 3.94 414 -0.000007 0.029955 0.022348 0.9918 3.94 414 0.000005 0.026248 0.022175 0.9791 3.94 414 -0.000005 0.041499 0.007161 0.9829 5.17 414 -0.000003 0.036442 0.026638 0.9820 3.94 414 -0.000006 0.034381 0.024135 0.9970 3.94 414 -0.000001 0.008025 0.004145 0.9969 3.94 414 Mean S.D. %cv n -0.000006 0.030833 0.016016 0.000005 0.008779 0.008935 -83.3 28.5 55.8 14 14 14 0.9917 0.0063 0.6 14 A, B, and C are coefficients used to define the calibration curve. Page 18 Northwest Bioanalytieal Study No. NW BS00-088 Report No. NWBR0I-001 Table 2. Calibration Curve Summary for PFOA Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date 31-Oct-2000 01-Nov-2000 04-NOV-2000 O6 -N 0 V-2 OOO O8-N 0 V-2 OOO O9 -N 0 V-2 OOO lO-Nov-2000 I 2-N0V-2OOO I 3-N0V-2OOO I 4-N0V-2OOO I 5-N0V-2OOO I 6-N0V-2OOO I 8-N0V-2OOO 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 0.018750 0.001244 0.000002 0.018998 0.000186 0.000001 0.014032 0.001606 0.000000 0.014340 0.002050 -0.000001 0.014866 0.000095 -0.000002 0.014932 0.002985 0.000001 0.015103 0.009536 0.000001 0.010333 0.003017 0.000001 0.015660 0.002794 0.000008 0.013586 0.006940 0.000002 0.015457 0.005125 -0.000001 0.017638 0.007935 0.000000 0.020492 0.010441 0.000000 0.006597 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 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBRO1-001 Table 3. Calibration Curve Summary for PFHS Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 31-Oct-2000 01-Nov-2000 04-NOV-2000 06-NOV-2000 O8-N 0 V-2OOO O9 -N 0 V-2 OOO lO-Nov-2000 I 2-N0V-2OOO I 3-N0V-2OOO I 4-N0V-2OOO I 5-N0V-2OOO I 6-N0V-2OOO I 8-N0V-2OOO 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 0.031737 0.006465 -0.000010 0.032478 0.009418 -0.000008 0.031233 0.014139 -0.000015 0.034135 0.015590 -0.000015 0.035218 0.009051 -0.000011 . 0.030154 0.011565 -0.000008 0.028971 0.027667 -0.000006 0.020349 0.010603 -0.000008 0.030472 0.025208 -0.000006 0.032776 0.025491 -0.000008 0.030669 0.025839 -0.000007 0.028744 0.027330 -0.000008 0.032203 0.024941 -0.000002 0.007658 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 0.029057 0.017230 0.000003 0.007075 0.008299 -33.3 24.3 48.2 14 14 14 0.9954 0.0028 0.3 14 A, B, and C are coefficients used to define the calibration curve. Page 20 Northwest Bioanalytical Study No. NWBSOO-088 Report No. N VVBROI-001 Table 4. Calibration Curve Summary for PFOSAA Quadratic weighted l/x:. All concentrations are expressed as ppb. Run Date 31 -O ct-2000 0 1 -N ov -2 0 0 0 04-N O V -2000 06-N O V -2000 08-N O V -2000 09-N ov-2000 lO -Nov-2000 12-NOV-2000 13-NOV-2000 14-NOV-2000 15-NOV-2000 16-NOV-2000 20-N O V -2000 2 5-M ar-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 0.000002 0.022379 0.004347 0.000000 0.016980 0.005491 0 .0 0 0 0 0 0 0.016621 0.003312 0.000000 0 .018859 0.003795 0.000002 0.014599 0.003438 0.000004 0.017031 0.025660 0 .0 0 0 0 0 1 0.011371 0.000468 0.000004 0.019123 0.007920 0.000016 0.014974 0.016220 0.000004 0.012533 0.009564 0.000004 0.014478 0.010593 0.000003 0.020670 0.021239 0.0 0 0 0 0 1 0.005029 0.010607 0.9952 0.9940 0.9840 0.9827 0.9939 0.9901 0.9812 0.9982 0.9937 0.9802 0.9810 0.9859 0.9927 0.9928 1.60 1.60 1.60 1.60 1.60 1.60 1.60 1.60 1.60 1.60 1.60 1.60 1.60 1.60 501 501 501 501 501 501 501 501 501 501 501 501 501 501 M ean 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 calibration curve. Page 21 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBROI-OOl Table 5. Calibration Curve Summary for PFOSA Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 31 -O ct-2000 01-N ov-2000 04-N O V -2000 O6 -N 0 V-2 OOO O8 -N 0 V-2 OOO O9 -N 0 V-2 OOO lO -N ov-2000 I 2 -N 0 V-2 OOO I 3 -N 0 V-2 OOO I 5 -N 0 V-2 OOO I 6 -N 0 V-2 OOO I 8 -N 0 V-2 OOO 25-M ar-2001 Run Number 2 3 4 5 6 7 8 9 10 12 13 14 17 A B C R-Squared LLOQ ULOQ -0.000013 0.052859 0.003517 -0.000003 0.046250 0.010476 -0.000012 0.054175 0.011593 -0.000018 0.069706 0.019030 -0.000015 0.060806 0.009414 -0.000013 0.072938 0.011198 -0.000011 0.067435 0.045288 -0.000007 0.036838 0.013009 -0.000005 0.051854 0.018661 -0.000009 0.077880 0.003529 -0.000007 0.069240 0.029141 -0.000010 0.064050 0.019102 0.000000 0.015780 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 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 500 500 500 500 500 500 500 500 500 500 500 500 500 M ean S.D. %CV n -0.000009 0.056909 0.015334 0.000005 0.016948 0.011547 -55.6 29.8 75.3 13 13 13 0.9922 0.0044 0.4 13 A, B, and C are coefficients used to define the calibration curve.- Page 22 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBRO1-001 Table 6. Calibration Curve Summary for 1V1556 Quadratic weighted l/x:. All concentrations are expressed as ppb. Run Date 31-O ct-2000 01-N ov-2000 04-N O V -2000 O6 - N 0 V-2 OOO O8 -N 0 V-2 OOO O9 - N 0 V-2 OOO IO -N0 V-2 OOO I 2 - N 0 V-2 OOO I 3 - N 0 V-2 OOO I 4 - N 0 V-2 OOO I 5 - N 0 V-2 OOO I 6 - N 0 V-2 OOO I 8 - N 0 V-2 OOO 25-M ar-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 .0 1 8 3 7 3 0.0 0 1 9 2 3 0.000002 0.017583 0.005331 0.000002 0.007944 0.003887 0.000001 0 .0 0 7 7 1 7 0 .0 0 4 4 5 2 0.000002 0.009283 0.002596 0.000002 0.007610 0.002860 0.000002 0.008464 0.004466 0.000002 0.006106 0.003591 0.000003 0.008526 0.004733 0.000007 0.007051 0.006423 0.000003 0.006747 0.003029 0.000002 0.006485 0.002510 0.000002 0.008566 0.004178 0.000001 0 .0 0 2 6 5 0 0.001081 0.9972 0.9972 0.9903 0.9822 0.9949 0.9985 0.9975 0.9968 0.9962 0.9867 0.9911 0.9936 0.9942 0.9955 2.50 2.50 2.50 2.50 2.50 2.50 2.50 2.50 2.50 2.50 2.50 2.50 2.50 2.50 500 500 500 500 500 500 500 500 500 500 500 500 500 500 M ean S.D. %CV n 0.000002 0.000002 100.0 14 0.008793 0.003647 0.004209 0.001423 47.9 39.0 14 14 0.9937 0.0047 0.5 14 A, B, and C are coefficients used to define the calibration curve. Page 23 Northwest Bioanalytieal Study No. NWBS00-088 Report No. NVVBROt-OOi Table 7. Calibration Curve Summary for V1570 Quadratic weighted l/x \ All concentrations are expressed as ppb. Run Date 31-O ct-2000 01-N ov-2000 04-N ov-2000 06-N O V -2000 O8 - N 0 V-2 OOO O9 -N 0 V-2 OOO lO -Nov-2000 I 2 -N 0 V-2 OOO I 3 - N 0 V-2 OOO I 4 -N 0 V-2 OOO I 5 - N 0 V-2 OOO I 6 - N 0 V-2 OOO 2 O-N0 V-2 OOO 25-M ar-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 0.038561 0.012040 -0.000001 0 .0 3 6 2 4 8 0 .0 1 9 1 5 4 -0.000002 0.027976 0.012726 -0.000002 0.026862 0.016535 0.000000 0 .0 3 0 5 3 2 0.016991 0.000001 0 .0 2 4 2 2 3 0 .0 1 4 4 0 9 0.000002 0.028172 0.063424 -0.000002 0.018677 0.009480 0.000002 0.030589 0.027413 0.000020 0.025065 0.030430 0.000003 0.021180 0.014447 0.000006 0.022590 0.034515 0.000000 0.03 3 4 6 6 0.044312 0.000000 0 .0 0 2 6 0 6 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 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 500 500 500 500 500 500 500 500 500 500 500 500 500 500 M ean S.D. %cv n 0.000002 0.000006 300.0 14 0.026196 0.022841 0.008809 0.015953 33.6 69.8 14 14 0.9900 0.0055 0.6 14 A, B, and C are coefficients used to define the calibration curve. Page 24 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 8. Back-Calculated Concentrations of Calibration Standards for PFOS Quadratic weighted l/x :. All concentrations are expressed as ppb. , Run Date 31 -O ct-2000 01-N ov-2000 04-N O V -2000 06-N O V -2000 08-N O V -2000 09-N O V -2000 lO -N ov-2000 12-N O V -2000 13-N ov-2000 14-N O V -2000 15-N ov-2000 16-N O V -2000 Run Number 2 3 4 5 6 7 8 9 10 11 12 13 3.94 5.17 11.3 23.6 44.2 85.4 209 332 414 3.65 4.10 4 .0 0 3.94 4 .1 6 3.70 3.97 3.83 3.96 3.69 4 .2 6 3.56 4 .5 7 **7.53 3.67 4.53 3.84 3.76 4 .5 6 3.26 f4 .9 3 1*3.23 3.31 4.83 5.67 4.90 5.15 5.04 5.31 5.05 5 .3 7 4 .9 6 5 .7 4 5.02 5 .5 6 4.85 4.83 4.35 5.25 4 .5 7 6.11 4.53 5 .7 4 4.83 5.81 4 .8 6 4 .3 4 5.52 12.0 23 .4 45.0 84.2 224 10.7 23.3 42.3 84.5 203 11.4 23.7 46.7 84.5 198 11.4 23.9 43.4 83.6 207 10.5 21.2 44.9 83.7 205 12.6 24.1 45.7 86.9 213 12.4 25.7 45.3 82.8 203 10.7 23.2 43.5 77.3 *116 11.1 2 5 .6 44.5 87.0 215 11.3 22.8 42.9 81.8 193 12.2 26.7 46.7 89.3 227 10.3 22.2 40.9 77.1 184 11.9 24.8 47.0 86.6 212 11.0 22.5 41.1 87.8 207 12.0 25.1 49.0 89.1 2 2 0 10.2 23.0 42.0 79.6 195 12.3 24.2 45.1 85.5 222 11.3 24.0 40.4 75.9 208 11.8 26.3 50.7 90.5 **95.5 9.79 21.9 **28.5 64.6 210 10.8 25.9 47.0 96.6 245 10.1 2 0 .9 43.6 77.6 184 10.3 22.6 43.8 75.1 201 12.0 26.2 50.4 79.5 233 347 424 345 368 329 422 351 405 340 411 332 409 352 428 * 399 350 436 333 386 357 433 338 376 353 418 325 390 339 443 321 392 344 401 332 413 354 401 354 391 374 456 294 354 313 391 330 452 * Sample deactivated due to preparation error ** Sample deactivated as an outlier f LLOQ failed Page 25 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 8. Back-Calculated Concentrations of Calibration Standards for PFOS (Continued) Quadratic weighted l/x:. All concentrations are expressed as ppb. , Run Date I 8 -N 0 V-2 OOO Run N um ber 14 2 5 -M ar-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 5.11 11.3 23.9 44.8 83.0 209 340 408 0.383 0.461 0.784 1.55 2.63 6.03 13.9 16.0 24.6 9.6 9.0 6.9 6.5 5.9 7.3 6.7 4.7 6.0 0.8 -1.2 0.0 1.3 1.4 -2.8 0.0 2.4 -1.4 25 28 28 28 27 28 26 27 28 Page 26 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 9. Back-Calculated Concentrations of Calibration Standards for PFOA Quadratic weighted l/x:. All concentrations are expressed as ppb. Run Date Run N um ber 1.92 3.36 10.6 25.0 49.0 97.1 241 385 481 31-O ct-2000 2 01-N ov-2000 3 04-N O V -2000 4 O6 - N 0 V-2 OOO 5 O8-N 0 V-2OOO 6 O9 - N 0 V-2OOO 7 10 -N o v -2 0 0 0 8 I 2 -N 0 V-2OOO 9 I 3 - N 0 V-2 OOO I 4 - N 0 V-2OOO 15-N ov-2000 10 11 12 I 6 -N 0 V-2 OOO 13 1.94 1.88 1.85 1.94 2.05 1.80 1.89 1.92 2.03 1.98 2.17 1.77 2.17 **6.15 2.02 **3.54 2.22 1.77 2.30 1.59 2.28 1.70 1.82 2.22 3.49 3.36 3.30 3.64 3.27 3.49 3.14 3.63 3.22 3.03 3.06 3.34 2.75 3.22 3.53 2.92 3.19 2.97 3.92 2.72 3.16 3.22 3.28 2.81 9.80 10.7 10.0 10.5 9.53 11.0 10.6 10.5 9.85 10.3 10.4 10.8 9.73 11.2 11.0 10.0 10.8 10.6 10.6 9.75 9.24 10.7 10.4 10.3 24.9 26.6 24.0 25.7 2 1 .4 27.9 25.0 27.3 27.5 25.1 25.8 25.6 26.1 24.5 23.9 24.3 26.1 27.2 27.2 24.0 25.1 25.3 27.0 2 6 .0 47.2 89.3 49.5 99.2 51.6 98.9 48.7 95.3 49.2 90.5 51.0 102 47.0 84.0 55.5 92.8 49.6 97.8 50.8 95.0 49.2 92.7 50.2 95.0 49.5 95.4 50.9 103 51.0 94.5 52.3 99.6 52.2 47.1 93.0 87.0 53.6 96.8 **15.4 83.8 49.5 90.5 56.9 102 51.3 96.7 52.9 86.4 250 247 227 249 245 253 234 *164 253 237 244 243 238 255 235 251 249 242 **57.3 258 233 246 233 253 383 427 381 406 385 398 374 *' 382 387 394 399 386 378 365 416 412 386 381 418 339 415 372 369 470 443 472 478 456 478 482 509 481 471 501 437 484 467 477 467 463 473 445 482 494 480 466 523 * Sample deactivated due to preparation error ** Sample deactivated as an outlier Page 27 Northwest Bioanaiytical Study No. NWBSOO-088 Report No. NVVBRO1-001 Table 9. Back-Calculated Concentrations of Calibration Standards for PFOA (Continued) Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date Run Number 1.92 3.36 10.6 25.0 49.0 97.1 241 385 481 18-NOV-2000 14 1.77 3.29 9.90 25.1 48.7 96.5 243 404 441 2.20 2.90 12.5 25.6 46.1 93.9 248 398 486 25-Mar-2001 17 1.85 2.67 10.4 27.1 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 94.3 244 391 473 0.199 0.298 0.634 1.40 2.47 5.07 8.09 19.6 19.7 10.1 9.3 6.1 5.5 4.9 5.4 3.3 5.0 4.2 3.1 -4.8 -1.9 2.4 2.9 -2.9 1.2 1.6 -1.7 26 28 28 28 27 28 26 27 28 Page 28 i Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR0I-001 Table 10. Back-Calculated Concentrations of Calibration Standards for PFHS Quadratic weighted l/x2. All concentrations are expressed as ppb. R un Date R un N u m b e r 1.36 2.92 10.7 26.5 52.6 104 262 418 523 31-O ct-2000 2 1.30 3.01 11.2 26.0 49.7 98.7 268 419 530 1.42 2.77 11.2 2 7.4 52.0 102 266 455 478 01-N ov-2000 3 1.36 2.73 11.2 25.8 51.1 104 23S 417 513 1.35 3.12 10.6 27.1 55.7 100 268 442 532 04-N O V -2000 4 1.43 3.08 9.86 28.5 51.2 96.4 247 432 513 1.31 2.6 7 10.7 2 8 .7 53.1 106 271 4 2 4 524 O6 - N 0 V-2 OOO 5 1.40 1.36 2.86 2.72 11.0 11.5 26.6 28.8 51.5 55.5 87.1 102 252 *167 431 515 * 554 O8 - N 0 V-2 OOO 6 1.44 2.85 11.4 28.3 52.4 101 260 425 547 1.24 3.16 10.1 2 5 .7 53.8 96.3 247 4 30 516 O9 - N 0 V-2 OOO 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 IO -N 0 V-2 OOO 8 1.51 2 .3 7 10.9 2 6 .4 53.1 103 250 413 537 **5.46 2.69 11.1 28.1 54.0 107 272 413 515 I 2 - N 0 V-2 OOO 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 13-N ov-2000 10 1.35 2.85 11.1 2 6 .4 52.5 102 2 6 2 432 520 1.41 2.73 11.3 2 7 .9 48.8 99.6 273 4 3 4 492 I 4 - N 0 V-2 OOO 11 1.45 1.32 2.61 2.95 10.7 27.4 50.4 104 **79.3 416 488 10.8 28.0 **23.7 101 269 469 503 15-N ov-2000 12 1.55 2 .7 4 11.4 2 9 .4 55.4 120 276 475 561 1.30 2.47 10.2 2 5 .4 51.9 91.9 237 370 482 I 6 - N 0 V-2 OOO 13 1.23 2 .6 6 11.2 2 7 .3 55.1 104 2 7 0 407 521 1.59 2.64 10.8 27.3 56.3 89.6 255 420 542 * Sample deactivated due to preparation error ** Sample deactivated as an outlier Page 29 Northwest Bioanalytieal Study No. NWBS00-088 Report No. NWBRO1-001 Table 10. Back-Calculated Concentrations of Calibration Standards for PFHS (Continued) Quadratic weighted l/x:. All concentrations are expressed as ppb. R u n D a te R u n Num ber 1.36 2.92 10.7 26.5 52.6 104 262 418 523 18-NOV-2000 14 1.26 2.98 10.1 26.3 53.8 97.8 264 428 534 1.48 2.61 13.3 26.6 50.3 99.7 253 407 534 25-M ar-2001 17 1.39 2.46 10.4 28.0 55.4 103 277 440 521 1.52 2.52 10.6 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 Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 11. Back-Calculated Concentrations of Calibration Standards for PFOSAA Quadratic weighted l/x2. All concentrations are expressed as ppb. , Run Date Run Num ber 1.60 3 .10 10.6 25.6 50.6 101 251 401 501 31-O ct-2000 2 01-N ov-2000 3 04-N O V -2000 4 O6 - N 0 V-2 OOO 5 O8- N 0 V-2 OOO 6 O9 - N 0 V-2 OOO 7 IO -N 0 V-2 OOO 8 I 2 - N 0 V-2 OOO 9 13-N ov-2000 10 I 4 - N 0 V-2 OOO 11 I 5 - N 0 V-2 OOO 12 I 6 - N 0 V-2 OOO 13 2 O-N0 V-2 OOO 16 1.41 1.68 1.66 1.54 1.58 1.56 1.24 1.94 1.52 1.72 1.46 1.71 1.98 **8.58 1.61 **2.67 1.59 1.60 1.54 1.53 1.85 1.40 1.72 **5.99 1.52 1.72 3.26 3 .3 6 2.85 3.50 3.53 3.00 2 .7 7 3.56 2.88 3.23 2 .8 4 3.48 2.13 2 .7 0 3.09 3.15 3.22 2 .9 6 3.40 3.39 2.88 3.33 2.88 2.81. 3 .1 4 2.88 10.7 24.0 48.1 94.6 271 394 10.9 25.4 48.1 106 261 433 9.40 25.1 55.4 97.5 248 375 9.99 26.9 48.8 107 261 443 8.37 19.1 50.2 94.5 243 392 12.0 28.9 54.9 107 285 429 10.1 23.3 45.8 95.8 10.4 27.7 55.2 115 242 *186 379 * 8.73 26.6 47.4 96.4 257 432 11.7 26.7 51.7 106 255. 392 9.64 24.8 45.8 90.1 260 389 11.5 27.8 53.0 102 253 472 9.82 25.8 54.7 98.0 253 403 10.6 2 4.6 50.3 122 289 396 10.1 2 4 .6 50.3 99.6 2 5 0 376 10.2 27.0 51.5 104 269 420 11.1 24.2 50.2 98.0 275 4 0 2 11.2 26.3 44.9 99.5 264 403 9.75 28.5 59.2 105 **138 391 9.65 2 6.4 37.1 82.5 284 447 7.98 22.3 44.4 99.5 270 364 10.9 25.3 62.0 113 284 437 11.9 28.4 56.9 93.4 282 419 9.59 25.7 48.4 80.6 281 336 9.31 23.8 47.1 98.1 253 413 12.4 27.4 48.8 107 267 407 487 467 495 481 461 496 494 532 501 468 449 495 463 489 487 504 424 549 445 507 465 483 502 506 447 520 * Sample deactivated due to preparation error ** Sample deactivated as an outlier Page 3 1 Northwest Bioanalytical Study No. NWBS0-088 Report No. NWBRO1-001 Table 11. Back-Calculated Concentrations of Calibration Standards for PFOSAA (Continued) Quadratic weighted l/x". All concentrations are expressed as ppb. Run Date Run Number ' 25-Mar-200l 17 1.60 1.67 1.71 3.10 10.6 25.6 50.6 101 251 401 501 2.93 10.8 29.8 52.5 103 255 420 500 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 0.333 1.08 2.24 5.03 8.84 10.9 10.5 8.7 10.0 8.8 -1.3 -2.8 0.4 -0.4 -1.0 28 28 28 28 28 264 407 485 14.0 29.0 27.9 5.3 7.1 5.8 5.2 1.5 -3.2 26 27 28 Page 32 Northwest Bioanalytical Study No. NWBS00-088 Report No. NVVBRI-001 Table 12. Back-Calculated Concentrations of Calibration Standards for PFOSA Quadratic weighted 1/x3. All concentrations are expressed as ppb. Run Date Run N um ber 1.00 2.50 10.0 25.0 50.0 100 250 400 500 31 -Oct-2000 2 0.930 2.62 9.96 25.7 52.8 101 289 438 529 1.06 2.48 9.45 24.1 47.2 100 229 362 453 01-Nov-2000 3 0.913 2.40 8.86 25.1 52.1 99.1 238 380 497 1.10 2.56 9.78 26.7 50.4 104 255 432 491 04-Nov-2000 4 1.00 2.64 9.23 19.1 51.8 101 248 386 494 0.998 2.33 11.5 26.1 53.7 105 241 399 525 06-NOV-2000 5 0.934 2.63 10.1 26.9 48.7 104 248 395 521 1.03 2.60 9.67 25.7 48.4 86.1 *138 * 499 08-NOV-2000 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 09-NOV-2000 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 lO-Nov-2000 8 1.12 2.15 10.7 27.9 52.5 103 259 424 522 **1.67 2.04 10.1 23.6 47.1 105 252 366 467 12-NOV-2000 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 13-N o v -2 0 0 0 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 I5-Nov-2000 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 16-NOV-2000 13 0.788 1.22 2.06 . 8.94 2.85 10.8 24.4 47.6 86.3 29.0 54.2 95.7 234 286 385 479 382 547 18-Nov-2000 14 0.965 2.39 10.0 24.9 47.2 102 240 466 438 1.04 2.59 10.2 27.5 45.2 95.6 276 392 495 * Sample deactivated due to preparation error ** Sample deactivated as an outlier Page 33 Northwest Bioanalyticul Study No. NWBS00-088 Report No. NWBR01-001 Table 12. Back-Calculated Concentrations of Calibration Standards for PFOSA (Continued) , Quadratic weighted 1/x3. All concentrations are expressed as ppb. Run Date Run N um ber 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 98.8 251 404 497 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 h Page 34 Northwest Bioanalytieal Study No. NWBS00-088 Report No. NWBR1-001 Table 13. Back-Calculated Concentrations of Calibration Standards for M556 Quadratic weighted 1/x". All concentrations are expressed as ppb. Run Date Run Num ber 2.50 10.0 25.0 50.0 100 250 400 500 31 -O ct-2000 01-Nov-2000 04-NOV-2000 O-Nov-2000 O8 -N 0 V-2 OOO 09-Nov-2000 IO-N0 V-2 OOO I2 -N 0 V-2 OOO I3 -N 0 V-2 OOO I4 -N 0 V-2 OOO I5 -N 0 V-2 OOO I6 -N 0 V-2 OOO I8 -N 0 V-2 OOO 2 3 4 5 6 7 8 9 10 11 12 13 14 2.33 9.67 24.3 51.9 95.2 255 388 499 2.70 9.81 25.8 49.3 104 249 438 470 2.55 9.86 25.9 55.5 107 246 403 505 2.48 9.52 23.6 47.4 96.2 241 421 478 2.38 8.49 19.4 53.2 96.1 248 388 485 2.63 11.8 26.4 52.2 104 263 416 500 2.02 8.91 22.7 46.0 86.0 235 385 492 2.98 10.7 28.8 58.2 107 *200 * 538 2.28 8.40 26.1 46.3 98.1 255 413 494 2.75 11.0 25.7 51.4 102 250 409 481 2.51 9.73 25.7 49.3 95.5 253 400 488 2.50 9.91 25.5 51.8 100 238 432 490 2.37 9.94 23.7 47.6 97.9 244 402 487 2.63 10.3 24.0 50.9 109 271 394 500 2.61 9.22 23.4 50.6 97.8 233 376 499 2.43 9.95 26.7 51.0 107 264 421 502 2.52 10.3 25.5 52.3 96.5 261 429 458 2.43 10.4 26.0 46.8 88.5 248 403 516 2.77 9.58 27.2 57.3 103 **127 392 453 2.33 8.48 24.2 **33.4 81.4 272 439 505 2.46 8.06 22.9 46.3 105 276 388 483 2.66 10.1 23.9 57.7 104 260 427 464 2.70 10.0 27.2 53.3 92.8 255 414 499 2.32 9.10 25.3 52.2 87.3 271 359 513 2.69 9.91 23.3 48.0 96.4 242 434 454 2.25 11.4 26.6 48.1 97.0 256 420 503 * Sample deactivated due to preparation error ** Sample deactivated as an outlier Page 35 Northwest Bioanalytical Study No. NWBS00-088 Report No. NVVBRl-001 Table 13. Back-Calculated Concentrations of Calibration Standards for IY1556 (Continued) Quadratic weighted l/x:. All concentrations are expressed as ppb. Run Date Run Num ber 2.50 10.0 25.0 50.0 100 250 400 500 2 5 -Mar-2001 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 4.1 0.4 -1.8 0.0 1.8 -1.9 1.2 2.3 -2.0 28 28 28 27 28 26 27 28 Page 36 Northwest Bioanalytical Study No. NWBS0O-08S Report No. NWBROt-OOl Table 14. Back-Calculated Concentrations of Calibration Standards for M570 Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date Run N um ber 1.00 2.50 10.0 25.0 50.0 100 250 400 500 31 -O ct-2000 2 0.828 2.29 10.1 23.6 48.1 93.7 262 392 . 486 1.18 2.66 9.94 25.9 50.6 109 252 431 475 01-Nov-2000 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 04-NOV-2000 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 06-NOV-2000 5 0.930 1.10 2.09 9.52 23.9 44.9 97.3 234 384 486 2.75 10.3 26.6 56.0 110 *183 * 538 08-NOV-2000 6 0.952 2.50 8.31 25.8 49.0 100 251 404 496 1.08 2.35 10.6 25.7 51.9 107 249 404 488 09-NOV-2000 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 lO -N ov-2000 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 I2 -N 0 V-2 OOO 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 I3 -N 0 V-2 OOO 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 I4 -N 0 V-2 OOO 11 1.10 2.78 9.29 26.7 57.0 104 **133 399 440 0.813 2.87 9.11 25.9 37.9 81.5 276 444 508 I5 -N 0 V-2 OOO 12 **1.53 2.39 7.28 22.1 45.2 101 259 369 457 1.02 2.62 10.3 25.2 62.8 112 269 439 495 I6 -N 0 V-2 OOO 13 1.16 1.93 10.8 28.4 57.9 100 276 422 497 1.03 1.83 9.19 26.1 52.0 83.4 275 340 495 2 O-N0 V-2 OOO 16 0.933 1.10 2.61 9.04 24.1 46.9 96.9 241 423 449 2.13 12.0 26.1 48.4 107 260 404 523 * Sample deactivated due to preparation error ** Sample deactivated as an outlier Page 37 Northwest Bioanalytieal Study No. NWBS00-088 Report No. NWBR0I-001 Table 14. Back-Calculated Concentrations of Calibration Standards for IVI570 (Continued) Quadratic weighted 1/x'. All concentrations are expressed as ppb. Run Date Run Num ber 25-Mar-2001 17 1.00 1.03 1.05 2.50 1.98 **1.64 10.0 25.0 50.0 100 9.84 29.0 52.3 102 10.0 24.8 50.4 90.5 250 252 241 400 500 424 508 419 458 Mean S.D. %CV %Bias n 1.02 0.106 10.4 2.0 25 2.40 9.76 25.3 50.7 101 255 408 487 0.304 1.03 2.09 4.84 7.92 13.4 26.4 26.9 12.7 10.6 8.3 9.5 7.8 5.3 6.5 5.5 -4.0 -2.4 1.2 1.4 1.0 2.0 2.0 -2.6 25 28 28 28 28 26 27 28 Page 38 Northwest Bioanalytieal Study No. NWBSOO-088 Report No. NWBROl-Ol Table 15. Analytical QC Summary for PFOS All concentrations are expressed as ppb. Run Date Run Number 3 1 -O ct-2000 2 01-Nov-2000 3 04-Nov-2000 4 O6 -N 0 V-2 OOO 5 O8 -N 0 V-2 OOO 6 O9 -N 0 V-2 OOO 7 lO-Nov-20001 8 I 2 -N 0 V-2 OOO 9 I 3 -N 0 V-2 OOO 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 129 135 125 124 131 130 105 122 147 128 137 108 136 134 ' 132 127 139 136 136 133 141 103 High QC 332 ppb Dilution QC 335 ppb DF=2 323 322 369 354 314 322 291 283 343 320 302 ' 293 323 318 299 304 1 327 312 322 294 319 320 330 323 350 Page 39 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 15. Analytical QC Summary for PFOS (Continued) AH concentrations are expressed as ppb. Run Date Run Number 16-NOV-2000 13 I 8-N0V-2 OOO 14 25-Mar-2001 17 Low QC 6.40 ppb 6.65 5.98 5.87 6.06 6.26 5.95 Medium QC High QC 126 ppb 332 ppb 126 297 129 319 130 126 . 338 336 137 367 135 349 Dilution QC 335 ppb DF=2 307 312 359 335 342 345 335 338 471 Mean S.D. %CV %Theoretical %Bias n 6.26 0.430 6.9 97.8 -2.2 28 129 10.1 7.8 102.4 2.4 28 321 22.1 6.9 96.7 -3.3 28 345 42.6 12.3 103.0 3.0 12 Page 40 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBROl-OOl Table 16. Analytical QC Summary for PFOA All concentrations are expressed as ppb. Run Date Run Number 31-Oct-2000 2 01-Nov-2000 3 04-NOV-2000 4 O6-N0V-2 OOO 5 O8-N 0 V-2 OOO 6 O9-N0V-2 OOO 7 IO-N0 V-2 OOO 8 I 2-N0V-2 OOO 9 I 3-N0V-2OOO 10 I4-N0V-2OOO 11 I 5-N0 V-2OOO 12 I 6-N0 V-2OOO 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 Medium QC 145 ppb 156 147 144 144 149 159 140 147 154 159 147 130 154 160 151 150 159 158 153 155 158 127 143 160 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 Page 41 Northwest ioanalytieal Study No. NWBSOO-088 Report No. NWBRO1-001 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 Low QC 4.81 ppb 3.92 3.90 4.28 4.06 Medium QC 145 ppb 147 151 163 159 High QC 385 ppb 386 394 412 422 Dilution QC 386 ppb 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 6.1 100.8 0.8 28 404 18.6 4.6 104.7 4.7 12 Page 42 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 17. Analytical QC Summary for PFHS All concentrations are expressed as ppb. Run Date Run Low QC N um ber 4.48 ppb 31-Oct-2000 2 01-Nov-2000 3 04-NOV-2000 4 O6-N0V-2OOO 5 O8-N0V-2OOO 6 O9-N0V-2OOO 7 lO-Nov-2000 8 I 2-N0V-2OOO 9 I 3-N0V-2 OOO 10 14-Nov-2000 11 I 5-N0V-2OOO 12 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 I 6-N0V-2OOO 13 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=2 367 365 378 418 431 401 Page 43 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 17. Analytical QC Summary for PFHS (Continued) All concentrations are expressed as ppb. Run Date Run Low QC N um ber 4.48 ppb 18-NOV-2000 14 3.74 3.85 25-Mar-2001 17 3.85 3.72 Medium QC 156 ppb 155 148 153 153 High QC 417 ppb 454 397 448 427 Dilution QC 418 ppb DF=2 391 401 414 390 403 449 Mean S.D. %CV %Theoretical %Bias n 4.10 0.287 7.0 91.5 -8.5 28 155 8.40 5.4 99.4 -0.6 28 405 21.0 . 5.2 97.1 -2.9 28 401 25.0 6.2 95.9 -4.1 12 Page 44 Northwest Bioanalytieal Study No. NWBS00-088 Report No. NWBR01-001 Table 18. Analytical QC Summary for PFOSAA All concentrations are expressed as ppb. Run Date Run Number 31-O ct-2000 2 01-Nov-2000 3 04-NOV-2000 4 06-Nov-2000 5 O8 -N 0 V-2 OOO 6 O9 -N 0 V-2 OOO 7 IO-N0 V-2 OOO 8 I 2 - N 0 V-2 OOO 9 1 3 -N 0 V-2 OOO 10 I 4 -N 0 V-2 OOO 11 I 5-N0V-2 OOO 12 I6-N0V-2 OOO . 13 Low QC 4.60 ppb M edium QC High QC 151 ppb 401 ppb Dilution QC 401 ppb DF=2 4.43 160 393 4.03 157 394 *5.84 150 485 5.21 172 488 4.26 151 391 4.10 162 388 3.77 136 366 4.18 138 35 6 5.22 176 4.35 157 3.50 153 3.93 128 4.23 163 4.55 181 4.15 . 153 5.55 172. 5.24 151 5.06 172 3.71 168 4.52 150 *3.39 158 3.70 116 443 434 359 409 415 430 380 389 415 323 399 371 451 427 419 491 422 4.10 . 137 419 401 4.15 157 412 399 424 * >fc 25% deviation from theoretical Page 45 Northwest Bioanalytical Study No. NVVBS00-088 Report No. NWBR0I-001 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 M edium QC High QC 151 ppb 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 %Bias n 4.31 0.667 15.5 93.7 -6.3 28 157 15.3 9.7 104.0 4.0 28 408 39.4 9.7 101.7 1.7 28 * > 25% deviation from theoretical 438 66.3 15.1 109.2 9.2 12 Page 46 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 19. Analytical QC Summary tor PFOSA All concentrations are expressed as ppb. Run Date Run Low QC N um ber 4.00 ppb 31-Oct-2000 2 01-Nov-2000 04-NOV-2000 4 O6-N0V-2OOO 5 O8-N0V-2OOO 6 09-Nov-2000 7 lO-Nov-2000 8 I 2-N0V-2OOO 9 13-Nov-2000 10 I 5-N0V-2OOO 12 , 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 I 6-N0 V-2OOO 13 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 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBROl-OOl Table 19. Analytical QC Summary for PFOSA (Continued) All concentrations are expressed as ppb. Run Date Run Number 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 9.7 101.8 1.8 26 * > 25% deviation from theoretical 430 51.3 11.9 107.5 7.5 12 Page 48 Northwest Bioaualytieal Study No. NWBS00-088 Report No. NWBR01-00I Table 20. Analytical QC Summary for M556 All concentrations are expressed as ppb. Run Date Run Low QC Medium QC N um ber 4.00 ppb 150 ppb 31 -O ct-2000 2 01-Nov-2000 3 04-NOV-2000 4 O6 - N 0 V-2 OOO 5 O8 -N 0 V-2 OOO 6 O9 -N 0 V-2 OOO 7 10 -N o v -2 0 0 0 8 I 2 -N 0 V-2 OOO 9 13-Nov-2000 10 I 4 - N 0 V-2 OOO 11 15-Nov-2000 12 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 3.56 161 149 163 171 156 163 141 146 172 160 155 132 161 *182 158 176 164 175 163 157 156 *112 I 6 - N 0 V-2 OOO 13 3.98 3.81 139 154 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 * > 20% deviation from theoretical Page 49 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRI-001 Table 20. Analytical QC Summary for M556 (Continued) All concentrations are expressed as ppb. Run Date Run Low QC M edium QC N um ber 4.00 ppb 150 ppb I 8-N0V-2 OOO 14 3.87 3.69 150 157 25-M ar-2001 17 4.09 3.52 168 162 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 n 3.94 0.437 11.1 98.5 -1.5 28 157 14.3 9.1 104.7 4.7 28 411 29.3 7.1 102.8 2.8 28 * > 20% deviation from theoretical 430 65.5 15.2 107.5 7.5 12 Page 50 Northwest Biounalytical Study No. NWBS00-08S Report No. NWBRO1-001 Table 21. Analytical QC Summary for M570 All concentrations are expressed as ppb. Run Date Run Number 31-Oct-2000 2 01-Nov-2000 3 04-NOV-2000 4 O6-N 0V-2OOO 5 O8-N0V-2OOO 6 O9-N0V-2OOO 7 lO-Nov-2000 8 I 2-N0V-2OOO 9 I 3-N0 V-2OOO 10 I 4-N0V-2OOO 11 I 5-N0 V-2OOO 12 I 6-N0 V-2OOO 13 Low QC 4.00 ppb 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 High QC Dilution QC 150 ppb 400 ppb 400 ppb DF=2 164 410 160 416 152 178 147 165 133 146 *182 476 *491 400 385 362 379 446 161 422 154 364 131 409 165 421 427 OO *r --< 154 384 173 397 158 420 176 326 166 408 154 383 155 452 414 *114 429 *490 424 141 423 413 161 415 399 435 * > 20% deviation from theoretical Page 51 Northwest Bioanalytical Study No. NWBS00-088 Report No. N WBRO1-001 Table 21. Analytical QC Summary for M570 (Continued) All concentrations are expressed as ppb. Run Date Run Low QC N um ber 4.00 ppb 20-NOV-2000 16 *2.76 3.33 25-Mar-2001 17 3.20 *2.89 Medium QC 150 ppb High QC 400 ppb Dilution QC 400 ppb DF=2 169 372 415 151 *484 421 391 165 461 383 159 411 400 *648 Mean S.D. %cv %Theoretical %Bias n o t"i! 3.72 0.596 16.0 93.0 28 158 15.6 9.9 105.3 5.3 28 413 38.1 9.2 103.3 3.3 28 * > 20% deviation from theoretical 436 72.1 16.5 109.0 9.0 12 Page 52 Northwest Bioanalytical Study No. NWBS00-088 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 2.94 5.00 7.70 3.85 PFHS Concentration* <LLOQ(1.36) 3.72 1.99 3.82 6.12 4.28 <LLOQ(1.36) 10.4 <LLOQ(2.41) 21.2 28.1 21.6 180 25.7 11.0 1.81 7.09 PFOSAA 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I,00) <LLOQ(1.00) <LLOQ(2.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <LLQQ(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) M570 Concentration* <LLOQ(1.00) <LLOQ(l .00) 5.15 3.28 6.55 <LLOQ(1.00) 2.37 1.74 <LLOQ(2.00) 4.81 1.53 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 1.91 * 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 53 Northwest Bioanalytical Study No. NW BS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0187 0192 0193 0194 0196 0197 0198 0199 0210 0216 0217 0228 0229 0230 0231 PFOS Concentration PFOA PFHS Concentration** Concentration* PFOSAA Concentration* PFOSA Concentration* M556 Concentration* 31.1 3.56 <LLOQ(1.36) 3.69 <LLOQ(1.00) <LLOQ(2.50) 35.7 6.93 6.05 6.66 <LLOQ(1.00) <LLOQ(2.50) 90.2 6.41 71.3 3.14 <LLOQ(1.00) 3.58 24.5 4.44 1.41 <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) 11.6 1.95 <LLOQ(1.36) 1.64 <LLOQ(1.00) <LLOQ(2.50) 38.9 5.46 <LLOQ(1.36) 4.95 <LLOQ(1.00) <LLOQ(2.50) 71.9 7.43 <LLOQ(1.36) 4.12 <LLOQ(1.00) 5.94 54.8 7.37 30.0 <LLOQ(2.60) <LLOQ(2.00) <LLOQ(5.00) 33.9 5.44 4.14 4.76 <LLOQ(2.00) 7.16 38.2 4.79 3.12 2.42 <LLOQ(1.00) <LLOQ(2.50) 43.6 5.16 6.86 5.34 <LLOQ(1.00) 5.59 16.6 3.89 6.83 <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) 122 10.4 145 4.93 <LLOQ(1.00) 4.35 No result No result No result No result (Insufficient No result (Insufficient sample (Insufficient sample (Insufficient sample sample volume) (Insufficient sample volume) volume) volume) volume) No result (Insufficient sample volume) 93.9 7.8 17.8 6.07 <LLOQ(1.00) 8.55 M570 Concentration* 2.04 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 7.26 2.42 5.03 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) No result (Insufficient sample volume) 23 * Seram 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 54 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 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(1.36) 3.23 <LLOQ(1.36) <LLOQ(1.36) 11.2 4.60 2.33 <LLOQ(1.36) <LLOQ(2.41) 1.50 2.27 <LLOQ(2.41) PFOSAA Concentration* 3.19 <LLOQ(1.60) 3.11 2.04 15.3 4.54 <LLOQ(1.60) 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(2.00) <LLOQ(1.00) <LLOQ(1.00) <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(1.00) 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) * 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 55 Northwest Bioanalytical Study No. NW BS00-088 Report No. N \V BR 01-001 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00)~ <LLOQ(1.00) M556 Concentration* <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 10.1 <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 seium 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 56 Northwest Bioanalytical Study No. NW BS00-088 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 2*7.3 34.4 124 56.7 106 52.0 63.4 27.6 59.9 31.9 59.5 46.9 PFOA Concentration* 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 6.21 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) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) cLLOQ(l.OO) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 M570 Concentration* Concentration* 3.21 4.8 3.82 1.78 <LLOQ(2.50) 3.09 <LLOQ(2.50) 3.42 <LLOQ(2.50) 4.35 2.58 4.73 <LLOQ(2.50) 2.28 9.59 31 3.46 19.7 9.45 ' 1.84 <LLOQ(2.50) . 2.83 3.83 2.71 2.74 2.27 5.88 2 <LLOQ(2.50) 3.01 3.26 4.14 8.22 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 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) o f the target concentration. Tire statistical error o f any individual result may exceed the QC acceptance criteria. Page 57 i Northwest Bioanalytical Study No. NWBS00-088 Repon No. NVVBRO1-001 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1,00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <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 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. Tire method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 58 Northwest Bioanalytical Study No. N W B S00-0881 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0589 0590 0592 0593 0598 0599 0604 0606 0607 0608 0610 0611 0621 0627 0628 0629 0631 PFOS Concentration 31.0 33.4 35.1 165 25.6 77.1 18.0 37.6 48.2 52.3 29.0 20.3 23.2 72.7 29.8 37.6 54.5 PFOA Concentration* 7.57 6.37 3.15 7.94 5.40 7.44 3.54 5.71 5.72 8.01 5.36 2.19 4.57 4.65 2.64 4.86 7.68 PFHS Concentration* 3.71 8.80 1.75 129 1.91 21.8 2.85 2.84 2.55 1.82 7.30 <LLOQ(1.36) 3.13 20.0 <LLOQ(1.36) <LLOQ(1.36) 11.4 PFOSAA Concentration* 2.84 9.81 2.99 2.40 2.56 6.25 <LLOQ(1.60) 4.69 10.3 8.98 4.23 3.66 3.95 5.02 6.26 8.71 6.72 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <LLOQ(2.50) 9.8 <LLOQ(2.50) <LLOQ(2.50) 4.05 4.42 <LLOQ(2.50) 4.11 7 3.42 3.38 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 2.64 2.55 4.63 M570 Concentration* <LLOQ(1.00) 4.02 2.22 <LLOQ(.1.00) 4.75 5.91 : 1.5 7.17 2.82 3.57 11.8 <LLOQ(1.00) 2.12 1.51 3.69 <LLOQ(1.00) <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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 59 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0649 0657 0658 0664 0665 0666 0667 0673 0676 0678 0679 0680 0681 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(1.36) 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 PFOSAA 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(1.60) PFOSA Concentration* <LLOQ(2.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <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( 1.00) ' 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(1.00) <LLOQ(1.00) <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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 60 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0711 0712 0713 0714 0719 0720 0721 0723 0725 0741 0748 0752 0753 0754 0763 0769 0771 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 81.0 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(1.36) 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) M556 Concentration* 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(1.00) 2.93 <LLOQ(1.00) 1.61 i <LLOQ(1.00) 4.44 1.19 <LLOQ(1.00) <LLOQ(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 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 61 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <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(l .00) <LLOQ(1.00) <LLOQ(1.00) 3.73 1.59 1.42 <LLOQ(1.00) 8.16 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 62 Northwest Bioanalytical Study No. NWBS00-088 Repoit No. NWBRO1-001 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 9.96 3.75 5.84 6.01 6.14 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* 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(1.00) 1.7 1.55 3.22 9.81 3.24 1.98 <LLOQ(1.00) 7.85 1.42 26.7 <LLOQ(1.00) 2.93 Serum sample lesults 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 63 Northwest Bioanalytical Study No. NW BS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations 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 20.1 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(1.36) 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <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 1 <LLOQ(1.00) 1 1.08 1.7 4.28 2.91 1.54 1.31 3.79 1.8 2.95 cLLOQ(l.OO) 1.51 9.05 * Serum sample results obtained using plasma curves may vai^ 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 manix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentr ation. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 64 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 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 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 PFHS Concentration** Concentration* 3.25 <LLOQ(1.36) 3.52 2.18 5.39 <LLOQ(1.36) 2.47 1.44 5.45 3.46 3.46 <LLOQ(1.36) 7.16 2.54 9.81 5.11 3.01 <LLOQ(1.36) 6.18 74.2 3.89 <LLOQ(1.36) 56.1 416 5.06 39.6 8.05 51.9 6.33 2.94 4.25 35.7 8.62 6.40 PFOSAA Concentration* 1.64 <LLOQ(1.60) <LLOQ(1.60) 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) . <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <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(1.00) 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 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 65 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBRO1-001 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 PFHS Concentration** Concentration* 4.09 <LLOQ(1.36) 5.32 10.4 3.11 <LLOQ(1.36) 3.57 9.07 6.22 1.92 2.64 2.19 4.66 7.91 3.43 1.59 6.98 1.77 5.85 12.4 2.90 9.41 5.63 13.3 3.08 <LLOQ(1.36) 5.04 36.2 3.09 <LLOQ(1.36) 5.60 2.60 5.40 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) cLLOQ(l.OO) 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(1.00) <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 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 66 Northwest Bioanalytical Study No. NWBS0O-O88 Report No. N \V BR 01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. 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 PFHS Concentration** Concentration* 4.35 4.70 4.90 10.4 6.85 4.55 4.15 20.3 4.21 2.00 4.59 3.47 5.51 2.39 4.33 3.25 4.28 8.63 3.61 2.44 3.71 <LLOQ(1.36) 4.38 11.5 5.80 10.5 5.22 2.86 5.21 2.57 11.9 4.07 11.0 9.77 PFOSAA Concentration* 2.13 5.66 4.24 1.79 6.23 5.01 7.87 <LLOQ(1.60) 2.27 4.08 5.29 2.51 5.60 3.61 9.22 5.94 4.22 PFOSA Concentration* <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ( 1.00) M556 Concentration* <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(1.00) 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 nan (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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 67 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. 1174 1175 1177 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 54.1 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <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) 1 <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(2.00j * Semin 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) o f the target concentration. The statistical enor o f any individual result may exceed the QC acceptance criteria. Page 68 Northwest Bioanalytical V Study No. NW BS00-088 Report No. NWBRO1-001 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) <LLOQ(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) <Ll.OQ(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 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 69 Northwest Bioanalytical Study No. NWBSOO-088 Repon No. NWBRO1-001 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 11839 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 37.1 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 <LLOQ(2.00) <LLOQ(2.00) 45.4 2.63 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). * * Results are from a rejected ran (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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 70 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 11840 11841 11842 11843 11844 11845 11846 11847 11848 11849 11850 11851 11852 11853 11854 11855 11856 PFOS Concentration 42.2 127 74.8 146 29.7 196 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 67.2 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 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 71 Northwest Bioanalytical Study No. NW BS00-088 : Report No. NWBRO1-001 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 67.6 42.7 35.4 97.9 47.5 51.5 78.1 72.1 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* 241 257 1.89 3.15 33.9 42.4 <LLOQ(1.36) 2.97 6.45 3.47 2.83 1.38 61.4 2.50 9.61 76.5 4.10 PFOSAA Concentration* <LLOQ(2.60) 4.69 6.23 6.64 2.93 4.53 18.2 6.98 5.56 14.3 4.44 3.26 2.97 2.09 4.71 3.62 11.6 PFOSA Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <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 1.14 9.65 4.3 <LLOQ(1.00) 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 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 tire concentration for each QC must be within +20% (25% for PFOSA and PFOSAA) o f the target concentration. Tire statistical error o f any individual result may exceed the QC acceptance criteria. Page 72 Northwest Bioanalytical Study No. NW BS00-088 Report No. NWBRO1-001 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 : 11.6 PFHS Concentration* 2.52 220 9.16 <LLOQ(1.36) 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(1.00) <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) M5S6 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(1.00) <LLOQ(1.00) 1.31 <LLOQ( 1.00) 19.6 <LLOQ(1.00) 3.67 2.52 <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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 73 Northwest Bioanalytical Study No. NW BS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. 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 PFHS Concentration** Concentration* 8.55 4.44 5.00 1.49 2.84 2.57 3.96 4.19 3.92 1.58 3.41 <LLOQ(1.36) 4.76 2.52 4.58 7.03 6.24 <LLOQ(1.36) 4.71 6.13 5.08 5.63 2.69 1.47 3.34 <LLOQ(1.36) 5.68 5.81 2.88 <LLOQ(l .36) 3.48 4.19 5.83 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) ` M556 Concentration* <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(1.00) 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. . Page 74 Northwest Bioanalytical Study No. NW BS00-088 Report No. NWBRO1-001 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 20.1 64.8 16.7 41.3 18.2 16.6 36.2 32.4 59.4 54.6 ' 26.2 37.6 16.8 54.9 41.7 24.6 32.5 PFOA Concentration* 4.77 5.35 3.23 6.21 3.30 2.66 8.05 5.55 4.88 5.24 3.36 4.49 3.01 4.53 4.42 2.40 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(1.60) 2.71 <LLOQ(1.60) <LLOQ(1.60) 4.97 1.71 18.3 23.8 2.62 <LLOQ(1.60) 2.77 1.95 5.31 2.39 <LLOQ(1.60) 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) M556 Concentration* 5.46 4.43 <LLOQ(2.50) 3.34 <LLOQ(2.50) <LLOQ(2.50) 4.3 2.88 6.53 12 <LLOQ(2.50) 4.27 2.79 4.95 3.7 <LLOQ(2.50) 3.24 M570 Concentration* 2.87 <LLOQ(1.00) <LLOQ(l .00) 2.98 <LLOQ(1.00) <LLOQ(1.00) 4.88 1.23 3.52 4.1 <LLOQ(1.00) 22.7 2.28 <LLOQ(1.00) 1.13 1.68 17.1 * 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 75 Northwest Bioanalytical Study No. NW BS00-088 Report No. NWBRO1-001 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 1611 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 Concentration* 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 Concentration* 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) M556 Concentration* <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(1.00) 15.2 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 1.61 2 <LLOQ(1.00) <LLOQ(1.00) 1.49 <LLOQ(l .00) 5.75 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). * * Results are front 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 76 Northwest Bioanalytical Study No. NW BS00-088 Report No. NWBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. 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 11.5 15.0 20.5 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(l .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(1.60) 6.09 2.15 PFOSA Concentration* <LLOQ(D00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) 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(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) 3.91 <LLOQ(.1.00) <LLOQ(1.00) <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) o f the target concentration. The statistical error o f 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(1.36) 8.96 <LLOQ(1.36) 4.17 38.5 <LLOQ(1.36) 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* 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(1.00) 3.77 3.43 3.47 1.21 <LLOQ(1.00) 2.82 2.74 2.65 2.97 * 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 78 Northwest Bioanalytical Study No. NW BS00-088 Report No. NWBR01-01 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(1.36) <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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* 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(1.00) <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 * 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 79 Northwest Bioanalytical Study No. NW BS00-088 Report No. NWBRO1-001 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(1.36) 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) M556 Concentration* 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 i 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(1.00) 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 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 80 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBRO1-001 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 PFHS Concentration** Concentration* 4.15 1.51 3.82 2.43 10.1 7.12 7.17 90.8 4.87 3.72 3.94 4.98 8.89 15.8 5.69 7.12 4.61 2.83 <LLOQ(2.88) <LLOQ(2.41) 3.06 2.36 4.31 15.4 5.54 2.21 5.30 3.75 6.65 8.06 19.5 20.4 6.63 4.84 PFOSAA 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(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ( 1.00) 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 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 81 Northwest Bioanalytical Study No. NW BS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. 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(1.36) 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) . <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <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 * 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 82 Northwest Bioanalytical Study No. NW BS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 2158 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(1.60) 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(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** M556 Concentration* 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 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 coll 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) o f the target concentration The statistical error o f any individual result may exceed the QC acceptance criteria. Page 83 Northwest Bioanalytical Study No. NW BS00-088 Report No. NWBRO1-001 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(1.92) 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(1.36) 4.73 <LLOQ(1.36) 3.79 3.79 2.25 <LLOQ(1.36) PFOSAA Concentration* <LLOQ(1.60) 2.95 2.92 <LLOQ(1.60) 3.69 2.96 3.21 <LLOQ(1.60) 4.18 <LLOQ(1.60) 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(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** M556 Concentration* <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* 136 2.32 2.93 <LLOQ( 1.00) <LLOQ(1.00) 1.85 2.55 <LLOQ(1.00) 1.29 3.59 2.48 1.2 4.55 <LLOQ(1.00) <LLOQ(l .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 must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 84 Northwest Bioanalytical Study No. NWBS00-O88 Report No. NWBRO1-001 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(1.92) 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(l,36) 4.20 27.2 10.5 <LLOQ(1.36) PFOSAA Concentration* <LLOQ(1.60) 13.1 <LLOQ(1.60) 2.19 <LLOQ(1.60) 2.93 5.02 6.43 <LLOQ(1.60) 4.39 2.50 3.41 5.19 10.3 7.78 3.39 <LLOQ(l .60) 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(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.0G)** <LLOQ(1.00)** <LLOQ(1.00)** 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 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected fun (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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 85 Northwest Bioanalytical Study No. NW BS00-088 Report No. NWBRO1-001 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 2517 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 54.1 51.6 30.2 38.6 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(1.60) 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(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) M556 Concentration* 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) 2.81 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(1.00) 3.9 * 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 86 Northwest Bioanalytical Study No. NW BS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 2526 2528 2531 2567 2570 2575 2577 2584 2585 2590 2593 2597 9433 9434 9435 9436 9437 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(1.92) 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(1.36) <LLOQ(1.36) 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(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(1.00) <LLOQ(1.00) <LLOQ(1.00) <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(l .00) 34.4 4.19 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.00) <LLOQ( 1.00) 2.92 22.2 10.8 <LLOQ(1.00) 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 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 87 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 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 15.0 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(2.41) 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(2.60) 4.81 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) * 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 88 Northwest Bioanalytical Study No. NW BS00-088 Repon No. NWBRO1-001 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) 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 89 Northwest Bioanalytical Study No. NW BS00-088 Report No. NWBRO1-001 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) * 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) o f the target concentration. The statistical error o f 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. NW BS00-088 Repon No. NWBRO1-001 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 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) o f the target concentration. The statistical error o f any individual result may exceed the QC acceptance criteria. Page 91 Northwest Bioanalytical Sample No. 2168 Table 23. Repeat Analysis Table for PFOS Study No. NW BS00-088 Report No. NWBRO 1-001 Treatment Ped Time Oh Original Cone, ppb Original Reason Reassay Reassay Reported Run for Cone. Run Cone. Number Reassay ppb Number ppb >ULOQ(414) 10 1 515 14 515 Reason for Reported Cone. 1 Sample No. 2168 Table 24. Repeat Analysis Table for PFHS Treatment Ped Time Oh Original Cone, ppb Original Run Number >ULOQ(523) 10 Reason for Reassay 1 Reassay Cone. ppb 712 Reassay Reported Run Cone. Number ppb 14 712 Reason for Reported Cone. 1 REASONS FOR REASSAY: 1). Greater than the ULOQ. REASONS FOR REPORTED CONC: 1). Original result outside of quantitation range. Reassay results reported. Page 92 Northwest Bioanalytical Study No. NWBS00-0S8 Report No. NWBROI-OOl Figure I. Representative Calibration Curve for PFOS Analytical Run 7 analyzed on 09-Nov-2000 Calibration Standards for PFOS (ny/niL) Regression Method QUADRATIC * Weighting Factor * l/X**2 Quadratic Limit * 2000 Figure 2. Representative Calibration Curve for PFOA Analytical Run 7 analyzed on 09-Nov*2000 Calibration Standards for PFOA (ng/mL) Regression Method " QUADRATIC Weighting Factor* I/X**2 Quadratic Limit * 3190 Instrument Response Page 93 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBRO1-001 Figure 3. Representative Calibration Curve for PFHS Analytical Run 7 analyzed on D`)-Nov2000 Calibration Standards for PFHS (ng/mL) Regression Method * QUADRATIC Weighting Factor l/X**2 Quadratic Limit * 1410 Instntment Response Figure 4. Representative Calibration Curve for PFOSAA Analytical Run 7 analyzed on 09-Nov-2000 Calibration Standards for PFOSAA (ng/mL) Regression Method - QUADRATIC - Weighting Factor * l/X**2 Quadratic Limit **4160 Instrument Response Page 94 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBROl-OOl Figure 5. Representative Calibration Curve for PFOSA Analytical Run 7 analyzed on 0*>-Nov-2000 Calibration Standard for PFOSA (ng/mL) Regression Method * QUADRATIC Weighting Factor l/X**2 Quadratic Lim it 2S30 Instnrmcnl Response Instrument Response Figure 6. Representative Calibration Curve for M556 Analytical Run 7 analyzed on 09-Nov-2000 Calibration Standards for M556 (ng/mL) Regression Method QUADRATIC Weighting Factor* l/X '*2 Quadratic Limit * *1620 0 50 100 150 200 250 300 350 400 450 500 Nominal Cone. (ng/mL) Page 95 Northwest Bioanalytical Study No. NWBS00-0S8 Report No. NWBRO1-001 Figure 7. Representative Calibration Curve for M570 Analytical Run 7 analyzed on 09-Nov-2000 Calibration Standards for MS70 fng/mL) Regression Method QUADRATIC - Weighting Factor I/X **2 Quadratic Limit *23900 Instrument Response Page 96 Northwest Bioanalytical Figure 8. Human Serum Blank for PFOS Study No. NWBS00-088 Report No. NWBR01-001 Internai Standard: THPPOS Use Area Absolute Rtention Time xpected RT 4:54 Currant Method Noise Thres. 5.0 5.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 12 12 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 *0008807-012 7 0 1 2 S0088 CONTROl_BCANK 1 Thu. Nov 9. 2000 9:08 PM 8:59 in 1 period Na Comment 306 1: 8:59 MRM. 571 scans 499.0->80.0 Area 26722 HetQht 1744 Start Time End Time Integration Width Retention Time Integration Type itiikiM a 4:30 5:17 0:46.3 4:49 A-BV mm 101 t :35 201 3:10 intensity : 1746 cps 501 7.54 Time) -c ITHPFOS use as Internal Standard Expected RT 4:15 ] Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $0008807-012 7 012 S00088 C0NTR0LJ5LANK 1 No Comment Thu. Nov 9. 2000 9:06 PM a: 59 in 1 penod 1: 8:59 MRM, 571 scans 427.0->407.0 Area 0 Height 0 Start Time End Time Integration Width Retention Time intecration Tvoe imwMfi 0:00.0 0:00.0 0:00.0 0:00.0 EEI intensity : 2 5 ops Page 97 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Figure 9. Human Serum Blank for PFOA jHFA ------------------------- internal Standara: fH P F O S Use Area Absolute Retention Time Expected R T 4:27 ') Current Method Noise Three. 1.0 t.o Quant Thres. ~<5T 0.9 Min. Width Mult width Base, width ISO R T Win. {secs) Smooth 20 1 50000807*012 7 012 S0088 CONTRO (._6LANK f Thu. Nov 9. 2000 9:08 PM 3:59 in 1 period 1: 8:59 MRM . 571 scans 413.0^169.0 Area HaglK 2655 m Start Time End Time Integration Width Retention Time Integration Type 4:13 4:46 0:32.1 4.-26 A * 08 EE! 100 90 SO 70 60' 30lo so 20 10 0 .101 1:33 intensity : 227 cps - ft i 428 ^ r 111 20t 3:10 301 4:45 401 6:19 SOI 7:54 Ticmaneil--y ITHPFOS use as internal Standard Expected RT 4:15 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S0008807-012 7 012 SOOO08 C O N T R O L _ B L A N K 1 Thu. Nov 9. 2000 9:08 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 427.0->407.0 Area 0 Heiqhi 0 Start Time End Time Integration Width Retention Time imeoration Type iti+H H & ii 0:00.0 0:00.0 0:00.0 0:00.0 s ty I00-1 90 SO TO- 97 60 SO 20 69 40 30 20 10 O' 101 I :33 No Comment 287 201 3:10 301 4:45 intensity : 25 cps 438 480 460:119 501 7:54 Cnr " Page 98 Northwest Bioanalytical Sturiy No. NWBSOO-088 Report No. NWBR01-00I Figure 10. Human Serum Blank for PFHS Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 3:37 Current Method Noise Thres. 3.0 3.0 Quant Thres. 0.5 0.5 Min. Width 44 MuIt. Width 12 12 8ase. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $0008807*012 7 012 S00068 CONTRL.BLANK 1 Thu, Nov 9. 2000 9:08 PM a:59 in 1 period No Comment 1: 8:59 MRM. 571 scans 399.0->80.0 Area 1410 Height 126 Start Time End Time Integration Width Retention Time Integration Tyoe l+HMMfll > CD CD 3:29 3:59 0:30.3 3:46 IKISA ITHPFQS use as Internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 10 8ase. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S0B807-O12 7 012 S00088 Cl Thu, Nov 9. 2000 9:08 PM 8:59 in 1 period 100-j 1: 8:59 MRM. 571 scans 90 427.0*>407.0 Area 0 Height o Start Time End Time Integration Width Retention Time Integration Tvpe IMHHMi 0:00.0 0:00.0 0:00.0 0:00.0 s jj 90 70 97 60 50*.2 0 69 40 30 20 10 0 101 t :35 No Comment 287 201 301 3:10 4:43 intensity : 23 cps 433 480 460:119 Soinp Time . Page 99 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Figure 11. Human Serum Blank for PFOSAA IPFOSAA Internai Standard: THPFOS Usa Area Absolut Rtention Time Expected RT 5:56 I Current Method Noise Thres. 4.0 4.0 Quant Thres. 1.5 t.5 Min. Width 3 3 Mult. Width 13 13 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $0008807*012 7 012 S00088 CONTROL.BIANK t Thu. Nov 9. 2000 9:08 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 584.1->419.1 No Comment Area 1020 Heiqht 129 Start Time End Time Integration Width Retention Time loteoration Type Itl+HHifl 5:51 fl:06 0:15.1 5:58 A-BB QU intensity : 162 cps ITHPFOS use as Internai Standard Expected RT 4:t5 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S0G8Q07-012 7 012 S00088 CONTROL^BLANK 1 No Comment Thu. Nov 9. 2000 9:08 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 427.0->407.0 Area 0 Heioht 0 Start Time End Time Intearation Width Retention Time Intearation Type ItliM H iil 0:00.0 0:00.0 0:00.0 0:00.0 Page 100 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Figure 12. Human Serum Blank for PFOSA Ip f o s a Internai Standard: THPF0S Use Area Absokiie Rtention Time Expected RT 3:35 Current Method Noise Thres. 3.0 3.0 Quant Thres. 0.3 0.3 Min. Width 5 5 Mult Width 10 10 Base. Width ISO 150 RT Win. (secs) 20 20 Sm ooth 1 50008807-012 7 012 S00088 CONTROL_BLANK 1 No Comment Thu. Nov 9. 2000 9:08 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 498.0->78.0 Area 3039 Height 202 Start Time End Time Intearation Width Retention Time Integration Type im kM ifai 5:11 5:50 0:38.8 5:42 A -W ms intensity : 209 cps 362 S&Ti r-- Timeji ITHPFOS use as internal Standard Expected RT 4:15 3 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Mm. Width 3 3 Mult Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 50008807-012 7 012 S0088 CONTROL_SLANK 1 No Comment Thu. Nov 9. 2000 9:08 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 427.0*>407.0 Area 0 Height 0 Start Time End Time Intearation Width Retention Time Integration Tyoe Itl+hW il 0:00.0 0:00.0 0:00.0 0:00.0 E ffl intensity : 23 cps Page 101 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Figure 13. Human Serum Blank for M556 IMS56 Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5:25 I Current Method Noise Thres. 0.4 0.4 Quant Thres. 0.1 0.1 Min. Width 33 Mull Width 10 10 8ase. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $0008807*012 7 012 S00088 CONTROL_BLANK 1 No Comment Thu. Nov 9, 2000 9:08 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 556.0->498.0 Area 155 Hekjht 55 Start Time End Time Inteqration Width Retention Time intearation Tvoe > CD CD 5:20 5:27 0:07.8 5:25 100 90 SO TO* 60 30 40 30 20 344 230 293 10 0- *7! 201 301 401 1 :33 3:1 0 4 :4 3 6:19 intensity : 37 cps 501 5cri 7 :5 4 Time| ITHPFOS . use as Internal Standard Expected RT 4:1S I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $0008807*012 7 012 S00088 CONTROL_BLANK 1 No Comment Thu. Nov 9. 2000 9:08 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 427.0->407.0 Area 0 Hekjht 0 Start Time End Time Intearation Width Retention Time Intearation Tvoe Itl+ M M B l 0:00.0 0:00.0 0:00.0 0:00.0 lE O Page 102 Northwest Bioaiialytical Study No. NWBS00-088 Report No. NWBRO1-001 Figure 14. Human Serum Blank for IVI570 internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5:38 Current Method Noise Thres. 3.0 3.0 Quant Thres. 0.5 0.5 Min. Width 5 5 Mult. Width 15 15 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S0008807-012 7 012 S00088 C0NTR0L.8LANK 1 Thu. Nov 9. 2000 9:08 PM 8:59 in 1 period No Comment 1: 8:59 MRM. 571 scans 570.0- >419.1 Area 1074 heiaht 144 Start Time End Time Inteoration Width Retention Time Inteoration Type im H H a 0 CD < 5:37 5:56 0:18.9 5:44 mm intensity : 151 cps ifHPFOS use as Internal Standard Expected RT 4:1S Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mull Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $00088074)12 7 012 S00088 CONTROLALANK 1 No Comment Thu. Nov 9. 2000 9:08 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 427.0->407.0 Area 0 Heiaht 0 Start Time End Time Inteoration Width Retention Time Inteoration Tvoe itiew H w 0:00.0 0:00.0 0:00.0 0:000 m intensity : 25 ops Page 103 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBROl-OOl Figure 15. Human Serum Blank with Internal Standard (QCO) for PFOS Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 4:54 Current Method Noise Thres. 5.0 5.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult Width 12 12 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 30008807-001 7 001 S00088 QCO 1 Thu. Nov 9, 2000 7:00 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 499,0>80.0 No Comment Area 39395 Height 2605 Start Time End Time Integration Width Retention Time Integration Type 4:34 5:32 0:57.7 4:50 A-8V intensity : 2606 ops T--^ M --- p 401 501 Sc*. r r 6:19 7 5 4 Timefe ITHPFOS use as Internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 SOOQ087-OO1 7 001 S00088 QCO t No Comment Thu. Nov 9.2000 7:00 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 100 90' 427.0->407.0 Area 273196 Height 35433 Start Time End Time Integration Width Retention Time Integration Type ItliH H I CD CD < 4:12 4:40 0:33.1 4:26 Elffl 30 70 60 50 40 30 20 10* 0 101 1 -.35 201 281 301 4:45 intensity : 35434 cps 401 SCI Scrii- 6:19 7:54 Tim*I. Page 104 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-00I Figure 16. Human Serum Blank with Internal Standard (QCO) for PFOA (PFOT----------------------------------- 1 J Internal Standard: THPFO S Absolute Retention Time expected RT 4:27 Current Method Noise Thres. 1.0 t.O Quant Thres. 0.9 0.9 Min. Width 33 M ull Width 99 Base. Width l 150 RT Win. (secs) 20 20 Smooth 1 1 soooaao7-ooY 7 001 SOO80 QCO 1 (t h p f q s " use as Internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 02 0.2 Min. Width ___ 3 Mult. Width _10_ 3 10 Base. Width 150 150 RT Win. (secs) __ 20 20 Smooth 1 S0008807-001 7 001 S00088 QCO 1 Thu, Nov 9, 2000 7:00 PM 6:59 in 1 period 1: 8:59 MRM. 571 scans 427.0->407.0 No Comment Area 273196 Heiqht 35433 Start Time End Time inteoration Width Retention Time Inteoration Type Itl+kM l 4:12 4:46 0:33.1 4;25 A-BB IE n intensity : 35434 cps Page 105 Northwest Bioanalytieal Study No. NWBS00-088 Report No. NWBR0I-00I Figure 17. Human Serum Blank with Internal Standard (QCO) for PFHS IPFHS Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 3:37 I Current Method Noise Thres. 3.0 3.0 Quant Thres. 0.5 0.5 Min. Width 44 Mutt. Width 12 12 Base. Width 150 ISO RT Win. ( s e e s ) 20 20 Smooth 1 1 7 001 S00088 QCO 1 Thu, Nov 9. 2000 7:00 PM 3:59 in 1 period 1: 8 :5 9 M R M , 5 7 1 scans 399.0>60.0 intensity : 200 cps Area 1769 HeiQht 193 Start Time End Time (ntearation Width Retention Time Integration Type itm sw M 3:39 3:59 0:19.9 3:50 fi SB E itn 412 U j jtiiiijjifti/.ip i iA tOt 1:33 20t 3:10 501 4:45 401 6:19 501 Sc-Mi 7:54 Timel ITHPFOS use as internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Mm. width 3 3 Mult Width 10 10 Base. Width 1S0 1S0 RT Win. (secs) 20 20 Smooth 1 1 <0008807-001 7 001 S00088 QCO 1 No Comment Thu. Nov 9. 2000 7:00 PM 3:59 in 1 period 1: 8:59 MRM. 571 scans 427.0->407.0 Area 273196 Height 35433 Start Time End Time Integration Width Retention Time Integration Type ItNHHMiBl c0o0 < 4:12 4:46 0:33.1 4:26 saw S'O SO- " TO SO- 30 40 30 20 10 0-1----.--- ,--- 1----1---- 101 201 1:33 3:10 301 4:45 intensity : 33454 cps 401 ' SOl" 6:1$ 7:5- Page 106 Northwest BLoaiialyticul Study No. NWBS00-088 Report No. NWBRO1-001 Figure 18. Human Serum Blank with Internal Standard (QCO) for PFOSAA IPFOSAA Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5:56 | Current Method Noise Thres. 4.0 4.0 Quant Thres. 1.5 1.5 Min. Width 3 3 Mult. Width 13 13 Base. Width 150 150 RT Win. (secs) 20 20 Smooth t 1 S00aa07-001 7 0 0 1 sooosa QCO 1 Thu. Nov 9. 2000 7:00 PM 8:59 in 1 period 1: S:59 MRM, 571 scans 584.1-419.1 No Comment Area 0 Hetaht 0 Start Time End Time Integration Width Retention Time Integration Type Itl+MHffl 0:00.0 0:00.0 0:00.0 0:00.0 U fi intensity : 92 cps ITHPFOS use as Internal Standard Expected RT 4:15 Current Method Noise Thres. 1 0 .0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S0008807-001 7 001 S00008 QCO 1 No Comment Page 107 Northwest Bioaualytieal Study No. NWBS00-088 Report No. NWBRO1-001 Figure 19. Human Serum Blank with Internal Standard (QCO) for PFOSA IPFOSA " ' ' Internai Standard: THPFOS Use Area Absohite Rtention Time Expected RT 5:35 I Current Method Noise Thres. 3.0 3.0 Quant Thres. 0.3 0.3 Min. Width 5 5 Mult. Width 10 10 Base. Width 150 150 RTWin. (secs) 20 20 Smooth 1 1 soooaes000aa07-00 7 001 QCO 1 No Comment Thu. Nov 9. 2000 7:00 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans too90- 498.0*>78.0 -J < 00 Area 0 HeiQht 0 Start Time End Time Integration Width Retention Time Integration Type 0:00.0 0:00.0 0:00.0 0:00.0 HD 6040- 561 intensity : 59 ops JTHPFOS use a s internai Standard Expected RT 4:15 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult Width 10 10 Base. Width 150 150 RTWin. (secs) 20 20 Smooth 1 1 $0008807-001 7 001 S00088QC0 1 Thu. Nov 9. 2000 7:00 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 427.0->407.0 No Comment Area 273198 HeiQht 35433 Start Time End Time Integration Width Retention Time Integration Type itkH fld 4:12 4:46 0:33.1 4:26 A-BB eq intensity : 35434 cps Page 108 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Figure 20. Human Serum Blank with Internal Standard (QCO) for 1VI556 IM556 Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5:25 I Current Method Noise Thres. 0.4 0.4 Quant Thres. 0.1 0.1 Mm. Width 3 3 Mutt. Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S0006807-001 7 001 S 0 0 0 8 8 QCO 1 No Comment Thu. Now 9. 2000 7:00 PM 8:59 in 1 period 100- 1: 8:59 MRM. 571 scans 90- 556.0*>498.0 Area 0 Height 0 Start Time End Time Intearation Width Retention Time Integration Type iti+wHin 0:00.0 0:00.0 0:00.0 0:00.0 mm 00 70- 29 605040- 2- 10 0 101 I :33 intensity : 17 ops 238 2 0 9 391 4 16 201 3:10 301 4:45 401 6:19 501 7:54 SC4fir-- Time & |TH P " " use as Internal Standard ~l Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mull Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 0008807*001 7 001 S00088 QCO 1 No Comment Thu. Nov 9. 2000 7:00 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 90- 427.0->407.Q Area 273196 Height 35433 Start Time End Time intearation Width Retention Time Intearation Tvoe Itl4l-HH^| 4:12 4:46 0:33.1 4:28 A *BB HQ SO- 70 60 50 40 30 20 10- 0-I---.---- 1--- --- 1----r"* ?" 101 201 301 1:35 3:10 4:4! intensity : 35454 ops 401 6:19 501 7:54 bO^fl r^-- TimeJ.-: Page 109 Northwest Bioanalytieal Study No. NWBSOO-088 Report No. NWBROl-Ol Figure 21. Human Serum Blank with Internal Standard (QCO) for M570 IM570 Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5:38 | Current Method Noise Thres. 3.0 3.0 Quant Thres. 0.5 0.5 Min. Width 55 Mult. Width 15 15 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $0008807*001 7 001 S00088 QCO 1 No Comment ITHPFS use as Internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 sOOO8807-001 7 001 S00088 QCO 1 No Comment Thu. Nov 9, 2000 7:00 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 427.0->407.0 Area 273196 HeiQht 35433 Start Time End Time Inteoration Width Retention Time Inteoration Tvoe ITT3W B <CDO < 4:12 4:48 0:33.1 4:26 EQ] lOO-i 90 80 70 80 50 40 30 20 10 101 2010-1------ .------ 1------ .------ ,-- 1:35 3:10 301 4:45 intensity : 35434 ops 401 6:19 SOI 7:54 Soaftt" " Time) < Page 110 Northwest Bioanalytieal StiKly No. NWBSOO-088 Report No. NWBRO1-001 Figure 22. Low Standard (3.94 ppb) for PFOS Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 4:54 Current Method Noise Thres. 5.0 5.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 12 12 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S000aa07*002 7 002 sooosa Std1 1 1 Thu. Nov 9. 2000 7:11 PM 9:59 in 1 period 1: 8:59 MRM. 571 scans 499.0>80.Q Area 48519 Hekjht 3423 Start Time End Time Intecration Width Retention Time Intearation Type itiiW M B 4:31 5:28 0:56.7 5:01 A-BV mm No Comment intensity : 3423 cps 313 - f ---r--* 1 t o i 201 301 401 501 dCftp I :35 3:1 0 4:45 6:19 7:54 Tim;: ITHPFOS use as Internal Standard Expected RT 4:15 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 MulL Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $0008607*002 7 002 S000Q8 Std1 1 1 Thu. Nov 9. 2000 7:11 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 427.0->407.0 Area 270289 Height 36113 Start Time End Time Intearation Width Retention Time intearation Type ItliH H B 4:12 4:47 0:35.0 4:25 A *BB mm No Comment Page 111 Northwest Bioanalytieal Study No. NWBS00-088 Report No. NWBROl-OOl Figure 23. Low Standard (1.92 ppb) for PFOA |rrM Internai Standard: TH PPO S Use Area Absolute Retention Time Expected R T 4:27 Current Method Noise Thres. 1.0 1.0 Quant Thres. . 0.9 Min. Width 33 Mutt. Width 99 Base. Width r a r 150 RT Win. (sees) 0 20 Smooth 11 $0008807-002 7 002 S00088 SW1 t 1 Thu. Nov 9. 2000 7:11PM 8:59 in 1 period 1: 8:59 M RM , 571 scans 4t3.0>t69.0 Area 9583 Height 722 Start Fune End Time Integration Width Retention Time Integration Type 4:02 4: 0:52.9 4:28 75 SB No Comment intensity : 734 cps ITHPFOS use as Internal Standard Expected RT 4:15 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mull Width 10 10 8a$e. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S0008807-002 7 002 S00088 Std1 1 1 Thu. Nov 9. 2000 7:11 PM 8:59 in 1 period 100-1 1: 8:59 MRM, 571 scans 90- 427.0->407.0 Area 270289 Heiqht 36113 Stan Time End Time integration Width Retention Time Integration Tvoe - Itl+MMH co CD < 4:12 4:47 0:35.0 4:25 00 80 7060- 40- 2010 0 No Comment 230 10t 201 301 I :33 3 :1 0 4 :4 3 intensity: 36114 cps 401 6:19 501 aCjftp ~ 7:54 Timej..''. Page 112 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Figure 24. Low Standard (1.36 ppb) for PFHS IPFHS Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 3:37 I Current Method Noise Thres. 3.0 3.0 Quant Thres. 0.5 0.5 Min. Width 4 4 Mult, width 12 12 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $0008807-002 7 002 S00088 Sld1 1 1 No Comment ITHPFOS use as Internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 150 RT Win. (secs). 20 20 Smooth 1 1 S0008807-002 7 002 S00088 Stdt 1 t Thu. Nov 9. 2000 7:1 1 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 427.0-407.0 Area 270289 Height 36113 Start Time End Time Integration Width Retention Time Integration Tvoe 4:12 4:47 0:35.0 4:25 A-BB No Comment intensity : 36114 cps Northwest Btoaiialytical Study No. NWBS00-088 Report No. NWBROl-OOl Figure 25. Low Standard (1.60 ppb) for PFOSAA IPFOSAA Internai Standard: THPFOS Use Area Absolute Retention Time Expected RT 5:56 I Current Method Noise Thres. 4.0 4.0 Quant Thres. 1.5 1.5 Min. Width 3 3 Muit. Width 13 13 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S0006807-002 7 002 S00088 Std1 1 1 No Comment Thu. Nov 9,2000 7:11 PM 8:59 in 1 period 100 1: 8:59 MRM. 571 scans 584.1->419.1 Area 8684 Heiqht 727 Start Time End Time Intearation Wdth Retention Time Intearation Type iti+W H S 5:37 8:07 0:30.3 5:56 A-as 90 30 70 SO SO- 40 30 20 10 0-!ilAy.itigli >1fth,,slkii 101 2I t :3S 3 :1 0 intensity : 7S0 cps 376 SOI SiijTii-- 7 :54 Tim* : ITHPFOS use as Internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Muit. Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $0008607-002 7 002 S00068 Std1 t 1 Thu. Nov 9. 2000 7:1 1 PM 8:59 in 1 period too 1: 8:59 MRM. 571 scans 427.0->407.0 Area 270289 Heiqht 36113 Start Time End Time intearation Width Retention Time Intearation Tyoe ItllM H H 4:12 4:47 0:35.0 4:25 A-BB m 90- ao- 70 60 50 40 30 20 10 0 No Comment 10! 1 :35 201 3:10 301 4:43 intensity : 36114 cps 460:1! 9' SOI Sonp-- Tin*.*] : Page 114 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR0I-001 Figure 26. Low Standard (1.00 ppb) for PFOSA IPFOSA ' Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5:35 Current Method Noise Three. 3.0 3.0 Quant Thres. 0.3 0.3 Min. Width 5 5 MulL Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S00Q8807-0O2 7 002 S00088 Std1 1 1 Thu. Nov 9. 2000 7:1 1 PM 8:59 in t period 1: 8:59 MRM, 571 scans 498.0->78.0 Area 23612 Heiqht 2540 Start Time End Time intearation Width Retention Time Intearation Type 5:15 5:55 0:39.7 5:41 A-BB so No Comment Intensity : 2543 cps ITHPFOS ' use as internal Standard Expected RT 4:15 Current Method Noise Three. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 MulL Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S008807-002 7 002 S00088 Std1 1 1 Thu. Nov 9. 2000 7:11 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 427.0-407.0 Area 270289 HeiQht 36113 Start Time End Time Intearation Width Retention Time Intearation Type itN k H rtl C(0O < 4:12 4:47 0:35.0 4:25 00 No Comment intensity : 36 M 4 cps Page 115 Northwest Bioanalytieal Study No. NWBS00-088 Report No. NWBR1-001 Figure 27. Low Standard (2.50 ppb) for V556 Internai Standard: THPFOS Use Area Absolute Retention Time Expected RT 5.42 Current Method Noise Thres. 0.4 0.4 Quant Thres. Min. Width 0.1 3 0.1 a Mult, width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S0G88O7-O3 7 003 S00068 Std2 1 1 Thu, Nov 9. 2000 7:23 PM 8.98 in 1 period 100- 1: 0.98 MRM. 571 scans 90- 55fl.0->498.0 30- Area 5991 Height 769 Start Time End Time integration Width Retention Time Integration Tvoe 5.15 5.63 0.47 5.44 A -88 70so3040- No Comment ITHPFOS use as Internal Standard Expected R T 4.25 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 to Base. Width 150 150 RTWIn. (secs) 20 20 Smooth 11 S0008807-003 7 003 S00088 Std2 1 1 No Comment Page 116 Northwest Bioaiuilytical Study No. NWBS00-088 Report No. NWBR01-001 Figure 28. Low Standard (1.00 ppb) for M570 |MS7 Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5:38 I Current Method Noise Thres. 3.0 3.0 Quant Thres. 0.5 0.5 Min. Width 5 5 Mull Width 15 15 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 SQ088Q7-002 7 002 S00088 Std1 1 1 Thu. Nov 9, 2000 7:11 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 57Q.0->419.1 No Comment Area 9166 Hekjht 1238 Start Time End Time Intearation Width Retention Time Intearation Type fti+ k w a l 5:28 5:56 0:27.4 5:43 A-BB 0 B intensity : 12 4 6 cps ITHPFOS use as internal Standard Expected RT 4:15 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S008807-002 7 002 S00088 Stdl 1 1 Thu. Nov 9. 2000 7:1 1 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 427.0-407.0 Area 270289 Heiqht 36113 Start Time End Time Intearation Width Retention Time Intearation Tvoe 4:12 4:47 0:35.0 4:25 A-BB No Comment intensity : 3 6 1 14 ops Page 117 Northwest Bioanalytieal Study No. NWBS00-088 Report No. NWBRO1-001 Figure 29. High Standard (414 ppb) for PFOS IPFOS ' Internai Standard: THPFOS Use Area Asohite Rtention Time Expected RT 4:54 Current Method Noise Three. 5.0 5.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mutt. Width 12 12 Base. Width 150 150 RT Win, (secs) 20 20 Smooth 1 1 S008607-010 7 010 S00088 Std9 1 1 Thu, Nov 9. 2000 8:45 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 499.0*>80.0 Area 3453475 HeiQht 285223 Start Time End Time tntearation Width Retention Time Inteoration Tvoe 4:22 8:04 1:42 5:01 > CD < 100 90 SO TO60 S0 40 30 20 10 0- No Comment 101 201 I :33 3:1 0 intensity : 235227 ops 313 401 6:13 501 7:54 ITHPFOS use as internal Standard Expected RT 4:15 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mutt. Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S008807-010 7 010 S00068 Std9 1 1 No Comment Page 118 Northwest Bioanalytical Study No. NWBS00-08S Report No. NWBRO1-001 Figure 30. High Standard (481 ppb) for PFOA |KrUA ' "* Internal Standard: THPFOS Use Area *} Noise Thres. Quant Thres. Min. Width Current Method 1.0 1.0 0.9 0.9 33 AOsokjte Retention Time Expected RT 4:27 Mult. Width Base. Width R T Win. (secs) 99 iM 1S0 i t 20 Smooth i 1 7 010 S0008S Stdfl 1 1 ITHPFOS use as internal Standard Expected RT 4:! 5 1 Current Method Noise Thres. 10.Q 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S008807-010 7Q1OSOOO80SUJ9 1 1 Thu. Nov 9. 2000 8:45 PM 8:59 in 1 period 100-1 1: 8:59 MRM. 571 scans 90- 427.0-407.0 Area 225323 Heiqhl 28708 Start Time End Time Intearation Width Retention Time Intearation Tv m 4:12 4:46 0:34.0 4:26 A 88 30 70SO- 40- ItH W H S i S D 2100-` No Comment 101 201 ! :3i 3 :1 0 30! 4.43 intin si ty : 2 3 7 1 0 cps 401 3:19 501 `aC-jfii ~~ 7:5 4 Time] r. Page 119 Northwest Bioanalytieal Study No. NWBSOO-088 Report No. NWBRO1-001 Figure 31. High Standard (523 ppb) for PFHS |Pf~HS internai Standard: THPFOS Use Area Absolule Rtention Time Expected RT 3:37 I Current Method Noise Thres. 3.0 3.0 Quant Thres. 0.5 0.5 Min. Width 44 Mull width 12 12 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $0008807*01Q 7 010 S00088 Std9 t 1 Thu. Nov 9, 2000 8:45 PM 8:59 in 1 period 1: 3:59 MRM, 571 scans 399.0->80.0 Area 2879090 Height 274134 Start Time End Time Inteoration Width Retention Time Integration Tyoe L tum a 3:20 4:46 1:25 3:48 A BV HGD No Comment intensity : 274143 cps ITHPFOS use as internai Standard Expected RT 4:l 1 Current Method Noise Three. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 SOOO08O7-O1Q 7 010 S00088 Std9 1 1 No Comment Thu. Nov 9. 2000 8:45 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 427.0->407.0 Area 225323 Height 28708 Start Teme End Time Integration Width Retention Time integration Tvoe rffTPsw s 0m < 4:12 4:46 0:34.0 4:26 cara so so- 70- so so- 40 30 20 10- o-l-- i-- -- i-- i-- r^p- io i 201 301 1:35 3:10 4:4! intensity : 23710 cps 401 6 :1? SOI Soabr-- 7:5 4 Tirne| : Page 120 Northwest Bioanalytieal Study No. NWBS00-088 Report No. NWBR0I-001 Figure 32. High Standard (501 ppb) for PFOSAA (PFOSAA Use Area Absolute Retention Time Expected RT 5:56 i Current Method Noise Thres. 4.0 4 0 Quant Thres. 1.5 1.5 Min. Width 3 3 Mull Width 13 13 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S0O0S807-O10 7 010S00088 Std9 1 1 Thu. Nov 9, 2000 8:45 PM 8:59 in 1 period 1: 8:50 MRM. 571 scans 584.1->419.1 Area 1556445 Height 774924 Start Time End Time Integration Width Retention Time Integration Type LtlflH a > ID < 5:29 6:52 1:23 5:56 E lB No Comment intensity: 174931 cps ITHPFOS use as Internai Standard Expected RT 4:15 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S003807-0I0 7 010 S0088 Std9 1 1 Thu. Nov 9. 2000 6:45 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 427.0->407.0 Area 225323 Height 28708 Start Time End Time Integration Width Retention Time integration Type 4:12 4:46 0:34.0 4:26 A . SB tOO-i 90 30 70 30 50 40- SO SO- 10- No Comment 281 101 201 1:35 3:10 301 4;45 intensity : 23710 cps 400:119 301 7:34 Scurii--- Ttmej : Page 121 Northwest Bioanalytieal Study No. NWBSOO-088 Report No. NWBRO1-001 Figure 33. High Standard (500 ppb) for PFOSA 1PFOSA Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5.35 I Current Method Noise Thres. 3.0 3.0 Quant Thres. 0.3 0.3 Min. Width 5 5 Mult Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 50008807*010 7 010 S00088 Sld9 1 1 Thu. Nov 9. 2000 8:45 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 90' 498.0->78.0 Area 7776824 HeiQht 682348 Start Time End Time intearatian Width Retention Time Integration Type 5:12 8:39 1:27 5:41 30 70 60- so- 40 30 m + H H id s f f l 20 10 0 No Comment 101 201 1:35 3:10 intensity : $32470 cps 31 4:45 401 6:19 501 S c if tr r 7:54 Time| >a CCOD << ITHPFOS " use as Internal Standard Expected RT Current Method Noise Thres. 10.0 10.0 Quant Hires. 0 2 0.2 Min. Width 3 3 Mult Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $0008807*010 7 010 S00088 Std9 1 1 Thu. Nov 9. 2000 8:45 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 427.0->407.0 Area 225323 HeiQht 28708 Start Time End Time Integration Width Retention Time Integration Tvoe l+ l+ l- H H ? % 4:12 4:46 0:34.0 4:26 hq 1009030 7060- 403020- 281 intensity : 28710 cps 101 201 1:35 3:10 301 4:45 6:19401 501 Scan r - 7:5 4 Tirriej < Page 122 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-00I Figure 34. High Standard (500 ppb) for M556 IM556 Internai Standard: THPFOS Use Area Absolute Rtention Time Expected RT 5:25 I Current Method Noise Thres. 0.4 0.4 0.1Quant Thres. 0.1 Min. Width Mult. Width 33 10 10 Base. Width RT Win. (secs) Smooth 150 150 20 20 11 s0008807*010 7 010 S00088 Std9 1 1 Thu. Nov 9. 2000 8:45 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 556.0*>498.0 Area 964595 HeiQht 111295 Stari Time ' End Time Integration Width Retention Time Intearabn Tvoe 4:55 6:04 1:09 5:26 >CO < No Comment intensity : U 1295 cps ITHPFOS use as Internat Standard Expected RT 4:15 10.0 10.0I Current Method Noise Thres. Quant Thres. 0.2 0.2 Min. Width Mult Width 33 10 10 Base. Width RT Win. (secs) Smooth 150 20 150 20 11 S008807-01 7 010 S00088 Std9 1 1 Thu. Nov 9. 2000 8:45 PM 8:59 in 1 penod 1: 8:59 MRM, 571 scans 427.0**407.0 Area 225323 Height 28708 Start Time End Time Integration Width Retention Time Integration Tvoe > (D CD 4:12 4:46 0:34.0 4:26 100 90 80 70 60 50 40 30 20- t- No Comment 281 1I 201 1.35 3:10 301 4:45 intensity : 28710 cps 401 6:19 SOI Src-ifip-- 7 :5 4 Tin*ie| . Page 123 # ** Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBR01-001 Figure 35. High Standard (500 ppb) for IVI570 |MS7Q Internai Standard: THPFOS Use Area Absolute Retention Time Expected RT 5:38 Current Method Noise Three. 3.0 3.0 Quant Thres. 0.5 0.5 Min. Width 55 Mult. Width 15 15 Base. Width RT Win. (secs) Smooth 150 150 20 20 11 $0008807*010 7 010 S00088 Std9 1 1 No Comment ITHPFOS use as Internal Standard Expected RT 4:15 10.0 10.0I Current Method Noise Thres. Quant Thres. 0.2 0.2 Min. Width Mult Width 33 10 10 Sase. Width RT Wm. (secs) Smooth 150 150 20 20 11 30008807*010 7 010 S00088 Std9 1 1 No Comment Page 124