Document a1qxb5aGgDKxX44Yj9QMGGDrb

Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Quantitative Determination of PFOS and Related Compounds in Human Serum by LC/5/IS/1VIS Sample Analysis Report for Protocol EPI-0013 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: C/:_,_z/c._:_._ Connie O. Sakashita,B.S., NW'B Project Manager APPROVED FOR RELEASE BY: Rodger L. Foltz, Ph.D., N_l'Technical Director DATE: /- _-O_Z- Page 1 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Q UALITY ASSURANCE STATEMENT LABORATORY: Northwest Bioanalytical (NWB) A Division of NWT, Inc. 112l East 3900 South Salt Lake City, UT 84124 SPONSOR: 3M Company Corporate Occupational 220-3W-05 St. Paul, MN 55144 Medicine, Medical Department COMPOUND(S): NWB STUDY NUMBER: SPONSOR STUDY NUMBER: PFOS, PFOA (POAA), PFHS, PFOSA, PFOSAA, M556, M570 NWBS00-128 EPI-0013 NWB STUDY TITLE: Quantitative Determination of PFOS and Related Compounds in Human Serum by LC/MS/MS The clinical study described in this report is not'included within the definition of a GLP regulated nonclinical study. However, Northwest Bioanalytical conducts all projects in accordance with the guidelines of the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58), the OECD Principles of Good Laboratory Practice and the Japanese MI-IW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety of Drugs (Ordinance No. 21, PAB Notification No. 424.) The following inspections were performed by the NWB QAU per SOP. Inspection and Reporting Statement. Inspection Date 28 Nov 2000 20-23 Mar 2001 05-06 Apr 2001 02-04 May 2001 31 Dec 2001 - 07 Jan 2002 09 Jan 2002 Phase of Study Analytical Plan Sample Analysis Sample Receipt QC Preparation Report Draft/Raw Data Final Report _Reports to NWB Management are issued monthly. Date Inspection Report Issued To NWB Project Manager tNWB Management 28 Nov 2000 30 Nov 2000 23 Mar 200t 31 Mar 2001 06 Apr 2001 30 Apr 2001 04 May 2001 31 May 2001 07 Jan 2002 31 Jan 2002 09 Jan 2002 31 Jan 2002 As can reasonably be establi.shed, the methods and procedures described and the results incorporated into this final report accurately reflect the raw data. ws, NWB QAU Compliance Auditor Date _' " Page 2 NorthwestBioanalytical COMPLIANCE STATEMENT StudyNo. NWBS00-128 ReportNo. NWBR01-066 The clinical study described in this report is not included within the definition of a GLP regulated nonclinical study. However, to the best of our knowledge, this project was conducted in accordance with the guidelines of the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58) and according to the methods and procedures described within this report. In addition, the study followed the guidelines of the OECD Principles of Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety of Drugs (Ordinance No. 21, PAB Notification No. 424.) Any known incidents that may have affected the quality or integrity of the project or reported data is included in this report. This report represents an accurate record of the raw data. Connie O. Sakashita, B.S. NWB Project Manager , .. _ NWB Technical Director Date Date / - _--0'"z.._ Page 3 Northwest Bioanalytical TABLE OF CONTENTS Study No. NWBS00-128 Report No. NWBR01-066 SIGNATURE PAGE ........................................................................................................................ 1 QUALITY ASSURANCE STATEMENT ...................................................................................... 2 COMPLIANCE STATEMENT ....................................................................................................... 3 TABLE OF CONTENTS ................................................................................................................. 4 LIST OF TABLES ........................................................................................................................... 4 LIST OF FIGURES .......................................................................................................................... 5 1. INTRODUCTION .................................................................................................................... 8 2. METHODOLOGY ................................................................................................................... 9 3. SAMPLE ANALYSIS ........................................................................................................... 11 4. RESULTS AND DISCUSSION ...., ....................................................................................... 13 5. REFERENCES ...................................................................................................................... 19 6. DATA RETENTION ............................................................................................................. 20 LIST OF TABLES Table 1. Calibration Curve Sum_mary for PFOS ............................................ ..... .......................... 21 Table 2. Calibration Curve Summary for PFHS ......................................... .................................. 22 Table 3. Calibration Curve Summary for PFOA .......................................................................... 23 Table 4. Calibration Curve Summary for PFOSAA ..................................................................... 24 Table 5. Calibration Curve Summary for PFOSA ........................................................................ 25 Table 6. Calibration Curve Summary for M556 ........................................................................... 26 Table 7. Calibration Curve Summary for M570 ........................................................................... 27 Table 8. Back-Calculated Concentrations of Calibration Standards for PFOS ............................ 28 Page 4 Northwest Bioanalytical Study No. NWBS00- 128 Report No. NW'BR01-066 Table 9. Back-Calculated Concentrations of Calibration Standards for PFHS ............................ 30 Table 10. Back-Calculated Concentrations of Calibration Standards for PFOA .............. .'........... 32 Table 11. Back-Calculated Concentrations of Calibration Standards for PFOSAA ..................... 36 Table 12. Back-Calculated Concentrations of Calibration Standards for PFOSA ........................ 39 Table 13. Back-Calculated Concentrations of Calibration Standards for M556 .......................... 41 Table 14. Back-Calculated Concentrations of Calibration Standards for M570 .......................... 43 Table 15. Analytical QC Summary for PFOS ............................................................................... 45 Table 16. Analytical QC Summary for PFHS ............................................................................... 48 Table 17. Analytical QC Summary for PFOA .............................................................................. 51 Table 18. Analytical QC Summary for PFOSAA ......................................................................... 54 Table 19. Analytical QC Summary for PFOSA ............................................................................ 57 Table 20. Analytical QC Summary for M556 ............. .................................................................. 60 r Table 21. Analytical QC Summary for M570 ............................................................................... 62 Table 22. Study Sample Concentrations ........................................................................................ 65 Table 23. Repeat Analysis Table for PFOS ................................................................................ 104 LIST OF FIGURES Figure 1. Representative Calibration Curve for PFOS ................................... ............................ 105 Figure 2. Representative Calibration Curve for PFHS ............................................................... 105 Figure 3. Representative Calibration Curve for PFOA ............................................................... 106 Figure 4. Representative Calibration Curve for PFOSAA .......................................................... 106 Figure 5. Representative Calibration Curve for PFOSA ............................................................. 107 Figure 6. Representative Calibration Curve for M556 ............................................................... 107 Figure 7. Representative Calibration Curve for M570 ............................................................... 108 Page 5 NorthwestBioanalytical StudyNo. NWBS00-128 ReportNo. NWI3RO[-066 Figure 8. Human Plasma Blank for PFOS .................................................................................. I09 Figure 9. Human Plasma Blank for PFHS .................................................................................. 110 Figure 10. Human Plasma Blank for PFOA ............................................................................... 111 Figure 11. Human Plasma Blank for PFOSA.A .......................................................................... 112 Figure 12. Human Plasma Blank for PFOSA ............................................................................. 113 Figure 13. Human Plasma Blank for M556 ................................................................................ 114 Figure 14. Human Plasma Blank for M570 ................................................................................ 115 Figure 15. Human Plasma Blank with Internal Standard (QC0) for PFOS ................................ I 16 Figure 16. Human Plasma Blank with Internal Standard (QC0) for PFI-IS ................................ 117 Figure 17. Human Plasma Blank with Internal Standard (QC0) for PFOA ................................ 118 Figure 18. Human Plasma Blank with Internal Standard (QC0) for PFOSAA ........................... 119 Figure 19. Human Plasma Blank with Internal Standard (QC0) for PFOSA ............................. 120 Figure 20. Human Plasma Blank with Internal Standard (QC0) for M556 ................................ 121 Figure 21. Human Plasma Blank with Internal Standard (QC0) for M570 ................................ 122 Figure 22. Low Standard for PFOS ............................................................................................. 123 Figure 23. Low Standard for PFHS ............................................................................................. 124 Figure 24. Low Standard for PFOA ............................................................................................ I25 Figure 25. Low Standard for PFOSAA ....................................................................................... 126 Figure 26. Low Standard for PFOSA .......................................................................................... 127 Figure 27. Low Standard for M556 ............................................................................................. 128 Figure 28. Low Standard for M570 ...................................................... ....................................... 129 Figure 29. High Standard for PFOS ............................................................................................ 130 Figure 30. High Standard for PFHS ............................................................................................ 131 Figure 31. High Standard for PFOA ........................................................................................... 132 Page6 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Figure 32. High Standard for PFOSA.A ...................................................................................... 133 Figure 33. High Standard for PFOSA ............................................................................... '.......... 134 Figure 34. High Standard for M556 ............................................................................................ 135 Figure 35. High Standard for M570 ............................................................................................ 136 Page 7 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Quantitative Determination of PFOS and Related Compounds in Human Serum by LC/MS/MS Sample Analysis for Protocol EPI-0013 1. INTRODUCTION This report summarizes the analyticalresults from the quantitationofPFOS, PFHS, PFOA,PFOSAA, PFOSA, M556, and M570 in human serum samples for 3M Company in supportof Protocol EPI-0013 [5.1]. The LC/MS/MS method for the analytes exhibited a quadraticresponse andhad targetLLOQ andULOQ values of 1.00ppb (2.50 ppb for M556) and 500 ppb for the analytes. The testing facility was 3M Company (Corporate Occupational Medicine, Medical Department, 220-3W-05, St. Paul, MN 55144), and the Study Director was Jeffrey H. Mandel, M.D. The Study Contacts at 3M Company were Jean Burris, M.P.H, R.N., and James Lundberg, Ph.D. The following is a list of NWB supervisory personnel involved in the completion of this work: Connie O. Sakashita, B.S. (NWB Project Manager); Tonya Felix, M.A. (NWB Acting Project Manager); Patrick Bennett, M.S., M.B.A. (NW'BLaboratory Director); Rodger L. Foltz, Ph.D. (NWB Technical Director). Laboratory personnel involved in the completion of this study included Suzarme Newman, B.S. (NWB Research Scientist), Toni Peacock, B.S. (NWB Assistant Scientist) and Emily Yardimci, B.S. (NWB Associate Research Scientist). NWB SOPs and guidelines were used in the conduct of this study and were available to stud3/personnel in electronic and hard copy formats. Date Study Initiated: 15-Nov-2000 Date Analyses Completed: 1l-May-2001 The clinical study described in this report is not included within the definition ofa 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 Page 8 Northwest B ioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety of Drugs (Ordinance No. 21, PAB Notification No. 424). Any changes to or deviations from the original protocol (Analytical Plan) were documented through approved protocol amendments or deviation memos and are retained within the raw data. 2. METHODOLOGY The assay used for this study is reported in Northwest Bioanalytical reports NWBR00108 [5.2] and NWBR00-122 [5.3]. Chinese human plasma was used for the calibration curves and quality control samples. Serum sample results obtained using plasma curves are discussed in N'W'BR00-122. Samples for this study were received at NWB on the following dates: Receipt Date 22-Nov-2000 21-Feb-2001 06-Mar-2001 15-Mar-2001 05-Apr-2001 Reference Material Number of Samples Received 100 108 330 16 125 Storage Condition (except during analysis) -20 C -20 C -20 C -20 C -20 C Analyte PFOS (FC-95) PFHS PFOA (FC-143) PFOSAA(FC-129) PFOSA M556 M570 THPFOS Lot Number 193 SE-036 245 617 214 NBl13047-8D 118506-26 59909 Purity 100% 100% 100% 53.8% 100% 99.89% 99.75% 90.0% Expiration Date 31-Dec-2010 01-Jan-2010 31-Dec-2010 31-Dec-2010 31-Dec-2010 31-Dec-2010 31-Dec-2010 31-Dec-2010 Source 3M 3M 3M 3M 3M 3M 3M 3M Storage Conditions Room temperature* -20 C Room temperature* Room temperature Room temperature Room temperature Room temperature Room temperature *Stored dry Page 9 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Eight or more calibration standards were prepared on the day of each run by adding 100 _L of blank human plasma and 400 _.tLof 50 mM ammonium acetate in water (unadjusted pH -6.9) to 13 x 100 mm polypropylene tubes. After a brief vortex mixing, 10.0 i.tLof the appropriate spiking solution was added. The absolute purity ofPFOS, PFOSA, PFOA, and PFHS reference material was not available prior to the conduct of this study. Therefore, the reference material purity was assumed to be 100%. 3M contracted with Centre Analytical Laboratories, Inc., in State College, Pennsylvania to determine the absolute concentration ofPFOS, PFHS, and PFOA in NWB stock solutions used to prepare the analytical standards and controls used for this studies. All arrangements for purity determinations and the transfer of NWB solutions to Centre Analytical Laboratories, Inc., were performed by 3M. Based on Centre Analytical Laboratories' results, the concentrations of plasma calibrator and quality control samples were corrected using the foUowing factors: Analyte PFOS PFHS PFOA Correction Factor 0.836 0.909 0.855 The final calibration standard concentrations in human plasma for each analyte can be found in Tables 8 - 14. NOTE: Due to the use of different matrix pools with different persistent levels, there are several standard concentrations in these tables. However, only eight (for M556) or nine (all other analytes) standards are used for a single curve. The target calibration curve range is 1.00 ppb (2.50 ppb M556) to 500 ppb prior to correction for purity. In addition, blank plasma samples, both with and without internal standard (designated as QC0s and Blanks, respectively), were assayed in each analytical run. Analytical QCs were prepared in human plasma on October 27, 2000, March 8, 2001, April 5, 2001 and May 2, 2001 and frozen in a -20 C freezer. For each run, analytical QC levels were assayed in duplicate. In addition, for each dilution level, dilution QCs Page 10 Northwest Bioanalytica[ Study No. NWBS00- 128 Report No. NWBR01-066 were run in triplicate in any analytical run that contained diluted subject samples. The QC concentrations are shown below: Analyte PFOS PFHS PFOA PFOSA.A PFOSA M556 M570 Low QC Concentrations* All concentrations are expressed as ppb. Medium High 5.75, 6.40 4.48 4.32, 4.81 4.30, 4.60 4.00 4.00 4.00 126 156, 157 145 150, 151 150 150 150 331,332 417, 418 385 400, 401 400 400 400 Dilution DF=5 348 * The target QC concentrations are 4.00 ppb, 150 ppb and 400 ppb prior to correction for purity. Each analyte has different QC concentrations based upon the persistent levels of the analyte in the human plasma used. The internal standard (THPFOS) was added to all plasma and serum samples (except Blanks) for a final concentration of approximately 200 ppb. The analytical method consisted of a liquid:liquid extraction procedure followed by evaporation and reconstitution of the extract residue with 20 mM ammonium acetate in water: 20 mM ammonium acetate in methanol (30:70, v/v). The samples were analyzed by liquid chromatography/tandem mass spectrometry using an API 3000. The instrument was operated in the multiple reaction monitoring (MR.M) mode under optimized conditions for PFOSI PFHS, PFOA, PFOSA.A, PFOSA, M556 and M570 detection of the negative ions formed by TurbolonSpray TM ionization. 3. SAMPLE ANALYSIS PFOS, PFHS, PFOA, PFOSA.A, PFOSA, M556, M570, and THPFOS chromatographic peaks were integrated using the MacQuan software (version 1.6) with a smooth factor of one. Quantitation was based upon quadratic regression analysis of weighted (1/x 2) calibration curves using area ratio vs. concentration utilizing Watson DMLIMS software (version 6.1.1.04). The samples were injected in a systematic order. Page 11 Northwest B ioanalytical Study No. NWBS00-128 Report No. NWBR0 [-066 For sample 11689, the measured concentration of PFOS was corrected for the persistent level of analyte present in the dilution matrix. The concentration is reported as a whole number and has not been rounded to 3 significant figures. 3.1. Acceptance Criteria For an analytical run to be accepted, it must have met the acceptance criteria listed below which are consistent with regulatory and industry recommendations. CaIibration Curve Each run will include calibration standards in duplicate at six or more concentrations covering the lower to upper limit ofquantitation. For all analytes except PFOSA and PFOSAA, at least three-fourths of the calibration standard's back-calculated concentrations must be within + 15% (+ 20% for LLOQ) of their individual target concentrations. For PFOSA and PFOSAA, at least three-fourths of the calibration standard's back-calculated concentrations must be within + 20% (+_2_5% 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 of Quantitation The back-calculated concentrations of at least one of the duplicate lowest points in the calibration curve must be within _+25% of the target concentration for PFOSA and PFOSAA to qualify as the LLOQ and within + 20% of the target concentration to qualify as the LLOQ for all other analytes. If this criterion is not met, the next level is subjected to the same test and the LLOQ raised accordingly. Quality Control Samples Each analytical run will include low, medium and high QC samples in duplicate. The measured concentrations of at least two-thirds of all analytical QCs must be within + 20% of their target concentrations (+ 25% for PFOSA and PFOSA.A), and no two QCs at the same concentration can be outside the limit. If study samples require Page 12 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 dilution, a dilution QC will be analyzed in triplicate for each dilution level (except for PFOSA and PFOSAA which should not be diluted with control matrix). At least two dilution QCs at each level must be within + 20% of its target concentrations in order to accept diluted study samples at that level. The dilution QC acceptance is independent of the undiluted analytical QC acceptance. 4. RESULTS AND DISCUSSION Serum sample results obtained using plasma curves for PFHS, PFOA, PFOSAA, PFOSA, M556, and M570 did not meet NWB SOP requirements for validation. Results may vary on average up to 26% from results obtained using human serum calibration curves at some concentration levels for PFHS, PFOA, PFOSA.A, M556, and M570. For PFOSA, results may vary on average up to 43% from results obtained using human serum calibration curves. These data are reported in Assay Revalidation Addendum Report NWBR00-122 [5.3]. However, in order to obtain the lower limit of quantitation of less than 5 ppb required by the sponsor, it was necessary to use plasma calibration curves. Each accepted run met the acceptance criteria set for the calibration curve points, for the lower limit of quantitation (LLOQ) and for the analytical quality control (QC) samples. Run Analyte No. 1 PFOS 1 PFOSA 1 PFOSAA 1 PFOA 1 PFHS 1 M556 1 M570 2 PFOS 2 PFOSA 2 PFOSAA 2 PFOA 2 PFHS Regression Status Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Extraction Date 27-Nov-2000 27-Nov-2000 27-Nov-2000 27-Nov-2000 27-Nov-2000 27-Nov-2000 27-Nov-2000 27-Nov-2000 27-Nov-2000 27-Nov-2000 27-Nov-2000 27-Nov-2000 Assay Date LLOQ ULOQ 27-Nov-2000 27-Nov-2000 27-Nov-2000 27-Nov-2000 27-Nov-2000 27-Nov-2000 27-Nov-2000 28-Nov-2000 28-Nov-2000 28-Nov-2000 28-Nov-2000 28-Nov-2000 3.94 414 1.00 500 1.60 501 1.92 481 1.36 523 2.50 500 1,00 500 3.94 414 1.00 500 1.60 501 1.92 481 1.36 523 Comment Page 13 Northwest Bioanatytica[ Study No. NWBS00-128 Report No. NWBR01-066 Run Analyte No. 2 M556 2 M570 3 PFOS Regression Status Accepted Accepted Extraction Date 27-Nov-2000 27-Nov-2000 Assay Date 28-Nov-2000 28-Nov-2000 3 PFOSA -- 3 PFOSAA 3 PFOA - ., , ...... - - ,. ...... - - 3 PFHS - 3 M556 - 3 M570 4 PFOS Accepted 2 l-Mar-2001 23-Mar-2001 4 PFOSA Accepted 2 l-Mar-2001 23-Mar-2001 4 PFOSAA Accepted 2 l-Mar-2001 23-Mar-2001 4 PFOA Accepted 2 l-Mar-2001 23-Mar-2001 ..... 4 PFHS Accepted 21-Mar-2001 23-Mar-2001 4 M556 Rejected 2 l-Mar-2001 23-Mar-2001 4 M570 Rejected 21-Mar-2001 23-Mar-2001 5 PFOS Accepted 22-Mar-2001 24-Mar-200 t 5 PFOSA Accepted 22-Mat-2001 24-Mar-2001 5 PFOSAA Accepted 22-Mar-200 l 24-Mar-2001 5 PFOA Accepted 22-Mar-2001 24-Mar-2001 5 PFHS Accepted 22-Mar-2001 24-Mar-2001 5 lv1556 Accepted 22-Mar-2001 24-Mar-2001 5 M570 Accepted 22-Mar-200 i 24-Mar-200 [ LLOQ ULOQ Comment 2.50 500 1.00 500 Run aborted due to power outage (repeated in run 6) Run aborted due to power outage (repeated in run 6) Run aborted due to power outage (repeated in run 6) L Run aborted due to power outage (repeated in run 6) Run aborted due to power outage (repeated in run 6) Run aborted due to power outage (repeated in run 6) Run aborted due to power outage (repeated in run 6) 3.94 414 ,1.00 500 1.60 501 1.92 481 i 1.36 523 2.50 500 QCs failed 1.00 500 QCs failed 3.94 414 1.00 500 1.60 501 1.92 481 1.36 523 2.50 500 1.00 500 6 PFOS ..Accepted 6 PFOSA Accepted 6 PFOSA.A Accepted 6 PFOA Accepted 6 PFHS Accepted 26-Mar-2001 ] 26-Mar-2001 26-Mar-2001 26-Mar-2001 4.27_ 414 1.40 500 26-Mar-2001 26-Mar-2001 2.80 502 26-Mar-2001 26-Mar-2001 2.11 482 I 26-Mar-2001 26-Mar-2001 I 2.09 523 Page 14 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Run Analyte No. Regression Status Extraction Date Assay Date LLOQ ULOQ Comment 6 M556 6 M570 7 PFOS 7 PFOSA 7 PFOSAA 7 PFOA 7 PFHS 7 M556 7 M570 8 PFOS 8 PFOSA 8 PFOSAA 8 PFOA 8 PFHS 8 M556 8 M570 9 PFOS 9 PFOSA 9 PFOSAA 9 PFOA 9 PFHS 9 M556 9 M570 l0 PFOS. 10 PFOSA 10 PFOSAA 10 PFOA 10 PFHS l0 lVI556 10 M570 11 PFOS ,w, 11 PFOSA 11 PFOSAA Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Rejected Rejected Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Rejected 26-Mar-2001 26-Mar-200 3.20 26-Mar-2001 26-Mar-2001 1.80 26-Mar-2001 26-1Vlar-2001 4.27 26-Mar-2001 26-1VIar-2001 1.40 26-Mar-2001 26-Mar-2001 2.80 26-Mar-2001 26-Mar-2001 2.11 26-Mar-2001 26-Mar-2001 2.09 26-Mar-2001 26-Mar-2001 3.20 26-Mar=2001 26-Mar-2001 1.80 28-Mar-2001 28-Mar-2001 4.27 28-Mar-2001 28-Mar-2001 1.40 28-Mar-2001 28-Mar-2001 2.80 28-Mar-2001 28-Mar-2001 2. I I 28-Mar-2001 28-Mar-2001 2.09 =, , 28-Mar-2001 28-Mar-2001 3.20 28-Mar-2001 28-Mar-2001 1.80 28-Mar-2001 28-Mar-2001 4.27 28-Mar-2001 28-Mar-2001 1.40 28-Mar-2001 28-Mar-2001 2.80 28-Mar-2001 28-Mar-2001 2.11 28-Mar-2001 28-Mar-2001 2.09 28-Mar-2001 28-Mar-2001 3.20 28-Mar-2001 ! 28-Mar-2001 1.80 30-Mar-2001 30-Mar-2001 4.27 30-Mar-2001 30-Mar-2001 1.40 30-Mar-2001 30-Mar-2001 2.80 30-Mar-2001 30-Mar-200 l 2.11 30-Mar-2001 30-Mar-2001 2.09 30-Mar-2001 30-Mar-2001 3.20 30-Mar-2001 30-Mar-2001 1.80 30-Mar-2001 30-Mar-2001 4.27 30-Mar-2001 30-Mar-2001 1.40 30-Mar-2001 30-Mar-2001 2.80 501 501 414 500 502 482 523 501 501 414 500 502 482 523 501 501 414 500 502 482 523 501 Low QCs failed 501 Curve and QC fail 414 500 502 482 523 50l 501 414 500 502 Curve fails Page 15 Northwest B ioanalytical Smdy No. NWBSO0-128 Report No. NWBR0 I.-066 Run Analyte Regression No. Status Extraction Date Assay Date LLOQ ULOQ Comment 11 PFOA Rejected 30-Mar-200 30-Mar-2001 2. LL 482 Curve fails I l PFHS Accepted 30-Mar-2001 30-Mar-2001 2.09 523 11 M556 Accepted 30-Mar-2001 30-Mar-200 i 3.20 50 l l I M570 Rejected 30-Mar-200 t 30-Mar-200 L L.80 501 Curve fails 12 M556 Accepted 12 M570 Accepted 13 PFOS 13 PFOSA 13 PFOSAA 13 PFOA 13 PFHS 13 M556 13 M570 14 PFOS 14 PFOSA 14 PFOSAA 14 PFOA 14 PFHS 14 M556 14 M570 15 PFOS 15 PFOSA 15 PFOSA.A 15 PFOA 15 PFHS 15 M556 15 M570 16 PFOS L6 PFOSA Accepted Accepted Accepted Accepted Accepted Rejected Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted .o Accepted Accepted ,.,, Accepted 28-Mar-200L 0t-Apr-200l 28-Mar-200L 01-Apr-2001 02-Apr-2001 02-Apr-2001 02-Apr-2001 02-Apr-2001 02-Apt-2001 02-Apr-2001 02-Apt-2001 02-Apr-2001 02-Apr-2001 02-Apr-2001 02-Apt-2001 02-Apr-2001 02-Apt-2001 02-Apr-2001 04-Apr-2001 07-Apr-2001 04-Apt-2001 07-Apr-2001 04-Apr-2001 07-Apr-2001 04-Apr-2001 07-Apt-2001 04-Apr-2001 07-Apr-200 i 04-Apt-200 t 07-Apt-2001 04-Apt-2001 07-Apr-2001 06-Apr-2001 .... 06-Apt-2001 09-Apr-2001 . 09-Apt-2001 06-Apt-2001 09-Apr-2001 06-Apr-2001 09-Apt-2001 06-Apt-2001 09-Apr-2001 06-Apr-2001 ..... 06-Apr-2001 09-Apr-2001 09-Apr-2001 09-Apr-2001 .... 09-Apr-2001 1l-Apr-2001 l l-Apr-2001 3.20 1.80 4.27 1.40 2.80 2. I 1 2.09 3.20 1.80 4.27 1.40 2.80 2.11 2.09 3.20 1.80 4.27 1.40 2.80 2. I 1 2.09 3.20 1.80 4.27 1.40 50L Run 12 was a reinjection of ran 9 for M556 and M570 only 501 Run 12 was a reinjection of ran 9 for M556 and M570 only 414 500 502 482 523 501 Low QCs failed 501 414 500 502 482 523 50L 501 414 500 502 482 523 501 501 414 500 . ..... ] 16 PFOSA.A Rejected 09-Apr-2001 l l-Apt-2001 2.80 502 [ Curve fails Page 16 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Run Analyte No. 16 FFOA 16 PFHS 16 Ivi556 16 M570 17 PFOS 17 PFOSA 17 PFOSAA 17 PFOA 17 PFHS 17 M556 17 M570 18 PFOS 18 PFOSA 18 PFOSAA 18 PFOA 18 PFHS 18 M556 18 M570 19 PFOS Regression Status Extraction Date Rejected Accepted Rejected Rejected Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted 09-Apr-2001 09-Apr-2001 09-Apr-2001 09-Apt-2001 10-Apr-2001 10-Apr-2001 10-Apr-2001 10-Apr-2001 10-Apr-2001 10-Apr-2001 10-Apr-2001 19-Apr-2001 19-Apr-2001 Accepted Accepted Accepted Accepted Rejected Rejected 19-Apt-2001 19-Apt-2001 19-Apr-2001 19-Apr-2001 19-Apr-2001 09-Apr-2001 Assay Date l [-Apr-2001 1l-Apr-2001 1l-Apt-2001 l l-Apr-2001 12-Apr-200l 12-Apr-2001 12-Apr-2001 12-Apr-2001 12-Apr-2001 12-Apt-2001 12-Apt-2001 23-Apt-2001 23-Apt-2001 23-Apt-2001 23-Apr-2001 23-Apt-2001 23-Apr-2001 23-Apr-2001 14-Apr-2001 19 PFOSA Rejected 09-Apr-2001 14-Apt-2001 19 PFOSAA 19 PFOA 19 PFHS Accepted Accepted Rejected 09-Apr-2001 09-Apr-2001 09-Apr-2001 14-Apr-2001 14-Apr-2001 14-Apr-2001 19 M556 19 M570 20 PFOS Accepted Accepted Accepted 09-Apr-2001 09-Apr-2001 06-Apr-2001 14-Apr-2001 I4-Apr-200I 13-Apr-2001 20 PFOSA Accepted 06-Apr-2001 13-Apr-2001 LLOQ ULOQ Comment 2. l I 2.09 3.20 1.80 4.27 1.40 2.80 2.11 2.09 3.20 1.80 4.27 1.40 2.80 2.11 2.09 3.20 1.80 4.02 1.30 2.80 2.11 2.09 3.20 1.80 4.27 1.40 482 ,=, 523 501 501 414 500 502 482 523 501 501 4 [4 500 Curve fails Curve fails Curve fails 502 .I 482 523 501 501 Curve and Low QC failed 414 Reinjection of run 16: Analyte results not needed 500 Reinjection of run 16: Analyte results not needed 502 Reinjectionofrun 16 482 Reinjection of run 16 523 Reinjection of run 16: Analy_e results not needed 501 Reinjection of run 16 501 Reinjection of run 16 414 !Pre-study assay evaluation _(new Chinese plasma pool and QCs) 500 Pre-study assay evaluation (new Chinese plasma pool and QCs) Page 17 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBROl-066 Run Analyte Regression No. Status Extraction Date Assay Date LLOQ ULOQ Comment 20 PFOSAA Accepted 06-Apr-2001 13-Apr-2001 2.80 502 ! Pre-study assay evaluation !(new Chinese plasma pool and QCs) 20 PFOA Accepted 06-Apr-2001 13-Apr-2001 2. l 0 482 Pre-study assay evaluation (new Chinese plasma pool and QCs) 20 PFHS Accepted 06-Apr-2001 13-Apr-200 l 2.09 523 Pre-study assay evaluation (new Chinese plasma pool and QCs) 20 I M556 Rejected 06-Apr-2001 13-Apr-2001 1.60 501 Pre-study assay evaluation (new Chinese plasma pool and QCs); Low QC fail. , 20 M570 Accepted 06-Apr-2001 13-Apr-2001 1.90 501 Pre-study assay evaluation (new Chinese plasma pool and QCs) 21 PFOSAA Accepted 17-Apr-2001 22-Apr-2001 2.80 502 Run was analyzed for PFOSAA, PFOA and M570 only 2t PFOA Accepted 17-Apr-2001 22-Apr-2001 2.11 482 Run was analyzed for PFOSAA, PFOA and M570 only 21 M570 Accepted 17-Apr-2001 22-Apr-2001 1.80 501 Run was analyzed for PFOSAA, PFOA and M570 only 22 M570 Accepted 19-Apr-2001 24-Apr-2001 1.80 501 Reinjection of run 18 for M570 only 23 PFOS Accepted 02-May-2001 05-May-2001 3.86 414 Pre-study assay evaluation of new low QC 23 PFOSA Accepted 02-May-2001 05-May-2001 1.50 501 :Pre-studyassay evaluation of new low QC 23 PFOSAA Accepted 02-May-2001 05-May-2001 2.40 501 Pre-study assay evaluation of new low QC 23 PFOA Accepted 02-May-2001 05-May-2001 2.31 482 Pre-study assay evaluation of new low QC 23 PFHS Accepted 02-May-2001 05-May-2001 2.50 523 Pre-study assay evaluation of new low QC 23 M556 Accepted 02-May-2001 05-May-2001 3.80 501 Pre-study assay evaluation of new low QC 23 M570 Accepted 02-May-2001 05-May-200 l 2.30 501 ' Pre-study assay evaluation of new low QC 24 PFOSAA Rejected 10-May-2001 10-May-2001 1.50 501 Sample preparation error 24 PFOA Rejected 10-May-2001 10-May-2001 25.4 482 Sample preparation error Page 18 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Run Analyte Regression No. Status 24 PFHS Rejected 24 M570 Rejected 25 PFOSA.A Accepted 25 PFOA Accepted 25 PFHS Rejected 25 M570 Accepted Extraction Date 10-May-2001 10-May-2001 1 l-May-2001 [ 1-May-2001 1l-May-2001 1l-May-2001 Assay Date LLOQ ULOQ Comment I0-May-200 l 2.50 10-May-2001 2.30 1l-May-2001 1.30 1l-May-2001 1.44 1 l-May-200 [ 1.36 1l-May-2001 1.00 523 Sample preparation error 501 Sample preparation error 500 481 522 Analyte results not needed 500 In run 4 for PFOSA and PFOSAA, one of the medium QC samples gave extremely high results. These results appear to skew the overall statistics for these analytes. Without this "outlier", the overall %CV was 9.2% for PFOSA and 12.3% for PFOSA.A. The overall %Bias was 2.0% for PFOSA and 5.3% for PFOSAA. In run 8 for PFOA, one of the low QC samples gave an extremely low result of 0.161 ppb. This result appears to skew the overall statistics for the analyte. Without this "outlier", the overall %CV was 14.1% and the %Bias was -i 0.0%/ Any known circumstances that may have affected the quality or integrity of the data are included in this report. 5. REFERENCES 5.1. 3M Company Protocol EPI-0013. "Identification of Fluorochemicals in Sera of American Red Cross Blood Donors in the United States." September 29, 2000. 5.2. C. Sakashita. "Quantitative Determination ofPFOS, PFOSA, PFOSA.A, POAA, PFHS, M556 and M570 in Human Serum by LC/MS/MS.'" Assay Revalidation Report. NWB Study NWBS00-040. NWB Report NWBR00-108. January 24, 2001. 5.3. C. Sakashita. "Quantitative Determination ofPFOS, PFOSA, PFOSA.A, POAA, PFHS, M556 and M570 in Human Serum by LC/MS/MS." Assay Revalidation Addendum Report. NWB Study NWBS00-040. NWB Report NWBR00-122. November 20, 2001. Page 19 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 6. DATA RETENTION The raw data and final report for this study will be stored in the NWB Archives, 1121 East 3900 South, Salt Lake City, UT 84124 per regulations and contract agreement. After submission of the final report to the Sponsor, remaining study samples will be stored under required conditions until confirmation of Sample Disposition/Return Authorization is received from the Sponsor. 3M Company will be notified concerning final disposition of records at completion of contract obligations. Page 20 NorthwestBioanalytical StudyNo. NWBS00-128 ReportNo. NWBR01-066 Table 1. Calibration Curve Summary for PFOS Quadratic weighted i/xz. All concentrations are expressed as ppb. Run Date 27-Nov-2000 28-Nov-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-200 L 28-Mar-2001 30-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apt-2001 1l-Apr-2001 12-Apr-2001 23-Apr-2001 Run Number 1 2 4 5 6 7 8 9 10 11 13 14 15 16 17 18 A B C -0.00003! -0.000027 0.000002 -0.000002 -0.000001 0.000003 0.000000 0.000000 0.000000 0.000001 -0.000003 -0.000010 0.000004 -0.000006 -0.000009 -0.000002 0.052622 0.049661 0.039134 0.009354 0.010776 0.03572.1 0.037629 0.010093 0.0! 1733 0.047343 0.045861 0.039827 0.045781 0.058787 0.055527 0.017703 0.012630 0.017690 0.020796 0.001128 -0.003903 0.024340 0.025011 0.007090 0.002809 0.024473 0.035036 0.014677 0.046887 -0.001384 0.020155 0.000222 R-Squared 0.9958 0.9926 0.9869 0.9985 0.9867 0.9943 0.9931 0.9895 0.9947 0.9733 0.9973 0.9925 0.9919 0.9942 0.9976 0.9935 LLOQ 3.94 3.94 3.94 3.94 4.27 4.27 4.27 4.27 4.27 4.27 4.27 4.27 4.27 4.27 4.27 4.27 ULOQ 414 414 414 414 414 414 414 414 414 414 414 414 414 414 414 414 Mean S.D. %CV n -0.000005 0.000010 -200.0 16 0.035472 0.015479 0.017605 0.014172 . .. ,, 49.6 91.6 16 16 0.9920 0.0060 0.6 16 A, B, and C are coefficients used to define the calibration curve. Page 21 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Table 2. Calibration Curve Summary for PFHS Quadratic weighted t/x2. All concentrations are expressed as ppb, Run Date 27-Nov-2000 28-Nov-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 30-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 11-A.pr-2001 12-Apr-2001 23-Apr-2001 Run Number 1 2 4 5 6 7 8 9 i0 11 13 14 15 16 17 18 -= A B C R-Squared LLOQ ULOQ -0.000013 -0.000013 -0.000002 -0.000002 -0.000002 -0.000004 -0.000003 -0.000002 -0.000001 0.000000 -0.000004 -0.000006 -0.000002 -0.000007 -0.000007 -0.000004 0.030678 0.031308 0.021861 0.007620 0.008120 0.023053 0.025470 0.008701 0.008569 0.028707 0.02t870 0.021837 0.022158 0.029426 0.026000 0.011306 0.025452 0.026252 0.020425 0.006999 -0.002637 0.006759 0.002418 0.002381 0.003686 0.027904 0.016367 0.012060 0.030931 0.013375 0.009029 0.008022 0.9949 0.9950 0.9959 0.9966 0.9953 0.9902 0.9892 0.9972 0.9836 0.9813 0.9858 0.9915 0.9901 0.9881 0.9970 0.9875 1.36 523 1.36 523 1.36 523 1.36 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 2.09 523 Mean: -0.000004 0.020418 0.013089 0.9912 S.D. 0.000004 0.008650 0.010370 0.0050 %CV n -100.0 42.4 79.2 0.5 / 16 16 16 16 I A, B, and C are coefficients used to define the calibration curve. Page 22 Northwest Bioanalytical Study No. NWI3S00-t28 Report No. NWBR0t-066 Table 3. Calibration Curve Summary for PFOA Quadratic weighted l/xz. All concentrations are expressed as ppb. Run Date 27-Nov-2000 28-Nov-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-200 ! 28-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 12-Apr-2001 14-Apr-2001 22-Apr-2001 23-Apr-2001 1l-May-2001 Run Number 1 2 4 5 6 7 8 9 10 A -0.000001 -0.000002 0.000001 -0.000001 0.000000 0.000003 0.000002 0.000000 0.000000 13 14 15 , ,, 17 19 21 18 25 -0.000001 -0.000003 0.000002 . ., 0.000000 -0.000001. 0.000000 -0,000002 -0.000001 B C 0.01.5479 0.005741 0.016334 0.015052 0.008393 0.007706 0.007290 0.002187 0.007392 -0.000487 0.008327 0.004956 0.008675 0.015973 0.007316 0.00586 t 0.007744 .... 0.008171 0.003135 p. 0.003088 0.009779 0.000405 0.007753 0.019137 0.007833 0.004324 0.007768 0.001433 0.015981 -0.001298 0.016857 0.000933 0.012990 -0,002765 R-Squared LLOQ ULOQ 0.9933 0.9877 0.9842 0.9979 0.9898 0.9865 0.9825 0.9940 0.9964 1.92 481 1.92 481 1.92 481 t.92 481 2.11 482 2. I 1 482 2.11 482 2. I 1 482 2.11 482 0.9901 2.11 482 0.9926 2.11 482 0,9872 2.11 482 0.9945 2.11 482 0.9954 2.11 482 0.9878 2.11 482 r--- 0.9905 2; 11 482 0,9962 1,44 481 Mean S.D, %CV n 0.000000 0.000002 NCL 17 0.010240 0.003645 35.6 17 0.005022 0.006254 124.5 17 0.9910 0.0045 0.5 17 A, B, and C are coefficients used to det"methe calibration curve. NCL = not calculable Page 23 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Table 4. Calibration Curve Summary for PFOSA.A Quadratic weighted l/x x. All concentrations are expressed as ppb. Run Date 27-Nov-2000 28-Nov-2000 23-Mar-2001 24-Mar-200 [ 26-Mar-2001 26-Mar-2001 .. 28-Mar-2001 28-Mar-2001 30-Mar-2001 02-Apt-2001 07-Apr-2001 09-Apt-2001 12-Apr-2001 14-Apt-2001 22-Apt-2001 23-Apr-2001 11-May-2001 Run Number 1 2 4 5 6 7 8 9 10 13 14 15 17 19 21 18 25 A B C R-Squared LLOQ ULOQ 0.000000 0.000005 0.000001 0.000001 0.000002 0.000001 0.000001 0.000002 0.000003 0.000008 0.000001 0.000014 0.000006 0.000012 0.000004 0.000004 0.000002 0.013246 0.012198 =,. 0.007894 0.006730 0.008322 0.007111 0.005138 0.006742 0.007717 0.024032 0.033688 0.029651 0.025674 0.026710 0.007075 0.007908 0.012005 0.007247 0.010441 0.004964 0.010546 .--= -0.001 t 61 -0.001354 -0.004421 0.011207 0.008093 0.015403 0.011384 0.017800 0.007502 -0.009422 -0.004642 0.000878 0.000362 0.9804 0.9797 0.9685 0.9935 0.9836 0.9760 0.9798 0.9666 0.9848 0.9884 0.9867 0.9846 0.9944 0.9813 0.9735 0.9744 0.9937 1.60 501 1.60 501 1.60 501 1.60 501 2.80 502 2.80 502 2.80 502 2.80 502 2.80 502 2.80 502 2.80 502 2.80 502 2.80 502 2.80 502 2.80 502 2.80 502 1.30 =,, 500 Mean S.D. %CV nl 0.000004 0.000004 100.0 I7 0.014226 0.009564 67.2 17 0.004990 0.007661 153.5 17 0.9818 0.0083 0.8 17 A, B, and C are coefficients used to define the calibration curve. Page 24 Northwest Bioanalytical Study No. NWBS00-128 Repo_ No. NWBR01-066 Table 5. Calibration Curve Summary for PFOSA Quad_tic weighted |/x 2. All concentrations are expressed _ ppb. Run Date 27-Nov-2000 28-Nov-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Ma_2001 28-May2001 28-Mar-2001 30-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apv2001 09-Apv2001 l l-Apr-2001 12-Ap_2001 23-Apv2001 Run Number i 2 4 5 6 7 8 9 10 11 13 14 15 16 17 18 A B C R-Squared -0.000041 -0.000025 0.000002 -0.000002 -0.000001 -0.000002 0.000001 0.000000 -0.000003 0.000018 -0.000008 -0.000011 -0.000006 0.000034 -0.000010 0.000007 0.096146 0.087183 0.034802 0.018868 0.023192 0.034174 0.032420 0.022395 0.023907 0.108434 0.108295 0.097511 0.119455 0.124021 0.129002 0.040292 0.018081 0.015131 0.013699 0.003711 -0.012070 0.000108 0.015115 0.000709 0.000482 0.040511 0.054874 0.020730 0.031195 -0.030446 0.003170 0.010493 0.9920 0.9931 0.9847 0.9985 0.9931 0.9956 0.9965 0.9848 0.9934 0.9882 0.9885 0.9819 0.9923 0.9870 0.9944 0.9936 LLOQ ULOQ 1.00 500 1.00 500 1.00 500 1.00 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 1.40 500 Mean S.D. %CV n -0.000003 0.000016 -533.3 16 0.068756 0.042828 62.3 t6 0.011593 0.020139 173.7 16 0.9911 0.0047 0.5 16 A, B, and C arecoefficien_ usedto define_ecalib_tioncurve. Page25 Northwest Bioanalytical Study No. NWBS00-123 Report No. NWBR01-066 Table 6. Calibration Curve Summary for M556 Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date 27-Nov-2000 28-Nov-2000 24-Ma_2001 26-Mar-2001 26-Ma_200! 28-Ma_2001 30-Mar-2001 30-Ma_2001 01-Apr-2001 07-Ap_2001 09-Ap_2001 12-Apr-2001 14-Ap_2001 23-Ap_2001 Run Number 1 2 5 6 7 8 10 11 12 14 15 17 19 18 A B C R-Squared LLOQ LrLOQ 0.000001 0.000003 0.000001 0.000001 0.000001 0.008245 0.007109 0.002937 0.003973 0.006232 0.002637 0.006480 0.003249 -0.002024 -0.005748 0.9851 0.9931 0.9943 0.9809 0.9928 2.50 500 2.50 500 2.50 500 3.20 501 3.20 501 0.000001 0.000001 0.000003 0.004865 0.002628 0.004105 -0.004285 0.000476 0.002505 0.9923 0.9939 0.9789 3.20 501 3.20 501 3.20 501 0.000001 0.000001 0.000003 0.000002 0.000003 0.000002 0.002392 0.007457 0.006599 0.006819 0.006308 0.003128 0.001473 0.002028 0.008776 -0.003271 -0.001438 0.001358 0.9825 0.9924 0.9891 0.9913 0.9886 0.9870 3.20 501 3.20 501 3.20 501 3.20 501 3.20 501 3.20 501 Mean S.D. %CV n o 0.000002 0.000001 50.0 14 0.005200 0.001993 38.3 14 0.000873 0.004007 459.0 14 0.9887 0.0051 0.5 14 A,B, and C arecoefficien_ _edto define _ecalib_tioncu_e. Page 26 Northwest Bioanal_ical Smdy No. NWBS00-128 Repo_ No. NWBR01-066 Table 7. Calibration Curve Summary for M570 Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date 27-Nov-2000 28-Nov-2000 24-Mar-2001 26-Mar-200I 26-Ma_2001 28-Mar-2001 30-Mar-2001 01-Apr-2001 02-Ap_2001 07-Apr-2001 09-Ap_2001 12-Ap_2001 14-Apr-200l 22-Apv2001 24-Apr-2001 ll-May-2001 Run Number 1 2 5 6 7 8 10 12 13 14 15 17 19 21 22 25 A B C R-Squared LLOQ ULOQ -0.000003 0.000002 0.000000 0.000002 0.000001 0.000002 0.000001 0.000001 0.000007 -0.000001 0.000011 0.000004 0.000009 0.000001 0.000018 0.000000 0.022236 0.021764 0.003326 0.003649 0.017625 0.013605 0.003548 0.003371 0.027857 0.034478 0.032868 0.030324 0.030213 0.003114 0.038537 0.004063 0,026662 0.021002 0.003631 -0.000239 0.009909 0.006783 0.001744 0.002595 0,035353 0.018645 0.046246 0.016921 0.008691 -0.002037 0.040536 -0.001174 0.9910 0.9902 0.9937 0.9851 0.9880 0.9911 0.9859 0.9779 0.9890 0.9854 0.9863 0.9936 0,9817 0.9880 0,9873 0.9955 1.00 500 1.00 500 1.00 500 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.80 501 1.00 500 Mean _ S.D, %CV n 0.000003 0.000005 166.7 16 0,018161 0.013225 72.8 16 0,014704 0.015506 105.5 16 0.9881 0.0045 0.5 16 A,B, and C _ecoefficien_used _ define _ecal_rationcurve, Page 27 Northwest Bioanalytical Study No. NWB S00-128 Report No. NWBR01-066 Table 8. Back-Calculated Concentrations of Calibration Standards Quadratic weighted l/x 2. All concentrations are expressed as ppb. for PFOS Run Date 27-Nov-2000 Run Number 1 28-Nov-2000 2 23-Mar-2001 4 24-Mar-200 l 5 26-Mar-2001 6 26-Mar-2001 7 28-Mar-2001 8 28-Mar-2001 9 "' 30-Mar-2001 10 3.94 4.27 5.17 5.50 11.3 11.7 23.6 24.0 44.2 44.5 85.4 85.5 209 332 414 1 4.04 5.05 11.1 24.1 48.3 80.9 234 307 432 3.98 5.02 11.4 *44.7 *'18.9 77.2 209 321 417 4.05 4.91 10.9 25.4 49.5 84.5 234 299 450 4.00 5.24 10.6 "42.1 *'18.1 74.2 204 319 416 4.01 5.70 10.6 26.0 41.2 81.4 232 293 419 3.42 5.60 11.3 20.3 48.5 89.2 186 380 399 3.99 5.05 11.6 23.2 46.8 82.0 209 351 421 3.94 5.07 11.6 24.2 44.0 81.3 205 314 415 4.13 4.95 11.4 22.1 42.0 73.8 191 319 419 4.46 5.64 13.7 23.7 53.9 81.8 223 368 399 4.75 5.64 11.4 25.7 46.6 80.7 214 365 392 3.85 5.34 11.4 23.8 41.9 86.0 218 304 422 4.25 5.23 12.4 24.8 52.8 86.1 203 332 437 4.54 5.26 11.0 24.3 40.5 80.3 190 340 406 5.01 5.55 11.3 26.7 49.0 89.0 207 335 415 4.07 4.86 10.0 23.0 46.2 76.3 224 314 415 I 4.55 4.89 13.0 24.7 45.4 81.5 199 345 391 4.54 5.10 10.8 23.8 44.1 86.6 221 342 413 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to preparation error Page 28 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Table 8. Back-Calculated Concentrations of Calibration Standards for PFOS Quadratic weighted l/x 2. All concentrations are expressed as ppb. (Continued) Run Date 30-Mar-2001 Run Number 11 02-Apr-2001 13 07-Apr-2001 14 09-Apr-2001 15 ll-Apr-2001 16 12-Apr-2001 17 23-Apr-2001 18 3.94 4.27 5.17 5.50 11.3 11.7 23.6 24.0 44.2 44.5 85.4 85.5 209 332 414 5.45 3.63 4.16 4.59 4.24 4.47 5.00 4.03 4.66 3.92 4.45 ***2.26 4.61 4.33 4.97 5.49 5.28 5.54 5.75 4.96 5.11 5.46 5.37 5.69 5.20 5.38 5.25 5.25 10.6 20.5 11.1 24.2 11.1 24.8 11.5 22.9 12.2 26.9 11.2 21.3 10.5 25.9 10.5 23.5 11.1 22.8 11.6 24.5 11.3 25.4 12.5 23.3 11.2 25.3 11.3 22.9 44.9 52.8 44.9 46.0 46.3 42.0 47.1 45.0 47.4 47.7 44.2 45.9 44.9 48.1 81.5 204 311 397 106 169 381 428 85,4 213 351 426 86.2 208 337 374 88.3 225 373 409 81.9 195 329 380 90.8 223 359 407 80.4 206 320 394 72.9 224 328 395 87.9 209 342 417 86.4 196 328 435 82.6 207 341 405 76.0 201 314 377 90.0 230 364 426 Mean S.D. %CV %Bias n 3.93 0.208 5.3 -0.3 8 4.42 0.411 9.3 3.5 23 5.21 5.30 11.1 11.4 23.9 24.0 46.4 46.2 81.3 84.1 210 335 411 0.290 0.263 0.407 0.830 2.01 1.57 3.18 3.39 4.48 6.80 15.1 23.8 17.8 5.6 5.0 3.7 7.3 8.4 6.5 6.9 7.3 5.5 8.1 7.2 7.1 4.3 0.8 -3.6 -1.8 -2.6 1.3 0.0 5.0 3.8 -4.8 -1.6 0.5 0.9 -0.7 8 24 8 24 6 24 6 24 8 24 32 32 32 *** Sample deactivated due to unacceptable internal standard response Page 29 Northwest Bioanalytical Table 9. Back-Calculated Concentrations of Calibration Standards for PFFIS Study No. NWBS00-128 Report No. N_VBR01-066 Quadratic weighted l/x 2. All concentrations are expressed as ppb. Run Date 27-Nov-2000 Run Number 1 28-Nov-2000 2 23-Mar-2001 4 24-Mar-2001 5 26-Mar-2001 6 26-Mar-2001 7 28-Mar-2001 8 28-Mar-2001 9 30-Mar-2001 10 1.36 2.09 2.92 3.65 10.7 11.5 26.5 27.1 52.6 53.2 104 105 262 418 523 1.39 2.66 10.8 27.4 54.5 98.9 278 373 508 1.46 2.54 11.4 *54.5 **26.8 106 271 415 564 1.42 2.78 10.7 28.0 57.6 101 274 386 536 1.42 2.46 10.9 *50.7 **25.0 102 257 421 534 1.41 3.13 10.6 28.1 52.5 98.5 283 405 527 1.31 2.7l 10.8 28.5 48.1 104 237 449 512 1,33 2.76 11.1 26,5 55,2 99,5 261 432 528 1.48 2.58 11.3 27.3 53.8 101 255 389 545 2.08 3.70 11.0 26.9 50.8 98.2 247 409 525 2.12 3.64 10.7 28.7 62.9 102 271 441 516 2.42 3.23 11.6 27.3 52.6 90.7 242 398 472 1.94 3.39 12.4 29.4 54.0 108 294 418 594 2.20 2.96 12.3 30.9 60.1 94.6 236 437 533 2.30 3.21 11.3 27.6 52.9 104 243 415 545 2.22 3.66 11.6 26.4 52.3 105 255 455 496 1.99 3.49 12.0 28.8 55.5 96.2 254 412 544 2.11 2.83 13.2 31.4 51.1 107 223 465 550 2.27 3.71 10.3 28.8 58.8 91.3 239 374 565 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to preparation error Page 30 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Table 9. Baek-Caleulated Coneentrations of Calibration Standards for PFHS (Continued) Quadratic weighted l/x 2. All concentrations are expressed as ppb. Run Date Run 1.36 2.09 2.92 3.65 10.7 11.5 26.5 27.1 52.6 Number 30-Mar-2001 11 2.62 2.90 1.89 3.36 12.0 24.6 11.1 28.0 02-Apr-2001 13 1.77 2.88 2.68 3.61 10.9 27.4 11.7 27.2 07-Apr-2001 14 09-Apt-2001 15 1.97 2.94 2.43 3.59 2.60 3.30 1.75 3.56 11.4 26.7 11.9 30.9 11.0 28.0 10.7 27.2 1l-Apt-2001 16 2.28 2.97 11.3 26.6 2.23 3.20 12.7 29.3 12-Apr-2001 17 2.12 3.87 **'1.93 3.29 10.9 28.5 12.0 28.3 23-Apt-2001 18 2.54 3.15 1.94 3.33 10.7 27.1 11.0 26.4 53.2 104 105 262 418 523 53.2 66.3 52.9 57.4 51.5 54.6 56.4 55.9 53.8 58.5 53.0 55.8 50.2 63.9 99.0 249 406 502 114 230 468 537 107 255 439 506 108 266 445 485 98.0 270 431 497 103 268 422 523 110 264 449 514 99.4 263 411 498 85.9 251 433 482 106 288 445 514 103 248 419 552 98.0 253 425 519 114 251 427 502 107 282 398 522 Mean S.D. %CV %Bias n 1.40 0.0585 4.2 2.9 8 2.19 2.70 3.32 11.0 11.5 27.6 28.0 53.6 55.6 0.266 0.205 0.305 0.288 0.717 0.715 1.60 3.19 4.29 12.1 7.6 9.2 2.6 6.2 2.6 5.7 6.0 7.7 4.8 -7.5 -9.0 2.8 0.0 4.2 3.3 1.9 4.5 23 8 24 8 24 6 24 6 24 *** Sample deactivated due to unacceptable internal standard response 101 102 258 422 523 2.59 7.17 17.1 24.2 26.4 2.6 7.0 6.6 5.7 5.0 -2.9 -2.9 -1.5 1.0 0.0 8 24 32 32 32 Page 31 Northwest Bioanalytical Study No. NWB S00-128 Report No. NWBR01-066 Table 10. Back-Calculated Concentrations of Calibration Standards Quadratic weighted l/x z. All concentrations are expressed as ppb. for PFOA Run Date 27-Nov-2000 28-Nov-2000 23-Mar-2001 24-Mar-2001 Run Number 1 2 4 5 1.92 3.36 10.6 25.0 49.0 97.1 241 385 481 1.88 3.04 9.65 25.3 51.6 87.9 252 356 457 2.13 3.14 11.5 *53.4 **22.5 103 261 387 503 1.77 2.97 10.2 28.0 52.8 93.6 244 390 478 2.37 2.78 10.9 *46.6 *'19.9 94.2 247 372 483 1.54 2.87 12.5 27.4 50.2 90.7 256 383 492 2.40 3.40 10.7 20.7 48.5 99.6 222 400 465 1.89 3.05 10.4 24.4 51.5 92.7 243 399 477 2.05 3.38 10.6 26.2 51.4 94.9 236 380 480 Mean S.D. %CV %Bias n 2.00 3.08 10.8 25.3 51.0 94.6 245 384 480 0.295 0.222 0.869 2.63 1.48 4.79 !4.1 14.4 12.9 14.8 7.2 8.0 10.4 2.9 5.1 5.8 3.8 2.7 4.2 -8.3 1.9 1.2 4.1 -2.6 1.7 -0.3 -0.2 8 8 8 6 6 8 34 10 10 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to sample preparation error Page 32 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Table 10. Back-Calculated Concentrations of Calibration Standards for PFOA Quadratic weighted l/x 2. All concentrations are expressed as ppb. (Continued) Run Date 26-Mar-2001 Run Number 6 26-Mar-2001 ,7 28-Mar-2001 8 28-Mar-2001 9 30-Mar-2001 10 02-Apt-2001 13 07-Apr-2001 14 09-Apt-2001 15 12-Apt-2001 17 2.11 2.49 1.87 *4.06 2.45 2.06 2.44 2.40 2.09 2.03 2.30 1.83 *3.48 2.06 *4.56 1.84 2.30 2,13 **'1.13 3.56 , 10.8 25.2 49.2 97.3 241 386 482 3.57 3.25 3.37 2.72 "1.68 2.73 3.26 3.07 3.10 3.69 9.76 24.0 49.0 92.5 244 355 501 10.3 26.8 59.1 93.8 255 396 466 11.5 23.1 46.7 87.7 234 387 440 10.2 29.1 52.2 103 275 385 501 7.94 27.8 55.8 90.6 249 372 477 13.2 26.0 46.7 93.2 245 400 480 11.4 25.5 48.8 99.5 242 392 465 10.0 23.9 55.2 96.2 251 392 470 11.4 25.7 52.4 95.3 236 389 474 10.1 24.8 49.1 94.9 256 386 479 3.48 10.2 25.1 49.5 95.0 250 419 489 4.55 10.5 23.8 50.1 94.9 238 390 437 3.54 10.4 25.1 45.5 85.6 240 390 459 "*5.97 13,2 23.9 52.7 95.5 238 408 498 *0.842 7.81 25.3 45.7 98.2 228 389 431 4.05 10.9 27.1 53.9 101 261 407 498 2.95 11.0 26.1 47.2 102 225 380 489 4.03 11.3 24.6 49.9 91.7 246 408 472 * Sample deactivated as an outlier (not included in summary statistics) *** Sample deactivated due to unacceptable internal standard response Page 33 Northwest Bioanalytical Study No. NWB S00-128 Report No. NWBR01-066 Table 10. Back-Calculated Concentrations of Calibration Standards for PFOA Quadratic weighted l/x 2. AU concentrations are expressed as ppb. (Continued) Run Date 14-Apr-2001 22-Apr-2001 23-Apr-2001 Run Number 19 21 18 2.11 2.13 *6.30 1.71 2:62 2.40 1.85 3.56 10.8 25.2 49.2 97.3 241 386 482 3.41 *6.57 3.35 3.45 3.82 3.21 10.4 26.2 47.9 94.7 225 382 506 12.2 23.8 49.9 93.1 275 364 474 10.4 24.8 51.8 95.2 226 384 466 10.7 28.4 48.9 99.2 213 435 489 10.7 27.5 49.8 80.4 262 388 483 10.9 23.4 54.2 92.6 255 381 465 Mean S.D. %CV %Bias n 2.16 0.266 12.3 2.4 19 3.43 0.449 13.1 -3.7 20 10.7 25.5 50.5 94.4 245 391 475 1.24 1.64 3.42 5.09 14.1 16.8 20.1 11.6 6.4 6.8 5.4 5.8 4.3 4.2 -0.9 1.2 2.6 -3.0 1.7 1.3 -1.5 24 24 24 24 34 24 24 * Sample deactivated as an outlier (not included in summary statistics) Page 34 Northwest B ioanalytical Study No. NWB S00-128 Report No. NWBR01-066 Table 10. Back-Calculated Concentrations of Calibration Standards for PFOA Quadratic weighted 1/x2. All concentrations are expressed as ppb. (Continued) Run Date 1l-May-2001 Run Number 25 1.44 2.88 10.1 24.5 48.5 96.6 241 385 481 1.46 2.95 9.39 25.2 45.5 90.0 245 399 482 1.33 3.14 11.0 26.3 45.6 94.6 242 371 487 Mean S.D. %CV! %Bias n 1.40 3.05 10.2 25.8 45.6 92.3 245 384 480 ISD ISD ISD ISD ISD ISD 14.1 14.4 12.9 ISD ISD ISD ISD ISD ISD 5.8 3.8 2.7 -2.8 5.9 1.0 5.3 -6.0 -4.5 1.7 -0.3 -0.2 2 2 2 2 2 2 34 10 10 ISD = insufficient data points for statistical calculations Page 35 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Table 11. Back-Calculated Concentrations of Calibration Standards Quadratic weighted l/x 2. All concentrations areexpressed as ppb. for PFOSAA Run Date Run 1.60 3.10 10.6 25.6 50.6 101 251 401 501 Number 27-Nov-2000 1 1.81 3.48 10.3 26.6 61.0 97.6 303 395 538 2g-Nov-2000 1.39 2.80 9.64 *50.8 *'17.1 77.2 252 369 467 I 2 1.45 2.36 8.59 24.5 51.0 92.0 282 364 491 1.77 3.84 12.0 *58.2 **22.6 101 293 399 491 23-Mar-2001 4 *7.76 4.18 10.6 24.9 46.5 94.5 301 321 525 1.32 3.23 10.3 17.3 59.0 108 243 459 460 24-Mar-2001 5 1.62 2.75 I 1.0 25.6 55.3 103 272 413 511 1.80 2.59 10.3 26.8 49.2 97.0 255 369 484 Mean S.D.[ %CV %Bias n 1.59 3.15 10.3 24.3 53.7 96.3 275 386 496 0.207 0.641 0.987 3.54 5.72 9.20 23.3 40.7 27.2 13.0 20.3 9.6 14.6 10.7 9.6 8.5 10.5 5.5 -0.6 1.6 -2.8 -5.1 6.1 -4.7 9.6 -3.7 - 1.0 7 8 8 6 6 8 8 8 8 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to sample preparation error Page 36 Northwest Bioanalytical Study No. NWB S00-128 Report No. NWBR01-066 Table 11. Back-Calculated Coneentrations of Calibration Standards for PFOSAA Quadratic weighted 1/x2. All concentrations are expressed as ppb. (Continued) Run Date 26-Mar-2001 Run Number 6 26-Mar-2001 7 28-Mar-2001 8 28-Mar-2001 9 30-Mar-2001 10 02-Apt-2001 13 07-Apr-2001 14 09-Apr-2001 15 12-Apr-2001 17 1.30 2.80 4.30 10.3 11.8 25.3 26.8 50.3 51.8 100 102 250 252 400 402 500 502 2.68 3.87 2.99 4.57 3.63 4.22 2.44 3.48 3.28 2.92 3.05 3.75 3.68 4.64 2.43 3.02 2.98 3.21 3.21 3.82 12.0 '19.7 11.3 10.4 10.6 14.6 11.8 9.06 14.6 10.6 23.8 48.1 86.7 250 26.7 65.1 99.3 287 28.1 59.3 90.3 292 26.7 45.8 108 282 24.9 58.9 97.5 242 27.2 51.7 101 269 33.2 59.2 110 257 21.9 52.8 88.1 302 28.0 48.4 103 253 25.9 47.1 111 271 2.32 5.07 3.13 4.16 11.0 27.2 54.9 101 280 10.7 24.3 54.1 97.1 262 2.68 3.97 3.29 3.72 12.1 29.8 49.7 107 266 12.1 20.8 54.2 107 244 2.87 3.34 3.18 4.62 9.14 26.5 49.8 107 268 10.8 26.9 56.0 111 286 3.20 3.67 11.9 29.5 50.8 102 240 ***0.932 3.88 12.0 26.8 51.6 '105 254 * Sample deactivated as an outlier (not included in summary statistics) *** Sample deactivated due to unacceptable internal standard response 358 505 461 463 463 446 380 459 378 503 439 481 380 516 386 473 417 459 419 495 433 513 q, 388 443 422 454 451 468 410 435 421 490 381 503 420 510 Page 37 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Run Date 14-Apr-2001 22-Apt-2001 23-Apr-2001 1l-May-2001 Table 11. Back-Calculated Concentrations of Calibration Standards for PFOSA.A Quadratic weighted l/x 2. All concentrations are expressed as ppb. (Continued) Run 1.30 2.80 Number 19 2.32 3.30 21 2.32 3.73 18 3.26 3.18 25 1.45 2.84 1.24 2.33 4.30 10.3 11.8 25.3 26.8 50.3 51.8 100 102 250 252 400 402 500 502 4.35 10.7 25.5 54.0 113 254 425 510 4.45 11.3 23.9 57.1 87.2 310 340 478 2.75 10.1 26.7 55.7 103 217 393 492 4.79 13.0 26.5 54.8 112 238 453 500 3.04 12.7 31.8 53.2 99.2 289 413 467 3.81 8.77 22.2 51.4 110 290 403 459 i0.6 28.3 52.3 102 266 428 495 10.3 23.2 48.1 94.5 257 386 472 Mean S.D. %CV %Bias n 1.35 2.97 ISD 0.437 ISD 14.7 3.8 6.1 2 25 3.88 10.5 11.4 25.8 26.5 50.2 53.5 98.3 102 262 267 407 410 484 480 0.634 ISD 1.50 ISD 2.90 ISD 4.48 ISD 8.01 ISD 22.9 ISD 32.1 ISD 24.6 16.3 ISD 13.2 ISD 10.9 ISD 8.4 ISD 7.9 ISD 8.6 ISD 7.8 ISD 5.1 -9.8 1.9 -3.4 2.0 -1.1 -0.2 3.3 -1.7 0.0 4.8 6.0 1.8 2.0 -3.2 -4.4 24 2 23 2 24 2 24 2 24 2 24 2 24 2 24 ISD = insufficient data points for statistical calculations Page 38 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Table 12. Back-Calculated Concentrations of Calibration Standards Quadratic weighted l/x 2. All concentrations are expressed as ppb. for PFOSA Run Date 27-Nov-2000 Run Number 1 28-Nov-2000 2 23-Mar-2001 4 24-Mar-2001 5 26-Mar-2001 6 26-Mar-2001 7 28-Mar-2001 8 28-Mar-2001 9 30-Mar-2001 10 30-Mar-2001 11 1.00 1.40 2.50 2.90 10.0 10.4 25.0 25.4 50.0 50.4 100 250 400 500 1.10 0.893 1.08 0.906 0.984 0.906 0.935 1.08 1.38 1.38 "2.12 1.41 *0.353 1.36 1.53 1.25 1.39 1.51 *2.96 1.39 2.57 9.38 27.4 52.7 2.46 10.0 "46.1 *'18.1 2.40 9.06 26.8 50.2 2.70 10.2 *48.6 *'19.1 2.94 9.66 26.3 50.7 2.80 10.6 17.0 49.6 2.47 10.1 24.6 51.2 2.40 10.1 26.3 49.2 2.93 9.65 24.1 3.10 "16.2 26.6 3.01 10.3 26.6 2.79 10.0 26.1 3.21 11.1 25.2 2.74 10.1 25.5 3.37 10.2 30.2 2.65 8.72 21.7 2.47 12.1 27.1 2.83 9.54 26.4 2.91 11.1 23.8 2.95 9.56 24.4 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to sample preparation error 97.7 287 378 569 87.8 242 349 497 97.9 283 354 560 93.3 256 377 480 93.2 285 370 522 106 240 43 l 458 98.1 255 406 517 98.4 247 382 497 43.9 94.7 245 382 491 58.7 101 260 453 471 50.7 88.9 251 423 461 46.4 110 273 377 518 54.8 99.8 240 409 527 45.6 96.8 247 401 479 51.2 106 254 388 500 49.8 89.4 304 387 471 48.9 92.0 238 409 488 48.9 104 261 416 492 50.3 99.9 259 383 448 58.4 "154 203 476 524 Page 39 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Table 12. Back-Calculated Concentrations of Calibration Standards for PFOSA Quadratic weighted l/x 2. All concentrations are expressed as ppb. (Continued) Run Date 02-Apr-2001 Run Number 13 07-Apt-2001 14 09-Apr-2001 15 1l-Apr-2001 16 12-Apr-2001 17 23-Apr-2001 18 1.00 1.40 2.50 2.90 10.0 10.4 25.0 25.4 50.0 50.4 100 250 400 500 1.06 1.66 1.14 1.66 *2.32 1.40 1.59 1.23 .m 1.47 ***0.557 1.44 1.33 2.93 3.32 3.23 2.58 2.77 3.11 2.67 3.I6 2.55 2.86 3.00 3.01 10.2 26.1 9.31 24.0 10.9 29.4 10.1 18.9 9.77 28.9 9.74 23.9 9.79 22.9 9.03 26.6 10.5 29.5 11.0 25.2 9.87 28.1 9.81 23.4 52.2 99.3 262 429 517 51.2 97.3 249 393 452 52.0 109 285 426 502 48.0 97.7 227 399 457 51.8 112 281 429 518 46.7 92.5 232 364 472 55.6 88.9 285 346 473 54.6 111 241 416 533 47.5 103 223 386 536 47.4 102 247 403 501 49.5 83.9 256 405 481 50.8 115 269 389 503 Mean S.D %CV i %Bias n 0.986 0.0884 9.0 -1.4 8 1.40 0.158 11.3 0.0 19 2.59 2.92 9.89 10.1 24.7 25.6 50.6 0.201 0.244 0.493 0.758 3.90 2.63 1.26 7.8 8.4 5.0 7.5 15.8 10.3 2.5 3.6 0.7 -1.1 -2.9 -1.2 0.8 1.2 8 24 8 23 6 24 6 * Sample deactivated as an outlier (not included in summary statistics) *** Sample deactivated due to unacceptable internal standard response 50.6 98.9 256 398 497 3.78 7.71 21.8 29.0 30.3 7.5 7.8 8.5 7.3 6.1 0.4 -1.1 2.4 -0.5 -0.6 24 31 32 32 32 Page 40 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Table 13. Back-Calculated Concentrations of Calibration Standards Quadratic weighted l/x 2. All concentrations are expressed as ppb. for M556 Run Date Run 2.50 3.20 Number 27-Nov-2000 1 2.81 10.0 10.7 25.0 25.7 50.0 50.7 100 101 250 251 400 401 500 501 10.2 27.5 56.0 98.1 287 421 555 28-Nov-2000 24-Mar-2001 ......... 26-Mar-2001 26-Mar-2001 28-Mar-2001 30-Mar-2001 30-Mar-2001 2.23 8.65 *45.7 ** 17.3 84.1 235 360 451 2 2.20 9.06 24.5 48.3 91. l 269 378 499 2.83 10.7 "53.6 **21.2 106 274 404 486 5 2.05 9.42 24.5 52.5 104 256 407 504 2.98 10.0 24.7 49.8 99.5 248 384 499 I 6 3.16 9.86 23. l 43.9 86.7 234 361 497 3.08 13.9 25.7 60.8 97.4 271 460 496 7 3.15 10.5 25.7 55.1 85.8 258 445 468 3.15 12.1 26.0 45.1 101 263 381 506 8 3.13 9.57 29.3 53.8 91.5 234 373 508 *4.76 12.2 25.6 47.5 96.3 255 440 504 F, l0 2.75 12.4 27.1 49.3 96.9 245 407 485 3.55 10.4 24.0 47.4 l 01 265 416 496 Il 3.36 12.2 23.8 52.0 102 247 364 445 3.00 10.2 23.2 58.2 *145 209 487 538 01-Apr-2001 12 3.90 10.7 29.4 56.4 102 263 398 498 2.63 8.84 23.4 52.9 80.0 289 383 490 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to sample preparation error Page 41 Northwest Bioanalytical Study No. NWBS00-128 Report No. N3,VBR01-066 Run Date 07-Apr-2001 09-Apt-2001 12-Apt-2001 14-Apr-2001 23-Apr-2001 Table 13. Back-Calculated Coneentrations of Calibration Standards for M556 (Continued) Quadratic weighted l/x 2. All concentrations are expressed as ppb. Run 2.50 3.20 10.0 10.7 25.0 25.7 50.0 50.7 100 101 250 251 400 401 500 501 Number 14 3.47 9.97 28.4 49.5 99.9 258 425 478 2.95 11.4 20.9 54.3 104 239 427 477 15 2.68 8.84 27.5 49.7 108 254 421 459 3.93 9.80 24.8 52.2 103 266 416 489 17 2.67 10.5 25.8 46.2 97.3 226 368 490 3.68 11.4 26.2 54.6 105 255 441 523 19 3.21 9.15 25.9 51.3 106 225 408 530 3.30 11.0 23.8 55,8 96.2 303 348 488 18 2.89 10.2 25.8 51.1 81.9 253 402 461 3.65 9.66 23.7 53.8 115 295 419 488 Mean S.D. %CV %Bias n 2.52 3.20 9.67 10.7 25.3 25.4 51.7 51.9 97.1 97.9 262 255 392 409 499 492 0.400 0.387 0.765 1.29 1.47 2.12 3.38 4.29 8.23 8.74 18.9 22.7 22.3 34.9 33.6 22.4 15.9 12.1 7.9 12.1 5.8 8.3 6.5 8.3 8.5 8'9 7.2 8.9 5.7 8.5 6.7 4.6 0.8 0.0 -3'.3 0.0 1.2 -1.2 3.4 2.4 -2.9 -3.1 4.8 1.6 -2.0 2.0 -0.2 -1.8 6 21 6 22 4 22 4 22 6 21 6 22 6 22 6 22 Page 42 Northwest Bioanalytieal Run Date 27-Nov-2000 Run Number 1 28-Nov-2000 2 24-Mar-2001 5 26-Mar-2001 6 26-Mar-2001 7 28-Mar-2001 8 30-Mar-2001 10 01 -Apr-2001 12 02-Apr-2001 13 Study No. NWBS00-128 Report No. NWBR01-066 Table 14. Baek-Caleulated Concentrations of Calibration Standards Quadratic weighted l/x 2. All concentrations are expressed as ppb. for M570 1.00 1.80 2.50 3.30 10.0 10.8 25.0 25.8 50.0 50.8 100 101 250 251 400 401 500 501 1.05 1.01 0.991 *1.56 0.927 1.15 2.47 9.76 26.4 58.7 94.4 275 390 530 2.09 10.1 *50.6 **18.6 87.5 266 374 472 2.16 8.82 23.2 52.0 88.8 269 374 480 2.90 11.4 *58.7 *'21.2 101 274 407 507 2.07 10.3 26.0 55.4 96.9 263 414 507 2.40 9.59 26.1 50.6 97.2 241 382 492 1.60 2.96 10.5 24.6 48.6 90.0 238 354 489 2.08 3.37 * 18.0 28.3 *69.4 108 296 461 474 2.04 3.40 9.97 25.7 56.3 89.3 274 462 464 1.49 3.55 10.2 27.4 44.2 105 262 385 469 1.89 3.04 9.96 25.8 60.0 101 228 405 503 1.90 2.84 12.3 25.4 48.3 94.2 262 435 473 1.87 2.55 12.8 28.6 48.7 98.3 234 413 468 2.08 2.73 9.87 26.2 47.6 109 279 410 500 2.15 3.70 i 0.3 32.2 56.2 103 254 387 508 1.60 2.53 8.98 22.4 53.2 '86.3 297 370 496 1.53 2.87 10.3 27.1 54.5 98.1 258 426 522 2.25 3.19 10,3 24.4 54.2 101 266 382 450 * Sample deactivated as an outlier (not included in summary statistics) ** Sample deactivated due to sample preparation error Page 43 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Table 14. Back-Calculated Coneentrations of Calibration Standards for M570 (Continued) Quadratic weighted l/x 2. All concentrations are expressed as ppb. RunDate 07-Apr-2001 Run Number 14 09-Apt-2001 15 12-Apr-2001 17 14-Apt-2001 19 22-Apr-2001 21 24-Apt-2001 22 1l-May-2001 25 1.00 1.80 2.50 3.30 10.0 10.8 25.0 25.8 50.0 50.8 100 101 250 251 400 401 500 501 1.65 3.24 10.9 30.4 52.3 109 263 436 475 2.11 2.80 10.8 19.4 52.0 102 231 426 466 1.98 2.39 8.68 26.3 48.4 107 255 403 448 1.86 3.60 10.1 27.6 54.8 107 279 424 491 2.03 2.78 ***0.564 2.92 11.5 28.1 11.3 24.7 50.5 103 229 387 517 51.2 104 248 416 501 1.46 2.18 1.94 "3.02 3.44 9.54 25.8 3.19 10.2 24.0 2.56 10.9 25.2 3.40 12.4 27.2 52.4 112 240 418 521 56.6 88.5 310 340 477 54.0 106 214 395 502 48.9 101 214 448 518 1.68 3.12 10.1 22.5 53.7 119 268 390 508 2.15 2.76 10.4 29.0 52.8 86.3 263 406 470 1.03 2.64 10.3 26.8 50.8 99.5 257 435 466 1.01 2.12 9.85 24.6 46.9 98.6 267 370 508 Mean S.D. %CV %Bias n 1.02 0.0677 6.6 2.0 7 1.89 0.246 t3.0 5.0 22 2.36 3.04 10.0 10.5 25.5 26.2 52.4 0.302 0.371 0.736 1.01 1.36 2.72 4.12 12.8 12.2 7.4 9.6 5.3 10.4 7.9 -5.6 -7.9 0.0 -2.8 2.0 1.6 4.8 8 24 8 23 6 24 6 52.1 95.5 101 264 257 393 407 495 488 3.64 4.94 8.50 10.9 25.4 23.2 30.6 21.7 22.4 7.0 5.2 8.4 4.1 9.9 5.9 7.5 4.4 4.6 2.6 -4.5 0.0 5.6 2.4 -1.8 1.5 -1.0 -2.6 23 8 24 8 24 8 24 8 24 * Sample deactivated as an outlier (not included in summary statistics) *** Sample deactivated due unacceptable internal standard response Page 44 NorthwestBioanalytical StudyNo. NWBS00-128 ReportNo. NV/BR01-066 Table 15. Analytical QC Summary for PFOS All concentrations are expressed as ppb. Run Date Run Number Low QC 6.40 ppb Low QC 5.75 ppb Medium QC 126 ppb Medium QC 126 ppb High QC 332 ppb High QC 332 ppb 27-Nov-2000 28-Nov-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 i ........... Preparation Date 1 2 4 5 6 7 8 9 27-Oct-2000 05-Apr-2001 27-Oct-2000 05-Apr-2001 27-Oct-2000 08-Mar-2001 5.91 6.13 6.49 5.82 *4.60 6.50 6.36 6.49 5.88 6.49 6.70 5.88 5.58 6.29 5.65 5.14 121 127 121 125 135 "192 134 131 **74.2 119 139 123 117 133 .......... 141 140 320 372 347 351 354 333 343 362 304 344 326 323 348 323 357 344 >+90% deviation fi'om theoretical * Sample deactivated due to unacceptable internal standard response High QC 331 ppb 05-Apr-2001 High QC 348 ppb DF=5 08-Mar-2001 Page 45 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Table 15. Analytieal QC Summary for PFOS (Continued) All concentrations are expressed as ppb. Run Date Run Number Low QC 6.40 ppb 30-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apt-2001 09-Apr-2001 1l-Apr-2001 12-Apr-2001 Preparation Date 10 11 13 14 15 16 17 27-Oct-2000 6.08 5.74 6.60 5.82 6.47 6.65 6.21 6.22 5.78 ....... 5.84 6.99 6.51 6.25 6.20 Low QC 5.75 ppb Medium QC 126 ppb 05-Apr-2001 27-Oct-2000 127 138 126 118 130 137 123 125 132 135 130 122 137 141 Medium QC 126 ppb 05-Apr-2001 High QC 332 ppb 27-Oct-2000 High QC 332 ppb High QC 331 ppb 08-Mar-2001 05-Apr-2001 324 332 328 *'149 346 330 373 330 332 i .... 357 339 345 357 352 High QC 348 ppb DF=5 08-Mar-2001 353 357 365 ** Sample deactivated due to unacceptable internal standard response Page 46 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Table 15. Analytical QC Summary for PFOS (Continued) All concentrations are expressed as ppb. Run Date 23-Apt-2001 Run Number Low QC 6.40 ppb Preparation 27-Oct-2000 Date 18 Low QC 5."/5 ppb Medium QC 126 ppb Medium QC !26 ppb High QC 332 ppb 05-Apt-2001 27-Oet-2000 05-Apr-2001 27-Oet-2000 '6.57 138 6.84 130 High QC 332 ppb 0g-Mar-2001 High QC 331 ppb 05-Apr-2001 296 330 High QC 348 ppb DF=5 08-Mar-2001 Mean S.D %CV %Theoretical %Bias n 6.11 0.492 8.1 95.5 -4.5 30 6.71 ISD ISD 116.7 16.7 2 132 13.7 10.4 104.8 4.8 29 134 348 339 313 ISD 16.3 15.8 ISD ISD 4.7 4.7 ISD 106.3 104.8 102.1 94.6 6.3 4.8 2.1 -5.4 2 8 21 2 358 6.11 1.7 102.9 2.9 3 ISD = insufficient data points for statistical calculation Page 47 Northwest Bioanalytical Run Date 27-Nov-2000 Run Number Preparation Date 1 28-Nov-2000 2 23-Mar-2001 4 24-Mar-2001 5 26-Mar-2001 6 26-Mar-2001 7 28-Mar-2001 8 28-Mar-2001 9 Table 16. Analytical QC Summary for PFHS All concentrations are expressed as ppb. Low QC 4.48 ppb 27-Oct-2000 Low QC 4.48 ppb 05-Apr-2001 Medium QC 156 ppb 27-Oct-2000 Medium QC 157 ppb 05-Apr-2001 High QC 417 ppb 27-Oct-2000 3.61 161 382 4.28 148 443 3.70 157 411 3.86 153 445 4.29 155 428 4.06 171 406 3.96 164 414 4.02 161 460 4.85 ** 128 5.07 157 4.71 157 4.95 135 5.31 158 4.35 158 4.32 158 3.92 158 ** Sample deactivated due to unacceptable internal standard response Smdy No. NWB S00-128 Report No. NWBR01-066 High QC 417 ppb 08-Mar-2001 High QC 418 ppb 05-Apr-2001 373 396 411 407 420 383 392 415 Page 48 Northwest Bioanalytical Run Date 30-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 11-Apr-2001 12-Apr-2001 Table 16. Analytical QC Summary for PFHS (Continued) All concentrations are expressed as ppb. Run Number Preparation Date 10 11 13 14 15 16 17 Low QC 4.48 ppb 27-Oct-2000 Low QC 4.48 ppb 05-Apr-2001 Medium QC 156 ppb 27-Oct-2000 Medium QC 157 ppb 05-Apr-2001 High QC 417 ppb 27-Oct-2000 '3.48 136 4.29 146 4.08 151 4.06 154 4.20 158 4.38 158 4.87 153 4.25 149 3.92 156 3.68 152 4'.85 155 3.62 155 4.14 157 4.43 153 * >+90% deviation from theoretieal ** Sample deactivated due to unacceptable internal standard response Study No. NWBS00-128 Report No. NWBR01-066 High QC 417 ppb 08-Mar-2001 413 345 391 **200 428 436 408 378 444 401 387 383 397 404 High QC 418 ppb 05-Apr-2001 Page 49 Norlhwest Bioanalytical Run Date 23-Apr-2001 Table 16. Analytieal QC Summary for PFHS (Continued) All concentrations are expressed as ppb. Run Number Preparation Date 18 Low QC 4.48 ppb 27-Oct-2000 Low QC 4.48 ppb 05-Apt-2001 3.87 4.05 Medium QC 156 ppb 27-Oct-2000 Medium QC 157 ppb 05-Apt-2001 166 145 High QC 417 ppb 27-Oct-2000 Study No. NWB S00-128 Report No. NWBR01-066 High QC 417 ppb 08-Mar-2001 High QC 418 ppb 05-Apr-2001 397 389 Mean S.D. %CV %Theoretical %Bias n 4.25 3.96 155 0.467 ISD 7.17 11.0 ISD 4.6 94.9 88.4 99.4 -5.1 -I 1.6 -0.6 30 2 29 156 424 401 393 ISD 25.3 22.6 ISD ISD 6.0 5.6 ISD 99.4 101.7 96.2 94.0 -0.6 1.7 -3.8 -6.0 2 8 21 2 ISD = insufficient data points for statistical calculation Page 50 Noithwest Bioanalytical Study No. NWBS00-128 Report No. NWBROI-066 Table 17. Analytical QC Summary for PFOA All concentrations are expressed as ppb. Run Date Run Number Preparation Date Low QC 4.81 ppb 27-Oct-2000 Low QC 4.32 ppb 05-Apr-2001 Low QC 4.32 ppb 02-May-2001 Medium QC I Medium QC 145 ppb 145 ppb 27-Oct-2000 05-Apr-2001 High QC 385 ppb 27-Oet-2000 High QC 385 ppb 08-Mar-2001 High QC 385 ppb 05-Apr-2001 27-Nov-2000 1 4.55 154 403 4.30 28-Nov-2000 2 4.35 3.92 160 429 151 416 162 439 23-Mar-2001 4 24-Mar-2001 5 "2.72 4.85 4.09 159 412 152 381 143 390 26-Mar-2001 6 *3.69 4.12 151 *'124 377 393 4.81 152 395 26-Mar-2001 7 5.47 146 348 4.93 140 384 28 -Mar-2001 8 4.63 151 404 28-Mar-2001 9 "0.161 4.33 3.89 156 158 ......... 157 375 404 I 433 * >+20% deviation fiom theoretical ** Sample deactivated due to unacceptable internal standard response Page 51 Northwest Bioanalytieal Study No. NWB S00-128 Report No. N_VBR01-066 Table 17. Analytieal QC Summary for PFOA All concentrations are expressed as ppb. (Continued) Run Date 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 12-Apr-2001 14-Apr-2001 22-Apr-2001 23-Apr-2001 Run Number Preparation Date 10 13 14 15 Low QC 4.81 ppb 27-Oot-2000 Law QC 4.32 ppb 05-Apt-2001 4.29 4.14 4.56 4.15 "5.97 4.77 4.45 "3.61 Law QC 4.32 ppb 02-May-2001 Medium QC I Medium QC 145 ppb 145 ppb High QC 385 ppb 27-Oct-2000 05-Apt-2001 27-Oct-2000 151 155 145 139 145 136 159 147 17 4.17 4.07 19 "3.79 5.04 21 4.03 3.90 18 3.82 4.67 151 158 131 * 109 143 170 141 151 >+90% deviation from theoretical High QC 385 ppb 08-Mar-2001 393 382 381 336 381 361 406 351 372 375 377 401 401 361 High QC 385 ppb 0S-Apt-2001 370 414 Page 52 t Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Table 17. Analytieal QC Summary for PFOA (Continued) All concentrations are expressed as ppb. Run Date I l-May-2001 Run Number Preparation Date 25 Low QC 4.81 ppb 27-Oct-2000 Low QC 4.32 ppb 05-Apr-200l Low QC 4.32 ppb 02-May-2001 4.16 4.65 Medium QC Medium QC 145 ppb 145 ppb 27-Oct-2000 05-Apr-2001 High QC 385 ppb 27-Oct-2000 150 148 High QC 385 ppb 0g-Mar-2001 High QC 385 ppb 05-Apr-2001 386 398 Mean S.D. %CV %Theoretical %Bias n 4.19 4.25 0.970 ISD 23.2 'ISD 87.1 98.4 -12.9 -1.6 30 2 4.41 149 148 " 406 382 ISD ! ! .5 4.5 ! 22.3 22.5 ISD 7.7 3.0 5.5 5.9 102.1 102.8 102.1 105.5 99.2 2.1 2.8 2.1 5.5 -0.8 2 29 4 8 22 ISD = insufficient data points for statistical calculation 392 18.6 4.7 101.8 1.8 4' Page 53 Northwest Bioanalytical Table 18. Analytical QC Summary for PFOSAA All concentrations are expressed as ppb. Study No. NWBS00-128 Report No. NWBR01-066 Run Date 27-Nov-2000 28-Nov-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 Run Number Preparation Date 1 2 4 5 6 7 8 9 Low QC 4.60 ppb 27-Oct-2000 Low QC 4.30 ppb 05-Apt-2001 Low QC 4.30 ppb 02-May-2001 Medium QC 151 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 High QC 401 ppb 27-Oct-2000 4.22 *3.38 4.50 3.66 "2.38 4.11 4.22 4.11 4.55 4.98 4.85 4.26 *6.56 4.31 4.16 4.41 141 398 167 425 150 378 165 368 172 463 *374 456 157 422 157 389 *'71.5 130 146 135 145 142 , 183 175 * >+95% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response High QC 401 ppb 08-Mar-2001 348 445 365 384 415 383 440 415 High QC 400 ppb 05-Apr-2001 t Page 54 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Table 18. Analytical QC Summary for PFOSAA All concentrations are expressed as ppb. (Continued) Run Date 30-Mar-2001 02-Apr-2001 07-Apt-2001 09-Apt-2001 12-Apt-2001 14-Apr-2001 22-Apr-2001 23-Apt-2001 Run Number Preparation Date 10 13 14 15 17 19 21 18 Low QC 4.60 ppb 27-Oct-2000 5.47 4.96 *6.00 5.38 5.41 4.70 4.61 3.71 5.23 5.04 4.60 5.43 *6.60 4.64 Low QC 4.30 ppb 05-Apt-2001 Low QC 4.30 ppb 02-May-2001 Medium QC 151 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apt-2001 High QC 401 ppb 27-Oct-2000 149 170 154 153 166 154 170 165 178 '189 160 123 149 "218 4.41 167 5.33 169 * >+_5% deviation from theoretical High QC 401 ppb 08-Mar-2001 380 376 412 360 452 439 426 380 465 448 420 429 432 413 High QC 400 ppb 05-Apr-2001 398 427 Page 55 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Table 18. Analytieal QC Summary for PFOSAA All concentrations are expressed as ppb. (Continued) Run Date 1l-May-2001 Run Number Preparation Date Low QC 4.60 ppb 27-Oct-2000 25 Low QC 4.30 ppb 05-Apt-2001 .q Low QC 4.30 ppb 02-May-2001 4.34 3.95 Medium QC 151 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apt-2001 High QC 401 ppb 27-Oct-2000 143 145 High QC 401 ppb 08-Mar-2001 Higl_ QC 400 ppb 05-Apr-2001 424 407 Mean S.D %CV %Theoretical %Bias n 4.68 0.882 18.8 101.7 1.7 30 4.87 4.15 ISD ISD ISD ISD 113.3 96.5 13.3 -3,5 2 2 167 44.2 26.5 110.6 10.6 29 156 13.9 8.9 104.0 4.0 4 ISD = insufficient data points for statistical calculations 412 35.1 8.5 102.7 2.7 8 410 33.2 8.1 102.2 2.2 22 414 13.8 3.3 103.5 3.5 4 Page 56 Northwest Bioanalytical Table 19. Analytical QC Summary for PFOSA All concentrations are expressed as ppb. Run Date 27-Nov-2000 28-Nov-2000 23-Mar-2001 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 28-Mar-2001 Run Number Preparation Date 1 2 4 5 6 7 8 9 Low QC 4.00 ppb 27-Oct-2000 Low QC 4.00 ppb 05:Apr-2001 Medium QC 150 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apt-2001 High QC 400 ppb 27-Oct-2000 4.39 147 399 4.12 162 466 4.86 146 416 3.97 158 386 *2.33 180 434 4.47 *328 417 3.94 156 423 4.21 158 399 3.85 ,,m 3.85 **72.6 133 4.80 141 3.98 133 .4.16 146 3.58 155 3.84 173 3.82 157 * >+9.5% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response Study No. NWB S00-128 Report No. NWBR01-066 High QC 400 ppb 08-Mar-2001 High QC 400 ppb 05-Apt-2001 311 457 369 396 431 406 447 408 Page 57 Northwest Bioanalyt!cal Table 19. Analytieal QC Summary for PFOSA All concentrations are expressed as ppb. (Continued) Run Date 30-Mar-2001 30-Mar-2001 02-Apr-2001 07-Apr-2001 09-Apr-2001 11-Apr-2001 12-Apr-2001 Run Number Preparation Date 10 11 13 14 15 16 17 Low QC 4.00 ppb 27-Oct-2000 4.16 3.96 *5.14 4.08 4.21 4.39 4.79 4.46 4.19 3.92 *5.84 4.95 4.53 4.38 Low QC 4.00 ppb 05-Apt-2001 Medium QC 150 ppb 27-Oet-2000 144 161 138 124 148 159 150 147 157 157 ] 165 127 155 170 Medium QC 150 ppb 05-Apr-2001 High QC 400 ppb 27-Oct-2000 * >4-9-5%deviation from theoretical ** Sample deactivated due to unacceptable internal standard response Study No. NWBS00-128 Report No. NW'BR01-066 High QC 400 ppb 0g-Mar-2001 400 368 392 *'170 431 361 456 424 423 422 404 425 437 403 High QC 400 ppb 05-Apt-2001 Page 58 Northwest Bioanalytical Table 19. Analytical QC Summary for PFOSA All concentrations are expressed as ppb. (Continued) Run Date 23 -Apr-200 i Run Number Preparation Date 18 Low QC 4.00 ppb 27-Oct-2000 Low QC 4.00 ppb 05-Apr-2001 4.95 4.73 Medium QC 150 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 178 170 High QC 400 ppb 27-Oct-2000 Study No. NWBS00-128 Report No. NWBR01-066 High QC 400 ppb 08-Mar-2001 High QC 400 ppb 05-Apr-2001 392 436 Mean S.D. ! %CV %Theoretical %Bias n 4.24 0.596 14.1 106.0 6.0 30 4.84 ISD ISD 121.0 21.0 2 158 35.3 22.3 105.3 5.3 29 174 ISD ISD 116.0 16.0 2 418 24.9 6.0 104.5 4.5 8 ISD = insufficient data points for statistical calculations 408 34.9 8.6 102.0 2.0 21 414 ISD ISD 103.5 3.5 2 Page 59 Northwest Bioanalytical Study No. NWBS00-128 Report No. N_VBR01-066 Table 20. Analytieal QC Summary for M556 All concentrations are expressed as ppb. Run Date Run Number Low QC 4.00 ppb Low QC 4.00 ppb Medium QC 150 ppb Medium QC 150 ppb High QC 400 ppb High QC 400 ppb High QC 400 ppb Preparation Date 27-Oct-2000 05-Apr-2001 27-Oct-2000 05-Apr-2001 27-Oct-2000 08-Mar-2001 05-Apr-2001 27-Nov-2000 1 4.09 133 423 3.23 161 439 28-Nov-2000 2 _4.52 144 393 3.60 166 24-Mar-2001 5 4.77 160 389 402 3.60 156 401 26-Mar-2001 6 3.52 **79.4 367 ,.= 4.07 137 428 \ 26-Mar-2001 7 4.45 137 354 *2.73 124 404 28-Mar-2001 8 *6.68 164 426 4.15 166 388 30-Mar-2001 10 *4.85 149 382 ._. 4.06 171 30-Mar-2001 11 ***7.47 146 4.28 126 0 l-Apr-20Ol 12 "5.69 162 4.35 158 385 369 *'173 396 388 * >:t:20% deviation from theoretical ** Sample deactivated due to unacceptable internal standard response *** Sample deactivated due to carryover Page 60 Northwest Bioanalytieal J Study No. NWBS00-128 Report No. NWBR01-066 Table 20. Analytieal QC Summary for M556 (Continued) All concentrations are expressed as ppb. Run Date 07-Apr-2001 09-Apr-2001 12-Apr-2001 14-Apr-2001 23-Apt-2001 Run Number Preparation Date Low QC 4.00 ppb 27-Oet-2000 14 4.73 3.51 15 4.02 "3.14 17 4.40 4.29 19 3.75 4.71 18 Low QC 4.00 ppb 05-Apr-2001 4.51 4.11 Medium QC 150 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 High QC 400 ppb 27-Oct-2000 152 145 171 164 164 162 155 "115 407 387 180 160 High QC 400 ppb 08-Mar-2001 434 395 395 387 396 406 High QC 400 pph 05-Apr-2001 381 395 Mean S.D %CV %Theoretical %Bias n 4.21 4.31 152 170 406 395 388 0.818 ISD 15.5 ISD 21.0 20.3 ISD 19.4 ISD 10.2 ISD 5.2 5.1 ISD 105.3 107.8 101.3 113.3 101.5 98.8 97.0 5.3 7.8 1.3 13.3 1.5 -1.3 -3.0 25 2 25 2 6 19 2 * >:t20% deviation fiom theoretical ISD = insufficient data points for statistical calculations Page 61 Northwest B ioanalytical Study No. NWB S00-128 Report No. NWBR01-066 Table 21. Analyfieal QC Summary for M570 All concentrations arc expressed as ppb. Run Date 27-Nov-2000 28-Nov-2000 24-Mar-2001 26-Mar-2001 26-Mar-2001 28-Mar-2001 30-Mar-2001 01-Apr-2001 Run Number Preparation Date Low QC 4.00 ppb 27-Oct-2000 1 3.61 "3.07 2 4.10 3.59 5 3.81 3.89 6 3.63 4.00 7 4.75 3.26 8 "5.01 3.25 10 4.64 3.54 12 3.78 3.60 Low QC 4.00 pph 05-Apt-2001 Low QC 4.00 ppb 02-May-2001 Medium QC 150 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 High QC 400 ppb .27-Oet-2000 149 388 163 451 151 383 169 394 168 415 165 412 **74.2 140 150 133 156 161 150 180 166 169 >:t.20% deviation from theoretical * Sample deactivated due to unacceptable internal standard response High QC 400 ppb 0g-Mar-2001 338 447 344 403 433 396 359 379 411 364 High QC 400 ppb 05-Apr-2001 Page 62 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Table 21. Analytieal QC Summary for M570 (Continued) All concentrations are expressed as ppb. Run Date 02-Apt-2001 07-Apr-2001 09-Apt-2001 12-Apt-2001 14-Apr-2001 22-Apt-2001 24-Apr-2001 Run Number Preparation Date 13 14 15 17 19 21 22 Low QC 4.00 ppb 27-Oct-2000 4.55 3.99 4.80 4.37 3.91 *2.69 4.38 4.28 4.17 4.26 *5.54 3.89 Low QC 4.00 ppb 05-Apr-2001 Low QC 4.00 ppb 02-May-2001 Medium QC 150 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 High QC 400 ppb 27-Oct-2000 *3.11 4.18 156 162 159 156 168 163 172 "185 158 120 146 *207 178 168 * >:t20% deviation from theoretical High QC 400 ppb 08-Mar-2001 High QC 400 ppb 05-Apt-2001 405 352 446 423 380 375 447 446 413 423 . 447 413 373 393 Page 63 Northwest Bioanalytical Study No. NWBS00-128 Report No. N_VBR01-066 Table 21. Analytical QC Summary for M570 (Continued) All concentrations are expressed as ppb. Run Date =- 1l-May-2001 Run Number Preparation Date Low QC 4.00 ppb 27-Oct-2000 25 Low QC " 4.00 ppb Low QC 4.00 ppb 05-Apr-2001 02-May-2001 Medium QC 150 ppb 27-Oct-2000 Medium QC 150 ppb 05-Apr-2001 High QC 400 ppb 27-Oct-2000 4.51 143 *2.83 149 High QC 400 ppb 08-Mar-2001 High QC 400 ppb 05-Apr-2001 417 408 Mean S.D. %CV %Theoretical %Bias n 4.01 3.65 3.67 160 160 407 402 398 0.621 ISD ISD 16.6 16.3 25.0 35.4 19.2 15.5 ISD ISD 10.4 10.2 6.1 8.8 4.8 100.3 91.3 91.8 106.7 106.7 101.8 100.5 99.5 0.3 -8.8 -8.3 6.7 6.'/ 1.8 0.5 -0.5 28 2 2 27 4 6 22 4 * >-_:20%deviation from theoretical ISD = insufficient data points for statistical calculations Page 64 Northwest Bioanalytieal Sample ID 10956 PFOS Concentration (ppb) 54.1 10957 51.3 10958 80.5 10959 69.3 10960 37.3 10961 10962 I 10963 48.4 55.7 .... 42.0 10964 114 10965 45.0 10966 29.2 10967 31.7 10968 42.8 10969 37.9 10970 46.7 10971 13.4 10972 24.0 10973 34.1 Table 22. Study Sample Concentrations All concentrations are expressed as ppb. PFHS* Concentration (ppb) 3.10 5.45 12.4 3.01 2.95 2.79 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 8.00 <LLOQ(2.09) <LLOQ(2.09) 9.26 2.96 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 3.68 PFOA* Concentration (ppb) 3.95 6.64 22.2 13.9 5.13 2.77 4.44 6.58 7.07 3.90 <LLOQ(2.11) <LLOQ(2.11) 5.17 <LLOQ(2. I 1) 3.35 <LLOQ(2.11 ) <LLOQ(2.11) 5.11 PFOSAA* Concentration (ppb) 3.68 <LLOQ(2.80) 7.59 4.13 <LLOQ(2.80) <LLOQ(2.80) 4.21 3.55 9.05 <LLOQ(2.80) 2.81 4.58 <LLOQ(2.80) 4.23 3.08 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(I.40) <LLOQ(1.401 <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) Study No. NWBS00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ(1.80) 3.10 <LLOQ(I.80) 2.26 <LLOQ(1.80) 6.18 <LLOQ(I.80) <LLOQ(1.80) 4.97 2.55 <LLOQ(1.80) <LLOQ(1.80) 4.72 <LLOQ(1.80) <LLOQ(I.80) <LLOQ( 1.80) <LLOQ(1.80) <LLOQ(I.80) The method acceptance criteria states that the measured concentration for each QC must be within +90% (:.+_25%for PFOSA and PFOSA.A) office target coneentratiott. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 65 Northwest Bioanalytical Sample ID 10974 10975 10976 10977 10978 10979 10980 10981 10982 10983 10984 10985 10986 10987 10988 10989 10990 10991 PFOS Concentration (ppb) 51.8 35.8 44.0 99.7 48.7 44.2 57.7 25.8 46.4 38.6 75.1 41.9 57.7 14.0 39.2 68.9 38.6 36.6 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppbl <LLOQ(2.09) 5.73 2.62 5.98 <LLOQ(2.09) <LLOQ(2.091 3.66 4.98 7.28 <LLOQ(2.09) <LLOQ(2.09) 6.97 3.26 <LLOQ(2.09) 2.17 2.53 <LLOQ(2.09) 2.11 PFOA* Concentration (ppb) 3.37 3.04 7.32 6.94 3.23 3.16 4.86 2.59 2.20 <LLOQ(2.111 17.4 2.22 5.04 <LLOQ(2. l 1) <LLOQ(2.111 5.28 4.42 <LLOQ(2.11) PFOSAA* Concentration (ppb) 3.46 3.43 3.43 8.67 4.47 <LLOQ(2.80) 4.33 <LLOQ(2.80) <LLOQ(2.80) 3.90 3.44 <LLOQ(2.80) 5.09 <LLOQ(2.80) <LLOQ(2.80/ <LLOQ(2.80) <LLOQ(2.80) 3.45 PFOSA* Concentration (ppb) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.401 <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) Study No. NWBS00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.201 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570 _ Concentration (ppb) <LLOQ(I.80) 2.03 <LLOQ(I.80) <LLOQ(1.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(I.80) 5.13 <LLOQ(1.80) <LLOQ(I.80) 2.86 <LLOQ(I.80) 3.3 l <LLOQ(I.80/ 3.16 <LLOQ(1.80) <LLOQ(I.80/ The method acceptance criteria states that the measured concentration for each QC must be within +90% (+95% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using calibration curves (see Results and Discussion section). : Page 66 Northwest Bioanalytical Sa ml;e ID 10992 10993 10994 10995 10996 10997 10998 10999 11000 11001 11002 11003 11004 11005 11006 11007 Jl1008 11009 PFOS Concentration (ppb) 19.4 18.9 44.6 61.6 39.2 25.6 70.6 101 42.3 16.3 127 65.2 40.1 25.8 39.1 36.8 26.2 19.5 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) <LLOQ(2.09) <LLOQ(2.09) 2.18 2.26 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 8.84 <LLOQ(2.09) <LLOQ(2.09) 3.45 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.17 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (ppb) <LLOQ(2.11) 2.29 2.51 4.38 3.69 <LLOQ(2.11) 6.92 8.54 <LLOQ(2.11) <LLOQ(2.1 I) 9.90 2.84 3.43 <LLOQ(2.11) <LLOQ(2.11) 9.12 4.76 <LLOQ(2.11) PFOSAA* Concentration (ppb) <LLOQ(2.80) 3.62 <LLOQ(2.80) 4.11 5.76 <LLOQ(2.80) 5.16 4.69 <LLOQ(2.80) <LLOQ(2.80) 6.22 3.69 3.63 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.01 PFOSA* Concentration (ppb) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(|.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.401 <LLOQ(1.40) Study No. NWB S00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ{3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(1.80) 5.11 <LLOQ(1.80) 2.99 16.4 <LLOQ(1.80) <LLOQ(1.80) 3.99 <LLOQ(1.80) <LLOQ(1.80) 2.17 2.58 <LLOQ(1.80) <LLOQ(I.80) <LLOQ(1.80) The method acceptance criteria states that the measured concentration for each QC must be within :t:20% (+95% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 67 Northwest Bioanalytical ........... Sample ID 11010 11011 11012 11013 11014 11015 11016 11017 11018 "'i10'19 11020 11021 11022 11023 I 1024 11025 11026 | 1027 PFOS Concentration (ppb) 40.9 33.6 23.0 47.8 38.7 105 42.2 27.7 19.0 84.9 33.3 19.4 15.1 50.3 57.5 57.5 48.8 48.7 Study No. NWBS00-128 Report No. NWBR01-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) 2.18 <LLOQ(2.09) 2.26 7.39 <LLOQ(2.09) 2.29 8.70 <LLOQ(2.09) 2.20' 2.67 2.59 <LLOQ(2.09) 3.58 3.59 <LLOQ(2.09) <LLOQ(2.09) 2.74 5.70 PFOA* Concentration (ppb) 2.78 5.50 3.73 8.05 4.25 10.2 7.65 3.55 3.75 17.0 3.80 2.47 <LLOQ(2.11) 3.83 5.91 7.68 3.97 6.74 PFOSAA* Concentration (ppb) 3.95 6.00 <LLOQ(2.80) 4.93 6.10 6.49 4.12 3.34 <LLOQ(2.80) 3.96 4.63 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 7.77 7.48 3.49 4.95 PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ( 1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) M556" Concentration (ppb) <LLOQ(3.20) 12.7 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) .<LLOQ(3.20) j M570" Concentration (ppb) <LLOQ(I.80) 5.18 5.33 1.88 <LLOQ(1.80) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(I.80) 2.00 <LLOQ(I.80) <LLOQ(1.80) <LLOQ(1.80) 2.53 2.45 <LLOQ(1.80) 2.20 2.26 The method acceptance criteria states that the measured concentration for each QC must be within +20% (::E25%for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 68 Northwest Bioanalytical Sample ID 11028 11029 11030 11031 11032 11033 11034 11035 11036 11037 11038 11039 11040 11041 11042 11043 11044 11045 PFOS Concentration (ppb) 45.2 21.9 36.7 54.5 39.8 63.2 26.4 38.6 26.4 17.3 41.1 60.7 44.7 42.8 55.7 27.1 34.2 49.0 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) 2.13 <LLOQ(2.09) <LLOQ(2.09) 8.04 <LLOQ(2.09) 4.36 9.84 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.23 2.85 <LLOQ(2.09) 3.07 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.16 PFOA* Concentration (ppb) ' 6.43 3.61 6.17 4.69 3.95 6.34 4.68 9.98 2.95 <LLOQ(2.11) 3.17 7.45 4.35 10.1 3.84 2.39 5.38 6.15 PFOSA.A* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) 3.00 <LLOQ(2.80) 3.25 3.25 4.83 <LLOQ(2.80) <LLOQ(2.80) 4.44 7.37 <LLOQ(2.80) <LLOQ(2.80) 3.19 3.85 <LLOQ(2.80) 2.84 <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) Study No. NWBS00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) ' <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ(1.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(I:80) 5.51 <LLOQ(I.80) <LLOQ(1.80) 1.84 2.57 <LLOQ(I.80) 5.93 <LLOQ(I.80) <LLOQ(I.80) 2.04 <LLOQ(I.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(I.80) The method acceptance criteria states that the measured concentration for each QC must be within +90% (:25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using calibration curves (see Results and Discussion section). Page 69 Northwest Bioanalytical _Sample ID 11046 11047 11048 11049 11050 11051 11052 11053 11054 11055 11056 11057 11058 11059 11060 11061 11062 11063 PFOS Concentration (ppb) 56.9 73.8 70.8 33.5 40.4 26.7 44.3 44.8 49.6 27.5 27.0 51.9 53.2 48.7 36.4 18.3 58.1 25.8 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb, PFHS* Concentration (ppb) 2.11 3.75 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 3.03 2.39 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2".09) <LLOQ(2.09) PFOA* Concentration (ppb) 5.98 7.45 8.77 4.71 4.11 <LLOQ(2.11) 3.41 8.70 5.27 3.32 6.01 7.40 5.78 6.82 4.67 2.34 20.2 5.08 PFOSA.A* Concentration (ppb) 4.34 3.84 27.6 <LLOQ(2.80) 6.39 3.11 8.78 <LLOQ(2.80) 2.99 3.13 <LLOQ(2.80) <LLOQ(2.80) 6.47 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.401 <LLOQ(1.40) <LLOQ(I.40) Safdy No. NWBS00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) 5.88 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ(1.80) <LLOQ(I.80) 7.82 <LLOQ(I.80) <LLOQ(I.80) 2.51 <LLOQ(I.80) 2.96 2.02 <LLOQ(I.80) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(I.80) 5.38 4.14 <LLOQ(1.80) 1.93 <LLOQ(1.80) The method acceptance criteria states that the measured concentration for each QC must be within +90% (+95% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using calibration curves (see Results and Discussion section). Page 70 Northwest B ioanalytical Sample I ID ,.. 11064 PFOS Concentration (ppb) 56.0 11065 56.5 11066 30.1 11067 31.5 11068 6.63 11069 27.6 11070 205 11071 ............ 11072 27.6 49.4 11073 47.6 11074 29.7 11075 69.7 11076 27.4 11077 42.6 11078 46.9 11079 32.3 11080 43.4 10556 14.1 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) 2.96 2.91 2.27 8.26 <LLOQ(2.09) <LLOQ(2.09) 2.63 2.73 3.74 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.42 <LLOQ(2.09) 5.27 <LLOQ(2.09) 3.88 PFOA* Concentration (ppb) 9.41 3.86 3.69 8.37 <LLOQ(2.11) 5.53 34.1 4.60 14.1 4.78 3.59 6.18 ..... 4.63 6.26 6.02 5.79 8.73 4.18 PFOSA.A* Concentration (ppb) ,,,, <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2,80) <LLOQ(2.80) 3.23 <LLOQ(2.80) 5.28 <LLOQ(2.80) <LLOQ(2.80) 3.35 3.67 5.54 <LLOQ(2.80) 4.38 3.88 3.44 <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (pph) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) I' <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) Study No. NWB S00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3_20_ <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) [ 5.29 <LLOQ(1.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(1.80) 1.89 <LLOQ(1.80) 2.13 3.35 _LLOQ(1.80) <LLOQ(I.80) <LLOQ( 1.80) <LLOQ(I.80) <LLOQ(1.80) 1.89 <LLOQ(1.80) 3.46 2.01 Tile method acceptance criteria states that the measured concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error assoeiated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 71 Northwest Bioanalytical Sample ID 10557 10558 10559 10560 10561 10562 10563 10564 10565 10566 10567 10568 10569 10570 10571 10572 10573 10574 PFOS Concentration (pph) 22.5 33.1 35.4 16.9 40.0 25.3 56.0 18.1 47.2 29.5 23.3 13.6 18.5 19.9 20.7 26.0 30.6 21.1 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) 2.42 10.4 12.6 <LLOQ(2.09) 2.38 2.09 3.49 <LLOQ(2.09) 6.23 3.55 2.37 <LLOQ(2.09) 2.41 <LLOQ(2.09) 2.81 5.16 2.10 <LLOQ(2.09) PFOA* Concentration (pph) 5.84 8.55 3.55 3.37 10.5 4.54 : 7.83 5.37 8.44 10.0 6.88 2.21 3.43 3.53 3.77 4.30 6.29 3.19 PFOSAA* Concentration (pph) 2.81 3.51 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.48 <LLOQ(2.80) <LLOQ(2.80) <LLOQ{2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2._0) 4.07 <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.401 <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) Study No. NWBS00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ(I.80) 4.26 <LLOQ(I.80) 2.47 2.40 2.60 <LLOQ(I.80) <LLOQ(I.80) 2.57 2.64 5.8R <LLOQ(I.80) <LLOQ(1.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(I.80) 2.31 <LLOQ(I. 80) The method acceptance criteria states that the measured concentration for each QC must be within +90% (+95% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. sample results for PFOA, PFHS,PFOSA.A, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using calibration curves (see Results and Discussion section). Page 72 Northwest Bioanalytical Sample ID 10575 PFOS Concentration (ppb) <LLOQ(4.27) 10576 20.3 10577 23.6 10578 63.7 10579 37.4 10580 44.1 10581 9.83 10582 25.7 10583 39.2 10584 13.5 10585 37.6 10586 32.1 10587 11.0 10588 18.1 10589 37.2 10590 52.6 10591 38.2 10592 51.7 Table 22. Study Sample Coneentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) <LLOQ(2.09) 3.13 2.54 5.97 2.28 <LLOQ(2.09) <LLOQ(2.09) 2.10 2.56 <LLOQ(2.09) 3.67 2.71 8.05 <LLOQ(2.09) 4.96 8.80 4.18 11.2 PFOA* Concentration (ppb) <LLOQ(2.11) 4.17 4.60 9.31 7.36 6.25 5.84 4.11 9.18 " 4.81 7.23 3.87 3.50 6.97 6.73 .] 1.8 6.75 13.6 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) 2.92 5.14 <LLOQ(2.80) 3.24 2.92 <LLOQ(2.80) 3.26 <LLOQ(2.80) 4.84 <LLOQ(2.80) <LLOQ(2.80) 3.10 4.40 <LLOQ(2.80) 3.29 2.98 PFOSA* Concentration (ppb) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) Study No. NWBS00-128 Report No. NW'BR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.201 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ(1.80) <LLOQ(I.80) <LLOQ(1.80) 2.37 3.16 <LLOQ(1.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(I.80) 3.19 <LLOQ(1.80) 1.89 <LLOQ(I.80) 3.41 <LLOQ(1.80) 5.84 4.29 19.0 The method acceptance criteria states that the measured concentration for each QC must be within :f_20%(:V_25%for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary fi'om results obtained using serum calibration curves (see Results and Discussion section). Page 73 Northwest Bioanalytical Sample I PFOS ID Concentration (ppb) 10593 30.9 10594 74.2 10595 37.1 10596 21.8 10597 14.3 10598 29.9 10599 18.0 10600 47.7 10601 43.5 10602 20.8 10603 23.5 10604 10.2 10605 25.2 10606 27.6 10607 36.7 10608 30.8 10609 29.7 10610 65.8 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) 6.75 10.2 2.56 2.39 <LLOQ(2.09) 2.89 2.51 3.16 <LLOQ(2.09) 3.20 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(1.36) 3.62 1.72 2.76 1.87 PFOA* Concentration (ppb) 6.20 13.9 4.59 3.91 3.36 9.69 4.10 7.19 3.04 5.09 5.23 2.67 3.49 7.16 7_89 8.13 6.53 13.7 PFOSAA* Concentration (ppb) <LLOQ(2.80) 6.71 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.58 3.13 <LLOQ(2.80) 3.35 3.24 3.01 <LLOQ(1.60) <LLOQ(I.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(I.60) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.00) <LLOQ(I.O0) <LLOQ(I.O0) <LLOQ(1.00) <LLOQ(I.00) Study No. NWBS00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ(1.80) 2.11 <LLOQ(1.80) 2.40 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 3.78 2.05 1.93 <LLOQ(1.80) <LLOQ(1.80) The method acceptance criteria states that the measured concentration for each QC must be within +70% (+95% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 74 Northwest Bioanalytieal Sample! ID 10611 10612 10613 10614 10615 10616 10617 10619 10620 10621 10622 10623 10624 10625 10626 10627 10628 PFOS Concentration (ppb) 22.2 32.0 67.6 57.6 36.0 27.7 25.g 22.7 54.3 14.0 35.5 11.7 25.3 35.2 41.7 31.8 25.4 10629 1.... 36.3 Table 22. Study Sample Coneentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) <LLOQ(I.36) 11.4 1.49 5.36 <LLOQ(I.36) J-, <LLOQ(I.36) 3.31 2.16 6.80 <LLOQ(I.36) <LLOQ(I.36) <LLOQ(I.36) 3.70 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(I.36) 2.84 PFOA* Concentration (ppb) 5.82 7.23 10.7 10.1 4.01 5.76 5.24 4.40 9.52 2.47 6.63 4.1.3 5.89 4.17 7.28 6.28 6.87 <LLOQ(I.36) 4.55 PFOSAA* Concentration (ppb) <LLOQ(I.60) <LLOQ(I.60) <LLOQ(I.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(I.60) <LLOQ(I.60) <LLOQ(I.60) 2.42 <LLOQ(1.60) 2.59 <LLOQ(I.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(I.60) <LLOQ(I.60) <LLOQ(1.60) <LLOQ(I.60) PFOSA* Concentration (ppb) <LLOQ(I.O0) <LLOQ(I.O0) <LLOQ(I.O0) <LLOQ(1.O0) <LLOQ(I.O0) <LLOQ(I.O0) <LLOQ(1.O0) <LLOQ(I.O0) <LLOQ(I.O0) <LLOQ(I.O0) <LLOQ(1.O0) <LLOQ(I.O0) <LLOQ(1.00) <LLOQ(1.007 <LLOQ(I.O0) <LLOQ(I.O0) <LLOQ(I.O0) <LLOQ(I.O0) Study No. NWBS00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (pph) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(1.80) 3.92 <LLOQ(I.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(I.80) 13.0 <LLOQ(I.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.39 3.36 1.88 4.42 <LLOQ(I.80) Tile method acceptance criteria states that the measured concentration for each QC must be within :t.20% (+9_5%for PFOSA and PFOSA.A) of the target concentration, Tile statistical error associated with any individual result may exceed the QC acceptance criteria, Serum sample results for PFOA, PFHS, PFOSA.A, PFOSA, M556 and M570 obtained using plasma calibration curves may vary fi'om results obtained using serum calibration curves (see Results and Discussion section). Page 75 Northwest Bioanalytical Sample ID 10630 10631 10632 10633 10634 10635 10636 10637 10638 10639 10640 10641 10642 10643 10644 10645 10646 10647 PFOS Concentration (ppb) 30.3 54.1 41.4 87.2 30.6 36.8 26.3 12.7 45.2 44.7 19.3 19.8 80.9 40.5 23.9 26.5 .... 48.7 26.7 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) 1.99 1.51 1.47 <LLOQ(1.36) <LLOQ(I.36) 1.79 1.84 <LLOQ(I.36) 2.80 <LLOQ(l.36) 2.36 <LLOQ(I.36) 2.08 2.29 3.45 <LLOQ(1.36) 1.60 1.40 PFOA '_ Concentration (ppb) 4.65 8.91 5.23 5.78 7.36 5.27 3.48 3.52 8.02 9.13 4.73 3.07 5.93 7.21 7.29 5.04 ,, 10.5 7.51 PFOSAA*, Concentration (ppb) <LLOQ(1.60) 2.28 <LLOQ(1.60) 2.35 <LLOQ(1.60) <LLOQ(I.60) 3.32 1.61 1.62 4.68 <LLOQ(2.80) 1.78 2.99 2.45 <LLOQ(I.60) <LLOQ(1.60) 3.00 3.34 PFOSA* Concentration (ppb) <LLOQ(1.00) <LLOQ(I.O0) <LLOQ(1.O0) <LLOQ(1.O0) <LLOQ(I.O0) <LLOQ(I.O0) <LLOQ(I.O0) <LLOQ(I.O0) <LLOQ(1.O0) <LLOQ(I.00) <LLOQ(I.40) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) Study No. NWB S00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ(1.80) <LLOQ(I.80) 3.03 2.65 <LLOQ(1.80) <LLOQ(1.80) 2.67 <LLOQ(1.80) <LLOQ(1.80) 2.12 <LLOQ(1.80) 1.83 3.65 <LLOQ(1.80) 2.41 <LLOQ(1.80) 3.48 6.35 The method acceptance criteria states that the measured concentration for each QC must be within +90% (:t25% for PFOSAand PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 76 Northwest Bioanalytical Sample ID 10648 10649 10650 10651 10652 10653 10654 10655 10656 10657 10658 10659 10660 10661 10662 10663 10664 10665 PFOS Concentration (pph) 16.7 39.0 14.3 28.6 32.7 11.7 28.5 15.9 33.9 48.1 45.7 18.7 26.1 28.6 44.5 26.9 31.4 44.9 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) <LLOQ(I.36) 1.58 <LLOQ(I.36) 1.36 2.12 <LLOQ(I.36) 2.19 2.64 2.23 3.02 3.79 2.94 6.70 2.68 <LLOQ(2.09) 2.85 <LLOQ(2.09) 2.57 PFOA* ' Concentration (ppb) 3.49 10.I 2.86 5.69 11.4 2.13 11.4 4.26 2.14 3.46 5.80 4.57 4.58 5.56 6.28 2.80 3.28 5.48 PFOSAA* Concentration (ppb) 4.28 4.64 <LLOQ(1.60) <LLOQ(1.60) 2.81 <LLOQ(1.60) 2.43 <LLOQ(I.60) <LLOQ(I.60) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 5.09 <LLOQ(2.80) 4.40 PFOSA* Concentration (pph) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.401 <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.401 <LLOQ(I.40) Study No. NWBS00-12R Report No. NWBR01-066 M556" Concentration (pph) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) .= <LLOQ(I.80) 2.95 <LLOQ(I.80) 1.84 m <LLOQ(I.80) 2.51 9.66 2.83 <LLOQ(I.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(I.80) 4.30 <LLOQ(1.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(1.80) The method acceptance criteria states that the measured concentration for each QC must be within _'1:20%(_'t:25%for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 77 Northwest Bioanalytieai Sample ID 10666 10667 10668 10328 10329 10330 10331 PFOS Concentration (ppb) 29.9 40.8 19.8 24.3 50.6 47.7 31.7 10332 10333 10334 10335 10336 10337 10338 10339 10340 10341 10342 30.8 31.9 24.6 19.3 42.5 32.1 19.3 28.4 39.2 14.8 23.1 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(I.36) 3.86 3.50 8.44 PFOA* Concentration (ppb) 4.65 4.41 4.30 4.90 7.92 18.7 5.39 PFOSAA* Concentration (ppb) 4.52 <LLOQ(2.80) <LLOQ(2.80) 2.59 4.83 5.56 <LLOQ(I.60) PFOSA* Concentration (ppb) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) 5.15 1.65 <LLOQ(I.36) <LLOQ(I.36) <LLOQ(I.36) 1.52 <LLOQ(I,36) <LLOQ(l.36) <LLOQ(I.36) <LLOQ(I.36) 4.89 4.08 1.87 <LLOQ(I.00) 4.05 <LLOQ(1.60) <LLOQ(1.00) 3.23 <LLOQ(I.60) <LLOQ(1.00) 3.20 <LLOQ(1.60) <LLOQ(1.00) 3.62 2.22 <LLOQ(1.00) 5.76 <LLOQ(I.60) <LLOQ(I.00) 2.46 <LLOQ(1.60) <LLOQ(1.00) 4.59 <LLOQ(I.60) <LLOQ(I.00) 5.02 4.66 <LLOQ(1.00) 3.84 <LLOQ{ 1.60) <LLOQ(I.00) 8.59 2.17 <LLOQ(I.00) Study No. NWBS00-128 Report No. NWBR0 i-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570" Concentration (ppb) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(I.00) 1.95 <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) .. 1.76 <LLOQ(I.00) <LLOQ(I.00) 1.21 6.28 3.92 <LLOQ(I.00) 1.35 <LLOQ(1.00) <LLOQ(I.00) The method acceptance criteria states that the measured concentratian for each QC must be within +90% (+_25%for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS0 PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using calibration curves (see Results and Discussion section). Page 78 Northwest Bioanalytical Sample 1D 10343 10344 10345 10346 1034"/ 10348 10349 10350 10351 10352 10353 10354 10355 10356 10357 10358 10359 10360 PFOS Concentration (ppb) 29.6 44.9 45.6 39.8 14.7 17.7 33.0 30.5 34.8 18.0 23.8 31.6 95.7 26.5 22.0 43.5 71.0 17.0 Table 22. Study Sample Concentrations All concentrations are expressedas (Continued) ppb. PFHS* Concentration (pph) <LLOQ(1.36) <LLOQ(1.36) 2.07 2.44 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) 2.58 6.40 <LLOQ(2.09) 2.02 3.17 1.43 <LLOQ(I,36) <LLOQ(1.36) 4.08 1.37 <LLOQ(I.36) PFOA* Concentration (pph) 6.45 3.03 5.74 4.38 2.28 3.58 4.94 2,35 3.95 <LLOQ(2.11) 6.55 4,74 10.7 3.80 4.05 4.92 5,30 4.90 PFOSAA* Concentration (pph) 3.42 4.92 <LLOQ(I.60) 1.83 <LLOQ(I.60) <LLOQ(I.60) 2.05 4.32 <LLOQ(I.60) <LLOQ(2.80) <LLOQ(I.60) <LLOQ(1.60) 2.38 <LLOQ(I.60) 1.84 3.40 1.96 1.79 PFOSA* Concentration (ppb) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.40) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.O0) <LLOQ(I.O0) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) Study No. NWBS00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(3.20) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570" Concentration (pph) 1.50 2.51 <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) 2.83 1.39 5.37 3.17 <LLOQ(1.80) <LLOQ(1.00) <LLOQ(I.O0) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) 1.51 1.03 1.28 The method acceptance criteria states that the measured concentration for each QC must be within +_20%(+25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSA.A, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 79 Northwest B ioanalytical Sample ID 10361 10362 10363 10364 10365 10366 10367 PFOS Concentration (ppb) 7.70 41.7 34.7 22.8 22.6 21.9 '- 17.7 10368 10369 10370 10371 10372 10373 10374 10375 10376 10377 10378 74.3 ill 24.7 71.8 59.5 52.8 29.7 49.2 21.1 88.4 100 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) <LLOQ(1.36) 3.02 1.41 <LLOQ(I.36) <LLOQ(l.36) <LLOQ(I.36) <LLOQ(2.09) <LLOQ(l.36) <LLOQ(I.36) <LLOQ(1.36) 7.12 12.0 3.87 <LLOQ(1.36) 10.8 <LLOQ(1.36) 6.67 1.37 PFOA* Concentration (ppb) 2.53 5.90 4.93 3.92 3.07 4.96 <LLOQ(2.11) I. 9.98 3.53 3.98 7.18 5.03 20.0 4.85 4.40 3.54 15.8 5.57 PFOSAA* Concentration (ppb) <LLOQ(I.60) <LLOQ(1.60) <LLOQ(1.60) 1.83 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(2.80) 10.3 <LLOQ(1.60) 2.75 5.41 <LLOQ(1.60) 1.79 1.94 <LLOQ(I.60) <LLOQ(I.60) 7.53 4.93 PFOSA* Concentration (ppb) <LLOQ(I.O0) <LLOQ(1.O0) <LLOQ(1.O0) <LLOQ(I.O0) <LLOQ(1.O0) <LLOQ(1.O0) <LLOQ(I.40) <LLOQ(1.O0) <LLOQ(I.O0) <LLOQ(1.001 <LLOQ(I.O0) <LLOQ(I.O0) <LLOQ(1:00) <LLOQ(I.O0) <LLOQ(I.O0) <LLOQ(I.O0) <LLOQ(I.O0) <LLOQ(1.00) Study No. NV/B S00-12 g Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(3.20) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50/ <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.501 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570" Concentration (ppb) <LLOQ(I.O0) 3.01 1.59 <LLOQ(] .00) 1.85 <LLOQ(1.00) <LLOQ(1.80) <LLOQ(I.O0) 3.02 <LLOQ(1.00) 3.89 2.62 10.6 <LLOQ(1.001 2.20 1.62 2.31 1.52 The method acceptance criteria states that the measured concentration for each QC must be within _+_20%(:t25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 80 Northwest Bioanalytical Sample i PFOS ID i Concentration (ppb) 10379 54.6 10380 31.3 10381 34.8 10382 35.8 10383 15.6 10384 24.7 10385 28.3 10386 41.4 10387 11.7 10388 79.1 10389 28.4 10390 15.8 10391 48.4 10392 55.5 10393 20.9 10394 21.7 10395 40.0 10396 36.3 Table 22, Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) <LLOQ{I.36) 1.49 <LLOQ(1.36) 1.72 <LLOQ(I.36) <LLOQ(1.36) 2.03 5.75 <LLOQ(I.36) <LLOQ(2.09) 1.60 <LLOQ(1.36) 2.45 1.61 1.41 1.65 4.73 1.81 PFOA* Concentration (ppb) 3.88 4.22 3.92 2.81 2.80 2.56 4.89 3.30 2.43 5.93 4.29 3.09 7.41 5.34 2.91 2.18 4.92 5.66 PFOSAA* Concentration (ppb) 3.27 <LLOQ(I.60) 2,56 <LLOQ(I.60) <LLOQ(I.60) 2.34 <LLOQ(1.60) 8.31 <LLOQ(1.60) 4.38 <LLOQ(I.60) <LLOQ(I.60) 3.27 2.54 1.98 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) PFOSA* Concentration (ppb) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.40) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I,00) <LLOQ(I.00) Study No. Na,VBS00 - 128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(3.20) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570" Concentration (ppb) <LLOQ(1.00) 1,72 1.69 1.70 2.84 <LLOQ(I.00) 1.40 1.33 <LLOQ(I.00) <LLOQ(I.80) 1.29 2.42 3.07 4.03 3.12 <LLOQ(1.00) 1.41 2.32 The method acceptance criteria states that the measured concentration for each QC must be within +90% (+95% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHSI PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using calibration curves (see Results and Discussion section). Page 81 Northwest Bioanal3aieal Sample 1D 10397 10398 10399 10400 10401 10402 10403 10404 -- 10405 10406 10407 10408 10409 10410 10411 10412 10413 PFOS Concentration (ppb) 28.2 ...... 36.9 38.9 27.5 32.0 25.234.3 30.6 36.5 24.1 27.0 80.4 28.8 88.8 32.3 53.5 16.8 10414 27.0 Study No. NWBS00-128 Report No. NWBR01-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) 6.51 5.10 5.63 <LLOQ(I.36) 2.79 <LLOQ(I.36) 3.92 3.56 r .... 1.69 6.87 <LLOQ(1.36) 1.90 1.61 15.2 <LLOQ(I.36) 1.87 <LLOQ(I.36) l <LLOQ(I.36) PFOA* Concentration (ppb) 4.57 5.59 3.38 4.57 5.63 <LLOQ(I.92) 2.97 2.78 7.05 6.27 4.62 10.6 3.49 . 13.8 3.26 8.98 2.53 3.17 PFOSAA* Concentration (ppb) <LLOQ(I.60) <LLOQ(I.60) 2.00 1.72 <LLOQ(2.80) 2.12 <LLOQ(1.60) 4.71 <LLOQ(I.60) 1.78 2.44 2.83 1.75 3.43 1.68 7.34 <LLOQ(I.60) 2.57 PFOSA* Concentration (ppb) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.40) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) M556" Concentration (pph) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(3.20) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) n <LLOQ(2150) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570" Concentration (ppb) 1.62 4.39 <LLOQ(I.00) 1.34 <LLOQ(! .80) 4.05 <LLOQ(I.00) 1.34 <LLOQ(I.00) 2.03 6.76 1.81 <LLOQ(I.00) 4.60 <LLOQ(1.00) 3.45 <LLOQ(I.00) 1.42 The method acceptance criteria states that the measured concentration for each QC must be witlfin :_:20% (+95,/ofor PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 82 Northwest Bioanalytical Sample ID 10415 10416 10417 10418 10419 10420 10421 10422 10423 10424 10425 10426 10427 11883 11884 11885 I 1886 11887 PFOS Concentration (ppb) 207 17.2 37.7 29.1 30.6 56,6 33,6 14.4 36.7 38.8 30.8 115 57.7 17.8 26.1 26.5 26.6 60.1 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) 2.09 <LLOQ(I.36) 4.54 <LLOQ(1.36) <LLOQ(I.36) 2.70 1.83 <LLOQ(1.36) <LLOQ(1.36) 1.39 <LLOQ(I.36) <LLOQ(1.36) <LLOQ(1.36) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (ppb) 14.9 <LLOQ(1.92) 4.28 4.43 2.82 11.5 4.61 2.40 5.76 3.38 3.59 10.3 5,95 2.40 <LLOQ(2.11) 6.13 4.07 26.7 PFOSAA* Concentration (ppb) 7.76 <LLOQ(l.60) <LLOQ(I.60) <LLOQ(I.60) <LLOQ(I.60) 2.58 <LLOQ(I.60) <LLOQ(I.60) <LLOQ(1.60) <LLOQ(I.60) <LLOQ(I.60) 12.9 1.91 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2,80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.O0) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) Study No. NWBS00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) 5.07 1.63 1.78 <LLOQ(1.00) 3.20 7.63 <LLOQ(1.00) 2.21 <LLOQ(1.80) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(1.80) 1.93 The method acceptance criteria states that tile measured concentration for each QC must be within +20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 83 Northwest Bioanalytical Sample ID 11888 11889 11890 11891 11892 11893 11894 11895 11896 10756 10757 10758 10759 10760 10761 10762 10763 10764 PFOS Concentration (ppb) 91.8 33.8 23.2 71.3 30.2 35.0 22.0 12.5 34.2 166 77.9 133 160 38.1 90.5 41.7 36.4 30.3 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) 7.34 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 3.60 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 4.51 4.27 11.6 2.78 1.71 1.50 <LLOQ(1.36) <LLOQ(I.36) <LLOQ(1.36) PFOA* Concentration (ppb) 10.1 5.85 3.64 6.40 7.40 4.90 4.55 4.48 4.71 29.0 11.7 6.25 15.3 5.39 8.54 6.09 6.25 3.29 PFOSAA* Concentration (ppb) 3.64 3.43 <LLOQ(2.80) 4.04 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 60.1 52.9 7. l 8 8.11 <LLOQ(I.60) 12.2 1.80 <LLOQ(I.60) <LLOQ(1.60) PFOSA* Concentration (ppb) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ( 1.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) Study No. NW/3 S00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) 12.9 9.21 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570" Concentration (ppb) 13.3 <LLOQ( 1.80) <LLOQ(I.80) <LLOQ( 1.80) <LLOQ(1.80) 2.90 <LLOQ(I.80) <LLOQ(1.80) <LLOQ(I.80) 3.75 <LLOQ( 1.00) 5.21 1.28 1.55 <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) Tile method acceptance criteria states that the measured concentration for each QC must be within :t:20% (_+_25%for PFOSA and PFOSA.A) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using calibration curves (see Results and Discussion section). Page 84 Northwest Bioanalytical Sample l PFOS ID Concentration (ppb) 10765 96.1 10766 40.7 10767 34.1 10768 28.1 10769 54.7 10770 42.7 10771 26.8 10772 36.1 10773 66.6 10774 77.2 10775 46.8 10776 159 10777 49.1 10778 31.0 10779 22.7 10780 57.3 t_ 10781 10782 43.9 . .... 79.0 .. Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) 3.73 7.70 <LLOQ(I.36) 4.56 4.64 <LLOQ(I.36) 1.57 2.00 15.6 2.25 <LLOQ(1.36) 4.24 2.76 <LLOQ(I.36) <LLOQ(I.36) 3.76 2.78 4.71 PFOA* Concentration (ppb) 11.7 6.54 6.81 5.96 6.69 4.14 4.70 4.34 5.78 8.75 9.30 29.8 6.08 2.21 5.12 7.72 6.04 9.85 PFOSAA* Concentration (ppb) 1.75 <LLOQ(I.60) <LLOQ(I.60) <LLOQ(I,60) 2.19 <LLOQ(1.60) <LLOQ(1.60) 3.44 2.89 8.08 8.98 56.6 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 3.56 1.68 3.38 PFOSA* Concentration (ppb) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) Study No. NWBS00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 12.2 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570" Concentration (ppb) 2.82 <LLOQ(1.00) 1.65 <LLOQ(I.00) 1.18 1.59 4.22 <LLOQ(I.00) 2.77 1.86 <LLOQ(1.00) 2.45 <LLOQ(1.00) 2.07 <LLOQ(I.00) 1.73 <LLOQ(1.00) <LLOQ(1.00) The method acceptance criteria states that the measured concentration for each QC must be within +90% (+95% for PFOSA and PFOSA.A) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSA.A, PFOSA, M556 and M570 obtained using plasma serum calibration curves (see Results and Discussion section). Page 85 calibration curves may vary fi'om results obtained using Northwest Bioanalytical Sample ID 10783 10784 10785 10786 10787 10788 10789 10790 10791 10792 10793 10794 10795 10796 10797 10798 10799 10800 PFOS Concentration (ppb) 54.2 37.3 31.6 38.9 73.0 33.8 49.3 55.2 69.8 22.0 31.1 74,2 105 40.2 52.5 58.2 117 75.1 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) 1.78 2.12 1.91 5.22 6.27 2.19 2.00 <LLOQ(1.36) 2.67 1.38 1.64 3.86 2.09 19.8 4.12 4.96 1.70 3.15 PFOA* Concentration (ppb) 7.46 5.89 4.88 4.79 1812 5.34 7.30 6.45 7.16 4.02 5.08 10.6 5.51 8.76 4.32 7.87 13.1 8.95 PFOSAA* Concentration (ppb) 4.60 <LLOQ(1.60) <LLOQ(I.60) <LLOQ(1.60) 2.28 <LLOQ(I.60) 1.95 4.51 2.36 <LLOQ(1.60) 2.31 13.7 1.96 2.09 1.76 1.81 5.44 8.62 PFOSA* Concentration (ppb) <LLOQ(I.O0) <LLOQ(I.O0) <LLOQ(I.O0) <LLOQ(1.O0) <LLOQ( 1.00) <LLOQ(1.O0) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1,00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(1.00) Study No. NWBS00-128 Report No. NWBR01-066 M556 _ Concentration (ppb) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50} <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570" Concentration (ppb) 2.05 <LLOQ(I.O0) <LLOQ(I.O0) 1.98 2.16 <LLOQ(1.00) 1.61 <LLOQ(I.00) 1.57 1.21 <LLOQ(I.00) <LLOQ(1.00) 2.67 <LLOQ(1.00) 4.69 1.97 1.27 2.97 The method acceptance criteria states that the measured concentration for each QC must be within :f_.20%(+95% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained ush_g serum calibration curves (see Results and Discussion section). Page 86 Northwest Bioanalytical Sample ID PFOS Concentration (ppb) 10801 48.7 10802 33.3 10803 32.6 10804 68.5 10805 45.5 10806 110 10807 33.9 10808 40.3 10809 29.8 10810 "" 10811 42.9 7 32.6 10812 69.9 10813 27.4 10814 38.4 10815 55.1 10816 50.1 10817 106 10818 67.6 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) 2.48 <LLOQ(I.36) 8.59 <LLOQ(1.36) 4.35 11.5 3.52 1.86 1.79 <LLOQ(2.09) <LLOQ(2.09) 3.77 <LLOQ(2.09) 2.82 <LLOQ(2.09) 4.39 4.58 9.17 PFOA* Concentration (ppb) 6.21 4.47 4.31 17.8 6.93 21.8 7.08 2.70 4.72 3.54 4.45 7.50 2.85 6.57 8.35 2.60 7.17 11.4 PFOSA.A* Concentration (ppb) <LLOQ(I.60) 6.91 <LLOQ(1.60) 3.71 <LLOQ(I.60) 3.35 <LLOQ(1.60) <LLOQ(1.60) 3.58 3.58 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 6.45 4.05 3.04 3.25 <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(I.O0) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.00) <LLOQ(I.00) <LLOQ(I.00) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) Study No. NWBS00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) 1.22 2.16 <LLOQ(I.00) 3.03 <LLOQ(I.00) 5.59 1.68 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(I.80) 2.99 2.46 1.95 3.66 <LLOQ(!.80) 5.68 <LLOQ(I.80) 5.34 The method acceptance criteria states that the measured concentration for each QC must be within +90% (+95% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 87 Northwest Bioanalytical Sample I PFOS ID Concentration (pph) 10819 37.1 10820 71.0 10821 45.3 10822 54.4 10823 35.9 10824 109 10825 72.7 10826 30.6 10827 10828 10829 59.4 143 Not Received 10830 34.3 10831 75.8 10832 44.5 10833 68.9 10834 49.8 10835 71.3 10836 35.5 Study No. NWBS00-128 Report No. NWBR01-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) <LLOQ(2.09) 2.96 <LLOQ(2.09) 10.7 <LLOQ(2.09) <LLOQ(2.09) J 14.1 2.47 5.37 3.33 Not Received 4.97 9.32 4.10 3.29 5.53 4.02 3.82 PFOA* Concentration (ppb) 4.65 3.88 4.17 7.46 7.14 6.50 m 6.90 3.42 8.35 13.4 Not Received 5.75 13.5 4.87 10.7 3.62 10.7 4.66 PFOSAA.* Concentration (ppb) 3.21 4.70 <LLOQ(2.80) 15.1 <LLOQ(2.80) 9.12 <LLOQ(2.80) 3.76 6.62 8.59 Not Received <LLOQ(2.80) 4.28 <LLOQ(2.80) 3.51 5.10 <LLOQ(2.80) <LLOQ(2.80) PFOSA* Co_lcentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.401 <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) Not Received <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) 3.91 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) Not Received I ] <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ( 1.80) 2.09 <LLOQ(I.80) 4.37 5.51 4.18 <LLOQ(I.80) <LLOQ(1.80) <LLOQ(1.80} 4.03 Not Received 8.31 5.26 <LLOQ(I.80) 10.8 <LLOQ(I.80) 4.47 <LLOQ(1.80) The method acceptance criteria states that the measured concentration for each QC must be within +_.20%(+95% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 88 Northwest Bioanalytical Sample ID 10837 PFOS Concentration (ppb) Not Received 10838 10839 36.5 Not Received -i0840 10841 10842 10843 10844 10845 . 10846 10847 10848 10849 10850 10851 10852 10853 10854 34.1 68.2 154 41.8 70.7 Not Received 65.8 92.4 44.2 51.5 40.7 70.5 19.3 31.7 50.5 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) Not Received 7.12 Not Received 2.50 22.4 12.1 2.34 9.59 Not Received 18.7 12.9 <LLOQ(2.09) 2.98 <LLOQ(2.09) 4.00 <LLOQ(2.09) <LLOQ(2.09) 2.46 PFOA* Concentration (ppb) Not Received 8.60 Not Received 6.97 5.68 18.2 4.37 14.9 ,Not Received 13.3 9.46 3.27 7.02 <LLOQ(2.11) 6.49 2.95 4.70 3.97 PFOSAA* Concentration (ppb) Not Received <LLOQ(2.80) Not Received <LLOQ(2.80) 4.33 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) Not Received 2.85 4.10 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.65 PFOSA* Concentration (ppb) Not Received <LLOQ(1.40) Not Received <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) Not Received <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) Study No. NWBS00-128 Report No. NWBR01-066 M556" Concentration (ppb) Not Received <LLOQ(3.20) Not Received <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) Not Received <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) Not Received 5.75 Not Received 2.83 <LLOQ(1.80) <LLOQ(I.80) 8.20 6.61 Not Received 2.83 3.57 <LLOQ(I.80) 1.99 <LLOQ(I.80) 2.11 <LLOQ(1.80) 3.44 <LLOQ(1.80) The method acceptance criteria states that the measured concentration for each QC must be within +90% (_+.25%for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 89 Northwest Bioanalytical Sample 1D 10855 10856 10857 10858 10859 10860 10861 10862 10863 10864 10865 10866 10867 10868 11649 11650 11651 11652 PFOS Concentration (ppb) 18.5 36.3 81.9 54.7 19.5 Not Received 39.9 37.8 70.6 58.3 56.8 24.0 57.4 22.9 17.6 28.3 48.8 23.5 Study No. NW'BS00-128 Report No. NWBR01-066 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) <LLOQ(2.09) 7.00 2.48 <LLOQ(2.09) <LLOQ(2.09) Not Received 2.57 4.03 <LLOQ(2.09) 2.34 6.25 <LLOQ(2.09) 2.28 4.80 <LLOQ('2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (ppb) 2.16 4.66 12.0 4.82 <LLOQ(2.11) Not Received 3.35 4.23 4.20 3.80 3.85 3.03 5.32 3.46 3.96 3.49 4.07 2.71 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) Not Received 5.15 <LLOQ(2.80) 3.11 <LLOQ(2.80) 24.7 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.20 3.24 25.1 <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) Not Received <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) Not Received <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) 3.88 <LLOQ(3.20) 5.12 <LLOQ(3.20) M570" Concentration (ppb) 2.53 <LLOQ(1.80) <LLOQ(1.80} <LLOQ(1.80) <LLOQ(I.80) Not Received 3.21 2.23 3.10 <LLOQ(I.80) <LLOQ(I.80) 2.35 3.95 2.79 <LLOQ(1.80) 2.06 <LLOQ(I.80) <LLOQ(I.80) The method acceptance criteria states that the measured concentration for each QC must be within +90% (+95% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary fi'om results obtained using calibration curves (see Results and Discussion section). Page 90 Northwest Bioanalytical Sample ID 11653 11654 ., 11655 11656 11657 11658 11659 11660 11661 11662 11663 11664 11665 11666 11667 11668 11669 11670 PFOS Concentration (ppb) 25.2 329 31.2 31.5 70.3 27.4 43.9 17.7 46.4 44.6 14.0 64.1 45.0 37.7 9.45 29.9 31.9 28.3 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) <LLOQ(2.09) 6.91 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.54 11.8 <LLOQ(2.09) <LLOQ(2.09) 10.9 <LLOQ(2.09) 2.48 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (ppb) 4.76 16.7 3.77 3.13 6.63 2.94 3.61 3.13 3.91 4.92 3.77 6.96 4.49 5.07 <LLOQ(2.11) 3.81 6.28 4.08 PFOSAA* Concentration (ppb) 3.89 36.9 <LLOQ(2.80) <LLOQ(2.80) 13.3 <LLOQ(2.80) <LLOQ(2.80) 3.42 4.90 2.82 4.98 9.91 5.04 2.83 <LLOQ(2.80) 5.86 3.77 2.92 PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1A0) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) Study No. NWBS00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) 12.2 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) 4.21 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(I.80) 1.96 <LLOQ(1.80) <LLOQ(1.80) 2.43 <LLOQ(1.80) 2.63 2.06 <LLOQ(I.80) 2.03 <LLOQ(I.80) 2.86 <LLOQ(I.80) 1.82 <LLOQ(1.80) 3.64 The method acceptance criteria states that the measured concentration for each QC must be within +90% (:t:25% for PFOSA and PFOSA.A) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSA.A, PFOSA, M556 and M570 obtained using plasma calibration curves'may serum calibration curves (see Results and Discussion section). Page 91 vary from results obtained using Northwest Bioanalytical 'Sample I PFOS ID Concentration (ppb) 11671 37.7 11672 30.7 11673 36.2 11674 37.5 11675 14.2 11676 12.0 11677 43.4 11678 32.2 11679 17.0 11680 44.5 11681 15.8 11682 9.20 11683 40.3 11684 42.3 11685 24.4 11686 14.6 11687 36.1 11688 17.2 Table 22. Study Sample ConCentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) 2.16 <LLOQ(2.09) <LLOQ(2.09) 3.91 3.99 <LLOQ(2.09) 3.22 3.83 <LLOQ(2.09) 7.24 <LLOQ(2.09) <LLOQ(2.09) 8.61 <LLOQ(2.09) <LLOQ(2.09) 4.12 2.11 <LLOQ(2.09) PFOA* Concentration (ppb) 4.44 5.43 2.68 4.44 3.22 2.33 3.60 3.57 2.56 6.79 5.41 <LLOQ(2.11) 6.21 4.48 2.34 5.38 4.10 <LLOQ(2.11) PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.39 2.96 <LLOQ(2.80) 5.66 <LLOQ(2.80) <LLOQ(2.80) 4.72 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 4.43 PFOSA* Concentration (ppb) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1 40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) Study No. NWBS00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ(I.80) <LLOQ(I.80) 2.37 <LLOQ(I.80) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(I.80) 2.65 <LLOQ(1.80) 2.62 <LLOQ(1.80) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) The method acceptance criteria states that the measured concentration for each QC must be within +90% (+95% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using calibration curves (see Results and Discussion section). Page 92 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Sample ID 11689 11690 11691 11692 11693 11694 11695 11696 11697 11698 11699 11700 11701 11702 11703 11704 11705 PFOS Concentration (ppb) 1656"* 25.6 24.4 14.2 27.1 33.4 20.8 14.5 108 124 22.9 25.5 14.1 39.0 12.0 78.7 12.0 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) 9.87 <LLOQ(2.09) 2.59 <LLOQ(2.09) 2.58 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.28 <LLOQ(2.09) <LLOQ(2.09) 3.27 <LLOQ(2.09) 6.54 <LLOQ(2.09) PFOA* Concentration (ppb) 4.32 2.92 3.13 2.71 3.91 <LLOQ(2.11) 3.04 <LLOQ(2.11) 12.2 12.0 4.24 3.48 3.11 5.61 <LLOQ(2.11) 12.9 3.09 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) 3.88 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.03 13.0 9.58 <LLOQ(2.80) 5.45 <LLOQ(2.80) 6.74 2.97 15.6 <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) 3.58 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) ** Concentration corrected for amount of persistent PFOS in dilution matrix. M570" Concentration (ppb) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.80) 2.14 <LLOQ(I.80) <LLOQ(I.80) <LLOQ(I.80) 2.07 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(1.807 <LLOQ(I.80) 3.70 <LLOQ(1.807 3.68 <LLOQ(1.80) The method acceptance criteria states that the measured concentration for each QC must be within +90% (+95% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary fi'om results obtained using serum calibration curves (see Results and Discussion section). Page 93 Northwest Bioanalylical Study No. NWBS00-128 Report No. NWBR01-066 Table 22.Study Sample Coneentrations (Continued) All concentrations are expressed as ppb. Sample ID 11706 11707 11708 11709 11710 11711 11712 11713 11714 11715 11716 11717 11718 11719 11720 11721 11722 11723 PFOS Concentration (ppb) 22,3 17,5 14.5 43.5 35.9 30.3 11.1 50.8 18,4 ...... 36.8 12.6 13.2 17.6 16.1 25.2 37.4 8.26 30.2 PFHS, Concentration (ppb) <LLOQ(2.09) <LLOQ(2,09) <LLOQ(2.09) <LLOQ(2.09) 3.37 <LLOQ(2,09) <LLOQ(2.09) 3.76 <LLOQ(2.09) i ........... <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.25 <LLOQ(2.09) <LLOQ(2.09) 2.26 <LLOQ(2.09) 5.64 PFOA* Concentration (ppb) 3.35 3.87 2.43 5.13 2.90 3.45 3.39 11.2 3.80 4.04 <LLOQ(2.11) <LLOQ(2.11) 5.15 3.22 2.11 4.13 2.53 4.19 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.48 <LLOQ(2.80) 20.6 6.13 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 2.63 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.21 PFOSA* Concentration (ppb) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(l.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.401 <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1,40) <LLOQ(1,40) M556" Concentration (ppb) <LLOQ(3,20) <LLOQ(3,20) <LLOQ(3.20) <LLOQ(3,20) <LLOQ(3.20) <LLOQ(3,20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3,20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ(1.80) 1,96 <LLOQ(I.80) 4.82 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(I.80) 5.27 <LLOQ(1.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(1.80) 1.55 5.50 <LLOQ(I.80) <LLOQ(I.80) 1.95 <LLOQ(I.80) The method acceptance criteria states that the measured Concentration for each QC must be within :f.20%(:t:25% for PFOSA and PFOSA.A) of the target concentration. The statistical error associated with ally individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 94 Northwest Bioanalytical -, Sample ID 11725 11726 11727 11729 11731 11732 11735 11739 11745 11746 11748 11749 11750 11751 11752 11753 11754 11756 PFOS Concentration (ppb) 16.6 20.2 25.7 21.6 63.4 30.3 20.5 54.6 26.9 24.6 31.1 17.6 20.8 6.60 45.3 29,2 37.8 36.4 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 4.77 <LLOQ(2.09) <LLOQ(2.09) 9.42 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 5.48 <LLOQ(2.09) <LLOQ(2.09) 3.61 <LLOQ(2.09) 4.53 PFOA* Concentration (ppb) <LLOQ(2.11) 2.78 8.48 4.08 10.2 4.07 3.05 5.41 4.97 3.76 3.31 4.36 4.37 <LLOQ(2.11) 4.09 2.28 3.66 8.37 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) 2.90 7.58 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 5.86 4.48 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 2.95 7.38 3.59 PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.407 <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) Study No. NWBS00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ(I. 80) <LLOQ(1.80) 2.68 <LLOQ(I.80) 3.10 2.85 <LLOQ(1.80) <LLOQ(I.80) 2.06 <LLOQ(1.80) <LLOQ(I.80) 1.94 <LLOQ(1.80) 1.85 2.05 <LLOQ(1.80) <LLOQ(I.80) 6.89 The method acceptance criteria states that the measured concentration for each QC must be within +90% (+95% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exeeed the QC acceptance criteria. m sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 95 NorthwestBioanalytical Sample ID I 1757 11758 11759 11761 11762 11763 11765 11766 11767 11768 11769 11771 11772 11773 11156 11157 11158 11159 PFOS Concentration (ppb) 34.1 24.8 17.9 17.2 20.0 28.3 22.3 49.1 16.6 14.8 26.0 6.03 40.4 9.26 44.3 28.0 21.5 40.0 StudyNo. NWB S00-128 ReportNo. NWBR01-066 Table 22.Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) 6.63 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 4.13 <LLOQ(2.09) <LLOQ(2.09) 2.16 4.10 3.04 PFOA* Concentration (ppb) 3.58 4.65 4.20 <LLOQ(2.11) 2.82 6.68 2.62 4.74 2.97 2.52 4.17 2.76 7.03 <LLOQ(2.11) 6.33 3.28 4.16 4.72 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.20 3.55 4.33 <LLOQ(2.80) 7.58 <LLOQ(2.80) 3.18 3.25 2.81 <LLOQ(2.80) 2.87 3.1 t <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I,40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) 6.60 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) 2.02 2.22 <LLOQ(1.80) 2.59 2.85 2.94 4.62 2.93 <LLOQ(I.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(1.80) 1.93 <LLOQ(1.80) 3.84 <LLOQ(I.80) <LLOQ(1.80) <LLOQ(1.80) The method acceptance criteria states that the measured concentration for each QC must be within +90% (+95% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using calibration curves (see Results and Discussion section). Page 96 Northwest Bioanalyfical Sample 1D 11160 PFOS Concentration (ppb) 31.5 11161 20.7 11162 30.9 11163 56.8 11164 76.4 11165 93.3 11166 17.7 11167 11.1 11168 48.1 1.1169 36.6 11170 41.4 11171 48.1 11172 50.3 11173 42.7 11174 65.4 11175 52.6 11176 24.3 1 t 177 30.8 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) <LLOQ(2.09) <LLOQ(2.09) 3.08 2.40 4.42 13.7 3.64 <LLOQ(2.09) 3.33 3.51 <LLOQ(2.09) 5.19 15.3 <LLOQ(2.09) 3.24 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (ppb) 2.74 3.03 6.16 4.63 9.41 5.53 <LLOQ(2.11) <LLOQ(2.11) 4.69 5.19 8.30 4.74 5.31 4.77 6.58 5.50 <LLOQ(2.11) 3.33 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.14 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) Study No. NWB S00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ(1.80) <LLOQ(1.80) 2.04 <LLOQ(1.80) 4.60 <LLOQ(1.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(1.80) 1.97 1.96 <LLOQ(I.80) 3.96 3.37 <LLOQ(1.80) <LLOQ(1.80) The method acceptance criteria states that the measured concentration for each QC must be within :1r.20%(+95% for PFOSA and PFOSA.A) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary fi'om results obtained using calibration curves (see Results and Discussion section). Page 97 Northwest Bioanalytical Sample! ID 11178 11179 11180 11181 11182 11183 11184 11185 11186 11187 11188 11189 11190 11191 11192 11193 11194 11195 PFOS Concentration (ppb) 41.0 35.2 28.3 92.8 50.0 37.4 48.8 71.6 21.7 15. l 23.2 52.6 81.9 24.3 27.1 34.3 17.1 45.6 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 12.4 25.7 5.94 9.40 4.31 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) PFOA* Concentration (ppb) 9.73 3.68 3.44 4.16 14.2 <LLOQ(2.11) 5.68 9.01 4.50 <LLOQ(2.11) <LLOQ(2.11) 13.2 6.91 3.26 5.59 7.09 <LLOQ(2.11) 7.49 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 9.91 <LLOQ(2.80) <LLOQ(2.80) 2.92 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) Study No. NWB S00-128 Report No. NWBR01-066 M556" Concentration (ppb) 3.84 <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) 2.88 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(1.80) 1.97 <LLOQ(I.80) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(I.80) 7.86 3.99 <LLOQ(I.80) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(I.80) The method acceptance criteria states that the measured concentration for each QC must be within +90% (:E25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed file QC acceptance criteria. sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using calibration curves (see Results and Discussion section). Page 98 Northwest Bioanalytical Sample ID 11196 11197 11198 11199 11200 11201 11202 11203 11204 11205 11206 ! 1207 11208 11209 11210 ,, 11211 11212 .. 11213 PFOS Concentration (ppb) 18.2 21.4 38.2 28.8 26.2 24.1 42.1 25.2 31.1 12.8 24.3 44.2 15.9 25.7 29.3 _,,, 47.5 69.6 51.9 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) <LLOQ(2.09) <LLOQ(2.09) 11.1 <LLOQ(2.09) <LLOQ(2.09) 4.20 10.7 2.79 3.27 2.26 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 4.41 <LLOQ(2.09) <LLOQ(2.09) ,. <LLOQ(2.09) PFOA* Concentration (pph) 4.69 3.76 3.02 <LLOQ(2.11) 2.87 3.00 6.93 3.45 5.55 2.47 6.67 5.25 3.61 4.69 4.32 2.81 7.25 5.10 PFOSA.A* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 4.64 <LLOQ(2.80) 3.34 3.98 PFOSA _ Concentration (ppb) <LLOQ(I.40) <LLOQ(I.40) <LLOQ0.40) <LLOQ(I.40) <LLOQ(1.40) 2.09 <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) .. <LLOQ(I.40) Study No. NWBS00-128 Report No. Na,VBR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ(I.80) 2.07 <LLOQ(I.80) <LLOQ(1.80) <LLOQ(1.80) 2, <LLOQ(I.80) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(I.80) 1.96 <LLOQ(1.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(1.80) 3.30 2.10 The method acceptance criteria states that the measured concentration for each QC must be within _+_20%(+95% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 99 Northwest Bioanalytical Sample ID 11214 11215 11216 11217 11218 11219 11220 11221 11222 11223 11224 11225 11226 11227 11228 11229 11230 11231 PFOS Concentration (ppb) 36.4 122 42.5 41.4 57.9 19.4 29.8 46.0 26.5 41.5 64.9 29.9 18.7 23.1 4 t.4 45.9 85.2 62.9 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) 6.25 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.91 <LLOQ(2.09) <LLOQ(2.09)" <LLOQ(2.09) 19.2 5.21 66.3 <LLOQ(2.09) <LLOQ(2.09) 2.33 <LLOQ(2.09) 3.22 2.45 2.51 PFOA* Concentration (ppb) 3.57 5.93 5.22 6.32 6.89 <LLOQ(2.11) 2.94 6.44 2.73 5.80 4.30 4.50 5.01 4.61 6.50 5.43 7.01 3.53 PFOSAA* Concentration (ppb) 4.34 3.21 2.98 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 4.60 6.36 PFOSA* Concentration (ppb) <LLOQ(I.40) <LLOQ( 1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) Study No. NWBS00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(I.80) <LLOQ(I.80) 3.01 <LLOQ(I.80) 3.12 <LLOQ(1.80) <LLOQ(1.80) <LLOQ(I.80) <LLOQ(I.80) 4.02 <LLOQ(I.80) <LLOQ(I.80) <LLOQ(1.80) 2.07 2.57 <LLOQ(1.80) The method acceptance criteria states that the measured concentration for each QC must be witldn _-17.20(%=t.25%for PFOSA and PFOSA_A) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSA.A, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 100 Northwest Bioanalytical Sample ID 11232 11233 11234 11235 11236 11237 11238 11239 11240 11241 11242 11243 11244 11245 11246 11247 11248 11249 PFOS Concentration (ppb) 21.6 30.0 39.0 22,0 26.7 80.0 37.8 24.7 37.2 139 65.9 27,0 64.9 29,7 28.2 19.0 36.2 36.3 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.23 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 2.64 <LLOQ(2.09) 5.3 9.47 <LLOQ(2.09) 3.73 2.22 <LLOQ(2.09) <LLOQ(2.09) 5.00 <LLOQ(2.09) PFOA* Concentration (ppb) 4.87 3. l 0 4.81 3.39 4.13 9.10 4.97 4.41 3.29 20.6 6.87 3.01 8.74 5.21 2,44 3.14 5.70 5.58 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.18 <LLOQ(2,80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 3.83 <LLOQ(2.80) <LLOQ(2,80) <LLOQ(2.80) <LLOQ(2.80) 3,26 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.801 PFOSA* Concentration (ppb) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.401 <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1,40) <LLOQ(I.40) <LLOQ(1.401 Study No. NWB S 00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3,20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) 4.44 2.15 2.58 <LLOQ(1.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(I.80) 6.15 2.56 1.88 <LLOQ(I,80) <LLOQ(1.80) 2.49 <LLOQ(I.80) <LLOQ(I.80) 2.17 <LLOQ(1.80 / The method acceptance criteria states that the measured concentration for each QC must be within +90% (+95% for PFOSA and PFOSAA) of the target concentration. Tlae statistical error associated with any individual result may exceed the QC acceptance criteria. Serum sample results for PFOA, PFHS, PFOSA.A, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 101 Northwest Bioanalytical Sample ID 11250 11251 11252 11253 11254 11256 11257 11258 11259 11260 11261 11262 11263 11264 11265 11266 11267 11268 PFOS Concentration (ppb) 26.1 34.6 13.1 56.8 50.8 47.8 33.8 23.1 7.63 34.7 12.6 17.7 226 42.2 24.7 27.2 36.8 39.7 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) 4.07 2.19 <LLOQ(2.09) 4.36 <LLOQ(2.09) 7.07 <LLOQ(2.09) <LLOQ(2.09) <LLOQ(2.09) 4.14 3.80 <LLOQ(2.09) <LLOQ(2.09) 5.11 2.45 <LLOQ(2.09) 11.3 <LLOQ(2.09) PFOA* Concentration (ppb) 2.32 5.07 <LLOQ(2.11) 7.39 4.81 2.64 5.55 4.33 <LLOQ(2.1 I) 5.12 2.53 4.07 52.3 3.54 5.69 3.47 2.84 2.47 PFOSAA* Concentration (ppb) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 21.2 3.65 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) 7.22 <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(1.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(I.40) <LLOQ(1.40) Study No. NWBS00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ(1.80) <LLOQ(I.80) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(1.80) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(I.80) <LLOQ(1.80) 1.87 <LLOQ(1.80) <LLOQ(I.80) <LLOQ(1.80) <LLOQ(I.80) 1.86 ' <LLOQ(I.80) The method acceptance criteria states that the measured concentration for each QC must be within :k20% (:t.25% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary fi'om results obtained ushlg calibration curves (see Results and Discussion section). Page 102 Northwest Bioanalytical ,Sample I_D 11269 PFOS Concentration (ppb) 25.2 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. PFHS* Concentration (ppb) 3.67 PFOA* Concentration (ppb) 2.54 PFOSAA* Concentration (ppb) <LLOQ(2.80) PFOSA* Concentration (ppb) <LLOQ(I.40) Study No. NWBS00-128 Report No. NWBR01-066 M556" Concentration (ppb) <LLOQ(3.20) M570" Concentration (ppb) <LLOQ(1.80) NOTE: The method acceptance criteria states that the measured concentration for each QC must be within +90% (+95% for PFOSA and PFOSAA) of the target concentration. The statistical error associated with any individual result may exceed the QC acceptance criteria. * Serum sample results for PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 obtained using plasma calibration curves may vary from results obtained using serum calibration curves (see Results and Discussion section). Page 103 Northwest Bioanalytical Study No. NWB S00-128 Report No. NWBR01-066 Table 23. Repeat Analysis Table for PFOS Sample ID 11699 Original Cone. ppb >ULOQ(414) OriginalRun Number 10 Reason for Reassay 1 Reassay Cone. ppb 1670 Reassay Run Number 17 * Concentration corrected for amount of persistent PFOS in dilution matrix. Reported Cone. ppb 1656' Reason for Reported Cone. 1 REASONS FOR REASSAY: 1). Greater than the ULOQ. REASONS FOR REPORTED CONC: 1). Original result outside of quantitation Page 104 range. Reassay results reported. Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Figure l. Representative Calibration Curve for PFOS 18 16 14 12 _s "5 6 4 2 0 14 12 |0 g A_alytic.,dRun I analyzedon 27-Nov-2000Calibration$t,-md_dsfor PFOS(ppb) Regression Method - QUADRATIC - WeishtinB Factor- l/X*"2 Qua_adc Limit = 849 A t i I I t i t I 50 100 150 200 250 300 350 400 450 Nominal Cone. Figure 2. Representative Calibration Curve for PFHS Aa,dydcal Run I amdyzed on 27-Nov-2000 Cal_radon Staadar_ forPFHS (ppb) P..egres._mMedmd - QUADRATIC - Weighdag Factor- I/X**2 QuadraticLimit - 1190 4 ? 0 100 200 300 400 $00 600 Nominal Cone.. Page 105 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Figure 3. Representative Calibration Curve for PFOA AnalyticRauln Ianaly_ oa 27-Nov.200C0alibradoSnlandat_['oPrFOA (ppb) Regr_/on Method= QUADRATIC - Weighting Factor - I/X"2 Qu.,,_-aLtiimcit- 104410 g 7 6 i4 2 [ 0 0 8 7 6 u I i I I I ] I I I 50 100 150 200 2.50 J(X} 350 400 450 $00 Nominal Conc. Figure 4. Representative Calibration Curve for PFOSAA Anai_cal RunI analyzedon 27-Nov-2000Calibr'_ionStandardfosr PFOSAA(.ppb) Regn_ssionM_-_xl - QUADRATIC - Weighting Facto-r I/X"2 Quad_dc Limk - -I 11000 0 100 2O0 JCO 4OO ;SO0 6C0 Nomiaal Cone.. Page 106 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Figure 5. Representative Calibration Curve for PFOSA Anal_i_l Run I analFtx"don 27-Nov-2000 Calibration Stand.Ta'dsfor PFOSA {ppb) RegressionMethod- QUADRATIC - Weighting Factor- I/X'*2 Quadratic Limit - 1160 '15 4O g 30 i: "q 15 I0 5 0 5.0 4.5 4.0 I ) ! l l [ I ) I 1OO 1_0 200 250 300 350 400 450 :500 Nominal Cone. Figure 6. Representative Calibration Curve for M556 Aralytical Run I analTze, d on 27-Nov-2QO0CalibrationStandardfsorMS56 _pb) Relp'_alon Mthod- QUADRATIC - Weighting Factor = I/X**2 Quadratic Limit - -5890 i xs _2.0 1.5 1.0 0.50 _ t '1 I t ! I I 100 150 200 250 300 350 40Q 450 NomimdCone. Page 107 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Figure 7. Representative Calibration Curve for M570 Analytical RunI analyzedon 27-Nov-20OOCalibrationStandardst'orM$70 (ppb) Regresaion Method - QUADRATIC - Weighting Factor= l/X*'2 Quadratic Limit = 3420 12 I0 8 j' 2 0 t _ I I I $0 tOO 150 200 250 300 350 400 450 500 Nominal Cone. Page 108 Northwest Bioanalytical Figure 8. Human Plasma Blank for PFOS Study No. NWBS00-128 Report No. NWBR01-066 0.(30 0,00 o.== 20" I00 :if .! ...... :.::., =-2. " ; IL . . ,o,,_o, _o, ._, ._o_,,,,_ . . . I.S9 :: ._.17 4.7'4 '6."_2 .. 7.90 r_*l| Page 109 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Figure 9. Human Plasma Blank for PFHS Page ll0 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Figure 10. Human Plasma Blank for PFOA 0.00 0.00 0._0 0._0 .... ::i.' i._:_i:,_._ 20- :..tO- ::::_::!..:: : O" ::." : I._9-. :3.17 4,74 ::/.6.:32 7.90 T_rne_ Page 1[ 1 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Figure ll. Human Plasma Blank for PFOSAA Page 112 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Figure 12. Human Plasma Blank for PFOSA ':: .. !;I::C L._!;:::I.,:_,:._:. 101 ":: ITHPFO5 ExpectedRT 4,63 _Peas InlectaJShlnda_d Cu/retrtl M_lhod J Noise Thres. _ 10.0 Min, Wid|h MUlL Wid|h Base.Wldlh RTWin. (sees) (_=41St_mi'_o.oth _ ] 10 1SO 20 0.21 s0012801-011 1 011 _g128 CONTROL BLANK I NO Comment I_on, Nov Z702000 7:20 PM 8,_B in I _i(xl I: 8.98 _RM, 571 427,0-> 40_.0 "7. _':. :i:i; :.!:,.:........... _:_!!i:_::i_ Area 0 Hei_jh 0 Slarl Time 0.00 End Time 0.00 Ime_a_on Width 0.(_ Inl_;llion Type ,o- 2.0. 1oo .,: ..:L.... {::,:i!:_,:i_: :: :_:_._i:::: I01 20t 301 401 501 3_m .... 1.59 :3.17: 4.74 . 6.32 7,90 Timej_ Page ll3 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR0 [-066 Figure 13. Human Plasma Blank for _vI556 0 0 Page 114 Northwest Bioanalyticat S tudy No. NWBS00-128 Report No. NWBR0 [-066 Figure 14. Human Plasma Blank for M570 Page 115 Northwest B ioanalytica[ S tudy No. NWB S00-128 Report No. NWBR01-066 Figure 15. Human Plasma Blank with Internal Standard (QC0) for PFOS Page 116 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR0 L-066 Figure 16. Human Plasma Blank with Internal Standard (QC0) for PFHS Page ll7 Northwest Bioanaly_ical Study No. NWBSO0- [ 28 Report No. NWBR01-066 Figure 17. Eluman Plasma Blank with Internal Standard (QC0) for PFOA Page 118 Northwest Bioanalydcal Study No. NWBSO0-128 Report No. NWBR0 [-066 Figure 18. Human Plasma Blank with Internal Standard (QC0) for PFOSAA Page 119 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWB R0 L-066 Figure 19. Human Plasma Blank with Internal Standard (QC0) for PFOSA {_:O_a Use Area A_lule Rt,lerlllon Time Ex_ed Rr 5.70 Inmrn.lllSlanda,d: rHPFOS Ctwtmlt Mefhod I N_se Th,es. _ 2.0 /,,tin. WkIth Mull. Width 8_e. Width RTWin. |SeeS) _ Slm'h(o_o. _ _ $ 10 150 20 1.0i s_O12801,.012 1 012 S00128 QCO I No Comme_ ,,_n, Nov 27, 21_0 7".32 PM I :: '!:i: ;." . ' :: : :. -.:.i".. .:.: !!!:z.';i(_ ::!!::_:.:_...,::i_:!:_!:i_:ii'._;::'5:.i_i_ . :: :i':'.-.-" ':;/::::::-:.:'. ;. ':::.:.i ":-:i_,-i! :::_-i!::!:ii!:i:,::!:":!_:;:..".:]!.:_:_i:_:!?::_:_ Ht+_h, l_, nine End "time s_ ._%:_: ;6a :i.;:!:i_:!i__i:i_:;Lii.:_:_:i.-':!_..!i:::_:_:.!_:',:,:i:::,i_:.?_(::__!:i::.i_;;_:;i._::_::.':i:<]:::i.._'::;_.:'i:_;]:_i:;_cg:ii.=i;'',i__J:.i:.__;::::.::ii_i':i:?;_:_;::i_;*.g:_:_;!:;ii!-::!i__;:i_)i_:_i':_!:!i_::i__!i!_::':i__,.-i;:ii__:;_.:T_i';:ii!:_i_:}i_ii:_iii_Y:i_ii_ 6.I0 :'_:.::i_:_':i:_:_!i:ii!-__i'i_?? _: _::_:i:r:'._:_:Si:i!_',_,E::i"-I: ::__i:!_ :_ !-<_:_:__::_:?-':-i_?_.i!_:i_3 ,..., , ,_. r-a-_w'r'_ :i::- :'_:.::"':_:_':.i:_::_._.:_.l9'!:'_':;_-_::_:"" :._:_: :,_:_:_:_::c__::.: ::_ _:_.:_:::::a iTHI_O$ use as lnt_n,111$t,II_I_ ExpectedRT 4.53 I Noi_Thres. _u_rt,nt Mea.,od [ IO.O I 10.O _ 1_i'es. _ Min. V_dlh [ Mull Width _ 0,2 31 3 10 B;_e. Wlclth _ 150 RTW_n. _ 1201 20 Smo_h I 11 s0012801.012 I 012 _:_0128(_7-.0_l _S_ _ _{_:_:._._;_ NOComment _ _:_:_:; _ : '_1::'._ :_ ._;_" _" 4 _ :: _: :: _ _ _ :._ _ _ _ _ _ _4:_ _4 _ ] _ _ _1 t_ _, 2_ _ _ 8.98in I p_'lod : it :]_}ii_-_!i!_:!::!ii!i!_?'i}i_'i:.":i:!:':;i":!'i:::.l:!i=:i-_'ii!-!:_':-i:_.{-._-.::}_:i;_'i-_.-:'.__{i:!_'_._ii_j_ Area Hei[_f S,_nme 185736 _r,Jll EInncde_Ttiam_eon W_h 4.:]O 40..8_4 ::':;':'..-_.[$_!:__::[2:.2_{:.:' ::;!!i:,: 7:::. !: _:_i]:_._" _!:*,_ _:.,.:Pk'_:_:.:._-[]a-:_.,T_! : .,u-f .:_z,::_'_:!=_::_._:_:,::_,:.:_.__:, -. :.:-I_ _:_:_:_.:__'.:::'_:_ :_:-"=a-'_r__:_:_.:_-.'__ ..... i+""__ _+ "";!_": "._...... _...... '_"_ "'_4t:[_ _ ""_':" " ' "4..... ":' _ 60 ":_]>:,_!::':i_:]e_?g;"?:::]i::_ "'-::': ':5{] :{:_:_ :_!_:_:f!{:]]:!.-:.__:'{:-_-_{ I '_O :.,:...i_!i?i-::'%i_:i.i::::.:_:i-_i-__-:i:_?.;;?!:'.5_?::i:;.'i'_!i3!:i!_!:_:i:_}?}_-t_{:J;_::::!giT!i!'_:_'_ I_II_ _o ' : _o[ ....'..'.:: _4 10_ 101 I ._9 . " :..- .}.. :_.: .:: :7: ::::i::: _:::i:_i_: ::>::%::7;===================== 181 r- ._ " -:394 .... " _16 " ":_".:- 201 301 :_.17 4.74 .401 _Ol 6.]a ..... 7.?o _$_n -h__1_" . :lqm,,tg Page 120 Northwest B ioanalytica[ Study No. NWBS00-128 Report No. NWBR01-066 Figure 20. Human Plasma Blank with Internal Standard (QC0) for M556 Page 121 Northwest Bioanalytical Study No. NWBS00-128 Report No. NWBR01-066 Figure 21. Human Plasma Blank with Internal Standard (QC0) for M570 iTHPFOS Exlx_c_edRT 4.63 use as Inlemal SI,mda_d Currefll Me(h(xJ ] " Noise TI_eS. _ 1O.0 /rUn. Width 3 Mull. Width 10 Base._dth 150 RTWin. [sect) 20 QuaN STih'nr_etsh. _ 0.21 10012801-012 1 012 ._012_ (_('-.0I NO Commenl NOV 27, 2000 7"12PM ------ ::': "';': ::':"_:!_: . 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Tim_- Page 129 Northwest Bioanalytical Figure 29. High Standard for PFOS S tudy No. NWBS00-128 Report No. NWBR0 [-066 iTHPFOS useaSInternal St_d_d F.x.p_ed RT 4.63 Curtem Mehod J Noise Tl_es. _ Qua_ ThreL _ M|n, V_d_h _ Mull. Width _ Ba_. Width _ RTWin. (sees| [_ S,,_h I 10,0 0.2 3 I0 150 20 1I s0012801-080 1080 $00128 S_9 2 I No Commenl me_ral_onVV[dh 046 J_-_'{ ::'':'::i.:" "_:;::::._'::_.a:_:::i=i:-_::_'L: : .?L:'.::!':I_:.:!I[::='_:I4:_. ::i_'l_:_(:ii | ".:r.o.ot.. ._.=,:,oi":_',_-.=: ,:o'2=:,-:_1._.:::o.:_:.,:y:...:..43o::._,:,':=!,::_.o.._i,::=.i_:::..o:,:_;i,::i.5.,_ T'_dr_ Page 130 Northwest B ioanalytica[ Figure 30. High Standard for PFHS Study No. NWBS00-128 Report No. NWBR01-066 ItH_OS USe_S Inietnal SUlnd_d ExpectedRT 4,63 I Currem Method _oisTeh,_ I_1o_ lo.o _ 11_res. _ Min. Width _ Muir. 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