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Northwest Bioanalytical A6_ IAH Study No. NWBS00-088 Report No. NWBROl-OOl Quantitative Determination of PFOS and Related Compounds in Human Serum by LC/MS/MS Sample Analysis Report for Protocol E P I-0 0 1 1 N orthw est Bioanalytical (NWB) A Division of NW T Inc. 1121 E ast 3900 South Salt L ake City, UT 84124 fcOr> u) co o~~Qpron CM uD ys* i :Ax-, ^ o * CD --J PREPARED FOR: 3M Company Corporate Occupational Medicine, Medical Department 220-3 W-05 St. Paul, MN 55144 AUTHOR: Connie O. Sakashita, B.S., NWB Project M anager DATE: /h30-O I DATE: //- i 0- 0/ Page 1 no CB' 000339 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBR01-001 QUALITY ASSURANCE STATEMENT LABORATORY: Northwest Bioanalytical (NWB) A Division of NWT Ine. 1121 East 3900 South Salt Lake City, UT 84124 SPONSOR: 3M Company Corporate Occupational Medicine, Medical Department 220-3W-05 St. Paul, MN 55144 COMPOUND(S): PFOS and Related Compounds NWB STUDY NUMBER: NWBSOO-088 SPONSOR STUDY NUMBER: EPI-0011 NWB STUDY TITLE: Quantitative Determination of PFOS and Related Compounds in Human Serum by LC/MS/MS The clinical study described in this report is not included within the definition of a GLP regulated nonclinical study. However, Northwest Bioanalytical conducts all studies within the guidelines of the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58), the OECD Principles of Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety of Drugs (Ordinance No. 21, PAB Notification No. 424.) The following inspections were performed by the NWB QAU per SOP. Inspection and Reporting Statement. Date of Inspection Phase of Study Date Report Sent to Date Report Sent to NWB Project Manager NWB Management* 22-25 Sep 2000 16 Oct 2000 07-13 Nov 2000 20-25 Oct 2001 27 Nov 2001 03 Dec 2001 Sample Receipt Analytical Plan Sample Analysis Report Draft/Raw Data 2ndReport Draft/Raw Data Final Report 25 Sep 2000 16 Oct 2000 14 Nov 2000 25 Oct 2001 27 Nov 2001 03 Dec 2001 29 Sep 2000 31 Oct 2000 30 Nov 2000 31 Oct 2001 30 Nov 2001 31 Dec 2001 Reports to NWB Management are issued monthly. As can reasonably be established, the methods and procedures described and the results incorporated into this final report accurately reflect the raw data. 4~s%Lb _______ tacy Lynn Chain, B.A. NWB Quality Assurance Compliance Auditor M~c3-( Date Page 2 000340 Northwest Bioanulytical Studv No. NWBS00-088 Report No. NWBR01-001 COMPLIANCE STATEMENT The clinical study described in this report is not included within the definition o f a GLP regulated nonclinical study. However, to the best o f our knowledge, this project was conducted in accordance with the guidelines o f the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58) and according to the methods and procedures described within this report. In addition, the study followed the guidelines o f the OECD Principles o f Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety o f Drugs (Ordinance No. 21, PAB Notification No. 424.) Any known incidents that m ay have affected the quality or integrity o f the project or reported data is included in this report. This report represents an accurate record o f the raw data. (UrrwuJ. Connie O. Sakashita, B.S. NWB Project Manager Rodger L. Foltz, Ph.D. NWB Technical Director / /-ao-o/ Date n - ? q -<f / Date Page 3 030341 Northwest Bioanalytieal TABLE OF CONTENTS Study No. NWBS00-088 Report No. NWBR0t-00l SIGNATURE P A G E .................................................................................................................................. I QUALITY ASSURANCE STA TEM EN T..............................................................................................2 COMPLIANCE STATEM ENT................................................................................................................. 3 TABLE OF CO NTEN TS............................................................................................................................ 4 LIST OF TA B LE S....................................................................................................................................... 4 LIST OF F IG U R E S ............................... 5 1. IN TR O D U C TIO N .................................................. 8 2. M ETH O D O LO G Y ............................................................................................................................. 9 3. SAMPLE A N A L Y SIS......................................................................................................................12 4. RESULTS AND D ISCU SSIO N ..................................................................................................... 13 5. R E FE R E N C E S................................... 17 6. DATA R ETEN TIO N ........................................................................................................................17 LIST OF TABLES Table 1. Calibration Curve Summary for PF O S................................................................................. 18 Table 2. Calibration Curve Summary for P F O A ................................................................................19 Table 3. Calibration Curve Summary for P F H S .................................................................................. 20 Table 4. Calibration Curve Summary for PF O SA A ...........................................................................21 Table 5. Calibration Curve Summary for PFO SA ........................... .................................................. 22 Table 6. Calibration Curve Summary for M 556................................................................................. 23 Table 7. Calibration Curve Summary for M 570.................................................................................. 24 Table 8. Back-Calculated Concentrations o f Calibration Standards for P F O S .............................. 25 Page 4 030342 Northwest Bioanalytieal Study No. NVVBS00-088 Report No. NWBR01-001 Table 9. Back-Calculated Concentrations o f Calibration Standards for PFOA.............................. 27 Table 10. Back-Calculated Concentrations o f Calibration Standards for P F H S .......... .................29 Table I t. Back-Calculated Concentrations o f Calibration Standards for PFOSAA..................... 31 Table 12. Back-Calculated Concentrations o f Calibration Standards for P F O S A ........................33 Table 13. Back-Calculated Concentrations o f Calibration Standards for M 5 5 6 ...........................35 Table 14. Back-Calculated Concentrations o f Calibration Standards for M 5 7 0 ...........................37 Table 15. Analytical QC Summary for P F O S .................................................................................... 39 Table 16. Analytical QC Summary for PFO A .................................................................................... 41 Table 17. Analytical QC Summary for P F H S .................................................................................... 43 Table 18. Analytical QC Summary for PFO SA A ...............................................................................45 Table 19. Analytical QC Summary for PFOS A ..................................................................................47 Table 20. Analytical QC Summary for M 5 5 6 .................................................................................... 49 Table 21. Analytical QC Summary forM 570 .................................................................................... 51 Table 22. Study Sample Concentrations.............................................................................................. 53 Table 23. Repeat Analysis Table for PF O S....................................................................... 92 Table 24. Repeat Analysis Table for PF H S........................................................................................ 92 LIST OF FIGURES Figure 1. Representative Calibration Curve for P F O S ......................................................................93 Figure 2. Representative Calibration Curve for PFO A ......................................................................93 Figure 3. Representative Calibration Curve for P F H S ......................................................................94 Figure 4. Representative Calibration Curve for PFO SA A................................................................ 94 Figure 5. Representative Calibration Curve for P F O S A .................................................................. 95 Figure 6. Representative Calibration Curve for M 5 5 6 ......................................................................95 Page 5 000343 Nortilwest ioanalytieal Study No. NWBS00-083 Report No. NWBR01-00I Figure 7. Representative Calibration Curve for M 5 7 0 ................ 96 Figure 8. Human Serum Blank for PFO S............................................................................... 97 Figure 9. Human Serum Blank for P F O A .............................................................................................98 Figure 10. Human Serum Blank for PF H S ........................................................................................... 99 Figure 11. Human Serum Blank for P F O S A A ...................................................................................100 Figure 12. Human Serum Blank for P F O S A ...................................................................................... 101 Figure 13. Human Serum Blank fo rM 5 5 6 ..........................................................................................102 Figure 14. Human Serum Blank for M 570..........................................................................................103 Figure 15. Human Serum Blank with Internal Standard (QC0) for P F O S ............ ................ 104 Figure 16. Human Serum Blank with Internal Standard (QC0) for PFOA...................................105 Figure 17. Human Serum Blank with Internal Standard (QC0) for P F H S ................................... 106 Figure 18. Human Serum Blank with Internal Standard (QC0) for PFO SA A ............................ 107 Figure 19. Human Serum Blank with Internal Standard (QC0) for P F O SA ................................108 Figure 20. Human Serum Blank with Internal Standard (QC0) for M 5 5 6................................. .109 Figure 21. Human Serum Blank with Internal Standard (QC0) for M 5 7 0 ...................................110 Figure 22. Low Standard (3.94 ppb) for PFO S...................................................................................111 Figure 23. Low Standard (1.92 ppb) for P F O A ..................................................................................112 % Figure 24. Low Standard (1.36 ppb) for PFH S...................................................................................113 Figure 25. Low Standard (1.60 ppb) for PFO SA A ............................................................................114 Figure 26. Low Standard (1.00 ppb) for PFO SA ............................................................................... 115 Figure 27. Low Standard (2.50 ppb) forM 556............................................................ 116 Figure 28. Low Standard ( l .00 ppb) for M 570...................................................................................117 Figure 29. High Standard (414 ppb) for PF O S...................................................................................118 Page 6 030344 Northwest Bioanalytical Study No. NWBS00-083 Report No. NWBR01-001 Figure 30. High Standard (481 ppb) for P F O A ............................................................................... 119 Figure 31. High Standard (523 ppb) for P F H S ..................................................................... .120 Figure 32. High Standard (501 ppb) for PF O SA A ..........................................................................121 Figure 33. High Standard (500 ppb) for P F O SA .............................................................................122 Figure 34. High Standard (500 ppb) for M 5 5 6 ........................................................................ 123 Figure 35. HighStandard (500 ppb) for M 570....................... 124 ( Page 7 030345 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NVVBROl-OOl Quantitative Determination of PFOS and Related Compounds in Human Serum by LC/MS/MS Sample Analysis Report for Protocol EPI-0011 1. IN T R O D U C T IO N This report summarizes the analytical results from the quantitation o f PFOS, PFOA, PFHS, PFOSAA, PFOSA, M556, and M570 in human serum samples for 3M Company in support o f Protocol EPI-0011 [5.1]. The LC/MS/MS method for the analytes exhibited a quadratic response for the following LLOQ and ULOQ values: A n aly te PFOS PFOA PFHS PFOSAA PFOSA M556 M570 LLOQ 3.94 ppb 1.92 ppb 1.36 ppb 1.60 ppb 1.00 ppb 2.50 ppb 1.00 ppb ULOQ 414 ppb 481 ppb 523 ppb 501 ppb 500 ppb 500 ppb 500 ppb . The testing facility was 3M Company (Corporate Occupational Medicine, Medical Department, 220-3W-05, St. Paul, MN 55144), and the Study Director was Jeffrey H. Mandel, M.D., M.P.H. James K. Lundberg served as the technical contact at 3M. The following is a list o f NWB supervisory personnel involved in the completion o f this work: Connie 0 . Sakashita, B.S. (NWB Project Manager); Patrick Bennett, M.S., M.B.A. (NWB Laboratory Director); Rodger L. Foltz, Ph.D. (NWB Technical Director). Laboratory personnel involved in the completion o f this study included Suzanne Newman, B.S. (NWB Research Scientist); Emily Yardimci, B.S. (NWB Scientist). NWB SOPs and guidelines were used in the conduct o f this study and were available to study personnel in electronic and/pr hard copy formats. Page 8 03034t Northwest Bioanalytical Study No. NVVBS00-088 Report No. NWBROl-OOl Date Study Initiated: 22-Sep-2QQ0 Date Analyses Completed: 25-Mar-2001 However, Northwest Bioanalytical conducts all studies within the guidelines of'the U.S. FDA Good Laboratory Practice Regulations for Nonclinical Laboratory Studies (Title 21 CFR Part 58), the OECD Principles o f Good Laboratory Practice and the Japanese MHW Good Laboratory Practice Standard Ordinance for Nonclinical Laboratory Studies on the Safety o f Drugs (Ordinance No. 21, PAB Notification No. 424). Any changes to or deviations from the original protocol (Analytical Plan) were documented through approved protocol amendments or deviation memos and are retained within the raw data. 2. M ETHODOLOGY The assay used for this study is reported in Northwest Bioanalytical reports NWBROO108 [5.2] and NW BR00-122 [5.3]. Chinese human plasma was used for the calibration curves and quality control samples. Serum sample results obtained using plasma curves are discussed in NWBR00-122. Samples for this study were received at NWB on the following dates: Receipt Date 21-Sep-2000 22-Sep-2000 21-Feb-2001 Number o f Samples Received 526 73 62 Storage Condition (except during analysis) -20 C -20 C -20 C Page 9 030347 Northwest Bioanalytical Study No. NVVBSOO-083 Report No. NVVBRO1-001 Reference Material Analyte PFOS PFOA PFHS PFOSAA PFOSA M556 M570 THPFOS Lot Number Purity Expiration Date Source 193 100% 31-Dec-2010 3M 245 100% 31-Dec-2010 3M SE-036 100% 01-Jan-2010 3M 617 53.8% 31-D ec-2010 3M 214 100% 31-D ec-2010 3M NB113047-8D 99.89% 31-Dec-2010 3M 118506-26 99.75% 31-Dec-2010 3M 59909 90% 31-Dec-2010 3M Storage Conditions Room temperature* Room temperature* -20 C Room temperature Room temperature Room temperature Room temperature Room temperature *Stored dry The reference material purity for PFOS, PFOSA, PFHS, and PFOA was not available prior to the conduct o f this study. Therefore, the reference material purity was assumed to be 100%. 3M contracted with Centre Analytical Laboratories, Inc., in State College, Pennsylvania to determine the absolute concentration o f PFOS, PFOA, and PFHS in NWB stock solutions used to prepare the analytical standards and controls used for this studies. All arrangements for purity determinations and the transfer o f NWB solutions to Centre Analytical Laboratories, Inc., were perform ed by 3M. Based on Centre Analytical Laboratories' results, the concentrations o f plasma calibrator and quality control samples were corrected using the following factors: Analyte PFOS PFOA PFHS Correction Factor 0.821 0.961 1.043 Eight or more calibration standards were prepared on the day o f each run by adding 100 pL o f blank human Chinese plasma and 400 pL o f 50 mM ammonium acetate in Page 10 030348 Northwest Bioanalyticul Study No. NWBS00-088 Report No. NWBRO1-001 water (unadjusted pH ~6.9) to 13 x 100 mm polypropylene tubes. After a brief vortex mixing, 10.0 pL o f the appropriate spiking solution was added.The final calibration standard concentrations in human Chinese plasma for each analyte are listed below: Analyte Calibration Standard Concentrations* PFOS 3.94, 5.17, 11.3, 23.6, 44.2, 85.4,209, 332, and 414 ppb PFOA 1.92, 3.36, 10.6, 25.0, 49.0, 97.1, 241, 385, and 481 ppb PFHS 1.36,2.92, 10.7, 26.5, 52.6, 104, 262,418, and 523 ppb PFOSAA 1.60, 3.10, 10.6,25.6, 50.6, 101, 251, 401, and 501 ppb PFOSA 1.00,2.50, 10.0, 25.0, 50.0,100, 250, 400, and 500 ppb M556 2.50,10.0, 25.0, 50.0, 100, 250,400, and 500 ppb M570_____________1.00,2.50, 10.0, 25.0, 50.0, 100, 250, 400, and 500 ppb________ * The target calibration curve range is 1.00 ppb to 500 ppb (except for M556 which has a LLOQ of 2.50 ppb). Each analyte has a different final curve range based upon the persistent levels of the analyte in the human Chinese plasma used. In addition, blank plasma samples, both with and without internal standard (designated as QCOs and Blanks, respectively), were assayed in each analytical run. Analytical QCs were prepared in human Chinese plasma on October 6, 2000, October 11, 2000, and October 27, 2000'and stored in a -20 C freezer. For each run, analytical QC levels were assayed in duplicate. In addition, for each dilution level, dilution QCs were run in triplicate in any analytical run that contained diluted subject samples. The QC concentration levels are shown in the following table. Analyte PFOS PFOA PFHS PFOSAA PFOSA M556 M570 Low 6.40 4.81 4.48 4.60 4.00 4.00 4.00 QC Concentrations All concentrations are expressed as ppb. M edium High High, DF = 2 126 332 335 145 385 386 156 417 418 151 401 401 150 400 400 150 400 400 150 400 400 Page 11 000349 Northwest Bioanalytical Study No. NWBSO-088 Report No. NWBR01-001 The internal standard (THPFOS) was added to all plasma and serum samples (except Blanks) for a final concentration o f approximately 200 ppb. The analytical method consisted o f a liquidtliquid extraction procedure followed by evaporation and reconstitution o f the extract residue with 20 mM ammonium acetate in water: 20 mM ammonium acetate in methanol (30:70 v/v). The samples were analyzed by liquid chromatography/tandem mass spectrometry using a PE Sciex API 3000. The instrument was operated in the multiple reaction monitoring (MRM) mode under optimized conditions for PFOS, PFOA, PFHS, PFOSAA, PFOSA, M556 and M570 detection of the negative ions formed by TurboIonSprayTM ionization. 3. SAMPLE ANALYSIS PFOS, PFOA, PFHS, PFOSAA, PFOSA, M556, M570, and THPFOS chromatographic peaks were integrated using the PE Sciex M acQuan software (version 1.6) with a smooth factor o f one. Quantitation was based upon quadratic regression analysis o f weighted (1/x2) calibration curves using area ratio vs. concentration utilizing Watson DMLIMS software (version 6.1.1.04). The samples were injected in a systematic order. 3.1. Acceptance Criteria For an analytical run to be accepted, it must have met the acceptance criteria listed below which are consistent with regulatory and industry recommendations. Calibration Curve Each run will include in duplicate calibration standards at six or more concentrations covering the lower to upper limit o f quantitation. For all analytes except PFOSA and PFOSAA, at least three-fourths of the calibration standard's back-calculated concentrations must be within 15% ( 20% for LLOQ) o f their individual target concentrations. For PFOSA and PFOSAA, at least three-fourths o f the calibration Page 12 000350 Northwest Bioanalytieal Study No. NWBS00-088 Report No. NWBR01-001 standard's back-calculated concentrations must be within 20% ( 25% for LLOQ) o f their individual target concentrations. A calibration standard will be considered an outlier if it is greater than two times the acceptance criteria for that standard. Lower Limit o f Quantitation The back-calculated concentrations o f at least one o f the duplicate lowest points in the calibration curve must be within 25% o f the target concentration for PFOSA and PFOSAA to qualify as the LLOQ and within 20% o f the target concentration to qualify as the LLOQ for all other analytes. If this criterion is not met, the next level is subjected to the same test and the LLOQ raised accordingly. Quality Control Samples Each analytical run will include low, medium and high QC samples in duplicate. The measured concentrations o f at least two-thirds o f all analytical QCs must be within 20% o f their target concentrations ( 25% for PFOSA and PFOSAA), and no two QCs at the same concentration can be outside the limit. If study samples require dilution, a dilution QC will be analyzed in triplicate for each dilution level (except for PFOSA and PFOSAA which should not be diluted with control matrix). At least two dilution QCs at each level must be within 20% o f its target concentrations in order to accept diluted study samples at that level. The dilution QC acceptance is independent o f the undiluted analytical QC acceptance. 4. RESULTS AND DISCUSSION Serum sample results obtained using plasma curves for PFOA, PFHS, PFOSAA, PFOSA, M556, and M570 did not meet NWB SOP requirements for validation. Results may vary on average up to 26% from results obtained using human serum calibration curves at some concentration levels for PFOA, PFHS, PFOSAA, M556, and M570. For PFOSA, results may vary on average up to 43% from results obtained using human serum Page 13 030351 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 calibration curves. However, in order to obtain the lower limit o f quantitation less than 5 ppb required by the Sponsor, it was necessary to use plasma curves. Each accepted run met the acceptance criteria set for the calibration curve points, for the lower limit o f quantitation (LLOQ) and for the analytical quality control (QC) samples. Run ID 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 PFOS R esu lt Rejected Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted N /A N /A Accepted PFOA R esu lt Rejected Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted N/A N/A Accepted PFHS R esu lt Rejected Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted N /A N /A Accepted PFOSAA Result Rejected Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Rejected N /A Accepted Accepted C om m ents All analytes rejected due to sample preparation error LLOQ raised for PFOS Low QCs failed for PFOSAA. N/A = not analyzed Run ID l PFOSA R esu lt Rejected 2 Accepted 3 Accepted 4 Accepted 5 Accepted M556 Result Rejected Accepted Accepted Accepted Accepted M570 R esu lt Rejected Accepted Accepted Accepted Accepted C om m ents A ll analytes rejected due to sample preparation error n0 3ft 0/ l 3o t5*2 Page 14 Northwest Bioanalytical .Study No. NWBS00-Q88 Report No. NWBR01-001 Run ID 6 7 8 9 10 11 PFOSA R esu lt Accepted Accepted Accepted Accepted Accepted Rejected 12 A ccepted 13 A ccepted 14 Accepted 15 Rejected 16 N /A 17 A ccepted M556 Result Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted N/A N/A Accepted M570 Result Accepted Accepted Accepted Accepted Accepted Accepted Accepted Accepted Rejected N/A Accepted Accepted C om m ents Standard curve failed for PFOSA. Reinjection o f Run 1 1 for PFOSAA only. Low QCs failed for M 570 Standard curve failed for PFOSA N/A = not analyzed Because o f the limited sample volume available, several samples in this study were analyzed at a dilution factor o f 2. High QC samples, diluted at a factor o f 2, were also analyzed in triplicate. METH00040 did not meet the validation acceptance criteria for analysis o f QC samples containing PFOSA or PFOSAA at concentrations above the ULOQ (analyzed after dilution). Samples containing PFOSA or PFOSAA at concentrations less than the ULOQ and analyzed after diluting with control matrix were not evaluated for accuracy and precision during method validation. PFOSA and PFOSAA accuracy and precision for the diluted high QC samples from 3 separate runs was determined to assess the validity o f diluting samples with Chinese plasma when samples have PFOSA or PFOSAA concentrations less than the ULOQ. (Refer to PFOSAA results in Runs 12, 13, and 16 and PFOSA results in Runs 12, 13, and 14.) Both intra- and inter-assay precision were <15% and intra- and inter-assay accuracy deviated <15% from target (data not shown). Therefore, the accuracy and precision obtained after diluting samples with Chinese plasma when samples have PFOSA or Page 15 030353 Northwest Bioanalytieal Study No. NWBS00-088 Report No. NWBR01-001 PFOSAA concentrations less than the ULOQ is acceptable and PFOSA and PFOSAA results from diluted samples will be reported. The lack o f dilution data prior to analysis o f diluted o f high QC samples did not affect the quality o f the assay or integrity of the PFOSA and PFOSAA data. Sample 230 was analyzed on Run 1 which had to be rejected for all analytes due to sample preparation error. There is insufficient sample for reanalysis. SOP Deviations Samples 2193 to 2363 and 2366 to 2500 were analyzed for PFOSA in Run 11 and Run 15. The standard curves did not meet the acceptance criteria in either run and therefore, PFOSA results were rejected. There was insufficient sample to reanalyze. Since the runs failed, no standard or QC data from the runs is included in this report. A ll subject PFO SA sample results obtained in Runs 11 and 15 were less than the LLOQ. The standard curve failed due to scatter and less than three-fourths o f the standards were w ithin the acceptance criteria. However, the mean o f the low QC results in the two runs ranged from 109.8 to 114.3% o f target and the LLOQ samples for run 15 deviated less than + 5% o f target. Since there is insufficient sample volume to repeat the analyses, the client has requested that the <LLOQ results be reported as conditional information. The criteria specified in the analytical plan for rejection o f calibration standards was not followed for the M 570 curve in run 12. Standard 1 , replicate 1 was deactivated as an outlier even though the % deviation from target was less than 2 times the acceptance criteria for that standard prior to deactivation. As a general practice, both LLOQs are deactivated if both LLOQ results are outside of the specified acceptance criteria. For this run, when both LLOQs were deactivated, the calculated concentration o f Std 1, replicate 1, deviated 61% from target and replicate 2 was 11% from target. This indicated that Std 1, repl 1 was a true outlier and Std 1, repl 2 was originally not fitting the curve because Std l, repl 1 was skewing the curve. When Page 16 03034 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Std 1, repl 2 is reactivated, it has a deviation o f 2% from target. Therefore, the regression will be accepted with only Std 1, repl 1 deactivated as an outlier. Since the regression is scientifically sound and acceptance criteria for the run are met, this deviation does not effect the quality o f the data or integrity o f the study. 5. REFERENCES 5.1. 3M Company Protocol EPI-0011. "Identification o f Fluorochemicals in Sera o f Children in the United States." March 16, 2000. 5.2. C. Sakashita. "Quantitative Determination ofPFO S, PFOSA, PFOSAA, POAA, PFHS, M556 and M570 in Human Serum by LC/MS/MS." Assay Revalidation Report. NWB Study NWBS00-040. NWB Report NW BR00-108. January 24, 2001. 5.3. C. Sakashita. "Quantitative Determination ofP FO S, PFOSA, PFOSAA, POAA, PFHS, M556 and M570 in Human Serum by LC/MS/MS." Assay Revalidation Addendum Report. NWB Study NWBS00-040. NWB Report NWBR00-122. November 20, 2001. 6. DATA RETENTION The raw data and final report for this study will be stored in the NWB Archives, 1121 East 3900 South, Salt Lake City, UT 84124 per regulations and contract agreement. After submission o f the final report to the Sponsor, remaining study samples will be stored under required conditions until confirmation of Sample Disposition/Retum Authorization is received from the Sponsor. 3M Company will be notified concerning final disposition o f records at completion o f contract obligations. Page 17 0Q035 Northwest Bioanulytical Study Nu. NWBS00-088 Report No. NWBROl-OOl Table 1. Calibration Curve Summary for PFOS Quadratic-weighted l/x:. All concentrations are expressed as ppb. Run Date 31-Oct-2000 01-Nov-2000 04-NOV-2000 06-NOV-2000 08-NOV-2000 09-NOV-2000 lO-Nov-2000 12-NOV-2000 13-NOV-2000 14-NOV-2000 15-NOV-2000 16-NOV-2000 18-NOV-2000 25-Mar-2001 Run Number 2 3 4 5 6 7 8 9 10 11 12 13 14 17 A B C R-Squared LLOQ ULOQ -0.000005 0.027791 0.010909 -0.000005 0.027419 0.006602 -0.000007 0.030558 0.012087 -0.000017 0.038499 0.015935 -0.000011 0.035306 0.007489 -0.000010 0.039703 0.010533 -0.000008 0.035218 0.033595 -0.000003 0.020611 0.020473 -0.000007 0.029955 0.022348 0.000005 0.026248 0.022175 -0.000005 0.041499 0.007161 -0.000003 0.036442 0.026638 -0.000006 0.034381 0.024135 -0.000001 0.008025 0.004145 0.9956 0.9990 0.9961 0.9953 0.9960 0.9894 0.9921 0.9912 0.9918 0.9791 0.9829 0.9820 0.9970 0.9969 3.94 3.94 3.94 3.94 3.94 3.94 3.94 3.94 3.94 3.94 5.17 3.94 3.94 3.94 414 414 414 414 414 414 414 414 414 414 414 414 414 414 Mean S.D. %CV n -0.000006 0.030833 0.016016 0.000005 0.008779 0.008935 -83.3 28.5 55.8 .14 14 14 0.9917 0.0063 0.6 14 A, B, and C are coefficients used to define the calibration curve. Page 18 03035 Northwest Biounalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 2. Calibration Curve Summary for PFOA Quadratic weighted l/x:. All concentrations are expressed as ppb. Run Date 31-Oct-2000 01-Nov-2000 04-NOV-2000 06-NOV-2000 08-NOV-2000 09-NOV-2000 lO-Nov-2000 12-NOV-2000 13-NOV-2000 14-NOV-2000 lS-Nov-2000 16-NOV-2000 18-NOV-2000 25-Mar-2001 Run Number 2 3 4 5 6 7 8 9 10 11 12 13 14 17 A B C R-Squared LLOQ ULOQ 0.000001 0.018750 0.001244 0.000002 0.018998 0.000186 0.000001 0.014032 0.001606 0.000000 0.014340 0.002050 -0.000001 0.014866 0.000095 -0.000002 0.014932 0.002985 0.000001 0.015103 0.009536 0.000001 0.010333 0.003017 0.000001 0.015660 0.002794 0.000008 0.013586 0.006940 0.000002 0.015457 0.005125 -0.000001 0.017638 0.007935 0.000000 0.020492 0.010441 0.000000 0.006597 0.002091 0.9967 0.9980 0.9945 0.9941 0.9971 0.9961 0.9941 0.9961 0.9936 0.9842 0.9903 0.9922 0.9921 0.9921 1.92 481 1.92 481 1.92 481 1.92 481 1.92 481 1.92 481 1.92 481 1.92 481 1.92 481 1.92 481 1.92 481 1.92 481 1.92 481 1.92 481 Mean S.D. %CV n 0.000001 0.000002 200.0 14 0.015056 0.003547 23.6 14 0.004003 0.003414 85.3 14 0.9937 0.0035 0.4 14 A, B, and C are coefficients used to define the calibration curve. Page 19 000357 Northwest Bioanalytieal Study No. NWBSOO-OS8 Report No. NWBROI-OOl Table 3. Calibration Curve Summary for PFHS Quadratic weighted llx 1. All concentrations are expressed as ppb. Run Date 31-Oct-2000 01-Nov-2000 04-NOV-2000 06-Nov-2000 O8-N0V-2OOO O9-N0V-2OOO 10-Nov-2000 I2-N0V-2OOO I3-N0V-2OOO I4-N0V-2OOO I5-N0V-2OOO I6-N0V-2OOO I8-N0V-2OOO 25-Mar-2001 Run Number 2 3 4 5 6 7 8 9 10 11 12 13 14 17 A B C R-Squared LLOQ ULOQ -0.000009 0.031737 0.006465 -0.000010 0.032478 0.009418 -0.000008 0.031233 0.014139 -0.000015 0.034135 0.015590 -0.000015 0.035218 0.009051 -0.000011 0.030154 0.011565 -0.000008 0.028971 0.027667 -0.000006 0.020349 0.010603 -0.000008 0.030472 0.025208 -0.000006 0.032776 0.025491 -0.000008 0.030669 0.025839 -0.000007 0.028744 0.027330 -0.000008 0.032203 0.024941 -0.000002 0.007658 0.007909 0.9976 0.9979 0.9965 0.9952 0.9964 0.9977 0.9946 0.9983 0.9979 0.9964 0.9887 0.9930 0.9922 0.9937 1.36 523 1.36 523 1.36 523 1.36 523 1.36 523 1.36 523 1.36 523 1.36 523 1.36 523 1.36 523 1.36 523 1.36 523 1.36 523 1.36 523 Mean S.D. %CV n -0.000009 0.029057 0.017230 0.000003 0.007075 0.008299 -33.3 24.3 48.2 14 14 14 0.9954 0.0028 0.3 14 A, B, and C are coefficients used to define the calibration curve. Page 20 GS0358 Northwest Bioanalytical Study No. NWBS00-088 Report No. NVVBR01-00I Table 4. Calibration Curve Summary for PFOSAA Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date 31-Oct-2000 01-Nov-2000 04-NOV-2000 O6-N0V-2OOO O8-N0V-2OOO O9-N0V-2OOO lO-Nov-2000 I2-N0V-2OOO I3-N0V-2OOO I4-N0V-2OOO I5-N0V-2OOO I6-N0V-2OOO 2O-N0V-2OOO 25-Mar-2001 Run Number 2 3 4 5 6 7 8 9 10 11 12 13 16 17 A B C R-Squared LLOQ ULOQ -0.000001 0.023946 -0.003099 0.000002 0.022379 0.004347 0.000000 0.016980 0.005491 0.000000 0.016621 0.003312 0.000000 0.018859 0.003795 0.000002 0.014599 0.003438 0.000004 0.017031 0.025660 0.000001 0.011371 0.000468 0.000004 0.019123 0.007920 0.000016 0.014974 0.016220 0.000004 0.012533 0.009564 0.000004 0.014478 0.010593 0.000003 0.020670 0.021239 0.000001 0.005029 0.010607 0.9952 0.9940 0.9840 0.9827 0.9939 0.9901 0.9812 0.9982 0.9937 0.9802 0.9810 0.9859 0.9927 0.9928 1.60 1.60 1.60 1.60 1.60 1.60 1.60 1.60 1.60 1.60 1.60 1.60 1.60 1.60 501 501 501 501 501 501 501 501 501 501 501 501 501 501 Mean S.D. %CV n 0.000003 0.000004 133.3 14 0.016328 0.004833 29.6 14 0.008540 0.007974 93.4 14 0.9890 0.0062 0.6 14 A, B, and C are coefficients used to define the calibration curve. Page 21 000359 Northwest Bioanalytieal Study Nu. NWBS00-088 Report No. NWBR1-001 Table 5. Calibration Curve Summary for PFOSA Quadratic weighted 1/x1. All concentrations are expressed as ppb. Run Date 31-Oct-2000 01-Nov-2000 04-Nov-2000 06-Nov-2000 08-Nov-2000 09-Nov-2000 10-Nov-2000 12-Nov-2000 13-Nov-2000 15-N o v -2 000 16-Nov-2000 18-Nov-2000 25-Mar-2001 Run Number 2 3 4 5 6 7 8 9 10 12 13 14 17 A B C R-Squared LLOQ ULOQ -0.000013 0.052859 0.003517 -0.000003 0.046250 0.010476 -0.000012 0.054175 0.011593 -0.000018 0.069706 0.019030 -0.000015 0.060806 0.009414 -0.000013 0.072938 0.011198 -0.000011 0.067435 0.045288 -0.000007 0.036838 0.013009 -0.000005 0.051854 0.018661 -0.000009 0.077880 0.003529 -0.000007 0.069240 0.029141 -0.000010 0.064050 0.019102 0.000000 0.015780 0.005386 0.9949 0.9961 0.9918 0.9964 0.9958 0.9921 0.9914 0.9930 0.9911 0.9855 0.9812 0.9945 0.9945 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 Mean S.D. %CV n -0.000009 0.056909 0.015334 0.000005 0.016948 0.011547 -55.6 29.8 75.3 13 13 13 0.9922 0.0044 0.4 13 A, B, and C are coefficients used to define the calibration curve. Page 22 0S03fcd Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR.01-001 Table 6. Calibration Curve Summary for IVI556 Quadratic weighted l/x:. All concentrations are expressed as ppb. Run Date 31-Oct-2000 01-Nov-2000 04-NOV-2000 O6-N0V-2OOO O8-N0V-2OOO O9-N0V-2OOO lO-Nov-2000 I2-N0V-2OOO I3-N0V-2OOO I4-N0V-2OOO I5-N0V-2OOO I6-N0V-2OOO I8-N0V-2OOO 25-Mar-2001 Run Number 2 3 4 5 6 7 8 9 10 11 12 13 14 17 A B C R-Squared LLOQ ULOQ -0.000001 0.018373 0.001923 0.000002 0.017583 0.005331 0.000002 0.007944 0.003887 0.000001 0.007717 0.004452 0.000002 0.009283 0.002596 0.000002 0.007610 0.002860 0.000002 0.008464 0.004466 0.000002 0.006106 0.003591 0.000003 0.008526 0.004733 0.000007 0.007051 0.006423 0.000003 0.006747 0.003029 0.000002 0.006485 0.002510 0.000002 0.008566 0.004178 0.000001 0.002650 0.001081 0.9972 0.9972 0.9903 0.9822 0.9949 0.9985 0.9975 0.9968 0.9962 0.9867 0.9911 0.9936 0.9942 0.9955 2.50 2.50 2.50 2.50 2.50 2.50 2.50 2.50 2.50 2.50 2.50 2.50 2.50 2.50 500 500 500 500 500 500 500 500 500 500 500 500 500 500 Mean S.D. %CV n 0.000002 0.000002 100.0 14 0.008793 0.003647 0.004209 0.001423 47.9 39.0 14 14 0.9937 0.0047 0.5 14 A, B, and C are coefficients used to define the calibration curve. Page 23 0005& Northwest Bioanalytieal Study No. NWBS00-088 Report No. NWBROl-OOl Table 7. Calibration Curve Summary for V1570 Quadratic weighted t/x3. All concentrations are expressed as ppb. Run Date 31-Oct-2000 01-Nov-2000 04-NOV-2000 06-NOV-2000 08-NOV-2000 09-NOV-2000 10-Nov-2000 12-NOV-2000 13-Nov-2000 14-NOV-2000 lS-Nov-2000 l-Nov-2000 20-NOV-2000 25-Mar-2001 Run Number 2 3 4 5 6 7 8 9 10 11 12 13 16. 17 A B C R-Squared LLOQ ULOQ -0.000006 0.038561 0.012040 -0.000001 0.036248 0.019154 -0.000002 0.027976 0.012726 -0.000002 0.026862 0.016535 0.000000 0.030532 0.016991 0.000001 0.024223 0.014409 0.000002 0.028172 0.063424 -0.000002 0.018677 0.009480 0.000002 0.030589 0.027413 0.000020 0.025065 0.030430 0.000003 0.021180 0.014447 0.000006 0.022590 0.034515 0.000000 0.033466 0.044312 0.000000 0.002606 0.003896 0.9924 0.9952 0.9860 0.9908 0.9961 0.9863 0.9950 0.9951 0.9938 0.9807 0.9847 0.9802 0.9914 0.9929 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 1.00 500 Mean S.D. %CV n 0.000002 0.000006 300.0 14 0.026196 0.022841 0.008809 0.015953 33.6 69.8 14 14 0.9900 0.0055 0.6 14 A, B, and C are coefficients used to define the calibration curve. Page 24 000362 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 8. Back-Calculated Concentrations of Calibration Standards for PFOS Quadratic weighted 1/x2. All concentrations are expressed as ppb. Run Date 31 -O ct-2000 01 -N ov-2000 04-NOV-2000 06-NOV-2000 08-NOV-2000 09-NOV-2000 10-Nov-2000 12-NOV-2000 13-NOV-2000 14-Nov-2000 15-Nov-2000 16-NOV-2000 Run Number 2 3 4 5 6 7 8 9 10 11 12 13 3.94 5.17 11.3 23.6 44.2 85.4 209 332 414 3.65 4.10 4.00 3.94 4.16 3.70 3.97 3.83 3.96 3.69 4.26 3.56 4.57 **7.53 3.67 4.53 3.84 3.76 4.56 3.26 f4.93 f3.23 3.31 4.83 5.67 12.0 23.4 45.0 84.2 224 347 424 4.90 10.7 23.3 42.3 84.5 203 345 368 5.15 11.4 23.7 46.7 84.5 198 329 422 5.04 11.4 23.9 43.4 83.6 207 351 405 5.31 10.5 21.2 44.9 83.7 205 340 411 5.05 12.6 24.1 45.7 86.9 213 332 409 5.37 12.4 25.7 45.3 82.8 203 352 428 4.96 10.7 23.2 43.5 77.3 *116 * 399 5.74 11.1 25.6 44.5 87.0 215 350 436 5.02 11.3 22.8 42.9 81.8 193 333 386 5.56 12.2 26.7 46.7 89.3 227 357 433 4.85 10.3 22.2 40.9 77.1 184 338 376 4.83 11.9 24.8 47.0 86.6 212 353 418 4.35 11.0 22.5 41.1 87.8 207 325 390 5.25 12.0 25.1 49.0 89.1 220 339 443 4.57 10.2 23.0 42.0 79.6 195 321 392 6.11 12.3 24.2 45.1 85.5 222 344 401 4.53 11.3 24.0 40.4 75.9 208 332 413 5.74 11.8 26.3 50.7 90.5 **95.5 354 401 4.83 9.79 21.9 **28.5 64.6 210 354 391 5.81 10.8 25.9 47.0 96.6 245 374 456 4.86 10.1 20.9 43.6 77.6 184 294 354 4.34 10.3 22.6 43.8 75.1 201 313 391 5.52 12.0 26.2 50.4 79.5 233 330 452 * Sample deactivated due to preparation error ** Sample deactivated as an outlier t LLOQ failed Page 25 000363 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Table 8. Back-Calculated Concentrations of Calibration Standards for PFOS (Continued) Quadratic weighted t/x2. All concentrations are expressed as ppb. Run Date 18-NOV-2000 Run Number 14 25-Mar-2001 17 3.94 5.17 11.3 23.6 44.2 85.4 209 332 414 3.88 5.45 11.0 23.1 44.6 83.3 206 357 388 4.03 4.71 12.3 24.2 42.4 85.9 208 333 422 3.98 4.71 11.1 25.5 44.7 81.6 211 344 423 4.26 .4.93 11.4 24.0 44.7 82.6 202 344 390 Mean S.D. %CV %Bias n 3.97 5.11 11.3 23.9 44.8 83.0 209 340 408 0.383 0.461 0.784 1.55 2.63 6.03 13.9 16.0 24.6 9.6 9.0 6.9 6.5 5.9 7.3 6.7 4.7 6.0 0.8 -1.2 0.0 1.3 1.4 -2.8 0.0 2.4 -1.4 25 28 28 28 27 28 26 27 28 Page 26 000364 Northwest Bioaiialytical Study No. NWBS00-088 Report No. NWBRI-001 Table 9. Back-Calculated Concentrations of Calibration Standards for PFOA Quadratic weighted l/x:. All concentrations are expressed as ppb. Run Date Run N um ber 1.92 3.36 10.6 25.0 49.0 97.1 241 385 481 3 1 -O ct-2000 2 01-Nov-2000 3 04-Nov-2000 4 06-NOV-2000 5 08-NOV-2000 6 09-NOV-2000 7 I0-Nov-2000 8 I2-N 0 V-2OOO 9 I3-N 0 V-2OOO 10 I4-N 0V-2OOO 11 I5-N 0V-2 OOO 12 I6-N 0 V-2OOO 13 1.94 1.88 1.85 1.94 2.05 1.80 1.89 1.92 2.03 1.98 2.17 1.77 2.17 **6.15 2.02 **3.54 2.22 1.77 2.30 1.59 2.28 1.70 1.82 2.22 3.49 3.36 3.30 3.64 3.27 3.49 3.14 3.63 3.22 3.03 3.06 3.34 2.75 3.22 3.53 2.92 3.19 2.97 3.92 2.72 3.16 3.22 3.28 2.81 9.80 24.9 47.2 89.3 250 383 470 10.7 26.6 49.5 99.2 247 427 443 10.0 24.0 51.6 98.9 227 381 472 10.5 25.7 48.7 95.3 249 406 478 9.53 21.4 49.2 90.5 245 385 456 11.0 27.9 51.0 102 253 398 478 10.6 25.0 47.0 84.0 234 374 482 10.5 27.3 55.5 92.8 *164 * ' 509 9.85 27.5 49.6 97.8 253 382 481 10.3 25.1 50.8 95.0 237 387 471 10.4 25.8 49.2 92.7 244 394 501 10.8 25.6 50.2 95.0 243 399 437 9.73 26.1 49.5 95.4 238 386 484 11.2 24.5 50.9 103 255 378 467 11.0 23.9 51.0 94.5 235 365 477 10.0 24.3 52.3 99.6 251 416 467 10.8 26.1 52.2 93.0 249 412 463 10.6 27.2 47.1 87.0 242 386 473 10.6 27.2 53.6 96.8 **57.3 381 445 9.75 24.0 **15.4 83.8 258 418 482 9.24 25.1 49.5 90.5 233 339 494 10.7 25.3 56.9 102 246 415 480 10.4 27.0 51.3 96.7 233 372 466 10.3 26.0 52.9 86.4 253 369 523 * Sample deactivated due to preparation error ** Sample deactivated as an outlier Page 27 000365 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBR01-00I Table 9. Back-Calculated Concentrations of Calibration Standards for PFOA (Continued) Quadratic weighted I/x1. All concentrations are expressed as ppb. Run Date Run Number 1.92 3.36 10.6 25.0 49.0 97.1 241 385 481 18-NOV-2000 14 1.77 3.29 9.90 25.1 48.7 96.5 243 404 441 2.20 2.90 12.5 25.6 46.1 93.9 248 398 486 25-Mar-2001 17 1.85 2.67 10.4 27.1 49.4 95.5 234 395 474 2.26 3.15 10.9 25.9 50.4 94.2 241 416 455 Mean S.D. %CV %Bias n 41*. oo 1.98 3.20 10.4 25.6 50.4 94.3 244 391 473 0.199 0.298 0.634 1.40 2.47 5.07 8.09 19.6 19.7 10.1 9.3 6.1 5.5 4.9 5.4 3.3 5.0 4.2 3.1 -1.9 2.4 2.9 -2.9 1.2 1.6 -1.7 26 28 28 28 27 28 26 27 28 Page 28 00036o Northwest Bioatialytical Study No. NWBSOO-88 Report No. NWBR01-001 Table 10. Back-Calculated Concentrations of Calibration Standards for PFHS Quadratic weighted l/x \ All concentrations are expressed as ppb. Run Date Run N um ber 1.36 2.92 10.7 26.5 52.6 104 262 418 523 31-Oct-2000 0 1 -N ov-2000 04-NOV-2000 06-NOV-2000 O8-N 0V-2OOO O9-N 0 V-2 OOO IO-N0 V-2OOO I 2 -N 0V-2 OOO I3-N 0 V-2 OOO I4-N 0V-2 OOO I5-N 0 V-2 OOO 16-NOV-2000 2 3 4 5 6 7 8 9 10 11 12 13 1.30 3.01 1.42 2.77 1.36 2.73 1.35 3.12 1.43 3.08 1.31 2.67 1.40 2.86 1.36 2.72 1.44 2.85 1.24 3.16 1.44 2.80 1.26 3.05 1.51 2.37 **5.46 2.69 1.35 2.88 **3.07 2.97 1.35 2.85 1.41 2.73 1.45 2.61 1.32 2.95 1.55 2.74 1.30 2.47 1.23 2.66 1.59 2.64 11.2 26.0 49.7 98.7 268 419 530 11.2 27.4 52.0 102 266 455 478 11.2 25.8 51.1 104 238 417 513 10.6 27.1 55.7 100. 268 442 532 9.86 28.5 51.2 96.4 247 432 513 10.7 28.7 53.1 106 271 424 524 11.0 26.6 51.5 87.1 252 431 515 11.5 28.8 55.5 102 *167 * 554 11.4 28.3 52.4 101 260 425 547 10.1 25.7 53.8 96.3 247 430 516 11.2 26.8 51.9 101 256 . 409 518 11.0 26.4 52.3 101 251 468 515 10.9 26.4 53.1 103 250 413 537 11.1 28.1 54.0 107 272 413 515 10.6 25.4 51.4 96.8 256 391 529 10.9 28.3 55.3 103 270 439 530 11.1 26.4 52.5 102 262 432 520 11.3 27.9 48.8 99.6 273 434 492 10.7 27.4 50.4 104 **79.3 416 488 10.8 28.0 **23.7 101 269 469 503 11.4 29.4 55.4 120 276 475 561 10.2 25.4 51.9 91.9 237 370 482 11.2 27.3 55.1 104 270 407 521 10.8 27.3 56.3 89.6 255 420 542 * Sample deactivated due to preparation error ** Sample deactivated as an outlier Page 29 000367 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBRO1-001 Table 10. Back-Calculated Concentrations of Calibration Standards for PFHS (Continued) Quadratic weighted l/x~. All concentrations are expressed as ppb. Run Date Run Number 1.36 2.92 10.7 26.5 52.6 104 262 418 523 18-NOV-2000 14 1.26 2.98 10.1 26.3 53.8 97.8 264 428 534 1.48 2.61 13.3 26.6 50.3 99.7 253 407 534 25-Mar-2001 17 1.39 2.46 10.4 28.0 55.4 103 277 440 521 1.52 2.52 10.6 27.5 55.3 103 258 427 474 Mean S.D. %CV %Bias n 1.39 2.78 10.9 27.2 52.9 101 260 427 519 0.0963 0.208 0.631 1.09 2.07 5.94 11.2 22.9 21.7 6.9 7.5 5.8 4.0 3.9 5.9 4.3 5.4 4.2 o1 bo 2.2 -4.8 1.9 2.6 0.6 -2.9 2.2 -0.8 26 28 28 28 27 28 26 27 28 Page 30 0SG3GS Northwest ioanalytical Study No. NWBS00-088 Report No. NWBROl-OOl Table 11. Back-Calculated Concentrations of Calibration Standards for PFOSAA Quadratic weighted l/x:. All concentrations are expressed as ppb. Run Date Run N um ber 1.60 3.10 10.6 25.6 50.6 101 251 401 501 31 -Oct-2000 2 01-Nov-2000 3 04-NOV-2000 4 06-Nov-2000 5 08-NOV-2000 6 09-NOV-2000 7 10-Nov-2000 8 I 2-N 0V-2OOO 9 13-N o v -2 0 0 0 10 I4 -N 0 V-2OOO 11 I5-N 0 V-2OOO 12 I 6-N 0 V-2OOO 13 2 O-N0 V-2OOO 16 1.41 1.68 1.66 1.54 1.58 1.56 1.24 1.94 1.52 1.72 1.46 1.71 1.98 **8.58 1.61 **2.67 1.59 1.60 1.54 1.53 1.85 1.40 1.72 **5.99 1.52 1.72 3.26 10.7 24.0 48.1 94.6 271 394 487 3.36 10.9 25.4 48.1 106 261 433 467 2.85 9.40 25.1 55.4 97.5 248 375 495 3.50 9.99 26.9 48.8 107 261 443 481 3.53 8.37 19.1 50.2 94.5 243 392 461 3.00 12.0 28.9 54.9 107 285 429 496 2.77 10.1 23.3 45.8 95.8 242 379 494 3.56 10.4 27.7 55.2 115 *186 * 532 2.88 8.73 26.6 47.4 96.4 257 432 501 3.23 11.7 26.7 51,7 106 255. 392 468 2.84 9.64 24.8 45.8 90.1 260 389 449 3.48 11.5 27.8 53.0 102 253 472 495 2.13 9.82 25.8 54.7 98.0 253 403 463 2.70 10.6 24.6 50.3 122 289 396 489 3.09 10.1 24.6 50.3 99.6 250 376 487 3.15 10.2 27.0 51.5 104 269 420 504 3.22 11.1 24.2 50.2 98.0 275 402 424 2.96 11.2 26.3 44.9 99.5 264 403 549 3.40 9.75 28.5 59.2 105 **138 391 445 3.39 9.65 26.4 37.1 82.5 284 447 507 2.88 7.98 22.3 44.4 99.5 270 364 465 3.33 10.9 25.3 62.0 113 284 437 483 2.88 11.9 '28.4 56.9 93.4 282 419 502 2.81. 9.59 25.7 48.4 80.6 281 336 506 3.14 9.31 23.8 47.1 98.1 253 413 447 2.88 12.4 27.4 48.8 107 267 407 520 * Sample deactivated due to preparation error ** Sample deactivated as an outlier Page 31 000369 Northwest Biuanajytical Study No. NWBSOO-088 Report No. NWBR01-00I Table 11. Back-Calculated Concentrations of Calibration Standards for PFOSAA (Continued) Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date Run Number ' 25-Mar-2001 17 1.60 1.67 1.71 3.10 10.6 25.6 50.6 101 251 401 501 2.93 10.8 29.8 52.5 103 255 420 500 2.54 10.5 24.2 49.1 94.5 249 429 456 Mean S.D. %CV %Bias n 1.62 0.164 10.1 1.3 25 3.06 10.3 25.7 50.4 100 0.333 1.08 2.24 5.03 8.84 10.9 10.5 8.7 10.0 8.8 -1.3 -2.8 0.4 -0.4 - 1.0 28 28 28 28 28 264 407 485 14.0 29.0 27.9 5.3 7.1 5.8 5.2 1.5 -3.2 26 27 28 Page 32 000370 Northwest Bioanalytical Study Nu. NWBS00-088 Report No. NVVBRl-001 Table 12. Back-Calculated Concentrations of Calibration Standards for PFOSA Quadratic weighted l/x \ All concentrations are expressed as ppb. Run Date Run Number 1.00 2.50 10.0 25.0 50.0 too 250 400 500 31-Oct-2000 2 0.930 2.62 9.96 25.7 52.8 101 289 438 529 1.06 2.48 9.45 24.1 47.2 100 229 362 453 01-Nov-2000 3 0.913 2.40 8.86 25.1 52.1 99.1 238 380 497 1.10 2.56 9.78 26.7 50.4 104 255 432 491 04-Nov-2000 4 1.00 2.64 9.23 19.1 51.8 101 248 386 494 0.998 2.33 11.5 26.1 53.7 105 241 399 525 06-Nov-2000 5 0.934 2.63 10.1 26.9 48.7 104 248 395 521 1.03 2.60 9.67 25.7 48.4 86.1 *138 * 499 O8-N0V-2OOO 6 0.992 2.63 8.92 28.0 49.4 104 261 413 545 0.985 2.57 9.69 26.0 46.9 97.0 235 368 482 O9-N0V-2OOO 7 1.04 2.71 10.4 28.9 50.5 105 271 444 521 0.945 2.38 8.88 24.5 47.2 91.4 215 394 461 lO-Nov-2000 8 1.12 2.15 10.7 27.9 52.5 103 259 424 522 **1.67 2.04 10.1 23.6 .47.1 105 252 366 467 I2-N0V-2OOO 9 0.979 2.58 11.4 25.8 56.6 107 251 422 541 1.00 2.53 9.14 22.1 45.8 91.7 232 385 473 13-Nov-2000 10 1.12 2.81 10.8 26.6 53.1 98.2 258 426 477 0.850 2.32 9.74 25.9 43.7 85.7 245 390 521 I5-N0V-2OOO 12 **1.61 3.03 8.79 26.1 50.1 114 294 416 544 0.921 2.62 8.99 21.3 52.4 91.2 232 388 422 I6-N0V-2OOO 13 0.788 2.06 . 8.94 24.4 47.6 86.3 234 385 479 1.22 2.85 10.8 29.0 54.2 95.7 286 382 547 I8-N0V-2OOO 14 0.965 2.39 10.0 24.9 47.2 102 240 466 438 1.04 2.59 10.2 27.5 45.2 95.6 276 392 495 * Sample deactivated due to preparation error ** Sample deactivated as an outlier Page 33 030371 Northwest Bioanulytical Study No. NWBS00-088 Report No. NWBROl-OOl Table 12. Back-Calculated Concentrations of Calibration Standards for PFOSA (Continued) Quadratic weighted l/x \ All concentrations are expressed as ppb. Run Date Run Number 1.00 2.50 10.0 25.0 50.0 100 250 400 500 25-Mar-2001 17 0.900 2.36 10.3 28.0 48.3 101 236 410 505 1.14 2.30 10.3 25.8 48.4 95.1 241 432 479 Mean S.D. %CV %Bias n 0.999 2.51 9.87 25.6 49.7 98.8 251 404 497 0.0978 0.232 0.781 2.28 3.14 7.01 20.0 26.7 33.7 9.8 9.2 7.9 8.9 6.3 7.1 8.0 6.6 6.8 -0.1 0.4 -1.3 2.4 -0.6 -1.2 0.4 1.0 -0.6 24 26 26 26 26 26 25 25 26 h Page 34 0003V2 Northwest Bioanalyticai Study No. NWBSOO-088 Report No. NWBROl-OQl Table 13, Back-Calculated Concentrations of Calibration Standards for M556 Quadratic weighted l/x:. All concentrations are expressed as ppb. Run Date Run Number 2.50 10.0 25.0 50.0 100 250 400 500 31-Oct-2000 2 2.33 9.67 24.3 51.9 95.2 255 388 499 2.70 9.81 25.8 49.3 104 249 438 470 01-Nov-2000 3 2.55 9.86 25.9 55.5 107 246 403 505 2.48 9.52 23.6 47.4 96.2 241 421 478 04-NOV-2000 4 2.38 8.49 19.4 53.2 96.1 248 388 485 2.63 11.8 26.4 52.2 104 263 416 500 O6-N0V-2OOO 5 2.02 8.91 22.7 46.0 86.0 235 385 49,2 2.98 10.7 28.8 58.2 107 *200 * 538 O8-N0V-2OOO 6 2.28 8.40 26.1 46.3 98.1 255 413 494 2.75 11.0 25.7 51.4 102 250 409 481 O9-N0V-2OOO 7 2.51 9.73 25.7 49.3 95.5 253 400 488 2.50 9.91 25.5 51.8 100 238 432 490 lO-Nov-2000 8 2.37 9.94 23.7 47.6 97.9 244 402 487 2.63 10.3 24.0 50.9 109 271 394 500 I2-N0V-2OOO 9 2.61 9.22 23.4 50.6 97.8 233 376 499 2.43 9.95 26.7 51.0 107 264 421 502 I3-N0V-2OOO 10 2.52 10.3 25.5 52.3 96.5 261 429 458 2.43 10.4 26.0 46.8 88.5 248 403 516 I4-N0V-2OOO 11 2.77 9.58 27.2 57.3 103 **127 392 453 2.33 8.48 24.2 **33.4 81.4 272 439 505 I5-N0V-2OOO 12 2.46 8.06 22.9 46.3 105 276 388 483 2.66 10.1 23.9 57.7 104 260 427 464 16-Nov-2000 13 2.70 10.0 27.2 53.3 92.8 255 414 499 2.32 9.10 25.3 52.2 87.3 271 359 513 I8-N0V-2OOO 14 2.69 9.91 23.3 48.0 96.4 242 434 454 2.25 11.4 26.6 48.1 97.0 256 420 503 * Sample deactivated due to preparation error ** Sample deactivated as an outlier Page 35 000373 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRl-001 Table 13. Back-Calculated Concentrations of Calibration Standards for M556 (Continued) Quadratic weighted l/x2. All concentrations are expressed as ppb. Run Date Run Number 2.50 10.0 25.0 50.0 100 250 400 500 25-Mar-2001 17 2.71 10.1 27.4 51.0 99.1 247 420 507 2.26 10.4 23.7 47.9 94.0 240 431 460 Mean S.D. %CV %Bias n 2.51 9.82 25.0 0.205 0.872 1.90 8.2 8.9 7.6 0.4 -1.8 0.0 28 28 28 50.9 ' 98.1 3.49 6.83 6.9 7.0 1.8 -1.9 27 28 253 409 490 11.9 20.5 20.2 4.7 5.0 4.1 1.2 . 2.3 -2.0 26 27 28 Page 36 i 000374 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBROl-OOl Table 14. Back-Calculated Concentrations of Calibration Standards for M570 Quadratic weighted t/x1. All concentrations are expressed as ppb. Run Date Run Number 1.00 2.50 10.0 25.0 50.0 100 250 400 500 31 -Oct-2000 2 01828 2.29 10.1 23.6 48.1 93.7 262 392 . 486 1.18 2.66 9.94 25.9 50.6 109 252 431 475 01-Nov-2000 3 1.07 2.22 9.01 25.2 54.1 100 239 383 485 0.992 2.43 9.48 27.2 50.1 106 259 441 482 04-NOV-2000 4 0.974 2.74 8.15 18.7 49.4 96.4 239 389 466 1.02 2.29 11.8 28.0 55.0 105 269 427 506 06-NOV-2000 5 0.930 2.09 9.52 23.9 44.9 97.3 234 384 486 1.10 2.75 10.3 26.6 56.0 110 *183 * 538 08-NOV-2000 6 0.952 2.50 8.31 25.8 49.0 100 251 404 496 1.08 2.35 10.6 25.7 51.9 107 249 404 488 09-NOV-2000 7 0.805 2.08 9.40 24.8 45.9 94.4 247 392 452 1.23 2.66 10.6 27.0 53.8 105 246 463 499 lO-Nov-2000 8 1.01 **0.653 9.16 24.3 52.0 98.0 240 403 468 **6.51 **1.29 9.43 23.5 50.3 118 276 402 498 I2-N0V-2OOO 9 0.964 2.40 9.29 23.1 48.8 96.7 235 375 482 **1.93 2.89 9.84 25.7 53.4 105 264 432 510 13-Nov-2000 10 1.05 2.33 10.7 24.0 50.3 100 258 407 437 1.03 2.13 10.9 27.1 45.7 98.2 258 401 543 I4-N0V-2OOO 11 1.10 2.78 9.29 26.7 57.0 104 **133 399 440 0.813 2.87 9.11 25.9 37.9 81.5 276 444 508 I5-N0V-2OOO 12 **1.53 2.39 7.28 22.1 45.2 101 259 369 457 1.02 2.62 10.3 25.2 62.8 112 269 439 495 I6-N0V-2OOO 13 1.16 1.93 10.8 28.4 57.9 100 276 422 497 1.03 1.83 9.19 26.1 52.0 83.4 275 340 495 2O-N0V-2OOO 16 0.933 2.61 9.04 24.1 46.9 96.9 241 ' 423 449 1.10 2.13 12.0 26.1 48.4 107 260 404 523 * Sample deactivated due to preparation error ** Sample deactivated as an outlier Page 37 000375 Northwest Oioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 14. Back-Calculated Concentrations of Calibration Standards for M570 (Continued) Quadratic weighted l/x \ All concentrations are expressed as ppb. Run Date Run Number 25-Mar-2001 17 1.00 1.03 1.05 2.50 1.98 **1.64 10.0 25.0 50.0 100 9.84 29.0 52.3 102 10.0 24.8 50.4 90.5 250 252 241 400 500 424 508 419 458 Mean S.D. %CV %Bias n 1.02 0.106 10.4 2.0 25 2.40 0.304 12.7 -4.0 25 9.76 25.3 50.7 101 1.03 2.09 4.84 7.92 10.6 8.3 9.5 7.8 -2.4 1.2 1.4 1.0 28 28 28 28 255 408 487 13.4 26.4 26.9 5.3 6.5 5.5 2.0 2.0 -2.6 26 27 28 Page 38 0S0S7 Northwest Bioaiialytical Study No. NWBSOO-088 Report No. NWBR0I-001 Table 15. Analytical QC Summary for PFOS All concentrations are expressed as ppb. Run Date Run Number 31-Oct-2000 2 01-Nov-2000 3 04-NOV-2000 4 06-NOV-2000 5 08-NOV-2000 6 09-NOV-2000 7 10-Nov-2000 8 12-NOV-2000 9 13-NOV-2000 10 14-NOV-2000 11 15-NOV-2000 12 Low QC 6.40 ppb 6.62 6.18 . 6.79 7.16 6.57 6.63 6.03 5.30 6.70 5.98 6.00 5.96 6.36 6.38 6.18 6.31 6.71 6.38 5.31 6.73 6.50 5.84 M edium QC High QC 126 ppb 332 ppb 129 135 125 124 131 130 105 122 147 128 137 108 136 134 132 127 139 136 136 133 141 103 323 322 369 354 314 322 291 283 343 320 302 293 323 318 299 304 327 312 322 294 ' 319 330 Dilution QC 335 ppb DF=2 320 323 350 Page 39 00377 Northwest Biounalytical Study No. NWBSOO-088 Report No. NWBR01-001 Table 15. Analytical QC Summary for PFOS (Continued) All concentrations are expressed as ppb. Run Date Run Number 16-NOV-2000 13 18-Nov-2000 14 25-Mar-2001 17 Low QC 6.40 ppb 6.65 5.98 5.87 6.06 6.26 5.95 M edium QC 126 ppb High QC 332 ppb Dilution QC 335 ppb DF=2 126 297 307 129 319 312 359 130 338 335 126 . 336 342 345 137 367 335 135 349 338 471 Mean S.D. %CV %Theoretical %Bias n 6.26 129 321 345 0.430 10.1 22.1 42.6 6.9 7.8 6.9 12.3 97.8 102.4 96.7 103.0 -2.2 2.4 -3.3 3.0 28 28 28 12 Page 40 000378 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBROl-OOl Table 16. Analytical QC Summary for PFOA All concentrations are expressed as ppb. Run Date Run Number 31-Oct-2000 2 01-Nov-2000 3 04-NOV-2000 4 06-NOV-2000 5 08-NOV-2000 6 09-NOV-2000 7 10-Nov-2000 8 12-NOV-2000 9 13-NOV-2000 10 14-NOV-2000 11 15-NOV-2000 12 16-NOV-2000 13 Low QC 4.81 ppb 4.87 4.90 4.78 4.68 5.51 5.09 4.45 5.10 4.81 4.18 4.22 4.15 4.23 4.66 4.72 5.45 5.05 4.80 4.19 4.67 4.09 4.50 4.43 4.65 Medium QC 145 ppb 156 147 144 144 149 159 140 147 154 159 147 130 154 160 151 150 159 158 153 155 158 127 143 160 High QC 385 ppb 399 380 396 408 384 383 342 368 423 388 369 356 375 385 382 353 391 353 371 371 419 422 420 421 Dilution QC 386 ppb DF=2 396 425 406 388 391 402 Page 41 OSOS #'9 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBROl-OOl Table 16. Analytical QC Summary for PFOA (Continued) All concentrations are expressed as ppb. Run Date Run Number 18-NOV-2000 14 25-Mar-2001 17 Low QC 4.81 ppb 3.92 3.90 4.28 4.06 M edium QC 145 ppb 147 151 163 159 High QC 385 ppb 386 394 412 422 Dilution QC 386 ppb DF=2 392 416 381 404 401 449 Mean S.D. %CV %Theoretical %Bias n 4.58 0.432 9.4 95.2 -4.8 28 151 8.80 5.8 104.1 4.1 28 388 23.6 6.1 100.8 0.8 28 404 18.6 4.6 104.7 4.7 12 Page 42 000380 Northwest Bioanalyfical Study No. NWBS00-088 Report No. NWBR0I-001 Table 17. Analytical QC Summary for PFHS All concentrations are expressed as ppb. Run Date Run Low QC N um ber 4.48 ppb 31-Oct-2000 2 01-Nov-2000 3 04-NOV-2000 4 06-NOV-2000 5 08-NOV-2000 6 09-NOV-2000 7 10-Nov-2000 8 12-NOV-2000 9 13-NOV-2000 10 14-NOV-2000 11 15-NOV-2000 12 4.35 4.60 4.34 4.44 4.37 4.40 4.10 4.14 3.99 3.89 4.09 4.67 3.76 4.00 3.99 4.57 4.32 4.15 4.08 3.80 4.06 3.84 16-NOV-2000 13 3.63 4.12 Medium QC 156 ppb 160 151 144 146 163 160 144 150 157 157 154 134 162 158 154 166 171 158 167 155 164 150 146 167 High QC 417 ppb 403 400 420 432 404 409 364 386 404 413 371 397 408 404 391 410 404 435 385 396 373 400 401 396 Dilution QC 418 ppb D F -2 367 365 378 418 431 401 Page 43 000381 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBROl-OOl Table 17. Analytical QC Summary for PFHS (Continued) All concentrations are expressed as ppb. Run Date Run Low QC N um ber 4.48 ppb I8-N0V-2OOO 14 3.74 3.85 25-Mar-2001 17 3.85 3.72 M edium QC High QC 156 ppb 417 ppb 155 : 454 148 397 153 448 153 427 Dilution QC 418 ppb DF=2 391 401 414 390 403 449 Mean S.D. % cv %Theoretical %Bias n 4.10 0.287 7.0 91.5 -8.5 28 155 8.40 5.4 99.4 -0.6 28 405 21.0 . 5.2 97.1 -2.9 28 401 25.0 6.2 95.9 -4.1 12 Page 44 000382 Northwest Bioanalytieal Study No. NVVBSO-088 Report No. NWBROI-OOl Table 18. Analytical QC Summary lor PFOSAA All concentrations are expressed as ppb. Run Date Run Number 31-Oct-2000 2 01-Nov-2000 3 04-N o v -2 000 4 06-NOV-2000 5 08-NOV-2000 6 09-NOV-2000 7 10-Nov-2000 8 12-NOV-2000 9 13-NOV-2000 10 14-NOV-2000 11 15-N o v -2 0 0 0 12 16-NOV-2000 13 Low QC 4.60 ppb 4.43 4.03 *5.84 5.21 4.26 4.10 3.77 4.18 5.22 4.35 3.50 3.93 4.23 4.55 4.15 5.55 5.24 5.06 3.71 4.52 *3.39 3.70 4.10 4.15 M edium QC 151 ppb 160 157 150 172 151 162 136 138 176 157 153 128 163 181 153 172. 151 172 168 150 158 116 137 157 High QC 401 ppb 393 394 485 488 391 388 366 356 443 434 359 409 415 430 380 389 415 323 399 371 451 427 419 412 Dilution QC 401 ppb DF=2 419 491 422 401 399 424 * > 2 5 % deviation from theoretical Page 45 G383 Northwest Bioanalytical Study No. NWDSOO-088 Report No. NWBROl-OOl Table 18. Analytical QC Summary for PFOSAA (Continued) All concentrations are expressed as ppb. Run Date Run Number 20-NOV-2000 16 2 5-M a r-2 001 17 Low QC 4.60 ppb 3.81 *3.24 4.86 3.72 Medium QC 15.1 ppb High QC 401 ppb Dilution QC 401 ppb DF=2 164 361 411 155 472 414 397 173 429 426 173 420 422 *634 Mean S.D. %CV %Theoretical %Bias n 4.31 0.667 15.5 93.7 -6.3 28 157 15.3 9.7 104.0 4.0 28 408 39.4 9.7 101.7 1.7 28 * > 2 5 % deviation from theoretical 438 66.3 15.1 109.2 9.2 12 Page 46 0S0384 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBROl-OOl Table 19. Analytical QC Summary for PFOSA All concentrations are expressed as ppb. Run Date Run Low QC N um ber 4.00 ppb 31 -Oct-2000 2 01-Nov-2000 j 04-Nov-2000 4 06-Nov-2000 5 08-Nov-2000 6 09-Nov-2000 7 10-Nov-2000 8 12-Nov-2000 9 13-Nov-2000 10 I5-Nov-2000 12 / 3.74 4.10 4.72 *5.03 4.16 4.04 3.66 3.49 4.75 4.15 4.05 3.70 4.38 4.58 4.65 4.20 4.76 4.74 4.27 3.88 16-Nov-2000 13 4.54 3.72 Medium QC 150 ppb 154 158 151 161 147 158 127 155 183 145 164 126 166 164 163 153 172 172 171 *111 150 149 High QC 400 ppb 423 412 488 471 401 433 357 342 462 423 371 350 419 412 363 363 422 357 432 443 369 391 Dilution QC 400 ppb DF=2 421 455 475 350 360 453 * > 25% deviation from theoretical Page 47 000383 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBR01-001 Table 19. Analytical QC Summary lor PFOSA (Continued) All concentrations are expressed as ppb. Run Date Run Low QC N um ber 4.00 ppb 18-NOV-2000 14 4.28 4.23 25-Mar-2001 17 4.50 4.07 Medium QC 150 ppb 156 147 180 180 High QC 400 ppb 385 417 450 444 Dilution QC 400 ppb DF=2 428 423 397 437 438 *552 Mean S.D. %CV %Theoretical %Bias n 4.24 0.399 9.4 106.0 6.0 26 156 16.6 10.6 104.0 4.0 26 407 39.4 9.7 101.8 1.8 26 * > 25% deviation from theoretical 430 51.3 11.9 107.5 7.5 12 Page 48 000386 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBROl-OOl Table 20. Analytical QC Summary for M556 All concentrations are expressed as ppb. Run Date Run Low QC Medium QC N um ber 4.00 ppb 150 ppb 31-Oct-2000 01-Nov-2000 04-Nov-2000 O6-N0V-2OOO O8-N0V-2OOO O9-N0V-2OOO lO-Nov-2000 I2-N0V-2OOO I3-N0V-2OOO I4-N0V-2OOO I5-N0V-2OOO 2 3.95 3.93 3 *4.81 4.62 4 4.08 3.70 5 3.57 3.30 6 4.74 3.63 7 3.63 4.11 8 4.25 4.18 9 3.56 4.00 10 . 4.49 4.29 11 3.36 4.51 12 *3.14 3.56 161 149 163 171 156 163 141 146 172 160 155 132 161 *182 158 176 164 175 163 157 156 *112 I6-N0V-2OOO 13 3.98 3.81 139 154 High QC 400 ppb 417 406 449 *492 397 393 373 383 444 431 367 398 417 423 384 404 421 357 394 384 427 420 416 407 Dilution QC 400 ppb DF=2 402 464 416 397 385 427 * > 20% deviation from theoretical Page 49 0G0387 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRI-001 Table 20. Analytical QC Summary for M556 (Continued) All concentrations are expressed as ppb. Run Date Run Low QC M edium QC N um ber 4.00 ppb 150 ppb 18-Nov-2000 14 3.87 3.69 150 157 25-Mar-2001 17 4.09 3.52 168 162 High QC 400 ppb 382 424 455 434 Dilution QC 400 ppb DF=2 416 419 406 403 392 *627 Mean S.D. %CV %Theoretical %Bias n 3.94 0.437 11.1 98.5 -1.5 28 157 14.3 9.1 104.7 4.7 28 411 29.3 7.1 102.8 2.8 28 * > 20% deviation from theoretical 430 65.5 15.2 107.5 7.5 12 Page 50 000388 Northwest Biounalytical Study No. NWBS00-08S Report No. NWBRO1-001 Table 21. Analytical QC Summary for M570 All concentrations are expressed as ppb. Run Date Run Low QC N um ber 4.00 ppb 31-Oct-2000 2 01-Nov-2000 3 04-Nov-2000 4 06-Nov-2000 5 08-NOV-2000 6 09-NOV-2000 7 10-Nov-2000 8 12-NOV-2000 9 13-NOV-2000 10 14-Nov-2000 11 15-NOV-2000 12 3.70 3.99 4.52 *5.13 3.68 4.06 *3.10 3.60 4.48 3.85 *3.13 3.51 *2.97 3.37 3.94 4.30 4.12 *4.85 3.43 4.32 3.29 3.64 16-Nov-2000 13 3.25 3.65 Medium QC 150 ppb 164 160 152 178 147 165 133 146 *182 161 154 131 165 *184 154 173 158 176 166 154 155 *114 141 161 High QC 400 ppb 410 416 476 *491 400 385 362 379 446 422 364 409 421 427 384 397 420 326 408 383 452 429 423 415 Dilution QC 400 ppb DF=2 414 *490 424 413 399 435 * > 20% deviation from theoretical Page 51 000389 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 21. Analytical QC Summary for M570 (Continued) All concentrations are expressed as ppb. Run Date Run Low QC N um ber 4.00 ppb 20-NOV-2000 16 *2.76 3.33 25-Mar-2001 17 3.20 *2.89 Medium QC 150 ppb 169 151 165 159 High QC 400 ppb 372 *484 461 411 Dilution QC 400 ppb DF=2 415 421 391 383 400 *648 Mean S.D. % cv %Theoretical %Bias n 3.72 0.596 16.0 93.0 -7.0 28 158 15.6 9.9 105.3 5.3 28 413 38.1 9.2 103.3 3.3 28 * > t 20% deviation from theoretical 436 72.1 16.5 109.0 9.0 12 Page 52 000390 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations All concentrations are expressed as ppb. Sample No. 0021 0056 0087 0104 0109 0122 0123 0126 0127 0128 0131 0133 0136 0149 0151 0167 0174 PFOS Concentration 11.1 27.1 18.1 67.3 19.4 36.8 29.0 39.6 42.8 81.2 68.0 65.2 83.8 39.3 29.8 77.6 36.1 PFOA Concentration** 2.13 5.79 3.95 6.14 2.65 3.35 3.37 3.77 <LLOQ(2.88) 5.60 4.68 6.91 8.65 2.94 5.00 7.70 3.85 PFHS Concentration* <LLOQ(1.36) 3.72 1.99 3.82 6.12 4.28 <LLOQ(1.36) 10.4 <LLOQ(2.41) 21.2 28.1 21.6 180 25.7 11.0 1.81 7.09 PFOSAA Concentration* <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 4.54 3.03 <LLOQ(1.60) <LLOQ(2.60) 5.50 5.45 2.11 <LLOQ(1.60) 2.33 3.11 6.32 4.06 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( .00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 2.7 4.62 <LLOQ(2.50) <LLOQ(5.00) 7.33 6.1 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570 Concentration* <LLOQ(1.00) <LLOQ(1.00) 5.15 3.28 6.55 <LLOQ( 1.00) 2.37 1.74 <LLOQ(2.00) 4.81 1.53 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) 1.91 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 53 CS03B1 Northwest Bioanalytical Study No. NWBS00-O88 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. PFOS Concentration PFOA PFHS Concentration** Concentration* PFOSAA Concentration* PFOSA Concentration* M556 Concentration* 0187 31.1 3.56 <LLOQ(1.36) 3.69 <LLOQ(1.00) <LLOQ(2.50) 0192 35.7 6.93 6.05 6.66 <LLOQ(1.00) <LLOQ(2.50) 0193 90.2 6.41 71.3 3.14 <LLOQ(1.00) 3.58 0194 24.5 4.44 1.41 <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) 0196 11.6 1.95 <LLOQ(l.36) 1.64 <LLOQ(1.00) <LLOQ(2.50) 0197 38.9 0198 71.9 5.46 <LLOQ(1.36) 7.43 <LLOQ(1.36) 4.95 4.12 <LLOQ(1.00) <LLOQ(1.0Q) <LLOQ(2.50) 5.94 0199 54.8 7.37 30.0 <LLOQ(2.60) <LLOQ(2.00) <LLOQ(5.00) 0210 33.9 5.44 4.14 4.76 <LLOQ(2.00) 7.16 0216 38.2 4.79 3.12 0217 43.6 5.16 6.86 2.42 <LLOQ(1.00) <LLOQ(2.50) 5.34 <LLOQ(1.00) 5.59 0228 16.6 3.89 6.83 <LLOQ(1.60) <LLOQ(1.00) <LLOQ(2.50) 0229 122 10.4 145 4.93 <LLOQ(1.00) 4.35 0230 No result No result No result No result (Insufficient No result No result (Insufficient sample (Insufficient sample (Insufficient sample sample volume) (Insufficient sample (Insufficient volume) volume) volume) volume) sample volume) 0231 93.9 7.8 17.8 6.07 <LLOQ(1.00) 8.55 M570 Concentration* 2.04 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) 7.26 2.42 5.03 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) No result (Insufficient sample volume) 23 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 54 000332 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0247 0250 0251 0259 0269 0270 0290 0296 0308 0315 0329 0341 0342 0344 0356 0358 0365 PFOS Concentration 42.4 37.7 51.3 38.3 92.3 25.7 28.7 23.3 23.7 94.2 29.6 53.0 38.3 31.1 45.8 30.0 26.8 .. PFOA Concentration* 2.92 6.11 4.32 5.07 8.71 5.09 4.08 4.28 3.56 4.74 2.66 4.89 5.88 3.26 7.85 .4.32 <LLOQ(2.88) PFHS Concentration* 11.4 2.51 16.1 11.3 75.4 <LLOQ(1.36) 3.23 <LLOQ(1.36) <LLOQ(1.36) 11.2 4.60 2.33 <LLOQ(1.36) <LLOQ(2.41) 1.50 2.27 <LLOQ(2.41) PFOSAA Concentration* 3.19 <LLOQ(1.60) 3.11 2.04 15.3 4.54 <LLOQ(1.60) 2.62 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 6.61 1.98 <LLOQ(2,60) 4.37 3.53 <LLOQ(2.60) PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.00) M556 Concentration* 2.88 <LLOQ(2.50) 4.94 5.88 8.4 4.42 <LLOQ(2.50) <LLOQ(2.50) 3.54 <LLOQ(2.50) 3.21 3.77 , <LLOQ(2.50) <LLOQ(5.00) 9.71 <LLOQ(2.50) <LLOQ(5.00) M570 Concentration* 1.06 2.67 3.11 <LLOQ(1.00) 5.16 1 2.53 <LLOQ( 1.00) 1.36 2.15 2 2.59 1.28 <LLOQ(2.00) 26.6 1.3 <LLOQ(2.00) * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. 030333 Page 55 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0366 0367 0370 0385 0386 0387 0388 0398 0404 0405 0407 0410 0411 0415 0420 0421 0423 PFOS Concentration 41.5 67.7 87.4 50.2 96.5 56.5 24.2 31.4 69.1 77.2 17.8 49.3 106 53.2 35.7 65.9 184 PFOA Concentration* 4.88 7.21 9.35 9.02 6.85 6.83 3.46 2.61 4.27 6.62 2.46 4.94 5.78 5.21 5.49 5.63 9.20 PFHS Concentration* <LLOQ(1.36) 4.78 37.4 7.08 74.1 35.3 1.94 4.32 49.3 24.3 <LLOQ(1.36) 2.54 33.9 41.3 2.61 2.20 89.3 PFOSAA Concentration* 3.94 4.85 7.33 1.97 3.24 3.28 2.09 3.20 5.10 4.54 3.79 8.78 8.72 4.39 3.26 9.82 6.71 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00r cLLOQ(l.OO) M556 Concentration* <LLOQ(2.50) <LLOQ(2.50) 3.82 <LLOQ(2.50) 3.35 2.56 <LLOQ(2.50) <LLOQ(2.50) 2.61 3.29 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570 Concentration* 1.48 1.49 6.63 3.74 8.3 1.47 3.69 <LLOQ(1.00) 1.17 10.1 <LLOQ( 1.00) 2.48 3.19 4.12 1.74 4.25 3.29 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected.for the persistent level of analyte in the dilution matrix. Tire method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 56 003S4 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0425 0432 0456 0463 0465 0466 0470 0476 0478 0493 0495 0498 0499 0500 0521 0524 0526 PFOS Concentration 31.9 46.1 34.4 34.7 42.5 2*7.3 34.4 124 56.7 106 52.0 63.4 27.6 59.9 31.9 59.5 46.9 PFOA Concentration** 6.79 7.06 8.30 3.97 6.90 4.03 4.39 14.6 9.05 7.56 6.14 5.19 5.28 4.72 11.0 7.20 4.29 PFHS Concentration* 5.36 3.05 3.69 7.64 6.21 6.75 3.21 7.36 34.8 50.5 3.11 18.1 2.98 21.2 6.52 37.5 2.07 PFOSAA Concentration* 4.17 4.62 3.01 3.61 3.28 3.56 3.54 11.3 5.59 8.83 3.50 4.17 4.52 8.94 5.31 3.44 11.2 PFOSA Concentration* <LLOQ(1.00) <LLOQ(l.Q0) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1,00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) cLLOQ(l.OO) <LLOQ(1.00) M556 M570 Concentration* Concentration* 3.21 4.8 3.82 1.78 <LLOQ(2.50) 3.09 <LLOQ(2.50) 3.42 <LLOQ(2.50) 4.35 2.58 4.73 <LLOQ(2.50) 2.28 9.59 31 3.46 19.7 9.45 - 1.84 <LLOQ(2.50) . 2.83 3.83 2.71 2.74 2.27 5.88 2 <LLOQ(2.50) 3.01 3.26 4.14 8.22 6.39 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 57 000325 Northwest Bioanalytical Study No. NWBS0Q-088 Repon No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0527 0528 0530 0531 0532 0534 0541 0542 0545 0548 0572 0578 0583 0585 0586 0587 0588 PFOS Concentration 15.4 30.3 98.1 97.9 38.1 34.6 54.0 29.5 36.9 75.7 20.4 77.6 70.1 64.8 39.5 58.2 46.0 PFOA Concentration* 2.52 5.10 8.12 6.43 6.81 4.39 6.88 5.18 8.01 9.00 3.00 7.66 5.54 6.25 5.73 7.36 5.77 PFHS Concentration* 4.78 17.0 150 72.0 11.0 5.63 1.70 <LLOQ(1.36) 7.32 52.0 <LLOQ(1.36) 80.6 14.6 34.5 20.5 22.0 11.6 PFOSAA Concentration* 4.18 2.09 11.5 10.3 1.84 2.59 5.55 5.11 2.68 3.98 8.92 4.48 12.9 4.82 1.82 9.06 3.59 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(l.Q0) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.0Q) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) cLLOQ(l.OO) M556 Concentration* <LLOQ(2.50) 2.66 5.91 3.67 <LLOQ(2.50) 2.8 3.24 3.15 2.79 <LLOQ(2.50) 3.25 5.4 6.81 2.82 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570 Concentration* 3.38 4.46 1.62 1.71 1.02 1.66 5.05 4.13 3.66 2.13 1.75 1.27 5.09 4.5 * 6.77 1.7 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 58 0G03* Northwest Bioanalytical Study No. NWBS00-088 ` Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0589 0590 0592 0593 0598 0599 0604 0606 0607 0608 0610 0611 0621 0627 0628 0629 0631 PFOS Concentration 31.0 33.4 35.1 165 25.6 77.1 18.0 37.6 48.2 52.3 29.0 20.3 23.2 72.7 29.8 37.6 54.5 PFOA Concentration** 7.57 6.37 3.15 7.94 5.40 7.44 3.54 5.71 5.72 8.01 5.36 2.19 4.57 4.65 2.64 4.86 7.68 PFHS Concentration* 3.71 8.80 1.75 129 1.91 21.8 2.85 2.84 2.55 1.82 7.30 <LLOQ(1.36) 3.13 20.0 <LLOQ(1.36) <LLOQ(1.36) 11.4 PFOSAA Concentration* 2.84 9.81 2.99 2.40 2.56 6.25 <LLOQ(1.60) 4.69 10.3 8.98 4.23 3.66 3.95 5.02 6.26 8.71 6.72 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.0Q) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1,00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <LLOQ(2.50) 9.8 <LLOQ(2.50) <LLOQ(2.50) 4.05 4.42 <LLOQ(2.50) 4.11 7 3.42 3.38 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 2.64 2.55 4.63 M570 Concentration* <LLOQ(1.00) 4.02 2.22 <LLOQt 1.00) 4.75 5.91 1.5 7.17 2.82 3.57 11.8 <LLOQ(1.00) 2.12 1.51 3.69 <LLOQ( 1.00) <LLOQ( 1.00) * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 59 000327 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0649 0657 0658 0664 0665 0666 0667 0673 0676 0678 0679 0680 0681 0689 0695 0697 0700 PFOS Concentration 28.8 27.4 19.7 55.1 31.9 16.3 57.8 34.3 25.6 50.0 30.2 44.6 31.9 40.1 28.1 27.8 17.8 PFOA Concentration* <LLOQ(2.88) 5.90 2.91 3.80 4.96 3.17 7.41 4.21 4.91 7.09 3.16 5.80 4.81 5.35 4.08 4.29 3.90 PFHS Concentration* <LLOQ(2.41) 6.25 <LLOQ(1.36) 3.80 4.68 <LLOQ(1.36) 37.1 1.38 1.64 7.21 <LLOQ(1.36) 2.35 5.19 <LLOQ(1.36) 2.65 1.56 1.83 PFOSAA Concentration* <LLOQ(2.60) 3.71 2.34 4.67 3.36 3.19 3.95 8.58 4.54 11.2 5.15 9.12 4.18 3.97 5.70 3.65 <LLOQ(1.60) PFOSA Concentration* <LLOQ(2.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <LLOQ(5.00) 3.25 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 3.4 <LLOQ(2.50) 3.7 <LLOQ(2.50) 4.86 <LLOQ(2.50) 2.91 3.46 <LLOQ(2.50) <LLOQ(2.50) M570 Concentration* <LLOQ(2.00) 1 3.78 <LLOQ( 1.00) ; 1.26 2.14 <LLOQ(1.00) 6.96 5.39 3.56 7.87 <LLOQ(1.00) 2.92 2.06 6.03 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 60 0 0 0 3 5 /0 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0711 0712 0713 0714 0719 0720 0721 0723 0725 0741 0748 0752 0753 0754 0763 0769 0771 PFOS Concentration 8.76 19.5 32.4 23.3 34.8 42.7 37.8 32.2 26.9 33.3 22.0 16.7 37.1 33.6 35.7 19.5 81.0 PFOA Concentration* 2.02 2.54 4.34 2.78 3.82 5.26 4.97 4.87 5.17 4.36 6.00 2.46 4.67 5.63 5.05 3.40 4.88 PFHS Concentration* <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) 1.96 1.82 4.88 8.24 9.44 1.42 1.85 5.04 <LLOQ(1.36) 1.38 <LLOQ(1.36) 7.10 4.87 2.43 PFOSAA Concentration* 2.23 3.76 2.71 <LLOQ(1.60) 4.90 3.05 5.34 4.95 8.99 3.66 3.67 3.52 2.96 5.97 4.60 <LLOQ(1,60) 3.34 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1,00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* 3.63 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 8.87 <LLOQ(2.50) 5.36 2.66 2.95 3.76 <LLOQ(2.50) <LLOQ(2.50) 5.12 <LLOQ(2.50) <LLOQ(2.50) 3.38 M570 Concentration* <LLOQ(1.00) 2.93 <LLOQ(1.00) 1.61 <LLOQ(1.00) 4.44 1.19 <LLOQ(1.00) <LLOQ(1.00) 2.51 1.81 1.34 5.36 <LLOQ(l.QQ) 1.13 <LLOQ(1.00) 14.2 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 61 0003 3 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO 1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0774 0775 0779 0783 0784 0785 0788 0792 0795 0796 0798 0799 0800 0813 0814 0823 0829 PFOS Concentration 27.9 41.4 27.9 28.8 39.1 70.6 51.1 54.2 32.3 17.6 40.2 54.4 34.1 12.2 40.7 56.3 41.8 PFOA Concentration** 2.49 9.11 4.44 7.14 5.65 6.97 7.34 5.54 5.70 4.61 4.33 3.54 5.98 3.84 5.47 6.59 4.36 PFHS Concentration* 3.65 8.85 8.86 3.50 9.21 41.3 36.4 4.68 9.86 3.11 2.55 3.60 <LLOQ(1.36) 4.31 2.39 1.70 13.2 PFOSAA Concentration* 5.19 5.06 2.04 5.92 3.27 1.71 3.87 3.18 2.05 <LLOQ(1.60) 7.35 4.12 6.89 2.20 5.76 3.78 5.30 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <LLOQ(2.50) 7.2 2.87 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 3.1 <LLOQ(2.5Q) 4.47 3.93 4.28 3.21 2.7 <LLOQ(2.50) 4.44 6.58 3.15 M570 Concentration* 3.25 14.3 1.3 4.58 cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) 3.73 1.59 1.42 <LLOQ(1.00) 8.16 <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) 8.26 1.83 * Serum sample results obtained using plasma curves may vary from results obtained front serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 62 00040 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0830 0840 0841 0845 0846 0848 0849 0859 0864 0866 0867 0869 0872 0876 0880 0881 0883 PFOS Concentration 32.0 49.7 33.1 67.7 39.3 27.2 33.4 59.5 74.3 43.8 26.7 31.7 58.1 50.1 71.7 45.7 42.8 PFOA Concentration* 6.12 5.70 5.68 5.77 4,44 3.26 3.76 8.31 4.23 9.42 3.86 6.81 6.46 6.10 8.95 3.92 5.09 PFHS Concentration* 3.80 2.71 19.5 5.21 2.04 2.77 3.24 12.6 13.0 18.5 8.01 <LLOQ(1.36) 3.48 6.68 5.35 <LLOQ(1.36) 18.4 PFOSAA Concentration* 10.3 2.96 6.56 20.7 7.87 4.27 3.86 6.56 2.25 2.10 2.01 4.79 9.96 3.75 5.84 6.01 6.14 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* 5.92 3.55 2.82 15.5 5.82 2.91 2.75 4.46 4.02 <LLOQ(2.50) <LLOQ(2.50) 6.17 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 4.09 <LLOQ(2.50) M570 Concentration* 18.4 5.64 3.54 4.44 <LLOQ(1.00) 1.7 1.55 3.22 9.81 3.24 1.98 <LLOQ(1.00) 7.85 1.42 26.7 <LLOQ( 1.00) 2.93 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 63 0S0401 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 0890 0906 0907 0909 0910 0916 0922 0928 0937 0938 0950 0953 0956 0970 0971 0986 0987 PFOS Concentration 17.3 36.3 59.4 36.8 24.4 17.6 40.7 74.6 39.3 43.9 24.8 30.3 27.5 40.4 11.4 20.1 58.2 PFOA Concentration** 3.80 4.47 6.43 4.09 3.13 2.85 8.18 6.55 3.61 7.20 4.90 8.51 3.62 6.62 2.62 2.57 4.35 PFHS Concentration* 3.91 <LLOQ(1.36) 7.14 <LLOQ(1.36) 1.87 <LLOQ(1.36) <LLOQ(1.36) 43.2 2.69 1.67 5.34 1.47 <LLOQ(1.36) 6.18 <LLOQ(1.36) <LLOQ(1.36) 3.94' PFOSAA Concentration* 2.69 21.7 4.84 4.41 7.23 2.11 8.51 3.86 6.95 4.06 5.12 5.69 2.24 9.69 <LLOQ(1.60) 2.46 16.2 PFOSA Concentration* cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) M556 Concentration* <LLOQ(2.50) 3.81 10.5 <LLOQ(2.50) 6.52 <LLOQ(2.50) 3.6 <LLOQ(2.50) 3.65 5.07 4.11 4.28 <LLOQ(2.50) 2.66 <LLOQ(2.50) <LLOQ(2.50) 3.42 M570 Concentration* 1 1.55 9.95 1.11 <LLOQ(1.00) 1.08 1.7 4.28 2.91 1.54 1.31 3.79 1.8 2.95 <LLOQ(1.00) 1.51 9.05 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. 000402 Page 64 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1001 1003 1005 1012 1013 1017 1019 1021 1023 1029 1030 1039 1042 1044 1048 1053 1057 PFOS Concentration 21.7 18.0 26.8 27.4 38.0 16.8 39.9 25.6 28.9 86.4 23.8 325 50.7 81.4 25.1 66.6 62.8 PFOA Concentration** 3.25 3.52 5.39 2.47 5.45 3.46 7.16 9.81 3.01 6.18 3.89 56.1 5.06 8.05 6.33 4.25 8.62 PFHS Concentration* <LLOQ(1.36) 2.18 <LLOQ(1.36) 1.44 3.46 <LLOQ(1.36) 2.54 5.11 <LLOQ(1.36) 74.2 <LLOQ(1.36) 416 39.6 51.9 2.94 35.7 6.40 PFOSAA Concentration* 1.64 <LLOQ(1.60) <LLOQ(1.60) 4.07 3.90 7.37 5.58 <LLOQ(1.60) 6.14 3.18 5.10 3.62 3.21 5.79 2.94 3.45 7.90 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) CLLOQ(I.OO) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) . <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.5Q) <LLOQ(2.50) 3.14 <LLOQ(2.50) <LLOQ(2.50) 2.54 <LLOQ(2.50) 2.68 4.01 <LLOQ(2.50) 4.25 <LLOQ(2.50) <LLOQ(2.50) 4.05 M57 Concentration* 2.32 <LLOQ(1.00) 4.31 <LLOQ( 1.00) 2.6 2.29 7.97 3.71 3.03 2.1 1.51 7.76 3.6 1.92 4.21 2.45 17.8 * Seram sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 65 CG0403 Northwest Bioanalytical Study No. NWBS00-088 Repon No. NWBRO1-0 0 1 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1059 1067 1068 1070 1072 1073 1082 1085 1088 1090 1101 1104 1113 1115 1117 1121 1122 PFOS Concentration 27.9 45.1 19.5 22.4 43.2 33.6 48.2 38.2 31.3 50.9 32.8 62.6 20.2 40.4 46.5 48.7 36.5 PFOA Concentration** 4.09 5.32 3.11 3.57 6.22 2.64 4.66 3.43 6.98 5.85 2.90 5.63 3.08 5.04 3.09 5.60 5.40 PFHS Concentration* <LLOQ(1.36) 10.4 <LLOQ(1.36) 9.07 1.92 2.19 7.91 1.59 1.77 12.4 9.41 13.3 <LLOQ(1.36) 36.2 <LLOQ(1.36) 2.60 11.9 PFOSAA Concentration* 7.44 3.17 <LLOQ(1.60) 2.72 6.89 7.83 4.62 2.98 2.16 4.99 1.73 6.31 <LLOQ(1.60) 1.74 6.89 5.10 2.96 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* 5.33 <LLOQ(2.5Q) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 5.99 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 2.97 5.8 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 4.01 <LLOQ(2.50) M570 Concentration* <LLOQ(1.00) 1.01 1.58 <LLOQ( 1.00) <LLOQ(1.00) 3.69 3.6 1.83 <LLOQ(1.00) 6.28 5.83 2.25 <LLOQ( 1.00) 1.4 1.91 4.77 2.5 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 66 000404 Northwest Bioanalytical Study No. NWBS00-088 Report No. N3VBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1124 1126 1129 1133 1136 1144 1147 1152 1153 1154 1155 1157 1166 1168 1171 1172 1173 PFOS Concentration 20.7 33.1 52.0 26.7 27.1 30.1 30.1 17.7 31.3 22.5 31.7 53.0 34.8 53.7 55.2 118 43.4 PFOA PFHS Concentration** Concentration* 4.35 4.70 4.90 10.4 6.85 4.55 4.15 20.3 4.21 2.00 4.59 3.47 5.51 2.39 4.33 3.25 4.28 8.63 3.61 2.44 3.71 <LLOQ(1.36) 4.38 11.5 5.80 10.5 5.22 2.86 5.21 2.57 11.9 4.07 11.0 9.77 PFOSAA Concentration* 2.13 5.66 4.24 1.79 6.23 5.01 7.87 <LLOQ(1.60) 2.27 4.08 5.29 2.51 5.60 3.61 9.22 5.94 4.22 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1,00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <LLOQ(2,50) 2.5 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 3.29 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 4.01 <LLOQ(2.50) <LLOQ(2.50) 4.33 6.36 14.9 <LLOQ(2.50) M570 Concentration* 3.15 4.22 5.69 <LLOQ(1.00) <LLOQ( 1.00) 1.88 2.15 1.56 <LLOQ(1.00) 2.31 1.69 3.28 <LLOQ( 1.00) 12.5 17 48 6.27 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 67 000405 Northwest Bioanalytical Study No. NWBS0Q-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1174 1175 1177 1178 1179 11797 11798 11799 11800 11801 11802 11803 11804 11805 11806 11807 11808 PFOS Concentration 39.6 28.6 73.8 51.5 49.0 27.9 69.7 142 131 42.9 647 110 120 90.2 98.9 66.6 54.1 PFOA Concentration** 5.35 3.95 9.51 4.87 6.85 3.37 9.74 22.1 7.13 6.52 23.3 8.61 9.03 9.64 7.51 5.74 5.57 PFHS Concentration* 17.2 <LLOQ(1.36) 14.3 1.74 18.3 8.71 58.2 268 82.9 10.4 873 80.8 181 65.5 44.7 44.3 21.8 PFOSAA Concentration* 8.52 3.23 3.66 17.0 6.21 <LLOQ(2.60) <LLOQ(2.60) 6.31 5.26 <LLOQ(2.60) 3.02 15.4 2.90 3.51 <LLOQ(2.60) <LLOQ(2.60) 3.76 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.0Q) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) M556 Concentration* 4.4 <LLOQ(2.50) 4.76 6.17 5.77 <LLOQ(5.00) <LLOQ(5.00) 11.9 <LLOQ(5.00) <LLOQ(5.00) 13.7 6.01 <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) M570 Concentration* 1.97 1.01 13.4 3.45 7.04 <LLOQ(2.00) <LLOQ(2.00) 16.9 10.8 <LLOQ(2.00) 4.4 2.92 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00j * Semm sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 68 G0040 Northwest Bioanalytical V Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 11809 11810 11811 11812 11813 11814 11815 11816 11817 11818 11819 1182 11820 11821 11822 11823 11824 PFOS Concentration 418 21.8 90.9 199 39.7 419 47.3 88.5 81.5 143 68.9 38.1 118 26.0 52.5 28.8 52.6 PFOA Concentration** 70.0 3.56 6.70 11.4 5.69 65.6 7.47 19.5 6.05 10.2 7.35 4.26 9.34 <LLOQ(2.88) 5.09 <LLOQ(2.88) 6.65 PFHS Concentration* 484 5.99 136 109 12.5 469 8.13 "19.3 142 105 5.17 13.0 167 6.77 19.9 <LLOQ(2.41) <ULOQ(2.41) PFOSAA Concentration* <LLOQ(2.60) <LLOQ(2.60) 7.90 2.98 2.72 <LLOQ(2.60) 10.0 6.18 5.47 <LLOQ(2.60) <LLOQ(2.60) 5.36 3.00 <LLOQ(2.60) 4.90 3.24 3.83 PFOSA Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) M556 Concentration* <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) 7.38 <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) M570 Concentration* 5.52 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 6.64 <LLOQ(2.00) 35.1 <LLOQ(2.00) <LLOQ(2.00) 10.9 2 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 69 000407 Northwest Bioanalytical Study No. NWBSOO-088 Repon No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 11825 11826 11827 11828 11829 1183 11830 11831 11832 11833 11834 11835 11836 11837 11838 11839 1184 PFOS Concentration 92.1 46.1 131 164 83.9 57.7 34.7 28.1 32.0 188 76.6 685 55.9 160 17.6 101 37.1 PFOA Concentration** 20.54 5.32 8.71 7.63 6.91 11.6 4.13 3.05 3.19 18.5 5.97 23.0 6.43 7.44 3.40 25.9 5.07 PFHS Concentration* 20.9 <LLOQ(2.41) 101 132 24.1 21.8 5.53 6.04 7.86 228 7.85 933 <LLOQ(2.41) 135 <LLOQ(2.41) 20.2 1.44 PFOSAA Concentration* 7.02 <LLOQ(2.60) 15.7 <LLOQ(2.60) 5.09 2.39 4.52 <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) 3.23 2.65 3.55 <LLOQ(2.60) <LLOQ(2.60) 8.27 1.70 PFOSA Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(1.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(1.00) M556 Concentration* 8.74 <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(2.50) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) 13.5 13.8 <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) 9.47 <LLOQ(2.50) M570 Concentration* 35.6 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 2.4 <LLOQ(1.00) 3.32 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 9.14 6.01 11.3 <LLOQ(2.00) <LLOQ(2.00) 45.4 2.63 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. 000408 Page 70 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 11840 11841 11842 11843 11844 11845 11846 11847 11848 11849 11850 11851 11852 11853 11854 11855 11856 PFOS Concentration 42.2 127 74.8 146 29.7 196 88.0 14.9 162 145 613 54.1 170 431 93.1 103 20.3 PFOA Concentration** 8.99 9.54 5.40 10.8 3.47 20.2 6.77 <LLOQ(2.88) 21.9 13.6 22.5 4.76 7.44 67.2 15.9 19.6 <LLOQ(2.88) PFHS Concentration* 2.56 171 <LLOQ(2.41) 108 <LLOQ(2.41) 235 141 <LLOQ(2.41) 274 64.0 864 12.9 135 490 10.5 20.8 <LLOQ(2.41) PFOSAA Concentration* 3.58 <LLOQ(2.60) 8.33 <LLOQ(2,60) <LLOQ(2.60) <LLOQ(2.60) 7.35 <LLOQ(2.60) 7.77 19.7 <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) 8.05 <LLOQ(2.60) PFOSA Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2,00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) M556 Concentration* <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) 16 15.4 13 <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) 9.46 <LLOQ(5.00) M570 Concentration* <LLOQ(2.00) <LLOQ(2.00) 2.17 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 21.9 3.76 4.31 29.9 <LLOQ(2.00) 7.19 2.17 <LLOQ(2.00) <LLOQ(2.00) * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution mattix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 71 000403 Northwest Bioanalytical Study No. NWBS00-088 ' Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 11857 11858 1186 1199 1214 1217 1229 1232 1239 1240 1248 1254 1255 1261 1264 1269 1273 PFOS Concentration 199 144 39.3 62.2 44.2 70.7 37.7 53.5 37.5 67.6 42.7 35.4 97.9 47.5 51.5 78.1 72.1 PFOA Concentration** 20.0 20.8 10.2 8.64 5.55 6.72 3.05 6.70 3.46 10.3 4.40 5.44 9.80 6.27 8.51 16.4 7.52 PFHS Concentration* 241 257 1.89 3.15 33.9 42.4 <LLOQ(1.36) 2.97 6.45 3.47 2.83 1.38 61.4 2.50 9.61 76.5 4.10 PFOSAA Concentration* <LLOQ(2.60) 4.69 6.23 6.64 2.93 4.53 18.2 6.98 5.56 14.3 4.44 3.26 2.97 2.09 4.71 3.62 11.6 PFOSA Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <LLOQ(5.00) 12.1 2.79 5.76 2.61 <LLOQ(2.50) 6.33 4.46 <LLOQ(2.50) 4.12 3.09 <LLOQ(2.50) 3.24 3.59 5.35 3.34 4.91 M570 Concentration* <LLOQ(2.00) 18.7 1.14 9.65 4.3 <LLOQ(1.00) 1.56 13.8 4.45 6.12 1.77 1.81 3.22 3.44 6.9 2.48 5.23 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 72 0S040 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1291 1294 1296 1299 1311 1314 1323 1337 1339 1356 1358 1364 1368 1372 1387 1393 1395 PFOS Concentration 37.9 119 39.9 27.7 36.0 51.7 95.4 65.4 27.8 24.3 37.1 33.3 61.7 34.8 35.0 134 110 PFOA Concentration* 6.74 17.5 4.74 6.57 6.05 5.35 15.1 6.41 7.17 3.15 3.96 5.10 13.3 5.88 6.76 7.71 11.6 PFHS Concentration* 2.52 220 9.16 <LLOQ(1.36) 3.67 18.1 10.5 5.46 <LLOQ(1.36) 1.58 1.60 3.19 8.18 <LLOQ(1.36) 3.26 88.2 129 PFOSAA Concentration* 6.93 6.71 18.7 <LLOQ(1.60) 5.39 7.14 5.54 9.47 2.26 3.27 9.17 6.95 3.93 6.66 4.53 7.42 9.89 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <LLOQ(2.50) 13.1 6.84 <LLOQ(2.50) <LLOQ(2.50) 5.59 <LLOQ(2.50) 5.09 <LLOQ(2.50) <LLOQ(2.50) 6.09 5.4 5.84 <LLOQ(2.50) 2.96 4.44 2.6 M570 Concentration* 3.56 16.3 7.38 1.9 1.12 1.05 5.85 3.93 <LLOQ(1.00) <LLOQ( 1.00) 1.31 <LLOQ(1.00) 19.6 <LLOQ( 1.00) 3.67 2.52 <LLOQ( 1.00) * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentr ation. The statistical error of any individual result may exceed the QC acceptance criteria. Page 73 S0411 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1398 1400 1407 1408 1409 1410 1411 1412 1418 1420 1423 1424 1427 1431 1433 1435 1438 PFOS Concentration 37.6 32.5 24.3 34.7 34.0 21.3 31.5 .35.1 36.2 34.5 22.7 29.3 17.6 27.6 20.3 19.0 56.9 PFOA Concentration** 8.55 5.00 2.84 3.96 3.92 3.41 4.76 4.58 6.24 4.71 5.08 2.69 3.34 5.68 2.88 3.48 5.83 PFHS Concentration* 4.44 1.49 2.57 4.19 1.58 <LLOQ(1.36) 2.52 7.03 <LLOQ(1.36) 6.13 5.63 1.47 <LLOQ(1.36) 5.81 <LLOQ(1.36) 4.19 22.4 PFOSAA Concentration* 5.02 3.17 5.69 4.69 3.88 3.40 4.26 14.1 10.4 5.18 1.82 2.47 4.95 4.45 1.89 2.60 2.91 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1,00) <LLOQ(l.QQ) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) ` M556 Concentration* <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 2.73 3.48 2.74 <LLOQ(2.50) 5.44 5.77 2.77 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 4.54 <LLOQ(2.50) <LLOQ(2.50) 2.72 M570 Concentration* 3.69 1.25 1.54 1.84 1.06 1.42 3.85 4.53 <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) 1.52 1.98 1.42 1.24 1.72 2.46 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected inn (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 74 000412 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1439 1448 1455 1461 1467 1468 1470 1472 1482 1483 1491 1493 1494 1496 1498 1503 1510 PFOS Concentration 20.1 64.8 16.7 41.3 18.2 16.6 36.2 32.4 59.4 54.6 26.2 37.6 16.8 54.9 41.7 24.6 32.5 PFOA Concentration** 4.77 5.35 3.23 6.21 3.30 2.66 8.05 5.55 4.88 5.24 3.36 4.49 3.01 4.53 4.42 2.40 3.21 PFHS Concentration* 9.34 21.8 <LLOQ(1.36) 19.2 5.74 3.46 5.69 1.77 17.2 8.66 3.73 10.6 <LLOQ(1.36) 38.3 <LLOQ(1.36) 2.73 13.7 PFOSAA Concentration* 3.57 9.13 <LLOQ(1.60) 2.71 <LLOQ(1.60) <LLOQ(1.60) 4.97 1.71 18.3 23.8 2.62 <LLOQ(1.60) 2.77 1.95 5.31 2.39 <LLOQ( 1.60) PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ( 1.00) M556 Concentration* 5.46 4.43 <LLOQ(2.50) 3.34 <LLOQ(2.50) <LLOQ(2.50) 4.3 2.88 6.53 12 <LLOQ(2.50) 4.27 2.79 4.95 3.7 <LLOQ(2.50) 3.24 M570 Concentration* 2.87 <LLOQ(1.00) <LLOQ( 1.00) 2.98 <LLOQ(1.00) <LLOQ(1.00) 4.88 1.23 3.52 4.1 <LLOQ( 1.00) 22.7 2.28 <LLOQ(1.00) 1.13 1.68 17.1 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 75 000413 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1512 1513 1517 1524 1529 1537 1538 1542 1545 1558 1559 1574 1582 1590 1597 1603 1611 PFOS Concentration 26.4 34.1 62.8 28.9 26.5 10.4 35.9 17.2 28.9 50.8 61.0 25.0 26.0 39.3 31.5 25.4 37.3 PFOA Concentration* 2.63 4.37 5.76 4.82 4.56 <LLOQ(1.92) 2.36 2.14 3.89 7.92 10.5 4.75 3.20 6.61 9.93 5.53 13.0 PFHS Concentration* 12.1 5.13 58.8 4.30 2.73 <LLOQ(1.36) 11.2 <LLOQ(1.36) 2.28 13.8 14.2 6.47 <LLOQ(1.36) 4.27 3.34 <LLOQ(1.36) 1.52 PFOSAA Concentration* 1.73 3.27 <LLOQ(1.60) 1.66 3.83 <LLOQ(1.60) 4.33 <LLOQ(1.60) 6.05 10.4 8.56 2.17 1.89 5.56 2.8 5.99 6.68 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 6.23 6.06 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 2.5 4.44 6.92 <LLOQ(2.50) 3.07 8.75 2.74 <LLOQ(2.50) 5.62 M570 Concentration* 4.33 1.9 <LLOQ(1.00) 15.2 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) 1.61 2 <LLOQ(1.00) <LLOQ(1.00) 1.49 <LLOQ( 1.00) 5.75 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. 000414 Page 76 Northwest Bioanalytical Study No. NWBS00-088 Repon No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1616 1618 1620 1624 1626 1630 1634 1637 1640 1643 1646 1647 1652 1653 1663 1665 1668 PFOS Concentration 30.0 26.1 21.8 45.4 25.0 13.6 22.7 35.7 li:9 17.5 15.8 18.8 34.7 44.2 11.5 15.0 20.5 PFOA Concentration** 4.67 3.08 3.19 5.54 3.15 3.13 2.56 3.08 2.46 2.33 2.34 3.79 6.21 7.80 2.15 <LLOQ(1.92) 2.9 PFHS Concentration* 3.79 5.35 1.87 41.5 1.55 <LLOQ(1.36) 7.25 23.3 <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) <LLOQ(1.36) 5.59 4.54 <LLOQ(1.36) <LLOQ(1.36) 2.29 PFOSAA Concentration* <LLOQ( 1.60) 4.69 <LLOQ(l,6Q) 1.60 <LLOQ(1.60) <LLOQ(1.60) 1.73 <LLOQ(1.60) <LLOQ(1.60) <LLOQ(1.60) 2.26 2.81 5.50 7.02 <LLOQ(1.60) 6.09 2.15 PFOSA Concentration* <LLOQ(D00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <LLOQ(2.50) 2.77 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 3.75 4.14 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) M570 Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) 3.91 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) * Serum sample results obtained using plasma curves may vary front results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 77 000415 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1669 1677 1678 1679 1680 1690 1692 1700 1707 1709 1716 1719 1721 1722 1735 1748 1766 PFOS Concentration 33.9 27.6 15.9 28.1 23.0 38.1 42.6 22.4 42.4 42.5 33.3 21.2 26.1 28.6 27.5 27.2 43.6 PFOA Concentration* 6.64 2.58 2.46 4.27 2.69 4.97 8.11 2.14 3.56 4.74 4.57 4.55 4.96 3.25 5.88 3.44 5.28 PFHS Concentration* 3.25 3.31 <LLOQ(1.36) 3.52 <LLOQ(1.36) <LLOQ(1.36) 8.96 <LLOQ(1.36) 4.17 38.5 <LLOQ(1.36) 2.25 1.93 <LLOQ(1.36) 1.97 3.14 7.07 PFOSAA Concentration* 6.72 2.38 3.13 2.39 3.74 12.8 11.2 6.01 5.07 3.71 6.99 1.93 1.67 <LLOQ( 1.60) 7.19 2.25 5.68 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* 2.87 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 5.49 <LLOQ(2.50) 4.96 4.06 <LLOQ(2.5Q) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 3.66 <LLOQ(2.50) <LLOQ(2.50) M570 Concentration* 2.33 1.32 1.74 2.39 6.08 1.01 1.57 <LLOQ(1.00) 3.77 3.43 3.47 1.21 <LLOQ(1.00) 2.82 2.74 2.65 2.97 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 78 0G04io Northwest Bioanalytical Study No. NWBS00-0S8 Report No. NWBROl-OOl Table 22. Study Sample Concentrations (Continued) All concentr ations are expressed as ppb. Sample No. 1778 1781 1788 1806 1809 1816 1817 1819 1822 1825 1830 1834 1837 1842 1857 1875 1876 PFOS Concentration 25.3 32.4 49.7 67.7 12.7 33.9 29.3 29.3 48.8 20.5 19.9 28.7 71.8 32.2 21.3 28.3 25.0 PFOA Concentration* 5.66 4.02 5.74 7.17 1.95 5.93 4.40 4.12 6.01 4.76 4.29 5.75 8.95 5.37 5.70 4.91 5.60 PFHS Concentration* 1.65 1.67 19.6 94.2 <LLOQ(1.36) <LLOQ(1.36) 12.4 7.59 17.8 2.65 2.79 15.7 4.69 9.45 <LLOQ(1.36) 1.58 8.53 PFOSAA Concentration* 1.70 3.58 5.97 4.75 <LLOQ(1.60) 11.6 3.54 2.90 9.63 2.44 1.62 3.68 12.9 1.69 5.07 2.18 2.24 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) cLLOQ(l.OO) cLLOQ(l.OO) cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* 2.62 <LLOQ(2.50) 5.25 <LLOQ(2.50) <LLOQ(2.50) 9.82 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 2.78 9.88 <LLOQ(2,5Q) 19.1 7.29 4.54 <LLOQ(2.50) 2.79 M570 Concentration* 6.74 6.82 1.12 <LLOQ(1.00) <LLOQ( 1.00) <LLOQ(1.00) 1.56 2.62 2.01 2.04 2.47 3.06 38.1 3.89 <LLOQ(1.00) 1.88 1.72 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 79 000417 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1886 1887 1888 1898 1909 1911 1912 1913 1934 1942 1953 1954 1956 1959 1961 1962 1965 PFOS Concentration 52.6 16.9 40.5 18.3 149 35.3 46.2 43.9 51.2 50.1 74.3 55.5 30.6 23.8 31.0 16.2 75.2 PFOA Concentration** 9.49 3.22 8.11 5.26 16.1 6.28 7.32 9.06 6.99 8.54 7.94 5.09 5.05 4.26 5.54 4.12 6.65 PFHS Concentration* 2.01 <LLOQ(1.36) 2.39 3.40 170 2.44 3.17 3.52 4.44 4.83 18.9 1.64 10.7 3.42 12.3 <LLOQ(1.36) 87.9 PFOSAA Concentration* 19.6 4.81 5.31 2.22 3.81 2.40 6.16 2.93 4.90 3.22 5.18 6.62 3.20 3.87 2.95 <LLOQ(1.60) 5.62 PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLQQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* 9.53 <LLOQ(2.50) 6.41 <LLOQ(2.50) 2.76 4.56 2.65 <LLOQ(2.50) <LLOQ(2.50) 3.02 2.76 4.45 <LLOQ(2,50) <LLOQ(2.50) 3.06 <LLOQ(2.50) 4.22 M570 Concentration* <LLOQ(1.00) 1.38 1.22 i 1.03 1.28 1.15 1.58 5.23 13.1 1.95 4.27 3.76 4.77 2.37 2.27 <LLOQ(1.00) 2.13 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution manix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 80 000418 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 1982 1996 2000 2002 2003 2022 2038 2041 2050 2052 2054 2056 2074 2075 2076 2078 2079 PFOS Concentration 18.2 27.1 93.7 96.8 52.2 34.7 70.4 22.8 41.5 25.8 20.7 45.6 48.5 38.8 39.4 86.8 59.9 PFOA Concentration** 4.15 3.82 10.1 7.17 4.87 3.94 8.89 5.69 4.61 <LLOQ(2.88) 3.06 4.31 5.54 5.30 6.65 19.5 6.63 PFHS Concentration* 1.51 2.43 7.12 90.8 3.72 4.98 15.8 7.12 2.83 <LLOQ(2.41) 2.36 15.4 2.21 3.75 8.06 20.4 4.84 PFOSAA Concentration* 3.93 3.43 8.19 2.93 8.86 1.80 2.35 1.88 2.64 <LLOQ(2.60) 3.50 5.44 4.60 2.19 6.49 8.81 2.40 PFOSA Concentration* cLLOQ(l.OO) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* <LLOQ(2.50) <LLOQ(2.50) 9.14 <LLOQ(2.50) 3.48 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 3.28 <LLOQ(5.00) 2.84 <LLOQ(2.50) 2.77 2.93 3.48 10.2 5.37 M570 Concentration* 2.25 <LLOQ(1.00) 17.9 2.45 3.08 2.63 5.81 cLLOQ(l.OO) 8.4 <LLOQ(2.00) <LLOQ(1.00) 1.49 3.03 5.4 4.24 42.5 14.8 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (+25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 81 000419 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 2082 2087 2089 2099 2104 2112 2114 2115 2121 2124 2127 2140 2141 2144 2150 2151 2156 PFOS Concentration 86.6 34.4 21.0 47.1 55.3 80.5 42.8 28.0 55.1 42.5 62.1 26.1 29.7 37.0 39.2 23.9 46.6 PFOA Concentration* 6.87 8.42 4.61 5.29 6.83 10.7 4.48 5.83 4.10 6.95 8.96 3.67 6.77 4.06 4.24 3.37 7.95 PFHS Concentration* 84.1 1.55 2.16 4.23 47.6 62.2 3.39 5.04 19.2 15.9 27.9 2.81 <LLOQ(1.36) 2.65 9.88 1.64 13.6 PFOSAA Concentration* 9.70 7.75 4.61 5.82 <LLOQ(1.60) 5.79 4.62 5.3 4.52 4.33 3.43 2.28 <LLOQ(1.60) 6.25 6.59 <LLOQ(1.60) 3.94 PFOSA Concentration* <LLOQ( 1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) M556 Concentration* <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 3.32 <LLOQ(2.50) 2.75 3.38 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 6.14 9.89 <LLOQ(2.50) <LLOQ(2.50) M570 Concentration* 1.97 <LLOQ(l .00) <LLOQ(1.00) 2.09 1.36 1.64 3.76 4.04 9.68 4.14 <LLOQ(1.00) <LLOQ(1.00) <LLOQ( 1.00) 1.1 2.36 <LLOQ( 1.00) 3.82 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 82 0G04& Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 2158 2162 2164 2168 2171 2173 2174 2176 2179 2181 2184 2186 2191 2193 2200 2220 2227 PPOS Concentration 36.4 48.1 36.2 515 65.5 49.5 63.5 73.2 123 116 53.3 50.2 40.2 40.1 41.5 42.4 69.9 PFOA Concentration* 6.93 5.10 5.08 20.2 7.09 5.23 14.0 8.55 9.96 11.5 10.5 8.36 4.52 6.62 5.66 5.61 7.47 PFHS Concentration* 6.10 14.1 4.51 712 37.3 18.2 5.92 59.2 107 55.4 5.07 3.11 <LLOQ(1.36) 31.9 12.1 8.01 104 PFOSAA Concentration* 4.02 1.81 2.58 4.04 5.69 4.68 5.23 2.68 7.47 18.1 3.94 7.97 3.37 6.45 4.73 7.73 <LLOQ(1.60) PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(l.OO)** cLLOQ(l.OO)** <LLOQ(1.00)** <LLOQ(1.00)** M556 Concentration* 2.55 <LLOQ(2.50) <LLOQ(2.50) 16.4 <LLOQ(2.50) 5.08 3.92 3.49 4.01 13.4 6.68 3.88 2.97 4.54 <LLOQ(2.50) <LLOQ(2.50) 5.59 M570 Concentration* 2.48 2.12 3.35 7 2.8 8.34 17.7 3.47 9.76 4.82 7.53 5.6 1.08 6.58 1.42 6.69 6.75 * Serum sample results obtained using plasma curves may vary front results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. Tire method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 83 000421 Northwest fioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 2230 2234 2236 2239 2244 2246 2248 2260 2265 2273 2298 2307 2323 2327 2335 2341 2348 PFOS Concentration 66.6 36.1 39.8 17.2 26.2 34.7 60.8 6.67 44.8 28.3 17.7 43.9 25.5 24.3 26.5 43.4 34.7 PFOA Concentration* 7.92 5.77 5.97 2.77 2.91 5.06 6.72 <LLOQ( 1.92) 5.09 3.45 2.22 5.52 3.65 5.47 3.18 7.21 4.45 PFHS Concentration* 84.2 14.8 25.4 12.5 3.44 4.20 29.6 <LLOQ(1.36) 10.4 1.79 <LLOQ(1.36) 4.73 <LLOQ(1.36) 3.79 3.79 2.25 <LLOQ(1.36) PFOSAA Concentration* <LLOQ(1.60) 2.95 2.92 <LLOQ( 1.60) 3.69 2.96 3.21 <LLOQ(1.60) 4.18 <LLOQ(1.6Q) 3.16 8.03 <LLOQ(1.6Q) 2.22 <LLOQ(1.60) 5.43 5.20 PFOSA Concentration* <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.0Q)** <LLOQ(1.00)** M556 Concentration* <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 2.94 <LLOQ(2.50) 5.33 <LLOQ(2.50) 4.53 7.59 M570 Concentration* 1,36 2.32 2.93 <LLOQ(1.00) <LLOQ(1.00) 1.85 2.55 <LLOQ(l.Q0) 1.29 3.59 2.48 1.2 4.55 <LLOQ(1.00) <LLOQ(1.00) 10.6 6.4 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 84 000422 Northwest Bioanalytical Study No. NWBS00-088 Report No. N\VBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 2349 2350 2351 2353 2355 2358 2360 2363 2365 2366 2368 2376 2386 2395 2397 2400 2406 PFOS Concentration 40.8 76.4 36.9 34.0 36.2 61.8 29.9 29.7 42.4 65.7 42.8 43.2 11.2 61.8 77.2 62.4 29.1 PFOA Concentration* 3.86 8.86 3.79 3.86 4.72 10.3 7.43 3.52 3.56 5.24 5.39 4.20 <LLOQ(1.92) 4.45 7.81 7.37 3.76 PFHS Concentration* 4.49 ' 20.3 1.76 4.51 1.62 1.79 <LLOQ(1.36) 2.65 7.62 7.92 10.5 4.50 <LLOQ(l,36) 4.20 27.2 10.5 <LLOQ(1.36) PFOSAA Concentration* <LLOQ(1,60) 13.1 <LLOQ(1.60) 2.19 <LLOQ(1.60) 2.93 5.02 6.43 <LLOQ(1.60) 4.39 2.50 3.41 5.19 10.3 7.78 3.39 <LLOQ( 1.60) PFOSA Concentration* <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** cLLOQ(l.OO)** <LLOQ(1.00)** <LLOQ(1.00) <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.0Q)** <LLOQ(1.00)** <LLOQ(l,0Q)** <LLOQ(1.00)** <LLOQ(1.00)** M556 Concentration* <LLOQ(2.50) 6.83 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 4.72 4.53 3.67 <LLOQ(2.50) <LLOQ(2.50) 3.77 <LLOQ(2.50) <LLOQ(2.50) 13.4 5.09 2.55 3.62 M570 Concentration* 5.22 16.8 cLLOQ(l.OO) 1.45 1.33 13.4 1.05 3.12 3.33 4.88 3.54 4.58 <LLOQ( 1.00) 19.5 2.89 10.4 3.5 * Serum sample results obtained using plasma curves may vary front results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 85 0Si)43 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 2431 2433 2436 2438 2440 2474 2491 2493 2495 2496 2499 2500 2514 2516 2517 2522 2524 PFOS Concentration 50.6 27.7 33.0 61.9 23.6 42.9 40.1 34.4 20.8 28.0 28.0 26.3 36.9 54.1 51.6 30.2 38.6 PFOA Concentration* 4.80 5.50 9.32 7.05 6.95 3.60 5.82 7.11 3.08 5.40 2.42 3.02 4.05 6.95 11.3 3.27 3.68 PFHS Concentration* 5.57 2.93 3.45 3.34 1.66 1.79 10.3 5.99 2.53 6.77 73.9 10.2 4.29 2.08 73.4 1.39 2.02 PFOSAA Concentration* 2.82 5.46 2.95 11.2 <LLOQ(1.60) 9.55 2.44 6.14 <LLOQ(1.60) 5.36 <LLOQ(1.60) <LLOQ(1.60) 4.66 10.1 3.02 <LLOQ(1.60) 4.65 PFOSA Concentration* <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00)** <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) M556 Concentration* 9.74 3.47 4.67 4.89 <LLOQ(2.50) 3.25 <LLOQ(2.50) 4.34 2.58 3.15 <LLOQ(2.5Q) <LLOQ(2.5Q) <LLOQ(2.50) 3.68 4.49 <LLOQ(2.50) 4.69 M570 Concentration* 9.19 <LLOQ( 1.00) 2.81 7.48 <LLOQ(1.00) 1.35 1.49 2 8.11 5.24 <LLOQ( 1.00) <LLOQ( 1.00) <LLOQ(1.00) 2.41 <LLOQ( 1.00) <LLOQ(1.00) 3.9 * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 86 000424 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 2526 2528 2531 2567 2570 2575 2577 2584 2585 2590 2593 2597 9433 9434 9435 9436 9437 PFOS Concentration 37.0 122 27.3 29.0 42.7 52.1 21.6 217 58.5 45.0 32.9 43.8 38.2 45.7 35.7 35.1 14.7 PFOA Concentration* 4.49 5.87 2.75 4.44 3.71 5.92 <LLOQ(1.92) 34.2 6.27 5.52 6.98 5.67 9.14 4.55 6.29 6.78 <LLOQ(2.88) PFHS Concentration* 3.65 2.90 1.99 <LLOQ(1.36) <LLOQ(1.36) 32.6 2.17 497 1.66 2.12 <LLOQ(1.36) 15.2 4.97 11.7 25.5 <LLOQ(2.41) <LLOQ(2.4l) PFOSAA Concentration* 4.26 4.63 1.96 2.21 3.73 8.19 <LLOQ(1.60) 8.82 9.68 2.13 2.10 3.85 5.78 3.71 <LLOQ(2.60) 4.01 <LLOQ(2.60) PFOSA Concentration* <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.00) <LLOQ(1.00) <LLOQ(i.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.00) <LLOQ(2.QO) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) M556 Concentration* <LLOQ(2.50) 12.3 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 7.53 <LLOQ(2.50) 6.27 10.9 <LLOQ(2.50) <LLOQ(2.50) <LLOQ(2.50) 5.43 <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) M570 Concentration* <LLOQ(1.00) 34.4 4.19 <LLOQ(1.00) <LLOQ(1.00) <LLOQ(2.00) <LLOQ(1.00) 2.92 22.2 10.8 <LLOQ(1.00) 3.16 <LLOQ(2.00) 2.23 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected nin (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 87 S0425 Northwest Bioanalytical Study No. NWBS00-088 Report No. NAVBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 9438 9439 9440 9441 9442 9443 9444 9445 9446 9447 9448 9449 9450 9451 9452 9453 9454 PFOS Concentration 47.7 40.5 15.0 48.0 32.3 51.6 42.1 98.9 25.2 39.8 20.4 45.1 29.8 40.1 43.5 30.5 40.2 PFOA PFHS Concentration** Concentration* 8.15 5.81 6.54 6.65 <LLOQ(2.88) <LLOQ(2.41) 5.05 <LLOQ(2.41) 4.41 4.22 7.49 <LLOQ(2.41) 6.64 9.06 6.35 88.7 3.73 <LLOQ(2.41) <LLOQ(2.88) 33.0 3.31 <LLOQ(2.41) 5.66 <LLOQ(2.41) 3.18 <LLOQ(2.41) 3.69 <LLOQ(2.41) 4.96 22.3 3.54 4.48 3.95 <LLOQ(2.41) PFOSAA Concentration* <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) 4.23 <LLOQ(2.60) 7.41 <LLOQ(2.60) 3.61 <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) 4.60 <LLOQ(2.60) 5.18 <LLOQ(2.60) <LLOQ(2.60) 4.81 PFOSA Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) M556 Concentration* <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) M570 Concentration* <LLOQ(2.00) 10.3 <LLOQ(2.00) 2.37 <LLOQ(2.00) <LLOQ(2.00) 5.59 4.88 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 6.54 4.1 <LLOQ(2.00) 2.95 <LLOQ(2.00) <LLOQ(2.00) * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (2 5 % for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 88 000425 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 9455 9456 9457 9458 9459 9460 9461 9462 9463 9464 9465 9466 9467 9468 9469 9470 9471 PFOS Concentration 25.8 66.1 35.8 31.6 62.8 18.8 29.2 40.9 28.0 17.2 16.5 50.0 49.7 49.1 80.5 28.9 55.6 PFOA Concentration* 4.74 14.94 <LLOQ(2.88) 3.39 6.12 4.09 4.08 <LLOQ(2.8S) 3.71 <LLOQ(2.88) <LLOQ(2.88) 7.50 5.98 7.10 18.64 5.32 11.5 PFHS Concentration* 3.84 20.5 2.49 3.58 3.35 17.1 <LLOQ(2.41) 23.0 3.4 2.98 <LLOQ(2.41) <LLOQ(2.41) <LLOQ(2.41) <LLOQ(2.41) 38.1 7.78 40.2 PFOSAA Concentration* 15.8 5.70 5.49 <LLOQ(2.60) 3.32 <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) 2.71 4.24 10.5 <LLOQ(2.60) 10.8 PFOSA Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) M556 Concentration* <LLOQ(5.00) 7.24 <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) M570 Concentration* <LLOQ(2.00) 7.38 <LLOQ(2.00) 5.13 2.08 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 3.67 <LLOQ(2.0Q) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matr ix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the taTget concentration. The statistical error of any individual result may exceed the QC acceptance criteria. G427 Page 89 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 9472 9473 9474 9475 9476 9477 9478 9479 9480 9481 9482 9483 9484 9485 9486 9487 9488 PFOS Concentration 54.9 34.7 43.3 57.2 40.0 22.4 33.6 14.1 42.2 33.8 33.9 ' 24.7 10.2 37.4 32.7 46.7 22.0 PFOA Concentration* 3.93 4.96 4.95 7.03 <LLOQ(2.88) 2.97 5.15 <LLOQ(2.88) 5.99 5.37 <LLOQ(2.88) <LLOQ(2.88) <LLOQ(2.88) 4.45 4.23 6.81 4.36 PFHS Concentration* 9.60 12.2 6.56 4.70 10.2 <LLOQ(2.41) <LLOQ(2.41) <LLOQ(2.41) 2.58 <LLOQ(2.41) 12.39 <LLOQ(2.41) <LLOQ(2.41) 6.54 <LLOQ(2.41) 6.40 <LLOQ(2.41) PFOSAA Concentration* 3.56 <LLOQ(2.60) 2.74 <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) 3.89 <LLOQ(2.60) <LLOQ(2.60) 6.08 <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) 4.76 4.41 3.59 <LLOQ(2.60) PFOSA Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) M556 Concentration* <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) 5.26 <LLOQ(5.00) M570 Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 2.79 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 3.12 <LLOQ(2.00) * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) of the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 90 000428 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBR01-001 Table 22. Study Sample Concentrations (Continued) All concentrations are expressed as ppb. Sample No. 9489 9490 9491 9492 9493 9494 9495 9496 9497 9498 9499 9500 9501 9502 9503 9504 9505 PFOS Concentration 27.0 21.2 60.9 30.3 31.6 20.3 41.4 33.1 97.9 49.7 29.3 30.3 35.6 17.8 29.3 34.3 27.0 PFOA Concentration** 3.04 3.88 6.41 <LLOQ(2.88) 5.43 <LLOQ(2.88) 7.57 4.76 14.64 2.93 3.76 <LLOQ(2.88) 4.70 <LLOQ(2.88) 3.22 5.14 4.75 PFHS Concentration* <LLOQ(2.41) 12.2 37.6 <LLOQ(2.41) <LLOQ(2.41) <LLOQ(2.41) 4.56 3.10 114 67.3 8.67 <LLOQ(2.41) <LLOQ(2.41) <LLOQ(2.41) <LLOQ(2.41) 10.4 4.54 PFOSAA Concentration* 6.87 <LLOQ(2.60) <LLOQ(2.60) <LLOQ(2.60) 3.83 <LLOQ(2.60) 9.31 3.04 <LLOQ(2.60) <LLOQ(2.60) 2.61 <LLOQ(2.60) 5.47 2.74 <LLOQ(2.60) <LLOQ(2.60) 5.37 PFOSA Concentration* <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) MS56 Concentration* <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) <LLOQ(5.00) M570 Concentration* 11.3 <LLOQ(2.00) 2.45 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 8.68 <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) <LLOQ(2.00) 3.02 <LLOQ(2.00) <LLOQ(2.00) 2.62 <LLOQ(2.00) * Serum sample results obtained using plasma curves may vary from results obtained from serum curves (see Results and Discussion). ** Results are from a rejected run (see Results and Discussion). The concentrations of any diluted samples have been corrected for the persistent level of analyte in the dilution matrix. The method acceptance criteria states the concentration for each QC must be within 20% (25% for PFOSA and PFOSAA) o f the target concentration. The statistical error of any individual result may exceed the QC acceptance criteria. Page 91 000429 Northwest Bioanalytical Sample No. 2168 Table 23. Repeat Analysis Table for PFOS Study No. NWBSOO-088 Report No. NWBRO1-001 Treatment Ped Time Oh Original Cone, ppb Original Reason Reassay Reassay Reported Run for Cone. Run Cone. Number Reassay ppb Number ppb >ULOQ(414) 10 1 515 14 515 Reason for Reported Cone. 1 Sample No. 2168 Table 24. Repeat Analysis Table for PFHS Treatment Ped Time Oh Original Cone, ppb Original Reason Reassay Reassay Reported Reason for Run for Cone. Run Cone. Reported Cone. Number Reassay ppb Number ppb >ULOQ(523) 10 1 712 14 712 1 REASONS FOR REASSAY: 1). Greater than the ULOQ. REASONS FOR REPORTED CONC: 1). Original result outside of quantitation range. Reassay results reported. Page 92 000430 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBRO1-001 Figure I. Representative Calibration Curve for PFOS Analytical Run 7 analyzed on 09Nov-2000 Calibration Standards fur PFOS (ng/ntL) Regression Method * QUADRATIC - Weighting Factor I/X**2 Quadratic Limit * 2000 Figure 2. Representative Calibration Curve for PFOA Analytical Run 7 analyzed on Q9-Nov-2000 Calibration Standards for PFOA (ng/mL) Regression Method QUADRATIC Weighting factor l/X**2 Quadratic Limit - 3190 Page 93 0S0431 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Figure 3. Representative Calibration Curve for PFHS Analytical Run 7 analyzed on l)`)*Nov2000 Calibration Standards for PFHS (ng/mL) Regression Method QUADRATIC - Weighting Factor * l/X**2 Quadratic Limit* 1410 Insiiument Response Figure 4. Representative Calibration Curve for PFOSAA Analytical Run 7 analyzed on 09-Nov-2000 Calibration Standards for PFOSAA (ng/mL) Regression Method QUADRATIC - Weighting Factor l/X**2 Quadratic Limita -4160 Inanimcnt Response Page 94 030432 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRO1-001 Figure 5. Representative Calibration Curve for PFOSA Analytical Run 7 analyzed un 09-Nov-2Q00 Calibration Standards for PFOSA (tig/mL) Regression Method QUADRATIC Weighting Factor * l/X**2 Quadratic Limit - 2330 Instrument Rponse Instrument R ponse Figure 6. Representative Calibration Curve for M556 Analytical Run 7 analyzed oil 09-Nov-2Q00 Calibration Standards for MSS6 (ng/mL) Regression Method QUADRATIC - Weighting Factor 1/X**2 Quadratic Limit - - !620 0 50 100 150 200 250 300 3S0 4Q0 450 500 Nominal Cone. (ng/mL) Page 95 00433 Northwest Bioanalytical Study No. NW8S0-0S8 Report No. NWBRO1-001 Figure 7. Representative Calibration Curve for M570 Analytical Run 7 analyzed on 09-Nov-2000 Calibration Standards for MS70 (ny/mL) Regression Method QUADRATIC * Weighting Factor * I/X "2 Quadratic Limit * *23900 ent Response 0 50 100 150 200 250 300 350 400 450 500 Nominal Cone. (ng/mL) Page 96 0G0434 Northwest Bioanalytieal Figure 8. Human Serum Blank for PFOS Study No. NWBS00-088 Report No. NWBROI -0 0 1 1' ' w --1 Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 4:54 Currant Method Noise Thres. 50 5.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 12 12 Base, width 150 150 RT Win. (secs) 20 20 Smooth 1 1 30008807*012 7 012 S00088 CONTROU_BLANK 1 Thu. Nov 9. 2000 9:08 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 499.Q->80.0 No Comment -+ - * iI Area 28722 HeiQht 1744 Stan Time End Time Inteoration Width Retention Time inteqraHon Type 4:30 5:17 0:48.3 4:49 A -B V mi l'tHPFS----------------usa as Internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mutt Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $0008807-012 7 012SOO88CONTROL.BLANK1 Thu. Nov 9. 2000 9:08 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans No Comment 427.Q->407.0 Area 0 Heiahr 0 Start Time End Time Inteoration Width Retention Time inteoration Type 0:00.0 0:00.0 0:00.0 0:00.0 intensity : 25 cps Page 97 000435 Northwest Bioanalytical Figure 9. Human Serum Blank for PFOA Study No. NWBS00-088 Report No. NWBRQl-001 (PUJA---------------------------------1 internal Standard: THPFOS * AOsokrte Retention Time Expected RT 4:27 Current Method Noise Three. t.O 1.0 Quant Thres. ii, Q.9 Min. Width 33 Mud Width 99 Base. Width 1ST 150 RT Win (secs) 0 20 Smooth 11 *0009807-012 7 012 S0008S CONTROL.BLANK t Thu. Nov 9. 2000 9:00 PM S:S9 in 1period 1: 9:59 MRM. 571 scans 413.0-1S9.0 No Comment 231 Area 2055 Height 213 Start Time End 'rime Integration Width Retention Time integration Type I t l+MHB 4FT3 <:<4 0:32.1 4 3TT5i ma M10' * .101 1 :33 33 intensity : 227 ops 303 SOI 7:34 Taicmjn*r|$T" ItHffSS""' .......... use as Internal Standard Expected RT 4:15 Current Method Noise Thres. tO.Q 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 M ult Width 10 10 Base. Width 150 150 RT VMn. (secs) 20 20 Smooth 1 1 30008607-012 7 012 S00088 CNTROU.BLANK 1 Thu. Nov 9. 2000 9:08 PM 8:59 in 1 period No Comment 1: 8:59 MRM. 571 scans 427.0->407.0 Area Q HeiQht 0 Start Time End Time Intearation Width Retention Time imearaiion Type itl4hHai 0:00.0 0:00.0 0:00.0 0:00.0 mW intensity: 23 ops Page 98 0S043 Northwest Bioanalvtieal Sturiy No. NWBSOO-088 Report No. NWBR0I-00I Figure 10. Human Serum Blank for PFHS Internal Slandard: THPFOS Use Area Absolute Retention Time Expected RT 3:37 Current Method Noise Threa. 3.0 3.0 Quant Thres. 0.5 0.5 Min. Width 44 Mult. Width 12 12 Base, width 150 150 RT Win. (secs) 20 20 Smooth 1 1 sOO8807-012 7 012 S00068 CONTROL BLANK 1 Thu, Nov 9. 2000 9:08 PM 8:59 in 1 period 10Q i 1: 8:59 MRM, S71 scans 90- 399.0'>80.0 Area 1410 Height 128 Start Time End Time Integration Width Retention Time Integration Type 3:29 3:59 0:30.3 3:48 A - BB HQ 307060- 40- 20- ITH^S use as Internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 to Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S008807-Q12 7 012 S00088 CONTROL_BLANK 1 Thu. Nov 9. 2000 9:08 PM 8:59 in 1 period No Comment 1: 8:59 MRM. 571 scans 427.0->407.0 -* * X 1 Area 0 Height 0 Start Time End Time Integration Width Retention Time Integration Tvoe 0:00.0 0:00.0 0:00.0 0:00.0 H IU J I intensity : 133 cp* 501 Scaoi 7 :54 Timely Page 99 000437 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBR01-00! Figure 11. Human Serum Blank for PFOSAA IPFOSAA ~1 Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5:56 Current Method Noise Thres. 4.0 4.0 Quant Thres. 1.5 t.S Min. Width 3 3 Mult. Width 13 13 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 *0008807.012 7 012 SOOQ60 CQNTROLJ3LANK 1 No Comment Thu. Nov 9. 2000 9:09 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 5 8 4 .1 . >419.1 Area ! 020 Height 129 Start Time End Time Integration Width Retention Time Integration Type 5:51 6:06 0:15.1 5:58 A BB 0153 ITHPFOS use as Internal Standard Expected RT 4:15 Current Method Noise Thres. 10,0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S008807-012 7 012S00088CONTROl_SLANK 1 No Comment Thu. Nov 9. 2000 9:08 PM 8:59 In 1 period 1: 8:59 MRM. 571 scans 427.0->407.0 Area 0 Height 0 Start Time End Time Integration Width Retention Time integration Type i+ u -m m 0:00.0 0:00.0 0:00.0 0:00.0 00 Page 100 000438 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBR01-001 Figure 12. Human Serum Blank for PFOSA IPFOSA ~l Internal Standard: THPPQS Use Area Absolute Retention Time Expected RT 5:35 Current Method Noise Thres. 3.0 3.0 Quant Thres. 0.3 0.3 Min. Width 5 5 Mult. Width 10 10 Base. Width 150 150 RT Win. tsecsl 20 20 Smooth 1 1 *0008807-012 7 012 S00068 CONTRQL.BLANK t No Comment Thu. Nov 9. 2000 9:08 PM 8:59 in 1 period t: 8:59 MRM, 571 scans 498.0*78.Q Area 3039 Height 202 Start Time End Time Integration Width Retention Time Integration Tyoe Itl+ t H ffl 5:11 5:50 0:38.8 5:42 AW BED 3*2 intensity : 209 cps 493 501 7:54 ITHPFOS use as Internal Standard Expected RT 4:15 I Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 SOOO08O7-O12 7 012 S00088 CONTROl^BLANK 1 No Comment Thu. Nov 9. 2000 9:08 PM 8:59 in t period 1: 8:59 MRM. 571 scans 427.0->407.0 m X * -* 4- Area Heioht 0 0 Start Time End Time Intearatfon width Retention Time integration Tyoe 0:00.0 0:00.0 0:00.0 0:00.0 ih ia I intensity : 23 cps Page 101 000439 Northwest Bioanalyticai Study No. NWBS00-088 Report No. NWBRO1-001 Figure 13. Human Serum Blank for M556 IM556 internal Standard: THPFOS Usa Area Absolute Retention Time Expected RT 5:25 I Current Method Noise Thres. 0.4 0.4 Quant Thres. 0.1 0.1 Min. Width 33 M ult Width 10 10 8asa. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 s0003807-012 7 012 S00038 CONTROL.8LANK 1 No Comment Thu. Nov 9. 2000 9:08 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 556.0->498,Q Area 155 Heraht 55 Start Time End Time inteqnallon Width Retention Time Integration Type im H H M 5:20 5:27 0:07.8 5:25 A - BB B id IthTO------ use as internal Standard Expected RT 4:15 1 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S0008807-012 7 012 soooaa CONTRQL_BLANK t Thu. Nov 9. 2000 9:08 PM 8:59 in 1 period toon No Comment 287 intensity : 25 $ps 1: 8:59 MRM. 571 scans 90 427.0**407.0 30- Area 0 Heiahl 0 Start Time End Time ntearaon width Retention Time intearatton Type ItU H H fl 0:00.0 O'.QO.Q 0:00.0 0:00.0 003 70 60- 50 20 69 40 164 30 20 10 0 101 201 I :35 3:10 367 430480 11 30t 4.45 401 6.19 501 Tirr.*{. ; Page 102 0 G0 4 4 0 Northwest Bioaiialytical Study No. NWBS00-088 Report No. NWBRO1-001 Figure 14. Human Serum Blank for 1YI570 Im sto Internal Standard: THPFQS Use Area I Current Method Noise Thres, 3.0 3.0 Quant Thres. 0,5 0.5 Min. Width 5 5 Absolute Retention Time Mutt, width 15 15 Expected RT 5.38 Base. Width 150 ISO RT Win. (secs) 20 20 Smooth 1 1 S00088Q7-012 7 012 SOOS8 CONTROU_0LANK I Thu. Nov 9, 2000 9:08 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 570.0-4ig.1 No Commant -* - 4 I 1 Area 1074 Height 144 Start Time End Time integration Width Retention Time Integration Type 5:37 5:58 0:18.9 5:44 A 88 ay Il'H P ftJ S use as Internal Standard Expected RT 4:15 1 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 t S000807-012 7 012 S088 CONTROL_BLANK 1 No Comment Thu. Nov 9. 2000 9:08 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 427.0->407.0 Area 0 Height 0 Start Time End Time Integration Width Retention Time integration Type 0:00.0 0:00.0 0:00.0 0:00.0 intensity: 23 ops Page 103 000441 Northwest Bioamilytical Study No. NWBSOO-088 Report No. NWBRO1-001 Figure 15. Human Serum Blank with Internal Standard (QCO) tor PFOS IPFOS internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 4:54 1 Current Method Noise Thres- 5.0 5.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mutt. Width 12 12 Sasa. Width 150 150 RT Win. (sacs) 20 20 Smooth 1 1 sQQQaa07*QQ1 7 Q1 S00Q86 QCO 1 Thu. Nov 9. ZOQQ 7:00 PM 8:59 in t period 1: 8:59 MRM, 571 scans 499O*>0O.O No Comment Area 39395 Height 2805 Start Time End Time Integration Width Retention Time Integration Type 4:34 5:32 0:57.7 4:50 A -B V BlAl it H P F O S use as Internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 1Q.Q Quant Thres. 0.2 0.2 Min. Width 3 3 M ult Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 sOOO0BO7-OOt 7 001 S0088 QCO 1 No Comment Thu. Nov 9. 2000 7:QQ PM 8:59 in 1 period 100- 1: 8:59 MRM, 571 scans 427.0-407.0 Area 273196 Height 35433 Start Time End Time Integration Width Retention Time integration Type itiiN M i C(OO < 4:12 4:46 0:33.1 4:26 sa 90* RO TO SO- 30- 4030so to- 231 TOI 1:33 201 3:10 301 4:43 intensity : 334 34 epe 401 6:19 SOI 7:34 TiCrrift.r Page 104 000442 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBRO1-001 Figure 16. Human Serum Blank with Internal Standard (QCO) for PFOA Internal Standard: THpFOS Absolute Retention Time Expected RT 4:27 Current Method J Noise Ihres. 1.0 1.0 Quant Three 0.9 0.9 Min. width 33 Mull Width 99 Base. Width i5 150 RT Win. (secs) 0 20 Smooth 1 ! 7 0O1 S0088 QCO 1 [ W F 1 --------------------------------1 usa as Internal Standard Expected RT 4:15 Current Method Noise Three. 10.0 10.0 Quant Thras. 0.2 Q.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 150 RT Win. (sacs) 20 20 Smooth t 1 S0Q08607-0O1 7 001 200068 QCO t No Comment Thu. Nov 9. 2000 7:00 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans lOO-i 90- 427.0->4070 Area 273196 Height 35433 Start Time End Time Integration Width Retention Time integration Type [ts ii 4:12 4:46 0:33.1 4:26 A - 88 807060504030* 20- 10- 281 Tot 1 2oT 1:35 3.1' 301 4:45 intensity : 35434 ops 401 6:19 501 7:54 T5iCmi*r|r-.-- Page 105 000443 Northwest Bioanalytieul Study No. NWBS00-088 Report No. NWBRO1-001 Figure 17. Human Serum Blank with Internal Standard (QCO) for PFHS IPFHS Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 3:37 1 Current Method Noise Three. 3.0 3.0 Quant Thres. 0.5 0.5 Min. Width 44 Muit Width 12 12 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 SQ0Q8807-! 7 001 SO0O88 QCO 1 No Comment Thu. Nov 9. 2000 7:00 PM 3:59 in 1 period I00-] 1: 3:59 MRM. 571 scans 399.0*>80.0 Area 1769 Hetqht 193 Start Time End Time Integration Width Retention Time Integration Type Itl +HHMfi 3:39 3:59 0:19.9 3:50 A - B0 mm 90eo70eo* 40- 20- 101 t :33 intensity : 200 eps 412 itHPgas .... ........ use as Internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 M ult Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 s00cae07-001 7 001 soooea QCO 1 Thu. Nov 9. 2000 7:00 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 4 2 7 .0-M 07.0 N Comment Area 273198 Height 35433 Sian Time End Time integration Width Retention Time Integration Tvoe ItN kM fel 4:12 4:40 0:33.1 4:2S A -S B mm Page 106 000444 Northwest Bioanalytiual Study No. NWBS00-088 Report No. NWBRO1-001 Figure 18. Human Serum Blank with Internal Standard (QCO) for PFOSAA IPFOSAA Internai Standard: THPFOS Use Area Absolute Retention Time Expected RT 5:50 I Current Method Noise Hires. 4.0 4.0 Quant Three. 1.5 1.5 Min. Width 3 3 Mult Width 13 13 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $0008807-001 7 001 S00088 QCO 1 Thu. Nov 9. 2000 7:00 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 584.1-419.1 No Comment Area 0 Heioht 0 Start Time End Time Iniearaiion Width Retention Time Integration Tvoe m im a i 0*00.0 0:00.0 0:00.0 0:00.0 00 intensity : 92 cps use as Internal Standard Expected RT 4:15 Current Method Noise Hires. 10.0 10.0 Quant Three. 0.2 0.2 Min. Width 33 Mult. Width 10 10 Base, width 150 150 RT Win. (secs) 20 20 Smooth 1 1 SOO8807-001 7 001 S00068 QCO 1 NO Comment Thu. Nov 9. 2000 7:00 PM 8:59 In 1 period 1: 3:59 MRM. 571 scans 427.0->4O7.Q Area 273196 Heiqht 35433 Start Hme End Time Inteoration Width Retention Time Inteoration Type 4:12 4:48 0:33.1 4:26 A -B 8 00 SO BO- 70- 6030- 40- 30- 20- 10- 0-1------ 1------ i------ .------ 1------ 1 .... 101 201 -501 1:35 3:10 4:43 intensity : 33434 ops -- P-- 401 6.19 30! 7:34 Page 107 000445 Northwest Bioanalytical Study No. NWBS0Q-088 Report No. NWBR01-001 Figure 19. Human Serum Blank with Internal Standard (QCO) for PFOSA IppoSa 1 ' internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5:35 Current Method Noise Thres. 3.0 3.0 Quant Hires. 0.3 0.3 Min. Width 5 S Mult. Width to to Base. Width 150 150 RT Win. (secs) 20 20 Smooth t 1 $0008807-00 1 7 001 soooae QCO I No Comment Thu. Nov 9. 2000 7:00 PM 8:59 in 1 period 1: 8:59 MRM. 371 scans 498.0-*7S,0 Area 0 Height 0 s u i t Time End Time Integration Width Retention Time Integration Type 0:00 0 0:00.0 0:00.0 0:00.0 too9030701 6050 40- 26 124 liliteM M S B 361 to t I :33 intensity : 59 cps ITHPFS ~ use as Internal Standard Expected RT 4:15 I Current Method Noise Three. 1Q.0 1Q.0 Quant Thres. 0.2 0.2 Min. Width 33 M ult Width 10 10 Base. Width ISO 150 RT Win. (secs) 20 20 Smooth 1 1 S0008807-001 7 001 S00088 QCO 1 No Comment Thu, Nov 9. 2000 7:00 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 427.0-407.Q Area 273198 Height 35433 Start Time End Time Integration Width Retention Time integration Type itl+ H H fl 4:12 4:48 0:33.1 4:28 A B8 E ia ltW9080- 70- 60- 50- 40- 30- 2010-- t t 1 :35 20t 3:10 301 4.4! intensity : 35434 cps 401 6:19 50t i-lflI' 7 34 Tir**| : Page 108 000446 Northwest Biouiulytical Study No. NWBS00-088 Report No. NWBROt-OOl Figure 20. Human Serum Blank with Internal Standard (QCO) for IV1556 IM54a Internal Standard: THPFOS Use Area I Current Method Noise Thres. 0.4 0.4 Quant Thres. 0.1 0.1 Min. Width 3 3 Absolute Retention Time Mult. Width 10 10 Expected RT 5.25 Base. Width 150 150 RT Win. (sacs) 20 20 Smooth I 1 S00Q88Q7-Q1 7 001 S00088 QCO t Thu. Nov 9. 2000 7:00 PM 8:59 in I period 1: 8:59 MRM, 571 scans 550.0->498.Q No Comment Area 0 Height 0 Start Time End Tima Integration width Retention Tima Integration Type 0:00.0 0:00.0 0:00.0 0:000 ISSU |Th p F5 3 use as internal Standard Expected RT 4:15 1 Current Method Noise Thres. 10.0 10.0 Quant Three. 0.2 0.2 Min. Width 3 3 Mutt Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 30008807-001 7 001 S00088 QCO 1 No Comment Thu. Nov 9. 2000 7:00 PM 8:59 in 1 period 1 : 8:59 MRM. 571 scans 90- 4- 4 I m 427.0->407.0 Area 273196 Meiqhl 35433 Start Time End Time Intearation width Retention Time Integration Type 4:12 4:46 0:33.1 4:28 A -B 8 am 80- 70- 80- 50- 40- 30- 20- !0- 0-|--- ,----,--- .--- ,---- 10I 2 0 1 1-.35 3 :1 0 301 4:45 intensify : 35434 cps 401 501 6:19 Tinr*J.-; Page 109 000447 Northwest Bioanalytkal Study No. NWBS00-088 Report No. NWBRO1-001 Figure 21. Human Serum Blank with Internal Standard (QCO) for M570 IM570 Internai Standard: THPFOS Use Area ADsoUite Rtention Time Expected RT 5:38 I Current Method Noise Thres. 3.0 3.0 Quant Thres. 0.5 0.5 Min. Width 5 5 Mutt. Width 15 15 Base. Width 150 150 RTWln. (secs) 20 20 Smooth 1 1 S0008807-001 7 001 S00088 QCO I Thu. Nov 9. 2000 7:00 PM 8:59 in 1 penod 1: 3:59 MRM. 571 scans 570.0-419.1 No Comment Height Start Time End Time integration Width Retention Time Integration Type ItHHHHftI 0:00.0 0:000 E intensity : 71 cps ITHPFQ^ use as Internal Standard Expected RT 4:15 j Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 150 RTWln. {secs) 20 20 Smooth 1 1 30008607*001 7 001 S00088 QCO 1 Thu. Nov 9. 2000 7:00 PM 9:59 in 1 period 1: 9:59 MflM, 571 scans 427.0-407.Q No Comment Area 273198 Heiqhl 35433 Start Time End Time Inteoration Width Retention Time Integration Type itUMHtil 4:12 4:48 0:33.1 4.28 A BB HQ intensity : 354 34 cps Page 110 000448 Northwest ioanalytieal Study No. NWBSOO-088 Report No. NWBROl-OOl Figure 22. Low Standard (3.94 ppb) for PFOS IPFOS Internal Standard: THPFOS Usa Area Absolute Retention Time Expected RT 4:54 Current Method Noise Thres. 5.0 5.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult, width 12 12 Base, width 150 150 RT Win. (secs) 20 20 Smooth 1 SOQ088Q7-QQ2 7 002 S00088 S tdl 1 t Thu. Now 9. 2000 7:11 PM 3:59 m 1 period 1: 8:59 MRM. 571 scans 100- so- 499.0*>80.0 Area 46519 HeiqM 3423 Start Time End Time integration Width Retention Time Integration Type 4:31 5:28 0:56.7 5:01 A-BV 3070- so- 40- OE M i S S 2,> to- No Comment ITHPO use as Internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 1Q.Q Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $0008607*002 7 002 500088 Std1 1 1 Thu. Nov 9. 2000 7:11 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 427.0-M7.0 Area 270289 Height 36113 Start Time End Time Integration Width Retention Time Integration Type (tj+m i 4:12 4:47 0:35.0 4:25 A-BB s ts No Comment in te n sity: 3 1 14 ops Page 111 000445 Northwest Biounalytieal Study No. NVVBS00-088 Report No. NWBROl-OOl Figure 23. Low Standard (1.92 ppb) for PFOA Internai Standard: THPFQS Use Area Absolute Retention Time Sipected RT 4:27 Current Method Noise Thres. 1.0 1.0 Quant Thres. 0.4 0.9 Min. Width 33 Mull. Width a9 Base. Width iso 150 RT Win. (secs) 0 20 Smooth t t S0QM07-002 7 002 soooaa sid i 11 ITH^FOS uso as internal Standard Expected RT 4:15 Current Method Noise Thres. to.o 10.0 Quant Three. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 150 RT win. (secs) 20 20 Smooth 1 1 SQQ0807-Q02 7 002 soooaa suti 1 1 Thu, Nov 9. 2000 7:11 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans too90- 427.0->407.0 80- Area 270289 Heiqnt 38113 Start Time End Time intearatkm width Retention Time integration Tvoe 4:12 4:47 0:35.0 4:25 A . SB SO40- 230 intensity : 3 6 114 ops to i I :35 2\ 3:10 301 4:43 460:119 501 7:34 5'jfir-- Time| -. Page 112 004S0 Northwest Bioaiialytical Study No. NWBSOO-088 Report No. NWBRO1-001 Figure 24. Low Standard (1.36 ppb) for PFHS IPFHS Internal Standard: THPFOS Usa Area I Current Method Noise Thres. 3.0 3.0 Quant Thres. O.S 0.5 Min. Width 44 Absoluta Retention Time Mult, width 12 12 Expected RT 3:37 Base. Width RT Win. (sacs) ISO 20 ISO 20 Smooth t 1 S08B07-02 7 002 S00088 Std1 1 1 Thu. Nov 9. 2000 7:1 1 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 399.0*>80.0 Area 14877 Haiqht 1486 Start Time End Time Intearatlon Width Retention Time Integration Type 3:25 4:01 0:35.9 3:48 A - 8B im M H fii e s q No Comment in U n s ity : 1492 eps itH P F O S use aa Internal Standard Expected RT 4:15 I Current Method Noise Three. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 M ult Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S0008807-002 7 002 S00088 Stdi 1 1 Thu. Nov 9. 2000 7:11 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 100-1 90- 427.0->407.0 Area 270289 Hekjht 38113 Start Time End Time fnteoration Width Retention Time Inteoraon Type a 4:12 4:47 0:35.0 4:25 A-aa ik 807080- 403020- No Comment 280 intensity : 361 1 4 cps 1I I :35 230:110 301 4:43 40.1t 9 501 7:34 bTi<rr.ftJr.< Page 113 0G0451 Northwest Bioanalytical Study No. NWDS0O-O88 Report No. NWBRQ1-00I Figure 25. Low Standard (1.60 ppb) for PFOSAA Ip f q Sa a Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5:56 I Current Method Noise Three. 4.0 4.0 Quant Thres. 15 1.5 Min. Width 3 3 Mult. Width 13 13 Base, width 150 150 RT Win. (secs) 20 20 Smooth 1 1 30000807-002 7 002 SOQOaa Std1 1 Thu. Nov 9. 2000 7:11 PM 8:59 in 1 period 100-1 1: 8:59 MRM. 571 scans 90- 584.1->419.1 Area 8684 Hekiht 727 Start Time End Time Inteoratlon Width Retention Time Intaoration Tyoe Itl+M Hii 5:37 8:07 0:30.3 5:56 A -aa mM 307060- 40*020 10 0- 1 :$5 intensity : 750 cps 376 IthfrFS............. use as Internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult, width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 SOOO80O7-OO2 7 002 S00088 Sldt 1 1 Thu. Nov 9. 2000 7:11 PM 6:59 in 1 period 1: 8:59 MRM. 571 scans 427.0->407.0 Area 270289 Heiqht 36113 Start Time End Time inteoratlon Width Retention Time Inteqration Type Itlik M l 4:12 4:47 0:35.0 4:25 A - 88 S IS No Comment Page 114 000452 Northwest Bioanalytkal Study No. NWBS00-088 Report No. NWBROl-OOl Figure 26. Low Standard (1.00 ppb) for PFOSA IpfoSa imamat Standard: THPFOS Use Area Absolute Retention Time Expected RT 5:35 I Current Method Noise Thres. 3.0 3.0 Quant Thres. 0.3 0.3 Min. Width 5 S Mult. Width 10 to 8ase. Width 150 150 RT Win, (secs) 20 20 Smooth 1 1 SQ08807-002 7 Q2 soooaa Std1 1 1 Thu, Nov 9. 2000 7 I t PM 8:59 In period 1: 8:59 MRM, 571 scans IDO90 498.0->78.Q Area 23612 Weioht 2540 Start Time End Time integration Width Retendon Tima Inteoration Type iilM stettl 5:15 5:55 0:39.7 5:41 A * SB ESQ SO TO SOSO' 40- 30- 20- 10- 0- No Comment intensity : 2543 cps 361 1VWQ5 "" ------ use as internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 MulL Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $0006507-002 7 002 S00068 Std1 1 1 Thu. Nov 9. 2000 7:11 PM 8:59 in t period 1: 8:59 MRM. 571 scans 427.0->407.0 Area 270289 Hekiht 36113 Start Time End Time integration Width Retention Time Inteoration Type m+M Hl 4:12 4:47 0:35.0 4:25 a-as Istigo No Comment Page 115 000463 Northwest ioanalytieal Study No. NWBS00-088 Report No. NWBR01-001 Figure 27. Low Standard (2.50 ppb) for IYI556 IM65S Internat Standard: THPFOS Use Area Absolute Retention Time Expected RT 5.42 I Current Method Noise Thres. 0.4 0.4 Quant Thres. 0.1 0.1 Min. Width 33 Mult. Width to 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 30008607-003 7 003 S00088 St2 1 1 Thu. Nov 9, 2000 7:23 PM 8.98 in 1 period 1: 8.98 MRM, 571 scans 558.0->498.0 Area 5991 Heidhl 769 Start Time End Time Inteqration Width Retention Time Inteqration Tvoe L-tlitefaHM 5.15 5.63 0.47 5.44 A-BB m i No Comment ITHPFOS use as Internal Standard Expected RT 4.25 I Current Method Noise Thres. 10.0 10.0 Quant Three. 0.2 0.2 Min. Width 33 Mult. Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 30008807-003 7 003 SOOO0 SW2 1 1 No Comment Page 116 0464 Northwest Bioaindytieal Study No. NWBSOO-088 Report No. NWBRO1-001 Figure 28. Low Standard (1.00 ppb) for M570 IMS7 Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5:38 I Current Melhod Noise Thres. 3.0 3.0 Quant Thres. 0.5 0.5 Min. Width S5 Mult, width 15 15 3ase. Width 1S0 150 RT Win. (secs) 20 20 Smooth 1 1 30008807-002 7 002 SOOO08 Sld1 1 1 Thu. Nov 9. 2000 7:11 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 100-1 90- 570.0-419.1 30- Area 9166 Height 1236 Start Time End Time Integration Width Retention Time Integration Tvoe Itl+H H M 5:29 5:58 0:27.4 5:43 A-SB HQ 6040- 2100-` No Comment use as Internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 30008807-002 7 002 S0008S Sldt 1 1 Thu. NOv 9. 2000 7:11 PM 8:59 in period 1: 8:59 MRM, 571 scans 1Q-1 90- 427.0->407.Q -oj o0 Area 270289 Height 36113 Start Time End Time integration Width Retention Time Integration Type 4:12 4:47 0:35.0 4:25 A-SB ItH M H 1 S&AI 605040- 20ta ci No Comment 10315 230 50! 4.43 intensity : 36114 cps 401 6:1*3 SCI Scn< 7 :54 Tin'i| < Page 117 000455 Northwest Bioanalytical Study No. NWBSOO-088 Report No. NWBR01-001 Figure 29. High Standard (414 ppb) for PFOS IPFOS " Internat Standard: THPFQS Usa Area Aosotule Retention Time Expected RT 4:54 Current Method Noise Thres. 5.0 5.0 Quant Thres. 0.2 0.2 Min. Width 33 Utufr. Width 12 12 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S008807-010 7 010S00Q88Std9 1 t No Comment Thu, Nov 9. 2000 8:45 PM 8:59 in T period 1: 8:59 MRM. 571 scans 499 0-30.0 Area 3453475 Height 285223 Start Time End Time Integration Width Retention Time Integration Tvoe li.L4feHfll 4:22 8:04 1:42 5:01 A -B V E ico ro soTO SOso40- 302010- 101 2010-1------- 1-------1-------.------1-- 1:33 3:10 intensity : 239227 epa 313 4:45 6:19 501 7:54 STcmafatiOjj ItHfrftte ............... use as internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 M ult Width 10 10 Base. Width 150 150 RT Win. (saca) 20 2Q Smooth 1 1 $0008807-010 7 010 S00088 Std9 1 1 Thu. Nov 9, 2000 8:45 PM 8:59 in 1 period 100* t: 8:59 MRM. 571 scans 90- 427.0*407.Q Area 225323 Height 28708 Start Time End Time Integration Width Retention Time Integraon Tyne a s 4:12 4:46 0:34.0 4:26 A-BS e 8070SO SO4030' 20- 10- No Comment 231 101 201 301 1 :35 3:10 4:43 intensity : 23710 ops Tim*j:<4I 6:19 501 7:54 ktiiWir-- - Page 118 S04* Northwest Bioanalytieal Study No. NWBSOO-088 Report No. NWBR.01-001 Figure 30. High Standard (481 ppb) for PFOA |HPO*---------------- "" Incarnai Standard: THPFOS Usa Area Absolute Retention Time ExpeaedRT 4:27 Current Metnod Noise Thres. 1.0 1.0 Quant Thres. d.9 0.9 Min. Width 33 Mult. Wioth 99 Base. Width 1S0 RT Win. (secs) i t 20 Smooth 11 sOOQ98Q7*QlO 7 o to S00M Std 1 1 Thu, Nov 9. 2000 a:45 PM 9:59 in 1 period 1: 9:59 MRM, 571 scans 413.0** 169.0 m ?z + - Area iSiUSS Height 14592 Stan Time End Time integration Width Retention Time integration Type ^5 5 A 'U " ns ~ 3 8 -------A -a v B2E1 No Comme intensity : 143333 cpi ITHpftSs use as Internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult. Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 S0008807-Q10 7 010S 00068S td91 1 Thu. Nov 9. 2000 5:45 PM 5:59 in 1 period IDO-i 1: 3:59 MRM, 571 scans 90- 427.0**407.0 Area 225323 Height 28705 Start Time End Time Intearation Width Retention Time integration Type itl+w H ai 4:12 4:48 0:34.0 4:28 A-BB 307060- 403020- No Comment intensity : 23710 ops 101 201 301 401 301 'iOrif* I :3S 3:10 4 .43 S :I9 ?;34 Timej r. Page 119 0S0457 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBR01-001 Figure 31. High Standard (523 ppb) l'or PFHS IPFHS Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 3:37 I Current Method Noise Thres. 3.0 3.0 Quant Thres. 0.5 0.5 Min. Width 4 4 Mult. Width 12 12 Base, width ISO 150 RT Win. (secs) 20 20 Smooth 1 1 30000807-010 7 010 S00088 Sld9 1 1 Thu. Nov 9. 2000 8:45 PM 0:59 in 1 period 1: 8:59 MRM. 571 scans 399.O->0O.Q Area 2879090 Heiqht 274134 Start Time End Time intearation Width Retention Time Intearation Type iti-t-M H i 3:20 4:46 1:25 3:48 A -B V mm No Comment intensity : 274143 ops ITHPFOS use as Internal Standard Expected RT 4:1 I Current Method Noise Three. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 M ull Width 10 10 Base. Width 150 150 RTWIn. (secs) 20 20 Smooth 1 1 30000807-010 7 010 S00098 Std9 1 1 Thu. Nov 9. 2000 3:45 PM 8:59 in 1 period t: 6:59 MRM. 571 scans 427.0->407.0 Area 225323 Height 28708 Start Time End Time Intearation Width Retention Time intearation Type Itl+HHMifiN 4:12 4:46 0:34.0 4:26 A -as HBI No Comment Page 120 0G0458 Northwest Bioanalytieal Study No. NWBSOO-088 Report No. NWBRO1-001 Figure 32. High Standard (501 ppb) for PFOSAA 1PFQSAA ~" ' Iniemai Standard: THPFOS Usa Area Absoiute Rtention Time Expected RT 5:56 Current Method Noise Thres. 4.0 4 0 Quant Thres. 1.5 1.5 Min. Width 3 3 Mult. Width 13 13 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 50008807-010 7 010 S00066 S109 1 1 Thu. Nov 9, 2000 8:45 PM 8:59 in 1 period t: 8:59 MRM. 571 scans S84.1419.t Area 1S56445 Height 174924 Start Time End Time Integration Width Retention Time Integration Type im HHHB 5:29 0:52 1:23 5:58 A - BV sa No Comment intensity: i 74931 ps IflHPWS""" ~l use as Internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 M ull Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 50006807-010 7 010 S00088 Std9 1 1 Thu. Nov 9. 2000 8:45 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 427.0->407.0 Area 225323 Height 28708 Start Time End Time Integration Width Retention Time Integration Type itirra s iu > aa 4:12 4:48 0:34.0 4:26 No Comment Page 121 000469 Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBRQl-001 Figure 33. High Standard (500 ppb) for PFOSA IPFOSA Internal Standard: THPPOS Use Area Absoluta Retention Time Expected RT 5:35 Current Method Noise Thres, 3.0 3.0 Quant Thres. 0.3 0.3 Min. Width 5 5 M ult Width 10 10 Base. Width ISO 150 RT Win. (sacs) 20 20 Smooth 1 1 SOB807-010 7O1OSoa08Std9 1 1 Thu. Nov 9. 2000 8:45 PM 8:59 in 1 period 1: 8:59 MRM. 571 scans 498.0*>78.0 Area 777B824 Heioht 682348 Stan Time End Time integration Width Retention Time Integration Type Itl+N H I 5:12 8:39 1:27 5:41 A -B V 100-1 9030701 60- 40- 20- No Comment "T 1:3S 201 3:10 intensity : 632470 dps 361 1 301 4:45 401 6 :I9 501 Scartpr- 7:54 Timej irnpflte--------- use as Internai Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Ttiras. 0.2 0.2 Min. WWlh 3 3 M ult Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $0008807-010 7 010 S00088 Std9 1 1 Thu. Nov 9. 2000 8:45 PM 8:59 in 1 period 1: 8:59 MRM. 57t scans 427.0->407.0 Area 225323 Height 28708 Start Time End Time Integration Width Retention Time Integration Type 4:12 4:48 0:34.0 4:26 mCD < 100-1 903070 60- 40- O- 10- No Comment 281 lOI '201 1-35 3:10 30t 4:45 intensity : 287IO cps r r401 ~50~ Scan 6:1' 7:54 Time Page 122 0S4& Northwest Bioanalytical Study No. NWBS00-088 Repon No. NWBRO1-001 Figure 34. High Standard (500 ppb) for M556 IM55 Internai Standard: THPFOS Use Area Absolut Rtention Time Expected RT 5:25 I Current Method Noise Thres. 0.4 0.4 Quant Thres. 0.1 0,1 Min. Width 33 Mult. Width 10 10 Base. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $0008807-010 7 010 S0088 Std9 1 1 Thu. Nov 9. 2000 8:45 PM 8:59 in 1 period t: 8:59 MRM. 571 scans 556.0->498.0 Area 964595 HeiQht 111295 Start Time End Time intearation Width Reteniion Time Intearation Type itiikHa 4:55 8:04 1:09 5:26 A -B V gam No Comment [THPFOS use as Internai Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 33 Mult. Width 10 10 8asa. Width 150 150 RT Win. (secs) 20 20 Smooth 1 1 $0008807-010 7 010 S0Q088 Std9 1 1 Thu. Nov 9. 2000 a:45 PM 9:59 in 1 period 1: 8:59 MRM, 571 scans 427.0-*407.0 Area 225323 Height 28708 Start Time End Time Intearation Width Retention Time Intearation Type ItH H HM 4:12 4:48 0:34.0 4:28 A - 88 OEJ 100-i 908070- 60- 504030- 20- 10- No Comment 281 to i I :35 201 3:10 301 4:45 intensity : 28? 10 cps --I----T" 401 5 0 1 Scali t 6:19 7 :5 4 Tirr.e|-. Page 123 OG0 4 6 i Northwest Bioanalytical Study No. NWBS00-088 Report No. NWBROl-OOl Figure 35. High Standard (500 ppb) for M570 IM570 Internal Standard: THPFOS Use Area Absolute Retention Time Expected RT 5:30 ! Current Method Noise Three. 3.0 3.0 Quant Thres. 0.5 0.5 Min. Width 55 Mutt. Width 15 15 8ase. Width t50 150 RT Win. (secs) 20 20 Smooth 1 1 30008007*010 7 010 SQ0088 Std9 1 1 Thu. Nov 9. 2000 0:45 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 57Q.Q->419.1 Area 2494791 Heiaht 303847 Start Time End Time Integration width Retention Time Integration Type itiiK H fiH 5:21 0.40 1:24 5:43 SS > a < No Comment intensity : 303353 cps lYHrtttd----------- use as Internal Standard Expected RT 4:15 Current Method Noise Thres. 10.0 10.0 Quant Thres. 0.2 0.2 Min. Width 3 3 Mult Width 10 10 Base. Width 150 150 RT wm. (secs) 20 20 Smooth 1 1 30008007*010 7 010 S00088 Std9 1 t Thu. Nov 9. 2000 0:45 PM 8:59 in 1 period 1: 8:59 MRM, 571 scans 427.0*>407.0 Area 225323 Height 28708 Start Time End Time Integration Width Retention Time integration Type ItliH H H M 4:12 440 0:34.0 4:26 A-BB mm No Comment intensity : 23710 cps Page 124 ,(K 6 2