Ta 425 Walnut Street, Suite 1800 Cincinnati, Ohio 45202?3957 Tel: 513.381.2838 Fax: 513.381.0205 ROBERT A. BILOTT 513.357.9638 bilott@taftlaw.com June 11, 2019 BY EMAIL AND REGULAR U.S. MAIL Timothy Begley U.S. Food and Drug Administration Center for Food Safety and Applied Nutrition Outreach and Information Center 5001 Campus Drive, HFS-009 College Park, MD 20740-3835 Re: PFAS in US Food Supply Dear Mr. Begley: Within the last week, information has become available to the public confirming detections of certain PFAS in foods found within the US as a result of recent FDA testing. Please confirm the extent to which FDA was aware of the data collected on behalf of the 3M Company in 2001 that confirmed elevated levels of PFAS in the US food supply, including the following found in food1 from six different US cities: 0 14,700 PFOA in Bread (Cleveland, TN) . 2,350 PFOA in Apples (Decatur, AL) . 1,130 PFOA in Apples (Pensacola, FL) 0 1,090 PFOA in Ground Beef (Port St. Lucie, FL) . 852 PFOS in Milk (Pensacola, FL) . 693 PFOS in Milk (Columbus, GA) 1 Note that, at the time, the lowest level the analytical laboratory being used could quantify the PFAS in the food was 500 ppt, so any results below 500 were reported as (not quantifiable). A copy of the text of the report is attached (without the appendices). Taft Stettinius Hollister LLP Chicago Cincinnati Cleveland Columbus/ Dayton lndianapolis/ Northern Kentucky .f Phoenix 25162608.1 Timothy Begley June 11, 2019 Page 2 587 PFOS in Ground Beef (Mobile, AL) 573 PFOS in Milk (Cleveland, TN) 543 PFOA in Green Beans (Mobile, AL) 524 PFOA in Bread (Pensacola, FL) 504 PFOA in Ground Beef (Port St. Lucie, FL) Please also confirm the extent to which FDA (or any other agency) has assessed the impact of the American public having been exposed to such levels of PFAS in food for such an extended period of time, without their knowledge. Encl. 25162608.1 Very truly yours, WWQ. l?wv Robert A. Bilott SUMMARY OF ANALYTICAL RESULTS: FOOD STUDY The Multi-City Study was originally designed by Battelle Memorial Institute (Columbus, OH), to obtain preliminary data about the presence of fluorochemicals in foods and in drinking water to understand the potential sources of human exposure. The Multi-City Study paired each of three cities having manufacturing or commercial use of ?uorochemical products (test cities) with three cities that do not (control cities). Information on residues in selected foods was obtained from analyses of food samples collected in a market basket study. The market basket sampling of the original Multi- City Study design was implemented by Pace Analytical Services, Inc., Minneapolis, MN. The samples were analyzed for PFOS, PFOA, and FOSA by Centre Analytical Laboratories, Inc., State College, PA. The distributions of the PFOS, PFOA, and FOSA residue data by food and city category reveal similar patterns of residue concentrations in the control and test cities for each type of food. A total of 12 samples were found to contain levels of ?uorochemical residues above the limit of quanti?cation. Of the 12 samples with measurable ?uorochemical residue levels, eight were samples collected in test cities. Measurable quantities of PFOS were found in ?ve samples: four whole milk samples (three from test cities) and a ground beef sample (test city). PFOS residues found in the foods ranged from non?quanti?able levels to 0.852 ng/g. Measurable quantities of PFOA were found in seven samples: two ground beef samples (neither from test cities); two bread samples (one from a test city); two apple samples (both from test cities); and one green bean sample (from a test city). PFOA residue levels ranged from non-quanti?able levels to 2.35 ng/ g. A value of 14.7 ng/ was found for PFOA in a bread sample from a control city, but was considered ?suspect? by Centre Analytical. ANALYTICAL REPORT STUDY TITLE Analysis of PFOS, FOSA and PFOA From Various Food Matrices Using I-IPLC Electrospray/Mass Spectrometry DATA REQUIREMENTS EPA TSCA Good Laboratory Practice Standards 40 CFR 792 STUDY DIRECTOR Karen Smith, Centre SPONSOR REPRESENTATIVE Susan A. Beach, 3M ANALYTICAL REPORT COMPLETION DATE June 21, 2001 PERFORMING LABORATORY TESTING FACILITY Centre Analytical Laboratories, Inc. (Centre) 3048 Research Drive State College, PA 16801 Phone: 814-231-8032 STUDY SPONSOR 3M Environmental Technology and Safety Services Building PO Box 33331 St. Paul, MN 55133?3331 PROJECT IDENTIFICATION Centre Protocol Number: 00P-023-057 Centre Study Number: 023-057 Total Pages: 151 Centre Study No.: 023-057 Centre Protocol No: GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT Centre Study Number 023-057, entitled ?Analysis of PFOS, FOSA and PFOA From Various Food Matrices Using HPLC Electrospray/Mass Spectrometry,? conducted for 3M Environmental Technology and Safety Services, was performed in compliance with EPA TSCA Good Laboratory Practice Standards (40 CFR, Part 792) by Centre Analytical Laboratories, Inc. with the following exceptions: l. The FOSA reference substance (analytical standard) used in this study has not been characterized under 2. Specimen (egg sample) identi?cation for three samples was not according to 792.130(c) because the labels became removed from the containers. oblleol Karen Smith Date Study Director Centre Analytical Laboratories, Inc. 24mm. /;Wa as 0 Susan A. Beach Date Sponsor Representative 3M Environmental Technology and Safety Services Centre Analytical Laboratories, Inc. Page 2 of 151 Centre Study No.: 023-057 Centre Protocol No: 00P-023-05 7 QUALITY ASSURANCE STATEMENT Centre Analytical Laboratories? Quality Assurance Unit reviewed Centre Study Number 023-057, entitled, ?Analysis of PFOS, FOSA and PFOA From Various Food Matrices Using HPLC Electrospray/Mass Spectrometry?. All phases were reviewed for conduct according to Centre Analytical Laboratories? Standard Operating Procedures, the Study Protocol, and all applicable Good Laboratory Practice Standards. All ?ndings were reported to the Study Director and to management. Date Reported Date Reported Date Reported Date to to Centre to Sponsor Phase Inspected Study Director* Management Management 1. Protocol Review 02/14/01 03/23/01 02/26/01 03/23/01 2. Extraction and 02/14/01 03/23/01 02/26/01 03/23/01 Forti?cation 3. Raw Data and Draft Report 04/ 10-13/01 05/21/01 06/04/01 06/15/01 Review 4. Raw Data and Dra? Report 05/30/01 06/01/01 06/04/01 06/ 15/01 Review 5. Final Report 06/19/01 06/20/01 06/21/01 06/21/01 Review *The Study Director resided at the sponsor until 05/01/01 at which time a protocol amendment transferred Study Director duties to Centre Analytical Laboratories. MWR WE Naomi Lovallo Date Senior Quality Assurance Auditor Centre Analytical Laboratories, Inc. Page 3 of 151 Centre Study No.: 023-057 Centre Protocol No: 00P-023-057 CERTIFICATION OF AUTHENTICITY This report, for Centre Study Number 023?057, is a true and complete representation of the raw data for the study. Submitted by: Centre Analytical Laboratories, Inc. 3048 Research Drive State College, PA 16801 (814) 231?8032 Study Director, Centre: 0212210 Men SmIthj Date Study Director Centre Analytical Laboratories, Inc. Centre Analytical Laboratories, Inc. Facility Management: 0% )6hn Flaherty Date Laboratory Manager Centre Analytical Laboratories, Inc. Spo or Representative, 3M 0.0M mgr/o, Susan A. Beach Date 3M Environmental Technology and Safety Services Centre Analytical Laboratories, Inc. Page 4 of 151 Centre Study No.: 023-057 Centre Protocol No: 00P-023-057 STUDY IDENTIFICATION Analysis of PFOS, FOSA and PFOA From Various Food Matrices Using HPLC Electrospray/Mass Spectrometry CENTRE PROTOCOL NUMBER: 00P-023-057 TYPE OF STUDY: Residue TEST SYSTEM: Green beans, apples, pork muscle, cow milk, chicken muscle, chicken eggs, bread, hot dogs, catfish and ground beef TEST MATERIAL: PFOS, FOSA and PFOA SPONSOR: 3M Environmental Technology and Safety Services Building 2-3E-09 PO Box 33331 St. Paul, MN 55133-3331 STUDY DIRECTOR: Karen Smith Centre Analytical Laboratories, Inc. Phone: (814) 231-8032 TESTING FACILITY: Centre Analytical Laboratories, Inc. 3048 Research Drive State College, PA 16801 ANALYTICAL PHASE Study Initiation Date: 01/09/01 TIMETABLE: Analytical Start Date: 01/11/01 Analytical Termination Date: 05/22/01 Centre Analytical Laboratories, Inc. Page 5 of 151 Centre Study No.: 023-057 Centre Protocol No: GOP-02305 7 PROJECT PERSONNEL The Study Director for this project at Centre Analytical Laboratories, Inc. was Karen Smith. The following personnel from Centre Analytical Laboratories, Inc., were associated with various phases of the study: Em Title Karen Smith Scientist Emily Stauffer Scientist Angela Morgan Technician Tiffany Proctor Technician Rickey Keller Sample Custodian Lawrence Ord Sample Custodian Dave Bell Scientist Sharareh Zolghadr Technician Jason Farabaugh Scientist Mitra Arjmand Technician Yu Qiong Tan Technician Ling Ling Liu Technician Xiaoming Zhu Technician Centre Analytical Laboratories, Inc. Page 6 of 151 Centre Study No.: 023-057 . Centre Protocol No: 00P-023-057 TABLE OF CONTENTS Page TITLE PAGE 1 GOOD LABORATORY PRACTICE COMPLIANCE STATEMENT 2 QUALITY ASSURANCE STATEMENT 3 - CERTIFICATION OF AUTHENTICITY 4 STUDY IDENTIFICATION 5 PROJECT PERSONNEL 6 TABLE OF CONTENTS 7 LIST OF TABLES 8 LIST OF FIGURES 9 a LIST OF APPENDICES 11 1.0 SUMMARY 12 2.0 OBJECTIVE 12 3.0 INTRODUCTION 12 4.0 TEST SYSTEM 13 5.0 REFERENCE MATERIAL 14 - 6.0 EXPERIMENTAL DESIGN 15 7.0 DESCRIPTION OF ANALYTICAL METHOD 15 7.1 Extraction Procedure 15 7.2 Preparation of Standards and Forti?cation Solutions 15 7.3 Chromatography 16 7.4 Instrument Sensitivity l7 . 7.5 Description of Instrument and Operating Conditions 17 7.6 Quantitation and Example Calculation 18 8.0 RESULTS AND DISCUSSION 20 9.0 CIRCUMSTANCES THAT MAY HAVE AFFECTED THE DATA 21 10.0 RETENTION OF DATA AND SAMPLES 21 11.0 TABLES 22 12.0 FIGURES 41 13.0 APPENDICES 65 Centre Analytical Laboratories, Inc. Page 7 of 151 Centre Study No?: 023-057 Centre Protocol No: COP-023057 LIST OF TABLES Page Table 1. Summary of PFOS, FOSA and PFOA. Fortification Recoveries 23 Table II. Summary of PFOS, FOSA and PFOA Residues Found in Samples 26 Centre Analytical Laboratories, Inc. Page 8 of 151 Figure 1. Figure 2. Figure 3. Figure 4. Figure 5. Figure 6. Figure 7. Figure 8. Figure 9. Figure 10. Figure 11. Figure 12. Figure 13. Figure 14. Figure 15. Figure 16. Centre Study No.: 023-057 Centre Protocol o: OOP-OZ3-057 LIST OF FIGURES Page Typical Calibration Curve for PFOS 42 Typical Calibration Curve for FOSA 43 Typical Calibration Curve for PFOA 44 Chromatogram Representing a 0.5 ng/mL mixed calibration standard of PFOS, FOSA and PFOA 45 Chromatogram Representing a 2.5 ng/mL mixed calibration standard of PFOS, FOSA and PFOA 46 Chromatogram Representing a Control Apple Sample (Centre ID: 0009347 Blank A1, Data Set: 020901C Apple) 47 Chromatogram Representing a Control Apple Sample Forti?ed with 2.5 ng/g of PFOS, FOSA and PFOA (Centre ID: 0009347 A1, Data Set: 020901C Apple) 48 Chromatogram Representing an Apple Sample (Centre ID: 0012927, Sponsor ID: Publix, 18257, Data Set: 020901C Apple) 49 Chromatogram Representing a Control Green Bean Sample (Centre ID: 0009346 Blank A2, Data Set: 020601C Bean) 50 Chromatogram Representing a Control Green Bean Sample Fortified with 2.5 ng/g of PFOS, FOSA and PFOA (Centre ID: 0009346 A2, Data Set: 020601C Bean) 51 Chromatogram Representing a Green Bean Sample (Centre ID: 0012910, Sponsor ID: Bruno?s, 18341, Data Set: 020601C Bean) 52 Chromatogram Representing a Control Pork Muscle Sample (Centre ID: 0009348 Blank Al, Data Set: 011501A Pork) 53 Chromatogram Representing a Control Pork Muscle Sample Forti?ed with 2.5 ng/g of PFOS, FOSA and PFOA (Centre ID: 0009348 A1, Data Set: 011501A Pork) 54 Chromatogram Representing a Pork Muscle Sample (Centre ID: 0012795, Sponsor ID: Winn-Dixie, 18227, Data Set: 011501A Pork) 55 Chromatogram Representing a Control Milk Sample (Centre ID: 0009349 Blank A1, Data Set: 020701A Milk) 56 Chromatogram Representing a Control Milk Sample Fortified with 2.5 ng/ of PFOS, FOSA and PFOA (Centre ID: 0009349 A1, Data Set: 020701A Milk) 57 Centre Analytical Laboratories, Inc. Page 9 of 151 Figure 17. Figure 18. Figure 19. Figure 20. Figure 21. Figure 22. - Figure 23. Centre Study No.: 023-057 Centre Protocol No: LIST OF FIGURES (CONTINUED) Chromatogram Representing a Milk Sample (Centre 0012871, Sponsor ID: Winn?Dixie, 18202, Data Set: 020701A Milk) 58 Chromatogram Representing a Control Chicken Egg Sample (Centre ID: 0009342 Blank A3, Data Sets: 050901A Egg for PFOS, 012401A Egg for FOSA, and 052101A Egg for PFOA) 59 Chromatogram Representing a Control Chicken Egg Sample Forti?ed with 2.5 ng/g of PFOS, FOSA and PFOA (Centre ID: 0009342 A3, Data Sets: 050901A Egg for PFOS, 012401A Egg for FOSA, and 052101A Egg for PFOA) 60 Chromatogram Representing a Chicken Egg Sample (Centre ID: 0012861, Sponsor Save, 18167 and 21226, Data Sets: 050901A Egg for PFOS, 012401A Egg for FOSA, and 052101A Egg for PFOA) 61 Chromatogram Representing a Control Bread Sample (Centre 0009343 Blank Al, Data Set: 020901A Bread) 62 Chromatogram Representing a Control Bread Sample Fortified with 2.5 ng/g of PFOS, FOSA and PFOA (Centre ID: 0009343 A1, Data Set: 020901A Bread) 63 Chromatogram Representing 3 Bread Sample (Centre ID: 0012887, Sponsor ID: Albertson?s, 18244, Data Set: 020901A Bread) 64 Centre Analytical Laboratories, Inc. Page 10 of 151 Centre Study No.: 023-057 Centre Protocol No: 00P-023-057 LIST OF APPENDICES Page Appendix A Study Protocol 00P-OZ3-057 (Centre Study No. 023-057), Amendments and Deviation 65 Centre Analytical Laboratories. Inc. Page 11 of 151 Centre Study No.: 023?057 Centre Protocol No: 1.0 SUMMARY The purpose of this study was to analyze residues of PFOS, FOSA and PFOA in various food matrices as specified in Centre Protocol 00P-023-057. The analytical method used for this study was entitled, ?Method of Analysis for the Determination of Fluorochemicals in Green Beans, Apples, Pork Muscle, Cow Milk, Chicken Muscle, Chicken Eggs, Bread, Hot Dogs, and Cat?sh by The limit of quanti?cation for PFOS, FOSA and PFOA in food was 0.5 Average fortification recoveries and relative standard deviations were 101% i 9.0% for PFOS, 96% i 13% for FOSA and 104% i 14% for PFOA. Residues ranging from non-quantifiable levels to 0.852 (ng/g) for PFOS, non- quantifiable levels for FOSA, and non-quanti?able to 2.35 ng/g for PFOA (one value of 14.7 (ng/g) was found for PFOA but was considered suspect) were found in the food samples. 2.0 OBJECTIVE The objective of this study was to determine levels of PFOS, FOSA and PFOA in food samples collected from local grocery stores from six test cities outlined in BM Quality Assurance Project Plan for Empirical Human Exposure Assessment Multi-City Study Sampling Task using the analytical method entitled ?Method of Analysis for the Determination of Fluorochemicals in Green Beans, Apples, Pork Muscle, Cow Milk, Chicken Muscle, Chicken Eggs, Bread, Hot Dogs, and Cat?sh by 3.0 INTRODUCTION This report details the results of the residues of PFOS, FOSA and PFOA detected in green beans, apples, pork muscle, cow milk, chicken muscle, chicken eggs, bread, hot dogs, cat?sh and ground beef, using the analytical method entitled, ?Method of Analysis for the Determination of Fluorochemicals in Green Beans, Apples, Pork Muscle, Cow Milk, Chicken Muscle, Chicken Eggs, Bread, Hot Dogs, and Cat?sh by Complete details of the analytical methodology can be found in Appendix A. The study was initiated on January 09, 2001, when the study director signed the protocol 00P-023-057. The complete protocol and amendments can be found in Appendix A. The analytical start date was January 11, 2001, and the analytical termination date was May 22, 2001. Centre Analytical Laboratories, Inc. Page 12 of 151 Centre Study No.: 023-05 7 Centre Protocol No: 00P-OZ3-057 4.0 TEST SYSTEM The food samples analyzed in this study were received frozen from Pace Analytical on December 09, 2000 and stored frozen upon receipt. Pace Analytical collected the samples for 3M Environmental Laboratory. The samples were then logged in on December 18, 2000 by Centre personnel and transferred to different frozen storage locale. All of the samples were processed according to the method, ?Method of Analysis for the Determination of Fluorochernicals in Green Beans, Apples, Pork Muscle, Cow Milk, Chicken Muscle, Chicken Eggs, Bread, Hot Dogs, and Cat?sh by Exact details of processing can be found on page 91 of this report. After processing, the samples were stored in a freezer at a temperature of or below until used and placed back into a freezer immediately after use. At the request of the sponsor, the egg samples were returned frozen to 3M Environmental Laboratory on February 26, 2001 for possible reanalysis. The egg samples were returned unanalyzed from 3M Environmental Laboratory to Centre Analytical Laboratories, Inc. These samples were received frozen from 3M Environmental Laboratory on May 03, 2001 for PFOS and PFOA re~extraction and analysis. They were assigned different 3M and Centre lD?s. The food samples used for the controls and matrix spikes were the same samples used in the method validation study (Centre Study No. 023-043). They were purchased from Giant, Store #111 in State College, PA and assigned the following sample IDs upon log in at Centre: Centre Sample ID Sample Description 0009341 Chicken Muscle 0009342 Chicken Eggs 0009343 White Bread 0009344 Hot Dogs 0009345 Catfish 0009346 Green Beans 0009347 _Apples 0009348 Pork Muscle 0009349 Whole Milk 0100006 Ground Beef All of the control samples were purchased on September 27, 2000 except for the ground beef, which was purchased on January 03, 2001. The samples were stored in a refrigerator :t until processed. All of these control samples were processed with dry ice in a Hobart food chopper on October 02, 2000 except for the ground beef, which was processed on January 03, 2001. After processing, the samples were stored in a freezer at a temperature of or below until used and placed back into a freezer immediately after use. Centre Analytical Laboratories. Inc. Page 13 of 151 Centre Study No.2 023-057 Centre Protocol No: 00P-023-057 Sample login and chain of custody information can be found in the raw data package associated with this study. Storage records will be kept at Centre Analytical Laboratories, Inc. and a true copy of the storage records can be found in the raw data package associated with this study. 5.0 REFERENCE MATERIAL PFOS was received at Centre on June 05, 2000, FOSA was received on February 15, 2000 and PFOA was received on July 06, 2000 from 3M Environmental Technology and Services. Characterization of the reference materials PFOS and PF 0A was performed at Centre on August 31, 2000 and November 06, 2000, respectively, and documentation can be found in raw data package associated with this report. The characterization of FOSA is in progress and the necessary information will be added upon complete characterization of the reference materials. All analyses were completed prior to standard expiration dates. The available information for the reference material is listed below. FOSA was stored at room temperature and PFOS and PFOA were stored frozen at Compound TCR Substance No. Batch No. Purim Expiration Date PFOS TCR00017-46 NA 97.9 08/31/01 FOSA SD-029 L-15709 95.1 02/15/01 PFOA TCR99030-30 332 95.0 10/31/01 Molecular structures of PFOS, FOSA and PFOA are given below. PFOS Chemical Name Per?uorooctane sulfonate Molecular weight 499 Note: The neutral molecule and standard form which PFOS (anion) is derived from is potassium per?uorooctane sulfonate molecular weight 538. FOSA Chemical Name Per?uorooctane sulfonylarnide Molecular weight 499 C3F17S Centre Analytical Laboratories, Inc. Page 14 of 151 Centre Study No.: 023-057 Centre Protocol No: 00P-023-05 7 PFOA Chemical Name Per?uorooctanoate Molecular weight 413 C7F1 5000' Note: The neutral molecule and standard form which PF OA (anion) is derived from is ammonium per?uoroctanoate molecular weight 431. 6.0 EXPERIMENTAL DESIGN Each sample was extracted in duplicate. A set contained one matrix blank and two matrix blanks spiked with known amounts of PFOS, FOSA and PFOA and 6 10 samples. The re-extracted egg sets also included one reagent blank. The extracts were analyzed by Samples with residues below the linear range of the calibration curve were not quanti?ed; however, residues in the control samples were calculated extrapolation of the calibration curve, in order to correct forti?cation recoveries. 7.0 DESCRIPTION OF ANALYTICAL METHOD Analytical method entitled ?Method of Analysis for the Determination of Fluorochemicals in Green Beans, Apples, Pork Muscle, Cow Milk, Chicken Muscle, Chicken Eggs, Bread, Hot Dogs, and Catfish by was used for this study. 7.1 Extraction Procedure Five grams of processed sample were weighed into 50 mL polypropylene centrifuge tubes and forti?ed (if necessary). The samples were extracted with ACN followed by a SPE column (?orisil, silica gel, carbon and clean up. The column eluate was collected and concentrated to near dryness. Final volume was adjusted to 2 mL with 2% ascorbic acid in methanol. The samples were analyzed using electrospray 7.2 Preparation of Standards and Forti?cation Solutions Standard stock solutions of PFOS, PFOA and FOSA were prepared on September 18, 2000, September 26, 2000 and October 03, 2000, respectively. Forti?cation and calibration standard solutions were prepared on October 17, 2000 as speci?ed in Centre Analytical Laboratories? analytical method entitled, ?Method of Analysis for the Determination of Fluorochemicals in Green Beans, Apples, Pork Muscle, Cow Milk, Centre Analytical Laboratories, Inc. Page 15 of 151 Centre Study No.: 023-057 Centre Protocol No: 00P-OZ3-057 Chicken Muscle, Chicken Eggs, Bread, Hotdogs, and Catfish by Individual stock standard solutions of PFOS, FOSA and PFOA were prepared at concentrations of 100 ug/mL by taking 10 mg of the standard (corrected for purity and salt content where. applicable) and bringing it up to 100 mL with methanol. From these solutions, a 1 pg/mL mixed fortification standard solution was prepared by taking 1 mL of each stock and bringing the volume up to 100 mL with methanol. The 1 ug/mL mixed forti?cation standard was diluted ten-fold with methanol to make the 0.1 ug/mL mixed forti?cation standard. Then, the 0.1 t1 g/mL mixed standard was diluted ten-fold with methanol to make the 0.01 ug/mL forti?cation standard. calibration standards were prepared in methanol at the following] concentrations 50, 25, 10, 5.0, 2.5, 1.0, and 0.5 ng/mL according to the following table: Initial Concentration Volume Diluted to Final concentration (ng/mL) (IDL) (HIL) (Dani) 1000 5.0 100 50 1000 2.5 100 25 1000 1.0 100 10 50 10.0 100 5.0 25 10.0 100 2.5 10 10.0 100 1.0 5 .0 10.0 100 0.5 New standard stock, forti?cation and calibration solutions were made for PFOS and PFOA in order to perform the egg re-extraction and analysis. The PFOS standard stock solution was prepared on March 14, 2001 and the PFOA standard stock solution was. prepared on April 11, 2001. Mixed fortification and calibration solutions of PFOS and PFOA were prepared from the stock solutions on May 03, 2001 as described above. The only modification from the above procedure is that FOSA was omitted from the mix since the re-extraction and analysis was for PFOS and PFOA only. The stock standard solution and all fortification and calibration standard solutions were stored in a refrigerator i when not in use. Documentation of standard preparation can be found in the raw data associated with this report. 7.3 Chromatography Quantification of PFOS, FOSA and PFOA was accomplished by analysis using electrOSpray The retention times of PFOS, FOSA and PFOA were 5.4 min, 6.0 min and 5.3 min., respectively. The matrices did not contribute any interfering peaks corresponding to the Centre Analytical Laboratories, Inc. Page 16 of 151 Centre Study No.: 023-057 Centre Protocol No: 00P-023-057 analyte retention times; however, there were some occasions where the control matrices; appeared to contain analyte. 7.4 Instrument Sensitivity The smallest standard amount injected during the chromatographic run was 0.5 ng/mL which is equivalent to 0.2 ng/g of PFOS, FOSA and PFOA in matrix. 7.5 Description of Instrument and Operating Conditions A Micromass Quattro Ultima coupled to a Hewlet Packard HPLC system was used. Data acquisition and processing were performed using 3.4 software. Detailed operating conditions are listed below: Instrument: Micromass Quattro Ultima ELECTROSPRAY ION SOURCE: Capillary: 2.0 kV Hexapole 2: Hexapole l: 0 Source Block Temp.: Aperture 1: 0 Desolvation Temp: ANALYZER: LM Res 1: 10.5 LM Res 2: 12.0 HM Res 1: 10.5 HM Res 2: 12.0 Energy 1: 1.0 Energy 2: 2.0 Entrance: -2 Multiplier: 650 Exit: 2 GAS FLOWS AND PRESSURE: Desolvation N2 Flow Rate: ~700 L/hr Nebuliser N2 Flow Rate: ~150 L/hr Gas Cell Pressure: ~0.0031 mbar Computer: COMPAQ Professional Workstation AP200 Software: Microsoft Windows NT: Version 4 Build 1381: Service Pack 5 Micromass Limited: 3.4 Build 004 HPLC Equipment: Hewlett Packard (HP) Series 1100 HP Binary Pump HP Vacuum Degasser HP Autosampler HP Column Oven HPLC Column: Genesis 08, cm 2.1 mm id 4 Column Temperature: Mobile Phase (A) 2 mM Ammonium Acetate in Type I Water Centre Analytical Laboratories, Inc. Page 17 of 151 Centre Study No.: 023-057 Centre Protocol No: 00P-023-057 Mobile Phase (B) Methanol Time (min) A Flow Rate (mUmin) 0.0 60.0 40.0 0.3 0.4 60.0 40.0 0.3 1.0 10.0 90.0 0.3 7.0 10.0 90.0 0.3 7.5 0.0 100.0 0.3 9.0 0.0 100.0 0.4 9.5 60.0 40.0 0.4 13.5 60.0 40.0 0.4 14.0 60.0 40.0 0.3 Total run time 14 min Injected Volume: 15 11L Ions monitored Analyte Parent ion Daughter ion Dwell gsecs) - Coll Ener eV Cone (V) PFOA 413 369 0.2 10 3O FOSA 498 78 0.2 40 30 PFOS 499 99 0.2 50 30 7.6 Quantitation and Example Calculation Fifteen microliters of sample or calibration standard was injected into the The peak area was measured and the standard curve was generated (using 1/x weighted linear regression) by software using seven concentrations of standards. The residue concentration in food samples was determined using the following equations: Equation 1 was used to calculate the amount of analyte found (in ng/mL, based on peak area) using the standard curve (linear regression parameters) generated by the software program. Quation 1: Analyte found (ng/mL) (Peak area - intercept} slope The component residue concentration (in ng/g) in matrix was determined by using Equation 2. Centre Analytical Laboratories, Inc. Page 18 of 151 Centre Study No.: 023-057 Centre Protocol o: 00P-023-057 Euation 2: Analyte found (ng/ g) [analyte found (ng/mL) - average analyte found in blanks (ng/mL)] DF FV (mL) sample weight where DF dilution factor and FV final volume Note: the process of subtracting the average analyte found in the blanks was done only for control matrix spikes or if a reagent blank contained residue. For samples fortified with known amounts of analytes prior to extraction, Equation 3 was used to calculate the percent recovery. Equation 3: analyte found (mg/g) analyte added (mg/g) 100 Recovery An example of a calculation using an actual sample follows: Pork sample Centre 0009348 Al (Set No.: 011501A Pork), fortified at 2.5 ng/g of PFOS, FOSA and PFOA: (Calculation is using values from FOSA) Where: peak area 149454 intercept 2524.48 slope 25194.9 ?nal volume 2 mL dilution factor 1 sample weight 5 ng/g added (fort level) 2.5 ng/g amt found in control 0 (NQ Not quantifiable; assumed to be 0) From equation 1: L149484 2524.481 25194.9 ll Analyte found (ng/mL) 5.83 ng/mL Centre Analytical Laboratories, Inc. Page 19 of 151 Centre Study No.: 023-057 Centre Protocol No: 00Pa023-057_ From equation 2: Analyte found (ng/g) (5.832 01x 1 2 5.0 2.33 ng/g From equation 3: Recovery 2.33 100 2.5 93% Note: This example calculation was done using rounded numbers, and therefore may be different from the values shown in the RAW DATA. Any residues found for PFOA were adjusted for PFOA purity This was done by taking the residue found (mg/g) for PFOA and multiplying by the purity (0.95). Other statistical methods used in analyzing this data were: Standard Deviation Relative Standard Deviation (RSD or Coe??icient of Variation Standard Deviation 100% Mean 8.0 RESULTS AND DISCUSSION Average forti?cation recoveries and relative standard deviations were 101% i 9.0% for PFOS, 96% i 13% for FOSA and 104% i 14% for PFOA. A summary of all of the forti?cation recoveries can be found in Table I. Residues ranging from non-quantifiable levels to 0.852 (ng/g) for PFOS, non- quantifiable levels for FOSA, and non-quantifiable to 2.35 ng/g for PFOA (one value of 14.7 (ng/g) was found for PFOA but was considered suspect) were found in the food samples. The residues found in all of the samples are detailed in Table 11. Centre Analytical Laboratories, Inc. Page 20 of 151 Centre Study No.: 023-057 Centre Protocol No: 00P-023-05 7 Typical calibration curves and chromatograms representing standards, Controls, forti?cations, and samples are depicted in Figures 1-23. In this study, analytes were not quanti?ed below 0.5 ng/g. If lower detection levels are required, a more de?nitive study, including extraction blanks in addition to matrix blanks, could be done. Initially the PFOA standard and forti?cation solutions were not corrected for purity, as purity information had not been received at the time. Purity data was received after residue analyses were completed and the residues found were then corrected for PFOA purity. All ng/g residues of PFOA in this report have been adjusted to re?ect the purity of the PFOA used in this study. There was some PFOA contamination from the lab while performing the extraction for eggs. It was believed to be coming from the extraction solvent itself. Using a different brand and lot number of ACN alleviated the problem because upon reanalysis, there were no quanti?able residues of PFOA in the egg samples. 9.0 CIRCUMSTANCES THAT MAY HAVE AFFECTED THE DATA There were no circumstances that may have affected the quality or integrity of the data. 10.0 RETENTION OF DATA AND SAMPLES When the ?nal report-is complete, all original paper data generated by Centre Analytical Laboratories, Inc. will be shipped to the sponsor. This does not include facility-speci?c raw data such as instrument logs, however exact copies of temperature logs will be submitted. Exact copies of all raw data, as well as a signed copy of the ?nal analytical report and all original facility-speci?c raw data, will be retained in the Centre Analytical Laboratories, Inc. archives for the period of time speci?ed in 40 CFR 792.195 Retained samples of reference substances are archived by the sponsor. Centre Analytical Laboratories, Inc. Page 21 of 151 Centre Study No.: 023-057 Centre Protocol No: 11.0 TABLES Centre Analytical Laboratories, Inc. Page 22 of 151 Centre Study No.2 023-057 Centre Protocol No: Table I. Summary of PFOS, FOSA and PFOA Forti?cation Recoveries Extraction Analysis Fort Level Recovery Centre ID Sample Description Date Date (nag) PF OS FOSA PFOA 0009341 Al Chicken 01/11/01 2.5 104 93 94 0009341 Bl Chicken 01/11/01 01/11-12/01 10 89 84 87 0009341 A2 Chicken 01/11/01 01/12/01 2.5 110 94 98 0009341 B2 Chicken 01/11/01 01/12/01 10 91 89 91 0009341 A3 Chicken 01/ 12/01 01/15/01 2.5 108 107 106 0009341 B3 Chicken 01/12/01 01/15/01 10 106 105 111 0009341 A4 Chicken 01/12/01 01/15/01 2.5 106 105 107 0009341 B4 Chicken 01/ 12/01 01/15/01 10 97 90 98 0009348 Al Pork 01/15/01 01/15-16/01 2.5 105 93 116 0009348 Bl Pork 01/15/01 01/15-16/01 10 99 86 110 0009348 A2 Pork 01/15/01 01/16/01 2.5 98 87 105 0009348 B2 Pork 01/ 15/01 01/16/01 10 84 76 95 0009348 A3 Pork 01/ 16/01 01/16/01 2.5 98 93 106 0009348 B3 Pork 01/16/01 01/16/01 10 81 78 91 0009348 A4 Pork 01/ 16/01 01/16-17/01 2.5 90 86 93 0009348 B4 Pork 01/16/01 01/16-17/01 10 82 79 92 0009344 A1 Hot Dog 01/17/01 01/17-18/01 2.5 102 100 0009344 B1 Hot Dog 01/17/01 01/17-18/01 10 95 92 0009344 A1 Hot Dog 01/ 17/01 01/ 18/01 2.5 - - 97 0009344 1 Hot Dog 01/17/01 01/18/01 10 - 95 0009344 A2 Hot Dog 01/17/01 01/18/01 2.5 113 106 114 0009344 B2 Hot Dog 01/17/01 01/18/01 10 95 91 87 0009344 A3 Hot Dog 01/18/01 01/18-19/01 2.5 99 94 102 0009344 B3 Hot Dog 01/ 18/01 01118.19/01 10 89 77 89 0009344 A4 Hot Dog 01/18/01 01/19/01 2.5 104 95 96 0009344 B4 Hot Dog 01/ 18/01 01/19/01 10 91 84 84 0009345 Al Fish 01/19/01 01/19-20/01 2.5 100 68 105 0009345 B1 Fish 01/19/01 01/19-20/01 10 87 56 87 0009345 A2 Fish 01/ 19/01 01/20/01 2.5 86 85 0009345 B2 Fish 01/ 19/01 01/20/01 10 86 86 0009345 A2 Fish 01/30/01 01/31/01 2.5 - 126 - 0009345 B2 Fish 01/30/01 01/31/01 10 - 110 - 0009345 A3 Fish 01/22/01 01/22?23/01 2.5 111 76 1 1 0009345 B3 Fish 01/22/01 01/22-23/01 10 95 65 101 0009345 A4 Fish 01/22/01 01/23l01 2.5 106 73 103 0009345 B4 Fish 01/22/01 01/23/01 10 89 62 89 Rejected due to an unacceptable recovery. Replaced with re-extracted data. - Not Analyzed For Centre Analytical Laboratories, Inc. Page 23 of 151 Centre Study No.: 023-057 Centre Protocol No: 00P-023-057 Table I continued: Summary of PFOS, FOSA and PFOA Fortification Recoveries Extraction Analysis Fort Level Recovery Centre ID Sample DescriJLtion Date Date (ngg) PFOS FOSA PFOA 0009342 A1 Egg 01/23/01 01/23-24/01 2.5 104 96 84 0009342 1 Egg 01/23/01 01/23-24/01 10 98 80 67 0009342 A2 Egg 01/23/01 01/24/01 2.5 117 106 78 0009342 BZ Egg 01/23/01 01/24/01 10 101 98 77 0009342 A3 Egg 01/24/01 01/24-25/01 2.5 115 109 105 0009342 B3 Egg 01/24/01 01/24-25/01 10 92 90 85 0009342 A4 Egg 01/24/01 01/25/01 2.5 117 111 90 0009342 B4 Egg 01/24/01 01/25/01 10 102 97 82 0009346 Al Green Bean 02/05/01 02/05/01 2.5 98 114 129 0009346 B1 Green Bean 02/05/01 02/05/01 10 106 106 128 0009346 A2 Green Bean 02/06/01 ()2/07/01 2.5 92 99 124 0009346 B2 Green Bean 02/06/01 02/07/01 10 111 103 130 0009346 A3 Green Bean 02/08/01 02/09/01 2.5 99 100 125 0009346 B3 Green Bean 02/08/01 02/09/01 10 94 97 125 0009346 A4 Green Bean 02/08/01 02/12/01 2.5 83 85 103 0009346 B4 Green Bean 02/08/01 (32/12/01 10 96 95 1 12 0009349 A1 Milk 02/07/01 02/09-10/01 2.5 99 103 129 0009349 B1 Milk 02/07/01 02/09-10/01 10 91 90 128 0009349 A2 Milk 02/07/01 02/ 10/01 2.5 114 101 123 0009349 B2 Milk 02/07/01 02/10/01 10 9O 91 123 0009349 A3 Milk 02/08/01 02/10/01 2.5 101 103 126 0009349 B3 Milk 02/08/01 02/10/01 10 89 91 129 0009349 A4 Milk 02/08/01 02/10-1 1/01 2.5 1 13 103 124 0009349 B4 Milk 02/08/01 02/10-11/01 10 93 94 123 0009347 A1 Apple 02/09/01 02/12/01 2.5 113 110 122 0009347 B1 Apple 02/09/01 02/12/01 10 105 104 119 0009347 A2 Apple 02/12/01 0?2/13/01 2.5 111 107 108 0009347 B2 Apple 02/12/01 02/13/01 10 100 102 101 0009347 A3 Apple 02/12/01 02/13-14/01 2.5 109 105 110 0009347 B3 Apple 02/12/01 02/13-14/01 10 98 96 100 0009347 A4 Apple 02/12/01 02/ 14/01 2.5 108 101 102 0009347 B4 Apple 02/12/01 02/14/01 10 99 96 99 Centre Analytical Laboratories, Inc. Page 24 of 151 Centre Study No.: 023-05 7 Centre Protocol No: 00P-023-057 Table I continued: Summary of PFOS, FOSA and PFOA Fortification Recoveries Extraction Analysis Fort Level Recovery Centre ID Sample Description Date Date (ng/g) PFOS FOSA PFOA 0009343 A1 Bread 02/08?09/01 02/11/01 2.5 87 106 118 0009343 B1 Bread 02/08-09/01 02/11/01 10 96 96 109 0009343 A2 Bread 02/08-09/01 02/11/01 2.5 106 101 119 0009343 B2 Bread 02/08-09/01 02/11/01 10 94 93 106 0009343 A3 Bread 02/12-13/01 02/14/01 2.5 106 103 103 0009343 B3 Bread 02/ 12-13101 10 99 92 97 0009343 A4 Bread 02/12?13/01 02/14/01 2.5 11 109 106 0009343 B4 Bread 02/12-13/01 02/14/01 10 102 100 100 0100006 A1 Ground Beef 02/13/01 02/14-15/01 2.5 104 104 100 0100006 Bl Ground Beef 02/ 13/01 02/14?15/01 10 103 99 95 0100006 A2 Ground Beef 02/ 13/01 (12/15/01 2.5 [11 102 103 0100006 B2 Ground Beef 02/13/01 0215/01 10 103 98 98 0100006 A3 Ground Beef 02/ 14/01 02/ 15/01 2.5 121 123 120 0100006 B3 Ground Beef 02/ 14/01 02/15/01 10 106 116 114 0100006 A4 Ground Beef 02/14/01 02/15-16/01 2.5 112 108 105 0100006 B4 Ground Beef 02/14/01 02/15-16/01 10 102 101 102 0009342 A1 Egg 05/07?08/01 05/08/01 2.5 111 - - 0009342 B1 Egg 05/07o08/01 05/08/01 10 99 - - 0009342 A2 Egg 05/07?08/01 05/08?09/01 2.5 111 - - 0009342 B2 Egg 05/07-08/01 05108-09/01 10 102 - - 0009342 A3 Egg 05/08-09/01 05/09/01 2.5 106 - - 0009342 B3 Egg 05/08-09/01 05/09/01 10 94 - - 0009342 A4 Egg 05/08o09/01 05/09-10/01 2.5 109 - - 0009342 B4 Egg 05/08-09/01 05/09-10/01 10 102 - - 0009342 A1 Egg 05/18/01 05/18/01 2.5 - - 110 0009342 Bl Egg 05/ 18/01 05/18/01 10 - - 99 0009342 A2 Egg 05/18/01 05/18-19/01 2.5 - - 102 0009342 132 Egg 05/18/01 05/18-19/01 10 - - 108 0009342 A3 Egg 05/20-21/01 05/21/01 2.5 - - 96 0009342 B3 Egg 05/20-21/01 05/21/01 10 - - 96 0009342 A4 Egg 05/20-21/01 05/21-22/01 2.5 - 95 0009342 B4 Egg 05/20-21/01 05/21-22/01 10 - - 96 AVERAGE: 101 96 104 STD DEV: 9.0 13 14 RELATIVE STD DEVNot Analyzed For Centre Analytical Laboratories. Inc. Page 25 of 151 Centre Study No.: 023-057 Centre Protocol No: 00P-023-057 Table II. Summary of PFOS, FOSA and PFOA Residues Found in Samples Residue Found Centre ID Data Set No. SLonsor ID Store Name Location Matrix PFOS FOSA PFOA 0012776 011 101A Chicken 18249 Publix Port St. Lucie, FL Chicken NQ NQ NQ 0012776 Dup 01 1101A Chicken 18249 Publix Port St. Lucie, FL Chicken NQ NQ 0012777 011101A Chicken 18226 Winn?Dixie Port St. Lucie, FL Chicken NQ NQ NQ 0012777 Dup 011101A Chicken 18226 Winn?Dixie Port St. Lucie, FL Chicken NQ NQ NQ 0012778 011 101A Chicken 18239 Albertson?s Port St. Lucie, FL Chicken NQ 0012778 Dup 011101A Chicken 18239 Albertson?s Port St. Lucie, FL Chicken NQ NQ NQ 0012779 011101A Chicken 18356 Delchamps II Mobile, AL Chicken NQ NQ 0012779 Dup 011101A Chicken 18356 Delchamps 11 Mobile, AL Chicken NQ NQ NQ 0012780 011101A Chicken 18197 Winn-Dixie Columbus, GA Chicken NQ NQ NQ 0012780 Dup 011101A Chicken 18197 Winn-Dixie Columbus, GA Chicken NQ NQ 0012781 011101B Chicken 18345 Delchamps I Mobile, AL Chicken NQ NQ NQ 0012781 Dup 011101B Chicken 18345 Delchamps I Mobile, AL Chicken NQ NQ NQ 0012782 011101B Chicken 18209 Piggly Wiggly Columbus, GA Chicken NQ NQ 0012782 Dup 011101B Chicken 18209 Piggly Wiggly Columbus, GA Chicken NQ NQ NQ 0012783 011101B Chicken 18335 Bruno?s Mobile, AL Chicken NQ NQ NQ 0012783 Dup 011101B Chicken 18335 Bruno?s Mobile, AL Chicken NQ NQ NQ 0012784 011101B Chicken 18323 Kroger?s Decatur, AL Chicken NQ NQ NQ 0012784 Dup 011101B Chicken 18323 Kroger?s Decatur, AL Chicken NQ NQ NQ 0012785 0111013 Chicken 18312 Winn-Dixie Decatur, AL Chicken NQ NQ NQ 00127 85 Dup 011101B Chicken 18312 Winn-Dixie Decatur, AL Chicken NQ NQ NQ 0012786 011201A Chicken 18301 Haloway Decatur, AL Chicken NQ 0012786 Dup 011201A Chicken 18301 Haloway Decatur, AL Chicken NQ NQ NQ 0012787 011201A Chicken 18187 Cub Columbus, GA Chicken NQ NQ NQ 0012787 Dup 011201A Chicken 18187 Cub Columbus, GA Chicken NQ NQ NO 0012788 01 1201A Chicken 18174 Bi-Lo Cleveland, TN Chicken NQ NQ NQ 0012788 Dup 01 1201 A Chicken 18174 Bi-Lo Cleveland, TN Chicken NQ NQ NQ 0012789 01 1201 A Chicken 18163 Save-a-Lot Cleveland, TN Chicken NQ NQ 0012789 Dup 011201A Chicken 18163 Save-a-Lot Cleveland, TN Chicken NQ NQ NQ 0012790 011201A Chicken 18283 Albertson?s Pensacola, FL Chicken NQ NQ 0012790 Dup 011201A Chicken 18283 Albertson?s Pensacola, FL Chicken NQ NQ NQ 0012791 011201B Chicken 18260 Food World Pensacola, FL Chicken NQ NQ NQ 0012791 Dup 011201B Chicken 18260 Food World Pensacola, FL Chicken NQ NQ NQ NQ Not Quanti?able. The residue detected, if any, was below the limit of the study which is 0.5 ng/g. *Value is based on wet weight (5.0 sample processed as received) Values rejected based on unacceptable recoveries. Data has been replaced with either reanalysis or re-extraction values. Results rejected based on apparent contamination. Data has been replaced with re?extracted values. - Not analyzed for Centre Analytical Laboratories, Inc. Page 26 of 151 Centre Study No.: 023-057 Centre Protocol No: 00P-023-057 Table II continued: Summary of PFOS, FOSA and PFOA Residues Found in Samples Residue Found Centre ID Data Set No. Sponsor ID Store Name Location Matrix PFOS FOSA PFOA 0012792 01 1201B Chicken 18151 Watson?s Cleveland, TN Chicken NQ NQ 0012792 Dup 011201B Chicken 18151 Watson?s Cleveland, TN Chicken NQ NQ 0012793 011201B Chicken 18272 Food World 11 Pensacola, FL Chicken NQ 0012793 Dup 011201B Chicken 18272 Food World II Pensacola, FL Chicken NQ NQ NQ 0012794 01 1501A Pork 18250 Publix Port St. Lucie, FL Pork NQ NQ 0012794 Dup 011501A Pork 18250 Publix Port St. Lucie, FL Pork NQ NQ NO 0012795 011501A Pork 18227 Winn-Dixie Port St. Lucie, FL Pork NO NO NQ 0012795 Dup 011501A Pork 18227 Winn-Dixie Port St. Lucie, FL Pork NQ 0012796 011501A Pork 18238 Albertson's Port St. Lucie, FL Pork NQ NQ 0012796 Dup 01 1501A Pork 18238 Albertson?s Port St. Lucie, FL Pork NQ . NQ 0012797 01 1501A Pork 18357 Delchamps 11 Mobile, AL Pork NQ NQ NQ 0012797 Dup 011501A Pork 18357 Delchatnps 11 Mobile, AL Pork NQ NQ NQ 0012798 011501A Pork 18198 Winn-Dixie Columbus, GA Pork NQ NQ NQ 0012798 Dup 01 1501 A Pork 18198 Winn-Dixie Columbus. GA Pork NQ NO NO 0012799 011501B Pork 18346 Delchamps I Mobile, AL Pork NQ NQ NQ 0012799 Dup 011501B Pork 18346 Delchamps I Mobile, AL Pork NQ NQ 0012800 011501B Pork 18210 Piggly Wiggly Columbus, GA Pork NQ NQ NO 0012800 Dup 01 1501B Pork 18210 Piggly Wiggly Columbus, GA Pork NQ NQ NQ 0012801 011501B Pork 18334 Bruno?s Mobile, AL Pork NQ NQ NQ 0012801 Dup 011501B Pork 18334 Bruno?s Mobile, AL Pork NQ NQ NQ 0012802 01 1501B Pork 18322 Kroger?s Decatur, AL Pork NQ 0012802 Dup 01 1501B Pork 18322 Kroger?s Decatur, AL Pork NQ 0012803 011501B Pork 18311 Winn-Dixie Decatur, AL Pork NQ NQ NQ 0012803 Dup 0115013 Pork 18311 Winn-Dixie Decatur, AL Pork NQ NQ NQ 0012804 01 1601A Pork 18299 Haloway Decatur, AL Pork NQ NQ NQ 0012804 Dup 01 1601A Pork 18299 Haloway Decatur, AL Pork NQ NQ NQ 0012805 011601A Pork 18186 Cub Columbus, GA Pork NQ NQ NQ 0012805 Dup 011601A Pork 18186 Cub Columbus, GA Pork NQ NQ NQ 0012806 01 1601A Pork 18175 Bi-Lo Cleveland, TN Pork NQ 0012806 Dup 01 1601A Pork 18175 Bi-Lo Cleveland, TN Pork NQ NQ NQ 0012807 01 1601 A Pork 18164 Save-a-Lot Cleveland, TN Pork NQ 0012807 Dup 01 1601A Pork 18164 Save-a-Lot Cleveland, TN Pork NQ NQ NQ NQ Not Quanti?able. The residue detected, if any, was below the limit of the study which is 0.5 ng/g. *Value is based on wet weight (5.0 sample processed as received) . Values rejected based on unacceptable recoveries. Data has been replaced with either reanalysis or re-extraction values. Results rejected based on apparent contamination. Data has been replaced with re-extracted values. - Not analyzed for Centre Analytical Laboratories, Inc. Page 27 of 151 Centre Study No.: 023-057 Centre Protocol No: GOP-023057 Table II continued: Summary of PFOS, FOSA and PFOA Residues Found'in Samples Residue Found Centre ID Data Set No. Sponsor ID Store Name Location Matrix PFOS FOSA PFOA 0012808 01 1601A Pork 18282 Albertson?s Pensacola, FL Pork NQ NQ 0012808 Dup 01 1601A Pork 18282 Albertson?s Pensacola, FL Pork NQ NQ NQ 0012809 0116013 Pork 18261 Food World Pensacola, FL Pork NQ NQ NQ 0012809 Dup 011601B Pork 18261 Food World Pensacola, FL Pork NQ NQ NQ 0012810 011601B Pork 18152 Watson?s Cleveland, TN Pork NQ NQ 0012810 Dup 01 1601B Pork 18152 Watson?s Cleveland, TN Pork NQ NQ 0012811 0116013 Pork 18271 Food World 11 Pensacola, FL Pork NQ NQ NQ 0012811 Dup 0116013 Pork 18271 Food World 11 Pensacola, FL Pork NQ NQ NQ 0012812 011701A Hot Dog 18251 Publix Port St. Lucie, FL Hot Dog NQ NQ 0012812 Dup 011701A Hot Dog 18251 Publix Port St. Lucie, FL Hot Dog NQ NQ 0012813 011701A Hot Dog 18228 Winn~Dixie Port St. Lucie, FL Hot Dog NQ NQ 0012813 Dup 011701A Hot Dog 18228 Winn-Dixie Port St. Lucie, FL Hot Dog NQ NQ 0012814 011701A Hot Dog 18240 Albertson?s Port St. Lucie, FL Hot Dog NQ NQ 0012814 Dup 011701A Hot Dog 18240 Albertson?s Port St. Lucie, FL Hot Dog NQ NQ 0012815 011701A Hot Dog 18358 Delchamps II Mobile, AL Hot Dog NQ NQ 0012815 Dup 011701A Hot Dog 18358 Delchamps 11 Mobile, AL Hot Dog NQ NQ 0012816 011701A Hot Dog 18199 Winn-Dixie Columbus, GA Hot Dog NQ NQ 0012816 Dup 011701A Hot Dog 18199 Winn-Dixie Columbus, GA Hot Dog NQ NQ 0012812 01 1701AR Hot Dog 18251 Publix Port St. Lucie0012812 Dup 01 1701AR Hot Dog 18251 Publix Port St. Lucie0012813 011701AR Hot Dog 18228 Winn-Dixie Port St. Lucie0012813 Dup 011701AR Hot Dog 18228 Winn-Dixie Port St. Lucie0012814 01 1701AR Hot Dog 18240 Albertson?s Port St. Lucie0012814 Dup 011701AR Hot Dog 18240 Albertson?s Port St. Lucie0012815 011701AR Hot Dog 18358 Delchamps 11 Mobile0012815 Dup 011701AR Hot Dog 18358 Delchamps II Mobile, AL Hot Dog - NQ 0012816 01 1701AR Hot Dog 18199 Winn~Dixie Columbus0012816 Dup 011701AR Hot Dog 18199 Winn-Dixie Columbus0012817 011701B Hot Dog 18347 Delchamps 1 Mobile0012817 Dup 011701B Hot Dog 18347 Delchamps 1 Mobile0012818 0117013 Hot Dog 18211 Piggly Wiggly Columbus0012818 Dup 011701B Hot Dog 1821] Piggly Wiggly ColumbusNot Quanti?able. The residue detected. if any, was below the limit of the study which is 0.5 ng/g. *Value is based on wet weight (5.0 sample processed as received) Values rejected based on unacceptable recoveries. Data has been replaced with either reanalysis or re-extraction values. Results rejected based on apparent contamination. Data has been replaced with re-extracted values. - Not analyzed for Centre Analytical Laboratories, Inc. Page 28 of 151 Centre Study No.: 023-057 Centre Protocol No: Table II continued: Summary of PFOS, FOSA and PFOA Residues Found in Samples Residue Found Centre ID Data Set No. Sponsor ID Store Name Location Matrix PFOS FOSA PFOA 0012819 01170113 Hot Dog 18336 Bruno?s Mobile0012819 Dup 011701B Hot Dog 18336 Bruno?s Mobile0012820 0117018 Hot Dog 18324 Kroger's Decatur0012820 Dup 011701B Hot Dog 18324 Kroger?s Decatur0012821 01 1701B Hot Dog 18313 Winn-Dixie Decatur. AL Hot Dog NQ NQ 0012821 Dup 01 1701B Hot Dog 18313 Winn-Dixie Decatur0012822 011801A Hot Dog 18302 Haloway Decatur0012822 Dup 01 1801A Hot Dog 18302 Haloway Decatur, AL Hot Dog NQ NQ 0012823 011801A Hot Dog 18188 Cub Columbus0012823 Dup 011801A Hot Dog 18188 Cub Columbus0012824 01 1801A Hot Dog 18176 Bi-Lo Cleveland0012824 Dup 011801A Hot Dog 18176 Bi-Lo Cleveland, TN Hot Dog NQ NQ 0012825 01 1801A Hot Dog 18165 Save-a?Lot Cleveland0012825 Dup 01 1801A Hot Dog 18165 Save-a-Lot Cleveland0012826 011801A Hot Dog 18285 Albertson?s Pensacola0012826 Dup 011801A Hot Dog 18285 Albertson?s Pensacola0012827 0118013 Hot Dog 18263 Food World Pensacola, FL Hot Dog NQ NQ 0012827 Dup 011801B Hot Dog 18263 Food World Pensacola0012828 011801B Hot Dog 18153 Watson?s Cleveland, TN Hot Dog NQ NQ 0012828 Dup 011801B Hot Dog 18153 Watson?s Cleveland0012829 011801B Hot Dog 18273 Food World 11 Pensacola0012829 Dup 011801B Hot Dog 18273 Food World 11 Pensacola0012830 011901A Fish 18252 Publix Port St. Lucie, FL Fish NQ NQ NQ 0012830 Dup 011901A Fish 18252 Publix Port St. Lucie, FL Fish NQ NQ NQ 0012831 011901A Fish 18229 Winn-Dixie Port St. Lucie, FL Fish NQ NQ NQ 0012831 Dup 01 1901A Fish 13229 Winn-Dixie Port St. Lucie, FL Fish NQ NQ NQ 0012832 011901A Fish 18241 Albertson?s Port St. Lucie, FL Fish NQ NQ 0012832 Dup 011901A Fish 18241 Albertson?s Port St. Lucie, FL Fish NQ NQ NO 0012833 011901A Fish 18359 Delchamps 11 Mobile, AL Fish NQ NQ NQ 0012833 Dup 011901A Fish 18359 Delchamps 11 Mobile, AL Fish NQ NQ NQ 0012834 011901A Fish 18200 Winn-Dixie Columbus, GA Fish NQ NQ NQ 0012834 Dup 011901A Fish 18200 Winn-Dixie Columbus, GA Fish NQ NQ Not Quanti?able. The residue detected, if any, was below the limit of the study which is 0.5 ng/g. *Value is based on wet weight (5.0 sample processed as received) Values rejected based on unacceptable recoveries. Data has been replaced with either reanalysis or re?extraction values. Results rejected based on apparent contamination. Data has been replaced with re?extracted values. - Not analyzed for Centre Analytical Laboratories, Inc. Page 29 of 151 Centre Study No.: 023-057 Centre Protocol No: Table 11 continued: Summary of PFOS, FOSA and PFOA Residues Found in Samples Residue Found Centre ID Data Set No. Smor ID Store Name Location Matrix PFOS FOSA PFOA 0012835 011901B Fish 18348 Delchamps Mobile, AL Fish NQ NQ 0012835 Dup 011901B Fish 18348 Delchamps Mobile, AL Fish NQ NQ 0012836 01 1901B Fish 18212 Piggly Wiggly Columbus, GA Fish NQ NQ 0012836 Dup 011901B Fish 18212 Pigeg Wiggly Columbus, GA Fish NQ NQ 0012837 011901B Fish 18337 Bruno?s Mobile. AL Fish NQ 0012837 Dup 011901B Fish 18337 Bruno?s Mobile, AL Fish NQ NQ 0012838 011901B Fish 18325 Kroger?s Decatur, AL Fish NQ NQ 0012838 Dup 011901B Fish 18325 Kroger?s Decatur, AL Fish NQ NQ 0012839 0119013 Fish 18314 Winn-Dixie Decatur, AL Fish NQ NQ 0012839 Dup 011901B Fish 18314 Winn-Dixie Decatur, AL Fish NQ NQ 0012835 013001A Fish 18348 Delchamps Mobile, AL Fish NQ - 0012835 Dup 013001A Fish 18348 Delchamps Mobile, AL Fish - NQ - 0012836 013001A Fish 18212 Piggly Wiggly Columbus, GA Fish - NQ - 0012836 Dup 013001A Fish 18212 Piggly Wiggly Columbus, GA Fish - NQ - 0012837 013001A Fish 18337 Bruno?s Mobile, AL Fish - NQ - 0012837 Dup 013001A Fish 18337 Bruno's Mobile, AL Fish - NQ - 0012838 013001A Fish 18325 Kroger?s Decatur, AL Fish NQ - 0012838 Dup 013001A Fish 18325 KrOger?s Decatur, AL Fish - NQ - 0012839 013001A Fish 18314 Winn-Dixie Decatur, AL Fish - NQ - 0012839 Dup 013001 A Fish 18314 Winn-Dixie Decatur, AL Fish - NQ - 0012840 012201A Fish 18303 Haloway Decatur, AL Fish NQ NQ NQ 0012840 Dup 012201A Fish 18303 Haloway Decatur, AL Fish NQ NQ NQ 0012841 012201A Fish 18177 Bi-Lo Cleveland, TN Fish NQ NQ NQ 0012841 Dup 012201A Fish 18177 Bi-Lo Cleveland, TN Fish NQ NQ NQ 0012842 012201A Fish 18166 Save-a-Lot Cleveland, TN Fish NQ NQ NQ 0012842 Dup 012201A Fish 18 166 Save-a-Lot Cleveland, TN Fish NQ NQ 0012843 012201A Fish 18284 Albertson?s Pensacola, FL Fish NQ NQ NQ 0012843 Dup 012201A Fish 18284 Albertson?s Pensacola, FL Fish NQ NQ NQ 0012844 012201A Fish 18262 Food World Pensacola, FL Fish NQ NQ 0012844 Dup 012201A Fish 18262 Food World Pensacola, FL Fish NQ NQ 0012845 012201B Fish 18154 Watson?s Cleveland, TN Fish NQ NQ NQ 0012845 Dup 012201B Fish 18154 Watson?s Cleveland, TN Fish NQ NQ NQ NQ Not Quanti?able. The residue detected, if any, was below the limit of the study which is 0.5 ng/ g. *Value is based on wet weight (5.0 sample processed as received) Values rejected based on unacceptable recoveries. Data has been replaced with either reanalysis or re-extraction values. 2 Results rejected based on apparent contamination. Data has been replaced with re-extracted values. - Not analyzed for Centre Analytical Laboratories, Inc. Page 30 of 151 Centre Study No: 023057 Centre Protocol No: 00P-023-05 7 Table 11 continued: Summary of PFOS, FOSA and PFOA Residues Found in Samples Residue Found Centre ID Data Set No. Sponsor ID Store Name Location Matrix PFOS FOSA PFOA 0012846 012201B Fish 18274 Food World II Pensacola, FL Fish NQ NQ NQ 0012846 Dup 012201B Fish 18274 Food World 11 Pensacola, FL Fish NQ 0012903 020501A Bean 18256 Publix Port St. Lucie, FL Green Bean NQ NQ NQ 0012903 Dup 020501A Bean 18256 Publix Port St. Lucie, FL Green Bean NQ NQ NQ 0012904 020501A Bean 18234 Winn-Dixie Port St. Lucie, FL Green Bean NQ NQ 0012904 Dup 020501A Bean 18234 Winn-Dixie Port St. Lucie, FL Green Bean NQ NQ 0012905 020501A Bean 18245 Albertson?s Port St. Lucie, FL Green Bean NQ NQ 0012905 Dup 020501A Bean 18245 Albertson?s Port St. Lucie. FL Green Bean NQ NQ NQ 0012906 020501A Bean 18363 Delehamps 11 Mobile, AL Green Bean NQ NQ 0.543 0012906 Dup 020501A Bean 18363 Delchamps 11 Mobile, AL Green Bean NQ NQ NQ 0012907 020501A Bean 18204 Winn-Dixie Columbus, GA Green Bean NQ NQ NQ 0012907 Dup 020501A Bean 18204 Winn-Dixie Columbus, GA Green Bean NQ NQ NQ 0012908 020601C Bean 18352 Delchamps I Mobile, AL Green Bean NQ NQ NQ 0012908 Dup 020601C Bean 18352 Delchamps I Mobile, AL Green Bean NQ NQ NQ 0012909 020601C Bean 18216 Piggly Wiggly Columbus, GA Green Bean NQ NQ NQ 0012909 Dup 020601C Bean 18216 Pi ggly Wiggly Columbus, GA Green Bean NQ - NQ NQ 0012910 020601C Bean 18341 Bruno?s Mobile, AL Green Bean NQ NQ NQ 0012910 Dup 020601C Bean 18341 Bruno?s Mobile, AL Green Bean NQ 0012911 020601C Bean 18329 Kroger?s Decatur, AL Green Bean NQ NQ 0012911 Dup 020601C Bean 18329 Kroger?s Decatur, AL Green Bean NQ NQ 0012912 020601C Bean 18318 Winn-Dixie Decatur, AL Green Bean NQ NQ NQ 0012912 Dup 020601C Bean 18318 Winn-Dixie Decatur, AL Green Bean NQ NQ NQ 0012913 020801C Bean 18307 Haloway Decatur, AL Green Bean NQ NQ 0012913 Dup 020801C Bean 18307 Haloway Decatur, AL Green Bean NQ NQ 0012914 020801C Bean 18193 Cub Columbus, GA Green Bean NQ NQ 0012914 Dup 020801C Bean 18193 Cub Columbus, GA Green Bean NQ NQ NQ 0012915 020801C Bean 18182 Bi-Lo Cleveland, TN Green Bean NQ NQ NQ 0012915 Dup 020801C Bean 18182 Bi?Lo Cleveland, TN Green Bean NQ NQ NQ 0012916 020801C Bean 18289 Albertson?s Pensacola, FL Green Bean NQ NQ NQ 0012916 Dup 020801C Bean 18289 Albertson?s Pensacola, FL Green Bean NQ NQ NQ 0012917 020801C Bean 18267 Food World Pensacola, FL Green Bean NQ NQ NQ 0012917 Dup 020801C Bean 18267 Food World Pensacola, FL Green Bean NQ NQ NQ NQ Not Quanti?able. The residue detected, if any, was below the limit of the study which is 0.5 ng/ g. *Value is based on wet weight (5.0 sample processed as received) Values rejected based on unacceptable recoveries. Data has been replaced with either reanalysis or re?extraction values. Results rejected based on apparent contamination. Data has been replaced with re?extracted values. - Not analyzed for Centre Analytical Laboratories, Inc. Page 31 of 151 Centre Study No.: 023-057 Centre Protocol No: 00P-023-057 Table 11 continued: Summary of PFOS, FOSA and PFOA Residues Found?in Samples Residue Found Centre ID Data Set No. Sponsor ID Store Name Location Matrix PFOS FOSA PFOA 0012918 020801D Bean 36868 Watson?s Cleveland, TN Green Bean NQ NQ NQ 0012918 Dup 020801D Bean 36868 Watson's Cleveland, TN Green Bean NQ NQ NQ 0012919 020801D Bean 18278 Food World II Pensacola, FL Green Bean NQ NQ 0012919 Dup 020801D Bean 18278 Food World II Pensacola, FL Green Bean NQ NQ 0012867 020701A Milk 18254 Publix Port St. Lucie, FL Milk NQ NQ 0012867 Dup 020701A Milk 18254 Publix Port St. Lucie, FL Milk NQ NQ 0012868 020701A Milk 18231 Winn-Dixie Port St. Lucie, FL Milk NQ NQ 0012868 Dup 020701A Milk 18231 Winn-Dixie Port St. Lucie, FL Milk NQ 0012869 020701A Milk 18243 Albertson?s Port St. Lucie, FL Milk NQ NQ NQ 0012869 Dup 020701A Milk 18243 Albertson?s Port St. Lucie, FL Milk NQ NQ NQ 0012870 020701A Milk 18361 Delchamps II Mobile, AL Milk NQ NQ 0012870 Dup 020701A Milk 18361 Delchamps II Mobile, AL Milk NQ NQ 0012871 020701A Milk 18202 Winn-Dixie Columbus, GA Milk NQ NQ NQ 0012871 Dup 020701A Milk 18202 Winn-Dixie Columbus, GA Milk 0.693 NQ NQ 0012872 020701B Milk 18350 Delchamps I Mobile, AL Milk NQ NQ NQ 0012872 Dup 020701B Milk 18350 Delchamps I Mobile, AL Milk NQ NO 0012873 020701B Milk 18214 Piggly Wiggly Columbus, GA Milk NQ NQ NQ 0012873 Dup 020701B Milk 18214 Piggly Wiggly Columbus, GA Milk NQ NQ NQ 0012874 0207018 Milk 18339 Bruno?s Mobile, AL Milk NQ NQ NQ 0012874 Dup 020701B Milk 18339 Bruno?s Mobile, AL Milk NQ NQ NQ 0012875 020701B Milk 18327 Kroger?s Decatur, AL Milk NQ NQ NQ 0012875 Dup 020701B Milk 18327 Kroger?s Decatur, AL Milk NQ NQ NQ 0012876 020701B Milk 18316 Winn-Dixie Decatur, AL Milk NQ NO NO 0012876 Dup 020701B Milk 18316 Winn~Dixie Decatur, AL Milk NQ NQ NQ 0012877 020801A Milk 18305 Haloway Decatur, AL Milk NQ NQ NQ 0012877 Dup 020801A Milk 18305 Haloway Decatur. AL Milk NQ 0012878 020801A Milk 18190 Cub Columbus, GA Milk NQ NQ NQ 0012878 Dup 020801A Milk 18190 Cub Columbus, GA Milk NQ NQ 0012879 020801A Milk 18179 Bi-Lo Cleveland, TN Milk NQ NQ NQ 0012879 Dup 020801A Milk 18179 Bi-Lo Cleveland, TN Milk NQ NQ NQ 0012880 020801A Milk 18168 Save-a-Lot Cleveland, TN Milk NQ NQ NQ 0012880 Dup 020801A Milk 18168 Save-a-Lot Cleveland, TN Milk 0.573 NQ NQ NQ Not Quanti?able. The residue detected, if any, was below the limit of the study which is 0.5 ng/ g. *Value is based on wet weight (5.0 sample processed as received) 1 Values rejected based on unacceptable recoveries. Data has been replaced with either reanalysis or re-extraction values. Results rejected based on apparent contamination. Data has been replaced with re-extracted values. - Not analyzed for Centre Analytical Laboratories, Inc. Page 32 of 151 Centre Study No.: 023-057 Centre Protocol No: 00P-023-057 Table 11 continued: Summary of PFOS, FOSA and PFOA Residues Found in Samples Residue Found Centre ID Data Set No. Smnsor ID Store Name Location Matrix PFOS FOSA PFOA 0012881 020801A Milk 18287 Albertson?s Pensacola, FL Milk NQ NQ NQ 0012881 Dup 020801A Milk 18287 Albertson?s Pensacola, FL Milk NQ NQ NQ 0012882 0208018 Milk 18265 Food World Pensacola, FL Milk 0.852 NQ NQ 0012882 Dup 020801B Milk 18265 Food World Pensacola, FL Milk NQ NQ NQ 0012883 020801B Milk 18156 Watson?s Cleveland, TN Milk NQ NQ 0012883 Dup 020801B Milk 18156 Watson?s Cleveland, TN Milk NQ NQ NQ 0012884 0208018 Milk 18276 Food World 11 Pensacola, FL Milk NQ NQ NQ 0012884 Dup 020801B Milk 18276 Food World 11 Pensacola, FL Milk 0.605 NQ 0012926 020901C Apple 18205 Winn-Dixie Columbus, GA Apple NQ NQ NQ 0012926 Dup 020901C Apple 18205 Winn-Dixie Columbus, GA Apple NQ NQ NQ 0012927 020901C Apple 18257 Publix Port St. Lucie, FL Apple NQ NQ NQ 0012927 Dup 020901C Apple 18257 Publix Port St. Lucie, FL Apple NQ NQ 0012928 020901C Apple 18235 Winn-Dixie Port St. Lucie, FL Apple NQ NQ NQ 0012928 Dup 020901C Apple 18235 Winn-Dixie Port St. Lucie, FL Apple NQ NQ 0012929 020901C Apple 18246 Albertson?s Port St. Lucie, FL Apple NQ NQ 0012929 Dup 020901C Apple 18246 Albertson?s Port St. Lucie, FL Apple NQ NQ NQ 0012930 020901C Apple 18364 Delchamps II Mobile, AL Apple NQ NO 0012930 Dup 020901C Apple 18364 Delchamps 11 Mobile, AL Apple NQ NQ NQ 0012931 021201A Apple 18353 Delchamps I Mobile, AL Apple NQ NQ NQ 0012931 Dup 021201A Apple 18353 Delchamps I Mobile, AL Apple NQ NQ NQ 0012932 021201A Apple 18217 Piggly Wiggly Columbus, GA Apple NQ NQ NQ 0012932 Dup 021201A Apple 18217 Piggly Wiggly Columbus, GA Apple NQ NQ NQ 0012933 021201A Apple 18342 Bruno?s Mobile, AL Apple NQ NQ NQ 0012933 Dup 021201A Apple 18342 Bruno?s Mobile, AL Apple NQ NQ NQ 0012934 021201 A Apple 18330 Kroger?s Decatur, AL Apple NQ NQ NQ 0012934 Dup 021201A Apple 18330 Kroger?s Decatur, AL Apple NQ NQ 2.35 0012935 021201A Apple 18319 Winn-Dixie Decatur, AL Apple NQ NQ NQ 0012935 Dup 021201A Apple 18319 Winn?Dixie Decatur, AL Apple NQ NQ NQ 0012936 021201B Apple 18308 Haloway Decatur, AL Apple NQ NQ NQ 0012936 Dup 021201B Apple 18308 Haloway Decatur, AL Apple NQ NQ NQ 0012937 021201B Apple 18194 Cub Columbus, GA Apple NQ NQ 0012937 Dup 021201B Apple 18194 Cub Columbus, GA Apple NQ Not Quanti?able. The residue detected, if any, was below the limit of the study which is 0.5 ng/g. *Value is based on wet weight (5.0 sample processed as received) Values rejected based on unacceptable recoveries. Data has been replaced with either reanalysis or re-extraction values. Results rejected based on apparent contamination. Data has been replaced with re-extracted values. - Not analyzed for Centre Analytical Laboratories, Inc. Page 33 of 151 Centre Study No: 023-057 Centre Protocol No: 00P-023-057 Table 11 continued: Summary of PFOS, FOSA and PFOA Residues Found in Samples Residue Found Centre ID Data Set No. Sponsor ID Store Name Location Matrix PFOS FOSA PFOA 0012938 02120113 Apple 18183 Bi-Lo Cleveland, TN Apple NQ NQ NQ 0012938 Dup 0212013 Apple 18183 Bi-Lo Cleveland, TN Apple NQ NQ NQ 0012939 021201B Apple 18170 Save-a?Lot Cleveland, TN Apple NQ 0012939 Dup 021201B Apple 18170 Save-a-Lot Cleveland, TN Apple NQ NQ 0012940 021201B Apple 18290 Albertson?s Pensacola, FL Apple NQ NQ NQ 0012940 Dup 021201B Apple 18290 Albertson's Pensacola, FL Apple NQ NQ 0012941 021201C Apple 18268 Food World Pensacola, FL Apple NQ 1 .13 0012941 Dup 021201 Apple 18268 Food World Pensacola, FL Apple NQ NQ 0012942 021201C Apple 18159 Watson?s Cleveland, TN Apple NQ NQ 0012942 Dup 021201C Apple 18159 Watson?s Cleveland, TN Apple 0012943 021201C Apple 18279 Food World 11 Pensacola, FL Apple NQ NQ 0012943 Dup 021201C Apple 18279 Food World Pensacola, FL Apple NQ NQ NQ 0012885 020901 A Bread 18255 Publix Port St. Lucie, FL Bread NQ NQ NQ 0012885 Dup 020901A Bread 18255 Publix Port St. Lucie, FL Bread NQ NQ 0012886 020901A Bread 18233 Wianixie Port St. Lucie, FL Bread NQ NQ NQ 0012886 Dup 020901A Bread 18233 Winn-Dixie Port St. Lucie, FL Bread NQ NQ NQ 0012887 020901A Bread 18244 Albertson?s Port St. Lucie, FL Bread NQ NQ NQ 0012887 Dup 020901A Bread 18244 Albertson?s Port St. Lucie, FL Bread NQ NQ 0012888 020901A Bread 18362 Delchamps 11 Mobile, AL Bread NQ NQ NQ 0012888 Dup 020901A Bread 18362 Delchamps Mobile, AL Bread NQ NQ NQ 00 128 89 020901 A Bread 18203 Winn-Dixie Columbus, GA Bread NQ NQ NQ 0012889 Dup 020901A Bread 18203 Winn-Dixie Columbus, GA Bread NQ NQ NQ 0012890 0209018 Bread 18351 Delchamps I Mobile. AL Bread NQ NQ 0012890 Dup 0209013 Bread 18351 Delchamps I Mobile, AL Bread NQ NQ NQ 0012891 02090113 Bread 18215 Piggly Wiggly Columbus, GA Bread NQ NQ NQ 0012891 Dup 0209013 Bread 18215 Piggly Wiggly Columbus, GA Bread NQ NQ NQ 0012892 020901B Bread 18340 Bruno?s Mobile, AL Bread NQ NQ NQ 0012892 Dup 0209013 Bread 18340 Bruno?s Mobile, AL Bread NO NO NQ 0012893 020901B Bread 18328 Kroger?s Decatur, AL Bread NQ NQ NQ 0012893 Dup 0209018 Bread 18328 Kroger?s Decatur, AL Bread NQ NQ NQ 0012894 020901B Bread 183 17 Winn-Dixie Decatur, AL Bread NQ NQ NQ 0012894 Dup 0209013 Bread 18317 Winn-Dixie Decatur, AL Bread NQ NQ Q. NQ Not Quanti?able. The residue detected, if any, was below the limit of the study which is 0.5 ng/g. *Value is based on wet weight (5.0 sample processed as received) Values rejected based on unacceptable recoveries. Data has been replaced with either reanalysis or re-extraction values. Results rejected based on apparent contamination. Data has been replaced with re~extracted values. - Not analyzed for . A Sample result fell below 0.5 ng/g when adjusting for purity of PFOA. Centre Analytical Laboratories, Inc. Page 34 of 151 Centre Study No.: 023-057 Centre Protocol No: 00P-023-057 Table II continued: Summary of PFOS, FOSA and PFOA Residues Found in Samples Residue Found Centre ID Data Set No. Sponsor ID Store Name Location Matrix PFOS FOSA PFOA 0012895 021301A Bread 18306 Haloway Decatur, AL Bread NQ NQ NQ 0012895 Dup 021301A Bread 18306 Haloway Decatur, AL Bread NQ NQ NQ 0012896 021301A Bread 18192 Cub Columbus, GA Bread NQ NQ 0012896 Dup O21301A Bread 18192 Cub Columbus, GA Bread NQ NQ NQ 0012897 021301A Bread 18181 Bi-Lo Cleveland, TN Bread NQ NQ NQ 0012897 Dup 021301A Bread 18181 Bi-Lo Cleveland, TN Bread NQ NQ NQ 0012898 021301A Bread 18172 Save-a-Lot Cleveland, TN Bread NQ NQ 0012898 Dup 021301A Bread 18172 Save-a-Lot Cleveland, TN Bread NQ NQ 0012899 021301A Bread 18288 Albertson's Pensacola, FL Bread NQ NQ NQ 0012899 Dup 021301A Bread 18288 Albertson?s Pensacola, FL Bread NQ NQ NQ 0012900 021301B Bread 18266 Food World Pensacola. FL Bread NQ NQ 0012900 Dup 021301B Bread 18266 Food World Pensacola, FL Bread NQ NQ NQ 0012901 021301B Bread 18158 Watson?s Cleveland, TN Bread NQ NQ NQ 0012901 Dup 021301B Bread 18158 Watson?s Cleveland, TN Bread NQ NQ NQ 0012902 021301B Bread 18277 Food World 11 Pensacola, FL Bread NQ NQ NQ 0012902 Dup 021301B Bread 18277 Food World 11 Pensacola, FL Bread NQ NQ 0.524 001275 8 021301C Beef 18248 Publix Port St. Lucie, FL Ground Beef NQ NQ 0012758 Dup 021301C Beef 18248 Publix Port St. Lucie, FL Ground Beef NQ NQ 0.504 0012759 021301C Beef 18225 Winn-Dixie Port St. Lucie. FL Ground Beef NQ NQ NQ 0012759 Dup 021301C Beef 18225 Winn-Dixie Port St. Lucie, FL Ground Beef NQ NQ NQ 0012760 021301C Beef 18237 Albertson?s Port St. Lucie, FL Ground Beef NQ NQ 1.09 0012760 Dup 021301C Beef 18237 Albertson?s Port St. Lucie, FL Ground Beef NQ NQ 0012761 021301C Beef 18355 Delchamps 11 Mobile, AL Ground Beef NQ NQ NQ 0012761 Dup 021301C Beef 18355 Delchamps 11 Mobile, AL Ground Beef NQ NQ NQ 0012762 021301C Beef 18196 Winn-Dixie Columbus, GA Ground Beef NQ NQ NQ 0012762 Dup 021301C Beef 18196 Winn-Dixie Columbus, GA Ground Beef NQ NQ NQ 0012763 021301D Beef 18344 Delchamps I Mobile, AL Ground Beef 0.570 NQ NQ 0012763 Dup 021301D Beef 18344 Delchamps 1 Mobile, AL Ground Beef 0.587 NQ NQ 0012764 021301D Beef 18208 Piggly Wiggly Columbus, GA Ground Beef NQ NQ NQ 0012764 Dup 021301D Beef 18208 Piggly Wiggly Columbus, GA Ground Beef NQ NQ NQ 0012765 021301D Beef 18333 Bruno?s Mobile, AL Ground Beef NQ NQ NQ 0012765 Dup 021301D Beef 18333 Bruno?s Mobile. AL Ground Beef NQ NQ NQ NQ Not Quanti?able. The residue detected, if any, was below the limit of the study which is 0.5 ng/g. *Value is based on wet weight (5.0 sample processed as received) Values rejected based on unacceptable recoveries. Data has been replaced with either reanalysis or re-extraction values. Result is suspect. Apparent contamination. "4 Results rejected based on apparent contamination. Data has been replaced with re-extracted values. - Not analyzed for Centre Analytical Laboratories, Inc. Page 35 of 151 Centre Study No.: 023-057 Centre Protocol No: Table 11 continued: Summary of PFOS, FOSA and PFOA Residues Found in Samples Residue Found Centre ID Data Set No. iponsor ID Store Name Location Matrix PFOS FOSA PFOA 0012766 021301D Beef 18321 Kroger?s Decatur, AL Ground Beef NQ NQ NQ 0012766 Dup 021301D Beef 18321 Kroger?s Decatur, AL Ground Beef NQ NQ 0012767 021301D Beef 18310 Winn~Dixie Decatur, AL Ground Beef NQ NQ NQ 0012767 Dup 0213011) Beef 18310 Winn-Dixie Decatur, AL Ground Beef NQ 0012768 021401A Beef 18300 Haloway Decatur, AL Ground Beef NQ NQ NQ 0012768 Dup 021401A Beef 18300 Haloway Decatur, AL Ground Beef NQ NQ NQ 0012769 021401A Beef 18185 Cub Columbus, GA Ground Beef NQ NQ NQ 0012769 Dup 021401A Beef 18185 Cub Columbus, GA Ground Beef NQ NQ NQ 0012770 O21401A Beef 18173 Bi?Lo Cleveland, TN Ground Beef NQ NQ 0012770 Dup 021401A Beef 18173 Bi-Lo Cleveland, TN Ground Beef NQ NQ NQ 0012771 021401A Beef 18162 Save-a-Lot Cleveland, TN Ground Beef NQ NQ 0012771 Dup 021401A Beef 18162 Save-a~Lot Cleveland, TN Ground Beef NQ NQ NQ 0012772 021401A Beef 18281 Albertson?s Pensacola, FL Ground Beef NQ NQ NQ 0012772 Dup 021401A Beef 18281 Albertson?s Pensacola, FL Ground Beef NQ NQ 0012773 0214013 Beef 18259 Food World Pensacola, FL Ground Beef NQ NQ NQ 0012773 Dup 0214013 Beef 18259 Food World Pensacola, FL Ground Beef NQ NQ NQ 0012774 021401B Beef 18161 Watson?s Cleveland, TN Ground Beef NQ NQ NQ 0012774 Dup 0214018 Beef 18161 Watson?s Cleveland, TN Ground Beef NQ NQ NQ 0012775 021401B Beef 18270 Food World 11 Pensacola, FL Ground Beef NQ NQ NQ 0012775 Dup 021401B Beef 18270 Food World II Pensacola, FL Ground Beef NQ NQ NQ 0012847 012301A Egg 18253 Publix Port St. Lucie, FL Egg NQ 0012847 Dup 012301A Egg 18253 Publix Port St. Lucie, FL Egg NQ 0012848 012301A Egg 18230 Winn-Dixie Port St. Lucie, FL Egg NQ 0012848 Dup 012301A Egg 18230 Winn~Dixie Port St. Lucie, FL Egg NQ 0012849 012301A Egg 18242 Albertson?s Port St. Lucie, FL Egg NQ 0012849 Dup 012301A Egg 18242 Albertson's Port St. Lucie, FL Egg NQ 0012850 012301A Egg 18360 Delchamps 11 Mobile, AL Egg NQ 0012850 Dup 012301A Egg 18360 Delchamps II Mobile, AL Egg NQ 0012851 012301A Egg 18201 Winn-Dixie Columbus, GA Egg NQ 0012851 Dup 012301A Egg 18201 Winn-Dixie Columbus, GA Egg NQ 0012852 01230113 Egg 18349 DelchampsI Mobile, AL Egg NQ 0012852 Dup 012301B Egg 18349 Delchamps I Mobile, AL Egg NQ NQ Not Quanti?able. The residue detected, if any, was below the limit of the study which is 0.5 ng/ g. *Value is based on wet weight (5.0 sample processed as received) Values rejected based on unacceptable recoveries. Data has been replaced with either reanalysis or re-extraction values. Results rejected based on apparent contamination. Data has been replaced with re-extracted values. - Not analyzed for Centre Analytical Laboratories, Inc. Page 36 of 151 Centre Study No.: 023-057 Centre Protocol No: Table 11 continued: Summary of PFOS, FOSA and PFOA Residues Found in Samples Residue Found Centre ID Data Set No. Sponsor ID Store Name Location Matrix PFOS FOSA PFOA 0012853 0123013 Egg 18219 Peggy?s Port St. Lucie, FL Egg NQ 0012853 Dup 0123013 Egg 18219 Peggy?s Port St. Lucie, FL Egg NQ 0012854 0123013 Egg 18213 Piggly Wiggly Columbus, GA Egg NQ 0012854 Dup 0123013 Egg 18213 Piggly Wiggly Columbus, GA Egg NQ 0012855 012301B Egg 18338 Bruno?s Mobile, AL Egg NQ 0012855 Dup 0123013 Egg 18338 Bruno's Mobile, AL Egg NQ 0012856 0123013 Egg 18326 Kroger?s Decatur, AL Egg NQ 0012856 Dup 0123013 Egg 18326 Kroger?s Decatur, AL Egg NQ 0012857 012401A Egg 18315 Winn-Dixie Decatur, AL Egg NO 0012857 Dup 012401A Egg 18315 Winn?Dixie Decatur, AL Egg 0012858 012401A Egg 18304 Haloway Decatur, AL Egg NQ 0012858 Dup 012401A Egg 18304 Haloway Decatur, AL Egg 0012859 012401A Egg 18189 Cub Columbus, GA Egg NQ 0012859 Dup 012401A Egg 18189 Cub Columbus, GA Egg 0012860 012401A Egg 18178 Bi?Lo Cleveland, TN Egg NQ 0012860 Dup 012401A Egg 18178 Bi?Lo Cleveland, TN Egg NO 0012861 012401A Egg 18167 Save-a-Lot Cleveland, TN Egg NQ 0012861 Dup 012401A Egg 18167 Save-a?Lot Cleveland, TN Egg NQ 0012862 0124013 Egg 18286 Albertson?s Pensacola. FL Egg NQ 0012862 Dup 0124013 Egg 18286 Albertson?s Pensacola, FL Egg NO 0012863 0124013 Egg 18264 Food World Pensacola, FL Egg NQ 0012863 Dup 012401B Egg 18264 Food World Pensacola, FL Egg NQ 0012864 0124013 Egg 18296 Farmer?s Market Mobile, AL Egg NO 0012864 Dup 012401B Egg 18296 Farmer?s Market Mobile, AL Egg 0012865 0124013 Egg 18155 Watson's Cleveland, TN Egg NQ 0012865 Dup 0124013 Egg 18155 Watson's Cleveland, TN Egg NQ 0012866 0124013 Egg 18275 Food World II Pensacola, FL Egg NQ 0012866 Dup 0124013 Egg 18275 Food World 11 Pensacola, FL Egg NQ 0106429 050801A Egg 21213 Winn-Dixie Port St. Lucie, FL Egg NQ - 0106429 Dup 050801A Egg 21213 Winn-Dixie Port St. Lucie, FL Egg NQ - 0106430 050801A Egg 21214 Albertson?s Port St. Lucie, FL Egg NQ - 0106430 Dup 050801A Egg 21214 Albertson?s Port St. Lucie, FL Egg NQ - NQ Not Quanti?able. The residue detected, if any, was below the limit of the study which is 0.5 ng/g. *Value is based on wet weight (5.0 sample processed as received) Values rejected based on unacceptable recoveries. Data has been replaced with either reanalysis or re-extraction values. Results rejected based on apparent contamination. Data has been replaced with re-extracted values. - Not analyzed for Centre Analytical Laboratories, Inc. Page 37 of 151 Centre Study No.: 023?057 Centre Protocol No: 00P-023-057 Table II continued: Summary of PFOS, FOSA and PFOA Residues Found in Samples Residue Found (nglg)* Centre ID Data Set No. Sponsor ID Store Name Location Matrix PFOS FOSA PFOA 0106431 050801A Egg 21216 Winn-Dixie Columbus, GA Egg NQ 0106431 Dup 050801A Egg 21216 Winn-Dixie Columbus, GA Egg NQ - 0106432 050801A Egg 21217 Delchamps 1 Mobile, AL Egg NQ - 0106432 Dup 050801A Egg 21217 Delchampsl Mobile, AL Egg NQ - 0106433 050801A Egg 21218 Peggy?s Port St. Lucie, FL Egg NQ 0106433 Dup 050801A Egg 21218 Peggy?s Port St. Lucie, FL Egg NQ - 0106434 0508018 Egg 21219 Piggly Wiggly Columbus, GA Egg NQ - 0106434 Dup 0508018 Egg 21219 Piggly Wiggly Columbus, GA Egg NQ - 0106435 0508018 Egg 21221 Kroger?s Decatur. AL Egg NQ - 0106435 Dup 0508018 Egg 21221 Kroger?s Decatur. AL Egg NQ - 0106436 0508018 Egg 21222 Winn-Dixie Decatur, AL Egg NQ - 0106436 Dup 0508018 Egg 21222 Winn-Dixie Decatur, AL Egg NQ - 0106437 0508018 Egg 21223 Haloway Decatur, AL Egg NQ - 0106437 Dup 050801B Egg 21223 Haloway Decatur, AL Egg NQ - 0106438 0508018 Egg 21224 Cub Columbus, GA Egg NQ - 0106438 Dup 0508018 Egg 21224 Cub Columbus, GA Egg NQ - 0106439 050901A Egg 21225 Bi-Lo Cleveland, TN Egg NQ - 0106439 Dup 050901A Egg 21225 Bi-Lo Cleveland, TN Egg NQ - 0106440 050901A Egg 21226 Save-a-Lot Cleveland, TN Egg NQ - 0106440 Dup 050901A Egg 21226 Save?a-Lot Cleveland, TN Egg NQ 0106441 050901A Egg 21227 Albertson?s Pensacola, FL Egg NQ - 0106441 Dup 050901A Egg 21227 Albertson?s Pensacola, FL Egg NQ - 0106442 050901A Egg 21228 Food World Pensacola. FL Egg NQ - 0106442 Dup 050901A Egg 21228 Food World Pensacola, FL Egg NQ - 0106443 050901A Egg 21229 Farmer?s Market Mobile, AL Egg NQ - 0106443 Dup 050901A Egg 21229 Farmer?s Market Mobile, AL Egg NQ - 0106444 0509018 Egg 21230 Watson?s Cleveland, TN Egg NQ - 0106444 Dup 0509018 Egg 21230 Watson's Cleveland, TN Egg NQ - 0106445 0509018 Egg 21231 Food World 11 Pensacola, FL Egg NQ - 0106445 Dup 0509018 Egg 21231 Food World 11 Pensacola, FL Egg NQ - 0106446 0509018 Egg na 51 Egg NQ - 0106446 Dup 0509018 Egg na 3 Egg NQ - NQ Not Quanti?able. The residue detected, if any, was below the limit of the study which is 0.5 ng/g. *Value is based on wet weight (5.0 sample processed as received) Values rejected based on unacceptable recoveries. Data has been replaced with either reanalysis or re- extraction values. Results rejected based on apparent contamination. Data has been replaced with re-extracted values. N=ot analyzed for Sample labels fell off during second shipping and there was no way of telling samples apart. Centre Analytical Laboratories, Inc. Page 38 of 151 Centre Study No.: 023?057 Centre Protocol No: Table II continued: Summary of PFOS, FOSA and PFOA Residues Found in Samples Residue Found Centre ID Data Set No. Sponsor ID Store Name Location Matrix PFOS FOSA PFOA 0106447 0509013 Egg na Egg NQ - 0106447 Dup 0509013 Egg na 35 Egg NQ - 0106448 0509013 Egg na 3 Egg NQ - 0106448 Dup 0509013 Egg na Egg NQ 0106429 051801A Egg 21213 Winn?Dixie Port St. Lucie, FL Egg - - NQ 0106429 Dup 051801A Egg 21213 Winn-Dixie Port St. Lucie, FL Egg - - NQ 0106430 051801A Egg 21214 Albertson?s Port St. Lucie, FL Egg - - NQ 0106430 Dup 051801A Egg 21214 Albertson?s Port St. Lucie, FL Egg - - NO 0106431 051801A Egg 21216 Winn-Dixie Columbus, GA Egg - - NQ 0106431 Dup 051801A Egg 21216 Winn-Dixie Columbus, GA Egg - - NQ 0106432 051801A Egg 21217 Delchamps I Mobile, AL Egg - - NQ 0106432 Dup 051801A Egg 21217 Delchamps 1 Mobile, AL Egg - - NQ 0106433 051801A Egg 21218 Peggy?s Port St. Lucie, FL Egg - - NQ 0106433 Dup 051801A Egg 21218 Peggy?s Port St. Lucie, FL Egg - - NQ 0106434 0518013 Egg 21219 Piggly Wiggly Columbus, GA Egg - - NQ 0106434 Dup 0518013 Egg 21219 Piggly Wiggly Columbus, GA Egg - NQ 0106435 0518013 Egg 21221 Krogcr?s Decatur, AL Egg - NO 0106435 Dup 0518013 Egg 21221 Kroger?s Decatur, AL Egg - - NQ 0106436 0518013 Egg 21222 Winn-Dixie Decatur, AL Egg - - NO 0106436 Dup 0518013 Egg 21222 Winn-Dixie Decatur, AL Egg - - NQ 0106437 0518013 Egg 21223 Haloway Decatur, AL Egg - - NQ 0106437 Dup 0518013 Egg 21223 Haloway Decatur, AL Egg - - NQ 0106438 0518013 Egg 21224 Cub Columbus, GA Egg - - NQ 0106438 Dup 0518013 Egg 21224 Cub Columbus, GA Egg - - NQ 0106439 052101A Egg 21225 Bi-Lo Cleveland, TN Egg - - NO 0106439 Dup 052101151 Egg 21225 Bi-Lo Cleveland, TN Egg - - NQ 0106440 052101A Egg 21226 Save-a?Lot Cleveland, TN Egg - - NO 0106440 Dup 052101A Egg 21226 Save-a?Lot Cleveland, TN Egg - - NO 0106441 052101A Egg 21227 Albertson?s Pensacola, FL Egg - - NO 0106441 Dup 052101A Egg 21227 Albertson?s Pensacola, FL Egg - - NO 0106442 052101A Egg 21228 Food World Pensacola, FL Egg - - NQ 0106442 Dup 052101A Egg 21228 Food World PensacolaNot Quanti?able. The residue detected, if any, was below the limit of the study which is 0.5 nyg. *Value is based on wet weight (5.0 sample processed as received) Values rejected based on unacceptable recoveries. Data has been replaced with either reanalysis or re?extraction values. Results rejected based on apparent contamination. Data has been replaced with re-extracted values. Not analyzed for Sample labels fell off during second shipping and there was no way of telling samples apart. Centre Analytical Laboratories, Inc. Page 39 of 151 Centre Study No.: 023-057 Centre Protocol No: 00P-023-057 Table 11 continued: Summary of PFOS, FOSA and PFOA Residues Found in Samples Residue Found Centre ID Data Set ?No. Sponsor Store Name Location Matrix PFOS FOSA PFOA 0106443 052101A Egg 21229 Farmer's Market Mobile, AL Egg - - NQ 0106443 Dup 052101A Egg 21229 Farmer?s Market Mobile, AL Egg - - NQ 0106444 0521018 Egg 21230 Watson?s Cleveland, TN Egg - - NQ 0106444 Dup 052101B Egg 21230 Watson?s Cleveland, TN Egg - - NQ 0106445 052101B Egg 21231 Food World Pensacola, FL Egg - - NQ 0106445 Dup 0521013 Egg 21231 Food World 11 Pensacola, FL Egg - - NQ 0106446 052101B Egg na Egg - - NQ 0106446 Dup 052101B Egg na 3 Egg - - NQ 0106447 0521018 Egg na Egg - - NQ 0106447 Dup 052101B Egg na Egg - - NQ 0106448 0521018 Egg na 5 Egg - - NQ 0106448 Dup 052101B Egg Not Quanti?able. The residue detected, if any, was below the limit of the study which is 0.5 ng/g. *Value is based on wet weight (5.0 sample processed as received) Values rejected based on unacceptable recoveries. Data has been replaced with either reanalysis or re?extraction values. Results rejected based on apparent contamination. Data has been replaced with re-extracted values. - Not analyzed for Sample labels fell off during second shipping and there was no way of telling samples apart. Centre Analytical Laboratories, Inc. Page 40 of 151