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4 A te & 'i t 3 J1R ENVIRONMENTAL LABORATORY REPORTNO. FACT-TOX-I30 Laboratory Report Analytical Report of Data for PFOS Dietary LC50 Study with Mallards (Sera and Liver) Laboratory Report No. FACT-TOX-130 (W1902) Attachment A Sera Table o f Results Day 8 Day 22 Testing Laboratory 3M Environmental Technology & Safety Services 3M Environmental Laboratory Fluorine Analytical Chemistry Team (FACT) 2-3E-09 935 Bush Avenue, St. Paul, MN 55106 000' > FACT-TOX-130 Study: Product Number(Test Substance): Matrix: Method/Revision; Analytical Equipment System Number. Instrument Software/Verrion: Filename: R-Squared Value: Slope: Y-Interccpt Dates of ExtnctMxVAnalyst: Dates of Analysis/Analyst: Date of Data Reduction/Analyst- Sample Data MALLARD SERUM Day Greap Dose Sample f Method Blk H 20 Blk-1 ICO Blk-2 H 20 Blk-3 ICO Blk-4 Matrix Blk Rabbit Serum Blk-1 Rabbit Serum Blk-2 Rabbit Serum Blk-3 Q C -J0ppbM S Rabbit Scrum Blk-4 RBS06299-MS-I l.0ppm-M SD RBS06299-MSD-L RBS06299-M5-2 RBS06299-MSD-2 RBS06299-MS-3 RJB$06299MSD>3 RBS06299-MS-4 RBS06299-M5D-4 Groapl 5938 0.0 mg/kg 5939 5940 5941 5942 9195 9196 9197 9198 9199 9200 8401 8402 8403 8404 Groepl 9.10 mg/kg food 9190 9191 9192 9193 9194 GraapJ 18.3 mg/kg food 5958 5959 5960 5961 5962 G rup4 36.6 mg/kg food 61 5969 5970 5971 5972 C n m fS 5988 73.2 rajA l food 5989 5990 5991 5992 G n iy C 146 mg/kg food 5998 5999 6000 9173 9174 Gr*op7 293 mg/kg food 9180 9181 9183 G raapl 586 mg/kg food 5978 5979 5981 G reap9 1171 mg/kg food NS Limit of (Juanntatioo (LOQ) PFOS - 0.005 ug/mL PFOS Dietary LC50 Study with Mallards PFOS Mallard Scrum ETS-8-4.1 and ETS-S-3.1 Soup 020199, Amelia 062498 Masslynx3 2 See Attachments See Attachments See Attachments See Attachments 06/29/99 MCH 07/01/99, 07/06/99,07/08/99 DRB/MEE 07/02/99,0707/99,07/09/99 DRB/MEE IPFOSI Reported (ag/mL) r %Rcc <LOQ <LOQ <LOQ <L0Q 0.00742 <LOQ 0.00730 0.00967 107% 74% 103% 78% 96% 126% 99% 119% <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 0.0103 0.00686 <LOQ <LOQ <LOQ 0.00674 <LOQ 0.00819 0.0230 8.81 7.68 8.79 4.04 7.60 9.31 25.6 11.45 8.89 13.7 27.3 29.2 17.7 44.3 34.2 37.8 41.6 51.3 57.8 52.0 63.6 50.6 35.7 81.2 38.6 67.2 58.9 71.2 68.4 94.5 t59 NA Average IPFOStag/mL orttR ec RSD<%) StdL Dtv^ug/mL) <LOQ 0.00813 - 1 Outlier 30 Wb 101% 1 0 ppm 100% NA 16.4 O.OOI33 5% 27% <LOQ - 5 Outliers NA 26.5 7 J8 1.96 49.8 13.8 31.9 30.5 9.75 17.0 48.1 8.19 34.8 53.9 18.8 9.57 65.8 6.29 43.4 107 46.5 NA NA PFOS Pcrfhmrooctanesulfooate Extraction volume ratio equals initial votame/fioal volume. Date EmcmJ/By: 7/06/99, 7/07/99,07/14/99 LAC Date Verified/8y. 08/09/99 OML NA-ooC applicable NS - no sample analyzed ETS-S-5.1 Excel Version 5.(V95 TOX-130-scn-2.xls 000 3/8/01 -J/f FACT-TOX-UO Study: Product NumberfTort Substance): Matrix: MethodHevmoa. Analytkal Equipment System Nw t a . Instrument SoftwareVosk: Filename: R-Squand Value Slop: Y-lntereepc Oaiea o f Extractk/Analyst Dates of Analysis/Analyse Date of Data Roducooo'Analyst Sam ple Data PROS Dietary ICJO Study with Mallards PFOS Mallard Seram ETS-t-4.1 mAETS-6-3. I Soup 020199 Masslyna 3.2 Sec Attachment! See Atzachmcnti Sec Attachments See Attachments 07/07/99 RWW 07/12/99,07/15/99 DRB/GML 07/13/99.07/16/99 DRB/KJH MALLARD SERUM Day 22 Croup Dow Method Blk Matrix Blk Q C -S O ** 1000 ppb Croopl 0.0 mg/kg food Croop2 9.10 m ^kg food Cronp3 11.3 mg/kg food GrmejM 36.6 mg/kg food CroapS 7X2 mg/kg food Graup* 146 mg/kg food Group? 293 mg/kg food Croopl 516 mg/kg food "Group* 1171 mg/kg food Sample# H20Blk-l H20 Bdt*2 H 20 Blk-3 H20 Blk-4 Rabbit Scrum BDc-l Rabbit S e rin Btk2 Rabbit Scremi Blk-3 Rabbit Scrum Blk-4 RS07O79*MS~1 RBS07079*MSD-I RBS07079-MS-2 RBS07079-MSD-2 RBSO7079-MS-I RBS07079-MSD-1 RBSC707P-MS-2 RBS0TO79-MSD-2 6495 6496 6497 6496 6499 6500 5929 5930 5931 5932 5933 5934 5935 5936 5937 9IS5 9166 9167 918 9119 5953 5954 5955 5956 5957 5963 5964 5965 5966 5967 5983 S9M IW 6966 967 5994 5995 5996 5997 9175 9176 9177 9171 9179 5943 5944 5945 5947 $943 ira b si Reported (ag/tnL) erH Ree <LOQ <10Q <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 104% 100% 103% 99% 99% 97% 107% 95% <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 1.05 1.09 161 1.04 1.5 4.40 3.81 4.70 4.92 3.75 4.30 $.63 7.27 7.01 9.69 245 10.0 6.32 7.23 1.43 1X2 11.9 16.2 24.0 mi 1X3 8.43 10.1 16.5 21.5 29.7 15.2 39.4 51.6 25.5 Average IFPO5]0/mL urHRuc RSD(%) Sid. Dev^ng/mL) <LOQ <LOO 101% 100% NA NA 2% % <LOQ 1.49 4.32 613 11.3 11.9 13.4 34.0 NA NA NA 47.3 0.704 12.0 0520 29.1 1.99 66.1 7.49 4X0 7.94 415 5.51 455 15.4 NA PFOS 0.010 ug/mL NA to t applicable Daw Emcrnd/By: Date Verified/ By: 07/14/99, 07/16/99,07/20/99 ] 01/09/99 O f L Gip 9 tentative value, evaporated to kyness. Extraction volume rado equals initial vofumrfbuJ BTS4-5.1 Excel Version 3.0/95 TQX>l30-ecra*Xxls 000" 3M ENVIRONMENTAL LABORATORY REPORTNO. FACT-TOX-130 Laboratory Report Analytical Report of Data for PFOS Dietary LC50 Study with Mallards (Sera and Liver) Laboratory Report No. FACT-TOX-130 (W1902) Attachment B Liver Table o f Results Day 4-7 Day 8 Day 22 Testing Laboratory 3M Environmental Technology & Safety Services 3M Environmental Laboratory Fluorine Analytical Chemistry Team (FACT) 2-3E-09 935 Bush Avenue, St. Paul, MN 55106 * Study: Product NumbetfTest Substance): Matrix: FA C T -T O X -130 PFOS Dietary LCSO Study with Mallards PFOS Mallard Liver M ALLARD L IV E R DAY 4-7 Dose Method Blk QC - I.Oppm** G roup 7 293 mg/kg food G ro u p s 586 mg/fcg food Group9 1171 mg/kg food Sample # MLL09279-H20 Blk-11 MLL09279-H20 BDc-12 ... MLL09279-9196-0-MS-11 M L L 0 9 2 7 9 -9 196-O-MSD-11 MLL09279-9199-0-MS-I2 M L L 0 9 2 7 9 -9 199-O-MSD -12 9182, Day7 5980, DayS 5982, Day6 5946, Day7 5976, Day4 5949, Day4 5952, Day5 5950, Day5 5974, Day5 5 9 5 1 , Day5 5973, Day6 5948, Day6 5975, Day7 PFOS Calc. Cone. tig/g 0.00 0.00 31.1 182 677 536 148106 216457 196822 179996 115890 122122 172280 137062 146732 185296 131286 120973 177851 Concentraioo of PFOS ug/g o r % Ree. <LOQ <LOQ 56% 325% 61% 49% 148 216 197 180 116 122 172 137 147 185 131 121 178 Limit o f Quantitation (LOQ) PFOS: approx. 0.030ug/g NA - not applicable **The MS/MSD and group 1 samples were re-extracted on 10/08/99 to confirm matrix effects. LAC 10/08/99 Mean PFOS ug/g o r % Rec. <LOQ 191% 55% 198 198 145 RSD<%) Std. Dcv.(ug/g) MS/MSD RPD NA 141% 23% 70.7 9.23 18.2 18.3 26.6 FACT-M-2.1 Excel Veraion 5/95 TOX-130-livcr-2.xb 3/8/01 10:44 AM O O O V ?, Study: Product NumbetfTest Substance): Matrix: FACT-TOX-130 PFOS Dietary LC50 Study with Mallards PFOS Mallard Liver MALLARD LIVER DAY 8 Group Dose Method Blk Sample # H 20 Blk-I H20BBC-2 PFOS Calc. Cone. ng/g 0.00 0.00 Concentration of PFOS ug/g o r % Rec. <LOQ <LOQ M ein PFOS ng/g o r % Rec. RSD (%) Std. Dev^ug/g) M S/M SD R PD QC-IOOppb H 20 Blk-3 H20BU-4 MLL06299-3938-0-MS-1 MLL06299-5938-0-MSD-1 0.00 0.00 88.0 89.4 <LOQ <LOQ 74% 75% <LOQ NA 1.0 ppm MLL06299-5940-0-MS-2 802 73% 100 ppb tOOppb MLL06299-59404)-MSD-2 MLL06299-9196-0-MS-3 799 84.4 72% 76% 73% MLL06299-9196-0-MSD-3 733 66% 5% 1.0 ppm MLL06299-8401-O-MS-4 915 76% 1.0 ppm MLL06299*8401-0-MSD-4 894 75% 74% 2% G ro u p l 5938 0.00 <LOQ 0.0 mg/kg food 3939 0.00 <LOQ 3940 0.00 LOQ * 3941 0.00 <LOQ 3942 9195 9196 0.00 <LOQ 0.00 <LOQ 92.8 0.0928 9197 9198 0.00 <LOQ 0.00 <LOQ 9199 9200 8401 8402 132 0.132 0.00 <LOQ 0.00 <LOQ 0.00 <LOQ Gronp2 9.10 mg/lcg food 8403 8404 9190 9191 0.00 0.00 6828 3714 <LOQ <LOQ 6.83 3.71 <LOQ - 2 Outliers NA NA Groap3 18.3 mg/kg food Group4 36.6 mg/kg food G roups 73.2 mg/kg food Group6 146 mg/kg food Group7 293 mg/kg food G roups 9192 9193 9194 5958 5959 5960 5961 5962 5968 3969 5970 5971 5972 5988 5989 5990 5991 5992 5998 5999 6000 9173 9174 9180 9181 9183 9184* 5978 4690 2902 5217 4760 11542 6158 4202 6562 14690 14901 9864 20377 16505 15347 16890 29729 51544 34849 38069 35398 32775 55034 32084 59768 56336 50650 248075 32469 4.69 2.90 5.22 4.76 11.5 6.16 4.20 6.56 14.7 14.9 9.86 20.4 16.5 153 16.9 29.7 51.5 34.8 38.1 35.4 32.8 55.0 32.1 59.8 56.3 50.6 248 32.5 4.67 6.65 153 29.7 38.8 55.6 32.1 1.50 43.7 2.90 24.8 3.78 49.8 14.78 28.1 10.9 8.29 4.61 386 mg/kg food firoup9-117l mg/kg food 5979 5981 NS 75542 70474 NA 75.5 70.5 NA 59.5 NA 39.6 23.5 NA Lindt o f Quantitation (LOQ) PFOS: approx. 0.030ug/g NA - not applicable NS - no sample analyzed * One outlier, not included in any calculations FACT-M-2.1 Excel Version 3/93 T0X-130-liver-2.xls 3/8/01 10:44 AM Study: Product NumbetfTest Substance): M ania: FACT-TOX-130 PFOS Dietary LC50 Study with Mallards PFOS Mallard Uver M A LL A R D L IV E R DAY 22 Doie Sample* Method Blk H 20 Blk-1 H 20 Blk-2 H 20 BDc-3 Q C -lO O ppb H20Blk-4 6495-0-MS-l 6495-O-MSD-l 649643-MS-2 1.0 ppm 6496-0-MSD-2 6497-0-MS-3 6497-0-MSD-3 6498-0-MS-4 G roupl 0.0 mg/kg food 6498-0-MSD-4 6495 6496 9497 6498 6499 6500 5929 5930 5931 5932 5933 5934 5935 5936 5937 Gronp2 9.10 mg/kg food 9185 9186 9187 9188 9189 Groop3 18.3 mg/kg food 5953 5954 5955 5956 5957 Groop4 36.6 mg/kg (bod 5963 5964 5965 5966 Groop5 73.2 mg/kg food 5967 5983 5984 5985 Gronp6 146 mg/kg food 5986 5987 5993 5994 5995 5996 5997 Cronp7 293 mg/kg food 9175 9176 9177 9178 9179 G ronpl 586 mg/kg food 5943 $944 5945 G rop9-ll7l ng/kiiood 5947 5977 PFOS - Pcrfluorooctanesulfonale Limit o f Quantitation (LOQ) PFOS: approx. 0.030ug/g NA * not applicable PFOS Cale. C one ng/g 1.72 1.09 1.07 1.51 107 101 111 126 1033 till 1093 1053 22.2 19.3 12.8 13.2 8.53 13.4 5.63 4.51 1.72 3.10 8.99 8.49 9.36 4.83 5.51 911 876 1569 735 1038 1802 2186 1930 2667 1594 1626 3035 3154 3639 5366 10254 8812 7957 10847 8195 13976 7737 8374 14015 19574 7494 5633 7687 12522 12663 18754 9763 24677 27443 16261 Concentra Don of PFOS ug/g o r % Ree. <LOQ <LOQ <LOQ <LOQ 90% 85% 94% 107% 87% 93% 91% 88% <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 0.911 0.B76 1.57 0.735 1.04 1.80 2.19 1.93 2.67 1.59 1.63 3.03 3.15 3.64 5.37 10.3 8.81 7.96 10.8 8.20 14.0 7.74 8.37 14.0 19.6 7.49 5.63 7.69 12.5 12.7 18.8 9.76 24.7 27.4 16.3 Mean RSD (%) PFOS Std. Devdag/c) ag/gor % Ree. MS/MSD RPD <LOQ NA <LOQ NA 94% 9% 90% 3% <LOQ NA NA 31.4 1.03 0.322 20.3 2.04 0.413 40.0 3.36 1.35 13.9 9.21 1.28 38.1 12.7 4.85 34.8 9.20 3.20 38.8 20.2 7.82 NA NA FACT-M-2.1 Excel Version 5/95 TOX-l30-liver-2.xls 3/S/D1 10:44 AM t-'-r / v o o o / t' V Laboratory R eport-R evision 1 Analytical Report of Data for PFOS Dietary LC50 Study with Mallards (Sera and Liver) Laboratory Report No. FACT-TOX-130 (W1902) Testing Laboratory 3M Environmental Technology & Safety Services 3M Environmental Laboratory Fluorine Analytical Chemistry Team (FACT) 2-3E-09 935 Bush Avenue, St. Paul, MN 55106 Laboratory Contact Kris Hansen, Ph.D. Bldg. 2-3E-09 P.O .Box 3331 St. Paul, MN 55133-3331 Phone: (651)778-6018 FAX: (651) 778-6176 Revision Date: March 19, 2001 Page l o f6 000? i 3M ENVIRONMENTAL LABORATORY REPORT NO. FACT-TOX-130 1 Introduction .* , :1 This study was designed to quantitatively assess perfluorooctanesulfonate (PFOS, C8F17S03-, CAS # 279539-3) levels in die sera and liver of mallard ducks exposed to PFOS through d iet Details o f dosing conditions, clinical observations and other toxicity data were generated by the in-life testing facility (W ildlife International) and are not included in this report Subsets o f the nine groups o f test animals were sacrificed on day 8 and day 22, post-dose. Sera and liver collected from the sacrificed animals were sent to the 3M Environmental Lab and analyzed quantitatively for PFOS. Tissues from some animals that died before the scheduled sacrifice date were collected and analyzed also; results are included in this report With few exceptions, PFOS levels in the sera and livers o f the mallards increased with dose group. Additionally, considering the average PFOS levels within each dose group, both liver and sera levels o f PFOS declined dramatically between day 8 and day 22. In most animals, for a specific time point, the ratio o f PFOS concentration in sera (pg/mL) to PFOS concentration in liver (pg/g) was greater than 1. No data was collected for analytes other than PFOS. Although rigorous quality control measures and 3M Environmental Laboratory Standard Operating Procedures were followed, the acquisition o fthis data was not necessarily collected according to applicable Good Laboratory Practices. Data presented here is the highest quality data available at this time. In-phase testing was conducted according to applicable Good Laboratory Practices. The conduct o f the in-life phase is the sole responsibility of Wildlife International Ltd. See attachment C for the in-life protocol 2 Sample Receipt The Environmental Lab received 60 liver, 58 bile, 46 blood, and 46 serum specimens, frozen, on 05/19/99. Upon specimen receipt, a 3M chain o f custody was initiated. The Environmental Lab received 50 liver, 50 bile, 50 blood, and 50 serum samples, frozen, on 06/29/99. Upon specimen receipt, a 3M chain o f custody was initiated. A copy o f each form can be found in an Attachment to this report. There is no holding time criteria associated with these samples for LC/ESMSMS analysis. M ethods- AriidyticatitnU -V . . JV ' ,, "I iVj-,.,' A nalytical methods ETS-8-4.1, Extraction o f Potassium Perfluorooctanesulfonate or Other Fhiorochemical Compounds from Serum for Analysis Using HPLC-Electrospray/Mass Spectrometry with thefollowing exceptions: Due to toe small volume o f mallard sera available, standard curves were prepared in methanol instead o f from mallard sera. Available sample volumes were so sm all there was not enough sera for matrix spike studies. As an indicator o f gross error, rabbit serum was used as a surrogate matrix. Sixteen matrix spikes were prepared in rabbit sera. PFOS lot 171 was used as reference material. ETS-8-6.0, Extraction o fPotassium Perfluorooctanesulfonate or Other Fhiorochemical Compounds from Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry with thefollowing exception: Page 2 o f6 ooo? }M ENVIRONMENTAL LABORA TORY REPORT NO. FACT-TOX-130 Due to the small amount o f mallard liver available, standard curves were prepared in methanol instead o f from mallard liver. Twelve matrix spikes were prepared from the mallard liver. As described in the method, all results are reported in terms o f pg of analyte per gram of liver (wet weight). PFOS lot 171 was used as reference material. ETS-8-5.1, Analysis o f Potassium Perfluorooctanesulfonate or Other Fluorochemicals in Serum Extracts Using HPLC-Electrospray/Mass Spectrometry ETS-8-7.0, Analysis o f Potassium Perfluorooctanesulfonate or Other Fluorochemical in Liver Extracts Using HPLC-Electrospray/Mass Spectrometry Sam ple preparation -H PLC/ESM SM S: ion-pairing extraction Analyte is extracted from a sample matrix with ion pairing reagent [tetrabutyl ammonium hydrogen sulfate (TBA)] in a pH-controlled environment The cationic reagent selectively targets anionic fluorochemicals. Once the anion-TBA pair is formed, the analyte is transferred into a non-polar organic solvent (methyl-iertbutyl ether), dried, and reconstituted in methanol for MS analysis. HPLC/ESM SM S In HPLC, an aliquot o f extract is injected and passed through a reverse phase liquid chromatographic column. Based on the affinity o f the analyte for the stationary phase in the column relative to the liquid mobile phase, the analyte is retained for a characteristic amount of time. For example, in a standard solution PFOS may elute at 8.0 minutes. Retention times between a standard PFOS solution and the analyte extracted from tissue in this analysis were matched on the HPLC system to within 1%. Following HPLC separation, ESMSMS provides a rapid and accurate means for analyzing a wide range o f organic compounds, including fluorochemicals. Electrospray, an ionization technique used prim arily for detection o f molecular ions, is generally operated at relatively mild temperatures. Molecules are ionized, and a primary ion, characteristic o f the analyte, is selected. Ions are accelerated for collision with argon gas resulting in fragmentation of the selected species; subsequent collisions create smaller secondary ionic fragments unique to die primary ion, which are detected. For example, for PFOS (CgFiTSOj") analysis, ion 499 is selected as the characteristic primary ion. This ion is fragmented into other ions such as 80 amu (corresponding to S 0 3"), and 230 amu (C3F6S0 3'). Each o f these secondary fragments is detected and can be used to differentiate PFOS from other compounds that might have the same characteristic 499 amu primary ion, but different chemical compositions and secondary ion fragmentation patterns. 5.1 Calibration For quantitative determinations, a mid-level, calibration curve verification (CCV) standard in methanol was analyzed every 5 to 10 samples to monitor instrumental drift Calibration curve verification standards are acceptable if instrumental response is within +/- 30% o f die expected value. In this study, all CCV standards were acceptable. Quantitation o f the target analytes is based on linear regression analysis (weighted 1/x) o f two curves, prepared in methanol, bracketing each group of samples. Quantitation of each analyte is based on the response o f one or more specific daughter ions using the multiple response-monitoring mode o f die instrum ent Page 3 o f6 OOO 3M ENVIRONMENTAL LABORA TORY REPORTNO. FACT-TOX-I30 3M lot #217 (purity 86.9%) o f PFOS was used for calibration standards. As purity information was not available at the time o f data collection, reported results have not been corrected. 5.2 Blanks Two to four extraction blanks, utilizing water as surrogate matrix, were extracted with each batch of samples. Blanks were acceptable if no target analyte was detected above the limit o f detection for a specific analyte. In this study, all blanks were acceptable. 5.3 Surrogates 1,1,2,2-Tetra-hydroperfhrorooctanesulfonate was used as a surrogate in this analysis. Surrogate response was monitored to confirm gross instrumental failure, if necessary. Surrogate response was acceptable for all analyses. 5.4 Matrix Spikes Over the course of the analysis, twenty-eight matrix spikes were prepared in the mallard liver matrix. W ith two exceptions, all matrix spikes showed acceptable recoveries of greater than 50%. O fthe four matrix spikes extracted on 9/27/99, two were recovered outside the acceptable range o f +/-50%. One sample had a PFOS recovery o f 49% and a second sample showed PFOS recovery o f325%. These outlying recoveries were confirmed, but no obvious error was readily identified. An error in spiking the matrix is suspected. Because the remaining 26 matrix spikes were within die acceptable criteria, no further action was taken to explain these two anomalies. Finally, due to a miscalculation early in die data reduction process, eight additional matrix spikes were extracted to confirm what was thought to be b w recovery. Upon discovery o f the calculation error, die original matrix spikes were confirmed to be acceptable and die additional reextractions were not used. Because there was so little mallard sera available, rabbit sera was used as a surrogate matrix in this study. Sixteen matrix spikes were prepared in rabbit sera. All matrix spikes showed acceptable recovery o f 70130%. 5.5 Laboratory Control Samples Laboratory Control Sandies are not a component o f this study. 5.6 Sample Related Comments Samples were not analyzed for any residual or potential metabolite other than PFOS. Other matrices submitted with this study w ill be analyzed as needed upon written request from the sponsor. In die event of further analysis, an additional report w ill be generated. W ith few exceptions, PFOS levels in the sera and livers o f the mallards increased with dose group. Additionally, considering the average PFOS levels within each dose group, both liver and sera levels o fPFOS declined dramatically between day 8 and day 22. Sera levels o f PFOS measured in animals sacrificed on day 22 are between 20-35% o f the sera levels o f PFOS measured on day 8. Levels o f PFOS in the livers of animals sacrificed on day 22 were, on average, 30% lower than those levels determined in the livers o f animals sacrificed on day 8. In most animals, for a specific time point, the ratio o f PFOS concentration in .sera (pg/mL) to PFOS concentration in liver (pg/g) was greater titan 1. Page 4 o f6 3MENVIRONMENTAL LABORATORY REPORT NO. FACT-TOX-liO D ata Quality Objectives andp a id Integrity No circumstances existed during the present study that would have adversely affected the quality or integrity of the data. The following data quality objectives were followed during the study: Linearity - The coefficient of determination (^ 2 ) o f the standard curve was equal to or greater than 0.985 using 1/x weighting. Limits of quantitation - PFOS in sera is 0.005-0.010 pg/mL; PFOS in liver is approximately 0.030 p g / g Acceptable precision o f duplicates - < 20%, determined by MS/MSD analysis Acceptable recoveries o f spikes- 70% to 130% for sera; 50% to 150% for liver Use o f confirmatory methods - Given die selectivity o f die analytical tool used (HPLC-ESMSMS) and lack o f a viable alternative for analysis, no confirmatory methods were used. Demonstration of specificity - Specificity was demonstrated by chromatographic retention time (matched to standards to within 3%) and the response o f at least one characteristic product ion arising from collisions o f an analyte-specific parent ion. The characterization o f the reference material (PFOS, lot #171), with respect to purity, stability, and homogeneity, was not complete on the date this report was issued. Once the characterization is complete, a copy o fthe report will on file in die 3M Environmental Lab archives. Given the parameters listed above, assuming spike recoveries form a suitable indication o f endogenous analyte recovery, and assuming that rabbit sera is a suitable surrogate for mallard sera, sera data are quantitative to +/- 30%; liver data is quantitative to +/- 50%. The validity o f these assumptions has not been verified by other techniques. If more accuracy is required, additional matrix should be supplied so samples can be evaluated versus a standard curve extracted from the same matrix as the samples. Attachm ents i A ttachm ent A: Table of results o f sera analysis A ttachm ent B: Table o f results o f liver analysis A ttachm ent C: In-life protocol A ttachm ent D: Sample receipt A ttachm ent E: Extraction and analytical data PageSof SM ENVIRONMENTAL LABORA TORY REPORT NO. FACr-TOX-130 ;t e a Kris Hansen, PhD ., Principal Analytical Investigator 0 3 / 2 3 /o / Date -- r , . l.Fi.**v, f 23 ---- _ QAU review by Robert V oyksnC T ^^, Y.L. h V **(*-*f i 1 r*7> Pa*p6of6 > Jr ' . * ; 3M ENVIRONMENTAL LABORA TORY REPORT NO. FACT-TOX-! 30 < 0 . /r < - ------- ----------------------------------- 6 / o * / + Kris Hansen, PhD ., Principal Analytical Investigator Date QAU review by R obot Voyksner P6of6 . vj& o ^ ' 000^^3