Document ev0j9NjzOqygjDN1G1D3Rn17q

BACK TO MAIN Laboratory R eport-Revision 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 1 of6 BACK TO MAIN 3MENVIRONMENTAL LABORATORY REPORT NO. FACT-TOX-130 1 Introduction . . This study was designed to quantitatively assess perfluorooctanesulfonate (PFOS, C8F17S03-, CAS # 2795 39-3) levels in the 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 (Wildlife 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 of 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 f this data was not necessarily collected according to applicable Good Laboratory Practices. Data presented here is die 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 o f Wildlife International Ltd. See attachment C for die in-life protocol. 2 Sample Receipt pA-'*>n".*%vn i i n gfM| 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 fiver, 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. 3 Holding Times There is no holding time criteria associated with these samples for LC/ESMSMS analysis. 4 : Methods - Analyticdiand Preparatory,,, ' Analytical methods ETS-8-4.1, Extraction o f Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds from Serum for Analysis Using HPLC-Electrospray/Mass Spectrometry with thefollowing exceptions: Due to die small volume o f mallard sera available, standard curves were prepared in methanol instead o f from mallard sera. Available sample volumes were so small, 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 f Potassium Perfluorooctanesulfonate or Other Fluorochemical Compounds from Liver for Analysis Using HPLC-Electrospray/Mass Spectrometry with thefollowing exception: Page2of6 BACK TO MAIN 3M 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 of Potassium Perfluorooctanesulfonate or Other Fluorochemical in Liver Extracts Using HPLC-Electrospray/Mass Spectrometry Sam ple preparation -HPLC/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-ierfbutyl 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 of the analyte for 1he stationary phase in die column relative to die 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 die 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 primarily 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 (CgFnSOs") 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 (C3F6S 0 3'). Each of 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 Analysis Viti ^ . .V.r \ 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% of the 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 o f each analyte is based on the response o f one or more specific daughter ions using the multiple response-monitoring mode o f the instrument. Page3of6 BACK TO MAIN M ENVIRONMENTAL LABORATORY REPORTNO. FACT-TOX-liO 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 of detection for a specific analyte. In this study, all blanks were acceptable. 5.3 Surrogates 1,1,2,2-Tetra-hydroperfluorooctanesulfonate 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 o f the analysis, twenty-eight matrix spikes were prepared in the mallard liver matrix With two exceptions, all matrix spikes showed acceptable recoveries of greater than 50%. O f die four matrix spikes extracted on 9/27/99, two were recovered outside die acceptable range of +/-50%. One sample had a PFOS recoveiy o f 49% and a second sample showed PFOS recovery o f 325%. These oudying 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 low recoveiy. Upon discovery o f the calculation error, the original matrix spikes were confirmed to be acceptable and die additional re extractions were not used. Because there was so litde 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 70 130%. ' 5.5 Laboratory Control Samples Laboratory Control Samples 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. O ther matrices submitted with this study will be analyzed as needed upon written request from the sponsor. In die event of further analysis, an additional report will be generated. 6 Data 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 of PFOS 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 die fivers of animals sacrificed on day 22 were, on average, 30% lower than those levels determined in the fivers o f animals sacrificed on day 8. In m ost animals, for a specific time point, the ratio o f PFOS concentration in sera (pg/mL) to PFOS concentration in liver (|ig/g) was greater than 1. Page4of6 BACK TO MAIN 3M ENVIRONMENTAL LABORATORY REPORT NO. FACT-TOX-I30 7 Data Quality Objectives and Data Integrity No circumstances existed during the present study that would have adversely affected the quality or integrity o f the data. The following data quality objectives were followed during the study: Linearity - The coefficient of determination (r*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 |ig / 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 the selectivity o f die analytical tool used (HPLC-ESMSMS) and lack o f a viable alternative for analysis, no confirmatory methods were used. Demonstration o f 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 of the report will on file in the 3M Environmental Lab archives. Given die 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. 8 Attachments Attachment A: Table o f results of sera analysis Attachment B: Table of results o f liver analysis Attachment C: In-life protocol Attachment D: Sample receipt Attachment E: Extraction and analytical data Page5of6 BACK TO MAIN 3M ENVIRONMENTAL LABORA TORY REPORT NO. FACT-TOX-IO Sig n a tu res ' 1 . ..; v v'fetfcr.;;-. , V V,_-; Mark Ellefeon, Technologist /v h ^ -- ---------- Kris Hansen, PhD ., Principal Analytical Investigator .... QAU review by Robert Voyksner _ ... . Y.L- z> 3,6> s / & / Date O SfZZlO l Date *3 Page 6 o f6 9 Signatures BACK TO MAIN 3MENVIRONMENTAL LABORATORY REPORT NO. FACT-TOX-130 X4 - --------------- Kris Hansen, PhJD., Principal Analytical Investigator & /06/& -0 Date QAU review by Robert Voyksner W s^ x r 5 . Pagati ef6 ^ 0 ^ ' ' BACK TO MAIN 3MENVIRONMENTAL LABORATORY REPORT NO. 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 9tm 1 rsf5 fcf F A C T -T O X -130 Study: Product NumbcrfTcst Substance): Matrix: M c th od/R e vision; Analytical Equipment System Num ber Instrument Softwarc/Vetsion: Filename: R-Squared Value: Slope: Y-Intercept: Dates of Extraction/Analyst: Dates o f Analysis/Analyst Date o f Data Reduction/Analyst: Sample Data PFOS Dietary LC50 Study with Mallards PFOS Mallard Serum ETS-8-4.1 and ETS-8-5.1 Soup 020199, Amelia 062498 Masslynx 3.2 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 MALLARD SERUM Pay 8 Group Dose Sample 4 |PFO S| R eported (ug/mL) or %Rec Average | PFO S Jug/mL or %Rec RSD(%) Std. Dev.(ug/mL) Method Bile Matrix Blk QC - 50 ppb" MS 1.0 ppm - MSD H 2 0 Blk-1 H 20 Blk-2 H 2 0 Blk-3 H 20 Blk-4 Rabbit Serum Blk-1 Rabbit Serum Blk-2 Rabbit Serum Blk-3 Rabbit Serum Blk-4 RBS06299-MS-1 RBS06299-MSD-1 RBS06299-MS-2 RBS06299-MSD-2 RBS06299-MS-3 RBS06299-MSD-3 RBS06299-MS-4 RBS06299-MSD-4 <LOQ <LOQ <LOQ <LOQ 0.00742 <LOQ 0.00730 0.00967 107% 74% 103% 78% 96% 126% 99% 119% <LOQ NA 0.00813 - 1 Outlier 16.4 0.00133 SOppb 101% 5% l.Oppan 100% 27% G ro u p 1 0.0 mg/leg 5938 5939 5940 5941 5942 9195 9196 9197 9198 9199 9200 8401 8402 8403 8404 <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 0.0103 0.00686 <LOQ <LOQ <LOQ 0.00674 <LOQ 0.00819 0.0230 <LOQ - 5 Outliers NA Gronp2 9.10 mg/kg food 9190 9191 9192 9193 9194 8.81 7.68 8.79 4.04 26.5 7.60 7.38 1.96 Group3 18.3 mg/kg food 5958 5959 5960 5961 5962 9.31 25.6 11.45 8.89 13.7 49.8 13.8 6.86 Gronp4 36.6 mg/kg food 3968 5969 27.3 29.2 5970 5971 5972 17.7 44.3 31.9 34.2 30.5 9.75 Group5 73.2 mg/kg food Group6 146 mg/Vg food 5988 5989 5990 5991 5992 5998 5999 6000 9173 9174 37.8 41.6 51.3 57.8 52.0 63.6 50.6 35.7 81.2 38.6 . 48.1 53.9 17.0 8.19 34.8 18.8 Group7 293 mg/kg food Group8 586 mg/kg food 9180 9181 9183 5978 5979 5981 67.2 58.9 9.57 . 71.2 65.8 6.29 68.4 94.5 . 43.4 159 107 46.5 Group 9 1171 mg/kg food NS NA NA NA Limit of Quantitation (LOQ) PFOS - 0.005 ug/mL PFOS - Periluorooctanesulfonate Extraction volume ratio equals initial volume/final volume. Date Entered/By: Date Verified/By: 7/06/99, 7/07/99, 07/14/99 LAC 08/09/99 GML NA - not applicable NS - no sample analyzed BACK TO MAIN ETS-8-5.1 Excel Version 5.0/95 TOX-130-sera-2.xls 3/8/01 FA CT-TO X -130 BACK TO MAIN Study: Product NumbcifTcst Substance): Matrix: Mcthod/Revis ion: Analytical Equipment System Number: Instrument Software/Vcrsion: Filename: R-Squared Value: Slope: Y-lntereept: Dates of Extraction/Analyst Dates of Analysis/Analyst: Date of Data Reduction/Analyst Sample Data PFOS Dietary LC50 Study with Mallards PFOS Mallard Serum ETS-8-4.1 and ETS-8-5.1 Soup 020199 Masslynx 3.2 See Attachments See Attachments See 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 Group Sample # Dose Method BUc M atrix BDc QC - 50 ppb lOOOppb Groopl 0.0mg/kg food Group2 9.10 mg/kg food GroapJ 18.3 mg/kg food Group4 36.6 mg/kg food H20 Blk-l H 20 Blk-2 H20 Blk-3 H20 Blk-4 Rabbit Scrum Blk-l Rabbit Scram Blk-2 Rabbit Scram Blk-3 Rabbit Seram Blk-4 RBS07079-MS-1 RBS07079-MSD-1 RBS07079-MS-2 RBS07079-MSD-2 RBSQW79-MS-1 RBS07079-MSD-1 RBS07079-MS-2 RBS07079-MSD-2 6495 6496 6497 6498 6499 6500 5929 5930 5931 5932 5933 5934 5935 5936 5937 9185 9186 9187 9188 9189 5953 5954 5955 5956 5957 5963 5964 5965 5966 5967 {PFOS1 Reported (ug/mL) or %Rec <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 104% 100% 103% 99% 99% 97% 107% 95% <LOQ <LOQ <LOQ <LOQ <L0Q <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 1.05 1.09 2.68 1.04 1.58 4.40 3.81 4.70 4.92 3.75 4.30 5.83 7.27 7.01 9.69 Average (PFOSJog/mL or %Rec RSD(%) Std. Dev.(ug/mL) <LOQ NA <L0Q 101% 100% NA 2% 6% <LOQ 1.49 4.32 6.82 NA NA 47.3 0.704 12.0 0.520 29.1 1.99 Group5 5983 24.5 73.2 mg/kg food 5984 10.0 I& 8985 6.52 8986 7.23 66.1 Gronp6 8987 5993 8.43 11.3 7.49 12.2 146 mg/kg food 5994 11.9 5995 16.2 5996 5997 24.0 42.0 30.1 18.9 7.94 Group? 9175 10.3 293 mg/kg food 9176 9177 8.43 10.1 9178 16.5 41.2 9179 21.5 13.4 5.51 Groups 5943 29.7 586 mg/kg food 5944 15.2 5945 39.4 45.3 5947 51.6 34.0 15.4 ` *Group9 5943 25.5 NA N A 1171 mg/kg food Lindt of Quantitaboo (LOQ) PFOS * 0.010 ug/mL PFOS - Periluorooctanesulfonate NA not applicable *Grp 9 tentative value, evaporated to dryness. Date Entered/By: 07/14/99,07/16/99, 07/20/99 LAC Extraction volume ratio equals initial volume/final volume. Date Verified/ By: 08/09/99 GML ETS-8-5.1 Excel Version 5.095 TOX-130-sera-2-xls 3/8/01 BACK TO 3M ENVIRONMENTAL LABORA TOR Y REPORTNO. FACT-TOX-130 L aboratory R eport 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 Number(Test Substance): Matrix: FACT-TOX-130 PFOS Dietary LC50 Study with Mallards PFOS Mallard Liver BACK TO MAIN MALLARD LIVER DAY 4-7 Group Dose Method Blk QC - 50 ppb** QC -1.0 ppm** Group 7 293 mg/kg food Group8 586 mg/kg food Group9 1171 mg/kg food Sample # MLL09279-H20 Blk-11 MLL09279-H2O Blk-12 MLL09279-9196-0-MS-11 MLL09279-9196-O-MSD-11 MLL09279-9199-0-MS-12 MLL09279-9199-O-MSD-12 9182, Day7 5980, Day5 5982, Day6 5946, Day7 5976, Day4 5949, Day4 PFOS Calc. Cone, ng/g 0.00 0.00 31.1 182 677 536 148106 216457 196822 179996 115890 122122 Concentralon of PFOS ug/g or % Ree. <LOQ <LOQ 56% 325% 61% 49% 148 216 197 180 116 122 5952, Day5 5950, Day5 5974, Day5 172280 137062 146732 172 137 147 5951, Day5 5973, Day6 5948, Day6 5975, Day7 185296 131286 120973 177851 185 131 121 178 PFOS Periluorooctanesulfonate Limit of 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 or % Ree. <LOQ 191% 55% 198 198 145 RSD (%) Std. Dev.(ug/g) MS/MSD RPD NA 141% 23% 70.7 9.23 18.2 18.3 26.6 fa FACT-M-2.1 Excel Version 5/95 TOX-130-liver-2.xls 3/8/01 10:44 AM Study: Product NumbeifTest Substance): Matrix: FACT-TOX-130 PFOS Dietary LC50 Study with Mallards PFOS Mallard Liver BACK TO MAIN MALLARD LIVER DAY 8 Group Dose Sample # Method Blk H 20 Blk-1 H 20 Blk-2 H20 Blk-3 QC - 100 ppb H20 BIk-4 MLL06299-5938-0-MS-1 MLL06299-5938-0-MSD-1 1.0 ppm MLL06299-5940-0-MS-2 100 ppb MLL06299-5940-0-MSD-2 MLL06299-9196-0-MS-3 MLL06299-9196-0-MSD-3 1.0 ppm MLL06299-8401-0-MS-4 MLL06299-8401-0-MSD-4 Groupl 5938 0.0 mg/kg food 5939 5940 5941 5942 9195 9196 9197 9198 9199 9200 8401 8402 8403 8404 Group2 9190 9.10 mg/kg food 9191 9192 9193 9194 Group3 5958 18.3 mg/kg food 5959 5960 5961 5962 ' Group4 36.6 mg/kg food 5968 5969 5970 5971 5972 GroupS 5988 73.2 mg/kg food 5989 5990 5991 5992 Group6 5998 146 mg/kg food 5999 6000 9173 9174 Group7 9180 293 mg/kg food 9181 9183 9184* Group8 5978 586 mg/kg food 5979 5981 Group9-U71 mg/kg food NS PFOS " Perfluorooctanesulfonate Limit of Quantitation (LOQ) PFOS: approx. 0.030ug/g NA = not applicable NS = no sample analyzed * One outlier, not included in any calculations PFOS Calc. Cone. ng/g 0.00 0.00 0.00 0.00 88.0 89.4 802 799 84.4 73.3 915 894 0.00 0.00 0.00 0.00 0.00 0.00 92.8 0.00 0.00 132 0.00 0.00 0.00 0.00 0.00 6828 3714 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 75542 70474 NA Concentration of PFOS ug/g or % Ree. <LOQ <LOQ <LOQ <LOQ 74% 75% 73% 72% 76% 66% 76% 75% <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ 0.0928 <LOQ <LOQ 0.132 <LOQ <LOQ <LOQ <LOQ <LOQ 6.83 3.71 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 15.3 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 75.5 70.5 NA ' Mean PFOS ng/g or % Rec. <LOQ 100 ppb 73% 1.0 ppm 74% <LOQ - 2 Outliers 4.67 ' 6.65 15.3 29.7 38.8 ' 55.6 #* 59.5 NA RSD (/.) Std. Dev.fug/e) MS/MSD RPD NA 5% 2% NA NA 32.1 1.50 43.7 2.90 24.8 3.78 49.8 14.78 28.1 10.9 8.29 4.61 39.6 23.5 NA FACT-M-2.1 Excel Version 5/95 TOX-130-liver-2.xls 3/8/01 10:44 AM Study: Product Number(Test Substance): Matrix: FACT-TOX-130 PFOS Dietary LC50 Study with Mallards PFOS Mallard Liver BACK TO MAIN MALLARD LIVER DAY 22 Group Dose Sample # Method Blk H20 Blk-1 H20 Blk-2 QC -100 ppb H20 Blk-3 H20 Blk-4 6495-0-MS-l 6495-O-MSD-l 6496-0-MS-2 1.0 ppm 6496-0-MSD-2 6497-0-MS-3 6497-0-MSD-3 6498-0-MS-4 6498J3-MSM Groupl 0.0 mg/kg food 6495 6496 9497 6498 6499 6500 5929 5930 5931 5932 5933 5934 5935 5936 5937 Groap2 9.10 mg/lcg food 9185 9186 9187 9188 9189 Gronp3 18.3 mg/kg food 5953 5954 5955 5956 5957 Groap4 36.6 mg/kg food 5963 5964 5965 5966 Gronp5 73.2 mg/kg food 5967 5983 5984 5985 5986 5987 Groap6 146 mg/kg food 5993 5994 5995 5996 Group7 293 mg/kg food 5997 9175 9176 9177 9178 9179 Group8 586 mg/kg food 5943 5944 5945 Group9>l 171 mg/kg food 5947 5977 PFOS - Periluorooctanesulfonate - Limit of Quantitation (LOQ) PFOS: approx. 0.030ug/g NA =*not applicable PFOS Calc. Cone. ng/g 1.72 1.09 1.07 1.51 107 101 111 126 1033 1111 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 Concentration of PFOS ug/g or % 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 0.876 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. Dev.iuu/e) ug/g or % 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-130-liver-2.xls 3/8/01 10:44 AM