Document 5kJqe1xYrOv6VbqNNnYbXyOvN

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 .B ox 3331 St. Paul, MN 55133-3331 Phone: (651)778-6018 FAX: (651) 778-6176 Revision Date: March 19, 2001 Page 1of6 CQQ762 SM ENVIRONMENTAL LABORATORY REPORTNO. FACT-TOX-130 1 Introduction *'*:' ' This study was designed to quantitatively assess perfluorooctanesulfonate (PFOS, C8F17S03-, CAS # 279539-3) levels in the sera and liver o fmallard ducks exposed to PFOS through d ie t D etails 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 W ith few exceptions, PFOS levels in toe sera and livers o f toe m allards increased w ith dose group. Additionally, considering the average PFOS levels w ithin each dose group, both liver and sera levels o f PFOS declined dramatically between day 8 and day 22. In m ost animals, for a specific tim e point, toe ratio o f PFOS concentration in sera (pg/m L) 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 O perating Procedures were followed, toe acquisition o f this data was not necessarily collected according to applicable Good Laboratory Practices. D ata presented here is toe 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 W ildlife International Ltd. See attachm ent C for toe 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 f l i i i i Tilines r::. There is no holding time criteria associated w ith these samples for LC/ESMSMS analysis. A nalytical m ethods ETS-8-4.1, Extraction o f Potassium Perfluorooctanesulfonate or O ther Fluorochem ical Compounds from Serum for Analysis Using HPLC-Electrospray/M ass Spectrom etry with thefollow ing exceptions: Due to toe small volume o f m allard sera available, standard curves were prepared in m ethanol instead o f from m allard sera. Available sample volumes were so small, there was not enough sera for m atrix spike studies. As an indicator o f gross error, rabbit serum was used as a surrogate matrix. Sixteen m atrix 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 Fluorochem ical Compounds from Liver for Analysis Using HPLC-Electrospray/M ass Spectrom etry with thefollow ing exception: Pagc2of6 3M ENVIRONMENTAL LABORA TOR Y REPORT NO. FACT-T0X-I3Q Due to the small amount o f m allard liver available, standard curves were prepared in m ethanol instead o f from m allard liver. Twelve m atrix spikes were prepared from die m allard liver. As described in the m ethod, all results are reported in terms o f pg o f analyte per gram of liver (w et weight). PFOS lot 171 was used as reference material. ETS-8-5.1, Analysis o f Potassium PerQuorooctanesulfonate or Other Fluorochemicals in Serum Extracts U sing HPLC-Electrospray/M ass Spectrometry ETS-8-7.0, Analysis o f Potassium PerQuorooctanesulfonate or Other Fluorochemical in Liver Extracts Using HPLC-Electrospray/M ass Spectrometry Sam ple p rep aratio n -H PLC /ESM SM S: ion-pairing extraction A nalyte is extracted from a sample m atrix with ion pairing reagent [tetrabutyl ammonium hydrogen sulfate (TBA)] in a pH -controlled environm ent The cationic reagent selectively targets anionic fluorochem icals. Once the anion-TBA pair is formed, the analyte is transferred into a non-polar organic solvent (m ethyl-tertbutyl ether), dried, and reconstituted in m ethanol for MS analysis. H PLC /ESM SM S In HPLC, an aliquot o f extract is injected and passed through a reverse phase liquid chrom atographic colum n. Based on the affinity o f the analyte for die stationary phase in die column relative to the liquid m obile phase, die analyte is retained for a characteristic amount o f 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 die HPLC system to w ithin 1%. Follow ing HPLC separation, ESMSMS provides a rapid and accurate means for analyzing a w ide 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 m ild temperatures. M olecules are ionized, and a prim ary ion, characteristic o f the analyte, is selected. Ions are accelerated for collision w ith argon gas resulting in fragmentation o f the selected species; subsequent collisions create smaller secondary ionic fragments unique to the prim ary ion, which are detected. For example, for PFOS (C8F 17S 0 3') analysis, ion 499 is selected as the characteristic prim ary ion. T his ion is fragmented into other ions such as 80 amu (corresponding to SOj"), and 230 amu (CjFiSCV). E ach o f these secondary fragments is detected and can be used to differentiate PFOS from other com pounds that m ight have the same characteristic 499 amu prim ary ion, but different chemical com positions and secondary ion fragmentation patterns. 5.1 Calibration For quantitative determinations, a m id-level, calibration curve verification (CCV) standard in m ethanol w as analyzed every 5 to 10 samples to m onitor instrumental d rift Calibration curve verification standards are acceptable if instrumental response is within +/- 30% o f the expected value. In this study, all CCV standards were acceptable. Q uantitation o f the target analytes is based on linear regression analysis (weighted 1/x) o f tw o curves, prepared in methanol, bracketing each group o f samples. Quantitation o f each analyte is based a n the response o f one or more specific daughter ions using the multiple response-monitoring m ode o f the instrum ent Page3of6 C00764 3M ENVIRONMENTAL LABORATORY REPORT NO. FACT-TOX-130 3M lot #217 (purity 86.9% ) o f PFOS w as used for calibration standards. As purity information was not available at the time o f data collection, reported results have not been coirected. 5.2 Blanks Tw o to four extraction blanks, utilizing w ater as surrogate matrix, were extracted w ith each batch o f sam ples. Blanks w ere acceptable if no target analyte w as detected above the lim it o f 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 w as m onitored to confirm gross instrum ental failure, if necessary. Surrogate response was acceptable for all analyses. 5.4 Matrix Spikes O ver the course o f the analysis, tw enty-eight m atrix spikes were prepared in the m allard liver matrix. W ith tw o exceptions, all m atrix spikes show ed acceptable recoveries o f greater than 50%. O f the four matrix spikes extracted on 9/27/99, tw o w ere recovered outside die acceptable range o f +/-50%. One sample had a PFOS recovery o f 49% and a second sam ple showed PFOS recovery o f 325%. These outlying recoveries w ere confirmed, but no obvious error w as readily identified. A n error in spiking the m atrix is suspected. Because the remaining 26 m atrix spikes w ere w ithin the acceptable criteria, no further action was taken to explain these two anom alies. Finally, due to a m iscalculation early in die data reduction process, eight additional matrix spikes w ere extracted to confirm w hat w as thought to be low recovery. Upon discovery o f the calculation error, die original m atrix spikes were confirmed to be acceptable and die additional reextracticms w ere not used. Because there was so little m allard sera available, rabbit sera was used as a surrogate m atrix in this study. Sixteen m atrix spikes w ere prepared in rabbit sera. A ll m atrix spikes showed acceptable recovery o f 70130%. 5.5 Laboratory Control Samples Laboratory Control Samples are not a com ponent o f this study. 5.6 Sample Related Comments Samples w ere not analyzed for any residual or potential metabolite other than PFOS. O ther matrices subm itted w ith this study w ill be analyzed as needed upon w ritten request from the sponsor. In the event o f further analysis, an additional report w ill be generated. W ith few exceptions, PFOS levels in the sera and livets o f die mallards increased w ith dose group. A dditionally, considering the average PFO S levels w ithin each dose group, both liver and sera levels o f PFOS declined dram atically betw een 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 cm day 8. Levels o f PFOS in the livers o f anim als sacrificed on day 22 w ere, on average, 30% lower than those levels determined in the livers o f anim als sacrificed on day 8. In m ost animals, for a specific tim e point, the ratio o f PFOS concentration in sera (pg/tnL) to PFOS concentration in liver (pg/g) w as greater than 1. Page4af6 007^5 3MENVIRONMENTAL LABORATORY REPORTNO. FACT-TOX-130 7 Data Quality Objectives and Data Integrity * * y No circumstances existed during die present study that w ould have adversely affected the quality or integrity o f the data. The following data quality objectives were followed during die study: Linearity - The coefficient o f determination (r*2) o f the standard curve was equal to or greater than 0.985 using 1/x weighting. Lim its o f quantitation - PFOS in sera is 0.005-0.010 pg/mL; PFOS in liver is approxim ately 0.030 pg / 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 U se o f confirmatory methods - G iven the selectivity o f die analytical tool used (HPLC-ESM SM S) and lack o f a viable alternative for analysis, no confirmatory methods were used. D em onstration o f specificity - Specificity was dem onstrated by chromatographic retention tim e (m atched to standards to within 3%) and die response o f at least one characteristic product km arising from collisions o f an analyte-specific parent ion. The characterization o f die reference m aterial (PFOS, lot #171), w ith respect to purity, stability, and hom ogeneity, was not complete on die date this report was issued. Once the characterization is com plete, a copy o f 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 m allard sera, sera data are quantitative to +/- 30%; liver data is quantitative to +/- 50%. The validity o f these assun^ptions has not been verified by other techniques. I f more accuracy is required, additional m atrix should be supplied so samples can be evaluated versus a standard curve extracted from die sam e matrix as the samples. A ttachm ent A: T able o f 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 Page5 of6 Q0Q7GG M ENVIRONMENTAL LABORA TORY REPORTNO. FACT-TOX-/30 K ris Hansen, PhD ., Principal Analytical Investigator QAU review by Robert Voyksner Y .L - h ^ 03/ZZ// D ate Page6 of6 7G7 3M ENVIRONMENTAL LABORA TORY REPORT NO. FACT-TOX-130 K ris Hansen, P hD ., P rincpal Analytical Investigator 0 6 /0 6 /0 -0 D ate QAU review by Robert Voyksner Nl !E n tp n n frv \ 000768 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 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 600769 FACT-TOX-130 Study: Product Number^Test Substance}: Matrix: Method/Revisiofi: Analytical Equipment System N um ber Instrument Software/Version: F il e n am e: R-Squared Vainer Slope: Y-Inlercepfc Dales of Extract}on/Analyst D a ta o f Analysis/Analyst Date o f Data Redaction/Analyse Sam ple D ata MALLARD SERUM Day C reep Dew Sample # Method Blk H 2 0 BDt-l H 2 0 BOc-2 Matrix Blk H 20 Btk-3 H 20 B tk -4 Rabbit Seram Btk-l Rabbit Scrum Bik-2 QC-50ppb-M S l.O ppm -M SD Rabbit Scrum Blk-3 Rabbit Serum BIk-4 RBS06299-MS-I RBS06299-MSD-I RBS06299-MS-2 RBS06299-MSD-2 RBS06299-MS-3 RBS06299-MSIV3 RBS06299-MS-4 Greepi OOmg/kg RBS06299-M5D-4 5938 3939 5940 5941 5942 9195 9196 9197 9198 9199 9200 8401 8402 Greep2 9.l0m f/kgfood 8403 8404 9190 9191 9192 9193 9194 Groups 18.3 m g/kj food 5958 5959 5960 5961 5962 Grop4 36.6 mgfltg food 3961 5969 5970 5971 5972 C reeps 73.2 m f/k | food 5918 5989 5990 Greap6 146 m ^ k f food 5991 5992 5998 5999 6000 9173 9174 Creep? 293 mg/kg food 9180 9181 GreepS 586 mg/kg food 9183 5978 5979 Graap 1171 m ^ k f food 5981 NS Until o r QumitKKia (LOQ) FFOS - 0.003 o g/m l PFOS Dietary LC50 Study with Mallards PFOS Mallard Serum ETS-S-4.1 and ETS-8-5.1 Soup 020199, Amelia 062498 Mass)ynx3.2 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 (u f/a L ) or %Rec <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 23.6 11.45 8.19 13.7 27.3 29.2 17.7 44.3 34.2 37.8 41.6 51.3 57.8 510 63.6 50.6 35.7 81.2 38.6 67.2 58.9 71.2 68.4 94.5 159 NA Average (PrO S)eftaL rK R tt RSD(%) Std. Der.<ug/aL) <LOQ NA 000813 - 1 Outlier 16.4 0.00133 30 Ft* 101% 5% 1.0 ppm 100% 27% <LOQ - 3 Omltaa NA 26.5 7.38 1.96' 49.8 13.8 31.9 30.5 9.75 17.0 48.1 8.19 34.1 33.9 18.8 9.57 6S.I 6.29 *43.4 107 46.5 NA NA PFOS Pcrfiuoraoctancsulfonale Extraction volume ratio equals initial volumeffinai volume. Date Emered/By: 7/06/99,7/07/99,07/14/99 LAC D ue Verified/ By: 08/09/99 GML NA - not applicable NS " no sample analyzed ETS*8-5.I Excel Verston 50/95 TOX-l30-sem-2.xls 3/8/01 000770 FCT-TOX-130 Study: Froduct Numba(Tc>t Subn aa ce): Matrix: MttfaoMUvwoi: Analytical Eqiripmeet S y rian N um ber butrament SoftwamVersioa: Filename: R-Squared Value: Slope: Y-bitercept Daw ofExtraction^Analyst Daw ofAnalysin'Analyst Date ofData Reduction'Analyse Sample Data MALLARD SERUM Day 22 Group Dm Sem ple! Method B& H 20B Ik-l K 20B & 4 M ania BOt K 20B lk-3 K 2 0 Btk-4 Rabbit Scram BIk-l Q c-so * Rabbit Scram BOt-2 Rabbit Seram Blfc-3 Rabbit S c ra n Blk-4 R BS 07079-M S -I RBS0TO79-MSD-1 lOOOppb RBS07079-MS*2 RBS07079-M 5D -2 RBS97C79-MS-1 RBS0707B>MSD~1 RBS07079>MS'2 RBS07079-MSD-2 C raopl 0.0 m p itf feed 649$ 496 6497 491 6499 6300 3929 5930 5931 5932 5933 5934 5935 5936 5937 9.l0m /kg food 9115 9116 9117 CroopJ 15.3 m A f food 9 in 9119 5933 5954 5955 5956 5957 Groopd 36.6 m p ftj food 5963 5964 5965 5966 5967 Gronp$ 7 3 4 w ^ h g food JW J 5954 1955 5956 957 Cronpd 146 m f/lg feed 5993 5994 5995 5996 5997 G roup? 293 n p l q food 9175 9176 9177 9175 9179 G roup! 516 rnf/Vf food 943 5944 Group 1171 ma'Vcfbod 5945 5947 5943 V m t o f Q uanttaaca (LOQ) FTPS ~ 0.010 m /m L FFOS Dietary IC JO Study with Maliardi FFOS Mallard Serum BTS*5-4. 1 and BTS-5-5. 1 Soup 020199 M asslytn 3.2 See Attachment! Sc Attachments See Attachmen ts See Attachments 07/07/99 RWW 07/12/99,07/15/99 DRB/OML 07/13/99,07/16/99 DRB/KJH (P F O S I Reported (of/mL) or% Ree <LOQ <LOQ <LOQ <lo q <LOQ <UX3 <LOQ <LOQ 104% 100% 103% 99% 99% 97% 107% 95% <L0Q <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ <LOQ IO Q <LOQ <LOQ <LOQ <LOQ <LOO 1.05 1.09 2.61 1.04 141 4.40 3.11 4.70 4.92 3.75 4.30 5.53 7.27 7.01 9.69 24J iao 6.52 7.23 1.43 124 11.9 164 24.0 MM 104 1.43 la i 164 21.5 29.7 154 39.4 51.6 254 A rarsfa (FFO S)t|/m L arSR ec RSD<%) Std. Dcv^uf'm L) <LOQ LOQ 101% 100% NA NA 2% 6% <LOQ 1.49 442 6.52 114 15.9 13.4 34.0 U NA NA 474 0.704 12.0 01520 29.1 149 66.1 7.49 42.0 7.94 414 541 454 15.4 NA f M - NrA ucrim Lauifcnato* Dale Emaed'By: Dale Verified/By: 07/14/99.07/16/99.07/20*9 LAC 06/09/99 GML *Grp 9 tentative value, evaporated to drynms. Bam crioa volume redo equate bridal vofcnm/Baal volume. BTS4-5.I Excd Vtnkm S.0/9S TOX-l30*era-2jUa 3/1/01 c 00771 SMENVIRONMENTAL LABORATORY REPORTNO. FACT-TOX-HO 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 c r* 0772 Study: Product NumberfTest Substance): M atrix: FA C T-TO X -130 PFOS D ietary LC50 Study with Mallards PFOS M allatd liv e r MALLARD LIVER DAY 4-7 G roup Dose M ethod Blk Sam ple tt M LL09279-H2O BBc-11 MLL09279-H2O BDc-12 PFOS C alc. Cone. 8/8 0.00 0.00 C oncentraloii orPFO S ng/g o r % Ree. <LOQ <LOQ QC - 50ppb** M LL09279-9196-0-M S-11 31.1 56% Q C - l.Oppm** MLLQ9279-9196-0-MSD-V1 M LL09279-9199-0-M S-12 MLL09279-9199-0-M SD-12 182 677 536 325% 61% 49% G roup 7 2!>J mg/kg food 9182, Day7 148106 148 G roups 586 mg/kg food 5980, D ty5 5982, Day 5946, Day7 216457 196822 179996 216 197 180 G ronp9 1171 mg/kg food 5976. Day4 5949, Day4 115890 122122 116 122 5952, Day5 5950, Day5 5974, D iy5 5951. Day5 5973, Day6 172280 137062 146732 185296 131286 172 137 147 185 131 5948, Day 5975, Day7 120973 177851 121 178 PFOS - Perfluorooctanesulfonate Lim it o f Q uantitation (LOQ) PFOS: approx. O.OJOug/g NA - not applicable " T h e MS/MSD and group 1 samples were ro*xuacted on 10/08/99 to confirm m atrix effects. LAC 10/08/99 M ean PFOS ng/g o r % Rec. <LOQ 191% 55% 198 198 145 R SD (% ) Sid. Dev.(ug/g) MS/MSD RPD NA 141% 23% 70.7 9.23 18.2 18.3 26.6 FACT-M-2.1 Excel Version 5/95 T O X -130-liver-2.xls 3/8/01 10:44 AM 000773 Product NumbeiCTcst Substance): M atrix: F A C T -T O X -130 PFOS Dietary LC50 Study with Mallards PFOS M allard Liver MALLARD LIVER DAY 8 Dose S am ples M ethod B lit Q C -lO O ppb 1.0 ppm lOOppb 1.0 ppm 0.0 mg/kg food G roup2 9.10 mg/kg food 18.3 mg/kg food G raup4 36.6 mg/kg food G roap5 73.2 mg/kg food G roop6 146 mg/kg food G ronp7 293 mg/kg food G roups 586 mg/lcg food H 20 BIk-I H 20 Blk-2 H 20B IV -3 H 20 BIk-4 MLL06299-59384M4S-1 MLL06299-593WV-MSD-I M IX06299-594O4-M S-2 M U.06299-5940-0-MSD-2 MLL06299-9196-0-MS-3 M LL06299-9196-0-M SD-3 MLL06299-8401-O.MS-4 M LL06299-8401-0-M SD -4 5938 5939 5940 5941 5942 9195 9196 9197 9198 9199 9200 8401 8402 8403 8404 9190 9191 9192 9193 9194 5958 5959 5960 5961 5962 5968 5969 5970 5971 5972 59B8 5989 5990 5991 5992 5998 5999 6000 9173 9174 9180 9181 9183 9184* 5979 5981 NS Limit o f Quantitation (LOQ) PFOS: approx. 0.030ug/g NA - not applicable NS - no sam ple analyzed * One outlier, not included in any calculations p ro s 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 C oncentration ofp r o s ng/g o r % Ree. <LOQ <LOQ <LOQ <LOO 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 M ean p ro s ug/g o r % Ree. <LOQ lOOppb 73% 1.0 ppm 74% 4.67 6.65 153 29.7 38.8 - 55.6 59.5 NA R SD (% ) S id . D cv^vf/f) 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 T 0X -130-liver-2.xls 3/8/01 10:44 AM 000774 Product NumberfTest Substance): M atrix: F A C T -T O X -130 PFOS Dietary LC50 Study with M allardl PFOS M allard Liver MALLARD LIVER DAY 22 Dose Sample # M ethod Blk Q C -lO O ppb 1.0 ppm G roupl 0.0 mg/kg food G ronpZ 9.10 mg/lcg food G roup3 18.3 mg/kg food G rop4 36.6 mg/kg food G ranpS 73.2 mg/kg food C reeps 146 mg/kg food G rnnp7 293 mg/kg food G roups 586 mg/kg food H 20 Blk-1 H 20 BDt-2 H 20 BDc-3 m O B Ik-4 6495-O-MS-l 6495-0-M SD -l 64964LMS-2 649641-MSD-2 6497-0-MS-3 6497-0-MSD-3 6498-0-MS-4 6498-0-MSD-4 6495 6496 9497 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 5983 S984 5985 5986 5987 5994 5995 5996 5997 9175 9176 9177 9178 9179 5943 5944 5945 5947 PFOS - Pcrflunrooctm em lrotate Lim it o f Quantilation (LOQ) PFOS: approx. 0.030ug/g NA - not applicable PFOS C ate. Codc. ng/g 1.72 1.09 1.07 1.51 107 101 111 126 1033 mi 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 C oncentration o f PFOS ug/g o r 54 Rcc. <LOQ <LOQ <LOQ <LOO 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 J.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 M enu RSD (% ) PFOS S td. D ev.(ug/g) ug/g o r % Rcc. M S/M SD RPD <LOQ NA <LOQ NA 94% 9% 90% 3% <LOQ 1.03 2.04 3J6 9.21 127 9.20 20.2 NA NA NA 31.4 0222 20.3 0.413 40.0 1.35 13.9 1.28 38.1 4.85 34.8 320 38.8 7.82 NA FACT-M-2.1 Excel Version 5/95 T0 X-I30-liver-Zxls 3/8/01 10:44 AM coo r