Document zQXzQLzraLDVmbOo1mGV5Gp67
Corporate Health Physics Corporate Industrial Hygiene & Ergonomics Corporate Occupational Medicine Corporate Toxicology 3M Medical Department
3M Center, Building 220-2E-02 PO Box 33220 ' St. Paul, MN 55133-3220 651 733 1110
A R X L G 'O l O
3M May 3, 2000
Facsimile
Dr. Jennifer Seed 202-260-1279 USEPA Headquarters Ariel Rios Building 1200 Pennsylvania Avenue, N. W. Washington, DC 20460
Re: Serum measurements for Argus Studies 418-013 (through lactation) and 418-015 (during gesatation)
Dear Jennifer:
I am including in this fax the two sets of serum perfluorooctanesulfonate measurements from the following two studies:
1. Oral (Gavage) Pharmacokinetic Recovery Study of PFOS in Rats, Argus Laboratories Protocol No. 418-015, 3M Reference No. T-6295.14, AdvancedBioanalyticalServices Study No. FACT-TOX-111.
2. Oral (Gavage) Pharmacokinetic Study of PFOS in Rats, Argus Laboratories Protocol No. 418-013, 3M Reference No. T-6295.12, Advanced Bioanalytical Services Study No. FACT-TOX-110.
The informnation which I have included relates to the analytical studies indicated above in bold italics. Included are pages 10-19 of FACT-TOX-111 and pages 13-23 of FACT-TOX-110. 3M has previously sent the in-life reports and protocols for the analytical phase to the attention of Dr. Hernandez.
I would be happy to meet with you and your EPA colleagues and consultants to provide whatever assistance you may desire in understanding the toxicological information that is being provided.
Please contact me with any questions or if you would like to arrange a meeting.
Sincerely,
John L. Butenhoff, Ph.D., CIH, DABT Senior Laboratory Manager Corporate Toxicology (651)733-1962
004008
MAY. 3 . 2 0 0 0 1 1 :5 7 A M ENVIRONMENTAL LAB 2 3E 09
NO. 1 9 2 6 P. 2
Table 2:
Inter-Assay Precision and Accuracy for PFOS Quality Control Samples in Rat Serum for Study #FACT-TOX-lll
PFOS Concentration (ua/mL)
Run No.
QCl
QC2 QC3
QC4
QC4
0.2 6 18
100
100
Cl in 10 Dilution) (1 in 20 Dilution)
1 0.232 6.17 18.2
NA
NA
0.212 6.28 18.4
NA
NA
0.210
6.11
18.2
NA
NA
0.216 5.97 18.2
NA
NA
2 0.216 6.00 18.1
NA
NA
0.227 6.09 19.0
NA
NA
0224 6.07 19.8
NA
NA
0.219 6.18 18.5
NA
NA
3 0.211 5.97 18.8
116
NA
0.210 5.84 18.2
114
NA
0.217 6.07 18.8
113
NA
0.214 5.99 17.9
106
NA
4
0.222
6.48
19.3
NA
112
0.233 6.23 19.7
NA
109
0.214 6.54 19.6
NA
117
0.225 6.30 18.5
NA
113
Mean
0.219
6.14
18.7
112
113
RSD (%) RE
3.43 9.39
3.08 3.28 2.38 3.86
3.61 12.3
2.78 12.7
RSD = (SD/N[ean)x 100%
RE = [(Mean-Nommal)/Nominal] x 100%
NA: Not applicable.
ADVANCED
BIOANALYTCAL SE R V IC E S. INC.
Page 10 of 19
99ADJA03.MI.DOC
004009
BIOANALYTICAL SE R V IC E S, INC,
Table 3:
Inter-Assay Precision and Accuracy for PFOS Calibration Standards in R at Serum for Study # F A C T -T O X -lll
Rim No. STD1 0.05
STD2 0.1
STD3 0.25
1 0.0496 0.0993 0.238 0.0513 0.101 0.243
2 0.0470 0.101 0.244 0.0538 0.101 0.244
3 0.0490 0.105 0.254 0.0511 0.0980 0.242
4 0.0522 0.0950 0.246 0.0491 0.104 0.246
Mean 0.0504 RSD(%) 4.24
RE 0.775
0.100 3.04 0.425
0.245 1.80 -2.16
RSD = (SD/Mean) x 100%
RE = [(Mean-Nomiiial)/Nominal] x 100%
PFOS Concentration QifjftnL)
STD4 STD5 STD6 STD7
0.5 1 2 4
0.493 0.957
2.13
4.39
0.491 0.963
2.12
438
0.542 0.899 2.03
430
0.539 0.928 2.03
4.43
0.482 0.980
2.15
4.49
0.487 0.937
2.01
439
0.484 0.953
2.11
4.47
0.481 0.958 2.13
4.50
0.500 0.947 2.09
4.42
5.08 2.66 2.67 1.52
-0.0325 -531 4.49 10.5
STD8 8
7,72 7.76 7.67 7.77 7.80 739 7.59 7.89 7.70 1.98 -3.76
STD9 16 16.0 15.5 16.0 15.8 16.9 15.8 15.9 15.3 15.9 2.98
-0.651
STD10 20 20.4 20.0 20.6 19.8 20.4 19.2 20.6 20.0 20.1 2.34
0.626
ENVIRONMENTAL LAB 2 3E 09
O"i
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_ 0 0 4 0 3 .0
Page U o f 19
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MAY, 3. 2 0 0 0 1 1 :5 7 A M ENVIRONMENTAL LAB 2 3E 09
NO. 1 9 2 6 P, 4
Table 4: Calibration Curve Statistics for the Determination of PFOS in Rat Serum for Study #FACT-T0X-1U
Run No. Quadratic
Linear
Coefficient (A) Coefficient (B)
1 -0.0004154 2 -0.0005419 3 -0.0006070 4 -0.0002665
Mean -0.0004577 y = Ax2+ Bx + C, weighted lY
V'
0.1025 0.1001 0.1046 0.1036
0.1027
Intercept (C)
-0.0006090 -0.0004172 -0.0001313 -0.0004533 -0.0004027
Coefficient of Determination
fr2) 0.9977 0.9959 0.9968 0.9966
0.9968
ADVANCED BIOANALYTICAL SE R V IC E S. INC.
Page 12 of 19
99ADJA03.M1:DOC
004011
ENVIRONMENTAL LAB 2 3E 09
Table S: Concentrations of PFOS in R at Serum Samples from Study tiFACT-TOX-111 Following the 0 mg/kg Dose
Sampling Time
___ (day)
0 7 14 15 21 22
PFOS Concentration (pg/mL)
Rat Number*
13726 13726P 13727
13727P
13728
13728P
13731
13734
/
0.215 NS 0.121
NS
0.0930
'N S
0.0842
0.118
0.176 NS 0.0835
NS
0.0711
NS
0.0873
0.0644
0.0822 NS 0.0638
NS
0.0530
NS NS 0.0594
0.168 NS 0.0932
NS
0.0605
NS
0.0610
0.0665
0.0849 0.0712 0.0587 <LLQiO,Q452]<(0.05) <LLQ[0.0385]<(0.05) <LLQ[0.0343]<(0.05) NS <LLQ[0.0390]<(0.05)
0.0597 NS 0.0517
NS <LLQ[0.043 L]<(0.05) NS
NS <LLQ[0.0446]<(0.05)
*Rat Number with a "P" indicates pup sample. <LLQ - Less than the Lower Limit o f Quantitation (0.05 pg/mL). NS: No sample.
' NO. 1 9 2 6
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P
Page 13 of 19
99ADJA03.MI.DOC
1:58AM ENVIRONMENTAL LAB 2 3E 09
m
UMD> rn n O
SB
Table 5:
Sampling Time (day)
(Continued) Concentrations o f PFOS In R at Serum Samples from Study #FACT-TOX-ll 1 Following tbe 0 rag/kg Dose
13734P
L3735
PFOS Concentration (jig/mL)
Rat Number*
I3735P
13736
13736P
13737 13737P
0 NS
0.0947
NS
0.113
NS 0.0877 NS
7 NS
0.0700
NS
0.108
NS 0.0767 NS
14
NS <LLQ[0.Q492]<(0.05)
NS
<LLQ[0.0474]<(0.05)
NS
0.0553 NS
15 NS
0.0574
NS
0.0693
NS 0.111 NS
21 <LLQ[0.0409]<(0.05)<LLQ0-0418J<(0.05) <LLQ[0.0401]<(0.05) <LLQ[0.0491]<(0.05) <LLQ[0.0409]<(0.05) 0.0531 0.0518
22 NS <LLQ[0.0370]<(0.05) NS
0.0592
NS 0.0570 NS
*Rat Number with a "P" indicates pup sample. <LLQ= Less than the Lower Limit o f Quantitation (0.05 ng/mL). NS: No sample.
NO. 1 9 2 6
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Page 14 o f 19
99ADJA03.MI-DOC
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i- Table 6: Concentrations of PFOS In R at Seram Samples from Study #FA CT-TO X -lll Following the 0.1 mg/kg Dose
Sampling Time (day) 13739 13739P
0 9.78 NS 7 9.50 NS 14 1.82 NS 15 5.88 NS 21 1.81 2.34 22 1.33 NS
13740
12.1 7.85 1.99 7.83 4.00 1.47
PFOS Concentration (pg/mL) Rat Number*
13740P 13741 13741P 13744 13744P
NS 11.6 NS 9.88 NS NS 7.59 NS 9.18 NS NS 1.51 NS 1.96 NS NS 6.67 NS 6.04 NS 2.12 2.69 1.88 3.04 2.29 NS 1.19 NS 0.882 NS
13745
/ 9.88 7.40 2.55 5.80 2.34 1.09
13745P 13746
NS 11.1 NS 8.49 NS 2.03 NS 6.65 1.88 2.84 NS 0.945
13746P
NS NS NS NS 2.37 NS
*Rat Number with a "P" indicates pup sample. NS: No sample.
ENVIRONMENTAL LAB 2 3E 09
CJ
CSC
NO, 1 9 2 6
C04Q14
Page 15 o f 19
99ADJAQ3.MIDOC
--1
Table 6:
(Continued) Concentrations of PFOS in R at Serum Samples from Study #FACT-TOX-l11 Following the 0.1 mg/kg Dose
Sampling
PFOS Concentration (jig/mL)
Time
Rat Number*
H
(day)
13748 13748P
13749 13749P
0 10.2 NS
7 NS NS
14 1.35 NS
15 536 NS
21 3.94 1.74
22
0.942
NS
10.7 NS 8.61 NS 1.87 NS 8.40 NS 3.27 2.07 1.22 NS
RatNumber with a "P" indicates pup sample. NS: No sample.
ENVIRONMENTAL LAB 2 3E 09
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NO, 1 9 2 6
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Page ]$ o f 19
99ADJA03.MI.DCX:
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Table 7: Concentrations o f PFOS in R at Serum Samples from Study tfFACT-TOX-111 Following the L6 mg/kg Dose
Sampling Time (day) 13751
0 155 7 149 14 21.2 15 95.6 21 38.5 22 17.1
1375IP
NS NS NS NS 35.0 NS
13752 13752P
164 NS 169 NS 24.1 NS 109 NS 34.8 33.9 19.5 NS
PFOS Concentration (itg/mL) Rat Number*
13753 13753P 13754 13754P
213 NS 198 NS 157 NS 152 NS 21.6 NS 21.2 NS 112 NS 103 NS 32.6 28.3 37.1 23.4 18.2 NS 9.48 NS
13755 /
191 138 NS 125 112 NS
13756 13756P
188 NS 158 NS 31.0 NS 108 NS 40.4 47.4 19.9 NS
13758
188 143 27.7 86.9 37.0 14.3
*Rat Numberwith a "P" indicates pup sample. NS: No sample.
ENVIRONMENTAL LAB 2 3E 09
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NO. 1 9 2 6
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Page 17 o f 19
99ADJA03MI.DOC
(A ID >
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Table 7:
(Continued) Concentrations of PFOS in R at Sernm Samples from Study #FA CT-TO X -lll Following the 1.6 mg/kg Dose
Sampling Time
(day)
PFOS Concentration (jigftnL)
Rat Number*
13758P
13759
13759P
0 NS 7 NS 14 NS IS NS 21 25.6 22 NS
198 133 20.4 99.4 33.0 15.4
NS' NS NS NS 26.3 NS
*Rat Number with a "P* indicates pup sample. NS: No sample.
O O
Page 18 o f 19
99ADJA03.MI.DOC
?=
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<n >Pg
mm --iD
Table 8: Repeat Analysis o f R at Serum Samples from Study #FACT-TOX-l 11
Rat Treatment Time Number
Original Cone.
Mg/mi
Original Curve Number
13753
3 DayO >ULQ-222.9138>(200)
3
Reason for
Reassay
1
Reassay Cerne. MR/ml
/
213
Reassay Curve Number
4
Repealed Cone. Ufi/ml
213
Reason for Reported
Cone.
1
>ULQ: Greater than die Upper Limit o f Quantitation. REASONS FOR REASSAY: 1). Run 3 concentration exceeded calibration range. REASONS FOR REPORTED CONC: 1). Run 4 concentration within calibration range.
<-T*i O?C
ENVIRONMENTAL LAB 2 3E 09
NO. 1 9 2 6
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Page 19 o f 19
99ADJA<B-MIJDOC
MAY. 3. 2 0 0 0 1 0 : 5 4 A M ENVIRONMENTAL LAB 2 3E 09
Table S: Concentrations o f PFOS in R at Serum Samples from Study #FACT-TOX-110 Following the 0 mg/kg Dose
(0 03> m nD
<z|
ni n
-(1"fi H
90
a?
Sampling Time (day) 19501 19502 19503
19504
PFOS Concentration (pg/mL)
Rat Number*
19504F
19505
19505F 19506 19506F
19507
0 0.112 0.0701 0.0607
0.0514
NS
0.0550
NS 0.309 NS
0.0545
7 0.397 0.0535 NS
0.0926
NS
0.0514
NS 0.219 NS
0.0586
15 0.0803 0.0690 NS <LLQ[0.0432]<(0.05) NS
0.0609
NS 0.199 NS
0.0648
21 NS NS NS <LLQ[0.0258]<(0.05) 0.0845 <LLQ[0.0353]<(0.05) 0.0880 0.0820 0.267 <LLQp).0247]<(0.05)
<LLQ = Less than the Lower Limit o f Quantitation (0.05 pg/mL). *Rat Number with "F" indicates fetal sample, NS: No sample.
Oo
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o Page 13 o f 24
99ADJA02.MIDOC
p
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MAY. 3 . 2 0 0 0 1 0 : 5 4 A M ENVIRONMENTAL LAB 2 3E 09
ADVANCED BiOANALYTICAL
SE R V IC E S. INC.
I Table 5:
(Continued) Concentrations of PFOS in Rat Serum Samples from Study 4FACT-TOX-1 10 Following the 0 mg/kg Dose
Sampling Time
PFOS Concentration (pg/mL) Rat Number*
(day) 19507F
19508
19509
19509F 19510 19511
19512
19512F
0 NS
0.0548
<LLQ[0.0483]<(0.05) NS 0.0664 0.0619 <LLQ[0.0449]<(0.05) NS
7 NS <LLQ[0.0395]<(0.05) <LLQ[0.Q481J<(0.05) NS 0.0636 0 2 5 0 0.197
NS
15 NS <LLQ[0.0454]<(0.05) <LLQ[0.0458]<(0.05) NS 0.0614 0.176
0.238
NS
21 0.0842
NS
<LLQ[0.0269]<(0.05) 0.102 NS NS
0.0833
0.219
<LLQ - Less than the Lower Limit of Quantitation (0.05 jig/mL). *Rat Number with "F" indicates fetal sample. NS: No sample.
NO. 1 9 2 4
004020
Page 14 o f24
99ADJA02.MI.DOC
BOANALYTICAL SE R V IC E S, INC.
00402
Page 15 o f 24
99ADJA02.MI.DOC
MAY. 3. 2 0 0 0 1 0 : 5 4 A M ENVIRONMENTAL LAB 2 3E 09
NO. 1 9 2 4
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99ADJA02i4I.DOC c n
Page 16 o f2 4 .
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Page 17 o f 24
99ADJA02.MT.DOC
MAY, 3 . 2 0 0 0 1 0 : 5 4 A M ENVIRONMENTAL LAB 2 3E 09
Table 7: Concentrations of PFOS In R at Serum Samples from Study #FACT-TOX-l 10 Following the 0.4 mg/kg Dose
_________________________ PFOS Concentration (ng/mL) _______________________
Sampling Time _________________________ ______ Rat Number*________________________________
____ (fry)
19533 19533F 19534 19534F 19535 19536 19536F 19537 19538 19539 19540 19541
0 53.9 NS 46.9 NS 50.1 38.6 NS 56.6 46.5 45.2 42.9 44.4 7 44.3 NS 50.0 NS 56.6 36.6 NS 58.4 48.1 44.6 45.8 NS 15 47.3 NS 56.1 NS 48.2 43.3 NS 50.7 53.5 37.2 48.6 NS 21 20.4 42.5 20.5 41.4 NS 16.2 3 2 3 NS NS NS NS NS
*Rat Number with "F* indicates fetal sample. NS: No sample.
NO. 1 9 2 4
FageltoTM
99ADM02.MI.DOC
MAY. 3. 2 0 0 0 1 0 : 5 5 A M ENVIRONMENTAL LAB 2 3E 0 9
inai
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Table 7:
(Continued) Concentrations of PFOS in R at Seram Samples from Study #FACT-TOX-l 10 Following the 0.4 mg/kg Hose
PFOS Concentration (pg/mL)
Sampling Time
Rat Number*
19542 19543 19543F 19544 19545 19546 19546F 19547 19548
0 453 46.3 NS 45.8 47.9 43.5 NS 42.2 57.6 7 40.6 46.1 NS 42.8 NS 46.5 NS 42.2 60.0 15 44.0 43.9 NS 49.1 NS 47.3 NS 43.3 58.0 21 NS 23.0 34.1 NS NS 35.8 48.4 NS 65.7 '
*Rat Number with "F" indicates fetal sample. NS: No sample.
NO. 1 9 2 4
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Page 19 of 24
99ADJA02.MIDOC
cn
BIOANALYTICAL SE R V IC E S, INC,
Table 8: Concentrations of PFOS In R at Serum Samples from Study #FACT-TOX-l10 Following the 1.6 mg/kg Dose
Sampling Time
(day)
19549 19550
19551
PFOS Concentration (pg/mL) Rat Number
19552 19553 19554 19555 19556 19557 19558 19559 19560
0 166 200 184 165 182 203 166 199 198 196 171 200
7 NS 216 NS NS 160 189 195 186 NS 171 160 171
IS NS 160 NS NS 135 176 225 202 NS 164 192 215
21
NS NS
NS NS NS NS NS 251 NS NS 237 79.4
NS: No sample.
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ENVIRONMENTAL LAB 2 3E 09
NO. 1 9 2 4
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Page 20 of24
99AOJA02.MLDOC
MAY. 3 . 2 0 0 0 1 0 : 5 5 A M ENVIRONMENTAL LAB 2 3E 0 9
0) OJ> in
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me
n
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--iD
Table 8:
(Continued) Concentrations of PFOS in R at Serum Samples from Study #FACT-TOX-ll 0 Following the 1.6 mg/kg Dose
Sampling Time
(day)
19560F
19561
PFOS Concentration (pgfaiL) Rat Number*
19562 19562F 19563
0
NS 193
185
NS
163
7
NS 181
179
NS
168
15
NS 219
142
NS
183
21 131 NS 63.7 102 NS
19564
185 169 159 NS
*Rat Number with "F" indicates fetal sample. NS: No sample.
NO. 1 9 2 4
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Page 2] o f 24 .
99ADJA02.MJ.DOC
CT3
MAY. 3. 2 0 0 0 10 : 5 5 A M ENVIRONMENTAL LAB 2 3E 0 9
Table 9: Concentrations of PFOS in R at Seram Samples from Study #FACT-TOX-l10 Following the 3.2 mg/kg Dose
Sampling Time
(day) 19565 19566
19567
PFOS Concentration (pg/mL) Rat Number* .
19568 I9568F 19569 19569F 19570 19571 19571F L9572 19572F
0 370 337 366 339 NS 334 NS 351 348 NS 357 NS 7 392 280 327 340 NS 323 NS 337 371 NS 305 NS
15 345 311 294 336 NS 314 NS 269 308 NS 317 NS 21 NS NS NS 241 228 142 176 NS 165 166 123 166
*Ral Number with "F" indicates fetal sample. NS: No sample.
NO. 1 9 2 4
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99ADJA02-MI-DOC
MAY. 3. 2 0 0 0 1 0 : 5 5 A M ENVIRONMENTAL LAB 2 3E 0 9
Table 9:
(Continued) Concentrations of PFOS in R at Serum Samples from Study #FACT-TOX-110 Following tbe 3 J mg/kg Dose
Sampling Time (day) 19573
0 364 7 343 15 317 21 NS
19574
365 393 299 NS
19575
413 387 284 NS
PFOS Concentration (y.R/mL) Rat Number*
19576 19577 19577F 19578
19579
19579F
19580
383 417 NS 395 NS 361 NS 221
NS 373 387 NS 378 NS NS 399 NS 357 NS NS 386 NS 323 226 NS 186 181 NS
*Rat Number with T indicates fetal sample. NS: No sample.
NO. 1 9 2 4
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99ADJA02.MLD0C
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