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WAAZLCMCN 3301 KINSMAN BLVD. LQX3WUURIeS IANTERICA. INC. . Chemical& BioMedicaSlciencesDivision P.O.BOX 7645 MADISON, WISCONSIN 53707 PHONE (608)241-4471 TLX 703956HAZAAL Mi,),UsD FINAL REPORT JANINE GLEASON MINNESOTA MINING & MANUFACTURING TOXICOLOGY SERVICES ST. PAUL, MN 55101 COMPANY T-3752 PURCHASE ORDER NUMBER: T357842, REL. 4513 L4 s NUMBER: SAMPLE ENTERED: REPORT PRINTED: 50503499 05/15/85 02/12/85 ENCLOSED: ACUTE ORAL TOXICITY CAU REPORT RAW DATA APPENDIX - METHOD, SUMMARY, PATHOLOGY SIGNED: STEVEN M. GLAZA STUDY DIRECTOR ACUTE TOXICOLOGY DATE BY AND FOR HAZLETON LABORATORIES AMERICA, INC. RAW DATA FOR THIS STUDY ARE KEPT ON FILE AT HAZLETON .AMERICA, INC., MADISON, WISCONSIN. LABORATORIES IWIFHIAAZILC%CN LAEK3RMr3Rir=S ATAERICA. IN= Chemical& BioMedicaSlciencesDivision 3301KINSMAN BLVD. a P.O.soX 7545 , #AADISON,WISCONSIN 53707 - PHONE (608)241-4471- TLX 703956HAZRAL MDS UD SAMPLE NUMBER: 50503499 T-3752 PAGE 2 OECD ORAL SCREEN Obiective: To determine the acute oral toxicity produced when a test material is administered bv oral gavaae to rat5 according to the Organi5ation of Economic C@operation ;nd Development'5 Guidelines for Testina Chemicals, Section 401, Acute Oral Toxicity, adopted May 12, 1981. Test Material: T-3752 Phvsical Description: Brown St@bilit%j of Test Material: granular solid Sponsor has purity and stability determinations on file. Test Animal: Youna adult male and female albino rats of the SpragueDawleV strain we;e procured, maintained in group cages in temperatureand humidity-controlled quarters, provided continuous access to Purina Rodent Chow and water, and held for an acclimation period of at least 7 days. Acclimated animals were chosen at random for the study. Test animals were housed bV 5eX in groups of five and identified by animal number and correspon@ina ear tao. Food and water were available ad libitum throughout the siudy, except for an overnight per'iod just before test material administration when food, but not water, was withheld. Reason for Species Selection: The rat is the animal classically used due to its small 5ize., ready availability, and 16roe amount of background data. ,Method: Five male and five female rats weighing between 195 and 234 g were used for each dosage level. The study consisted of three dosage levels (0.20, 2iO and 5.0 g/ka). Preparation and Administration of Test Material: For each dose level, the appropriate amount of test material was mixed with corn oil and heated and stirred on a stir plate to a uniform suspension. The suspension Wa5 cooled to room temperature prior to dosina. An individual dose was calculated for each animal based upon its fasted body weight and administered by gavage. The d05e Volume Wa5 15.0 tnl/kg of body weight. Observations: The animals were observed for clinical signs and mortality at lp 2.5 and 4 hours followina test material administration. The animals were observed dailv th;reafter for 14 days for clinical sions and twice dailvI for mortalltvI. All animals were weiched just before test material administration: at 7 days and at study termination or at death. Patholoa,j:@ At 5tUdkJ termination surviving animals were euthanatized. Animai-s which died durino the study or were euthanatized received a aross necroos%j examinaiion and all abnormalities were recorded. ')HAZLOZON L&BOR4=MIES APAE-RICA, INC. Chemical& BloMedicalSciencesDivision 3301 KINSMAN BLVD. o P.O.BOX 7645 * MADISON, WISCONSIN 53707 9 PHONE (608)241-4471 TLX 70!."ilH)A5Z6RAL MDS UD SAMPLE NUMBER: 50503499 T-3752 PAGE 3 OECD ORAL SCREEN SUMMARY (CONTINUED) Test Animal: Albino Rat5 - Sprague-Dawley strain Source: Harlan Sprague-Dawley, Madison Wl Date Animals Received: 05/22/85 Temperature and Humidity of Animal Room: 19 to 24 Decrees C.; 42 to 60% Relative Humidity Vehicle: Corn-oil Method of Administration: Oral Gavaae Date Test Started: 05/30/85 Date Test Completed: 06/20/85 Estimated Oral LD50*: Male - Between 0.20,and 2.0 a/kg of body weight Female - Between 0.20 and 2.0 9/kg of body weicht Mortality Summary (Number of Deaths) Dorzaae Levef (g/ka) 0.20 2.00 5.00 Hours Days 0-4 1 2 3 4 5 6 m F* M F M F M F M F M F M F 0 0 00 0 0 0 0 00 a0 00 0 0 4 5 1 - - - -0 0 45 1 7-14 MF 0 .0 Total m F Both 0/5 0/5 0/10 5/5 5/5 10/10 5/5 10/10 Dosage Level (g/kg) Male 0.20 2.00 5.00 Female 0.20 2.00 5.00 Averaae initial 224 212 196 201 215 211 Body Weights (a) Day 7 Terminal 263 --- --- 294 --- --- 209 ----- 219 ----- HAZLMMON L"Bcxqx%3miAte4EBMIrA. INC. Chemical& B[oMedicaSlciencesDivision 3301KINSMAN BLVD. 0 p.o.BOX 7545 - MADISON, WISCONSIN 63707 PHONE (608)241-4471o TLX 703956HAZRAL MDS UD SAMPLE NUMBER: 50503499 T-3752 PAGE 4 OECD ORAL SCREEN (CONTINUED) Clinical Sions Hours Dav5 1.0 2.5 4.0 . 1 2 3 4 5 6 89 Dosaae Level - 0.20 9/kg Males Appeared normal 4 3 2 0 0 0 455 55 5 HQooactivitQ 0 0 2 555 00 000 0 D i1 @rrhea 1 2 2 5 10 a00 00 a Yellow-stained abdomen a 0 0 442 0 0 00 0 0 Red-stained face 0 0 0 551 000 0aa Famale.t Appeared normal 4 3 4 000455 555 Hy poactivity 0 0 a 3550 0000 0 Diarrhea 1 2 1 400 00000 0 Yellow-stained abdomen 0 0 0 033 10 0 0 0 0 Red-stained face 0 0 0 22 00 00000 10 11 12 5 55 00 0 0 00 00 0 00a 555 000 00 0 00 0 00a 13 14 55 00 00 00 00 55 00 00 00 00 Do5aan Level - 2.00 g/kg Appeared normal '5 1 0 Diarrhea 0 1 1 Hvpoactivity 0 4 5 R;d-stained face 0 0 0 Yellow-stained anal area Ataxia Bradvpnea Death 0 0 0 0 0 0 0 0 0 0 0 0 Appeared normal 5 3 0 Hypoactivity 0 2 5 Diarrhea 0 1 4 Red-stained face 0 0 0 Prostration 0 a 0 BradtiDnea 0 0 0 Red-5tained anal area 0 0 0 Death 0 0 0 Males 0 0 ------- - - - - 0 0 ------- - - - - 1 a ------- - - - - 1 0 ------- - - - - - 1 0 ------- - - - - 1 0 ------- - - - - 1 0 ------- - - - - 4 1 ------- - - - - - Female5 0 -------- - - - - 1 -- -- -- -- - - - - 0 -------- - - - - 1 -------- - - - - 1 -------- - - - - 1 -- -- -- -- - - - - - 1 -------- - - - - 5 -------- - - - - - HAZLOMON LAEOMP.4OX3RIr=S At.IERIC.A.INC. Chemical& BioMedicaSlciencesDivision 3301KINSMAN BLVD. o P.O.BOX 7545o MADISON,WISCONSIN 53707o PHONE (60&2t41-447e1 TLX703956HAZRAL MDS UD SAMPLE T-3752 NUMBER: 50503499 PAGE 5 OECD ORAL SCREEN (CONTINUED) Clinical Sions (continued) Hours 1.0 2.5 4.0 Dav5 12 3 4 5 6 8 9 10 11 12 13 14 Dosaae Level - 5.00 g/kg Males Appeared normal 5 4 0 0 0 -- ----- - - - - - Diarrhea 0 1 1 1 0 - - - - -- - - - - - - Hypoactivity 0 0 4 1 0 - - -- - - - - - - - - Red-stained face 0 0 0 1 0 - ----- - - - - - - Dark-stained uroaenital area 0 0 0 1 0 - -- - - - - - - - - - - Death 0 0 0 4 1 - - -- - - - - - - - -- Females Appeared normal 3 3 0 0 -- ----- - - - - - - Diarrhea 2 2 2 0 -- ----- - - - - - - Hvooactivitv 0 0 5 0 - - - -- - - - - - - - - D;@th 0 0 0 5 --- ----- - - - - - HAZLC%ON Lai"z.=CX:IiEB AKAERICA. INC. 3301 @,'INSMANBLVD. 0 P.O.BOX 7645 * MADISON, WISCONSIN 53707 Chemical& B!oMedicalSciencesDivision PHONE (6082)41-4471o TLX 703956 HAZRAL MDS UD SAMPLE NUMBER: 50503499 T-3752 PAGE 6 OECD ORAL SCREEN Dosage Level: Animal Number Sex C34524 m C34518 m C34504 m C34510 m C34509 m C34465 F C34499 F C34466 F C34464 F C34473 F (CONTINUED) PATHOLOGY 0.20 g/kg of body weight Date Dosed: 06/06/85 Test Day Died Sacrificed - 14 - 14 - 14 Necrop5y Comments No visible lesions. No visible lesions. No visible lesions. - 14 - 14 - 14 - 14 - 14 - 14 No visible No visible No visible No visible No visible No visible lesions. lesions. lesions. lesions. lesions. lesions. - 14 Liver - hepatic anomaly at junction of median lobes, 8 x 5 mm, liver-like. HAZLETON LABCX*Aa'CRIES AAAERICA, lt'JC. Chemical& BlaMedicalSciencesDivision 3301 KINSMAN BLVD. o P.O.BOX 7545 9 MADISON, WISCONSIN 537(-,-"PHONE (608)241-4471a TLX 703956HAZRAL MDS UD SAMPLE NUMBER: 50503499 T-3752 PAGE 7 OECD ORAL SCREEN Doseae Level: Animal Number Sex C34483 m C34480 m C34481 m C34477 m C34512 m C34493 F C34463 F C34485 F C34469 F C34492 F (CONTINUED) PATHOLOGY (continued) 2.00 g/kg of body weight Date Dosed: 06/04/85 Test Day Died Sacrificed Necropsy Comments 1 Red parinasal discharge; dark red, bilateral periocular discharge; parineum - moist, 5tained clear -Yellow, 1 Red perinasal discharge; perineum - moist, I stained clear yellow; eye - white intraocular material. 1 Red perinasal discharge; dark red, bilateral periocular discharge; perineum - 5tained clear yellow. 1 Red perina5al discharge; perineum - moist, stained clear yellow; 2 Red perina5al dischaurge; perineum - moist with clear fl id; bilateral red ocular discharge; jejunum and ileum - contain dark brown m'aterial. 1 - I - 1 - 1 - 1 - Perineum 5tained yellow; small intestine contains tan to yellow mucoid material. Perineum stained yellow; small intestine contains tan to yellow mucoid material. Perineum - stained yellow; jejunum contains dark brown mucoid material. Perinsum stained yellow.; small intestine contains tan to.yellow mucoid material. Perineum 5tained yellow; small intestine contains tan to -,@ellow muccid material. IFIH"ALZLOZON LAeK3FUUZX41ES ANERICA. INC. Chemical& B!oMedicaSlciencesDivision 3301 KINSMAN BLVD. 0 P.O.BOX 7645 o MADISON, WISCONSIN 53707 9 PHONE (608)241-4471o TLX 703956HAZRAL MDS UD SAMPLE NUMBER: 50503499 T-3752 PAGE a OECD ORAL SCREEN Dosaae Level: Animal Number Sex C34505 m C34479 m C34513 m C34503 m C34507 m C34500 F C34495 F C34484 F C34498 F C34467 F (CONTINUED) PATHOLOGY (continued) 5.00 g/kg of body weight Date Dosed: 05/29/85 Test Day Died Sacrificed 3 2 2 2 - 2 - 2 - 2 - 2 - Necropsy Comments Stomach - contains dark brown semisolid material. No visible lesions. Stomach - contains dark brown semisolid material. Stomach-- multiple areas on glandular 2 x 3 mm. dark brown mucose, up to No visible lesions. No visible lesions. No visible lesions. Upper thoracic cavity contains dark red, clotted material. 2 - 2 - No visible lesions. No visible- lesions. Deviation from the protocol: During the studv period the temperature of the animal room ranoed from 19 to 24 dearee; C. This deviation is not considered to have @ad an effect on the-validity of the study. References: Orcanisation for Economic Cooperation and DevelODment's Guidelines fo; Testing of Chemicals., Section 401, Acute Ora'l Toxicity... adopted May 12, 1981. QUALITY ASSURANCE STATEMENT Acute Oral Toxicity Study in Rats Study No. 50503499 The report as herein attached for the above-mentioned study has been reviewed by the assigned Quality Assurance Unit of Hazleton-Laboratories America, Inc. It has been found to accurately identify and/or describe the authorized methods and standard operating procedures followed in the conduct of the study. Purthermore,*the Quality Assurance Unit has conducted the following inspections of the testing facilities utilized in the conduct of this study and has submitted written reports of said inspections to the study director and/or.management. Date of Inspection 5/21-23/85 7/12/85 Type of Inspection Process Audit Report Review Date Issued to Management 5/23/85 7/12/85 Diana E. Skalitzky Inspector, Quality Assurance Unit Date 'feetMaterial Wk Density T-3,7Q!s AIR (9/121) 0 ACUTE ORAL TOXICITY (LD50 ) RECORD Vehl 1 -CQIZO oli-- RT SPOclOs Famteds D#te Source UgLr leh to-S-15 Ti.@@'- Date Bece -c&. I-IM(- Ro Done Volume /kit) Dose Tim 1 0&0) Sax Anisai -No./Bar Tag W.r-s qSaq qSD I Iq 10 qqla q Tecia, a Fasted Body Welailt (g) Actual Dose (al Day 7 Bo y weight (a) DEaPya4 14 5-odyWeight (a) 557 Ioq2 )7 ao o 3. -3.5-3-4 13.-6 3.3 Q9.1 see ftr_i led bv Dosage 0. 30 (R/ka) Dose Volume )il,O-(Ml/k&) AnAPVAinl0,cRir8a0tmm,o'auaet*lateeVladostN0"IDeo4W.o/got T!@g N-p. 4 Dose qqqi__lq4(d, q4la4_ q475 q@ 44'71 4,4A99 Tects. ow & Pretanted Body Weigist Fasted Body Weigi(lRt) Actual Done .20 -oo 3,o 3.0 Z.15 3.C, 3.0 Day 7 BodY WeiRlit (R) 14 a Day 14 Body WeiRlit (g) ZZO 211 210 Z13 Z-365 VA gas V rifi&'d hv Done liours 04 a QA 144 Ti Date ills "A - not Applicable MORTALITY (NO. DIED/NO. DOSZD) 1 2 3 4 5 6 7 8 no n Ikostnot modmintatered Reviewed - 9 10-- 11 no C'16 D C) 0 fiex Test Material -T--2j'75Q ACUTE ORAL TOXICITY (LD ) RECORD 50 Vehicle Wk Density 6!A (g/mi) Species Pastedt Dpte Source Time 3.'00 Date Tech. f-IZ d-C) a) Dose-Vol~ tsounlikg) Animl No.IVAr T&R no a qqch'3 q Protasted 5-ody V -- Fasted Body Weialit (g) 00 Actual Does (mi 3.0 5, X (it)- Day I l@od Weight (g) "Itro 'I a DMCI Dav 14 body Weight 6Mf- Dose Tim 3.0 -3.a PgA Li.5'1. .,rf@ 977 a.,@1.2 Tech. 1 fy9 3.a '1.'5 U&IIP 1 9 111 ck 0.5-154ii;@, 3A DoW@ Ve-ritted byl RT Becel Roo tqf5 Date Doan" (g/kg) Dose VolunO 15-D (mliks) Animal LO./gar Tag Pretasted Body WelList Fasted bodl Weight it) .70 ArActual Done pi 3.1 pre D"Dacaa't 7 Body Weight (g) - Day Day 14 Body Weight (a) 11%9 - :205' 20& ;21 3.1 13.1 it.oo Teel%. Dot 3.;l sto man VaKLLLed-hil IV9 16, MORTALITY (NO. DILPD/NO. DOSED) Dogia Level liours 04 2- -3 4 sit 6 7 8 10 11 ?.0 --. c2.L) Technician [4 Li Date NA - Not.Applicable 6 st----- -olo-sinto,ble-ernot administered Reviewed by ACUTE ORAL TOXICITY 4LO50 RECORD Test material-T- Vehicle eof-fd -oil- RT Bulk Density @J 19 48/al) species source.--%kaelon - Date Recol C) Dosage Done Volume ISO 4t Fastedi DiptoS-;M-SS Time -3:le_WTeck. -i*M Roo -Dose Time 1-1 C&L. Tech. ai Sax Animal Roo/Eat TaR 44-11 40-1"5 4523 1;at Pretasied Body Weight (&I lAq - --- FB8tC4 body WSLRI%T (g) 11 195 q Actual Done 401 Day 7 Body Weight (g) Day 14-Pody Welaht 13.0 1 ati 1 F,6CLa a -i-IScf ipi wwn L@-j/-I /,0.751915 '753 C1*65 pass@ Ve-ri Dosage' S.0 (g/kkit) (alC/5kg) Done Volume 15,o (al/kg) Animal.-Ho./zar T-a m 5 qsoo dql,q4i5 q q so 4 4495 Teel&. PretastedBody W*ILIit(g) A Y- Fasted body Weigist(R) Actual Dogto Day 7 Body WeiRlit (R) 12C)b .3.% -S-3- 3-aL 3.4 pt-,-UT-ia7- Pit cr '3,5 Day 14 Body Welatit(a) giab 1945 lqq!5 a))@ Verifiedhvl- is. MORTALITY (00. 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"BACK LAVBL LO ,J,A almbPvAT 7349? 730 @l 1/3 AIPIPEARRWOUL lo llii2 13 r\ V7 yii 'Yia '-1/3 OATE ti $Ian reason& al sign rwaselit, atiobt Not swident MA not Applicable HAZLF;'C(ONLABORATORIES 3301 KINSMAN BLVD. P.O. BOX 7545 AMERICA, INC. MADISON, Wl 53707 (608)241-4471 TLX 703956 H.AZ.RA.L,,MDSUD PROTOCOL TP2069 Acute Oral Toxicity Study in Rats (OECD Guidelines) Study No. 50503499 for 3M St. Paul, Minnesota by Hazleton Laboratories America, Life Sciences Division 3301 Kinsman Boulevard Madison, Wisconsin 53704 Inc. May 21, 1985 1985, Hazleton Laboratories America, Inc. Chemical & BioMedical Sciences Division PROTOCOL TP2069 Acute Oral Toxicity Study in Rats (OECD Guidelines) Study No.: Study Location: Test Material: Sponsor's Representative: Study Director: Proposed Timetable Starting Date: Completion Date: Final Report Date: 50503499 Hazleton Laboratories America, Life Sciences Division 3301 Kinsman Boulevard Madison, Wisconsin' 53704 Inc. T-3752 Janine Gleason Steven M. Glaza Week Week Week of May 27, 1985 of June 17, 1985 of July 15, 1985 OBJECTIVES To determine the acute oral toxicity produced when the test material is administered by the oral route (gavage) to rats. All aspects of this study will conform to the Organisation for Economic Cooperation and Development's Guidelines for Testing of Chemicals, Section 401, adopted May 1 12, 1981 and 2 Principles of Good Laboratory Practice. All procedures will be done according to Hazleton Laboratories America, Inc. (HLA) Standard Operating Procedures (SOPS) referenced in th.isprotocol. Test Material: Physical Description: Purity and Stability: Storage Conditions: Test Material Retention: Safety Precautions: TEST MATERIAL T-3752. Brown granular solid. Sponsor has purity and stability determinations on file. Store at room temperature. Any unused test material will be returned to the Sponsor 30 days after issuance of the final report. Laboratory personnel will take the normal necessary precautions in handling a substance of unknown toxicity. Laboratory clothing, latex gloves, safety glasses, and a particle mask approved for toxic dusts must be worn. 2 TEST SYSTEM Animal Model Young adult male and female albino rats (approximately 7 weeks of age) of the Sprague-Dawley strain will be obtainea-@rom Harlan Sprague-Dawley, Madison, Wisconsin. Rats will be selected at random from healthy.animals that had been acclimated at HLA for at least 1 week. An adequate.number of extras will be purchased in order that no animal in obviously poor health is placed on test. The weight variation in animals used on test will not exceed +20% of ,the mean weight (i.e., mean - 250 g, range 200 to 300 g). Reason for Species Selection The rat is the animal classically used due to its small size, ready availability, and large amount of background.data. Identification Each animal will be assigned an individual animal number and ear tag which will accompany data collected from that animal throughout the study (OP-GENB 24). Housing_ and Maintenance The following environmental conditions will be maintained in the animal room used for this study (OP-TARC 230). 0 Temperature: 22*C +20 Relative humidity: 50% +20% Air change: At least 107changes an hour of filtered 100% outside air Light cycle: 12 hours light/12 hours dark Temperature and humidity will be monitored throughout the study. Variations from prescribed environmental conditions will be documented. 3 Animal husbandry and housing at HLA comply with standards outlined in the 3 "Guide for the Care and Use of Laboratory Animals." Care will be taken to ensure that the animals are not disturbed for reasons other than data collection and routine maintenance. The animals will be individually housed in screert-bottomstainless steel cages held on racks, with absorbent pan liners in the urine- and feces-collecting pans. Pan liners will be changed at least three times each week. Feed and water will be provided ad libitum. The diet will be Purina Rat Chow"0. No contaminants are expected to be present in the feed or water which would interfere and affect the results of the study. PROCEDURES Experimental Design Initially, a single dose of 5.0 g/kg will be administered to 10 animals (five males and five females). If no test material-related mortality is produced at this level, no further testing is required. If any mortality occurs at the 5.0-g/kg dose level, at the Sponsor's request, three or four geometrically spaced dose levels may be added. Each dose level will consist of 10 animals (five males and five females). Animals will be assigned to groups according to HLA Standard Operating Procedure OP-TOX 42. Test Material Preparation and Administration The test material will be suspended in an appropriate vehicle. Individual dosages will be calculated based upon the animal's body weight taken just before administration of the test material and administered by gavage. 4 Justification of Route of Administration This is the method for administering a known quantity of test substance and has been the route of choice historically. Observations The animals will be observed individually for clinical signs and mortality at 1.0, 2.5, and 4 hours after test material administration. The animals will be observed daily thereafter for at least 14 days for clinical signs and twice daily (morning and afternoon) for mortality. The duration of observations may be extended when considered necessary. The time of death will be recorded as precisely as possible. Individual body weights will be recorded just prior to study initiation and at 7 and 14 days following test material.administration and at death. Changes in body weight will be calculated and recorded when survival exceeds 1 day. Pathology All test animals, whetber dying during the study or sacrificed at' termination, will be subjected to a gross necropsy examination and abnormalities recorded. Report The final report will contain a description of the test material, a' -description of how the study was conducted, response data for clinical signs, mortality and body weights by sex, a discussion of the data, and gross pathology findings. 5 Maintenance of Raw Data and Records Original data or copies thereofwill be available at HLA to facilitate auditing the study during its progress and prior to acceptance of the final report. When the final report is completed,all original paper data, as well as the final report, will be retained in the archives of HLA, Madison, Wisconsin (OP-GEN 44). REFERENCES 1. Organisation for Economic Cooperation and Development's Guidelines for Testing of Chemicals, Section 401, Acute Oral Toxicity, adopted May 21, 1981. 2. Organisation for Economic Cooperation and Development's Principles for Good Laboratory Practive, Annex 2, 1981. 3. DHEW Publications No. (NIH) 78-23 (1978). 6 PROTOCOL APPROVAL o./IIt) a innseeorG.llseeason J@a nlnsorts Representative 3M jr-laq-1@!cj- Date Steven M. Glaza 0 Study Director Group Leader, Acute Toxicology Hazleton Laboratories America, Inc. (1107S/tji) Date