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Corning H2ZIetonInc. P.O.Box 7545 \IadisonW,i 53707-7545 D, lii,erie3s3:01 Kipis?ptBalnvd. Madison,Wl S3704 608.241.4471 608.241.7227F2X Sponsor: 3M St.Paul,Minnesota FINAL REPORT CORNING Hazleton F90 V WR 3 0 W7 StudyTitle: 5-DailyDose DermalAbsorption/ToxiciSttyudyofT-6564inRabbits Author: F.Bud W. McDonald Study CompletionDate: April28,1997 Performin-Laboratory: Coming HazletonInc. 3-'10Kinsman Boulevard Madison,Wisconsin 53704 LaboratoryProjectIdentification: CHW 6329-185 Page I of50 Corning PharmaceuticalServices QUALITY ASSURANCE STATEM:ENT CHW6329-185 This report has been reviewed by the Quality Assurance Unit of Coming Hazleton Inc.,in accordance with theFood and Drug Administration(FDA) Good Laboratory Practice Standards,21 CFR 58. The followinginspectionswere conducted and findingsreported to the Study Directorand management. Written statusreportsof inspectionsand findings are issuedto Coming Hazleton management according to standardoperatingprocedures. InspectionDates From To 09/30/96 12/02/96 01/03/97 01/1')/97 09/30/96 12/02/96 0 1/0'1/97 01/14/97 Phase ProtocolReview Sample Handling ProtocolAmendment Data/Report Review Date Reported to Studv Directo 10/01/96 12/02/96 01/0'>/97 01/14/97 Date Reported to Manacement 10/01/96 12/02/96 01/0')/97 01/14/97 Representative,QualityAssurance Unit 2 Date STUDY EDENTI[FICATION CHW 6329-195 5-DailyDose DermalAbsorption/ToxiciSttyudy ofT-6564 inRabbits TestMaterial T-6564 Sponsor 3M ToxicologyService MedicalDepartment 3M Center,Bldg.@20-2-E-02 P.O.Box 33220 St.Paul,MN 551'3')-3220 Sponsor'sRepresentative Roger G. Perkins,PhD, DABT 3M ToxicologyService MedicalDepartment 3M Center,Bldg.220-2E-02 P.O.Box 33220 St.Paul,MN 55133-3220 (612)73'1--'1222 StudyDirector Study Location Study Timetable Study InitiatiDoante Experimental(In-lifSet)artDate In-lifEend Date ExperimentalTerminationDate StudyCompletion Date F.Bud W. McDonald Coming HazletonInc. P.O.Box 7545 Madison,Wl 5')707-7545 (608)242-7901 Coming HazletonInc. 3301 Kinsman Boulevard Madison,Wl 5"3704 October25, 1996 October28, 1996 November 25, 1996 April28, 1997 April28, 1997 3 Acute Studies StevenM. Glaza Manager Francis(Bud)W. McDonald StudyDirector JeffreyB. Mcks In-lifSeupervisor Rose M. Bridge AdministrativSeupervisor ToxicologySupport Kathy Myers Manager CalvinL. Horton Supervisor KEY PERSONNEL CHW 6329-185 Laboratory Animal Medicine Cindy J.Cary,DVM Diplomate,ACLAM Supervisor Anatomical Pathology Thomas E.Palmer,PhD AnatomicalPathologist DeborahL. Pirkel/ Jack Serfort Supervisors NecTopsy QualityAssurance SherryR. W. Petsel Manager 4 CONTENTS CHW 6329-185 QUALITY ASSURANCE STATEMENT STUDY IDENTIFICATION .......................................2............... KEY PERSONNEL 4 SUMMARY 7 OBJECTIVE 9 REGULATORY COMPLIANCE ..............................................9............... TEST AND CONTROL MATERIALS .........................................9................ Identification 9 Purityand Stabilit.y......................................................9................ Storageand Retention....................................................1.0................ SafetyPrecaution.s.......................................................1.0............... TEST SYSTEM .................................................................1.0................ TestAnimal.............................................................1.0................ Housing ................................................................1.0................ Animal Diet II Selectioonf TestAnimals II Study Design......................................................................................I................ JustificatifoonrSpeciesSelectio.n..........................................I.I................ PROCEDURES 11 Preparatioonf Exposure Area ..............................................I.I................ Dose Administratio.n......................................................................1.2................ Reason forRoute ofAdministratio.n........................................1.2................ Observationsof Animals ..................................................1.3................ Blood Sample Collections/Shipme.n.t.......................................1.3................ Pathology...............................................................1.4............... Shipment ofBileand Tissues..............................................1.4................ StatisticAanlalyses.......................................................14................ Locationof Raw Data,Records,and FinalReport..............................1.4............... CHW 6329-185 RESULTS ................................................................1.5................ Body Weights ...........................................................1.5................. Clinical Obsmations .........................................................1.5.................. Dermal Irritatio.n............................................................1.5.................. Pathology ...................................................................1.5.................. DISCUSSION ..................................................................1.6................. SIGNATURE ..................................................................1.6.................. REFERENCE ..................................................................1.6.................. TABLE I Individualand Mean Body Weights (g).......................................1.7.................. 2 IndividualClinicalSigns...................................................1.8.................. 3 IndividualDermal IrritatioSncores- Group I (Control)- DistilleWdater (0.0mg/kg/day)..........................1.9.................. 4 IndividualDermal IrritatioSncores- Group 2 - T-6564 (10.0mg/kglday) ........................................2.0.................. APPENDIX A .................................................................2.1.................. IndividualAnimal PathologyData .............................................2.2.................. APPENDIX B .................................................................3.4.................. ProtocolTP6)51 .............................................................1.5.................. Amendment No. I to the Protocol..............................................4.9.................. 6 SUNINLKRY CHW 6329-185 This studywas done to assessthesystemicabsorption/toxicaintdy relativsekinirritancy ofT-6564 when appliedtotheskinof rabbitfsor5 consecutivedays. The studywas conductedusingthreemale and threefemaleacclimatedrabbitsof the Hm:(NZW)SPF strainforeachtreatmengtroup- Group Control/ Dose Level Nurhberof Animals TestMaterial (mg/kglday) Males Females I(Control) Distillewdater 0.0 2 T-6564 10.0 a Administeredata dosevolume of 0.5nilag of body weight. The back of each rabbitwas clippedfreeofhairand a singledose oftherespective controlor testmaterialwas administeretdotheskinoftherabbitsfor5 consecutivedays. The treatmentsitesremained intactT.he areaof applicatiownas coveredwith a gauze patchsecuredwith papertapearound alledgeiand overwrapped with Saran Wrap's and Elastoplasttla&petoprovidean occlusivedressingforeach approximate2'j-houerxposure period. Clinicaolbservationwsere conductedpredoseon Day I and atapproximately1,2.5,and 4 hoursaftereachcontrolor testmaterialadministration Days I through5. Mortality checkswere conductedtwicedailyon Days 2 through29 (a.m.mortalitcyheck onlyon Dav 29).Additionalclinicaolbservationwsere conducteddailyon Days 6 throuah29. Bodv weightswere determinedon Day -5 forrandomizationpurposes,beforethefirst controlor testmaterialadministratio(nDay 1),and atthescheduledsacrificienterval (Day 29).The initiadlermalirritatiroenadingwas made beforethefirsctontrolor test materialadministratio(nrecordedastheDay I reading).Subsequentreadingsof dermal irritatiwoenre made aftereach patchremovalon Days 2 through6 and on Day I-'IA. bloodsample (approximatel4y mL) was collectefdrom eachanimalon Days -3,8, 15, and 22. Inadditiona,tthetimeofnecropsy(Day 29),approximatel2y040 mL of blood was obtainedfrom each controlanimaland approximately20 mL ofbloodwas obtained 7 CHW 6329-185 from each Group 2 animal.Allsampleswere centifugedand separatesamplesof serum and cellulafrractionwsere obtainedand sentfrozenon dry icetotheSponsor. On Day 29,theanimalswere anesthetizewdithsodium pentobarbitabll,edviatheposterior vena cava,exsanguinatedand necropsied.T'hewhole liverb,ile,an approximateI-cm x 1-cm sectionof thedermalapplicatiosnitea,nd bothkidneys(collecteadsone sample) were collectefdrom allariimalsw,eighed(volumeonlydeterminedforbile)a,nd sent frozentothe Sponsor. Applicatioonf T-6564 didnotresulitnany testmaterial-relatcehdangesinbody weight gain ormacroscopicfindingsatnccropsy.Allanimalsappearednormal throughoutthe study.In thedistillewdatercontrolanimals,no dermalirritatiwoans observedinone animaland slighto severedermalirritatiwoans observedintheotherfiveanimals.In theanimalstreatedwith T-6564,slighdtermalirritatiwoans seen inthreeanimals,and moderatetoseveredermalirritatiwoans seen intheotherthreeanimals.The reasonfor theunexpecteddermal irritatiionnthedistillweadtercontrolgroup was not determined. 8 OBJECTIVE CHW 6329-185 The objectivoefthisstudywas toassessthesystemicabsorption/toxiacnidtyrelative skinirritancoyf a testmaterialwhen appliedtotheskinofrabbitsfor5 consecutivedays. REGULATORY COMPLIANCE This studywas conductedinaccordancewiththeUaitedStatesFood and Drug AdministratioGnood LaboratoryPracticeRegulationfsorNonclinicalLaboratory Studies2,1 CFR 58,withtheexceptionthatanalysiosfthetestmaterialmixturesfor concentratiohno,mogeneity/solubiliatnyd,stabilitwyas notconducted.All procedures usedinthisstudywere incompliancewiththeAnimal WelfareAct Regulations.In the opinionoftheSponsorand studydirectort,hestudydidnotunnecessarildyuplicateany previouswork. Allproceduraltimespresentedinthisreportfallwithintheacceptable rangesasspecifieidntheWisconsinfacilitoyfComing HazletonInc.(CHW) Standard OperatingProcedure(SOP). TEST AND CONTROL MATERIALS Identification The testmaterialwas identifieadsT-6564 and was describedas.a clear,colorlessliquid. The controlmaterialwas distillewdater(NeenahSprings;ExpirationMay 20, 1997)and was describedasa clear,colorleslsiquid. Purityand Stability The Sponsorassumes responsibiliftoyrtestmaterialpurityand stabilitdyeterminations (includinugndertestconditions)A.nalysisof thetestmateriamlixturesfor concentratiohno,mogeneity/solubiliatnyd,stabiliwtays notconducted.The purityand stabilitoyfthecontrolmaterialwere consideredtobe adequateforthepurposesof this study. 9 CHW 6329-185 Storageand Retention The controland testmaterialwsere storedatroom temperatureA. reservesampleofthe controland testmaterialwsas takenand storedina freezersettomaintaina temperature of-20*C :t10*. The controlmaterialreservesamplewillbe retainedatCHW forone yearinaccordancewith CHW SOP. The testmaterialreservesample was senttothe Sponsor.Any unused testmaterialwas returnedtotheSponsoraccordingtoCHW SOP. Any remainingcontrolmaterialmay be used forothertestinagnd willnot be discarded afterissuanceof the finalTeporL SafetyPrecautions The controland testmaterialhandlingprocedureswere accordingtoCHW policies. SOPs and TEST SYSTEM TestAnimal Adultalbinorabbitosf theHra:(NZW)SPF straiwnere receivedfrom HR.P,Inc., Kalamazoo,Michigan on October 16,1996. Housina, Afterreceiptt,heanimalswere acclimatedfora periodofatleast7 days. Durinc, acclimatioannd throughoutthestudy,theanimalswere individuallhyoused in suspended stainlesssteelcages.Envirorunentaclontrolsfortheanimalroom were settomaintaina temperatureof 19' to2')*C, a relativheumidityof50% 20%, and a 12-hour light/12-hoduarrklightincgycle.In caseswhere variationfsrom therequired temperatureand humidityconditionsexistedt,heywere documented and consideredto have had no adverseeffecton thestudyoutcome. 10 CHW 6329-185 Animal.Diet The animalswere providedaccesstowaterad libitumand a measuredamount of LaboratoryRabbitDietHF #5326,PNU Feeds,Inc.The feedisroutinelyanalyzedby the manufacturerfornutritionaclomponentsand environmentalcontaminants.Samples of thewaterareperiodicallaynalyzed.Therewere no known contaminantsinthefeedor wateratlevelsthatwould be expectedto interf@rweithor affectheresultsofthe study. SelectionofTest Animals The animalswere identifiebdy animal number and correspondingeartagand were placed intostudygroupsusinga stratifibeoddy weightrandomizationprogram. The randomizationbody weightswere determinedon Day -5. Study Design Animals weighing from 2,0-'t1o82,270g and approximately14 to 18 weeks ofage at initiatiofn treatmenwtere placedintothefollowingstudygroups: Group Control/ Dose Level Dose Volume Number ofAnimals TestMaterial (mg/kg/day)(mL/kg/day) Males Females 1 (Control) Distillewdater 0.0 0.5 2 T-6564 10.0 0.5 JustificatiofnorSpeciesSelection Historicalltyh,eNew ZealandWhite albinorabbithas been theanimalofchoicebecause ofthelargeamount ofbackgroundinformatioonn thisspecies. PROCEDURES PreparationofExposure Area On theday beforethefirsctontro!ortestmaterialapplicationt,heback and,ifnecessary (toobtainunblemishedskin)t,heflanksof eachrabbitwas clippedfreeof hairwithan CHW 6329-185 electric.clippTehre. clippedareamade up approximately20% ofthetotalbody surface area.The testsites(intacstkin)were inspectedforinterferilnegsionsi,rritatiorn, defectsthatwould precludetheuse ofany oftheanimals.The animalswere clippedas neededthroughoutthestudy(Days 4,13 and 29). Dose Administration Allanimalsreceivedfiveconsecutivdeays of administrationftherespectivceontrolor testmaterial.The firsdtay oftreatmentwas designatedasDay 1-. Group 1. An individuadlose was calculateadnd measured basedon each animal's body weighton thefirsdtay oftreatmentT.he contromlaterial(distillweadter)was appliedtothetestsiteata dose volume of0.5mL/kg ina thinand uniformlayer. The rateof applicatiownas approximately0.04mL/cM 2 . Group 2. An individuadloseofthetestmateriamlixture(T-6564and distilled water)ata concentratioonf20 mg/mL was calculateadnd measured based on each animal'sbody weighton thefirsdtay of treatment.The testmaterialmixturewas appliedtothetestsiteata dose volume of0 .5 mL/k-g of body ,veight in a thin and uniformlayer.The rateof applicatiownas'approximately0.04mL/cm 2 . Each areaofapplicatioinnGroups Iand 2 was coveredwitha 4-ply5-cm x 5-cm gauze patch.Each gauze patchwas securedwithpapertapearound alledges and ovenvrapped with Saran WrapO and Elastoplastt'aspetoprovidean occlusivedressing.Collarswere used torestraitnheanimalsduriniezach adt)roximat2e')-hourexposureperiod. Approximately2-'h)oursaftereach controlortestmaterialapplicationt,herestraining collarsand patcheswere removed and theapplicatiosniteswere rinsedwith tapwaterand driedwith disposablepapertowels. Reason forRoute of Administration T'hedermal routeisa potentiarlouteofexposureinhumans. 12 CHW 6329-185 Observations of Animals Clinical observations were conducted predose on Day I and at approximately 1, 2.5, and 4 hours aftereach controlor testmaterialadministrationon Days I through 5. Mortality checks were conducted twicedailyon Days 2 through 29 (am. mortalitycheck only on Day 29). Additionalclinicaolbservationswere conducted dailyon Days 6 through 29. Body weights were determined on Day -5 forrandomization purposes,beforethe first controlor testmaterialadministratio(nDay 1),and atthe scheduled sacrificeinterval (Day 29). The initiadlermal irritatiorneadingwas made beforethe firstcontrolor testmaterial applicationaccording to theDraize technique(recordedas the Day I reading). Subsequent readingsof dermal irritatiownere made within '0 to 37 minutes 4:@er each patchremoval (Days 2 through 6) and on Day 13. Blood S2mple Collections/Shipment A blood sample (approximately4 mL) was collectedfrom a marginal ear vein of each animal on Days -'38,, 15,and 22. In addition,atthe time of necropsy (Day 29), approximately 20 to 40 mL of blood was obtainedfrom each controlanimal and approximately 20 mL of blood was obtainedfrom each Group 2 animal viathe posterior vena cava. All samples were storedatroom temperatureuntilcentfi@ffigeAdf.ter centrifugations,eparatesamples of senim and cellularfractionswere obtained and stored in a freezersetto maintain a temperatureof -20'C IO*C untils-hipped to theSponsor. The serum and cellularfractionsamples obtained on Days -'3,8,and 15 were shipped frozen(on dry ice)to the Sponsor (James D. Johnson,3M E.T. & S, Bldg. 2-')E-09,935 Bush Avenue, St.Paul,MN, 55106) on Day 17. The serum and cellularfractionsamples obtained on Days 22 and 29 were shipped tothe Sponsor one week afterthe experimental (in-lifed)ateof terminationinthe same manner as the samples obtained priorto Day 22. The Sponsor isresponsiblefortheretentionand dispositionof the samples. CHW does not accept any responsibilitfyorthe analysisof the samples collectedin thisstudy nor are theseresultspresentedin thisreport. 13 CHW 6329-185 Pathology At terminationof the in-lifexperimentalphase (Day 29),animals were anesthetizedwith sodium pentobarbitalb,led viathe posteriorvena cava, exsanguinated,and necropsied in random order. The sitesof controlor testmaterialapplicationwere washed with warm tap water before the necropsy procedure. Allanimals were subjectedto an abbreviated gross necropsy examination and any abnormalitieswere recorded. The whole liver,bile, an approximate I-cm x I-cm sectionof the dermal applicationsite,and both kidneys (collectedas one sample) were collectedfrom allanimals,weighed (volume only determined forbile),and immediately placed ina freezersetto maintain a temperature of -20'C 10. After necropsy,the animals were discarded. Shipment of Bile and Tissues One week afterthedate of in-lifexperimentaltermination,the tissues(whole livers, dermal applicationsites,and kidneys)and bilewere sentfrozen(on dry ice)to the Sponsor (James D. Johnson, 3M E.T. & S, Bldg. 2-')E-09,9')5 Bush Avenue, St.Paul, NfN, 55106), along with documentation of theircorrespondincyweights or volumes. The Sponsor isresponsibleforthe retentionand dispositionof the samples. CHW does not accept any responsibilitfyorthe analysisof the samples collectedin thisstudy nor are theseresultspresented inthisreport. StatisticaAlnalyses No statisticalnalyseswere requiredby the protocol. Location of Raw Data, Records, and Final Report The raw data,records,and an originalsigned copy of the finalreportwillbe retainedin the archivesof CHW in accordance with CHW SOP. 14 RESULTS CHW 6329-185 Body Weights Individuaalnd mean body weightsareinTable 1. Allanimals,withtheexceptionof Animal No. F60987 (Group2 male),exl'ubitead weightlossfrom randomizationto initiati(oinn-lifeT)h.isweightlosscanbe attributteodtheacclimatioonftheanimalsto restrainincgollarcsonductedfor3 days(approximatel2y3 hours/day)beforetheinitial controland testmaterialadministratioAnl.l animalsgainedweightfrom initiation (Day 1)toterminatio(nDay 29). ClinicalObser-vations IndividuacllinicaslignsareinTable2. Allanimalsappearednormal throuchoutthe study. Dermal Irritation Individualdermal irritatisocnoresareinTables3 and 4. The controlmaterial(distilled water)didnotproducedermalirritatiionnone animal.Four othercontrolanimals exhibitedslightomoderate ervthema,slighetdema and/orslighdtesquamationreactions. Slighttosevereerythemaand edema reactionasnd slightdesquamationwere observedin theothercontrolanimal.No explanatiofnortheunexpecteddermalirritatiionnthe distillewdatercontrolgroupwas found.The testmaterialT,-6564,producedslightto moderate erythemaand edema reactionisnfiveanimals.One oftheseanimalsalsohad slighdtesquainationon theapplicatiosnite.Slighttosevereerythema and edema reaction(swithsubcutaneoushemorrhaging)s,lighdtesquamationand coriaceousness, and moderate fissurinwgere obser-vedintheotheranimal treatedwith T-6564. Patho]oU Individuaalnimalpathologydata(tissuweeights,bilevolumes,and grosspathology observationsa)representedinAppendix A. Observedatnecropsyon the liverof one Group 2 femalewas a singlef,irm,green,pedunculatedmass (0.7x 0.3x 0.-'clm) attachedtotheventralsurfaceoftherightmedian lobenearthe gallbladderT.he findines CHW 6329-185 inthisanimalswas not consideredto be testmaterialrelatedN.o visiblelesionswere seen inany oftheotheranimalsatnecropsy. DISCUSSION The acutesystemicabsorption/toxiciatnyd relativsekinirritancoyfT-6564 was evaluatedinmale and femalealbinorabbitwshen administeredermallyfor 5 consecutivdeays. Applicationofthismaterialdidnotresulitnany testmaterial-related changesinbody weightgainor macroscopicfindingsatnecropsy.Allanimalsappeared normalthroughoutthestudy.Slighttoseveredermalirritatiwoans observedinthe distillewdatercontrolanimalsand intheanimalstreatewdithT-6564. SIGNATURE F.Bud W. McDonald Date StudyDirector Acute Studies REFERENCE 1. Draize,J.H.,"AcuteDermal Toxicity(SingleExposure),I"n:AppraisaloftheSafety of ChemicalsinFoods,Drugs and Cosmetics-Dermal ToxicityA,ssociatioonf Food and Druc,OfficialosftheU.S.,pp.54-56(1959). 16 Table I Individualand Mean Body Weights (g) CHW 6329-185 Animal Number Males Random -ization Day 1 29 Animal Number Females Random -ization Day 1 29 Group 1 (Control)-DistilleWdater (0.0mg/Wday) F60982 F60983 F60984 Mean 2,213 2,20-3 2,258 2,225 2,11--1 2,764 2,097 2,67-3 2,102 2,646 2,104 2,694 F60988 F60989 F60990 Mean 2,297 2,246 2,298 2,280 2,142 2,101 2,114 2,714 2,677 2,783 2,119 2,725 Group 2 - T-6564 (10.0mg/kg/dav) F60985 F60986 F60987 2,196 2,199 2,26-) 2,0-)8 2,58-) 2,086 2,597 2,270 2,82-) F60991 F60992 F6099'j 2,210 2,181 2,269 2,068 2,047 2,207 2,676 2509 2,8-35 Mean 2,219 2,131 2,668 Mean 2,220 2,107 2,673 17 Table 2 IndividualClinicaSligns CHW 6329-185 Animal Number Sex Observation Day 11 Day 2 Day 3 Day 4 Day 5 Hour Hour Hour Hour Hour Day(s) 1 2.5 4 1 2.5 4 1 2.5 4 1 2.5 4 1 2.5 4 6 7 8-11 12 13-15 16-29 F60982 M Appeared normal F60993 M Appeared normal F60994 M Appeared normal Group I (Control-)DistillWeadter (0.0mgnwday) ol z V or .01 f ee eV ol e F60988 F60989 F60990 F Appeared normal F Appeared normal F Appeared normal e e F60985 M F60986 M F60997 M Appc=d normal Appeared normal Appeared normal Group 3 -T-6564 (10.0mg/kglday) V V e of e of e F60991 F Appeared normal e .1 ol .1 e .1 .1 e F60992 F Appeared normal .1 / V .1 F60993 F Appeared normal oo' VV Each animal appeared normal priortocontrolortestmaterialadministration. Conditionexists. 18 CHW 6329-185 Table 3 IndividualDermal IrritatioSncoresGroup I (Control)- DistilleWdater (0.0mg/kc,,,/day) Dermal Reaction Erythema Edema Atonia Desquarnation Coriaceousness Fissuri9n Erythema Edema Atonia Desquamation Coriaceousness Fissuri9n Erythema Edema Atonia Desquamation Coriaceousness Fissuring Males Study Day -1 2 4 5 6 13 Animal No. F60982 0 1 1 122 1 011 1111 0 000 000 000000 1 00 00 000 00 00 000 Animal No. F60983 00 00000 0 00 0000 0000 000 0 000 000 0000 000 0000 000 Animal No. F60984 000 122 1 00001 10 0 0 000 00 0 0 000 0 1 0 0 000 00 0 0 00000 Females Study Day 1 2 3 4 5 6 13 Animal No. F60988 01 1 1 22 1 00 1 1 1 10 00 0 0 0 00 000 0000 00 0 0 00 0 000 0000 Animal No. F60989 0 1 1 1 12 1 001 1 1 10 00 0 0 00 0 00 0 0 00 0 00 0 0 00 0 000 0000 Animal No. F60990 01 1 12 31 00 1 1 3 00 0 00 0 0 000000 1 00 00 000 00 0 0 00 0 19 Table 4 IndividualDermal IrritatioSncoresGroup 2 -T-6564 (10.0mg/kc,,/day) CHW 6329-185 Dermal Reaction Males Study Day 1 2 3 4 5 6 13 Animal No. F60985 Erythema Edema Atonia Desquamation Coriaceousness Fissuring 00 1 1 1 10 00001 10 0 0 00 00 0 0 0 00 00 0 00 00 00 0 00 00 00 0 Animal No. F60986 Erythema Edema Atonia Desquamation Coriaceousness Fissurincy 00 0 122 1 000022 1 0 0 0 0 0 0- 0 0 0 0000 1 00 0000 0 0 0 0000 0 Animal No. F60987 Erythema Edema Atonia Desquamation Coriaceousness Fissurina 00 1 1 1 1 0 0001 1 1 0 0 0 0000 0 0 0 0000 0 0 0 00000 0 0 0000 0 a Subcutaneoushemorrhaizing. Females Study Day 12 4 5 6 13 Animal No. F60991 00 1 1 1 10 00 0 0 0 1 0 00 00 000 0000 000 000 0000 00 0 0 00 0 Animal No. F60992 0 1 2 2 3 "3a 2 0 1 1 233 1 000 0000 000000 1 000 01 1 0 0 0 0 0 00 2 Animal No. F60993 01 22221 01 1 1 1 10 00 0 0 0 00 00 00 000 0000 000 00 00000 -)o APPENDIX A IndividualAnimal PathologyData CHW 6329-185 21 Individual APPENDIX A Animal Pathology Data Corning Hazleton Inc. Madison, Wisconsin USA ------------------------------------------------------------------------------------------------------------------- ANIMAL NUMBER: F60902 SEX: MALE DOSE GROUP; I SACRIFICE STATUS: SCHEDULED, TERMINAL SACRIFI DATE OF DEATH: 11/2S/96 STUDY DAY OF DEATH: 29 STUDY WEEK OF DEATH: S TERMINAL BODY WEIGHT: NOT E DATE AND TIME OF NECROPSY: 11/2S/96 14:22 PROSECTOR: DAVID SCHUETTE RECORDER: STEVE VAN ADES POST-FIX WEIGHER: NOT AVAILABLE PATIIOLOGIST: DR. TOM PALMER WEIGHER: STEVE VAN ADEST ------------------------------------------------------------------------------------------------------------------- ABSOLUTE ORGAN WEIGHT ORGAN WEIGHT RELATIVE ORGAJ4 TO BRAIN 0R 0 ORGAN NAME ---------------------- (GRAMS) -------- TO BODY WEIGHT (t) -------- WEIGHT PATIO -------- STA ------ DERM APPL. SITE KIDNEY (KD) JIS) 0.9747 IS.2166 --------------- --------------- WEIGHT WEIGHT LIVER (LI) 86.3171 -------- -------- WEIGHT BILE (ML) (BI) 1.6 -------- -------- WEIGill ------------------------------------------------------------------------------------------------------------------- G R 0 S S P A T It0 L 0 0 Y 0 8 S 8 R V A T 1 0 N S . . . ORGAN NAME SEVERITY, KEYWORD(S) OR PHRASE FREE-TEXT COMMENTS AND NOTES ---------------------- --------------------------------------- ----------------------------------------------- GENERAL COMMENT (GC) . .. .. .. . ... .. .. .. . .. .. .. .. .. .. .. .. .. . .. .. .. . -ABBR NEC PERFORM -NO MACROSCOPIC LESIONS ------------------------------------------------------------------------------------------------------------------- APPENDIX A Individual Animal Pathology Data Corning Hazleton Inc. Madison, Wisconsin USA ------------------------------------------------------------------------------------------------------------------- ANIMAL NUMBER: P60903 SEX: MALE DOSE GROUP: I SACRIFICE STATUS: SCHEDULED, TERMINAL SACRIPI DATE or DEATHI 11/2S/96 STUDY DAY OF DEATHI 29 STUDY WEEK OF DEATH: S TERMINAL BODY WEIGHTs NOT E DATE AND TIME OF NECROPSYT 11/25/96 14:23 PROSECTOR: DEBBIE PIRKEU RECORDER- STEVE VAN ADES POST-FIX WEIGHER: NOT AVAILABLE PATHOLOGIST: DR. TOM PALMER WEIGHER.- STEVE VAN ADEST ------------------------------------------------------------------------------------------------------------------- ORGAN NAME ---------------------- ABSOLUTE ORGAN WEIGHT (GRAMS) -------- ORGAN WEIGHT RELATIVE TO BODY WEIGHT (t) -------- ORGAN TO BRAIN WEIGHT RATIO -------- 0 RG ST A ------ DER14APPL. SITE (IS) 1.27S] ........ ........ WRIGHT KIDNEY (KD) 14.0416 -------- -------- WEIGHT LIVER (LI) 83,7942 -------- -------- WEIGHT BILE IML) (BI) 0.6 -------- -------- WEIOIIT -------------------------------------------------------------------------------------------------------------------- GR PA TH 0 L0G Y 0B S ERV AT 10 N S ORGAN NAME SEVERI;Y: KEYWORO(D:ISOR PHRASE FREE-TEXT COMMENTS AND NOTES ---------------------- --------------------------------------- ------------------------------------------------ t-i GENERAL COMMENT (GC) . . . . . . . . . . . . . . . ..... . . . . . . . . . . . . . . . . . . . . . . . . . . . -ABBR NEC PERFORM -NO 14ACROSCOPIC LESIONS -------------------------------------------------------------------------------------------------------------------- APPENDIX A individual Animal Pathology Data Corning Hazleton Inc. Madison, Wisconsin USA ------------------------------------------------------------------------------------------------------------------- ANIMAL NUMBER: F60984 SEXT MALE DOSE GROUPI I SACRIFICE STATUS: SCHEDULED, TERMINAL BACRIPT DATE OF DEATH: 11/2S/96 STUDY DAY OF DEATH: 29 STUDY WEEK OF DEATH: 5 TERMINAL BODY WEIGHTI NOT E DATE _ AND TIME OF NECROPSYs 11/25/96 14:34 PROSECTOR: DAVID SCHUETTE RECORDER: STEVE VAN ADES POST FIX WEIGHERT NOT AVAILABLE PATHOLOGIST: DR. TOM PALMER WRIC;HERT STEVE VAN ADEST ------------------------------------------------------------------------------------------------------------------- ABSOLUTE ORGAN WEIGHT ORGAN WEIGHT RELATIVE ORGAN TO BRAIN 0R 0 ORGAN_NAME (GRAMS) TO BODY WRIGHT 11) WEIGHT RATIO S TA ----- ---------------- -------- -------- -------- ------ DERM APPL. SITE (IS) 0.8S39 -------- -------- WEIGHT KIDNEY JKD) IS.5098 -------- -------- WRIGHT LIVER (LI) 06.3868 -------- -------- WEIGHT BILE (ML) (BI) o.6 ........ -------- WRIGHT ------------------------------------------------------------------------------------------------------------------- 0 R 0 s S P A T It0 L 0 G Y 0 8 S E R V A T 1 0 N S ORGAN NAME SEVERITY, KEYWORD(S) OR PHRASE FREE-TEXT COMMENTS AND NOTES ---------------------- --------------------------------------- ----------------------------------------------- GENERAL COMMENT (OC) . . . . . . . . . . I . . . ... . . . . . I . . . . . . . . . -ABOR NEC PERFORM -NO MACROSCOPIC LESIONS ------------------------------------------------------------------------------------------------------------------- APPENDIX A Individual Animal Pattiology Data Corning Hazleton Inc. Madison, Wisconsin USA ------------------------------------------------------------------------------------------------------------------- ANIMAL NUMBER: F6098S SEX: MALE DOSE GROUPI 2 SACRIFICE STATUS: SCHEDULED, TERMINAL SACRTFI DATE OF DEATH: 11/2S/96 STUDY DAY OF DEATI(I 29 STUDY WEEK OF DEATH: 5 TERMINAL BODY WEIGHTI HOT E DATE AND TIME OF NECROPSY: 11/25/96 14:S9 PROSECTOR: DAVID SCHUETTE RECORDERT STEVE VAN ADES POST-FIX WEIGHER: NOT AVAILABLE PAT[IOLOGIST: DR. TOM PALMER WEIGHER: STEVE VAN ADEST ------------------------------------------------------------------------------------------------------------------- ABSOLUTE ORGAN WEIGHT ORGAN WEIGHT RELATIVE ORGAN TO BRAIN 0 R0 ORGAN NAME ---------------------- (GRAMS) -------- TO BODY WEIGHT (t) -------- WEIGHT RATIO -------- ST A ------ DERN APPL. SITE (IS) 0.8180 -------- -------- WEIGHT KID N EY ((LKD) 13.2012 -------- -------- WEIGHT IVER 1) 62.45ss -------- -------- WRIGHT BILE (ML) (BI) 0.0 -------- -------- WRIGHT ------------------------------------------------------------------------------------------------------------------- G R 0 S S P A T If0 b 0 a Y 0 B S E R V A T 1 0 N S ORGAN NAME SEIE;I;Y: KEYWORD(S) OR PHRASE FREE-TEXT COMMENTS AND NOTES ---------------------- --------------------------------------- ----------------------------------------------- GENERAL COMMENT (GC) ABBR Hic,piR.FORM. . -NO MACROSCOPIC LESIONS ------------------------------------------------------------------------------------------------------------------- APPENDIX A individual Animal Pathology Data Corning Nazleton Inc. Madison, Wisconsin USA -------------------------------------------------------------------------------------------------------------------- ANIMAL NUMBER: P60986 SEX: MALE DOSE GROUP! 2 SACRIFICE STATUS: SCNEDULED, TERMINAL S)KCRIFIC DATE OF DEATH: 11/2S/96 STUDY DAY OF DEATH: 29 STUDY WEEK OF DEATH: S TERMINAL BODY WEIGHTI NOT B DATE AND TIME OF NECROPSY: 11/25/96 IS:00 PROSECTOR: DEBBIE PIRKEL RECORDER: STEVE VAN ADEST POST-FIX WEIGHER: NOT AVAILABLE PATIfOLOGISTi DR. TOM PALMER WEIGHER: STEVE VAN ADESTI -------------------------------------------------------------------------------------------------------------------- ABSOLUTE ORGAN WEIGHT ORGAN WEIGHT RELATIVE ORGAN TO BRAIN 0 Ra ORGAN NAME ---------------------- (GRAMS) -------- TO BODY WEIGHT (t) -------- WEIGHT RATIO -------- S TA T ------- DERM APPL. SITE KIDNEY (KD) LIVER (LI) (IS) 1.8205 13.4319 S7.22S6 --------------- -------- ---------------------- WEIGHT HEIGHT WEIGHT BILE (ML) (81) O.S -------- ........ WRIGHT -------------------------------------------------------------------------------------------------------------------- 0R 0S S PA TH 0 L00 Y 0 BS ER VA T 10N 3 . . . ORGAN NAME SEVERITY. KEYWORD(S) OR PHRASE FRER-TEXT COMMENTS AND NOTES ---------------------- ------------------------------7--------- ------------------------------------------------ GENERAL COMMENT JOC) .. .. .. . ... .. . .. .. .. .. .. .. .. .. .. . .. .. .. . .. ... . ti C7% -ABOR NEC PERFORM -NO MACROSCOPIC LESIONS -------------------------------------------------------------------------------------------------------------------- APPENDIX A Individual Animal Pathology Data Corning Hazleton Inc. Madison, Wisconsin USA ------------------------------------------------------------------------------------------------------------------- ANIMAL NUMBER: P60997 SEX: KALE DOSE GROUP: 2 SACRIFICE STATUS: SCHEDULED, TERMINAL SACRIPI DATE OF DEATHR 11/2S/96 STUDY DAY OF DEATH: 29 STUDY WEEK OF DEATNT S TERMINAL BODY WRIGHTI NOT B DATE AND TIME OF NECROPSY: 11/25/96 15:09 PROSECTOR: DEBBIE PIRKEL RECORDER: STEVE VAN )TDBS POST-FIX WEIGHER: NOT AVAILABLE PATHOLOGIST: DR. TOM PALMER WEIGHERI STEVE VAN ADEST -------------------------------------------------------------------------------------------------------------------- ORGAN NAME ---------------------- ABSOLUTE ORGAN WEIGHT (GRAMS) -------- ORGAN WEIGHT RELATIVE TO BODY WEIGHT (t) -------- ORGAN TO BRAIN WET014T RATIO -------- 0 R0 ST A ------ DERM APPL. SITE (IS) 0.7972 -------- -------- WEIGHT KIDNEY (KD) IS.8230 -------- -------- WEIGHT LIVER (61) 90.8606 -------- -------- WEIGHT BILE (ML) (81) 0.2 -------- -------- WEIGHT ------------------------------------------------------------------------------------------------------------------- . * . r.R 0 S S P A T It0 L 0 (1Y 0 B S C R V A T 1 0 N S ORGAN NAME SEVERITY, KEYWORD(S) OR PHRASE FRER-TEXT COMMENTS AND NOTES ---------------------- -------------------------------i-------- ----------------------------------------------- GENERAL COMMENT (GC) .. .. . ... .. .. .. .. .. .. .. . .. .. .. .. .. .. .. . .. .. .. -AADR NEC PERFORM -NO MACROSCOPIC LESIONS -------------------------------------------------------------------------------------------------------------------- APPENDIX A Individual Animal Pathology Data t'i 00 Corning Ha2leton rnc. Madison, Wisconsin USA ------------------------------------------------------------------------------------------------------------------- ANIMAL NUMBERI P60988 SEX: FEMALE DOSE GROUP: 1 SACRIFICE STATUSI SCHEDULED, TERMINAL SACRrpx DATE OF DEATHT 11/2S/96 STUDY DAY OF DEATHI 29 STUDY WEEK OF DEATH: S TERMINAL BODY WEIGHTT NOT E DATE AND TIME OF HECROPSY: 11/25/96 14:3S PROSECTOR: DEBBIE PIRKEL RECORDERI STEVE VAN ADES POST-FIX WEIGHER: NOT AVAILABLE PATHOLOGIST: DR. TOM PALMER WETC;HER: STEVE VAN ADEST ------------------------------------------------------------------------------------------------------------------- ABSOLUTE ORGAN WEIGHT ORGAN WEIGHT RELATIVE ORGAN TO BRAIN 0R0 ORGAN NAME ---------------------- (GRAMS) -------- TO BODY WEIGHT (t) -------- WEIGHT RATIO -------- 9 TA ------ DERM APPL. SITE KIDNEY (KD) LIVER (LI) BILE (ML) (BI) (IS) 2.0750 16.3783 82.S349 1.6 ---------------------........ ----------------------------- WEIGHT WRIGHT WEIGHT WEIGHT ------------------------------------------------------------------------------------------------------------------- . * . 0 R 0 S S P A T H 0 L 0 0 Y 0 8 S 2 R V A T 10 N S ORGAN NAME SEVERITY, KEYWORD(S) OR PHRASE FREE-TEXT COMMENTS AND NOTES ---------------------- --------------------------------------- ----------------------------------------------- GENERAL COMMENT (GC) .. ... .. . .. .. . .. ... . .. .. . . ... .. ABBR N iE C 'PiE RiFORiM * * . * ' ': -NO MACROSCOPIC LESIONS ------------------------------------------------------------------------------------------------------------------- APPENDIX A individual Animal Pathology Data Corning Hazleton Inc. Madison, Wisconsin USA ------------------------------------------------------------------------------------------------------------------- ANIMAL NUMBER! F60989 SEX: FEMALE DOSE GROUP: 1 SACRIFICE STATUS: SCHEDULED, TERMINAL SACRIPI DATE OF DEATHI 11/2S/96 STUDY DAY OF DEATH; 29 STUDY WEEK OF DEATH: 5 TERMINAL BODY WEIGHTI NOT E DATE AND TIME OF NECROPSY: 11/2S/96 14:49 PROSECTOR: DEBBIE PIRKEL RECORDER: STEVE VAN ADES POST-FIX WEIGHER: NOT AVAILABLE PATHOLOGIST: DR. TOM PALMER WEIGNERI STEVE VAN ADEST ------------------------------------------------------------------------------------------------------------------- ORGAN NAME ABSOLUTE ORGAN (GRAMS) WEIGHT ORGAN WEIGHT RELATIVE TO BODY WRIGHT (t) ORGAN TO 13RAIN WEIGHT RATIO 0R0 ST A ---- ----- ---- ---- ------ -------- ------ DERN APPL. SITE (IS) 1.1923 -------- KIDNEY (KDI 16.1610 WRIGHT LIVER (LI) 77.6OeS -------- WEIGHT BILE (ML) (BI) 1.8 -------- ----- WEIGHT ----------------------------------------------------------------------------------------------------------W-E-IG-H-T-- G R 0 s S P A T li0 L 0 0 Y 0 B S C R V A T 1 0 N s ORGAN NAME SEVERITY, KEYWORD(S) OR PHRASE FREE-TEXT COMMENTS AND NOTES ---------------------- --------------------------------------- ----------------------------------------------- t-i GENERAL COMMENT (GC) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . %.0 -Al3BR NEC PERFORM -NO MACROSCOPIC LESIONS -------------------------------------------------------------------------------------------------------------------- APPENDIX A Individual Animal Pathology Data Corning Hazleton Inc. Madison, Wisconsin USA -------------------------------------------------------------------------------------------------------------------- ANIMAL NUMBER: P60990 SEX: FEMALE DOSE GROUP: I SACRIFICE STATUST SCHEDULED, TERMINAL SACRIPIC DATE OF DEATHI 11/2S/96 STUDY DAY OF DEATH: 29 STUDY WEEK OF DEATH: 5 TERMINAL BODY WEIGHTs NOT EN DATE AND TIME OF NECROPSY: 11/2S/96 14:48 PROSECTOR: DAVID SCHUETTE RECORDER: STEVE VAN ADEST POST-FIX WEIGHER: HOT AVAILABLE 'PATHOLOGIST: DR. TOM PALMER WEIGHERI STEVE VAN ADESTI -------------------------------------------------------------------------------------------------------------------- ABSOLUTE ORGAN WEIGHT ORGAN WEIGHT RELATIVE ORGAN TO BRAIN 0 Ra ORGAN NAME ---------------------- (GRAMS) -------- TO BODY WEIGHT It) -------- WEIGHT RATIO -------- STA T ------- DERM APPL. SITE (IS) 0.7232 -------- -------- WEIGHT KIDNEY (KD) 13.4790 -------- -------- WEIGHT LIVER LI) 93 1001 -------- -------- WEIGHT BILE (MLI) (BI) i:i -------- -------- ---------------------------------------------------------------------------------------------------------W-EI-G-H-T ------- G R0 SS PAT R0 L0 0Y 0 8 SER VA T 10N 9 ORGAN NAME SEVERITY, KEYWORD(S) OR PHRASE FREE-TEXT COMMENTS AND NOTES ---------------------- --------------------------------------- ------------------------------------------------ GENERAL COMMENT (GC) . . . . . . . . . . . . . . . ... . . . . . . . . . . . . . . . . . . . . . . . . . . . . -ABBR NEC PERFORM -NO MACROSCOPIC LESIONS -------------------------------------------------------------------------------------------------------------------- APPENDIX A Individual Animal Pathology Data Corning Hazleton Inc. Madison, Wisconsin USA ------------------------------------------------------------------------------------------------------------------- ANIMAL NUM13ER- F60991 SEX: FEMALE DOSE GROUP! 2 SACRIFICE STATUS: SCHEDULED, TERMINAL SACRIPI DATE OF DEATH: 11/2S/96 STUDY DAY OF DEATH: 29 STUDY WEEK OF DEATH: 5 TERMINAL BODY WEIGHT: NOT E DATE AND TIME OF NECROPSY: 11/2S/96 IS:09 PROSECTORI DAVID SCHUETTE RECORDER: STEVE VAN ADESI POST-FIX-WEIG"ER:-NOT-AVAILABLE PATHOLOGIST: DR. TOM PALMER WEIGHER: STEVE VAN ADESTI -------- -------- --- ---------------------------------------------------------------------------------------------- ORGAN NAME ABSOLUTE ORGAN WEIGHT ORGAN WEIGHT RELATIVE ORGAN TO BRAIN 0RG ---------------------- (GRAMS) -------- TO BODY WEIGHT (t) -------- WEIGHT RATIO -------- 9TA I ------- DERM APPL. SITE (IS) 1.0478 -------- -------- WRIGHT KIDNEY (KD) 13.4087 -------- -------- WEIGHT LIVER ILI) SS.4184 -------- -------- WEIGHT BILE (ML) (BI) 0.2 -------- -------- ---------------------------------------------------------------------------------------------------------W-E-IG-I-IT------- G R0 SS PA TH0 L00 ORGAN NAME SEVE;1;1: IEYWORD(S) OR PHRASE ---------------------- -----------------------------I--------- GENERAL COMMENT (GC) .. .. .. . .. ... .. .. ... . -ABBR NEC PERFORM LIVER (LI) . . . . V 0B S ERV AT 10 NS . .. FREE-TEXT COMMENTS AND NOTES ------------------------------------------------ .. .. .. . .. ... .. .. .. . . .. ... '-"SS(ES) :A+TiC@E*D IO'V'ENTRAL SURFACE OF RIGHT MEDIAN LOBE BLADDER: SINGLE PEDTINCULATED MASS. 0.7 X 0.3 X 0 FIRM; SAME ON CUT SURFACE; REGIONAL LM (HEPATIC) -------------------------------------------------------------------------------------------------------------------- APPENDIX A Individual Animal Pathology Data Corning Hazleton Inc. Madison, Wisconsin USA -------------------------------------------------------------------------------------------------------------------- ANIMAL NUMBER: P60992 DATE OF DEATH: 11/2S/96 SEX: FEMALE STUDY DAY OF DEATH: DOSE GROUP: 2 SACRIFICE STATUS: 29 STUDY WEEK OF DEATH: S SCHEDULED, TERMINAL SACRTPI( TERMINAL BODY WEIGHT: NOT EN DATE AND TIME OF NECROPSY: 11/25/96 POST-FIX WEIGHER: NOT AVAILABLE 15;25 PROSECTOR: DEBBIE PIRKEL PATHOLOGIST: DR. TOM PALMER RECORDER: STEVE VAN ADEST WEIG14ER: STEVE VAN ADESTI -------------------------------------------------------------------------------------------------------------------- ORGAN NAME ---------------------- ABSOLUTE ORGAN WEIGHT (GRAMS) -------- ORGAN WEIGHT RELATIVE TO BODY WEIGHT (1) -------- ORGAN TO BRAIN WEIGHT RATIO -------- 0 R 43 8TA T ------- DERM APPL. SITE (IS) 1.3648 ........ ........ WEIGHT KIDNEY (KD) 13.S655 -------- -------- WEIGHT LIVER (LI) 82.SO47 -------- -------- HEIGHT BILE (ML) (BI) 0.5 -------- ........ HEIGHT -------------------------------------------------------------------------------------------------------------------- G R0 SS PAT H0 L00 Y 0 0 SER VA T 10N 3 .. . ORGAN NAME SEVERITY. KEYWORD(S) OR PHRASE FREE-TEXT COMMENTS AND NOTES ---------------------- --------------------------------------- ------------------------------------------------ GENERAL COMMENT (GC) . . . . . . . . . . . . . . ..... . . . . . . . . . . . . . . . . . . . . . . . . . . . . NJ -ABBR NEC PERFORM -NO MACROSCOPIC LESIONS -------------------------------------------------------------------------------------------------------------------- APPENDIX A Individual Animal Pathology Data Corning Hazleton Inc. Madison, Wisconsin USA -------------------------------------------------------------------------------------------------------------------- ANIMAL NUMBER: F60993 SEXT FEMALE DOSE GROUP: 2 SACRIFICE STATUS: SCHEDULED, TERMINAL SACRIFIC DATE OF DEATH: 11/25/96 STUDY DAY OF DRATHT 29 STUDY WEEK OF DEATH: 5 TERMINAL BODY WEIGHT: NOT EN DATE_AND TIME OF NECROPSYI 11/25/96 15:30 PROSECTOR: DEBBIE PIRKEL RECORDER: STEVE VAN ADEST POST FIX WEIGH ER: NOT AVAILABLE PATHOLOGIST; DR. TOM PALMER WEIGHERT STEVE VAN ADESTI -------------------------------------------------------------------------------------------------------------------- ORGAN NAME ---------------------- ABSOLUTE ORGAN WEIGHT (GRAMS) -------- ORGAN WEIGHT RELATIVE TO BODY WEIGHT It) -------- ORGAN TO BRAIN WEIGHT RATIO -------- 0 R0 ST AT ------- DERM APPL. SITE (IS) 0.9460 -------- -------- WEIGHTit KIDNEY (KD) 15.0657 -------- ---- WEIG,,T LIVER (LI) 91.6304 -------- W IG T BILE (ML) (BI) 0.4 -------- WEIGHT ---------------------------------------------------------------------------------------------------------------------------- 0 R0 SS P AT H0 L0 0Y 0 BS E RVA T 10 NS ORGAN NAME SEVE;I;Y: KEYWORD(S) OR PHRASE PRER-TEXT COMMENTS AND NOTES ---------------------- -----------------------------@-r------- ------------------------------------------------ GENERAL COMMENT (GC) . .. .. .. . ... .. .. .. .. .. .. .. .. . .. .. .. .. . .. .. . ... -ABBR NEC PERFORM -NO MACROSCOPIC LESIONS -------------------------------------------------------------------------------------------------------------------- APPENDIX B ProtocolTP6351 Amendment No. I totheProtocol CHW 6329-185 34 Corning HazlctonInc. P.O. Box 7S43 Niadi@.Wl 53,-07.7545 Delitvrie3s3:01Kint.liBnil-d. ALidso.. IX'lSJ704 608.241.4471 60S.241.7227 Fax CHW 6329-185 CORNING Hazleton Sponsor. 3M SL Paul.Minnesota PROTOCOL TP6351 StudyTitle: 5-DailyDose Dermal AbsorptiowToxicitSytudyofT-6564 inRabbits Date: October25. 1996 PerformingLaboratory: Coming HazletonInc. 3301 Kinsman Boulevard NiadisonW,isconsin 53704 Labor2tory ProjectIdentification: CHW 6329-185 Corning rharmaccutical SLr%ic" 35 CHW 6329-185 CHW 6329-195 TP6351 Page 2 STUDY MENTEFICATION 5-DailyDose Dermal Absorption/ToxiciSttyudyofT-6564 inRabbits CHW No. Test Material Sponsor Sponsor'sRepresentative Study Director Study Lor-ation Proposed Study Timetable ExperimentalStartDate ExperimentalTerminationDate DraftReportDate 6329-185 T-6564 3M ToxicologyService MedicalDeparanent 3M Center,Bldg.220-2E-02 P.O.Box 33220 St.Paul,MN 55133-3220 Roger G. Perkins,PhD, DABT 3M ToxicologyService MedicalDepartment 3M Center,Bldg.220-2E-02 P.OzBox 33220 SL Paul,MN 55 133-3220 (612)733-3222 F.Bud W. McDonald Coming HazletonInc. P.O.Box 7545 Madison,Wl 53707-7545 (608)242-7901 Coming HazletonInc. 3301 Kinsman Boulevard Madison,Wl 53704 Week of October28, 1996 Week of November 25, 1996 Week ofJanuar-y6, 1997 36 CHW 6329-185 CHW 6329-185 TP6351 Page 3 1. Study 5-DailyDose Dermal Absorptiorv7oxiciSttyudyinRabbits 2. Purpose To assessthesystemicabsorptioannd toxicitaynd relativsekinirtitancoyf a test materialwhen appliedtotheskinofrabbitfsorfiveconsecutivdeays 3. RegulatoryCompliance Thisstudywillbe conductedinaccordancewiththefollowingGood Laboratory PracticeRegulation&tStandards/Guidelwiintehstheexceptionthatanalysisof the testmaterialmixturesforconcentratiosno.lubilithyo,mogeneity,and stabiliwtiyll notbe conducted: Conduct asa NonregulatedStudy (Xl21 CFR 58 (FDA) 40 CFR 160(EPA-FtFRA) 40 CFR 792 (EPA-TSCA) C(81)30(Final()OECD) 59 NohSan No. 3850 (JapaneseNTAFF) NotificatioNnos. 313 and 970 (JapanesMeOHW) AliproceduresinthisprotocolareincompliancewiththeAnimal WelfareAct RegulationsI.n theopinionof theSponsorand studydirectort,hestudydoes not unnecessarildyuplicataeny previouswork. 4. QualityAssurance The protocols,tudyconduct,and thefinalreportwillbe auditedby theQuality AssuranceUnit inaccordancewiththeWisconsinfaciliotfy Coming Hazleton Inc.(CHW) StandardOperatingProcedures(SOPS)and policies. 5. TestNlaterial A. Identification T-6564 B. Phvsic2lDescription To be documented intheraw data 37 CHW 6329-185 CHW 6329-185 TP6351 Page 4 C- Purityand Stability The Sponsorassumesresponsibiliftoyrpurityand stabilidteyterminations (includinugndertestconditions)S.amplesoftestmaterial/vehimcilxeture(s) forconcentratiohno,mogeneity/solubilaintdy,stabiliatnyalyseswillnot be takenbeforeadministratiounlessrequestedotherwiseby the'Sponsor. These samples(iftaken)willbe senttotheSponsorafterexperimental termination. D. Storage Room temperature E. Reserve Samples Reservesample(s)of eachbatch/lootf testmaterialwillbe takenforthis study. The testmaterialreservesample(sw)illbe storedatCHW ina freezersetto maintaina temperaturoef -200C2:1(rCuntilreturnedtotheSponsorafter completionof thein-lifpehaseof thestudy. F. Retention Any unusedtestmaterialwillbe returnedtotheSponsoraftercompletionof allrelateidn-lifteesting. G. SafetyPrecautions As requirebdy CHW SOPs and policies 6. ControlNlater-ial A. ldentiric2tion Distiliewdater B. PhysicalDescription Clear,colorleslsiquid C. Purityand Stability The purityand stabiliotfythiscommerciallyavailablmeaterialisconsidered to be adequateforthepurposesofthisstudy. D. StorageConditions Room temperature 38 CHW 6329-185 CHW 6329-195 TP6351 Page 5 L Reserve Samples Reservesample(s)ofeach batch/lootfcontrolmaterialwillbe taken. The controlmaterialreservesample(sw)illbe storedatCHW ina freezerset tomaintaina temperaturoef -2VC I(rC. F. Retention Any remainingcontrolmateriamlay be usedforothertestinagnd willnotbe discardedafterissuanceof the finalreporl G. SafetyPrecautions As requiredby CHW SOPs and policies 7. ExperimentalDesign A. Animals (1) Species Rabbit (2) Strain/Source Hra:(NZW)SPF/HRP. Inc. (3) Age at Initiation Adult (4) Weight at Initiation 2.0to 3.0kg (5) Number and Sex 6 males and 6 females (6) Identification Individuanlumbered cartag (7) Husbandry (a) Housing Individualliyn, suspendedstainlesssteelr-ages 39 CHW 6329-185 CHW 6329-185 TP635i Page 6 (b) Food A measured&mount OfLAboratoryRabbitDietEF #5326 (PNC feeds,Inc.).The foodisroutinelaynalyzedby themanufacturer fornutritioncaolmponentsand environmentalcontaminants. (c) Water Ad libiliftrmom an automatiscystem.Samplesof thewaterare analyzedfortotaldissolvesdolidss,pecifiemdicrobiological contentselectedelements,heavy metals,organophosphatesa,nd chlorinatehdydrocarbons. (d) Contaminants There areno known contaminantisnthefood or waterthat would interferweiththisstudy. (e) Environment Environmentalcontrolfsortheanimalroom willbe setto maintaina temperaturoef 19*C to23*C, a relativheumidityof 5(r/2.:2(r/a.n,d a 12-hourlight/12-hoduarrkcycle.The dark cyclemay be interrupteddue toin-lifperocedures. (r)Acclimation At least7 days (8) SelectoirToensAtnimals Based on healthand body weightaccordingto CHW SOPS. An adequatenumber of extraanimalswillbe purchasedso that no animalinobviouslypoorhealthisplacedon test.The animalswill be placedintostudygroupsusinga stratifibeoddy weight randomizatiopnrogramwithinninedaysof studyinitiation. (9) JustiricatiofnorSpeciesSelection Historicalltyh,eNew ZealandWhite albinorabbithas been theanimal of choicebecauseof thelargeamount of backgroundinformationon thisspecies. 40 CHW 6329-185 CHW 6329-185 TP6351 Page 7 B. DoseAdministration (1) TestGroups Group ControV Dose Level TestMaterial (mg&gtday) I (Control) 2 Distilled Water 0.01 T-6564 -T- 10.0-- Number of Animals Males Females 3 3 3 3 To be administereadta dosevolume of 0.5mL/kg of body weight To be administereadta dosevolume of 0.01mL/kg of body weight (2) PreparatoifEoxnposuArreea On thdeaybefotrheeinittieasaltndcontrmoalteraipapllicatthieon, back and.ifnecessary(toobtainunblemishedskin)t,heflanksof each rabbitwillbe clippedfreeofhairwithan electricclipper.The shaved areawillconstitutaepproximatel2y01/.ofthetotalbody surfacearea. The treatmenstite(sintacstkin)willbe inspectefdorinterfering lesionsi,rritationr.defectsthat'woulpdrecludetheuseof any of the animals.The animalswillbe clippedasneeded throughoutthestudy. (3) Dose Administration Allanimalswillreceivefiveconsecutivdeays ofadministrationfthe respectivceontrolor testmaterialappliedtothesame respective applicatiosniteeachday. The testmaterial/vehicmliexturewillbe preparedfresheachday ofadministratioTnh.e firsdtay oftreatment willbe designateads Day 1. The controlmateriawlillbe applied undilutedata dose volumeof 0.5mL/kg. The Group 2 testmaterial willbe dilutedwithdistillweadterand appliedata dose volume of 0.01mL/k-S.The dosesfortheanimalsinGroups I and 2 willbe basedon theanimal'sbody weighttakenon Day Ibeforethefirst administratioand appliedtotheareaofexposureina thinand unifor-lmayer.The areaofapplicatio(nGroupsI and 2) willbe completelycoveredwitha 4-ply5.0-cmx 5.0-cmgauzepatch.All patcheswillbe securedwithpapertapearound alledges and overwrappedwithSaranWrap' and Elastoplasta*peto providean occlusivedressing.The rabbitwsillbe collareduringeach approximate23-hourapplicatiopneriod.The preparedtestmixtures willbe storedatroom temperaturuentiladministration. 41 CHW 6329-185 CHW 6329-185 TP6351 Page 8 (4) Reason for Route ofAdministration The dermalrouteisa potentiarlouteof exposureinhumans. (5) Removal orTestMaterial Approximately23 hoursaftereachtestor controlmateiiaalpplication, thepatchesand collarwsillbe removed and theresiduamlaterialwill be removed usingwateror an appropriatseolventi,fnecessary.The sitesoftestand controlmateriaalpplicatiownillbe washed with warm tap waterpriorto the tissuceollectiopnrocedure. C. ObservationofAnimals (1) ClinicalObservations Beforecontrolor testmateriaaldministratioant,approximately1,2.5. and 4 hoursaftereachadministrationf controland testmaterialon Days 1-5forclinicasliM dailythereaftfeorrclinicasligns,and twice daily(a.m.and p.m.)formortalittyhroughDay 29 (a.m.mortality onlyon Day 29). Observationmsay be extendedwhen directebdy the studydirector. (2) Reading or Dermal Irritation Beforetheiniticaolntrolortestmateriaaldministratiotnh,edermal irritatiroenadingwillbe made and recordedastheDay I reading (Attachment1). Additionadlermalirritatiroenadingwsillbe made within30 to 60 minutesafteerachpatchremoval(Days 2-6)and on StudyDay 13. Individuadlermalirritatiroencordswillbe maintained foreach animal. (3) Body Weights For randomizationb,eforetheinititaelstor controlmaterialapplication (Day 1),on Day 29,or atdeath(when survivaelxceedsI day) (4) Blood Sample Collections (a) Frequency Predose(anytimefrom up tofourdays beforethe initidaolse administratitoonDay 1),on Days S. 15,22,and atexperimental terminatio(nDay 29) 42 CH\k"6329-185 CHW 6329-185 TP6351 Page 9 (b)NlethadofCollection/Numbeorf Animals Blood samples(approximatel4ymL) willbe collectefdrom a marginalcarveinof allanimalsattheintervalpsredosethrough Day 22. From theposteriovrena cavk approximatel2y0 mL of blood willbe obtainedfrom each animalsacrificeidna moribund conditio(nifpossiblea)p,proximatel2y0 to40 mL of bloodwill be obtainedfrom each controlanimalsacrificeodn Day 29 (the maximum volume possiblweillbe obtained)a,nd approximately 20 mL of bloodwillbe obtainedfrom each Group 2 animal sacrificeodn Day 29. The bloodsampleswillbe storedatroom temperatureand then centrifugeda,nd theseparateserum and cellulafrractionstored ina freezesrettomaintain-20*C :tlO*C.The serum and cellulafrractionosbtainedthroughDay 15 willbe sentfrozenon dry icetotheSponsorone totwo weeks priorto in-life terminationT.he serum and cellulafrractionosbtainedafter Day 15 willbe sentfrozenon dryicetotheSponsorwithinone week afterin-lifterminationT.he Sponsorisresponsiblfeor theretentioannd dispositiooiftt.hesamples. The serum and cellulafrrictiosnampleswillbe shippedto: James D. Johnson 3M E.T.& S Bldg.2-3E-09 935 Bush Avenue St.Paul,MN 55106 James D. Johnsonor hisalternatweillbe notifierdegardingthe shipmentof thesamples. 43 CHW 6329-185 CHW 6329-195 TP6351 Page 10 D. Pathology (1) UnscheduledSacririctasnd Deaths Any animaldyingduringthestudyor sacrificeidn a moribund conditiownillbe subjectetdoan abbreviategdrossnectopsy . examinationand allabnormalitiewsillbe recorded.Animals ina m oribundconditiownillbe anesthetizewdithsodium pentobarbita(lvia injectioinnthemarginalearvein).bledviathevena cava,and cxsanguinatedT.he whole liverb,ile(allavailablea)n. approximate ]-= x 1-cmsectioonf thedemat applicatiosniteand bothkidneys (collecteadsone sample)willbe collectefdrom allanimalsdying duringthestudyorsacrificeidna moribund conditionw,eighed (volumeonlydeterminedforbile)a,nd immediatelyplacedintoa freezesrettomaintaina temperaturoef-200C 10*C. Afternecropsy, theanimalsWillbe discarded. (2) Scheduled Sacririce On Day 29,theanimalswillbe anesthetizewdithsodium pentobarbital (viainjectioinnthemarginalcarvein)b,ledviathevena cavz, exsanguinateda,nd subjectedtoan abbreviategdrossnecropsy examination.The animalswillbe necropsiedinrandom orderand all abnormalitiweisllbe recorded.The wholeliverb,ile(allavailable), an approximate1-= x 1-cm sectionofthedermalapplicatiosnitea,nd bothkidneys(collecteadsone sample)willbe collectedw,eighed (volumeonlydeterminedforbile)a,nd immediatelyplacedintoa freezesretto maintaina temperaturoef -20*C 10*C. Afternecrapsy, theanimalswillbe discarded. (3) TissueSample Shipment The samples(liverb,iled,ermalapplicatiosnitea,nd kidneys)willbe sentfrozenon dry icetotheSponsorwithinone week aftercollection. The samplesand theircorrespondinwgeightsor volumes willbe shippedtothepersonlisteidn Section7.C.(4).(bT)h.e Sponsoris responsiblfeortheretentioannd dispositionf thesamples. F- StatisticAanlalyses No statisticaanlalysesarerequired. 44 CHW 6329-185 CHW 6329-185 TP6351 Page II S. Report A finalreportincludintghoseitemslistebdelowwillbe submitted. Descriptionofthetestand controlmaterials Descriptionof the testsystem Procedures Dates of experimentailnitiatiaonnd termination Tabulationof mortalitdyataby sex and dose level Descriptioonf any toxiceffects/dermiarlritation Tabulationof mean body weightsby sex and dose level Gross pathologyfindings Grosspathologyreport(ifrequestebdy theSnidyDirector) Individuaalnimaltissueweightsand bilevolumes 9. Locationof Raw Data,Records,ReserveSample(s)a,nd FinalReport Originaldata,or copiesthereofw,illbe availablaetCHW tofacilitaatuediting thestudyduringitsprogressand beforeacceptanceof thefinalrqmrt. When the finalreportiscompleted,contromlateriarleservesample(s)a,lloriginaplaper dam includintghoseitemslistebdelowwillbe retaineidnthearchivesof CHW fora periodofone yearfollowinsgigningof thefinalreport.One yearafter signingof thefinalrepom alloftheaforementionemdaterialwsillbe senttothe Sponsorand a returnfeewillbe charged.The Sponsormay electto have the materialrsetaineidntheCHW Archivesforan additionapleriodof time and CHW willchargea storagefee.IftheSponsorchoosestohave CHW disposeof thematerialsa,disposalfeewillbe charged. Protocoland protocolamendments Dose preparatiornecords In-lifreecords Body weights Randomizationdata Dose administration Observations Anatomicalpathologyrecords Sample collectiornecords Shippingrecords Study coffespondence Finalreport(originaslignedcopy) 45 CHW 6329-185 CKW 6329-185 TP6351 Page 12 The followingsupportinrgecordswillbe retaineadtCHW butwillnotbe archivedwiththestudydata. Animal receipttacclimatrieocnords Water analysisrecords Animal room temperatureand humidityrecords Refrigeratoarnd freezertemperaturerecords Instrumentcalibratioannd maintenancerecords 46 CHW 6329-185 PROTOCOL APPROVAL CHW 6329-185 TP6351 Page 13 R.4G. P.Iki.P,hD.DABT Sponsor's Representative 3M F. Bud W. McDorald Study Director Acute Studies Coming HazletonInc. FLepresen6tive QualityAssuranceUnit Coming FAzletonInc. (6329-ISS)RD DAe t9 Date Date 47 CHW 6329-185 CHW 6329-185 TP6351 Page 14 Attachment I ScorinSgcaleforAcuteDermalReactions Erythema 0 -None I -Slight 2 - Moderate 3 -Severe Edema 0 - None I - Slight(barelyperceptiblteo well definedby definitreaising) 2 - Moderate (raisedapproximately I mm) 3 - Severe (raisedmore than I mm) Atonia 0 - None I - Slight(slightimpairmentof elasticity) 2 - Moderate (slow returnto normal) 3 - Marked (no elasticity) Desquamation 0 - None I - Slight(slighstcaling) 2 - Moderate (scalesand flakes) 3 - Marked (pronounced flakingwith denuded areas) Coriaceousness 0 - None I - Slight(decreasein pliability) 2 - Moderate (leatherytexture) 3 - Marked (tough and brittle) Fissuring 0 - None I - Slight(definitceracksin epidermis) 2 - Moderate (cracksin dermis) 3 - Marked (crackswith bleeding) 48 CHW 6329-185 Corning Hitlecon Inc. P.O. Bx -,54S .%Iadiwa.VI $370"-,-545 Deinvnes: JJCI Kimpmjm Bh4. Atiduon. Wi 53704 601.241.4471 608.241.,-2-17 Fix AMENDMENT CORNING NO. ITO THE PROTOCOL Hazl"on ProtocoNlo.:TP6351 5-DailyDose Dermal AbsorptiorVToxiciSttyudyofT-6564 inRabbits CHW 6329-185 Sponsor 3M ToxicologyService MedicalDepartment 3M Center,Bldg.220-2E-02 P.O.Box 33220 St.Paul,MN 55133-3220 Sponsor'sRepresentative Roger G. PerkinsP.hD. DABT TestingFacility Coming HazletonInc. 3301 Kinsman Boulevard Madison.Wl 53704 Study Director F.Bud W. McDonald Thisamendment modifiesthefolio%%inpgortionoftheprotocol: EffectivOectober28. 1996 1. Paae 7,7.ExperimentalDesign,B. DoseAdministration(,1)TestGroups.The testmaterialcan notbe administereadta doselevelof 10.0m-e/kgusinga dosevolume of 0.01mL/L-g.To beabletoadministerthetestmaterialat10.0mg&-g.increasethe dosevolume to0.5mukg. Replacethetableinthissectionoftheprotocol%%iththe l'ollowing: Cornin; rhamiccutical Smic" 49