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CoriiingHazletonInc. po. Box 7S4S Madison,TI 53707-754S Deliveries3;_301 Kinsman Blvd.,Madison,Wl 608.241.4471 608.241.7227 Fax 53 704 OC)RNING Hazleton Sponsor: 3M St.PauL Minnesota FINAL REPORT Study Tide: PrimaryEye Irritation/CorroSstiuodnyofT-6684 inRabbits (OECD Guidelines) Author: StevenM. Glaza Study CompletionDate: January28, 1997 PerformingLaboratory: Coming HazletonInc. 3301 Kinsman Boulevard Madison,Wisconsin 53704 LaboratoryProjectIdentification: CHW 61101151 Pagel of3l FB 3 1997 COMPLIANCE STATEMENT CHW 61101151 PrimaryEye Irritation/CorrosSitoundyofT-6684 inRabbits (OECD Guidelines) Thisstudywas conductedinaccordancewiththeOrganisatiofnorEconomic Cooperation and DevelopmentPrincipleosfGood LaboratoryPracticeC,(81)30(Final). StevenM. Glaza- Date StudyDirector Acute Stadies Coming HazletonInc. 2 QUALITY ASSURANCE STATEMENT CHW 61101151 Thisreporthas been reviewed by the QualityAssurance Unitof Coming Hazleton Inc.,in accordancewith the OrganisationforEcomonic Cooperationand Development (OECD) Principleosf Good LaboratoryPracticeC,(81)30(Final)T.he followinginspectionwsere conducted and findingsreportedto the Study Directorand management InspectionDates From To 12/03/96 12/03/96 01/23/97 01/23/97 Phase Dose Preparation Data/ReportReview Date Reported to Study Director 12/03/96 01/23/97 Date Reported to Management 12/03/96 01/23/97 RepresentativeQ,ualityAssurangi'Unit Date 3 STUDY EDENTMCATION CHW 61101151 PrimaryEye Irritation/CorrosSitoundyofT-6684 inRabbits (OECD Guidelines) Test Material Sponsor Sponsor'sRepresentative Study Director Study Location Study Timetable Study InitiatiDoante Experimental(In-lifSet)artDate In-lifEend Date ExperimentalTerminationDate Study CompletionDate T-6684 3M ToxicologyService MedicalDepartment 3M Center,Bldg.220-2E-02 P.O.Box 33220 St.PaijLMN 55133-3220 Roger G. Perkins,-PhD 3M To7deology Service MedicalDepartment 3M Center,Bldg.220-2E-02 P.O.Box 33220 St.Pa4 MN 55133-3220 (612)733-3222 StevenM. Glaza Coming HazletonInc. P.O.Box 7545 Madison,WI 53707-7545 (608)241-7292 Coming HazletonInc. 3301 Kinsman Boulevard Madison,WI 53704 November 27, 1996 December 3, 1996 December 17,1996 December 17,1996 January28, 1997 4 Acute Studies StevenM. Glaza Study Director Manager StevenR- Sorenson Study Coordinator JeffTeBy. Mcks In-lifSeupervisor Rose M. Bridge AdministrativSeupervisor KEY PERSONNEL QualityAssurance SherryR- W. Petsel Manager CHW 61101151 LaboratoryAmimal Medicine Cindy J.Cary,DVM Diplomate,ACLAM Supervisor ToxicologySupport Kathy Myers Manager CalvinL. Horton Supervisor CONTENTS CHW 61101151 CO@"LIANCE STATEMENT ................................................2............. QUALITY ASSURANCE STATEMENT ........................................3............ STUDY IDENTIFICATION ..................................................4............. KEY PERSONNEL ..........................................................5............ 'OBJECTIW ................................................................8............ TEST NlATERLkL ...........................................................8............ Identificati.o.n............................................................8............ Purityand Stabili.t.y.......................................................8............ Storage and Retention......................................................8............ SafetyPrecautions.........................................................8............ TEST SYSTEM ..........................................i...................9............ Test Animal ..............................................................9............ Housing ..................................................................9............ Animal Diet..............................................................9............ Animal Selectio.n..........................................................9............ Jusfificatifoonr SpeciesSelection............................................9............ PROCEDURES ............................................................1.0............ Preparationof Test Material.........................* ........................1.0............ Treatment ...............................................................1.0............ Reason forRoute of Administratio.n.........................................1.0............ Observations.............................................................1.0............ Termination.............................................................1.0............ StatisticAanlalyses ........................................................I.I........... LocationofRaw Data,Records,and FinalReport..............................I..I........... RESULTS/DISCUS SION ....................................................I.I........... SIGNATURE ..............................................................1.1............ REFERENCES ..............................................I...............1.2............ 6 CHW 61101151 TABLE I AveragePrimaryEye IrritatiSocnores....................................13............ 2 IndividuaElye IrritatiSocnores.........................................1.4............ 3 Sodium FluoresceiEnxaminations.......................................1.8............ 4 IndividuaBlody Weights(g)............................................18............ APPENDIX .............................................................1.9............ ProtocolTP2072 .......................................................2.0........... ProtocolAmendment No. I ..............................................3.1............ 7 OBJECTIVE CHW 61101151 The objectiveof thisstudywas to assesstherelativleevelof irritation/corrospiroonduced followinga singleexposure of a testmaterialto one eye of albinorabbits.' AU proceduresused inthisstudywere incompliancewiththe Animal Welfare Act Regulations.In theopinionofthe Sponsor and studydirectort,he studydid not unnecessarildyuplicateany previouswork. Allproceduraltimes presentedinthisreport fallwithinthe acceptablerangesas specifieidntheWisconsin facilitoyf Coming Hazleton Inc.(CHW) StandardOperatingProcedure(SOP). TEST MATERL4L Identification The testmaterialwas identifieads T-6684 and describedas an off-whiteliquid. Purityand Stability The Sponsor assumes responsibiliftoyrpurityand stabilitdyetermination(sincludingunder testconditions). Storage and Retention The testmaterialwas storedatroom temperature.Any unused testmaterialwillbe returnedto the Sponsor afterissuanceofthe finalreportaccordingto CHW SOP. SafetyPrecautions The testmaterialhandlingprocedureswere accordingto CHW SOPs and policies. 8 TEST SYSTEM CHW 61101151 Test Animal Adult albinorabbitsoftheHra:(NZW)SPF straiwnere procuredfrom BRP, Inc., Kalsim.qoo,Mchigan on October 30, 1996. Housing Afterreceip@theanimalswere acclimatedfora periodof atleast7 days. During acclimationand throughoutthe study,the animalswere individuallhyoused instainless steelcages. Environmentalcontrolsforthe animalroom were setto maintaina temperatureof 19*to 23*C, a relativheumidityof 50% 20%, and a 12-hourlight/12-hour dark fightincgycle.In caseswhere variationfsrom theseconditionsexisted,theywere documented and consideredto have had no adverseeffecton thestudy outcome. Animal Diet The animalswere providedaccessto water ad libitumand a measured amount of LaboratoryRabbitDietBF #5326, PNff Feeds,Inc. The feedisroutinelaynalyzedby the manufacturerfornutritionaclomponents and environmentalcontaminants.Samples ofthe water areperiodicallaynalyzed.There were no known contaminantsinthe feedor water atlevelsthatcouldbe expectedto interferweith or affecthe resultsofthe study. Animal Selection Three healthy,acclimatedmale rabbitsw,eighing from 2,526 to 2,685 g and approximately 17 weeks of age,were selectedatrandom and identifiebdy animal number and correspondingeartag.The animals'eyeswere examined on theday before testmaterial administratiounsingsodium fluoresceidnye procedures.Only those animalswith no sign of ocularinjuryor irritatiwoenre used. Justiricatiofn.orSpeciesSelection Historicalltyh,e New ZealandWhite albinorabbithas been the anirnalofchoicebased on itslargeorbitand nonpigmented iris. 9 PROCEDURES CHW 61101151 Preparationof TestMaterial The testmaterialwas administereads received.The pH ofthetestmaterialwas not able tobe determined. Treatment Each rabbitreceived0.1 mL of theundilutedtestmaterialplacedintotheevertedlower Rd of therighteye,withthelefteye servingastheuntreatedcontrol.The upper and lower lidswere gentlyheldtogetherforI secondto preventlossofmaterialand thenreleased. The eyesoftherabbitsremainedunflushedimmediatelyaftertreatment. Reason forRoute ofAdministration Ifistoricaltlhye,ocularroutehas been therouteof choicebased on themethod of Draize.' Observations The treatedeyeswere observedforocularirritatiaotn1,24,48, 72,and 96 hours and Days 7 and 14 aftertreatment.Irritatiwoans gradedand scoredaccordingto theDraize techniqueusinga penlightasthesourceof ifluminationS.odium fluoresceienxaminations were used to aidinrevealinpgossiblecornealinjuryattheobservationcsonductedat24 hours. Animals were weighed beforetestmaterialadministratioand atweekly intervals throughoutthestudy. Termination At terminatioonf thein-lifpehase,aU animalswere euthanizedand discarded. 10 StatisticaAlnalyses No statistiacnaallyseswere requiredby theprotocol. CHW 61101151 LocationofRaw Data,Records,and FinalReport The raw data,records,and an originaslignedcopy ofthefinarleportwillbe retainedin thearchivesof CHW inaccordancewithCHW SOP. RESULTS/DISCUSSION Average primaryeye irritatisocnoresareinTable 1,withindividuaelyeirritatisocnoresin Table2. Sodium fluoresceienxaminationsand theindividuablody weightsareinTables3 and 4,respectively. The testmaterialT-6684,when evaluatedforitsprimaryeyeirritatipoontentiailnrabbits, produced a cornealopacityinone animal,ifida@lmvolvementintwo animals,and slighto moderate conjunctivailrritatiionnallthreeanimals.AR treatedeyeshad returnedto a normal appearanceby Day 14 aftertreatment. SIGNATURE StevenM. Glam Date StudyDirector Acute Studies REFERENCES CHW 61101151 1. "Acute Eye Irritation/CorrosioOnr,g"anisationforEconomic Cooperation and Development GuidelinesforTestingof Chemicals,Section405 (adoptedMay 12, 1981). 2. Draize,J.H., "Eye Mucosa," In: Appraisalofthe Safetyof ChemicalsinFoods, Drugs and Cosmefics- Dermal Toxicity,AssociationofFood and Drug Officialosf theU.S.,pp.49-50 (1959). 12 Table 1 Average Primary Eye IrritationScores Observafion Period Average Score* I Hour 12.3 24 Hour 6.7 48 Hour 6.7 72 Hour 5.3 96 Hour 4.0 Day 7 0.7 Day 14 0.0 The averageprimary eye irritation scoreisthe totaleye irritatisocnorefor 0 theanimalsdividedby thenumber of animals(3)ateach observafion period. CHW 61101151 13 Table 2 IndividualEye IrritatioSncores CHW 61101151 Animal Number Comea A B iris c Conjunctivae D E F Total Score*- F61209' I I F612IOu 0 0 F6121 1' 0 0 I Hour ii 2 1i 2 0 2 1 id 18.0 1 id 13.0 1 0 6.0 Mean 12.3 F61209 0 0 F61210 0 0 F61211 0 0 24 Hours 0 2' 1 id 8.0 0 2' 1 0 6.0 0 2 1 0 6.0 Mean 6.7 Cornea A - Degree of opacity B - Area of involvement iris C - Degree ofiridal irritation Conjunctivae D -Redness E - Chemosis F -Discharge Totalscore=(AxBx5)+ (Cx5) + [(D+E+F)x2]. b Blanching. d Purulentdischarge. i Injected. t No painresponseaftertestmaterialinsfillation. u Excessivepawing atthetreatedeye aftertestmaterialinstillation. 14 Table 2 (Continued) Individual Eye IrritationScores CHW 61101151 Animal Number Comea A B F61209 0 0 F61210 0 0 F61211 0 0 F61209 0 0 F61210 0 0 F61211 0 0 Cornea A - Degree of opacity B -Area ofinvolvement Totalscore=(AxBx5) b Blanching. d Purulentdischarge. Iris c Conjunctivae D E F Total Score* 48 Hours 0 2b I id 8.0 0 2 1 0 6.0 0 2 1 0 6.0 Mean 6.7 72 Hours 0 2 0 1 0 1 1 id 8.0 1 0 4.0 1 0 4.0 Mean 5.3 Iris C - Degree of iridal irritation Conjunctivae D -Redness E - Chemosis F - Discharge (Cx 5)+ [(D+E+F)x2]. 15 Table 2 (Continued) IndividualEye IrritatioSncores CHW 61101151 Animal Number Comea A B Iris Conjunctivae Total c D E F Score* 96 Hours F61209 0 0 0 1 1 0 4.0 F61210 0 0 0 1 1 0 4.0 F61211 0 0 0 1 1 0 4.0 Mean 4.0 Day 7 F61209 0 0 F61210 0 0 F61211 0 0 0 1 0 0 2.0 0 0 0 0 0.0 0 0 0 0 0.0 Mean 0.7 Cornea * -Degree ofopacity * -Area ofinvolvement Iris C - Degree ofiridat irritation Conjunctivae D -Redness E - Chemosis F - Discharge Totalscore=(AxB x5) (Cx5)+ [(D+E+F)x2]. 16 Table 2 (Continued) IndividualEye IrritatioSncores CHW 61101151 Animal Number Comea A B Iris Conjunctivae c D E F Total Score* Day 14 F61209 0 0 F61210 0 0 F61211 0 0 0 0 0 0 0.0 0 0 0 0 0.0 0 0 0 0 0.0 Mean 0.0 Cornea A -Degree of opacity B -Area ofinvolvement Iris C - Degree ofiridal irritation Conjunctivae D - Redness E - Chemosis F - Discharge Totalscore=(AxB xS)+(Cx5)+ [(D+E+F)x2]. 17 Table 3 Sodium FluoresceinExaminations Animal ObservationPeriod Number Preinitiation 24 Hour F61209 NEG NEG F61210 NEG NEG F61211 NEG NEG NEG Negativestainretention. CHW 61101151 Table 4 IndividuaBlody Weights(g) Animal Number Sex F61209 m F61210 m F61211 m Initial 2,685 2,526 2,632 Day 7 14 2,802 2,684 2,814 2,900 2,796 2,992 18 APPENDIX ProtocolTP2072 ProtocolAmendment No. I CHW 61101151 19 CHW 61101151 Sample SubmittalForm Thisformistobe usedwhensubmifibsiagnplasforovutine acidelestinSgp.eciatlestfnegedscanbe eashyarnvigodby contactifntg AcuteSILdieDseparknoWat(605)241-7292. CHWStudyNo. CotIOtIC( Encfosewithsaqplosandsendto: ComingHazletolnrc. 3301Knsnm Boulevard Mad=, Wisemsin 53704 Submktod by: e iz DateSan0a Sort: Company- Nwdmr ofReports Required: Ful GLP Compliance: -Y-, Y., FDA (21CFR U) -Kb -EPA(TSCA--40CFR792) EPA(FIFRA--40CFRiGO) -MA.FF :3K:OECD LIO+W Sample Name: 7- q w PhysicaDlescription* L6 T- (o(.8c F T--,G4 c, SpociWHancHingPrwA..to,A. .@s c AISKC-Q7-24VV-e, (.)7-7597-Y, e) Testmateriaplurkyand stabwtyWmation "uc&V underlostC"dkbm)on filweithSponsor Yes - No TestmixturearmlysifsorconcentralbrVtxnvWohy/stabft tobe conducted: Yes* - bySponsor- byCM Sample Disposal: ReturntoSponsoratfokwing addrom No -9 - 1A)o-U 3 rv,<;C-o u Y3 - ;S -o2- Sample StorageRequirements: Room tompsmurs RoHgemted Other- D*ms c(acootdkvtocw SOPS At addkionalcosttoSponsor(CKW wlicontact Sponsoras tothen additioncahlarges). AcuteOralToxicitIynRats -TP8084 -TP3206 -TP3013 XTP20-69 - Up anddownLDSO procedure FHSA scrow SM.SFat5.09&g ConductdefinesdtudIydeathoccursat5.0og EPA screenS;M-SFatS.0gtkg ConductdermadstudyI deathoccursat5.0gAg OECD sef"n SM-SFat5.0g/kg Conducdtfn;@ tudIydeath=. t5.0g*g Speciailnstructions: Acute DermalToxicitIynRabbits -TP3207 FHSA sason;SM-SF at2.0g/kg -TP3016 EPA screenS:M-5F at2.0gAg ConductdefinedstudyI deathoccursat2.0gtkg -TP20-70 OECD screenS:M.SF &12,0gfkg - Conductdafkwdstudy0 deathoccursat2.0g/kg Specialinstruciions: 1:@ A4Jb DEP,(*hAL Rd?S.UR!a @FX Fo--r--C-H-'UW-soOnly P I tissueDateI;=rector. \.--z Ln PrimarySkihkrmtion _TP3208 FHSA; 6 tabbks-Iabmdect I huactsketrabbk TP3014 EPA; 6 rabbhs-1lmactshokabbft :YTP2071 OECD; 3 robbks-lIrtacstke/mbbk -TP4206 DOT corrosiv6irfa,bbb-1btactsftofrabbk -TP714S Phototoxic6kyr-a.bbb-2k"ctshes/rabbk (onesitweithUVA exposure) SpocW instructions: PrimaryEye Irritation -TP6360 Low-votumeprocedure6; rabbitusnwashed -TP3200 FHSA;6 rabbiutnswashed -TP2012 1978EPA:6 rabbitusrwashed,3washed -TP301 S 1982EPA,6. rabbitusrvwashad ->(_TP2072OECD; 3 tabbksunwashed - 3rabbitwsashedat4 sownds - 3 rabbiwtasshedat30seconds SpeciaIlnstructions: uuinea Pig Sensitization -TP2017 EPA Magnusson-Kiigmamnaximization -TP6164.EC OECMC Magnussun-Kligmamnaximization -TP2008 Buehlersensitization -TP6289 Photoanargenciocntacdtermatft(iAsrmstrong) Speciailnstructions: Wtidecopy-CHW Yellowcopy-Submitter 20 CHW 6110115 1_ w"HAwZLIC-OCC)N SCO N S IN P 0 t T 0 f f C E 8 0 X 7 64 5 AAADISON. WISCIONSIN 93707-7545 a CORNW.V. Labwamy Sol-n C&IOPW Sponsor: 3M St. Paul, Minnesota PROTOCOL TP2072 Study Title: Primary Eye Irritation/CorrosioSntudy in Rabbits (OECD Guidelines) DLta: June 1, 1993 Performing Laboratory: Hazleton Wisconsin, Inc. 3301 Kinsman Boulevard Madison, Wisconsin 53704 Laboratory Project Identification: HWI 21 CHW 61101151 TP2072 Page 2 STUDY IDENTIFICATION PrimaryEye Irritation/CorrosioSntudy in Rabbits (OECD Guidelines) HWI No. Test Material Sponsor Sponsor's Representative Study Director Study Location Proposed Study Timetable Experimental Start Date ExperimentalTerminationDate Final ReportDate C-1/CZ/fS'( (See samplesubmittalform) 3M ToxicologyServices 220-2E-02 3M Center St. Paul,MN 55144 John L. Butenhoff,PhD 3H ToxicologyServices 220-2E-02 3M Center St. Paul, KN 55144 (612) 733-1962 Steven M. Glaza HazletonWisconsin,Inc. P.O. Box 7545 Madison, VI 53707-7545 (608)241-7292 HazletonWisconsin,Inc. BuildingNo. 3 3802 Packers Avenue Madison, WI 53704 Week of I Week of /.2 Week of .2 -,T-'t7 22 CHW 61101151 TP2072 Page 3 PrimaryEye Irritation/CorrosioSntudy in Rabbits(OECDGuidelines) 2. Purpose To assessthe relativelevelof irritation/corrosipornoduced follow'nga singleexposureof a test materialto one eye of albino rabbits 3. RtgulatoryCompliance. This studywill be conductedin accordancewith the followingGood LaboratoryPracticeRegulations/Standards/Guidelines: Conduct as a NonregulatedStudy 21 CFR 58 (FDA) 40 CFR 160 (EPA-FIFRA) 40 CFR 792 (EPA-TSCA) C(81)30(Final)(OECD) NotificationNo. 3850, August 10, 1984 (JapaneseKAFF) NotificationNo. 313, March 31, 1982,and as amendedby NotificationNo. 870, October5, 1988 (JapaneseMOHW) All proceduresin this protocolare in compliancewith the Animal WelfareAct Regulations. In the opinionof the Sponsorand study director,the study does not unnecessarilyduplicateany previous work. 4. Ouality Assurance For regulatedstudies,the protocol,studyconduct,and the final reportwill be auditedby the QualityAssuranceUnit in accordance with HazletonWisconsin(HWI) StandardOperatingProcedures(SOPS) and policies. 5. Test Material A. Identification (Seesample submittalfarm) B. PhysicalDestription (See samplesubmittalform) C. Purityand Stability The Sponsorassumesresponsibilityfor purityand stability determination(sincludingunder testconditions).Samplesof testmaterial/vehicmliexture(s)(ifapplicablef)or concentrations,olubility,homogeneity,and stabilityanalyses will be taken beforeadministratioinf requestedby the Sponsor. These samples(if taken)will be sentto the Sponsor afterexperimentalterminationfor possibleanalysis. 23 CHW 61101151 TP2072 Page 4 D. Storage (See sample submittalform) E. Reserve Samples Studies of less than 4 weeks in experimentalduration will not have reserve samples retained. Reservesample(s)of each batch/lotof test materialwill be taken if this study is more than 4 weeks in experimental duration. The test material reserve sample will be stared at HWI in a freezerset to maintain a temperatureof below C*C for 10 years per HWI SOP. The Sponsorwill be contactedafter 10 years for disposition in accordancewith the appropriateregulatoryGood Laboratory Practices. F. Retention Any unused test material will be discardedafter issuanceof the final report, unless directed otherwiseby the Sponsor. G. Safety Precautions As required by HWI SOPs and policies 6. ExperimentalDesign A. Animals (1) Species Rabbit (2) Strain/Source Hra:(NZW)SPF/HazletonResearch Products, Inc. (3) Age at Initiation Adult (4) Weight at Initiation 2.0 to 3.5 kg (5) Number and Sex 3 of any sex per group (6) Identification Individualnumbered ear tag 24 CHW 61101151 TP2072 Page 5 (7) Husbandry (a) HouSing Individually,in screen-bottomstainlesssteel cages (heavygauge). (b) Lod A measured amount of High Fiber Rabbit Chov? 15326 (PurinaMills, Inc.). The food is routinelyanalyzed by the manufacturerfor nutritionalcomponentsand environmental contaminants. (c) Water Ad libftum from an automatic system. Saoiplesof the water are analyzed by HWI for total dissolvedsolids, hardness,ct:nd specifiedmicrobiolOgical content and for sele d elements, heavy metals, organophosphates and chlorinated hydrocarbons. (d) @oniaminants There are no known contaminants In the food or water that would Interferewith this study. (e) Environment Environmentalcontrols for the animal room will be set to maintain a temperatureof 19 to 23*C, a r!lative humidity of 50% 20%, and a 12-hour light/12-hourdark cycle. (f)Acclimation At least 7 days (8) Selection of--TestAni-mal-s Based on health and body weight according to HWI SOPS. An adequate number of extra animals will be purchased so that no animal in obviouslypoor health is placedon test. The rabbits'eyes will be examinedusing sodium fluorescein dye procedures on the day before test material administration. Only animalswith no sign of corneal injuryor eye abnormalitieswill be used. (9) Justificationfor SpeciesSelection Historically, the New ZealandWhite albino rabbit has been the animal of choice based upon its large orbit and nonpigmented iris. 25 CHW 61101151 TP2072 Page 6 B. Dose Admini tration (1) Dose--Administration Beforeadministrationof liquidtest materials,the pH of the materialwill be d1etermined(if possible). Each rabbitwill receive0. mL of undilutedliquidtest materialor the weight equivalentof 0.1 mL of solid test material(not to exc:ed0.1 g). If necessary,solidtest materialswill be fi ely groundinto a dust or powder. The test materialwill be placed into the evertedlower lid of the rabbit'seye. The upperand lower lids will then be gently held together for I second before releasing to preventloss of material. If the test materialis an aerosol,the test eye will be held open and the test material administeredin a single burst of about I second from a distanceof approximately10 cm directlyin front of the eye. The eyes of the Group I rabbitswill remain unflushed for approximately24 hours following instillationof the test material. After24 hours,a washout may be used if consideredappropriate. If specifi:dby the Sponsor,the treated eyes of two other groups f animals (three animals/group)will be washed with lukewarm tap water for approximately30 seconds beginning approximately4 and 30 seconds, respectively, after instillationof the test material. The volumeand velocityof the flow should not cause injury. The right eye of each animalwill be treatedwith the test material and the left eye will serve as the untreatedcontrol. (2) Reason for Route of Administration Historically,the ocular route has been the route of choice based on the method of Draize. C. Observationof Animals (1) Readingof Ocular Irritation The treatedeyes of all animals will be examinedfor ocular irritationat approximately1, 24. 48, and 72 hours aftertreatment. If no irritationor injuryis presentat 72 hours, the 'groupwill be terminated. If irritatioins present at 72 hours, additional observationsmay be made at 96 hours and at 7, 14, and 21 days. If at any of these time points there is no irritation,the groupwill be terminated. If injuryis still presentat 21 days, additional observationsmay be requested by the Sponsor. After recording the 24-hour observations, sodium fluoresceinmay be used to aid in revealingpossiblecorneal injury. 26 CHW 61101151 TP2072 Page 7 Irritationwill be gradedand scoredusingthe Draize technique(Attachment1). All eye abnormalitiewsillbe recorded. All animalsthat have a damagedeye producing unduestressor discomfortwill be broughtto the attentionof the studydirectoror designeeaccordingto HWI policy. (2)Body Weights Before tesvmaterial administratioannd weekly thereafter (whenapplicable). D. fatholociy Any animalsdying during the studywill be subjectedto an abbreviatedgross necrapsyexaminationand all abnormalities will be recorded.After necropsy,the animalswill be discardedand no tissueswill be saved. At terminationof the experimentalphase, survivinganimalswill be designatedto be sacrificedand discarded. E. StatisticaAlnalyses No statisticalanalysesare required. 7. Report A finalreportincludingthoseitemslistedbelowwill be submitted: Descriptionof the testmaterial Descriptionof the test system Procedures Datesof experimentalinitiationand termination Summarytable showingthe irritationdata at each observationperiod Any specialobservationsthatwere recorded 8. ds, and Final Report Uriginaldata, or copiesthereof,will be availableat HWI to facilitateauditingthe studyduring its progressand before acceptanceof the finalreport. When the finalreportis completed, all originalpaperdata, includingthoseitemslistedbelowwillbe retainedin the archivesof HWI accordingto HWI SOP. Protocol and protocol amendments Dose preparationrecords In-liferecords Body weights Dose administration Observations Anatomicalpathologyrecords(if applicable) Study correspondence Finalreport(originalsignedcopy) 27 CHW 61101151 TP2072 Page 8 The followiingsupportingrecords will be retainedat NWI but will not be arch ved with the study data. Animal receipt/acclimationrecords Water analysis records , Animal room temperature and humidity records Refrigeratorand freezer temperaturerecords Instrument calibration and maintenance records CHW 61101151 PROTOCOL APPROVAL TP2072 Page 9 L. Butenhoff, PhD Sponsor's Representative 3M Steven M. Glaza u Study Director Acute Toxicology Hazleton Wisconsin, Inc. 1?(Itzem Representative Quality Assurance Unit Hazleton Wisconsin, Inc. (TP2072.3M) C,7," Date/ Date Date 29 CHW 61101151 TP2072 Page 10 Attachment I SCALE FOR 6= ING OCULAR LESIONS (OUIZE TECKNIUM) (A)222cl Degreeof density(area@t dum takenforreading) No "City ............................................................0 .................. Scattereodr diffusearea,detailsof Irisctearlyvisibl.e...................1.* ......... Easilydiscernibletranslucenatreas,dotalIs of irisatfghttyobscure.d...........2*..... Dpate=entareas,no detailsof irisvisible,sizeof pupilbarelydiscernib.le......3.*.. OpsqLm,Iris irwisfbt.e..........................................4.*...................... (9)Area of CorreaInvolved Cm-quorter(or toss),but not Rem ...................................I.................. Greaterthenam-4*mrter,but tossthenhalf.............................2............... Greaterthenhalf,but It" thanthree-qlmrte.r.s.........................3.............. Greater than three-qlmrtm tipto what* area.............................4............... A x & x S TotalNaxi@ o 80 (2)Ldl (A)Vattmg Mormt ......................................................0 ............................ Folds@bow norml, carqmtion,swltlng,clmu=rreat Injectio(nwrtor allof theme er combinatioonf anythereof)Iristoatiltreactingto tight(sluggisrheactionto Positive.)..................................................1.*.......................... No reactiotno tight,kwrhw, grossdestructioCnwy or allof these.).........2.*.... Ax5 TotalMaxi@ - 10 (3)Comfuncti (A)Redness(refersto potpebratand butborconjunctivaeexcludingcorrwoand Iris) Vesselsriomt ................................................0.......................... Vesselsdefinitelyinjectedabovenwmt ................................I ................ Norediffuse,deepercrimsonred, individuavlesselsnot easfty discernibl.e........2.... Diffusebeefyred...............................................3*........................ chemsis No smetting..................................................0........................... Any swttfrtoabovenw@t (includesnictitatinwgembrww).....................I.......... Obvioustwettingwith partialeversionof the lids.........................2.*............ Swellingwith tfdsabouthalfclosed..................................3.*................. Swellingwith tidsabouthalf closedto completelyclosed.....................4*.......... (C)Dfschar No discharge..................................................0.......................... Arw moumt dif ferent fram norrat (do" not inclucie smt i wwmts observed in inner contka ofnormt animis).........................................I..................... Dischargewithmoisteninogf the lidsard hairsjustadjacento the lid.s .........2..... Dischargewithmoisteningof the lfdsand hairs. considerablaereaaroundthe eye...3 Score (A 4 8 4 C) x 2 Total Nagimm - 20 thetotalscorefortheeye is thesLaof allscaresobtafrwdfor thecomes. iris.and conjumtivee. Indicateaspositiveffe". (FKSAinterpretation) 30 CHW 61101151 CHW No. Itrl PROTOCOL AMENDMENTS Amendment No. I Effective N-,JLcti4.r--.42-1,M't(.. Portionof ProtocolBeing Modified: Applicablesectionsof the protocol, Reasonfor Modification:To identifythe locationwhere the studywill be conducted and to reflect a company name change from HazletonWisconsin,Inc. (HWI) to CorningHazleton Inc. (CHW).replacewhereverapplicablethe followingchanges Modification: CorningHazletonInc. (CHW) 3301 Kinsman Boulevard. Madison, Wl 53704 (G21/01-07-91) Study DirectorApproval: i@o@ 31