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6295.23; ST-46 Protocol. AR6-9182, 050400 3M MEDICAL DEPARTMENT, CORPORATE TOXICOLOGY Protocol for Study Nos. T-6295.23; ST-46 ExploratoryIn-VitroPercutaneousAbsorptionStudyofTheophylline,Salicylic os R--6 `Reconstituted EpidermisModel Study Objective: M`TohdiselstbudyyciosnddeuscitginnegdatsoigmapilnefaabmsiolriaprtiitoynwsittuhdythoenStkwinoEptrheivciRoeucsolnyscthiatruatcetderEipzieddermis cfloumoproouchnedmsic(atlhecoophmyploluinneda(npdersfalluicoyrloiocctayclisdulifnoanaptaep,eKr*)b.y DSouupcpeotr,ticnt.gaa)na,lyatsicwaelllwoasrkonfeor tphairstsotfumdeytwhiolldbaenddoinnestirnutmheentnqeuwalCiofircpaotriaont.e TAoxMicToTloagsysaLyabwoirllatboerycoinndBuucitleddinagt 2th3e6eansd of the absorption study the test compounds. to determine if SkinEthic viability was affectedbyapplication of Research Client: 3M Specialty Chemicals Division 3M Center, Building 236 Saint Paul, MN 55144 Sponsor: 3M Specialty Chemicals Division 3M Center, Building 236 Saint Paul, MN 55144 Study Location: 3M Strategic Toxicology Laboratory 3M Center, Building 270-35-06 room SB314 Saint Paul, MN 55144 Study Director: John Butenhoff, Ph.D. Senior Laboratory Manager 3M Medical Dept. / Corporate Toxicology 3M Centr, Building 220-2E-02 Saint Paul, MN 55144 Ph.: 651-733-1962 FAX: 651-733-1773 Study Toxicologist: Kathy Thompson, MP.H. Senior. Toxicologist 3M Medical Dept. / Corporate Toxicology 3M Center, Building 220-2E-02 Saint Paul, MN 55144 Ph: 651-733-9578 FAX: 651-733-1773 Proposed Study Timeline Start Date: Wednesday, April 12%, 2000 EAnnadlyDtaitcea:l CFroimdpayl,etAiproinlD1a4t%e,:2T00B0D Final Report Completion Date: TBD 604435 T-6295.23; ST-46 Protocol. 05/0400 | Regulatory Compliance: p`Trhoitsosctoluadyndwiclllasbseifpieerdfoasrmaed"CilnastsheC3SMtuSdtyr"ataesgiecxpTloaxiinceodliongyTLOaXborSaOtPor0y9u5n0d,eSrtraatdeefgiinced. Toxicology Lab GLP Program Procedure. Test Material: `LTihaeisfolnu,o3roMchCehmeimcialcatlesst Dmiavtiesriioanl.wTihllebedrpurgovtiesdtedmabteyrDiaalnwHilalkebse,suPprpoldiuecdtbRyesSpiongsmiab.ility Identification: Names: TPehrefolpuhoyrloloicnteyl(suTlHfEo)nate, K* (PFOS, K* salt) Salicylic Acid (SA) Molecular Formulas: CiFnSOsK* (PFOS) C7-H8-N4-02 (THE) C7-H6-03 (SA) Lot Number: Documentation will be kept on file by the Sponsor for PFOS (Lot 217) and by the Corporate Toxicology Analytical Laboratory for THE and SA. Purity: CDoorcpuomreantteaTtoixoincwoillolgbyeAkneapltyotincfailleLabbyortahteoSrpyofnosroTrHfoEr aPnFdOSS,A.andbythe Stability: CDoorcpuomreantteatTiooxnicwoillolgbyeAkneapltytoincaflilLeawbiotrhattoherySpfoornTsoHrEfoarnPdFSOAS., and by the Storage Conditions: Upon receipt, test material will be stored tightly sealed at room temperature. Characteristics: Information on synthesis methods, composition or other characteristics that definethetest material will be kept on file with the Sponsor for PFOS, andbythe Corporate Toxicology Analytical LaboratoryforTHE and SA. SkinEthic Preparation Procedure: aTshepeSrklihneEtmhaincufRaecctounrsetristuitnesdtrEupcitdioenrsmi(sscweiAllttbaecphrmeepnatreOdnei)m.meAdbisaotrepltyiounpotnesatrirnigval will begin on April 13, 2000. using aseptic techniques. All handling of SkinEthic material will be done 04436 2 T-6295.23; ST-46 Protocol. 05/0400 | Materials: a Twelve filters SkinEthic Human Reconstituted Epidermis, Size 0.63 cm', and twelve blank @ a ASdkdiintEitohniaclMeamipnttyen1a2ncweelMlecdulituumre(psluaptpelsi(edBebcytomnanDuifcakcitnusroenr)) a Heating Block (37C) a Incubator (37C, S%CO, saturated humidity) Reagents: R1e0c2e7p7t8o1r),M1e.d5i%uBmo-viPnheosSpehartuemBAulfbfuermeidnS(aSliignmea(,GAi-b8c0o2B2RLLoCta#t3#91H40260901-)07a5d,deLdofot#r FC compound @ Compound application vehicle~ Milli-Q Water @ @ T1r%ypSsionap(SSioglumtai,olnot(T#w3e9eHn092502,,Maclalii#nTc-k7r4o1d8t), lot #H285 N13H32) Q MTT (Sigma, lot #39H5076, cat #M-2128) Procedure: @ bUlnapnakcfkilatenrdwemlalisntaacicnorSdkiinngetthoicmaRneucfoancsttuirteurt'esd iEnpsitdreurctmiiosns(RinEpc)ontsrkoinllceedlltceumlptuarneds and humidity incubator. @ eBnevfiorroenpmreondtuacltcaopnpdliitciaotniosnf, oe2xrpohsouerRsEtp0 eaqnudilbiblraantkefwiilttehr waemlblisentot sattamnodsaprhderreo.om a Place 0.6 ml receptor medium in each well of 12-well culture plates. Transfer block. REp and blank filters gently with forceps to each well and place on heating 2 Evenly apply 200 ul ofTHE and SA compound solutions to REp and blank filter surface in triplicate, of blank application 200 ul of PFOS vehicle (water) compound solution to the remainder and in quadruplicate, start timer: and 200 ul 1. THE applied as saturated water solutionof 6 mg/ml 2. SA applied as saturated water solution of2 mg/ml 3. PFOS applied asasolution of 0.025 mg/ml (50 uM) a TmreadnisfuemraRfEtepr 0a.n2d5bhlra,n0k.5fihltre,r1gehnrt,l2yhwri,t4hbfro,racenpds6tohrn.ew well containing receptor Atendofexperiment, polypropylene vial for place later the receptor analysis. medium of each plate well into a 604437 3 T-6295.23; ST-46 Protocol. osia00 | @ rWiansseh3thteimReEspwiatnhdsbalmaenkvofillutemresuorffawcaete3r.tiGmeenstwliytwhi2p0e0culeLanoefd1s9%ursfoaacepwsiotlhutiaocn,otatnodn tip. Save washing fluids and tips in a polypropylene vial for later analysis. sCaomnpdluecstfMoTr TneRgeadtuivceticoonntraosls(awyaotneroanpeplsiacmaptlieonfoonrleya)cthotdeesttecrommipneouSnEdvaianbdiltitwyo. @ dCiugtesrtemfaorin4i8nghosukrisn wmietmhbTrraynpesisnaantd4b0laC.nk fAifltteerrshionmtoogsemnailzlaptiieocnesanwditchenstcriisfsuorgsatainodn p(o1l0y0p0rgo)pyfloern1e0vimailn,fofrilltaetrersuapnealrynsaitsa.nt through a0.45 jum filter and save in a Numberofanalytical samples generated : total =182: AS.urfPaFcOeSW:ashing FluiBdas:tt=6hrs B. THE: 6att=6hrs C sa: 6att=6hrs D. Water: 4att=6hrs Receptor Medium: FE.. TPFHOES:: Gceacah actth=0a.2t5hthrrs=s,,000..552hhrr5ss,, 11..00hhrrss,, 22.00hhrsr,44..s00hhr,rss,, 66..00hhrrss. G. SA: H. Water: Geachatt=025hrs, 4cachatt=025 hrs, 0.5 0.5 hrs, hrs, 1.0 1.0 hrs, hrs, 2.0hrs, 2.0 hrs, 4.0 4.0 hrs, hrs, 6.0 6.0 hrs hrs 1DigePsFtOFSi:ltered Supern6aatratnt=:6hrs J. THE: 4att=6hrs K SA: 4att=6hrs `Ship samples on dry ice to: Dave Ehresman, BS Toxicology Specialist 33MM CMeendtiecra,lBDueipltd.in/gCo2r3p6o-rCat1e46Toxicology PSahi:n6t5P1a-ul7,36M-8N41505144 tforrimaentahlyylsuirsiocfatchide,teasntdc1o,m3p-doiumnetdhyalnudritcheacpirdesfourmTedHEm,etgaebnotliistiecsa(c3i-dmfeotrhySlAx,anntohnienef,or1,3,7- PROS). 004438 4 T-6295.23; ST-46 Protocol. [ZT Data Analysis: Analytical results will be used to derive maximal flux rate in jig/hour/cm'. The flux rate. obtained for THE and SA will be comparedtothat reported in the paper byDoucet,et. al. Mass balance recovery should be 90+ 10%. MTT results will be used to determine if skin viability was affected (as compared to negative control) by application of the test compounds. Responsibilities: Kathy Thompson will be responsible for performing the experimeandt sending specimens for analysis; Dave Ehresman will be responsible for analytical evaluation of the samples. Kathy Thompsonwil draft afinal report and ensure the report receives appropriate. 3M review befor a final reporit issued, to be signed by Kathy Thompson and Dave Ehresman. References: Doucet, O., N. Garcia and L. Zastrow. Skin Culture Model: a Possible Alternative to the UseofExcised Human Skin for Assessing In Vitro Percutaneous Absorption. Toxicology in Vitro 12 (1998) 423-430. 04439 5 . T-6295.23; ST-46 Protocol. Signatures: 05/0400 | John Butenhoff, Ph.D. Date Senior Laboratory Manager Study Director Kathy Thompson, MP.H. Date Senior Toxicologist Study Toxicologist Sponsor Representative. Date 004440 6