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CONFIDENTIAL
DFT44S/985198
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ABIOTIC DEGRADATION: HYDROLYSIS AS A FUNCTION (PRELIM INARY TEST)
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KDD003174
Sponsor
:] DJCDaheucaePkmpsowonbnatetSrLespraWebcooiraralkttosyrCyhemicals NUJSA08023
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Research Laboratory ESIEHPuNyu2fenG3fotiL7lnkAPgXdNoDn Life Sciences Ltd DFirnaaflt:: 223FeDbercueamryb1e9r 919998
EID907 642
DPT445/985198 CONTENTS
Page COMPLIANCE WITH GOOD LABORATORY PRACTICE STANDARDS............................... 3 QUALITY ASSURANCE STATEMENT........................................................................................... 4 RESPONSIBLE PERSONNEL........................................................................................................ 5 SUMMARY............................................................................................................................................. 6 INTRODUCTION................................................................................................................................... 7 TEST SUBSTANCE............................................................................................................................... 8 METHODS.............................................................................................................................................. 9 RESULTS................................................................................................................................................. 11 DISCUSSION...............................................................................................................................................12 CONCLUSION.............................................................................................................................. 13
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EID907643
DPT445/985198
Huntingdon
Life Sciences
COMPLIANCE WITH GOOD LABORATORY PRACTICE STANDARDS
Hydrolysis as a Function of pH
TPrhaectsitcuedsytadnedscarridbseadnidnIthciosnrseidpeorrtthweadsactoangdeuncetreadteidntcoobmepvlaialindc.e with the follwihgGood Laboratory The UK Good Laboratory Practice Regulations 1997 (Statutory Instrument No 6S4). EC Council Directive 87/18/EEC of 18 December 1986 (Official Journal No L 15/29). OECD Principles of Good Laboratory Practice (as revised in 1997), ENV/MC/CHEM(98)17.
AHStu.unLdt.yinCDgodimroenbc,tLoBri.fSecS.,cPiehn.Dce.s Ltd.
Date
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Huntingdon
Life Sciences
QUALITY ASSURANCE STATEMENT
c
Hydrolysis as a Function of pH
The following have been inspected or audited in relation to this study
Study Phases Inspected
Date of Inspection
Date ofReporting
Protocol
18 August 1998
19August 1998
PHryodcreoslsysBisased Inspections 2 December 1998
3 December 1998
Report
IS January 1999
15 January 1999
PanrodtCocooml:pAannyaMudaintaogfetmheenptroastoicnodlicfoatretdhiasbsotvued.y was conducted and reported to the Study Director
Prcooruontdcineuescstaebndadasrneeddpreientipstoipvreetcetpdirotooncsea:dpupArretosoperrimaabtpeolouCytotemhdepotaninmtyheMitshatiynspasegtueomdfyestnwutadasysiwinnepdrriecoagctareerdrsisaebdinoosvupete..ctTiohnessaenwdearuedits of
cRoenpdourctteAduadnidt:reTphoirstreedptoortthheasSbtuedeynDauirdeictetodrbayndthCe oQmupalaintyyAMsasnuaragnecmeeDnteapsaritnmdeicnatt.eTd haibsoavued. it was
rTehseulmtsettohoredfsl,epcrtothceedruarwesdaantad. observations were found to be accurately described and the reported
DHPr.einpCcaoirmptmable,AnBtu.oSdifct.Qoru,ality Assurance, Huntingdon Life Sciences Ltd.
Date
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RESPONSIBLE PERSONNEL
c
Hydrolysis as a Function of pH
DPT445/985198
Huntingdon
Life Sciences
The following staffmember has reviewed this report
T(S.cCie.nCtiofwiclMyna,nEaugreCr,hPemro.d, uCc.tCChheamra.,cMter.Ris.aSt.iCon. , Eye)
The following staffmember was responsible for the conduct ofthe work and reporting of the results. P(S.cWieonotidsst,, PHr.oNd.uCc.t Characterisation)
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The hydrolysis
3 SUMMARY as a function of pH was studied according to EEC guidelines.
Threahpdereopscreecnluitrmarteiivndea, reoyqfusttihuvedalyeennsvhtiotroownhemadleft-nhltaif(te2a5tfitmeCre)5.s d(ta%y)soaftgprHea4te,r7thaanndo9naenyde5a0r uCndleersscothnadniti1o0n%s mhyodrreolysis
c jwasfound to be hydrolytically stable under acidic, neutral and basic conditions.
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INTRODUCTION
TfuhnectpiounrpoofsepHo.f this series of tests was to investigate the hydrolytic behaviour o '------ ------Z------ r1 a
Tanhdettheestrewqausirceomnednutcstoedf thine aAcncnoerdxatnocEeuwroitpheathneCOomECmDissGiounidDeilriencetsivfeor92T/e6s9t/iEngECo.f Chemicals (1981)
TSphoenpsorortoonco1l7wJualsy a1p9p9r8oavnedd bbyythHeuSnttuindgydDonireLctiofer oSnci1e3nAceusguMsat n1a9g9e8m. ent on 7 July 1998, by the
The experimental phase of the study was undertaken between 9 November 1998 and 27 November 1998.
Location of study
: HEIESPuynu2efgn3fltoai7lnnkPgdXdon Life Sciences Ltd
PstroimreadriyndtahteaafrrcohmivtehseotfeHstsunpteinrfgodromneLdiafet HScuinetnincgesd.on Life Sciences and a copy of the final repourtoare';
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Identity: Chemical name:
Intended use: Appearance: Storage conditions: Lot number: Expiry date: Purity: Date received:
TEST SUBSTANCE
DPT445/985198
Sfluurofraocmtaonntoinmtehres polymerisation of Pale yellow slurry Room temperature 3 2 years from date of receipt 25% 23 June 1998
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METHODS
DPT445/985198
PRELIMINARY INVESTIGATION Preparation of buffer solutions Buffer solutions were prepared using the following volumes: pH 4.0 : (wD1ii2tsh.o9dpgiuu)rmiwfieehrdyedwdraoistgeseorn.lvoerdthionpphuorsipfiheadtewdaotedre(c1a9h0y0drmatle).(T2h7e.6vgo)luamnde wciatrsicadajcuisdtemd otono2h0y0d0ramtel pH 7.0 : Ph1yoMdtarsossocidhuilmuomrdicihhayycdiddrro.ogxTeihdneeovr(to3hl0oupmmheol)swpwahsaataseda(j6ud.sd8tee1ddgta)onw2da0s0th0deimssploHwlviewthdapisnuapridufjirueifdsiteewddawtteoar.te7r.0(19w0i0thm1l)M, pH 9.0 : D(13Mi.s6o0hdyigdu)rmowcteherlteorardbiicossaroactlievd.eddeTcihanehpyvudorrliauftimeede(3ww3.aa1stegar)d(ja1un9sdt0e0pdomttoals)2s0aiun0m0d mtdhilehwypdiHtrhowgpeuansriofairdetjdhuowspteahdtoesrtp.oh9a.t0e with The pH of the buffer solutions were measured using a pH meter.
PROCEDURE ps2fArseeau4l0laeamb.ica0gqstpene5etuadldsnoinotnttic1tsfgbnee2tomw,h(0at1etipaht0lhheseoi0enseruratrecrmpemtqsounHulo(rnd)s5eisetrtaoedwdoaidfatfnapiyc(seiHtasnhaam)flcgeo)tlha.eyfri^rnTtecbhsstohuhaeuneifolntrftrrweieetonsrdailpgnl.tseeecoscdruoltbubiwl|vuataiea(tttohiaitoobnepwnnurp(sfabrppfosaeewrxtrermh.eiivomroTiaedonahtuiotea5tesodf0bllryjyaouepCt1dsetpt8lqeride0noudsuximrflwwiieimngbeeig)rtra.ahdetfDtaeeepr1leduyukMepr.1agetT0teorshidom5otedh0wdyiienuoiCwufmafe)tceefinreswhdei,eyitecarhdtroneenergdolsadetxmttnutihaode,reteaesne5seonut0aaosfrlfuteetChewrddeeruit2tiatnhhne.nt4aitsidno,ltt The test was performed in duplicate at each pH value. A((a16ctemmteoalln)c)ihtoarnifsldafeem. e0Tp.h2slaieMnmfgipantlqaiemulsesewooulpeusorteirsotoipnodispniwuestmet(er1deh0tyihmndetrlnoo)xasoinedfapelfayer(sae0et.edt5eb1smyt0lsim)oownlluvcetihoroerlnuoasmmdwaedtteeordirgcerbafrepleafhmosykro.esv, edtdoiluawtnihndigcchtooopluverodilf.uieAmdleiwqwuaoitfetesr The pH values offee solutions were measured over fee period offee test.
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ION CHROMATOGRAPHY CONDITIONS
Instrument:
DDPieoiornkneiexnx-GEPPlEm4D0e-rP2IuSPmSupl2s0ed0 EAluetcotsroamchpelmerical Detector Dionex ASRS-II Membrane Suppressor
Column:
PLRP-S (25 cm x 4.6 mm internal diameter)
Column temperature:
Ambient
Mobile phase composition:
AanqdueImouMs ssoolduiutimoncacrobnotnaaintein/ gace2tmonMitrialem(m75o:n2i5umv/vh)ydroxide
Regenerant solution
50mN aqueous sulphuric acid
Flow rate:
1ml/min
Injection volume:
100 pi
Detector:
Conductivity mode
Retention time:
Approximately 6 minutes
The peak observed at 6 minutes corresponds to the perfluorohexylethy1sulphonate ion which, from ilcneovfmoerlpsmoanotefinotnI"o"snulyp.plied by t)hien Sthpoenwsoart,erresporelusbeniltisty9t2es%t soamf tphleesacwtiivllebiengqrueadnietHinfUitetfCdvsorr*nesflmaetq'ifuv' eenttolytthhies
PREPARATION OF CALIBRATION
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CALCULATIONS
t ,a *> f
The concentrations of
Z 3 in the analysed solutions (CA) were calculated from standards
introduced before and after samples (bracketing standards) by the following equation:
CA(mg/l) =
sample peak area x standard concentration (mg/1) mean peak area of bracketing standards
The concentrations of} equation:
tn the test solutions (C,) were calculated from the following
Ct(mg/1) = CA(mg/1) x dilution factor
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