Document MGqGZogK8KMeDoDeRXqRVomna
Co
T5T9-7S7E.._Y +T%h BBAACCKKTTOONMAIN
SSRRPPTT
RREEPPOORRTT
OETERNINATION
DETERMINATION
OF
OF
THE
THE
PARTITION
PARTITION
COEFFICIENT
COEFFICIENT
(N-OCTANOL/WATER)
(N-OCTANOLIWATER)
OOFF
T-5674
T-5874
BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC)
BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC)
HWNOOOTTTOOOXXX sPPurrboosjjteeaccnttce11223118221778557
NOTOX substance 38187
- Page 1of 14 Page 1 of 14 -
22779933..00000011
RECEIVED
Viv:fi~, a-99a.s..e..
TOAILULOGYY
I EEx;;hiigbl~iitt 2793
]
3M _MMNN0011553322223355
----EE ------------------------ BACK TO MAIN
vse Noro praject 121275 T-5874
NOTOX Project 121275
steven oF cir comme STATEMENT OF GLP COMPLIANCE HOTOX 6.1, *s-tertageniose, The etherlanss
NOTOX B.V., 's-Hertogenbosch, The Netherlands
Th Stuy described in this report xa condistd fn compar ith the The study described in this report was conducted in compliance with the mn most recent edition of: The 62D Prinptes of Good Laboratory Practice The OECD Principles of Good Laboratory Practice whic are sssantatty in conoraity with: which are essentially in conformity with: The nia States ond ard bug Agestration. Tite 21 Gate of Federal The United States Food and Drug Administration. Title 21 Code of Federal Teams rare Regulations Part 58. The nites states viranmentel Protection Ager (FIT). Title 40 code The United States Environmental Protection Agency (FIFRA). Title 40 Code Srna negsiations Fore 18 of Federal Regulations Part 160. The United States Evicammental Protection Agency (TSC). Title 40 Code of The United States Environmental Protection Agency (TSCA). Title 40 Code of Fr regain Fart 79 Federal Regulations Part 792.
stay otvestr:
Study Director:
os. 8. de Vries Drs. R. de Vries bates ee in
eer Page 2 -
22779933..00000022
aunorsszss 3M MN01532236
TT-55087744
~_BACKTOMAIN BACK TO MAIN
NOTOK Project 121275
NOTOX Pro~ect 121275
QUALITY ASSURANCE STATEMENT
QUALITY ASSURANCE STATEMENT
NOTOX 8.V., *s-Hertogenbosch, The Netherlands,
NOTOX B.V., 's-Hertogenbosch, The Netherlands.
SSStttuuudddyyy pspprreoocccieeddfuuirrceessprwowecereresesesssuubbvjjeeecrctet attloosoppeerriiinoosddpiiecccteiidnnssappteeccpttiieoornnissodiaacnndd iggneetnneeerrrvaaallls.nnoonn
study specific processes were also inspected at periodic intervals.
TmThehitishsodrrseeppooarrnttd wwraaesssualautusddiittaeecddcurbbyaytettlhhyee NNrOeOTfTOlOXeXctQQuuaatllhiiettyyraAAssssdauutrraaa.nnccee UUnniitt aanndd tthhee
methods and results accurately reflect the raw data.
DDAATTEESS OOFFAGQUAADUUITSIINNSSPPEECCTTIIOONNSS/! AUDITS
RREEPPOORRTTIINNGG DDAATTEESS
2255 MMaarrcchh 11999944
2255 MMaarrcchh 11999944
28 Maren 1994
28 March 1994
.
28 March 1994
28 March 1994
2201 Aapprriinl 1199994
20 prin 199
21 April 1994
Quanity Assurance Manager
Quality Assurance Manager
C0. Mitchel 8.5c.
C.J. Mitchell B.Sc.
DDaatete:: OA ok Gy
- rages Page 3 22779933..00000033
3M _MMNN0011553322223577
--
TT--55887744
REPORT APPROVAL
REPORT APPROVAL
STUDY DIRECTOR:
STUDY DIRECTOR"
HANAGENENT:
MANAGEMENT:
ackmomaw
BACK TO MAIN
NNOOTTOOXX PPrroojjeecctt 112211227755
ors. R. de Vries
Drs. R. de Vries
da 1 -
Xe--
Date: Spe 9. wan
JS3.eAAcM.tHiN.o.Wn. hevvaaadnn HHPeehllyvvsooiiicrrottChemistry
Section head Physico Chemistry
Nn
PP:
\
Or. Tona C. Enninga.
--
I~Tre. cIhlonnicaaCl. DEirnencitnogra
Technical Director
ote:oglob lggu
- paged Page 4 22779933..00000044
33M uMNN0011S53322223388
TT T-Ts-5887744
BACK TOMAN
BACK TO MAIN
NNOOTTOOXX PPrroojjeecctt 112211227755
PPRREEFFAACCEE. SSppoonnssoorr
SSttuuddyy MMoonniittoorr TTeessttiinngg FFaacciilliittyy
SSttuuddyy DDiirreeccttoorr SSttuuddyy ppllaann
TTEESSTT SSUUBBSSTTAANNCCEE
IIddeennttiiffiiccaattiioonn DeDsesccrriippttiioonn BaBattcchh PuPurriittyy SSttoorraaggee ccoonnddiittiioonnss coSSnttaadbbiiitlliiiottnyysuunnddeerr ssttoorraaggee
conditions
EExxppiirryy ddaattee
33CMManBBaeedllaggsiiturumanat-- CC11hheemmiiccaall EEBCC 8BCE--ae22nl00ga77id00uanstZZrNWaTIaIOtNNODRRiEEiCCHHTT
Belgium
MMrr.. RR.HH.. CCooxx NNHOOaTTnOObXXaBBk..eVVn..vetienrg 3 5H5T22ha33em11baNk0eDDeDtnhwe'*ersstl--eaHHrneeidrrnsttgoogg3eennbboosscchh
The Netherlands
Oorrss.. RR.. ddee VVrriieess SCStotamarprtlt:"ete33d00: MMa0ar7rcchhApr11i99l99441994
Completed: 07 April 1994
TT-55887744 CCrreeaamn ssoolliidd 223334 110000%8 AAtt rroooom tteemmppeerraattuurree iinn tthhee ddaarrkk
sSttaabbllee JJaannuuaarryy 0011,, 11999966
- Ppaaggees5 -22779933..00000055
I3MM_MMNND011553322223399
TT T-Ts-5887744
_BBACAKCKTTOOMMAAINN | NNOOTTOOXX PPrroojjeecctt 112211227755
PPUURRPPOOSSEE AANNDD PPRRIINNCCIIPPLLEE
TTthheeestppuusrruppboosssteeancooeff btthheeetwessettnuuddyyn-owwcaatssanttoool ddeeatntdeerrmmwiiantneeer.tthhee ppaarrttiittiioonn ccooeeffffiicciieenntt ooff tthhee
test substance between n-octanol and water.
TTohhfeethppeaarrtteiiqttuiiioolnnibccrooieeuffaffiicccoiineecnnettntr((annt--ioooccnttsaannooilln//wvaaattteewrro))ph((aPPsoouwe)) syiisssteddmeeffiicnnoeenddsisaatssinttghheeofrraattiioo onnf--ooccttthaaennooellquaiannlddibwwraaittueemrr..concentrations in a two phase system consisting of
TT1hhieequirrdeettCeehnnttriiooornnatottgiimrmeaepnooyff aa(HPssLuuCbb)ssttaacnnhccreeomaiitnnogaararrpeehvvieecrrsseesddy--sppthheaasseeisHHiirggehhlaPtPeeedrrffootrrommaainntcscee
pTplhaaierrqttuiiiHdttPiiLooCnnhmrceocotmoehaeftoffodfigicrciiaispeehnnuyttsef(((uHnnlP--LooCccf)totaranncoohTllro/lgovwmaaaPtttoeeoyrrg))r.v.aaplhuiesc
system is
between 0
related
and 6.
to
its
TURUhssueiisnntggHPaLlttCshhoeembHeHePPtLLhCCoadpmpmeleititshheoodudds,,eiffuiilmtmhppeuufrorriittteiisleetossgsPaaurorbewestaoovfnfacleummeiisnnioosrrbeatfiwmsmeippoxeorrtnttuaar0nneccaeeno..df 6TcT.hhoeempoHHuPPnLLCdCsmmbeeuttthhoodd
wmiIshussitcnnhoottalrsaaeopapcpptlbleiiwcciaaatbpbhlpleleitethtdooe sesiftltruroeotnnnhgtge aotarcecsiitddsssursafaunnabddcseta-bbnaaascsceeetssi,,viesmmeeaattgaaemllnitxstcc.uoormmepplleeoxxfeessc,,ompssouuubbnssdttsaannccbeeusst
which react with the eluent or surface-active agents.
GGUUIIDDEELLIINNEESS
TgThuheeidesslttiuunddeyys:pprroocceedduurree ddeessccrriibbeedd iinn tthhiiss rreeppoorrtt wwaass bbaasseedd oonn tthhee ffoolllloowwiinngg
guidelines:
OGOrurgigad~nepilizizanatetiioofnnor ffooTrrestEEiccnoognnoomomiifccChCCeoom--ioocppaeelrrsaa,ttiioognnuiadanendldinDDeeevvneeoll.ooppmm11ee7nn:tt ("(OPOEEaCCrODt))i,,tioOOnEECCDD cGc(ouoHeiePfdfLeff)liiiccniimeeeenntthtfoodr(("nnT--eoo(sccatttdaiaonnnpogotlel/dlowwfaaMttaCeerhrrce))mhicHH3ai0il,ggshh,1P9P8gee9urr)iff.dooerrlmmiaannnecceenoLL.iiqquu1i1i7dd: CChh"rrPooammraatttiootgigorrnaapphhyy
(HPLC) method" (adopted March 30, 1989).
EAE,uurrooMppeeetaahnnodsEEccoofnnoroommiitccheCCdooemmtmmeuurnnaiiittnyyat((iEEoEECCn)),,ofEEEEpCCh-y-DsOiiicrroee-ccctthiievvmeeic99a22l//6699proEEEpECCe,,rtiAAennsnn,eexxAV.V,,: PPaarrtt A"",PPaaMrretttiihttoiidoosnn ccfoooreefffftiihcceiieednnettt".e.rmiEEnEEaCCtiPPouunbbllioicfcaattpiihooynnsicnnooo..-chLLe33m88i33,,calDDeeccpeersmobbpeeerrrti11e99s99,32.. A.8:
AARRCCHHIIVVIINNGG
pNNrOOoTTtOOoXXcoBBl..V,V.. rwweiipllollrt,aarrccthehsiitvveesuttbhhseetaffnoocllelloowwriiennfggerdedanatctaea fsfooarrmplaaett allneedaassttraw1i00dayyteeaaa.rrss":
protocol, report, test substance reference sample and raw data.
TTEESSTT SSYYSSTTEEMM AANNDD RRAATTIIOONNAALLEE
ATAheHHiiggshhtatPPieeorrnffoaorrrmymaannpccheeaseLLiiwqqauusiiddbCoChnhrdroeomdmaattsooigglrriaacppahhCiwwgii.tthh Thaae ssmppoeebccittlrreoopphhpoohttaosomeseettwrreiiscc7d5de/et2te5eccttoorr..
dT((hevv~/s/vvc))rsitbaaaetccdieetotonoinannirityttrrhiiepllheeas//sevwecaatttiweeoarrns..
b"BoBmoonettdthhehdodHHPPsLLioCClficciiahnnessmCtti1rr8cuu.amnleenTnhtateaanttaiimloooynnbsiilaasenn.dd
phcaosnediwtaisons75/a2r5e conditions are
described in the section "method of chemical analysis".
TThhee tteesstt ssyysstteema wwaass rreeccooggnniizzeedd bbyy tthhee iinntteerrnnaattiioonnaall gguuiiddeelliinneess ((OOEECCDD,, EEEECC))..
-o -- pPaaggees6 -22779933..00000066
I3MM_MMNND011553322224400
on
_BackTomam BACK TO MAIN ron re NOTOX Project 121275
-- REFERENCE SUBSTANCES or seesor ve ee eterrseer3 $s duimloats for ani Jalan seth repirtud vars yaad vo line, Six chemicals for which log Pow has been reported were used to calibrate Ee the elution time in units of log Pow- The mixture of reference substances
consisted of:
formemee Twa Reference substance Bra - benzylalcohol (p.a., Merck) EERE -- ttoolluueennee ((pp..aa..,, MMeerrcckk)) RR i - 1,4-dichlorobenzene (z.s., Merck) Br ii - fluoranthene (98%, GC, Aldrich Chemic) EE eT - dibenzyl (99%, GC, Aldrich Chemie) | - 2,4-DDT (99%, HPLC, Riedel de Hahn, Se~Ize, FRG) a ---------- log Pow values according to the OECD guldellne.
log PowI
1.1
22..77
3.4 4.7 4.8 6.2
renc1 e PERFORMANCE OF THE TEST
rent on Preparation of the solutions pommern Solutions of the reference substances (except for ethylmethylketone) were Ty prepared in methanol (HPLC-grade, Labscan Limited Co., Dublin, Ireland) at a SpET ES concentration of 1.5-2 g/l. A mixture of the reference s~Yostances was S Eh E ahr iS :STtEn prepared by adding 125 ~l of each solution to a volumetric flask.
Subsequently, this flask was made up with mobile phase to a final volume of
LBOe atest1 tretio 1 sme capo 25.0 ml.
For the determination of to (retention time of the unretarded component), a
Fr ser of to ni or ei omen solution of formamide (p.a., Merck, Darmstadt, FRG) in methanol was prepared Trt I Bar BT at a concentration of 1.7 g/l and thereafter diluted i0 times with mobile gicphase. B rssweenr of tooo 5 ctsone A stock solution of T-5874 was prepared by dissolving 165 mg test substance iSp t EiRoIr oStSpAreLtnsSnS1 Bi in 50.0 ml acetonitrile (3 minutes sonication). The stock solution was
diluted 10 times with mobile phase, resulting in the test solution.
etor not Performance of the test ee oe se nt.frensepa 2 me 1 The solutions were injected in the following sequence: the mixture of Ii ne te tobe rs semen st reference substances, mobile phase, the Formamide solution, the test Sts I SE TRL solution (in duplicate), mobile phase, the mixture of reference substances SES and the formamide solution. ennmoar Temperature of measurement ere otest i a nr es ig The temperature of the mobile phase was recorded several times during the me measurements.
Cr Page 7 -
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22779933..00000077
T-s87a
T-5874
----
B_AeCaKckTTOoMmAaInN
NNoOTTOOXX PPrroojjeecctt 112211227755
HMEETTHHOODD OOFF CCHHEEMMIICCAALL AAWNAALLYYSSIISS
TTahrheee
ccdoeonsndcdriiittbiieoodnnssbueulssoeewdd: ffoorr
tthhee
HHiigghh
PPeerrffoorrmmaannccee
LLiiqquuiidd
Chromatographic
Chromatographic
method
method
are described below:
Aannaallyyssitss
coCtoluummnn MMoobbiillee pphhaassee
FlFDleootwwection DIIenntjjeeeccctttiiiooonnn vvoolluummee
LGLyiieCChhrr5oossuppnhhee(rrMeri1c00k00, RRPDP--a11r88m;;sta11d22t55, xxFA44G)((1I..DD..)) d7L8D~i11=n22i555te~d((mvv//Cvvo()).M,eraacDcckuee,bttlooiDnnnaii,rttmrrsiiItllraeeedlt((a,HHnPPdLLF)CRC/G--i)gglrrlaaidde-e,,g L(1(iHMmmiii1lit1leniidpptoorrCoee.,CCoorDrpup.b.,linBB,eeddffIoorrreddl,,andMMAA),,IMiUUlSSlAA))i-Q WU11V0amlawtltlmiAXn== 221100 nmmn
i0 ul
mmma;; wLLaaatbbessrccaann
water
IInnssttrruumseennttaattiioonn
AHHuPPtLLoCCsaPPmuupmmlpper DAeutteocstaomrpler
Detector
IInntteeggrraattoorr
SS1ee5rr5ii-ee2ss004411(00PeLLrCCkin((PPEeelrrnkkeiirnn) EEllmmeerr,, NNoorrwwaallkk,, CCTT,, UUSSAA)) SBISepSpaeSecc-cht2t,0rroooMkFooL(,nnPiiettrUookSrrAi)n3311E0l0m00er(()LLODCC AAnnaallyyttiiccaall,, RRiivviieerraa SBSPpeac44h22,9900FL((,S$ppUeeSccAtt)rraa PPhhyyssiiccss,, SSaann JJoossee,, CCAA,, UUSSAA))
DDAATTAA HHAANNDDLLIINNGG
UUvssaiilnnuggesHHiicggahhn PbPeeerrffaoocrrcmmuaarnnaccteeelyLLiidqqeuutiieddrsCCihhnrreoodmmaafttroooggrrnaappthhhyye,, cehesrsppoeemccaiitaaollgllryyaphlliaacrrggeeret1l0oeggntPPiooowyn data. vTTtooahleuttehphsiiassrctaieennntddi,,obenttahhceecoecfuccfraaiappctaaiecceliinytttyy.deFftaaTecchrtetoomrricnaep((dkak''c))iFtrowywmaassftahuucessteeoddrc,,hrwosassmiinancctceeoaglrciiattuplhaiiitsscedpprrrooefpptroooerrnntttiiitooohnnneaalldatttaoo. trrheeetteenpnttaiirootnnitoiofofntthcheeoefssfuuibbcssitteaannntcc.ee cTchooenncceecrrannpeeadcdit((yttr;))Faacantndodr tthhweeasuunncrraeelttcaaurlrdadetededdccoofnmrppomoonneetnnhtte ((ttoo)):: Kk == ((ttre -- ttoo)Iltlo vFFerrroosmnustthheeTogrreekss'gylltt_ss(y-oovffalttuheh)ee wrraeesffeerrcoeennnsccteerusscuutbbessdtt,aannccueesssi,,ngaalpiplnleooattr ooffregl1or0ggessPPoyoiwon((axxn--avvlaayllsuuiees)). TvTthheheeresuloTsooggglokkk',,g kvvvaaallluuu(eeeys-ovofafolfueeeaat)cchhhewaccrsooemmfppceooornnneeesnnntcrtteucosotffuebdstt,thhaeenucstteieesnssgttwissltuiuhbnbessattkraannnoccwreenegvwr1aae0sssgsiPccoooonysmppaavarraneealldudyesswwiiistt.hh
the logk values of the reference substances with known log Pow values.
- Ppaaggees8 -22779933..00000088
I3MM MMN0N105153322224422
TTT" BACKTOMAN |
BACK TO MAIN
TT-55687744
NOTOK
NOTOX
Project
Project
112211227755
RREESSUULLTTSS
RRpehepapsrreee)ss,eennttathatetiivvmeeixtHHuPPrLLCeC ccohfhrroormneafatetoorggernracamensssouofbfsttthahenecettesesstatndssooltluuhtetiioofnno,,rnatthsheeidebbllaasnnok-kl~ut((mimooobnbiilaleere
shown in Figures 1 to 4. phase), the mixture of reference
shown in Figures 1 to 4.
substances
and
the
formamide
solution
are
IIpnneaktthheeatHHP4PL.LCC1 ccmhihrnrouomtmeaasttooggarrnaadmmssa oosfmfalTT]--5588p7e74a4,k, uuatssiinn7gg.7ddemetitenecucttteiiosonnwesartte2211o00bsennrmm,v,edoo.nneeBellatarwrgegeeen
p11t.he.66eakaalnnaaddrtge444 .1m mpieinamnukuitnteedusset,er, sisvseeeavdnvederfraaralol nssm snmtaahallellll mpaeppjaeeoakarkkssactwowes7erp.r7eeoneomonbbitsnseuerortvevfeesddt.w.eseTtIrettsvuwoabbassssteaaarnvsssecsueudmm. weehddBeertttwhehaeaaesttn
thethe
the
snall(er) peaks derived large peak derived from
small(er) peaks derived
fron impurities. the major component
from impurities.
of
test
substance
whereas
TTnhheeeastuto,fenvwaeasnstsddeet(teeir.rmesiinnee0dd.89ttooanbbdee 000...999000 mmmiiinnnuuuttteeesss).aass aa mmeeaann vvaalluuee ooff bbootthh
measurements (i.e 0.89 and 0.90 minutes).
TT1hh0eeg mPmoyeeaannavnvdaalluuPeeossy ovofaflutthehese,arrreeetteesnnuttiaiononanrittizimmeeedss,,inkk'T' abvvlaaelluuee1s.s,, Thlloeoggplkk'o' tvvaoalfluueelsso,g, Poy
Figure 5. l((oxxg--vvaaPfelluwlee))andvveerPrsSouwlss
Tog k' values log k'
ar((eyy--vsvaualmluumee)a) rizffrerodomn
intthheeTarrbeeleffeerrle.ennccTeehe
ssuupbblosstttaannoccfeesslogi1ss
PSoswhhoowwnn
iinn
Figure 5.
[mm Tw[T[a mmm]r 7a] TTaabbllee 11 RReessuullttss ooff tthhee tteesstt..
Substance
trZ
k'
log k'
log Pow
Pow
bbteoenlnzuzyeynlleaallccoohhooll
1r2.i21e4 || o1zs 0.274 || -oo0.s5m6e3 || 12i.a7i
1Ft1lo,aul4-ou-dredianicenchthihloeornrosobbeennzzeennee | 222s..0e288499 ||
1.503
2s22a9 2.229
||
o000..331m47887 ||
a323..y474
d2dfiil4bbu-eeo0nnr0zza1yyn!lthene
54sa..ao60zr77 ||
5.330
sesoo 3.547
||
oo00..ds75e25os70 ||
e44a..zs78
2,4-DDT
9.12
9.190
0.963
6.2
ptteeeassktt ss1uubbssttaannccee
7.00 | 7.5 | osm | se: |
pppseeeeaaavkkkera22il ((msmmaaajjloolrr cpcooemmappk..s)) |[1744....6700/5054 [0.37735.]..5552293558.47|-00.100..0.558/4480771.54|2.27a544...4644 + |
several small peaks 1.6/4 0.79/ 3.47 -0.1010.54 2.2/4.4
L aMetan ecatuesortthe tcoetenrtieenpttheiesloef boythbchocotmtogeaSnsD (520.972, et) *
Mean value of the retention tlmes of both chromatograms.
=
Interpolated from the regression line: y = 0.28B~ - 0.730 (r=0.972, n=6)
Note : The calculations were performed using not rounded values.
39.8 aot 39221....8555110xxx1i1l000O24447 2.5104 1.50xi02/
2.51xi04
The temperature of the mobile phase vas 20.2-20.6C during the measurements.
The temperature of the mobile phase was 20.2-20.6C during the measurements.
- PPaaggees9 -22779933..00000099
_3MMNMON105135232224433
-- T3874
T-~874
CHRMNEL RB
CHRt-!NEL A
_ _BBACaKckTTOoMmAaIwN NOTOX Project 121275
NOTOX Pro~ect 121275
TWIECT a7-nd-a agiadiSS STORED T0 BIN 4 52
= shit,
~
" " :~ -
4o R5
68 ~ 7.~9
DATA SAVED TO xTH o 53
381367121206 38196/!'2i 286 FILE 1 METHOD B. FiLE suaLveTs Kan R,NRL'-..--':_=.:T : KRH
peace: Re495 mma1s i 2 Zi ms 2 3 De al 3: PoaETh Em .~ 33 f2i8e ITME 6 ? EOIN 7 : REET 8 : LE nh 9 5 SEDonh i~ a ni LY it i De iE i 2 i LAE Nl ~~ --:_. 1 anas Nm 14 ioEwEd aLkR 4~ 3 Tee ma 17
re aes TFjT ~ :'_
E~. 49=, 2. 459
!. @83: 4 ....-,-., :
2. r5 .R;R
@. ,~6F_-: ._--" 476
i. 977
q~. 6_--.:6 i. ;:=.64 - ...... ~ ......
ii. 2-_:2
q~:'. -":=,'.:~ 2. 914
196.
@. "15 ~. 2.5
;:~. 34 ~4. =..-.:-
"~. ~-!"i &. ~:,~ "_:... ~
!.. 7 i i. 9J
--_'. !:7
_-'.:. 19 -'.:. ~!
4 r.:=. 7. 69
A7-nd4-2a Areas
WN 10 (!7-.C-14-94
RS: 44;
INDEX
._=.'5
10
ssmmesmse J -:::99 gem ee b~._,i ~' Saar -:..:~-_Rt ~2 sues 5--.:I't 9 OSCHEaRR 7!75 ow i .'3::::'::" mane 7;-'IR_~__ '-'~'-",., Gear r~-=,:::8 @:2 BRE i7'37 @_-.: naa --.-:26'8 92 Gsteaaat ~ '-',:, ._, -'-, vem -..-.,.., ?=r._..,,0 EusRsEm 1~!RTF!7 TREE 5694 zszess 2 .::_:2665
Che TRY PSsF'S= i. CH= "A" sm 53
B i H
FFiigguurree
11 THHP-PL5LCC674cchhrrionommnaaottbooigglrreaamnphooaffsett.hhee tteesstt ssoolluuttiioonn ooff 333300 mmgg/lll T-5874 in mobile phase.
CoHCloobluiumlmnen phase DeMFFtolleobowwiclteiopnhase DIIenntjjeeeccctttiiiooonnn vvoolluummee
tL7i5iC/Ch2hr5rooss(ppvhhiever)r
1ai00c00etoRRPnP--i11t88r;;ile11/22N55ixkl41i((-I10..0D..v))atemmr8m;;
dpe
dp=5
un
um
711Ww5,a/m2ll5//atmmii(nnxv/v)21a0cemtmonitrile/Milli-Q water
UV1,0'1at ~ = 210 nm
i0 ul
onNtTohterteee:e:bbalaTaTtuhnhmeekapp((eeosaatenkkeess FFbcbiheeggtutureweeeeeeeenn23))..00
aaTnnrdcee11f..o66ceemiinnIuuttevesassewaesrveesosaaelldssaotohobabstseerrtvvheeeddseidnnpetthhoee
Therefore It was assumed that these peaks
cechhhorroommmaatttooggBrraaLnmssYooff
did not derive
from the test substance.
n
- PPaaggee i100 --
S3M_MNMON105135322224444
22779933..00001100
_-- T-5074
T-5874
BBAACCKK TTOO MMAAIINN NNOOTTOOXX PPrroojjeecctt 1122112277~5
CHANNEL A
INJECT 67-04-54 ASit4:a4 STORED TO BIN 8 56 :::TFiPED TO BIN ~ 5~
r
DATA SAVED TO BIN #56wERe0
DRTR SS'4EB TO BIN # 55
8138/121286 FILE 4. METHOD e.
METHOD ~._
RHRLYST: KRH
07-4-4 03:34:04 ~I,7-04-94 _4'~: _-<4:84
RUN 43 INDEX 13 RUN iS:
i !4 i} E ',---', !S
EI $1dasDLEesEz P 5: w 7S7aa 3faa2383
TAL see.
RRTT ema ne amaas sfaww amna vceimoa mafaaern cp gaassaeasr YH SRW
seaze
CHe CR
CH=
PS=
F'S=
1.
eBinN s5e@
FFiigguurree 22 HHPPLLCC cchhrroommaattooggrraamm ooff aa bbllaannkk ((mmoobbiillee pphhaassee)).
CMCooolbluiumlmne phase
FplMFeo1otboewwiclteiopnhase
Injection Detection
Injection
vvoolluumsee
7LLi5iCc/h2hr5rooss(ppvhh/ever)r
ai10c000etRoRPnP-i-1t18r8;i; le11/22M55xix44lNi((-l1.q.O0.w.))atemmrnm;;
dge5
dp=5
um
#m
7LU1W5m.m//2l5na/mti(innvx /v=)
2
aceton~trile/Milli-~
10 nn
water
10UV,
10
ulat
~I
X
:
210
nm
- PPaagge eIlI -22779933..00001111
I3MM MMNON105153322224455
EE
Tsar T-5874
BBACAKTTOC OMMAK AIINN |
HOTOX Project 121275
NOTOX Project 121275
CHANEL B INJEST @7-ge-as asia? STORED T0 BIN #57
CH@HNEL 8
=
9 l-':-
DATA SAVED TO BINeEP#.o50 7
:
3ATR SRVED TO BIN #
FsIaLuEss/1521zs6 METOD 5 RN7-p4es-3s FILE 1,
HETH09
AHELVST: KRM ANALY'._--;T : KRH
~7-04-94
[EO1 sm nBaTe avemra ac
@, 822--
~, 14
-! -i.g& 82
3 ois 83 rane 2
@, 145
-'.-3, 2..=,.
78~:9
5i e FETS2245FE are 4
a $79
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~'-.~., 7'9
3542
g wim WE Seas E,
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6771
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',:J, ~77
i, -~ ~
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: siz UE Siam :9
G. 1"_'. :---'
1= 6-i
54.,.-..(~
Poi ph uaa 9
~...44 3: & 7
9. :-:, 4 ~-~ ~-~ ~-3 ~: 4 i~,
3 San ph Tm ! -'-_-~
O. '-- ....
:2. ~ 4
= -* -~ ~--<_'~
ogee RE mand i i
-; n ....!~ =
2, ,:= '-' ........
G0 sss sa mind 12
i5..=_,24
4. ~.-::.~ ~-~:-'::-'~:--.:4 ~i
#0 BE gd anna 4 -..-"
-.-',--, ~,, -'~
4 ':"~-"~'-.',:i
i g3E 23 ida 14
~-3, --.--~ ~
g ~~:;
1.~---:~i
RLman seei NE sSanmea 15
i]:, 272
9, !g ~4577@
9isaIlr Tame 16 89:58"-17
-
cHe tRT F_:H= "R"
PSs 1. omPS: 5
FFiigguurree 33 HHphPPaLLsCCe.cchhrroommaattooggrraamm ooff tthhee mmiixxttuurree ooff rreeffeerreennccee ssuubbssttaanncceess iinn mmoobbiillee phase.
NCCoooblliuulmmenn phase DeMFFtolloebowiwclteiopnhase DIIenntjjeeeccctttiiiooonnn vvoolluummee
L7L5ii/CC2hh5rrooss(ppvhhieev)rr 1ai00c00etaRRnPP--i11t88r;;ile11/22M55ixx1441i((-1I0..D0..v))ateamrmn;; ddpe=55 uumm W7iL5a/aml2l5t//mmii(nnv/v=) 21a0centaonitr~le/Milli-g water UiV01,0"uulat ~ = 210 nm
- rPaaggee 1122 -22779933..00001122
. _MNO1532248
3M MN01532246
T5674
T-5874
--------
B_sAaCcKkTTOomMaAmINn
NOTOK
NOTO
Project
Project
112211227755
CHANNEL A DWISST 07-ad-q4 A7iI7ied STORED TO SIN 8 43 :=TrI-|F:EEI TO BIN # 49
hor
Ta 207
-
65
DATA
I~RTFi
S...A.. VvE~D
TO
BIN
BIH
+
#
43
49
'TI-I
seFaIsLE6/1121236 meme r ILE io
METHOTj
NRLVSTS KR 8NSLVST: KRH
cence mean PESK#
8RE8~
13 0T.i3k3e 2
1. 189
3 5.73 3:
6.7'_-3."
4 amas 4
IEL 44
: V%8s 5
&.c='-,',,_,..,.,
sisi ~
54, =._, ~-," ,'-3'
$ sae 7
6. 24#_',
gi FfEiT 9
-_'.1 H-'--." 4
TeI3 weem,ealsss -i#t
A .4.::~
7-naas g7iizies Gee RY PER 4 .17-~4-'.q. 4 [~7:-<7:43 " " -|~.H= ;;~" F':~= ~ "
eR 6 MEX Bin as RUN
~
I NI~EX
6
B i N 49
BT meee
RT
SeE8 BC
0ea.a3s5 2aS6vt2eae ma2r
,5
EEga7nn3 ._...:;5
sir7e8taa3ee~r:z3a:8oae8eo
nThH 'I.- TTHaed
TEEE :--:'. q7 mEeEaE ....-':
"eases
Figure 4
Figure
HHmPPoLLbCCilecchhrrpohomamsaaettooggrraanm
ooff
aa
ffoorrmmaammiiddee
ssoolluuttiioonn
ooff
00..22
g/1
g/1
in
in
mobile phase.
CoHCoolbluuimmlnne phase FDelMFtloooebwwiclteiopnhase IDnejteeccttiioonn volure
Injection volume
7LL5ii1CC2hh5rrooss(ppvhh1ever)r
ai1c000e0tRoRPPn--i11t88r;;ile11/22M55ixd141i((-1IQ..0D..v))atemmrmn;;
dy=5
dp=5
un
um
75125 (vfv) acetonitrilelMilli-Q
LWn,/maitnx = 210m i ml/min
water
U1V0,'u1at X = 210 nm
10 #l
-
Ppaaggee
13
13
- -
22779933..00001133
_3MMNMON105135232224477
-- acktomam
BACK TO MAIN
T-s674
MOTO Progect 121275
NOTOX Pro~ect 121275
T-5874
11331/0044/19944 TTRRI3
PPooww
1.000 fremont
1.000
fd
| 0.808 [seProomnonfont fet
o 0.800
Fr
oy i
Qg
0.600
0.4500
[rrTr T f eT od
(0400 0. 400
k
frm
' 0.200 0. 200
a
| LS |i
0O ..000000
=:=
A
0.0 1.0 2.0 3.0 4.0 5.0 6.0
|
|
0.0 1.0 2.0 3.0 4.0 .5.0 6.0
|
~ i
1loogg PPooww
reference substances. FFiigguurree 55
PPlloott
ooff
lloogg
PPoowy
((xx--vvaalluuee))
vveerrssuuss
lloogg
kk''
((yy--vvaalluuee))
from
from
the
the
reference substances.
.
- paged -
Page 14 -
33M UMN0NT0S153322224488
22779933..00001144