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Study Report
Analysis of Impurities i
1
(non-GLP study)
October 14, 2003
Chemicals EvaKluuartiuonmeanLdaRbeosreaatrochryInstitute, Japan
(Company Sanitized. Does not contain' TSCA CBE -
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Table of Contents
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2. Conducting the SY...
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Figures
Fig. 1: HPLC chromatogram for analysis of impurities.
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Study No. 33619
2
`CompanySanitized.Doesnot containTSCACBI
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Title:
AnalysisofImpurities Joc.r study)
Commissioned by: DuPont KK 1-8-1 Shimo-meguro, Meguro-ku, Tokyo 153.0064
Testing Facility: ~~ Kurume Laboratory C1h9e-m14icCahluso-Emvaalcuhait,ioKnuraunmde-Rsehseia,rFcuhkIunostkiatuPter,efJeacptaunre(C3E0R-I0)023
Purpose of Study:
Schedule:
To determine the levels of impurities present J a--)
Study began on: TSetsutdydactoem:pleted on:
JJuullyy 2288,,22000033 October 14, 2003
Personnel:
ReCsoeoradricnhaetror:
YTaosmuokhoikMoAYTOSSUHNIODBAE," Testing Section 1
Approval of Study Report: [signed] Yasuko MATSUNOBE SOcttuodbyeCroo1r4,di2n0a0t3or
~~
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*Transato's Note: Spellings of personal namesmayned tobe verified.
Study No. 33619
3 Company Sanitized. Does notcontainTSCACar
Summary
TiotfSltudey
Analysis of Impurities
cr12 sud)
Study Conditions
(1) Concentration of sample furnished: 10.0 g/L. (2) Analysis: Analysisof impurities by high-performance liquid chromatography
(HPLC)
Test Rests Contentof Sample Furnished: I`TmepsutrsiutbystAance: Impurity B
97.80%
038%
1.82%
(The impurities were labeled "A" and "B" in the order of increasing retention time on
the HPLC chromatogram.)
Study No. 33619
4 CompanySantee Doe noottccoonnttaaiinn TSCACE.
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N1.aTmeest,
A
Lotvo {i}
2. Conducting the Study in secti`onHi2g.h1-bpeerlfoowrm(a1n0c.e0li/qLuisdolcuhtrioonmsatoofgtrhaepshaym(plHePLfuCr)nissahmepdl)ewseprreepaanraeldyzaesdduensdcreirbtehde cwointdhiintitohnessianmspelcetiwoenr2e.2coonmptuhteendexftropamget.he Tsuhrefatcesetasruebasstoafncteheatnedstismupbusrtiatnycceoantnednts impurity peaks on the resulting HPLC chromatogram. 2.1 Preparation of Samples for Analysis the operHatPiLonCs siandmipclaetsedfoirn atnhaelfylzoiwngstchheesmaembpelleowf.urnished were prepared by carrying out
Flow Scheme
* Bacreitnagteuipntwoa2t0erm(L7/3(mVe/tVh)a,nomle"a's/u1r0imnmgoflla/sLk)ammonium
HPLC sample (sample farmished 10.0 g/L solution) #1: Methanol solution containing 10 mmol/L ammonium acetate
Study No. 33619
5
CompanySantizea, noes
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RE * Do6sHotconTtGaAiSany
-- 2.2 HPLC Analysisof Samples Furnished followi"nTghecoHndPiLtiConssam(speleesFipgr.e1p)a.red in section 2.1 above were analyzed based on the
Apparatus: Pump: Detector: Column oven: Degasser:
Column: Column temperature:
Eluting solvent:
Flow rate: Injection rate:
Detector output:
Liquid chromatograph-mass spectrometer
LC-10ADve (Shimadzu Corp.)
RID-10A (Shimadzu Corp.)
CTO-10ACve (Shimadzu Corp.)
DGU-12AM (Shimadzu Corp.)
L-column 40C
ODS
(CERD);
15
cm
x
4.6
mm
LD.
Methanol"'/10
BN)
mmol/L
ammonium
acetate
in
water
1.0 mLmin
10L
1x10" RIUV/
23 CalculationofTest Substance and Impurity Contents followi`nTghefocromnutlean.tsoThfethtehirtedsdtescuibmsatlanpcleacaendwatsheriomupnudreitdieosf,wearned ctahlecruelsautletds biandsiecdaotendttheo. -- the second decimal place.
Content1 ((%9%)) = AARREEAAS(s)o),x109
where AREA (5): AREA (0:
dSeutrefcatceedaroenaHofPLaCpecahkrofmoaartotgesrtasmu(b4sVt'asnecce)or impurity iSmupumriotfiaelsldpeetaekctseudrfoanceHaPrLeaCs cfohrrotemsattsougbrsatamn(c4eVs'asnedc)
--_ Study No. 33619
6 CompanySanitzed. Dos noteon contain TSCA.oy
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3. Test Results
The results of analysis are given below.
Retention time (minutes)
Peak surface area V-sec)
2236865
Content (%)
97.80
41633 Tow 1 -- | oagmiz [100 |
Figure
1
*2: The impurities were labeled "A" and "B" in the orderof increasing retention time on
the HPLC chromatogram.
remaininIgn aidnditthieon to the afburonvieshiemdp.uriHtoiweesv,etrh,erea wseapsarbateelliyevecdontdoubcet aluso osome ethanol
Co--------
a0
residual ethanolwaspresent.
sample fumished were the two
fore, it appears
types detected in the
that theonly impurities
present study.
present
in
the
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Study No. 33619
7 `Company Sanitized. Doesnotcontain TSCA car
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~~
Study No. 33619
8 CompanyS`anStzaodn.iDDooteessinnooztlcceoonndtlaai.inn TSCA CEL esem