Document KG12N20ZgQkB2QLGRYg2x1OKr

r A M M . 5$l 483 Accession No. Study No. C03-3619 33619 Study Report Analysis of Impurities ir (non-GLP study)' / '" "x October 14, 2003 Chemicals Evaluation and Research Institute, Japan --Kurume Laboratory-- Company Sanitized. Does no! contain TSCA CB Table o f Contents T i tle ..........................................................................................................................................3 Commissioned by................................................................................................................... 3 Testing Facility...................................................................................................................... 3 Purpose of Study.......................................................................... 3 Schedule.................................................................................................................................. 3 Personnel................................................................................................................. 3 Approval of Study Report.....................................................................................................3 S u m m a ry .................................................................. 4 1. Test Substance....................................................................................................................... 5 2. Conducting the Study............................................................................................................ 5 3. Study R esults......................................................................................................................... 7 Figures Fig. 1: HPLC chromatogram for analysis of impurities. Study No. 33619 2 'Company Sanitized. Does not contain TSCA CM Title: Analysis of Impurities i '(non-GLP study) Commissioned by: DuPont KK 1-8-1 Shimo-meguro, Meguro-ku, Tokyo 153-0064 Testing Facility: Kurume Laboratory Chemicals Evaluation and Research Institute, Japan (CERI) 19-14 Chuo-machi, Kurume-shi, Fukuoka Prefecture 830-0023 Purpose of Study: To determine the levels of impurities present i Schedule: Study began on: Test date: Study completed on: July 28, 2003 July 28, 2003 October 14, 2003 Personnel: Coordinator: Researcher: Yasuko MATSUNOBE, Testing Section 1 Tomohiko YOSEQDA Approval of Study Report: [signed] Yasuko MATSUNOBE Study Coordinator October 14, 2003 *Translator's Note: Spellings of personal names may need to be verified. Study No. 33619 3 Company Sanitized. Does no! contain TSCA c q i Summary Title of Study Analysis of Impurities in non-GLP study) Study Conditions (1) Concentration of sample furnished: 10.0 g/L (2) Analysis: Analysis of impurities by high-performance liquid chromatography (HPLC) Test Results Content of Sample Furnished: Test substance: Impurity A Impurity B 97.80% 0.38% 1.82% (The impurities were labeled "A" and "B" in the order of increasing retention time on the HPLC chromatogram.) Study No. 33619 1. Test Name: Lot No.: 2. Conducting the Study High-performance liquid chromatography (HPLC) samples prepared as described in section 2.1 below (lO.Og fL solutions of the sample furnished) were analyzed under the conditions in section 2.2 on the next page. The test substance and impurity contents within the sample were computed from the surface areas of the test substance and impurity peaks on the resulting HPLC chromatogram. 2.1 Preparation of- Sarapfesfor Analysis HPLC samples for analyzing the sample furnished were prepared by carrying out the operations indicated in the flow scheme below. Flow Scheme Sample furnished 200 mg Bring up to 20 mL (m ethanof VlO mmol/L ammonium acetate in water (7/3 V/V), measuring flask) HPLC sample (sample furnished 10.0 g/L solution) *1: Methanol solution containing 10 mmol/L ammonium acetate / ' ' `" ''N Study No. 33619 5 0es m eoftfaih 2.2 HPLC Analysis of Samples Furnished The HPLC samples prepared in section 2.1 above were analyzed based on the following conditions (see Fig. 1). Apparatus: Liquid chromatograph-mass spectrometer Pump: LC-lOADvp (Shimadzu Corp.) Detector: RED-10A (Shimadzu Coip.) Column oven: CTO-lOACvp (Shimadzu Corp.) Degasser: DGU-12AM (Shimadzu Corp.) Column: L-column ODS (CERI); 15 cm x 4.6 mm I.D. Column temperature: 40C Eluting solvent: Methanol*1/ 10 mmol/L ammonium acetate in water Flow rate: Injection rate: Detector output: 1.0 mL/min 10 (J.L lxlO"4 RIU/V 2.3 Calculation of Test Substance and Impurity Contents The contents of the test substance and the impurities were calculated based on the following formula. The third decimal place was rounded off, and the results indicated to the second decimal place. Content (%) = AREl ^ xl00 AREA (0 where AREA (s): AREA (t): Surface area of a peak for a test substance or impurity detected on HPLC chromatogram (juV-sec) Sum of all peak surface areas for test substances and impurities detected on HPLC chromatogram (pV-sec) Study No. 33619 'Company Sanitized. Does not contain TSCA CSj 6 3. Test Results ______ The results of analysis are given below. Retention time Peak surface area (minutes) OaV-sec) Test substance 5.80 2236865 Impurity A*2 4.16 8714 Impurity B*2 6.89 41633 Total -- 2287212 Content (%) 97.80 0.38 1.82 100 Figure 1 *2: The impurities were labeled "A" and "B" in the order of increasing retention time on the HPLC chromatogram. In addition to the above impurities, there was believed to be also some ethanol remaining in the samples furnished. However, a separately conducted s t u d ) f l |B H H | "residual ethanol was p resen ^T m ex ero ieri^p p e^ ^h aU h e only impurities present in the sample furnished were the two types detected in the present study. Study No. 33619 7 Company Sanitized. Does not contain TSCA cm PKNO Translation: Language Services F. Metreaud December 3, 2003 Study No. 33619 me$.mrnm3BSM. 8 s -J ffi: '5-