Fluensulfone ... - IR-4 Project

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SUMMARY PTRL West <strong>Project</strong> No. 1977W Report 2 Page 12 A method for quantitation of MCW-2 and its metabolites in tomato, pepper, cucumber and melon was successfully validated. Control matrices were fortified at 0.01 mg/kg (the LOQ) and 0.10 mg/kg (10x LOQ). MCW-2 and its metabolites butene sulfonic acid (M- 3627) and thiazole sulfonic acid (M-3625) were extracted from fortified tomatoes, pepper, cucumber and melon with acetonitrile:water. The extract was subjected to further cleanup involving an SPE cartridge cleanup. The final samples were analyzed by LC- MS/MS for quantitation of MCW-2, butene sulfonic acid and thiazole sulfonic acid. The limit of quantitation for all three analytes in all matrices is 0.01 ppm. The limit of detection was 0.45 ng/mL in solution. INTRODUCTION Makhteshim-Agan of North America, Inc. contracted with PTRL West, Inc. to conduct method development and validation of an analytical method for determination of MCW-2 and its metabolites commonly named butene sulfonic acid and thiazole sulfonic acid in tomato, pepper, cucumber and melon. The study is designed to comply with OPPTS 860.1340 and SANCO/825/00 rev.7 dated 17/03/04 guidelines. The study was initiated on January 15, 2010. This study was conducted from January 19 to May 13, 2010. The study was conducted at PTRL West, Inc., 625-B Alfred Nobel Drive, Hercules, CA 94547 under an approved protocol according to the US EPA FIFRA Good Laboratory Practice Standards, 40 CFR §160 (Appendix A).
MATERIALS AND METHODS Reference Substances PTRL West <strong>Project</strong> No. 1977W Report 2 Page 13 The reference substance of MCW-2 (lot number 326-115-01, PTRL Sample No. 1785W- 003C) was supplied by LABService with a stated purity of 99.05%. The expiration date on the certificate of analysis is May 31, 2010 and it was stored refrigerated upon receipt. The reference standard of thiazole sulfonic acid sodium salt (M-3625, lot number 381- 174-00, PTRL Sample No. 1788W-003) was supplied by Makhteshim Chemical Works with a stated purity of 90.9%. The expiration date on the certificate of analysis is December 31, 2011 and it was stored refrigerated upon receipt. The reference standard of butene sulfonic acid sodium salt (M-3627, lot number 215PAL2, PTRL Sample No. 1785W-021) was supplied by PharmAgra Labs, Inc. with a stated purity of 99.1%. The expiration date on the certificate of analysis is September 10, 2010 and it was stored at room temperature. See Appendix B for the certificates of analysis. All stock and working solutions were stored at < 0°C in amber bottles with Teflon ® -lined screw-top caps. All solutions were prepared using pipettmen with diposable plastic tips, avoiding reuse of any glassware as carryover of the metabolites was suspected. All reference substances were concluded to be stable in solution throughout the study period based on comparison of chromatograms generated over the study period. Reagents and Solvents All solvents were HPLC grade unless noted: Acetonitrile (ACN) Formic Acid Water Glassware and Miscellaneous Equipment Balance Bottle, amber, with Teflon ® -lined cap, various sizes Bottle, plastic, 250 mL centrifuge Centrifuges, Mistral 3000E and Eppendorf 5415C Graduated Cylinder, various sizes Microfilterfuge tube, Rainin 0.45 UM Nylon-66
Page 1 and 2: TITLE Method Validation of an Analy
Page 3 and 4: PTRL West Project No. 1977W Report
Page 5 and 6: STUDY PERSONNEL PTRL West Project N
Page 11: PTRL West Project No. 1977W Report
Page 17 and 18: 3. Add 50 ml of ACN:HPLC water (1:1
Page 19 and 20: Injection Volume: 20 µL Solvent Sy
Page 21 and 22: Retention Time: Butene sulfonic aci
Page 41: D. Impact on Study: Prepared By: No

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