A Method for Residue Analysis of Benfuracarb and Its Metabolites Carbofuran, 3-Hydroxy-carbofuran and 3-Keto-carbofuran in Crops by Gas Chromatography
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A procedure has been developed for the analysis of residues of benfuracarb and its metabolites, carbofuran, 3-hydroxy-carbofuran (3-OH-CF) and 3-keto-carbofuran (3-C=O-CF) in eleven crops. The crops were homogenized after addition of silver nitrate solution (or milled in a case of rice grain) and extracted with solvents. The extract was cleaned up by column chromatography and subjected to gas chromatography (GC). The silver nitrate solution was used to prevent the decomposition of benfuracarb by N-S bond cleavage during the homogenization and extraction. Of the four compounds benfuracarb and carbofuran were extracted with methanol from the crops. The extract was concentrated, water was added and the extract was again extracted with dichloromethane. The extraction of 3-OH-CF and 3-C=O-CF were accomplished by the aid of hydrolysis of conjugated 3-OH-CF and 3-C=O-CF by dipping the homogenate in 0.25N hydrochloric acid and refluxing, followed by the extraction with dichloromethane. The extract containing benfuracarb and carbofuran or 3-OH-CF and 3-C=O-CF was then subjected to a cleanup procedure using silica gel and Florisil column chromatography. The concentrated eluate was analyzed by GC employing a quartz capillary column. Recoveries from fortified samples were 75-100% for benfuracarb, 73-100% for carbofuran, 76-99% for 3-OH-CF and 76-99% for 3-C=O-CF at 0.05 and 0.5ppm levels. The overall detection limit was 0.005ppm for all compounds.
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