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Determination of Spinosad in Vegetables and Fruits by High-Performance Liquid Chromatography with UV and Mass Spectrometric Detection After Gel Permeation Chromatography and Solid-Phase Extraction Cleanup on a 2-Layered Column

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A simple and reliable method was developed for the determination of spinosyns A and D, the active ingredients of spinosad, in vegetables and fruits, by high-performance liquid chromatography with UV detection (HPLC-UV) and confirmation by mass spectrometry (MS); the method uses selected gel permeation chromatography (GPC) and a 2-layered column for solid-phase extraction system. An aliquot of the crude sample extract obtained by acetonitrile extraction is loaded into the GPC system. The fraction containing spinosyns A and D is selectively collected and loaded directly onto a 2-layered column consisting of graphitized carbon (upper layer) and cyclohexyl-bonded silica gel (lower layer). After the column is washed with the GPC mobile phase acetonecyclohexane (3 7), the column is eluted with acetonitrile containing 2% triethylamine. The eluate is used for HPLC-UV/MS analysis. Average recoveries from fortified cabbage, green perilla, fig, and strawberry at analyte concentrations of 0.05 and 0.25 g/g were >85%, and the relative standard deviations were <9%. The detection limits for spinosyns A and D in green perilla were 0.005 g/g by UV detection and 0.001 g/g by MS detection.
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Document Type: Research Article

Affiliations: 1: Aichi Prefectural Institute of Public Health, Tsuji-machi, Kita-ku, Nagoya, Aichi 462-8576, Japan. 2: Tokai COOP Federation, Food Safety and Quality Research Center, Sagamine, Yazako, Nagakute-cho, Aichi 480-1103, Japan. 3: Meijo University, Faculty of Agriculture, Department of Environmental Bioscience, Shiogamaguchi, Tempaku-ku, Nagoya, Aichi 468-8502, Japan.

Publication date: 2006-11-01

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  • The Journal of AOAC INTERNATIONAL publishes refereed papers and reviews in the fields of chemical, biological and toxicological analytical chemistry for the purpose of showcasing the most precise, accurate and sensitive methods for analysis of foods, food additives, supplements and contaminants, cosmetics, drugs, toxins, hazardous substances, pesticides, feeds, fertilizers and the environment available at that point in time. The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better methods of preparing samples for analysis; collaborative studies substantiating the performance of a given method; statistical techniques for evaluating data. The Journal will also publish other articles of general interest to its audience, e.g., technical communications; cautionary notes; comments on techniques, apparatus, and reagents.
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