title: 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.
abstract: 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 acetone-cyclohexane (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 microg/g were >85%, and the relative standard deviations were <9%. The detection limits for spinosyns A and D in green perilla were 0.005 microg/g by UV detection and 0.001 microg/g by MS detection.
authors.affiliation: Aichi Prefectural Institute of Public Health, Tsuji-machi, Kita-ku, Nagoya, Aichi 462-8576, Japan. eiji_ueno@pref.aichi.lg.jp
authors.forename: Eiji
authors.initials: E
authors.lastname: Ueno
authors.forename: Harumi
authors.initials: H
authors.lastname: Oshima
authors.forename: Hiroshi
authors.initials: H
authors.lastname: Matsumoto
authors.forename: Isao
authors.initials: I
authors.lastname: Saito
authors.forename: Hiroto
authors.initials: H
authors.lastname: Tamura
mesh_terms: D002850:Chromatography, Gel; D002851:Chromatography, High Pressure Liquid; D004338:Drug Combinations; D005638:Fruit / Q000737:chemistry*; D007306:Insecticides / Q000032:analysis*; D018942:Macrolides / Q000032:analysis*; D013058:Mass Spectrometry; D010573:Pesticide Residues / Q000032:analysis; D012997:Solvents; D013056:Spectrophotometry, Ultraviolet; D014675:Vegetables / Q000737:chemistry*
chemical_list: D004338:Drug Combinations; D007306:Insecticides; D018942:Macrolides; D010573:Pesticide Residues; D012997:Solvents; C415329:spinosad