title: [Validation study on a rapid multi-residue method for determination of pesticide residues in vegetables and fruits by LC-MS/MS].
abstract: A validation study was conducted on a rapid multiresidue method for determination of pesticide residues in vegetables and fruits by LC-MS/MS. Pesticide residues in the vegetables or fruits were extracted with acetonitrile in a disposable tube using a homogenizer, followed by salting out with anhydrous magnesium sulfate and sodium chloride in the presence of citrate salts for buffering. The extract was purified with a double-layered cartridge column (graphite carbon black/primary secondary amine silica gel; GCB/PSA). For citrus fruits a purification step with a C18 column was added (this column was connected to the GCB/PSA column). After removal of the solvent, the extract was resolved in methanol/water and analyzed by means of LC-MS/MS. The method was validated according to the method validation guideline of the Ministry of Health, Labour and Welfare of Japan; recovery tests were performed on 8 kinds of vegetables and fruits [cabbage, cucumber, Japanese radish, onion, potato, spinach, Amanatsumikan (a citrus fruit) and apple] by fortification of 161 pesticide residues at the concentrations 0.01 and 0.05 μg/g (each concentration of pesticide residue was extracted from 2 samples on 5 separate days). The trueness of the method for 127 pesticides in all 8 commodities was 70-120% with satisfactory repeatability and within-run reproducibility. This method is concluded to be applicable for determination of pesticide residues in vegetables and fruits.
authors.affiliation: Osaka Prefectural Institute of Public Health, 1-3-69 Nakamichi, Higashinari-ku, Osaka 537-0025, Japan. sts-tkt@iph.pref.osaka.jp
authors.forename: Satoshi
authors.initials: S
authors.lastname: Takatori
authors.forename: Haruna
authors.initials: H
authors.lastname: Yamamoto
authors.forename: Naoki
authors.initials: N
authors.lastname: Fukui
authors.forename: Satoko
authors.initials: S
authors.lastname: Yamaguchi
authors.forename: Yoko
authors.initials: Y
authors.lastname: Kitagawa
authors.forename: You
authors.initials: Y
authors.lastname: Kakimoto
authors.forename: Masakazu
authors.initials: M
authors.lastname: Osakada
authors.forename: Masahiro
authors.initials: M
authors.lastname: Okihashi
authors.forename: Keiji
authors.initials: K
authors.lastname: Kajimura
authors.forename: Hirotaka
authors.initials: H
authors.lastname: Obana
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D005504:Food Analysis / Q000379:methods*; D005506:Food Contamination / Q000032:analysis*; D005638:Fruit / Q000737:chemistry*; D010573:Pesticide Residues / Q000032:analysis* / Q000302:isolation & purification*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014675:Vegetables / Q000737:chemistry*
chemical_list: D010573:Pesticide Residues