title: [Validation study of a method for multiresidue analysis of pesticides in cereals and pulses using supercritical fluid extraction].
abstract: Supercritical fluid extraction (SFE) was applied to extraction of pesticides from cereals and pulses. Residues were extracted from homogenized samples mixed with water-absorbent polymer and supercritical carbon dioxide in a stainless steel tube, followed by elution with acetonitrile. Co-extractives were removed by means of mini-column clean-up. Measurement was performed by GC-MS/MS. Calibration was achieved by preparing matrix-matched calibration standards to counteract matrix effects. With the Japanese method validation guideline for pesticide residues as a reference, the method was assessed in 5 agricultural products spiked with 334 pesticides at 0.01 and 0.1 µg/g. Compounds at each level were extracted from 2 samples on 5 separate days. The trueness of the method for 137 pesticides in all samples was 70-120%, and the repeatability and within-run reproducibility were also consistent with the guideline. The trueness of the method for the other 101 pesticides was in the range of 50-70%, though the repeatability and within-run reproducibility were satisfactory. This method is available as a multiresidue analysis method for cereals and pulses.
authors.affiliation: Nara Prefectural Institute for Hygiene and Environment, Nara-shi, Nara, Japan. k.uranishi@ihe.pref.nara.jp
authors.forename: Katsushige
authors.initials: K
authors.lastname: Uranishi
authors.forename: Hirokazu
authors.initials: H
authors.lastname: Yamashita
authors.forename: Akiko
authors.initials: A
authors.lastname: Okayama
authors.forename: Keigo
authors.initials: K
authors.lastname: Yamamoto
mesh_terms: D002523:Edible Grain / Q000737:chemistry*; D007887:Fabaceae / Q000737:chemistry*; D005504:Food Analysis / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D013058:Mass Spectrometry / Q000379:methods*; D010573:Pesticide Residues / Q000032:analysis* / Q000302:isolation & purification; D015203:Reproducibility of Results
chemical_list: D010573:Pesticide Residues