LC-MS/MSによる農産物を主原料とした加工食品中の残留農薬一斉分析法の検討

摘要

A rapid multi-residue method for determination of pesticide residues in processed foods manufactured from agricultural products was examined. Five mL water was added to 5g sample in a polypropylene tube, and the tube was left to stand at room temperature for 30min. Then, 20mL acetonitrile was added to the sample. The mixture was homogenized in a nigh-speed homogenizer, followed by salting out with 1g NaCl and 4g anhydrous MgSO_4. After centrifugation, the organic layer was purified on a graphitized carbon/PSA cartridge column. After removal of the solvent, the extract was resolved in methanol-water and analyzed with LC-MS/MS. The recoveries of 93 pesticides fortified into 5 kinds of processed foods [Chinese cabbage kimchi, marmalade, raisin, umeboshi(pickled plum)and Worcester sauce] were examined at the concentrations of 0.02 and 0.1μg/g(n= 5). The recoveries of 61 pesticides in all foods were 70-120% with relative standard deviation below 20% at both concentrations. Seventy-four processed foods obtained from markets in Japan were examined with this method. Pesticide residues over the maximum residue limit(0.01μg/g)were detected in 2 processed foods.%農産物を主原料とした加工食品を対象として,迅速な農薬の一斉分析法を検討した.均一化した試料5gに水5mLを加えて室温で30分間放置後，ァセトニトリル20mLを加えてホモジナイズ抽出した.塩化ナトリウム1gおよび無水硫酸マグネシウム4gを加えて塩析•脱水した.分離した有機層をグラフアイトカーボン/PSAカートリッジを用いて精製し,LC-MS/MSで測定した.93農薬について，白菜キムチ.マーマレード，レーズン，梅干しおよびウスターソースで添加回収試験(0.02および0.1μg/g添加,5試行)を実施した.その結果,すべての食品において平均回収率70〜120%(併行精度20%以下)を満たした農薬数は,61農薬であった.本法により巿販の加工食品74品目について実態調査を行ったところ，2品目で食品衛生法の一律基準値を超過した.