LC-MS/MSによる農産物中の残留農薬一斉分析法の妥当性評価

摘要

A multi-residue method for 122 pesticides in agricultural products was validated in accordance with Japanese guidelines for residual agricultural chemicals in food. The sample was extracted with acetonitrile. Co-extractives were removed by GPC-graphitized carbon column SPE, followed by silica gel/PSA cartridge column SPE. The pesticides in the test solution were determined by LC-MS/MS using scheduled MRM in combination with polarity switching. Validation tests were performed on spinach, brown rice, soybean, orange and tomato fortified at 0.01 and 0.1 μg/g. The pesticides at each level were analyzed in two samples per day on five different days. In conclusion, among 122 pesticides tested for each level,121 pesticides (but not disulfoton) were found to meet all of the guideline criteria.%LC-MS/MSによる農産物中の残留農薬一斉分析法について，「食品中に残留する農薬等に関する試験法の妥当性評価ガイドライン」に従って評価を行った.試料からアセトニトリルで抽出したのち，GPC-グラフアイトカーボンSPEで精製し，さらに，シリカゲル/PSA連結SPEにより精製してScheduled MRMおよびESIポジティブ/ネガティブスイッチングモードを組み合わせたLC-MS/MSにより測定した.5種類の農産物，122種類の農薬成分を対象にして添加濃度0.01μg/gおよび0.1μg/gで，分析者1名が1日2併行で5日間の枝分かれ試験を行って.真度(回収率)，併行精度および室内精度を求めた.その結果，両濃度でガイドラインに示される目標値を満たした農薬成分は農産物5種類ともにジスルホトンを除く121種類であった.