LC-MS/MSを用いた野菜および果実中の残留農薬迅速一斉分析法の妥当性確認

摘要

A validation study was carried out on a rapid method for the simultaneous determination of pesticide residues in vegetables and fruits by LC-MS/MS. Preparation of the test solution was performed by a solid-phase extraction technique with QuEChERS(STQ method). Pesticide residues were extracted with acetonitrile using a homogenizer, followed by salting-out and dehydration at the same time. The acetonitrile layer was purified with C18 and PSA mini-columns. The method was assessed for 130 pesticide residues in 14 kinds of vegetables and fruits at the concentration level of 0.01 μg/g according to the method validation guideline of the Ministry of Health, Labour and Welfare of Japan. As a result 75 to 120 pesticide residues were determined satisfactorily in the tested samples. Thus, this method could be useful for a rapid and simultaneous determination of multi-class pesticide residues in various vegetables and fruits.%LC-MS/MSを用いた野菜および果実中の残留農薬迅速一斉分析法の妥当性確認を行った.試験溶液の調製には.QuEChERS法と固相抽出法を組み合わせたSTQ法を用いた.抽出溶媒にアセトニトリルを用い，ホモジナイズ抽出を行った後，塩析および脱水を同時に行った.得られたァセトニトリル層をC18(30mg)/PSA(30mg)連結ミニ固相カラムおよびC18(50mg)ミニ固相カラムを用いて精製し試験溶液とした.厚生労働省通知の妥当性評価ガイドラインに従い，14種類の野菜および果実を対象として，一律基準濃度における残留農薬130成分の一斉分析法の妥当性確認を実施した.その結果，それぞれの野菜および果実において，75〜120成分の農薬が対象となる場合に.分析法の性能はガイドラインの目標値(真度:70〜120%,併行精度:25%未満.室内精度:30%未満)を満たした.以上のことから，本試験法は残留農薬の迅速一斉分析法として有用であると考えられた.