LC/MS/MSによる加工食品中のカルバメート系農薬分析法

摘要

A rapid analytical method for the simultaneous determination of carbamate pesticides in processed foods was established by liquid chromatography coupled with tandem mass spectrome-try (LC/MS/MS). The pesticides were extracted from samples with acetonitrile using accelerated solvent extract equipment, except for the fine powder type spices, which were extracted in an ultrasonic bath. The crude extract was cleaned up with a multi-solvent GPC column (Shodex Asahipak GF-310 HQ) using acetonitrile as a mobile phase. The eluent from the column at the retention time between 13 to 18min was concentrated under nitrogen gas and dissolved in a mixture of acetonitrile-water-0.2 mol/L ammonium formate buffer pH 6.0 (10:9:1). An aliquot was injected into the LC/MS/MS using electrospray ionization (ESI) with acquisition in the positive mode.rnThe recoveries of 29 kinds of pesticide from dried fruits (raisin, prune and mango) and spices (turmeric, masala, sage, thyme and red pepper) fortified at levels of 0.1 and 0.01 μg/g were mostly in the range of 50 to 150% and those from soybean paste and soy sauce fortified at 0.01 μg/g were 46.9 to 122.6% (C.V. 3.8 to 37.6%), except for 4 kinds of pesticide. The determination limits (S/N ≧10) corresponded to 0.001 to 0.05 μg/g of the pesticides in red pepper.%平成18年5月29日に農薬，飼料添加物および動物用rn医薬品についてポジティブリスト制度が施行され，約800rn品目の農薬等に食品中の残留基準（暫定を含む）が設定さrnれて規制されることになった．また，規制の対象も生鮮食rn品のほか，加工食品にも拡大された．これらの農薬等の残rn留検査においては，高感度で精度の高い分析法であることrnに加えて，迅速，簡便な分析法が要求される．