LC-MS/MSによる穀物加工食品および粉ミルク中のセレウリドの分析法

摘要

An LC-MS/MS method for analysis of cereulide, an emetic toxin produced by Bacillus cereus, was developed. Cereulide was extracted from samples, fried rice, pan-fried noodles, red bean paste and baby formula, with methanol and purified using Oasis HLB cartridges. LC separation was performed on a C18 column with a mixture of formic acid solution and methanol containing ammonium formate as a mobile phase, and the mass spectrometer was operated in the positive electrospray ionization mode. Performance evaluation showed that trueness was higher than 70% and repeatability and reproducibility were within 10%. The limits of quantification were lower than 1 μ/kg.%セレウス菌嘔吐毒であるセレウリドのLC-MS/MSによる分析法を開発した．試料にはチャーハン，焼きそば，小豆あんおよび乳児用粉ミルクを用い，メタノールで抽出後，Oasis HLBカートリッジにより精製し，試験溶液とした．LC-MS/MSの移動相にはギ酸アンモニウム含有のギ酸溶液およびメタノールの混液を採用し，ESI（＋）で測定した．開発した分析法の性能評価を実施したところ，すべての試料において貞慶70％以上，併行・室内精度10％以下の結果が得られた．なお，定量限界はμg/kg以下とrn見積もられた．