分散固相抽出および多機能カラムを用いたGC-MS/MSによる畜産物中の残留農薬一斉分析法

摘要

厚生労働省通知の畜水産物中残留農薬一斉試験法では，精製にゲル浸透クロマトグラフィー（GPC）を用いている.本研究では，より簡便な試験溶液調製法を検討した.抽出溶媒にアセトニトリルーエタノール（1：1）混液を用い，冷却遠心分離と分散固相抽出および多機能カラムを組み合わせた精製を行うことで，脂肪を含む爽雑物質のクリーンアップを効率良く行うことができた.これにより，GPCを用いずに，試験溶液の調製を簡便かつ迅速に行うことができた.本法による添加回収試験では，検討した131成分のうち115成分以上の農薬が回収率70～120％，相対標準偏差15％未満であった.定量下限値は，0.001～0.01μg/gの範囲で設定可能であった.%A simple clean-up method was developed for the simultaneous determination of pesticide resi­dues in livestock products by GC-MS/MS. The pesticide residues were extracted with acetonitrile-ethanol (1:1), and matrix components such as adipose were effectively eliminated by a combina­tion of refrigerated centrifugation, dispersive solid-phase extraction, and multifunctional column chromatography. In this method, samples are treated quickly and easily without the need for gel-permeation chromatography. Among 131 pesticides tested, 115 showed recovery within the range from 70 to 120%, with relative standard deviations of less than 15%. The quantification limits for the 115 pesticides in livestock products were 0.001 to 0.01 μg/g.