Validation Study on a Method for Multiresidue Analysis of Pesticides in Vegetables and Fruits with Supercritical Fluid Extraction

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  • 超臨界流体抽出(SFE)による野菜・果実中の残留農薬の一斉分析法の妥当性評価
  • チョウリンカイ リュウタイ チュウシュツ(SFE)ニ ヨル ヤサイ ・ カジツ チュウ ノ ザンリュウ ノウヤク ノ イッセイ ブンセキホウ ノ ダトウセイ ヒョウカ

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Abstract

Supercritical fluid extraction (SFE) was applied to extraction of pesticides from vegetables and fruits. Residues were extracted from homogenized samples mixed with water-absorbent polymer with supercritical carbon dioxide in a stainless steel tube, followed by elution with acetone. Co-extractives were removed by means of mini-column clean-up. Measurement was performed by GC-MS/MS. Calibration was achieved by preparing matrix-matched calibration standards to counteract matrix effects. With the Japanese method validation guideline as a reference, the method was assessed in 5 agricultural products spiked with 334 pesticides at 0.01 and 0.1 μg/g. Compounds at each level were extracted from 2 samples on 5 separate days. The trueness of the method for 189 pesticides in all samples was 70–120%, and the repeatability and within-run reproducibility were also consistent with the guideline. The trueness of the method for the other 71 pesticides was in the range of 50–70%, though the repeatability and within-run reproducibility were satisfactory. This method is available as a multiresidue analysis method for vegetables and fruits.

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