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平面固相萃取-液质联用法多残留分析中农药的一种新的净化概念。

Planar solid phase extraction--a new clean-up concept in multi-residue analysis of pesticides by liquid chromatography-mass spectrometry.

机构信息

Institute of Food Chemistry, University of Hohenheim, Garbenstrasse 28, 70599 Stuttgart, Germany.

出版信息

J Chromatogr A. 2011 Sep 16;1218(37):6540-7. doi: 10.1016/j.chroma.2011.06.108. Epub 2011 Jul 13.

Abstract

Efficient clean-up is indispensable for preventing matrix effects in multi-residue analysis of pesticides in food by liquid and gas chromatography coupled to mass spectrometry. As a completely new approach, highly automated planar chromatographic tools were applied for powerful clean-up, called high-throughput planar solid phase extraction (HTpSPE). Thin-layer chromatography (TLC) was used to completely separate pesticides from matrix compounds and to focus them into a sharp zone, followed by extraction of the target zone by the TLC-MS interface. HTpSPE resulted in extracts nearly free of interference and free of matrix effects, as shown for seven chemically representative pesticides in four different matrices (apples, cucumbers, red grapes, tomatoes). Regarding the clean-up step, quantification by LC-MS provided mean recovery (against solvent standards) of 90-104% with relative standard deviations of 0.3-4.1% (n=5) for two spiking levels of 0.1 and 0.5 mg/kg. Clean-up of one sample was completed in a manner of minutes, while running numerous samples in parallel at reduced costs, with very low sample and solvent volumes.

摘要

高效的清理对于防止食品中多残留农药的液相和气相色谱-质谱联用分析中的基质效应是必不可少的。作为一种全新的方法,高度自动化的平面色谱工具被应用于强大的净化,称为高通量平面固相萃取(HTpSPE)。薄层色谱(TLC)用于完全将农药与基质化合物分离,并将其聚焦到一个尖锐的区域,然后通过 TLC-MS 接口提取目标区域。HTpSPE 得到的提取物几乎没有干扰和基质效应,这在四种不同基质(苹果、黄瓜、红葡萄、西红柿)中的七种化学代表性农药中得到了证明。关于净化步骤,通过 LC-MS 定量,对于 0.1 和 0.5mg/kg 两个加标水平,相对于溶剂标准的平均回收率(90-104%),相对标准偏差为 0.3-4.1%(n=5)。一个样品的净化在几分钟内完成,同时以降低的成本并行运行多个样品,样品和溶剂的体积非常低。

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