Gilbert-López Bienvenida, García-Reyes Juan F, Molina-Díaz Antonio
Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, 23071 Jaén, Spain.
Talanta. 2009 Jul 15;79(2):109-28. doi: 10.1016/j.talanta.2009.04.022. Epub 2009 Apr 18.
A demanding task in pesticide residue analysis is yet the development of multi-residue methods for the determination of pesticides in vegetables with relatively high fat content (i.e. edible oils and fatty vegetables). The separation of pesticides and other chemical contaminants from high-fat food samples prior to subsequent steps in the analytical process is yet a challenging issue to which much effort in method development has being applied. This review addresses the main sample treatment methodologies for pesticide residue analysis in fatty vegetable matrices. Even with the advent of advanced hyphenated techniques based on mass spectrometry these complex fatty matrices usually require extensive sample extraction and purification. Current methods involve the use of one or the combination of some of the following techniques for both the sample extraction and clean-up steps: liquid-liquid partitioning, solid-phase extraction (SPE), gel-permeation chromatography (GPC), matrix solid-phase dispersion (MSPD), etc. An overview of methods developed for these contaminants in fatty vegetables matrices is presented. Sample extraction and purification techniques are discussed and their most recent applications are highlighted. This review emphasizes that sample preparation is a critical step, but also the determination method is, and cannot be treated separately from sample treatment. In recent years, the appearance and use of new, more polar pesticides has fostered the development of liquid chromatography/mass spectrometry (LC-MS) besides gas chromatography. The main features of LC-MS for the analysis of multi-class pesticides in fatty vegetable samples will be also underlined, with an emphasis on the multi-class, multi-residue strategy and the difficulties associated.
在农药残留分析中,一项具有挑战性的任务是开发用于测定脂肪含量相对较高的蔬菜(即食用油和多脂蔬菜)中农药的多残留方法。在分析过程的后续步骤之前,从高脂肪食品样品中分离农药和其他化学污染物仍然是一个具有挑战性的问题,为此在方法开发方面已经付出了很多努力。本综述阐述了多脂蔬菜基质中农药残留分析的主要样品处理方法。即使基于质谱的先进联用技术已经出现,但这些复杂的多脂基质通常仍需要进行大量的样品提取和净化。目前的方法在样品提取和净化步骤中涉及使用以下一种或几种技术的组合:液液分配、固相萃取(SPE)、凝胶渗透色谱(GPC)、基质固相分散(MSPD)等。本文概述了针对多脂蔬菜基质中这些污染物开发的方法。讨论了样品提取和净化技术,并突出了它们的最新应用。本综述强调样品制备是关键步骤,但测定方法也是如此,而且不能与样品处理分开对待。近年来,新型、极性更强的农药的出现和使用,除了气相色谱法外,还推动了液相色谱/质谱联用(LC-MS)技术的发展。还将强调LC-MS用于分析多脂蔬菜样品中多类农药的主要特点,重点是多类、多残留策略以及相关的困难。