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分散液液微萃取法检测水果、蔬菜和中草药中 12 种商品的高灵敏度和高选择性有机磷筛查。

Highly sensitive and selective organophosphate screening in twelve commodities of fruits, vegetables and herbal medicines by dispersive liquid-liquid microextraction.

机构信息

Department of Chemistry, Hong Kong Baptist University, Kowloon Tong, Hong Kong, PR China.

出版信息

Anal Chim Acta. 2013 May 2;775:58-66. doi: 10.1016/j.aca.2013.02.043. Epub 2013 Mar 13.

Abstract

The article describes a simple sample pretreatment procedure for the analysis of ten organophosphorus pesticides using dispersive liquid-liquid microextraction (DLLME) followed by gas chromatography-mass spectrometry (GC-MS) in three distinctively different types of matrices: fresh fruits, fresh vegetables and dried herbs. The method was carefully developed, focusing on the chemistry of various dispersive solvents, to achieve simultaneous, comprehensive extraction and preconcentration in a great span of selected matrices. According to matrix-matched validation study, the set of optimized DLLME conditions has been proven robust to determine target OPPs within a wide linear range from 0.1 to 1000 μg L(-1). With limited usage of organic extractants, remarkable enrichment factors up to 100-fold were obtained, enabling ultra-trace pesticide quantification down to sub-ppt levels at 0.12-4.92 ng kg(-1). Practical application of the method was illustrated by quantitative recovery (70-119%) and good precision (2.6-10% R.S.D.) in a representative range of three fruits and four vegetable commodities featured by the CODEX Alimentarius classification as well as their unique matrix compositions. A careful selection of dried herbs was further classified based on their morphological structures to validate analytical ruggedness of the method. Compared with existing methods for food analysis vis-à-vis OPPs, the present method is superior in terms of high sample throughput, minimal solvent consumption, and small sample size requirement. An additional, significant aspect of this universal DLLME method is that it models sample pretreatment methods with wide coverage of analytical matrices that are more effective, more comprehensive, and more flexible than those currently being used.

摘要

本文描述了一种使用分散液液微萃取(DLLME)结合气相色谱-质谱(GC-MS)分析十种有机磷农药的简单样品预处理方法,该方法适用于三种不同类型的基质:新鲜水果、新鲜蔬菜和干草药。该方法经过精心开发,重点研究了各种分散溶剂的化学性质,以实现各种选定基质中同时、全面的提取和预浓缩。根据基质匹配验证研究,已证明优化的 DLLME 条件集能够在 0.1 至 1000μg/L 的宽线性范围内对目标 OPPs 进行准确测定。通过有限使用有机溶剂,获得了高达 100 倍的富集因子,能够在 0.12-4.92ng/kg 的超痕量农药定量下限下进行超痕量农药定量。该方法通过在代表性范围内对三种水果和四种蔬菜商品的定量回收(70-119%)和良好的精密度(2.6-10%RSD)进行了实际应用,这些商品的特点是符合食品法典委员会的分类,并且具有独特的基质组成。进一步根据其形态结构对精心挑选的干草药进行分类,以验证该方法的分析稳健性。与现有的食品分析中 OPPs 相关方法相比,本方法在高样品通量、最小溶剂消耗和小样品量要求方面具有优势。这种通用 DLLME 方法的另一个重要方面是,它模拟了具有更有效、更全面和更灵活的分析基质覆盖范围的样品预处理方法,优于目前使用的方法。

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