色谱2012，Vol.30Issue(2)：146-153,8.DOI:10.3724/SP.J.1123.2011.10012
QuEChERS样品前处理-液相色谱-串联质谱法测定蔬菜中66种有机磷农药残留量方法评估
Evaluation of QuEChERS methods for the analysis of 66 organophosphorus pesticide residues in vegetables by liquid chromatography-tandem mass spectrometry
摘要
Abstract
A comparison was made between the two versions of QuEChERS sample preparation method for the extraction of 66 organophosphorus pesticides (OPPS) in vegetables. The two QuEChERS methods were the original method without buffer published in 2003, and the AOAC Official Method 2007. 01 with acetate buffer. The adsorption behaviors of primary secondary amine (PSA) sorbent and C18 sorbent on the OPPS were studied. The method of after-extraction addition was used to evaluate matrix effects for OPPS in matrix of broccoli, tomato, green soybean, radish and shallot during liquid chromatography-tandem mass spectrometry (LC-MS/ MS) analysis. As a result, the QuEChERS method with acetate buffer gave higher and more consistent recoveries for some of OPPS. The PSA sorbent and C18 sorbent can adsorb dibrom, so the QuEChERS method was not suitable for the analysis of dibrom. The maximum matrix effects were in the extracts of broccoli during LC-MS/MS analysis. In this article, OPPS were extracted using the QuEChERS method with acetate buffer, and analysed by LC-MS/MS under the optimized conditions with monitoring 132 MS/MS transitions of precursor ions (two for each pesticide) in one single run. Recoveries for all but dibrom at fortification levels of 10, 40,80 μg/kg in broccoli, tomato, green soybean, radish and shallot ranged from 55% to 122% with relative standard deviations of 1. 6% - 18%. The limits of quantification (S/N≥10) were 0. 1 -8 μg/kg. Based on these results, the analytical method was proven to be highly efficient, robust and sensitive, and suitable for the monitoring of the maximum residue limits (MRLs) of 66 OPPS in vegetables.关键词
QuEChERS/液相色谱-串联质谱/有机磷农药/蔬菜/基质效应/吸附Key words
QuEChERS/liquid chromatography-tandem mass spectrometry ( LC-MS/MS)/organophosphorus pesticides (OPPS)/vegetable/matrix effects/adsorption分类
化学化工引用本文复制引用
王连珠,周昱,陈泳,王瑞龙,林子旭,林德娟,郑少惠..QuEChERS样品前处理-液相色谱-串联质谱法测定蔬菜中66种有机磷农药残留量方法评估[J].色谱,2012,30(2):146-153,8.基金项目
福建省自然科学基金项目(2011J01386). （2011J01386）
