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一种改良的 QuEChERS 提取和气相色谱-串联质谱法测定大米中 124 种农药的多残留方法。

A multi-residue method for the determination of 124 pesticides in rice by modified QuEChERS extraction and gas chromatography-tandem mass spectrometry.

机构信息

Center of Analysis and Testing, Sichuan Academy of Agricultural Sciences, Chengdu, Sichuan 610066, China.

出版信息

Food Chem. 2013 Jun 1;138(2-3):1198-205. doi: 10.1016/j.foodchem.2012.11.089. Epub 2012 Nov 28.

Abstract

A modified QuEChERS method for simultaneous determination of 124 pesticide residues in rice was established and validated. The rice samples were initially extracted with acetonitrile (MeCN), and the targeted pesticides were purified following the dispersive solid phase extraction (d-SPE) cleanup method and detected by gas chromatography-tandem mass spectrometry (GC-MS/MS). The efficiency of citrate-buffered and unbuffered method in liquid extraction procedure was compared; the amount of primary secondary amine (PSA) was optimised. In the method validation, correlation coefficients (r(2)) were higher than 0.990 with the linear ranging from 10 to 200 μg kg(-1). At the fortification levels of 20-200 μg kg(-1), average recoveries ranged from 70% to 122.7% with the RSD <20%.

摘要

建立并验证了一种改良的 QuEChERS 方法,用于同时测定大米中的 124 种农药残留。大米样品最初用乙腈(MeCN)提取,目标农药通过分散固相萃取(d-SPE)净化方法进行净化,并用气相色谱-串联质谱(GC-MS/MS)检测。比较了柠檬酸缓冲和非缓冲方法在液体提取过程中的效率,优化了仲胺(PSA)的用量。在方法验证中,线性范围为 10-200μgkg-1 时,相关系数(r(2))均高于 0.990。在 20-200μgkg-1 的添加水平下,平均回收率在 70%-122.7%之间,RSD<20%。

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