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[离线分散固相萃取-气相色谱-串联质谱法测定蔬菜中107种农药残留]

[Determination of 107 pesticide residues in vegetables using off-line dispersive solid-phase extraction and gas chromatography-tandem mass spectrometry].

作者信息

Shen Weijian, Yu Keyao, Gui Qianwen, Jiang Yuan, Zhao Zengyun, Shen Chongyu, Wu Bin, Chu Xiaogang

机构信息

Food Laboratory of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing, China.

出版信息

Se Pu. 2009 Jul;27(4):391-400.

PMID:19938491
Abstract

A screening method was developed for the determination of 107 pesticide residues in vegetables using off-line dispersive solid-phase extraction (DSPE) and gas chromatography-tandem mass spectrometry (GC-MS/MS). The pesticides interested were extracted from the samples with acetonitrile (saturated by n-hexane) containing 1% acetic acid and simultaneously separated by liquid-liquid partitioning with adding anhydrous magnesium sulfate plus sodium acetate following by a simple cleanup step known as dispersive solid-phase extraction. The extracts were determined by GC-MS/MS using external standard method. The method was reliable and stable that the recoveries of almost all pesticides were in the range from 60% to 130% at the spiked level of 10 microg/kg into four vegetable matrixes (garlic, green bean, radish 8 and spinach) and the relative standard deviations (RSDs) were all not more than 15.3%. The linearity of the method was good between 0.05 mg/L and 1 mg/L, and all limits of quantification (LOQs) less than 10 microg/kg. The method is selective with no interference, especially in the complicated garlic matrix.

摘要

建立了一种采用离线分散固相萃取(DSPE)和气相色谱 - 串联质谱(GC - MS/MS)测定蔬菜中107种农药残留的筛查方法。用含1%乙酸的乙腈(正己烷饱和)从样品中提取目标农药,加入无水硫酸镁和乙酸钠进行液 - 液分配同时分离,随后通过称为分散固相萃取的简单净化步骤进行处理。提取物采用外标法通过GC - MS/MS测定。该方法可靠且稳定,在四种蔬菜基质(大蒜、绿豆、萝卜和菠菜)中添加水平为10μg/kg时,几乎所有农药的回收率在60%至130%之间,相对标准偏差(RSD)均不超过15.3%。该方法在0.05mg/L至1mg/L之间线性良好,所有定量限均小于10μg/kg。该方法具有选择性,无干扰,特别是在复杂的大蒜基质中。

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