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采用分散固相萃取结合液相色谱-质谱法测定水果和蔬菜中的三嗪类除草剂。

Determination of triazine herbicides in fruits and vegetables using dispersive solid-phase extraction coupled with LC-MS.

作者信息

Ji Feng, Zhao Lixia, Yan Wei, Feng Qinzhong, Lin Jin-Ming

机构信息

State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing, China.

出版信息

J Sep Sci. 2008 Apr;31(6-7):961-8. doi: 10.1002/jssc.200700610.

Abstract

A simple, rapid, and sensitive liquid chromatography-mass spectrometry (LC-MS) method was successfully developed for the determination of three chloro-s-triazine herbicides, viz. atrazine, simazine, and propazine, two thiomethyl-s-triazine ones, viz. ametryn and prometryn, and prometon in fruits and vegetables. The instrumental parameters affecting LC separation and MS detection were investigated and the best conditions were selected. Samples were extracted and purified by dispersive solid-phase extraction (dispersive-SPE) with a primary-secondary amine sorbent. Three typical representative samples (luffa, broad bean, and grape) were selected to investigate the effect of different matrices on pesticide recoveries and assay precision after spiking at 0.05 mg/kg. Matrix composition did not interfere significantly with the determination of these pesticides. The recoveries were, with a few exceptions, in the range of 80-110% with relative standard deviations less than 10% (n = 5). In addition, this method was also applied to 21 different kinds of agriculture products collected from the local market, and two of the six triazines could be detected and quantified.

摘要

成功开发了一种简单、快速且灵敏的液相色谱-质谱联用(LC-MS)方法,用于测定水果和蔬菜中的三种氯代-s-三嗪类除草剂,即莠去津、西玛津和扑灭津,两种硫甲基-s-三嗪类除草剂,即莠灭净和扑草净,以及扑灭通。研究了影响LC分离和MS检测的仪器参数并选择了最佳条件。样品通过用伯仲胺吸附剂进行分散固相萃取(分散-SPE)来提取和净化。选择了三个典型代表性样品(丝瓜、蚕豆和葡萄),研究在0.05 mg/kg加标后不同基质对农药回收率和测定精密度的影响。基质组成对这些农药的测定没有显著干扰。除少数例外情况外,回收率在80%-110%范围内,相对标准偏差小于10%(n = 5)。此外,该方法还应用于从当地市场收集的21种不同农产品,六种三嗪类除草剂中的两种能够被检测和定量。

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