Multiresidue method for determination of 90 pesticides in fresh fruits and vegetables using solid-phase extraction and gas chromatography-mass spectrometry
Multiresidue method for determination of 90 pesticides in fresh fruits and vegetables using solid-phase extraction and gas chromatography-mass spectrometry
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DOI：
10.1016/s0021-9673(03)01211-1
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发表时间：
2003-10-10
影响因子：
4.1
通讯作者：
Zupancic-Kralj, L
中科院分区：
文献类型：
--
作者：
Stajnbaher, D;Zupancic-Kralj, L
建立了果蔬中90种不同理化性质农药的多残留分析方法。该方法涉及使用涡旋混合的丙酮的快速和小规模提取程序。采用高交联聚苯乙烯-二乙烯基苯柱（LiChrolut EN）固相萃取（SPE）对水稀释的丙酮提取液中的农药进行净化和预浓缩。对于大多数水果和蔬菜样品来说，这种部分净化是足够的，但其中一些含有更多共提取物质的样品需要进一步净化（谷物、菠菜、胡萝卜等）。采用二乙氨丙基（DEA）改性硅胶，有效去除有机酸、糖类等有机物的干扰，采用气相色谱-质量选择检测器（GC-MS）测定农药残留。在0.01 ~ 0.50 mg/kg浓度范围内，除大多数极性农药（甲胺磷、乙酰甲胺磷、氧乐果）不能用该方法测定外，大多数水果和蔬菜的农药回收率均>80%。大多数农药的定量限为0.01 mg/kg，大多数相对标准偏差（R.S.D.s）低于10%。(C)2003 Elsevier B. V.保留所有权利。
A multiresidue method for analysis of 90 pesticides with different physico-chemical properties in fruits and vegetables was developed. The method involves a rapid and small-scale extraction procedure with acetone using vortex mixing. Solid-phase extraction (SPE) on a highly cross-linked polystyrene divinylbenzene column (LiChrolut EN) was used for clean-up and pre-concentration of the pesticides from the water-diluted acetone extracts. For most fruit and vegetable samples this partial clean-up was sufficient, but some of them with more co-extracting substances need further clean-up (cereals, spinach, carrots, etc.). Diethylaminopropyl (DEA) modified silica was used for efficient removal of interferences caused by various organic acids, sugars, etc. The pesticide residues were determined by gas chromatography with a mass selective detector (GC-MS). The majority of pesticide recoveries for various fruits and vegetables were >80% in the concentration range from 0.01 to 0.50 mg/kg, except for the most polar pesticides (methamidophos, acephate, omethoate) which cannot be determined by this method. The limit of quantitation for most of the pesticides was 0.01 mg/kg with majority of relative standard deviations (R.S.D.s) below 10%. (C) 2003 Elsevier B.V. All rights reserved.