Determination of Residual Imidacloprid in Vegetables and Fruits by Spe and GC-MS
摘 要
研究了固相萃取(SPE)-气相色谱(GC)-质谱联用(MS)方法测定吡虫啉在蔬菜水果中残留量的方法.样品用乙腈均质提取,二氯甲烷定容.回收率为80.0%~89.0%,相对标准偏差<5.5%,检出限为0.006 3 mg·kg-1.
Abstract
Hyphenated GC-MS was applied to the determination of residual imidacloprid in vegetables and fruits. The sample was pretreated and the imidocloprid was extracted with acetonitrile. After filtration,an aliquot of the acetonitrile solution was taken and evaporated to dryness. Two mL of CH2Cl2 was added to the residue,and the solution was separated on the florisil solid-phase extraction column. The eluate was taken and ready for GC-MS analysis after evaporation to dryness and taking up the residue with 2.0 mL of CH2Cl2. The operation conditions of GC-MS analysis were optimized and the selected ion mode (SIM) was taken. Limit of detection obtained by the proposed method was 0.006 3 mg·kg-1,which is much lower then those required by some foriegn standards. In the analysis of samples of rape and frozen taro by this method,RSD′s found were less than 5.5%,and recoveries in the range of 80.0%-89.0% were obtained.
中图分类号 O637.37
所属栏目 工作简报
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收稿日期 2005/4/6
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备注刘永波(1977-),男,山东昌邑人,硕士,工程师,主要从事气相色谱、气质联机的开发与应用.
引用该论文: LIU Yong-bo,LIU Hai-shan,WANG Hong-fang. Determination of Residual Imidacloprid in Vegetables and Fruits by Spe and GC-MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2007, 43(1): 23~25
刘永波,刘海山,王红芳. 固相萃取-气相色谱-质谱联用法测定蔬菜、水果中吡虫啉残留量[J]. 理化检验-化学分册, 2007, 43(1): 23~25
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参考文献
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【3】Amadeo R,Fernandez-Alba,Antonio Valverde,et al. Determination of imidacloprid in vegetable samples by high-performance liquid chromatography with diode-array detection[J]. J Chromatogr A,1996(721):97.
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【5】Vilchez J L,El-Khattabi R. Determination of imidacloprid in water and soil samples by gas chromatography–mass spectrometry[J]. J Chromatagr A,1996(746):289.
【6】林维宣.各国食品中农兽药残留限量规定[M].大连:大连海事大学出版社. 2002.
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