高效液相色谱-串联质谱法测定蔬菜中氯虫苯甲酰胺和氟虫双酰胺残留  

Determination of Flubendiamide and Chlorantraniliprole Residues in Vegetables Using Liquid Chromatography-Tandem Mass Spectrometry

作　　者：钱鸣蓉[1] 章虎[1] 吴俐勤[1] 刘飞 王祥云[1] 何红梅[1] 陈志民[1] 

机构地区：[1]浙江省农业科学院农产品质量标准研究所,杭州310021 [2]赛默飞世尔科技(中国)有限公司色谱质谱部,上海201206

出　　处：《分析化学》2010年第5期702-706,共5页Chinese Journal of Analytical Chemistry

基　　金：浙江省重大科技攻关项目(No.2005C12007);杭州市科技发展计划(No.20080632B08)资助

摘　　要：建立了蔬菜中氯虫苯甲酰胺和氟虫双酰胺残留量的高效液相色谱-串联质谱同时分析方法。蔬菜样品加入乙腈高速匀浆,提取液中加入无水MgSO4和NaCl,振荡离心后,取上清液稀释后直接进样,液相色谱-串联质谱电喷雾正离子扫描同时分析氯虫苯甲酰胺和氟虫双酰胺。以甘蓝、白菜、黄瓜、辣椒、番茄和茭白6种蔬菜为基质进行4个添加水平和5次重复性实验,结果表明,添加浓度为0.01～5mg/kg,蔬菜中氯虫苯甲酰胺和氟虫双酰胺添加回收率为85.4%～105%,相对标准偏差(RSD,n=5)为2.5%～12%,氯虫苯甲酰胺和氟虫双酰胺的方法检出限(LOD)分别为0.0003和0.002mg/kg,定量限(LOQ)分别为0.001和0.006mg/kg。本方法操作简单,灵敏度、回收率和重复性均良好。An analytical method to determine chlorantraniliprole and flubendiamide residues in vegetables by high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） was developed. The acetonitrile was added into the vegetable samples to extract chlorantraniliprole and flubendiamide residues. Then the mixture was homogenized with high speed and added with some anhydrous magnesium sulfate and sodium chloride. After shaking thoroughly and centrifugation, the upper layer was transferred and diluted for direct analysis. HPLC-MS/MS with electriospray in positive ion scan mode was used to determine chlorantraniliprole and flubendiamide simultaneously. The fortified recoveries of chlorantraniliprole and flubendiamide in vegetable matrices including cabbage, Chinese cabbage, cucumber, pepper, tomato and wild rice stem were 85.4%-105% at fortification levels ranging from 0.01 mg/kg to 5 mg/kg. Relative standard deviations were 2.5%-12%（n=5）. The limit of detection was 0.0003 mg/kg for chlorantraniliprole and 0.002 mg/kg for flubendiamide. The LOQ was 0.001 mg/kg for chlorantraniliprole and 0.006 mg/kg for flubendiamide. The method has the advantage of simplicity, repeatability and sensitivity.

关 键 词：氯虫苯甲酰胺 氟虫双酰胺 高效液相色谱-串联质谱 残留 

分 类 号：TS255.5[轻工技术与工程—农产品加工及贮藏工程]