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食品研究与开发:2016,37(9):152-155
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QuEChERS-UPLC-MS/MS法测定食品中 (Z)-和(E)-毒虫畏残留
陈其勇1,王飞1,宓捷波1,吴若昕2
(1. 天津出入境检验检疫局,天津 300456;2. 天津大学 材料科学与工程学院,天津 300072)
Determination of(Z)- and(E)-Chlorfenvinphos in Food by QuEChERS and UPLC-MS/MS
CHEN Qi-yong1, WANG Fei1, MI Jie-bo1, WU Ruo-xin2
(1. Tianjin Entry-Exit Inspection and Quarantine Bureau, Tianjin 300456, China; 2. School of Material Science and Engineering, Tianjin University, Tianjin 300072, China)
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投稿时间:2015-03-03    
中文摘要: 建立了食品中农药(Z)-和(E)-毒虫畏残留量的超高压液相色谱-串联质谱(UPLC-MS/MS)测定方法;样品采用 QuEChERS 法进行前处理;以 0.1 %甲酸水溶液为流动相,梯度洗脱及正离子源(ESI)电离方式,采用超高压液相色谱串联质谱仪在选择离子监测模式下进行快速测定,保留时间和离子相对丰度比定性、外标法定量;方法定量下限为0.02 mg/kg;毒虫畏(Z)-和(E)-两种同分异构体得到很好的分离。在大米、小麦 2 种粮谷类样品,卷心菜、苹果、洋葱、柑 橘 4 种蔬果类样品和猪肉、牛肾 2 种动物源食品中添加不同浓度的毒虫畏时,其平均添加回收率在 72.7 %~105.2 %之 间,相对标准偏差(n=10)小于 10 %。
Abstract:A UPLC-MS/MS method for the determination of (Z)- and (E)- chlorfenvinphos in food was es- tablished. Chlorfenvinphos in the targeted samples was extracted and cleaned up using QuEChERS. The mobile phase was ultrapure water with 0.1 % formic acid in it. Rapid analysis were carried out by ultra-performance liquid chromatography-tandem mass spectrometry under electrospray ionization (ESI) and operated in positive mode with gradient elute, qualitative analysis by the retention times and relative intensities of selected ions and quantitation by external standard. Determination limits of this method were 0.02 mg/kg. The mean recoveries ranged from 72.7 %-105.2 % of fortified samples of 2 grain cereals, which were rice and wheat, and 4 vegeta- bles and fruits, which were cabbage, apple, onion and orange, and 2 animal-derived food, that were pork and beef kidney, with RSD(n=10)less than10 %.
文章编号:201609035     中图分类号:    文献标志码:A
基金项目:天津检验检疫局科技计划项目(TK076-2013);国家认监委计划项目(2012B313r)
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