高效液相色谱-串联质谱法同时测定蔬菜中4种杀菌剂的残留量  

Simultaneous Determination of 4 Fungicides in Vegetables by High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：王玉健 庞道标 黄惠玲 徐志伟 庄鹏 董存柱[2] 

机构地区：[1]海南出入境检验栓疫局检验检疫技术中心,海口570311 [2]海南大学环境与植物保护学院,海口570228

出　　处：《食品工业》2015年第5期290-295,共6页The Food Industry

基　　金：国家自然科学基金项目(31360447);国家质检总局科技计划项目(2013IK153);海南省重点科技计划项目(ZDXM20120039,ZDXM20120040);海南省自然科学基金项目(212018);海南出入境检验检疫局科研项目(HIKJ2007-05)

摘　　要：建立了高效液相色谱-串联质谱法同时测定蔬菜中多效唑、甲霜灵、硫菌灵、甲基硫菌灵等4种杀菌剂残留量的方法,对提取条件、流动相、质谱条件进行研究,并对质谱断裂机理进行了初步推断。待测样品采用Qu ECh ERS法前处理,直接用乙腈提取,采用电喷雾离子源（ESI）、多反应监测正离子模式扫描,外标法定量。目标化合物在1~20 ng/m L范围内质量浓度与峰面积呈良好的线性关系,方法的检出限为0.005 mg/kg。茄子、西红柿、辣椒等样品中添加水平为0.005,0.010和0.020 mg/kg时,4种杀菌剂的平均回收率范围分别为94.0%~104%,相对标准偏差为3.29%~12.1%。方法快速、简便、准确,可用于蔬菜中多效唑、甲霜灵、硫菌灵、甲基硫菌灵等4种杀菌剂残留量的定性、定量检测。A high performance liquid chromatography tandem mass spectrometry method was established for the simultaneous determination of four fungicides, including paclobutmzol, metalaxyl, thiophanate-ethyl and thiophanate-methyl in vegetables. The effect of extmtion condition, mobile phase, and tandem mass spectrometry parameters were investigated. And the possible fragmentation mechanisms of fungicides were presumed. The sample was pretreated by QuEChERS method and extracted with acetonilrile. The analysis was carried out under the multiple reaction monitoring （MRM） mode by employing external standard method. The calibration curves were linear in the range of 1-20 ng/mL. The limits of detection （LOD） were 0.005 mg/kg. The average recoveries of targeted compounds in eggplant, tomato and chili were between 94.0% and 104% at spiked levels of 0.005, 0.010 and 0.020 mg/ kg with relative standard derivation （RSDs） of 3.29%~12.1%. The method was fast, convenient, accurate. And it could be used as a reliable means for simultaneous quantitative determination of four targeted fungicides in vegetables.

关 键 词：多效唑 甲霜灵 硫菌灵 甲基硫菌灵 蔬菜 高效液相色谱-串联质谱 断裂机理 

分 类 号：TS255.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]