QuEChERS-高效液相色谱-串联质谱法测定水产品中乙撑硫脲残留  

Determination of Ethylenethiourea Residues in Aquatic Products Using QuE ChE RS-High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：郑坤明 徐佳 陈源 陈冬花 卢平[2] 张钰萍[2] 胡德禹[2] ZHENG Kun-ming;XU Jia;CHEN Yuan;CHEN Dong-hua;LU Ping;ZHANG Yu-ping;HU De-yu(Fujian CCIC-Faifrreach Food Safety Testing Co.,Ltd.,Fuzhou 350000,China;Research and Development Center for Fine Chemicals,State Key Laboratory Breeding Base of Green Pesticide and Agricultural Bioengineering,Key Laboratory of Green Pesticide and Agricultural Bioengineering,Ministry of Education,Guizhou University,Guiyang 550025,China)

机构地区：[1]福建中检华日食品安全检测有限公司,福州350028 [2]贵州大学,精细化工研究开发中心绿色农药与农业生物工程国家重点实验室培育基地和教育部重点实验室,贵阳550025

出　　处：《农药》2020年第8期582-585,共4页Agrochemicals

基　　金：国家自然科学基金(21667007);贵州省科技计划项目(黔科合支撑[2019]2347号)。

摘　　要：[目的]建立水产品中乙撑硫脲残留量的高效液相色谱-串联质谱(LC-MS/MS)检测分析方法。[方法]采用QuEChERS的前处理方法,样品用1%氨水的乙腈提取,经PSA和GCB净化,通过Eclipse XDB-C18色谱柱分离,采用多反应监测模式(MRM)检测,并用外标法定量。[结果]在优化的条件下,乙撑硫脲相关系数R2大于0.999,其在花蛤、小龙虾、鲤鱼中的回收率为79.8%~102.6%,相对标准偏差均小于4%,检出限分别为0.001、0.003、0.002 mg/kg。[结论]该方法简捷、准确,可达到乙撑硫脲在水产品中的残留检测要求。[Aims]This study aims to develop adetermination and analysis method of ethylenethiourea in aquatic products with liquid chromatography-tandem mass spectrometry(LC-MS/MS).[Methods]The samples were extracted with 1%ammonia acetonitrile,and cleaned up by PSA and GCB,separated on a Eclipse XDB-C18,detected under multiple reactions monitoring(MRM)mode,quantifiedwithexternal standard calibration curves.[Results]Satisfactory linearity(R2≥0.999)of the method were obtained for all analytes,the average recoveries were 79.8-102.6%,the relative standard deviations were less than 4%in clam,crayfish and carp.The limits of detection of ethylenethiourea in three matrices were 0.001,0.003 and 0.002 mg/kg,respectively.[Conclusions]This method is simple and accurate,suitable for rapid determination and analysis of ethylenethiourea in aquatic products.

关 键 词：乙撑硫脲 高效液相色谱-串联质谱 花蛤 小龙虾 鲤鱼 残留 

分 类 号：TQ450.2[化学工程—农药化工]