液相色谱-串联质谱法同时测定红茶和绿茶中7种硫代氨基甲酸酯类除草剂  

Determination of Seven Thiocarbamate Herbicides in Black Tea and Green Tea by Liquid Chromatography Coupled with Tandem Mass Spectrometry Detection

作　　者：沈金灿[1] 谢丽琪[1] 肖来龙[1] 靳宝辉[1] 叶刚[1] 肖陈贵[1] 

机构地区：[1]深圳出入境检验检疫局食品检验检疫技术中心,深圳518067

出　　处：《分析化学》2009年第12期1795-1799,共5页Chinese Journal of Analytical Chemistry

基　　金：十一五国家支撑计划分课题(No.2006BAK02A08-x);深圳出入境检验检疫局博士资金(No.SZ2007106)项目资助

摘　　要：建立了红茶和绿茶中7种硫代氨基甲酸酯类除草剂(禾草敌、克草敌、灭草敌、野麦畏、禾草丹、茵草敌和丁草敌)的高效液相色谱-串联质谱(LC-MS/MS)检测方法。样品制备后,取2.0 g样品,加6 mL水浸润1 h。然后加入2.5 g NaCl,并用20 mL乙腈分两次进行提取,提取液吹氮浓缩后过HLB柱,并用3 mL乙腈洗脱。洗脱液浓缩后用2.0 mL正己烷-丙酮(7∶3,V/V)溶解残渣,然后过Envi-Carb固相萃取柱,再用5 mL正己烷-丙酮洗脱,洗脱液浓缩后用乙腈-水(5∶5,V/V)定容。采用LC-MS/MS电喷雾电离,多反应监测模式对样品进行分析。以D3-甲萘威为内标,测定7种硫代氨基甲酸酯除草剂的线性范围为0～200μg/L,线性相关系数在0.9954～0.9988范围内,检出限在0.093～1.77μg/L范围内。在添加浓度5～20μg/kg范围内,7种硫代氨基甲酸酯除草剂的回收率均在77.3%～91.5%,相对标准偏差(RSD)小于15%。本方法被成功用于红茶和绿茶样品中硫代氨基甲酸酯除草剂的测定。A method for the determination of seven kinds of thiocarbamate herbicides, molinate, pebulate, vernolate, triallate, thibencarb, eradicane and butylate in black tea and green tea has been developed. After homogenization, 2.0g tea sample was soaked with 6 mL water for 1 h. 2.5g NaCl was then added, and the sample was extracted twice by 20 mL acetonitrile. After concentration, the extract was put through HLB column and eluted by 3 mL aeetonitrile. The eluate was then concentrated and dissolved with 2.0 mL hexane-acetone （7：3, V/V） mixture. The preparation was cleaned by Envi-Carb column and eluted with 5 mL hexane-acetone. After concentration, the residue was dissolved by acetonitrile-water （5：5, V/V） solution. Detection was achieved by electrospray ionization （ESI） in positive mode using multiple reaction monitoring. D3-carbaryl was used as the internal standard, the linear range for the herbicides was 0-200μg/L and the limit of detection were from 0.093 to 1.77μg/L, with the correlation coefficients（r） varying from 0.9954 to 0.9988. The recoveries of all thiocarbamate herbicides were from 77.3% to 91.5% at the spiked levels of 5-20μg/kg. The RSD of each compound was less than 15%. Black tea and green tea samples were success- fully analyzed by the proposed method with satisfactory results.

关 键 词：硫代氨基甲酸酯 除草剂 液相色谱 质谱 茶叶 

分 类 号：TS272.7[农业科学—茶叶生产加工]