液相色谱-串联质谱法测定果蔬中的涕灭威及其代谢物

Determination of Aldicarb and Its Metabolites in Fruits and Vegetables by Liquid Chromatography-Tandem Mass Spectrometry

[目的]建立液相色谱-串联质谱法(LC/MS)测定果蔬(番茄、黄瓜、韭菜、马铃薯、西瓜、苹果和橙子)中涕灭威及其代谢物的分析方法。[方法]样品经组织捣碎,乙腈提取,经氨基柱和二氯甲烷+甲醇(95∶5)净化洗脱处理,2 mL甲醇定容,采用Phenomenex H 18色谱柱分离。[结果]涕灭威及其代谢物在0.01和0.02 mg/kg 2个添加水平下回收率均为84.667%~104.333%,RSD均为0~5.37%,试验方法检出限为0.01 mg/kg,相关系数均大于0.9993。[结论]该方法操作简便、快捷,安全性高,只通过一种检测方法便可同时测定果蔬中涕灭威及其代谢物的残留量,准确度和灵敏度高,定量下限低于或等于国家农药残留限量标准。

[Objective]To establish a method for the aldicarb and its metabolites detection of 7 vegetables and fruits(tomato,cucumber,leek,potato,watermelon,apple,and orange)by liquid chromatography-tandem mass spectrometry.[Method]The samples were mashed,and then extracted with acetonitrile,the extraction was purified by the amino column and dichloromethane+methanol(95∶5).After constant volume with 2 mL methanol,the target analytes were separated on a Phenomenex H 18 column.[Result]The recovery rates of aldicarb and its metabolites were 84.667%-104.333%,RSD were 0-5.37%at two added levels of 0.01 and 0.02 mg/kg.The detection limit of the experimental method was 0.01 mg/kg.The correlation coefficients were all greater than 0.9993.[Conclusion]The method is simple,fast and safe.It can simultaneously determine aldicarb and its metabolites in vegetables and fruits with only one detection method.The accuracy and sensitivity are high,and the lower limit of quantification is less than or equal to national pesticide residue limit standards.