高效液相色谱串联质谱法分析水和饮料中13种常见农药  

Analysis of Thirteen Pesticides in Water and Beverages by LC-MS/MS

作　　者：叶海英[1] 梁晨[1] 吴忠平[1] 陈永生[1] 张玉荣[1] 

机构地区：[1]上海市公安局刑事科学技术研究管理中心,上海市现场物证重点实验室,上海200083

出　　处：《农药》2012年第1期47-50,共4页Agrochemicals

基　　金：上海市科技攻关项目(052112036)

摘　　要：[目的]建立利用液相色谱串联质谱法检测水和6种饮料中13种常见农药的分析方法。[方法]空白检材加入内标和13种农药混标后用乙腈提取,离心后取上清液直接进样分析。液相色谱采用C18色谱柱,流动相用含甲酸铵和甲酸的水、乙腈梯度洗脱,质谱采用电喷雾离子源(ESI),正离子多反应监测(MRM)模式扫描。[结果]13种农药的检测限为0.1～50μg/L;日内及日间精密度均在15%以下。[结论]方法简便、快速、灵敏、选择性高,可应用于实际案例的分析。[Aims] To establish a method for the simultaneous analysis of 13 pesticides in water and 6 beverages by liquid chromatography tandem mass spectrum （LC-MS/MS）. [Methods] After spiking the internal standard and 13 pesticides standard mixture to the blank water and blank beverage, the samples were extracted by acetonitrile and centrifugated. The supernatant was injected to the apparatus directly. The samples were separated by the C18 column with water and acetonitrile （both contained ammonium formate and formic acid） as the mobile phase using gradient elution method. The positive electric spray ionization（ESI） mode was adopted and multiple reaction monitoring （MRM） mode was used to analyze target compounds. [Results] The limits of detection（LOD） ranged from 0.1 to 50 μg/L, and the deviation of intra- and inter- day precision were less than 15%. [Conclusions] This newly developed method is simple, rapid, sensitive and has high selectivity, which is suitable for analysis of the actual cases.

关 键 词：高效液相色谱串联质谱 农药 饮料 水 

分 类 号：O657.63[理学—分析化学] O661.1[理学—化学] R123.1[医药卫生—环境卫生学]