高效液相色谱-串联质谱同位素内标法测定茶叶中25种有机磷农药残留  

Determination of 25 organophosphorus pesticide residues in tea by isotope-labelled internal standard quantitation and high performance liquid chromatography tandem mass spectrometry

作　　者：王敏[1] 韩芳[2,3] 张蕾[2] 金葆康[1] 郑平[2,3] 胡艳云[2,3] 宋伟[2] 吕亚宁[2] 

机构地区：[1]安徽大学化学化工学院,合肥230039 [2]安徽出入境检验检疫局,合肥230022 [3]食品安全分析与检测安徽省重点实验室,合肥230022

出　　处：《分析试验室》2013年第4期76-81,共6页Chinese Journal of Analysis Laboratory

基　　金：安徽省科研公关项目(1106c080536);国家质检总局科研项目(2008IK174;2009IK166)资助

摘　　要：建立了以同位素为内标同时测定茶叶中25种有机磷类农药残留的高效液相色谱-串联质谱(LC-MS/MS)方法。茶叶样品经乙酸乙酯-正己烷提取,氨基石墨化炭黑固相萃取柱净化,氘代二嗪农同位素内标校正,采用多反应监测模式,液相色谱-电喷雾质谱法测定。比较了三种同位素内标物,实验结果表明,使用氘代二嗪农为内标物对所有的有机磷都有良好的基质校正效果,目标物的平均回收率为70%～108%,相对标准偏差(RSDs)为2.5%～11%,方法的定量限(LOQs)均小于8.0μg/kg,所有分析物的线性关系良好,相关系数都大于0.997。该方法可满足茶叶样品中多种痕量有机磷农药残留的分析要求。A sensitive and effective isotope-labelled internal standard method for rapid determination of 25organophosphorus pesticides in tea has been developed. The sample was extracted by mixture of ethyl acetate and n-hexane, purified using Carb-NH2 solid phase extraction （SPE） cartridges and high performance liquid chromatography tandem mass spectrometric （LC-MS/MS） detection. For accurate quantitative analysis, three isotope-labelled organophosphorus were compared, and stable Diazinon-dl0was chosen as the internal standard at last. The average recoveries of each pesticide were 70% ~ 108% at three spiked concentration levels, and the relative standard deviations （RSDs） were between 2.5 % and 11.3 % , the limits of quantitation （LOQs） were all below 8.0 μg/kg, and good linear relationships were observed with the correlation coefficients r2 〉 0. 997 for all analytes. The recovery, repeatability of method can meet analysis requirements of organophosphorns residues in tea.

关 键 词：茶叶 有机磷类农残 同位素内标 高效液相色谱串联质谱法 固相萃取法 

分 类 号：O657.63[理学—分析化学]