超高效液相色谱-串联质谱法测定中草药中氨基甲酸酯类农药残留量  

UPLC-MS/MS determination of carbamate pesticides in traditional Chinese medicine

作　　者：李娜[1] 刘磊[1] 邵辉[1] 李辉[1] 张玉婷[1] 宋海菲[1] 郭永泽[1] 

机构地区：[1]天津市农业科学院中心实验室,天津300381

出　　处：《药物分析杂志》2011年第12期2266-2272,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：国家重大专项子课题(2009ZX09502-027-2)项目资助

摘　　要：目的:结合固相萃取技术,克服了中草药样品中复杂的基质干扰问题,建立超高效液相色谱-串联质谱(UPLC-MS/MS)法检测中药材中15种氨基甲酸酯类杀虫剂的残留量。方法:样品中残留的农药经乙腈提取,PSA固相萃取柱净化后,采用UPLC-MS/MS法进行测定。结果:15种农药在其各自的浓度范围内,线性关系良好,相关系数在0.995～0.999之间。在定量限(LOQ)、5倍定量限和10倍定量限3个添加浓度水平,平均加标回收率在61.8%～98.1%之间;RSD在1.8%～14.8%之间。结论:该方法操作简便,净化效果好,灵敏度高,可为中药材中氨基甲酸酯类杀虫剂污染状况调查提供检测方法支持。Objective：An ultra performance liquid chromatography-tandem mass spectrometric method was developed for the determination of 15 carbamate pesticides in traditional Chinese medicine.Method：Pesticides were extracted with acetonitrile,cleaned up by PSA solid phase extraction column,and then analyzed by UPLC-MS/MS.Result：The standard calibration curves for 15 carbamate pesticides showed high correlation coefficient（0.995-0.999） over their respective concentration range.The average recovery of 15 carbamate pesticides at the three fortification levels（LOQ,5 LOQ and 10 LOQ） was between 61.8% and 98.1% with the relative standard deviation between 1.8% and 14.8%.Conclusion：It was indicated that the method developed in this study is easier,more sensitive and has a better purification effect.So,this method can be further applied to investigate the contamination status of traditional Chinese medicine by the carbamate pesticides.

关 键 词：氨基甲酸酯类 中草药 农药残留 超高效液相色谱-串联质谱法 

分 类 号：R917[医药卫生—药物分析学]