超高效液相色谱-串联质谱法测定人参、黄芪中多种除草剂残留量  

Determination of 55 Herbicides in ginseng and milkvetch root by UPLC-MS/MS

作　　者：张玉婷[1] 李娜[1] 邵辉[1] 刘磊[1] 李辉[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：《分析试验室》2011年第8期27-32,共6页Chinese Journal of Analysis Laboratory

基　　金：国家重大专项子课题(2009ZX09502-027-2)资助

摘　　要：建立了人参和黄芪中55种除草剂残留量的超高效液相色谱-串联质谱检测方法。样品中残留的药物经乙腈提取,石墨化碳黑固相萃取柱净化,甲醇-二氯甲烷洗脱,最后采用电喷雾串联质谱在正离子多反应监测模式下进行测定。55种农药的检测限和定量限分别为0.4～20μg/kg和2～100μg/kg。在各自的浓度范围内,55种药剂的线性关系良好,相关系数在0.992和0.999之间。在定量限(LOQ)和10倍定量限两个浓度水平做添加回收率试验,平均加标回收率在73.4%～95.4%之间;RSD在1.8%～15%之间,符合多残留分析的要求。可为中药材中除草剂的污染状况调查提供检测方法支持。An ultra performance liquid chromatography-tandem mass spectrometric method was developed for the determination of 55 herbicides in ginseng and milkvetch root.The pesticides were extracted with acetonitrile,cleaned-up by an ENVI-Carbon solid phase extraction cartridge,eluted with methanol-dichlormethane,and finally analyzed by ultra performance liquid chromatography tandem mass spectrometry（UPLC-MS/MS） in multiple reaction monitoring（MRM） mode via positive electrospray ionization.The method was validated at two fortification levels in ginseng and milkvetch root.The validation results were as follows.The calibrations for the fifty-five herbicides all showed high correlation coefficients over their respective range,with the correlation coefficients between 0.992 and 0.999.The average recoveries of the fifty-five herbicides at the two fortification levels of LOQ and 10 LOQ were between 73.4% and 95.4%,with the relative standard deviations（RSD） between 1.8% and 15%.The limits of determination（S/N3） and the limits of quantification（S/N≥10） of all the herbicides were 0.4～20 μg/kg and 2～100 μg/kg.It is indicated that the method developed in this study is easy,sensitive and has a good purification effect.The sensitivity,accuracy and precision of the method are all acceptable,and it can meet the requirements of the multiple pesticides residue analysis.So,this method can be further applied to investigating the contamination status of traditional Chinese medicine by herbicides.

关 键 词：除草剂 人参 黄芪 超高效液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学]