QuEChERS/GC-MS/MS测定人参中41种农药残留

Determination of 41 Kinds of Pesticide Residues in Ginseng by Gas Chromatography-Tandem Mass Spectrometry with QuEChERS

建立了QuEChERS结合气相色谱-串联质谱(GC-MS/MS)测定人参中41种农药残留的分析方法,采用选择反应监测(SRM)模式,外标法定量,并考察了Original、Acetate和Citrate 3种QuEChERS前处理方法对人参基质中目标农药的提取效率和净化效果。结果表明,采用Original QuEChERS前处理方法时,41种农药在一定浓度范围内的线性良好,相关系数(r)大于0.995,方法的检出限(LOD,S/N=3)为2.0~6.0μg/kg,定量下限(LOQ,S/N=10)为5.0~20.0μg/kg。在10、20、100、200μg/kg 4个加标水平下的回收率为86.7%~115%,相对标准偏差(RSD)均小于15%。该方法样品前处理简单、高效、准确、灵敏,适用于人参中多农药残留的筛选与测定。

A multi-residue analysis method was developed for the determination of 41 kinds of pesticides in ginseng by gas chromatography-tandem mass spectrometry(GC-MS/MS)with QuEChERS.The samples were extracted using three QuEChERS methods,i.e.original,acetate and citrate,respectively.The final extracts were evaluated by GC-MS/MS in selected reaction monitoring(SRM)mode,and quantified by external standard method.The extraction efficiency and purification effect of the three methods were investigated.Results showed that when the original QuEChERS method was selected,which was the most suitable for the tested pesticides,there were good linear relationships for the 41 pesticides in a certain concentration range,with their correlation coefficients(r)higher than 0.995.The limits of detection(LODs,S/N=3)and the limits of quantification(LOQs,S/N=10)of this method were between 2.0-6.0μg/kg and 5.0-20.0μg/kg,respectively.Recoveries at four spiked levels of 10,20,100 and 200μg/kg ranged from 86.7%-115%with the relative standard deviations(RSDs)less than 15%.The method is simple,effective,accurate and sensitive,and is applicable for the screening and detection of multi-pesticide residues in ginseng.