采用APGC-QTof建立中药材中71种常见农药的快速筛查法

Rapid screening and verification of 71 pesticide residues in Chinese medicinal materials by APGC-QTof

目的:利用高分辨质谱建立不同中药基质中71种适合气相分离农药的快速筛查方法。方法:选择西洋参、金银花、枸杞子、大枣和白花蛇舌草,分别代表根、花、果实、全草等不同基质类型的中药材样品,经简化QuEChERS法提取净化后,采用APGC/Xevo G2-XS QTof系统进行测定,结合UNIFI筛查平台建立71种常用农药的数据库,完成快速筛查分析。并通过分析不同中药基质中的假阳性率、假阴性率和检测限,验证方法的准确性。结果:经验证快速筛查方法在各样品基质中均能获得满意的假阳性率和假阴性率结果(<5%),94%以上农药检测灵敏度低于10μg·kg^(-1),符合农药多残留快速筛查方法的验证要求。结论:本研究通过APGC-QTof系统和UNIFI农药数据库,实现了在不需使用对照品对照的情况下即可完成对71种常用农药的快速筛查。所建立的前处理方法提取效率高,操作简便快捷,筛查方法灵敏度、准确性高,可用于上述5种中药中农药多残留的快速筛查。

Objective:To develop a rapid screening method for the simultaneous determination of 71 kinds of pesticide residues in Chinese medicinal materials based on the accurate mass.Methods:Panacis Quinquefolii Radix,Lonicerae Japonicae Flos,Lycii Fructus,Jujubae Fructus and Hedyotisdiffusa were chosen as typical samples,representing different matrix such as root,flower,fruit and whole grass,respectively.71 kinds of pesticides,which are representative and frequently-used in TCMs,were pointed as research indicators,and the simplified QuEChERS was applied to extract pesticide residues in the samples.And APGC/Xevo G2-XS QTof combining UNIFI scientific information system was used for data acquisition and analysis.Finally the accuracy of the method was verified by analyzing the false positive rate,false negative rate and the limit of detection in different Chinese medicinal materials.Results:The established rapid screening method offered satisfactory false positive and negative results(≤5%),and the limit of detection of 94% analytes was below 10 μg·kg^-1 which were in accordance with validation requirements of multi-residual rapid screening. Conclusion:In this study,through the combination of APGC-QTof and UNIFI chemical database,the effective and rapid screening of 71 kinds of pesticides has been achieved without the use of reference control. The pretreatment method is efficient and easy to operate.The screening method has high sensitivity and accuracy.And it can be used for rapid screening of pesticide residues in the five kinds of Chinese medicinal materials.