QuEChERS结合在线GPC-GC-MS/MS法测定川牛膝中24种农药残留

Determination of 24 Pesticides in Chuan Niuxi (Cyathulae Radix) by QuEChERS-Online Gel Permeation Chromatography Coupled with Gas Chromatography-Mass Spectrometry

目的:建立QuEChERS结合在线凝胶渗透色谱-气相色谱-串联质谱法(GPC-GC-MS/MS法)测定川牛膝中24种农药残留的方法。方法:粉碎混匀后的川牛膝样品经乙腈提取,采用QuEChERS净化处理,以在线凝胶渗透色谱气质联用法进行分析,用农药残留的特征碎片离子建立气质联用检测条件,采用内标法定量。结果:在0.0~0.5μg/mL质量浓度范围内,线性关系良好,24种农药残留检测限范围为0.001~0.008 mg/kg,定量限为0.003~0.020 mg/kg,回收率为68.4%~111.9%,相对标准偏差为0.7%~8.8%。结论:该方法操作简便、批量处理时间短、定性定量准确、灵敏度高,适合道地药材川牛膝中农药残留的检测。

Object:A method for the simultaneous determination of 24 pesticides in Chuan Niuxi(Cyathulae Radix)by QuEChERS coupled with online gel permeation chromatography-gas chromatography-mass spectrometry(GPC-GC-MS/MS)was developed.Methods:Chuan Niuxi(Cyathulae Radix)powder was extracted with acetonitrile and purified by QuEChERS method.The identification and quantification were performed by GPC-GC/MSMS in MRM mode and internal standard method,to evaluate the method from the recovery,precision,detection limit and actual samples respectively.Results:The linear relationship was good with the mass concentration range from 0.0μg/mL to 0.5μg/mL.The average recoveries of pesticide residues in Chuan Niuxi(Cyathulae Radix)ranged from 68.4%to 111.9%at different spiked levels with relative standard deviation between 0.7%to 8.8%.The limits of detection of the method was 0.001-0.008 mg/kg and the limit of quantitation was 0.003-0.020 mg/kg.Conclusion:The method is easy to operate,short in batch processing time,accurate in qualitative and quantitative analysis,and high in sensitivity.It is suitable for the determination of pesticide residues in Chuan Niuxi(Cyathulae Radix).