In order to improve the efficiency and accuracy of pesticide residue detection in raw materials of troditional Chinese medicinal materials.To establish a rapid method for the determination of 154 kinds of pesticide residues in traditional Chinese medicinal materials by liquid chromatography-tandem mass spectrometry(LC-MS/MS)combined with automatic QuEChERS.The pretreatment conditions and in-strument conditions were optimized and the matrix effect was evaluated.The samples were added with water,then extracted with acetonitrile containing 1％(v/v)acetic acid,extracted and purified with automatic QuEChERS equipment,the purified solution is filtered through the fil-ter membrane,and determined by LC-MS/MS in multi-reaction monitoring(MRM)mode and quantified by matrix matching external stan-dard method.The linearities of 154 kinds of pesticides ranged from 2.0～100.0 μg/L,with correlation coefficients more than 0.999.The results showed that the recoveries for all compounds spiked at levels of 0.01、0.02、0.10 mg/kg,which were 60.7％～96.2％,68.3％～93.5％,and 64.2％～97.5％respectively,with relative standard deviations(RSDs)were 0.4％～8.3％、0.3％～4.9％、1.0％～10.4％.The method was applied to the determination of 56 batches of traditional Chinese medicinal materials.The results showed that pesticide residues were detected in 27 batches of traditional Chinese medicinal materials,and a total of 45 pesticides were detected,including the banned pesticides chlordimeform,terbufos and carbofuran in the Chinese pharmacopoeia.Therefore,the developed method was simple,rapid,sensitive and automatic,and was suitable for the rapid detection of pesticide residues in traditional Chinese medicinal materials.
关键词
中药材/农药多残留分析/全自动QuEChERS/液相色谱-串联质谱法
Key words
Chinese traditional medicinal materials/pesticide multi-residue analysis/automatic QuEChERS/liquid chromatography-tan-demmass spectrometry
维普
万方数据