高效液相色谱-质谱联用法测定白芍药材中23种农药残留

Determination of 23 pesticide residues in Paeoniae radix Alba using high performance liquid chromatography coupled with mass spectrometry

采用高效液相色谱-质谱联用法(HPLC-MS)定量检测了白芍药材中的23种农药残留,样品经乙腈提取后再用PSA(N-丙基乙二胺)进行分散固相萃取。方法的定量限(LOQ)为0.75～12.17μg/kg;在0.01和0.1 mg/kg两种添加水平下,除极性较大的噻虫嗪和吡虫啉外,其余农药的回收率均在70%～120%之间,相对标准偏差(RSD)在2.8%～18.9%之间。该方法净化效果好、灵敏度高、重现性好,可用于白芍样品中农药残留的日常检测。

A method of high performance liquid chromatography coupled with mass spectrometry（HPLC-MS） for simultaneous determination of 23 pesticides in traditional Chinese medicine Paeoniae radix Alba was developed.P.radix was extracted with acetonitrile,and then purified using a preliminary sample treatment step based on primary-secondary amine（PSA） dispersive solid-phase extraction.Limits of quantification（LOQ） were between 0.75-12.17 μg/kg.Recovery between 70% and 120% were obtained for all pesticides at 0.01 and 0.1 mg/kg levels,except for polar pesticides such as thiamethoxam and imidacloprid.This method is accurate,reproducible and has good cleanup effect.It could be applied in pesticide residue analysis in P.Radix.