超高效液相色谱-串联质谱法测定元胡中19种农药残留量

Determination ofResidues of 19 Pesticides in Rhizoma Corydalis by Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry

本文建立了元胡中超高效液相色谱-串联质谱法同时测定19种农药残留量的检测方法。样品经乙腈提取,多壁碳纳米管净化,超高效液相色谱-串联质谱仪测定,ESI+扫描,以多反应监测(MRM)方式采集数据,外标法定量。在5~200μg/L范围内,19种农药具有良好的线性关系(r>0.99);在3个不同浓度加标水平下,各农药的平均回收率在71.0%~115%,RSD为1.6%~9.8%,方法的定量限为0.1~4.01μg/kg。经实际样品确证分析,该方法简便、快速、准确、重现性好、灵敏度高,适用于元胡中多种农药的同时检测。

An ultra- performance liquid chromatography- tandem mass spectrometry（UPLC-MS/MS） method was developed for determining the residues of the 19 pesticides in rhizoma corydalis.The sample was firstly extracted with acetonilrilc,then cleaned up using multi-walled carbon nanotube and detected by UPLC- MS/MS.The residues of the 19 pesticides were detected by multiple reaction monitoring（MRM） mode in the positive ion mode.The linear ranges were from 5 to 200μg/L with the correlation coefficients above 0.99 for all the 19 pesticides.The average recoveries at three spiked levels were 71.0%～ 115%with the relative standard deviations of 1.6%～9.8%.The limits of detection were 0.1 ～ 4.0 μg/kg.The method is rapid,accurate,reproducible,sensitive and easy,and suitable for the determination of multiple pesticide residues in rhizoma corydalis.