气相色谱-串联质谱法测定玉龙县人参中农药残留量

Simultaneous determination of pesticide residues in Yulong County ginseng by gas chromatography-tandem mass spectrometry

采用固相萃取净化前处理技术,结合气相色谱-串联质谱(GC-MS/MS)法建立了人参中11种农药同时检测的方法。样品用1%冰乙酸和乙腈的混合溶液提取,提取液离心后,上清液经填有无水硫酸镁、乙二胺-N-丙基硅烷(PSA)、十八烷基硅烷键合硅胶、硅胶和石墨化炭黑的固相萃取柱净化,浓缩、复溶后进行GC-MS/MS测定,采用多反应监测模式,内标法定量。当11种农药加标水平为0.004,0.01 mg/kg时回收率为54%~103%,方法的相对标准偏差小于15%;检出限(S/N=3)不高于6μg/kg;在10~1000μg/L范围内线性关系良好。方法适用于复杂基质中农药的多残留检测。

A method for simultaneous determination of eleven pesticide residues in ginseng was based on solid-phase extraction（ SPE） pre-processing technology and gas chromatography-tandem mass spectrometry（ GC-MS/MS）. The pesticides interested were extracted from the samples with a mixed solution of 1 % acetic acid and acetonitrile. The extracting solution was separated by centrifugation to give a supernatant. The SPE column was filled with anhydrous magnesium sulfate,ethylenediamineN-propyl silane（ PSA）,octadecylsilane bonded silica,silica gel and graphitized carbon black. The supernatant was purified by the above SPE column and then concentrated,dissolved and determined by GC-MS/MS with the multiple reaction monitoring（ MRM） mode and internal standard method.The recoveries for eleven pesticides in the samples spiked with the standards of 0. 004 and 0. 01mg/kg were from 54 % to 103 %,and the relative standard deviations were less than 15 %. All the detection limits（ S/N = 3） were no higher than 6 μg/kg. The linearities of this method were good between 10 and 1000 μg/L. The method is characterized by simple pretreatment,short analysis time,high sensitivity and accuracy,and can meet the requirements for the analysis of multiple pesticide residues in complex matrix.