QuEChERS结合气相色谱-质谱快速测定人参提取物中25种农药残留  

Fast Pesticide Multiresidue Analysis in Panax Ginseng Extract by Gas Chromatography Mass Spectrometry with QuEChERS

作　　者：赖青海 王琳琳[1] 石垚[1] 余河水[1] 李薇[1] 曹满 宋新波[1] 

机构地区：[1]天津中医药大学,天津300193 [2]天津中一制药有限公司,天津300193

出　　处：《中国实验方剂学杂志》2015年第11期55-60,共6页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：天津市科技计划项目(12TXGCCX03800)

摘　　要：目的：采用改良的QuEChERS法联合气相色谱-质谱技术,建立一种快速检测人参提取物中25种农药残留的分析方法。方法：样品以乙腈提取,经氯化钠、无水硫酸镁盐析后,上清液加入乙二胺-N-丙基硅烷和石墨炭黑分散固相萃取剂进行净化,并采用基质匹配标准曲线法进行定量分析。结果：异狄氏醛,p,p＇-滴滴涕和甲氧滴滴涕在人参提取物中表现出相对较强的基质效应（ME〉130%）,而对硫磷则呈显著的基质效应（ME〉150%）,采用基质匹配标准曲线法校正后,25种农药在0.01-1 mg·L^-1线性关系良好,相关系数r〉0.995 4,3个添加水平（0.1,0.5,1.0μg·g^-1）的平均回收率在81.8%-110.7%,RSD均〈15%,定量限（LOQ）在3-48μg·kg^-1。结论：该方法能有效减少基质效应,并具有良好的准确度、重复性和灵敏度,适合于人参提取物中多农药残留的测定。Objective： To establish the chromatographic method for rapid determination of 25 pesticide residues in Ginseng extract by QuEChERS-GC-MS. Method： The samples were extracted with acetone which included acetonitrile, the sodium chloride, anhydrous magnesium sulfate salting out process, and cleaned up by PSA and GCB, and reduced the matrix effect by Matrix matched standard curve method. Result： The endrin aldehyde, p, p＇-DDT, methoxyehlor showed relatively strong matrix effects （ME 〉 130% ）, and parathion showed strong matrix effects （ME 〉 150% ） , after the correction of matrix calibration curve, the linear range was 0.01-1 mg ·L^-1 and r 〉0.995 4, the recovery range was 81.8%-110.7% in 3 adding level （0. 1, 0.5, 1.0 μg·g^-1） , RSD 〈 15%, LOQ was 3-48 μg·kg^-1. Conclusion： The method is accurate, sensitive and suitable for the determination of pesticide residues in ginseng extract.

关 键 词：QUECHERS 人参提取物 农药 气质联用 

分 类 号：R284.1[医药卫生—中药学]