GC-MS/MS同时测定杭白菊中68种农药残留

Simultaneous Determination of 68 Pesticide Residues in Chrysanthemum Morifolium by GC-MS/MS

关键词:  杭白菊  农药残留  气相色谱-三重四极杆串联质谱  QuEChERS

Key words:  Chrysanthemum morifolium  pesticide residues  GC-MS/MS  QuEChERS

摘要:

目的 采用GC-MS/MS建立同时测定杭白菊中68种农药残留的分析方法。方法 样品采用QuEChERS前处理程序，经1%冰醋酸浸泡30 min后，乙腈提取，经装有无水硫酸镁900 mg、PSA 300 mg、十八烷基键合硅胶300 mg、硅胶300 mg和石墨化炭黑90 mg的分散固相萃取净化管净化，采用GC-MS/MS动态多反应监测模式，进行定性定量分析。结果 68种农药在各自浓度范围内线性关系良好，相关系数r均>0.993。在20，100，200 μg·kg^-1 3个不同加标水平下，除六氯苯、甲基五氯苯硫醚、苯氟磺胺、p，p'-滴滴伊和氯氟氰菊酯外，大部分农药的回收率均在70.0%~120.0%之间，RSD在0.4%~13.9%之间。方法的检出限为0.2~25.6 μg·kg^-1，定量限为0.8~85.5 μg·kg^-1。结论 该方法简单、快速、高效、灵敏，可为杭白菊中多农药残留的快速筛查和测定提供一种有效的分析手段。

Abstract:

OBJECTIVE To establish a multi-residue analytical method for the determination of 68 pesticides in Chrysanthemum morifolium by GC-triple quadrupole mass spectrometry (GC-MS/MS). METHODS Samples were treated with QuEChERS pretreatment method. They were extracted with acetonitrile after soaking in 1% acetic acid for 30 min, and then purified by dispersed solid-phase extraction and purification tubes containing 900 mg of anhydrous magnesium sulfate, 300 mg of PSA, 300 mg of octadecyl-bonded silica, 300 mg of silica gel and 90 mg of graphitized carbon black. The GC-MS/MS dynamic multiple reaction monitoring (dMRM) mode was used for the qualitative and quantitative analysis. RESULTS The linear relationship of each pesticide residue was good (r>0.993) in their respective concentration range. The recoveries of most pesticides were between 70.0% and 120.0% at 3 spiked levels of 20, 100, 200 μg·kg^-1, with the relative standard deviations (RSD) from 0.4% to 13.9%, except hexachlorobenzene, methyl-pentachlorophenyl sulfide, dichlofluanid, DDE-p,p' and cyhalothrin. The limits of detection (LOD) were 0.2-25.6 μg·kg^-1, and the limits of quantification (LOQ) were 0.8-85.5 μg·kg^-1. CONCLUSION The method is simple, rapid, efficient and sensitive, which can be used for the simultaneous anlysis and screening of pesticide multiresidues in Chrysanthemum morifolium.