QuEChERS自动样品制备系统结合在线凝胶渗透色谱-气相色谱-质谱法测定蔬菜中41种农药残留

Determination of 41 kinds of pesticide residues in vegetables by QuEChERS automated sample preparation system and online gel permeation chromatography gas chromatography-mass spectrometry

中文关键词:  农药残留  QuEChERS自动样品制备系统  在线凝胶渗透色谱  气相色谱-质谱法  蔬菜

英文关键词:pesticide residue  QuEChERS automated sample preparation system  online gel permeation chromatography  gas chromatography-mass spectrometry  vegetable

中文摘要:

      目的 建立QuEChERS自动样品制备系统结合在线凝胶渗透色谱-气相色谱质谱联用法测定蔬菜中41种农药残留的分析方法。方法 采用QuEChERS自动样品制备系统进行前处理。样品经乙腈提取, 无水硫酸镁、氯化钠、柠檬酸三钠和柠檬酸二钠盐析后, 经N-丙基乙二胺(PSA)和无水硫酸镁混合型固相分散净化, 以选择离子扫描模式进行检测, 外标法定量。对QuEChERS自动样品制备系统与手动QuEChERS方法对回收率的影响进行比较。结果 使用QuEChERS自动样品制备系统与手动QuEChERS方法进行前处理对蔬菜中大多数农药的回收效果差异不显著, 都能满足日常检测要求。41种农药在0.02~1.0 mg/L范围内具有较好的线性关系, 相关系数均大于0.99。在0.05、0.10、0.20和0.50 mg/kg 4个添加水平下, 除甲胺磷、三氯杀螨醇、氯氟氰菊酯、氟氰戊菊酯、百菌清外, 菠菜中其他农药的回收率为70.61%~129.43%。除百菌清、杀螟硫磷、虫螨腈、哒螨灵和氯氰菊酯外, 其他农药添加回收率的RSD为1.12%~18.76%。结论 本方法快速准确, 可用于蔬菜中农药残留的检测。

英文摘要:

      Objective To establish a method for the determination of 41 kinds of pesticide residues in vegetables prepared by QuEChERS automated sample preparation system and detected by online gel permeation chromatography coupled with gas chromatography-mass spectrometry (GPC-GC-MS). Methods The samples were prepared by QuEChERS automated sample preparation system, extracted with acetonitrile, followed by salting-out with anhydrous magnesium sulfate, sodium chloride, sodium citrate and citric acid disodium, and cleaned up by N-propyl ethylenediamine (PSA) and anhydrous magnesium sulfate. The extracts were detected by selected ion scan mode (SIM) and quantified by the external standard method. Results The recoveries of most pesticides in vegetables had no significant difference between QuEChERS automated sample preparation system and manual QuEChERS method, and these two methods could meet the daily testing requirements. The linearities of 41 kinds of pesticides ranged from 0.02 mg/L to 1.0 mg/L were good, with correlation coefficients more than 0.99. The recoveries for all compounds spiked at levels of 0.05, 0.10, 0.20 and 0.50 mg/kg were 70.61%~129.43%, except methamidophos, dicofol, cyhalothrin, flucythrinate and chlorothalonil. The relative standard deviations were 1.12%~18.76%, except chlorothalonil, fenitrothion, clorfenapry, pyridaben and cypermethrin. Conclusion The method is rapid and accurate, which can be used for the determination of pesticide residues in vegetables.