[关键词]
[摘要]
针对6种欧盟及日本进出口果蔬中重点检测,但在我国食品安全国家标准中暂无检测标准的农药物质进行研究,建立一种改进的QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe)提取净化方法结合气相色谱-串联质谱技术(Gas Chromatography-tandem Mass Spectrometry,GC-MS/MS)检测方法,能快速检测叶菜类蔬菜基质中邻苯基苯酚钠、二甲基敌草索等6种农药多残留。样品采用乙腈提取、无水MgSO4 与NaCl盐析除水后,经N-丙基乙二胺(PSA)固相材料净化,使用GC-MS/MS在多反应监测模式(Multi Reaction Monitoring,MRM)下分析检测。结果表明:6种农药物质在0.002~0.5 μg/mL范围内线性关系良好,相关系数R均大于0.998,方法检出限(RSN=3)为0.15~2.32 μg/kg,平均回收率为84.50%~106.23%,相对标准偏差为0.96%~8.35%,此结果均符合欧盟农药残留分析质量控制程序要求与日本和欧盟对农残“一律标准”中农药限量要求。将建立的检测方法应用于其他蔬菜中高发农药物质的检测,检测效果良好。该方法重复性好、耗时短、易操作,为邻苯基苯酚钠、二甲基敌草索等多种农药残留的检测提供了新的检测技术和依据。
[Key word]
[Abstract]
In this study, given the fact that six kinds of pesticides are mainly detected in fruits and vegetables imported and exported from the European Union and Japan, but there are no detection standards in China's national food safety standards, an improved QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction and purification method combined with Gas Chromatography-Tandem Mass Spectrometry (GC-MS/MS) detection method was established. This method could rapidly detect six pesticide residues such as sodium o-phenylphenol and dimethyl dichloromethane in leafy vegetable substrates. The sample was extracted with acetonitrile, salted out with anhydrous MgSO4 and NaCl to remove water, purified with N-propylethylenediamine (PSA) solid-phase material, and analyzed and detected using GC-MS/MS in multiple reaction monitoring (MRM) mode. The results showed that the six pesticides had a good linear relationship in the range from 0.002 to 0.5 μg/mL, with all the correlation coefficient R being greater than 0.998, the detection limit (RSN=3) being 0.15-2.32 μg/kg, the average recovery being 84.50%~106.23%, and the relative standard deviation being 0.96%~8.35%. The results are in accordance with the requirements of the quality control procedures for pesticide residues in the European Union and the pesticide limit requirements of the "uniform standard" for agricultural residues in Japan and the European Union. The established detection method was further applied to the detection of high-incidence pesticide substances in other vegetables, with good detection results. The method established in this study is reproducible, time efficiency, and easy to operate, which provides a new detection technology and basis for the detection of various pesticide residues such as sodium o-phenylphenol and dimethyl dichloromethane.
[中图分类号]
[基金项目]
国家重点研发计划项目(2022YFF1100804);西南民族大学中央高校基本科研业务费专项(2020NTD04);四川省科技创新人才项目(2023JDRC0007)