改进QuEChERS技术结合气相色谱-质谱法检测蔬菜中6种农药残留

Determination of 6 kinds of pesticide residues in vegetables by improved QuEChERS technology combined with gas chromatography-mass spectrometry

中文关键词:  气相色谱-质谱法  邻苯基苯酚钠  二甲基敌草索  草乃敌  唑蚜威  解毒喹  唑嘧菌胺  叶菜类蔬菜

英文关键词:gas chromatography-mass spectrometry  2-hydroxybiphenyl sodium salt  chlorthal-dimethyl  diphenamid  triaguron  cloquintocet-mexyl  ametoctradin  leafy vegetables

中文摘要:

      目的 建立改进QuEChERS方法结合气相色谱-质谱法(gas chromatography-mass spectrometry, GC-MS)快速检测蔬菜中邻苯基苯酚钠、二甲基敌草索等6种在我国植源性食品安全国家标准中暂无检测标准, 但在出口欧盟及日本果蔬中重点检测的农药物质的分析方法。方法 样品经乙腈提取、MgSO4与NaCl盐析后, 使用N-丙基乙二胺(primary secondary amine, PSA)固相材料、石墨化炭黑(graphitized carbon black, GCB)净化提取, 采用Rtx-5MS毛细管色谱柱(30 m×0.25 mm, 0.25 μm)分离, 使用选择离子监测(selected ion monitoring, SIM)扫描模式, 对农药目标离子进行监测。结果 6种农药物质在0.002~0.500 μg/mL范围内线性关系良好, 相关系数(r)均大于0.998, 方法检出限为0.0033~0.0089 mg/kg, 均小于0.01 mg/kg, 平均回收率为77.0%~107.7%, 相对标准偏差为2.17%~9.86%。结论 该方法快速灵敏、重复性好、材料易得、成本低, 为邻苯基苯酚钠、二甲基敌草索等农药残留问题提供了新的参考检测方法。

英文摘要:

      Objective To establish an improved QuEChERS-gas chromatography-mass spectrometry (GC-MS) method for the rapid detection of 6 kinds of pesticide residues in vegetables, such as 2-hydroxybiphenyl sodium salt and chlorthal-dimethyl, etc., currently have no detection standards in the national standards for the safety of vegetable derived foods in China, but are mainly detected in fruits and vegetables exported to the European Union and Japan. Methods After the samples were extracted with acetonitrile, salted out with MgSO4 and NaCl, the extracts were purified with primary secondary amine (PSA) solid phase material and graphitized carbon black (GCB). The purified solution was a Rtx-5MS capillary column (30 m×0.25 mm, 0.25 μm) separation, using the selected ion monitoring (SIM) scan mode to monitor the pesticide target ions. Results The results showed that the linearity was good in the range of 0.002?0.500 μg/mL for these 6 kinds of pesticide substances, and the correlation coefficients (r) were greater than 0.998. The limits of detection of the method were 0.0033?0.0089 mg/kg, the average recoveries were 77.0%?107.7%, and the relative standard deviations were 2.17%?9.86%. Conclusion The method is rapid, sensitive, reproducible, easy to obtain, and low cost. It provides a new reference for the detection of pesticide residues such as 2-hydroxybiphenyl sodium salt and chlorthal-dimethyl.