静电场轨道阱高分辨质谱法快速筛查上海市流通环节蔬菜的农药残留

Rapid screening of pesticide residues of vegetables in circulation in Shanghai by orbitrap high resolution mass spectrometry

中文关键词:  静电场轨道阱高分辨质谱  快速筛查  蔬菜  农药残留

英文关键词:orbitrap high resolution mass spectrometry  rapid screening  vegetables  pesticide residues

中文摘要:

      目的 建立静电场轨道阱高分辨质谱法快速筛查蔬菜中农药多残留的方法。方法 使用QuEChERS法净化蔬菜样品, 结合静电场轨道阱高分辨质谱法开展809种农药的快速非靶向筛查。结果 62种阳性农药的筛查限(screening detection limit, SDL)为0.005~0.010 mg/kg, 定量限(limits of quantitation, LOQ)为0.01 mg/kg, 线性范围为10.0~200.0 μg/L, 线性相关系数(r2)为0.9917~0.9997, 日内精密度为2.77%~6.98% (n=5), 日间精密度为4.82%~10.8% (n=5)。200批次样品共检出62种农药, 不合格样品28批次, 不合格率为14.0%。豇豆的不合格情况比较突出, 不合格样品22批次, 主要的不合格项是灭蝇胺和噻虫胺。结论 该方法快速、准确、分析通量高, 在无标准品的情况下实现了蔬菜中809种农药的非靶向快速筛查, 可为蔬菜农药残留风险监测和质量控制提供支撑。

英文摘要:

      Objective To establish a rapid method for screening pesticide residues in vegetables by orbitrap high resolution mass spectrometry. Methods Vegetable samples were purified by QuEChERS method, 809 kinds of pesticides could be quickly and non-targeted screened by orbitrap high resolution mass spectrometry. Results The screening detection limit (SDL) of 62 kinds of positive pesticides was 0.005–0.010 mg/kg, and the limits of quantitation (LOQ) were 0.01 mg/kg. The linear range was 10.0–200.0 μg/L, the linear correlation coefficients (r2) were 0.9917–0.9997, the intra-day precisions were 2.77%–6.98% (n=5), and the inter-day precisions were 4.82%–10.8% (n=5). The 62 kinds of pesticides were detected in 200 samples, and there were 28 unqualified samples with the unqualified rate was 14.0%. The unqualified situation of cowpea was more prominent, and the unqualified samples were 22 batches, the main unqualified items were cyromazine and clothianidin. Conclusion The method has the advantages of rapid screening, high accuracy and high analytical throughput. It can realize the non-targeted rapid screening of 809 kinds of pesticides in vegetables without standard substances, which can provide support for the risk monitoring and quality control of pesticide residues in vegetables.