QuEChERS-气相色谱-三重四极杆质谱法测定蜂蜜中15种农药残留

Determination of 15 pesticides residue in honey by QuEChERS-gas chromatogram

中文关键词:  蜂蜜  农药残留  QuEChERS  气相色谱-三重四极杆质谱法

英文关键词:honey  pesticide residues  QuEChERS  gas chromatography-triple quadrupole mass spectrometry

中文摘要:

      目的 建立QuEChERS-气相色谱-三重四极杆质谱法(gas chromatography-triple quadrupole mass spectrometry, GC-MS/MS)检测蜂蜜中15种农药残留的方法。方法 蜂蜜样品经乙腈提取后, 用丙基乙二胺(primary secondary amine, PSA)粉末净化, 采用GC-MS/MS分析, 以保留时间和多反应监测(multiple reaction monitoring, MRM)离子对定性分析, 峰面积定量分析。结果 15种农药在10～200 μg/L浓度范围内的线性关系良好, 相关系数大于0.995。所有农药的定量限为0.012~0.205 μg/kg; 在0.04、0.10、0.20 mg/kg加标水平下, 15种农药的平均回收率为94.8%～111%, 相对标准偏差均小于10%(n=6)。结论 该方法简便、快捷、准确度及精密度好, 可以成为检测蜂蜜中农药残留的常规检测技术。

英文摘要:

      Objective To establish a method for the determination of 15 pesticide residues in honey by QuEChERS-gas chromatography triple quadrupole mass spectrometry (GC-MS/MS). Methods The honey samples were extracted with acetonitrile, purified with propyl ethylene diamine (PSA) powder, and analyzed by GC-MS/MS. The retention time and multiple reaction monitoring (MRM) ion pairs were used for qualitative analysis and peak area was used for quantification. Results The 15 pesticides had good linear relationship in the concentration range of 10?200 μg/L, and the correlation coefficients were greater than 0.995. The limits of the quantitation (LOQs) of all pesticides were 0.012?0.205 μg/kg, the recoveries of 15 pesticide residues spiked in honey at 3 spiked levels (0.04、0.10、0.20 mg/kg) were 94.8%?111%, and the relative standard deviations were all below 10% (n=6). Conclusion This method is simple, fast, accurate, and suitable for the determination of pesticide residues in honey.