液相色谱-四极杆/线性离子阱质谱法同时测定焙炒咖啡中154种农药及其代谢物残留

Simultaneous determination of 154 kinds of pesticides and their metabolite residues in roasted coffee by liquid chromatography-quadrupole/linear ion trap mass spectrometry

中文关键词:  液相色谱-四极杆/线性离子阱质谱法  农药残留  焙炒咖啡

英文关键词:liquid chromatography-quadrupole/linear ion trap mass spectrometry  pesticide residues  roasted coffee

中文摘要:

      目的 建立液相色谱-四极杆/线性离子阱质谱法同时检测焙炒咖啡中154种农药及其代谢物的方法。方法 样品经1%乙酸乙腈提取、氯化钠和无水硫酸镁盐析除水后, 使用增强型脂质去除产品Bond Elut EMR-Lipid去除提取液中的脂质, 再经Carbon S和N-丙基乙二胺(primary secondary amine, PSA)固相材料净化, 采用多反应监测、信息依赖性采集、增强子离子扫描(enhanced product ion scanning, EPI), 结合154种农药EPI谱库检索多步模式进行分析, 基质匹配外标法定量。结果 154种农药在2~200 ng/mL范围内线性关系良好(r>0.990), 在0.01、0.05和0.10 mg/kg的加标水平下, 平均回收率为70.4%~117.5%, 相对标准偏差(relative standard deviations, RSDs, n=6)为1.7%~14.9%, 检出限和定量限分别为0.07~3.00 μg/kg和0.25~10.00 μg/kg, 方法准确有效, 符合中国、欧盟和日本对农药残留限量的检测要求。结论 本方法简便、快捷、可靠, 可用于焙炒咖啡中154种农药残留的快速筛查和定量分析。

英文摘要:

      Objective To establish a method for the simultaneous detection of 154 kinds of pesticides and their metabolites in roasted coffee by liquid chromatography-quadrupole/linear ion trap mass spectrometry. Methods The samples were extracted with 1% acetic acid in acetonitrile, followed by salting-out and dehydration using sodium chloride and anhydrous magnesium sulfate. The lipids in the extract were then removed with the enhanced lipid removal product Bond Elut EMR-Lipid. Further purification was performed using Carbon S and primary secondary amine (PSA) solid-phase sorbents. Analysis was carried out via multiple reaction monitoring, information-dependent acquisition and enhanced product ion (EPI) scanning, combined with library searching against the EPI spectral library of 154 kinds of pesticides in a multi-step mode. Matrix-matched external standard method was adopted for quantitative determination. Results The linear relationship of 154 kinds of pesticides was good linearity with in the range of 2–200 ng/mL (r>0.990). At the spiked levels of 0.01, 0.05 and 0.10 mg/kg, the average recovery rates were 70.4%–117.5%. The relative standard deviations (RSDs, n=6) were 1.7%–14.9%. The limits of detection and limits of quantitation of the method were 0.07–3.00 μg/kg and 0.25–10.00 μg/kg, respectively. The method was accurate and effective. It complied with the testing requirements for pesticide residue limits in China, the European Union and Japan. Conclusion This method is simple, rapid and reliable, and can be used for the rapid screening and quantitative analysis of 154 kinds of pesticide residues in roasted coffee.