QuEChERS-三重四极杆液相色谱质谱联用法快速筛查花生中52种农药残留

Rapid screening 52 kinds of pesticide residues in peanuts by QuEChERS- triple-quadrupole liquid chromatography-mass spectrometry

中文关键词:  三重四极杆液相色谱质谱联用法  农药残留  筛查  花生

英文关键词:triple-quadrupole liquid chromatography-mass spectrometry  pesticide residues  screening  peanuts

中文摘要:

      目的 建立三重四极杆液相色谱质谱联用法快速筛选和确认花生中52种农药残留的分析方法。方法 样品经0.1%甲酸乙腈提取, 提取液经MgSO4、乙二胺-N-丙基硅烷化硅胶(primary secondary amine, PSA)和C18净化后, 采用Waters C18 (100 mm×2.1 mm, 1.7 μm)色谱柱分离, 在三重四极杆正离子反应监测模式下测定, 基质标准曲线结合外标法定量。结果 52种农药在0.001~0.1 μg/mL范围内线性良好, 相关系数均大于0.996, 方法的定量限为1~5 μg/kg, 通过实际样品加标回收实验, 52种农药在10 μg/kg的加标回收率为76.4%~107.6%, 相对标准偏差为3.5%~12.3%。结论 该方法适用于花生中农药残留的筛查检测及定量分析。

英文摘要:

      Objective To establish a rapid screening and identification method for 52 kinds of pesticide residues in peanut by triple-quadrupole liquid chromatography-mass spectrometry. Methods The samples were extracted by 0.1% formic acid-acetonitrile, and the extracted solution was purified by MgSO4, primary secondary amine (PSA) and C18. The solution was separated on a Waters C18 column (100 mm×2.1 mm, 1.7 μm). The positive ion reaction was monitored by triple quadrupole and quantified by matrix standard curve combined with external standard method. Results The 52 kinds of pesticides showed good linearity in the range of 0.001-0.1 μg/mL, and the correlation coefficients were all greater than 0.996. The limits of quantification of the method were 1?5 μg/kg. The recoveries of 52 kinds of pesticides at 10 μg/kg were 76.4%?107.6% in the experiment of spiked sample recovery. The relative standard deviations were 3.5%?12.3%. Conclusion This method is suitable for the screening and quantitative analysis of pesticide residues in peanuts.