QuEChERS-液相色谱-串联质谱法测定葵花籽中30种农药残留

Determination of 30 pesticide residues in sunflower seeds by QuEChERS–liquid chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  液相色谱-串联质谱法  葵花籽  农药残留

英文关键词:QuEChERS  liquid chromatography-tandem mass spectrometry  sunflower seeds  pesticide residues

中文摘要:

      目的 建立QuECHERS-液相色谱-串联质谱法测定葵花籽中30种农药残留的分析方法。方法 葵花籽用1%乙酸-乙腈溶液提取, QuEChERS试剂净化, 液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)测定, 多反应监测模式(multiple reaction monitoring, MRM)分析, 外标法定量。结果 30种农药分为2组, 第1组23种农药在10~100 μg/L范围内, 第2组7种农药在1~10 μg/L范围内, 这2组的峰面积与对应的质量浓度间都呈良好的线性关系, 相关系数大于0.9970。各组在3个添加水平的平均回收率为70%～120%(第1组10、20和100 μg/kg, 第2组1.0、2.0和10 μg/kg各3个添加水平), 相对标准偏差1.50%～9.57%(n=6), 定量限0.01～0.20 μg/kg。结论 该方法操作灵敏、准确、可靠, 能满足葵花籽中多种农药残留量的检测。

英文摘要:

      Objective To establish a method for rapid determination of 30 pesticide residues in sunflower seeds by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Sunflower seeds were extracted with 1% acetic acid-acetonitrile solution, purified with QuEChERS reagent, and determined by LC-MS/MS, then analyzed by multi-reaction monitoring mode (MRM), and quantified by external standard method. Results The thirty pesticides were divided into two groups, the two groups showed a good linear relationship between the peak area and the corresponding mass concentration of the first group in the range of 10?100 μg/kg, and the second group in the range of 1.0?10 μg/kg, the correlation coefficients were greater than 0.997. The average recoveries in the spiked level of 10, 20 and 100 μg/kg, and the second group at 1.0, 2.0 and 10 μg/kg were between 70% to 120%, the relative standard deviations (RSD) were between 1.50% to 9.57% (n=6), and the quantitative limit were between 0.01? 0.2 μg/kg. Conclusion The method is sensitive, accurate and reliable, which is suitable for monitoring pesticide residues in sunflower seeds.