QuEChERS-超高效液相色谱-串联三重四极杆质谱联用法快速测定蔬菜中吡虫啉等四种杀虫剂残留

Rapid determination of 4 pesticide residues in vegetables by QuEChERS and ultra performance liquid chromatography tandem mass spectrometry

中文关键词:  吡虫啉  啶虫脒  氯虫苯甲酰胺  茚虫威  蔬菜  残留  QuEChERS-超高效液相色谱-串联三重四极质谱法

英文关键词:imidacloprid  acetamiprid  chlorantraniliprole  indoxacarb  vegetables  residues  QuEChERS and ultra performance liquid chromatography tandem mass spectrometry

中文摘要:

      目的 建立QuEChERS-超高效液相色谱-串联三重四极杆质谱法测定蔬菜中吡虫啉、啶虫脒、氯虫苯甲酰胺和茚虫威残留的分析方法。方法 样品用乙腈提取, 提取液经N-丙基乙二胺(primary secondary amine, PSA)、石墨化炭黑(graphitized carbon black, GCB)混合分散剂净化, 采用电喷雾正离子扫描, 多反应监测模式, 外标法定量。结果 吡虫啉、啶虫脒、氯虫苯甲酰胺和茚虫威在5~200 μg/L范围内与峰面积具有良好的线性关系, 相关系数都在0.995以上, 4种杀虫剂在0.5、5.0、10.0 μg/kg 3个水平加标下, 回收率在89.2%~101.3%范围内, 相对标准偏差(relative standard deviation, RSD)在2.58%~4.85%。方法的检出限为0.003~0.054 μg/kg, 定量限为0.01~0.18 μg/kg。结论 该方法具有操作简单, 迅速, 准确度和灵敏度高等特点, 满足测定蔬菜中4种杀虫剂残留的检测要求。

英文摘要:

      Objective To establish a method for determination of 4 types of pesticide residues in vegetables by QuEChERS and ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Methods Samples were extracted by acetonitrile and purified by PSA(primary secondary amine) and GCB(graphitized carbon black, GCB), determined by UPLC-MS/MS, with positive electrospray ionization (ESI+) in multiple reaction monitoring (MRM) mode, and quantified by external standard method. Results All pesticides showed good linearity in the concentration range of 5200 μg/L (imidacloprid, acetamiprid, chlorantraniliprole and indoxacarb) with correlation coefficient above 0.995. The recovery rates of 4 types of pesticide were between 89.2%101.3%, and the relative standard deviations (RSDs) were between 2.58%4.85%. The limits of detection of the method were 0.0030.054 μg/kg, and the limits of quantification were 0.010.018 μg/kg. Conclusion This method is simple, rapid, sensitive and accurate, which is suitable for determination of 4 types of pesticide residues in vegetables.