QuEChERS-超高效液相色谱-三重四极杆质谱法快速检测主要原粮与油料中101种农药残留

Rapid determination of 101 kinds of pesticide residues in main raw grain and oil by QuEChERS-ultra performance liquid chromatography- triple quadrupole mass spectrometry

中文关键词:  QuEChERS  超高效液相色谱-三重四极杆质谱法  主要原粮与油料  农药残留

英文关键词:QuEChERS  ultra performance liquid chromatography-triple quadrupole mass spectrometry  main raw grain and oil  pesticide residues

中文摘要:

      目的 建立QuEChERS-超高效液相色谱-三重四极杆质谱法快速检测主要原粮与油料中101种常见农药残留的分析方法。方法 样品加入乙腈后涡旋混匀并超声提取, 采用无水硫酸镁和N-丙基硅烷化硅胶(primary secondary amine, PSA)固相吸附剂净化, 以乙腈-0.1%甲酸水溶液(V:V)作为流动相进行梯度洗脱, 采用T3色谱柱(100 mm×2.1 mm, 1.7 μm)分离, 在多反应监测(multiple reaction monitoring, MRM)模式下进行测定, 外标法定量。结果 101种农药残留在3个添加水平(50、100和200 μg/kg)下回收率在62.31%~119.74%之间, 相对标准偏差小于15%, 定量限为0.06~23.81 μg/kg。结论 该方法操作简便、快速, 有较高的灵敏度和准确度, 可应用于主要原粮与油料中农药残留日常筛查工作。

英文摘要:

      Objective To establish an analytical method for the rapid determination of 101 kinds of common pesticide residues in main raw grain and oil by QuEChERS-ultra performance liquid chromatography-triple quadrupole mass spectrometry. Methods After acetonitrile was added, the samples were vortex mixed and ultrasonically extracted, anhydrous magnesium sulfate and primary secondary amine (PSA) solid phase adsorbent were used to purify the samples, acetonitrile-0.1% formic acid aqueous solution (V:V) was used as mobile phase for gradient elution, the samples were separated by T3 column (100 mm×2.1 mm, 1.7 μm), determined by multiple reaction monitoring (MRM) and quantified by external standard method. Results 101 kinds of pesticide residues were detected at 3 kinds of addition levels (50, 100 and 200 μg/kg), the recoveries ranged from 62.31% to 119.74%, the relative standard deviations were less than 15%, and the limits of quantification were 0.06-23.81 μg/kg. Conclusion This method is simple, rapid, sensitive and accurate, and can be used in routine screening of pesticide residues in main raw grain and oil.