超高效液相色谱-串联质谱法测定食品中呋虫胺及2种代谢物残留量

Determination of dinotefuran and 2 kinds of metabolites residues in food by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  呋虫胺  呋虫胺代谢物  农药残留

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  dinotefuran  dinotefuran metabolites  pesticide residues

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)快速检测食品中呋虫胺及2种代谢物残留量的分析方法。方法 样品经乙腈超声提取, C18固相萃取(solid-phase extraction, SPE)小柱净化, 上清液氮吹至近干, 经初始比例液相流动相复溶后, UPLC-MS/MS测定, 外标法定量。结果 在0.1~200 μg/L范围内线性相关系数r2≥0.999, 粮谷、水果、蔬菜、鱼、肉、蛋、奶等22种基质中呋虫胺及其2种代谢物在5、10和50 μg/kg 3个加标水平下, 回收率为71.2%~105.6%, 相对标准偏差(relative standard deviation, RSD)为1.3%~9.8%。结论 该分析方法准确度和精密度高, 均达到农药残留检测要求, 适用于分析粮谷、水果、蔬菜、鱼、肉、蛋、奶中呋虫胺及代谢物残留量。

英文摘要:

      Objective To establish a method for the determination of dinotefuran and 2 kinds of metabolites residues in food by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted with acetonitrile, purified with C18 solid-phase extraction (SPE), dried by nitrogen, and dissolved by initial ratio of mobile phase. Then the samples were determined by UPLC-MS/MS and quantified by external standard method. Results The correlation coefficients of dinotefuran and 2 kinds of metabolites were 0.999 in the range of 0.1 to 200 μg/L, the recoveries were ranged from 71.2%?105.6% at 3 kinds of spike levels (5, 10 and 50 μg/kg), and the relative standard deviations (RSDs) were ranged from 1.3%?9.8%. Conclusion This method has high accuracy and precision, which meets the requirements of pesticide residue and is suitable for the analysis of dinotefuran and metabolite residues in grains, fruits, vegetables, fish, eggs and milk.