超高效液相色谱-三重四级杆质谱法测定牛干巴中2种喹噁啉类药物残留

Determination of 2 kinds of quinoxaline drug residues in dry-cured beef by ultra performance liquid chromatography/triple qudrupole tandem mass spectrometry

中文关键词:  卡巴氧  喹赛多  牛干巴  超高效液相色谱-三重四级杆质谱法

英文关键词:carbadox  cyadox  dry-cured beef  ultra performance liquid chromatography/triple qudrupole tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-三重四级杆质谱法测定牛干巴中卡巴氧及喹赛多的含量的分析方法。方法 样品经乙酸乙酯-乙腈提取, 正己烷脱色净化后, 以乙腈-0.1%甲酸溶液为流动相, 经ACQUITYTMBEH18柱分离, 采用多反应监测正离子模式进行定性及定量分析。结果 卡巴氧及喹赛多的检出限分别为0.2和2.0 μg/kg, 3个加标水平回收率范围为66.4%~115.0%, 相对标准偏差为4.2%~8.2%。结论 该方法灵敏度高、重复性好、准确度高、分析时间短、样品前处理操作简便, 适用于牛干巴中卡巴氧及喹赛多的测定。

英文摘要:

      Objective To establish a method for the determination of carbadox and cyadox in dry-cured beef by ultra performance liquid chromatography/triple qudrupole tandem mass spectrometry. Methods The dry-cured beef sample was extracted with ethyl acetate-acetonitrile, and then decolorizated and purificated with N-hexane. Target compounds were separated with ACQUITYTMBEH18 column with acetonitrile-water (0.1% formate) as mobile phase, and then characterized by mass spectrometry in the positive electrospray ionization under multiple reaction monitoring mode (MRM). Results Limits of detection of carbadox and cyadox were 0.2 μg/kg and 2.0 μg/kg, respectively. The recoveries at 3 spiked concentrations were from 66.4% to 115.0% and the relative standard deviations were from 4.2%-8.2%. Conclusion This method has higher sensitivity, good repeatability, higher accuracy, shorter analysis time and convenient sample pretreatment, which is suitable for the detection of carbadox and cyadox in dry-cured beef.