超高效液相色谱-串联质谱法同时测定鳗鱼中6种咪唑类药物残留

Simultaneous determination of 6 kinds of imidazoles residues in eel 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  鳗鱼  咪唑类  抗生素  残留

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  eel  imidazoles  antibiotic  residue

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)测定鳗鱼肉糜中6种咪唑类抗生素(甲苯咪唑、氨基甲苯咪唑、羟基甲苯咪唑、左旋咪唑、甲硝唑、羟基甲硝唑)残留的分析方法。方法 采用乙酸乙酯溶液提取, MCX柱净化后进行超高效液相色谱分离, 电喷雾串联质谱进行检测, 多离子反应监测(multiple reaction monitoring, MRM)模式定量。结果 6种咪唑类抗生素的检出限均小于1 μg/kg; 该方法在0~20 μg/kg范围内线性关系良好, 相关系数均大于0.999。添加水平为5、10、15 μg/kg时, 化合物的平均回收率范围为70.5%~92.6%, 相对标准偏差(relative standard deviation, RSD)均小于14.3% (n=6)。结论 该方法简单、快速、灵敏, 适用于鳗鱼肉糜中6种咪唑类药物残留的同时快速测定。

英文摘要:

      Objective To establish a method for the determination of 6 kinds of imidazoles residues (mebendazole, aminomebendazole, 5-hydroxymebendazole, levamisole, metronidazole, metronidazole-OH) in eel by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The sample was extracted with ethyl acetate, and separated by UPLC after purified by MCX solid phase extraction, determined by positive electrospray ionization, and quantified by multiple reaction monitoring (MRM) mode. Results The limits of detection (LOD) for the 6 kinds of imidazoles residues were less than 1 μg/kg. The calibration curve showed good linearity within the concentrations of 0?20 μg/kg, all correlation coefficients were greater than 0.999. The recoveries were ranged from 70.5% to 92.6% for 6 kinds of imidazoles residues with 3 spiked levels of 5, 10 and 15 μg/kg, the relative standard deviations (RSDs) were less than 14.3% (n=6). Conclusion This method is simple, fast and sensitive, and suitable for the simultaneous rapid determination of imidazoles residues in eel.