超高效液相色谱-串联质谱法测定饲料中9种氨基糖苷类抗生素

Determination of 9 kinds of aminoglycosides in feed by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  饲料  氨基糖苷类抗生素  超高效液相色谱-串联质谱法

英文关键词:feed  aminoglycosides  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-串联质谱法测定饲料中9种氨基糖苷类抗生素(aminoglycosides, AGs)的分析方法。方法 样品采用10 mmol/L磷酸二氢钾缓冲液作为提取液, 酶探针超声提取1 min, 通过阳离子交换固相萃取柱净化, 在电喷雾电离正离子模式下使用超高效液相色谱-串联质谱仪进行检测, 外标法定量。 结果 经方法学验证, 在5~1000 μg/L范围内, 9种AGs均呈现良好的线性关系, 方法的检出限为5~20 μg/kg, 定量限为20~80 μg/kg。在20~400 μg/kg添加浓度范围内, 饲料中9种AGs的平均回收率为76.2%~113.2%; 日内变异系数为1.1%~8.4%, 日间变异系数为1.1%~11.6%。结论 该方法稳定、灵敏, 可同时实现饲料中9种AGs的检测, 满足饲料中AGs日常监测应用需求。

英文摘要:

      Objective To establish an analytical method for the determination of 9 kinds of aminoglycosides (AGs) in feed by ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with 10 mmol/L potassium phosphate buffer solution using enzyme probe ultrasound for 1 min, and purified by cation exchange solid phase extraction column. The samples were detected by ultra performance liquid chromatography-tandem mass spectrometry in electrospray ionization positive ion mode, and quantified by external standard method. Results Verified by square law, the linear relationships of the 9 kinds of AGs were good in the range of 5?1000 μg/L, with the detection limits of 5-20 μg/kg and the quantitation limits of 20?80 μg/kg. The average recoveries of 9 kinds of AGs in feed ranged from 76.2% to 113.2% at the concentration of 20?400 μg/kg; the intra-day coefficients of variation were 1.1%–8.4%, and the intra-day coefficients of variation were 1.1%?11.6%. Conclusion This method is stable and sensitive, and can simultaneously detect 9 kinds of AGs in feed, thus meeting the daily monitoring application requirements of AGs in feed.