超高效液相色谱-串联质谱法检测牛奶中7种氨基糖苷类药物残留

Detection of seven aminoglycoside residues in Milk by UPLC-MS-MS

关键词:  牛奶  氨基糖苷类  超高效液相色谱-串联质谱

Key words:  milk  aminoglycosides  Ultra-HPLC-MS-MS

摘要:

应用超高效液相色谱-串联质谱技术,建立了牛奶中7种氨基糖苷类药物(链霉素、双氢链霉素、庆大霉素、卡那霉素、丁胺卡那霉素、安普霉素、大观霉素)的检测方法。样品经乙酸铵缓冲液提取后,通过固相萃取柱净化；采用甲酸铵溶液作为流动相进行梯度洗脱,经CORTECS HILIC色谱柱分离,通过多反应监测模式进行测定。在0.1～5 μg/mL的范围内线性关系良好,相关系数均大于0.996。在20、50、200 μg/kg添加水平下,平均回收率为86%～108%,相对标准偏差均小于15%。检测限为10 μg/kg,定量限为20 μg/kg,该法准确、简单、快速。

Abstract:

A method of Ultra-HPLC-MS/MS was developed to determine seven aminoglycoside (streptomycin,dihydrostrepmycin,gentamycin,kanamycin,amkacin , apramycin, spectinomycin) residues in milk. The samples were extracted by Ammonium acetate buffer solution and separated by a cation exchange chromatographic column . The HPLC separation was performed on ACQUITY CORTECS HILICcolumn with a linear gradient elution program of ammonium formate solution as the mobile phase. Selective reaction monitoring was used for the selective detection . There was a good line correlation in the range of 0.1～5μg/mL, the correlation coefficient was greater than 0.996. The average recorvery was 86%～108% and RSD were both less than 15%. The limit of detection was10μg/kg and limit of quantification was 20μg/kg. The method was accurate,convenient and fast.