HPLC-MS/MS检测2种中兽药制剂中非法添加庆大霉素的研究

Detection of Illegally Added Gentamycin in Traditional Chinese Medicine for Animals by Ultra-HPLC-MS-MS

关键词:  兽用中药制剂  庆大霉素  超高效液相色谱-串联质谱

Key words:  Traditional Chinese Medicine for Animals  Gentamycin  Ultra-HPLC-MS-MS

摘要:

应用超高效液相色谱-串联质谱技术,建立了兽用中药制剂穿心莲注射液和鱼腥草注射液中非法添加庆大霉素的检测方法。样品经水溶解后,稀释。采用20mmol/L HFBA乙腈与20mmol/L HFBA水溶液作为流动相进行梯度洗脱,经ACQUITY HSS PFP色谱柱分离,通过多反应监测模式进行测定。庆大霉素在0.04～2 μg/mL的范围内线性关系良好,相关系数0.9994。平均回收率为98.2%～100.3%,相对标准偏差均小于2.4%。检测限为0.2%,定量限为0.4%,该法准确、简单、快速。

Abstract:

A method of Ultra-HPLC-MS/MS was developed to determine gentamycin illegally added in traditional chinese medicine for animals. The samples were dissolved and diluted. The HPLC separation was performed on ACQUITY HSS PFP column with a linear gradient elution program of 20mmol/L HFBA acetonitrile and 20mmol/L HFBA aqueous solution as the mobile phase. Selective reaction monitoring was used for the selective detection .The linearity of gentamycin ranged 0.04～2 μg/mL with coefficient 0.9994. The average recorvery was 98.2%～100.3% and RSD were both less than 2.4%. The limit of detection was 0.2 % and limit of quantification was 0.4%. The method was accurate,convenient and fast.