超高效液相色谱-串联质谱法检测清瘟败毒散中非法添加金刚烷胺的研究

Determinatiaon of Amantadine Illegally Added in QingWenBaiDuSan by Ultra-HPLC-MS-MS

关键词:  清瘟败毒散  金刚烷胺  超高效液相色谱-串联质谱

Key words:  Qingwen Baidu San  amantadine  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清瘟败毒散中非法添加金刚烷胺的检测方法。样品经提取液提取后，稀释。采用0.2%甲酸水溶液与甲醇作为流动相进行梯度洗脱，经BEH C18色谱柱分离，通过多反应监测模式进行测定。金刚烷胺在0.05～25 ng/mL的范围内线性关系良好，相关系数大于0.999；平均回收率为86.9%～95.2%，批内、批间相对标准偏差均小于3.8%，检测限为0.025 mg/g，定量限为0.1 mg/g。该法准确、简单、快速，可用于清瘟败毒散中非法添加金刚烷胺的检测。

Abstract:

A method of Ultra-HPLC-MS/MS was developed to determine amantadine illegally added in Qingwen Baidu San of traditional chinese medicine for animals. The samples were extracted and diluted. The HPLC separation was performed on BEH C18 column with a linear gradient elution program of methanol and 0.2% formic acid solution as the mobile phase. Selective reaction monitoring was used for the selective detection .The linearity of amantadine ranged 0.05 to 25 ng/mL with coefficient greater than 0.999. The average recorvery was 86.9%～95.2% and RSD of intra-batch and inter-batch were both less than 3.8%. The limit of detection was 0.025 mg/g and limit of quantification was 0.1 mg/g. The method was accurate,convenient, fast and can be used as a determination for illegally added amamtadine in Qingwen Baidu San.