HPLC-MS/MS检测双黄连注射液中非法添加13种喹诺酮类药物的研究

Determination of illegally added 13 quinolones in ShuangHuangLian injection by HPLC-MS/MS

关键词:  中兽药制剂  喹诺酮类药物  高效液相色谱-串联质谱法

Key words:  traditional Chinese medicine for animal  Quinolones  HPLC-MS/MS

摘要:

建立了高效液相色谱—串联质谱法检测兽用中药制剂双黄连注射液中中非法添加13种喹诺酮类药物的方法。样品经0.2%甲酸溶液溶解后稀释,以0.2%甲酸溶液与甲醇作为流动相进行梯度洗脱,采用多反应监测模式进行测定。13种喹诺酮类药物检测限(LOD)为0.1~0.5 ng/mL,定量限(LOQ)为1~5 mg/mL,在5.0~200 ng/mL范围内线性关系良好,相关系数均大于0.99在5 mg/mL、10 mg/mL、20mg/mL 三个添加浓度下,平均回收率90.9%～101.9%,相对标准偏差为0.6%～3.8%。该法准确、简单、快速。

Abstract:

A method of HPLC-MS/MS was developed to the determination 13 quinolones illegally added of in traditional Chinese medicine for animal . The sample was dissolved and diluted with 0.2% formic ,then Separate with HPLC which was using gradient elution with methanol and 0.2% formic acid. Qualitative and quantitative analysis of the 13 quinolones were carried out in multiple reactions monitoring mode (MRM)。The limits of detection (LODs) of 13 quinolones were in the range of 0.1~0.5 ng/ mL,the limits of quantitation (LOQs) of 13 quinolones were in the range of 1~5 mg/ mL . The correlation coefficient of 13 quinolones ranged from 5.0 ~ 200 ng / mL was greater than 0.99. The results showed that when the concentrations of 13 quinolones were between 5 and 20 mg/mL, the average recoveries ranged from90.9% to 101.9%, with relative standard deviations of 0.6% - 3.8%. The method was accurate, simple and fast.