氟喹诺酮类药物粉剂中非法添加四种喹噁啉类药物的UPLC检测方法研究

Study on the Determination Method of Quinoxalines in Quinolones Powder by UPLC

关键词:  超高效液相色谱法  氟喹诺酮类粉剂  喹噁啉类

Key words:  SUPLC  Squinolones powder.  Squinoxalines

摘要:

建立了超高效液相色谱法测定氟喹诺酮类粉剂中非法添加喹乙醇、乙酰甲喹、卡巴氧以及喹烯酮的方法。采用purospher RP-18 色谱柱( 2.1×100 mm,粒径2.0 μm ),以磷酸溶液和甲醇-乙腈( 7.5：7.0 )为流动相进行梯度洗脱,流速0.3 mL/min,柱温30℃,进样量为5 μL,采用二极管阵列检测器,采集波长范围为200~400 nm,分辨率为 1.2 nm,记录光谱图和365 nm波长处的色谱图。结果显示,四种喹噁啉类药物的浓度在0.2 ~ 100 μg/mL范围内的线性良好,相关系数r均为0.9999,回收率在98.2％～100.2%范围内,RSD在0.27％～0.89% 之间,检测限200 mg/Kg。本方法快速、准确,可用于氟喹诺酮类粉剂中非法添加喹噁啉类药物的定性和定量检测。

Abstract:

A method for detection of olaquindox, maquindox, carbadox, quinocetone in quinolones Powder by UPLC was developed. Purospher RP-18 column ( 2.1×100 mm, 2.0 μm) was used with the mobile phase consisted of phosphoric acid solution and methanol-acetonitrile( 7.5:7.0 ). The flow rate was 0.3 mL/min; the column temperture was 30℃; the wavelength range was 200~400nm. The result showed that the standard curves for four quinoxalines were in good linearity within a concentration range of 0.2～100 μg/mL( r=0.9999 ), the recoveries for quinoxalines in quinolones powder ranged between 98.2% and 100.2% with the RSD from 0.27% to 0.89%. The limit of detection( LOD ) was 200 mg/Kg. The method was fast and accurate, and could be used for identification and determination of the quinoxalines in quinolones powder.