氟喹诺酮类制剂中非法添加对乙酰氨基酚和安乃近的测定方法研究

Dtermination of Paracetamol and Metamizole Sodium in the Fluoroquinolones

为了建立氟喹诺酮类制剂中非法添加对乙酰氨基酚和安乃近的测定方法。采用TLC法进行快速筛查;采用HPLC-PDA法进行确证与判定。以十八烷基键合硅胶为填充剂,以磷酸盐缓冲液(取磷酸二氢钠3.0 g,加水1 000 m L使溶解,加三乙胺0.5 m L,用氢氧化钠饱和溶液调节p H值至7.0)为流动相A,甲醇为流动相B,梯度洗脱,流速为1.0 m L/min,二极管阵列检测器,提取波长为244 nm。采用峰纯度检查和光谱相似度检查辅助对照品比对方法,对非法添加药物进行确证。TLC法简便快速,专属性强,可作为非法添加的快速初筛;HPLC-PDA法准确、可靠,可用于同时测定氟喹诺酮类制剂中非法添加的对乙酰氨基酚和安乃近。

To establish a method to identify illegally added paracetamol and metamizole sodium in the fluoroquinolones.Rapid screening was performed by TLC method and final determination was performed by high performance liquid chromatography with photodiode array detector（HPLC-PDA）. It was tested with C18 column,using gradient elution with phosphate buffer（dissolve sodium dihydrogen phosphate 3.0 g to 1000 m L,add triethylamine 0.5 m L,adjusting p H to 7.0 by sodium hydroxide）and methanol as the mobile phase at a flow rate of 1.0 m L/m L.The extract wavelength was 244 nm.Peak purity test and spectrum similar test were used to determine the paracetamol and metamizole sodium except the method of comparison between sample and reference. In conclusion,the method is simple,accurate and reliable for the determination of paracetamol and metamizole sodium in the fluoroquinolones.