止痢散、杨树花口服液中非法添加盐酸小檗碱检测方法的建立

To establish a method for the determination of illegally added berberine hydrochloride in Zhili Powder and Yangshuhua Koufuye

关键词:  盐酸小檗碱  止痢散  杨树花口服液  高效液相色谱-二极管阵列检测法

Key words:  Berberine Hydrochloride  Zhili Powder  Yangshuhua Koufuye  HPLC-PDA

摘要:

建立止痢散、杨树花口服液中非法添加盐酸小檗碱的HPLC-PDA检测方法,采用十八烷基键合硅胶为填充剂,乙腈-0.05 mol/L磷酸二氢钾溶液(用磷酸调pH值至3.0)(25∶75)为流动相,等度洗脱,流速为1.0 mL/min,二极管阵列检测器,提取波长为345 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。按外标法以峰面积计算,盐酸小檗碱在止痢散和杨树花口服液中的平均回收率分别为99.8% 和99.7%,RSD分别为0.3% 和0.4%；线性方程为Y=41435X-15904,R2^{=0.9999；检测限分别为0.2 g/kg,0.2 g/L。该检测方法专属型强,灵敏度高,操作简便,准确可靠,可用于测定止痢散、杨树花口服液中非法添加的盐酸小檗碱。}

Abstract:

A method for the determination of berberine hydrochloride illegally added in Zhili Powder and Yangshuhua Koufuye was developed by the high performance liquid chromatography with photo diode array detector. It was tested with C18 column, using Acetonitrile -0.05 mol/L potassium dihydrogen phosphate solution (Adjust the pH to 3.0 with phosphoric acid) (V:V=25:75) as mobile phase for Isometric elution, flow rate was 1 mL per minute. The extract wavelength was 345 nm. Peak purity test and spectrum similar test were used to determine the illegally added drug except the method of comparison between sample and reference. The peak area is calculated according to the external standard method, the mean recovery of berberine hydrochloride in Zhili Powder and Yangshuhua Koufuye was 99.8% and 99.7%, and RSD was 0.3% and 0.4% respectively. The linear equation is Y=41435X-15904, R2^=0.9999, and the detection limits are 0.2 g/kg and 0.2 g/L respectively. In conclusion, the method is specificity, sensitive, simple, accurate and reliable, which can be used to determine berberine hydrochloride illegally added in Zhili Powder and Yangshuhua Koufuye.