盐酸屈他维林的晶体结构及其含量测定方法

Crystal Structure and Content Determination of Drotaverine Hydrochloride

通过乙醇结晶得到盐酸屈他维林的单晶,并采用粉末X射线衍射和单晶X射线衍射,确定了自制盐酸屈他维林是带有0.5个乙醇分子的、含碳氮双键的喹啉结构。采用电位滴定法和紫外分光光度法,分别建立了盐酸屈他维林含量测定的两种方法。使用紫外分光光度法测得样品在4~12μg/mL范围内线性关系良好,精密度、重复性和稳定性的RSD(相对标准偏差)分别为0.15%、0.31%、0.25%,回收率在98.1%~100%之间,该方法测得3批供试品含量分别为100.15%、101.56%、99.74%;电位滴定法显示样品范围在0.1~0.3 g内有良好的线性关系,重复性RSD为0.47%,平均回收率为99.9%,测得3批样品含量分别为99.51%、101.87%、100.03%。结果表明:两种方法均能用于盐酸屈他维林的含量检测,满足原料药质量要求。

Single crystal of drotaverine hydrochloride was prepared by crystallization in ethanol,and it is confirmed that the self-made drotavarine hydrochloride has a quinoline structure with a carbon-nitrogen double bond and 0.5 ethanol molecule through powder X-ray diffractometry and single-crystal X-ray diffraction.Using ultraviolet(UV)spectrophotometry and potentiometric titration,two methods for content determination of drotaverine hydrochloride were established.The sample has a good linear relationship in the range of 4-12 μg/mL through UV spectrophotometry.Its relative-standard-deviations of precision,repeatability and stability are 0.15%,0.31% and 0.25%,respectively,with the recovery rate of 98.1%-100%.By UV method,the content of the three batches of test product is 100.15%,101.56%,and 99.74%,respectively;Meanwhile,the potentiometric titration method shows the sample has a good linear relationship in the range of 0.1-0.3 g,when the repeatability of relative standard deviation is 0.47% and the average recovery rate is 99.9%,the content of three batches of samples is 99.51%,101.87%,and 100.03%,respectively.The results show that two methods could be used for content determination of drotavarine hydrochloride which meets the quality requirements of active pharmaceutical ingredient.