摘要
目的建立高效液相色谱法测定盐酸伊伐布雷定及其片剂中有关物质的方法。方法采用CHIRALPAK AD-H手性柱,流动相为正己烷-异丙醇（0.1%三乙胺）（60∶40）,检测波长为286 nm,柱温为25℃,流速为0.8mL.min-1,对R-盐酸伊伐布雷定进行分析;采用Kromasil C18柱,流动相为乙腈-pH 7.6磷酸盐缓冲液（30∶70-40∶60）梯度洗脱,检测波长为220nm,柱温为25℃,流速为1.0mL.min-1,对其他有关物质进行分析。结果 R-异构体测定中,检测限为2.12ng,定量限为20ng,精密度RSD为1.11%（n=6）,重复性试验与样品测试均未检出R-异构体;其他有关物质测定中,系统适用性试验盐酸伊伐布雷定和相邻峰的分离度为1.91,主峰与杂质A、杂质B、杂质C达到基线分离,专属性试验结果良好。有关物质测定平均值为0.62%。结论该方法准确、可靠、简便,适用于测定盐酸伊伐布雷定片的质量控制。
Objective To establish a HPLC method for determination of the related substances in Ivabradine Hydrochloride and Ivabradine Hydrochloride Tablets.Methods The method for analysis of the related substance of R-ivabradine hydrochloride was as followed.The chiralhplc column CHIRALPAK AD-H was used.The mobile phase consisted of n-hexane and isopropanol（0.1% triethylamine）（60∶40）.The detective wavelength was set at 286nm and the column temperature was 25℃.The flow rate was 0.8mL·min-1.The method for analysis of the other related substances was as followed.The Kromasil C18 column was used.The mobile phase consisted of acetonitrile-（pH 7.6）buffer phosphate（30∶70-40∶60）with gradient elution.The flow rate was 1.0mL·min-1.The detective wavelength was set at 220nm and the column temperature was 25℃.Results In determination of R-isomerizes of Ivabradine Hydrochloride,the limit of detection was 2.12ng,the limit of quantitation was 20ng,RSD=1.11%（n=6）,and R-isomerizesin the repeatability and the determination tests was not detected.In determination of the other related substances,the resolution of impurities was well in the system test.The resolution of ivabradine peak and adjacent impurity peak was 1.91.The main peak and the other peaks were separated in baseline.The specificity was well.The average determination of the related substances in Ivabradine Hydrochloride Tablets was 0.62%.Conclusion The method is accurate,reliable and simple,and suitable for the quality control of Ivabradine Hydrochloride Tablets.
出处
《中国药事》
CAS
2011年第5期476-480,共5页
Chinese Pharmaceutical Affairs
