Seerapu Sunitha, Srinivasan B P
Department of Quality Assurance, Delhi Institute of Pharmaceutical Sciences and Research (DIPSAR), Goverment of N. C. T. of Delhi, M. B. Road, Pushp Vihar, Sector-3, New Delhi-110 017, India.
Indian J Pharm Sci. 2010 Sep;72(5):667-71. doi: 10.4103/0250-474X.78545.
A simple, sensitive, precise and robust reverse-phase high-performance liquid chromatographic method for analysis of ivabradine hydrochloride in pharmaceutical formulations was developed and validated as per ICH guidelines. The separation was performed on SS Wakosil C18AR, 250×4.6 mm, 5 μm column with methanol:25 mM phosphate buffer (60:40 v/v), adjusted to pH 6.5 with orthophosphoric acid, added drop wise, as mobile phase. A well defined chromatographic peak of Ivabradine hydrochloride was exhibited with a retention time of 6.55±0.05 min and tailing factor of 1.14 at the flow rate of 0.8 ml/min and at ambient temperature, when monitored at 285 nm. The linear regression analysis data for calibration plots showed good linear relationship with R=0.9998 in the concentration range of 30-210 μg/ml. The method was validated for precision, recovery and robustness. Intra and Inter-day precision (% relative standard deviation) were always less than 2%. The method showed the mean % recovery of 99.00 and 98.55 % for Ivabrad and Inapure tablets, respectively. The proposed method has been successfully applied to the commercial tablets without any interference of excipients.
开发了一种简单、灵敏、精确且稳健的反相高效液相色谱法，用于分析药物制剂中的盐酸伊伐布雷定，并根据国际协调会议（ICH）指南进行了验证。分离在SS Wakosil C18AR 250×4.6 mm、5μm柱上进行，以甲醇:25 mM磷酸盐缓冲液（60:40 v/v）为流动相，用正磷酸逐滴调节至pH 6.5。在285 nm处监测时，在0.8 ml/min的流速和室温下，盐酸伊伐布雷定呈现出一个清晰的色谱峰，保留时间为6.55±0.05 min，拖尾因子为1.14。校准曲线的线性回归分析数据显示，在30 - 210μg/ml的浓度范围内，线性关系良好，R = 0.9998。该方法在精密度、回收率和稳健性方面进行了验证。日内和日间精密度（相对标准偏差%）始终小于2%。该方法对伊伐布雷定片和Inapure片的平均回收率分别为99.00%和98.55%。所提出的方法已成功应用于市售片剂，无辅料干扰。
