Department of Pharmaceutics, Faculty of Pharmacy, Hamdard University, Hamdard Nagar, New Delhi 110 062, India.
Saudi Pharm J. 2013 Jan;21(1):93-102. doi: 10.1016/j.jsps.2011.11.006. Epub 2011 Dec 4.
Stability-indicating high-performance thin-layer chromatographic (HPTLC) method for the analysis of ropinirole HCl was developed and validated as per the ICH guidelines. The method employed the mobile phase and toluene-ethyl acetate-6 M ammonia solution (5:6:0.5, v/v/v) was optimized with the help of a design expert. Densitometric analysis of ropinirole HCl was carried out in the absorbance mode at 250 and 254 nm. Compact spots for ropinirole HCl were found at R f value of 0.58 ± 0.02. The linear regression analysis data for the calibration plots showed R (2) = 0.9989 ± 0.0053 with a concentration range of 100-3000 ng spot(-1). The method was validated for precision, accuracy, ruggedness, robustness, specificity, recovery, limit of detection (LOD) and limit of quantitation (LOQ). The LOD and LOQ were 12.95 and 39.25 ng spot(-1) respectively. Drug was subjected to acidic, alkaline, oxidative, dry heat, wet heat and photo degradation stress. All the peaks of degradation products were well resolved from the standard drug peak with significant difference of R f. The acidic and alkaline stress degradation kinetics of ropinirole, were found to be in first order, showing high stability (t 1/2, 146.37 h(-1); t 0.9, 39.11 h(-1)) in the acidic medium and low stability (t 1/2, 97.67 h(-1); t 0.9, 14.87 h(-1)) in the alkaline environment.
开发并验证了一种用于盐酸罗匹尼罗分析的稳定性指示高效薄层色谱（HPTLC）方法，符合 ICH 指南。该方法使用了移动相，在设计专家的帮助下优化了甲苯-乙酸乙酯-6M 氨溶液（5:6:0.5，v/v/v）。盐酸罗匹尼罗的分光光度分析在 250nm 和 254nm 处的吸光度模式下进行。盐酸罗匹尼罗的斑点紧凑，R f 值为 0.58±0.02。校准图谱的线性回归分析数据表明 R （2）=0.9989±0.0053，浓度范围为 100-3000ng 点（-1）。该方法经过精密度、准确度、耐用性、鲁棒性、专属性、回收率、检测限（LOD）和定量限（LOQ）验证。LOD 和 LOQ 分别为 12.95 和 39.25ng 点（-1）。药物经过酸性、碱性、氧化、干热、湿热和光降解应激处理。所有降解产物的峰均与标准药物峰完全分离，R f 值有显著差异。盐酸罗匹尼罗的酸性和碱性应激降解动力学呈一级反应，在酸性介质中稳定性高（t 1/2，146.37 h（-1）；t 0.9，39.11 h（-1）），在碱性环境中稳定性低（t 1/2，97.67 h（-1）；t 0.9，14.87 h（-1））。
