Reddy P Sunil, Sudhakar Babu K, Kumar Navneet
Dr. Reddy's Laboratories Ltd., IPDO, Bachupally, Hyderabad-500072, A.P, India.
J Chromatogr Sci. 2013 Mar;51(3):242-9. doi: 10.1093/chromsci/bms134. Epub 2012 Sep 17.
A sensitive, stability-indicating gradient reverse phase high-performance liquid chromatography-ultraviolet method has been developed for the quantitative determination of process-related impurities and forced degradation products of rasagiline mesylate in pharmaceutical formulation. Efficient chromatographic separation was achieved on an ACE C8, 150 × 4.6 mm, 3 µm column with mobile phase containing a gradient mixture of solvents A and B. The flow rate of the mobile phase was 0.8 mL/min with column temperature of 30°C and detection wavelength at 210 nm. Rasagiline was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. Rasagiline was found to degrade significantly in acid and thermal stress conditions. The degradation products were well resolved from rasagiline and its impurities. The peak purity test results confirmed that the rasagiline peak was homogenous and pure in all stress samples and the mass balance was found to be more than 97%, thus proving the stability-indicating power of the method. The developed method was validated according to the guidelines of the International Conference on Harmonization with respect to specificity, linearity, limits of detection and quantification, accuracy, precision and robustness.
已开发出一种灵敏的、指示稳定性的梯度反相高效液相色谱 - 紫外法，用于定量测定药物制剂中甲磺酸雷沙吉兰的工艺相关杂质和强制降解产物。在ACE C8（150×4.6 mm，3 µm）色谱柱上，以含有溶剂A和B的梯度混合物的流动相实现了高效的色谱分离。流动相流速为0.8 mL/min，柱温为30°C，检测波长为210 nm。对雷沙吉兰进行了氧化、酸、碱、水解、热和光解降解等强制降解条件试验。发现雷沙吉兰在酸和热应激条件下显著降解。降解产物与雷沙吉兰及其杂质得到了很好的分离。峰纯度测试结果证实，在所有应激样品中雷沙吉兰峰均为均一纯峰，质量平衡大于97%，从而证明了该方法的指示稳定性能力。所开发的方法按照国际协调会议的指导原则，在专属性、线性、检测限和定量限、准确度、精密度和稳健性方面进行了验证。
