Jubilant Life Sciences Ltd., Analytical Research Department, R&D Centre, C-26, Sector-59, Noida, Uttar Pradesh 201 301, India.
J Pharm Biomed Anal. 2012 Jan 25;58:136-40. doi: 10.1016/j.jpba.2011.09.009. Epub 2011 Sep 19.
A novel, sensitive, stability indicating simultaneous dual wavelength reverse phase UV-HPLC method has been developed for the quantitative determination of potential impurities of fampridine active pharmaceutical ingredient. Efficient chromatographic separation was achieved on a C18 stationary phase in gradient mode and quantitation by ultraviolet dual wavelength detection. The method was validated according to ICH guidelines with respect to specificity, precision, linearity and accuracy. Regression analysis showed correlation coefficient value greater than 0.999 for fampridine and its seven impurities. Detection limit as low as 0.003% was achieved for fampridine N-oxide and 0.01% for other impurities. Accuracy of the method was established based on the recovery obtained between 93.3% and 110.0% for all impurities. The method was found to be specific, selective to the degradation products and robust. Peak purity analysis by PDA detector confirmed the specificity of the method. Major degradation of the drug substance was found to occur under oxidative stress conditions to form fampridine N-oxide.
一种新颖、灵敏、专属性强的同时双波长反相高效液相色谱法（RP-HPLC）已被开发用于定量测定苯丁胺的潜在杂质。在梯度模式下，采用 C18 固定相实现了高效的色谱分离，并通过紫外双波长检测进行定量。该方法按照 ICH 指南进行了专属性、精密度、线性和准确度验证。对于苯丁胺及其七种杂质，回归分析显示相关系数值大于 0.999。对于苯丁胺 N-氧化物，检测限低至 0.003%；对于其他杂质，检测限低至 0.01%。该方法的准确度是基于所有杂质的回收率在 93.3%至 110.0%之间来确定的。该方法被发现具有特异性、对降解产物具有选择性且稳健。通过 PDA 检测器进行的峰纯度分析证实了该方法的专属性。在氧化应激条件下，药物发生主要降解，形成苯丁胺 N-氧化物。
