Dr. Reddy's Laboratories Ltd., IPDO, Bachupally, Hyderabad 500072, AP, India.
J Pharm Biomed Anal. 2010 May 1;52(1):160-5. doi: 10.1016/j.jpba.2009.12.027. Epub 2009 Dec 28.
A novel stability-indicating normal phase liquid chromatographic (NP-LC) method was developed for the determination of purity of clopidogrel drug substance and drug products in bulk samples and pharmaceutical dosage forms in the presence of its impurities and degradation products. This method is capable of separating all the related substances of clopidogrel along with the chiral impurities. This method can be also be used for the estimation of assay of clopidogrel in drug substance as well as in drug product. The method was developed using Chiralcel OJ-H (250mmx4.6mm, 5microm) column. n-Hexane, ethanol and diethyl amine in 95:5:0.05 (v/v/v) ratio was used as a mobile phase. The eluted compounds were monitored at 240nm. Clopidogrel bisulfate was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. The degradation products were well resolved from main peak and its impurities, proving the stability-indicating power of the method. The developed method was validated as per International Conference on Harmonization (ICH) guidelines with respect to specificity, limit of detection, limit of quantification, precision, linearity, accuracy, robustness and system suitability.
一种新的用于在杂质和降解产物存在下测定氯吡格雷原料药和制剂中纯度的正相液相色谱（NP-LC）稳定性指示方法。该方法能够分离氯吡格雷的所有相关物质以及手性杂质。该方法还可用于测定原料药和制剂中氯吡格雷的含量。方法采用 Chiralcel OJ-H（250mmx4.6mm，5μm）柱。以正己烷、乙醇和二乙胺的 95:5:0.05（v/v/v）比例作为流动相。在 240nm 处监测洗脱化合物。硫酸氢氯吡格雷经受氧化、酸、碱、水解、热和光降解的应力条件。降解产物与主峰及其杂质很好地分离，证明了该方法的稳定性指示能力。所开发的方法符合国际协调会议（ICH）的指导原则，经过了专属性、检测限、定量限、精密度、线性、准确度、耐用性和系统适用性的验证。
