Pujeri Sudhakar S, Khader Addagadde M A, Seetharamappa Jaldappagari
Department of Chemistry, Mangalore University, Mangalagangotri, India.
Sci Pharm. 2012 Jan-Mar;80(1):115-26. doi: 10.3797/scipharm.1109-22. Epub 2011 Dec 5.
A simple, rapid and stability-indicating reversed-phase liquid chromatographic method was developed for the assay of varenicline tartrate (VRT) in the presence of its degradation products generated from forced decomposition studies. The HPLC separation was achieved on a C18 Inertsil column (250 mm × 4.6 mm i.d. particle size is 5 μm) employing a mobile phase consisting of ammonium acetate buffer containing trifluoroacetic acid (0.02M; pH 4) and acetonitrile in gradient program mode with a flow rate of 1.0 mL min(-1). The UV detector was operated at 237 nm while column temperature was maintained at 40 °C. The developed method was validated as per ICH guidelines with respect to specificity, linearity, precision, accuracy, robustness and limit of quantification. The method was found to be simple, specific, precise and accurate. Selectivity of the proposed method was validated by subjecting the stock solution of VRT to acidic, basic, photolysis, oxidative and thermal degradation. The calibration curve was found to be linear in the concentration range of 0.1-192 μg mL(-1) (R(2) = 0.9994). The peaks of degradation products did not interfere with that of pure VRT. The utility of the developed method was examined by analyzing the tablets containing VRT. The results of analysis were subjected to statistical analysis.
建立了一种简单、快速且具有稳定性指示功能的反相液相色谱法，用于在酒石酸伐尼克兰（VRT）强制降解研究产生的降解产物存在的情况下对其进行测定。高效液相色谱分离在C18 Inertsil柱（250 mm×4.6 mm内径，粒径5μm）上进行，采用由含三氟乙酸（0.02M；pH 4）的醋酸铵缓冲液和乙腈组成的流动相，以梯度程序模式运行，流速为1.0 mL min(-1)。紫外检测器在237 nm波长下运行，柱温保持在40℃。按照国际协调会议（ICH）指南对所建立的方法在特异性、线性、精密度、准确度、稳健性和定量限方面进行了验证。该方法被发现简单、特异、精密且准确。通过对VRT储备溶液进行酸性、碱性、光解、氧化和热降解，验证了所提出方法的选择性。校准曲线在0.1 - 192μg mL(-1)浓度范围内呈线性（R(2)=0.9994）。降解产物的峰不干扰纯VRT的峰。通过分析含VRT的片剂检验了所建立方法的实用性。对分析结果进行了统计分析。
