Kothapalli Pavan Kumar S R, Khagga Mukkanti, Mekala Nageswara Rao, Sigamani John Prasanna, Vundavilli Jagadeesh Kumar, Masani Narendra Kumar, Sharma Hemant Kumar
Aurobindo Pharma Limited Research Centre, 313, Bachupally, Hyderabad-500 090, Andhra Pradesh, India.
Sci Pharm. 2012 Jan-Mar;80(1):77-87. doi: 10.3797/scipharm.1107-14. Epub 2011 Oct 20.
A simple and sensitive ion chromatography method has been developed for the determination of cyclopropylamine (CPA) in nevirapine (NEV) and moxifloxacin HCl (MOX) pharmaceutical drug substances. Efficient chromatographic separation was achieved on a Metrosep C4, 5 μm (250 mm × 4.0 mm) column. The mobile phase consists of 5 mM hydrochloric acid containing 10% (v/v) acetonitrile and was delivered in an isocratic mode at a flow rate of 0.9 mL min(-1) at 27°C. A conductometric detector was used for the detection of the analyte. The drug substances were subjected to stress conditions including oxidation, thermal, photolytic and humidity for the evaluation of the stability-indicating nature of the method. The method was validated for specificity, precision, linearity, accuracy and solution stability. The limit of detection (LOD) and limit of quantification (LOQ) values are 0.10 μg mL(-1) and 0.37 μg mL(-1) respectively. The linearity range of the method is between 0.37 μg mL(-1) and 1.5 μg mL(-1) and the correlation coefficient is found to be 0.9971. The average recoveries of CPA in NEV and MOX are 97.0% and 98.0%, respectively.
已开发出一种简单且灵敏的离子色谱法，用于测定奈韦拉平（NEV）和盐酸莫西沙星（MOX）药物原料中的环丙胺（CPA）。在Metrosep C4，5μm（250mm×4.0mm）色谱柱上实现了高效的色谱分离。流动相由含10%（v/v）乙腈的5mM盐酸组成，在27°C下以0.9mL min⁻¹的流速等度输送。使用电导检测器检测分析物。对药物原料进行了氧化、热、光解和湿度等强制条件处理，以评估该方法的稳定性指示特性。该方法在特异性、精密度、线性、准确度和溶液稳定性方面进行了验证。检测限（LOD）和定量限（LOQ）值分别为0.10μg mL⁻¹和0.37μg mL⁻¹。该方法的线性范围在0.37μg mL⁻¹至1.5μg mL⁻¹之间，相关系数为0.9971。NEV和MOX中CPA的平均回收率分别为97.0%和98.0%。
