Kaila H O, Ambasana M A, Thakkar R S, Saravaia H T, Shah A K
National Facility for Drug Discovery through New Chemical Entities Development and Instrumentation support to Small Manufacturing Pharma Enterprises, Department of Chemistry, Saurashtra University, Rajkot - 360 005, India.
Indian J Pharm Sci. 2010 May;72(3):381-4. doi: 10.4103/0250-474X.70490.
A simple, precise and accurate HPLC method has been developed and validated for assay of lercanidipine hydrochloride in tablets and for determination of content uniformity. An isocratic separation was achieved using a Chromasil YMC Pack C(8), 150 × 4.6 mm i.d., 5µm particle size columns with a flow rate of 1 ml/min and using a UV detector to monitor the elute at 240 nm. The mobile phase consisted of 0.02 M ammonium dihydrogen phosphate buffer:methanol (35:65, v/v) with pH 3.5 adjusted with phosphoric acid. The method was validated for specificity, linearity, pre-cision, accuracy, robustness and solution stability. The specificity of the method was deter-mined by assessing interference from the placebo and by stress testing of the drug (forced degradation). The method was linear over the concentration range of 20-80 µg/ml (r(2)= 0.9992) with a limit of detection and quantitation of 0.1 and 0.3 µg/ml respectively. Intraday and interday system and method precision were determined and accuracy was between 99.3-101.9 %. The method was found to be robust and suitable for assay of lercanidipine hydrochloride in a tablet formulation and for determination of content uniformity. Degradation products resulting from the stress studies did not interfere with the detection of lercanidipine hydrochloride and the assay is thus stability-indicating.
已开发并验证了一种简单、精确且准确的高效液相色谱法，用于测定片剂中盐酸乐卡地平的含量及含量均匀度。采用Chromasil YMC Pack C(8) 柱（内径150×4.6 mm，粒径5μm），以1 ml/min的流速进行等度分离，使用紫外检测器在240 nm处监测洗脱液。流动相由0.02 M磷酸二氢铵缓冲液与甲醇（35:65，v/v）组成，用磷酸调节pH值至3.5。该方法在专属性、线性、精密度、准确度、稳健性和溶液稳定性方面均得到验证。通过评估安慰剂的干扰以及对药物进行强制降解试验来确定该方法的专属性。该方法在20 - 80 μg/ml的浓度范围内呈线性（r(2)= 0.9992），检测限和定量限分别为0.1和0.3 μg/ml。测定了日内和日间系统及方法的精密度，准确度在99.3 - 101.9%之间。结果表明该方法稳健，适用于片剂制剂中盐酸乐卡地平的含量测定及含量均匀度的测定。强制降解研究产生的降解产物不干扰盐酸乐卡地平的检测，因此该测定方法具有稳定性指示作用。
