Dabhi Batuk, Jadeja Yashwantsinh, Patel Madhavi, Jebaliya Hetal, Karia Denish, Shah Anamik
Department of Chemistry, Saurashtra University, Rajkot-360 005, Gujarat, India.
Sci Pharm. 2013 Jan-Mar;81(1):115-22. doi: 10.3797/scipharm.1209-15. Epub 2012 Nov 5.
A simple, precise, and accurate HPLC method has been developed and validated for the quantitative analysis of Dronedarone Hydrochloride in tablet form. An isocratic separation was achieved using a Waters Symmetry C8 (100 × 4.6 mm), 5 μm particle size column with a flow rate of 1 ml/min and UV detector at 290 nm. The mobile phase consisted of buffer: methanol (40:60 v/v) (buffer: 50 mM KH2PO4 + 1 ml triethylamine in 1 liter water, pH=2.5 adjusted with ortho-phosphoric acid). The method was validated for specificity, linearity, precision, accuracy, robustness, and solution stability. The specificity of the method was determined by assessing interference from the placebo and by stress testing the drug (forced degradation). The method was linear over the concentration range 20-80 μg/ml (r(2) = 0.999) with a Limit of Detection (LOD) and Limit of Quantitation (LOQ) of 0.1 and 0.3 μg/ml respectively. The accuracy of the method was between 99.2-100.5%. The method was found to be robust and suitable for the quantitative analysis of Dronedarone Hydrochloride in a tablet formulation. Degradation products resulting from the stress studies did not interfere with the detection of Dronedarone Hydrochloride so 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，用于定量分析片剂形式的盐酸决奈达隆。采用沃特世Symmetry C8（100×4.6 mm）、粒径5μm的色谱柱，以1 ml/min的流速和290 nm的紫外检测器实现等度分离。流动相由缓冲液：甲醇（40:60 v/v）组成（缓冲液：50 mM KH2PO4 + 1升水中含1 ml三乙胺，用正磷酸调节pH = 2.5）。该方法针对专属性、线性、精密度、准确度、稳健性和溶液稳定性进行了验证。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) = 0.999），检测限（LOD）和定量限（LOQ）分别为0.1和0.3 μg/ml。该方法的准确度在99.2 - 100.5%之间。发现该方法稳健，适用于片剂制剂中盐酸决奈达隆的定量分析。强制降解研究产生的降解产物不干扰盐酸决奈达隆的检测，因此该测定具有稳定性指示作用。
