Panda Sagar Suman, Patanaik Debasis, Ravi Kumar Bera V V
Department of Pharmaceutical Analysis and Quality Assurance, Roland Institute of Pharmaceutical Sciences, Khodasingi, 760010, Berhampur (Orissa), India.
Sci Pharm. 2012 Jan-Mar;80(1):127-37. doi: 10.3797/scipharm.1109-16. Epub 2011 Dec 5.
A simple, precise and accurate isocratic RP-HPLC stability-indicating assay method has been developed to determine diclofenac potassium and metaxalone in their combined dosage forms. Isocratic separation was achieved on a Hibar-C(18), Lichrosphere-100(®) (250 mm × 4.6 mm i.d., particle size 5 μm) column at room temperature in isocratic mode, the mobile phase consists of methanol: water (80:20, v/v) at a flow rate of 1.0 ml/min, the injection volume was 20 μl and UV detection was carried out at 280nm. The drug was subjected to acid and alkali hydrolysis, oxidation, photolysis and heat as stress conditions. The method was validated for specificity, linearity, precision, accuracy, robustness and system suitability. The method was linear in the drug concentration range of 2.5-30 μg/ml and 20-240 μg/ml for diclofenac potassium and metaxalone, respectively. The precision (RSD) of six samples was 0.83 and 0.93% for repeatability, and the intermediate precision (RSD) among six-sample preparation was 1.63 and 0.49% for diclofenac potassium and metaxalone, respectively. The mean recoveries were between 100.99-102.58% and 99.97-100.01% for diclofenac potassium and metaxalone, respectively. The proposed method can be used successfully for routine analysis of the drug in bulk and combined pharmaceutical dosage forms.
已开发出一种简单、精确且准确的等度反相高效液相色谱稳定性指示测定法，用于测定双氯芬酸钾和美他沙酮复方制剂中的这两种药物。在室温下，采用等度模式，在Hibar-C(18)、Lichrosphere-100(®)（250 mm×4.6 mm内径，粒径5μm）色谱柱上实现等度分离，流动相由甲醇:水（80:20，v/v）组成，流速为1.0 ml/min，进样体积为20μl，在280nm波长处进行紫外检测。将药物分别置于酸、碱水解、氧化、光解和加热等条件下作为强制降解试验。该方法在专属性、线性、精密度、准确度、耐用性和系统适用性方面得到了验证。该方法对于双氯芬酸钾和美他沙酮，在药物浓度范围分别为2.5 - 30μg/ml和20 - 240μg/ml时呈线性。六个样品的重复性精密度（RSD），双氯芬酸钾和美他沙酮分别为0.83%和0.93%，六个样品制备之间的中间精密度（RSD），双氯芬酸钾和美他沙酮分别为1.63%和0.49%。双氯芬酸钾和美他沙酮的平均回收率分别在100.99 - 102.58%和99.97 - 100.01%之间。所提出的方法可成功用于原料药及复方制剂中该药物的常规分析。
