Mulgund S V, Phoujdar M S, Londhe S V, Mallade P S, Kulkarni T S, Deshpande A S, Jain K S
Department of Pharmaceutical Chemistry, Sinhgad College of Pharmacy, Vadgaon (Bk), Pune-411 041, India.
Indian J Pharm Sci. 2009 Jan;71(1):35-40. doi: 10.4103/0250-474X.51950.
A simple, specific, accurate and stability-indicating reversed phase high performance liquid chromatographic method was developed for the simultaneous determination of mephenesin and diclofenac diethylamine, using a Spheri-5-RP-18 column and a mobile phase composed of methanol: water (70:30, v/v), pH 3.0 adjusted with o-phosphoric acid. The retention times of mephenesin and diclofenac diethylamine were found to be 3.9 min and 14.5 min, respectively. Linearity was established for mephenesin and diclofenac diethylamine in the range of 50-300 mug/ml and 10-60 mug/ml, respectively. The percentage recoveries of mephenesin and diclofenac diethylamine were found to be in the range of 99.06-100.60% and 98.95-99.98%, respectively. Both the drugs were subjected to acid, alkali and neutral hydrolysis, oxidation, dry heat, photolytic and UV degradation. The degradation studies indicated, mephenesin to be susceptible to neutral hydrolysis, while diclofenac diethylamine showed degradation in acid, H(2)O(2), photolytic and in presence of UV radiation. The degradation products of diclofenac diethylamine in acidic and photolytic conditions were well resolved from the pure drug with significant differences in their retention time values. This method can be successfully employed for simultaneous quantitative analysis of mephenesin and diclofenac diethylamine in bulk drugs and formulations.
建立了一种简单、特异、准确且具有稳定性指示作用的反相高效液相色谱法，用于同时测定美芬新和双氯芬酸二乙胺，采用Spheri-5-RP-18色谱柱，流动相为甲醇:水(70:30, v/v)，用正磷酸调至pH 3.0。结果发现美芬新和双氯芬酸二乙胺的保留时间分别为3.9分钟和14.5分钟。美芬新和双氯芬酸二乙胺的线性范围分别为50 - 300μg/ml和10 - 60μg/ml。美芬新和双氯芬酸二乙胺的回收率分别在99.06% - 100.60%和98.95% - 99.98%范围内。两种药物均进行了酸、碱和中性水解、氧化、干热、光解及紫外降解试验。降解研究表明，美芬新易受中性水解影响，而双氯芬酸二乙胺在酸性、过氧化氢、光解及紫外辐射条件下会发生降解。双氯芬酸二乙胺在酸性和光解条件下的降解产物与纯药物能很好地分离，其保留时间值有显著差异。该方法可成功用于原料药和制剂中美芬新和双氯芬酸二乙胺的同时定量分析。
