El Gammal Reem N, Hammouda Mohammed E A, El-Wasseef Dalia R, El-Ashry Saadia M
Department of Medicinal Chemistry, Faculty of Pharmacy, Mansoura University, 35516 Mansoura, Egypt.
Department of Pharmaceutical Chemistry, Faculty of Pharmacy, Horus University in Egypt (HUE), New Damietta, Egypt.
J Chromatogr Sci. 2018 Apr 1;56(4):367-374. doi: 10.1093/chromsci/bmy011.
A simple rapid and accurate micellar high performance liquid chromatographic method was improved and validated for the analysis of mixture containing gatifloxacin sesquihydrate (GTF) and prednisolone acetate (PRED) in their synthetic mixture and their combined preparation. The separation was achieved using a C18 column, micellar mobile phase consisted of 0.2 M sodium dodecyl sulfate, 12.5% n-propanol and 0.3% triethylamine in 0.02 M orthophosphoric acid at pH 7.0 at a flow rate of 1 ml/min with UV detection at 270 nm. The proposed method was found to be rectilinear over the concentration ranges of 5.0-45 μg ml-1 and 10-50 μg ml-1 with recovery percentage of 99.95 ± 0.82 and 100.07 ± 0.84 for GTF and PRED, respectively. The separation of both drugs was accomplished in a very short chromatographic run (<5 min), the method is reproducible (R.S.D. < 1.0%) and show satisfactory resolution between GTF and PRED (Rs) = 1.67. The developed method was validated according to International Conference on Harmonization (ICH) guidelines. The limit of detection of the proposed method was 0.33 and 0.21 μg ml-1, and the limit of quantitation was 0.99 and 0.64 μg ml-1 for GTF and PRED, respectively.
一种简单、快速且准确的胶束高效液相色谱法得到改进并经过验证，用于分析合成混合物及其复方制剂中含有的加替沙星倍半水合物（GTF）和醋酸泼尼松龙（PRED）。采用C18柱进行分离，胶束流动相由0.2 M十二烷基硫酸钠、12.5%正丙醇和0.3%三乙胺溶于0.02 M pH 7.0的正磷酸中组成，流速为1 ml/min，于270 nm处进行紫外检测。结果表明，该方法在5.0 - 45 μg/ml和10 - 50 μg/ml的浓度范围内呈线性，GTF和PRED的回收率分别为99.95 ± 0.82和100.07 ± 0.84。两种药物在极短的色谱运行时间（<5分钟）内实现分离，该方法具有可重复性（相对标准偏差<1.0%），且GTF和PRED之间的分离度令人满意（Rs = 1.67）。所开发的方法根据国际协调会议（ICH）指南进行了验证。该方法对GTF和PRED检测限分别为0.33和0.21 μg/ml，定量限分别为0.99和0.64 μg/ml。
