Pharmaceutical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr El-Aini St., Cairo 11562, Egypt.
Talanta. 2011 Dec 15;87:222-9. doi: 10.1016/j.talanta.2011.10.001. Epub 2011 Oct 10.
A simple, selective and precise stability-indicating reversed-phase liquid chromatographic method was developed and validated for the determination of ciclesonide. Ciclesonide was subjected to acid and alkali hydrolysis, oxidation, thermal and photo-degradation. The degradation products were well separated from the pure drug. The method was based on isocratic elution of ciclesonide and its degradation products on reversed phase C18 column (250 mm × 4.6 mm, 10 μm) - Phenomenex using a mobile phase consisting of ethanol-water (70:30, v/v) at a flow rate of 1 mL min(-1). Quantitation was achieved with UV detection at 242 nm. Linearity, accuracy and precision were found to be acceptable over the concentration range of 5-200 μg mL(-1). Desisobutyryl-ciclesonide was prepared by selective alkaline hydrolysis of the ester and proved to be the main degradation product. The proposed method was successfully applied to the determination of ciclesonide in bulk and in its pharmaceutical preparation.
建立并验证了一种用于测定昔萘酸氯米松的简单、专属且灵敏的反相高效液相色谱法。昔萘酸氯米松经酸、碱水解，氧化，热及光降解。降解产物与原料药能很好地分离。该方法基于昔萘酸氯米松与其降解产物在 Phenomenex 反相 C18 柱（250mm×4.6mm，10μm）上以乙醇-水（70:30，v/v）为流动相，采用等度洗脱，流速为 1mL/min，于 242nm 处进行紫外检测。在 5-200μg/mL 浓度范围内，线性、准确度和精密度均良好。通过选择性碱性水解酯得到主要降解产物去异丁酰基昔萘酸氯米松。该方法成功地应用于原料药及制剂中昔萘酸氯米松的测定。
