Goswami Nishant, Gupta V Rama Mohan, Jogia Hitesh A
Analytical Research and Development, Integrated Product Development, Dr. Reddy's Laboratories Ltd., Bachupally, Hyderabad-500 072, India. ; Singhania University, Pacheri Bari, Dist. Jhunjhunu, Rajasthan-333 515, India.
Sci Pharm. 2013 Apr-Jun;81(2):505-18. doi: 10.3797/scipharm.1301-21. Epub 2013 Feb 25.
A stability-indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed for the simultaneous determination of halometasone, fusidic acid, methylparaben, and propylparaben in topical pharmaceutical formulation. The desired chromatographic separation was achieved on an Agilent Zorbax CN (Cyano), 5 μm (250 × 4.6 mm) column using gradient elution at 240 nm detector wavelength. The optimized mobile phase consisted of a mixture of 0.01 M phosphate buffer and 0.1% orthophosphoric acid, pH-adjusted to 2.5 with an ammonia solution as solvent-A and acetonitrile as solvent-B. The developed method separated halometasone, fusidic acid, methylparaben, and propylparaben in the presence of known impurities/degradation products. The stability-indicating capability was established by forced degradation experiments and separation of known and unknown degradation products. The developed RP-HPLC method was validated according to the International Conference on Harmonization (ICH) guidelines. This validated method was applied for the simultaneous estimation of HM, FA, MP, and PP in commercially available cream samples. Further, the method can be extended for the estimation of HM, FA, MP, and PP in various commercially available dosage forms.
建立了一种稳定性指示反相高效液相色谱（RP-HPLC）法，用于同时测定局部用药物制剂中的卤米松、夫西地酸、对羟基苯甲酸甲酯和对羟基苯甲酸丙酯。在安捷伦Zorbax CN（氰基）5μm（250×4.6mm）色谱柱上，采用梯度洗脱，在240nm检测波长下实现了所需的色谱分离。优化的流动相由0.01M磷酸盐缓冲液和0.1%正磷酸的混合物组成，用氨溶液将pH值调至2.5作为溶剂A，乙腈作为溶剂B。所建立的方法在存在已知杂质/降解产物的情况下，可分离卤米松、夫西地酸、对羟基苯甲酸甲酯和对羟基苯甲酸丙酯。通过强制降解实验以及已知和未知降解产物的分离，确立了该方法的稳定性指示能力。所建立的RP-HPLC方法按照国际协调会议（ICH）指南进行了验证。该验证方法用于同时测定市售乳膏样品中的卤米松、夫西地酸、对羟基苯甲酸甲酯和对羟基苯甲酸丙酯。此外，该方法可扩展用于测定各种市售剂型中的卤米松、夫西地酸、对羟基苯甲酸甲酯和对羟基苯甲酸丙酯。
