Nalwade Santaji, Reddy Vangala Ranga, Kulkarni Dipak, Todamal Sandip
Department of Chemistry, Jawaharlal Neharu Technological University, Kukatpally, Hyderabad, Andhra Pradesh 500 072, India Analytical Research and Development, SAI Life Sciences Ltd., Pune 411 057, India
Analytical Research and Development, Integrated Product Development, Dr. Reddy's Laboratories Ltd., Bachupally, Hyderabad 500 072, India.
J Chromatogr Sci. 2015 Jan;53(1):127-34. doi: 10.1093/chromsci/bmu029. Epub 2014 Apr 30.
A novel, sensitive, stability-indicating, gradient, reverse-phase high-performance liquid chromatographic method has been developed for quantitative determination of halobetasol propionate and its impurities in topical dosage forms. The chromatographic separation was achieved on a Phenomenex Synergi polar reverse phase, 250 × 4.6 mm, 4 µm column. Mobile phase A comprises a mixture of 0.01 M KH2PO4 buffer containing 0.2% 1-octane sulfonic acid sodium salt (pH 3.0), acetonitrile and methanol in the ratio 80:15:05 (v/v/v), respectively, and mobile phase B contains a mixture of 0.01 M KH2PO4 buffer containing 0.2% 1-octane sulfonic acid sodium salt (pH 3.0), acetonitrile and methanol in the ratio 20:70:10 (v/v/v), respectively. The flow rate is 0.8 mL min(-1). The column compartment temperature is set at 40°C and the detection wavelength is set at 240 nm. The resolutions between Halobetasol propionate and all the impurities are >2.0 for all pairs of compounds. The drug product was subjected to International Conference on Harmonization (ICH)-prescribed hydrolytic, oxidative, photolytic and thermal stress conditions. The method is validated as per the ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision, robustness and ruggedness.
已开发出一种新颖、灵敏、稳定性指示、梯度反相高效液相色谱法，用于定量测定局部用剂型中丙酸氯倍他索及其杂质。色谱分离在Phenomenex Synergi极性反相柱（250×4.6 mm，4 µm）上进行。流动相A分别由含0.2% 1-辛烷磺酸钠盐的0.01 M KH2PO4缓冲液（pH 3.0）、乙腈和甲醇按80:15:05（v/v/v）的比例混合而成，流动相B分别由含0.2% 1-辛烷磺酸钠盐的0.01 M KH2PO4缓冲液（pH 3.0）、乙腈和甲醇按20:70:10（v/v/v）的比例混合而成。流速为0.8 mL min(-1)。柱温箱温度设定为40°C，检测波长设定为240 nm。丙酸氯倍他索与所有杂质之间的分离度对于所有化合物对均>2.0。该药品经过了国际协调会议（ICH）规定的水解、氧化、光解和热应激条件处理。该方法按照ICH指南在特异性、线性、检测限、定量限、准确度、精密度、稳健性和耐用性方面进行了验证。
