NG L L
Merck Sharp & Dohme Research Laboratories, Division of Merck & Co., Inc., West Point, PA 19486.
J Assoc Off Anal Chem. 1987 Sep-Oct;70(5):829-33.
The determination of the steroid acetates was evaluated for ruggedness of the method by using an octyldecylsilane column, 254 nm detection, and acetonitrile-water as mobile phase. Mobile phase pH, oven temperature, and columns from various manufacturers had no dramatic effect on the chromatography. The method was then optimized for dexamethasone acetate and cortisone acetate bulk drug and dosage forms. For dexamethasone acetate, the bulk drug substance should be dried at 105 degrees C before use, and the sample should be dissolved in 50% acetonitrile-buffer pH 6 for stability. Cortisone acetate, on the other hand, was found to be nonhygroscopic and hence could be used as received. For stability, the sample should be stored in 50% acetonitrile-buffer pH 4.
使用十八烷基硅烷柱、254 nm检测波长以及乙腈 - 水作为流动相，对甾体醋酸酯的测定方法进行了耐用性评估。流动相pH值、柱温箱温度以及不同厂家的色谱柱对色谱分析均无显著影响。然后针对醋酸地塞米松和醋酸可的松原料药及剂型对该方法进行了优化。对于醋酸地塞米松，原料药在使用前应在105℃下干燥，样品应溶解于pH 6的50%乙腈 - 缓冲液中以确保稳定性。另一方面，发现醋酸可的松不吸湿，因此可直接使用。为保证稳定性，样品应储存在pH 4的50%乙腈 - 缓冲液中。
