甾体药物安宫黄体酮中杂质的分离和鉴定

Isolation and identification of impurity in steroid drug Megestrol acetate

应用柱色谱方法对安宫黄体酮多次重结晶母液中所含的杂质进行了分离和纯化,并应用NMR和MS等波谱方法确定了5个孕甾烷型杂质的结构:17α-氧乙酰基-6α-甲基孕甾-3,20-二酮、17α-氧乙酰基孕甾4-烯-3,20-二酮、17α-氧乙酰基孕甾4-烯-20-酮、17α-氧乙酰基-6β-羟基-6α-甲基孕甾4-烯-3, 20-二酮、17α-氧乙酰基-6α-羟基-6β-甲基孕甾4-烯-3,20-二酮.为安宫黄体酮的质量控制及代谢研究提供了依据.

The impurity in the drug megestrol acetate was purified by chromatography methods and five known compounds 17α-acetoxy-6α-methylpregnan-3, 30-dione, 17α-acetoxypregn-4-en-3, 20-dione, 17α- acetoxypregn-4-en-20-one, 17α-acetoxy-6β-hydroxyl-6α-methylpregn-4-en-3, 20-dione, 17α-acetoxy-6α-hydro- xyl-6β-methylpregn-4-en-3, 20-dione determined by NMR and MS spectral analyses, were isolated from the mother liquid of the drug. Current study revealed the structures of all the impurities at a level of 0.1%, to provide evidences for the quality control of production and reference for the drug metabolism of of Megestrol acetate.