米非司酮母液中杂质的分离和结构鉴定

Isolation and structure identification of impurities from mother liquid of mifepristone

目的:研究药物米非司酮中的杂质。方法:运用硅胶柱层析和半制备高效液相进行分离和纯化,其结构通过NMR和HREIMS等技术进行鉴定。结果:从母液中分离得到3个化合物,其结构分别鉴定为17β-羟基-17α-(1-丙炔基)-雌甾-5,9-二烯-3-酮环缩乙二醇(Ⅰ),11-[4-(二甲基氨基)苯基]-17β-羟基-17α-(1-丙炔基)-雌甾-5,9-二烯-3-酮环缩乙二醇(Ⅱ),11-[4-(二甲基氨基)苯基]-17β-羟基-17α-(1-丙炔基)-雌甾-4,10,11-三烯-3-酮(Ⅲ)。结论 :3个杂质均为首次从药物米非司酮中确定,其中Ⅱ为新化合物。

OBJECTIVE To investigate impurities in mifepristone.METHODS Three compounds were isolated form mother liquid of mifepristone by silica gel column chromatography and semi-preparative HPLC.RESULTS Structures of these compounds were identified as 17α-hydroxy-17β-（1-propynyl）-3,3-ethylendioxy-estra-5,9-diene（Ⅰ）,11-[4-（dimethylamino）phenyl]-17β-hydroxy-17α-（1-propynyl）-3,3-ethylendioxy estra-5,9-diene（Ⅱ）,11-[4-（dimethylamino）phenyl]-17β-hydroxy-17α-（1-propynyl）-estra-4,9,11-trien-3-one（Ⅲ）by NMR and HREIMS data.CONCLUSION Three isolated compounds are isolated and identified from mifepristone for the first time.Compound Ⅱis a new compound.