国产醋酸甲地孕酮的质量研究:6-羟基-6-甲基-17α-乙酰氧基黄体酮差向异构体的分离与鉴定

用柱层析及薄层层析对国产醋酸甲地孕酮的杂质进行了分析,共分离出7个杂质点:Ⅰ₁,Ⅰ₂,Ⅰ₃,Ⅰ₄,Ⅰ₅,Ⅰ₆,Ⅰ₇,并对其中Ⅰ₃和Ⅰ₄进行分离纯制及光谱分析,确定其结构为6β-羟基-6α-甲基-17α-乙酰氧基黄体酮及其差向异构体6α-羟基-6β-甲基-17α-乙酰氧基黄体酮。本文报道了薄层层析条件(硅胶GF₂₅₄,展开剂:醋酸乙酯-甲苯=7:3)以及光谱鉴别的依据。

Studies on the purity of Chinese megestrol acetate: separation and identification of epimeric isomers of 6-hydroxy-6-methyl-17 alpha-acetoxy-progesterone

Two impurities are separated from Chinese megestrol acetate by column chromatography and thin-layer chromatography. On the basis of UV, IR, ¹HNMR, ¹³CNMR spectroscopy and EI mass spectrometry, these two impurities were identified as 6α-hydroxy-6β-methyl-17α-acetoxy-progesterone and its epimeric isomer 6β-hydroxy-6α-methyl-17α-acetoxy-progesterone. we report here the optimal TLC conditions (silica GF₂₅₄, ethyl acetate—toluene=7:3) and the spectral data.