Novaković J, Agbaba D, Vladimirov S, Zivanov-Stakić D
Department of Pharmaceutical Chemistry, Faculty of Pharmacy, Belgrade, Yugoslavia.
J Pharm Biomed Anal. 1990;8(3):253-7. doi: 10.1016/0731-7085(90)80034-m.
A densitometric method for determination of complex mixtures of conjugated oestrogens in raw material and tablets was developed. The proposed procedure comprised hydrolysis of sodium sulphate esters of oestrone, equilin, 17 alpha-oestradiol, equilenin, 17 alpha-dihydroequilin and 17 alpha-dihydroequilenin, the chloroform extraction of free oestrogens and methyltestosterone (internal standard) and separation on TLC plates using chloroform-cyclohexane-dioxane-triethylamine (4.5:4.1:0.6, v/v) as the solvent for development. Quantitative assay was achieved by direct scanning of the oestrogen spots at 280 nm. The proposed method is simple, rapid, reproducible and adequate to control the content of conjugated oestrogens in the raw material and in pharmaceutical preparations.
开发了一种用于测定原料和片剂中结合雌激素复杂混合物的密度测定法。所提出的方法包括对雌酮、马萘雌酮、17α-雌二醇、马萘雌烯酮、17α-二氢马萘雌酮和17α-二氢马萘雌烯酮的硫酸钠盐进行水解，用氯仿萃取游离雌激素和甲基睾酮（内标），并使用氯仿-环己烷-二氧六环-三乙胺（4.5:4.1:0.6，v/v）作为展开溶剂在薄层色谱板上进行分离。通过在280nm处直接扫描雌激素斑点进行定量测定。该方法简单、快速、可重现，适用于控制原料和药物制剂中结合雌激素的含量。
