Roos R W
J Chromatogr Sci. 1976 Nov;14(11):505-12. doi: 10.1093/chromsci/14.11.505.
A high-pressure, normal-phase partition chromatographic method for the identification and determination of conjugated and esterified estrogens in pharmaceutical tablet dosage forms is described. The method is based on the separation of the estrogen sulfate esters on a conventional diatomaceous earth-H20 column, followed by HCI-methanol hydrolysis, and finally a chromatographic separation on a chemically bonded ether (ETH-Permaphase) column and measurement. Mobile phases found useful were combinations of 2-propanol and n-heptane. Equillin and -dehydroestrone, a structurally related isomer, not separately determined in the proposed method, are determined as a sum by performing a chromatographic study of their corresponding 2, 4-dinitrophenylhydrazine derivatives. Studies have indicated several estrogen derivatives can be rapidly formed and then separated on the same column, providing a useful qualitative analysis scheme. Commercial tablet dosage forms were analyzed for conjugated and esterified estrogens and the results are presented.
描述了一种用于鉴定和测定药物片剂剂型中共轭雌激素和酯化雌激素的高压正相分配色谱法。该方法基于在常规硅藻土 - 水柱上分离硫酸雌激素酯，随后进行盐酸 - 甲醇水解，最后在化学键合醚（ETH - Permaphase）柱上进行色谱分离并测定。发现有用的流动相是2 - 丙醇和正庚烷的组合。在该方法中未单独测定的马萘雌酮和结构相关的异构体脱氢雌酮，通过对其相应的2,4 - 二硝基苯肼衍生物进行色谱研究，以总量形式测定。研究表明，几种雌激素衍生物可以快速形成，然后在同一柱上分离，提供了一种有用的定性分析方案。对市售片剂剂型中的共轭雌激素和酯化雌激素进行了分析，并给出了结果。
