“抗孕-53”差向异构体的键合相正相HPLC分析与熔融温度测定
BONDED NORMAL PHASE HPLC DETERMINATION OF ANORDRIN
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摘要: “抗孕-53”为应用广泛、简便而安全的探亲避孕药。本品存在二差向异构体,其生物活性差异甚大。本文以硅胶及各种键合相正相高压液相色谱法,研究了差向异构体的色谱行为,探讨了构型、分离系统及分离效果间的关系,建立了键合腈基或氨基-四氢呋喃/正己烷(3~3.5%)、UV λ225 nm检测的最佳分离和外标定量方法。还以差示扫描量热法研究了差向异构混合物组成与熔融热的相关性,为以熔融温度测定法作简易质量鉴定提供了依据。Abstract: Anordrin (2a, 17a-diethyl-A-nor-5a-androstane 2β, 17β-diol dipropionate) is one of the widely used effective oral steroidal contraceptives. It consists of two epimers with greatly different biological activity. Variation of quantity ratio between these two epimers often causes uncertainty of action. Therefore, it is necessary to develop a method for determining both epimers accurately.After careful study of the chromatographic behaviours and configurational relationship between these epimers in various chemically bonded and silica gel supports, a bonded normal phase HPLC determination method is proposed. Epimers can be separated with THF/n-hexane (3~3.5%) in cyano- or aminobonded silica gel column and detected by UV detector at 225 rim.This study also revealed a correlation of the composition of epimer mixture with its melting heat (by DSC). The result shows that measurement of melting heat can be used as a simple but effective method for monitoring the drug quality.
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