Vandenheuvel F A
J Chromatogr. 1977 Mar 11;133(1):107-25. doi: 10.1016/s0021-9673(00)89210-9.
Qualitative and quantitative effects of classical reactions on steroids observed by gas-liquid chromatography (GLC) under standardized conditions, including the double internal standard technique, are reported. Simple procedures applicable to nanogram amounts of reactants are described. Reactions studied include the conversion of keto groups to hydroxyl groups by NaBH4, and the removal of the pregnane side-chain with NaBiO3. GLC chromatograms readily provide information on effects on functional groups at positions 3, 11, 17, 20, and 21 and the retention times of many steroids unavailable from commercial sources. GLC data analysis provides relationships between steroid structure and retention time from which methods for the computation of retention times and steroid identification are designed. The accuracy of these methods is demonstrated.
报告了在标准化条件下,包括双内标技术,通过气液色谱法(GLC)观察到的经典反应对甾体的定性和定量影响。描述了适用于纳克量反应物的简单程序。所研究的反应包括用硼氢化钠将酮基转化为羟基,以及用铋酸钠去除孕烷侧链。GLC色谱图很容易提供有关对3、11、17、20和21位官能团的影响以及许多市售来源无法获得的甾体保留时间的信息。GLC数据分析提供了甾体结构与保留时间之间的关系,据此设计了计算保留时间和甾体鉴定的方法。证明了这些方法的准确性。