胆汁酸。LIX。通过制备型高效液相色谱法纯化5α-脱水鲤醇。

Bile acids. LIX. Purification of 5 alpha-anhydrocyprinol by preparative high-performance liquid chromatography.

作者信息

Shaw R, Elliott W H

出版信息

J Chromatogr. 1979 Sep 21;177(2):289-95. doi: 10.1016/s0021-9673(01)96325-3.

Abstract

26,27-Oxido-5 alpha-cholestane-3 alpha,7 alpha,12 alpha-triol can be obtained in a homogeneous state in gram quantities by passing it through one PrepPak-500/Silica cartridge mounted in a Waters Assoc. preparative liquid chromatograph. The elution solvent was methanol-chloroform (1:14). The isolated material was analyzed for purity by several chromatographic means and by elemental analysis, and was finally characterized by the usual spectroscopic means. Gas-liquid chromatography of its trimethylsilyl ether indicated the formation of a tetrakis-trimethylsilyl-26-chloro derivative, in addition to the expected tris-trimethylsilylated substance. The structure of the former compound is deduced from the fragmentation and isotope abundance in its mass spectrum and from chemical principles.

摘要

26,27-氧化-5α-胆甾烷-3α,7α,12α-三醇可以通过使其通过安装在沃特斯联合公司制备型液相色谱仪中的一个PrepPak-500/硅胶柱，以克量获得均相状态。洗脱溶剂为甲醇-氯仿（1:14）。通过几种色谱方法和元素分析对分离得到的物质进行纯度分析，最后通过常用的光谱方法进行表征。其三甲硅烷基醚的气液色谱表明，除了预期的三甲基硅烷基化物质外，还形成了一种四（三甲基硅烷基）-26-氯衍生物。根据其质谱中的碎片和同位素丰度以及化学原理推断出前一种化合物的结构。