丛粒藻烷类非烃化合物的分离、富集与气相色谱纯化、制备

摘要

气相制备色谱(pGC)作为分离、纯化高纯度单体化合物的有效手段, 被广泛应用于许多领域.国外地球化学方面已有众多关于化石燃料生物标志物的应用实例, 而国内这方面的应用相对较少.本文选取富含丛粒藻烷类生物标志物的茂名油页岩特殊样品, 尝试对非烃馏分中的目标化合物开展分离、富集和纯化、制备.在经过硅胶/氧化铝柱色谱初次分离后, 取非烃组分进行纯硅胶柱色谱二次分离, 之后再采用气相制备色谱开展精细分离和纯化, 成功制备出非烃组分中3个与丛粒藻烷相关联的目标化合物, 纯度高达95 %以上.以此为例, 介绍了气相制备色谱的使用原理和目标化合物分离、富集、纯化的经验.%Gas preparative chromatography (pGC) has found extensive application in several fields due to its high efficiency in the preparation of pure compounds; it proved to be effective for fossil fuel biomarker studies, as well. For the special oil shale extracts in the Maoming Basin, which display abundant occurrences of biomarker botryococcanes derived from the green alga Botryococcus braunii, certain target compounds that occurred in the polar fraction had to be separated and purified for structural studies. After primary separation with the conventional "SARA" method of silica gel/ aluminum oxide column chromatography and secondary separation by means of silica gel column chromatography, pGC was used to carry out the final delicate separation and preparation. In this procedure, three non-hydrocarbon target compounds were successfully extracted with high purity (>95%). Using this vivid example, the operating principle and procedure of pGC and the separation experience of target compounds are introduced in this paper.