胆甾型冠醚液晶固定相分离丁醇碳链异构体的GC研究

The Separation of Carbon Chain Isomers of Butanols with CH-B-15-C-5 as Stationary Phase,

以４’－胆甾烯氧羰基苯并－１５－冠－５（ＣＨ－Ｂ－１５－Ｃ－５）涂渍于硅烷化１０２白色担体上作为一种新型的ＧＣ固定相，对几种丁醇碳链异构体的气固色谱（ＧＳＣ）、普通气液色谱（ＧＬＣ）和冠醚液晶气液色谱（ＣＬ－ＧＬＣ）的分离效果进行了比较研究，并探讨了分离机理。经对ＣＨ－Ｂ－１５－Ｃ－５柱的麦克雷诺相常数的测定可知，该柱的极性中等偏弱。在ＣＬ－ＧＬＣ体系中，ＣＨ－Ｂ－１５－Ｃ－５是排列有序的冠醚液晶状态，因此在相同条件下，ＣＬ－ＧＬＣ的分离度高于ＧＬＣ的分离度，所得色谱峰形亦很好。我们认为体系中固定相分子是否排列有序对有机化合物的保留行为具有重要作用。实验表明，在柱温为７０－１５０℃的范围内，对丁醇碳链异构体的分离均能获得满意效果。如果采用ＣＬ－ＧＬＣ法分离较高沸点的有机化合物，则柱温度还可升高。一般认为ＧＳＣ的分离属吸附机理，用吸附等温线来描述固定相表面的吸附状况，ＧＳＣ的吸附等温线往往是非线性关系，故常得到非对称峰。该柱所得ＧＳＣ图均为对称色谱峰，这一实验结果提示人们，在ＧＳＣ的分离机制中，除吸附机理之外还应考虑其它因素。我们认为ＣＨ－Ｂ－１５－Ｃ－５经高温处理后在１２５℃以下为排列整齐有序的固态晶体，是?

A comparison study was made on the separation of carbon chain isomers of butanols with CH-B-15-C-5 as stationary phase in GSC, GLC and CL-GLC. The results of separation and the chromatographic characteristics of CH-B-15-C-5 are discussed. By determining the Mcreyoids phase constants, the polarity of the CH-B-15-C-5 column was known to be moderate to weak. In the CL-GLC system, CH-B-15-C-5 occurred as orderly arranged ether liquid crystals, and therefore, under similar experimental conditions, the resolution of the CL-GLC was higher than that of the GLC, with the chromatographic peaks of the former also better defined. We presume that whether or not the stationary phase molecules are in ordered arrangement in the system has great impact on the retention behavior of organic compounds.