【作者】 韩晶；

【导师】 王东援；

【作者基本信息】 沈阳药科大学 ， 药物分析， 2003， 硕士

【摘要】 经典薄层色谱法是一种以毛细作用力为主要推动力的色谱法。这种输液方式使它很难像柱色谱那样采用在线检测的方式。本工作最初针对这一弱点，以实现薄层色谱在线检测为目标，展开了全面研究。 首先从下行展开着手，希望在重力的作用下实现在线检测的目标。设计并实现了一种全新的下行展开输液方式。这种输液方式依靠盖板式输液分配器使流动相直接与硅胶层接触，改变了传统的依靠滤纸导引流动相的方式。工作中设计出了多种毛细引流装置以图实现在线检测，皆不理想。最终研究结果表明，在下行展开过程中流动相的主要输送力仍是毛细作用力，重力作用不占主导，因而在不依靠其他外力情况下，薄层色谱很难实现在线检测。然而在探索中，在线分离洗脱的方法被成功的发展出来。该法借助一种简单而有效的收集器在负压作用下可以进行在线分离洗脱。在此基础上，又实现了水平在线分离洗脱和原位洗脱两种方式。 这几种洗脱方式的效率很高，改变了传统的将载有样品的硅胶层刮下再洗脱的复杂操作，并被首先应用于中药纯品制备中，实现了对已分离薄层板的及时处理。实验中我们从大黄药材中分离提取出了大黄酚，大黄素甲醚和大黄素。对比了此法制备的产品与用硅胶柱层析法制备的产品的纯度。检测结果表明：原位洗脱法所得的重结晶产品纯度较高。 在线分离洗脱及原位洗脱方法较高的洗脱效率，使它成为薄层定量的一种可靠方法。本工作用这种方法对中药决明子中三种主要成分的含沈阳药科大学硕土学位论文 摘要量进行了测定，为薄层色谱分析处理中药提供了又一选择。 磷脂的分析是一个难点，该物质对高效液相色谱柱损害极大，而薄层扫描法的结果又不稳定。本工作使用原位洗脱和钥蓝法对蛋黄磷脂中 磷脂酚胆碱的含量进行了测定，结果满意。 通过对薄层色谱展开方法及洗脱方式的系统研究，澄清了一些误解和幻想，对薄层色谱的展开机理有了更深的认识。由此发展出来的在线 分离洗脱方式和原位洗脱方式为色谱工作提供了新的选择。更多还原

【Abstract】 Capillary force is the mainly driving force of the thin-layer chromatography (TLC). For this reason, the on-line detection that used in the column chromatography is difficultly realized in the classical TLC. In view of this weakness, we started our work to solve this problem.The descending development was studied firstly. We hoped to reach the aim with the help of the gravity. A new solvent-delivering model of descending development was developed. That changed the conventional fashion delivering the solvent by using filter paper. Many capillary-drafting instrument were designed in order to realize on-line detection, but they all cannot meet the need. The results of the experiments showed that the capillary force but not the gravity mainly delivers the solvent. So, without other outer force, it is difficult to reach the aim of on-line detection. However, with the help of a simple and effective collector and a negative pressure system, the method of separation coupling elution was developed successfully. Based on this principle, separation coupling elution in horizontal development and in-situ elution was developed.ABSTRACTThe efficient of these elution models is high. That reduces the complex operation procedure of scraping the spots off the silica layer. This method was applied in the preparation of pure substances of traditional Chinese medicine. Three kind of anthraquinone were separated and got from rhubarb. The purities of these three substances were better than those that were got by column chromatography.The high elution efficient of separation coupling elution and in-situ elution makes them reliable operation. The content of three anthraquinone in cassia were measured by these methods. That provides chromatographer with a new selection to analysis and deal with traditional Chinese medicine.The analysis of phosphalipids is a difficult problem, for it is harmful to the column of high performance liquid chromatography (HPLC), and the result that got by the TLC scanner were always instable. The in-situ elution and molybdenum blue reaction was used to measure the content of the phosphacholine (PC) in the egg yolk phosphalipids. The result is satisfied.Studied the methods of separation and elution systematically, a few of misunderstandings and fantasy were cleared up. The theory of the separation of the TLC was deeply recognized. The method that on-line elution in descending and horizontal development and the in-situ elution provide many new operations for the chromatographer.更多还原