【作者】 程明；

【导师】 张凤宝；

【作者基本信息】 天津大学 ， 化学工程， 2006， 硕士

【摘要】 色谱过程动力学是研究物质在色谱过程中运动规律的科学。其主要研究目的是解释色谱流出曲线的形状,探究影响色谱区域宽度扩张的因素和机理,从而为获得高效色谱柱系统和选择色谱分离条件提供理论指导。色谱分离过程的动力学研究是通过建立合适的色谱模型来对某一分离单元的分离过程进行模拟,通过优化模型参数达到理论值与实验值的最佳拟合,有助于研究色谱分离过程中的质量传递动力学和吸附过程。本文首先介绍了手性物质的拆分原理和方法,对高效液相色谱手性固定相的研究进行了概括性总结,并介绍了近年来常用色谱模型的分类、发展和研究应用,以及各种模型的优缺点。采用羰基咪唑活化法制备牛血清白蛋白手性固定相,以磷酸盐缓冲溶液为流动相,对色氨酸对映体具有很好的拆分效果,并且具有很好的稳定性。通过研究浓度对结合常数的影响确定了色氨酸对映体与牛血清白蛋白固定相的结合机理,方便了模型的选择。分别采用前沿分析法和逆向法确定色氨酸对映体的竞争型吸附等温线。根据结合机理和拟合结果,发现竞争型双朗格缪尔吸附等温模型和平衡扩散模型可以较好的描述该吸附过程,并通过对不同浓度下对映体混合物色谱分离峰形的拟合得到了相应的模型参数。实验结果表明:采用前沿分析法和逆向法确定的吸附等温线与吸附数据吻合很好,验证了所选模型的合理性。更多还原

【Abstract】 The study of adsorption behavior and mass transfer kinetics is the theoretical basis for developing high performance chromatography techniques. This method of simulation requires the prior determination of the proper column model. Therefore, the foundation of chromatography model is much helpful.In this study, we introduced the method and mechanism of chiral separation, summarized the chiral ststionary phase for HPLC, and presented theory research about the chromatography models of kinetic study in recent years.There was a good chiral separation effect for the enantiomers of tryptophan in which the stationary phase was silica-immobilized bovine serum albumin (BSA) prepared by CDI method and the mobile phase was a phosphate buffer. The stationary phase also had a good stability. The interaction mechanism was determined by researching on the influence of concentration on the retention factor, which was very convenient for model selection.Competitive adsorption isotherm data for the two enantiomers of tryptophan were measured by frontal analysis and inverse method. The competitive Bilangmuir isotherm model and equilibrium-dispersive model were selected by comparison of the experimental results and the interaction mechanism. The corresponding parameters were gained by simulating the chromatogram of racemic mixture at different concentration. The results showed a good agreement between the isotherm determined by frontal analysis and inverse method, and the adsorption data which confirmed the validation of the model selected.更多还原