Laboratory for Plant and Process Design, Department of Biochemical and Chemical Engineering, Technische Universität Dortmund, D-44221 Dortmund, Germany.
J Chromatogr A. 2013 Jan 25;1274:54-64. doi: 10.1016/j.chroma.2012.11.031. Epub 2012 Dec 12.
The selection of solvent systems in centrifugal partition chromatography (CPC) is the most critical point in setting up a separation. Therefore, lots of research was done on the topic in the last decades. But the selection of suitable operating parameters (mobile phase flow rate, rotational speed and mode of operation) with respect to hydrodynamics and pressure drop limit in CPC is still mainly driven by experience of the chromatographer. In this work we used hydrodynamic analysis for the prediction of most suitable operating parameters. After selection of different solvent systems with respect to partition coefficients for the target compound the hydrodynamics were visualized. Based on flow pattern and retention the operating parameters were selected for the purification runs of nybomycin derivatives that were carried out with a 200 ml FCPC(®) rotor. The results have proven that the selection of optimized operating parameters by analysis of hydrodynamics only is possible. As the hydrodynamics are predictable by the physical properties of the solvent system the optimized operating parameters can be estimated, too. Additionally, we found that dispersion and especially retention are improved if the less viscous phase is mobile.
在离心分配色谱(CPC)中,溶剂系统的选择是分离的最关键步骤。因此,在过去几十年中,人们对此进行了大量的研究。但是,对于与流体动力学和压力降限制有关的合适操作参数(流动相流速、转速和操作模式)的选择,主要还是依赖于色谱学家的经验。在这项工作中,我们使用流体动力学分析来预测最合适的操作参数。在选择了不同的溶剂系统以获得目标化合物的分配系数之后,我们对流体动力学进行了可视化。基于流动模式和保留时间,我们为用 200mlFCPC(®)转子进行的 nybomycin 衍生物的纯化运行选择了操作参数。结果证明,仅通过流体动力学分析选择优化的操作参数是可行的。由于溶剂系统的物理性质可以预测流体动力学,因此也可以估算优化的操作参数。此外,我们还发现,如果流动性较弱的相为流动相,则可以改善分散性,特别是保留时间。