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间歇进样技术作为在液液色谱中获得高浓度洗脱带的工具:周期性和半连续分离过程的理论研究。

Intermittent sample loading technique as a tool for obtaining high- concentration elution bands in recycling liquid-liquid chromatography: Theoretical study of periodic and semi-continuous separation processes.

机构信息

Kurnakov Institute of General & Inorganic Chemistry, Russian Academy of Sciences, Leninsky Prospekt 31, Moscow 119991, Russia.

Kurnakov Institute of General & Inorganic Chemistry, Russian Academy of Sciences, Leninsky Prospekt 31, Moscow 119991, Russia.

出版信息

J Chromatogr A. 2022 Aug 2;1676:463263. doi: 10.1016/j.chroma.2022.463263. Epub 2022 Jun 18.

DOI:10.1016/j.chroma.2022.463263
PMID:35752152
Abstract

To improve the efficiency of countercurrent chromatography (CCC) separations, we have previously proposed a new sample loading method called intermittent sample loading (ISL), in which continuous sample feed alternates with short periods of "clean" mobile phase feed to the CCC device. In semi-continuous separation processes, during sample feed periods, the sample is loaded in separate batches, each consisting of a series of intermittent sample loads. It was shown that the application of the intermittent sample loading method in the conventional isocratic CCC separations significantly increased process productivity and the concentration of compounds in the separated fractions. In this study, to further improve the CCC separations with intermittent sample loading, we discuss the application of the ISL method in the processes of close-loop recycling counter-current chromatography (CLR CCC). The advantage of the ISL CLR CCC over the ISL CCC is higher resolution and lower solvent consumption. Equations are presented that allow the simulation of periodic and semi-continuous ISL CLR CCC separations and the selection of optimal operational conditions for these separation processes. It is shown that the use of ISL technique in CLR CCC separations makes it possible to produce fractions of compounds with a much higher concentration than when using the conventional single sample loading method.

摘要

为了提高逆流色谱(CCC)分离的效率,我们之前提出了一种新的上样方法,称为间歇上样(ISL),即在 CCC 设备中连续进料与短时间“清洁”流动相进料交替进行。在半连续分离过程中,在进料期间,样品以单独的批次进行加载,每个批次由一系列间歇式上样组成。结果表明,间歇式上样方法在传统的等度 CCC 分离中的应用显著提高了过程的生产力和分离馏分中化合物的浓度。在这项研究中,为了进一步改进间歇式上样的 CCC 分离,我们讨论了间歇式上样方法在闭环循环逆流色谱(CLR CCC)中的应用。与 ISL CCC 相比,ISL CLR CCC 的优点是分辨率更高,溶剂消耗更低。提出了一些方程,可以模拟周期性和半连续的 ISL CLR CCC 分离,并选择这些分离过程的最佳操作条件。结果表明,在 CLR CCC 分离中使用 ISL 技术可以产生比使用传统的单次上样方法更高浓度的化合物馏分。

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