A method for purifying substances using a chromatographic column

一种层析柱、化合物的技术，应用在化学仪器和方法、有机化学、糖衍生物等方向，能够解决废混合溶剂不易处理、溶剂使用量大、纯化效率不高等问题，达到回用准确又、回用方便简单、减少开支的效果

Active Publication Date: 2014-10-08
SHENGQUAN HEALTANG CO LTD
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Problems solved by technology

[0006] In order to solve the problems of large amount of solvent used in the above chromatographic column purification material, low purification efficiency, and difficult disposal of waste mixed solvents produced, the present invention provides a Method for Purifying Substances Using Chromatography Column Using Density of Mixed Solvent as Control Index

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  • A method for purifying substances using a chromatographic column
  • A method for purifying substances using a chromatographic column

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Embodiment 1

[0042] Take 200g of the final crude product of fucoside, and measure its purity to be 40%, carry out chromatographic column purification, and change the polarity by changing the density of the eluent for elution.

[0043] (1) Initially use an eluent with a density of 0.65 to remove the top impurity 1 ( figure 1 The impurity point 1) in the impurity point 1), the obtained impurity 1 has a mass of 22g;

[0044] (2) Then slightly increase the polarity of the eluent, and the size of the gradient increases. The density increases slowly from 0.65-0.678, increasing the polarity by 0.002 each time. Adjust the TLC point of the column effluent after changing the density each time. Board conditions to determine. If the spot on the TLC plate does not change after adjusting the polarity, increase the density again; if the TLC spot plate changes after adjusting the density, then use the eluent of this density to pass through the column, and each time the polarity changes It is determined...

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Abstract

The invention relates to the technical field of purifying substances by using a chromatographic column, in particular to a method for purifying substances by using a chromatographic column, in which an eluent is eluted according to a density gradient. The crude product of fucoside compound was eluted with isohexane with a density of 0.65, and the impurity 1 was washed away; the density of the eluate was increased from 0.65, and the density was adjusted according to the condition of the TLC spot plate, and the density was increased by 0.002 each time, and the impurity point 2 was obtained by Change from small to large, and then from large to disappear, change the density of the eluent to 0.678, adjust the density according to the TLC spot, increase 0.002 each time, until the product point changes from small to large to disappear, and end the elution. The density gradient of the eluent used in the process of passing through the column is very small, more accurate, and the pure product can be obtained by passing through the column once; it is convenient to prepare the eluent; It is accurate, convenient and simple to use; by using the recovered eluent, an expense is also reduced.

Description

technical field [0001] The invention relates to the technical field of purifying substances by using chromatographic columns, in particular to a method for purifying substances by using chromatographic columns. Background technique [0002] Principle of column chromatography: The separation principle of column chromatography is to separate components according to the different adsorption forces of substances on silica gel. Generally, substances with higher polarity are easily adsorbed by silica gel, and substances with weaker polarity are not easily adsorbed by silica gel. When solvent elution is used, a series of processes of adsorption → desorption → re-adsorption → re-desorption occur. The components with strong adsorption force have a small moving distance and come out of the column; the components with weak adsorption force have a moving distance Big, first out of the column. [0003] Silica gel column chromatography mobile phase: use ethyl acetate:petroleum ether s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H1/06C07H15/18
Inventor 江成真张文岺刘顶王武宝
Owner SHENGQUAN HEALTANG CO LTD
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