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Countercurrent chromatographic separation process for reducing fixed phase

A technology of countercurrent chromatography and separation method, applied in material separation, analysis materials, measuring devices, etc., can solve the problems of low single-hour output of active ingredient monomers, low separation efficiency, long peak time, etc., to improve the single-hour output , high production efficiency, the effect of improving peak shape

Inactive Publication Date: 2005-07-13
TEA RES INST CHINESE ACAD OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to ensure good separation efficiency, there are often many active components whose distribution coefficients in the stationary phase and mobile phase are greater than or even much greater than 1, resulting in a long time for some active component monomers to elute, and the broadening of these peaks is serious
[0003] Publication No. 1301698A Chinese patent application discloses a method for separating catechin monomers from tea extracts. The stationary phase and mobile phase used are also the upper and lower phases formed after mixing various solvents. The above-mentioned separation method is applied in industrialized production. Due to the low separation efficiency, the single-hour yield of the active ingredient monomer in the plant extract is low, and the production efficiency is low.

Method used

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  • Countercurrent chromatographic separation process for reducing fixed phase
  • Countercurrent chromatographic separation process for reducing fixed phase
  • Countercurrent chromatographic separation process for reducing fixed phase

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1 The present invention is used to separate active ingredients in tea polyphenols

[0021] The countercurrent chromatograph is a domestic GS-10A type, and the composition of tea polyphenols is: epigallocatechin gallate (EGCG) accounts for 26.16%, epicatechin gallate (ECG) accounts for 5.87%, gallocatechin Gallate (GCG) accounted for 12.13%, epicatechin (EC) accounted for 9.43%, epigallocatechin (EGC) accounted for 8.92%, and catechin (D, L-C) accounted for 2.60%. Stationary phase and mobile phase are prepared separately. The stationary phase was prepared by taking 50ml petroleum ether and 350ml ethyl acetate, and the mobile phase was 2000ml pure distilled water. After pumping the stationary phase into the countercurrent chromatographic column, weigh 0.5 g of tea polyphenols and dissolve it in 40 ml of mobile phase, turn on the countercurrent chromatograph to 800 rpm, then pump the tea polyphenol solution in at a flow rate of 2.0 ml / min, and then Use the mobile...

Embodiment 2

[0024] Embodiment 2 The present invention is used to separate the active ingredient in the Pueraria lobata extract

[0025] The countercurrent chromatograph is a domestic GS-10A type, and the composition of isoflavones in Pueraria root extract is: puerarin (Puerarin) accounts for 36.16%, daidzein (Daidzein) accounts for 3.87%, daidzin (Daidzin) accounts for 17.13%, and the composition solvent The stationary phase and mobile phase in the system are prepared separately. The preparation of the stationary phase was prepared by taking 50ml of n-butanol, 200ml of ethyl acetate and 50ml of methanol, and the mobile phase was 1200ml of pure distilled water. After the stationary phase is pumped into the countercurrent chromatographic column, take by weighing Pueraria root extract 0.5g and dissolve it in 40ml mobile phase, open the countercurrent chromatograph to 800 rpm, then pump into the Pueraria root extract solution with a flow rate of 1.5ml / min, and then Use the mobile phase inste...

Embodiment 3

[0028] Embodiment 3 The present invention is used to separate active components in tea alkaloids

[0029] The countercurrent chromatograph is a domestic GS-10A type, and the composition of the active ingredients in the tea alkaloids is: caffeine (Caffeine) accounts for 53.28%, theophylline (Theophylline) accounts for 1.47%, theobromine (Theobromine) accounts for 15.93%. The stationary phase and mobile phase are prepared separately. The preparation of the stationary phase was prepared by taking 200ml of water (with a pH range of 4.5) and 300ml of methanol, and the mobile phase was 1500ml of chloroform. After pumping the stationary phase into the countercurrent chromatographic column, weigh 0.8 g of tea alkaloids and dissolve them in 30 ml of mobile phase, turn on the countercurrent chromatograph to 800 rpm, then pump in the tea alkaloids solution at a flow rate of 1.8 ml / min, and then Use the mobile phase instead to elute the alkaloid components in the column. According to th...

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Abstract

The present invention relates to a countercurrent chromatography for the separation of active ingredients in plant extracts. The methods used at present are all uniformly mixed according to the proportion of each solvent in the solvent system, and the upper and lower phases formed after the mixing are balanced are used as the stationary phase and the mobile phase respectively, resulting in a short peak time for some active component monomers. long, and the broadening of these peaks is severe. The present invention is characterized in that the stationary phase and the mobile phase in the solvent system are prepared separately, and the stationary phase is one or several combinations of alkanes, chlorinated organic solvents, ethyl acetate, fatty alcohols, and fatty ketones, The mobile phase is one or a combination of chlorine-containing organic solvents, fatty alcohols, and water, and the stationary phase and the mobile phase are selected from different substances. The invention shortens the peak-out time of the active ingredient monomer, improves the peak shape of the active ingredient monomer, applies the invention in industrial production, improves the single-hour output of the active ingredient monomer, and has high production efficiency.

Description

technical field [0001] The present invention relates to a countercurrent chromatography for the separation of active ingredients in plant extracts. Background technique [0002] Countercurrent chromatography is a liquid-liquid distribution technique developed in the 1980s, and has been widely used in the separation of bioactive components in plants, marine organisms, and microbial fermentation products. At present, the method adopted by countercurrent chromatography to separate plant extracts is to mix evenly according to the proportion of each solvent in the solvent system, and the upper and lower phases formed after the mixing balance are used as the stationary phase and the mobile phase respectively. Because the solvent system in this method has been fully distributed and balanced in the separation container before entering the countercurrent chromatograph, the stationary phase and mobile phase formed after separation will not dissolve each other when they are remixed in ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/42G01N30/74
Inventor 江和源
Owner TEA RES INST CHINESE ACAD OF AGRI SCI
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