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Method for purifying chicoric acid and monocaffeyltartaric acid from echinacea purpurea extract

A technology of caffeoyl tartaric acid and Echinacea purpurea extract, which is applied in the separation/purification of carboxylic acid esters, organic chemistry, pharmaceutical formulations, etc., to achieve the effects of easy handling, low elution cost, and production cost savings

Inactive Publication Date: 2009-02-18
HUNAN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, there is no process for simultaneously extracting and purifying cichoric acid and monocaffeoyl tartaric acid from Echinacea purpurea

Method used

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  • Method for purifying chicoric acid and monocaffeyltartaric acid from echinacea purpurea extract
  • Method for purifying chicoric acid and monocaffeyltartaric acid from echinacea purpurea extract
  • Method for purifying chicoric acid and monocaffeyltartaric acid from echinacea purpurea extract

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Separation and purification:

[0026] (1) Processing of sample solution: Take 3.755g of 4% Echinacea purpurea extract, add 18mL of water, dissolve it by ultrasonic extraction for 30min, filter under reduced pressure, wash the filter residue with 4mL of water, combine the filtrate, add 1mL of 18% hydrochloric acid, Make the pH between 1-4; that is, the sample solution.

[0027] (2) Configuration of different gradient eluents: configure three different gradient eluents with hydrochloric acid, the volume fraction of hydrochloric acid is respectively: A eluent=0.07%; B eluent=0.03%; C eluent= 0.015%.

[0028] (3) Column loading: wet-load the processed hpd100 non-polar macroporous adsorption resin into a 50cm×1.0cm glass chromatography column, and the volume of the macroporous adsorption resin is 35cm 3 , equilibrate the macroporous adsorption resin with 5 times column volume (BV) of A eluent, and then add the sample solution to the chromatography column every 1BV / 2-3 ...

Embodiment 2

[0038] (1) Separation and purification:

[0039] (1) Treatment of sample solution: Take 2000g of 4% Echinacea purpurea extract, add 5200mL of water, stir to dissolve it, filter under reduced pressure, wash the filter residue with 400mL of water, combine the filtrates, add 50% of hydrochloric acid 500mL, and obtain the above sample liquid.

[0040] (2) Configuration of different gradient eluents: configure three kinds of eluents with different gradients with sulfuric acid, the volume fraction of sulfuric acid is respectively: A eluent=0.05%; B eluent=0.03%; C eluent= 0.01%.

[0041] (3) Column loading: wet-load the treated macroporous adsorption resin into a glass chromatography column (100cm×8.0cm), the volume of the macroporous adsorption resin is 13500cm 3 , equilibrate the macroporous adsorption resin with 5 times the column volume (BV) A eluent, and then add the sample solution to the chromatography column at a speed of 3-10 minutes per 1 BV.

[0042] (4) Use A, B, and ...

Embodiment 3

[0049] (1) Separation and purification:

[0050] (1) Treatment of sample solution: Take 3000g of 4% Echinacea purpurea extract, add 8000mL of water, stir to dissolve it, filter under reduced pressure, wash the filter residue with 450mL of water, combine the filtrates, add 500% of hydrochloric acid 500mL, and obtain the above sample liquid.

[0051] (2) Configuration of different gradient eluents: configure three different gradient eluents with acetic acid, the volume fraction of acetic acid is respectively: A eluent=0.1%; B eluent=0.04%; C eluent=0.04%; 0.02%.

[0052] (3) Column loading: wet-load the treated macroporous adsorption resin into a glass chromatography column (100cm×8.0cm), the volume of the macroporous adsorption resin is 1350cm 3 , equilibrate the macroporous adsorption resin with 5 times the column volume (BV) A eluent, and then add the sample solution to the chromatography column at a speed of 3-10 minutes per 1 BV.

[0053] (4) Use A, B, and C three eluent...

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Abstract

The present invention discloses a method of purifying chicoric acid and caftaric acid from Echinacea purpurea extract. 3 to 5 percent of the Echinacea purpurea extract on the market is used as raw material; the raw material is dissolved in water according to the weight ratio of 1 to from 2 to 5 between the raw material and the water; the solution is filtered; acid is added into the solution; the pH of the solution is adjusted to be between 1 and 4; the sample solution is added into a chromatography column with non-polar macroporous adsorption resin; eluent of three different gradients are used for eluting in sequence; eluent in the 6th to 45th column is collected to acquire the caftaric acid; eluent in the 60th to 100th column is collected to prepare the chicoric acid; acid is added into the eluent; the volume percent of the acid is adjusted to be 0.05 to 1.0 percent; ethyl alcohol of 95 percent is used for desorption; after being decompressed and dried, the caftaric acid with the purity higher than 70 percent and the chicoric acid with the content higher than 75 percent can be prepared; and ultimately the caftaric acid and the chicoric acid with the purity higher than 95 percent can be prepared through recrystallization. The present invention has the advantages that the method is simple and rapid, the cost of the eluent is low, and the industrial production can be realized.

Description

technical field [0001] The invention relates to a method for purifying cichoric acid and monocaffeoyl tartaric acid from echinacea purpurea extract. Specifically, it is a method for simultaneously or individually purifying monocaffeoyl tartaric acid and cichoric acid by gradient elution of acid solutions with different concentrations. Background technique [0002] The main components of Echinacea purpurea include cichoric acid and monocaffeoyl tartaric acid. According to research, cichoric acid has immune regulation function, anti-inflammatory effect, and can inhibit hyaluronidase, anti-virus, and also inhibit HIV-1 and HIV-1 integrase effect. Therefore, it has become an immune enhancer and immune regulator that has received widespread attention in the world. At present, Echinacea purpurea extracts are available, but the content of cichoric acid is relatively low, generally only about 4%, which limits the further development and utilization of cichoric acid. Nigel B. Perr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/732C07C67/48A61K36/28
Inventor 陈波郭建伟谢继国
Owner HUNAN NORMAL UNIVERSITY
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