Process for preparing chicoric acid from echinacea purpurea

A technology of cichoric acid and echinacea, applied in the separation/purification of carboxylate, organic chemistry, etc., can solve the problems of high cost, high price, unsuitable for large-scale production, etc. Effect

Inactive Publication Date: 2005-03-02
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses expensive preparative liquid chromatography and expensive chromatographic reagents, the cost is very high, only a small amount of chicory acid standard can be prepared, and it is not suitable for large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Organic solvent extraction

[0038] 50kg of Echinacea purpurea root powder (cichoric acid content 1.1%), add 300L of 40% ethanol solution, reflux extraction at 90 ° C, the number of extractions is 3 times, each 2 hours, filter, merge the filtrate, obtain 850L of ethanol aqueous solution of cichoric acid, Recover ethanol, obtain 120L cichoric acid aqueous solution through concentration.

[0039] (2) Acidification

[0040] The aqueous solution of cichoric acid obtained above was adjusted to pH 3 with HCl having a normality of 6N. The acidified solution was centrifuged to obtain 115 L of clear liquid, and the precipitate was collected.

[0041] (3) Solvent extraction

[0042]Add the same volume of ethyl acetate to 115 L of clear liquid for extraction, extract three times, each time for 2 hours, and combine the extracts to obtain ethyl acetate extract. Add 20 L of ethyl acetate to the precipitate and stir for extraction, extract twice to obtain ethyl acetate extract...

Embodiment 2

[0048] (1) Organic solvent extraction

[0049] 50kg Echinacea purpurea root powder (cichoric acid content 1.1%), add 50% ethanol solution of 200L, reflux extraction at 70 DEG C, the number of times of extraction is 3 times, each 2 hours, filter, merge filtrate, obtain the ethanol aqueous solution 560L of cichoric acid, Concentrate and recover ethanol, and obtain 105L cichoric acid aqueous solution through concentration.

[0050] (2) Acidification

[0051] The aqueous solution of cichoric acid obtained above, with the H of normality 6N 2 SO 4 Adjust the pH to 1. The acidified solution was centrifuged to obtain 98 L of clear liquid, and the precipitate was collected.

[0052] (3) Solvent extraction

[0053] Add the same volume of ethyl acetate to 98 L of clear liquid for extraction, extract three times, each time for 2 hours, and combine the extracts to obtain ethyl acetate extract. Add 20 L of ethyl acetate to the precipitate and stir for extraction, extract twice to obta...

Embodiment 3

[0059] (1) Organic solvent extraction

[0060] 50kg of Echinacea purpurea root powder (cichoric acid content 1.1%), add 500L of 30% ethanol solution, reflux extraction at 70 ° C, the number of extractions is 3 times, each 2 hours, filter, and merge the filtrate to obtain 1460L of ethanol aqueous solution of cichoric acid, Concentrate and recover ethanol, and obtain 220L cichoric acid aqueous solution through concentration.

[0061] (2) Acidification

[0062] The aqueous solution of cichoric acid obtained above was treated with 6N H 2 SO 4 Adjust the pH to 2. The acidified solution was centrifuged to obtain 208 L of clear liquid, and the precipitate was collected.

[0063] (3) Solvent extraction

[0064] Add the same volume of ethyl acetate to 208 L of supernatant to extract three times for 2 hours each time, and combine the extracts to obtain ethyl acetate extract. Add 20 L of ethyl acetate to the precipitate and stir for extraction, extract twice to obtain ethyl acetate...

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Abstract

The process of preparing chicoric acid from echinacea purpurea includes organic solvent extraction, acidification, solvent extraction, resin separation, crystal in solvent and other technological steps. During organic solvent extraction, water solution of ethanol of 30-50 wt% concentration and in the amount of 4-10 times echinacea purpurea weight is used as the organic solvent to prepare water solution of chicoric acid at the temperature of 70-90 deg.c. During the acidification of water solution of chicoric acid, the pH value of the water solution of chicoric acid is regulated with acid solution to not greater than 3. The separation and purification process includes separation with macroporous resin, washing with deionized water, elution with ethanol aqua, concentration to obtain coarse chicoric acid product, dissolving the coarse chicoric acid product in water, pH regulation of the chicoric acid aqua to 1-3 and cooling to crystallize and to obtain chicoric acid product with purity over 96 %.

Description

technical field [0001] The present invention relates to a method for preparing cichoric acid from Echinacea purpurea. It is a method for preparing high-purity cichoric acid by using Echinacea purpurea as a raw material through processes such as organic solvent extraction, acidification, solvent extraction, resin separation, and solvent crystallization. Background technique [0002] Echinacea purpurea (Echinacea purpurea) is an immunostimulant and immunomodulator that is widely valued in the world at present, and its extract and preparation have attracted great attention at home and abroad. At present, Echinacea has been successfully introduced in my country. Chichoric acid is a derivative of caffeic acid, which is one of the most important immune active ingredients in Echinacea purpurea. It has physiological functions such as improving immunity, inhibiting HIV virus, and antiviral. [0003] Currently, only the crude extract of Echinacea purpurea, which is used as a raw mat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/48C07C69/732
Inventor 袁其朋吴启林
Owner BEIJING UNIV OF CHEM TECH
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