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Method for extracting glycyrrhizicacid, licorice flavone and licorice polysaccharide

A technology of licorice flavonoids and licorice polysaccharides, which is applied in the fields of medical medicine and chemical industry, can solve the problems of waste of resources in industrialized production, inconvenience, and low yield of flavonoids, and achieve the effects of improving comprehensive utilization, simple process route, and reducing production costs

Inactive Publication Date: 2006-07-19
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Licorice flavonoids, glycyrrhizic acid and glycyrrhizic polysaccharides are the main active ingredients of licorice. The existing extraction techniques are single or intermittent. Often, glycyrrhizic acid is simply extracted through a system, and the licorice residue is discarded or extracted from the residue after extraction. Licorice flavonoids, then extracted licorice polysaccharide
Chinese patent "A kind of licorice paste and its production process" (CN1144105) discloses a method of extracting licorice flavonoids from the residue after extracting glycyrrhizic acid from licorice, but the yield of flavonoids is very low, indicating that in the extraction of glycyrrhizic acid During the process, most of the licorice flavonoids are lost
The Chinese patent "Systematic separation and extraction of licorice flavonoids, glycyrrhizic acid, and licorice polysaccharide production method from licorice" (CN1359905A) discloses a method for systematically extracting glycyrrhizic acid, licorice flavonoids, and licorice polysaccharides, but the extraction and separation steps are too many and fundamental. Unable to achieve industrial production
The prior art, including the above-mentioned technology, does not fully consider the chemical structure of each component in licorice, and adopts an unreasonable segmentation and extraction method, resulting in waste of resources or inconvenience to industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1 (cold infiltration extraction)

[0021] Soak 1 Kg of licorice powder with 20 times of 20% ethanol ammonia (0.5% ammonia concentration) at room temperature for 2 hours, then extract by percolation, the percolation speed is 10ml / min, and the percolation liquid is concentrated under reduced pressure until the specific gravity is 1.08( 20°C), stir and extract 3 times with water-saturated n-butanol in a ratio of 1:1, combine the extracts to recover n-butanol under reduced pressure, dry the crude licorice flavonoids in an oven at a temperature of 70°C, and obtain 33.5 grams of flavonoids crude product, the total flavonoid content Add 95% ethanol to the raffinate phase until the alcohol concentration is 60%, leave it at room temperature for 24 hours, vacuum filter, and dry the filter residue in an oven at a temperature of 70°C to obtain 12.1 grams of crude licorice polysaccharide, with a content of 53.0%; Concentrate the filtrate under normal pressure to a specifi...

Embodiment 2

[0022] Embodiment 2 (reflux extraction)

[0023] 1Kg licorice powder was extracted 3 times with 20% ethanol according to 1:8, 1:6 and 1:6 reflux, each time for 2 hours, filtered, combined filtrate, recovered ethanol under reduced pressure, concentrated specific gravity 1.10 (20°C), and used acetic acid The ethyl ester was stirred and extracted 3 times at a ratio of 1:1, the extracts were combined, and the ethyl acetate was recovered under reduced pressure. The crude licorice flavonoids were dried in a vacuum oven (at a temperature of 60° C.) to obtain 34.8 g of the crude licorice flavonoids, with a total flavonoid content of 48.0%. Add 95% ethanol to the raffinate phase until the alcohol concentration is 50%, let it stand at room temperature for 24 hours, centrifugally filter, and vacuum-dry the filter residue (at a temperature of 60° C.) to obtain 13.5 grams of crude licorice polysaccharide, with a content of 54.0%; the supernatant is concentrated To a specific gravity of 1.2...

Embodiment 3

[0024] Embodiment 3 (warm soaking extraction)

[0025] Take 1Kg of licorice powder, soak and stir with 8 times of 20% ethanol at 45°C for 3 hours, repeat once, filter, combine the filtrate, recover the ethanol from the filtrate under reduced pressure, concentrate to a specific gravity of 1.08 (20°C), and use chloroform to press 1: Stir and extract 3 times at a ratio of 1, combine the extracts to recover chloroform under reduced pressure, freeze-dry to obtain 32.8 grams of flavonoid crude product, and the total flavonoid content is 51.7%; add 95% ethanol to the raffinate phase until the alcohol concentration is 70%, and statically Set aside for 24 hours, centrifugally filter, and vacuum-dry the filter residue (at a temperature of 60° C.) to obtain 13.3 grams of crude licorice polysaccharide, with a content of 50.0%; Stand still, centrifuge at 3000 rpm, wash the filter residue with cold water to pH 5, and dry it in an oven (at a temperature of 70° C.) to obtain 55.8 g of crude g...

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PUM

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Abstract

The synchronous extraction and separation method for glycyrrhizic acid, glycyrrhizic flavone and glycyrrhizic polysaccharide comprises: extracting the licorice powder with solvent for 1-3 times by cold seepage, warm leaching or reflux; mixing and condensing on reduced pressure the liquid; extracting with organic solvent, condensing to recover the solvent and obtain the coarse glycyrrhizic flavone; adding 95% ethanol into the extracted residue to adjust ethanol concentration as 50-80%, holding at low or normal temperature to obtain coarse glycyrrhizic polysaccharide by drying the precipitate ; condensing the supernatant, adjusting pH value to 1.5-2.0 with H2SO4 or HCl, holding at low or normal temperature, removing the supernatant, and obtaining coarse glycyrrhizic acid by cleaning with cold water or acid and drying the precipitate. This invention has simple process, improves comprehensive utilization level, and reduces cost for deep process.

Description

technical field [0001] The invention belongs to the fields of medical medicine and chemical industry, and particularly relates to a method for synchronously extracting and separating glycyrrhizic acid, licorice flavonoids and licorice polysaccharides from natural medicines. Background technique [0002] Licorice flavonoids, glycyrrhizic acid and glycyrrhizic polysaccharides are the main active ingredients of licorice. The existing extraction techniques are single or intermittent. Often, glycyrrhizic acid is simply extracted through a system, and the licorice residue is discarded or extracted from the residue after extraction. Licorice flavonoids, and then extracted licorice polysaccharides. Chinese patent "A kind of licorice paste and its production process" (CN1144105) discloses a method of extracting licorice flavonoids from the residue after extracting glycyrrhizic acid from licorice, but the yield of flavonoids is very low, indicating that in the extraction of glycyrrhiz...

Claims

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Application Information

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IPC IPC(8): C07D311/36C07D311/40C07J63/00C08B37/00
Inventor 敖明章
Owner HUAZHONG UNIV OF SCI & TECH
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