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Method for preparing glabridin

A technology of licorice and licorice, applied in the field of preparation of licorice, can solve the problems of low efficiency, long column chromatography elution period and the like, and achieves controllable process parameters, large preparation amount and short production cycle. Effect

Inactive Publication Date: 2011-11-23
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Supercritical CO 2 Extraction technology has been used in the extraction of licorice flavonoids. The difference is that the process of the present invention uses supercritical CO 2 In the purification stage, the defects of long elution period and low efficiency of column chromatography are solved

Method used

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  • Method for preparing glabridin

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Effect test

Embodiment 1

[0020] Take Glycyrrhiza glabra, take 1kg, put it into a microwave extraction tank, add 8 times the amount of 80% ethanol for microwave extraction for 60 minutes, filter the liquid, add 6 times the amount of 80% ethanol solution for microwave extraction for 30 minutes, combine the extracts twice and concentrate under reduced pressure Alcohol-free, take 1% sodium hydroxide solution to adjust the concentrated solution to be neutral, transfer it to a separatory funnel, add an equal volume of ethyl acetate to extract 3 times, and extract the extract with 5% sodium bicarbonate solution for 2 times, and concentrate the organic phase , Add 50g of polyamide and dry to obtain a sample. Take chloroform, methanol, and aqueous solution in a mixing ratio of 7:5:3, remove the phase as an entrainer, crush the sample and add it to the extraction kettle, adjust the parameter pressure to 12MPa, extract the temperature to 40°C, and feed liquid CO 2 Fluid, after reaching the above parameters, CO ...

Embodiment 2

[0022] Take Glycyrrhizae glabra and crush it, take 1kg, put it into a microwave extraction tank, add 6 times the amount of 70% ethanol for microwave extraction for 40 minutes, extract 3 times, combine the 2 extractions, concentrate under reduced pressure and alcohol-free, take 0.5% sodium hydroxide solution to adjust the concentrated solution Neutral, transfer to a separatory funnel, add an equal volume of ethyl acetate to extract 4 times, the extract is back extracted 3 times with 5% sodium bicarbonate solution, the organic phase is concentrated, and 80g of polyamide is added to dry to obtain a sample. Take chloroform, methanol, and aqueous solution in a mixing ratio of 8:5:3, remove the phase as an entrainer, crush the sample and add it to the extraction kettle, adjust the parameter pressure to 16MPa, extract the temperature at 30°C, and feed liquid CO 2 Fluid, after reaching the above parameters, CO 2 The flow rate was controlled at 120ml / min, the entrainer flow rate was 2m...

Embodiment 3

[0024] Take Glycyrrhizae glabra and crush it, take 5kg, put it into a microwave extraction tank, add 6 times the amount of 70% ethanol for microwave extraction for 40 minutes, extract 3 times, combine the 2 extractions, concentrate under reduced pressure and alcohol-free, take 0.2% sodium hydroxide solution to adjust the concentrated solution Neutrality, transferred to a separatory funnel, added 2 times the volume of ethyl acetate to extract 3 times, the extract was back-extracted 2 times with 5% sodium bicarbonate solution, the organic phase was concentrated, the organic phase was concentrated, and 400g of polyamide was added to dry to obtain sample. Take chloroform, methanol, and aqueous solution in a mixing ratio of 8:6:3, remove the phase as an entrainer, crush the sample and add it to the extraction kettle, adjust the parameter pressure to 14MPa, extract the temperature at 35°C, and feed liquid CO 2 Fluid, after reaching the above parameters, CO 2 The flow rate was contr...

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Abstract

The invention belongs to the field of natural product separation and in particular relates to a method for preparing glabridin. The method comprises the following steps of: A, crushing glycyrrhiza glabra serving as a raw material, performing microwave extraction by using 70 to 80 percent ethanol in an amount which is 7 to 8 times weight of the raw material, concentrating an extracting solution under reduced pressure, regulating a concentrated solution to be neutral by using a sodium hydroxide solution, extracting by using ethyl acetate, performing back extraction on extract liquor by using a 5 percent sodium hydroxide solution, concentrating an organic phase until a small volume, and adding polyamide resin for drying to obtain a sample; and B, adding the sample into a supercritical CO2 extraction kettle, introducing CO2 fluid and an entrainer, extracting for 2 to 3 hours, resolving an extract, and crystallizing by using ethanol to obtain the high-purity glabridin. The method has the advantages of simple operation, short production period, high yield and suitability for industrial production.

Description

Technical field: [0001] The invention belongs to the field of separation of natural products, in particular to a preparation method of glabridin. Background technique: [0002] Glabridin is a flavonoid substance, CAS No. 59870-68-7, melting point 156-158°C, molecular formula C 20 h 20 o 4 , molecular weight 324.3, molecular structure formula: [0003] [0004] Glabridin is a flavanone isolated from Glycyrrhiza glabra, which shows a strong anti-free radical oxidation effect in the cytochrome P450 / NADPH oxidation system, and can significantly inhibit the free radicals produced during the metabolism process in the body. Radicals, so as to prevent oxidation-sensitive biological macromolecules (low-density lipoprotein LDL, DNA) and cell walls from being oxidized and damaged by free radicals, so as to prevent certain pathological changes related to free radical oxidation, such as atherosclerosis, cell Aging, etc., in the cosmetics industry, it is called "whitening gold". I...

Claims

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Application Information

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IPC IPC(8): C07D493/04
CPCY02P20/54
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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