Method for extracting and purifying glabridin from glycyrrhiza glabra residues

A technology of glabridin and licorice residue, applied in the field of separation and purification, can solve problems such as cost increase, difficult industrialization, cumbersome operation steps, etc., and achieve the effects of reducing production cost, facilitating recovery and utilization, and high extraction efficiency

Active Publication Date: 2016-07-20
青海倍力甘草科技发展有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purified content ranges from 40% to 90%. The existing method is multi-step column passing and multi-step

Method used

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  • Method for extracting and purifying glabridin from glycyrrhiza glabra residues

Examples

Experimental program
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Effect test

Embodiment 1

[0023] (1) Extraction:

[0024] Add 2kg of licorice residue and 14.5kg of ethyl acetate in sequence to a 20L extraction tank; extract for 2 hours, release the extract, and extract the grass residue once more with 9kg of ethyl acetate as above, combine the filtrates twice, and distill out the ethyl acetate under reduced pressure. The concentrate is ready for use.

[0025] (2) Separation:

[0026] 600g of silica gel was packed into the column, and 2L of petroleum ether was added to the column again. Load the concentrate in (1), add petroleum ether: ethyl acetate = 3:2 mixture to elute, monitor by TLC, collect the glabridin part, steam under reduced pressure at 45-50°C until no liquid drops drop down, and obtain orange Yellow oil 20-30g.

[0027] (3) Crystallization:

[0028] Add 100 mL of dichloromethane to the above oil, stir for 1 hour, filter with suction, rinse the filter cake with 20 mL of dichloromethane, dry the filter cake at 40°C for 1 hour, and obtain 6 grams of gl...

Embodiment 2

[0030] (1) Extraction:

[0031] Add 2kg of licorice residue and 14.5kg of 95% ethanol to a 20L extraction tank in turn; reflux extraction for 2 hours, release the extract, extract once again with 9kg of 95% ethanol as above, combine the filtrates twice, evaporate 95% ethanol under reduced pressure, and concentrate Things to spare.

[0032] (2) Separation:

[0033] Add 600g of silica gel and 1.5L of petroleum ether to a 3L Erlenmeyer flask successively, pack the column, and then add 2L of petroleum ether to flush the column. Load the concentrate in (1), add petroleum ether: dichloromethane = 2:1 mixture to elute, monitor by TLC, collect the glabridin part, evaporate under reduced pressure at 35-40°C until no liquid drops drop down, and obtain orange Yellow oil 20-30g.

[0034] (3) Crystallization:

[0035] Add 200 mL of petroleum acetone to the above oil, stir for 1 h, filter with suction, and dry the filter cake to obtain 6.2 g of glabridin, yield 0.31%, content: 93%.

Embodiment 3

[0037] (1) Extraction:

[0038] Add 2kg of licorice residue and 14kg of methanol in sequence to a 20L extraction tank; reflux extraction for 2 hours, release the extract, extract the grass residue once more with 9kg of methanol as above, combine the two filtrates, distill out the methanol under reduced pressure, and use the concentrate for later use.

[0039] (2) Separation:

[0040] Add 600g of silica gel and 1.5L of petroleum ether to a 3L Erlenmeyer flask successively, pack the column, and then add 2L of petroleum ether to flush the column. Load the concentrate in (1), add petroleum ether: ethanol = 3:1 mixture to elute, monitor by TLC, collect the glabridin part, steam under reduced pressure at 50-55°C until there is no droplet, and an orange oil is obtained Material 20-30g.

[0041] (3) Crystallization:

[0042] Add 100 mL of toluene to the above oil, stir for 1 h, filter with suction, rinse the filter cake with 20 mL of toluene, and dry the filter cake at 40°C for 1 h...

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Abstract

The invention belongs to the technical field of separation and purification, and particularly relates to a method for extracting and purifying glabridin from glycyrrhiza glabra residues. The method comprises the following steps: (1) extraction: sequentially adding the glycyrrhiza glabra residues and an extraction solvent into an extraction tank, performing reflux extraction twice, and distilling off the solvent under reduced pressure, so as to obtain a concentrate for later use; (2) separation: sequentially adding silica gel and petroleum ether into a conical flask for column packing, performing sample loading on the concentrate obtained in Step (1), adding an elution solvent for elution, performing TLC (Thin Layer Chromatography) detection to collect a glabridin component, and distilling off the solvent under reduced pressure at 30 to 70 DEG C, so as to obtain an orange oily matter; (3) crystallization: adding a crystallization solvent into the oily matter obtained in Step (2), performing stirring and suction filtration, and flushing and drying a filter cake to obtain the glabridin. The method is high in extraction efficiency, the operation steps are convenient and efficient, and the production cost is greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of separation and purification, and in particular relates to a method for extracting and purifying glabridin from licorice glabra residue. Background technique [0002] Glabridin is currently the most effective and safest natural whitening additive in the cosmetics industry, known as the whitening gold in the cosmetics industry. However, due to its extremely high production cost, the price of glabridin in the market is very expensive, and it can only appear in foreign high-end brands. Glycyrrhiza glabra is a flavonoid monomer component with a very low content in Glycyrrhiza glabra. Its preparation method is obtained by extracting and purifying Glycyrrhiza glabra or Glycyrrhiza glabra residue. The method for separating glabridin either has a low extraction rate or complicated steps, resulting in high cost and long time-consuming, and it is difficult to realize industrial production. [0003] In terms of ext...

Claims

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Application Information

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IPC IPC(8): C07D493/04
CPCC07D493/04
Inventor 骆俊才王长江于晓丽胡建彪李宗龙
Owner 青海倍力甘草科技发展有限责任公司
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