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Method for extracting, separating and purifying glabridin from glycyrrhiza glabra residues

A technology of licorice glabra residue and glabridin, applied in chemical instruments and methods, organic chemistry, lignin derivatives, etc., to achieve high extraction rate, high purity, and simple operation

Pending Publication Date: 2022-07-01
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In summary, in the prior art research on the extraction of flavonoids from traditional Chinese medicines or plants by deep eutectic solvents, most of the attention is paid to the extraction rate of flavonoids by deep eutectic solvents, and the separation and purification of flavonoids in the extract. , and the recycling of deep eutectic solvents has not been paid attention to

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  • Method for extracting, separating and purifying glabridin from glycyrrhiza glabra residues
  • Method for extracting, separating and purifying glabridin from glycyrrhiza glabra residues
  • Method for extracting, separating and purifying glabridin from glycyrrhiza glabra residues

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Embodiment 1

[0032] Example 1: Extraction of Glycyrrhizin

[0033] (1) preparation of extraction solvent: choline chloride and propionic acid are stirred at room temperature for 0.5h in a water-bath magnetic stirring pot in a molar ratio of 1:2-4 to obtain a transparent and uniform deep eutectic solvent, which is 10% by volume, Deionized water was added to 20% and 30% to configure the extraction solvent.

[0034] (2) Extraction: take 2 kg of Glycyrrhiza glabra slag, dry at 60°C for 12 hours, pulverize, and pass through an 80-mesh sieve to obtain Glycyrrhiza glabra slag powder. Take 2g of Glycyrrhiza glabra slag powder respectively in a 100mL conical flask, add the extraction solvent prepared in step (1) according to the material-to-liquid ratio of 1:20, 1:30 or 1:40 mg / mL, and divide the extraction solvent into 1-3 times Add, 30-80 ℃ ultrasonic-assisted extraction for 0.5-2h, suction filtration to obtain the glabridin crude extract, HPLC to determine the content of glabridin, calculate th...

Embodiment 2

[0035] Example 2: Screening of extraction solvents and extraction conditions

[0036] (1) preparation of extraction solvent: choline chloride is respectively mixed with formic acid, acetic acid, glycolic acid, lactic acid and propionic acid in a molar ratio of 1:4, stirring at room temperature for 30min to obtain a transparent and uniform deep eutectic solvent, by volume The percentage is 20%, and deionized water is added to configure it as an extraction solvent. Another 90% ethanol was prepared as the extraction solvent.

[0037](2) Extraction: take 2 kg of Glycyrrhiza glabra slag, dry at 60°C for 12 hours, pulverize, and pass through an 80-mesh sieve to obtain Glycyrrhiza glabra slag powder. Take 2g of Glycyrrhiza glabra slag powder in a 100mL conical flask, add extraction solvent according to the material-to-liquid ratio of 1:20 mg / mL, extract at 60 °C for 1 h, and filter with suction to obtain a crude extract of Glycyrrhiza glabra. The content of Glycyrrhizin is determine...

Embodiment 3

[0040] Embodiment 3: the screening of extractant and the amount of extractant

[0041] (1) preparation of extraction solvent: choline chloride and propionic acid are stirred at room temperature for 0.5h in a water-bath magnetic stirring pot in a molar ratio of 1:4 to obtain a transparent and uniform deep eutectic solvent, which is 10% by volume and deionized Water, configured as extraction solvent.

[0042] (2) Extraction: take 2 kg of Glycyrrhiza glabra slag, dry at 60°C for 12 hours, pulverize, and pass through an 80-mesh sieve to obtain Glycyrrhiza glabra slag powder. Take 10g of Glycyrrhiza glabra slag powder in a 500mL conical flask, add the extraction solvent prepared in step (1) according to the material-to-liquid ratio of 1:20mg / mL, 40 ℃ ultrasonic-assisted extraction for 1h, and suction filtration to obtain the crude extract of Glycyrrhiza liquid, the extraction rate of glabridin was 0.49 mg / g.

[0043] (3) extraction: get petroleum ether, cyclohexane, ethyl acetate...

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Abstract

The invention discloses a method for extracting glabridin from glycyrrhiza glabra residues and separating and purifying the glabridin, which comprises the following steps: by taking glycyrrhiza glabra residues as a raw material, extracting the glabridin by using a choline chloride / propionic acid eutectic solvent under the assistance of ultrasonic waves, extracting an extracting solution by using ethyl acetate, and carrying out gradient rotary evaporation on an extracting agent phase to obtain a glabridin crude extract; the glabridin crude extract is adsorbed, separated and purified by using macroporous resin, so that relatively high purity and recovery rate of the glabridin are achieved; and carrying out ethanol sedimentation and centrifugation on the extract phase to obtain xylooligosaccharide, carrying out rotary evaporation on the supernatant, adding deionized water for sedimentation and centrifugation to obtain lignin, further removing moisture from the supernatant through a reverse osmosis membrane, and recovering the eutectic solvent. According to the method for extracting and purifying the glabridin from the glycyrrhiza glabra residues, the green eutectic solvent is adopted, separation and purification of the glabridin, the xylooligosaccharide and the lignin are achieved, meanwhile, the eutectic solvent is recycled, the extraction efficiency is high, and the method is green and environmentally friendly.

Description

technical field [0001] The invention belongs to the technical field of extraction, separation and purification of functional components in traditional Chinese medicines or plants, and in particular relates to a method for extracting licorice from licorice dregs and separating and purifying the extract. Background technique [0002] Glycyrrhiza glabra is a leguminous dicotyledonous plant, containing glycyrrhizic acid, triterpenoid saponins, liquiritin, isoglycyrrhizin, polysaccharides and other substances, with anti-inflammatory, antibacterial, whitening and other effects. Glycyrrhiza glabra is extracted from Glycyrrhiza glabra by factories to produce a large amount of Glycyrrhiza glabra slag, in which there are still many small-molecule functional components such as flavonoids. Among them, Glycyrrhiza glabra is one of the main flavonoid components in Glycyrrhiza glabrata, and only exists In Glycyrrhiza glabra, it has pharmacological effects such as anti-oxidation, lowering b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/04C07G1/00C07H3/06C07H1/08
CPCC07D493/04C07G1/00C07H3/06C07H1/08
Inventor 刘晓云周俊周华曾庆达吴昊
Owner NANJING UNIV OF TECH
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