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Separation and purification method of high-purity glabridin

A technology for the separation and purification of glabridin, which is applied in organic chemistry and other fields, can solve the problems of difficult further improvement of product purity, low product yield, complicated operation, etc., and achieve the effects of easy quality control, high yield and efficient process

Inactive Publication Date: 2010-09-15
CHENGDU PUSH BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent 200510023860.8 discloses a production method of high-purity glabridin. In this method, the glabridin extract is ultra-filtered, then further adsorbed by polymer resin, rinsed with eluent and recrystallized to obtain a purity of more than 90%. Glabridin, but the purity of the product is difficult to further improve, and this method uses ultrafiltration technology and polymer resin separation method, complicated operation, high cost and low product yield

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  • Separation and purification method of high-purity glabridin
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  • Separation and purification method of high-purity glabridin

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Embodiment 1

[0033] The separation and purification method of the glabridin monomer of the present embodiment is carried out according to the following process steps:

[0034](1) Extraction of effective parts: take 10KG of Glycyrrhiza glabra, add 80L of ethanol solution with a concentration of 20% by volume, heat and extract at 60°C for three times, and the extraction time is 3, 2, and 1 h respectively, and the extracts are combined, Concentrate under reduced pressure at the temperature of 40 ℃~50 ℃, recover ethanol to dryness, obtain 3L of extract material extract, HPLC detects (mobile phase: acetonitrile-water (50:50) wavelength: 292nm flow rate: 1ml / min C18 ( 250×4.6mm) injection volume: 10ul) This extract contains glabridin (see figure 1 ).

[0035] (2), enrichment of effective part and impurity removal: add equal volume of ethyl acetate to extract 3 times after the extract extract is suspended with tap water of 3 times the quality, and detect that the product has been extracted in a ...

Embodiment 2

[0040] The separation and purification method of the glabridin monomer of the present embodiment is carried out according to the following process steps:

[0041] (1), extraction of effective parts: take 20KG of Glycyrrhiza glabra, add 160L of ethanol solution with a volume percentage concentration of 60%, heat and extract at 50 ° C for three times, the extraction time is respectively 3, 2, 1h, and the extracts are combined, Concentrate under reduced pressure at a temperature of 40°C to 50°C, recover ethanol to dryness, and obtain 6L of extract material, which is detected by HPLC (mobile phase: acetonitrile-water (50:50), wavelength: 292nm, flow rate: 1ml / min C18 (250×4.6mm), injection volume: 10ul) This extract contains glabridin (see figure 2 ).

[0042] (2), enrichment of effective parts and impurity removal: after the extract extract is suspended with 3 times of tap water, add an equal volume of dichloromethane for repeated extraction, and detect that the product has bee...

Embodiment 3

[0047] The separation and purification method of the glabridin monomer of the present embodiment is carried out according to the following process steps:

[0048] (1) Extraction of effective parts: take 30KG of Glycyrrhiza glabrata, add 340L of ethanol solution with a volume percentage concentration of 95%, heat and extract three times at 40°C, and the extraction time is 3, 2, and 1 h respectively, and the extracts are combined, Concentrate under reduced pressure at a temperature of 40°C to 50°C, recover ethanol to dryness, and obtain 10 L of the extract, which is detected by HPLC to contain glabridin (see image 3 ).

[0049] (2), enrichment of effective parts and impurity removal: after the extract extract is suspended with 3 times of tap water, an equal volume of chloroform is added for repeated extraction, and the product has been extracted in large quantities by HPLC detection (see Figure 4 ), until the glabridin can not be detected in the aqueous phase, remove the pola...

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Abstract

The invention discloses a high-efficiency separation and purification method of a glabridin monomer. The method comprises the steps of: extracting raw material dried roots of Glycyrrhiza Glycyrrhiza glabra L which is a leguminous plant with an organic reagent A; and then extracting with an organic reagent B; carrying out chromatography by using polyamide columns and macroporous adsorbent resin columns; and finally separating and purifying a target area solution by using high effective liquid chromatogram columns; carrying out on-line test by using HPLC (High Performance Liquid Chromatography), and purposely collecting a glabridin monomer solution to obtain the glabridin monomer with the concentration higher than 98%. The invention has the advantages of high production quantity, high yield rate and good production quality, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for separating and purifying licorice from leguminous plant licorice, belonging to the technical field of separation and purification of monomer active components in plants. Background technique [0002] Glycyrrhiza Glycyrrhiza (Glycyrrhiza glabra L.) is mainly produced in Northeast my country, North China and Northwest provinces and regions, born on riverbank terraces, ditchside, field side, roadside, Europe, Mediterranean area, Kazakhstan, Uzbekistan, Turkmenistan, Kyrgyzstan, Tajikistan, Russian Siberia and Mongolia are also produced. The flavonoids in Glycyrrhiza glabra have obvious anti-ulcer, antibacterial, anti-inflammatory, and hypolipidemic effects, as well as obvious free radical scavenging and antioxidant effects. Glabridin is the main flavonoid component in Glycyrrhiza glabra. one, whose molecular formula is C 20 H 20 O 4 , the molecular weight is 324.3704, and the structural formula is shown in formula ...

Claims

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Application Information

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IPC IPC(8): C07D493/04
Inventor 董维珍郭建华文焕松刘丁夏柯
Owner CHENGDU PUSH BIOLOGICAL TECH
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