Method for simultaneously extracting and separating glycyrrhizic acid and glycyrrhiza flavonoids of glycyrrhiza based on continuous chromatography

A technology of total flavonoids of licorice and continuous chromatography is applied in the field of natural medicine extraction to achieve the effect of simplifying the extraction process, having good properties and high purity

Active Publication Date: 2017-06-27
DALIAN POLYTECHNIC UNIVERSITY
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  • Abstract
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Problems solved by technology

The new method for extracting and separating glycyrrhizic acid and total flavonoids of licorice has not been reported at home and abroad

Method used

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  • Method for simultaneously extracting and separating glycyrrhizic acid and glycyrrhiza flavonoids of glycyrrhiza based on continuous chromatography
  • Method for simultaneously extracting and separating glycyrrhizic acid and glycyrrhiza flavonoids of glycyrrhiza based on continuous chromatography
  • Method for simultaneously extracting and separating glycyrrhizic acid and glycyrrhiza flavonoids of glycyrrhiza based on continuous chromatography

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Crush the roots or stems of licorice, take 2000g of licorice powder and add 12L of ammonia alcohol solution in a beaker, stir evenly, pour it into the diafiltration device, then slowly add 68L of 0.5% ammonia water, The ammonia alcohol aqueous solution of 70% ethanol, setting inflow speed is 5ml / min, adjusts outflow speed and inflow speed to be consistent, collects leachate, obtains licorice extract. Load the licorice extract to a continuous chromatographic device equipped with D941 resin for adsorption at a flow rate of 14.08ml / min, set the single-column running time to 107min, collect the sample effluent, and use 70% ethanol solution at a flow rate of 14.00ml / min elutes a small amount of total flavonoids of licorice adsorbed on the resin, and collects the ethanol eluent 1, then uses 0.5mol / L NaOH aqueous solution to elute glycyrrhizic acid at a flow rate of 7.89ml / min, and collects the NaOH eluent. Combine the sample effluent and the ethanol eluent 1, spin the combin...

Embodiment 2

[0030] Crush the roots or stems of licorice, take 1000g of licorice powder and add 6L of ammonia alcohol solution in a beaker, stir evenly, pour it into the diafiltration device, then slowly add 34L of 0.5% ammonia water, 70 % ethanol ammonia alcohol aqueous solution, set the inflow rate to 5ml / min, adjust the outflow rate to be consistent with the inflow rate, collect the leachate, and obtain the licorice extract. Load the licorice extract to a continuous chromatographic device equipped with D941 resin for adsorption at a flow rate of 14.08ml / min, set the single-column running time to 107min, collect the sample effluent, and use 70% ethanol solution at a flow rate of 14.00ml / min elutes a small amount of total flavonoids of licorice adsorbed on the resin, and collects the ethanol eluent 1, then uses 0.5mol / L NaOH aqueous solution to elute glycyrrhizic acid at a flow rate of 7.89ml / min, and collects the NaOH eluent. Combine the sample effluent and the ethanol eluent 1, spin th...

Embodiment 3

[0032]Crush the roots or stems of licorice, take 4000g of licorice powder and add 24L of ammonia alcohol solution in a beaker, stir evenly, pour it into the diafiltration device, then slowly add 136L of 0.5% ammonia water, 70 % ethanol ammonia alcohol aqueous solution, set the inflow rate to 5ml / min, adjust the outflow rate to be consistent with the inflow rate, collect the leachate, and obtain the licorice extract. Load the licorice extract to a continuous chromatographic device equipped with D941 resin for adsorption at a flow rate of 14.08ml / min, set the single-column running time to 107min, collect the sample effluent, and use 70% ethanol solution at a flow rate of 14.00ml / min elutes a small amount of total flavonoids of licorice adsorbed on the resin, and collects the ethanol eluent 1, then uses 0.5mol / L NaOH aqueous solution to elute glycyrrhizic acid at a flow rate of 7.89ml / min, and collects the NaOH eluent. Combine the sample effluent and the ethanol eluent 1, spin t...

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Abstract

The invention relates to a method for simultaneously extracting and separating glycyrrhizic acid and glycyrrhiza flavonoids of glycyrrhiza based on continuous chromatography and belongs to the field of natural medicine extraction. Radix glycyrrhizae is smashed and then undergoes extraction by ammonia and alcohol, continuous chromatographic adsorption, ethanol eluting 1, combined spin, polyamide adsorption, ethanol eluting 2 and rotary drying to obtain glycyrrhiza flavonoids; NaOH aqueous solution elution, pH adjustment, spin drying, filtering drying and recrystallization are performed to obtain glycyrrhizic acid. A production device adopted for the method is a continuous chromatographic separation system which is controlled under a logic control valve and is composed of 12 chromatographic columns, and the chromatographic column in the system is divided into four areas which are an adsorption area, a flavonoid analysis area, a glycyrrhizic acid analysis area and a resin regeneration area. The production process is simple to operate, the glycyrrhizic acid and glycyrrhiza flavonoids can be extracted simultaneously, waste of the glycyrrhiza flavonoids in conventional industrial production is reduced, the acid liquor pollution is avoided, so that the yield and purity of the obtained glycyrrhizic acid and glycyrrhiza flavonoids are high, and the method can be suitable for large-scale production.

Description

technical field [0001] The invention relates to the field of extraction of natural medicines, in particular to a method for simultaneously extracting and separating glycyrrhizic acid and total flavonoids of licorice based on continuous chromatography technology. Background technique [0002] Licorice ( Glycyrrhiza uralensis Fisch) is a member of the Fabaceae (Leguminosae) Papilionaceae (Tapiliantae Taub.) Glycyrrhizae ( Glycyrrhiza ) is a perennial herb plant widely distributed in my country and rich in resources, and its roots and rhizomes are important traditional Chinese medicines in my country. The main active ingredients in licorice are triterpenoids and total flavonoids, among which glycyrrhizic acid and liquiritin are important monomer components in triterpenoids and total flavonoids respectively, and have strong pharmacological activity. [0003] At present, in traditional Chinese medicine processing enterprises, the extraction and separation of active ingredient...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/256C07H1/08C07J63/00A61K36/484
CPCA61K36/484C07H1/08C07H15/256C07J63/008
Inventor 朱靖博丁燕李清潭
Owner DALIAN POLYTECHNIC UNIVERSITY
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