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Method for purifying glycyrrhizic acid by using preparative chromatography technology

A technology of glycyrrhizic acid and chromatography, which is applied in the field of separation and purification of herbal medicinal components, can solve the problems of narrow separation range, large amount of solvent treatment, cumbersome process, etc., and achieves easy industrial production, low solvent consumption, and good separation selectivity Effect

Pending Publication Date: 2022-06-10
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Due to the similar structure, it is very difficult to separate the two isomers. The general purification method cannot be separated and the yield is low, resulting in a lot of waste. The main disadvantages of the production method are as follows:
[0008] 1. Repeated crystallization is easy to damage the product structure;
[0009] 2. Aqueous two-phase extraction, with less optional extraction systems, narrow separation range, difficult post-processing, easy emulsification, and difficult solvent recovery;
[0010] 3. Macroporous adsorption resin has problems such as cumbersome process, large amount of solvent treatment, low yield, poor process stability, and unguaranteed product purity, which restricts the large-scale production of its high-quality products;
[0011] 4. The supercritical carbon dioxide extraction method has the disadvantages of high extraction conditions, high cost, and potential safety hazards at high temperature and high pressure;

Method used

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  • Method for purifying glycyrrhizic acid by using preparative chromatography technology
  • Method for purifying glycyrrhizic acid by using preparative chromatography technology
  • Method for purifying glycyrrhizic acid by using preparative chromatography technology

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Experimental program
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Effect test

Embodiment 1

[0034] 15 g of glycyrrhizic acid extract was dissolved in 300 mL of 50% acetone water to prepare a sample solution with a concentration of 50 mg / mL, and the sample loading amount was 5%. Using polar groups to modify silica gel (C18 connected diamino modified packing, the bonding amount is 2.28μmol / m 2 ) packed chromatographic column (column size 50×250mm, particle size 30μm, pore size Filler mass 300g). Elute with acetone: acetic acid water (1%, v / v)=10:90, flow rate 50mL / min, collect 30~98min according to the peak shape curve after the target peak, the target analytical solution is concentrated and dried by the prior art, the obtained The content of glycyrrhizic acid in the product is 91.76% (the related substance impurity A is 2.51%, the isomer impurity 18α glycyrrhizic acid is 3.11%), and the yield is 93.8%.

Embodiment 2

[0036] 5 g of glycyrrhizic acid extract was added into 50 mL of 50% methanol water to dissolve, and the sample solution with a concentration of 100 mg / mL was prepared, and the sample loading amount was 10%. Silica gel modified with polar groups (C8-linked amide modified packing, the bonding amount is 2.41 μmol / m 2 ) packed chromatographic column (column size 20×250mm, particle size 10μm, pore size Filler mass 50g). Elute with methanol: formic acid water (0.5%, v / v)=20:80, flow rate 50mL / min, collect 35-90min according to the peak shape curve after the target peak, the target analytical solution is concentrated and dried by the prior art, the obtained The content of glycyrrhizic acid in the product is 93.25% (the related substance impurity A is 2.08%, the isomer impurity 18α glycyrrhizic acid is 2.86%), and the yield is 92.5%.

Embodiment 3

[0038]10 kg of glycyrrhizic acid extract was added to dissolve in 100 L of 50% ethanol water to prepare a sample solution with a concentration of 100 mg / mL, and the sample loading amount was 8%. Modified silica gel with polar groups (C4-linked amino-modified packing, the bonding amount is 2.69 μmol / m 2 ) packed chromatographic column (column size 1000×250mm, particle size 30μm, pore size Filler mass 120kg). Elute with ethanol: oxalic acid water (2%, v / v)=25:75, flow rate 20L / min, collect 32~98min according to the peak shape curve after the target peak, the target analytical solution is concentrated and dried by the prior art, the obtained The content of glycyrrhizic acid in the product is 93.25% (the related substance impurity A is 2.08%, the isomer impurity 18α glycyrrhizic acid is 2.48%), and the yield is 90.5%.

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Abstract

The invention provides a method for separating and purifying glycyrrhizic acid by using preparative chromatography, which is characterized in that glycyrrhizic acid is purified by using a glycyrrhizic extract as a raw material, using a preparative chromatography separation and purification means, adopting a polar group modified silica gel filler and using an organic solvent as an eluent to obtain a glycyrrhizic acid product with the content of more than 90% (related substance impurity Alt; 3% of isomer impurity 18 alpha glycyrrhizic acid lt; 5%). The method has the characteristics of effective removal of isomer impurities, control of limited impurity content, high recovery rate, high product content, less solvent consumption, good stability, simple process flow, simple and controllable operation and the like, and is suitable for production separation and purification.

Description

technical field [0001] The method relates to the technical field of separation and purification of plant medicinal components, in particular to a method for separating and purifying glycyrrhizic acid using preparative chromatography. ). Background technique [0002] Licorice is a licorice plant of the Leguminosae subfamily Papiliantae Taub and is an important traditional Chinese medicine in my country. Medicines are food. Its main active ingredient is glycyrrhizic acid (Glyrrhizicacid), also known as glycyrrhizin, glycyrrhizin, which is a triterpenoid saponin extracted from the dried roots and rhizomes of licorice. In recent years, it has also been used to prevent and treat viral hepatitis, cancer and AIDS. In the pharmaceutical industry, glycyrrhizic acid is usually made into water-soluble glycyrrhizate, such as monoammonium glycyrrhizate as the raw material for the production of preparations. In 1992, monoammonium glycyrrhizate was designated by the Ministry of Health a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00B01D15/08
CPCC07J63/008B01D15/08
Inventor 丰加涛梁鑫淼钟正升
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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