A method for efficiently separating and purifying high-purity glycyrrhizic acid

A technology for separating and purifying glycyrrhizic acid, which is applied in chemical instruments and methods, organic chemistry, steroids, etc., can solve the problems of high-purity glycyrrhizic acid being expensive, difficult to enter the international market, and difficult to obtain high-purity, etc. To achieve green environmental protection industrial production, conducive to industrial production, the effect of fast speed

Active Publication Date: 2020-07-31
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

[0003] my country is a big exporter of licorice, but currently it is limited to the export of licorice raw materials and crude products, the value is low and it is difficult to enter the international market, and the price of high-purity glycyrrhizic acid is very expensive, so find a suitable for industrial production of high-purity licorice. The way is very realistic
[0004] At present, most of the industrial production of glycyrrhizic acid in my country still uses the traditional recrystallization method, two-phase extraction method or adsorption resin method. These methods either have low purification efficiency or are difficult to obtain high-purity products, and each has its own advantages and disadvantages.

Method used

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  • A method for efficiently separating and purifying high-purity glycyrrhizic acid

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Effect test

Embodiment 1

[0015] 1) Preparation of glycyrrhizic acid extract: take 10 g of licorice root and crush it into a coarse powder with a particle size of 60 mesh, use 100 mL of 70% (V / V) ethanol solution for ultrasonic extraction for 3 hours, filter and concentrate until the solid content is about 100 mg / mL, Glycyrrhizic acid extract;

[0016] 2) Preparation of crude glycyrrhizic acid: the hydrophilic SPE column (filler is XAmide, filler particle size is 5 μm,

[0017] Loading capacity is 1g) After activating and equilibrating with 4 times column volume of 50% (V / V) ethanol, take 10 mL of the glycyrrhizic acid extract obtained in step (1) and load it on the above-mentioned balanced SPE column, and use 4 times column volume Rinse with 50% (V / V) ethanol solution, add formic acid to adjust the pH to 3.5 in the above activation, equilibration, sample loading and rinsing steps, and add ammonium bicarbonate, the salt concentration should be 2mM, and finally use 5 times the column volume 20% (V / V) e...

Embodiment 2

[0020] 1) Preparation of glycyrrhizic acid extract: take 1 kg of licorice root and rhizome and crush it into a coarse powder with a particle size of 120 mesh, use 10L of 60% ethanol for ultrasonic extraction for 5 hours, filter the filter residue and continue to use 10L of 60% ethanol for ultrasonic extraction for 5 hours, filter, and combine the filtrates. Concentrate to a solid content of about 150mg / mL to obtain a glycyrrhizic acid extract;

[0021] 2) Preparation of glycyrrhizic acid crude product: the hydrophilic SPE column (filler is Click XIon, filler particle size is 60 μm,

[0022] Loading capacity is 50g) with 6 times of column volume 60% (V / V) ethanol activation, balance, take the glycyrrhizic acid extract obtained in step (1) 20mL load on the SPE column of above-mentioned equilibrium, use 4 times of column volume Rinse with 50% (V / V) ethanol solution. For the above activation, equilibration, sample loading and rinsing steps, formic acid should be added to adjust th...

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Abstract

The invention provides a method for efficiently separating and purifying high-purity glycyrrhizic acid from licorice. Specifically, the glycyrrhizic acid extract obtained by concentrating the licorice extract is subjected to hydrophilic solid-phase extraction (SPE) to obtain crude glycyrrhizic acid, and the crude product is subjected to one-step reverse-phase preparation high-performance liquid chromatography to obtain pure glycyrrhizic acid. The characteristics of the present invention are: the present invention has prepared high-purity glycyrrhizic acid; after SPE treatment, the content of glycyrrhizic acid is increased from 13% in the extract to 64% in the crude product of glycyrrhizic acid, which greatly simplifies the complexity of the sample, and is The further purification of the sample creates favorable conditions; SPE has a large single-time treatment capacity and high efficiency, and is suitable for pretreatment and enrichment of target substances; reversed-phase preparative chromatography can obtain glycyrrhizic acid with a purity of 99%, which is conducive to industrial production.

Description

technical field [0001] The invention belongs to the field of natural medicine extraction, in particular to a high-efficiency separation method of high-purity glycyrrhizic acid Background technique [0002] Glycyrrhizic acid (Glycyrrhizic Acid), also known as glycyrrhizin, its molecular formula is C 42 h 62 o 16 , the molecular weight is 822.92. Glycyrrhizic acid is the main active ingredient of the traditional Chinese medicine licorice. Modern pharmacological studies have found that glycyrrhizic acid has anti-inflammatory, anti-tumor, immune-regulating, anti-atherosclerosis, and liver-protecting effects. Clinically, it is widely used in the treatment of chronic viral hepatitis, bronchitis and AIDS. Glycyrrhizic acid is a sweetener with high sweetness, low calorie and strong health care effect. It is an ideal sweetener for obesity, diabetes and heart disease patients. In addition, glycyrrhizic acid also has the functions of correcting flavor, moistening throat, and anti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00C07H15/256C07H1/08
CPCC07H1/08C07H15/256C07J63/008
Inventor 梁鑫淼余文怡刘艳芳金红利沈爱金薛兴亚
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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