CN111217883A - Preparation method of glycyrrhizic acid - Google Patents
Preparation method of glycyrrhizic acid Download PDFInfo
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- CN111217883A CN111217883A CN201811404463.9A CN201811404463A CN111217883A CN 111217883 A CN111217883 A CN 111217883A CN 201811404463 A CN201811404463 A CN 201811404463A CN 111217883 A CN111217883 A CN 111217883A
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- glycyrrhizic acid
- ethanol
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- drying
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J63/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by expansion of only one ring by one or two atoms
- C07J63/008—Expansion of ring D by one atom, e.g. D homo steroids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/24—Condensed ring systems having three or more rings
- C07H15/256—Polyterpene radicals
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- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a preparation method of glycyrrhizic acid, in particular to a method for extracting glycyrrhizic acid by adopting a homogenate-ultrasonic method. The processing steps comprise: drying liquorice in the shade, crushing, adding 50-60% ethanol which is 1-2 times of the raw materials, and placing the mixture in a homogenizer for mixing and homogenizing; after homogenizing, placing the material in an ultrasonic device, adding 50-60% ethanol solution which is 3-5 times of the raw material, performing ultrasonic extraction for 90-120 min, concentrating under reduced pressure, and recovering ethanol to obtain concentrated solution; and (3) loading the obtained concentrated solution onto a column by using 80-100-mesh polyamide resin, eluting, collecting eluent, concentrating and drying to obtain glycyrrhizic acid. The invention has the advantages of rapidness, high efficiency, small using amount of solvent and the like, and has good reproducibility, and the resin can be repeatedly used.
Description
Technical Field
The invention relates to a preparation method of glycyrrhizic acid, belonging to the field of extraction of effective components of traditional Chinese medicines.
Background
The Glycyrrhrizae radix belongs to perennial herb of Leguminosae. As one of the traditional Chinese medicinal materials, the liquorice has various medicinal effects, such as the effects of tonifying spleen and qi, clearing away heat and toxic materials, regulating various medicines and the like. The Glycyrrhrizae radix contains multiple chemical components, wherein the effective components are ferriferrous saponin compounds (glycyrrhizic acid, glycyrrhetinic acid), flavonoid compounds (liquiritin, isoliquiritin), and Glycyrrhiza polysaccharide. According to related researches, people have successfully separated various effective components from liquorice at present, and more than 100 effective components are separated from the liquorice only by flavonoid compounds. Therefore, as the value of the effective components of licorice is increasingly recognized, the extraction and purification technology of the effective components of licorice also becomes a hot spot of the current research.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for preparing glycyrrhizic acid, which has high efficiency and selectivity, simple and convenient operation, high yield and few by-products and can be realized industrially.
The technical scheme of the invention is carried out according to the following steps:
a. drying liquorice in the shade, crushing, adding 50-60% ethanol which is 1-2 times of the raw materials, and placing the mixture in a homogenizer for mixing and homogenizing for 15 min;
b. after homogenizing, placing the material in an ultrasonic device, adding 50-60% ethanol solution which is 3-5 times of the raw material, performing ultrasonic extraction for 90-120 min, concentrating under reduced pressure, and recovering ethanol to obtain concentrated solution;
c. and (3) passing the obtained concentrated solution through a polyamide resin column of 80-100 meshes, eluting by 60-70% of resin volume which is 4-6 times of the resin volume, collecting eluent, concentrating and drying to obtain glycyrrhizic acid.
The power of the homogenizer in the step a is 200W, and the rotating speed of the homogenizer is 10000-20000 r/min.
The ultrasonic extraction conditions in the step b are as follows: the frequency is 40KHz, and the ultrasonic temperature is 50-70 ℃.
The mass ratio of the resin dosage to the raw materials in the step c is 1: 1.
The invention has the advantages that:
1. the invention adopts plant homogenate extraction method to process raw materials, realizes the completion of crushing and extraction in one step, and simultaneously avoids heating, thereby effectively avoiding the damage of the total flavone component.
2. The method adopts homogenate-ultrasonic extraction of glycyrrhizic acid, and has the advantages of low production cost, rapidness, high efficiency and high extraction rate.
The present invention will be further described with reference to specific embodiments, but the scope of the invention as claimed is not limited to the following embodiments.
The specific implementation mode is as follows:
example 1:
drying Glycyrrhrizae radix in the shade, pulverizing, adding 1 time of 50% ethanol, placing in a homogenizer, and mixing and homogenizing at 200W and 10000r/min for 15 min; homogenizing, placing the material in an ultrasonic device with frequency of 40KHz, adding 50% ethanol solution 3 times of the material, performing ultrasonic extraction at 50 deg.C for 90min, concentrating under reduced pressure, and recovering ethanol to obtain concentrated solution; adding the obtained concentrated solution into 80 mesh polyamide resin column, eluting with 70% 4 times of resin volume, collecting eluate, concentrating, drying to obtain glycyrrhizic acid with extraction rate of 92.9%, and UV detecting to obtain total flavone h content of 89.4%.
Example 2:
drying Glycyrrhrizae radix in the shade, pulverizing, adding 2 times of 60% ethanol, placing in a homogenizer, and mixing and homogenizing at 15000r/min under 200W for 15 min; homogenizing, placing the material in an ultrasonic device with frequency of 40KHz, adding 60% ethanol solution 5 times of the raw material, performing ultrasonic extraction at 60 deg.C for 100min, concentrating under reduced pressure, and recovering ethanol to obtain concentrated solution; adding the obtained concentrated solution into 100 mesh polyamide resin column, eluting with 5 times of resin volume of 60%, collecting eluate, concentrating, drying to obtain glycyrrhizic acid with extraction rate of 96.3%, and UV detecting to obtain total flavone content of 93.5%.
Example 3:
drying Glycyrrhrizae radix in the shade, pulverizing, adding 55% ethanol 2 times of the raw materials, placing in a homogenizer, and mixing and homogenizing at 200W and 20000r/min for 15 min; homogenizing, placing the material in an ultrasonic device with frequency of 40KHz, adding 55% ethanol solution 4 times of the material, performing ultrasonic extraction at 70 deg.C for 120min, concentrating under reduced pressure, and recovering ethanol to obtain concentrated solution; adding the obtained concentrated solution into 100 mesh polyamide resin column, eluting with 6 times of resin volume of 65%, collecting eluate, concentrating, drying to obtain glycyrrhizic acid with extraction rate of 93.6%, and UV detecting to obtain total flavone content of 97.3%.
Claims (4)
1. A preparation method of glycyrrhizic acid is characterized by comprising the following steps:
a. drying liquorice in the shade, crushing, adding 50-60% ethanol which is 1-2 times of the raw materials, and placing the mixture in a homogenizer for mixing and homogenizing for 15 min;
b. after homogenizing, placing the material in an ultrasonic device, adding 50-60% ethanol solution which is 3-5 times of the raw material, performing ultrasonic extraction for 90-120 min, concentrating under reduced pressure, and recovering ethanol to obtain concentrated solution;
c. and (3) passing the obtained concentrated solution through a polyamide resin column of 80-100 meshes, eluting by 60-70% of resin volume which is 4-6 times of the resin volume, collecting eluent, concentrating and drying to obtain glycyrrhizic acid.
2. The method for preparing glycyrrhizic acid according to claim 1, wherein the power of the homogenizer in step a is 200W, and the rotation speed of the homogenizer is 10000-20000 r/min.
3. The method for preparing glycyrrhizic acid according to claim 1, wherein the ultrasonic extraction conditions in step b are as follows: the frequency is 40KHz, and the ultrasonic temperature is 50-70 ℃.
4. The method for preparing glycyrrhizic acid according to claim 1, wherein the mass ratio of the resin amount to the raw materials in step c is 1: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811404463.9A CN111217883A (en) | 2018-11-23 | 2018-11-23 | Preparation method of glycyrrhizic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811404463.9A CN111217883A (en) | 2018-11-23 | 2018-11-23 | Preparation method of glycyrrhizic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111217883A true CN111217883A (en) | 2020-06-02 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811404463.9A Pending CN111217883A (en) | 2018-11-23 | 2018-11-23 | Preparation method of glycyrrhizic acid |
Country Status (1)
| Country | Link |
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| CN (1) | CN111217883A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112940067A (en) * | 2021-02-05 | 2021-06-11 | 广州贝塔健康生物科技有限公司 | Comprehensive extraction method of liquorice and application of liquorice in cosmetics |
-
2018
- 2018-11-23 CN CN201811404463.9A patent/CN111217883A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112940067A (en) * | 2021-02-05 | 2021-06-11 | 广州贝塔健康生物科技有限公司 | Comprehensive extraction method of liquorice and application of liquorice in cosmetics |
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Application publication date: 20200602 |