CN111100181A - Method for extracting glycyrrhizic acid crude product from liquorice - Google Patents
Method for extracting glycyrrhizic acid crude product from liquorice Download PDFInfo
- Publication number
- CN111100181A CN111100181A CN201911414312.6A CN201911414312A CN111100181A CN 111100181 A CN111100181 A CN 111100181A CN 201911414312 A CN201911414312 A CN 201911414312A CN 111100181 A CN111100181 A CN 111100181A
- Authority
- CN
- China
- Prior art keywords
- extraction
- glycyrrhizic acid
- extracting
- licorice
- solvent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
-
- 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
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/36—Control of physical parameters of the fluid carrier in high pressure liquid systems
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/045—Standards internal
Landscapes
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Biotechnology (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a method for extracting a glycyrrhizic acid crude product from liquorice. Mixing a licorice medicinal material and an organic solvent according to a certain proportion, adding a pH regulator into a mixed system, controlling the pH value of the system to be less than or equal to 4, and performing multi-stage extraction on glycyrrhizic acid in the medicinal material; the first-grade extracting solution is used for further purifying glycyrrhizic acid, and the subsequent-grade glycyrrhizic acid extracting solution can be continuously applied to the extraction of the licorice medicinal materials in the next round/batch. According to the extraction method of the glycyrrhizic acid crude product, the glycyrrhizic acid is efficiently extracted, so that the damage of the glycyrrhizic acid is avoided; the used organic solvent can be efficiently recovered by modern means, the problems of wastewater treatment and environmental protection in the traditional glycyrrhizic acid extraction process are solved, the nutrient components such as starch, protein and the like in the licorice dregs are well preserved, and the efficient utilization of the licorice resource is realized.
Description
Technical Field
The invention relates to the technical field of medicinal material extraction, in particular to a method for extracting a glycyrrhizic acid crude product from liquorice.
Background
The licorice is the dried root and rhizome of glycyrrhiza (Glycyrrhiza uralensis Fisch.) of Glycyrrhiza of Leguminosae, Glycyrrhiza inflata (G.inflataBat.), Glycyrrhiza glabra (G.Glabral.), is a commonly used bulk drug and is reputed as "nineteen herbs" and "old people". The Glycyrrhrizae radix contains various components such as saponins, triterpenes, flavonoids, coumarin, sterol, alkaloid, volatile oil, organic acid, amino acids, etc. Glycyrrhizic acid is the pentacyclic triterpenoid saponin compound which is most and earliest researched from the components of the liquorice at present. It is a sweet component of licorice, also called glycyrrhizin, and has sweetness 200-300 times that of sucrose. Glycyrrhizic acid has antiallergic, antitumor, antiulcer, and antiinflammatory effects. Glycyrrhizic acid is widely applied to the fields of medicines, foods and cosmetics mainly in the forms of ammonium salt, potassium salt, zinc salt, glycyrrhetinic acid and the like.
The glycyrrhizic acid content in the licorice root rhizome is about 1-12%, and the glycyrrhizic acid mainly exists in the forms of free acid, sodium salt, calcium salt, potassium salt and magnesium salt. The extraction method of glycyrrhizic acid mainly comprises water extraction, dilute ammonia water extraction, ammonia alcohol extraction, microwave-assisted extraction, etc. Because of low solvent cost, safe application and high extraction rate of effective components, the dilute ammonia water extraction method is the main extraction method of glycyrrhizic acid in the current industrial production. However, the process of extraction uses ammonia water, which causes the extracted dregs to contain a large amount of ammonia, the dregs to have bad smell during storage, the starch in the medicinal materials and other nutrient components to be damaged, and the subsequent application of the dregs is greatly limited; on the other hand, the process adopts an alkali dissolution and acid precipitation process to obtain glycyrrhizic acid powder, the strong acid solution has about 20 percent of destructive effect on glycyrrhizic acid, and a large amount of acid water generated by the process brings great pressure to environmental protection. At present, most domestic glycyrrhizic acid powder manufacturers stop due to the environmental protection requirements and the limitation of cost improvement.
Along with the year-by-year shortage of liquorice resources in China in recent years and the strong advocated national aspects of green manufacturing and environmental protection, the extraction of the liquorice needs to be developed in a clean and efficient extraction process.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The invention aims to provide a method for extracting a glycyrrhizic acid crude product from liquorice, which realizes the high-efficiency extraction of glycyrrhizic acid and avoids the damage of glycyrrhizic acid; the used organic solvent can be efficiently recovered by modern means, the problems of wastewater treatment and environmental protection in the traditional glycyrrhizic acid extraction process are solved, the nutrient components such as starch, protein and the like in the licorice dregs are well preserved, and the efficient utilization of the licorice resource is realized.
In order to achieve the purpose, the invention provides a method for extracting a glycyrrhizic acid crude product from liquorice, which comprises the following steps: crushing liquorice: crushing a licorice medicinal material into licorice medicinal powder, and controlling the granularity of the licorice medicinal powder to be 30-200 meshes; and primary extraction: mixing organic solvent and water to obtain first solvent, and mixing with the above Glycyrrhrizae radix powder in a ratio of (2-20): 1 (volume/weight, V/W), stirring, adding pH regulator, adjusting pH, stirring and extracting for 0.5-3 hr, filtering, and collecting primary extractive solution and residue; the primary extracting solution is the glycyrrhizic acid crude product.
In an embodiment of the present invention, in the licorice crushing step, the grain size of the licorice powder is preferably 30 to 100 mesh.
The invention also provides a method for extracting the glycyrrhizic acid crude product from the liquorice, which comprises the following steps: crushing liquorice: crushing a licorice medicinal material into licorice medicinal powder, and controlling the granularity of the licorice medicinal powder to be 30-200 meshes; primary extraction: mixing organic solvent and water to obtain first solvent, and mixing with the Glycyrrhrizae radix powder in a ratio of (2-20): 1(V/W), stirring, adding a pH regulator, regulating the pH value, stirring and extracting for 0.5-3 hours, filtering, and collecting a first-stage extracting solution and first-stage medicine residues; and K-level extraction: mixing the first solvent and the residue obtained in the previous stage of extraction with a solvent of (2-20): 1(V/W), stirring, adding a pH regulator, regulating the pH value, stirring and extracting for 0.5-3 hours, filtering, and collecting a K-grade extracting solution and K-grade medicine dregs; and starting from K-2 to execute the K-level extraction until N-level extraction is performed, so that a complete round of extraction is completed, wherein N is more than or equal to 2 and less than or equal to 8, and the primary extracting solution is the glycyrrhizic acid crude product.
In an embodiment of the present invention, in each round of extraction process, the first solvent further includes each stage of extraction solution other than the first stage of extraction solution in the previous round/batch of extraction, and this measure can recycle the solution, improve the utilization rate of the solvent, and simultaneously avoid the problems of wastewater treatment and environmental protection in the traditional glycyrrhizic acid extraction process.
In one embodiment of the present invention, in the primary extraction step, the organic solvent is at least one selected from the group consisting of alcohols, alcohol derivatives, and ketones.
In one embodiment of the present invention, in the first extraction step, the organic solvent is at least one selected from methanol, ethanol, ethyl acetate and acetone.
In an embodiment of the present invention, in the primary extraction step, the water accounts for 0 to 30% by volume of the first solvent.
In one embodiment of the present invention, in the primary extraction step, the first solvent is one selected from methanol-ethanol and ethanol-ethyl acetate.
In an embodiment of the present invention, in the primary extraction step, the ratio of the first solvent to the licorice powder is preferably (4-9): 1 (volume/weight, V/W).
In one embodiment of the present invention, in the first extraction step and the K-extraction step, the pH adjusting agent is at least one selected from the group consisting of: h2SO4、HCl、H3PO4Polyphosphoric acid, CH3COOH, citric acid, oxalic acid, cation exchange resin, a buffer system with pH less than or equal to 2, and solutions with different concentrations prepared by at least one of the substances; preferably, the pH regulator is H2SO4-HCl. The buffer system with the pH value less than or equal to 2 is preferably a glycine-hydrochloric acid buffer system, and is further preferably a glycine-hydrochloric acid buffer system of 0.1-0.3M.
In one embodiment of the present invention, in the first extraction step and the K-extraction step, the pH is adjusted to 4 or less.
In one embodiment of the present invention, the pH is adjusted to between 0.5 and 4 in the first extraction step and the K-extraction step.
In one embodiment of the present invention, in the first extraction step and the K-extraction step, the time for stirring extraction after adding the pH adjuster is preferably 0.3 to 1 hour.
Compared with the prior art, the invention has the following beneficial effects:
the method for extracting the glycyrrhizic acid crude product from the liquorice uses the organic solvent and the pH regulator to extract the glycyrrhizic acid, so that on one hand, the extraction rate of the glycyrrhizic acid is improved, and the loss and the damage of the alkali-dissolving and acid-precipitating steps in the traditional process are avoided; on the other hand, the extraction solvent used in the extraction process is circularly applied to extract the medicinal materials, so that the utilization rate of the organic solvent is improved, and the components such as water-soluble protein, starch and the like in the liquorice dregs are well reserved by using the organic solvent. In addition, the organic solvent used in the extraction process can be recycled, so that the pollution problem caused by water extraction in the traditional glycyrrhizic acid extraction process is avoided.
Drawings
Fig. 1 is a process flow diagram of a method for extracting crude glycyrrhizic acid from licorice according to an embodiment of the present invention.
Detailed Description
The following detailed description of specific embodiments of the invention is provided, but it should be understood that the scope of the invention is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The following describes a method for extracting crude glycyrrhizic acid from licorice by way of several examples.
Example 1
(1) Crushing and crushing a licorice medicinal material to ensure that the granularity of the medicinal powder is all 40-mesh standard sieve;
(2) primary extraction: taking 1kg of the licorice powder, adding 5L of methanol-ethanol (V/V, 15/85), stirring uniformly, adding appropriate amount of 0.2M glycine-hydrochloric acid (V/V, 1/4), controlling the pH value of the mixed system to be 2-4, stirring and extracting for 30 minutes, filtering, and respectively collecting grade 1 extract and dregs;
(3) two-six stage extraction: extracting the medicinal materials by the same method for five stages, namely 6 stages, and collecting the extraction solution and the dregs respectively;
(4) and (3) separating and purifying glycyrrhizic acid: the 1-grade extracting solution is used for separating and purifying glycyrrhizic acid, filtrate obtained after the glycyrrhizic acid in the 1-grade extracting solution is purified is subjected to solvent recovery, and the other grades of extracting solutions are used for extracting a new batch of licorice medicinal materials.
Example 2
(1) Crushing and crushing a licorice medicinal material to ensure that the granularity of the medicinal powder is all 40-mesh standard sieve;
(2) primary extraction: mixing 1kg of the Glycyrrhrizae radix powder with 5L of the mixture of the 2-6 grade extractive solution of example 1, stirring, adding appropriate amount of 0.2M glycine-hydrochloric acid (V/V, 1/4), controlling pH of the mixture system to 2-4, stirring and extracting for 30 min, filtering, and collecting the 1 grade extractive solution and residue respectively;
(3) two-six stage extraction: extracting the medicinal materials by the same method for five stages, namely 6 stages, and collecting the extraction solution and the dregs respectively;
(4) and (3) separating and purifying glycyrrhizic acid: the 1-grade extracting solution is used for separating and purifying glycyrrhizic acid, filtrate obtained after the glycyrrhizic acid in the 1-grade extracting solution is purified is subjected to solvent recovery, and the other grades of extracting solutions are used for extracting a new batch of licorice medicinal materials.
Example 3
(1) Crushing and crushing a licorice medicinal material to ensure that the granularity of the medicinal powder is all passed through a standard sieve of 60 meshes;
(2) primary extraction: collecting 1kg of the Glycyrrhrizae radix powder, adding 8L of ethanol, stirring, adding appropriate amount of 5M sulfuric acid-hydrochloric acid (V/V, 1:1), controlling pH of the mixed system to 2-4, stirring and extracting for 30 min, filtering, and collecting 1-stage extractive solution and residue respectively;
(3) second-fifth stage extraction: extracting the medicinal materials by four stages (5 stages) by the same method, and collecting the extractive solutions and residues;
(4) and (3) separating and purifying glycyrrhizic acid: the 1-grade extracting solution is used for separating and purifying glycyrrhizic acid, filtrate obtained after the glycyrrhizic acid in the 1-grade extracting solution is purified is subjected to solvent recovery, and the other grades of extracting solutions are used for extracting a new batch of licorice medicinal materials.
Example 4
(1) Crushing and crushing a licorice medicinal material to ensure that the granularity of the medicinal powder is all passed through a standard sieve of 60 meshes;
(2) primary extraction: mixing 1kg of the Glycyrrhrizae radix powder with 8L of the mixture of the 2-5 grade extractive solution of example 3, stirring, adding appropriate amount of 5M sulfuric acid-hydrochloric acid (V/V, 1:1), controlling pH of the mixture system to 2-4, stirring and extracting for 30 min, filtering, and collecting the 1 grade extractive solution and residue respectively;
(3) second-fifth stage extraction: extracting the medicinal materials by four stages (5 stages) by the same method, and collecting the extractive solutions and residues;
(4) and (3) separating and purifying glycyrrhizic acid: the 1-grade extracting solution is used for separating and purifying glycyrrhizic acid, filtrate obtained after the glycyrrhizic acid in the 1-grade extracting solution is purified is subjected to solvent recovery, and the other grades of extracting solutions are used for extracting a new batch of licorice medicinal materials.
The present invention further provides statistics on the extraction rate of glycyrrhizic acid in examples 1-4 above.
Example 1 and example 2 Glycyrrhetinic acid extraction statistics
The detection method comprises the following steps: high performance liquid chromatography
(1) Chromatographic conditions and system applicability test: octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile-0.01 mol/L phosphoric acid solution (38: 62) is used as a mobile phase; the detection wavelength is 252 nm; the flow rate is 1 ml/min; sample introduction amount: 10 mu L of the solution; the theoretical plate number is not lower than 2000 calculated according to the ammonium glycyrrhizinate peak, and the separation degree of the ammonium glycyrrhizinate peak and the internal standard substance peak is in accordance with the requirement.
(2) Preparation of internal standard solution: taking about 70mg of n-butyl p-hydroxybenzoate, accurately weighing, placing in a 100ml measuring flask, dissolving with diluted ethanol, diluting to scale, and shaking.
(3) Preparation of control solutions: precisely weighing about 20mg of monoammonium glycyrrhizinate as reference substance, placing into a 100ml measuring flask, adding diluted ethanol for dissolving, precisely adding 5ml of internal standard solution, diluting with diluted ethanol to scale, and shaking up.
(4) Sample solution preparation
Primary extracting solution: precisely transferring 2mL to 100mL volumetric flasks, precisely adding 5mL of internal standard solution, and diluting with diluted ethanol to a scale;
second-sixth stage extract: precisely transferring 5mL to 100mL volumetric flasks respectively, precisely adding 5mL of internal standard solution, and diluting with diluted ethanol to a scale;
the glycyrrhizic acid concentration and extraction rate of each stage of the extract liquid in example 1 and example 2 were counted, and the data are shown in table 1.
Table 1 glycyrrhizic acid extraction statistics of example 1 and example 2
As shown in the table above, after the licorice medicinal material is extracted by the method for 6 grades, the extraction of the glycyrrhizic acid is basically complete, the glycyrrhizic acid content in the dregs of a decoction is lower than 1%, and the starch, fat and other nutritional ingredients in the dregs of a decoction are well protected, so that a better basis is provided for the subsequent application of the licorice dregs of a decoction.
(II) Glycyrrhetinic acid extraction statistics of examples 3 and 4
The detection method comprises the following steps: high performance liquid chromatography
(1) Chromatographic conditions and system applicability test: octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile-0.01 mol/L phosphoric acid solution (38: 62) as mobile phase; the detection wavelength was 252 nm. The theoretical plate number is not lower than 2000 calculated according to the ammonium glycyrrhizinate peak, and the separation degree of the ammonium glycyrrhizinate peak and the internal standard substance peak is in accordance with the requirement.
(2) Preparation of internal standard solution: taking about 70mg of n-butyl p-hydroxybenzoate, accurately weighing, placing in a 100ml measuring flask, dissolving with diluted ethanol, diluting to scale, and shaking.
(3) Preparation of control solutions: precisely weighing about 20mg of monoammonium glycyrrhizinate as reference substance, placing into a 100ml measuring flask, adding diluted ethanol for dissolving, precisely adding 5ml of internal standard solution, diluting with diluted ethanol to scale, and shaking up.
(4) Sample solution preparation
Primary extracting solution: precisely transferring 2mL to 100mL volumetric flasks, precisely adding 5mL of internal standard solution, and diluting with diluted ethanol to a scale;
second-fifth grade extract: precisely transferring 5mL to 100mL volumetric flasks respectively, precisely adding 5mL of internal standard solution, and diluting with diluted ethanol to a scale;
the glycyrrhizic acid concentration and extraction rate of each stage of the extract liquid in example 3 and example 4 were counted, and the data are shown in table 2.
Table 2 example 3 and example 4 glycyrrhizic acid extraction statistics
As shown in the table above, after the licorice medicinal material is extracted by the method for 5 grades, the extraction of the glycyrrhizic acid is basically complete, the glycyrrhizic acid content in the dregs of a decoction is lower than 1%, and the starch, fat and other nutritional ingredients in the dregs of a decoction are well protected, so that a better basis is provided for the subsequent application of the licorice dregs of a decoction.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (9)
1. A method for extracting a glycyrrhizic acid crude product from liquorice is characterized by comprising the following steps:
crushing liquorice: crushing a licorice medicinal material into licorice medicinal powder, and controlling the granularity of the licorice medicinal powder to be 30-200 meshes; and
primary extraction: mixing organic solvent and water to obtain first solvent, and mixing with the Glycyrrhrizae radix powder in a ratio of (2-20): 1(V/W), stirring, adding a pH regulator, regulating the pH value, stirring and extracting for 0.5-3 hours, filtering, and collecting a primary extracting solution and dregs; the primary extracting solution is the glycyrrhizic acid crude product.
2. A method for extracting a glycyrrhizic acid crude product from liquorice is characterized by comprising the following steps:
crushing liquorice: crushing a licorice medicinal material into licorice medicinal powder, and controlling the granularity of the licorice medicinal powder to be 30-200 meshes;
primary extraction: mixing organic solvent and water to obtain first solvent, and mixing with the Glycyrrhrizae radix powder in a ratio of (2-20): 1(V/W), stirring, adding a pH regulator, regulating the pH value, stirring and extracting for 0.5-3 hours, filtering, and collecting a first-stage extracting solution and first-stage medicine residues; and
and (3) K-level extraction: mixing the first solvent and the residue obtained in the previous stage of extraction with a solvent of (2-20): 1(V/W), stirring, adding a pH regulator, regulating the pH value, stirring and extracting for 0.5-3 hours, filtering, and collecting a K-grade extracting solution and K-grade medicine dregs; and
starting from K-2, executing the K-level extraction till N-level extraction, thereby completing a complete round of extraction, wherein N is more than or equal to 2 and less than or equal to 8,
wherein the primary extracting solution is a glycyrrhizic acid crude product.
3. The method of claim 2, wherein the first solvent further comprises the first extraction liquid of each stage of the previous extraction process except the first extraction liquid during each extraction process.
4. The method for extracting the crude glycyrrhizic acid from licorice root as claimed in claim 2, wherein in said primary extraction step, said organic solvent is at least one selected from the group consisting of alcohols, alcohol derivatives and ketones.
5. The method for extracting crude glycyrrhizic acid from licorice root as claimed in claim 2, wherein in said primary extraction step, said organic solvent is at least one selected from the group consisting of methanol, ethanol, ethyl acetate and acetone.
6. The method for extracting the crude glycyrrhizic acid from licorice root as claimed in claim 2, wherein in the primary extraction step, the water accounts for 0-30% by volume of the first solvent.
7. The method for purifying glycyrrhetate according to claim 2, wherein the pH regulator is at least one selected from the group consisting of: h2SO4、HCl、H3PO4Polyphosphoric acid, CH3COOH, citric acid, oxalic acid, cation exchange resin, a buffer system with pH less than or equal to 2, and solutions with different concentrations prepared from at least one of the substances.
8. The method for extracting crude glycyrrhizic acid from licorice root as claimed in claim 2, wherein in said first extraction step and said K extraction step, the pH value is adjusted to be not more than 4.
9. The method for extracting crude glycyrrhizic acid from licorice root as claimed in claim 2, wherein in said first extraction step and said K extraction step, the pH is adjusted to 0.5-4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911414312.6A CN111100181A (en) | 2019-12-31 | 2019-12-31 | Method for extracting glycyrrhizic acid crude product from liquorice |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911414312.6A CN111100181A (en) | 2019-12-31 | 2019-12-31 | Method for extracting glycyrrhizic acid crude product from liquorice |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111100181A true CN111100181A (en) | 2020-05-05 |
Family
ID=70425594
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911414312.6A Pending CN111100181A (en) | 2019-12-31 | 2019-12-31 | Method for extracting glycyrrhizic acid crude product from liquorice |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111100181A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112723636A (en) * | 2020-12-16 | 2021-04-30 | 洛阳蓝斯利科技有限公司 | Method for treating liquorice acidified wastewater and recovering and separating effective components in liquorice acidified wastewater |
| WO2021134407A1 (en) * | 2019-12-31 | 2021-07-08 | 中国医药健康产业股份有限公司 | Method for extracting crude product of glycyrrhizic acid and glycyrrhizic flavone from licorice and purifying to obtain glycyrrhizinate |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1524870A (en) * | 2003-02-27 | 2004-09-01 | 中国科学院过程工程研究所 | Method for extracting glycerrhizic acid from licorice |
| CN102304165A (en) * | 2011-07-12 | 2012-01-04 | 北京服装学院 | Method for extracting and purifying glycyrrhizic acid by ion-exchange fibers |
| CN103159809A (en) * | 2013-03-25 | 2013-06-19 | 宁夏紫荆花制药有限公司 | Preparation method of high-purity glycyrrhizic acid |
| CN103965152A (en) * | 2013-01-25 | 2014-08-06 | 武汉普赛特膜技术循环利用有限公司 | Extraction and preparation method for licorice effective ingredients |
| CN105061525A (en) * | 2015-07-17 | 2015-11-18 | 江苏天晟药业有限公司 | Preparation method of mono-ammonium glycyrrhizinate |
| CN105541957A (en) * | 2016-03-04 | 2016-05-04 | 脱德明 | Extraction method for increasing content of glycyrrhizic acid in leftover materials of liquorice |
| CN106279345A (en) * | 2016-08-15 | 2017-01-04 | 晨光生物科技集团股份有限公司 | A kind of industrialized preparing process of thick glycyrrhizic acid |
| CN106478761A (en) * | 2016-08-30 | 2017-03-08 | 青海省青海湖药业有限公司 | A kind of preparation method of mono-ammonium glycyrrhizinate |
| CN110156865A (en) * | 2019-06-20 | 2019-08-23 | 邵阳学院 | A kind of green method extracting glycyrrhizic acid inclusion compound from Radix Glycyrrhizae |
| CN110452282A (en) * | 2019-09-23 | 2019-11-15 | 山东花物堂生物科技有限公司 | A kind of Radix Glycyrrhizae acid extraction and purification process |
-
2019
- 2019-12-31 CN CN201911414312.6A patent/CN111100181A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1524870A (en) * | 2003-02-27 | 2004-09-01 | 中国科学院过程工程研究所 | Method for extracting glycerrhizic acid from licorice |
| CN102304165A (en) * | 2011-07-12 | 2012-01-04 | 北京服装学院 | Method for extracting and purifying glycyrrhizic acid by ion-exchange fibers |
| CN103965152A (en) * | 2013-01-25 | 2014-08-06 | 武汉普赛特膜技术循环利用有限公司 | Extraction and preparation method for licorice effective ingredients |
| CN103159809A (en) * | 2013-03-25 | 2013-06-19 | 宁夏紫荆花制药有限公司 | Preparation method of high-purity glycyrrhizic acid |
| CN105061525A (en) * | 2015-07-17 | 2015-11-18 | 江苏天晟药业有限公司 | Preparation method of mono-ammonium glycyrrhizinate |
| CN105541957A (en) * | 2016-03-04 | 2016-05-04 | 脱德明 | Extraction method for increasing content of glycyrrhizic acid in leftover materials of liquorice |
| CN106279345A (en) * | 2016-08-15 | 2017-01-04 | 晨光生物科技集团股份有限公司 | A kind of industrialized preparing process of thick glycyrrhizic acid |
| CN106478761A (en) * | 2016-08-30 | 2017-03-08 | 青海省青海湖药业有限公司 | A kind of preparation method of mono-ammonium glycyrrhizinate |
| CN110156865A (en) * | 2019-06-20 | 2019-08-23 | 邵阳学院 | A kind of green method extracting glycyrrhizic acid inclusion compound from Radix Glycyrrhizae |
| CN110452282A (en) * | 2019-09-23 | 2019-11-15 | 山东花物堂生物科技有限公司 | A kind of Radix Glycyrrhizae acid extraction and purification process |
Non-Patent Citations (6)
| Title |
|---|
| 佟连生 等: "从甘草酸粗品制取甘草酸单铵盐", 《黑龙江医药化学》 * |
| 沙世炎等: "《中草药有效成分分析法 上》", 31 March 1982, 人民卫生出版社 * |
| 王巧娥 等: "《甘草深加工技术》", 31 January 2011, 中国轻工业出版社 * |
| 王巧娥: "甘草有效成分的新型提取技术及高速逆流色谱分离方法研究", 《中国优秀博硕士学位论文全文数据库 (博士)》 * |
| 邓保炜: "从甘草酸粗品制取甘草酸单铵盐", 《中国医药工业杂志》 * |
| 阚微娜: "微波辅助提取甘草中有效成分的研究及甘草的综合利用", 《中国优秀硕士学位论文全文数据库 医药卫生科技辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021134407A1 (en) * | 2019-12-31 | 2021-07-08 | 中国医药健康产业股份有限公司 | Method for extracting crude product of glycyrrhizic acid and glycyrrhizic flavone from licorice and purifying to obtain glycyrrhizinate |
| CN112723636A (en) * | 2020-12-16 | 2021-04-30 | 洛阳蓝斯利科技有限公司 | Method for treating liquorice acidified wastewater and recovering and separating effective components in liquorice acidified wastewater |
| CN112723636B (en) * | 2020-12-16 | 2022-11-22 | 洛阳蓝斯利科技有限公司 | Method for treating liquorice acidified wastewater and recovering and separating effective components in liquorice acidified wastewater |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109568389B (en) | Preparation method of high-purity cannabinol extract | |
| CN106892949B (en) | A method of extracting separation glycyrrhizic acid, glycyrrhiza total flavonoid simultaneously based on continuous chromatography technology | |
| CN102093456B (en) | Method for extracting astragaloside IV from astragalus | |
| CN111100181A (en) | Method for extracting glycyrrhizic acid crude product from liquorice | |
| CN101322758A (en) | Method for producing spina date seed extract using complex enzyme | |
| CN111018942B (en) | Preparation method of monovalent glycyrrhizinate | |
| CN102050851A (en) | Liquiritin and preparation method thereof | |
| CN111072731B (en) | Method for purifying and obtaining glycyrrhetate from liquorice | |
| CN104711301A (en) | Icaritin preparation method | |
| CN110934903A (en) | Method for extracting licoflavone from Glycyrrhrizae radix | |
| CN103385913A (en) | Radix Astragali extract and its preparation method and preparation | |
| CN110437151B (en) | Method for extracting norglaucine and glaucine from Mengolian medicinal herb black-bone leaves | |
| CN103156897B (en) | Method for removing pesticide residue dichloro-diphenyl trichloroethane (DDT) and benzene hexachloride from American ginseng extract | |
| CN101948392A (en) | Preparation method of hordenine | |
| CN103588745B (en) | A kind of method of Extraction and separation not this Kelin from Coleus forskohlii Briq. | |
| CN101205247B (en) | Method for preparing panaxoside monomer Re,Rh1,Rh2,Rg2,Rg3 by using ginseng stem and leaves | |
| CN101284861A (en) | Triterpenoid saponin compounds, preparation method and use | |
| CN104072626A (en) | Preparation method for clematichinenoside | |
| CN114931597A (en) | Preparation method of pulsatilla chinensis extract based on anti-inflammatory activity | |
| CN103330738B (en) | Method for synchronously separating effective components in liquorice | |
| CN107459548B (en) | A method of extraction prepares Balaenoptera borealis Lesson element from dioecious balanophora herb | |
| CN106831936A (en) | The method that liquid phase method prepares tanshinone IIA and dihydrotanshinone I is prepared using middle high-pressure | |
| CN105348338A (en) | Method for extracting and separating paederosidic acid from Saprosma merrillii Lo | |
| CN1869059B (en) | Method of preparing ginseng saponine monomer from ginseng leaf | |
| CN1869058B (en) | Method of preparing trialcohol group ginseng saponine and bialcohol group ginseng saponine from notoginseng |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200505 |
|
| RJ01 | Rejection of invention patent application after publication |