CN118026830A - Preparation method and application of licochalcone A - Google Patents
Preparation method and application of licochalcone A Download PDFInfo
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- CN118026830A CN118026830A CN202311806860.XA CN202311806860A CN118026830A CN 118026830 A CN118026830 A CN 118026830A CN 202311806860 A CN202311806860 A CN 202311806860A CN 118026830 A CN118026830 A CN 118026830A
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- KAZSKMJFUPEHHW-UHFFFAOYSA-N (2E)-3-[5-(1,1-dimethyl-2-propenyl)-4-hydroxy-2-methoxyphenyl]-1-(4-hdyroxyphenyl)-2-propen-1-one Natural products COC1=CC(O)=C(C(C)(C)C=C)C=C1C=CC(=O)C1=CC=C(O)C=C1 KAZSKMJFUPEHHW-UHFFFAOYSA-N 0.000 title claims abstract description 38
- IUCVKTHEUWACFB-UHFFFAOYSA-N Licochalcone A Natural products COC1=CC=C(C(C)(C)C=C)C=C1C=CC(=O)C1=CC=C(O)C=C1 IUCVKTHEUWACFB-UHFFFAOYSA-N 0.000 title claims abstract description 38
- KAZSKMJFUPEHHW-DHZHZOJOSA-N Licochalcone A Chemical compound COC1=CC(O)=C(C(C)(C)C=C)C=C1\C=C\C(=O)C1=CC=C(O)C=C1 KAZSKMJFUPEHHW-DHZHZOJOSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 33
- 238000000605 extraction Methods 0.000 claims abstract description 31
- 238000000926 separation method Methods 0.000 claims abstract description 14
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 80
- 239000000284 extract Substances 0.000 claims description 28
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 26
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 22
- 239000011347 resin Substances 0.000 claims description 17
- 229920005989 resin Polymers 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 239000000741 silica gel Substances 0.000 claims description 16
- 229910002027 silica gel Inorganic materials 0.000 claims description 16
- 235000006200 Glycyrrhiza glabra Nutrition 0.000 claims description 15
- 238000004108 freeze drying Methods 0.000 claims description 15
- 241000202807 Glycyrrhiza Species 0.000 claims description 14
- 238000011068 loading method Methods 0.000 claims description 14
- 235000001453 Glycyrrhiza echinata Nutrition 0.000 claims description 13
- 235000017382 Glycyrrhiza lepidota Nutrition 0.000 claims description 13
- 229940010454 licorice Drugs 0.000 claims description 13
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 239000003208 petroleum Substances 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 11
- 239000002024 ethyl acetate extract Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 239000002893 slag Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 claims description 6
- 230000008025 crystallization Effects 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- 239000003480 eluent Substances 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 5
- 239000007791 liquid phase Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- WGLUMOCWFMKWIL-UHFFFAOYSA-N dichloromethane;methanol Chemical group OC.ClCCl WGLUMOCWFMKWIL-UHFFFAOYSA-N 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- KDCIHNCMPUBDKT-UHFFFAOYSA-N hexane;propan-2-one Chemical compound CC(C)=O.CCCCCC KDCIHNCMPUBDKT-UHFFFAOYSA-N 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000004134 energy conservation Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 5
- 238000010992 reflux Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 244000303040 Glycyrrhiza glabra Species 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229930003935 flavonoid Natural products 0.000 description 2
- 235000017173 flavonoids Nutrition 0.000 description 2
- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 235000011477 liquorice Nutrition 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 241001278898 Glycyrrhiza inflata Species 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000002481 ethanol extraction Methods 0.000 description 1
- -1 flavonoid compound Chemical class 0.000 description 1
- 150000002215 flavonoids Chemical group 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000010898 silica gel chromatography Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of plant extraction and separation, and particularly relates to a preparation method and application of licochalcone A, wherein the preparation method comprises the following steps: s1, extracting; s2, extracting; s3, chromatography; s4, crystallizing. Compared with the prior art, the invention has the beneficial effects that: the invention provides a novel method for preparing licochalcone A with high purity and high yield, which has the advantages of stable process, simple operation, energy conservation and environmental protection, high content of the obtained product and high yield, and can realize large-scale generation.
Description
Technical Field
The invention belongs to the technical field of plant extraction and separation, and particularly relates to a preparation method and application of licochalcone A.
Background
Licochalcone A (Licochalcone A) is a flavonoid compound separated and purified from Glycyrrhiza plant, has molecular formula of C 21H22O4 and molecular weight of 338.4, and is in orange powder state at normal temperature, insoluble in water, and soluble in organic solvent and alkaline solution.
Licochalcone A is obtained by extracting and separating Saitoh and Shibata of Japanese scholars in Xinjiang in 1975 at the earliest time, and the chemical structure of licochalcone A is proved to be a specific component of G.Inflata B at., and the molecular structure of licochalcone A has higher flexibility. Modern pharmacological research shows that licochalcone A has antioxidant, antitumor, antiinflammatory, antibacterial, immunity promoting and other activities, and has wide application in skin care, food and medicine industry.
Because the content of licochalcone A in liquorice is extremely low, the process for obtaining the licochalcone A with high purity is extremely complex, the cost is high, and the licochalcone A sold in the market at present is only a licochalcone A crude product with different content. At present, licochalcone A is mainly extracted from Xinjiang licorice, mainly comprises extraction methods such as heating reflux, soaking, ultrasonic assistance, microwave assistance and the like, and the separation and purification method comprises extraction, perforation adsorption resin elution, various chromatographic methods, polyamide chromatographic methods, silica gel column chromatography and the like, or the combination of a plurality of separation methods. The methods have the defects of complex operation process, high equipment requirement, high solvent consumption, more generated wastes, long period, high cost and the like, are not suitable for industrial mass production, and the yield of the method cannot meet the market demand.
The invention provides a novel preparation method of licochalcone A, which has the characteristics of stable process, simple operation, high finished product content and capability of realizing large-scale production.
Disclosure of Invention
The invention aims to solve the problems and provides a preparation method of licochalcone A, which has the characteristics of stable process, simple operation, high finished product content and capability of realizing large-scale production.
In a first aspect of the present invention, there is provided a method for preparing licochalcone a, comprising the steps of:
S1, extracting: weighing the dried licorice residue, adding into 5-15 times of extractant by weight of the licorice residue, extracting to obtain extract, concentrating to obtain extract, recovering extractant, repeating the above extraction steps for 2-4 times, and mixing the extracts;
S2, extraction: dissolving the extract obtained in the step S1 with water with the weight of 2-6 times of that of the extract, then sequentially extracting with petroleum ether and ethyl acetate to obtain petroleum ether and ethyl acetate extract, collecting ethyl acetate extract, concentrating the extract into paste, and freeze-drying to obtain a sample A;
S3, chromatography: a, a; coarse separation of macroporous resin: dissolving ethyl acetate part with 15-25% ethanol 2-4 times of ethyl acetate part weight, loading in wet method, separating with macroporous resin, eluting with 75-85% ethanol, concentrating into paste with column volume of 5-7 column volumes, and lyophilizing to obtain sample B; b: separating by a silica gel column: dissolving the dried product obtained in the step a with ethanol, adding 1.2-1.8 times of silica gel, stirring uniformly, drying, grinding into powder, loading in a dry method, eluting to obtain a fraction, concentrating, and freeze-drying to obtain a sample C;
wherein the extract is an extract, the low polar compound is removed by petroleum ether extraction, the target compound belongs to a medium polar compound, and the target compound is positioned at the ethyl acetate position.
S4, crystallization: sample C was dissolved by adding 55-65% ethanol, ethanol: sample = 4-8:1 (weight ratio), dissolving at 45-55deg.C, cooling to 0-5deg.C at 2-4deg.C/min, standing at 2-8deg.C, filtering to obtain filter cake, and drying to obtain yellowish powder.
The extraction rate of the preparation method is more than 90%, and the purity is more than 98% through liquid phase detection.
Preferably, in step S3 chromatography, a; coarse separation of macroporous resin: dissolving ethyl acetate part in 20% ethanol 2-4 times of ethyl acetate part weight, filtering to obtain filtrate if insoluble substance is present; wet loading, macroporous resin separation, eluting with 80% ethanol, concentrating into paste with column volume of 6 column volumes, and freeze drying to obtain sample B; b: separating by a silica gel column: dissolving the dried product obtained in the step a with ethanol, adding 1.5 times of 200-300 mesh silica gel, stirring uniformly, drying, grinding into powder, loading in a dry method, eluting to obtain a fraction, concentrating, and freeze-drying to obtain a sample C.
More specifically, S4 crystallization: sample C was dissolved by adding 60% ethanol, ethanol: sample = 4-8:1 (weight ratio), dissolving at 50deg.C, cooling to 5deg.C at 2-4deg.C/min, and standing at 2-8deg.C for 48 hr.
The technical scheme of the invention is characterized in that:
Further, in the step S1, the extracting agent is an ethanol solution with a concentration of 70-95%, preferably an ethanol solution with a concentration of 80-95%.
And in the step S1, the specific steps of extraction may be: reflux-extracting at 70-85deg.C for 1-4 hr to obtain extractive solution. And the preferable conditions are as follows: firstly, adding the dried licorice slag into an extractant with the weight of 8-12 times that of the licorice slag, reflux-extracting for 2 hours at the temperature of 70-85 ℃, repeating for 3 times, and combining extractum. In order to ensure dissolution and reflux, extraction is more sufficient, and a temperature of 70-85 ℃ is adopted. The sample is flavonoid, can not be extracted by water alone, can fully extract the required substances by using a high proportion of solvent, can remove materials such as protein, polysaccharide and the like, and has lower ethanol toxicity compared with other organic solvents.
The specific step of extraction in step S1 may also be: soaking at normal temperature for 48h to obtain extractive solution, which is mainly used for ethanol extraction.
Further, in the step S3 of the above method, the sample is enriched by coarsely separating the macroporous resin column having any one of the types AB-8, D-101, XAD-16, HPD-100 and HPD-400, preferably HPD-400 or D-101; the silica gel column eluent was dichloromethane-methanol or n-hexane-acetone, the former was used, dichloromethane: methanol (volume ratio) =6: 1, using the latter, n-hexane: acetone (volume ratio) =4: 1.
The second aspect of the invention provides an application of the preparation method of licochalcone A in improving the extraction rate and purity of licochalcone A.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a novel method for preparing licochalcone A with high purity and high yield, which has the advantages of stable process, simple operation, energy conservation and environmental protection, high content of the obtained product and high yield, and can realize large-scale generation.
In the prior art, a polyacetamide column is used for extracting and preparing licochalcone A, and other component structures in liquorice also contain hydroxyl groups, so that not only can a good separation effect not be achieved, but also a large amount of compounds are adsorbed on the column and are difficult to elute, the yield is low, and the column is damaged (the polyacetamide column can be used for multiple times), so that the invention does not use the polyacetamide column; the preparation process does not use a first reagent, does not use a second reagent in the last step, greatly reduces the use of high-toxicity solvents, and has the yield of more than 90 percent.
Detailed Description
The present invention will be described in detail with reference to the following examples for better understanding of the present invention, but the present invention is not limited to the following specific examples.
Example 1:
S1: extraction of
Weighing 10kg of licorice residue, adding into 80kg of 80% ethanol, reflux-extracting at 85 ℃ for 2h to obtain an extract, concentrating to obtain an extract, recycling the extractant, repeating the extraction steps for 3 times, and combining the extracts;
S2: extraction
Dissolving the extract obtained in the step S1 with 3 times of water, then sequentially extracting with petroleum ether and ethyl acetate to obtain petroleum ether and ethyl acetate extract, collecting ethyl acetate extract, concentrating the extract into paste, and freeze-drying to obtain a sample A;
S3: chromatography
A, a; coarse separation of macroporous resin: dissolving the sample A in 2 times of 20% ethanol, loading by wet method, separating with HPD-400 macroporous resin, eluting with 80% ethanol, collecting eluate with column volume of 6 column volumes, concentrating into paste, and lyophilizing to obtain sample B;
b: separating by a silica gel column: dissolving a sample B in ethanol, adding 1.5 times of silica gel, uniformly stirring, drying and grinding into powder, loading in a dry method, and obtaining dichloromethane by using dichloromethane-methanol as eluent: methanol=6: 1, concentrating, freeze-drying to obtain a sample C;
S4: crystallization
Adding 5 times of 60% ethanol into the sample C, dissolving at 50deg.C, cooling to 5deg.C at 2-4deg.C/min, standing at 2-8deg.C for 48 hr, filtering to obtain filter cake, and drying to obtain 35.9g of light yellow licochalcone A product with extraction rate of 90% and purity of 98.05% by liquid phase detection. The extraction rate is the weight of the finished product divided by the solid content of licochalcone A in licorice slag, and is the same as follows.
Example 2:
S1: extraction of
Weighing 10kg of licorice slag, adding into 90kg of 90% ethanol, carrying out reflux extraction for 2h at 80 ℃ to obtain an extracting solution, concentrating to obtain an extract, recycling an extracting agent, repeating the extracting steps for 3 times, and merging the extracts;
S2: extraction
Dissolving the extract obtained in the step S1 with 3 times of water, then sequentially extracting with petroleum ether and ethyl acetate to obtain petroleum ether and ethyl acetate extract, collecting ethyl acetate extract, concentrating the extract into paste, and freeze-drying to obtain a sample A;
S3: chromatography
A, a; coarse separation of macroporous resin: dissolving the sample A in 2 times of 20% ethanol, loading by wet method, separating with HPD-400 macroporous resin, eluting with 80% ethanol, collecting eluate with column volume of 6 column volumes, concentrating into paste, and lyophilizing to obtain sample B;
b: separating by a silica gel column: dissolving a sample B in ethanol, adding 1.5 times of silica gel, uniformly stirring, drying and grinding into powder, loading in a dry method, and obtaining dichloromethane by using dichloromethane-methanol as eluent: methanol=6: 1, concentrating, freeze-drying to obtain a sample C;
S4: crystallization
Adding 5 times of 60% ethanol into the sample C, dissolving at 50deg.C, cooling to 5deg.C at 2-4deg.C/min, standing at 2-8deg.C for 48 hr, filtering to obtain filter cake, and drying to obtain 36.7g of light yellow licochalcone A product with extraction rate of 92% and purity of 98.72% by liquid phase detection.
Example 3:
S1: extraction of
Weighing 10kg of licorice slag, adding into 100kg of 95% ethanol, carrying out reflux extraction at 78 ℃ for 2 hours to obtain an extracting solution, concentrating into an extract, recycling an extracting agent, repeating the extracting steps for 3 times, and merging the extracts;
S2: extraction
Dissolving the extract obtained in the step S1 with 3 times of water, then sequentially extracting with petroleum ether and ethyl acetate to obtain petroleum ether and ethyl acetate extract, collecting ethyl acetate extract, concentrating the extract into paste, and freeze-drying to obtain a sample A;
S3: chromatography
A, a; coarse separation of macroporous resin: dissolving the sample A in 2 times of 20% ethanol, loading by a wet method, separating by D101 macroporous resin, eluting with 80% ethanol and 6 column volumes, concentrating into paste, and freeze drying to obtain a sample B;
b: separating by a silica gel column: dissolving a sample B in ethanol, adding 1.5 times of silica gel, uniformly stirring, drying and grinding into powder, loading by a dry method, and obtaining n-hexane by using n-hexane-acetone as eluent: acetone=4: 1, concentrating, freeze-drying to obtain a sample C;
S4: crystallization
Adding 5 times of 60% ethanol into the sample C, dissolving at 50deg.C, cooling to 5deg.C at 2-4deg.C/min, standing at 2-8deg.C for 48 hr, filtering to obtain filter cake, and drying to obtain 36.9g of light yellow licochalcone A product with an extraction rate of 93% and a purity of 98.26% by liquid phase detection.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be appreciated by persons skilled in the art that the above embodiments are not intended to limit the invention in any way, and that all technical solutions obtained by means of equivalent substitutions or equivalent transformations fall within the scope of the invention.
Claims (10)
1. The preparation method of licochalcone A is characterized by comprising the following steps:
S1, extracting: weighing the dried licorice residue, adding into 5-15 times of extractant by weight of the licorice residue, extracting to obtain extract, concentrating to obtain extract, recovering extractant, repeating the above extraction steps for 2-4 times, and mixing the extracts;
S2, extraction: dissolving the extract obtained in the step S1 with water with the weight of 2-6 times of that of the extract, then sequentially extracting with petroleum ether and ethyl acetate to obtain petroleum ether and ethyl acetate extract, collecting ethyl acetate extract, concentrating the extract into paste, and freeze-drying to obtain a sample A;
S3, chromatography: a, a; coarse separation of macroporous resin: dissolving ethyl acetate part with 15-25% ethanol 2-4 times of ethyl acetate part weight, loading in wet method, separating with macroporous resin, eluting with 75-85% ethanol, concentrating into paste with column volume of 5-7 column volumes, and lyophilizing to obtain sample B; b: separating by a silica gel column: dissolving the dried product obtained in the step a with ethanol, adding 1.2-1.8 times of silica gel, stirring uniformly, drying, grinding into powder, loading in a dry method, eluting to obtain a fraction, concentrating, and freeze-drying to obtain a sample C; s4, crystallization: sample C was dissolved by adding 55-65% ethanol, ethanol: sample = 4-8:1 (weight ratio), dissolving at 45-55deg.C, cooling to 0-5deg.C at 2-4deg.C/min, standing at 2-8deg.C, filtering to obtain filter cake, and drying to obtain yellowish powder.
2. The method for preparing licochalcone A according to claim 1, wherein the extraction rate is more than 90%, and the purity is more than 98% through liquid phase detection.
3. The method for preparing licochalcone a according to claim 1, wherein in step S3 chromatography, a; coarse separation of macroporous resin: dissolving ethyl acetate part in 20% ethanol 2-4 times of ethyl acetate part weight, filtering to obtain filtrate if insoluble substance is present; wet loading, macroporous resin separation, eluting with 80% ethanol, concentrating into paste with column volume of 6 column volumes, and freeze drying to obtain sample B; b: separating by a silica gel column: dissolving the dried product obtained in the step a with ethanol, adding 1.5 times of 200-300 mesh silica gel, stirring uniformly, drying, grinding into powder, loading in a dry method, eluting to obtain a fraction, concentrating, and freeze-drying to obtain a sample C.
4. The method for preparing licochalcone a according to claim 1, wherein S4 is devitrified: sample C was dissolved by adding 60% ethanol, ethanol: sample = 4-8:1 (weight ratio), dissolving at 50deg.C, cooling to 5deg.C at 2-4deg.C/min, and standing at 2-8deg.C for 48 hr.
5. The method for preparing licochalcone a according to claim 1, wherein in step S1, the extractant is 70-95% ethanol solution or 80-95% ethanol solution.
6. The preparation method of licochalcone A according to claim 1, wherein the specific steps of S1 extraction are as follows: reflux-extracting at 70-85deg.C for 1-4 hr to obtain extractive solution; firstly, adding the dried licorice slag into an extractant with the weight of 8-12 times that of the licorice slag, reflux-extracting for 2 hours at the temperature of 70-85 ℃, repeating for 3 times, and combining extractum.
7. The method for preparing licochalcone a according to claim 1, wherein the specific step of S1 extraction comprises:
soaking at normal temperature for 48h to obtain extractive solution.
8. The method for preparing licochalcone a according to claim 1, wherein in step S3, the macroporous resin column is any one of AB-8, D-101, XAD-16, HPD-100 and HPD-400, preferably HPD-400 or D-101.
9. The method for preparing licochalcone a according to claim 1, wherein in the step S3, the silica gel column eluent is dichloromethane-methanol or n-hexane-acetone, and the volume ratio of dichloromethane: methanol=6: 1, volume ratio n-hexane: acetone=4: 1.
10. Use of the method for preparing licochalcone a according to any one of claims 1-9 for increasing the extraction yield and purity of licochalcone a.
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