CN111233964A - Method for extracting and refining betulin and betulinic acid in cortex Betulae Pendulae - Google Patents
Method for extracting and refining betulin and betulinic acid in cortex Betulae Pendulae Download PDFInfo
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- CN111233964A CN111233964A CN202010178242.5A CN202010178242A CN111233964A CN 111233964 A CN111233964 A CN 111233964A CN 202010178242 A CN202010178242 A CN 202010178242A CN 111233964 A CN111233964 A CN 111233964A
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- betulin
- extracting
- betulinic acid
- refining
- birch bark
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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
Abstract
The invention provides a method for extracting and refining betulin and betulinic acid in birch bark, and relates to the technical field of extracting betulin and betulinic acid. The method for extracting and refining betulin and betulinic acid in the birch bark comprises the following steps: s1, pulverizing cortex Betulae Pendulae with a pulverizing device, adding 80% ethanol, heating and stirring, extracting the stirred liquid for several times, mixing the extractive solutions, and removing residue. According to the method for extracting and refining the betulinic acid and the betulinic acid in the birch bark, in use, the organic matter can be effectively separated by the separator, meanwhile, the macroporous adsorption resin is adopted, so that the liquid can be better adsorbed, the purity of the betulinic acid and the betulinic acid is effectively improved, the liquid can be better used by washing and eluting with ethyl acetate, and the purity of the betulinic acid and the betulinic acid is effectively improved.
Description
Technical Field
The invention relates to the technical field of betulin and betulinic acid extraction, in particular to a method for extracting and refining betulin and betulinic acid from birch bark.
Background
Birch bark is also called Betula alba, Betula platyphylla, soft bark of Betula platyphylla of Betulaceae, or bark of Betula platyphylla in spring, or harvested tree, and contains chemical components such as betulin, betulinic acid, and betulin.
In recent years, people find that natural plant birch bark contains a large amount of betulin and betulinic acid, and because the source of the raw material of the birch bark is wide, the betulin and the betulinic acid are favored to be extracted from the natural plant birch bark, but the prior process of extracting the betulin and the betulinic acid has an excessively complex extraction mode, so the purity of the betulin and the betulinic acid can be greatly reduced in use.
Disclosure of Invention
The invention aims to provide a method for extracting and refining betulin and betulinic acid in birch bark, which can effectively solve the problems in the background technology.
In order to achieve the purpose, the invention is realized by the following technical scheme: the method for extracting and refining betulin and betulinic acid in the birch bark comprises the following steps:
s1, pulverizing cortex Betulae Pendulae with a pulverizing device, adding 80% ethanol, heating and stirring, extracting the stirred liquid for several times, mixing the extractive solutions, and removing residue.
S2, adsorbing and eluting the combined extracting solution through macroporous adsorption resin, recovering the solvent, and adding dichloromethane to dissolve the precipitated crystals.
S3, standing and filtering the dissolved extracting solution, and washing the extracting solution to be neutral by water to obtain a betulin crude extract.
S4, adding dilute acid and aqueous solution of bicarbonate into the crude betulin extract, washing with pure water, and collecting the upper layer insoluble powder.
S5, dissolving the powdery insoluble substances in methanol, precipitating crystals, filtering, washing and drying to obtain betulin crystals.
Further, after S5, the method further includes the following steps:
s6, dissolving the betulin crystals in acetone, stirring by a stirring device to dissolve the betulin crystals, and adding an oxidant to react;
s7, adding methanol to terminate the reaction, adding water, volatilizing acetone by using vacuum equipment, extracting the rest aqueous solution for three times by using a solvent, washing the extracted aqueous solution, separating an organic layer by using a separator, removing the solvent by using the vacuum equipment, and collecting residues;
s8, dissolving the residue in tetrahydrofuran, adding a reducing agent, stirring, adding dilute hydrochloric acid after stirring to terminate the reaction, concentrating the solution by using vacuum equipment, adding ethyl acetate, washing, and separating out organic matters by using a separator;
and S9, removing ethyl acetate by adopting vacuum equipment, collecting the residue, eluting the residue by using ethyl acetate, collecting an eluent, removing the solvent by adopting decompression equipment, and obtaining the betulinic acid by adopting vacuum drying equipment.
Further, according to the operation procedure in S1, the extraction method is one or more of an immersion method, a reflux extraction method, a percolation method, a decoction method, and a continuous extraction method.
Further, according to the operation of S2, the pH value of dichloromethane is 2.0-2.5.
Further, according to the operation in S6, the oxidizing agent is jones reagent, and the reaction time is 1 to 2 hours.
Further, the drying time of the vacuum drying apparatus will be 16 to 24 hours according to the operation procedure in S9.
The invention provides a method for extracting and refining betulin and betulinic acid in birch bark. The method has the following beneficial effects:
the method for extracting and refining the betulinic acid and the betulinic acid in the birch bark has the advantages that in use, the organic matter can be effectively separated by the separator, meanwhile, the macroporous adsorption resin is adopted, the liquid can be better adsorbed, the purity of the betulinic acid and the betulinic acid is effectively improved, the liquid can be better used by washing and washing with ethyl acetate, and meanwhile, in use, the extraction mode is simple, and the betulinic acid can be conveniently extracted.
Detailed Description
Example 1: the invention provides a technical scheme that: the method for extracting and refining betulin and betulinic acid in the birch bark comprises the following specific implementation steps:
the method comprises the following steps of 1, crushing the birch bark by using crushing equipment, adding 80% ethanol, heating and stirring, extracting stirred liquid for a plurality of times, combining extracting solutions, and removing residues, wherein the extracting method is one or more of a dipping method, a reflux extracting method, a percolation method, a decoction method and a continuous extracting method, and the extracting solution can be extracted and processed in use, so that the use is convenient.
And 2, adsorbing, eluting and recovering a solvent from the combined extracting solution through macroporous adsorption resin, adding dichloromethane into a precipitated crystal for dissolving, wherein the pH value of the dichloromethane is 2.0-2.5, and the extracting solution can be better adsorbed through the macroporous adsorption resin, so that the purity of the betulin is effectively improved, the pH value of the dichloromethane is 2.0-2.5, the adsorbed extracting solution is convenient to dissolve, and the use is convenient.
And 3, standing and filtering the dissolved extracting solution, and washing the extracting solution to be neutral by using water to obtain a crude betulin extract which is convenient for treating the dissolved extracting solution.
And 4, adding dilute acid and a bicarbonate water solution into the crude betulin extract, washing with pure water, collecting upper-layer powdery insoluble substances, dissolving the crude betulin extract with the dilute acid and the bicarbonate water, and washing with the pure water to collect powdery insoluble substances conveniently.
And 5, dissolving the powdery insoluble substances in methanol, separating out crystals, filtering, washing and drying to obtain betulin crystals, and treating the powdery insoluble substances to obtain the betulin crystals.
And 6, dissolving the betulin crystals in acetone, stirring by a stirring device to dissolve the betulin crystals, adding an oxidant which is an Jones reagent for reaction for 1-2 hours, adding acetone into the betulin crystals to dissolve the betulin crystals, adding the Jones reagent for reaction for 1-2 hours, and better enabling the dissolved solution to react completely.
And 7, adding methanol to terminate the reaction, adding water, volatilizing acetone by using vacuum equipment, extracting the rest aqueous solution for three times by using a solvent, washing the extracted aqueous solution, separating an organic layer by using a separator, removing the solvent by using the vacuum equipment, collecting residues, and using the vacuum equipment so as to volatilize the acetone and facilitate use.
And 8, dissolving the residue in tetrahydrofuran, adding a reducing agent, stirring, adding dilute hydrochloric acid after stirring to terminate the reaction, concentrating the solution by using vacuum equipment, adding ethyl acetate for washing, separating out organic matters by using a separator, adding a reducing agent into the residue to enable the residue to be better dissolved, concentrating by using the vacuum equipment, conveniently washing by using the ethyl acetate, and separating out the organic matters by using the separator after washing.
And 9, removing ethyl acetate by adopting vacuum equipment, collecting the residue, eluting the residue by using ethyl acetate, collecting an eluent, removing the solvent by adopting decompression equipment, and obtaining the betulinic acid by adopting vacuum drying equipment, wherein the drying time of the vacuum drying equipment is 16-24 hours, the residue can be collected after the ethyl acetate is removed by adopting the vacuum equipment, and the solvent can be removed by eluting the residue, collecting the eluent and decompressing the eluent, and the eluent is dried by adopting the vacuum drying equipment, so that the betulinic acid can be obtained.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications are all within the scope of the present invention.
Claims (6)
1. The method for extracting and refining betulin and betulinic acid in the birch bark is characterized by comprising the following steps:
s1, pulverizing cortex Betulae Pendulae with a pulverizing device, adding 80% ethanol, heating and stirring, extracting the stirred liquid for several times, mixing the extractive solutions, and removing residue;
s2, adsorbing, eluting and recovering the solvent from the combined extracting solution through macroporous adsorption resin, and adding dichloromethane to dissolve the precipitated crystals;
s3, standing and filtering the dissolved extracting solution, and washing the extracting solution to be neutral by water to obtain a betulin crude extract;
s4, adding dilute acid and aqueous solution of bicarbonate into the crude extract of betulin, washing with pure water, and collecting the upper layer of powdery insoluble substance;
s5, dissolving the powdery insoluble substances in methanol, precipitating crystals, filtering, washing and drying to obtain betulin crystals.
2. The method for extracting and refining betulin and betulinic acid from birch bark as claimed in claim 1, wherein after S5, the method further comprises the following steps:
s6, dissolving the betulin crystals in acetone, stirring by a stirring device to dissolve the betulin crystals, and adding an oxidant to react;
s7, adding methanol to terminate the reaction, adding water, volatilizing acetone by using vacuum equipment, extracting the rest aqueous solution for three times by using a solvent, washing the extracted aqueous solution, separating an organic layer by using a separator, removing the solvent by using the vacuum equipment, and collecting residues;
s8, dissolving the residue in tetrahydrofuran, adding a reducing agent, stirring, adding dilute hydrochloric acid after stirring to terminate the reaction, concentrating the solution by using vacuum equipment, adding ethyl acetate, washing, and separating out organic matters by using a separator;
and S9, removing ethyl acetate by adopting vacuum equipment, collecting the residue, eluting the residue by using ethyl acetate, collecting an eluent, removing the solvent by adopting decompression equipment, and obtaining the betulinic acid by adopting vacuum drying equipment.
3. The method for extracting and refining betulin and betulinic acid in birch bark according to claim 1, comprising the following steps: according to the operation steps in S1, the extraction method is one or more of an immersion method, a reflux extraction method, a percolation method, a decoction method and a continuous extraction method.
4. The method for extracting and refining betulin and betulinic acid in birch bark according to claim 1, comprising the following steps: according to the operation procedure in S2, the pH value of the dichloromethane is 2.0-2.5.
5. The method for extracting and refining betulin and betulinic acid in birch bark as claimed in claim 2, wherein the method comprises the following steps: the oxidant was jones reagent according to the procedure in S6, with a reaction time of 1-2 hours.
6. The method for extracting and refining betulin and betulinic acid in birch bark as claimed in claim 2, wherein the method comprises the following steps: the drying time of the vacuum drying apparatus according to the operation procedure in S9 was 16 to 24 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010178242.5A CN111233964A (en) | 2020-03-14 | 2020-03-14 | Method for extracting and refining betulin and betulinic acid in cortex Betulae Pendulae |
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| CN202010178242.5A CN111233964A (en) | 2020-03-14 | 2020-03-14 | Method for extracting and refining betulin and betulinic acid in cortex Betulae Pendulae |
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| CN111233964A true CN111233964A (en) | 2020-06-05 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113461769A (en) * | 2021-07-14 | 2021-10-01 | 西安金泰生物技术有限公司 | Preparation method of betulin |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1634972A (en) * | 2004-11-12 | 2005-07-06 | 张梅 | Process for extracting and purifying betulin and betulinic acid |
| CN101200486A (en) * | 2006-12-13 | 2008-06-18 | 上海睿智化学研究有限公司 | Method for abstracting and purifying betulin in birch bark |
| CN101328201A (en) * | 2008-07-29 | 2008-12-24 | 浙江大学 | Method for extracting betulin from birch bark |
| CN102093458A (en) * | 2010-12-20 | 2011-06-15 | 大兴安岭林格贝有机食品有限责任公司 | Method for enriching and purifying betulin in birch barks |
| CN102321143A (en) * | 2011-07-08 | 2012-01-18 | 浙江天草生物制品有限公司 | Method for preparing high-purity betulin |
| CN110092811A (en) * | 2019-06-04 | 2019-08-06 | 哈尔滨市泽尼康药业有限公司 | A kind of preparation method of betulin |
-
2020
- 2020-03-14 CN CN202010178242.5A patent/CN111233964A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1634972A (en) * | 2004-11-12 | 2005-07-06 | 张梅 | Process for extracting and purifying betulin and betulinic acid |
| CN101200486A (en) * | 2006-12-13 | 2008-06-18 | 上海睿智化学研究有限公司 | Method for abstracting and purifying betulin in birch bark |
| CN101328201A (en) * | 2008-07-29 | 2008-12-24 | 浙江大学 | Method for extracting betulin from birch bark |
| CN102093458A (en) * | 2010-12-20 | 2011-06-15 | 大兴安岭林格贝有机食品有限责任公司 | Method for enriching and purifying betulin in birch barks |
| CN102321143A (en) * | 2011-07-08 | 2012-01-18 | 浙江天草生物制品有限公司 | Method for preparing high-purity betulin |
| CN110092811A (en) * | 2019-06-04 | 2019-08-06 | 哈尔滨市泽尼康药业有限公司 | A kind of preparation method of betulin |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113461769A (en) * | 2021-07-14 | 2021-10-01 | 西安金泰生物技术有限公司 | Preparation method of betulin |
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Application publication date: 20200605 |