CN112125934A - Extraction method of triterpenoid alcohol compound - Google Patents
Extraction method of triterpenoid alcohol compound Download PDFInfo
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- CN112125934A CN112125934A CN202011028793.XA CN202011028793A CN112125934A CN 112125934 A CN112125934 A CN 112125934A CN 202011028793 A CN202011028793 A CN 202011028793A CN 112125934 A CN112125934 A CN 112125934A
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Abstract
The invention provides an extraction method of a triterpenoid alcohol compound, and relates to the technical field of triterpenoid compound preparation. The extraction method of the triterpene alcohol compound comprises S1, preparing raw materials; s2, soaking; s3, primary extraction; s4, secondary extraction; s5, extracting; s6, concentrating and separating. The ganoderma lucidum waste is cleaned and crushed firstly, then is mixed with the fungal cell wall lytic enzyme and stands still, the ganoderma lucidum cell wall can be dissolved, then is extracted twice through ethanol, and the ganoderma lucidum cells are further crushed through ultrasonic waves emitted by an ultrasonic generator and high-frequency electromagnetic waves emitted by a microwave generator during extraction, so that the ganoderma lucidum cells are more thoroughly crushed, the efficiency of extracting the triterpene alcohol compound is higher, the triterpene alcohol compound is more thorough, and then the triterpene alcohol compound can be obtained through extraction, concentration and separation, so that the yield of the triterpene alcohol compound is higher, and the ganoderma lucidum cell wall lytic enzyme is worthy of great popularization.
Description
Technical Field
The invention relates to the technical field of preparation of triterpenoid compounds, in particular to an extraction method of triterpenoid compounds.
Background
The triterpene compounds are substances formed by connecting a plurality of isoprene end to end after hydroxyl is removed, most of the triterpene compounds have 30 carbon atoms, and a small part of the triterpene compounds have 27 carbon atoms, triterpene components (called ganoderic acid) are widely distributed in the nature, triterpene substances are contained in the active ingredients of shark oil, liquorice, schisandra chinensis and ganoderma lucidum, the ganoderma lucidum triterpene components have two types of pentacyclic terpene and tetracyclic triterpene, the triterpene components can be divided into three types of C30, C27 and C24 according to the number of carbon atoms contained in molecules, and the triterpene compounds can be divided into 7 basic skeletons according to functional groups and different side chains contained in the triterpene components.
The common extraction method of the triterpene alcohol compound generally comprises the steps of crushing, extracting by using a chemical reagent and then extracting and purifying, but the triterpene alcohol compound contained in the ganoderma lucidum is difficult to be completely extracted after being directly crushed, so that the yield is low.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides an extraction method of a triterpenoid alcohol compound, which solves the problem of low yield caused by difficult thorough extraction of the triterpenoid alcohol compound.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: a method for extracting a triterpene alcohol compound, comprising the steps of:
s1, raw material preparation
Firstly, mixing ganoderma lucidum waste and deionized water according to a mass ratio of 1: 4.5-5.5, slowly stirring for 10-13 min, completely filtering and removing deionized water, then putting into a drying box, drying at a low temperature of 65-75 ℃, grinding and crushing the dried ganoderma lucidum waste by using a grinder, filtering by using a 80-120 mesh screen, and removing large-particle impurities to obtain standby raw material powder;
s2, soaking
Mixing raw material powder and deionized water according to a mass ratio of 1: 2, stirring and mixing uniformly, then adding fungal cell wall lytic enzyme with the total mass of 0.8-1.5%, stirring uniformly, and standing for 1-3 h at room temperature;
s3, extracting for one time
Adding the solution after standing into a reaction kettle, then adding absolute ethyl alcohol with the same volume into the reaction kettle, stirring and mixing uniformly, raising the temperature in the reaction kettle to 68-88 ℃, standing for 2-4 h, transmitting ultrasonic waves into the reaction kettle for 3-5 times by using an ultrasonic generator in the standing process, wherein the transmitting time is 20-35 s each time, and filtering after standing to obtain a primary extracting solution and primary filter residue;
s4, secondary extraction
Adding the primary filter residue into a reaction kettle, then adding deionized water and absolute ethyl alcohol which are equal to those in S2 into the reaction kettle, stirring and mixing uniformly, raising the temperature in the reaction kettle to 68-88 ℃, standing for 2-4 h, emitting high-frequency electromagnetic waves into the reaction kettle for 4-7 times by using a microwave generator in the standing process, wherein the emitting time is 20-35S each time, and filtering after standing to obtain a secondary extracting solution and secondary filter residue;
s5, extraction
Uniformly mixing the primary extract and the secondary extract, adding chloroform with the same volume for extraction, standing at room temperature for 3-5 h, and filtering to remove filter residue to obtain an extract;
s6, concentrating and separating
And putting the extract into a vacuum tank, vacuumizing to reduce the vacuum degree to 100-200 Pa, raising the temperature to 60-75 ℃, and evaporating the liquid in the extract to obtain the triterpenoid compound.
Preferably, the ganoderma lucidum waste is waste residue left after ganoderma lucidum polysaccharide is extracted from ganoderma lucidum fruiting bodies.
Preferably, the frequency of the ultrasonic waves is 20-40 KHz, and the interval time of transmitting the ultrasonic waves every time is 10-15 min.
Preferably, the frequency of the high-frequency electromagnetic wave is 900-950 MHz, and the interval time of transmitting the high-frequency electromagnetic wave every time is 8-11 min.
(III) advantageous effects
The invention provides an extraction method of a triterpene alcohol compound. The method has the following beneficial effects:
the method comprises the steps of cleaning and crushing the ganoderma lucidum waste, mixing the ganoderma lucidum waste with the fungal cell wall lytic enzyme, standing, dissolving the ganoderma lucidum cell wall, extracting twice with ethanol, further crushing ganoderma lucidum cells by using ultrasonic waves emitted by an ultrasonic generator and high-frequency electromagnetic waves emitted by a microwave generator during extraction, and further crushing the ganoderma lucidum cells to ensure that the ganoderma lucidum cells are more thoroughly crushed, so that the efficiency of extracting the triterpenoid alcohol compound is higher, the extraction is more thorough, and then the extraction, concentration and separation are carried out to obtain the triterpenoid alcohol compound, so that the yield of the triterpenoid alcohol compound is higher, and the method is worthy of vigorous popularization.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
the embodiment of the invention provides an extraction method of a triterpene alcohol compound, which comprises the following steps:
s1, raw material preparation
Firstly, mixing ganoderma lucidum waste and deionized water according to a mass ratio of 1: 4.5, slowly stirring for 11min, completely filtering and removing deionized water, then putting the mixture into a drying box, drying at a low temperature of 70 ℃, grinding and crushing the dried ganoderma lucidum waste by using a grinder, filtering by using a 80-mesh screen to remove large-particle impurities to obtain standby raw material powder, adding deionized water to clean and remove impurities in the ganoderma lucidum waste, and grinding and crushing to facilitate extracting triterpene alcohol from the ganoderma lucidum waste;
s2, soaking
Mixing raw material powder and deionized water according to a mass ratio of 1: 2, adding fungal cell wall lytic enzyme with the total mass of 1.1 percent after uniformly stirring, standing at room temperature for 2 hours after uniformly stirring, wherein the fungal cell wall lytic enzyme can dissolve cell walls of ganoderma lucidum cells, so that triterpene alcohol compounds in the ganoderma lucidum cells can be conveniently extracted;
s3, extracting for one time
Adding the solution after standing into a reaction kettle, then adding absolute ethyl alcohol with the same volume into the reaction kettle, stirring and mixing uniformly, raising the temperature in the reaction kettle to 75 ℃, standing for 2 hours, transmitting ultrasonic waves into the reaction kettle for 4 times by using an ultrasonic generator in the standing process, wherein the transmitting time is 25s each time, filtering after standing is finished to obtain primary extracting solution and primary filter residue, and further crushing ganoderma lucidum cells by using the ultrasonic waves to enable triterpene alcohol in the ganoderma lucidum cells to be more convenient to extract;
s4, secondary extraction
Adding the primary filter residue into a reaction kettle, then adding deionized water and absolute ethyl alcohol which are equal to those in S2 into the reaction kettle, stirring and mixing uniformly, raising the temperature in the reaction kettle to 75 ℃, standing for 2 hours, emitting 5 times of high-frequency electromagnetic waves into the reaction kettle by using a microwave generator in the standing process, wherein the emitting time is 28S each time, filtering after standing to obtain a secondary extracting solution and secondary filter residue, and further crushing ganoderma lucidum cells by using the high-frequency electromagnetic waves to enable triterpene alcohol in the ganoderma lucidum cells to be more convenient to extract;
s5, extraction
Uniformly mixing the primary extract and the secondary extract, adding chloroform with the same volume for extraction, standing at room temperature for 3h, and filtering to remove filter residue to obtain extract;
s6, concentrating and separating
And putting the extract into a vacuum tank, vacuumizing to reduce the vacuum degree to 100Pa, raising the temperature to 68 ℃, and evaporating the liquid in the extract to obtain the triterpene alcohol compound.
The ganoderma lucidum waste is waste residue left after ganoderma lucidum polysaccharide is extracted from ganoderma lucidum sporocarp serving as a raw material, the frequency of ultrasonic waves is 25KHz, the interval time of transmitting the ultrasonic waves every time is 12min, the frequency of high-frequency electromagnetic waves is 900MHz, the interval time of transmitting the high-frequency electromagnetic waves every time is 9min, and the transmission interval time of the ultrasonic waves and the high-frequency electromagnetic waves is set so as to prevent components in the ganoderma lucidum waste from being damaged due to overheating liquid by the ultrasonic waves and the high-frequency electromagnetic waves.
Example two:
the embodiment of the invention provides an extraction method of a triterpene alcohol compound, which comprises the following steps:
s1, raw material preparation
Firstly, mixing ganoderma lucidum waste and deionized water according to a mass ratio of 1: 5.5, slowly stirring for 12min, completely filtering and removing deionized water, then putting the mixture into a drying box, drying at a low temperature of 72 ℃, grinding and crushing the dried ganoderma lucidum waste by using a grinder, filtering by using a 120-mesh screen to remove large-particle impurities to obtain standby raw material powder, adding deionized water to clean and remove impurities in the ganoderma lucidum waste, and grinding and crushing to facilitate extracting triterpene alcohol from the ganoderma lucidum waste;
s2, soaking
Mixing raw material powder and deionized water according to a mass ratio of 1: 2, adding fungal cell wall lytic enzyme with the total mass of 1.5 percent after uniformly stirring, standing at room temperature for 1h, wherein the fungal cell wall lytic enzyme can dissolve cell walls of ganoderma lucidum cells, so that triterpene alcohol compounds in the ganoderma lucidum cells can be conveniently extracted;
s3, extracting for one time
Adding the solution after standing into a reaction kettle, then adding absolute ethyl alcohol with the same volume into the reaction kettle, stirring and mixing uniformly, raising the temperature in the reaction kettle to 85 ℃, standing for 3 hours, transmitting 5 times of ultrasonic waves into the reaction kettle by using an ultrasonic generator in the standing process, wherein the transmitting time is 30s each time, filtering after standing is finished to obtain primary extracting solution and primary filter residue, and further crushing ganoderma lucidum cells by using the ultrasonic waves to enable triterpene alcohol in the ganoderma lucidum cells to be more convenient to extract;
s4, secondary extraction
Adding the primary filter residue into a reaction kettle, then adding deionized water and absolute ethyl alcohol which are equal to those in S2 into the reaction kettle, stirring and mixing uniformly, raising the temperature in the reaction kettle to 85 ℃, standing for 3 hours, emitting high-frequency electromagnetic waves into the reaction kettle for 4 times by using a microwave generator in the standing process, wherein the emitting time is 32S each time, filtering after standing to obtain secondary extracting solution and secondary filter residue, and further crushing ganoderma lucidum cells by using the high-frequency electromagnetic waves to enable triterpene alcohol in the ganoderma lucidum cells to be more convenient to extract;
s5, extraction
Uniformly mixing the primary extract and the secondary extract, adding chloroform with the same volume for extraction, standing at room temperature for 4h, and filtering to remove filter residue to obtain extract;
s6, concentrating and separating
Putting the extract into a vacuum tank, vacuumizing to reduce the vacuum degree to 150Pa, raising the temperature to 70 ℃, and evaporating the liquid in the extract to obtain the triterpene alcohol compound.
The ganoderma lucidum waste is waste residue left after ganoderma lucidum polysaccharide is extracted from ganoderma lucidum sporocarp serving as a raw material, the frequency of ultrasonic waves is 35KHz, the interval time of transmitting the ultrasonic waves every time is 15min, the frequency of high-frequency electromagnetic waves is 950MHz, the interval time of transmitting the high-frequency electromagnetic waves every time is 11min, and the transmission interval time of the ultrasonic waves and the high-frequency electromagnetic waves is set so as to prevent components in the ganoderma lucidum waste from being damaged due to overheating liquid by the ultrasonic waves and the high-frequency electromagnetic waves.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. A method for extracting a triterpene alcohol compound, which is characterized by comprising the following steps: the method comprises the following steps:
s1, raw material preparation
Firstly, mixing ganoderma lucidum waste and deionized water according to a mass ratio of 1: 4.5-5.5, slowly stirring for 10-13 min, completely filtering and removing deionized water, then putting into a drying box, drying at a low temperature of 65-75 ℃, grinding and crushing the dried ganoderma lucidum waste by using a grinder, filtering by using a 80-120 mesh screen, and removing large-particle impurities to obtain standby raw material powder;
s2, soaking
Mixing raw material powder and deionized water according to a mass ratio of 1: 2, stirring and mixing uniformly, then adding fungal cell wall lytic enzyme with the total mass of 0.8-1.5%, stirring uniformly, and standing for 1-3 h at room temperature;
s3, extracting for one time
Adding the solution after standing into a reaction kettle, then adding absolute ethyl alcohol with the same volume into the reaction kettle, stirring and mixing uniformly, raising the temperature in the reaction kettle to 68-88 ℃, standing for 2-4 h, transmitting ultrasonic waves into the reaction kettle for 3-5 times by using an ultrasonic generator in the standing process, wherein the transmitting time is 20-35 s each time, and filtering after standing to obtain a primary extracting solution and primary filter residue;
s4, secondary extraction
Adding the primary filter residue into a reaction kettle, then adding deionized water and absolute ethyl alcohol which are equal to those in S2 into the reaction kettle, stirring and mixing uniformly, raising the temperature in the reaction kettle to 68-88 ℃, standing for 2-4 h, emitting high-frequency electromagnetic waves into the reaction kettle for 4-7 times by using a microwave generator in the standing process, wherein the emitting time is 20-35S each time, and filtering after standing to obtain a secondary extracting solution and secondary filter residue;
s5, extraction
Uniformly mixing the primary extract and the secondary extract, adding chloroform with the same volume for extraction, standing at room temperature for 3-5 h, and filtering to remove filter residue to obtain an extract;
s6, concentrating and separating
And putting the extract into a vacuum tank, vacuumizing to reduce the vacuum degree to 100-200 Pa, raising the temperature to 60-75 ℃, and evaporating the liquid in the extract to obtain the triterpenoid compound.
2. The method for extracting a triterpene alcohol compound according to claim 1, wherein: the ganoderma lucidum waste is residue left after ganoderma lucidum polysaccharide is extracted from ganoderma lucidum sporocarp serving as a raw material.
3. The method for extracting a triterpene alcohol compound according to claim 1, wherein: the frequency of the ultrasonic waves is 20-40 KHz, and the interval time for transmitting the ultrasonic waves every time is 10-15 min.
4. The method for extracting a triterpene alcohol compound according to claim 1, wherein: the frequency of the high-frequency electromagnetic wave is 900-950 MHz, and the interval time of transmitting the high-frequency electromagnetic wave every time is 8-11 min.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007083823A1 (en) * | 2006-01-17 | 2007-07-26 | Kyushu University, National University Corporation | Androgen receptor-binding activity of genoderma mushroom-treated product |
| CN101530436A (en) * | 2009-04-20 | 2009-09-16 | 浙江省林业科学研究院 | Method of effectively extracting ganoderma triterpenoids and ganoderan from mythic fungus germ entity |
| CN102772448A (en) * | 2012-08-15 | 2012-11-14 | 苏州菩芸生物科技有限公司 | Lucid ganoderma triterpene extraction method |
| CN104910234A (en) * | 2015-05-26 | 2015-09-16 | 南京泽朗医药科技有限公司 | Preparation method of ganodermanontriol |
| CN105111267A (en) * | 2015-10-09 | 2015-12-02 | 上海市农业科学院 | Preparation method of ganoderol B |
| CN106722875A (en) * | 2016-12-07 | 2017-05-31 | 盐城工学院 | The extracting method and Ganoderma lucidum of a kind of ganodenic acid |
| CN109096407A (en) * | 2018-06-29 | 2018-12-28 | 江苏农林职业技术学院 | The combined extraction method of total triterpene and polysaccharide in a kind of ganoderma lucidum mushroom bran |
-
2020
- 2020-09-25 CN CN202011028793.XA patent/CN112125934A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007083823A1 (en) * | 2006-01-17 | 2007-07-26 | Kyushu University, National University Corporation | Androgen receptor-binding activity of genoderma mushroom-treated product |
| CN101530436A (en) * | 2009-04-20 | 2009-09-16 | 浙江省林业科学研究院 | Method of effectively extracting ganoderma triterpenoids and ganoderan from mythic fungus germ entity |
| CN102772448A (en) * | 2012-08-15 | 2012-11-14 | 苏州菩芸生物科技有限公司 | Lucid ganoderma triterpene extraction method |
| CN104910234A (en) * | 2015-05-26 | 2015-09-16 | 南京泽朗医药科技有限公司 | Preparation method of ganodermanontriol |
| CN105111267A (en) * | 2015-10-09 | 2015-12-02 | 上海市农业科学院 | Preparation method of ganoderol B |
| CN106722875A (en) * | 2016-12-07 | 2017-05-31 | 盐城工学院 | The extracting method and Ganoderma lucidum of a kind of ganodenic acid |
| CN109096407A (en) * | 2018-06-29 | 2018-12-28 | 江苏农林职业技术学院 | The combined extraction method of total triterpene and polysaccharide in a kind of ganoderma lucidum mushroom bran |
Non-Patent Citations (4)
| Title |
|---|
| HIROJI SATO，ET AL.: "Ganoderiol A and B, New Triterpenoids from the Fungus Ganoderma lucidum (Reishi)", 《AGRICULTURAL AND BIOLOGICAL CHEMISTRY》 * |
| YING QIAO，ET AL.: "Two Novel Lanostane Triterpenoids from Ganoderma Sinense", 《MOLECULES》 * |
| 刘超 等: "松杉灵芝的化学成分研究(Ⅱ)", 《中草药》 * |
| 李丽华 等主编: "《天然药物化学实验教程》", 30 June 2017, 中国医药科技出版社 * |
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