CN107266517A - A kind of method that active component is extracted in the tunning extract from Antrodia camphorata - Google Patents
A kind of method that active component is extracted in the tunning extract from Antrodia camphorata Download PDFInfo
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- CN107266517A CN107266517A CN201710616309.7A CN201710616309A CN107266517A CN 107266517 A CN107266517 A CN 107266517A CN 201710616309 A CN201710616309 A CN 201710616309A CN 107266517 A CN107266517 A CN 107266517A
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- antrodia camphorata
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- tunning
- tunning extract
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J9/00—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of more than two carbon atoms, e.g. cholane, cholestane, coprostane
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/007—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids using organic solvents
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- Oil, Petroleum & Natural Gas (AREA)
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- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of method that active component is extracted in tunning extract from Antrodia camphorata, it is characterised in that comprise the following steps:Step one, by Antrodia camphorata tunning extract and organic solvent by volume 5:1‑1:3 ratio is mixed, and mixed liquor is obtained by extraction in stirring;Step 2, mixed liquor is placed in low temperature environment, stirs 20 60min, and stir speed (S.S.) is 50 200rpm, obtains ice crystal;Step 3, at low ambient temperatures, ice crystal is squeezed and removed, surplus solution is obtained;Step 4, by surplus solution repeat step two and step 3 untill without ice crystal generation, obtains final solution;Step 5, cryogenic vacuum concentration is carried out by final solution, removes organic solvent, gained paste is active component.
Description
Technical field
The present invention relates to a kind of method that active component is extracted in tunning extract from Antrodia camphorata, belong to bio-chemistry separation
Technical field.
Background technology
Long-chain higher alkane (C12-C16) has higher log P values (6.6-8.8), therefore to the toxic action of cell
It is smaller, there is preferable biocompatibility, be commonly used to do the two-phase culture solvent of plant cell, microbial cell.There are many scholars
Research and utilization long-chain higher alkane is organic phase, carries out Johnst hairy root two-phase culture production alkannin, taxus chinensis in northeast two-phase
Culture production taxol, Dunaliella salina two-phase culture production carotenoid etc., can be effectively by metabolite from cell transfer
Organic phase is moved to, and accelerates the rate of release of metabolite, while cell growth inhibitory action is very small.
Long-chain higher alkane (C12-C16) has preferable extractive fermentation effect to many liposoluble active products, still
Its boiling point is higher, 215 DEG C of the boils up till of such as n-dodecane, and this causes that fermentation production can not be removed using the vacuum concentration of water-bath
Long-chain higher alkane solvent in thing extract and obtain activated product, temperature-sensitive can be made by being concentrated in vacuo using the higher oil bath of temperature
Property ingredient breakdown, and there is potential safety hazard;Good effect can not be obtained using ethanol equal solvent extraction long-chain higher alkane
Really, a large amount of ethanol are consumed, extraction yield is relatively low, active component remnants are more in the dodecane hydrocarbon after extraction, and in ethanol still
Part dodecane hydrocarbon can so be dissolved.
The content of the invention
The present invention is to solve to be difficult to extract active component from the tunning extract containing long-chain higher alkane
The problem of and carry out, it is therefore intended that a kind of method that active component is extracted during the tunning extract from Antrodia camphorata is provided.
Present invention employs following technical scheme:
The method that active component is extracted from Antrodia camphorata tunning extract that the present invention is provided, it is characterised in that bag
Include following steps:
Step one, by Antrodia camphorata tunning extract and organic solvent by volume 5:1-1:3 ratio is mixed,
And mixed liquor is obtained by extraction in stirring.
Step 2, mixed liquor is placed in low temperature environment, stirs 20-60min, stir speed (S.S.) is 50-200rpm, obtains ice
It is brilliant.
Step 3, at low ambient temperatures, ice crystal is squeezed and removed, surplus solution is obtained.
Step 4, by surplus solution repeat step two and step 3 untill without ice crystal generation, obtains final solution.
Step 5, by final solution carry out cryogenic vacuum concentration, remove organic solvent, gained paste be activity into
Point.
In the method for extraction active component, can also have from Antrodia camphorata tunning extract what the present invention was provided
Such feature:Wherein, Antrodia camphorata tunning includes Antrodia camphorata cereal product by solid-state fermentation and Antrodia camphorata situ extracting is sent out
Ferment product.
In the method for extraction active component, can also have from Antrodia camphorata tunning extract what the present invention was provided
Such feature:Wherein, the extractant in extract is the long-chain higher alkane that carbon atom number is 12-16.
In the method for extraction active component, can also have from Antrodia camphorata tunning extract what the present invention was provided
Such feature:Wherein, active component includes ergosterol, Android tonquinol, unrighted acid.
In the method for extraction active component, can also have from Antrodia camphorata tunning extract what the present invention was provided
Such feature:Wherein, in step one, organic solvent be acetone, ethanol or methanol in any one or it is any two kinds and
Mixed solvent above.
In the method for extraction active component, can also have from Antrodia camphorata tunning extract what the present invention was provided
Such feature:Wherein, in step one, the stir speed (S.S.) of stirring extraction is 300rpm, and mixing time is 30min.
In the method for extraction active component, can also have from Antrodia camphorata tunning extract what the present invention was provided
Such feature:Wherein, in step 2, the temperature range of low temperature is -10-0 DEG C.
In the method for extraction active component, can also have from Antrodia camphorata tunning extract what the present invention was provided
Such feature:Wherein, in step 3, the temperature of low temperature is 0 DEG C.
In the method for extraction active component, can also have from Antrodia camphorata tunning extract what the present invention was provided
Such feature, before step one, in addition to pre-treatment step:By Antrodia camphorata tunning extract 5000rpm centrifugations, go
Except solid impurity and residual moisture.
In the method for extraction active component, can also have from Antrodia camphorata tunning extract what the present invention was provided
Such feature is characterized in that, after step 5, in addition to extractant recycles step:Ice crystal thawing processing is obtained
Solution containing extractant, the production that the solution is continued with to carry out Antrodia camphorata tunning extract, preparation.
The effect of invention and effect
The method that active component is extracted from Antrodia camphorata tunning extract involved in the present invention, utilizes freeze concentration
Principle, the active component in Antrodia camphorata tunning is extracted from the long-chain higher alkane extract of Antrodia camphorata tunning
Out, compared with prior art with advantages below:The method of separation and Extraction is simple, active component recovery rate be up to 90% with
On, the active shortcoming that high temperature extracts destruction active component is overcome, the extraction separation of Heat sensitive active composition is particularly suitable for use in,
Product quality is easily controlled, it is to avoid high-temperature operation, safe and reliable, easily realizes industrialized production.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below
The method that conjunction embodiment extracts active component to the present invention from Antrodia camphorata tunning extract is specifically addressed.
Embodiment 1
The extract and separate of Antrodia camphorata cereal product by solid-state fermentation
In the present embodiment, Antrodia camphorata cereal is Antrodia camphorata highland barley.
Step one, 50g Antrodia camphorata highland barley product by solid-state fermentation powder is taken, dodecane hydrocarbon 500mL, 50 DEG C of stirring extractions is added
1h, extraction terminates rear suction filtration, obtains the extract of Antrodia camphorata highland barley product by solid-state fermentation, and 5000rpm centrifugations remove solid impurity
And residual moisture.
Step 2, by the extract of Antrodia camphorata highland barley product by solid-state fermentation and acetone by volume 5:1 ratio is mixed
Close, and stir extraction, stir speed (S.S.) is 300rpm, and extraction time is 30min, obtains mixed liquor.
Step 3, mixed liquor is placed in -10 DEG C of environment, stirs 20min, stir speed (S.S.) is 50rpm.
Step 4, under 0 DEG C of environment, squeezes rapidly removal by the ice crystal in mixed solution, obtains surplus solution.
Step 5, by surplus solution repeat step two and step 3 untill without ice crystal generation, obtains final solution.
Step 6, cryogenic vacuum concentration is carried out by final solution, removes acetone, gained paste is active component.
Step 7, obtains the solution containing dodecane hydrocarbon by ice crystal thawing processing, the solution is continued with to carry out ox
The preparation of the extract of antrodia highland barley product by solid-state fermentation.
According to the isolation and purification method of the present embodiment, the active component ergosterol of Antrodia camphorata highland barley solid state fermentation, Android
Tonquinol Antroquinonol, the extraction rate reached of unrighted acid are to 90%, and the dodecane hydrocarbon solution of recovery is colorless and odorless
Liquid, can continue to using come the preparation of the extract that carries out Antrodia camphorata highland barley product by solid-state fermentation.
Embodiment 2
The extract and separate of Cinnamomum kanahirai hay cereal highland barley product by solid-state fermentation
In the present embodiment, Antrodia camphorata cereal is Antrodia camphorata highland barley.
Step one, 50g Antrodia camphorata highland barley product by solid-state fermentation powder is taken, dodecane hydrocarbon 500mL, 50 DEG C of stirring extractions is added
1h, extraction terminates rear suction filtration, obtains the extract of Antrodia camphorata highland barley product by solid-state fermentation, and 5000rpm centrifugations remove solid impurity
And residual moisture.
Step 2, by the extract of Antrodia camphorata highland barley product by solid-state fermentation and acetone by volume 1:1 ratio is mixed
Close, and stir extraction, stir speed (S.S.) is 300rpm, and extraction time is 30min, obtains mixed liquor.
Step 3, mixed liquor is placed in -6 DEG C of environment, stirs 40min, stir speed (S.S.) is 90rpm.
Step 4, under 0 DEG C of environment, squeezes rapidly removal by the ice crystal in mixed solution, obtains surplus solution.
Step 5, by surplus solution repeat step two and step 3 untill without ice crystal generation, obtains final solution.
Step 6, cryogenic vacuum concentration is carried out by final solution, removes acetone, gained paste is active component.
Step 7, obtains the solution containing dodecane hydrocarbon by ice crystal thawing processing, the solution is continued with to carry out ox
The preparation of the extract of antrodia highland barley product by solid-state fermentation.
According to the isolation and purification method of the present embodiment, the active component ergosterol of Antrodia camphorata highland barley solid state fermentation, Android
Tonquinol Antroquinonol, the extraction rate reached of unrighted acid are to 97%, and the dodecane hydrocarbon solution of recovery is colorless and odorless
Liquid, can continue to using come the preparation of the extract that carries out Antrodia camphorata highland barley product by solid-state fermentation.
Embodiment 3
The extract and separate of Antrodia camphorata cereal product by solid-state fermentation
In the present embodiment, Antrodia camphorata cereal is Antrodia camphorata highland barley.
Step one, 50g Antrodia camphorata highland barley product by solid-state fermentation powder is taken, dodecane hydrocarbon 500mL, 50 DEG C of stirring extractions is added
1h, extraction terminates rear suction filtration, obtains the extract of Antrodia camphorata highland barley product by solid-state fermentation, and 5000rpm centrifugations remove solid impurity
And residual moisture.
Step 2, by the extract of Antrodia camphorata highland barley product by solid-state fermentation and acetone by volume 1:3 ratio is mixed
Close, and stir extraction, stir speed (S.S.) is 300rpm, and extraction time is 30min, obtains mixed liquor.
Step 3, mixed liquor is placed in 0 DEG C of environment, stirs 60min, stir speed (S.S.) is 200rpm.
Step 4, under 0 DEG C of environment, squeezes rapidly removal by the ice crystal in mixed solution, obtains surplus solution.
Step 5, by surplus solution repeat step two and step 3 untill without ice crystal generation, obtains final solution.
Step 6, cryogenic vacuum concentration is carried out by final solution, removes acetone, gained paste is active component.
Step 7, obtains the solution containing dodecane hydrocarbon by ice crystal thawing processing, the solution is continued with to carry out ox
The preparation of the extract of antrodia highland barley product by solid-state fermentation.
According to the isolation and purification method of the present embodiment, the active component ergosterol of Antrodia camphorata highland barley solid state fermentation, Android
Tonquinol Antroquinonol, the extraction rate reached of unrighted acid are to 93%, and the dodecane hydrocarbon solution of recovery is colorless and odorless
Liquid, can continue to using come the preparation of the extract that carries out Antrodia camphorata highland barley product by solid-state fermentation.
Embodiment 4
The extract and separate of Antrodia camphorata cereal product by solid-state fermentation
In the present embodiment, Antrodia camphorata cereal is Antrodia camphorata highland barley.
Step one, 50g Antrodia camphorata highland barley product by solid-state fermentation powder is taken, tetradecane hydrocarbon 500mL, 50 DEG C of stirring extractions is added
1h, extraction terminates rear suction filtration, obtains the extract of Antrodia camphorata highland barley product by solid-state fermentation, and 5000rpm centrifugations remove solid impurity
And residual moisture.
Step 2, by the extract of Antrodia camphorata highland barley product by solid-state fermentation and ethanol by volume 1:1 ratio is mixed
Close, and stir extraction, stir speed (S.S.) is 300rpm, and extraction time is 30min, obtains mixed liquor.
Step 3, mixed liquor is placed in -6 DEG C of environment, stirs 40min, stir speed (S.S.) is 90rpm.
Step 4, under 0 DEG C of environment, squeezes rapidly removal by the ice crystal in mixed solution, obtains surplus solution.
Step 5, by surplus solution repeat step two and step 3 untill without ice crystal generation, obtains final solution.
Step 6, cryogenic vacuum concentration is carried out by final solution, removes acetone, gained paste is active component.
Step 7, obtains the solution containing tetradecane hydrocarbon by ice crystal thawing processing, the solution is continued with to carry out ox
The preparation of the extract of antrodia highland barley product by solid-state fermentation.
According to the isolation and purification method of the present embodiment, the active component ergosterol of Antrodia camphorata highland barley solid state fermentation, Android
Tonquinol Antroquinonol, the extraction rate reached of unrighted acid are to 95%, and the tetradecane hydrocarbon solution of recovery is colorless and odorless
Liquid, can continue to using come the preparation of the extract that carries out Antrodia camphorata highland barley product by solid-state fermentation.
Embodiment 5
The extract and separate of Antrodia camphorata dodecane hydrocarbon situ extracting tunning
Step one, the extract in Antrodia camphorata dodecane hydrocarbon situ extracting zymotic fluid is taken out, as Antrodia camphorata fermentation production
Thing extract, measures 100mL, and 5000rpm centrifugations remove solid impurity and residual moisture.
Step 2, by Antrodia camphorata tunning extract and acetone by volume 1:1 ratio is mixed, and stirs extraction
Take, stir speed (S.S.) is 300rpm, extraction time is 30min, obtains mixed liquor.
Step 3, mixed liquor is placed in -6 DEG C of environment, stirs 40min, stir speed (S.S.) is 90rpm.
Step 4, under 0 DEG C of environment, squeezes rapidly removal by the ice crystal in mixed solution, obtains surplus solution.
Step 5, by surplus solution repeat step two and step 3 untill without ice crystal generation, obtains final solution.
Step 6, cryogenic vacuum concentration is carried out by final solution, removes acetone, gained paste is active component.
Step 7, obtains the solution containing dodecane hydrocarbon by ice crystal thawing processing, the solution is continued with to carry out ox
The preparation of the extract of antrodia dodecane hydrocarbon situ extracting zymotic fluid.
According to the isolation and purification method of the present embodiment, the active component ergot steroid of Antrodia camphorata dodecane hydrocarbon situ extracting fermentation
Alcohol, Android tonquinol Antroquinonol, the extraction rate reached of unrighted acid are to 97%, and the dodecane hydrocarbon of recovery is colourless
Liquid with no taste, can continue to the preparation of the extract for Antrodia camphorata dodecane hydrocarbon situ extracting zymotic fluid.
The effect of embodiment and effect
The method that active component is extracted from Antrodia camphorata tunning extract involved in the present invention, utilizes freeze concentration
Principle, the active component in Antrodia camphorata tunning is extracted from the long-chain higher alkane extract of Antrodia camphorata tunning
Out, compared with prior art with advantages below:The method of separation and Extraction is simple, active component recovery rate be up to 90% with
On, the active shortcoming that high temperature extracts destruction active component is overcome, the extraction separation of Heat sensitive active composition is particularly suitable for use in,
Product quality is easily controlled, it is to avoid high-temperature operation, safe and reliable, easily realizes industrialized production.
Further, higher alkane extractant can be reclaimed simultaneously, and the higher alkane extractant colorless and odorless of recovery is said
Bright tunning content therein is extremely low, may be reused, so as to reduce production cost, makes the active component in tunning
It is easy to large-scale industrial production.
Above-mentioned embodiment is the preferred case of the present invention, is not intended to limit protection scope of the present invention.
Claims (10)
1. the method for active component is extracted in a kind of tunning extract from Antrodia camphorata, it is characterised in that comprise the following steps:
Step one, by Antrodia camphorata tunning extract and organic solvent by volume 5:1-1:3 ratio is mixed, and is stirred
Mix and mixed liquor is obtained by extraction;
Step 2, the mixed liquor is placed in low temperature environment, stirs 20-60min, stir speed (S.S.) is 50-200rpm, obtains ice
It is brilliant;
Step 3, at low ambient temperatures, the ice crystal is squeezed and removed, surplus solution is obtained;
Step 4, by the surplus solution repeat step two and step 3 untill without ice crystal generation, obtains final
Solution;
Step 5, cryogenic vacuum concentration is carried out by the final solution, removes the organic solvent, and gained paste is described
Active component.
2. extracting the method for active component in the tunning extract according to claim 1 from Antrodia camphorata, its feature exists
In:
Wherein, the Antrodia camphorata tunning includes Antrodia camphorata cereal product by solid-state fermentation and the fermentation production of Antrodia camphorata situ extracting
Thing.
3. extracting the method for active component in the tunning extract according to claim 1 from Antrodia camphorata, its feature exists
In:
Wherein, the extractant in the extract is the long-chain higher alkane that carbon atom number is 12-16.
4. extracting the method for active component in the tunning extract according to claim 1 from Antrodia camphorata, its feature exists
In:
Wherein, the active component includes ergosterol, Android tonquinol, unrighted acid.
5. extracting the method for active component in the tunning extract according to claim 1 from Antrodia camphorata, its feature exists
In:
Wherein, in step one, the organic solvent be acetone, ethanol or methanol in any one or it is any two kinds and more than
Mixed solvent.
6. extracting the method for active component in the tunning extract according to claim 1 from Antrodia camphorata, its feature exists
In:
Wherein, in step one, the stir speed (S.S.) of the stirring extraction is 300rpm, and mixing time is 30min.
7. extracting the method for active component in the tunning extract according to claim 1 from Antrodia camphorata, its feature exists
In:
Wherein, in step 2, the temperature range of the low temperature is -10-0 DEG C.
8. extracting the method for active component in the tunning extract according to claim 1 from Antrodia camphorata, its feature exists
In:
Wherein, in step 3, the temperature of the low temperature is 0 DEG C.
9. extracting the method for active component in the tunning extract according to claim 1 from Antrodia camphorata, its feature exists
In, before step one, in addition to pre-treatment step:
By Antrodia camphorata tunning extract 5000rpm centrifugations, solid impurity and residual moisture are removed.
10. extracting the method for active component in the tunning extract according to claim 3 from Antrodia camphorata, its feature exists
In after step 5, in addition to extractant recycles step:
Ice crystal thawing processing is obtained into the solution containing the extractant, the solution is continued with to carry out the Cinnamomum kanahirai hay
Production, the preparation of sesame tunning extract.
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TWI657134B (en) * | 2018-09-21 | 2019-04-21 | 陳信行 | Organic soap manufacturing process |
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CN1799561A (en) * | 2005-09-28 | 2006-07-12 | 莱阳农学院 | Application of Antrodia camphorata mycelium fermented extract in preparation of anti-radiation damage medicine |
CN102078703A (en) * | 2009-11-30 | 2011-06-01 | 江淑华 | Low-temperature ultrasonic extraction method for plant |
CN103923743A (en) * | 2013-05-09 | 2014-07-16 | 刘立 | Extraction method for effective compositions of antrodia camphorata |
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2017
- 2017-07-26 CN CN201710616309.7A patent/CN107266517B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1799561A (en) * | 2005-09-28 | 2006-07-12 | 莱阳农学院 | Application of Antrodia camphorata mycelium fermented extract in preparation of anti-radiation damage medicine |
CN102078703A (en) * | 2009-11-30 | 2011-06-01 | 江淑华 | Low-temperature ultrasonic extraction method for plant |
CN103923743A (en) * | 2013-05-09 | 2014-07-16 | 刘立 | Extraction method for effective compositions of antrodia camphorata |
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Publication number | Priority date | Publication date | Assignee | Title |
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TWI657134B (en) * | 2018-09-21 | 2019-04-21 | 陳信行 | Organic soap manufacturing process |
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