CN104910234A - Preparation method of ganodermanontriol - Google Patents
Preparation method of ganodermanontriol Download PDFInfo
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- CN104910234A CN104910234A CN201510270095.3A CN201510270095A CN104910234A CN 104910234 A CN104910234 A CN 104910234A CN 201510270095 A CN201510270095 A CN 201510270095A CN 104910234 A CN104910234 A CN 104910234A
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- ganodermanontriol
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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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Abstract
The invention discloses a preparation method of ganodermanontriol. The method includes: crushing ganoderma lucidum dried at 60-80DEG C, performing sieving by a 60-80mesh sieve, placing the obtained coarse powder in a container, adding a 5-10 times amount of 50%-70% ethanol solution, putting the container into a 70DEG C constant temperature water bath pot to conduct ultrasonic extraction for 90-120min, subjecting the obtained extract to ultrasonic extraction 2-3 times, carrying out vacuum concentration on the extracted liquid into an extract and recovering ethanol, adding hot water into the obtained extract to conduct dissolving and pumping filtration, adding activated carbon decoloration crude extracted liquid according to a mass-to-volume ratio of 1:15-30, loading the crude extracted liquid on a macroporous resin column to perform adsorption, conducting elution with a 30-50% ethanol aqueous solution, collecting the eluent and performing vacuum concentration to obtain ganodermanontriol. The method for preparation of ganodermanontriol provided by the invention has the advantages of simple technological operation, high yield, and small pollution, and is suitable for production of high purity ganodermanontriol.
Description
Technical field
The present invention be more particularly directed to a kind of preparation method of ganodermanontriol, belong to biological technical field.
Background technology
Ganodermanontriol is triterpene compound, CAS 106518-63-2, molecular formula C
30h
48o
4, molecular weight 4722.7, molecular structural formula is as follows:
Ganodermanontriol is the triterpenes components in glossy ganoderma, and triterpenes is also one of effective constituent of glossy ganoderma, has cytotoxicity to human liver cancer cell, also can suppress the release of histamine, has hepatoprotective effect and has anti-allergic effects etc.
By literature search, existing ganodermanontriol preparation method is employing silica gel, gel chromatography is carried out point ethanol and put forward refluxing extraction, ethyl acetate extraction, and silica gel, gel chromatography carry out the step such as being separated.Due to complicated operation, preparation amount is less, and sample yield is low, is not suitable for suitability for industrialized production.
Summary of the invention
The object of the invention is to solve shortcomings and deficiencies of the prior art, a kind of preparation method of ganodermanontriol easy and simple to handle is provided.
To achieve these goals, the present invention is by the following technical solutions:
Will in 60 ~ 80 DEG C of dried glossy ganoderma raw material pulverizing, cross 60 ~ 80 mesh sieves, gained meal is placed in container, add the ethanolic soln of 5-10 times amount 50%-70%, container is put into thermostat water bath lixiviate 90 ~ 120min that temperature is 70 DEG C, gained extractive substance is placed in supersound extraction supersound extraction 2-3 time, extracting solution concentrating under reduced pressure reclaims ethanol, and be condensed into medicinal extract shape, gained medicinal extract heating water dissolves and suction filtration, and to add mass volume ratio be that the activated carbon decolorizing of 1:15 ~ 30 obtains crude extract, by macroporous resin column absorption on crude extract, with 3 ~ 6 times of column volumes, the aqueous ethanolic solution wash-out of 30 ~ 50%, collect elutriant vacuum concentration and make ganodermanontriol crystal.
The frequency of described supersound extraction is 20 ~ 40KHz, and extraction time is each 15 ~ 30min.
One in described macroporous resin optional HZ816, HPD100, D101, X-5, LSA-21, WLD.
Adopt this law to prepare ganodermanontriol, simple process is easy to operate, and not only product yield is high, and purity is high, low stain.
Further illustrate the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiments.
Embodiment
Embodiment 1:
By in 60 DEG C of dried glossy ganoderma raw material pulverizing, cross 60 mesh sieves, gained meal is placed in container, add the ethanolic soln of 5 times amount 50%, container is put into the thermostat water bath lixiviate 90min that temperature is 70 DEG C, gained extractive substance being placed in frequency is 20KHz supersound extraction supersound extraction 3 times, each 15min, extracting solution concentrating under reduced pressure reclaims ethanol, and be condensed into medicinal extract shape, gained medicinal extract heating water dissolves and suction filtration, and to add mass volume ratio be that the activated carbon decolorizing of 1:15 obtains crude extract, by D101 type macroporous resin column absorption on crude extract, with 3 times of column volumes, the aqueous ethanolic solution wash-out of 30%, collect elutriant vacuum concentration and make ganodermanontriol crystal.Detect through HPLC, content 92.5%.
Embodiment 2:
By in 70 DEG C of dried glossy ganoderma raw material pulverizing, cross 80 mesh sieves, gained meal is placed in container, add the ethanolic soln of 8 times amount 60%, container is put into the thermostat water bath lixiviate 100min that temperature is 70 DEG C, gained extractive substance is placed in 30KHz supersound extraction supersound extraction 3 times, each 20min extracting solution concentrating under reduced pressure reclaims ethanol, and be condensed into medicinal extract shape, gained medicinal extract heating water dissolves and suction filtration, and to add mass volume ratio be that the activated carbon decolorizing of 1:20 obtains crude extract, by LSA-21 type macroporous resin column absorption on crude extract, with 5 times of column volumes, the aqueous ethanolic solution wash-out of 40%, collect elutriant vacuum concentration and make ganodermanontriol crystal.Detect through HPLC, content 93.45%.
Embodiment 3:
By in 80 DEG C of dried glossy ganoderma raw material pulverizing, cross 80 mesh sieves, gained meal is placed in container, add the ethanolic soln of 10 times amount 70%, container is put into the thermostat water bath lixiviate 120min that temperature is 70 DEG C, gained extractive substance being placed in frequency is 40KHz supersound extraction supersound extraction 3 times, each 30min extracting solution concentrating under reduced pressure reclaims ethanol, and be condensed into medicinal extract shape, gained medicinal extract heating water dissolves and suction filtration, and to add mass volume ratio be that the activated carbon decolorizing of 1:30 obtains crude extract, by HZ816 type macroporous resin column absorption on crude extract, with 6 times of column volumes, the aqueous ethanolic solution wash-out of 50%, collect elutriant vacuum concentration and make ganodermanontriol crystal.Detect through HPLC, content 93.85%.
Claims (3)
1. the preparation method of a ganodermanontriol, it is characterized in that following steps: will in 60 ~ 80 DEG C of dried glossy ganoderma raw material pulverizing, cross 60 ~ 80 mesh sieves, gained meal is placed in container, add the ethanolic soln of 5-10 times amount 50%-70%, container is put into thermostat water bath lixiviate 90 ~ 120min that temperature is 70 DEG C, gained extractive substance is placed in supersound extraction supersound extraction 2-3 time, extracting solution concentrating under reduced pressure reclaims ethanol, and be condensed into medicinal extract shape, gained medicinal extract heating water dissolves and suction filtration, and to add mass volume ratio be that the activated carbon decolorizing of 1:15 ~ 30 obtains crude extract, by macroporous resin column absorption on crude extract, with 3 ~ 6 times of column volumes, the aqueous ethanolic solution wash-out of 30 ~ 50%, collect elutriant vacuum concentration and make ganodermanontriol crystal.
2. the preparation method of ganodermanontriol according to claim 1, it is characterized in that the frequency of described supersound extraction is 20 ~ 40KHz, extraction time is each 15 ~ 30min.
3. the preparation method of ganodermanontriol according to claim 1, is characterized in that the one in described macroporous resin optional HZ816, HPD100, D101, X-5, LSA-21, WLD.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510270095.3A CN104910234A (en) | 2015-05-26 | 2015-05-26 | Preparation method of ganodermanontriol |
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| CN201510270095.3A CN104910234A (en) | 2015-05-26 | 2015-05-26 | Preparation method of ganodermanontriol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112125934A (en) * | 2020-09-25 | 2020-12-25 | 福建福迩金生物科技有限公司 | Extraction method of triterpenoid alcohol compound |
-
2015
- 2015-05-26 CN CN201510270095.3A patent/CN104910234A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112125934A (en) * | 2020-09-25 | 2020-12-25 | 福建福迩金生物科技有限公司 | Extraction method of triterpenoid alcohol compound |
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Application publication date: 20150916 |
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| WD01 | Invention patent application deemed withdrawn after publication |