CN103421071A - Preparation method of high-purity ganodermanontriol - Google Patents
Preparation method of high-purity ganodermanontriol Download PDFInfo
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- CN103421071A CN103421071A CN2013103602287A CN201310360228A CN103421071A CN 103421071 A CN103421071 A CN 103421071A CN 2013103602287 A CN2013103602287 A CN 2013103602287A CN 201310360228 A CN201310360228 A CN 201310360228A CN 103421071 A CN103421071 A CN 103421071A
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Abstract
The invention discloses a preparation method of high-purity ganodermanontriol. The preparation method includes: crushing lucid ganoderma material, adding 5-10 times of dosage of 50-99% methanol solution, ultrasonically extracting for two to three times, adding macroporous resin columns into condensate extract for adsorption, eluting with 3-9 times of dosage of 10-50% ethanol solution, eluting with 5-10 times of dosage of 60-90% ethanol solution, condensing eluent to adjust pH to 1-3, adding petroleum ether, mixing well, collecting a petroleum ether layer and filtering, separating obtained solid with a high-speed counter current chromatograph, and collecting fraction for drying under reduced pressure. The preparation method of high-purity ganodermanontriol is simple to operate, high in yield, low in pollution and suitable for production of high-purity ganodermanontriol.
Description
Technical field
The invention belongs to the Natural Medicine Chemistry field, particularly a kind of preparation method of high purity glossy ganoderma ketone triol.
Background technology
Glossy ganoderma ketone triol is triterpene compound, CAS 106518-63-2, and molecular formula C30H48O4, molecular weight 4722.7, molecular structural formula is as follows:
Glossy ganoderma ketone triol is the triterpenes components in glossy ganoderma, and triterpenes is also one of effective constituent of glossy ganoderma, and human liver cancer cell is had to cytotoxicity, also can suppress the release of histamine, has hepatoprotective effect and has anti-allergic effects etc.
By literature search, existing glossy ganoderma ketone triol preparation method adopts silica gel, gel chromatography to divide ethanol to put forward refluxing extraction, ethyl acetate extraction, and silica gel, gel chromatography such as are separated at the step.Due to complicated operation, preparation amount is less, and the sample yield is low, is not suitable for the preparation of high purity glossy ganoderma ketone triol.
Summary of the invention
The objective of the invention is to solve shortcomings and deficiencies of the prior art, a kind of preparation method of high purity glossy ganoderma ketone triol easy and simple to handle is provided.
To achieve these goals, the present invention is by the following technical solutions:
A kind of preparation method of high purity glossy ganoderma ketone triol, it is characterized in that following steps: get glossy ganoderma raw material raw material pulverizing, add 5-10 doubly to measure the 50%-99% methanol solution, supersound extraction 2-3 time, add in macroporous resin column and adsorb after the extracting solution contracting, first with 3-9, doubly measure 10%-50% methanol solution wash-out, again with 5-10 times of 60%-90% methanol solution wash-out, the concentrated ph1-3 that regulates of elutriant, add sherwood oil fully to stir, the collection petroleum ether layer filters, and the gained solid separates with high-speed counter-current chromatograph, collects the flow point drying under reduced pressure and get final product.
A kind of in the optional HZ816 of described macroporous resin, HPD100, AB-8 and D101.
Described high-speed counter-current chromatograph separation condition is: get stone chloroform, methyl alcohol, water, press 3-7:2-5:1-3 and mix, get the phase that fixes mutually, lower be moving phase mutually, engine speed 700-1000rpm, flow velocity is 1-3ml/min.
Adopt this law to prepare glossy ganoderma ketone triol, simple process is easy to operate, and preparation amount is large, and the product yield is high, and low the pollution.
Further illustrate the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment
Embodiment 1:
Get the glossy ganoderma raw material pulverizing, claim 20kg, by 8 times of 90% methanol solution supersound extraction 30 minutes, extract 3 times, add after the extracting solution concentrating under reduced pressure in the HZ816 macroporous resin column and adsorb, with 5 times of column volumes, 50% methanol solution wash-out, use 8 times of column volumes, 85% methanol solution wash-out, the concentrated ph1 that regulates of elutriant, add sherwood oil fully to stir again, the collection petroleum ether layer filters, and obtains the solids crude extract.Get chloroform, methyl alcohol, water, press 3:2:1 and mix, fully after layering, get and fill with mutually the high speed adverse current chromatogram pipe phase that fixes, open and turn main frame, rotating speed 800rpm, pump into the lower stream phasing of doing mutually, after setting up running balance, flow rate regulation is 2ml/min simultaneously, dissolve medicinal extract by moving phase, by the sampling valve sample introduction, the light scattering detector on-line monitoring, collect target component, continuous production, flow point reclaims reagent, obtain glossy ganoderma ketone triol 1.2g, detect content 98.5% through HPLC.
Embodiment 2:
Get the glossy ganoderma raw material pulverizing, claim 20kg, by 7 times of 80% methanol solution supersound extraction 30 minutes, extract 2 times, add after the extracting solution concentrating under reduced pressure in the D101 macroporous resin column and adsorb, with 6 times of column volumes, 30% methanol solution wash-out, use 8 times of column volumes, 80% methanol solution wash-out, the concentrated ph3 that regulates of elutriant, add sherwood oil fully to stir again, the collection petroleum ether layer filters, and obtains the solids crude extract.Get chloroform, methyl alcohol, water, press 5:3:2 and mix, fully after layering, get and fill with mutually the high speed adverse current chromatogram pipe phase that fixes, open and turn main frame, rotating speed 850rpm, pump into the lower stream phasing of doing mutually, after setting up running balance, flow rate regulation is 3ml/min simultaneously, dissolve medicinal extract by moving phase, by the sampling valve sample introduction, the light scattering detector on-line monitoring, collect target component, continuous production, flow point reclaims reagent, obtain glossy ganoderma ketone triol 1.3g, detect content 98.5% through HPLC.
Embodiment 3:
Get the glossy ganoderma raw material pulverizing, claim 20kg, by 7 times of 85% methanol solution supersound extraction 30 minutes, extract 2 times, add after the extracting solution concentrating under reduced pressure in the AB-8 macroporous resin column and adsorb, with 4 times of column volumes, 40% methanol solution wash-out, use 10 times of column volumes, 75% methanol solution wash-out, the concentrated ph2 that regulates of elutriant, add sherwood oil fully to stir again, the collection petroleum ether layer filters, and obtains the solids crude extract.Get chloroform, methyl alcohol, water, press 4:3:2 and mix, fully after layering, get and fill with mutually the high speed adverse current chromatogram pipe phase that fixes, open and turn main frame, rotating speed 700rpm, pump into the lower stream phasing of doing mutually, after setting up running balance, flow rate regulation is 1ml/min simultaneously, dissolve medicinal extract by moving phase, by the sampling valve sample introduction, the light scattering detector on-line monitoring, collect target component, continuous production, flow point reclaims reagent, obtain glossy ganoderma ketone triol 1.4g, detect content 98.3% through HPLC.
Embodiment 4:
Get the glossy ganoderma raw material pulverizing, claim 20kg, by 7 times of 95% methanol solution supersound extraction 30 minutes, extract 3 times, add after the extracting solution concentrating under reduced pressure in the HPD100 macroporous resin column and adsorb, with 5 times of column volumes, 50% methanol solution wash-out, use 10 times of column volumes, 70% methanol solution wash-out, the concentrated ph1 that regulates of elutriant, add sherwood oil fully to stir again, the collection petroleum ether layer filters, and obtains the solids crude extract.Get chloroform, methyl alcohol, water, press 4:2:2 and mix, fully after layering, get and fill with mutually the high speed adverse current chromatogram pipe phase that fixes, open and turn main frame, rotating speed 850rpm, pump into the lower stream phasing of doing mutually, after setting up running balance, flow rate regulation is 2ml/min simultaneously, dissolve medicinal extract by moving phase, by the sampling valve sample introduction, the light scattering detector on-line monitoring, collect target component, continuous production, flow point reclaims reagent, obtain glossy ganoderma ketone triol 1.3g, detect content 97.7% through HPLC.
Claims (3)
1. the preparation method of a high purity glossy ganoderma ketone triol, it is characterized in that following steps: get glossy ganoderma raw material raw material pulverizing, add 5-10 doubly to measure the 50%-99% methanol solution, supersound extraction 2-3 time, add in macroporous resin column and adsorb after the extracting solution contracting, first with 3-9, doubly measure 10%-50% methanol solution wash-out, again with 5-10 times of 60%-90% methanol solution wash-out, the concentrated ph1-3 that regulates of elutriant, add sherwood oil fully to stir, the collection petroleum ether layer filters, and the gained solid separates with high-speed counter-current chromatograph, collects the flow point drying under reduced pressure and get final product.
2. the preparation method of high purity glossy ganoderma ketone triol according to claim 1, is characterized in that a kind of in the optional HZ816 of described macroporous resin, HPD100, AB-8 and D101.
3. the preparation method of high purity glossy ganoderma ketone triol according to claim 1, it is characterized in that described high-speed counter-current chromatograph separation condition is: get stone chloroform, methyl alcohol, water, pressing 3-7:2-5:1-3 mixes, get the phase that fixes mutually, lower mutually for moving phase, engine speed 700-1000rpm, flow velocity is 1-3ml/min.
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| CN2013103602287A CN103421071A (en) | 2013-08-19 | 2013-08-19 | Preparation method of high-purity ganodermanontriol |
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| CN2013103602287A CN103421071A (en) | 2013-08-19 | 2013-08-19 | Preparation method of high-purity ganodermanontriol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107625794A (en) * | 2017-09-28 | 2018-01-26 | 广东省微生物研究所（广东省微生物分析检测中心） | Purposes of the ganoderma lucidum alcohol extract in the preparation for preparing prevention and/or treatment Alzheimer's disease |
-
2013
- 2013-08-19 CN CN2013103602287A patent/CN103421071A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107625794A (en) * | 2017-09-28 | 2018-01-26 | 广东省微生物研究所（广东省微生物分析检测中心） | Purposes of the ganoderma lucidum alcohol extract in the preparation for preparing prevention and/or treatment Alzheimer's disease |
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Application publication date: 20131204 |
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| WD01 | Invention patent application deemed withdrawn after publication |