CN104910246A - Cucurbitacins preparation method - Google Patents
Cucurbitacins preparation method Download PDFInfo
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- CN104910246A CN104910246A CN201510281030.9A CN201510281030A CN104910246A CN 104910246 A CN104910246 A CN 104910246A CN 201510281030 A CN201510281030 A CN 201510281030A CN 104910246 A CN104910246 A CN 104910246A
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- raw material
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- hemsleyadin
- extraction
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J71/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton is condensed with a heterocyclic ring
- C07J71/0005—Oxygen-containing hetero ring
-
- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention discloses a cucurbitacins preparation method, which comprises: 1) taking a Hemsleya chinensis raw material, crushing, adding to a supercritical CO2 extraction kettle, setting the temperature of 30-50 DEG C and the pressure of 15-25 MPa, introducing liquid-state CO2, concurrently introducing methanol as an entrainer, extracting for 30-150 min, and resolving to obtain an extract, wherein the liquid-state CO2 flow rate is 1-5 ml/min/g of raw material, and the methanol flow rate is 0.1-0.3 ml/min/g; and 2) carrying out hot dissolving on the extract with ethanol, adding an equal volume of petroleum ether, adding a proper amount of an aqueous solution, collecting the petroleum ether layer to recover the reagent, adding an ethanol solution to carry out reflux dissolving, adding active carbon to decolorize, carrying out concentration crystallization on the decolorizing solution, re-crystallizing with an ethanol solution, and drying to obtain the finished product. The cucurbitacins preparation method of the present invention has characteristics of high extraction efficiency, simple purification process, and environmental protection, and is suitable for industrial production.
Description
Technical field
The invention belongs to biological technical field, particularly relate to a kind of preparation method of Hemsleyadin first.
Background technology
Hemsleyadin first, English name Cucurbitacins, molecular formula C30H42O6, molecular weight 498.656, CAS 60137-06-6, molecular structural formula:
Hymsleya amabilis is Curcurbitaceae Genus Hemsleya plant, has heat reliving and toxin-eliminating, effect of antisepsis and anti-inflammation.Be used for the treatment of bacillary dysentery, enteritis, bronchitis, acute tonsillitis.Hymsleya amabilis stem tuber contains Hemsleyadin first, Hemsleyadin second, panax japonicus saponin, Oleanolic Acid-β-glucose ester etc.Wherein Hemsleyadin is main function composition, and Hemsleyadin is the mixture of Hemsleyadin first and the Hemsleyadin second extracted in Curcurbitaceae Genus Hemsleya plant.Hemsleyadin first has clearing heat and detoxicating, the function of antisepsis and anti-inflammation.Mostly the technique of existing extraction Hemsleyadin is that extraction using alcohol extraction into ethyl acetate, extraction using alcohol macroporous resin are separated or organic reagent extracts silicagel column separation etc.Find no the processing method preparing Hemsleyadin first to disclose.
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 Hemsleyadin first is provided.
To achieve these goals, the present invention is by the following technical solutions:
A preparation method for Hemsleyadin first, is characterized in that following steps:
1) get hymsleya amabilis raw material pulverizing, add SCF-CO 2 still, set temperature 30 ~ 50 DEG C, pressure 15 ~ 25MPa, pass into liquid CO 2, flow is 1 ~ 5ml/min/g raw material, passes into methyl alcohol simultaneously and does entrainment agent, flow is 0.1 ~ 0.3ml/min/g, and extraction 30-150min, resolves to obtain extract;
2) suitable quantity of water solution is added again after above-mentioned extract ethanol thermosol adds equal-volume sherwood oil, collect petroleum ether layer and reclaim reagent, then add activated carbon decolorizing, destainer condensing crystal after adding ethanolic soln backflow dissolving, use ethanolic soln recrystallization again, be drying to obtain.
Overcritical SCF-CO 2 described in step 1) is: extraction temperature 50 DEG C, pressure 21MPa, and liquid CO 2 flow is 2ml/min/g raw material, and passing into methanol flow is 0.3ml/min/g, extraction 100min.
Advantage of the present invention is: adopt SCF-CO 2, efficiency is high, and the cycle is short, extracts product purity high, is easy to purifying, and environmental protection.
Embodiment
Embodiment 1:
Get 2kg hymsleya amabilis raw material pulverizing 60 order, drop into SCF-CO 2 still, pass into liquid CO 2, flow is 2ml/min/g raw material, pass into methyl alcohol and do entrainment agent, flow is 0.3ml/min/g, at pressure 21MPa, under the condition of temperature 50 C, extraction 100min, resolve to obtain extract, after adding equal-volume sherwood oil with 90% ethanol thermosol, add 1/3 v aqueous solution again, abundant mixing, static layering, collect petroleum ether layer and reclaim reagent, gac reflux decolour is added after dissolving with 90% ethanolic soln backflow again, concentrated 1/4 volume of destainer places crystallization, crystallisate uses 95% ethanolic soln recrystallization again, dry Hemsleyadin first 6g, detect through high performance liquid phase, content 98.3%.
Embodiment 2:
Get 2kg hymsleya amabilis raw material pulverizing 60 order, drop into SCF-CO 2 still, pass into liquid CO 2, flow is 1ml/min/g raw material, pass into methyl alcohol and do entrainment agent, flow is 0.2ml/min/g, at pressure 25MPa, under the condition of temperature 45 C, extraction 60min, resolve to obtain extract, after adding equal-volume sherwood oil with 95% ethanol thermosol, add 1 times of v aqueous solution again, abundant mixing, static layering, collect petroleum ether layer and reclaim reagent, after dissolving with 95% ethanolic soln backflow again, add gac reflux decolour, concentrated 1/4 volume of destainer places crystallization, crystallisate uses 90% ethanolic soln recrystallization again, dry Hemsleyadin first 5.6g, detect through high performance liquid phase, content 97.3%.
Embodiment 3:
Get 2kg hymsleya amabilis raw material pulverizing 40 order, drop into SCF-CO 2 still, pass into liquid CO 2, flow is 5ml/min/g raw material, pass into methyl alcohol and do entrainment agent, flow is 0.1ml/min/g, at pressure 15MPa, under the condition that temperature is 30 DEG C, extraction 150min, resolve to obtain extract, after adding equal-volume sherwood oil with 95% ethanol thermosol, add 1/2 v aqueous solution again, abundant mixing, static layering, collect petroleum ether layer and reclaim reagent, after dissolving with 95% ethanolic soln backflow again, add gac reflux decolour, concentrated 1/3 volume of destainer places crystallization, crystallisate uses 95% ethanolic soln recrystallization again, dry Hemsleyadin first 6.7g, detect through high performance liquid phase, content 97.5%.
Claims (2)
1. a preparation method for Hemsleyadin first, is characterized in that following steps:
1) get hymsleya amabilis raw material pulverizing, add SCF-CO 2 still, set temperature 30 ~ 50 DEG C, pressure 15 ~ 25MPa, pass into liquid CO 2, flow is 1 ~ 5ml/min/g raw material, passes into methyl alcohol simultaneously and does entrainment agent, flow is 0.1 ~ 0.3ml/min/g, and extraction 30-150min, resolves to obtain extract;
2) suitable quantity of water solution is added again after above-mentioned extract ethanol thermosol adds equal-volume sherwood oil, collect petroleum ether layer and reclaim reagent, then add activated carbon decolorizing, destainer condensing crystal after adding ethanolic soln backflow dissolving, use ethanolic soln recrystallization again, be drying to obtain.
2. the preparation method of Hemsleyadin first according to claim 1, it is characterized in that the overcritical SCF-CO 2 described in step 1) is: extraction temperature 50 DEG C, pressure 21MPa, liquid CO 2 flow is 2ml/min/g raw material, and passing into methanol flow is 0.3ml/min/g, extraction 100min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510281030.9A CN104910246A (en) | 2015-05-28 | 2015-05-28 | Cucurbitacins preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510281030.9A CN104910246A (en) | 2015-05-28 | 2015-05-28 | Cucurbitacins preparation method |
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| Publication Number | Publication Date |
|---|---|
| CN104910246A true CN104910246A (en) | 2015-09-16 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510281030.9A Pending CN104910246A (en) | 2015-05-28 | 2015-05-28 | Cucurbitacins preparation method |
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| CN (1) | CN104910246A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111411099A (en) * | 2020-05-14 | 2020-07-14 | 云南农业大学 | Hemsleya amabilis acetyl transferase, coding gene thereof and application of hemsleya amabilis acetyl transferase in preparation of cucurbitacin |
-
2015
- 2015-05-28 CN CN201510281030.9A patent/CN104910246A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111411099A (en) * | 2020-05-14 | 2020-07-14 | 云南农业大学 | Hemsleya amabilis acetyl transferase, coding gene thereof and application of hemsleya amabilis acetyl transferase in preparation of cucurbitacin |
| CN111411099B (en) * | 2020-05-14 | 2022-09-27 | 云南农业大学 | Hemsleya amabilis acetyl transferase, coding gene thereof and application of hemsleya amabilis acetyl transferase in preparation of cucurbitacin |
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| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150916 |