CN102344473A - Preparation method of gentian active ingredient - Google Patents
Preparation method of gentian active ingredient Download PDFInfo
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- CN102344473A CN102344473A CN2010102471383A CN201010247138A CN102344473A CN 102344473 A CN102344473 A CN 102344473A CN 2010102471383 A CN2010102471383 A CN 2010102471383A CN 201010247138 A CN201010247138 A CN 201010247138A CN 102344473 A CN102344473 A CN 102344473A
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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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Abstract
The invention relates to a preparation method of gentiopicroside. The method has simple operations, little pollution and small equipment investment and comprises technological steps of: adding gentian and rhizome powder into a CO2 supercritical extractor; extracting for 2-2.5 h with methanol as an entrainer to obtain an extract; absorbing the extract through a macroporous polymeric adsorbent; washing with 60-90% ethanol; collecting an eluent of 3-8 times of a column volume; recovering ethanol with reduced pressure and concentrating; and adding ethyl acetate for crystallization. The gentiopicroside prepared by the method of the invention has high product purity and is apt to realization of industrialized amplification.
Description
Technical field
The present invention relates to a kind of preparation method of rough gentian effective constituent, especially a kind of method of utilizing the supercritical extraction gentiopicrin.
Background technology
Gentiopicrin (Gentiopicroside)
Molecular formula: C
16H
20O
9
Molecular weight: 356.329
Structural formula:
Physico-chemical property: white, needle-shaped crystals has the color reaction of lactone glycoside compound.
Gentiopicrin is a kind of natural compounds, has desinsection, antimalarial isoreactivity, extensively is present in the Gentianaceae various plants.
In the prior art, the extraction separation of gentiopicrin mainly adopts organic solvent method etc., but the Determination of gentiopicroside that these extraction processes obtain is low, and extraction efficiency is low, and is seriously polluted in the production process, and unfavorable big production operation.Chinese patent CN101070335 " a kind of method for preparing high-purity gentiopicrin " has announced a kind of method for preparing the small batch gentiopicrin with high performance counter current chromatograph; Industrial scale is little; And solvent systems is complicated, and contains chloroform, is prone to make troubles and potential safety hazard to aftertreatment.
Summary of the invention
It is short that technical problem to be solved by this invention provides a kind of extraction time, and treatment capacity is bigger, the preparation method of the gentiopicrin that product purity is high.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
1) supercritical extraction: get rough gentian root and rhizome powder, join in the CO2 supercritical extraction device, methyl alcohol is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 1-4%, and extraction 2-2.5h gets extract;
2) macroporous resin adsorption: extract with deionized water and ethanol stepwise elution, keeps ethanol eluate through absorption with macroporous adsorbent resin, and decompression recycling ethanol also concentrates, and gets medicinal extract;
3) crystallization: add the ethyl acetate crystallization, separate, wash, be drying to obtain.
Above-mentioned preparation method is characterized in that said extraction conditions: pressure is 10-40Mpa, and temperature is 40-50 ℃, CO
2Flow is 2BV/h.
Above-mentioned preparation method, the model that it is characterized in that said macroporous adsorbent resin are one or more of AB-8, H-103, D-101.
Above-mentioned preparation method, the alcohol concn that it is characterized in that said wash-out macroporous adsorptive resins is 60-90%.
Above-mentioned preparation method, it is colourless to it is characterized in that said deionized water is eluted to effluent liquid.
Above-mentioned preparation method, the amount that it is characterized in that said collection macroporous adsorptive resins elutriant are 5 times of amount column volumes.
In sum, there is following advantage in the present invention: supercritical extraction speed is higher than general solvent extraction efficient, and solvent is easily separated, can not make the product decomposition loss; The macroporous resin normal-temperature operation has been removed water-soluble impurity more up hill and dale through stepwise elution, the more environmental protection of the some other technology of solvent ratio.
To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment:
Embodiment 1
Get rough gentian root and rhizome powder 100g, join CO
2In the supercritical extraction device, methyl alcohol is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 1%, extracting pressure 10MPa, 40 ℃ of temperature, CO
2Flow 2BV/h; Extraction time 2h; Get extract, through the AB-8 absorption with macroporous adsorbent resin, 90% ethanol elution; Collect the elutriant of 3 times of column volume amounts; Decompression recycling ethanol also concentrates, and adds the ethyl acetate crystallization, separates, washs, is drying to obtain gentiopicrin 5.43g; Detect through HPLC, purity is 98.7%.
Embodiment 2
Get rough gentian root and rhizome powder 100g, join CO
2In the supercritical extraction device, methyl alcohol is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 2%, extracting pressure 40MPa, 45 ℃ of temperature, CO
2Flow 2BV/h; Extraction time 2h; Get extract, through the H-103 absorption with macroporous adsorbent resin, 80% ethanol elution; Collect the elutriant of 8 times of column volume amounts; Decompression recycling ethanol also concentrates, and adds the ethyl acetate crystallization, separates, washs, is drying to obtain gentiopicrin 7.25g; Detect through HPLC, purity is 98.4%.
Embodiment 3
Get rough gentian root and rhizome powder 100g, join CO
2In the supercritical extraction device, methyl alcohol is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 4%, extracting pressure 15MPa, 45 ℃ of temperature, CO
2Flow 2BV/h; Extraction time 2.5h; Get extract, through the D101 absorption with macroporous adsorbent resin, 60% ethanol elution; Collect the elutriant of 5 times of column volume amounts; Decompression recycling ethanol also concentrates, and adds the ethyl acetate crystallization, separates, washs, is drying to obtain gentiopicrin 7.68g; Detect through HPLC, purity is 99.1%.
Claims (6)
1. the preparation method of a rough gentian effective constituent is characterized in that described method comprises the following steps:
1) supercritical extraction: get rough gentian root and rhizome powder, join CO
2In the supercritical extraction device, methyl alcohol is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 1-4%, and extraction 2-2.5h gets extract;
2) macroporous resin adsorption: extract with deionized water and ethanol stepwise elution, keeps ethanol eluate through absorption with macroporous adsorbent resin, and decompression recycling ethanol also concentrates, and gets medicinal extract;
3) crystallization: add the ethyl acetate crystallization, separate, wash, be drying to obtain.
2. according to the said preparation method of claim 1, it is characterized in that said extraction conditions: pressure is 10-40Mpa, and temperature is 40-50 ℃, CO
2Flow is 2BV/h.
3. according to the said preparation method of claim 1, the model that it is characterized in that said macroporous adsorbent resin is one or more among AB-8, H-103, the D-101.
4. according to the said preparation method of claim 1, the alcohol concn that it is characterized in that said wash-out macroporous adsorptive resins is 60-90%.
5. according to the said preparation method of claim 1, it is colourless to it is characterized in that said deionized water is eluted to effluent liquid.
6. according to the said preparation method of claim 1, the amount that it is characterized in that said collection macroporous adsorptive resins elutriant is that 3-8 doubly measures column volume.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102471383A CN102344473A (en) | 2010-08-06 | 2010-08-06 | Preparation method of gentian active ingredient |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102471383A CN102344473A (en) | 2010-08-06 | 2010-08-06 | Preparation method of gentian active ingredient |
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| CN102344473A true CN102344473A (en) | 2012-02-08 |
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| CN2010102471383A Pending CN102344473A (en) | 2010-08-06 | 2010-08-06 | Preparation method of gentian active ingredient |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709216A (en) * | 2013-12-10 | 2014-04-09 | 大兴安岭嘉迪欧营养原料有限公司 | Novel method for extracting gentiopicrin from wild gentian |
| CN103860639A (en) * | 2014-03-25 | 2014-06-18 | 中国科学院西北高原生物研究所 | Application of Gentiana tizuensis Franch. flower extracts in preparation of medicament for treating cardiovascular system diseases |
| WO2021213484A1 (en) * | 2020-04-24 | 2021-10-28 | 珠海岐微生物科技有限公司 | Application of radix gentianae macrophyllae and monomer compound thereof in killing mites |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704865A (en) * | 2009-10-22 | 2010-05-12 | 南京泽朗医药科技有限公司 | Method for preparing gentiopicroside |
-
2010
- 2010-08-06 CN CN2010102471383A patent/CN102344473A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704865A (en) * | 2009-10-22 | 2010-05-12 | 南京泽朗医药科技有限公司 | Method for preparing gentiopicroside |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709216A (en) * | 2013-12-10 | 2014-04-09 | 大兴安岭嘉迪欧营养原料有限公司 | Novel method for extracting gentiopicrin from wild gentian |
| CN103860639A (en) * | 2014-03-25 | 2014-06-18 | 中国科学院西北高原生物研究所 | Application of Gentiana tizuensis Franch. flower extracts in preparation of medicament for treating cardiovascular system diseases |
| WO2021213484A1 (en) * | 2020-04-24 | 2021-10-28 | 珠海岐微生物科技有限公司 | Application of radix gentianae macrophyllae and monomer compound thereof in killing mites |
| CN115607589A (en) * | 2020-04-24 | 2023-01-17 | 珠海岐微生物科技有限公司 | Application of gentiana macrophylla and monomer compound thereof in mite killing |
| CN115607589B (en) * | 2020-04-24 | 2024-06-04 | 广州岐微生物医药科技有限公司 | Application of gentiana macrophylla and monomer compound thereof in mite killing |
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Addressee: Suzhou Ruilanbo TCM Technology Development Co., Ltd. Document name: Notification that Application Deemed to be Withdrawn |
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Application publication date: 20120208 |