CN102241711A - Preparation method of rhapontin - Google Patents
Preparation method of rhapontin Download PDFInfo
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- CN102241711A CN102241711A CN2011101178690A CN201110117869A CN102241711A CN 102241711 A CN102241711 A CN 102241711A CN 2011101178690 A CN2011101178690 A CN 2011101178690A CN 201110117869 A CN201110117869 A CN 201110117869A CN 102241711 A CN102241711 A CN 102241711A
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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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- Medicines Containing Plant Substances (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to a preparation method of rhapontin. The preparation method comprises: crushing dried Polygonaceae Rheum herbs into coarse powder, placing the coarse powder in an extraction kettle for supercritical CO2 extraction, collecting the extract in a separation kettle, adding a base liquid for dissolving, filtering out insoluble substances, filtering the filtrate through an ultrafiltration membrane, collecting the permeate liquid, then concentrating the collected liquid by use of a nanofiltration membrane, adjusting the pH value of the concentrate for crystallization, filtering out the crystal, and recrystallizing by virtue of ethanol and water to obtain a product. The preparation method of rhapontin provided by the invention has the advantages of simplicity in technological operation, low energy consumption and easiness for realization of industrial production; and the obtained product is high in purity.
Description
Technical field:
The invention belongs to biological technical field, particularly relate to a kind of preparation method of ponticin, specifically relate to a kind of method that adopts supercritical extraction technique binding film isolation technique to prepare ponticin.
Background technology:
Ponticin:
Proterties: white, needle-shaped crystals, (254mn) is blue-fluorescence, FeCl under the ultraviolet lamp
3Reaction is blue black;
English name: (rhaponticin, rhaponitin or poniticin);
Chemical name: the 3-hydroxyl-5-[(1E)-and 2-(3-hydroxyl-4-p-methoxy-phenyl) vinyl] phenyl-β-D-glucoside;
Molecular formula: C
21H
24O
9
Molecular weight: 420;
Structural formula:
Ponticin is the derivative of toluylene.Mainly be present in the polygonaceae Rheum plant.Regulation can not detect ponticin under 2005 editions one rheum officinale item that records of Chinese Pharmacopoeia, generally believes that at present genuine rhubarb does not contain ponticin.Recent research show ponticin have antibiotic, microcirculation improvement, reducing blood-fat, hypoglycemic, antitumor, suppress anaphylaxis, regulate the immunity of organism system of defense, antithrombotic and effect such as anti-oxidant.Rheum officinale is geographic region such as Gansu, Ningxia kinds commonly used, owing to lack chemical reference substance, does not formulate content assaying method so far as yet.Be rational and effective exploitation resources of medicinal plant and uses thereof, and provide reference for further studying ponticin pharmacologically active mechanism of action, high-load ponticin extracts research and has bigger meaning.
The method of existing extraction ponticin is few, is mainly the method for column chromatography.Disclosed employing 90% alcohol reflux of document " Snowbell-leaf Tickelover Herb and the research of Radix Rumicis effective constituent and application ", concentrate the back aqueous precipitation, leach precipitation 95% dissolve with ethanol, solution adds the charcoal absorption removal of impurities, obtain product through macroporous resin purification and re-crystallization step again, this method adopts repeatedly refluxing extraction, and energy consumption is big, and last column operation sample loss is big.
Document " HPLC measures the ponticin content in the Rheum hotaoense C. Y. Cheng et C. T. Kao ", the document adopts 95% extraction using alcohol, concentrate the total medicinal extract of rheum officinale, make ponticin by soda acid removal of impurities repeatedly again, this method preparation process solvent usage quantity is big, and it is not high to make product purity.
Patent " a kind of method of from dock, extracting ponticin " (patent publication No.: CN 101475613), the method that this patent adopts is to be raw material with the dock, through pulverize, thermal backflow is extracted, filter, concentrate, extraction, macroporous resin adsorption and wash-out, concentrate, dry, get the ponticin extract, it is big that this method prepares the ponticin energy consumption.
Summary of the invention:
The technical problem to be solved in the present invention is the defective that overcomes traditional extraction technology, and a kind of preparation method of ponticin is provided, and this method is easy to operate, and energy consumption is low.
A kind of preparation method of ponticin, it is characterized in that may further comprise the steps: get polygonaceae Rheum dried plant and pulverize, place extraction kettle, sealing, set extraction, separate temperature required, pressure, open devices such as extractor, separator and carry out system warm-up, start high-pressure pump, feed a certain amount of properties-correcting agent, open CO
2The air inlet switch starts compression pump, makes pressure reach required scope, keep-up pressure extraction for some time, open separation reactor I, separation reactor I I, carry out lock out operation, collect extract, with the alkali lye dissolving, remove by filter insolubles, solution is added to and carries out ultrafiltration in the ultra-filtration equipment, seeing through liquid concentrates through nanofiltration membrane, concentrated solution adds dilute hydrochloric acid and is adjusted to pH5～7, and crystallization under normal temperature condition leaches crystal and promptly gets white, needle-shaped crystals with the alcohol-water recrystallization.
Described polygonaceae Rheum plant comprises rheum rhabarbarum, root and Rhizome of Sinkiang Rhubarb, North China rheum officinale etc.
Described extraction temperature is 35～45 ℃, and pressure is 25～35MPa, and the time is 1.5～3h, feeds CO
2Flow is 18～25L/h, and adding properties-correcting agent is ethanol, and consumption is 20～50% of a medicinal material amount.
Described separation reactor I temperature is 18～22 ℃, and pressure is 10～15MPa, and separation reactor I I temperature is 8～15 ℃, and pressure is 6～10MPa.
Described alkali lye is the sodium hydroxide or the potassium hydroxide solution of pH9～11.
Described ultrafiltration membrane permeate aperture is 5～15nm, and pressure is 0.5～1MPa.
It is 100～200 that described nanofiltration membrane sees through molecular weight, and pressure is 5～10MPa.
Beneficial effect of the present invention: adopt supercritical CO
2Extraction, energy consumption is low, extraction agent CO
2Cleanliness without any pollution, processing step is simple to operate, and fast, whole technology all adopts nontoxic reagent, and products obtained therefrom can be used for medicine, field of health care products.
Embodiment:
Embodiment 1:
Get rheum rhabarbarum medicine 1kg, pulverize, place extraction kettle, sealing, setting the extraction kettle temperature is 45 ℃, pressure is 25MPa, the separation reactor I temperature is 18 ℃, pressure is 15MPa, and separation reactor I I temperature is 8 ℃, and pressure is 10MPa, open devices such as extractor, separator and carry out system warm-up, start high-pressure pump, feed 200ml ethanol, open CO as properties-correcting agent
2The air inlet switch, start compression pump, make pressure reach required scope, extraction 1.5h keep-ups pressure, open separation reactor I, separation reactor I I carries out lock out operation, collects extract, sodium hydroxide solution dissolving with pH9, remove by filter insolubles, it is to carry out ultrafiltration in the 5nm ultra-filtration equipment that solution is added to the aperture, and seeing through pressure is 0.5MPa, seeing through liquid is that 200 nanofiltration membrane concentrates through seeing through molecular weight, seeing through pressure is 5MPa, and concentrated solution adds dilute hydrochloric acid and is adjusted to pH5, crystallization under normal temperature condition, leach crystal and promptly get white, needle-shaped crystals 18.4g, content 91.8% with 90% ethyl alcohol recrystallization.
Embodiment 2:
Get root and Rhizome of Sinkiang Rhubarb medicine 5kg, pulverize, place extraction kettle, sealing, setting the extraction kettle temperature is 35 ℃, pressure is 35MPa, the separation reactor I temperature is 20 ℃, pressure is 10MPa, and separation reactor I I temperature is 15 ℃, and pressure is 6MPa, open devices such as extractor, separator and carry out system warm-up, start high-pressure pump, feed 2.5L ethanol, open CO as properties-correcting agent
2The air inlet switch, start compression pump, make pressure reach required scope, extraction 3h keep-ups pressure, open separation reactor I, separation reactor I I carries out lock out operation, collects extract, potassium hydroxide solution dissolving with pH11, remove by filter insolubles, it is to carry out ultrafiltration in the 15nm ultra-filtration equipment that solution is added to the aperture, and seeing through pressure is 1MPa, seeing through liquid is that 100 nanofiltration membrane concentrates through seeing through molecular weight, seeing through pressure is 10MPa, and concentrated solution adds dilute hydrochloric acid and is adjusted to pH7, crystallization under normal temperature condition, leach crystal and promptly get white, needle-shaped crystals 7.4g, content 89.3% with 85% ethyl alcohol recrystallization.
Embodiment 3:
Get North China Elsholtzia 10kg, pulverize, place extraction kettle, sealing, setting the extraction kettle temperature is 38 ℃, pressure is 28MPa, the separation reactor I temperature is 20 ℃, pressure is 13MPa, and separation reactor I I temperature is 12 ℃, and pressure is 8MPa, open devices such as extractor, separator and carry out system warm-up, start high-pressure pump, feed 3L ethanol, open CO as properties-correcting agent
2The air inlet switch, start compression pump, make pressure reach required scope, extraction 2.5h keep-ups pressure, open separation reactor I, separation reactor I I carries out lock out operation, collects extract, sodium hydroxide solution dissolving with pH10, remove by filter insolubles, it is to carry out ultrafiltration in the 10nm ultra-filtration equipment that solution is added to the aperture, and seeing through pressure is 0.8MPa, seeing through liquid is that 200 nanofiltration membrane concentrates through seeing through molecular weight, seeing through pressure is 8MPa, and concentrated solution adds dilute hydrochloric acid and is adjusted to pH6, crystallization under normal temperature condition, leach crystal and promptly get white, needle-shaped crystals 21.5g, content 87.5% with 95% ethyl alcohol recrystallization.
Claims (2)
1. the preparation method of a ponticin, it is characterized in that may further comprise the steps: get polygonaceae Rheum dried plant and pulverize, place extraction kettle, sealing, set extraction, separate temperature required, pressure, open devices such as extractor, separator and carry out system warm-up, start high-pressure pump, feed a certain amount of properties-correcting agent, open CO
2The air inlet switch starts compression pump, makes pressure reach required scope, keep-up pressure extraction for some time, open separation reactor I, separation reactor I I, carry out lock out operation, collect extract, with the alkali lye dissolving, remove by filter insolubles, solution is added to and carries out ultrafiltration in the ultra-filtration equipment, seeing through liquid concentrates through nanofiltration membrane, concentrated solution adds acid and is adjusted to pH5～7, and crystallization under normal temperature condition leaches crystal and promptly gets white, needle-shaped crystals with the alcohol-water recrystallization.
2. the preparation method of a kind of ponticin as claimed in claim 1 is characterized in that described extraction temperature is 35～45 ℃, and pressure is 25～35MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101178690A CN102241711A (en) | 2011-05-06 | 2011-05-06 | Preparation method of rhapontin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101178690A CN102241711A (en) | 2011-05-06 | 2011-05-06 | Preparation method of rhapontin |
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| CN102241711A true CN102241711A (en) | 2011-11-16 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011101178690A Pending CN102241711A (en) | 2011-05-06 | 2011-05-06 | Preparation method of rhapontin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102702283A (en) * | 2012-05-08 | 2012-10-03 | 青海伊纳维康生物科技有限公司 | Method for quickly separating and preparing high-purity deoxyrhapontin and rhapontin |
| CN103421058A (en) * | 2012-05-25 | 2013-12-04 | 昆明制药集团股份有限公司 | Method used for separating and purifying deoxyrhaponticin with high efficiency and accuracy |
-
2011
- 2011-05-06 CN CN2011101178690A patent/CN102241711A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102702283A (en) * | 2012-05-08 | 2012-10-03 | 青海伊纳维康生物科技有限公司 | Method for quickly separating and preparing high-purity deoxyrhapontin and rhapontin |
| CN102702283B (en) * | 2012-05-08 | 2014-08-13 | 青海伊纳维康生物科技有限公司 | Method for quickly separating and preparing high-purity deoxyrhapontin and rhapontin |
| CN103421058A (en) * | 2012-05-25 | 2013-12-04 | 昆明制药集团股份有限公司 | Method used for separating and purifying deoxyrhaponticin with high efficiency and accuracy |
| CN103421058B (en) * | 2012-05-25 | 2015-12-02 | 昆药集团股份有限公司 | A kind of method of high-level efficiency clean cut separation purifying Rhapontin, deoxy- |
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Application publication date: 20111116 |