CN102391219A - Method for preparing blinin from golden Chinese gentian - Google Patents
Method for preparing blinin from golden Chinese gentian Download PDFInfo
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- CN102391219A CN102391219A CN2011103141154A CN201110314115A CN102391219A CN 102391219 A CN102391219 A CN 102391219A CN 2011103141154 A CN2011103141154 A CN 2011103141154A CN 201110314115 A CN201110314115 A CN 201110314115A CN 102391219 A CN102391219 A CN 102391219A
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- blinin
- artemisia santonica
- extract
- methanol solution
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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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- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The invention discloses a method for preparing blinin from golden Chinese gentian. The method comprises the following steps of: a, crushing the golden Chinese gentian into 60-80 meshes, adding the crushed product into a supercritical extraction kettle, introducing liquid CO2 and performing supercritical extraction for 2-3 hours under an extraction pressure of 15-25MPa at a temperature of 40-60 DEG C; and analyzing under a pressure of 5-10MPa at a temperature of 50-60 DEG C to obtain an extract; b, dispersing the extract with hot water, adding into macroporous resin for adsorption, eluting with an aqueous solution of ethanol, collecting the eluent and concentrating to obtain a precipitate; and c, dissolving the precipitate with chloroform, filtering, adding a proper amount of methanol solution, refrigerating and crystallizing, filtering and crystallizing, and re-crystallizing with methanol solution for 2-3 times, and drying to obtain the blinin. When the method disclosed by the invention is used for producing blinin, the technological flow is simple and easy to operate, the extraction efficiency is high, the preparation quantity is large, and industrial production is easy to realize.
Description
Technical field
The present invention relates to a kind ofly prepare the plain method of Artemisia santonica, particularly relate to a kind of method that adopts supercritical CO 2 extraction and Amberlyst process to prepare the Artemisia santonica element from conyza blinii from conyza blinii.
Background technology
Artemisia santonica plain (Blinin) is a terpenoid, molecular formula: C
22H
32O
6, molecular weight: 392.49, structural formula:
The Artemisia santonica element is white, needle-shaped crystals (acetone), is dissolved in sherwood oil, chloroform, is slightly soluble in methyl alcohol, acetone.Discover that the Artemisia santonica element has strong anti-inflammatory action.The Artemisia santonica element also is as the index property composition of weighing the medicinal material conyza blinii.
Conyza blinii is the herb of the little Artemisia santonica Conyza of the false fluffy platymiscium of composite family blinii Levl, and traditional medicine thinks that the conyza blinii nature and flavor are bitter, cold, and removing heat-phlegm is relieving cough and asthma, detoxification and promoting urination, the effect of cooling blood for hemostasis.Be usually used in being used for the cough due to lung-heat, phlegm is panted more, pharyngalgia, and aphtha, jaundice due to damp-heat, bleeding from five sense organs or subcutaneous tissue is had blood in stool, uterine bleeding, traumatic hemorrhage.
Through literature search, the general organic reagent of method for preparing artabsin extracts, and separates obtaining the Artemisia santonica element again with silicagel column through extraction.After all being the employing alcohol reflux like document " conyza blinii chemical ingredients and antiulcer activity research (I) " thereof and " conyza blinii hang down polarity part chemical constitution study ", behind sherwood oil, chloroform extraction, the silicagel column separation obtains the Artemisia santonica element repeatedly.As stated, existing preparation Artemisia santonica element method, technology is loaded down with trivial details, and the organic reagent usage quantity is big, and turnout is less, is not suitable for suitability for industrialized production, has restricted the plain application of Artemisia santonica.
Summary of the invention
The objective of the invention is to overcome the defective and the deficiency of prior art, provide a kind of and prepare the plain simple method of Artemisia santonica from conyza blinii.
The objective of the invention is to realize: a kind ofly prepare the plain method of Artemisia santonica, it is characterized in that following steps from conyza blinii through following technical scheme:
A gets conyza blinii and pulverizes the 60-80 order, adds in the supercritical extraction reactor, under extracting pressure 15-25MPa, temperature 40-60 ℃ condition, feeds the liquid CO 2 supercritical extraction 2-3 hour, at pressure 5-10MPa, temperature 50-60 ℃ of parsing, extract;
The above-mentioned extract of b disperses with hot water, adds in the macroporous resin to adsorb, and the aqueous ethanolic solution wash-out is collected elutriant and concentrated, and gets throw out;
C uses dissolved in chloroform to above-mentioned throw out, filters, and adds an amount of methanol solution, and the refrigeration crystallization leaches crystallization, uses methanol solution recrystallization 2-3 time again, is drying to obtain the Artemisia santonica element.
A kind of among the optional AB-8 of macroporous resin described in the step b, HZ816, D101 and the HPD100.
Ethanolic soln gradient elution described in the step b is: get the ethanol elution impurity of 4-8BV20-60% earlier, use 3-8BV70-95% ethanolic soln wash-out again.
Advantage of the present invention is: adopted the supercritical CO 2 extraction, solvent for use is that CO2 can recycle, does not pollute, and extraction time is short, and efficient is high; Method has also adopted the macroporous resin separation, and is simple to operate, and treatment capacity is bigger, is easy to suitability for industrialized production.
Embodiment
To combine embodiment to further specify the present invention below.
Embodiment 1:
Pulverize 60 orders behind the conyza blinii raw material drying, get 5kg and add in the supercritical extraction reactor, feed liquid CO 2; Be arranged on 50 ℃ of extracting pressure 15MPa, temperature, reach above-mentioned parameter after, adjustment liquid CO 2 flow velocity is 20kg/h; Dynamic extraction 3 hours; At pressure 5MPa, temperature transfers part to resolve down for 50 ℃, obtains extract 120g.Extract adds 2L hot water and disperse to add in the resin column that the 500gAB-8 resin is housed and adsorb, and gets the ethanol elution impurity of 4BV60%, uses 5BV 90% ethanolic soln wash-out effective constituent again, collects the elutriant concentrating under reduced pressure, places deposition.The throw out thing leaches with 100ml chloroform ultrasonic dissolution, filters, and adds the 20ml methanol solution, and the refrigeration crystallization leaches crystallization, uses the methanol solution recrystallization again 2 times, is drying to obtain the plain 8.5g of Artemisia santonica, detects content 98.1% through HPLC.
Embodiment 2:
Pulverize 80 orders behind the conyza blinii raw material drying, get 5kg and add in the supercritical extraction reactor, feed liquid CO 2; Be arranged on 60 ℃ of extracting pressure 19MPa, temperature, reach above-mentioned parameter after, adjustment liquid CO 2 flow velocity is 25kg/h; Dynamic extraction 2 hours; At pressure 8MPa, temperature transfers part to resolve down for 60 ℃, obtains extract 130g.Extract adds 2L hot water and disperse to add in the resin column that 500g HZ816 resin is housed and adsorb, and gets the ethanol elution impurity of 5BV50%, uses 5BV 80% ethanolic soln wash-out effective constituent again, collects the elutriant concentrating under reduced pressure, places deposition.The throw out thing leaches with 100ml chloroform ultrasonic dissolution, filters, and adds the 30ml methanol solution, and the refrigeration crystallization leaches crystallization, uses the methanol solution recrystallization again 3 times, is drying to obtain the plain 6.2g of Artemisia santonica, detects content 98.8% through HPLC.
Embodiment 3:
Pulverize 60 orders behind the conyza blinii raw material drying, get 5kg and add in the supercritical extraction reactor, feed liquid CO 2; Be arranged on 50 ℃ of extracting pressure 25MPa, temperature, reach above-mentioned parameter after, adjustment liquid CO 2 flow velocity is 20kg/h; Dynamic extraction 3 hours; At pressure 6MPa, temperature transfers part to resolve down for 50 ℃, obtains extract 110g.Extract adds 2L hot water and disperse to add in the resin column that 500g D101 resin is housed and adsorb, and gets the ethanol elution impurity of 6BV40%, uses 8BV75% ethanolic soln wash-out effective constituent again, collects the elutriant concentrating under reduced pressure, places deposition.The throw out thing leaches with 80ml chloroform ultrasonic dissolution, filters, and adds the 30ml methanol solution, and the refrigeration crystallization leaches crystallization, uses the methanol solution recrystallization again 3 times, is drying to obtain the plain 5.6g of Artemisia santonica, detects content 97.2% through HPLC.
Claims (3)
1. one kind prepares the plain method of Artemisia santonica from conyza blinii, it is characterized in that following steps:
A gets conyza blinii and pulverizes the 60-80 order, adds in the supercritical extraction reactor, under extracting pressure 15-25MPa, temperature 40-60 ℃ condition, feeds the liquid CO 2 supercritical extraction 2-3 hour, at pressure 5-10MPa, temperature 50-60 ℃ of parsing, extract;
The above-mentioned extract of b disperses with hot water, adds in the macroporous resin to adsorb, and the aqueous ethanolic solution wash-out is collected elutriant and concentrated, and gets throw out;
C uses dissolved in chloroform to above-mentioned throw out, filters, and adds an amount of methanol solution, and the refrigeration crystallization leaches crystallization, uses methanol solution recrystallization 2-3 time again, is drying to obtain the Artemisia santonica element.
2. according to claim 1ly prepare the plain method of Artemisia santonica, it is characterized in that a kind of among the optional AB-8 of the macroporous resin described in the step b, HZ816, D101 and the HPD100 from conyza blinii.
3. according to claim 1ly prepare the plain method of Artemisia santonica, it is characterized in that the ethanolic soln gradient elution described in the step b is: get the ethanol elution impurity of 4-8BV20-60% earlier, use 3-8BV70-95% ethanolic soln wash-out again from conyza blinii.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103141154A CN102391219A (en) | 2011-10-17 | 2011-10-17 | Method for preparing blinin from golden Chinese gentian |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103141154A CN102391219A (en) | 2011-10-17 | 2011-10-17 | Method for preparing blinin from golden Chinese gentian |
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| CN102391219A true CN102391219A (en) | 2012-03-28 |
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| CN2011103141154A Pending CN102391219A (en) | 2011-10-17 | 2011-10-17 | Method for preparing blinin from golden Chinese gentian |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106221281A (en) * | 2016-07-27 | 2016-12-14 | 韦罡 | A kind of natural plants Herba Acroptili repentis condensed cream and its preparation method and application |
| CN110960573A (en) * | 2019-12-24 | 2020-04-07 | 曹敏 | A fel Ursi extract, and its preparation method and application |
| CN115448968A (en) * | 2022-09-26 | 2022-12-09 | 贵州汇腾萃取技术应用研究院有限责任公司 | Supercritical CO 2 Method for extracting stigmasterol by combining method with chromatographic technology |
-
2011
- 2011-10-17 CN CN2011103141154A patent/CN102391219A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106221281A (en) * | 2016-07-27 | 2016-12-14 | 韦罡 | A kind of natural plants Herba Acroptili repentis condensed cream and its preparation method and application |
| CN110960573A (en) * | 2019-12-24 | 2020-04-07 | 曹敏 | A fel Ursi extract, and its preparation method and application |
| CN115448968A (en) * | 2022-09-26 | 2022-12-09 | 贵州汇腾萃取技术应用研究院有限责任公司 | Supercritical CO 2 Method for extracting stigmasterol by combining method with chromatographic technology |
| CN115448968B (en) * | 2022-09-26 | 2024-04-05 | 贵州汇腾萃取技术应用研究院有限责任公司 | Supercritical CO 2 Method for extracting stigmasterol by combining chromatography technology |
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Application publication date: 20120328 |