CN102060822A - Method for extracting esculetin from herba violae - Google Patents
Method for extracting esculetin from herba violae Download PDFInfo
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- CN102060822A CN102060822A CN2010106040108A CN201010604010A CN102060822A CN 102060822 A CN102060822 A CN 102060822A CN 2010106040108 A CN2010106040108 A CN 2010106040108A CN 201010604010 A CN201010604010 A CN 201010604010A CN 102060822 A CN102060822 A CN 102060822A
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- ethanol
- cichorigenin
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- violet herb
- philippine violet
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Abstract
The invention relates to a method for extracting esculetin from herba violae. The method comprises the following steps: using herba violae as a raw material to grind, adding 7-15 times of 60-90% ethanol to perform backflow extraction for 2-3 times; filtering, recycling ethanol under reduced pressure, diluting the concentrated solution with hot water; adding macroporous resin for adsorption; washing resin column with water to ensure that the solution has no caramel colour; using 4-6 BV of 50-80% ethanol to elute the active ingredient, recycling ethanol from eluent; adjusting the acidity of the hot solution for precipitation, filtering out the precipitate, dissolving the precipitate with ethyl acetate through refluxing; adding the solution in an aluminum peroxide column, recycling the obtained solution in a small-column container, and standing for crystallization; dissolving the obtained crystals with ethanol to perform refluxing and recrystallization; and drying the obtained crystals to obtain the esculetin product. By adopting the method to produce esculetin, the technology is simple, is easy to operate, has low production cost and high product purity.
Description
Technical field:
The present invention relates to a kind of extracting method of Cichorigenin, particularly relate to a kind of method of from Philippine Violet Herb, extracting Cichorigenin.
Background technology:
Cichorigenin is a coumarin kind compound, is aesculetin again, chemical name 6,7-dihydroxycoumarin, yellow needle crystal (rare alcohol), mp.268-270 ℃.Be soluble in methyl alcohol, ethanol and sodium hydroxide solution, dissolve in ethyl acetate and acetone soln, be dissolved in boiling water slightly, several ether, chloroform and water of being insoluble to.
That Cichorigenin has is antibiotic, anti-inflammatory and Antitussive and Expectorant Effect, and bacillary dysentery, acute enteritis are had better result of treatment, has antipyretic effect concurrently, and it is little that poison is paid effect, several no bitter tastes.
How the existing Cichorigenin that extracts extracts preparation from the bark of ash, owing to also contain similar materials such as Vitamin C2, fraxin and Fraxetin in the bark of ash, purifying is difficulty comparatively, and production cost is higher.Operational path gets ethanol extract for getting bark of ash meal alcohol reflux, and decompression and solvent recovery promptly gets general extractive to the medicinal extract shape.In above-mentioned medicinal extract, add water add thermosol it.Move in separating funnel, with equal-volume chloroform extraction secondary, after boiling off residual chloroform, the water layer that chloroform extraction is crossed adds equivalance ethyl acetate extraction secondary, combined ethyl acetate liquid, with anhydrous sodium sulfate dehydration, decompression and solvent recovery as for, residue is dissolved in the warm methyl alcohol, be concentrated in right amount, place crystallization, promptly have yellow needle crystal to separate out.Leach crystallization.Methyl alcohol, water is recrystallization repeatedly, promptly gets Cichorigenin.Patent " a kind of preparation method of Cortex Fraxini extract and purposes " for another example, the method of this patent disclosure is to adopt water boiling and extraction, and the macroporous resin separation and purification prepares the cortex fraxini coumarin composition, obtains the mixture of tonka bean camphor in the bark of ash, this method adopts water extraction, and extraction efficiency and yield are all very low.Because bark of ash resource is cut down everywhere now, destroy seriously, and growth cycle is longer, resource is comparatively nervous, and price is higher.
The Philippine Violet Herb per nnial herb, spring, Qiu Erji gather, and the roadside, field all can be planted, and not only can beautify the environment but also can be used as medicinal material and use.The Philippine Violet Herb herb contains glucoside, flavonoid, coumarins etc., and wherein Cichorigenin content is about 0.3%.The method of extracting Cichorigenin from Philippine Violet Herb is less, is mostly scientific research.As " research of water-soluble chemical component in the Philippine Violet Herb " and " Philippine Violet Herb The Chemical Constituents ", two pieces of documents all are to adopt with alcohol to soak extraction, underpressure distillation, behind the hot water dissolving, its suspension extracts with ethyl acetate, gets the ethyl acetate part, purification by silica gel column chromatography.These class methods are not suitable for suitability for industrialized production.
Summary of the invention:
The technical problem to be solved in the present invention provides a kind of industrial method that extracts Cichorigenin from Philippine Violet Herb, and technology is simple to operation.
In order to solve the problems of the technologies described above the object of the present invention is achieved like this:
A kind of method of extracting Cichorigenin from Philippine Violet Herb is characterized in that may further comprise the steps:
1) get the Philippine Violet Herb raw material, pulverizing adds 7-15 and doubly measures the 60-90% alcohol reflux 2-3 time, filters, and decompression recycling ethanol gets concentrated solution;
2) above-mentioned concentrated solution adds hot water dilution back and adds macroporous resin adsorption, and the washed resin post does not have fried sugar, gets 4-6BV50-80% ethanol elution effective constituent again, and elutriant reclaims ethanol, and precipitation is placed in acid adjustment while hot;
3) above-mentioned throw out leaches, the ethyl acetate backflow dissolving, and peroxidation aluminium post is crossed post liquid and is recycled to small volume placement crystallization;
4) leach above-mentioned crystallisate, the alcohol reflux dissolving concentrates small volume crystallization 1-2 time, the dry Cichorigenin product that gets.
Described step 2) a kind of among the optional ADS-17 of macroporous resin model, LSA-7, HZ806 or the AB-8.Preferred ADS-17 macroporous resin.
Described step 2) used sour optional hydrochloric acid and phosphoric acid in, adjusting acidity is pH1-3.Preferred 10% aqueous hydrochloric acid.
Aluminum oxide is an acidic alumina in the described step 3), and granularity is the 120-300 order.
Ethanol is the 40-99% ethanolic soln in the described step 4).
Why the present invention adopts Philippine Violet Herb is raw material, because Philippine Violet Herb is cheap and easy to get, and other tonka bean camphor component contents are lower, are easy to purifying.
The present invention adopts macroporous resin and alumina column in conjunction with removal of impurities, because macroporous resin has enrichment and removes the sugar effect, aluminum oxide has stronger adsorptivity to polarity flavones and glycosides, removed flavonoid impurity, effect better and silicagel column and extraction comparison have industrialized advantage.
Further specify 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 Philippine Violet Herb raw material pulverizing, get 1kg, add the 10kg60% alcohol reflux 2 times, the each extraction 2 hours, filter extracting solution, decompression recycling ethanol, concentrated solution adds the absorption of HZ806 (resin 500ml) macroporous resin column after adding the hot water dilution, absorption washes resin column earlier with water to there not being fried sugar after finishing, and gets 3L50% ethanol elution effective constituent again, elutriant reclaims ethanol, regulate pH1 with 10% hydrochloric acid soln while hot and place precipitation, throw out leaches, the ethyl acetate backflow dissolving, peracidity alumina (aluminum oxide 120-300 order, consumption 80g), crosses post liquid and be recycled to 1/5 volume placement crystallization, leach crystallisate, be concentrated into 1/3 volume crystallization 2 times after the dissolving of 60% alcohol reflux, crystallisate leaches, dry Cichorigenin light yellow crystal 2.1g, the content detection 95.2% of getting.
Embodiment 2:
Get the Philippine Violet Herb raw material pulverizing, get 1kg, add the 7kg90% alcohol reflux 3 times, the each extraction 1 hour filters the extracting solution decompression recycling ethanol, concentrated solution adds the absorption of LSA-7 (resin 600ml) macroporous resin column after adding the hot water dilution, absorption washes resin column earlier with water to there not being fried sugar after finishing, and gets 2.4L80% ethanol elution effective constituent again, elutriant reclaims ethanol, regulate pH3 with 10% hydrochloric acid soln while hot and place precipitation, throw out leaches, the ethyl acetate backflow dissolving, the conventional post post of peracidity aluminum oxide (aluminum oxide 120-300 order, consumption 100g), crosses post liquid and be recycled to 1/6 volume placement crystallization, leach crystallisate, be concentrated into 1/5 volume crystallization after the dissolving of 90% alcohol reflux, crystallisate leaches, dry Cichorigenin light yellow crystal 1.8g, the content detection 92.6% of getting.
Embodiment 3:
Get the Philippine Violet Herb raw material pulverizing, get 10kg, drop into 500L stainless steel extractor, add the 100kg80% alcohol reflux 2 times, extracted 2 hours at every turn, filter, extracting solution decompression recycling ethanol, concentrated solution add the absorption of ADS-17 (resin 5L) macroporous resin column after adding the hot water dilution, after absorption finishes, wash resin column earlier with water to there not being fried sugar, get 25L65% ethanol elution effective constituent again, elutriant reclaims ethanol, regulates pH1 with 10% hydrochloric acid soln while hot and places precipitation, throw out leaches, the ethyl acetate backflow dissolving, the conventional post post (aluminum oxide 120-300 order, consumption 1kg) of peracidity aluminum oxide, cross post liquid and be recycled to 1/4 volume placement crystallization, leach crystallisate, be concentrated into 1/3 volume crystallization twice after the dissolving of 80% alcohol reflux, crystallisate leaches, dry Cichorigenin light yellow crystal 21.5g, the content detection 98.2% of getting.
Embodiment 4:
Get the Philippine Violet Herb raw material pulverizing, get 10kg, drop into 500L stainless steel extractor, add the 100kg80% alcohol reflux 2 times, extracted 2 hours at every turn, filter, extracting solution decompression recycling ethanol, concentrated solution add the absorption of AB-8 (resin 7L) macroporous resin column after adding the hot water dilution, after absorption finishes, wash resin column earlier with water to there not being fried sugar, get 35L65% ethanol elution effective constituent again, elutriant reclaims ethanol, regulates pH2 with 10% hydrochloric acid soln while hot and places precipitation, throw out leaches, the ethyl acetate backflow dissolving, the conventional post post (aluminum oxide 120-300 order, consumption 1kg) of peracidity aluminum oxide, cross post liquid and be recycled to 1/4 volume placement crystallization, leach crystallisate, be concentrated into 1/3 volume crystallization twice after the dissolving of 80% alcohol reflux, crystallisate leaches, dry Cichorigenin light yellow crystal 17.5g, the content detection 92.3% of getting.
Claims (5)
1. method of extracting Cichorigenin from Philippine Violet Herb is characterized in that may further comprise the steps:
1) get the Philippine Violet Herb raw material, pulverizing adds 7-15 and doubly measures the 60-90% alcohol reflux 2-3 time, filters, and decompression recycling ethanol gets concentrated solution;
2) above-mentioned concentrated solution adds hot water dilution back and adds macroporous resin adsorption, and the washed resin post does not have fried sugar, gets 4-6BV50-80% ethanol elution effective constituent again, and elutriant reclaims ethanol, and precipitation is placed in acid adjustment while hot;
3) above-mentioned throw out leaches, the ethyl acetate backflow dissolving, and peroxidation aluminium post is crossed post liquid and is recycled to small volume placement crystallization;
4) leach above-mentioned crystallisate, the alcohol reflux dissolving concentrates small volume crystallization 1-2 time, the dry Cichorigenin product that gets.
2. according to the described method of from Philippine Violet Herb, extracting Cichorigenin of claim 1, it is characterized in that described step 2) a kind of among the optional ADS-17 of macroporous resin model, LSA-7, HZ806 or the AB-8.
3. according to the described method of from Philippine Violet Herb, extracting Cichorigenin of claim 1, it is characterized in that described step 2) in used sour optional hydrochloric acid and phosphoric acid, adjusting acidity is pH1-3.
4. according to the described method of extracting Cichorigenin from Philippine Violet Herb of claim 1, it is characterized in that aluminum oxide is an acidic alumina in the described step 3), granularity is the 120-300 order.
5. according to the described method of from Philippine Violet Herb, extracting Cichorigenin of claim 1, it is characterized in that ethanol is the 40-99% ethanolic soln in the described step 4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106040108A CN102060822A (en) | 2010-12-24 | 2010-12-24 | Method for extracting esculetin from herba violae |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106040108A CN102060822A (en) | 2010-12-24 | 2010-12-24 | Method for extracting esculetin from herba violae |
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| CN102060822A true CN102060822A (en) | 2011-05-18 |
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| CN2010106040108A Pending CN102060822A (en) | 2010-12-24 | 2010-12-24 | Method for extracting esculetin from herba violae |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408522A (en) * | 2013-08-22 | 2013-11-27 | 乐山师范学院 | Method for extracting high-purity aesculetin from euphorbia lathyris fruit |
| CN104316607A (en) * | 2014-09-25 | 2015-01-28 | 广东广发制药有限公司 | Method for determining content of esculetin in Herba Violae medicinal material |
| CN105770207A (en) * | 2014-12-26 | 2016-07-20 | 鲁南厚普制药有限公司 | Herba violae extract and application thereof |
| CN106120139A (en) * | 2016-07-15 | 2016-11-16 | 浙江真爱时尚家居有限公司 | A kind of production technology of tencel fiber woollen blanket |
| CN106167952A (en) * | 2016-07-15 | 2016-11-30 | 浙江真爱时尚家居有限公司 | A kind of production technology of soft wire protein fiber woollen blanket |
-
2010
- 2010-12-24 CN CN2010106040108A patent/CN102060822A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408522A (en) * | 2013-08-22 | 2013-11-27 | 乐山师范学院 | Method for extracting high-purity aesculetin from euphorbia lathyris fruit |
| CN103408522B (en) * | 2013-08-22 | 2015-10-28 | 乐山师范学院 | A kind of method extracting high-purity aesculetin from Euphorbia lathyris fruit |
| CN104316607A (en) * | 2014-09-25 | 2015-01-28 | 广东广发制药有限公司 | Method for determining content of esculetin in Herba Violae medicinal material |
| CN105770207A (en) * | 2014-12-26 | 2016-07-20 | 鲁南厚普制药有限公司 | Herba violae extract and application thereof |
| CN105770207B (en) * | 2014-12-26 | 2020-09-18 | 鲁南厚普制药有限公司 | Viola yedoensis makino extract and application thereof |
| CN106120139A (en) * | 2016-07-15 | 2016-11-16 | 浙江真爱时尚家居有限公司 | A kind of production technology of tencel fiber woollen blanket |
| CN106167952A (en) * | 2016-07-15 | 2016-11-30 | 浙江真爱时尚家居有限公司 | A kind of production technology of soft wire protein fiber woollen blanket |
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Application publication date: 20110518 |