CN101759689A - Preparation method of mangiferin - Google Patents
Preparation method of mangiferin Download PDFInfo
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- CN101759689A CN101759689A CN200910234065A CN200910234065A CN101759689A CN 101759689 A CN101759689 A CN 101759689A CN 200910234065 A CN200910234065 A CN 200910234065A CN 200910234065 A CN200910234065 A CN 200910234065A CN 101759689 A CN101759689 A CN 101759689A
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- mangiferin
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Abstract
The invention relates to a preparation method of mangiferin. The preparation method adopts the process steps of saturated limewater solution soaking and extraction, macroporous resin adsorption, stepwise elution of water and ethanol solution of different concentration, concentration and crystallization under reduced pressure, and recrystallization by adjusting acidity through methanol. The obtained product has the advantages of high purity, high yield and low cost. The process is easy to popularize and industrialize.
Description
Technical field:
The present invention relates to a kind of preparation method of Mangiferin, operations such as especially a kind of potass extraction, macroporous resin removal of impurities, acid adjustment crystallization prepare the method for Mangiferin.
Background technology:
Mangiferin
Molecular formula: C
19H
18O
11
Molecular weight: 422.33
Character: claim mangiferin again, the tabernaemontanus bulrush asphonin.Light lark needle crystal (50% ethanol).267～27 ℃ of fusing points.Specific rotation+43.3 ° (c=0.9, pyridine), 32 ° (ethanol).Slightly be dissolved in methyl alcohol, ethanol, water, dissolve in hot dilute methanol, hot Diluted Alcohol, be insoluble to non-polar solvent.
Mangiferin has the central nervous system of inhibition, anti-inflammatory, antibacterial, anti-herpes simplex virus, cholagogic and immunization, and liver injury has provide protection to the simulated high altitude acute hypoxia.Be mainly used in treatment trachitis and bronchitis.Ten application among the people divide extensively in Guangxi for Folium mangiferae treatment trachitis and bronchitis, and effect is remarkable.The surplus victory people of Guangxi ethnomedicine institute, Zhong Ming deliver the pharmacological action of having set forth Mangiferin in " Mangiferin pharmacological research progress " in " Chinese Chinese materia medica science and technology " 1999.6 (3).
Mangiferin is mainly derived from the Folium mangiferae and the rosaceous almond leaf of Anacardiaceae.Mango and almond distribute very extensive in Guangxi, mango and almond be as the main product cash crop in Guangxi, the most as fertilizer sources of its leaf and fuel.The pharmacological research of Mangiferin is more and more, and its effect is also extensively approved.The Mangiferin market outlook are very extensive.Mostly the method for the purifying of bibliographical information extraction at present Mangiferin is: decocting boils alcohol precipitation, methods such as ethanol-extracted resin separation purification.Mostly these methods are that yield is undesirable, cost is high, content is low.As Chinese patent CN1203083C " Rhizoma Anemarrhenae extract and preparation method thereof " and Chinese patent CN100475830C " preparation method of high purity mangiferin ", all used the extraction using alcohol operation in the disclosed method, increased product cost.
Summary of the invention:
The technical problem to be solved in the present invention provides a kind of Mangiferin system method.This method can reduce production costs, and improves product content, is convenient to the industrialization operation.
In order to solve the problems of the technologies described above, extractive technique scheme of the present invention is as follows:
The raw material pulverizing 30-60 order that will contain Mangiferin, add the saturated limewater solution soaking and extract, filter, it is 7～8 that solution is regulated pH, add macroporous resin column absorption, use the different solvents stepwise elution, contain the elutriant concentrating under reduced pressure of Mangiferin, place crystallization, get the Mangiferin crude product, Mangiferin crude product dissolve with methanol acid adjustment recrystallization, drying, promptly.
Contain a kind of in the Folium mangiferae of Anacardiaceae, rosaceous almond leaf of the raw material sources of Mangiferin, preferred almond leaf.
The immersion extraction conditions of Mangiferin is: adding the saturated limewater amount is that consumption is raw material weight 9-12 times, and soaking temperature 50-70 ℃, soak time 1-2 hour, soaking extraction time was 2-3 time.
Regulate a kind of of the optional hydrochloric acid of pH, sulfuric acid, phosphoric acid, preferred hydrochloric acid.
As the preparation method of claim 1 Mangiferin, it is characterized in that described macroporous resin column for can select a kind of of AB-8, ADS-17, X-5 for use, preferred AB-8
Macroporous resin different solvents stepwise elution operation is: at first with the removal of impurities of 6～8 times of amount column volume washing macroporous resins, then with 10～30% ethanol removal of impurities of 2～3 times of amount column volumes, at last with 4～5 times of amount column volume 60～70% ethanol elution Mangiferins.
Crystallization Procedure is: the Mangiferin elutriant is evaporated to ethanol degree 10-20 degree and places crystallization
The recrystallization operation is: the saturated dissolving of the methanol eddy of 60-70%, and regulate pH to 3-4 and place crystallization.
In sum, there is following advantage in the present invention:
1) utilize this parameter of adjusting solvent pH that extraction efficiency is improved.At first utilize Mangiferin in basic solvent relatively other components preferably solvability selection rate is improved, suitably add the stripping that heat soaking had not only improved the Mangiferin yield but also reduced impurity.
2) different solvents stepwise elution macroporous resin, removal of impurities is abundant.
3) the agent dissolves crystallization of different concns and adjusting PH, easier to be crystal formation, purity is higher
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:
The almond leaf is pulverized 30 orders, get 10kg (Mangiferin content 2.48%), add 120L saturated limewater solution and be heated to 50 ℃ of immersions 2 hours, soak and extract twice, it is 7 that united extraction liquid is regulated pH with hydrochloric acid, add the AB-8 macroporous resin column absorption of column volume 5L, with 30L water elution water-soluble impurity, use 10L30% ethanol elution alcohol dissolubility impurity more earlier, use 25L60% ethanol elution Mangiferin at last, the Mangiferin elutriant is concentrated into determining alcohol 20%, places crystallization, gets the Mangiferin coarse crystallization, dissolving refluxes in the methyl alcohol of Mangiferin coarse crystallization adding 60%, it is 3 that hydrochloric acid is regulated pH, places crystallization, finally obtains 206g content and be 96% Mangiferin finished product.
Embodiment 2:
Folium mangiferae is pulverized 50 orders, get 10kg (Mangiferin content 1.6%), add 100L saturated limewater solution and be heated to 60 ℃ of immersions 1.5 hours, soak and extract twice, it is 7.5 that united extraction liquid is regulated pH with sulfuric acid, add the AB-8 macroporous resin column absorption of column volume 5L, with 40L water elution water-soluble impurity, use 15L20% ethanol elution alcohol dissolubility impurity more earlier, use 20L70% ethanol elution Mangiferin at last, the Mangiferin elutriant is concentrated into determining alcohol 10%, places crystallization, gets the Mangiferin coarse crystallization, dissolving refluxes in the methyl alcohol of Mangiferin coarse crystallization adding 60%, it is 4 that hydrochloric acid is regulated pH, places crystallization, finally obtains 140g content and be 95% Mangiferin finished product.
Embodiment 3:
The almond leaf is crushed to 60 orders, get 10kg (Mangiferin content 2.2%), add 90L saturated limewater solution and be heated to 70 ℃ of immersions 1 hour, soak and extract twice, it is 8 that united extraction liquid is regulated pH with hydrochloric acid, add the AB-8 macroporous resin column absorption of column volume 5L, with 40L water elution water-soluble impurity, use 15L10% ethanol elution alcohol dissolubility impurity more earlier, use 25L60% ethanol elution Mangiferin at last, the Mangiferin elutriant is concentrated into determining alcohol 20%, places crystallization, gets the Mangiferin coarse crystallization, dissolving refluxes in the methyl alcohol of Mangiferin coarse crystallization adding 70%, it is 4 that hydrochloric acid is regulated pH, places crystallization, finally obtains 192g content and be 95.5% Mangiferin finished product.
Embodiment 4:
The almond leaf is crushed to 40 orders, get 10kg (Mangiferin content 2.4%), add 90L saturated limewater solution and be heated to 60 ℃ of immersions 1 hour, soak and extract twice, it is 7 that united extraction liquid is regulated pH with hydrochloric acid, add the AB-8 macroporous resin column absorption of column volume 5L, with 35L water elution water-soluble impurity, use 15L30% ethanol elution alcohol dissolubility impurity more earlier, use 20L65% ethanol elution Mangiferin at last, the Mangiferin elutriant is concentrated into determining alcohol 20%, places crystallization, gets the Mangiferin coarse crystallization, dissolving refluxes in the methyl alcohol of Mangiferin coarse crystallization adding 65%, it is 4 that phosphoric acid is regulated pH, places crystallization, finally obtains 200g content and be 96% Mangiferin finished product.
Claims (8)
1. the preparation method of a Mangiferin is characterized in that comprising following steps: will contain the raw material pulverizing 30-60 order of Mangiferin, and add the saturated limewater solution soaking and extract, it is 7～8 that the Mangiferin extracting solution is regulated pH, filter, add macroporous resin column absorption, use the different solvents stepwise elution, the elutriant concentrating under reduced pressure that contains Mangiferin, place crystallization, get the Mangiferin crude product, Mangiferin crude product dissolve with methanol acid adjustment recrystallization, drying promptly gets product.
2. preparation method as claimed in claim 1 is characterized in that described a kind of in the Folium mangiferae of Anacardiaceae, rosaceous almond leaf of the raw material sources of Mangiferin of containing
3. preparation method as claimed in claim 1 is characterized in that the immersion extraction conditions of described Mangiferin is: adding the saturated limewater amount is that consumption is raw material weight 9-12 times, and soaking temperature 50-70 ℃, soak time 1-2 hour, soaking extraction time was 2-3 time.
4. preparation method as claimed in claim 1 is characterized in that a kind of of the optional hydrochloric acid of described adjusting pH, sulfuric acid, phosphoric acid.
5. preparation method as claimed in claim 1, AB-8, ADS-17, X-5's is a kind of in order selecting for use to it is characterized in that described macroporous resin column
6. preparation method as claimed in claim 1, it is characterized in that described macroporous resin stepwise elution operation is: at first with the removal of impurities of 6～8 times of amount column volume washing macroporous resins, then with 10～30% ethanol removal of impurities of 2～3 times of amount column volumes, at last with 4～5 times of amount column volume 60～70% ethanol elution Mangiferins.
7. preparation method as claimed in claim 1 is characterized in that described placement Crystallization Procedure is: the Mangiferin elutriant is evaporated to ethanol degree 10-20 degree and places crystallization.
8. preparation method as claimed in claim 1 is characterized in that described recrystallization operation is: the saturated dissolving of the methanol eddy of 60-70%, and regulate pH to 2-3 and place crystallization.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910234065A CN101759689A (en) | 2009-11-20 | 2009-11-20 | Preparation method of mangiferin |
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| CN200910234065A CN101759689A (en) | 2009-11-20 | 2009-11-20 | Preparation method of mangiferin |
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| CN101759689A true CN101759689A (en) | 2010-06-30 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973985A (en) * | 2010-11-15 | 2011-02-16 | 广西中医学院 | Method for preparing mangiferin |
| CN106565693A (en) * | 2016-11-05 | 2017-04-19 | 林文练 | Method for extracting mangiferin |
| CN107266509A (en) * | 2017-07-20 | 2017-10-20 | 广西南宁桂知科技有限公司 | The technique that a kind of use mango leaf produces mangiferin |
| CN107383130A (en) * | 2017-07-20 | 2017-11-24 | 广西南宁桂知科技有限公司 | A kind of method that mangiferin is prepared using myrica rubra leaf |
| CN108892695A (en) * | 2018-09-27 | 2018-11-27 | 那坡康正天然植物提取有限责任公司 | A method of extracting mangiferin from mango leaf |
| CN109776515A (en) * | 2019-03-29 | 2019-05-21 | 广西工业职业技术学院 | The method of mangiferin is extracted from myrica rubra leaf |
| CN109912582A (en) * | 2019-03-29 | 2019-06-21 | 广西工业职业技术学院 | The method of mangiferin is extracted from mango leaf |
| CN113416182A (en) * | 2021-05-28 | 2021-09-21 | 西安金泰生物技术有限公司 | Mangiferin and preparation method thereof |
| CN113416183A (en) * | 2021-07-19 | 2021-09-21 | 永州德普瑞生物科技股份有限公司 | Method for extracting mangiferin from mango leaves |
-
2009
- 2009-11-20 CN CN200910234065A patent/CN101759689A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973985A (en) * | 2010-11-15 | 2011-02-16 | 广西中医学院 | Method for preparing mangiferin |
| CN101973985B (en) * | 2010-11-15 | 2013-06-05 | 广西中医学院 | Method for preparing mangiferin |
| CN106565693A (en) * | 2016-11-05 | 2017-04-19 | 林文练 | Method for extracting mangiferin |
| CN107266509A (en) * | 2017-07-20 | 2017-10-20 | 广西南宁桂知科技有限公司 | The technique that a kind of use mango leaf produces mangiferin |
| CN107383130A (en) * | 2017-07-20 | 2017-11-24 | 广西南宁桂知科技有限公司 | A kind of method that mangiferin is prepared using myrica rubra leaf |
| CN108892695A (en) * | 2018-09-27 | 2018-11-27 | 那坡康正天然植物提取有限责任公司 | A method of extracting mangiferin from mango leaf |
| CN109776515A (en) * | 2019-03-29 | 2019-05-21 | 广西工业职业技术学院 | The method of mangiferin is extracted from myrica rubra leaf |
| CN109912582A (en) * | 2019-03-29 | 2019-06-21 | 广西工业职业技术学院 | The method of mangiferin is extracted from mango leaf |
| CN113416182A (en) * | 2021-05-28 | 2021-09-21 | 西安金泰生物技术有限公司 | Mangiferin and preparation method thereof |
| CN113416182B (en) * | 2021-05-28 | 2022-03-29 | 西安金泰生物技术有限公司 | Mangiferin and preparation method thereof |
| CN113416183A (en) * | 2021-07-19 | 2021-09-21 | 永州德普瑞生物科技股份有限公司 | Method for extracting mangiferin from mango leaves |
| CN113416183B (en) * | 2021-07-19 | 2022-07-22 | 永州德普瑞生物科技股份有限公司 | Method for extracting mangiferin from mango leaves |
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Application publication date: 20100630 |