CN102329356A - Method for preparing chrysin-7-glucoside - Google Patents
Method for preparing chrysin-7-glucoside Download PDFInfo
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- CN102329356A CN102329356A CN201110210617A CN201110210617A CN102329356A CN 102329356 A CN102329356 A CN 102329356A CN 201110210617 A CN201110210617 A CN 201110210617A CN 201110210617 A CN201110210617 A CN 201110210617A CN 102329356 A CN102329356 A CN 102329356A
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- chrysin
- glycosides
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Abstract
The invention discloses a method for preparing chrysin-7-glucoside, which comprises the following steps of: crushing Malus sieboldii leaves, adding an aqueous solution in an amount which is 5 to 15 times weight of the crushed Malus sieboldii leaves, performing refluxing reaction for 2 to 3 times, filtering an extracting solution, concentrating under reduced pressure until the density is 1.02-1.05, adding 95 percent ethanol in a volume which is 2 to 3 times that of the concentrated solution for alcohol precipitation, removing a precipitate, adding active carbon into liquid for refluxing decolorization, filtering out the active carbon, concentrating until the volume is 1/2-1/4 of the original volume, regulating the pH to be 3-4, standing for crystallization, filtering out crystals, dissolving by using an ethanol solution, recrystallizing for 2 to 3 times, and drying to obtain the product. The method is simple and feasible and is suitable for industrial production; and the obtained product has high content.
Description
Technical field
The invention belongs to the natural product chemistry field, especially relate to a kind of preparation method of chrysin glycosides.
Background technology
The chrysin glycosides is a Flavonoid substances, is dissolved in basic soln, methyl alcohol, ethanol, acetone etc., is insoluble to sherwood oil, chloroform etc.The chrysin glycosides is to change into aglycon through hydrolysis in animal body, has anti-oxidant, antiviral, hypertension, hypoglycemic and antitumor action.
Siebold Crabapple has another name called Fruit of Pashi Pear, is rosaceous plant.Contain multiple nutritional components such as flavonoid, terpenoid, amino acid in the leaf of Malus sieboldii Mill, wherein flavonoid chrysin glycosides has anti-oxidant, antiviral, hypertension, hypoglycemic and diuretic properties.What be concerned by people especially is that its meta-bolites has tumor prevention and therapeutic action.But mostly leaf is to be used as fertilizer handles.
Existing chrysin glycosides preparation technology discloses less, is generally organic reagent and extracts.Like " the HPLC method is measured chrysin glycosides content in the leaf of Malus sieboldii Mill ", the document is taked the acetone supersound extraction, polyamide column ethanol gradient elution on the dry sample, condensing crystal, acetone recrystallization.This method adopts acetone extraction, and solvent boiling point is low, and is serious to operator and environmental hazard, the dry sample upper prop, and fractional dose is less, only suitable Laboratory Production.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of chrysin glycosides, this method is fit to suitability for industrialized production.
The objective of the invention is to realize through following technical scheme:
A kind of preparation method of chrysin glycosides is characterized in that: get leaf of Malus sieboldii Mill and pulverize, add 5-15 times of water gaging solution refluxing extraction 2-3 time; Extracting liquid filtering is evaporated to density 1.02-1.05, adds 2-3 times of volume of ethanol alcohol precipitation, removes deposition; Liquid adds the gac reflux decolour, leaches gac, is concentrated into the 1/2-1/4 volume; Regulate pH3-4 and place crystallization, crystallisate leaches uses dissolve with ethanol solution recrystallization 2-3 time again, is drying to obtain product.
Said amount of activated is the 1-3% of amount of liquid.
Sour optional hydrochloric acid or the sulphuric acid soln of said adjusting pH.
Advantage of the present invention is: the present invention adopts leaf of Malus sieboldii Mill to produce the chrysin glycosides, and raw material resources are abundant, still a kind of way that turns waste into wealth; Whole technological operation is simple, and toxicological harmless reagent uses, and is easy to suitability for industrialized production.
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 leaf of Malus sieboldii Mill and pulverize, take by weighing 5kg, add 50kg aqueous solution refluxing extraction 2 hours, filtering liq adds 40kg water refluxing extraction 2 hours again; Merge the filtration of extracted twice liquid and be evaporated to density 1.02, add 95% ethanol alcohol precipitation of 2 times of volumes, fully stir; Left standstill several hours, and removed deposition, liquid adds 1% gac reflux decolour 2 hours; Leach gac, be concentrated into 1/3 volume, hydrochloric acid is regulated pH3 and is placed crystallization; Crystallisate leaches and uses 75% dissolve with ethanol solution recrystallization 3 times again, dry yellow Siebold Crabapple glycosides 176g, the performance liquid detection level 98.5% of getting.
Embodiment 2:
Get leaf of Malus sieboldii Mill and pulverize, take by weighing 5kg, add 75kg aqueous solution refluxing extraction 2 hours, filtering liq adds 25kg water refluxing extraction 2 hours again; Merge the filtration of extracted twice liquid and be evaporated to density 1.05, add 95% ethanol alcohol precipitation of 3 times of volumes, fully stir; Left standstill several hours, and removed deposition, liquid adds 3% gac reflux decolour 2 hours; Leach gac, be concentrated into 1/2 volume, sulfuric acid is regulated pH3 and is placed crystallization; Crystallisate leaches and uses 70% dissolve with ethanol solution recrystallization 2 times again, dry yellow Siebold Crabapple glycosides 187g, the performance liquid detection level 98.1% of getting.
Embodiment 3:
Get leaf of Malus sieboldii Mill and pulverize, take by weighing 10kg, add 100kg aqueous solution refluxing extraction 2 hours, filtering liq adds 70kg water refluxing extraction 2 hours again; Merge the filtration of extracted twice liquid and be evaporated to density 1.04, add 95% ethanol alcohol precipitation of 3 times of volumes, fully stir; Left standstill several hours, and removed deposition, liquid adds 2% gac reflux decolour 2 hours; Leach gac, be concentrated into 1/4 volume, sulfuric acid is regulated pH4 and is placed crystallization; Crystallisate leaches and uses 90% dissolve with ethanol solution recrystallization 3 times again, dry yellow Siebold Crabapple glycosides 381g, the performance liquid detection level 98.3% of getting.
Embodiment 4:
Get leaf of Malus sieboldii Mill and pulverize, take by weighing 10kg, add 50kg aqueous solution refluxing extraction 2 hours, extract three times; Extracting liquid filtering is evaporated to density 1.02, adds 95% ethanol alcohol precipitation of 3 times of volumes, fully stirs; Left standstill several hours, and removed deposition, liquid adds 2% gac reflux decolour 2 hours; Leach gac, be concentrated into 1/2 volume, hydrochloric acid is regulated pH4 and is placed crystallization; Crystallisate leaches and uses 80% dissolve with ethanol solution recrystallization 2 times again, dry yellow Siebold Crabapple glycosides 375g, the performance liquid detection level 98.7% of getting.
Claims (3)
1. the preparation method of a chrysin glycosides is characterized in that: get leaf of Malus sieboldii Mill and pulverize, add 5-15 times of water gaging solution refluxing extraction 2-3 time; Extracting liquid filtering is evaporated to density 1.02-1.05, adds 95% ethanol alcohol precipitation of 2-3 times of volume, removes deposition; Liquid adds the gac reflux decolour, leaches gac, is concentrated into the 1/2-1/4 volume; Regulate pH3-4 and place crystallization, crystallisate leaches uses dissolve with ethanol solution recrystallization 2-3 time again, is drying to obtain product.
2. a kind of according to claim 1 preparation method of chrysin glycosides is characterized in that said amount of activated is the 1-3% of amount of liquid.
3. a kind of according to claim 1 preparation method of chrysin glycosides is characterized in that sour optional hydrochloric acid or the sulphuric acid soln of said adjusting pH.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110210617A CN102329356A (en) | 2011-07-26 | 2011-07-26 | Method for preparing chrysin-7-glucoside |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110210617A CN102329356A (en) | 2011-07-26 | 2011-07-26 | Method for preparing chrysin-7-glucoside |
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| CN102329356A true CN102329356A (en) | 2012-01-25 |
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| CN201110210617A Pending CN102329356A (en) | 2011-07-26 | 2011-07-26 | Method for preparing chrysin-7-glucoside |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5851792A (en) * | 1996-04-03 | 1998-12-22 | Shen; Jerome | Aglucone isoflavone enriched vegetable protein whey whey protein material aglucone isoflavone material high genistein content material and high daidzein content material and process for producing the same from a vegetable protein whey |
| WO2001051482A1 (en) * | 2000-01-11 | 2001-07-19 | Biorex Health Limited | Extraction of flavonoids |
| CN101880300A (en) * | 2010-04-27 | 2010-11-10 | 南京泽朗农业发展有限公司 | Purification process of geniposide |
| CN102070684A (en) * | 2010-12-24 | 2011-05-25 | 南京泽朗医药科技有限公司 | Method for extracting syringin |
-
2011
- 2011-07-26 CN CN201110210617A patent/CN102329356A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5851792A (en) * | 1996-04-03 | 1998-12-22 | Shen; Jerome | Aglucone isoflavone enriched vegetable protein whey whey protein material aglucone isoflavone material high genistein content material and high daidzein content material and process for producing the same from a vegetable protein whey |
| WO2001051482A1 (en) * | 2000-01-11 | 2001-07-19 | Biorex Health Limited | Extraction of flavonoids |
| CN101880300A (en) * | 2010-04-27 | 2010-11-10 | 南京泽朗农业发展有限公司 | Purification process of geniposide |
| CN102070684A (en) * | 2010-12-24 | 2011-05-25 | 南京泽朗医药科技有限公司 | Method for extracting syringin |
Non-Patent Citations (2)
| Title |
|---|
| 刘峰: "黄芩中黄芩苷的提取工艺研究", 《西北药学杂志》 * |
| 江星明: "HPLC 法测定三叶海棠叶中白杨素苷含量", 《湖南中医药大学学报》 * |
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Application publication date: 20120125 |
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