CN102002109A - Preparation method of dogwood polysaccharides - Google Patents
Preparation method of dogwood polysaccharides Download PDFInfo
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- CN102002109A CN102002109A CN2010105581135A CN201010558113A CN102002109A CN 102002109 A CN102002109 A CN 102002109A CN 2010105581135 A CN2010105581135 A CN 2010105581135A CN 201010558113 A CN201010558113 A CN 201010558113A CN 102002109 A CN102002109 A CN 102002109A
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Abstract
The invention relates to a preparation method of dogwood polysaccharides. The process comprises the following steps of: taking dry residues obtained after extracting total glucoside from dogwood pulp alcohol as a raw material, adding 5-10 (V/W) times of warm water, ultrasonically extracting for 1-2 h, combining the extracting solutions, concentrating, adding 30% of H2O2 and 3% trichloroacetic acid, centrifuging, taking the supernate, ultrafiltering, firstly adding a right amount of water into entrapped matter, then adding different concentrations of alcohol for fractional precipitation, filtering out high concentration alcohol precipitates and drying to obtain the product. The process has the advantages of simple operation, lower cost and higher purity and is beneficial to large production operation.
Description
Technical field:
The present invention relates to a kind of preparation method of skunk bush polysaccharide, especially a kind of method of utilizing supersound extraction, membrane sepn and fractionation precipitation to extract the purifying skunk bush polysaccharide.
Background technology:
Skunk bush (Fructus Corni) is the dry pulp of Cornaceae plant skunk bush Cornus Officinalis Sieb.et Zucc., has another name called Fructus Corni, medicine jujube, meat jujube etc.Be a kind of nourishing class rare medicinal herbs, have tonify the liver and kidney, effect that puckery essence is taken off admittedly.Recent study shows, skunk bush has anti-hemorrhagic shock, anticoagulant, immunomodulatory, anti-inflammatory, effect such as hypoglycemic, anti-oxidant, anticancer, antibiotic.Document " progress of skunk bush active chemical (Zhou Jinghua; Li Chunsheng, Li Diandong. Chinese Journal of New Drugs, 2001; 10 (11): 808.) " and " chemical research of skunk bush polysaccharide (Yang Yun; Liu Jianxin, Liu Cuiping, etc. CHINA JOURNAL OF CHINESE MATERIA MEDICA; 1999; 24 (10): 614.) ", clinical study proves that skunk bush is the main Chinese medicinal materials of treatment diabetes, coronary heart disease and essential hypertension.Modern study shows that main component has carbohydrate, organic acid and ester class, tannin class etc. in the skunk bush pulp, wherein polysaccharose substance is the indispensable important substance of life metabolism, have multiple biological activity, skunk bush polysaccharide has immunoregulatory activity and tangible antioxygenation.
The extracting method of relevant skunk bush polysaccharide reports that seldom method is relatively limited to.Existing method is that raw material degreasing, water are carried, concentrated, washing, drying, obtains product, and as " skunk bush polysaccharide extraction process and physico-chemical property researchs " such as Zhao Xiaohua, sherwood oil is used in degreasing, and consumption is big, toxicity is big; The used organic solvent kind of technology is many, causes effective constituent to run off easily.
Zhang Lijuans etc. " the extraction process optimization of skunk bush polysaccharide and to the cerebral ischemia re-pouring injured provide protection of the local kitchen range of rat ", document disclosed method are that ultrasonic water is carried, concentrated, ultrafiltration, alcohol precipitation, remove albumen, to wash dry gained skunk bush polysaccharide product purity not high.
Chinese patent " a kind of method of extracting skunk bush polysaccharide by zymohydrolysis " (application number: 200810120569.6), the method of this patent disclosure is to get the broken skunk bush dry powder that makes of skunk bush dried fruit digested tankage, adding quality is the distilled water of 15～60 times of skunk bush dry powder quality, add enzyme in 35～60 ℃, pH3.5～7.0 time enzymolysis 0.5h～4h, enzyme goes out after enzymolysis finishes, extracting solution concentrates alcohol precipitation, and centrifugal drying promptly gets the skunk bush polysaccharide extract, and product purity is low.
Summary of the invention:
Technical problem to be solved by this invention provides a kind of simple to operate, production safety, the skunk bush polysaccharide preparation method that purity is higher.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
A kind of preparation method of skunk bush polysaccharide is characterized in that comprising following steps:
1) extracts: the dry residue behind the total glycosides of skunk bush pulp alcohol extracting is added 5-10 doubly measure (V/W) warm water supersound extraction 1-2h, repeat 2-3 time, filter united extraction liquid;
2) removal of impurities: said extracted liquid concentrates, and adds an amount of 30%H
2O
2, to light yellow, it is muddy, centrifugal to no longer producing to add 3% Tricholroacetic Acid, gets supernatant liquor;
3) membrane sepn: the ultra-filtration membrane ultrafiltration of above-mentioned supernatant liquor gets trapped substance;
4) fractionation precipitation: above-mentioned trapped substance adds suitable quantity of water, adds 30% ethanol sedimentation earlier, and filtrate adds 50% ethanol again, filters, and filtrate adds 90% ethanol, generates precipitation, leaches precipitation and uses acetone, washing with alcohol successively, and vacuum-drying promptly gets the skunk bush polysaccharide product.
Warm water is 30-70 ℃ in the step 1), and ultrasonic frequency is 20KHz.
Step 2) H in
2O
2Consumption is the 1/4-1/2 of concentrated solution volume.
Ultra-filtration membrane is that molecular weight cut-off is 60000 hollow-fibre membrane in the step 3)
In sum, there is following advantage in the present invention: this process using warm water supersound extraction skunk bush polysaccharide, and solvent is simple; Used medicinal material is the residue behind the total glycosides of alcohol extracting, and cost is lower; Membrane sepn can effectively be removed small molecular weight impurity.
Adopt technique scheme to prepare skunk bush polysaccharide, simple to operate, cost is lower, and purity is higher, is beneficial to big production operation.
Below in conjunction with embodiment the present invention is further elaborated, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1
Get the dry residue 1kg behind the total glycosides of skunk bush pulp alcohol extracting, add 5L60 ℃ of warm water supersound extraction 2h, repeat united extraction liquid 3 times.Extracting solution is concentrated into 1/2 of original volume, is cooled to 25 ℃, adds 1.8L30%H
2O
2Stir, to light yellow, it is muddy to no longer producing to add 3% Tricholroacetic Acid, it is centrifugal to add whizzer, up to not having white suspendible from the liquid level intersection, tell clarified liq, use the ultra-filtration membrane ultrafiltration, trapped substance adds 400ml water, add the 400ml30% ethanol sedimentation, filtrate adds 600ml50% ethanol again, filters, filtrate adds 1400ml90% ethanol, place precipitation, leach precipitation, use 200ml acetone, 150ml washing with alcohol successively, vacuum-drying, promptly get skunk bush polysaccharide 11.8g, detect through HPLC, purity is 91.5%.
Embodiment 2
Get the dry residue 1kg behind the total glycosides of skunk bush pulp alcohol extracting, add 10L30 ℃ of warm water supersound extraction 1h, repeat 2 times, united extraction liquid, extracting solution are concentrated into 1/2 of original volume, are cooled to 25 ℃, add 2.5L30%H
2O
2, stir, to light yellow, it is muddy to no longer producing to add 3% Tricholroacetic Acid, it is centrifugal to add whizzer, up to not having white suspendible from the liquid level intersection, tells clarified liq, uses the ultra-filtration membrane ultrafiltration, trapped substance adds 650ml water, adds the 650ml30% ethanol sedimentation, and filtrate adds 940ml50% ethanol again, filter, filtrate adds 2250ml90% ethanol, places precipitation, leach precipitation, use acetone, washing with alcohol successively, vacuum-drying, promptly get skunk bush polysaccharide 12..9g, detect through HPLC, purity is 95.6%.
Embodiment 3
Get the dry residue 1kg behind the total glycosides of skunk bush pulp alcohol extracting, add 8L70 ℃ of warm water supersound extraction 1.5h, repeat united extraction liquid 2 times.Extracting solution is concentrated into 1/2 of original volume, is cooled to 25 ℃, adds 3.8L30%H
2O
2, stir, to light yellow, it is muddy to no longer producing to add 3% Tricholroacetic Acid, it is centrifugal to add whizzer, up to not having white suspendible from the liquid level intersection, tells clarified liq, uses the ultra-filtration membrane ultrafiltration, trapped substance adds 500ml water, adds the 500ml30% ethanol sedimentation, and filtrate adds 750ml50% ethanol again, filter, filtrate adds 1750ml90% ethanol, places precipitation, leach precipitation, use acetone, washing with alcohol successively, vacuum-drying, promptly get skunk bush polysaccharide 13.8g, detect through HPLC, purity is 87.2%.
Embodiment 4
Get the dry residue 1kg behind the total glycosides of skunk bush pulp alcohol extracting, add 7L50 ℃ of warm water supersound extraction 1h, repeat united extraction liquid 3 times.Extracting solution is concentrated into 1/2 of original volume, is cooled to 25 ℃, adds 7L30%H
2O
2, stir, to light yellow, it is muddy to no longer producing to add 3% Tricholroacetic Acid, it is centrifugal to add whizzer, up to not having white suspendible from the liquid level intersection, tells clarified liq, uses the ultra-filtration membrane ultrafiltration, trapped substance adds 450ml water, adds the 450ml30% ethanol sedimentation, and filtrate adds 680ml50% ethanol again, filter, filtrate adds 1600ml90% ethanol, places precipitation, leach precipitation, use acetone, washing with alcohol successively, vacuum-drying, promptly get skunk bush polysaccharide 10.4g, detect through HPLC, purity is 92.5%.
Embodiment 5
Get the dry residue 5kg behind the total glycosides of skunk bush pulp alcohol extracting, add 25L50 ℃ of warm water supersound extraction 2h, repeat united extraction liquid 2 times.Extracting solution is concentrated into 2/5 of original volume, is cooled to 25 ℃, adds 8L30%H
2O
2, stir, to light yellow, it is muddy to no longer producing to add 3% Tricholroacetic Acid, it is centrifugal to add whizzer, up to not having white suspendible from the liquid level intersection, tells clarified liq, uses the ultra-filtration membrane ultrafiltration, trapped substance adds 1200ml water, adds the 1200ml30% ethanol sedimentation, and filtrate adds 1800ml50% ethanol again, filter, filtrate adds 4200ml90% ethanol, places precipitation, leach precipitation, use acetone, washing with alcohol successively, vacuum-drying, promptly get skunk bush polysaccharide 58.6g, detect through HPLC, purity is 89.1%.
Claims (4)
1. the preparation method of a skunk bush polysaccharide is characterized in that comprising following steps:
1) extracts: the dry residue behind the total glycosides of skunk bush pulp alcohol extracting is added 5-10 doubly measure (V/W) warm water supersound extraction 1-2h, repeat 2-3 time, filter united extraction liquid;
2) removal of impurities: said extracted liquid concentrates, and adds an amount of 30%H
2O
2, to light yellow, it is muddy, centrifugal to no longer producing to add 3% Tricholroacetic Acid, gets supernatant liquor;
3) membrane sepn: the ultra-filtration membrane ultrafiltration of above-mentioned supernatant liquor gets trapped substance;
4) fractionation precipitation: above-mentioned trapped substance adds suitable quantity of water, adds 30% ethanol sedimentation earlier, and filtrate adds 50% ethanol again, filters, and filtrate adds 90% ethanol, generates precipitation, leaches precipitation and uses acetone, washing with alcohol successively, and vacuum-drying promptly gets the skunk bush polysaccharide product.
2. the preparation method of skunk bush polysaccharide according to claim 1 is characterized in that warm water is 30-70 ℃ in the step 1), and ultrasonic frequency is 20KHz.
3. the preparation method of skunk bush polysaccharide according to claim 1 is characterized in that step 2) in H
2O
2Consumption is the 1/4-1/2 of concentrated solution volume.
4. the preparation method of skunk bush polysaccharide according to claim 1 is characterized in that ultra-filtration membrane is that molecular weight cut-off is 60000 hollow-fibre membrane in the step 3).
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| CN2010105581135A CN102002109A (en) | 2010-11-25 | 2010-11-25 | Preparation method of dogwood polysaccharides |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102293250A (en) * | 2011-07-21 | 2011-12-28 | 河南中医学院 | Cornus officinalis sugar-reduced instant milk powder solid beverage |
| CN102293251A (en) * | 2011-07-21 | 2011-12-28 | 河南中医学院 | Cornus officinalis fruit milk |
| CN102532335A (en) * | 2011-10-29 | 2012-07-04 | 山东好当家海洋发展股份有限公司 | Method for extracting scallop polysaccharide by utilizing scallop waste liquid |
| CN102617748A (en) * | 2012-04-06 | 2012-08-01 | 华远医药研究院有限公司 | Method for purifying pullulan polysaccharide |
| CN102757512A (en) * | 2012-06-20 | 2012-10-31 | 安徽凯盈药业有限公司 | Microwave extraction and purification process of dogwood polysaccharide |
| CN106928376A (en) * | 2017-03-23 | 2017-07-07 | 李春生 | The separation method of skunk bush polysaccharide and its application |
| CN107129921A (en) * | 2017-07-13 | 2017-09-05 | 河南科技大学 | A kind of brewing method of cornel fruit vinegar beverage |
-
2010
- 2010-11-25 CN CN2010105581135A patent/CN102002109A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102293250A (en) * | 2011-07-21 | 2011-12-28 | 河南中医学院 | Cornus officinalis sugar-reduced instant milk powder solid beverage |
| CN102293251A (en) * | 2011-07-21 | 2011-12-28 | 河南中医学院 | Cornus officinalis fruit milk |
| CN102532335A (en) * | 2011-10-29 | 2012-07-04 | 山东好当家海洋发展股份有限公司 | Method for extracting scallop polysaccharide by utilizing scallop waste liquid |
| CN102617748A (en) * | 2012-04-06 | 2012-08-01 | 华远医药研究院有限公司 | Method for purifying pullulan polysaccharide |
| CN102617748B (en) * | 2012-04-06 | 2016-12-14 | 华远医药研究院有限公司 | A kind of purification process of pulullan polysaccharide |
| CN102757512A (en) * | 2012-06-20 | 2012-10-31 | 安徽凯盈药业有限公司 | Microwave extraction and purification process of dogwood polysaccharide |
| CN106928376A (en) * | 2017-03-23 | 2017-07-07 | 李春生 | The separation method of skunk bush polysaccharide and its application |
| CN106928376B (en) * | 2017-03-23 | 2019-01-15 | 李春生 | The separation method of skunk bush polysaccharide and its application |
| CN107129921A (en) * | 2017-07-13 | 2017-09-05 | 河南科技大学 | A kind of brewing method of cornel fruit vinegar beverage |
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Application publication date: 20110406 |