CN101805413A - Preparation method of ligustrum lucidum polysaccharide - Google Patents
Preparation method of ligustrum lucidum polysaccharide Download PDFInfo
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- CN101805413A CN101805413A CN 201010137438 CN201010137438A CN101805413A CN 101805413 A CN101805413 A CN 101805413A CN 201010137438 CN201010137438 CN 201010137438 CN 201010137438 A CN201010137438 A CN 201010137438A CN 101805413 A CN101805413 A CN 101805413A
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- ligustri lucidi
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Abstract
The invention relates to a preparation method of ligustrum lucidum polysaccharide; the process takes dry residue after ligustrum lucidum extracts triterpenoid as the raw materials, soaked in 30 to 50DEG C warm water with 3 to 5 times of amount every time (V/M) for 1 to 2h, repeatedly pressed for 2 to 3 times; the combined pressed liquid is concentrated into extract at low pressure and washed by absolute ethyl alcohol for 3 times, to prepare solid deionized water to be re-dissolved; and protein is removed through a Sevage method, deproteinized solution is concentrated by an ultrafilter film, to prepare the product. The process has the advantages of simple operation, lower cost, higher purity and facilitation to mass production operation.
Description
Technical field
The present invention relates to a kind of preparation method of Fructus Ligustri Lucidi polysaccharide, especially a kind of method of utilizing squeezing, Sevage method and ultrafiltration membrane technique to extract the purifying Fructus Ligustri Lucidi polysaccharide.
Background technology
Fructus Ligustri Lucidi polysaccharide be Glossy Privet Fruit have multiple efficacies basic substance it, modern pharmacological research shows that Fructus Ligustri Lucidi polysaccharide has effects such as anti-oxidant, anti-ageing, enhancing immunity, through identifying mainly by rhamnosyl pectinose, four kinds of sugar of glucose and Fucose are formed, and molecular weight is between 2-100 ten thousand.
Rhamnosyl is the derivative that hydroxyl is replaced by hydrogen, i.e. a 6-deoxy-L-mannose of 6 of seminoses.Claim methylpentose again.A kind of with fucose typical 6-deoxyhexamethylose arranged side by side.Be the 6th deoxidation of seminose, become at last-compound of CH3, natural distributed be the L type, also have to be called 6-deoxy-L-mannose (6-de-oxy-L-mannose).Molecular formula: C
6H
12O
5Pure product rhamnosyl is the colourless crystallization powder, and the water-soluble and methyl alcohol of energy is slightly soluble in ethanol, and its crystallization is two kinds of forms, α type and β type.The α type contains a part crystal water, loses crystal water after the heating, changes β type (molecular weight is 164.16) into; The very easily moisture absorption of β type, the moisture absorption changes the α type in air.Common is α-L-rhamnosyl, its molecular weight be 182.11 under common condition a-L-rhamnosyl hydrate crystallization, tabular crystal, fusing point 82-92 ℃, specific rotatory power-7.7 ° →+8.9 °, water-soluble and ethanol; β-L-rhamnosyl (anhydrous) is for needle-like crystal has water absorbability, and fusing point 122-126 ℃ ,+38.4 ° →+8.9 °, water-soluble and ethanol.Pleasantly sweet, in the aqueous solution, exist with the pyrans form.Reductibility is arranged, generate rhamnoic acid, generate the Arabic three hydroxyl dagger-axe diacid of L-through nitric acid oxidation with the bromine water oxidation.Then get rhamnitol with reduction with sodium amalgam.
L-arabinose, L (+)-pectinose that is otherwise known as, L (+)-arabinose, pectose etc., English name is L-Arabinose, molecular formula: C
6H
12O
5L-arabinose is a white crystalline powder, odorlessness, pleasantly sweet (sugariness be sucrose about 50%), and fusing point 159-160 ℃, relative density 1.625, specific rotatory power+190.5 ° →+104.5 ° (C=3), water-soluble, but solubleness is lower than sucrose; Stability to heat and acid is high.
Glucose (glucose) biochemistry is write a Chinese character in simplified form G, is aldohexose, chemical formula: C
6H
12O
6, molecular weight: 180.White crystal, soluble in water, it is sweet to distinguish the flavor of, 146 ℃ of fusing points.
Fucose (fucose) is a kind of of hexose, claims 6-deoxidation-L-semi-lactosi again, and can regard a kind of methyl the eleventh of the twelve Earthly Branches sugar as.The Fucose overwhelming majority that nature exists is the L-Fucose, and the Fucose of D configuration is found in some sugared sweet compounds only as rare sugar.The L-Fucose is present in marine alga and the natural gum relatively largely, also is found in the polysaccharide of some bacterium.Fucose extensively is present on the plasma membrane on various types of cells surface as the integral part of sugar chain in the glycoprotein.Fucose lacks a hydroxyl than general hexose on the 6th carbon atom, thus Fucose than other monose wetting abilities a little less than, and hydrophobicity is strong.Fucose in some blood-group substance molecule is the mark of certain blood group.α-L-Fucose crystallization, 145 ℃ of fusing points.Molecular formula: C
6H
12O
5, molecular weight: 164.
The extracting method of relevant Fructus Ligustri Lucidi polysaccharide reports that seldom method is relatively limited to.Existing method is the raw material degreasing, alcohol extracting, water are carried, are concentrated, extraction, decolouring, washing, drying, obtain product, as " content Determination of Polysaccharide in the Glossy Privet Fruit of the different places of production " such as Zhang Xinghui, Li Manling etc. " extraction and the assay of Glossy Privet Fruit different sites polysaccharide ".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.
Summary of the invention
Technical problem to be solved by this invention provides a kind of simple to operate, production safety, the Fructus Ligustri Lucidi polysaccharide preparation method that purity is higher.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
1) squeezing: the residue that Glossy Privet Fruit was extracted triterpenic acid squeezes at normal temperatures, and the dregs of a decoction add warm water soaking 3-5h, and normal temperature squeezing 2-3 time merges pressed liquor;
2) washing: the pressed liquor low-press thick is condensed to medicinal extract, uses absolute ethanol washing 3 times, get residual solids;
3) deproteinated: residual solids is redissolved with deionized water, removes a spot of residual protein with the Sevage method, gets deproteinated solution;
4) ultrafiltration: deproteinated solution is concentrated by ultra-filtration membrane, and holding back mutually, oven dry promptly gets Fructus Ligustri Lucidi polysaccharide.
Above-mentioned preparation method is characterized in that 1) the step squeeze pressure is 80-100Mpa, water temperature 30-50 ℃, the 3-5 that each consumption is a raw material doubly measures (V/W).
Above-mentioned preparation method is characterized in that 2) 3 consumptions of step dehydrated alcohol be respectively the medicinal extract quality 4-6 doubly, 3-5 doubly, 3-4 doubly (V/W).
Above-mentioned preparation method is characterized in that 3) the step condition: the deionized water consumption is 10 times of amounts of residual solids, and Sevage reagent is chloroform: propyl carbinol=5: 1 (V/V) mixed solution, consumption is 1/5 of the aqueous solution.
Above-mentioned preparation method is characterized in that 4) the step ultrafiltration membrane system is for gathering alum hollow fiber ultrafiltration membrane system, and molecular weight cut-off is 20000.
In sum, there is following advantage in the present invention: this process using is soaked squeezing and is extracted Fructus Ligustri Lucidi polysaccharide, and solvent is simple; Ultrafiltration also has good decolorizing effect except that the performance with tangible filtering colloidal impurity; The solubility with temperature of Fructus Ligustri Lucidi polysaccharide in water changes responsive, and crystallization effect is good; Consumption of organic solvent is few, and toxicity is low, produces safer.
Adopt technique scheme to prepare Fructus Ligustri Lucidi 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 residue 1kg that Glossy Privet Fruit extracted triterpenic acid, add each 3L30 ℃ warm water soaking, 80Mpa repeats to squeeze 2 times, merges pressed liquor.Pressed liquor simmer down to medicinal extract 282g successively uses 1.2L, 850ml, 850ml absolute ethanol washing medicinal extract.Residual solids is disperseed with the 3L deionized water, adds the 600ml chloroform: propyl carbinol=5: 1 (V/V) mixed solution removes deproteinize with the Sevage method.At last the poly-alum hollow fiber ultrafiltration membrane system of surplus solution by molecular weight cut-off 20000 concentrated, oven dry promptly get Fructus Ligustri Lucidi polysaccharide 3.8g, and through the HPLC detection, purity is 98.5%.
Embodiment 2
Get the residue 1kg that Glossy Privet Fruit extracted triterpenic acid, add each 4L40 ℃ warm water soaking, 90Mpa repeats to squeeze 2 times, merges pressed liquor.Pressed liquor simmer down to medicinal extract 294g successively uses 1.5L, 1.5L, 900ml absolute ethanol washing medicinal extract.Residual solids is disperseed with the 3L deionized water, adds the 600ml chloroform: propyl carbinol=5: 1 (V/V) mixed solution removes deproteinize with the Sevage method.At last the poly-alum hollow fiber ultrafiltration membrane system of surplus solution by molecular weight cut-off 20000 concentrated, oven dry promptly get Fructus Ligustri Lucidi polysaccharide 3.9g, and through the HPLC detection, purity is 98.6%.
Embodiment 3
Get the residue 1kg that Glossy Privet Fruit extracted triterpenic acid, add each 5L40 ℃ warm water soaking, 100Mpa repeats to squeeze 3 times, merges pressed liquor.Pressed liquor simmer down to medicinal extract 302g successively uses 1.5L, 1.2L, 1.2L absolute ethanol washing medicinal extract.Residual solids is disperseed with the 3L deionized water, adds the 600ml chloroform: propyl carbinol=5: 1 (V/V) mixed solution removes deproteinize with the Sevage method.At last the poly-alum hollow fiber ultrafiltration membrane system of surplus solution by molecular weight cut-off 20000 concentrated, oven dry promptly get Fructus Ligustri Lucidi polysaccharide 3.8g, and through the HPLC detection, purity is 99.2%.
Embodiment 4
Get the residue 1kg that Glossy Privet Fruit extracted triterpenic acid, add each 3L50 ℃ warm water soaking, 100Mpa repeats to squeeze 3 times, merges pressed liquor.Pressed liquor simmer down to medicinal extract 282g successively uses 1.6L, 1.4L, 850ml absolute ethanol washing medicinal extract.Residual solids is disperseed with the 3L deionized water, adds the 600ml chloroform: propyl carbinol=5: 1 (V/V) mixed solution removes deproteinize with the Sevage method.At last the poly-alum hollow fiber ultrafiltration membrane system of surplus solution by molecular weight cut-off 20000 concentrated, oven dry promptly get Fructus Ligustri Lucidi polysaccharide 4.0g, and through the HPLC detection, purity is 99.5%.
Claims (5)
1. the preparation method of a Fructus Ligustri Lucidi polysaccharide is characterized in that comprising following steps:
1) squeezing: the dry residue that Glossy Privet Fruit was extracted triterpenic acid adds warm water soaking 1-2h, and normal temperature squeezing 2-3 time merges pressed liquor;
2) washing: the pressed liquor low-press thick is condensed to medicinal extract, uses absolute ethanol washing 3 times, get residual solids;
3) deproteinated: residual solids is redissolved with deionized water, removes a spot of residual protein with the Sevage method, gets deproteinated solution;
4) ultrafiltration: deproteinated solution is concentrated by ultra-filtration membrane, and holding back mutually, oven dry promptly gets Fructus Ligustri Lucidi polysaccharide.
2. preparation method as claimed in claim 1 is characterized in that 1) the step squeeze pressure is 80-100Mpa, water temperature 30-50 ℃, the 3-5 that each consumption is a raw material doubly measures (V/W).
3. preparation method as claimed in claim 1 is characterized in that 2) 3 consumptions of step dehydrated alcohol be respectively the medicinal extract quality 4-6 doubly, 3-5 doubly, 3-4 doubly (V/W).
4. preparation method as claimed in claim 1 is characterized in that 3) the step condition: the deionized water consumption is 10 times of amounts of residual solids, and Sevage reagent is chloroform: propyl carbinol=5: 1 (V/V) mixed solution, consumption is 1/5 of the aqueous solution.
5. preparation method as claimed in claim 1 is characterized in that 4) the step ultrafiltration membrane system is for gathering alum hollow fiber ultrafiltration membrane system, and molecular weight cut-off is 20000.
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| CN 201010137438 CN101805413A (en) | 2010-04-01 | 2010-04-01 | Preparation method of ligustrum lucidum polysaccharide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570841A (en) * | 2012-07-26 | 2014-02-12 | 福建省安新食品有限公司 | High-efficiency extraction method for pleurotus geesteranus polysaccharide |
| CN104231102A (en) * | 2014-09-16 | 2014-12-24 | 贵州信邦制药股份有限公司 | Method for extracting polysaccharide ingredient from astragalus membranaceus and glossy privet fruit composition by alkaline extraction and alcohol deposition method and product produced by method |
| CN107652369A (en) * | 2017-09-15 | 2018-02-02 | 黄河科技学院 | A kind of anticoagulation Ligustrum japonicum Thunb.flower polysaccharide and its purification methods and uses |
Citations (3)
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| CN1513539A (en) * | 2003-04-01 | 2004-07-21 | 贵州信邦远东药业有限公司 | Preparation technology of supplementing kind capsule |
| CN1831015A (en) * | 2006-04-26 | 2006-09-13 | 贵州信邦远东药业有限公司 | Process for extracting fructus ligustri lucidi and Radixa stragali polysaccharide, the products and application thereof |
| WO2009021196A1 (en) * | 2007-08-08 | 2009-02-12 | Bionovo, Inc. | Extracts of ligustrum lucidum and uses thereof |
-
2010
- 2010-04-01 CN CN 201010137438 patent/CN101805413A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1513539A (en) * | 2003-04-01 | 2004-07-21 | 贵州信邦远东药业有限公司 | Preparation technology of supplementing kind capsule |
| CN1831015A (en) * | 2006-04-26 | 2006-09-13 | 贵州信邦远东药业有限公司 | Process for extracting fructus ligustri lucidi and Radixa stragali polysaccharide, the products and application thereof |
| WO2009021196A1 (en) * | 2007-08-08 | 2009-02-12 | Bionovo, Inc. | Extracts of ligustrum lucidum and uses thereof |
Non-Patent Citations (2)
| Title |
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| 《中成药》 20080430 邱蓉丽等 女贞子多糖的提取工艺研究 第612-614页 1-5 第30卷, 第4期 2 * |
| 《淮北煤炭师范学院学报（自然科学版）》 20080930 盛玮等 女贞子多糖超声提取工艺及抗氧化性的研究 第28-31页 1-5 第29卷, 第3期 2 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570841A (en) * | 2012-07-26 | 2014-02-12 | 福建省安新食品有限公司 | High-efficiency extraction method for pleurotus geesteranus polysaccharide |
| CN104231102A (en) * | 2014-09-16 | 2014-12-24 | 贵州信邦制药股份有限公司 | Method for extracting polysaccharide ingredient from astragalus membranaceus and glossy privet fruit composition by alkaline extraction and alcohol deposition method and product produced by method |
| CN107652369A (en) * | 2017-09-15 | 2018-02-02 | 黄河科技学院 | A kind of anticoagulation Ligustrum japonicum Thunb.flower polysaccharide and its purification methods and uses |
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Open date: 20100818 |