CN1560086A - Preparation process for fucosan sulfate of high sulfuric content - Google Patents
Preparation process for fucosan sulfate of high sulfuric content Download PDFInfo
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- CN1560086A CN1560086A CNA2004100236947A CN200410023694A CN1560086A CN 1560086 A CN1560086 A CN 1560086A CN A2004100236947 A CNA2004100236947 A CN A2004100236947A CN 200410023694 A CN200410023694 A CN 200410023694A CN 1560086 A CN1560086 A CN 1560086A
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- brown alga
- fucoidan
- chitosan
- fucosan
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Abstract
The invention is a method of preparing high sulfate-radical content fucosan sulphate, using hot water or acid water to extract brown alga so as to make the fucosan sulphate extract containing brown alga; concentrating the extract to 2-10 weight% of the amylase, regulating pH value to 5-8; during stirring, adding in chitosan solution, continuing stirring for 10-60 min; centrifuging or filtering to collect the generated deposit; using salt solution in 5-10 times weight to extract 2-4 times, centrifuging or filtering to collect clear solution; desalting the clear solution by dialyzing or ultrafiltering; after desalting, concentrating the amylase solution and then freeze-drying. It uses the character that chitosan can combine with sulfuric acid amylase to generate deposit so as to separate high-sulfur component from brown alga fucosan sulphate, and combines ultrafilteration, freeze-drying, etc to prepare the high sulfate-radical content fucosan sulphate.
Description
Technical field
The present invention relates to a kind of preparation method of high sulfate radical content fucoidan.
Background technology
Fucoidan (Fucoidan) is the water-soluble sulfated polysaccharide of a distinctive class in the brown alga, its composition is based on Fucose and organo-sulfate, also contain a spot of semi-lactosi, seminose, wood sugar, pectinose and uronic acid etc., for forming similar mixed polysaccharide mixture.According to the difference of organic sulfate radical content in the fucoidan, fucoidan can be divided into different components.Studies show that in a large number that fucoidan has anticoagulation, improves immunizing power, antitumor, antiviral, hypoglycemic, anti-inflammatory, radioprotective, inhibition ascites carcinoma isoreactivity.Particularly the high-sulfur component has shown great potential gradually at aspects such as AIDS virus resisting and treatment renal failures.Extracting method to fucoidan has carried out big quantity research, and (ZL98110253.0, ZL 95112292.4, ZL00105700.6) to have applied for multinomial patent of invention.But the method for the high sulfate radical content fucoidan of preparation from fucoidan is studied lessly, only limits at present with ion exchange method and hexadecyl brometo de amonio (CTAB) step-by-step precipitation method.According to the difference of ion exchange resin to different sulfate radical content fucoidan adsorptivity sizes, carry out gradient elution with salts solution, can obtain the fucoidan of different sulfate radical contents.Used ion exchange resin mostly is gel type resin because cost an arm and a leg and adsorptive capacity less, can't reach half industrialization or suitability for industrialized production level.The CTAB step-by-step precipitation method can be realized the fractional precipitation of different sulfate radical content fucoidans, but is difficult to extract the high-sulfur component from sediment composite, and the poor stability of CTAB.So there is not high sulfate radical content fucoidan to come out up to now yet.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing high sulfate radical content fucoidan, it can overcome the above-mentioned shortcoming of prior art.
A kind of preparation method of high sulfate radical content fucoidan is characterized in that making the extracting solution that contains the brown alga fucoidan with hot water or sour water lixiviate brown alga; The weight percentage that this extracting solution is concentrated into polysaccharide is 2-10%, transfers pH to 5-8; Under agitation, add chitosan solution, continue to stir 10-60min; Collect the precipitation that produces with centrifugal or filtration; The salts solution of precipitation with 5-10 times of weight extracted 2-4 time, and clear liquid is collected in centrifugal or filtration back; With this clear liquid dialysis or ultrafiltration desalination; Polysaccharide soln after the desalination is concentrated postlyophilization.
The present invention utilizes chitosan, chitosan energy and sulfated polysaccharide to isolate the high-sulfur component in conjunction with generating sedimentary characteristic from the brown alga fucoidan, and in conjunction with high sulfate radical content fucoidans of preparation such as ultrafiltration, lyophilizes.The method applied in the present invention has that processing step is simple, facility investment is few, non-environmental-pollution, product purity advantages of higher, is suitable for suitability for industrialized production.
Embodiment.
Get the dried sea-tangle of 5Kg and soaked 24 hours with the hydrochloric acid soln of the pH2 of 10 times of weight, extract 3 times, united extraction liquid is concentrated into 3000mL, and the weight percentage of polysaccharide is 5.2% in this extracting solution.Transfer pH to 6 with sodium hydroxide, under agitation condition, add the 60mL weight percentage and be 5% chitosan solution (viscosity 8cps), continue to stir 20min, make high sulfate radical content fucoidan and chitosan formation mixture and precipitate.Centrifugation precipitation, with precipitation with the 2M sodium chloride solution extraction of 10 times of weight 3 times, united extraction liquid, dialysis and through concentrating postlyophilization gets high sulfate radical content fucoidan 42g.By analysis, Fucose content is 43.8% in the product, sulfate radical content 39.6%.
The high sulfate radical content fucoidan of preparation can be used as the raw material of protective foods or medicine.By changing the ratio of polysaccharide in chitosan and sour water or the hot water extraction liquid, the content of sulfate radical in the adjustable product can prepare the fucoidan product of different sulfate radical contents according to different purposes like this.High sulfate radical content fucoidan product by the present invention preparation consist of Fucose content 25-50%, organic sulfate radical content 25-40%.
In the present embodiment, can change the hot water lixiviate into, be about to the water that dried sea-tangle chopping adds 15-25 times of weight, be heated to 70-95 ℃, be incubated 6-10 hour, get extracting solution with the sour water lixiviate.The NaCl aqueous solution described in the present invention can be used Na instead
2SO
4The aqueous solution, described sea-tangle can change wakame, Sargassum fusiforme, mouse tail algae or black wrack into.
Claims (4)
1, a kind of preparation method of high sulfate radical content fucoidan is characterized in that making the extracting solution that contains the brown alga fucoidan with hot water or sour water lixiviate brown alga; The weight percentage that this extracting solution is concentrated into polysaccharide is 2-10%, transfers pH to 5-8; Under agitation, add chitosan solution, continue to stir 10-60min; Collect the precipitation that produces with centrifugal or filtration; The salts solution of precipitation with 5-10 times of weight extracted 2-4 time, and clear liquid is collected in centrifugal or filtration back; With this clear liquid dialysis or ultrafiltration desalination; Polysaccharide soln after the desalination is concentrated postlyophilization.
2, press claims 1 described preparation method, it is characterized in that described brown alga is sea-tangle, wakame, Sargassum fusiforme, mouse tail algae or black wrack.
3, press claims 1 described preparation method, the molecular weight that it is characterized in that described chitosan is 3000-100,000, and the consumption of chitosan is the 10-50% of polysaccharide content in the extracting solution.
4, press claims 1 described preparation method, it is characterized in that described salts solution is NaCl or Na
2SO
4The aqueous solution, concentration are 1-4M.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410023694 CN1243026C (en) | 2004-03-12 | 2004-03-12 | Preparation process for fucosan sulfate of high sulfuric content |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200410023694 CN1243026C (en) | 2004-03-12 | 2004-03-12 | Preparation process for fucosan sulfate of high sulfuric content |
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| Publication Number | Publication Date |
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| CN1560086A true CN1560086A (en) | 2005-01-05 |
| CN1243026C CN1243026C (en) | 2006-02-22 |
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| CN 200410023694 Expired - Fee Related CN1243026C (en) | 2004-03-12 | 2004-03-12 | Preparation process for fucosan sulfate of high sulfuric content |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100540568C (en) * | 2007-04-20 | 2009-09-16 | 中国科学院海洋研究所 | A kind of method of extracting algal polysaccharide sulfate |
| CN101671399B (en) * | 2009-10-10 | 2011-05-11 | 山东大学威海分校 | Preparation method of fucoidan sulfuric ester with high purity and high-sulfate radical content |
| CN103288978A (en) * | 2013-06-08 | 2013-09-11 | 中国海洋大学 | Fucosan sulphate and preparation method and application thereof in preparation of antidiabetic alpha-glycosidase inhibitor |
| CN103980370A (en) * | 2013-06-27 | 2014-08-13 | 中国科学院海洋研究所 | Method used for recycling fucoidin from thallus laminariae |
| CN111760066A (en) * | 2020-06-09 | 2020-10-13 | 北京化工大学 | Hemostatic gel and preparation method and application thereof |
| CN112521431A (en) * | 2020-12-10 | 2021-03-19 | 山东省科学院生物研究所 | Anticoagulation fucoidan oligosaccharide and preparation method thereof |
-
2004
- 2004-03-12 CN CN 200410023694 patent/CN1243026C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100540568C (en) * | 2007-04-20 | 2009-09-16 | 中国科学院海洋研究所 | A kind of method of extracting algal polysaccharide sulfate |
| CN101671399B (en) * | 2009-10-10 | 2011-05-11 | 山东大学威海分校 | Preparation method of fucoidan sulfuric ester with high purity and high-sulfate radical content |
| CN103288978A (en) * | 2013-06-08 | 2013-09-11 | 中国海洋大学 | Fucosan sulphate and preparation method and application thereof in preparation of antidiabetic alpha-glycosidase inhibitor |
| CN103288978B (en) * | 2013-06-08 | 2015-10-28 | 中国海洋大学 | Fucoidan and preparation method thereof and the application in the antidiabetic alpha-glucosidase inhibitor of preparation |
| CN103980370A (en) * | 2013-06-27 | 2014-08-13 | 中国科学院海洋研究所 | Method used for recycling fucoidin from thallus laminariae |
| CN103980370B (en) * | 2013-06-27 | 2016-01-20 | 中国科学院海洋研究所 | A kind of method reclaiming fucoidin from sea-tangle |
| CN111760066A (en) * | 2020-06-09 | 2020-10-13 | 北京化工大学 | Hemostatic gel and preparation method and application thereof |
| CN111760066B (en) * | 2020-06-09 | 2022-03-04 | 北京化工大学 | Hemostatic gel and preparation method and application thereof |
| CN112521431A (en) * | 2020-12-10 | 2021-03-19 | 山东省科学院生物研究所 | Anticoagulation fucoidan oligosaccharide and preparation method thereof |
| CN112521431B (en) * | 2020-12-10 | 2022-03-29 | 山东省科学院生物研究所 | Anticoagulation fucoidan oligosaccharide and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1243026C (en) | 2006-02-22 |
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Granted publication date: 20060222 Termination date: 20100312 |