CN100540568C - A kind of method of extracting algal polysaccharide sulfate - Google Patents
A kind of method of extracting algal polysaccharide sulfate Download PDFInfo
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- CN100540568C CN100540568C CNB200710014573XA CN200710014573A CN100540568C CN 100540568 C CN100540568 C CN 100540568C CN B200710014573X A CNB200710014573X A CN B200710014573XA CN 200710014573 A CN200710014573 A CN 200710014573A CN 100540568 C CN100540568 C CN 100540568C
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- algal polysaccharide
- polysaccharide sulfate
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Abstract
The present invention relates to the marine chemical industry field of engineering technology, specifically a kind of method of from kelp-soaking liquid, extracting algal polysaccharide sulfate.Method: the flocculation agent that adds 1-10ml in the kelp-soaking liquid of every 150ml, stir and made its flocculation 10 minutes-8 hours in 2-10 minute, centrifugal, be deposited under the condition that pH is 2-6 swelling 1-24 hour, and stir dissolving in 1-4 hour, filter and filtrate is transferred to neutrality, concentrating under reduced pressure, then in concentrated solution, add ethanol, filter to such an extent that precipitate and washing, and after drying promptly get algal polysaccharide sulfate.It is flocculation agent that the present invention relates to chitosan and derivative thereof, and flocculation sediment from kelp-soaking liquid " carbohydrate gum " extracts algal polysaccharide sulfate then from " carbohydrate gum " of gained.Adopt the present invention can make resource obtain comprehensive utilization, and easy and simple to handle, reduced usage quantity to acid, alkali, saved resource, the algal polysaccharide sulfate of gained can reach the 5-16% of gained precipitation capacity simultaneously.
Description
Technical field
The present invention relates to the marine chemical industry field of engineering technology, specifically a kind of method of from kelp-soaking liquid, extracting algal polysaccharide sulfate.
Background technology
Algal polysaccharide sulfate or one-tenth controlling sulfate polyose are the iuntercellular polysaccharide that is present in all brown algas, the fucoidin that is otherwise known as, fucosan.From brown alga palmate sea-tangle, extracted first by Kylin in 1913.Algal polysaccharide sulfate is formed very complicated; alter a great deal in different brown alga kinds; studies show that in recent years, it has anticoagulation, activates blood circulation and disperses blood clots, regulating blood fat, antitumor, antiviral, strengthen cellular immunization and humoral immune function, anti-ageing, to the multiple biological activitys such as protection of matrix cells.
Later 1950s, owing to propagate the development of sea-tangle cause artificially, the surge of sea-tangle output is except that edible, for industrial production algin, iodine and N.F,USP MANNITOL provide high quality raw material.In seaweed industry, mainly be from the sea-tangle algae-residue, to extract algin, from kelp-soaking liquid, extract iodine, N.F,USP MANNITOL.Yet, the kelp-soaking liquid complicated component, except containing the high inorganic electrolyte of concentration, organism and colloids such as a large amount of fucoidins, algin, laminarin, amino acid, pigment, tannin are still arranged, extract in the technological process of N.F,USP MANNITOL in the sea-tangle comprehensive utilization, this class impurity is called " carbohydrate gum ".A large amount of existence of " carbohydrate gum " are not only given and are carried iodine and purification N.F,USP MANNITOL brings very burden and difficulty, have a strong impact on product yield and production cost, and " carbohydrate gum " fall as waste treatment in itself producing again, and this has caused the waste of resource again.
Summary of the invention
The invention provides a kind of method of easy and simple to handle, the extraction algal polysaccharide sulfate that economizes on resources.
For realizing purpose of the present invention, the technical solution used in the present invention method: the flocculation agent that adds 1-10ml in the kelp-soaking liquid of every 150ml, stir and made its flocculation 10 minutes-8 hours in 2-10 minute, then centrifugal 2-6 minute, separate and to obtain being deposited under the acidic conditions that pH is 2-6 swelling 1-24 hour, and stirring made resolution of precipitate in 1-4 hour, filter, filtrate is transferred to neutrality, concentrating under reduced pressure then adds ethanol and makes concentration arrive 60%-80% in concentrated solution, filter to such an extent that precipitate and washing, lyophilize promptly gets algal polysaccharide sulfate; Described flocculation agent is chitosan, chitosan carboxymethyl derivant or chitosan quaternary ammonium salt derivatives, and its molecular weight is 2000-76 ten thousand.
Described chitosan, carboxymethyl chitosan derivative or chitosan quaternary ammonium salt derivatives be its concentration at the 1-3% acid solution or the aqueous solution, acid solution is acetate or the aqueous hydrochloric acid of 1%-3%.
The time of described centrifugation is 2-6 minute, and rotating speed is 500-3000 rev/min.Described pH is that the condition of 2-6 is: transfer pH to reach 2-6 with hydrochloric acid.Described concentrating under reduced pressure, concentrated solution are the 1/10-1/20 of original solution.Washings is anhydrous diethyl ether or anhydrous propanone during described washing of precipitate.
The advantage that the present invention had is:
1. adopt the algal polysaccharide sulfate of method gained of the present invention can reach the 5-16% of gained precipitation capacity.
2. the method applied in the present invention is simple to operate, has reduced the usage quantity to acid, alkali, has saved resource.
3. the present invention extracts algal polysaccharide sulfate from " carbohydrate gum ", and is significant for the comprehensive utilization of resource.
Description of drawings
Fig. 1 extracts the infrared spectrum of algal polysaccharide sulfate for the present invention.
Embodiment
Embodiment 1
With the 1ml acid solutions is 1%, molecular weight is that 2000 chitosan acetic acid solution joins in the 150ml kelp-soaking liquid, stir and made its flocculation 4 hours in 2 minutes, then centrifugal 2 minutes with 500 rev/mins speed, separate that to obtain being deposited in pH be swelling 4 hours under 2 acidity (transferring pH with the hydrochloric acid) condition, and stir dissolving in 2 hours, filter, filtrate is transferred to neutrality (adopting 10%NaOH solution to transfer to neutrality), concentrating under reduced pressure, make concentrated solution reach 1/10 of original solution, then in concentrated solution, add alcohol concn and reach 65%, filter precipitation, precipitation is with anhydrous diethyl ether washing 2 times, carries out lyophilize with the FD-5N freeze drier of Tokyo physics and chemistry company, promptly get algal polysaccharide sulfate (referring to Fig. 1), the gained algal polysaccharide sulfate accounts for 10.51% of precipitation capacity.
Embodiment 2
With the 2ml acid solution is 2%, molecular weight is that 760,000 chitosan acetic acid solution joins in the 150ml kelp-soaking liquid, stir and made its flocculation 0.5 hour in 4 minutes, then centrifugal 3 minutes with 3000 rev/mins speed, separate that to obtain being deposited in pH be swelling 1 hour under 4 the acidic conditions, stir dissolving in 2 hours, filter, filtrate is transferred to neutrality, concentrating under reduced pressure then adds ethanol and makes concentration reach 70% in concentrated solution, filter to such an extent that precipitate, precipitation is washed 2 times with anhydrous diethyl ether, lyophilize promptly gets algal polysaccharide sulfate, and the gained algal polysaccharide sulfate accounts for 5% of precipitation capacity.
Embodiment 3
With the 8ml acid solution is that 3% molecular weight is that 80,000 chitosan salt acid solution joins in the 150ml kelp-soaking liquid, stir and made its flocculation 8 hours in 8 minutes, then centrifugal 5 minutes with 1500 rev/mins speed, separate that to obtain being deposited in pH be swelling 24 hours under 6 the acidic conditions, stir dissolving in 4 hours, filter, filtrate is transferred to neutrality, concentrating under reduced pressure then adds ethanol and makes concentration reach 75% in concentrated solution, filter to such an extent that precipitate, precipitation is washed 2 times with anhydrous propanone, vacuum-drying promptly gets algal polysaccharide sulfate, and the gained algal polysaccharide sulfate accounts for 11.1% of precipitation capacity.
Embodiment 4
With the 2ml acid solution is that 2% molecular weight is that 700,000 carboxymethyl chitosan sugar aqueous solution joins in the 150ml kelp-soaking liquid, stir and made its flocculation 0.5 hour in 4 minutes, then centrifugal 3 minutes with 1000 rev/mins speed, separate that to obtain being deposited in pH be swelling 8 hours under 4 the acidic conditions, stir dissolving in 3 hours, filter, filtrate is transferred to neutrality, concentrating under reduced pressure then adds ethanol and makes concentration reach 70% in concentrated solution, filter, precipitation is washed 2 times with anhydrous diethyl ether, vacuum-drying promptly gets algal polysaccharide sulfate, and the gained algal polysaccharide sulfate accounts for 14.2% of precipitation capacity.
Embodiment 5
With the molecular weight of 8ml 3% is that 760,000 chitosan Hydroxyproyl Trimethyl quaternary ammonium salt aqueous solution joins in the 150ml kelp-soaking liquid, stirred 8 minutes, flocculated 10 minutes, then centrifugal 4 minutes with 2000 rev/mins speed, separate that to obtain being deposited in pH be swelling 24 hours under 6 the condition, stir dissolving in 4 hours, filter, filtrate is transferred to neutrality, concentrating under reduced pressure, then adding ethanol in concentrated solution makes concentration reach 80%, filter, precipitation is washed 2 times with anhydrous propanone, vacuum-drying, promptly get algal polysaccharide sulfate, the gained algal polysaccharide sulfate accounts for 16.1% of precipitation capacity.
Embodiment 6
Difference from Example 1 is: the flocculation agent that is adopted is N, N, N-trimethyl chitin.
Embodiment 7
Difference from Example 2 is: the flocculation agent that is adopted is N, N, N-trimethyl chitin quaternary ammonium salt.
Embodiment 8
Difference from Example 3 is: the flocculation agent that is adopted is 2-(2-hydroxyl benzimidoyl) cm-chitosan.
Embodiment 9
Difference from Example 1 is: the flocculation agent that is adopted is 2-(2-hydroxyl-5-nitrobenzoyl imido grpup) cm-chitosan.
Embodiment 10
Difference from Example 1 is: the flocculation agent that is adopted is 2-(2-hydroxyl-5-chlorobenzene azomethine base) cm-chitosan.
Claims (5)
1. method of extracting algal polysaccharide sulfate, it is characterized in that: the flocculation agent that adds 1-10ml in the kelp-soaking liquid of every 150ml, stir and made its flocculation 10 minutes-8 hours in 2-10 minute, then centrifugal 2-6 minute, separate and to obtain being deposited under the acidic conditions that pH is 2-6 swelling 1-24 hour, and stirring made resolution of precipitate in 1-4 hour, filter, filtrate is transferred to neutrality, concentrating under reduced pressure then adds ethanol and makes concentration arrive 60%-80% in concentrated solution, filter to such an extent that precipitate and washing, lyophilize promptly gets algal polysaccharide sulfate; Described flocculation agent is chitosan carboxymethyl derivant or chitosan quaternary ammonium salt derivatives, and its molecular weight is 2000-76 ten thousand;
Described carboxymethyl chitosan derivative or chitosan quaternary ammonium salt derivatives be its concentration at the 1-3% acid solution or the aqueous solution, acid solution is acetate or the aqueous hydrochloric acid of 1%-3%.
2. the method for extraction algal polysaccharide sulfate according to claim 1 is characterized in that: the time of described centrifugation is 2-6 minute, and rotating speed is 500-3000 rev/min.
3. the method for extraction algal polysaccharide sulfate according to claim 1 is characterized in that: described pH is that the condition of 2-6 is: transfer pH to reach 2-6 with hydrochloric acid.
4. the method for extraction algal polysaccharide sulfate according to claim 1 is characterized in that: described concentrating under reduced pressure, concentrated solution are the 1/10-1/20 of original solution.
5. the method for extraction algal polysaccharide sulfate according to claim 1 is characterized in that: washings is anhydrous diethyl ether or anhydrous propanone during described washing of precipitate.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB200710014573XA CN100540568C (en) | 2007-04-20 | 2007-04-20 | A kind of method of extracting algal polysaccharide sulfate |
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| CNB200710014573XA CN100540568C (en) | 2007-04-20 | 2007-04-20 | A kind of method of extracting algal polysaccharide sulfate |
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| CN101037483A CN101037483A (en) | 2007-09-19 |
| CN100540568C true CN100540568C (en) | 2009-09-16 |
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| CNB200710014573XA Expired - Fee Related CN100540568C (en) | 2007-04-20 | 2007-04-20 | A kind of method of extracting algal polysaccharide sulfate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102784164A (en) * | 2012-07-27 | 2012-11-21 | 中国海洋大学 | Application of polysaccharide sulphate to preparation of tumor treatment neovascularization inhibitors and vascular disrupting agents |
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| CN101830996B (en) * | 2010-04-21 | 2012-01-04 | 江南大学 | Method for separating and purifying blue algae polysaccharide |
| CN102367284B (en) * | 2011-10-20 | 2013-04-10 | 广东中烟工业有限责任公司 | Porphyra polysaccharide as well as preparation method and application thereof |
| CN102367282B (en) * | 2011-10-20 | 2013-04-10 | 广东中烟工业有限责任公司 | Laminaria japonica polysaccharide, its preparation method and application |
| CN103923223A (en) * | 2013-01-11 | 2014-07-16 | 南通中国科学院海洋研究所海洋科学与技术研究发展中心 | Method for extracting fucoidan from fresh kelp blanching wastewater |
| 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 |
| CN103848924B (en) * | 2014-03-22 | 2016-03-02 | 吉林省辉南长龙生化药业股份有限公司 | Algal polysaccharide sulfate extracting method |
| CN103980373B (en) * | 2014-05-21 | 2016-03-09 | 吉林省辉南长龙生化药业股份有限公司 | A kind of algal polysaccharide sulfate extracting method |
| CN104448023B (en) * | 2014-12-19 | 2017-01-04 | 桂林市和胤祥新型材料有限公司 | A kind of method extracting polysaccharide sulfate from Thallus Laminariae (Thallus Eckloniae) |
| CN105154885B (en) * | 2015-09-11 | 2018-06-19 | 中国科学院海洋研究所 | A kind of high-efficient corrosion inhibitor application |
| CN106176799A (en) * | 2016-07-21 | 2016-12-07 | 中国科学院海洋研究所 | A kind of sulfated fucan is as the application of immunostimulant |
| CN106220749A (en) * | 2016-08-26 | 2016-12-14 | 山东招金膜天股份有限公司 | A kind of method of separation and Extraction sulfated fucan from Thallus Laminariae (Thallus Eckloniae) |
| SG11202100391VA (en) | 2018-07-27 | 2021-02-25 | Arc Medical Devices Inc | Highly sulfated fucans for the treatment of fibrous adhesions |
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Assignee: Huinan Changlong Biochemical Pharmaceutical Co., Ltd., Jilin Prov. Assignor: Institute of Oceanology, Chinese Academy of Sciences Contract record no.: 2011220000056 Denomination of invention: Method for extracting brown algae polysaccharide sulfated Granted publication date: 20090916 License type: Exclusive License Open date: 20070919 Record date: 20111214 |
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