CN101037483A - Method for extracting brown algae polysaccharide sulfated - Google Patents
Method for extracting brown algae polysaccharide sulfated Download PDFInfo
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- CN101037483A CN101037483A CN 200710014573 CN200710014573A CN101037483A CN 101037483 A CN101037483 A CN 101037483A CN 200710014573 CN200710014573 CN 200710014573 CN 200710014573 A CN200710014573 A CN 200710014573A CN 101037483 A CN101037483 A CN 101037483A
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Abstract
The invention relates to ocean chemical engineering technique field, concretely is a method for extracting fucoidan from a kelp soak solution, which includes steps: adding 1-10 ml flocculant to kelp soak solution per 150 ml, stirring for 2-10 min, flocculating for 10 min to 8 h, swelling for 1-24 h under condition that pH is 2-6 after centrifuging and depositing, stirring for 1-4 h to dissolve, filtrating and adjusting the filtrate to neutrality, decompressing and concentrating, adding ethanol to the concentrated solution, filtrating to obtain deposition, washing and drying the deposition to obtain the fucoidan. The invention relates to employs chitosan and its derivative as flocculant to flocculate and deposit ''sugar glue'' from kelp soak solution, and then extracts fucoidan from the ''sugar glue''. The advantages of the invention are: resources are utilized comprehensively, operation is simply, quantity of used acid and base is reduced, and quantity of the obtained fucoidan reaches 5-16% of quantity of the deposition.
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
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.
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 (6)
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, chitosan carboxymethyl derivant or chitosan quaternary ammonium salt derivatives, and its molecular weight is 2000-76 ten thousand.
2. the method for extraction algal polysaccharide sulfate according to claim 1, it is characterized in that: described chitosan, carboxymethyl chitosan derivative or chitosan quaternary ammonium salt derivatives for its concentration at the 1-3% acid solution or the aqueous solution, acid solution is acetate or the aqueous hydrochloric acid of 1%-3%.
3. 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.
4. 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.
5. 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.
6. 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 true CN101037483A (en) | 2007-09-19 |
| CN100540568C 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 (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830996A (en) * | 2010-04-21 | 2010-09-15 | 江南大学 | Method for separating and purifying blue algae polysaccharide |
| CN102367282A (en) * | 2011-10-20 | 2012-03-07 | 广东中烟工业有限责任公司 | Laminaria japonica polysaccharide, its preparation method and application |
| CN102367284A (en) * | 2011-10-20 | 2012-03-07 | 广东中烟工业有限责任公司 | Porphyra polysaccharide as well as preparation method and application thereof |
| CN103848924A (en) * | 2014-03-22 | 2014-06-11 | 吉林省辉南长龙生化药业股份有限公司 | Brown seaweed polysaccharide sulfate extraction method |
| 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 |
| 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 |
| CN103980373A (en) * | 2014-05-21 | 2014-08-13 | 吉林省辉南长龙生化药业股份有限公司 | Method for extracting fucoidan polysaccharide sulfate |
| CN104448023A (en) * | 2014-12-19 | 2015-03-25 | 桂林市和胤祥新型材料有限公司 | Method for extracting polysaccharide sulfate from laminaria japonica |
| CN105154885A (en) * | 2015-09-11 | 2015-12-16 | 中国科学院海洋研究所 | Application of efficient corrosion inhibitor |
| 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) |
| WO2020019077A1 (en) * | 2018-07-27 | 2020-01-30 | Arc Medical Devices Inc. | Low endotoxin fucan compositions, systems and methods |
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| 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 |
Family Cites Families (7)
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| JP3408180B2 (en) * | 1999-02-17 | 2003-05-19 | 株式会社沖縄発酵化学 | How to extract fucoidan |
| CN1157416C (en) * | 2001-06-15 | 2004-07-14 | 中国科学院化工冶金研究所 | Flocculating extraction process of seawweed polysaccharide |
| CN1344565A (en) * | 2001-10-19 | 2002-04-17 | 汤洁 | Fucoidin ester as antiviral immunoregulator and its prepn |
| CN1243026C (en) * | 2004-03-12 | 2006-02-22 | 中国海洋大学 | Preparation process for fucosan sulfate of high sulfuric content |
| JP2006160862A (en) * | 2004-12-07 | 2006-06-22 | Oki Bussan:Kk | Method for extracting fucoidan |
| US20070087996A1 (en) * | 2005-10-18 | 2007-04-19 | Hideaki Hagiwara | Method of extracting fucoidan |
| CN100425622C (en) * | 2006-09-28 | 2008-10-15 | 青岛明月海藻集团有限公司 | Process of comprehensive utilization sea-tangle for extracting fucoidin |
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2007
- 2007-04-20 CN CNB200710014573XA patent/CN100540568C/en not_active Expired - Fee Related
Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830996A (en) * | 2010-04-21 | 2010-09-15 | 江南大学 | Method for separating and purifying blue algae polysaccharide |
| CN102367282A (en) * | 2011-10-20 | 2012-03-07 | 广东中烟工业有限责任公司 | Laminaria japonica polysaccharide, its preparation method and application |
| CN102367284A (en) * | 2011-10-20 | 2012-03-07 | 广东中烟工业有限责任公司 | Porphyra polysaccharide as well as preparation method and application thereof |
| 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 |
| 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 |
| CN103848924A (en) * | 2014-03-22 | 2014-06-11 | 吉林省辉南长龙生化药业股份有限公司 | Brown seaweed polysaccharide sulfate extraction 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 |
| CN103980373A (en) * | 2014-05-21 | 2014-08-13 | 吉林省辉南长龙生化药业股份有限公司 | Method for extracting fucoidan polysaccharide sulfate |
| CN104448023A (en) * | 2014-12-19 | 2015-03-25 | 桂林市和胤祥新型材料有限公司 | Method for extracting polysaccharide sulfate from laminaria japonica |
| CN105154885A (en) * | 2015-09-11 | 2015-12-16 | 中国科学院海洋研究所 | Application of efficient corrosion inhibitor |
| 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) |
| WO2020019080A1 (en) * | 2018-07-27 | 2020-01-30 | Arc Medical Devices Inc. | Highly purified and/or modified fucan compositions for the treatment of fibrous adhesions |
| WO2020019077A1 (en) * | 2018-07-27 | 2020-01-30 | Arc Medical Devices Inc. | Low endotoxin fucan compositions, systems and methods |
| CN112533989A (en) * | 2018-07-27 | 2021-03-19 | Arc医疗器械股份有限公司 | Highly purified and/or modified fucoidan composition for treating fibrous adhesions |
| JP2021532137A (en) * | 2018-07-27 | 2021-11-25 | エーアールシー メディカル デバイス，インク． | Low endotoxin fucan composition, system and method |
| US11628183B2 (en) | 2018-07-27 | 2023-04-18 | ARC Medical Ine. | Highly purified fucans for the treatment of fibrous adhesions |
| US11642368B2 (en) | 2018-07-27 | 2023-05-09 | ARC Medical Inc. | Highly purified and/or modified fucan compositions for the treatment of fibrous adhesions |
| JP7302831B2 (en) | 2018-07-27 | 2023-07-04 | エーアールシー メディカル デバイス，インク． | Low endotoxin fucan composition, system and method |
| US11938145B2 (en) | 2018-07-27 | 2024-03-26 | ARC Medical Inc. | Low endotoxin fucan compositions, systems, and methods |
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| CN100540568C (en) | 2009-09-16 |
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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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