CN1670028A - Method for preparing L-fucoidan in sea tangle - Google Patents
Method for preparing L-fucoidan in sea tangle Download PDFInfo
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Abstract
The invention relates to a simple method for preparing L-fucoidan by a kind of sea-tangle from Qingdao as materials which comprises: extracting and purifying the said sea-tangle by the water extract and ethanol precipitation to get purified fucoidan sulfate, then hydrolyzing sulphuric acid, filtering and the filtrate desalting through a column, deoxidizing and decolouring, filtering and the filter liquor rotating and concentrating in vacuum, alcohol depositing, the filter liquor rotating and concentrating to get syrup in vacuum, alcohol depositing, the filter liquor rotating and concentrating to get syrup in vacuum, adding the right amount mixture of alcohol and acetone, and adding several L-fucoidan particles to standard seed and crystal. The production purity is 98.1 %, and the productivity is 16.2-17.0 % in the invention.
Description
Technical field
The present invention relates to the preparation method of L-fucose in refining monose preparation method's improvement and the application, particularly a main laminaria, it belongs to sea-tangle deep process technology field.
Background technology
Sea-tangle, be a kind of large edible phaeophyta, the herb of Zosteraceae plant sea tangle (Laminaria japonicaAresch), it belongs to the sea-tangle (laminaria) of phaeophyta (phaeophyta), Laminariales (laminariales), Laminariaceae (laminariceae).Have more than 50 to plant in this genus, extensively edible in the world has four kinds: sea-tangle (Laminariajaponica aresch), sharp buttocks sea-tangle (L.ochotensis-Miy), narrow leaf sea-tangle (L.angustata kjellm) and Changhai band (L.longissima Mijabe).The present self-sow of China and that propagate artificially is sea-tangle (Laminariajaponica aresch).In the seaweed industry early stage of development, China mainly concentrates on large extract of iodine, N.F,USP MANNITOL, algin etc. the comprehensive action research of sea-tangle.In recent years, owing to be subjected to the influence of chemosynthesis and other method, Market competition; Simultaneously,, cause three big products production costs to remain high, cause many sea-tangles processing enterprise to be in the edge of meagre profit or loss because at present processing technique for kelp exists problems such as water loss is big, power consumption is big, seriously polluted.Chinese Academy of Sciences ocean utilization such as Xu's ancestral flood, Li Zhien are original produces the waste residue that iodine, N.F,USP MANNITOL, algin production line produced, the success (having applied for patent) of waste liquid extraction algal polysaccharide sulfate, and formed industrialization, not only efficiently solve the problem of environmental pollution of sea-tangle processing industry, also reduced simultaneously the production cost of the said products significantly, improve the high added value of the comprehensive industry of sea-tangle, promoted further developing of China's seaweed industry and aquaculture.Further preparation L-fucose on this basis, will improve the quality scale of above-mentioned industry product greatly, for perfect technology platform is set up in the sea-tangle industrialization, thereby better synthesis is utilized the sea-tangle resource of China's abundant, creating bigger economic benefit, is the strong promotion to the high added value of the comprehensive industry of sea-tangle.
L-fucose (L-fucose) has another name called L-Fucose, 6-deoxidation-L-semi-lactosi, is a kind of with the naturally occurring rare saccharide of L-isomer.In vivo, the L-fucose mainly is present in the non-reducing end of mixture glycosidic linkages such as big polysaccharide protein and sugar ester and the molecular weight bigger sugar ester and blood group antigen.In addition, also be present in the exocellular polysaccharide (EPS) of certain micro-organisms, but it is present in the algal polysaccharide sulfate more.Algal polysaccharide sulfate is the intercellular a kind of polysaccharide of brown alga, is the viscous substance that brown alga emiocytosis produces, by brown alga utilizes light and nutrition essential.Its content is different and different with marine alga kind, the place of production, season and frond position.Its molecular weight is quite big, and molecular structure is very complicated, and mainly by 1, the poly-α that 2-connects-L-pyrans fucose is formed, and an active group-sulfuric ester is on average arranged on each monose, mainly is present in C
4Hydroxy position on, on a small quantity at C
3Hydroxy position on.Secondly, it also is attended by a spot of semi-lactosi, seminose, wood sugar, uronic acid, rhamnosyl and protein etc.
Discover monose both at home and abroad in a large number---the L-fucose plays an important role in the physiology of saccharide complex and biological function, can suppress lung tumors proliferation of cells (being anticarcinogenic effect), suppress white cell and form (being antiinflammation), treatment rheumatic arthritis and synthetic some immunizing antigen or the like as it.L-fucose content in the now existing lot of documents report cancer patients serum protein is higher to be because fucose acyltransferase height is active, and this just illustrates and exists some to get in touch between cell transformation effect (carcinogenesis) and the metabolism of L-Fucose; L-fucose content is higher in diabetic subject's serum, illustrates that it is to suppress a kind of potential inhibitor that inositol shifts; Free L-fucose level has been reacted the extent of metabolism of sugar chain in the saccharide complex in the tumour patient urine, can be used as tumor marker clinically.Find again that recently the L-fucose can promote human fibroblast's hyperplasia; Can be used as Green Tea Extract interferential protective material etc.Simultaneously, skin-moisturizing, skin effect and the antianaphylaxis effect in view of the L-fucose also is applied to the makeup aspect.Therefore, the L-fucose has broad application prospects in fields such as medicine, makeup.In addition, the L-fucose still is a kind of very important biochemical reagents, has many-sided biological activity.It is widely used in chemical analysis, biotechnology, cell engineering and sugared engineering etc.The preparation method of L-fucose has much in the prior art,, enzymic synthesis synthetic as: chemosynthesis, microorganism and adopt chemistry or enzymic hydrolysis to contain Microbial exopolysaccharides (EPS) of L-fucose or the like.Wherein, chemical synthesis process normally changes into the L-fucose by common monose such as L-arabinose, D-glucose, D-seminose, D-semi-lactosi or the like by a series of chemical reaction, and reactions steps is loaded down with trivial details and productive rate is low, is difficult to realize industrialization production; The microorganism synthesis method is similar to chemosynthesis, complex steps, and productive rate is low; The enzymic synthesis method is prematurity still at present, only is among the exploration; Contain the L-fucose Microbial exopolysaccharides (EPS) though chemistry or enzyme liberating method opened up a new way for effective preparation L-fucose, but because of the high viscosity that relates to the microbial polysaccharide fraction, the selection of bacterium chain or the like numerous factors, want the efficient production fucose, this method improvement of still needing.And be that the method that raw material prepares the L-fucose roughly has two kinds: phenylhydrazine crystallization process and alcohol crystal method with the brown alga.Someone studies preparation L-fucose from ditch siliquosa Pelvetia, black wrack, bladder wrack.There was the people to obtain crystalline L-fucose by optimizing the hydrolysis separation condition again up to 1966, but all because of the purity of product and of low quality.Its technology is perfect inadequately, is difficult to be applied to suitability for industrialized production.Find that after deliberation the chemical constitution content of algal polysaccharide sulfate of different sources and the molar ratio of monosaccharide component thereof have evident difference, its assay determination the results are shown in Table 1, table 2:
The chemical constitution of the algal polysaccharide sulfate of table 1 different sources
| The brown alga kind | L-fucose %) | Sulfate radical (%) | Nitrogen (%) | Ash content |
| Sargassum kjellmanianum Yendo | ????26.5 | ????14.8 | ????0.6 | ????20.8 |
| Mouse tail algae | ????25.4 | ????17.0 | ????1.0 | ????22.6 |
| The Purpleflower Holly Leaf sargassun | ????13.3 | ????12.6 | ????1.3 | ????20.8 |
| Sea-tangle (Dalian product) | ????24.0 | ????30.0 | ????0.9 | ????27.3 |
| Sea-tangle (Fujian product) | ????29.3 | ????30.8 | ????1.2 | ????29.8 |
| Sea-tangle (Qingdao product) | ????28.8 | ????30.2 | ????1.4 | ????31.2 |
The molar ratio of the algal polysaccharide sulfate monosaccharide component of table 2 different sources
| The brown alga kind | The L-fucose | Semi-lactosi | Wood sugar | Glucose |
| Sargassum kjellmanianum Yendo | ????1.00 | ????0.24 | ????0.05 | ????0.04 |
| Mouse tail algae | ????1.00 | ????0.24 | ????- | ????0.03 |
| The Purpleflower Holly Leaf sargassun | ????1.00 | ????0.36 | ????0.16 | ????0.08 |
| Sea-tangle (Dalian product) | ????1.00 | ????0.15 | ????- | ????- |
| Sea-tangle (Fujian product) | ????1.00 | ????0.09 | ????- | ????- |
| Sea-tangle (Qingdao product) | ????1.00 | ????0.36 | ????- | ????- |
Result of study shows that from the monosaccharide component of the algal polysaccharide sulfate of sea-tangle extraction mainly be L-fucose and D-semi-lactosi, and the monosaccharide component ratio in the algal polysaccharide sulfate that Qingdao product sea-tangle is extracted is 1.00: 0.36.The component that is contained with other phaeophyta sargassum kjellmanianum Yendo, mouse tail algae etc. has significant difference.Therefore, from sea-tangle is produced in Qingdao, isolate algal polysaccharide sulfate, and then to isolate the L-fucose with simple method be feasible.
Summary of the invention
The objective of the invention is to improve the high added value of the comprehensive industry of China sea-tangle, enlarge the sea-tangle deep process technology, a kind of preparation method who prepares L-fucose in the sea-tangle is provided, for determining that its application at field of medicaments has important significance for theories and using value, the high-value-use of sea-tangle resource is done the contribution that makes new advances.
The technical scheme that the present invention need solve is to have developed the preparation method of L-fucose in the sea-tangle, and it is a kind of preparation method of 6-deoxyhexamethylose class monose.
The present invention gets L-fucose in the sea-tangle at the enterprising one-step refining in algal polysaccharide sulfate basis of purifying.It is raw material that the present invention produces sea-tangle with Qingdao, at first extract Crude polysaccharides by water extraction and alcohol precipitation method, concrete grammar is: after sea-tangle is cut into shred, with certain density formaldehyde solution soaked overnight, add the distilled water boiling water extraction then, diatomite filtration, the filtrate dialysis, concentrate, 75% ethanol sedimentation, vacuum-drying gets thick algal polysaccharide sulfate.Crude polysaccharides is heavy water-soluble, at 0.05mol/L MgCl
2Have 20% ethanol sedimentation down, to remove water-soluble algin, the filtrate dialysis concentrates back 75% ethanol sedimentation, the algal polysaccharide sulfate that vacuum-drying can obtain purifying.
The preparation method of L-fucose is to be raw material with the sea-tangle in the sea-tangle of the present invention, through the algal polysaccharide sulfate that water extraction and alcohol precipitation method extracts and purifying obtains purifying; Again by following purification step:
1) get a certain amount of purification algal polysaccharide sulfate and add water and add the acid reaction that is hydrolyzed again, by the part by weight 1 of this polysaccharide and water, concentrated acid: 40-80: 1.96--19.6 adds water and adds acid again, and the back hydrolysis time of gently boiling is 3-4 hour;
2) after the hydrolyzed solution cooling, be neutralized to pH7 ± 0.2, filter, remove precipitation with barium carbonate;
3) with 2) filtrate of step gained is by 732 strong acid cation resin posts, collects effluent liquid, removes inorganic salt such as K, Na.Ca, Mg, uses this filtrate 0.5-1 volume distilled water wash doubly then, collect to merge effluent liquid and washings is positive resin flow part;
4) an amount of IRA-67 weak base anion resins is joined 3) go on foot in positive resin flow part of gained, the uninterrupted stirring observed the pH value to terminal, separates this resin anion(R.A) and removes uronic acid and sulfate; Use this parting liquid 0.05-0.1 volume this resin anion(R.A) of distilled water wash doubly again; Collecting merging parting liquid and washings is negative resin stream part;
5) with 4) the negative resin stream part vacuum concentration of step gained is to 1/100 of original volume, and again by the alcoholic acid volume ratio 1 of this concentrated solution and 95%: 10-20 adds 95% ethanol, and precipitation is removed in filtration; With this filtrate again vacuum concentration to 1/150 syrupy shape of original volume;
6) with 5) syrup of step gained, be dissolved in the 50-100 volume dehydrated alcohol doubly, filter, remove precipitation; This filtrate again vacuum concentration to 1/100 syrupy shape of original volume;
7) with 6) syrup of step gained, be dissolved in the 50-100 volume distilled water doubly, and add the 0.04-0.07 gac doubly of this distilled water weight, boiled 30 minutes, do not stop to stir, diatomite filtration while hot then, filtrate again vacuum concentration to 1/100 syrupy shape of original volume;
8) with 7) resulting syrup of step is transferred in the weighing bottle, adds 5.0-10.0 this syrup of anhydrous alcohol solution doubly of this syrup volume, adds the 2.0-4.0 acetone doubly of this syrup volume then, filters, and discard and leach thing;
9) with 8) step gained filtrate, charge seed by weight and drop into standard L-fucose crystal seed than 0.5 ‰, place 5 ℃ refrigerator, 3-7 days post crystallizations filter, and filtrate still places refrigerator, to treat further crystallization, get and leach crystallisate absolute ethanol washing 2 times, vacuum-drying more promptly gets rough L-fucose mixed crystal;
10) because 9) the rough L-fucose of step gained still contains the semi-lactosi of 18.9-21.7%, needs and will add the methyl alcohol-acetone mixing solutions of 50～60 times of volumes in the rough fucose mixed crystal, and wherein methyl alcohol-acetone volume ratio is 9: 5; 5 ℃ of dissolvings 5～8 hours, constantly stir, make the more ground stripping of L-fucose;
11) with 10) mixed solution of step gained filters, and gets filtrate, at 1/90 the syrupy shape of 55 ℃～60 ℃ vacuum concentration to original volume,
12) with 11) syrup of step gained joins in the dehydrated alcohol of 5.0-10.0 times of volume and dissolves, and charges seed by weight and drops into standard L-fucose crystal seeds than 5 ‰, and the refrigerator that places 5 ℃ filtered after 3～7 days, and vacuum-drying promptly gets the high L-fucose crystal of purity; Gained L-fucose crystalline productive rate is 16.2%～17.0%.
Described hydrolysis reaction, its temperature of reaction is: 100 ℃-110 ℃.
Described 3) Bu 732 strong acid cation resin post specifications are: Φ 3.5 * 54～60cm; The flow velocity that described filtrate is crossed resin column is: 1～2 times of resin column volume/hour; The flow velocity that described washings is crossed resin column be 1～2 times of resin column volume/hour; This filtrate and washings are spent 2～4 hours total times of resin column, can reach the purpose of desalination.
Described 4) the observation terminal point in the step is pH7 ± 0.2.
Described 5), 6), 7), 11) technology condition of vacuum concentration is in the step: vacuum degree control is at 0.09～0.1MPa, and controlled temperature is 55～60 ℃, vacuum concentration 3～4 hours.
The invention has the advantages that: because of the present invention 1) step algal polysaccharide sulfate of 10g is placed be furnished with agitator, there-necked flask that thermostat temperature is taken into account prolong, add 800ml water and transfer to 0.25mol/L, at 100 ℃-110 ℃ back hydrolysis 4 hours of gently boiling with sulfuric acid; Make monosaccharide component in the algal polysaccharide sulfate: L-fucose and D-semi-lactosi reflux gently boiling, and are decomposed and dissociate out.Because the monosaccharide component ratio in the algal polysaccharide sulfate that Qingdao product sea-tangle is extracted is 1.00: 0.36.The component that is contained with other phaeophyta sargassum kjellmanianum Yendo, mouse tail algae etc. has significant difference.Like this, it is feedstock production L-fucose method that the present invention produces sea-tangle with Qingdao, and its technology is simple, and the purity and the productive rate of the L-fucose product of decomposition are higher.Again owing to determined filtrate and be with the suitable flow velocity of crossing resin column: 1～2 times of resin column volume/hour; With determined washings cross the suitable flow velocity of resin column be 1～2 times of resin column volume/hour; This filtrate and washings are spent 2～4 hours total times of resin column, make that decomposing the L-fucose and the ionizable metal salt that dissociate out thoroughly breaks away from, and reach the purpose of desalination, have improved the purity of L-fucose product.Owing to determined 5), 6), 7) and, 11) technology condition of vacuum concentration is in the step: vacuum degree control is at 0.09～0.1MPa, and controlled temperature is 55～60 ℃, vacuum concentration 3～4 hours; Make that the quality and the productive rate of L-fucose product are all higher.
Embodiment
Below by embodiment to detailed description of the present invention;
Embodiment 1:
Getting Qingdao product sea-tangle is raw material, through the algal polysaccharide sulfate that water extraction and alcohol precipitation method extracts and purifying obtains purifying; Again by following purification step:
1) gets a certain amount of purification algal polysaccharide sulfate and add water and add the acid reaction that is hydrolyzed again, add water at 1: 80: 19.6 by the part by weight of this polysaccharide and water, concentrated acid and add acid again, at 100 ℃-110 ℃ back hydrolysis 4 hours of gently boiling;
2) after the hydrolyzed solution cooling, be neutralized to pH7 ± 0.2, filter, remove precipitation with barium carbonate;
3) with 2) filtrate of step gained is by 732 strong acid cation resin posts, collects effluent liquid, removes inorganic salt such as K, Na.Ca, Mg, uses this filtrate 1 volume distilled water wash doubly then, collect to merge effluent liquid and washings is positive resin flow part;
4) an amount of IRA-67 weak base anion resins is joined 3) go on foot in positive resin flow part of gained, the uninterrupted stirring observed the pH value to terminal, separates this resin anion(R.A) and removes uronic acid and sulfate; Use this parting liquid 0.1 volume this resin anion(R.A) of distilled water wash doubly again; Collecting merging parting liquid and washings is negative resin stream part;
5) with 4) the negative resin stream part vacuum concentration of step gained is to 1/100 of original volume, adds 95% ethanol at 1: 20 by this concentrated solution and 95% alcoholic acid volume ratio again, and precipitation is removed in filtration; With this filtrate again vacuum concentration to 1/150 syrupy shape of original volume;
6) with 5) syrup of step gained, be dissolved in the 80 volumes dehydrated alcohol doubly, filter, remove precipitation; This filtrate again vacuum concentration to 1/100 syrupy shape of original volume;
7) with 6) syrup of step gained, be dissolved in the 100 volumes distilled water doubly, and add 0.07 times gac of this distilled water weight, boiled 30 minutes, do not stop to stir, diatomite filtration while hot then, filtrate again vacuum concentration to 1/100 syrupy shape of original volume;
8) with 7) step resulting syrup be transferred in the weighing bottle, 10.0 times this syrup of anhydrous alcohol solution that adds this syrup volume, 4.0 times the acetone that adds this syrup volume then, the an amount of dehydrated alcohol that adds makes the syrup dissolving, add acetone again, as generate white floss, and need to filter, discard and leach thing;
9) with 8) step gained filtrate, charge seed by weight and drop into standard L-fucose crystal seed than 0.5 ‰, place 5 ℃ refrigerator, 3-7 days post crystallizations filter, and filtrate still places refrigerator, to treat further crystallization, get and leach crystallisate absolute ethanol washing 2 times, vacuum-drying more promptly gets rough L-fucose mixed crystal;
10) because 9) the rough L-fucose of step gained still contains the semi-lactosi of 18.9-21.7%, needs to add the methyl alcohol-acetone mixing solutions of 55 times of volumes in the rough fucose mixed crystal, and wherein methyl alcohol-acetone volume ratio is 9: 5; 5 ℃ of dissolvings 5～8 hours, constantly stir, make the more ground stripping of L-fucose;
11) with 10) mixed solution of step gained filters, and gets filtrate, at 1/90 the syrupy shape of 55 ℃～60 ℃ vacuum concentration to original volume;
12) with 11) syrup of step gained joins in the dehydrated alcohol of 10.0 times of volumes and dissolves, charge seed by weight again and drop into standard L-fucose crystal seed than 5 ‰, the refrigerator that places 5 ℃ is after 3～7 days, filter, vacuum-drying, promptly getting the high L-fucose crystal gained monose productive rate of purity is 16.2%, and molten point is 135 ℃-137 ℃, and specific rotatory power is [α]
D 20Be-76.9.
Embodiment 2:
Get algal polysaccharide sulfate 10g place be furnished with agitator, there-necked flask that thermostat temperature is taken into account prolong, add 400ml water and transfer to 0.5mol/L, at 100 ℃ of back hydrolysis 4 hours of gently boiling with sulfuric acid.All the other conditions are with embodiment 1.
Embodiment 3:
By algal polysaccharide sulfate sample and sulfuric acid part by weight is 10: 1.96, get a certain amount of algal polysaccharide sulfate sample and place an ampere pipe, and tube sealing hydrolysis 3 hours, all the other conditions are with embodiment 1.
Those of ordinary skill in the art can understand, and in protection scope of the present invention, makes amendment for the foregoing description, and it all is possible adding and replacing, and it does not all exceed protection scope of the present invention.
Claims (5)
1, the preparation method of L-fucose in the sea-tangle, it is a kind of preparation method of 6-deoxyhexamethylose class monose, it is characterized in that: described preparation method is to be raw material with the sea-tangle, through the algal polysaccharide sulfate that water extraction and alcohol precipitation method extracts and purifying obtains purifying; Again by following purification step:
1) get a certain amount of purification algal polysaccharide sulfate and add water and add the acid reaction that is hydrolyzed again, by the part by weight 1 of this polysaccharide and water, concentrated acid: 40-80: 1.96--19.6 adds water and adds acid again, and the back hydrolysis time of gently boiling is 3-4 hour;
2) after the hydrolyzed solution cooling, be neutralized to pH7 ± 0.2, filter, remove precipitation with barium carbonate;
3) with 2) filtrate of step gained is by 732 strong acid cation resin posts, collects effluent liquid, removes inorganic salt such as K, Na.Ca, Mg, uses this filtrate 0.5-1 volume distilled water wash doubly then, collect to merge effluent liquid and washings is positive resin flow part;
4) an amount of IRA-67 weak base anion resins is joined 3) go on foot in positive resin flow part of gained, the uninterrupted stirring observed the pH value to terminal, separates this resin anion(R.A) and removes uronic acid and sulfate; Use this parting liquid 0.05-0.1 volume this resin anion(R.A) of distilled water wash doubly again; Collecting merging parting liquid and washings is negative resin stream part;
5) with 4) the negative resin stream part vacuum concentration of step gained is to 1/100 of original volume, and again by the alcoholic acid volume ratio 1 of this concentrated solution and 95%: 10-20 adds 95% ethanol, and precipitation is removed in filtration; With this filtrate again vacuum concentration to 1/150 syrupy shape of original volume;
6) with 5) syrup of step gained, be dissolved in the 50-100 volume dehydrated alcohol doubly, filter, remove precipitation; This filtrate again vacuum concentration to 1/100 syrupy shape of original volume;
7) with 6) syrup of step gained, be dissolved in the 50-100 volume distilled water doubly, and add the 0.04-0.07 gac doubly of this distilled water weight, boiled 30 minutes, do not stop to stir, diatomite filtration while hot then, filtrate again vacuum concentration to 1/100 syrupy shape of original volume;
8) with 7) resulting syrup of step is transferred in the weighing bottle, adds 5.0-10.0 this syrup of anhydrous alcohol solution doubly of this syrup volume, adds the 2.0-4.0 acetone doubly of this syrup volume then, filters, and discard and leach thing;
9) with 8) step gained filtrate, charge seed by weight and drop into standard L-fucose crystal seed than 0.5 ‰, place 5 ℃ refrigerator, 3-7 days post crystallizations filter, and filtrate still places refrigerator, to treat further crystallization, get and leach crystallisate absolute ethanol washing 2 times, vacuum-drying more promptly gets rough L-fucose mixed crystal;
10) because 9) the rough L-fucose of step gained still contains the semi-lactosi of 18.9-21.7%, needs and will add the methyl alcohol-acetone mixing solutions of 50～60 times of volumes in the rough fucose mixed crystal, and wherein methyl alcohol-acetone volume ratio is 9: 5; 5 ℃ of dissolvings 5～8 hours, constantly stir, make the more ground stripping of L-fucose;
11) with 10) mixed solution of step gained filters, and gets filtrate, at 1/90 the syrupy shape of 55 ℃～60 ℃ vacuum concentration to original volume,
12) with 11) syrup of step gained joins in the dehydrated alcohol of 5.0-10.0 times of volume and dissolves, and charges seed by weight and drops into standard L-fucose crystal seeds than 5 ‰, and the refrigerator that places 5 ℃ filtered after 3～7 days, and vacuum-drying promptly gets the high L-fucose crystal of purity; Gained L-fucose crystalline productive rate is 16.2%～17.0%.
2, according to the preparation method of L-fucose in the described sea-tangle of claim 1, it is characterized in that: described hydrolysis reaction, its temperature of reaction is: 100 ℃-110 ℃.
3, according to the preparation method of L-fucose in the described sea-tangle of claim 1, it is characterized in that: described 3) Bu 732 strong acid cation resin post specifications are: Φ 3.5 * 54～60cm; The flow velocity that described filtrate is crossed resin column is: 1～2 times of resin column volume/hour; The flow velocity that described washings is crossed resin column be 1～2 times of resin column volume/hour; This filtrate and washings are spent 2～4 hours total times of resin column, can reach the purpose of desalination.
4, according to the preparation method of L-fucose in the described sea-tangle of claim 1, it is characterized in that: described 4) the observation terminal point in the step is pH7 ± 0.2.
5, according to the preparation method of L-fucose in the described sea-tangle of claim 1, it is characterized in that: described 5), 6), 7), 11) technology condition of vacuum concentration is in the step: vacuum degree control is at 0.09～0.1MPa, and controlled temperature is 55～60 ℃, vacuum concentration 3～4 hours.
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| CN102234336A (en) * | 2010-04-24 | 2011-11-09 | 中国科学院海洋研究所 | Fucoidan-galactosan sulfate, extracting, separating, and purifying method thereof, and application thereof |
| CN102511926A (en) * | 2011-12-23 | 2012-06-27 | 华南理工大学 | Method for extracting and separating laminarin with low molecular weight and application thereof in cigarette products |
| JP2013530909A (en) * | 2010-04-27 | 2013-08-01 | チャイナ シェンフア エナジー カンパニー リミテッド | Process for preparing industrial alumina using fluidized bed fly ash |
| CN106632525A (en) * | 2016-12-27 | 2017-05-10 | 厦门欣赛科技有限公司 | Method for separating sulfuric acid from a glucose-xylose solution |
| CN112513103A (en) * | 2018-07-27 | 2021-03-16 | Arc医疗器械股份有限公司 | High-purity fucoidan for treating fibrous adhesion |
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| US3240775A (en) * | 1962-07-30 | 1966-03-15 | Kelco Co | Preparation of alpha-l-fucosides and l-fucose from fucoidan |
| JPH1135591A (en) * | 1997-07-18 | 1999-02-09 | Masakuni Tako | Production of l-fucose from fucoidan separated from cladosiphon okamuranus tokida and its production |
| CN1115166C (en) * | 1998-05-29 | 2003-07-23 | 青岛海洋大学 | Preparation of polyfucose sulfate with varible molecular weight |
| JP2000351790A (en) * | 1999-06-07 | 2000-12-19 | Yaizu Suisankagaku Industry Co Ltd | Production of fucose-containing oligosaccharide, or its composition and fucose-containing oligosaccharide or its composition |
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| CN102234336A (en) * | 2010-04-24 | 2011-11-09 | 中国科学院海洋研究所 | Fucoidan-galactosan sulfate, extracting, separating, and purifying method thereof, and application thereof |
| CN102234336B (en) * | 2010-04-24 | 2013-12-25 | 中国科学院海洋研究所 | Fucoidan-galactosan sulfate, extracting, separating, and purifying method thereof, and application thereof |
| JP2013530909A (en) * | 2010-04-27 | 2013-08-01 | チャイナ シェンフア エナジー カンパニー リミテッド | Process for preparing industrial alumina using fluidized bed fly ash |
| CN102511926A (en) * | 2011-12-23 | 2012-06-27 | 华南理工大学 | Method for extracting and separating laminarin with low molecular weight and application thereof in cigarette products |
| CN106632525A (en) * | 2016-12-27 | 2017-05-10 | 厦门欣赛科技有限公司 | Method for separating sulfuric acid from a glucose-xylose solution |
| CN112513103A (en) * | 2018-07-27 | 2021-03-16 | Arc医疗器械股份有限公司 | High-purity fucoidan for treating fibrous adhesion |
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