CN106957374A - A kind of method that fucoidin and algin are extracted from algae - Google Patents
A kind of method that fucoidin and algin are extracted from algae Download PDFInfo
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- CN106957374A CN106957374A CN201610018164.6A CN201610018164A CN106957374A CN 106957374 A CN106957374 A CN 106957374A CN 201610018164 A CN201610018164 A CN 201610018164A CN 106957374 A CN106957374 A CN 106957374A
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- algin
- fucoidin
- algae
- extracted
- extractant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0063—Glycosaminoglycans or mucopolysaccharides, e.g. keratan sulfate; Derivatives thereof, e.g. fucoidan
Abstract
The invention discloses a kind of method that fucoidin and algin are extracted from algae, it the described method comprises the following steps：1) it will shred, then freezed at the beginning of dry algae, is then crushed to powdered；2) added in algae powder and promote 5-90 DEG C of immersion of decomposition agent；3) soak after terminating, suction filtration, washing, it is 10-40% that extractant to Extractant concentration is added after merging filtrate and cleaning solution, stand, centrifuging and taking precipitates to obtain algin crude product；4) in step 3) centrifugation obtained by extractant to Extractant concentration is added in supernatant is 60-90%, stand, centrifuging and taking precipitates to obtain fucoidin crude product.The present invention efficient under conditions of maintaining fucoidin and algin activity constant can extract fucoidin and algin, at the same have it is convenient, the advantages of nontoxic pollution-free and high product purity.
Description
Technical field
The present invention relates to biological and marine chemical industry technical field, brown alga is extracted from algae more particularly, to one kind
The method of carbohydrate gum and algin.
Background technology
Fucoidin is also known as algal polysaccharide sulfate, fucoidan, is that a class is present in all brown algas
Intercellular sulfated polysaccharides, its main component is the anion polymer of a-L fucose -4- sulfuric esters.In sea-tangle
The content of fucoidin is general in 0.3%-1.5%.Fucoidin being structurally characterized in that containing sulfate, sulfate mainly
The number of content directly affects the physiological property of fucoidin.Fucoidin has the anticoagulant effect of reducing blood lipid,
With obvious blood coagulation resisting function；It can also suppress growth of tumour cell, can effectively suppress mouse S-180 and
The growth of Heps tumour cells；At the same time as immunopotentiator, hematopoietic tissue caused by having preventive radiotherapy is damaged, thorn
Swash Radiation in jury and strengthen the immunologic function of cancer patient.Fucoidin or a kind of dietary fiber of high-quality.In people
There is more important physiological function in vivo, such as promote gastrointestinal peristalsis and the resistance suction of heavy metal and other toxin effect.
In a word, the numerous physiologically active of fucoidin, it is also increasing to the contribution in physianthropy.
Algin is the general designation of alginic acid and its derivative.Algin is in frond mainly with the presence of following several forms：
In the main presence in the form of the divalent metal salt such as calcium alginate in frond top layer；In the cell membrane of frond, mainly with
The forms such as calcium alginate, potassium alginate, alginic acid magnesium are present；Frond pulp it is main with sodium alginate, it is brown
The forms such as potassium alginate, alginic acid magnesium are present.Algin is a kind of organic polysaccharide class compound, is by Isosorbide-5-Nitrae-poly- β-D-
A kind of linear macromolecule polymer of mannuronic acid (M) and α-L- guluronic acids (G) composition, its relative molecular weight
In 32000-200000 or so.Algin can be widely used for food additives, pharmaceutical preparation, medical accessory, oral cavity
Dental material, organizational project, cell culture, clinical treatment etc..Due to containing polarized in the molecular structure of algin
Group, can be combined with heavy metal ion, thus can as Industrial Wastewater Treatment flocculant, can also be by algin
Combined as fixation support with certain micro-organisms, serve as activated sludge to handle organic wastewater etc..With people couple
The research and development of algin are utilized, it will be widely applied to more social fields, are that society brings higher warp
Ji benefit
At present, the extracting method of fucoidin and algin include acidifying-acid cure method, calcification-acid cure method, calcification-from
Sub- exchange process, enzymatic isolation method, ultrafiltration etc.；The extracting method of fucoidin include water extraction, sour formulation, alkaline extraction,
Calcium Chloride Method, enzymatic isolation method, ultrafiltration etc..Wherein acidity extraction algin and fucoidin, colloidal particle are small, no
Easily filtering, easily causes the Partial digestion of algin and fucoidin, it is often more important that a large amount of to use acid-base pair environment
Influence it is also very big, the waste water treatmentntrol difficult after extraction；The shortcoming that Hydrolyze method is extracted is that extracting liquid volume is excessive, is carried
Take algin and fucoidin in thing to mix, add the difficulty of separation and purifying, what enzymatic isolation method was extracted lacks
Point is that extraction time is long, and power consumption is big, and cost is higher；The shortcoming that ultrafiltration is extracted is that technical requirements are high, milipore filter
Easily pollution, unsuitable large-scale production.In addition, the difficulty of industrial facing is to be taken at present
Technique water consumption is too big, does not reach the requirement of resources conservation and sustainable use, needs the extraction of a clean and effective badly
Technique.
The content of the invention
It is an object of the present invention to provide a kind of method that fucoidin and algin are extracted from algae, this method
Efficiently, environmentally friendly, finished product purity is good, and pigment content is low, and finished product condition is high.
To reach above-mentioned purpose, present invention employs following technical scheme：
A kind of method that fucoidin and algin are extracted from algae, the described method comprises the following steps：
1) it will shred, then freezed at the beginning of dry algae, is then crushed to powdered；
2) added in algae powder and promote 5-90 DEG C of immersion of decomposition agent；
3) soak after terminating, suction filtration, washing, adding extractant to Extractant concentration after merging filtrate and cleaning solution is
10-40%, stands, centrifuging and taking precipitates to obtain algin crude product；
4) in step 3) centrifugation obtained by extractant to Extractant concentration is added in supernatant is 60-90%, stand,
Centrifuging and taking precipitates to obtain fucoidin crude product.
Preferably, the algae is selected from sea-tangle, yellow tang, undaria pinnitafida, sargassum fusifome, bark algae, bulk kelp, horse hair
Algae and the one kind become in thunder black pine algae.
Preferably, the step 1) in, cryogenic temperature be -200 to -20 degrees Celsius, refrigerant be selected from liquid nitrogen,
One kind in dry ice and low temperature refrigerator.
Preferably, the rush decomposition agent is selected from logical Qula, ethylenediamine tetra-acetic acid, sapn, tween and dodecyl sulphur
One kind in sour sodium.
Preferably, the concentration for promoting decomposition agent is 0.1-10%.
Preferably, the one kind of the extractant in ethanol, acetone, methanol, DMF, ether and isopropanol.
The present invention can under conditions of maintaining fucoidin and algin activity constant it is efficient extract fucoidin and
Algin, at the same have it is convenient, the advantages of nontoxic pollution-free and high product purity.
The present invention compared with prior art, with advantages below and beneficial effect：
1) efficiently：Crushed after freezing and the addition of decomposition agent makes eucaryotic cell structure destroy completely, beneficial to fucoidin and brown
The high efficiency extraction of phycocolloid.
2) it is environmentally friendly：Process cleans nontoxic pollution-free.
3) high-quality：Finished product purity is good；Pigment content is reduced, and finished product condition is improved.
Embodiment
With embodiment, the present invention is further detailed explanation below.
Embodiment 1
1st, Fresh Laminaria Japonica thoroughly washes clean is removed into silt, salinity and surface other impurities with running water.
2nd, the sea-tangle drying of washes clean, normal temperature keeps in dark place.
3rd, the sea-tangle after appropriate drying is taken, is just shredded, liquid nitrogen is then added in -200 DEG C of freezings, is then crushed to powder
Last shape.
4th, it is accurate to weigh the dry sea-tangle powder of 10g, add 300mL1% Qulas and lead to, 20 DEG C of immersion 24h.Immersion knot
Shu Hou, the above-mentioned immersion sample of suction filtration, and with 50mL water washing kelp residues, merging filtrate and cleaning solution obtain extract solution.
5th, absolute ethyl alcohol is added into extract solution untill concentration of alcohol is 20%, 1h is stood, centrifuging to be precipitated as
Algin crude product.Then absolute ethyl alcohol is added in centrifuged supernatant to concentration of alcohol up to 60%, 12h is stood, from
Gains in depth of comprehension are precipitated as fucoidin crude product.Crude product is washed with 95% ethanol, acetone respectively, is freezed.
6th, lyophilized rear example weight is weighed, the total recovery rate 8% of algin is calculated；The total recovery rate 10% of fucoidin,
Wherein carbohydrate 40%, sulfate radical 20%.
Embodiment 2
1st, fresh undaria pinnitafida thoroughly washes clean is removed into silt, salinity and surface other impurities with running water.
2nd, the undaria pinnitafida drying of washes clean, normal temperature keeps in dark place.
3rd, the undaria pinnitafida after appropriate drying is taken, is just shredded, liquid nitrogen is then added in -100 DEG C of freezings, is then crushed to
It is powdered.
4th, it is accurate to weigh the dry undaria pinnitafida powder of 10g, add 300mL1% ethylenediamine tetra-acetic acids, 20 DEG C of immersion 24h.
After immersion terminates, the above-mentioned immersion sample of suction filtration, and with 50mL water washing opotism dish slags, merging filtrate and cleaning solution
Obtain extract solution.
5th, anhydrous propanone is added into extract solution untill acetone concentration is 25%, 1h is stood, centrifuging to be precipitated as
Algin crude product.Then anhydrous propanone is added in supernatant to acetone concentration up to 70%, 12h is stood, centrifuges
It is precipitated as fucoidin crude product.Crude product is washed with 95% ethanol, acetone respectively, is freezed.
6th, lyophilized rear example weight is weighed, the total recovery rate 18% of algin is calculated；The total recovery rate 15% of fucoidin,
Wherein carbohydrate 45%, sulfate radical 10%.
Embodiment 3
1st, fresh yellow tang thoroughly washes clean is removed into silt, salinity and surface other impurities with running water.
2nd, the yellow tang drying of washes clean, normal temperature keeps in dark place.
3rd, the yellow tang after appropriate drying is taken, is just shredded, liquid nitrogen is then added in -150 DEG C of freezings, is then crushed to
It is powdered.
4th, it is accurate to weigh the dry yellow tang powder of 10g, add 300mL1% sapns, 90 DEG C of immersion 24h.Immersion knot
Shu Hou, the above-mentioned immersion sample of suction filtration, and with 50mL water washing yellow tang slags, merging filtrate and cleaning solution must be extracted
Liquid.
5th, anhydrous propanone is added into extract solution untill acetone concentration is 10%, 1h is stood, centrifuging to be precipitated as
Algin crude product.Then anhydrous propanone is added in supernatant to acetone concentration up to 90%, 12h is stood, centrifuges
It is precipitated as fucoidin crude product.Crude product is washed with 95% ethanol, acetone respectively, is freezed.
6th, lyophilized rear example weight is weighed, the total recovery rate 28% of algin is calculated；The total recovery rate 40% of fucoidin,
Wherein carbohydrate 30%, sulfate radical 25%.
Embodiment 4
1st, fresh sargassum fusifome thoroughly washes clean is removed into silt, salinity and surface other impurities with running water.
2nd, the sargassum fusifome drying of washes clean, normal temperature keeps in dark place.
3rd, the sargassum fusifome after appropriate drying is taken, is just shredded, dry ice is then added in -60 DEG C of freezings, is then crushed to powder
Last shape.
4th, it is accurate to weigh the dry sargassum fusifome powder of 10g, add 300mL1% tweens, 5 DEG C of immersion 24h.Immersion knot
Shu Hou, the above-mentioned immersion sample of suction filtration, and with 50mL water washing sargassum fusifome slags, merging filtrate and cleaning solution must be extracted
Liquid.
5th, absolute ethyl alcohol is added into extract solution untill methanol concentration is 25%, 1h is stood, centrifuging to be precipitated as
Algin crude product.Then absolute methanol is added in supernatant to methanol concentration up to 65%, 12h is stood, centrifuges
It is precipitated as fucoidin crude product.Crude product is washed with 95% ethanol, acetone respectively, is freezed.
6th, lyophilized rear example weight is weighed, the total recovery rate 12% of algin is calculated；The total recovery rate 15% of fucoidin,
Wherein carbohydrate 45%, sulfate radical 25%.
Embodiment 5
1st, fresh bark algae thoroughly washes clean is removed into silt, salinity and surface other impurities with running water.
2nd, the bark algae drying of washes clean, normal temperature keeps in dark place.
3rd, the bark algae after appropriate drying is taken, is just shredded, is then then crushed in -20 DEG C of freezings using low temperature refrigerator
It is extremely powdered.
4th, it is accurate to weigh the dry bark algae powder of 10g, add 300mL0.1% tweens, 40 DEG C of immersion 24h.Immersion
After end, the above-mentioned immersion sample of suction filtration, and with 50mL water washing bark algae-residues, merging filtrate and cleaning solution must be carried
Take liquid.
5th, dry DMF is added into extract solution untill DMF concentration is 30%, 1h is stood, centrifuging to precipitate
For algin crude product.Then dry DMF is added in supernatant to DMF concentration up to 90%, 12h is stood, from
Gains in depth of comprehension are precipitated as fucoidin crude product.Crude product is washed with 95% ethanol, acetone respectively, is freezed.
6th, lyophilized rear example weight is weighed, the total recovery rate 12% of algin is calculated；The total recovery rate 20% of fucoidin,
Wherein carbohydrate 30%, sulfate radical 10%.
Embodiment 6
1st, fresh bulk kelp thoroughly washes clean is removed into silt, salinity and surface other impurities with running water.
2nd, the bulk kelp drying of washes clean, normal temperature keeps in dark place.
3rd, the bulk kelp after appropriate drying is taken, is just shredded, liquid nitrogen is then added in -90 DEG C of freezings, is then crushed to powder
Shape.
4th, it is accurate to weigh the dry bulk kelp powder of 10g, add 300mL1% dodecyl sodium sulfates, 30 DEG C of immersion 24h.
After immersion terminates, the above-mentioned immersion sample of suction filtration, and with 50mL water washing bulk kelp slags, merging filtrate and cleaning solution are obtained
Extract solution.
5th, absolute ether is added into extract solution untill ether concentration is 40%, 1h is stood, centrifuging to be precipitated as
Algin crude product.Then absolute ether is added in supernatant to ether concentration up to 70%, 12h is stood, centrifuges
It is precipitated as fucoidin crude product.Crude product is washed with 95% ethanol, acetone respectively, is freezed.
6th, lyophilized rear example weight is weighed, the total recovery rate 18% of algin is calculated；The total recovery rate 15% of fucoidin,
Wherein carbohydrate 45%, sulfate radical 10%.
Embodiment 7
1st, new fresh sargassum thoroughly washes clean is removed into silt, salinity and surface other impurities with running water.
2nd, the sargassum drying of washes clean, normal temperature keeps in dark place.
3rd, the sargassum after appropriate drying is taken, is just shredded, liquid nitrogen is then added in -200 DEG C of freezings, is then crushed to
It is powdered.
4th, it is accurate to weigh the dry sargassum powder of 10g, add 300mL1% Qulas and lead to, 20 DEG C of immersion 24h.Immersion
After end, the above-mentioned immersion sample of suction filtration, and with 50mL water washing horse hair algae-residues, merging filtrate and cleaning solution must be carried
Take liquid.
5th, anhydrous isopropyl alcohol is added into extract solution untill isopropyl alcohol concentration is 25%, 1h is stood, centrifuging to sink
Form sediment for algin crude product.Then anhydrous isopropyl alcohol is added in supernatant to isopropyl alcohol concentration up to 85%, 12h is stood,
Fucoidin crude product must be precipitated as by centrifuging.Crude product is washed with 95% ethanol, acetone respectively, is freezed.
6th, lyophilized rear example weight is weighed, the total recovery rate 15% of algin is calculated；The total recovery rate 15% of fucoidin,
Wherein carbohydrate 50%, sulfate radical 30%.
Embodiment 8
1st, with running water by fresh change thunder black pine algae thoroughly washes clean, remove silt, salinity and surface other
Impurity.
2nd, the change thunder black pine algae drying of washes clean, normal temperature keeps in dark place.
3rd, the change thunder black pine algae after appropriate drying is taken, is just shredded, liquid nitrogen is then added and is freezed in -180 DEG C, then powder
It is broken to powdered.
4th, it is accurate to weigh the dry change thunder black pine algae powder of 10g, add 300mL10% dodecyl sodium sulfates, 20 DEG C
Soak 24h.After immersion terminates, the above-mentioned immersion sample of suction filtration, and become thunder black pine algae-residue with 50mL water washings, close
And filtrate and cleaning solution obtain extract solution.
5th, absolute ethyl alcohol is added into extract solution untill concentration of alcohol is 20%, 1h is stood, centrifuging to be precipitated as
Algin crude product.Then absolute ethyl alcohol is added in supernatant to concentration of alcohol up to 60%, 12h is stood, centrifuges
It is precipitated as fucoidin crude product.Crude product is washed with 95% ethanol, acetone respectively, is freezed.
6th, lyophilized rear example weight is weighed, the total recovery rate 48% of algin is calculated；The total recovery rate 50% of fucoidin,
Wherein carbohydrate 60%, sulfate radical 30%.
Applicant states that the present invention illustrates the detailed features and method of the present invention, but this by above-described embodiment
Invention is not limited to above-mentioned detailed features and method, that is, does not mean that the present invention has to rely on above-mentioned detailed features
And method could be implemented.Person of ordinary skill in the field is it will be clearly understood that any improvement in the present invention, right
The increase of the equivalence replacement and auxiliary material and step of selected material of the invention and step, the selection of concrete mode
Deng within the scope of all falling within protection scope of the present invention and being open.
Claims (6)
1. a kind of method that fucoidin and algin are extracted from algae, the described method comprises the following steps：
1) it will shred, then freezed at the beginning of dry algae, is then crushed to powdered；
2) added in algae powder and promote 5-90 DEG C of immersion of decomposition agent；
3) soak after terminating, suction filtration, washing, adding extractant to Extractant concentration after merging filtrate and cleaning solution is
10-40%, stands, centrifuging and taking precipitates to obtain algin crude product；
4) in step 3) centrifugation obtained by extractant to Extractant concentration is added in supernatant is 60-90%, stand,
Centrifuging and taking precipitates to obtain fucoidin crude product.
2. a kind of method that fucoidin and algin are extracted from algae according to claim 1, its feature
It is that the algae is selected from sea-tangle, yellow tang, undaria pinnitafida, sargassum fusifome, bark algae, bulk kelp, sargassum and change
One kind in thunder black pine algae.
3. a kind of method that fucoidin and algin are extracted from algae according to claim 1, its feature
Be, the step 1) in, cryogenic temperature be -200 to -20 degrees Celsius, refrigerant be selected from liquid nitrogen, dry ice and
One kind in low temperature refrigerator.
4. a kind of method that fucoidin and algin are extracted from algae according to claim 1, its feature
It is that the rush decomposition agent is selected from Qula is logical, in ethylenediamine tetra-acetic acid, sapn, tween and dodecyl sodium sulfate
One kind.
5. a kind of method that fucoidin and algin are extracted from algae according to claim 1, its feature
It is that the concentration for promoting decomposition agent is 0.1-10%.
6. a kind of method that fucoidin and algin are extracted from algae according to claim 1, its feature
It is, the one kind of the extractant in ethanol, acetone, methanol, DMF, ether and isopropanol.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107840896A (en) * | 2017-11-30 | 2018-03-27 | 江苏中大生物科技集团有限公司 | A kind of preparation method of sodium alginate |
| CN107973863A (en) * | 2017-11-30 | 2018-05-01 | 江苏中大生物科技集团有限公司 | A kind of sodium alginate preparation method based on powder morphology adsorbing separation |
| CN108329403A (en) * | 2018-02-01 | 2018-07-27 | 砀山海升果胶有限责任公司 | A kind of efficient pectous extracting method |
| CN110584135A (en) * | 2019-09-26 | 2019-12-20 | 河南工业大学 | A soluble dietary fiber extracted from brown algae and its preparation method |
| CN111454373A (en) * | 2020-04-07 | 2020-07-28 | 大连海宝渔业有限公司 | Method for separating sporophyll mucus of undaria pinnatifida |
| 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 |
| CN109851687B (en) * | 2019-03-01 | 2021-06-22 | 集美大学 | Method for separating and preparing fucoidin and algin from kelp |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107840896A (en) * | 2017-11-30 | 2018-03-27 | 江苏中大生物科技集团有限公司 | A kind of preparation method of sodium alginate |
| CN107973863A (en) * | 2017-11-30 | 2018-05-01 | 江苏中大生物科技集团有限公司 | A kind of sodium alginate preparation method based on powder morphology adsorbing separation |
| CN107840896B (en) * | 2017-11-30 | 2020-05-12 | 江苏中大生物科技集团有限公司 | Preparation method of sodium alginate |
| CN108329403A (en) * | 2018-02-01 | 2018-07-27 | 砀山海升果胶有限责任公司 | A kind of efficient pectous extracting method |
| CN108329403B (en) * | 2018-02-01 | 2019-09-27 | 砀山海升果胶有限责任公司 | A kind of efficient pectous extracting method |
| 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 |
| CN109851687B (en) * | 2019-03-01 | 2021-06-22 | 集美大学 | Method for separating and preparing fucoidin and algin from kelp |
| CN110584135A (en) * | 2019-09-26 | 2019-12-20 | 河南工业大学 | A soluble dietary fiber extracted from brown algae and its preparation method |
| CN111454373A (en) * | 2020-04-07 | 2020-07-28 | 大连海宝渔业有限公司 | Method for separating sporophyll mucus of undaria pinnatifida |
| CN111454373B (en) * | 2020-04-07 | 2022-03-01 | 大连海宝渔业有限公司 | Method for separating sporophyll mucus of undaria pinnatifida |
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