CN107674130A - A kind of method that algal polysaccharides are extracted from sea-tangle - Google Patents
A kind of method that algal polysaccharides are extracted from sea-tangle Download PDFInfo
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- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
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Abstract
The invention discloses a kind of method that algal polysaccharides are extracted from sea-tangle, it passes through following steps：（1）Fresh Laminaria Japonica is crushed, and adds the first leaching liquor and stirs 20 40 minutes, is filtered；（2）The second leaching liquor, agitation and filtration are added into the filter residue of step 1；（3）The 3rd leaching liquor, agitation and filtration are added into the filter residue of step 2；（4）First leaching liquor, the second leaching liquor and the 3rd leaching liquor are mixed, and are concentrated under reduced pressure, and adds ethanol and collects sediment；（5）The drying precipitate that step 4 is obtained obtains product.The algal polysaccharides that the method for the present invention obtains have higher yield, and have preferable sulfate content through experiment.The method rational technology of the present invention, advanced technology, suitable for the technological transformation of vast alkali carries factory, can provide higher levels of algal polysaccharides.
Description
Technical field
The present invention relates to the preparation of polysaccharide, especially a kind of method that algal polysaccharides are extracted from sea-tangle.
Background technology
Sea-tangle, it is a kind of raw brown alga plant in large-scale sea grown in low temperature seawater, belongs to seaweed plant, go for
The cooking methods such as mix, burn, stewing, boiling in a covered pot over a slow fire.Sea-tangle（Laminaria japonica）Phaeophyceae, Laminariaceae.Sporinite is large-scale, brown,
Flat belt-like, most long reachable 20M.Leaflet piece, shank and holdfast, holdfast are in rhizoid shape.Blade is epidermis, cortex and marrow
Formed, sporangium is arranged at blade bottom.With mucilage cavity, slip material can be secreted.Holdfast arborizations, to adhere to
Marine rock.It is grown on relatively low marine of water temperature.NORTH CHINA is coastal and Zhejiang, ALONG COASTAL FUJIAN are largely cultivated, and yield occupies the world
First.Rich in algin and iodine matter, the raw material of industry such as edible and extraction iodine, algin, mannitol.Its thallus can be used as medicine.
Algal polysaccharides are essentially from marine algas such as sea-tangle, deer's tail dish (sargassum fusifome), bulk kelp, yellow tang, bladder-wracks.Algal polysaccharides
Mainly include algin, fucoidin and laminaran.Isolated algin, fucoidin and laminaran from sea-tangle
Crude product is the powder of white yellowish.Purified obtained sodium alginate is white filiform；Fucoidin is milky
Powder；The two is dissolved in water, insoluble in organic solvents such as ethanol, acetone, chloroforms.Algal polysaccharides can stimulate various immunocompetences
The breaking up of cell (such as macrophage, T lymphocytes, bone-marrow-derived lymphocyte), ripe, breeding, make body immune system obtain it is extensive
Multiple and reinforcement.Algal polysaccharides contain sulfate mostly, and antivirus action and 5,042 1 contents are into positive correlation.Natural sulphur vinegar
The antiviral activity for changing polysaccharide is relevant with its sulfate group and its content, the size of molecular weight.Algal polysaccharides calcium composition
(CaSP) duplication and propagation of the energy selective depression virus in host cell, and the superfluous compound of the calcium ion formed and sulfate radical are
In host cell necessary to antiviral effect, CasP can suppress the duplication of a small number of envelope virus.
At present, using sea-tangle, to extract algal polysaccharides, typically using digesting, -ol is heavy, the heavy method of alkali carries -ol.The method processing
Step is very long, and its yield is often due to the factor such as degraded is restricted.Although have been developed that more gentle conditions are come at present
The extraction of algal polysaccharides is carried out, but China also has the heavy producer of substantial amounts of traditional alkali carries -ol and equipment.How technology is carried out
Improve so that the process conditions can produce the product for possessing higher value, be that those skilled in the art wish always
Prestige solves the problems, such as.
The content of the invention
In order to overcome deficiency of the prior art, it is an object of the invention to provide a kind of rational technology, advanced technology, marine alga
The high method that algal polysaccharides are extracted from sea-tangle of polysaccharide yield.
The technical solution adopted for the present invention to solve the technical problems is：A kind of side that algal polysaccharides are extracted from sea-tangle
Method, it is characterised in that：It passes through following steps：
（1）Fresh Laminaria Japonica is crushed, and adds first leaching liquor of 1.2-1.5 times of its weight, is stirred under 55-65 degrees Celsius
20-40 minutes, the first extract solution and filter residue are filtrated to get, the first extract solution is preserved under 5-10 degrees Celsius, first leaching
Extract includes the NaOH of 13-17 % by weight, and remaining is water；
（2）Second leaching liquor of 1.2-1.5 times of its weight is added into the filter residue of step 1,20- is stirred under 25-35 degrees Celsius
40 minutes, the second extract solution and filter residue are filtrated to get, the second extract solution is preserved under 5-10 degrees Celsius, the described second extraction
Liquid includes the EDTA-2Na of 3-5% ethanol, 7-12% NaOH and 0.1-0.2% by weight, and remaining is water；
（3）The 3rd leaching liquor of 1.2-1.5 times of its weight is added into the filter residue of step 2,20-40 is stirred under 5-15 degrees Celsius
Minute, it is filtrated to get the 3rd extract solution and filter residue, the 3rd described leaching liquor includes 7-12% ethanol by weight, 3-6%
NaOH and 0.1-0.2% EDTA-2Na, remaining is water；
（4）First leaching liquor, the second leaching liquor and the 3rd leaching liquor are mixed, and are concentrated under reduced pressure to the 5-10% of original volume, and
And the ethanol of 2.5-3 times of volume is added, collect sediment；
（5）The drying precipitate that step 4 is obtained obtains product.
In currently preferred aspect, in described step 1, Fresh Laminaria Japonica is crushed, and adds its weight 1.45
The first leaching liquor again, stir 30 minutes at 60 c, be filtrated to get the first extract solution and filter residue, the first extract solution is existed
Preserved under 7 degrees Celsius, first leaching liquor includes 15% NaOH by weight, and remaining is water.
In currently preferred aspect, in described step 2,1.45 times of its weight is added into the filter residue of step 1
Second leaching liquor, stirs 30 minutes under 30 degrees Celsius, is filtrated to get the second extract solution and filter residue, and the second extract solution is taken the photograph 7
Being preserved under family name's degree, the second described leaching liquor includes by weight 3.6% ethanol, 10% NaOH and 0.14% EDTA-2Na,
Remaining is water.
In currently preferred aspect, in described step 3,1.2-1.5 times of its weight is added into the filter residue of step 2
The 3rd leaching liquor, stirred 30 minutes under 10 degrees Celsius, be filtrated to get the 3rd extract solution and filter residue, the 3rd described leaching liquor
The EDTA-2Na of ethanol including by weight 10%, 5% NaOH and 0.14%, remaining is water.
In currently preferred aspect, in described step 4, the first leaching liquor, the second leaching liquor and the 3rd are extracted
Liquid mixes, and is concentrated under reduced pressure to the 7% of original volume, and adds the ethanol of 2.7 times of volumes, collects sediment.
In currently preferred aspect, in described step 4, the first leaching liquor, the second leaching liquor and the 3rd are extracted
After liquid mixing, before concentration, mixed leaching liquor weight 0.2-0.4% glycine, 0.35-0.60% are added wherein
The bentonite of magnesium chloride and 1-3%, stir 5-10 minutes, and filter and discard filter residue.
In currently preferred aspect, in described step 4, the first leaching liquor, the second leaching liquor and the 3rd are extracted
After liquid mixing, before concentration, add wherein the glycine of mixed leaching liquor weight 0.32%, 0.48% magnesium chloride and
2.4% bentonite, stir 7 minutes, and filter and discard filter residue.
The algal polysaccharides that the method for the present invention obtains have higher yield, and through experiment there is preferable sulfate to contain
Amount.The method rational technology of the present invention, advanced technology, suitable for the technological transformation of vast alkali carries factory, can provide more Gao Shui
Flat algal polysaccharides.
Embodiment
Embodiment 1
A kind of method that algal polysaccharides are extracted from sea-tangle, it passes through following steps：
（1）Fresh Laminaria Japonica is crushed, and adds first leaching liquor of 1.45 times of its weight, stirs 30 points at 60 c
Clock, the first extract solution and filter residue are filtrated to get, the first extract solution is preserved under 7 degrees Celsius, first leaching liquor includes pressing
15% NaOH of weight meter, remaining is water；
（2）Second leaching liquor of 1.45 times of its weight is added into the filter residue of step 1, is stirred 30 minutes under 30 degrees Celsius, mistake
Filter obtains the second extract solution and filter residue, and the second extract solution is preserved under 7 degrees Celsius, and the second described leaching liquor is included by weight
The ethanol of meter 3.6%, 10% NaOH and 0.14% EDTA-2Na, remaining is water；
（3）The 3rd leaching liquor of 1.2-1.5 times of its weight is added into the filter residue of step 2, is stirred 30 minutes under 10 degrees Celsius,
Be filtrated to get the 3rd extract solution and filter residue, the 3rd described leaching liquor include by weight 10% ethanol, 5% NaOH and
0.14% EDTA-2Na, remaining is water；
（4）First leaching liquor, the second leaching liquor and the 3rd leaching liquor are mixed, and are concentrated under reduced pressure to the 7% of original volume, and
The ethanol of 2.7 times of volumes is added, collects sediment；
（5）The drying precipitate that step 4 is obtained obtains product.
In the present embodiment, the Fresh Laminaria Japonica from 200 kilograms proceeds by extraction, and the weight for finally giving dry products is
1.47kg。
Embodiment 2
A kind of method that algal polysaccharides are extracted from sea-tangle, it passes through following steps：
（1）Fresh Laminaria Japonica is crushed, and adds first leaching liquor of 1.2 times of its weight, is stirred 40 minutes under 65 degrees Celsius,
The first extract solution and filter residue are filtrated to get, the first extract solution is preserved under 10 degrees Celsius, first leaching liquor is included by weight
17 % of gauge NaOH, remaining is water；
（2）Second leaching liquor of 1.2 times of its weight is added into the filter residue of step 1, is stirred 20 minutes under 35 degrees Celsius, is filtered
The second extract solution and filter residue are obtained, the second extract solution is preserved under 10 degrees Celsius, the second described leaching liquor is included by weight
The ethanol of meter 5%, 12% NaOH and 0.2% EDTA-2Na, remaining is water；
（3）The 3rd leaching liquor of 1.5 times of its weight is added into the filter residue of step 2, is stirred 40 minutes under 15 degrees Celsius, is filtered
Obtain the 3rd extract solution and filter residue, the 3rd described leaching liquor includes by weight 12% ethanol, 6% NaOH and 0.1%
EDTA-2Na, remaining is water；
（4）First leaching liquor, the second leaching liquor and the 3rd leaching liquor are mixed, and are concentrated under reduced pressure to the 10% of original volume, and
The ethanol of 2.5 times of volumes is added, collects sediment；
（5）The drying precipitate that step 4 is obtained obtains product.
In the present embodiment, the Fresh Laminaria Japonica from 200 kilograms proceeds by extraction, and the weight for finally giving dry products is
1.32kg。
Embodiment 3
A kind of method that algal polysaccharides are extracted from sea-tangle, it passes through following steps：
（1）Fresh Laminaria Japonica is crushed, and adds first leaching liquor of 1.5 times of its weight, is stirred 20 minutes under 55 degrees Celsius,
The first extract solution and filter residue are filtrated to get, the first extract solution is preserved at 5 c, first leaching liquor is included by weight
13% NaOH of meter, remaining is water；
（2）Second leaching liquor of 1.5 times of its weight is added into the filter residue of step 1, is stirred 40 minutes under 25 degrees Celsius, is filtered
The second extract solution and filter residue are obtained, the second extract solution is preserved at 5 c, the second described leaching liquor is included by weight
The EDTA-2Na of 3% ethanol, 7% NaOH and 0.1%, remaining is water；
（3）The 3rd leaching liquor of 1.2 times of its weight is added into the filter residue of step 2, is stirred 20 minutes at 5 c, filtering
Obtain the 3rd extract solution and filter residue, the 3rd described leaching liquor includes by weight 7% ethanol, 3% NaOH and 0.2%
EDTA-2Na, remaining is water；
（4）First leaching liquor, the second leaching liquor and the 3rd leaching liquor are mixed, and are concentrated under reduced pressure to the 5% of original volume, and
The ethanol of 3 times of volumes is added, collects sediment；
（5）The drying precipitate that step 4 is obtained obtains product.
In the present embodiment, the Fresh Laminaria Japonica from 200 kilograms proceeds by extraction, and the weight for finally giving dry products is
1.37kg。
Embodiment 4
Method described in the method and comparative example 1 of the present embodiment is essentially identical, and its difference is：In described step 4, by
After one leaching liquor, the second leaching liquor and the mixing of the 3rd leaching liquor, before concentration, mixed leaching liquor weight is added wherein
0.32% glycine, 0.48% magnesium chloride and 2.4% bentonite, stir and filter and discard filter residue.
In the present embodiment, the Fresh Laminaria Japonica from 200 kilograms proceeds by extraction, and the weight for finally giving dry products is
1.22kg。
Comparative example 1
The difference of the method for this comparative example and embodiment 1 is：The first leaching liquor using step 1 and leaching in step 1-3
Temperature raising degree is extracted.
In the present embodiment, the Fresh Laminaria Japonica from 200 kilograms proceeds by extraction, and the weight for finally giving dry products is
1.53kg。
Comparative example 2
The difference of the method for this comparative example and embodiment 1 is：The second leaching liquor using step 2 and leaching in step 1-3
Temperature raising degree is extracted.
In the present embodiment, the Fresh Laminaria Japonica from 200 kilograms proceeds by extraction, and the weight for finally giving dry products is
1.10kg。
Comparative example 3
The difference of the method for this comparative example and embodiment 1 is：The 3rd leaching liquor using step 3 and leaching in step 1-3
Temperature raising degree is extracted.
In the present embodiment, the Fresh Laminaria Japonica from 200 kilograms proceeds by extraction, and the weight for finally giving dry products is
0.73kg。
First, the determination of yield of laminarin
Embodiment 1-4 and comparative example 1-3 product are weighed and counted, is shown in table 1.
Table 1：Embodiment 1-4 and comparative example 1-3 Product yields
| Group number | Products weight/kg |
| Embodiment 1 | 1.47 |
| Embodiment 2 | 1.32 |
| Embodiment 3 | 1.37 |
| Embodiment 4 | 1.22 |
| Comparative example 1 | 1.53 |
| Comparative example 2 | 1.10 |
| Comparative example 3 | 0.73 |
From this, when using the leaching liquor and temperature of step 3 merely, the significantly decline of final product weight can be caused.
And when using the leaching liquor and temperature of step 1, the lifting of final product weight can be caused.This show using relatively low temperature and
During extract solution containing ethanol and EDTA-2Na, the decline of the yield of the polysaccharide extracted can be caused.
2nd, the sulfate assay of algal polysaccharides
This experiment passes through《PLA's Acta Pharmaceutica Sinica》03 phase in 2003《Brown alga sulfate presses polysaccharide sulfate assay-sulfuric acid
Barium turbidimetry research》Method contain to determine the sulfate in the algal polysaccharides of embodiment 1-4 and comparative example 1-3 product
Amount.The content of sulfate and the bioactivity of algal polysaccharides have the very big degree of association, and reflect polysaccharide to a certain extent
The height of hydrolysis degree.Using the instrument and medicine of 1 part of the paper, the methods of 2 parts is measured.Embodiment 1-
4 and comparative example 1-3 sulfate content is documented in table 2.
Table 2：Embodiment 1-4 and comparative example 1-3 sulfate content
| Group number | Sulfate content/% |
| Embodiment 1 | 27.03 |
| Embodiment 2 | 26.22 |
| Embodiment 3 | 25.79 |
| Embodiment 4 | 29.81 |
| Comparative example 1 | 17.47 |
| Comparative example 2 | 21.25 |
| Comparative example 3 | 26.54 |
There should be similar or identical sulfate content in view of the algal polysaccharides extracted in same main laminaria sample, I
Can expect, embodiment 1-4 sulfate content is higher, it is meant that the ratio of its polysaccharide without decomposing is higher.From
This is visible, and when carrying out embodiment 1-3 method extraction, its sulfate content is higher, shows that Polyose extraction process is more gentle.
In example 4, the extraction result of polysaccharide is best.In comparative example 1-3, comparative example 1-2 sulfate content is significantly lower than real
A 1-4 is applied, shows that the hydrolysis degree of wherein sulfate is higher.The sulfate content of comparative example 3 is similar with embodiment 1-3
Level, but its polysaccharide yield is very low, it sacrifices substantial amounts of yield in order to ensure gentle extraction.
Claims (7)
- A kind of 1. method that algal polysaccharides are extracted from sea-tangle, it is characterised in that：It passes through following steps：（1）Fresh Laminaria Japonica is crushed, and adds first leaching liquor of 1.2-1.5 times of its weight, is stirred under 55-65 degrees Celsius 20-40 minutes, the first extract solution and filter residue are filtrated to get, the first extract solution is preserved under 5-10 degrees Celsius, first leaching Extract includes the NaOH of 13-17 % by weight, and remaining is water；（2）Second leaching liquor of 1.2-1.5 times of its weight is added into the filter residue of step 1,20- is stirred under 25-35 degrees Celsius 40 minutes, the second extract solution and filter residue are filtrated to get, the second extract solution is preserved under 5-10 degrees Celsius, the described second extraction Liquid includes the EDTA-2Na of 3-5% ethanol, 7-12% NaOH and 0.1-0.2% by weight, and remaining is water；（3）The 3rd leaching liquor of 1.2-1.5 times of its weight is added into the filter residue of step 2,20-40 is stirred under 5-15 degrees Celsius Minute, it is filtrated to get the 3rd extract solution and filter residue, the 3rd described leaching liquor includes 7-12% ethanol by weight, 3-6% NaOH and 0.1-0.2% EDTA-2Na, remaining is water；（4）First leaching liquor, the second leaching liquor and the 3rd leaching liquor are mixed, and are concentrated under reduced pressure to the 5-10% of original volume, and And the ethanol of 2.5-3 times of volume is added, collect sediment；（5）The drying precipitate that step 4 is obtained obtains product.
- A kind of 2. method that algal polysaccharides are extracted from sea-tangle according to claim 1, it is characterised in that：In described step In rapid 1, Fresh Laminaria Japonica is crushed, and adds first leaching liquor of 1.45 times of its weight, is stirred 30 minutes at 60 c, The first extract solution and filter residue are filtrated to get, the first extract solution is preserved under 7 degrees Celsius, first leaching liquor is included by weight 15% NaOH of meter, remaining is water.
- A kind of 3. method that algal polysaccharides are extracted from sea-tangle according to claim 1, it is characterised in that：In described step In rapid 2, second leaching liquor of 1.45 times of its weight is added into the filter residue of step 1, is stirred 30 minutes under 30 degrees Celsius, is filtered The second extract solution and filter residue are obtained, the second extract solution is preserved under 7 degrees Celsius, the second described leaching liquor is included by weight The EDTA-2Na of 3.6% ethanol, 10% NaOH and 0.14%, remaining is water.
- A kind of 4. method that algal polysaccharides are extracted from sea-tangle according to claim 1, it is characterised in that：In described step In rapid 3, the 3rd leaching liquor of 1.2-1.5 times of its weight is added into the filter residue of step 2, is stirred 30 minutes under 10 degrees Celsius, Be filtrated to get the 3rd extract solution and filter residue, the 3rd described leaching liquor include by weight 10% ethanol, 5% NaOH and 0.14% EDTA-2Na, remaining is water.
- A kind of 5. method that algal polysaccharides are extracted from sea-tangle according to claim 1, it is characterised in that：In described step In rapid 4, the first leaching liquor, the second leaching liquor and the 3rd leaching liquor are mixed, and are concentrated under reduced pressure to the 7% of original volume, and is added Enter the ethanol of 2.7 times of volumes, collect sediment.
- A kind of 6. method that algal polysaccharides are extracted from sea-tangle according to claim 1, it is characterised in that：In described step In rapid 4, after the first leaching liquor, the second leaching liquor and the 3rd leaching liquor are mixed, before concentration, add wherein mixed Leaching liquor weight 0.2-0.4% glycine, 0.35-0.60% magnesium chloride and 1-3% bentonite, stir 5-10 minutes, and Filtering discards filter residue.
- A kind of 7. method that algal polysaccharides are extracted from sea-tangle according to claim 6, it is characterised in that：In described step In rapid 4, after the first leaching liquor, the second leaching liquor and the 3rd leaching liquor are mixed, before concentration, add wherein mixed The glycine of leaching liquor weight 0.32%, 0.48% magnesium chloride and 2.4% bentonite, stir 7 minutes, and filter and discard filter Slag.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111393535A (en) * | 2020-03-30 | 2020-07-10 | 福建大昌生物科技实业有限公司 | Extraction method of laminarin and application of laminarin in aquatic feed |
| CN113621089A (en) * | 2021-10-11 | 2021-11-09 | 山东洁壹选生物科技有限公司 | Algal polysaccharide extract and preparation method and application thereof |
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| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111393535A (en) * | 2020-03-30 | 2020-07-10 | 福建大昌生物科技实业有限公司 | Extraction method of laminarin and application of laminarin in aquatic feed |
| CN113621089A (en) * | 2021-10-11 | 2021-11-09 | 山东洁壹选生物科技有限公司 | Algal polysaccharide extract and preparation method and application thereof |
| CN113621089B (en) * | 2021-10-11 | 2021-12-17 | 山东洁壹选生物科技有限公司 | Preparation method and application of algal polysaccharide extract |
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Application publication date: 20180209 |