CN104892785B - A kind of extracting method of algal polysaccharides - Google Patents
A kind of extracting method of algal polysaccharides Download PDFInfo
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- CN104892785B CN104892785B CN201510285240.5A CN201510285240A CN104892785B CN 104892785 B CN104892785 B CN 104892785B CN 201510285240 A CN201510285240 A CN 201510285240A CN 104892785 B CN104892785 B CN 104892785B
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Abstract
The invention discloses a kind of extracting method of algal polysaccharides.The method is comprised the steps of：（1）Crushed after marine alga raw material cleaning, drying, cross 60 mesh sieves；（2）Sieving crushed material is with solid-to-liquid ratio 1:25 ~ 35 accurate addition distilled water carry out ultra high pressure extraction, and pressurize 200 ~ 400MPa, 30 ~ 70 DEG C of temperature；Pressurize 3 ~ 8 minutes, suction filtration takes filtrate, obtains algal polysaccharides crude extract；（3）To activated carbon decolorizing is added in crude extract, filter, mixed liquor is obtained；（4）Mixed liquor further it is concentrated, crystallize, filter, being dried to obtain trehalose sterling.The inventive method is simple, operation is easy, extraction time is short, it is adaptable to industrialized production, can obtain the algal polysaccharides product that purity is high, impurity is few, invaded and harassed from microorganism.
Description
Technical field
The present invention relates to a kind of extracting method of algal polysaccharides, more particularly to a kind of super-pressure assisted extraction algal polysaccharides
Method.
Background technology
Marine alga belongs to rudimentary plant, is the primary producer in ocean, is broadly divided into four major classes-blue-green algae, green alga, jujube
And brown alga, the microalgaes such as diatom, dinoflagellate, chrysophyceae are additionally included, its industry development has a high potential, with human lives and economic development
There is close relationship, be widely used in marine drug, functional food, bioactivator development and application, food additives, organic
The fields such as fertilizer, packaging material for food, cosmetics.
Polysaccharide compound extensively, exercises different functions in distributed in nature in organism, is the material of life
Basis.Numerous studies prove in recent years, from the natural polysaccharide of the extractions such as plant, bacterium, with wide material sources, toxic and side effect it is low,
It is safe, the advantages of immune enhancing function is extensive, thus polysaccharide is increasingly paid close attention to by researcher.Marine alga is used as ocean
Quantity and the most class of kind in plant, its polyoses content accounts for more than the 50% of dry mass, as at present most promising one
Class active material.Algal polysaccharides are the macromolecule carbon hydrates being connected by glycosidic bond by multiple identical or different monose
Thing, it is different according to its source, red seaweed polysaccharide, green algae polysaccharide, algal polysaccharide etc., the wherein type and quantity of algal polysaccharide can be divided into
At most.The unique structure of algal polysaccharides, stable chemical nature, are the efficient biological adsorption agents of a class, with immunological regulation, disease-resistant
Malicious, anti-oxidant, anti-inflammation etc. act on.
At present, marine alga Thick many candies are extracted both at home and abroad mainly using the method for diluted alkaline, olefin(e) acid and hot-water extraction.Its advantage is work
Skill is simple and convenient to operate, low cost, has the disadvantage that recovery rate is relatively low, loss of activity is big, Purification by filtration is difficult, which greatly limits
Algal polysaccharides large-scale industrial production.In recent years, such as microwave radiation exaraction, ultrasonic assistant are extracted, digest assisted extraction
New extractive technique grows up on the basis of traditional extraction.For example：
Patent CN103265645A relate to the device and method that a kind of ultrasonic assistant extracts algal polysaccharides, described dress
Put including the reactor for placing extraction tube, ultrasonic transmitter and temperature regulating device, the described method for extracting algal polysaccharides
Be by the raw materials such as sea-tangle crush after, through certain condition ultrasound after, use ethanol precipitation extract solution, filter to obtain marine alga Thick many candies, finally
Spray-dried or freeze-drying obtains algal polysaccharides sterling.The advantage of the method is to extract time-consuming short, is advantageously implemented automation
Production.
Patent CN102850410A discloses a kind of method that algal polysaccharides are extracted from beer waste yeast, and the method belongs to
Field of biotechnology.It is mainly characterized by with beer waste yeast as raw material, the enzyme that goes out is dried after impurity elimination, sea is obtained using surname extraction
Polysaccharides crude extract；Crude extract obtains purity and reaches after activated carbon decolorizing, de- albumen, ion exchange removal of impurities, concentration, crystallizing and drying
To 98.5% algal polysaccharides sterling.The method process is simple, safe operation and acquisition product purity are high.
CN1392160A provides the method that algal polysaccharides are extracted in flocculation, principal character will by cyclic ultrasonic breaking or
Water-boiling method obtain through refining the extraction feed liquid of algal polysaccharides is placed in reactor, adjust 20-60 DEG C of temperature, pH5-8, low whipping speed is
Under 300-1500rpm add flocculant extracted, algal polysaccharides crude product；Again algal polysaccharides crude product purify and sea is obtained
Polysaccharides product.Flocculation dosage is few needed for the method, it is possible to decrease extraction cost.
The above method is most to have the shortcomings that to overcome in addition to possessing the advantage of itself uniqueness, such as the cycle is long, carry
Take rate is not high or active ingredient destruction is big etc..In this context, superhigh pressure technique is applied to the present invention extraction of algal polysaccharides.
Superhigh pressure technique is to develop a kind of new process technology faster in recent years, with simple to operate, recovery rate it is high,
Time is short, impurity content is few, energy consumption is low, it is environmentally friendly the advantages of.It not only can effectively kill the microorganism in food, moreover it is possible to protect
Natural food color and nutritional ingredient are held, Recent study is increasingly extensive with application, is widely used to traditional Chinese medicine ingredients
Extract research.
The content of the invention
It is an object of the invention to provide a kind of extracting method of algal polysaccharides, this method is simple to operate, take short, recovery rate
Height, can obtain the algal polysaccharides product of high-purity.
1st, inventive technique scheme
The invention provides a kind of extracting method of algal polysaccharides.The extracting method is realized by following technical scheme：
（1）Crushed after marine alga raw material cleaning, drying, cross 60 mesh sieves；
Described marine alga raw material is sea-tangle, deer's tail dish, bulk kelp, yellow tang, bladder-wrack, undaria pinnitafida or any two kinds of sargassum
Combination.Further marine alga raw material is cleaned with clear water, and the marine alga about 12 ~ 18 hours after being cleaned with 30 ~ 55 DEG C of dryings, make this
The water content of marine alga is about 6 ~ 12%.
（2）Sieving crushed material is with solid-to-liquid ratio 1:25 ~ 35 it is accurate add the distilled water to carry out ultra high pressure extraction, pressurization 200 ~
400MPa, 30 ~ 70 DEG C of temperature；Pressurize 3 ~ 8 minutes, suction filtration takes filtrate, obtains algal polysaccharides crude extract；
（3）To activated carbon decolorizing is added in crude extract, filter, mixed liquor is obtained；
Described filter process is to make crude extract be 0.6% ~ 3.2% with the mass percent of activated carbon, is decolourized 30 ~ 75 points
Clock.
（4）Mixed liquor further it is concentrated, crystallize, filter, being dried to obtain trehalose sterling.
Described concentration process be using rotary evaporation in vacuo concentrate, thickening temperature be 50 ~ 100 DEG C, vacuum be 10 ~
30KPa.Further by step（3）In algal polysaccharides mixed liquor be concentrated into mass concentration for 70% ~ 87%.
Described crystallization process is under the conditions of the solution after concentration maintained into 15 ~ 45 DEG C of temperature, by volume 1:(1~
4.7) after adding absolute ethyl alcohol, addition mass percent is 0.3 ~ 2.8% crystal seed, stirred crystallization.
Described drying process is that to use temperature be 45 ~ 65 DEG C, and drying time is the spray drying of 1.5h, or first incited somebody to action
Algal polysaccharides crystal after filter is cooled to 2 DEG C, and being subsequently placed in carries out freeze-drying 1.5h in about -40 DEG C of freeze drying box, obtains sea
Polysaccharides sterling.
2nd, present invention solves the technical problem that and being beneficial in that：
（1）The inventive method is simple, operation is easy, time-consuming short, without the reagent or chemistry of the other assisted extractions of addition
Product, it is to avoid bring new impurity into；
（2）The algal polysaccharides finished product impurity content obtained through this method is low, and purity is up to more than 98.5%；The inventive method
Energy consumption is low, and improves extraction efficiency, controllable to cost, it is adaptable to the large-scale production of industrialization.
（3）Infringement of the inventive method to active component is small, can simultaneously be effectively kills the microorganism in finished product.
Specific embodiment
Following several specific embodiments are now enumerated to further illustrate the present invention program.It should be noted that following implement
Example is only used for help and understands the present invention program, is not the further restriction to the present invention program.
Embodiment 1
（1）After sea-tangle and sargassum raw material are cleaned with clear water, dried 12 hours at a temperature of being placed in 30 DEG C, the raw material contains
Water is about 12%；Then raw material is crushed, crosses 60 mesh sieves；
（2）Sieving crushed material is with solid-to-liquid ratio 1:25 accurate addition distilled water carry out ultra high pressure extraction, and pressurize 200MPa, temperature
It is 30 DEG C；Pressurize 3 minutes, suction filtration takes filtrate, obtains algal polysaccharides crude extract；
（3）To adding activated carbon to make crude extract be 0.6% with the mass percent of activated carbon in crude extract, carry out 30 minutes
Decolouring, filtering, be obtained mixed liquor；
（4）Mixed liquor is concentrated using rotary evaporation in vacuo, is 50 DEG C in temperature, and vacuum is by sea under conditions of 10KPa
It is 70% that polysaccharides mixed liquor is concentrated into mass concentration；Then the solution after concentration is maintained into temperature under the conditions of 15 DEG C, by body
Product compares 1:After 1 adds absolute ethyl alcohol, addition mass percent is 0.3% crystal seed, stirred crystallization, filtering；The last temperature at 45 DEG C
Degree is lower to obtain trehalose sterling using spray drying 1.5h, and recovery rate is 95%.
Embodiment 2
（1）After bulk kelp and yellow tang raw material are cleaned with clear water, dried about 14 hours at a temperature of being placed in 38 DEG C, the raw material
Water content is about 10%；Then raw material is crushed, crosses 60 mesh sieves；
（2）Sieving crushed material is with solid-to-liquid ratio 1:28 accurate addition distilled water carry out ultra high pressure extraction, and pressurize 267MPa, temperature
43℃；Pressurize 4.7 minutes, suction filtration takes filtrate, obtains algal polysaccharides crude extract；
（3）To adding activated carbon to make crude extract be 1.5% with the mass percent of activated carbon in crude extract, carry out 45 minutes
Decolouring, filtering, be obtained mixed liquor；
（4）Mixed liquor is concentrated using rotary evaporation in vacuo, is 66.7 DEG C in temperature, and vacuum is general under conditions of 17KPa
It is 75.7% that algal polysaccharides mixed liquor is concentrated into mass concentration；Then the solution after concentration is maintained into temperature under the conditions of 25 DEG C,
By volume 1:After 2.2 add absolute ethyl alcohol, addition mass percent is 1.1% crystal seed, stirred crystallization, filtering；Finally exist
Using spray drying 1.5h at a temperature of 51.7 DEG C, trehalose sterling is obtained, recovery rate is 97%.
Embodiment 3
（1）After yellow tang and bladder-wrack raw material are cleaned with clear water, dried about 16 hours at a temperature of being placed in 47 DEG C, the raw material
Water content be about 8%.Then raw material is crushed, crosses 60 mesh sieves；
（2）Sieving crushed material is with solid-to-liquid ratio 1:32 accurate addition distilled water carry out ultra high pressure extraction, and pressurize 334MPa, temperature
57℃；Pressurize 6.4 minutes, suction filtration takes filtrate, obtains algal polysaccharides crude extract；
（3）To adding activated carbon to make crude extract be 2.4% with the mass percent of activated carbon in crude extract, carry out 60 minutes
Decolouring, filtering, be obtained mixed liquor；
（4）Mixed liquor is concentrated using rotary evaporation in vacuo, is 83.4 DEG C in temperature, and vacuum is general under conditions of 24KPa
It is 81.4% that algal polysaccharides mixed liquor is concentrated into mass concentration；Then the solution after concentration is maintained into temperature under the conditions of 35 DEG C,
By volume 1:After 3.5 add absolute ethyl alcohol, addition mass percent is 2.0% crystal seed, stirred crystallization, filtering；Finally exist
Freeze-drying 1.5h is used at a temperature of 58.4 DEG C, trehalose sterling is obtained, recovery rate is 98%.
Embodiment 4
（1）After deer's tail dish and undaria pinnitafida raw material are cleaned with clear water, dried 18 hours at a temperature of being placed in 55 DEG C, the raw material
Water content is about 6%.Then raw material is crushed, crosses 60 mesh sieves；
（2）Sieving crushed material is with solid-to-liquid ratio 1:35 accurate addition distilled water carry out ultra high pressure extraction, and pressurize 400MPa, temperature
70 DEG C of degree；Pressurize 8 minutes, suction filtration takes filtrate, obtains algal polysaccharides crude extract；
（3）To adding activated carbon to make crude extract be 3.2% with the mass percent of activated carbon in crude extract, carry out 75 minutes
Decolouring, filtering, be obtained mixed liquor；
（4）Mixed liquor is concentrated using rotary evaporation in vacuo, is 100 DEG C in temperature, and vacuum is by sea under conditions of 30KPa
It is 87% that polysaccharides mixed liquor is concentrated into mass concentration；Then the solution after concentration is maintained into temperature under the conditions of 45 DEG C, by body
Product compares 1:After 4.7 add absolute ethyl alcohol, addition mass percent is 2.8% crystal seed, stirred crystallization, filtering；It is last first incited somebody to action
Algal polysaccharides crystal after filter is cooled to 2 DEG C, and being subsequently placed in carries out freeze-drying 1.5h in about -40 DEG C of freeze drying box, obtains sea
Polysaccharides sterling, recovery rate is 94%.
Claims (5)
1. a kind of extracting method of algal polysaccharides, it is characterised in that comprise the following steps：
(1) crushed after the cleaning, drying of marine alga raw material, cross 60 mesh sieves；
(2) sieving crushed material is with solid-to-liquid ratio 1:25~35 it is accurate add the distilled water to carry out ultra high pressure extraction, pressurization 200~
400MPa, 30~70 DEG C of temperature；Pressurize 3~8 minutes, suction filtration takes filtrate, obtains algal polysaccharides crude extract；
(3) to activated carbon decolorizing is added in crude extract, filter, mixed liquor is obtained；
(4) mixed liquor further it is concentrated, crystallize, filter, being dried to obtain algal polysaccharides sterling；
Wherein in the step (1), marine alga raw material is cleaned with clear water, and the marine alga 12~18 with 30~55 DEG C of dryings after clean
Hour, the water content for making the marine alga is 6~12%；Wherein in the step (4), by the solution after concentration maintain temperature 15~
Under the conditions of 45 DEG C, by volume 1:(1~4.7) after adding absolute ethyl alcohol, addition mass percent is 0.3~2.8% crystal seed,
Stirred crystallization；
Wherein in the step (4), trehalose sterling is obtained using freeze-drying, and freeze-drying is needed first by the marine alga after filtering
Many sugar crystals are cooled to 2 DEG C, are subsequently placed in -40 DEG C of freeze drying box and dry 1.5h.
2. algal polysaccharides extracting method according to claim 1, wherein in the step (1), marine alga raw material is sea-tangle, deer
Any two kinds of combination in waste dish, bulk kelp, yellow tang, bladder-wrack, undaria pinnitafida or sargassum.
3. algal polysaccharides extracting method according to claim 1, wherein in the step (3), crude extract and activated carbon
Mass percent is 0.6%~3.2%, is decolourized 30~75 minutes.
4. algal polysaccharides extracting method according to claim 1, wherein in the step (4), concentration uses vacuum rotating
It is concentrated by evaporation, thickening temperature is 50~100 DEG C, vacuum is 10~30KPa.
5. algal polysaccharides extracting method according to claim 4, it is characterised in that above-mentioned algal polysaccharides mixed liquor is concentrated into
Mass concentration is 70%~87%.
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| CN110183544A (en) * | 2019-06-06 | 2019-08-30 | 山东天易科技有限公司 | A kind of preparation method of algal polysaccharides |
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| 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 |
| CN115363208A (en) * | 2022-06-01 | 2022-11-22 | 广东省农业科学院蚕业与农产品加工研究所 | Preparation method of sargassum fusiforme aqueous extract for treating constipation |
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