CN108822226A - A method of extracting polysaccharide from microalgae algae-residue - Google Patents
A method of extracting polysaccharide from microalgae algae-residue Download PDFInfo
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- CN108822226A CN108822226A CN201810487476.0A CN201810487476A CN108822226A CN 108822226 A CN108822226 A CN 108822226A CN 201810487476 A CN201810487476 A CN 201810487476A CN 108822226 A CN108822226 A CN 108822226A
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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
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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Abstract
The method that the invention discloses a kind of to extract polysaccharide from microalgae algae-residue, includes the following steps：1）Sodium hydroxide solution is added in algae-residue, is stirred heating extraction, to get alkali extract after separation of solid and liquid；2）By step 1）Obtained alkali extract carries out concentration and removing protein, to get polysaccharide supernatant after separation of solid and liquid；3）Step 2 is added in dehydrated alcohol）It in obtained supernatant, stirs evenly, is then separated by solid-liquid separation, precipitating is Thick many candies；4）By step 3）Obtained Thick many candies washed and dried with dehydrated alcohol after to get polysaccharide powder.Present invention process process is reasonable, it is easy to operate, the algae-residue discarded after extracting phycochrome, algae oil rouge, phycochrome grease, algae albumen, phycochrome albumen is made full use of, turns waste into wealth and increases economic benefit, to extend microalgae recovery link, realize that high level high-qualityization of algae-residue utilizes.
Description
Technical field
The method that the present invention relates to a kind of to extract polysaccharide from microalgae algae-residue, belongs to field of biotechnology.
Background technique
Microalgae have the characteristics that photosynthetic efficiency is high, growth rate is fast, to the adaptable of environment, contain in cell
There are the metabolites such as lipid abundant, pigment, protein, polysaccharide, vitamin, microelement, these metabolites have important
Economic value has wide practical use in fields such as medicine, health care product, feed, chemical industry.
With the rise of microalgae industry, recent domestic increases the development and utilization of microalgae cell component.Chinese patent
CN102965182B proposes a kind of method for extracting algae oil rouge from schizochytrium using organic solvents such as n-hexanes.It is Chinese special
Sharp CN101585759A proposes the method that DHA unsaturated fatty acid is extracted from dino flagellate fermentation liquor.Chinese patent
CN1562943A proposes a kind of method for extracting gamma-linoleic acid from bloom blue algae using petroleum ether solvent.Some researchers
Be respectively adopted organic solvent extractionprocess, it is super face/subcritical abstraction method, complex solvent extraction method be extracted class Hu trailing plants in microalgae
Bu Su（Gong M Y, Bassi A J. Carotenoids from microalgae: A review of recent
developments[J]. Biotechnology Advances, 2016, 34(8): 1396-1412）.Chinese patent
CN100537532C is extracted carotenoid and edible glycerol using the method for supercritical carbon dioxide from Dunaliella salina.One
A little researchs use supercritical CO2Extraction and subcritical normal butane extraction fromPhaeodactylum tricornutum、Nannochloropsis oculataWithPorphyridium cruentumThree kinds of marine microalgaes are extracted ω -3 and ω -6
Polyunsaturated fatty acid, carotenoid（Rafael F, Ângelo P M, Simone M, et al.
Polyunsaturated ω-3 and ω-6 fatty acids, total carotenoids and antioxidant
activity of three marine microalgae extracts obtained by supercritical CO2 and
subcritical n-butane[J]. The Journal of Supercritical Fluids, 2018, 133(1):
437-443）.Some researchers also pass through reactor design and training strategy optimizes the protein content for improving chlorella
（Chen C Y, Lee P J, Tan C H, et al. Improving protein production of
indigenous microalga Chlorella vulgaris FSP-E by photobioreactor design and
cultivation strategies[J]. Biotechnology Journal, 2015, 10(6), 905-914.）.Especially
Ground more has researcher to be dedicated to studying shadow of the change to its biomass, fatty acid and carotenoid output of microdisk electrode strategy
It rings（Ma R J, Thomas-Hall S R, Chua E T, et al. LED power efficiency of biomass,
fatty acid, and carotenoid production in Nannochloropsis microalgae[J].
Bioresource Technology, 2018, 252: 118-1226）.However, preparing phycochrome, algae oil using microalgae
A large amount of algae-residue can be generated during rouge, algae albumen etc., if the wave of the polynary composition of high value in algae-residue will be caused by not being used
Take.In fact, algae-residue is still important biomass resource, correlative study show in algae-residue recycling cellular component also compared with
It is more, still have the potentiality of production high value added product.As contained protein 32.4%, total reducing sugar in scenedesmus oil-extracted algae slag
24.7%, grease 6.5%, ash content 10%, protein and total sugar content are relatively abundant（Yang Z, Guo R, Xu X, et al.
Hydrogen and Methane Production from Lipid-extracted Microalgal Biomass
Residues [J]. International Journal of Hydrogen Energy, 2011, 36(5): 3465-
3470.）.But rarely has the report for carrying out high-valued exploitation to algae-residue at present, have not been achievable the multi-component comprehensive benefit of microalgae cell
With.
Summary of the invention
To make up for the shortcomings of the above existing technologies, the present invention proposes a kind of method that polysaccharide is extracted from algae-residue, can lead to
It crosses algae-residue extraction and prepares polysaccharides.Using the extraction process, microalgae biomass development and utilization can be made full use of to generate in the process
A large amount of algae-residues realize the multi-component comprehensive utilization of microalgae cell, extend microalgae recovery link, to improve microalgae biomass exploitation benefit
Overall economy quality provides a kind of new method for the comprehensive development and utilization of microalgae resource.
To achieve the above object, the present invention adopts the following technical scheme that：
A method of it extracting polysaccharide from microalgae algae-residue, includes the following steps：
1）Extract algae-residue polysaccharide：Sodium hydroxide solution is added in algae-residue, is stirred heating extraction, after separation of solid and liquid to get
Alkali extract；
2）Remove heteroproteins：By step 1）Obtained alkali extract carries out concentration and removing protein, to get on polysaccharide after separation of solid and liquid
Clear liquid；
3）Alcohol precipitation algae-residue polysaccharide：Step 2 is added in dehydrated alcohol）It in obtained supernatant, stirs evenly, then carries out solid-liquid point
From precipitating is Thick many candies；
4）Prepare algae-residue polysaccharide powder：By step 3）Obtained precipitating washed and dried with dehydrated alcohol after to get polysaccharide powder.
The step 1）In, algae-residue be extracted phycochrome, algae oil rouge, phycochrome grease, algae albumen, in phycochrome albumen
Remaining part after any ingredient.
The step 1）In, the algae in algae-residue source is chlorella, Du Shi algae, micro- quasi- ball algae, chlamydomonas, scenedesmus, phaeodactylum tricornutum
Refer to one of algae, purple ball algae, spirulina, chrysophyceae, schizochytrium, hidden dinoflagellate, haematococcus pluvialis.
The step 1）In, naoh concentration 1wt%-21wt%, extraction conditions are：Solid-to-liquid ratio is 5-20:1 g/L,
Temperature is 30-75 DEG C, extraction time is 30-120 min.
The step 1）, step 2）With step 3）In, solid-liquid separating method is one of to stand, be centrifuged, filter.
The step 2）In, method for concentration is ultrafiltration or nanofiltration.
The step 2）, method of removing protein is one of Sevage method, trifluorotrichloroethane method, trichloroacetic acid method.
The step 3）In, the volume that dehydrated alcohol is added is 2-5 times of supernatant volume.
The step 4）In, drying means is vacuum drying or freeze-drying.
Using algae-residue polysaccharide powder made from above-mentioned extracting method, polyoses content is 80 ~ 95wt%.
Remarkable advantage of the invention is：The present invention takes full advantage of the characteristics of algae-residue constituent, with extract phycochrome,
Algae-residue after algae oil rouge, phycochrome grease, algae albumen, phycochrome albumen is raw material, using alkalinity extraction algae-residue polysaccharide, by removing
Foreign protein, alcohol precipitation and etc. prepare algae-residue polysaccharide, realize algae-residue high level high-qualityization utilize.This method process flow simultaneously is closed
Reason, it is easy to operate, algae-residue is turned waste into wealth and increases economic benefit, to extend microalgae recovery link, realizes microalgae cell
Multicomponent comprehensive utilization can provide a new way for the microalgae biomass development process of low cost.
Detailed description of the invention
Fig. 1 is the flow chart that polysaccharide is extracted from algae-residue.
Specific embodiment
Technical solution of the present invention described combined with specific embodiments below.It is as described below to implement for representativeness of the invention
Example can be used for explaining and support the present invention, but it is intended that the present invention is limited in any way, any without departing from the technology of the present invention
Plan content, and according to the technical essence of the invention to simple modification, equivalent change and modification made by following embodiment,
In the range of still falling within technical solution of the present invention.
Embodiment 1
1）Extract algae-residue polysaccharide：100 L 3wt% sodium hydroxide solutions are added to 500 g to the chlorella algae-residue for having mentioned phycochrome
In, it is stirred 120 min of heating extraction under the conditions of 30 DEG C, 10 h are stood under the conditions of 4 DEG C, abandons precipitating, supernatant is alkali carries
Liquid；
2）Remove heteroproteins：By step 1）Obtained alkali extract is concentrated into the 1/ of alkali extract volume by 3000 Da ultrafiltration membranes
2, using Sevage method removing protein, it is centrifuged 10 min under the conditions of 4000 r/min, abandons precipitating, supernatant, that is, polysaccharide supernatant；
3）Alcohol precipitation algae-residue polysaccharide：Step 2 is added in 150 L dehydrated alcohols）It in obtained supernatant, stirs evenly, then 8000
6 min are centrifuged under the conditions of r/min, precipitating is polysaccharide；
4）Prepare algae-residue polysaccharide powder：By step 3）Obtained precipitating is washed with dehydrated alcohol, washs 5 times, 50 200 mL/ time
DEG C, vacuum degree be -0.08 MPa under the conditions of be dried in vacuo 20 h to get polysaccharide powder；
5）The polyoses content for the algae-residue polysaccharide powder that this method is prepared is 82wt%, and polysaccharide obtained is examined by ultraviolet spectra
No protein absorption peak is surveyed, illustrates that foreign protein eliminates, acquisition is polysaccharide sterling.
Embodiment 2
1）Extract algae-residue polysaccharide：100 L 9wt% sodium hydroxide solutions are added to 1000 g to the dunaliella for having mentioned algae oil rouge
In slag, it is stirred 90 min of heating extraction under the conditions of 45 DEG C, 6 min are centrifuged under the conditions of 5000 r/min, abandons precipitating, supernatant
As alkali extract；
2）Remove heteroproteins：By step 1）Obtained alkali extract is concentrated into the 1/3 of alkali extract volume by 250 Da nanofiltration membranes,
Using trifluorotrichloroethane method removing protein, it is centrifuged 8 min under the conditions of 5000 r/min, abandons precipitating, supernatant, that is, polysaccharide supernatant；
3）Alcohol precipitation algae-residue polysaccharide：Step 2 is added in 120 L dehydrated alcohols）It in obtained supernatant, stirs evenly, then 8000
6 min are centrifuged under the conditions of r/min, precipitating is polysaccharide；
4）Prepare algae-residue polysaccharide powder：By step 3）Obtained precipitating is washed with dehydrated alcohol, washs 5 times, freezing 300 mL/ time
Dry 24 h are to get polysaccharide powder；
5）The polyoses content for the algae-residue polysaccharide powder that this method is prepared is 85wt%, and polysaccharide obtained is examined by ultraviolet spectra
No protein absorption peak is surveyed, illustrates that foreign protein eliminates, acquisition is polysaccharide sterling.
Embodiment 3
1）Extract algae-residue polysaccharide：100 L 15wt% sodium hydroxide solutions are added to 1500 g and have mentioned algae oil rouge, phycochrome
In spirulina algae-residue, it is stirred 60 min of heating extraction under the conditions of 60 DEG C, 6 min are centrifuged under the conditions of 5000 r/min, it is heavy to abandon
It forms sediment, supernatant is alkali extract；
2）Remove heteroproteins：By step 1）Obtained alkali extract is concentrated into alkali extract volume 1/4 by 250 Da nanofiltration membranes, adopts
With trichloroacetic acid method removing protein, it is centrifuged 6 min under the conditions of 6000 r/min, abandons precipitating, supernatant, that is, polysaccharide supernatant；
3）Alcohol precipitation algae-residue polysaccharide：Step 2 is added in 100 L dehydrated alcohols）It in obtained supernatant, stirs evenly, then 8000
6 min are centrifuged under the conditions of r/min, precipitating is polysaccharide；
4）Prepare algae-residue polysaccharide powder：By step 3）Obtained precipitating is washed with dehydrated alcohol, washs 5 times, freezing 400 mL/ time
Dry 24 h are to get polysaccharide powder；
5）The polyoses content for the algae-residue polysaccharide powder that this method is prepared is 86wt%, and polysaccharide obtained is examined by ultraviolet spectra
No protein absorption peak is surveyed, illustrates that foreign protein eliminates, acquisition is polysaccharide sterling.
Embodiment 4
1）Extract algae-residue polysaccharide：100 L 15wt% sodium hydroxide solutions are added to 2000 g to the chlamydomonas algae-residue for having mentioned algae albumen
In, it is stirred 30 min of heating extraction under the conditions of 75 DEG C, 4 min are centrifuged under the conditions of 8000 r/min, abandons precipitating, supernatant is
For alkali extract；
2）Remove heteroproteins：By step 1）Obtained alkali extract is concentrated into the 1/ of alkali extract volume by 3000 Da ultrafiltration membranes
2, using trichloroacetic acid method removing protein, it is centrifuged 6 min under the conditions of 6000 r/min, abandons precipitating, supernatant, that is, polysaccharide supernatant；
3）Alcohol precipitation algae-residue polysaccharide：Step 2 is added in 250 L dehydrated alcohols）It in obtained supernatant, stirs evenly, then 8000
6 min are centrifuged under the conditions of rpm/min, precipitating is polysaccharide；
4）Prepare algae-residue polysaccharide powder：By step 3）Obtained precipitating is washed with dehydrated alcohol, washs 5 times, 60 500 mL/ time
DEG C, vacuum degree be -0.08 MPa under the conditions of be dried in vacuo 20 h to get polysaccharide powder；
5）The polyoses content for the algae-residue polysaccharide powder that this method is prepared is 88wt%, and polysaccharide obtained is examined by ultraviolet spectra
No protein absorption peak is surveyed, illustrates that foreign protein eliminates, acquisition is polysaccharide sterling.
The foregoing is merely representative embodiments of the invention, are not intended to restrict the invention, although referring to aforementioned
Invention is explained in detail for embodiment, for those skilled in the art, still can be to aforementioned each reality
Technical solution documented by example is applied to modify or equivalent replacement of some of the technical features.It is all of the invention
Within spirit and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of method for extracting polysaccharide from microalgae algae-residue, it is characterised in that：Include the following steps：
1）Extract algae-residue polysaccharide：Sodium hydroxide solution is added in algae-residue, is stirred heating extraction, after separation of solid and liquid to get
Alkali extract；
2）Remove heteroproteins：By step 1）Obtained alkali extract carries out concentration and removing protein, to get on polysaccharide after separation of solid and liquid
Clear liquid；
3）Alcohol precipitation algae-residue polysaccharide：Step 2 is added in dehydrated alcohol）It in obtained supernatant, stirs evenly, then carries out solid-liquid point
From precipitating is Thick many candies；
4）Prepare algae-residue polysaccharide powder：By step 3）Obtained Thick many candies washed and dried with dehydrated alcohol after to get polysaccharide powder.
2. a kind of method for extracting polysaccharide from microalgae algae-residue according to claim 1, it is characterised in that：The step 1）
In, algae-residue is has extracted phycochrome, algae oil rouge, phycochrome grease, residue after any ingredient in algae albumen and phycochrome albumen
Part.
3. a kind of method for extracting polysaccharide from microalgae algae-residue according to claim 1, it is characterised in that：The step 1）
In, the algae in algae-residue source be chlorella, Du Shi algae, micro- quasi- ball algae, chlamydomonas, scenedesmus, Phaeodactylum tricornutum, purple ball algae, spirulina,
One of chrysophyceae, schizochytrium, hidden dinoflagellate and haematococcus pluvialis.
4. a kind of method for extracting polysaccharide from microalgae algae-residue according to claim 1, it is characterised in that：The step 1）
In, naoh concentration 1wt%-21wt%, extraction conditions are：Solid-to-liquid ratio is 5-20:1 g/L, temperature are 30-75 DEG C, extract
Time is 30-120 min.
5. a kind of method for extracting polysaccharide from microalgae algae-residue according to claim 1, it is characterised in that：The step
1）, step 2）With step 3）In, solid-liquid separating method is one of to stand, be centrifuged and filter.
6. a kind of method for extracting polysaccharide from microalgae algae-residue according to claim 1, it is characterised in that：The step 2）
In, method for concentration is ultrafiltration or nanofiltration.
7. a kind of method for extracting polysaccharide from microalgae algae-residue according to claim 1, it is characterised in that：The step 2）
In, method of removing protein is one of Sevage method, trifluorotrichloroethane method and trichloroacetic acid method.
8. a kind of method for extracting polysaccharide from microalgae algae-residue according to claim 1, it is characterised in that：The step 3）
In, the volume that dehydrated alcohol is added is 2-5 times of supernatant volume.
9. a kind of method for extracting polysaccharide from microalgae algae-residue according to claim 1, it is characterised in that：The step 4）
In, drying means is vacuum drying or freeze-drying.
10. a kind of algae-residue polysaccharide powder as made from claim 1-9 described in any item extracting methods, it is characterised in that：Algae-residue
The polyoses content of polysaccharide powder is 80 ~ 95wt%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111214846A (en) * | 2019-11-29 | 2020-06-02 | 云南绿A生物产业园有限公司 | Haematococcus pluvialis extract and preparation method thereof |
| CN117247849A (en) * | 2023-11-20 | 2023-12-19 | 山东悦翔生物有限公司 | Microalgae extraction method |
Citations (3)
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| EP0924220A2 (en) * | 1997-12-16 | 1999-06-23 | Wako Pure Chemical Industries, Ltd. | Inhibitor of the activation of beta-glucan recognition protein |
| CN103255662A (en) * | 2013-05-06 | 2013-08-21 | 青岛大学 | Preparation method of nanometer fibril enteromorpha cellulose |
| CN103819577A (en) * | 2014-03-24 | 2014-05-28 | 福州大学 | Method for preparing spirulina platensis polysaccharide |
-
2018
- 2018-05-21 CN CN201810487476.0A patent/CN108822226A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0924220A2 (en) * | 1997-12-16 | 1999-06-23 | Wako Pure Chemical Industries, Ltd. | Inhibitor of the activation of beta-glucan recognition protein |
| CN103255662A (en) * | 2013-05-06 | 2013-08-21 | 青岛大学 | Preparation method of nanometer fibril enteromorpha cellulose |
| CN103819577A (en) * | 2014-03-24 | 2014-05-28 | 福州大学 | Method for preparing spirulina platensis polysaccharide |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111214846A (en) * | 2019-11-29 | 2020-06-02 | 云南绿A生物产业园有限公司 | Haematococcus pluvialis extract and preparation method thereof |
| CN111214846B (en) * | 2019-11-29 | 2022-05-17 | 云南绿A生物产业园有限公司 | Haematococcus pluvialis extract and preparation method thereof |
| CN117247849A (en) * | 2023-11-20 | 2023-12-19 | 山东悦翔生物有限公司 | Microalgae extraction method |
| CN117247849B (en) * | 2023-11-20 | 2024-02-06 | 山东悦翔生物有限公司 | Microalgae extraction method |
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Application publication date: 20181116 |