CN107903334A - A kind of technique that green alga proteoglycan is extracted from fresh green alga - Google Patents
A kind of technique that green alga proteoglycan is extracted from fresh green alga Download PDFInfo
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- CN107903334A CN107903334A CN201711476197.6A CN201711476197A CN107903334A CN 107903334 A CN107903334 A CN 107903334A CN 201711476197 A CN201711476197 A CN 201711476197A CN 107903334 A CN107903334 A CN 107903334A
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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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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/14—Extraction; Separation; Purification
- C07K1/145—Extraction; Separation; Purification by extraction or solubilisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/14—Extraction; Separation; Purification
- C07K1/34—Extraction; Separation; Purification by filtration, ultrafiltration or reverse osmosis
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
A kind of technique that green algae polysaccharide is extracted from fresh green alga, includes the following steps：Fresh green alga is gathered, is cleaned, dehydration；Dewatered green alga is shredded, is put into grinding in colloid mill, and 40 55 DEG C of warm water is added into colloid mill, obtains green alga slurry；Green alga is starched and carries out hot water extraction, obtains leached slurry, the wherein temperature of hot water extraction is 60 75 DEG C；Leached slurry collects filtrate through coarse filtration；Filtrate to after less than 55 DEG C, then through ultrafiltration desalination, collects the filtrate after desalination through heat exchanger cooling down；The filtrate through vacuum concentration, alcohol steep, vacuum drying, obtains green alga proteoglycan dry powder again.The process advan of the present invention is in the natural green alga proteoglycan of acquisition, also, green algae polysaccharide yield and soluble protein yield can be maintained at higher level.
Description
Technical field
The invention belongs to green alga treatment process field, especially a kind of work that green alga proteoglycan is extracted from fresh green alga
Skill.
Background technology
Marine green algae（Scientific name：Sea lettuce, sliver sea lettuce, U. pertusa, Enteromorpha）It is a kind of algae of large-scale doctor's food homology.
Seaweed is an important component of China's abundant plant resources, related with the rise of utilization marine algae resource upsurge
The research of seaweed pharmacological effects and bioactive ingredients constantly expands and gos deep into.
Domestic and international studies have shown that green algae polysaccharide has extensive bioactivity and medicinal function, with good reducing blood lipid,
Antitumor, antiviral, antibacterial, adjust the various biologicals such as immunity, anti-oxidant, antifatigue, hypoglycemic and radioresistance activity.
At present, in green algae polysaccharide extractive technique, the green algae polysaccharide extracting method announced mainly has Hot water extraction, heat
Flooding-ultrasonic wave auxiliary law, hot water extraction-microwave assisting method, hot water extraction-papain combined extracting method etc..But
In order to improve the yield of green algae polysaccharide, these existing green algae polysaccharide extracting methods using membrane filtration come the deproteinized that desalts, together
When, by micromolecule polypeptide, soluble protein, mineral matter more when " discarded object " discarding, environment is not only polluted, and increase cost one
More than times.Also, these existing green algae polysaccharide extracting method raw material generally use green alga dry powder, and green alga dry powder is by fresh
Green alga is cleaned, dries, is obtained after crushing, and therefore, cost of material is higher；Also, expanded after the immersion of green alga dry powder particle, volume
10-20 times can be increased, green alga particle is bigger, and the dissolution rate of green algae polysaccharide is lower, largely effects on polysaccharide and solubility in green alga
The dissolution of albumen isoreactivity macromolecular substances.In addition, during being dried to fresh green alga, green alga can be inevitably brought
The change of proteoglycan isoreactivity macromolecular 3-D solid structure, is unfavorable for obtaining natural green alga proteoglycan, and natural green
The activity of algae proteoglycan is often more preferable, while also counteracts that the research of the three-dimensional structure to natural green-alga proteoglycan；In addition,
Drying is also easy to cause the inactivation of the soluble protein in plant.
The Chinese patent of Publication No. CN106519059A discloses a kind of sea grass polysaccharide（That is green alga）Preparation method, should
Method using fresh Enteromorpha be used as raw material, it is cleaned, dehydration, soak 8h, smash to pieces after, using Hot water extraction（Hot water temperature
For 80-105 DEG C）To extract sea grass polysaccharide.But this method still remains following defect：（1）It is short grained green in order to obtain
Algae, green alga need to soak 8h before smashing to pieces, take longer, inefficiency；（2）Smashed to pieces using bruisher, the green alga after smashing to pieces
Grain is uneven, influences the recovery rate of green alga proteoglycan；（3）The green algae polysaccharide preparation method of this patent is extracted with existing green alga
Method is the same, is all to be extracted using 80 DEG C of hot water, although hot water extraction can improve green algae polysaccharide to a certain extent
Dissolution rate, beneficial to the yield for improving green algae polysaccharide, still, the three-dimensional structure that high temperature is also easy to cause green alga proteoglycan becomes
Change, be unfavorable for obtaining the Large molecule active components such as natural green alga proteoglycan, and soluble protein also easily inactivates.Always
It, the recovery rate of existing green algae polysaccharide extracting method green algae polysaccharide and soluble protein is relatively low, also, is also unfavorable for obtaining
Obtain the Large molecule active components such as green alga proteoglycan naturally.
The content of the invention
The present invention is intended to provide a kind of technique that green alga proteoglycan is extracted from fresh green alga, which will not be to green alga
The 3-D solid structure of the biologically active macromolecular such as proteoglycan damages, and is conducive to obtain natural green alga albumen
Polysaccharide, also, green algae polysaccharide yield and soluble protein yield can be maintained at higher level.
A kind of technique that green alga proteoglycan is extracted from fresh green alga, includes the following steps：
（1）Fresh green alga is gathered, after cleaning up, dehydration（Also the salinity on frond surface can be got rid of while dehydration）, slough
At least moisture on frond surface 20%, obtains dewatered green alga；
（2）Dewatered green alga is shredded, is put into colloid mill, and 40-55 DEG C of warm water is added into colloid mill, is included
Green alga grain diameter is starched for micron-sized green alga；
（3）Green alga is starched and carries out hot water extraction, obtains leached slurry, wherein the temperature control of hot water extraction is at 60-75 DEG C；
（4）Leached slurry collects filtrate through coarse filtration；
（5）Filtrate, to after less than 55 DEG C, adds purified water to dilute through heat exchanger cooling down, then by ultrafiltration desalination, collects de-
Filtrate after salt；
（6）Filtrate after desalination obtains green alga proteoglycan through vacuum concentration, alcohol steep, vacuum drying（" green alga albumen is more
Sugar " is green algae polysaccharide and the general designation of green alga soluble protein）Dry powder.
The present invention using fresh green alga as raw material on the basis of, be 40-55 DEG C of temperature by the green alga of chopping and temperature
Water mixes, and warm water not only can soften green alga frond, but also advantageously reduces algae slurry viscosity, and warm water association colloid mill is to chopping
Green alga handled, can obtain green alga particle diameter and starched for micron-sized algae, green alga particle diameter is smaller, is more conducive to green algae polysaccharide and can
The dissolution of dissolubility albumen so that follow-up only to need the hot water that temperature is 60-75 DEG C to carry out the short time（90min）Extraction, so that it may reach
Green algae polysaccharide recovery rate to existing hot water extraction is horizontal（More than 13%）.Also, hot water extraction processing causes green algae polysaccharide and can
Dissolubility albumen is able to dissolve in the hot water.In addition, the temperature of hot water is 60-75 DEG C during hot water extraction, will not be to green alga egg
The 3-D solid structure of the biologically active macromoleculars such as white polysaccharide damages, and is conducive to obtain natural green alga albumen more
Sugar, meanwhile, the inactivation of soluble protein in green alga will not be caused, remains the soluble protein in green alga body as far as possible,
Soluble protein is important osmotic adjustment and nutriment, their increase and accumulation can improve the water conservation energy of cell
Power, plays a protective role the living matter and biomembrane of cell so that obtained dry powder is very suitable for making facial mask and battalion
Support health products.
In order to further improve the yield of green alga proteoglycan, in step（2）Afterwards, step（3）Preceding increase ultrasonication
Step.Sonicating step can make green alga particle further diminish, beneficial to the dissolution of green algae polysaccharide and soluble protein.
In specific implementation process, sonicating step is specially：Green alga is starched and carries out ultrasonication, the temperature of ultrasonication is
30-40 DEG C, time 3-5min, ultrasonic frequency 3800-7500 MHz.Warm water is conducive to cell of the ultrasonic wave to chlorella cell
Wall is crushed, beneficial to the dissolution of green alga proteoglycan.
In order to improve the yield of green alga proteoglycan, in step（2）Afterwards, step（3）Preceding increase enzymatic treatment step.Enzyme process
Processing step can make green alga particle further diminish, beneficial to the dissolution of green algae polysaccharide and soluble protein.It had been embodied
Cheng Zhong, enzymatic treatment step are specially：By in the green alga slurry input enzyme reaction tank after ultrasonication, enzyme additive amount is 0.8-
2%, for the temperature control in enzyme reaction tank at 35-45 DEG C, the time is 90-120 min.In enzyme reaction tank, the temperature in enzyme reaction tank
Degree control also ensure that enzyme still has higher activity at 35-45 DEG C, and enzyme decomposes chlorella cell, promote in green alga
The further dissolution of polysaccharide and soluble protein, meanwhile, warm water is also beneficial to the dissolving of the polysaccharide and soluble protein in green alga.
Certainly, in step（2）Afterwards, step（3）It is preceding also to increase sonicating step and enzymatic treatment step at the same time, this
When, step（3）Gained leached slurry green algae particle is up to nanoscale.Also, enzymatic treatment step is preferably disposed on ultrasonic wave
After processing step, ultrasonic wave is avoided to cause to inactivate to enzyme.Further, the step（2）The net of the discharging backstop of middle colloid mill
Bore dia is preferably 8-15 μm, has both avoided the mesh diameter of discharging backstop too big, has been carried even with supercritical ultrasonics technology and enzyme process
Take, green alga particle is also unable to reach nano level requirement, and then limits the dissolution of green algae polysaccharide and soluble protein；Avoid out again
Expect that the mesh diameter of backstop is too small, cause colloid mill yield too low, be unfavorable for industrialization production.
The step（1）The moisture for sloughing frond surface 20-30%, green alga water content is moderate, after chopping can will
Frond is cut into the fragment of 1-2cm, and more small offer condition is adjusted to stinging for colloid mill internal gear teeth.
The step（6）Obtained green alga proteoglycan dry powder can obtain finished product through crushing, sieving, packing.
The step（5）Ultrafiltration use molecular cut off as the filter membrane of 1000Da, not only protect green algae polysaccharide, but also retain
The loss of micromolecule polypeptide, soluble protein and mineral matter.
Collection step（4）Filter residue of the leached slurry after coarse filtration, and be dehydrated, dry, obtain green alga dietary fiber.
After coarse filtration, the salinity in green alga is distributed mainly in filtrate, and salinity is substantially free of in filter residue or containing a small amount of salinity.
Contain substantial amounts of dietary fiber in the filter residue, after being dehydrated, drying, obtain green alga dietary fiber, it can be used as feed etc..
Embodiment
The embodiment for now providing the present invention is as follows：
A kind of technique that green alga proteoglycan is extracted from fresh green alga, includes the following steps：
（1）Fresh green alga is gathered, after cleaning up, dehydration（Also the salinity on frond surface can be got rid of while dehydration）, slough
At least moisture on frond surface 20%, obtains dewatered green alga；
（2）Dewatered green alga is shredded, is put into colloid mill, and 40-55 DEG C of warm water is added into colloid mill, is included
Green alga grain diameter is starched for micron-sized green alga；
（3）Green alga is starched and carries out hot water extraction, obtains leached slurry, wherein the temperature control of hot water extraction is at 60-75 DEG C；
（4）Leached slurry collects filtrate through coarse filtration；
（5）Filtrate, to after less than 55 DEG C, adds purified water to dilute through heat exchanger cooling down, then by ultrafiltration desalination, collects de-
Filtrate after salt；
（6）Filtrate after desalination obtains green alga proteoglycan through vacuum concentration, alcohol steep, vacuum drying（" green alga albumen is more
Sugar " is green algae polysaccharide and the general designation of green alga soluble protein）Dry powder.
4 embodiments are now carried out according to the above-mentioned technique that green alga proteoglycan is extracted from fresh green alga（That is embodiment 1-
Embodiment 4）, and enumerate this 4 embodiments colloid mill discharging backstop mesh diameter, add colloid mill warm water temperature,
Hot water extraction treatment temperature, processing time is in table 1.
Meanwhile the present inventor additionally provides embodiment 5- embodiments 7.Wherein, embodiment 5- embodiments 7 and embodiment 2 be not
Be：In step（2）Afterwards, step（3）Preceding increase sonicating step, and enumerate the ultrasonic wave of embodiment 5- embodiments 7
The temperature of processing, time, ultrasonic frequency are in table 2.
The present inventor additionally provides embodiment 8- embodiments 10.Wherein, embodiment 8- embodiments 10 are different from embodiment 2
It is：In step（2）Afterwards, step（3）Preceding increase enzymatic treatment step, and enumerate the enzyme of the enzymatic treatment of embodiment 8- embodiments 10
Additive amount, temperature, time are in table 2.
In addition, the present inventor additionally provides embodiment 11- embodiments 13.Wherein, embodiment 11- embodiments 13 and embodiment 2
Difference be：In step（2）Afterwards, step（3）It is preceding to increase sonicating step and enzymatic treatment step successively.Side by side
Enzyme additive amount, temperature for the temperature of the ultrasonication of embodiment 11- embodiments 1, time, ultrasonic frequency and enzymatic treatment
Degree, time are in table 2.
The present inventor measures the yield of the green algae polysaccharide of the green alga proteoglycan of embodiment 1- embodiments 13 and soluble respectively
Rate, and be recited in table 3.
It can be seen that from the embodiment 1- embodiments 4 of table 3, the present invention grinds warm water association colloid so that subsequently only needs temperature
The short time is carried out for 60-75 DEG C of hot water（90min）Extraction, so that it may reach the green algae polysaccharide recovery rate water of existing hot water extraction
It is flat（More than 13%）, meanwhile, soluble protein recovery rate has also reached more than 12%.Also, can from embodiment 5- embodiments 7
Go out, after increasing sonicating step, the yield of green algae polysaccharide and soluble protein is all improved to some extent.From embodiment
8- embodiments 10 can be seen that after increasing enzymatic treatment step, the yield of green algae polysaccharide and soluble protein also has to a certain degree
Raising.It can be seen that from the comparison of the embodiment 5- embodiments 13 of table 3, while increase sonicating step and enzymatic treatment step
When rapid, the yield highest of green algae polysaccharide and soluble protein.
In addition, the temperature of hot water is 60-75 DEG C during hot water extraction, will not be biologically active to green algae polysaccharide etc.
The 3-D solid structure of macromolecular damages, and is conducive to obtain natural green algae polysaccharide, meanwhile, will not cause can in green alga
The inactivation of dissolubility albumen, remains the soluble protein in green alga body as far as possible so that obtained dry powder is very suitable for making
Make facial mask and nutrient and healthcare products.
In process of production, fresh green alga manually chooses miscellaneous algae, and cleaned machine, removes silt；The green alga cleaned up
It is dehydrated successively through dewaterer, shredding machine is shredded, colloid mill carries out defibrination, ultrasonic drilling machine carries out ultrasonic extraction（Can
Choosing）, Enzymatic Extraction tank carry out Enzymatic Extraction（It is optional）, multi-function extractor carry out hot water extraction, collect multi-function extractor
For supernatant in the first storage tank, the green alga extracting solution in the first storage tank removes thick dietary fiber, heat exchange through bag filter successively again
Device is cooled down, the second storage tank carries out temporarily storage, ultrafiltration apparatus desalination, the 3rd storage tank carry out temporarily storage, inspissator
Concentrated, alcohol steep, vacuum drying, obtain green alga proteoglycan dry powder.
Certainly, the temperature of ultrasonication of the invention, time, ultrasonic frequency are not limited to embodiment 5- embodiments 7
With the concrete numerical value of embodiment 10- embodiments 13, using the Parameter Conditions of existing ultrasonic extraction method green algae polysaccharide；This
The enzyme additive amount of the enzymatic treatment of invention, temperature, time are also not limited to embodiment 8- embodiments 10 and embodiment 10- embodiments
13 concrete numerical value, using the Parameter Conditions of existing Enzymatic Extraction green algae polysaccharide.In addition, the discharging of the colloid mill of the present invention
The mesh diameter of backstop is not limited to the concrete numerical value of embodiment 1- embodiments 13.
The embodiment of the present invention 1- embodiments 3 can do following improvement：
1）The step（1）The moisture for sloughing frond surface 20-30%, green alga water content is moderate, can be by algae after chopping
Body is cut into the fragment of 1-2cm, and more small offer condition is adjusted to stinging for colloid mill internal gear teeth；
2）The step（6）Obtained green alga proteoglycan dry powder can obtain finished product through crushing, sieving, packing；
3）The step（5）Ultrafiltration use molecular cut off not only to protect green algae polysaccharide, but also remain for the filter membrane of 1000Da
The loss of micromolecule polypeptide, soluble protein and mineral matter；
4）Collection step（4）Filter residue of the leached slurry after coarse filtration, and be dehydrated, dry, obtain green alga dietary fiber.Slightly
After filtering, the salinity in green alga is distributed mainly in filtrate, and salinity is substantially free of in filter residue or containing a small amount of salinity.Should
Contain substantial amounts of dietary fiber in filter residue, after being dehydrated, drying, obtain green alga dietary fiber, it can be used as feed etc..
Claims (10)
1. a kind of technique that green alga proteoglycan is extracted from fresh green alga, includes the following steps：
（1）Fresh green alga is gathered, after cleaning up, dehydration, sloughs the moisture at least frond surface 20%, obtain dewatered green
Algae；
（2）Dewatered green alga is shredded, is put into colloid mill, and 40-55 DEG C of warm water is added into colloid mill, is included
Green alga grain diameter is starched for micron-sized green alga；
（3）Green alga is starched and carries out hot water extraction, obtains leached slurry, wherein the temperature control of hot water extraction is at 60-75 DEG C；
（4）Leached slurry collects filtrate through coarse filtration；
（5）Filtrate, to after less than 55 DEG C, adds purified water to dilute through heat exchanger cooling down, then by ultrafiltration desalination, collects de-
Filtrate after salt；
（6）Filtrate after desalination obtains green alga proteoglycan dry powder through vacuum concentration, alcohol steep, vacuum drying.
A kind of 2. technique that green algae polysaccharide is extracted from fresh green alga according to claim 1, it is characterised in that：In step
（2）Afterwards, step（3）Preceding increase sonicating step.
A kind of 3. technique that green algae polysaccharide is extracted from fresh green alga according to claim 2, it is characterised in that ultrasonic wave
Processing step is specially：Green alga to be starched and carries out ultrasonication, the temperature of ultrasonication is 30-40 DEG C, time 3-5min,
Ultrasonic frequency 3800-7500 MHz.
A kind of 4. technique that green algae polysaccharide is extracted from fresh green alga according to claim 1, it is characterised in that：In step
（2）Afterwards, step（3）Preceding increase enzymatic treatment step.
5. a kind of technique that green algae polysaccharide is extracted from fresh green alga according to claim 4, it is characterised in that at enzyme process
Managing step is specially：By in the green alga slurry input enzyme reaction tank after ultrasonication, enzyme additive amount is 0.8-2%, in enzyme reaction tank
Temperature control at 35-45 DEG C, the time is 90-120 min.
A kind of 6. technique that green algae polysaccharide is extracted from fresh green alga according to claim 1, it is characterised in that：In step
（2）Afterwards, step（3）Preceding while when increasing sonicating step and enzymatic treatment step, enzymatic treatment step is arranged at ultrasound
After ripple processing step.
A kind of 7. technique that green algae polysaccharide is extracted from fresh green alga according to claim 1, it is characterised in that：The step
Suddenly（2）The mesh diameter of the discharging backstop of middle colloid mill is 8-15 μm.
A kind of 8. technique that green algae polysaccharide is extracted from fresh green alga according to claim 1, it is characterised in that：The step
Suddenly（1）The moisture for sloughing frond surface 20-30%.
A kind of 9. technique that green algae polysaccharide is extracted from fresh green alga according to claim 1, it is characterised in that：The step
Suddenly（5）Ultrafiltration use filter membrane of the molecular cut off for 1000Da.
A kind of 10. technique that green algae polysaccharide is extracted from fresh green alga according to claim 1, it is characterised in that：Collect
Step（4）Filter residue of the leached slurry after coarse filtration, and be dehydrated, dry, obtain green alga dietary fiber.
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| CN110250527A (en) * | 2019-07-19 | 2019-09-20 | 福建海兴保健食品有限公司 | A kind of technique for extracting dietary fiber from green alga residue |
| CN112144135A (en) * | 2020-09-30 | 2020-12-29 | 江苏康溢臣生命科技有限公司 | Preparation method of functional viscose containing chlorella protein algae extract |
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| CN110250527A (en) * | 2019-07-19 | 2019-09-20 | 福建海兴保健食品有限公司 | A kind of technique for extracting dietary fiber from green alga residue |
| CN112144135A (en) * | 2020-09-30 | 2020-12-29 | 江苏康溢臣生命科技有限公司 | Preparation method of functional viscose containing chlorella protein algae extract |
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