CN104862366B - A kind of technique from black sharkskin extraction collagen peptide, dermatan sulfate, hydroxyapatite and melanin - Google Patents
A kind of technique from black sharkskin extraction collagen peptide, dermatan sulfate, hydroxyapatite and melanin Download PDFInfo
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- CN104862366B CN104862366B CN201510340198.2A CN201510340198A CN104862366B CN 104862366 B CN104862366 B CN 104862366B CN 201510340198 A CN201510340198 A CN 201510340198A CN 104862366 B CN104862366 B CN 104862366B
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- hydroxyapatite
- dermatan sulfate
- collagen peptide
- sharkskin
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- XUMBMVFBXHLACL-UHFFFAOYSA-N Melanin Chemical compound O=C1C(=O)C(C2=CNC3=C(C(C(=O)C4=C32)=O)C)=C2C4=CNC2=C1C XUMBMVFBXHLACL-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229920000045 Dermatan sulfate Polymers 0.000 title claims abstract description 35
- 102000008186 Collagen Human genes 0.000 title claims abstract description 34
- 108010035532 Collagen Proteins 0.000 title claims abstract description 34
- 229920001436 collagen Polymers 0.000 title claims abstract description 34
- AVJBPWGFOQAPRH-FWMKGIEWSA-L dermatan sulfate Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@H](OS([O-])(=O)=O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@H](C([O-])=O)O1 AVJBPWGFOQAPRH-FWMKGIEWSA-L 0.000 title claims abstract description 33
- 229940051593 dermatan sulfate Drugs 0.000 title claims abstract description 33
- 108090000765 processed proteins & peptides Proteins 0.000 title claims abstract description 32
- 229910052588 hydroxylapatite Inorganic materials 0.000 title claims abstract description 29
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000000605 extraction Methods 0.000 title claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
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- 238000001179 sorption measurement Methods 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
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- 230000009849 deactivation Effects 0.000 claims description 6
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- 238000001556 precipitation Methods 0.000 claims description 6
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- 238000010612 desalination reaction Methods 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000003837 high-temperature calcination Methods 0.000 claims description 5
- 238000001728 nano-filtration Methods 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 239000002781 deodorant agent Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 239000008213 purified water Substances 0.000 claims description 4
- 108010019160 Pancreatin Proteins 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 229940055695 pancreatin Drugs 0.000 claims description 3
- 235000019834 papain Nutrition 0.000 claims description 3
- OEANUJAFZLQYOD-CXAZCLJRSA-N (2r,3s,4r,5r,6r)-6-[(2r,3r,4r,5r,6r)-5-acetamido-3-hydroxy-2-(hydroxymethyl)-6-methoxyoxan-4-yl]oxy-4,5-dihydroxy-3-methoxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](OC)O[C@H](CO)[C@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](OC)[C@H](C(O)=O)O1 OEANUJAFZLQYOD-CXAZCLJRSA-N 0.000 claims description 2
- 102000029816 Collagenase Human genes 0.000 claims description 2
- 108060005980 Collagenase Proteins 0.000 claims description 2
- 206010013786 Dry skin Diseases 0.000 claims description 2
- 108090000526 Papain Proteins 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
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- 239000012530 fluid Substances 0.000 claims description 2
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims description 2
- 229940055729 papain Drugs 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims 1
- 239000003292 glue Substances 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 238000001694 spray drying Methods 0.000 claims 1
- 239000008107 starch Substances 0.000 claims 1
- 235000019698 starch Nutrition 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
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- 238000002360 preparation method Methods 0.000 abstract description 2
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- 229920002683 Glycosaminoglycan Polymers 0.000 description 2
- 102000035195 Peptidases Human genes 0.000 description 2
- 102000016611 Proteoglycans Human genes 0.000 description 2
- 108010067787 Proteoglycans Proteins 0.000 description 2
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- 241000251468 Actinopterygii Species 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 241000725303 Human immunodeficiency virus Species 0.000 description 1
- 235000019738 Limestone Nutrition 0.000 description 1
- -1 N- acetylamino galactosamines Chemical class 0.000 description 1
- 102000011931 Nucleoproteins Human genes 0.000 description 1
- 108010061100 Nucleoproteins Proteins 0.000 description 1
- DMGNFLJBACZMRM-UHFFFAOYSA-N O[P] Chemical compound O[P] DMGNFLJBACZMRM-UHFFFAOYSA-N 0.000 description 1
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- XDVMCVGTDUKDHL-UHFFFAOYSA-N [amino(2-azaniumylethylsulfanyl)methylidene]azanium;dibromide Chemical compound Br.Br.NCCSC(N)=N XDVMCVGTDUKDHL-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- IAJILQKETJEXLJ-SKNVOMKLSA-N aldehydo-L-iduronic acid Chemical class O=C[C@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O IAJILQKETJEXLJ-SKNVOMKLSA-N 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
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- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 1
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- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
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- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000002434 immunopotentiative effect Effects 0.000 description 1
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- 210000004379 membrane Anatomy 0.000 description 1
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- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 1
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Abstract
The invention discloses a kind of technique from black sharkskin extraction collagen peptide, dermatan sulfate, hydroxyapatite and melanin, which is：By the pretreatment of black sharkskin, enzymolysis；Centrifuge out clear liquid and solid sediment；Clear liquid obtains collagen peptide and dermatan sulfate respectively through ultrafiltration or resin adsorption.Solid sediment through NaOH processing, be centrifugally separating to obtain hydroxyapatite and melanin.The invented technology feature is continuous acquisition collagen peptide, dermatan sulfate, hydroxyapatite and melanin, realizes the comprehensive utilization of sharkskin, reduces the discharge of waste in extraction preparation process, save production cost, business efficiency is improved, and this is simple for process, it can be achieved that industrialization.
Description
Technical field
A kind of technique from black sharkskin extraction collagen peptide, dermatan sulfate, hydroxyapatite and melanin belongs to day
Right product extracts field.
Background technology
Collagen peptide is easy to digest and assimilate, and there is protection gastric mucosa to prevent gastric ulcer, calcium uptake is promoted to prevent osteoporosis, promote
It is metabolized into skin collagen, blood pressure is inhibited to rise, and reduce various physiological functions such as serum cholesterol levels, lead to city
Field is continuously increased the demand of collagen peptide.
Dermatan sulfate is a kind of glycosaminoglycan, belongs to glycosaminoglycan, disaccharides mainly by N- acetylamino galactosamines and
L- iduronic acids are keyed with β -1,4 or β -1,3.It is breaking containing sugar-tablet in proteoglycans overall molecule structure,
It is connected with the nucleoprotein of proteoglycans by covalent bond.Dermatan sulfate all has wide in food, medicine and cosmetic field
Application prospect.
Hydroxyapatite (HAP) is the main inorganic composition of vertebrate skeletal and tooth, hydroxyl phosphorus in the enamel of people
The content of lime stone is 96% or more.With excellent biocompatibility, it is acknowledged as a kind of superior artificial bone of biological property
Material is widely used in clinic.Hydroxyapatite also has outstanding adsorption capacity, is used as the adsorption material of chromatography purifying
Material.It can also calcium tonic etc..
Melanin is not only a kind of bright protective agent, anti-rad, couplant, biological anti-oxidant and immunopotentiating agent, and
And still a kind of biological semiconductor materials.Recent study finds that melanin has anti-snake venom, anticancer, inhibits AIDS virus multiple
The effects that system, treatment parkinsonism.Some melanin are gradually applied in every field.Such as Semen sesami nigrum in the food industry, black
Melanin in rice, black soya bean is applied to beverage, candy, cake, chocolate, jam etc..Resist studies have shown that natural black pigment has
The functions such as aging are aoxidized and prevent, this will greatly promote application of the natural black pigment in health food.Natural black pigment is being changed
Industrial previous night is increasingly subject to welcome, and can be applied in the products such as hair blackening agent, suncream.
Now, it is increasingly not suitable with social development using fish-skin production single product, how improves the comprehensive utilization of fish-skin,
Have become the research topic of growing interest.In view of collagen, dermatan sulfate, the hydroxy-apatite contained in black sharkskin
Stone and melanin etc. make full use of collagen, dermatan sulfate, hydroxyapatite and melanin therein, are respectively prepared pure
Higher product is spent, the utility value of fish-skin is improved.
Currently, still without relevant coproduction patent report.
The present invention obtained from black sharkskin by using technologies such as enzymolysis, centrifugation, ultrafiltration or absorption fish skin collagen peptide,
Dermatan sulfate, hydroxyapatite and melanin product.
Invention content
The purpose of the present invention is to provide one kind extracting collagen peptide, dermatan sulfate, hydroxyapatite from black sharkskin
With the technique of melanin, it be using black sharkskin as raw material, be prepared into small molecule active collagen peptide, dermatan sulfate,
The technique of hydroxyapatite and melanin.
To achieve the goals above, the technical scheme is that：
The present invention is a kind of work from black sharkskin extraction collagen peptide, dermatan sulfate, hydroxyapatite and melanin
Skill, specific process step are as follows：
(1) the black sharkskin after drying cleaning crushes, and purified water is added, and is warming up to 65-90 DEG C, pretreatment
0.5-2.5 hours；
(2) pretreatment fluid in step (1) is cooled down, pH to 7.5-9.0 is adjusted with alkali, compound protease is added and carries out
Enzymolysis, hydrolysis temperature are 50-58 DEG C, and enzymolysis time is 4-12 hours；
(3) the enzymolysis liquid pH value in step (2) is adjusted to 3.0-6.0, is warming up to 75-90 DEG C, keep the temperature 10-30 minutes
Enzyme deactivation；
(4) material in step (3) is separated by solid-liquid separation, obtains clear liquid and solid sediment respectively；
(5) it by the clear liquid in step (4), is detached using Ultra filtration membrane or resin adsorption, obtains concentrate and permeate,
Concentrate is the aqueous solution of sulfur acid dermatan, and permeate is the aqueous solution containing collagen peptide；
(6) concentrate in step (5) is added to 90% or more the alcohol of 3-6 times of its weight, 2-4 hours is stood, obtains
Sediment is obtained, sediment is dissolved in water, and then adjusts pH to 10.5-11.5, adds the 0.5-3% hydrogen peroxide of solution weight,
6-8 hours are stood, the pH of filtrate is adjusted to 6-7 by filtering, and the alcohol of 4-7 times 90% or more of its volume is added, and stands 2-6
Hour, precipitation is collected, is dehydrated through absolute ethyl alcohol, dermatan sulfate is obtained through being dried under reduced pressure；
(7) by the permeate in step (5), through nanofiltration desalination, large aperture adsorption resin decoloration, porn star are spray-dried
To collagen peptide；
(8) solid sediment in step (4) is handled 1-4 hours with NaOH solution, is separated by solid-liquid separation, that isolates consolidates
Body through washing, high-temperature calcination, obtains hydroxyapatite；The liquid isolated, it is 1-3 that hydrochloric acid, which is added, and adjusts ph values, stands 2-6
Hour, sediment is washed, and drying obtains melanin.
In step (1), it is 2-6 times of shark dry hide weight to add the amount of purified water.
In step (2), the compound protease is pancreatin, alkali protease, Collagenase and papain
Any one is combined, and the additive amount of each enzyme is the 0.5%-2.0% of fish-skin dry weight.
In step (3), enzymolysis liquid pH value is adjusted to 3.0-6.0 before enzyme deactivation.
It is described to be separated by solid-liquid separation to centrifuge in step (4).
In step (5), the ultrafiltration membrane retention fractional dose is 6000-15000 dalton.
In step (5), the resin is the resin that specificity adsorbs dermatan sulfate.
In step (6), the temperature that is dried under reduced pressure is 65-80 DEG C.
In step (8), a concentration of 0.1M of NaOH solution.
The advantage of the invention is that：
1, the present invention prepares product using enzyme process, and simple for process, mild condition, low energy consumption.
2, the present invention can prepare multiple product simultaneously using black sharkskin, and raw material availability is high.
3, the molecular weight of collagen peptide prepared by the present invention is mainly distributed on 300-2000 dalton, is easy to be absorbed by the body.
4, the present invention realizes the comprehensive utilization of its value, considerably reduces waste pollution in fish-skin production process and asks
Topic.
Description of the drawings
Fig. 1 is the graph of molecular weight distribution of shark collagen peptide；
Fig. 2 is the infrared spectrum of shark melanin；
Fig. 3 is the infrared spectrum of shark dermatan sulfate.
Specific implementation mode
The invention will be further described with reference to the accompanying drawings and examples.
Embodiment 1
100kg black shark dry hides are crushed to 25 mesh, 400kg purified waters are added, are heated up 90 DEG C, are kept for 1 hour, cooling
To 53 DEG C, pH value 8.3 is adjusted, the compound protease (0.5kg alkali proteases and 0.5kg pancreatin) of 1kg is added, is stirred at 53 DEG C
Mix enzymolysis 10 hours, it is 4.5 to adjust pH value, is warming up to 90 DEG C of heating enzyme deactivation 20min, is cooled to 50 DEG C, is centrifuged, point
The clear liquid separated out carries out ultrafiltration through 10kDa films, for the permeate of ultrafiltration carry out nanofiltration (interception be 300 dalton) desalination,
Large aperture adsorption resin decoloration, deodorant obtain collagen peptide 42.79kg.To 95% alcohol for adding 4 times in liquid is concentrated by ultrafiltration, stand
2 hours, sediment is obtained, sediment is dissolved in water, and then adjusts pH to 11, adds 1% hydrogen peroxide of solution weight, stands 6
Hour, the pH of filtrate is adjusted to 6 by filtering, and the alcohol of 5 times 95% of its volume is added, and stands 2-4 hours, precipitation is collected, through nothing
Water-ethanol is dehydrated, and is dried under reduced pressure 4 hours through 70 DEG C and is obtained dermatan sulfate 1.35kg.The solid centrifuged out is with 0.1M's
After NaOH is handled 2 hours, centrifuged again, the solid isolated, washed, high-temperature calcination obtains hydroxyapatite
12.21kg.The akaline liquid isolated, it is 1 to adjust ph values with hydrochloric acid, stands 4 hours, and the washed drying of sediment obtains black
Plain 1.17kg.
Embodiment 2
100kg black shark dry hides are crushed to 30 mesh, 600kg purified waters are added, are heated up 85 DEG C, are kept for 2 hours, cooling
To 55 DEG C, pH value 8.0 is adjusted, the compound protease (1kg alkali proteases and 1kg clostridiopetidase As) of 2kg is added, is stirred at 55 DEG C
Enzymolysis 11 hours, it is 4.0 to adjust pH value, is warming up to 80 DEG C of heating enzyme deactivation 30min, is cooled to 60 DEG C, is centrifuged, detach
The clear liquid gone out carries out ultrafiltration through 15kDa films, and nanofiltration (interception be 300 dalton) desalination, big is carried out for the permeate of ultrafiltration
Aperture absorption resin decolorization, deodorant obtain collagen peptide 42.65kg.To 92% alcohol for adding 5 times in liquid is concentrated by ultrafiltration, 3 are stood
Hour, sediment is obtained, sediment is dissolved in water, and then adjusts pH to 11.5, adds 1.5% hydrogen peroxide of solution weight, quiet
It sets 7 hours, filters, the pH of filtrate is adjusted to 6.5, the alcohol of 6 times 92% of its volume is added, stand 2 hours, collect precipitation,
It is dehydrated through absolute ethyl alcohol, is dried under reduced pressure 3 hours through 80 DEG C and obtains dermatan sulfate 1.42kg.The solid 0.1M centrifuged out
NaOH handle 2 hours after, centrifuged again, the solid isolated, washed, high-temperature calcination obtains hydroxyapatite
11.83kg.The akaline liquid isolated, it is 3 to adjust ph values with hydrochloric acid, stands 5 hours, and the washed drying of sediment obtains black
Plain 1.04kg.
Embodiment 3
100kg black shark dry hides are crushed to 30 mesh, 500kg purified waters are added, are heated up 90 DEG C, are kept for 1.5 hours, drop
Temperature adjusts pH value 7.5, the compound protease (1.0kg papains and 1kg clostridiopetidase As) of 2kg is added, at 50 DEG C to 50 DEG C
Stirring enzymolysis 12h, it is 5.0 to adjust pH value, is warming up to 85 DEG C of heating enzyme deactivation 25min, is cooled to 55 DEG C, is centrifuged, point
The clear liquid separated out carries out nanofiltration through dermatan sulfate resin adsorption, for the permeate after absorption (interception is 300 dalton)
Desalination, large aperture adsorption resin decoloration, deodorant obtain collagen peptide 42.56kg.92% wine for adding 5 times is washed in concentrate to taking off
Essence stands 4 hours, obtains sediment, and sediment is dissolved in water, and then adjusts pH to 10.5, adds 1.0% peroxide of solution weight
Changing hydrogen, stands 8 hours, the pH of filtrate is adjusted to 6.3 by filtering, and the alcohol of 5.5 times 94% of its volume is added, and stands 4 hours,
Precipitation is collected, is dehydrated through absolute ethyl alcohol, is dried under reduced pressure 3.5 hours through 78 DEG C and obtains dermatan sulfate 1.37kg.It centrifuges out
Solid handled 3 hours with the NaOH of 0.1M after, centrifuged again, the solid isolated, washed, high-temperature calcination obtains hydroxyl
Base apatite 11.94kg.The akaline liquid isolated, it is 2 to adjust ph values with hydrochloric acid, stands 6 hours, the washed drying of sediment
Obtain melanin 1.09kg.
Embodiment the result shows that, black sharkskin pre-processes, digested by the present invention, centrifuges out clear liquid and solid precipitation
Object；Clear liquid obtains collagen peptide and dermatan sulfate respectively through ultrafiltration or resin adsorption.Solid sediment is through NaOH processing, centrifugation point
From obtaining hydroxyapatite and melanin.The invented technology feature is continuous acquisition collagen peptide, dermatan sulfate, hydroxyapatite
And melanin, the comprehensive utilization of sharkskin is realized, the discharge of waste in extraction preparation process is reduced, saves production cost,
Improve business efficiency；In addition this is simple for process, it can be achieved that industrialization.
Specific embodiments of the present invention are above are only, but the design concept of the present invention is not limited thereto, it is all to utilize this structure
Think, to the change of present invention progress unsubstantiality, the behavior for invading the scope of the present invention should all be belonged to.
1 shark collagen peptide amino acid of table forms
Claims (8)
1. a kind of technique from black sharkskin extraction collagen peptide, dermatan sulfate, hydroxyapatite and melanin, feature exists
In：It includes the following steps：
(1) the black sharkskin after drying cleaning crushes, and purified water is added, and is warming up to 65-90 DEG C, pre-processes 0.5-
2.5 hour；
(2) pretreatment fluid in step (1) is cooled down, pH to 7.5-9.0 is adjusted with alkali, compound protease is added and is digested,
Hydrolysis temperature is 50-58 DEG C, and enzymolysis time is 4-12 hours；
(3) the enzymolysis liquid pH value in step (2) is adjusted to 4.0-6.0, is warming up to 75-90 DEG C, keep the temperature enzyme deactivation in 20-30 minutes；
(4) material in step (3) is separated by solid-liquid separation, obtains clear liquid and solid sediment respectively；
(5) it by the clear liquid in step (4), is detached using Ultra filtration membrane or resin adsorption, obtains concentrate and permeate, concentrated
Liquid is the aqueous solution of sulfur acid dermatan, and permeate is the aqueous solution containing collagen peptide；
(6) concentrate in step (5) is added to 90% or more the alcohol of 3-6 times of its weight, 2-4 hours is stood, is sunk
Starch, sediment are dissolved in water, and then adjust pH to 10.5-11.5, add the 0.5-3% hydrogen peroxide of solution weight, stand
6-8 hours, the pH of filtrate was adjusted to 6-7 by filtering, and the alcohol of 4-7 times 90% or more of its volume is added, and stands 2-4 hours,
Precipitation is collected, is dehydrated through absolute ethyl alcohol, dermatan sulfate is obtained through being dried under reduced pressure；
(7) by the permeate in step (5), through nanofiltration desalination, large aperture adsorption resin decoloration, deodorant, spray drying obtains glue
Former peptide；
(8) solid sediment in step (4) is handled 1-4 hours with NaOH solution, is separated by solid-liquid separation, the solid isolated,
Through washing, high-temperature calcination, obtain hydroxyapatite；The liquid isolated, addition salt acid for adjusting pH value are 1-3, and it is small to stand 2-6
When, sediment is washed, and drying obtains melanin.
2. according to claim 1 a kind of from black sharkskin extraction collagen peptide, dermatan sulfate, hydroxyapatite and black
The technique of pigment, it is characterised in that in step (1), it is 2-6 times of shark dry hide weight to add the amount of purified water.
3. according to claim 1 a kind of from black sharkskin extraction collagen peptide, dermatan sulfate, hydroxyapatite and black
The technique of pigment, it is characterised in that in step (2), the compound protease be pancreatin, alkali protease, Collagenase and
The arbitrary combination of papain, the additive amount of each enzyme are the 0.5%-2.0% of fish-skin dry weight.
4. according to claim 1 a kind of from black sharkskin extraction collagen peptide, dermatan sulfate, hydroxyapatite and black
The technique of pigment, it is characterised in that described to be separated by solid-liquid separation to centrifuge in step (4).
5. according to claim 1 a kind of from black sharkskin extraction collagen peptide, dermatan sulfate, hydroxyapatite and black
The technique of pigment, it is characterised in that in step (5), the ultrafiltration membrane retention fractional dose is 6000-15000 dalton.
6. according to claim 1 a kind of from black sharkskin extraction collagen peptide, dermatan sulfate, hydroxyapatite and black
The technique of pigment, it is characterised in that in step (5), the resin is the resin that specificity adsorbs dermatan sulfate.
7. according to claim 1 a kind of from black sharkskin extraction collagen peptide, dermatan sulfate, hydroxyapatite and black
The technique of pigment, it is characterised in that in step (6), the temperature that is dried under reduced pressure is 65-80 DEG C.
8. according to claim 1 a kind of from black sharkskin extraction collagen peptide, dermatan sulfate, hydroxyapatite and black
The technique of pigment, it is characterised in that in step (8), a concentration of 0.1M of NaOH solution.
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| CN108794577A (en) * | 2018-06-26 | 2018-11-13 | 福州大学 | A kind of preparation method of antioxidation polypeptide |
| CN109078164B (en) * | 2018-08-22 | 2022-04-01 | 厦门肽王基因科技有限公司 | Application of shark skin mixed protein peptide of Astrocaryum platypomum as skeletal development promoter and microelement supplement |
| JP7095536B2 (en) * | 2018-10-01 | 2022-07-05 | ユーハ味覚糖株式会社 | Mucosal protection-related gene expression promoter and its uses |
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