CN110128530A - The technique for extracting collagen using sturgeon raw material - Google Patents
The technique for extracting collagen using sturgeon raw material Download PDFInfo
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- CN110128530A CN110128530A CN201910472055.5A CN201910472055A CN110128530A CN 110128530 A CN110128530 A CN 110128530A CN 201910472055 A CN201910472055 A CN 201910472055A CN 110128530 A CN110128530 A CN 110128530A
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- 102000008186 Collagen Human genes 0.000 title claims abstract description 43
- 108010035532 Collagen Proteins 0.000 title claims abstract description 43
- 241000881711 Acipenser sturio Species 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 37
- 229920001436 collagen Polymers 0.000 title claims abstract description 34
- 239000002994 raw material Substances 0.000 title claims abstract description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 57
- 239000000243 solution Substances 0.000 claims abstract description 36
- 239000000843 powder Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 19
- 239000004365 Protease Substances 0.000 claims abstract description 17
- 102000004190 Enzymes Human genes 0.000 claims abstract description 13
- 108090000790 Enzymes Proteins 0.000 claims abstract description 13
- 238000005238 degreasing Methods 0.000 claims abstract description 13
- 240000004808 Saccharomyces cerevisiae Species 0.000 claims abstract description 12
- 108091005804 Peptidases Proteins 0.000 claims abstract description 11
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 230000007071 enzymatic hydrolysis Effects 0.000 claims abstract description 8
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- 230000009849 deactivation Effects 0.000 claims abstract description 7
- 210000004712 air sac Anatomy 0.000 claims abstract description 6
- 238000005119 centrifugation Methods 0.000 claims abstract description 6
- 238000004042 decolorization Methods 0.000 claims abstract description 6
- 238000002604 ultrasonography Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 26
- 239000012528 membrane Substances 0.000 claims description 20
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 11
- 239000000919 ceramic Substances 0.000 claims description 11
- 229940088598 enzyme Drugs 0.000 claims description 11
- 238000001728 nano-filtration Methods 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 10
- 235000019419 proteases Nutrition 0.000 claims description 10
- 239000011780 sodium chloride Substances 0.000 claims description 8
- 108090000526 Papain Proteins 0.000 claims description 6
- 229940055729 papain Drugs 0.000 claims description 6
- 235000019834 papain Nutrition 0.000 claims description 6
- 229960000583 acetic acid Drugs 0.000 claims description 5
- 238000010612 desalination reaction Methods 0.000 claims description 5
- 239000012362 glacial acetic acid Substances 0.000 claims description 5
- 230000007062 hydrolysis Effects 0.000 claims description 5
- 238000006460 hydrolysis reaction Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 3
- 230000008961 swelling Effects 0.000 claims description 2
- 239000003610 charcoal Substances 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 claims 1
- 230000004206 stomach function Effects 0.000 claims 1
- 239000000047 product Substances 0.000 description 9
- 108090000765 processed proteins & peptides Proteins 0.000 description 8
- 241000251468 Actinopterygii Species 0.000 description 6
- 102000057297 Pepsin A Human genes 0.000 description 6
- 108090000284 Pepsin A Proteins 0.000 description 6
- 229940111202 pepsin Drugs 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000000605 extraction Methods 0.000 description 4
- 235000019750 Crude protein Nutrition 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000000284 extract Substances 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229920001184 polypeptide Polymers 0.000 description 3
- 102000004196 processed proteins & peptides Human genes 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 238000009360 aquaculture Methods 0.000 description 2
- 244000144974 aquaculture Species 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000855 fermentation Methods 0.000 description 2
- 230000004151 fermentation Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000000050 nutritive effect Effects 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 102000002322 Egg Proteins Human genes 0.000 description 1
- 108010000912 Egg Proteins Proteins 0.000 description 1
- 102000004317 Lyases Human genes 0.000 description 1
- 108090000856 Lyases Proteins 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 229960005188 collagen Drugs 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 210000004681 ovum Anatomy 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
- C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
- C07K14/78—Connective tissue peptides, e.g. collagen, elastin, laminin, fibronectin, vitronectin or cold insoluble globulin [CIG]
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P21/00—Preparation of peptides or proteins
- C12P21/06—Preparation of peptides or proteins produced by the hydrolysis of a peptide bond, e.g. hydrolysate products
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Zoology (AREA)
- Molecular Biology (AREA)
- Wood Science & Technology (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Medicinal Chemistry (AREA)
- Biophysics (AREA)
- Gastroenterology & Hepatology (AREA)
- Biotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
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- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
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Abstract
The invention discloses a kind of techniques for extracting collagen using sturgeon raw material, the following steps are included: 1) choosing clean sturgeon fish-skin and/or air bladder is raw material, then stripping and slicing is added in 5-10wt% sodium hydroxide solution and impregnates 5-10 hours, cleans material after filtering；2) the resulting material of step 1), which is added in degreasing mixed solution, carries out ungrease treatment, and ultrasound is carried out in treatment process, and the processing time is 1-2h, is cleaned up after the completion；3) the resulting material of step 2 is added in acid and is swollen, is then homogenized, after sodium hydroxide solution tune pH to 4.0-5.5, protease is added to be digested, yeast powder is added after the completion of enzymatic hydrolysis, temperature is controlled at 30-35 DEG C, carries out destroy the enzyme treatment after being stirred to react 2h；4) step 3) enzymolysis solution after enzyme deactivation carries out decolorization, and concentration is purified after centrifugation, finally spray-dried to obtain collagen protein powder.The present invention can rapidly extracting go out collagen, and collagen egg obtained purity is high, molecular weight is small, is easy to absorb.
Description
Technical field
The invention belongs to field of processing of aquatic products, are related to sturgeon product deep processing, and in particular to a kind of to utilize sturgeon
The technique of raw material extraction collagen.
Background technique
Sturgeon cultivation is the emerging industry in China, and certain status has been occupied in fish production.Along with China's agricultural
The paces of product restructuring and the juice of sturgeon cultivation, sturgeon cultivation industry have gradually occupied China's aquatic products and have supported
A critical role for growing industry, become a new growth point in China's freshwater aquaculture industry, fishery constitution adjustment and
One main direction of transferring fishermen's job, sturgeon cultivation industry rapidly develop.
National sturgeon yield increases sharply since 2000, and market capacity is limited, and the price of sturgeon marketable fish is caused to be held
It is continuous to reduce, aquaculture Benefit Drops.It is walked all the way by 600~700 yuan/kg at sturgeon cultivation initial stage the market price of sturgeon adult fish
Low, 30~50 yuan/kg till now, main cause is first is that since the market promotion much lags behind production；Second is that in industrial chain
A vital ring --- sturgeon process deeply industry develops slowly, and the fishery -ies product and deep processed product other than fresh and alive fish consumption exist
Type is rare, at high price in the market, and the consumer group is weak.
For sturgeon due to individual big, spur is few, is a kind of fish for being very suitable for processing after cultivation to certain specification.Sturgeon
Flesh of fish delicious, nutritive value are high, and the protein content of meat and ovum is up to 18% and 29%.In process, sturgeon fish-skin is with pair
The form of product generates, if cannot be used, will increase business burden.
Summary of the invention
The present invention provides it is a kind of using sturgeon raw material extract collagen technique, can rapidly extracting go out collagen egg
It is white, and collagen egg obtained purity is high, molecular weight are small.
The technical solution adopted by the present invention is that the technique for extracting collagen using sturgeon raw material, comprising the following steps:
1) choosing clean sturgeon fish-skin and/or air bladder is raw material, then stripping and slicing is added in 5-10wt% sodium hydroxide solution and soaks
Bubble 5-10 hours, cleans material after filtering；
2) the resulting material of step 1), which is added in degreasing mixed solution, carries out ungrease treatment, and ultrasound, processing are carried out in treatment process
Time is 1-2h, is cleaned up after the completion；
3) the resulting material of step 2 is added in acid and is swollen, is then homogenized, extremely with sodium hydroxide solution tune pH
After 4.0-5.5, protease is added and is digested, yeast powder is added after the completion of enzymatic hydrolysis, temperature is controlled at 30-35 DEG C, is stirred to react
Destroy the enzyme treatment is carried out after 2h；
4) step 3) enzymolysis solution after enzyme deactivation carries out decolorization, and concentration is purified after centrifugation, finally spray-dried to obtain collagen
Albumen powder.
Further, in step 1) when stripping and slicing, it is cut into the square block of long 5mm ~ 10mm.
Further, when being impregnated in step 1), sodium chloride solution is added in sodium hydroxide solution and is mixed, sodium chloride
Concentration be 5-10wt%, the solid-liquid ratio of sturgeon raw material and soaking solution is 1:10 g/mL.In preferred scheme, it can increase and stir
Mix step.
Further, the degreasant solution in step 2 is isopropanol, ethyl acetate and water by weight 0.5-2:1-2:10
Mixing, the solid-liquid ratio of raw material and degreasing mixed solution are 1:5 g/mL, in ultrasonication, supersonic frequency 32-40KHz,
Power is 300w.
Further, the acid in step 3) is glacial acetic acid, and concentration is 0.08 ~ 0.12mol/L, swelling time 5-8h.
Further, protease described in step 3) is papain and pepsin, and the additional amount of protease is
50-300U/mL, hydrolysis temperature are 28-35 DEG C, enzymolysis time 3-8h.
Further, in step 3) yeast powder additional amount be enzymolysis liquid quality 0.8-1.0%.
Further, it decolourizes constantly, active carbon to be added into enzymolysis liquid in step 4), additional amount is the 5wt% of enzymolysis liquid.
Further, it is first filtered using ceramic membrane when purifying concentration in step 4)；Desalination is carried out using nanofiltration membrane again
Concentration.
Further, wherein the aperture of ceramic membrane is 100-200nm, feed pressure 0.1-0.3MPa；Nanofiltration membrane it is saturating
Crossing molecular weight is 200D.
Protein is rich in sturgeon skin, crude protein accounts for 95% of butt or more, and crude protein accounts for 90% of butt or more in air bladder,
And collagen can account for 80% of crude protein or more in sturgeon fish-skin and air bladder, produce collagen using sturgeon fish-skin and air bladder,
Its content is high, and extraction efficiency is high, and efficient utilize for the by-product even leftover bits and pieces of sturgeon provides feasible processing approach, both
Sturgeon by-product processing channel is widened, sturgeon skin product category is enriched, moreover it is possible to make full use of its nutritive value, bringing for enterprise can
The economic benefit of sight.
The characteristics of the present invention is based on sturgeon raw materials first passes through the non-collagen foreign protein of aqueous slkali soaking removal raw material, then
Degreasing is carried out using organic solution, the lubricant component in raw material is removed, then carry out biological enzymolysis, technology is digested by compound bio
Raw material containing collagen is hydrolyzed to active collagen peptide, most obtains collagen protein powder through decoloration purifying spray drying afterwards.
The invention has the following advantages: the 1, present invention is impregnated in pretreatment using sodium hydroxide solution, it is former
Material is after base extraction, and the quantity of covalent bond is reduced in chain, and rigid structure weakens, and will lead to the reduction of viscosity, is easy to the later period
It extracts, and non-collagen can be removed, and sodium chloride is added simultaneously in sodium hydroxide solution, removal can be obviously shortened
Time, if individually impregnated with sodium hydroxide solution or sodium chloride solution, the time is needed more than for 24 hours, molten using the mixing of the two
Liquid is impregnated, and the time can be down to 5-10h.
2, when carrying out ungrease treatment, using isopropanol and ethyl acetate joint degreasing, while increasing ultrasonic treatment, have
Synergistic function, can be realized quick degreasing, and degreasing time can be controlled in 1-2h.It is handled using ultrasonic wave intervention, Neng Gou great
Width promotes degreasing efficiency and time, and does not influence the quality of collagen.
3, it in enzymolysis process, is digested using pepsin and papain, collagen passes through compound bio
Zymolysis technique is hydrolyzed to active small molecular polypeptide, by verifying, using pepsin and be dissolved in acid extract collagen it is more
Peptide is most effective, can improve yield to greatest extent；The present invention is by being directly added into yeast powder in the enzymatic hydrolysis later period, by fermentation process,
Can effectively remove fishy smell substance, and enzymatic hydrolysis is merged with fermentation process process, can simplification of flowsheet, an other side
Face, the fishy smell of aquatic products is mainly derived from fat oxidation and decomposes the various volatile small molecule substances generated, such as ketone, aldehyde, acids
Substance.This technique carries out defishying again after ungrease treatment, eliminates the source of fishy smell substance generation, fishy smell substance is avoided to exist
Generation again in production process, deodorization effect are good.
4, this technique is decolourized after enzyme deactivation using active carbon, while can also play the effect of absorption fishy smell substance,
After centrifugal treating, clear liquid is filtered with ceramic membrane, further removes the impurity in enzymolysis liquid, then be concentrated and take off by nanofiltration membrane
Salt, it is finally spray-dried to obtain collagen protein powder.
5, the molecular weight of collagen is generally between 100~300KD, using extraction process of the invention, through biology
Zymolysis technique and membrane filtration technique and combination will be further cut off after longer collagen peptide chain warp peracid lyase solution,
The collagen for forming low molecular weight can be such that the molecular weight of collagen polypeptide controls as far as possible in 3000D hereinafter, being easy to human body suction
It receives, after the film of special pore size distribution carries out separation concentration purification, obtains certain density active small molecular polypeptide slurries, most pass through afterwards
It crosses to dust and is dried to obtain collagen peptide high-purity molecular weight less than 3000D collagen active peptide white powder.
Specific embodiment
Embodiment 1:
The technique for extracting collagen using sturgeon raw material, comprising the following steps:
1) choosing clean sturgeon fish-skin is raw material, is cut into the square block of long 5mm ~ 10mm, and it is molten that 5wt% sodium hydroxide is then added
Impregnated 10 hours in liquid, the solid-liquid ratio of sturgeon raw material and solution is 1:10(g/mL), it is filtered after immersion and cleans material；
2) the resulting material of step 1), which is added in the solution that isopropanol is mixed with ethyl acetate and water by weight 1:2:10, carries out
The solid-liquid ratio of ungrease treatment, raw material and degreasing mixed solution is 1:5 (g/mL), carries out ultrasound in treatment process, supersonic frequency is
40KHz, power 300w, processing time are 2h, are cleaned up after the completion.
3) the resulting material of step 2 is added in glacial acetic acid and is swollen, be then homogenized, use sodium hydroxide solution
After adjusting pH to 4.0-5.5, papain and pepsin is added, the additional amount of protease is 60U/mL, hydrolysis temperature 28-
35 DEG C, enzymolysis time 8h, yeast powder is added in enzymatic hydrolysis after the completion, and the additional amount of yeast powder is the 1.0% of enzymolysis liquid quality, temperature
Control carries out destroy the enzyme treatment after being stirred to react 2h at 30-35 DEG C；
4) active carbon that enzymolysis liquid 5wt% is added in step 3) enzymolysis solution after enzyme deactivation carries out decolorization, and ceramic membrane is used after centrifugation
It is filtered, the aperture of ceramic membrane is 200nm, feed pressure 0.15MPa；Desalination and concentration, nanofiltration are carried out using nanofiltration membrane again
Film is 200D through molecular weight, finally spray-dried to obtain collagen protein powder.
By detecting and calculating, the collagen content in collagen protein powder has reached 97.9%, molecular weight 3000Da with
Under content account for 86.4%.
Embodiment 2:
The technique for extracting collagen using sturgeon raw material, comprising the following steps:
1) choosing clean sturgeon fish-skin is raw material, is cut into the square block of long 5mm ~ 10mm, and sodium hydroxide and chlorination is then added
Immersion 10h is carried out in the mixed solution of sodium, wherein the concentration of sodium chloride is 5wt%, and sodium hydroxide is also 5wt%, sturgeon raw material with
The solid-liquid ratio of solution is 1:10(g/mL), is stirred in soaking process, filters after the completion and cleans material；
2) the resulting material of step 1), which is added in the solution that isopropanol is mixed with ethyl acetate and water by weight 1:2:10, carries out
The solid-liquid ratio of ungrease treatment, raw material and degreasing mixed solution is 1:5 (g/mL), carries out ultrasound in treatment process, supersonic frequency is
40KHz, power 300w, processing time are 2h, are cleaned up after the completion.
3) the resulting material of step 2 is added in glacial acetic acid and is swollen, be then homogenized, use sodium hydroxide solution
After adjusting pH to 4.0-5.5, papain and pepsin is added, the additional amount of protease is 60U/mL, hydrolysis temperature 28-
35 DEG C, enzymolysis time 8h, yeast powder is added in enzymatic hydrolysis after the completion, and the additional amount of yeast powder is the 1.0% of enzymolysis liquid quality, temperature
Control carries out destroy the enzyme treatment after being stirred to react 2h at 30-35 DEG C；
4) active carbon that enzymolysis liquid 5wt% is added in step 3) enzymolysis solution after enzyme deactivation carries out decolorization, and ceramic membrane is used after centrifugation
It is filtered, the aperture of ceramic membrane is 200nm, feed pressure 0.15MPa；Desalination and concentration, nanofiltration are carried out using nanofiltration membrane again
Film is 200D through molecular weight, finally spray-dried to obtain collagen protein powder.
By detecting and calculating, the collagen content in collagen protein powder has reached 98.4%, molecular weight 3000Da with
Under content account for 89.5%.
Embodiment 3:
The technique for extracting collagen using sturgeon raw material, comprising the following steps:
1) choosing clean sturgeon fish-skin is raw material, is cut into the square block of long 5mm ~ 10mm, and sodium hydroxide and chlorination is then added
Immersion 5h is carried out in the mixed solution of sodium, wherein the concentration of sodium chloride is 10wt%, and sodium hydroxide is also 10wt%, sturgeon raw material with
The solid-liquid ratio of solution is 1:10(g/mL), is stirred in soaking process, filters after the completion and cleans material；
2) the resulting material of step 1) be added in the solution that isopropanol is mixed with ethyl acetate and water by weight 0.5:2:10 into
The solid-liquid ratio of row ungrease treatment, raw material and degreasing mixed solution is 1:5 (g/mL), carries out ultrasound, supersonic frequency in treatment process
For 32KHz, power 300w, the processing time is 2h, is cleaned up after the completion.
3) the resulting material of step 2 is added in glacial acetic acid and is swollen, be then homogenized, use sodium hydroxide solution
After adjusting pH to 4.0-5.5, papain and pepsin is added, the additional amount of protease is 300U/mL, and hydrolysis temperature is
28-35 DEG C, enzymolysis time 5h, yeast powder is added in enzymatic hydrolysis after the completion, and the additional amount of yeast powder is the 0.8% of enzymolysis liquid quality, temperature
Degree control carries out destroy the enzyme treatment after being stirred to react 2h at 30-35 DEG C；
4) active carbon that enzymolysis liquid 5wt% is added in step 3) enzymolysis solution after enzyme deactivation carries out decolorization, and ceramic membrane is used after centrifugation
It is filtered, the aperture of ceramic membrane is 200nm, feed pressure 0.2MPa；Desalination and concentration, nanofiltration membrane are carried out using nanofiltration membrane again
Be 200D through molecular weight, it is last spray-dried to obtain collagen protein powder.
By detecting and calculating, the collagen content in collagen protein powder has reached 97.9%, molecular weight 3000Da with
Under content account for 94.7%.
Claims (10)
1. the technique for extracting collagen using sturgeon raw material, which comprises the following steps:
1) choosing clean sturgeon fish-skin and/or air bladder is raw material, then stripping and slicing is added in 5-10wt% sodium hydroxide solution and soaks
Bubble 5-10 hours, cleans material after filtering；
2) the resulting material of step 1), which is added in degreasing mixed solution, carries out ungrease treatment, and ultrasound, processing are carried out in treatment process
Time is 1-2h, is cleaned up after the completion；
3) the resulting material of step 2 is added in acid and is swollen, is then homogenized, extremely with sodium hydroxide solution tune pH
After 4.0-5.5, protease is added and is digested, yeast powder is added after the completion of enzymatic hydrolysis, temperature is controlled at 30-35 DEG C, is stirred to react
Destroy the enzyme treatment is carried out after 2h；
4) step 3) enzymolysis solution after enzyme deactivation carries out decolorization, and concentration is purified after centrifugation, finally spray-dried to obtain collagen
Albumen powder.
2. technique according to claim 1, it is characterised in that: in step 1) when stripping and slicing, be cut into the square of long 5mm ~ 10mm
Shape.
3. technique according to claim 1, it is characterised in that: when being impregnated in step 1), be added in sodium hydroxide solution
Sodium chloride solution is mixed, and the concentration of sodium chloride is 5-10wt%, and the solid-liquid ratio of sturgeon raw material and soaking solution is 1:10 g/
mL。
4. technique according to claim 1, it is characterised in that: the degreasant solution in step 2 is isopropanol, ethyl acetate
It is mixed with water by weight 0.5-2:1-2:10, the solid-liquid ratio of raw material and degreasing mixed solution is 1:5 g/mL, is ultrasonically treated
Cheng Zhong, supersonic frequency 32-40KHz, power 300w.
5. technique according to claim 1, it is characterised in that: acid in step 3) is glacial acetic acid, concentration is 0.08 ~
0.12mol/L, swelling time 5-8h.
6. technique according to claim 1, it is characterised in that: protease described in step 3) is papain stomach function regulating
Protease, the additional amount of protease are 50-300U/mL, and hydrolysis temperature is 28-35 DEG C, enzymolysis time 3-8h.
7. technique according to claim 1, it is characterised in that: the additional amount of yeast powder is enzymolysis liquid quality in step 3)
0.8-1.0%。
8. technique according to claim 1, it is characterised in that: decolourize in step 4) constantly, activity is added into enzymolysis liquid
Charcoal, additional amount are the 5wt% of enzymolysis liquid.
9. technique according to claim 1, it is characterised in that: first use ceramic membrane to carry out when purifying concentration in step 4)
Filter；Desalination and concentration is carried out using nanofiltration membrane again.
10. technique according to claim 9, it is characterised in that: wherein the aperture of ceramic membrane is 100-200nm, charging pressure
Power is 0.1-0.3MPa；Nanofiltration membrane is 200D through molecular weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910472055.5A CN110128530A (en) | 2019-05-31 | 2019-05-31 | The technique for extracting collagen using sturgeon raw material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910472055.5A CN110128530A (en) | 2019-05-31 | 2019-05-31 | The technique for extracting collagen using sturgeon raw material |
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| CN110128530A true CN110128530A (en) | 2019-08-16 |
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Cited By (4)
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| CN110577975A (en) * | 2019-09-24 | 2019-12-17 | 福州海锐黎思生物科技有限责任公司 | Method for extracting and preparing swimming bladder collagen oligopeptide |
| CN111803434A (en) * | 2020-07-27 | 2020-10-23 | 烟台鲟臻生物科技有限公司 | Preparation method of sturgeon caviar extract |
| CN113136330A (en) * | 2021-05-15 | 2021-07-20 | 德州蓝力生物技术有限公司 | Production and treatment device and process of cod skin collagen peptide |
| WO2022217490A1 (en) * | 2021-04-14 | 2022-10-20 | 海南三元星生物科技股份有限公司 | Method for preparing collagen peptide |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110577975A (en) * | 2019-09-24 | 2019-12-17 | 福州海锐黎思生物科技有限责任公司 | Method for extracting and preparing swimming bladder collagen oligopeptide |
| CN111803434A (en) * | 2020-07-27 | 2020-10-23 | 烟台鲟臻生物科技有限公司 | Preparation method of sturgeon caviar extract |
| WO2022217490A1 (en) * | 2021-04-14 | 2022-10-20 | 海南三元星生物科技股份有限公司 | Method for preparing collagen peptide |
| CN113136330A (en) * | 2021-05-15 | 2021-07-20 | 德州蓝力生物技术有限公司 | Production and treatment device and process of cod skin collagen peptide |
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