CN105063154A - Method for extracting collagen from fish scales - Google Patents
Method for extracting collagen from fish scales Download PDFInfo
- Publication number
- CN105063154A CN105063154A CN201510603711.2A CN201510603711A CN105063154A CN 105063154 A CN105063154 A CN 105063154A CN 201510603711 A CN201510603711 A CN 201510603711A CN 105063154 A CN105063154 A CN 105063154A
- Authority
- CN
- China
- Prior art keywords
- fish scale
- enzymolysis
- slurries
- temperature
- enzymatic vessel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Peptides Or Proteins (AREA)
Abstract
The invention discloses a method for extracting collagen from fish scales, which comprises the following steps: fish scale pretreatment: cleaning, acid treatment, alkali treatment, grinding, cooking and cooling; irradiation treatment; enzymolysis: primary enzymolysis and secondary enzymolysis; activated carbon adsorption; filtration; concentration; sterilization; and spray drying. The production technique is simple, and the enzymolysis tank and filter plant are combined and matched so as to perform activated carbon filtration in the enzymolysis tank, thereby implementing the decolorization and fishy smell removal effects, enhancing the production efficiency and lowering the production cost. The membrane is adopted for filtration and concentration, so the method has the advantages of low energy consumption and high efficiency. The method has the characteristics of low requirements for the production environment, small damage to collagen and various amino acids, low environmental pollution and high operational safety. The whole production process does not need to use abundant acids, alkalis or other chemical raw materials. The production cycle is short, and the process from raw material pretreatment to finished product preparation only needs 20 hours or so. The final product has the advantages of high earning rate and high quality.
Description
Technical field
The present invention relates to the technology of preparing of collagen protein, specifically a kind of method extracting collagen protein from fish scale.
Background technology
Collagen protein is the protein that people's in-vivo content is maximum, distribution is the widest, and be the major protein components of reticular tissue, account for 25% of body total protein, it is mainly distributed in the skin of animal, bone, cartilage, cornea, in the tissue such as blood vessel.The collagen protein extracted in the reticular tissue of animal, because having special protein structure and health affinity, is widely used in food, and makeup wait the industry relevant to HUMAN HEALTH with medical treatment.
Livestock and poultry source animal tissues is the main path that people obtain natural collagen protein and collagen peptide thereof always, but due to the generation of the diseases such as mad cow disease (BSE), foot and mouth disease (FMD), bird flu, make the security of people to Lu Sheng mammalian collagen and goods thereof create query, the collagen protein deriving from livestock is in addition restricted in the application in the areas such as faith Islam.Progressively turning in marine organisms and developing collagen protein.In addition due to the difference of the aspects such as amino acid composition and degree of crosslinking, make aquatic animal especially its processing waste-Pi, bone, abundant collagen protein contained in squama has the unexistent advantage of a lot of livestock collagen proteins, as certain gelation, the dispersiveness of height, low viscosity, water-absorbent, retentiveness and emulsifying property etc., it is found that the collagen protein deriving from marine animal is obviously better than the collagen protein of terrestrial animal in some respects in addition, such as there is low antigenicity, hypoallergenic, denaturation temperature is low, solubility is high, easily by characteristics such as protease hydrolysiss.Therefore aquatic collagen protein progressively may substitute terrestrial animal collagen protein.
At present, the research of extracting collagen protein from fish scale is very many, and preparation technology comprises the steps such as the pre-treatment (comprising degreasing, deliming etc.) of fish scale, enzymolysis, the enzyme that goes out, decolouring, filtration, concentrated, degerming and spraying dry.Wherein, in the degreasing deliming of fish scale, the main strong acid and strong base that adopts processes at present, although strong acid and strong base degreasing deliming effect is very good, but strong acid and strong base not only causes environmental pollution, but also cause the heavy-metal residual of collagen product, seriously constrain the development of collagen protein.In the enzymolysis process of fish scale, the main method adopting long-time heating pressurization to boil glue and long-time enzymolysis solves the problem of fish scale enzymolysis at present, but glue is boiled in long-time heating pressurization and long-time enzymolysis can not solve the incomplete problem of fish scale enzymolysis completely, cause the problems such as wastage of material, energy consumption is high, extraction yield is low, affect the development of collagen protein.
Summary of the invention
The object of the present invention is to provide a kind of method extracting collagen protein from fish scale, there is the feature of low cost, less energy-consumption, high extraction, high-quality.
For achieving the above object, the invention provides following technical scheme:
From fish scale, extract a method for collagen protein, comprise the following steps:
(1) fish scale pre-treatment, comprises the following steps:
11) clean: cleaning fish scale, impurities removing, drains away the water;
12) acid treatment: add the sodium citrate solution that mass percent concentration is 5-6% in fish scale, makes the mass body volume concentrations of fish scale and sodium citrate solution be 350-420kg/m
3, at 20-25 DEG C of temperature, utilize the ultrasonication 2-3h that power is 120-240W, elimination sodium citrate solution, with pure water cleaning fish scale to neutral;
13) alkaline purification: add the lime aqueous solution that mass percent concentration is 2.5-3.5% in fish scale, makes the mass body volume concentrations of fish scale and lime aqueous solution be 350-420kg/m
3, at 20-25 DEG C of temperature, leave standstill and soak 10-14h, elimination lime aqueous solution, with pure water cleaning fish scale to neutral, drain away the water;
14) grind: get step 13) drain after fish scale, add pure water, make the mass body volume concentrations of fish scale and pure water be 350-420kg/m
3, wear into fish scale slurries with colloidal mill;
15) boiling: fish scale slurries are warming up to 100 DEG C, insulation 30-40min;
16) cool: after the fish scale slurries after boiling naturally cool to 55-60 DEG C, fish scale slurries are moved in enzymatic vessel;
(2) fish scale slurries are loaded sealing bag sealing, are laid in horizontal plane by radiation treatment, and adopt electron beam to carry out radiation treatment, irradiation dose is 50-150kGy, irradiation time 60-150s;
(3) enzymolysis, comprises primary enzymolysis and secondary enzymolysis;
31) primary enzymolysis: the pH value of the fish scale slurries in adjustment enzymatic vessel is to 6.0-6.7, add the papoid of the 0.6-0.7% of fish scale slurries quality, the enzyme activity of papoid is 220-300u/g, and in adjustment enzymatic vessel, temperature is to 58-60 DEG C, enzymolysis 1.5-2.5h;
32) secondary enzymolysis: in adjustment enzymatic vessel, liquid pH value is to 7.5-8.0, and add the trypsinase of the 0.4-0.6% of fish scale slurries quality, tryptic enzyme activity is 2800-3500u/g, in adjustment enzymatic vessel, temperature is to 56-58 DEG C, enzymolysis 1.5-2.5h;
(4) charcoal absorption: the active carbon powder adding the 0.8-1.2% of fish scale slurries quality in enzymatic vessel, in adjustment enzymatic vessel, temperature is to 56-58 DEG C, insulation 45-50min;
(5) filter: after fish scale slurries Filter Press in enzymatic vessel, then bag type filtering; Pressure filter adopts aperture to be 350-400 object barrier film; Bag type filtering adopts aperture to be 1-5 μm of millipore filtration;
(6) concentrated: filtrate is first that the micro-filtrate membrane filtration of 0.3-0.5 μm becomes micro-filtrate through aperture, is then that the ultrafiltration membrance filter of 0.01-0.02 μm becomes ultrafiltrated through aperture, be then that the nanofiltration membrane of 1-2nm concentrates through aperture, obtain nanofiltration liquid;
(7) sterilizing: nanofiltration liquid is sterilizing 8-10s at temperature 121-130 DEG C, then discharging when temperature is cooled to 45-55 DEG C;
(8) spraying dry: make it refine powdered by spraying in spray drying unit the nanofiltration liquid after sterilizing, obtain finished product.
As the further scheme of the present invention: described step 12) in, the compound method of citric acid solution is as follows: first according to disodium ethylene diamine tetraacetate: the mass ratio of citric acid is the ratio of 6-8:100, after taking disodium ethylene diamine tetraacetate and citric acid mixing, add pure water again, be mixed with the sodium citrate solution that mass percent concentration is 5-6%.
As the further scheme of the present invention: in described step (2), the operating parameter of electron beam is: beam energy 8-10MeV, power 9-12kW, frequency 300-360Hz.
As the further scheme of the present invention: described step (6) also comprises, do not transfer in enzymatic vessel by the ultra-filter retentate of ultra-filtration membrane by what obtain after ultrafiltration membrance filter, repeating step (3)-step (6), obtains nanofiltration liquid.
As the further scheme of the present invention: in described step (8), the Mono pump input speed of spray drying unit is 0.8-1.2kg/min, and inlet temperature is 160-178 DEG C, and air outlet temperature is 80-85 DEG C.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention adopts citric acid treatment and the ultrasonic wave technique that combines to carry out deliming to fish scale, lime aqueous solution is adopted to carry out degreasing to fish scale, avoid environmental pollution and heavy-metal residual problem that strong acid and strong base degreasing deliming causes, safety is natural more to make the collagen product for preparing.
After the present invention adopts milling treatment of colloid and digesting technoloy to obtain the fish scale slurries of preliminary exposition, then by after electron beam irradiation process, enzymolysis time can be shortened, improve degree of hydrolysis, enhance productivity, there is extraction yield high, relative molecular weight is little, purity is high, low cost of manufacture, the advantage of non-secondary pollution.
After electron beam irradiation process, use aspartic protease, Sumizyme MP enzymolysis fish scale slurries more successively, the area that fish scale slurries are contacted with proteolytic enzyme is larger, enzymolysis more rapidly, more complete, make protein macromolecule thoroughly be hydrolyzed into small molecules, improve the extraction yield of collagen protein.The terminal peptide splitting of chain in tropocollagen molecule gentle directionally can be made in production process of the present invention, collagen macromole is made to be hydrolyzed into micromolecular collagen peptide, the molecular-weight average of obtained collagen protein is less than 1300 dalton, and the molecular weight distribution of gained collagen protein is concentrated, more than 89% within 2000 dalton, more than 50% between 200-1300 dalton, collagen protein extraction yield reaches more than 95%, collagen content reaches more than 98%, human body more easily absorbs, and the functional zone be hidden in collagen protein can be discharged, dissociate and to have the bioactive peptide of various physiological function.
Production technique of the present invention is simple, enzymatic vessel and filtering device combinations is supported the use, can carry out activated carbon filtration, realize the effect of decoloration deodorization, both improve production efficiency, again reduce production cost in enzymatic vessel; Employing membrane filtration concentrates, and energy consumption is low, and efficiency is high; Less demanding to production environment, to collagen protein and various amino acid whose destructiveness little; Environmental pollution is little, operational safety; In whole production process, without the need to using the chemical feedstockss such as a large amount of bronsted lowry acids and bases bronsted lowries.Of the present invention with short production cycle, only need about 20h from the pre-treatment of raw material to final finished.The earning rate of the finished product is high, and quality is high.
Embodiment
Below in conjunction with the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1 (most preferred embodiment)
In the embodiment of the present invention, a kind of method extracting collagen protein from fish scale, comprises the following steps:
(1) fish scale pre-treatment, comprises the following steps:
11) clean: cleaning fish scale, impurities removing, drains away the water;
12) acid treatment: add the sodium citrate solution that mass percent concentration is 5.6% in fish scale, makes the mass body volume concentrations of fish scale and sodium citrate solution be 400kg/m
3, at 22 DEG C of temperature, utilize the ultrasonication 2.5h that power is 200W, elimination sodium citrate solution, with pure water cleaning fish scale to neutral; Wherein, the compound method of citric acid solution is as follows: first according to disodium ethylene diamine tetraacetate: the mass ratio of citric acid is the ratio of 7:100, after taking disodium ethylene diamine tetraacetate and citric acid mixing, then add pure water, be mixed with the sodium citrate solution that mass percent concentration is 5.6%;
13) alkaline purification: add the lime aqueous solution that mass percent concentration is 3% in fish scale, makes the mass body volume concentrations of fish scale and lime aqueous solution be 400kg/m
3, at 22 DEG C of temperature, leave standstill and soak 12h, elimination lime aqueous solution, with pure water cleaning fish scale to neutral, drain away the water;
14) grind: get step 13) drain after fish scale, add pure water, make the mass body volume concentrations of fish scale and pure water be 400kg/m
3, wear into fish scale slurries with colloidal mill;
15) boiling: fish scale slurries are warming up to 100 DEG C, insulation 35min;
16) cool: after the fish scale slurries after boiling naturally cool to 58 DEG C, fish scale slurries are moved in enzymatic vessel;
(2) fish scale slurries are loaded sealing bag sealing, are laid in horizontal plane by radiation treatment, and adopt electron beam to carry out radiation treatment, irradiation dose is 100kGy, irradiation time 90s; Wherein, the operating parameter of electron beam is: beam energy 9MeV, power 10kW, frequency 320Hz;
(3) enzymolysis, comprises primary enzymolysis and secondary enzymolysis;
31) primary enzymolysis: the pH value to 6.3 of the fish scale slurries in adjustment enzymatic vessel, add the papoid of 0.65% of fish scale slurries quality, the enzyme activity of papoid is 250u/g, temperature to 59 DEG C in adjustment enzymatic vessel, enzymolysis 2h;
32) secondary enzymolysis: liquid pH value to 7.8 in adjustment enzymatic vessel, add the trypsinase of 0.5% of fish scale slurries quality, tryptic enzyme activity is 3000u/g, temperature to 57 DEG C in adjustment enzymatic vessel, enzymolysis 2h;
(4) charcoal absorption: the active carbon powder adding 1% of fish scale slurries quality in enzymatic vessel, temperature to 57 DEG C in adjustment enzymatic vessel, insulation 48min;
(5) filter: after fish scale slurries Filter Press in enzymatic vessel, then bag type filtering; Pressure filter adopts aperture to be 380 object barrier films; Bag type filtering adopts aperture to be 2 μm of millipore filtrations;
(6) concentrated: filtrate is first that the micro-filtrate membrane filtration of 0.4 μm becomes micro-filtrate through aperture, is then that the ultrafiltration membrance filter of 0.015 μm becomes ultrafiltrated through aperture, be then that the nanofiltration membrane of 1.5nm concentrates through aperture, obtain nanofiltration liquid; Do not transfer in enzymatic vessel by the ultra-filter retentate of ultra-filtration membrane by what obtain after ultrafiltration membrance filter, repeating step (3)-step (6), obtains nanofiltration liquid.
(7) sterilizing: nanofiltration liquid is sterilizing 9s at temperature 125 DEG C, then discharging when temperature is cooled to 50 DEG C;
(8) spraying dry: make it refine powdered by spraying in spray drying unit the nanofiltration liquid after sterilizing, obtain finished product; The Mono pump input speed of spray drying unit is 1kg/min, and inlet temperature is 170 DEG C, and air outlet temperature is 82 DEG C.
Embodiment 2
In the embodiment of the present invention, a kind of method extracting collagen protein from fish scale, comprises the following steps:
(1) fish scale pre-treatment, comprises the following steps:
11) clean: cleaning fish scale, impurities removing, drains away the water;
12) acid treatment: add the sodium citrate solution that mass percent concentration is 5% in fish scale, makes the mass body volume concentrations of fish scale and sodium citrate solution be 420kg/m
3, at 20 DEG C of temperature, utilize the ultrasonication 2h that power is 240W, elimination sodium citrate solution, with pure water cleaning fish scale to neutral; Wherein, the compound method of citric acid solution is as follows: first according to disodium ethylene diamine tetraacetate: the mass ratio of citric acid is the ratio of 6:100, after taking disodium ethylene diamine tetraacetate and citric acid mixing, then add pure water, be mixed with the sodium citrate solution that mass percent concentration is 5%;
13) alkaline purification: add the lime aqueous solution that mass percent concentration is 2.5% in fish scale, makes the mass body volume concentrations of fish scale and lime aqueous solution be 420kg/m
3, at 20 DEG C of temperature, leave standstill and soak 14h, elimination lime aqueous solution, with pure water cleaning fish scale to neutral, drain away the water;
14) grind: get step 13) drain after fish scale, add pure water, make the mass body volume concentrations of fish scale and pure water be 420kg/m
3, wear into fish scale slurries with colloidal mill;
15) boiling: fish scale slurries are warming up to 100 DEG C, insulation 30min;
16) cool: after the fish scale slurries after boiling naturally cool to 55 DEG C, fish scale slurries are moved in enzymatic vessel;
(2) fish scale slurries are loaded sealing bag sealing, are laid in horizontal plane by radiation treatment, and adopt electron beam to carry out radiation treatment, irradiation dose is 50kGy, irradiation time 150s; Wherein, the operating parameter of electron beam is: beam energy 8MeV, power 12kW, frequency 300Hz;
(3) enzymolysis, comprises primary enzymolysis and secondary enzymolysis;
31) primary enzymolysis: the pH value to 6.0 of the fish scale slurries in adjustment enzymatic vessel, add the papoid of 0.6% of fish scale slurries quality, the enzyme activity of papoid is 220u/g, temperature to 58 DEG C in adjustment enzymatic vessel, enzymolysis 1.5h;
32) secondary enzymolysis: liquid pH value to 7.5 in adjustment enzymatic vessel, add the trypsinase of 0.4% of fish scale slurries quality, tryptic enzyme activity is 2800u/g, temperature to 56 DEG C in adjustment enzymatic vessel, enzymolysis 1.5h;
(4) charcoal absorption: the active carbon powder adding 0.8% of fish scale slurries quality in enzymatic vessel, temperature to 56 DEG C in adjustment enzymatic vessel, insulation 45min;
(5) filter: after fish scale slurries Filter Press in enzymatic vessel, then bag type filtering; Pressure filter adopts aperture to be 350 object barrier films; Bag type filtering adopts aperture to be 1 μm of millipore filtration;
(6) concentrated: filtrate is first that the micro-filtrate membrane filtration of 0.3 μm becomes micro-filtrate through aperture, is then that the ultrafiltration membrance filter of 0.01 μm becomes ultrafiltrated through aperture, be then that the nanofiltration membrane of 1nm concentrates through aperture, obtain nanofiltration liquid; Do not transfer in enzymatic vessel by the ultra-filter retentate of ultra-filtration membrane by what obtain after ultrafiltration membrance filter, repeating step (3)-step (6), obtains nanofiltration liquid.
(7) sterilizing: nanofiltration liquid is sterilizing 10s at temperature 121 DEG C, then discharging when temperature is cooled to 45 DEG C;
(8) spraying dry: make it refine powdered by spraying in spray drying unit the nanofiltration liquid after sterilizing, obtain finished product; The Mono pump input speed of spray drying unit is 0.8kg/min, and inlet temperature is 160 DEG C, and air outlet temperature is 80 DEG C.
Embodiment 3
In the embodiment of the present invention, a kind of method extracting collagen protein from fish scale, comprises the following steps:
(1) fish scale pre-treatment, comprises the following steps:
11) clean: cleaning fish scale, impurities removing, drains away the water;
12) acid treatment: add the sodium citrate solution that mass percent concentration is 6% in fish scale, makes the mass body volume concentrations of fish scale and sodium citrate solution be 350kg/m
3, at 25 DEG C of temperature, utilize the ultrasonication 3h that power is 120W, elimination sodium citrate solution, with pure water cleaning fish scale to neutral; Wherein, the compound method of citric acid solution is as follows: first according to disodium ethylene diamine tetraacetate: the mass ratio of citric acid is the ratio of 8:100, after taking disodium ethylene diamine tetraacetate and citric acid mixing, then add pure water, be mixed with the sodium citrate solution that mass percent concentration is 6%;
13) alkaline purification: add the lime aqueous solution that mass percent concentration is 3.5% in fish scale, makes the mass body volume concentrations of fish scale and lime aqueous solution be 350kg/m
3, at 25 DEG C of temperature, leave standstill and soak 10h, elimination lime aqueous solution, with pure water cleaning fish scale to neutral, drain away the water;
14) grind: get step 13) drain after fish scale, add pure water, make the mass body volume concentrations of fish scale and pure water be 350kg/m
3, wear into fish scale slurries with colloidal mill;
15) boiling: fish scale slurries are warming up to 100 DEG C, insulation 40min;
16) cool: after the fish scale slurries after boiling naturally cool to 60 DEG C, fish scale slurries are moved in enzymatic vessel;
(2) fish scale slurries are loaded sealing bag sealing, are laid in horizontal plane by radiation treatment, and adopt electron beam to carry out radiation treatment, irradiation dose is 150kGy, irradiation time 60s; Wherein, the operating parameter of electron beam is: beam energy 10MeV, power 12kW, frequency 360Hz;
(3) enzymolysis, comprises primary enzymolysis and secondary enzymolysis;
31) primary enzymolysis: the pH value to 6.7 of the fish scale slurries in adjustment enzymatic vessel, add the papoid of 0.7% of fish scale slurries quality, the enzyme activity of papoid is 300u/g, temperature to 60 DEG C in adjustment enzymatic vessel, enzymolysis 2.5h;
32) secondary enzymolysis: liquid pH value to 8.0 in adjustment enzymatic vessel, add the trypsinase of 0.6% of fish scale slurries quality, tryptic enzyme activity is 3500u/g, temperature to 58 DEG C in adjustment enzymatic vessel, enzymolysis 2.5h;
(4) charcoal absorption: the active carbon powder adding 1.2% of fish scale slurries quality in enzymatic vessel, temperature to 58 DEG C in adjustment enzymatic vessel, insulation 50min;
(5) filter: after fish scale slurries Filter Press in enzymatic vessel, then bag type filtering; Pressure filter adopts aperture to be 400 object barrier films; Bag type filtering adopts aperture to be 5 μm of millipore filtrations;
(6) concentrated: filtrate is first that the micro-filtrate membrane filtration of 0.5 μm becomes micro-filtrate through aperture, is then that the ultrafiltration membrance filter of 0.02 μm becomes ultrafiltrated through aperture, be then that the nanofiltration membrane of 2nm concentrates through aperture, obtain nanofiltration liquid; Do not transfer in enzymatic vessel by the ultra-filter retentate of ultra-filtration membrane by what obtain after ultrafiltration membrance filter, repeating step (3)-step (6), obtains nanofiltration liquid.
(7) sterilizing: nanofiltration liquid is sterilizing 8s at temperature 130 DEG C, then discharging when temperature is cooled to 55 DEG C;
(8) spraying dry: make it refine powdered by spraying in spray drying unit the nanofiltration liquid after sterilizing, obtain finished product; The Mono pump input speed of spray drying unit is 1.2kg/min, and inlet temperature is 178 DEG C, and air outlet temperature is 85 DEG C.
The index of the collagen product that foregoing invention embodiment obtains is as shown in table 1 below:
The index of the collagen product obtained by table 1 embodiment 1-3
As can be seen from the above table, it is 89.57-96.4% that the molecular weight of the collagen protein that the present invention obtains is less than 2000 daltonian peak area percent, wherein the daltonian peak area percent of 1300-200 is 53.75-73.37%, illustrate dipeptides that human body the most easily absorbs, tripeptides accounting and more than 50%.Collagen protein is white simultaneously, and without fishy smell.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (5)
1. from fish scale, extract a method for collagen protein, it is characterized in that, comprise the following steps:
(1) fish scale pre-treatment, comprises the following steps:
11) clean: cleaning fish scale, impurities removing, drains away the water;
12) acid treatment: add the sodium citrate solution that mass percent concentration is 5-6% in fish scale, makes the mass body volume concentrations of fish scale and sodium citrate solution be 350-420kg/m
3, at 20-25 DEG C of temperature, utilize the ultrasonication 2-3h that power is 120-240W, elimination sodium citrate solution, with pure water cleaning fish scale to neutral;
13) alkaline purification: add the lime aqueous solution that mass percent concentration is 2.5-3.5% in fish scale, makes the mass body volume concentrations of fish scale and lime aqueous solution be 350-420kg/m
3, at 20-25 DEG C of temperature, leave standstill and soak 10-14h, elimination lime aqueous solution, with pure water cleaning fish scale to neutral, drain away the water;
14) grind: get step 13) drain after fish scale, add pure water, make the mass body volume concentrations of fish scale and pure water be 350-420kg/m
3, wear into fish scale slurries with colloidal mill;
15) boiling: fish scale slurries are warming up to 100 DEG C, insulation 30-40min;
16) cool: after the fish scale slurries after boiling naturally cool to 55-60 DEG C, fish scale slurries are moved in enzymatic vessel;
(2) fish scale slurries are loaded sealing bag sealing, are laid in horizontal plane by radiation treatment, and adopt electron beam to carry out radiation treatment, irradiation dose is 50-150kGy, irradiation time 60-150s;
(3) enzymolysis, comprises primary enzymolysis and secondary enzymolysis;
31) primary enzymolysis: the pH value of the fish scale slurries in adjustment enzymatic vessel is to 6.0-6.7, add the papoid of the 0.6-0.7% of fish scale slurries quality, the enzyme activity of papoid is 220-300u/g, and in adjustment enzymatic vessel, temperature is to 58-60 DEG C, enzymolysis 1.5-2.5h;
32) secondary enzymolysis: in adjustment enzymatic vessel, liquid pH value is to 7.5-8.0, and add the trypsinase of the 0.4-0.6% of fish scale slurries quality, tryptic enzyme activity is 2800-3500u/g, in adjustment enzymatic vessel, temperature is to 56-58 DEG C, enzymolysis 1.5-2.5h;
(4) charcoal absorption: the active carbon powder adding the 0.8-1.2% of fish scale slurries quality in enzymatic vessel, in adjustment enzymatic vessel, temperature is to 56-58 DEG C, insulation 45-50min;
(5) filter: after fish scale slurries Filter Press in enzymatic vessel, then bag type filtering; Pressure filter adopts aperture to be 350-400 object barrier film; Bag type filtering adopts aperture to be 1-5 μm of millipore filtration;
(6) concentrated: filtrate is first that the micro-filtrate membrane filtration of 0.3-0.5 μm becomes micro-filtrate through aperture, is then that the ultrafiltration membrance filter of 0.01-0.02 μm becomes ultrafiltrated through aperture, be then that the nanofiltration membrane of 1-2nm concentrates through aperture, obtain nanofiltration liquid;
(7) sterilizing: nanofiltration liquid is sterilizing 8-10s at temperature 121-130 DEG C, then discharging when temperature is cooled to 45-55 DEG C;
(8) spraying dry: make it refine powdered by spraying in spray drying unit the nanofiltration liquid after sterilizing, obtain finished product.
2. the method extracting collagen protein from fish scale according to claim 1, it is characterized in that, in described step 12), the compound method of citric acid solution is as follows: first according to disodium ethylene diamine tetraacetate: the mass ratio of citric acid is the ratio of 6-8:100, after taking disodium ethylene diamine tetraacetate and citric acid mixing, add pure water again, be mixed with the sodium citrate solution that mass percent concentration is 5-6%.
3. the method extracting collagen protein from fish scale according to claim 1, is characterized in that, in described step (2), the operating parameter of electron beam is: beam energy 8-10MeV, power 9-12kW, frequency 300-360Hz.
4. the method extracting collagen protein from fish scale according to claim 1, it is characterized in that, described step (6) also comprises, and does not transfer in enzymatic vessel by the ultra-filter retentate of ultra-filtration membrane by what obtain after ultrafiltration membrance filter, repeating step (3)-step (6), obtains nanofiltration liquid.
5. the method extracting collagen protein from fish scale according to claim 1, is characterized in that, in described step (8), the Mono pump input speed of spray drying unit is 0.8-1.2kg/min, and inlet temperature is 160-178 DEG C, and air outlet temperature is 80-85 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510603711.2A CN105063154A (en) | 2015-09-21 | 2015-09-21 | Method for extracting collagen from fish scales |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510603711.2A CN105063154A (en) | 2015-09-21 | 2015-09-21 | Method for extracting collagen from fish scales |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105063154A true CN105063154A (en) | 2015-11-18 |
Family
ID=54492660
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510603711.2A Pending CN105063154A (en) | 2015-09-21 | 2015-09-21 | Method for extracting collagen from fish scales |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105063154A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106119330A (en) * | 2016-08-09 | 2016-11-16 | 中国计量大学 | A kind of preparation method of fish scale collagen range of hydrolysed peptides |
| CN106262940A (en) * | 2016-08-09 | 2017-01-04 | 福建农林大学 | A kind of gel embedding Hippocampus polypeptide microcapsule and preparation method thereof |
| CN109180808A (en) * | 2018-09-30 | 2019-01-11 | 青岛蓝色康典海洋生物科技有限公司 | A kind of fish scale collagen and its preparation method and application |
| CN109608540A (en) * | 2019-01-29 | 2019-04-12 | 广州华大生物科技有限公司 | A method of extracting collagen from fish scale |
| CN109628302A (en) * | 2018-12-28 | 2019-04-16 | 宁夏红山河食品股份有限公司 | A kind of meat products subsection enzymolysis device and enzyme solution |
| CN109880734A (en) * | 2019-03-30 | 2019-06-14 | 中国水产科学研究院黑龙江水产研究所 | Amino acid extraction element machine extracting method in a kind of flesh of fish |
| CN109897101A (en) * | 2019-03-14 | 2019-06-18 | 卓康(福建)生物科技有限公司 | A kind of collagen tripeptide and its production method and application |
| CN110074356A (en) * | 2019-06-04 | 2019-08-02 | 江南大学 | A kind of Java tilapia skin deliming degreasing method |
| CN113480637A (en) * | 2021-08-05 | 2021-10-08 | 广西南宁佰奥吉生物科技有限公司 | Preparation method of non-denatured type II collagen |
| CN115176896A (en) * | 2022-08-08 | 2022-10-14 | 标优美生态工程镇江有限公司 | Hydrolyzed fish protein pet feed and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103540635A (en) * | 2013-09-23 | 2014-01-29 | 石狮海星食品有限公司 | Preparation process of fish scale collagen protein |
| CN103773830A (en) * | 2014-01-21 | 2014-05-07 | 曾佳 | Method for extracting collagen from fish scales |
| CN104313102A (en) * | 2014-11-06 | 2015-01-28 | 伍曾利 | Method of preparing collagen |
| CN104726527A (en) * | 2015-03-24 | 2015-06-24 | 宁德市夏威食品有限公司 | Preparation technology for producing collagen through enzymolysis of fish scales |
-
2015
- 2015-09-21 CN CN201510603711.2A patent/CN105063154A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103540635A (en) * | 2013-09-23 | 2014-01-29 | 石狮海星食品有限公司 | Preparation process of fish scale collagen protein |
| CN103773830A (en) * | 2014-01-21 | 2014-05-07 | 曾佳 | Method for extracting collagen from fish scales |
| CN104313102A (en) * | 2014-11-06 | 2015-01-28 | 伍曾利 | Method of preparing collagen |
| CN104726527A (en) * | 2015-03-24 | 2015-06-24 | 宁德市夏威食品有限公司 | Preparation technology for producing collagen through enzymolysis of fish scales |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106262940B (en) * | 2016-08-09 | 2019-08-13 | 福建农林大学 | A kind of gel embedding hippocampus polypeptide microcapsule and preparation method thereof |
| CN106262940A (en) * | 2016-08-09 | 2017-01-04 | 福建农林大学 | A kind of gel embedding Hippocampus polypeptide microcapsule and preparation method thereof |
| CN106119330A (en) * | 2016-08-09 | 2016-11-16 | 中国计量大学 | A kind of preparation method of fish scale collagen range of hydrolysed peptides |
| CN106119330B (en) * | 2016-08-09 | 2019-09-24 | 中国计量大学 | A kind of preparation method of fish scale collagen range of hydrolysed peptides |
| CN109180808A (en) * | 2018-09-30 | 2019-01-11 | 青岛蓝色康典海洋生物科技有限公司 | A kind of fish scale collagen and its preparation method and application |
| CN109180808B (en) * | 2018-09-30 | 2021-12-21 | 青岛蓝色康典海洋生物科技有限公司 | Fish scale collagen and preparation method and application thereof |
| CN109628302A (en) * | 2018-12-28 | 2019-04-16 | 宁夏红山河食品股份有限公司 | A kind of meat products subsection enzymolysis device and enzyme solution |
| CN109608540A (en) * | 2019-01-29 | 2019-04-12 | 广州华大生物科技有限公司 | A method of extracting collagen from fish scale |
| CN109897101A (en) * | 2019-03-14 | 2019-06-18 | 卓康(福建)生物科技有限公司 | A kind of collagen tripeptide and its production method and application |
| CN109897101B (en) * | 2019-03-14 | 2020-06-26 | 卓康(福建)生物科技有限公司 | Collagen tripeptide and production method and application thereof |
| CN109880734A (en) * | 2019-03-30 | 2019-06-14 | 中国水产科学研究院黑龙江水产研究所 | Amino acid extraction element machine extracting method in a kind of flesh of fish |
| CN110074356A (en) * | 2019-06-04 | 2019-08-02 | 江南大学 | A kind of Java tilapia skin deliming degreasing method |
| CN113480637A (en) * | 2021-08-05 | 2021-10-08 | 广西南宁佰奥吉生物科技有限公司 | Preparation method of non-denatured type II collagen |
| CN115176896A (en) * | 2022-08-08 | 2022-10-14 | 标优美生态工程镇江有限公司 | Hydrolyzed fish protein pet feed and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105063154A (en) | Method for extracting collagen from fish scales | |
| CN103789381B (en) | A kind of method of Isin glue collagen rapid extraction | |
| CN101805775B (en) | Method for preparing collagen from deer sinew | |
| CN101724677B (en) | Method for extracting collagen polypeptide and hydroxyapatite in fish scales by cooking hot extrusion | |
| CN106359631B (en) | A kind of pure collagen milk powder and preparation method thereof | |
| CN104726527A (en) | Preparation technology for producing collagen through enzymolysis of fish scales | |
| CN104531817A (en) | Combined production method of hyaluronic acid, chondroitin sulfate, collagen peptide, bone meal fodder and soap | |
| CN104313102B (en) | method for preparing collagen | |
| CN109897101B (en) | Collagen tripeptide and production method and application thereof | |
| WO2016173222A1 (en) | Hypoallergenic, odor-reduced fish protein oligopeptide, industrialized preparation method for same, and applications thereof | |
| CN105018555A (en) | Preparation method of giant salamander skin collagen peptide | |
| CN112724244A (en) | Bovine bone collagen peptide and production method thereof | |
| CN105925649B (en) | Preparation method of low-molecular-weight degreased squid protein functional active peptide | |
| CN105969830A (en) | Method for extracting active collagen peptide from pigskin | |
| CN109722461B (en) | Deep sea fish collagen peptide and production method thereof | |
| CN112813127B (en) | Method for preparing collagen peptide from chondroitin sulfate ultrafiltration waste liquid | |
| CN103386144A (en) | Preparation method of fish collagen combined chitosan biological dressing | |
| CN107365824A (en) | A kind of preparation method for hydrolyzing Isin glue collagen Gly-His-Lys | |
| CN105054132B (en) | A kind of production technology of fish scale jelly | |
| CN110577975B (en) | Method for extracting and preparing swimming bladder collagen oligopeptide | |
| CN110564802A (en) | Extraction method of yak achilles tendon bone collagen | |
| CN109486890A (en) | A kind of technique preparing Fish protein hybrid peptide from crude fish protein | |
| CN110144373A (en) | Extract the method for chondroitin sulfate and collagen peptide respectively using animal cartilage | |
| CN113754759A (en) | Process for extracting multiple nutritional ingredients from fish scales | |
| CN103319628B (en) | The method of chondroitin sulfate is prepared in super-voltage micro jet ultrafiltration |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20151118 |
|
| RJ01 | Rejection of invention patent application after publication |