CN100370033C - Fishscale collagen production process - Google Patents
Fishscale collagen production process Download PDFInfo
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- CN100370033C CN100370033C CNB2005100449168A CN200510044916A CN100370033C CN 100370033 C CN100370033 C CN 100370033C CN B2005100449168 A CNB2005100449168 A CN B2005100449168A CN 200510044916 A CN200510044916 A CN 200510044916A CN 100370033 C CN100370033 C CN 100370033C
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- 238000004519 manufacturing process Methods 0.000 title claims description 17
- 230000037319 collagen production Effects 0.000 title claims description 10
- 241000251468 Actinopterygii Species 0.000 claims abstract description 65
- 102000008186 Collagen Human genes 0.000 claims abstract description 24
- 108010035532 Collagen Proteins 0.000 claims abstract description 24
- 229920001436 collagen Polymers 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000005507 spraying Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 102000004190 Enzymes Human genes 0.000 claims description 16
- 108090000790 Enzymes Proteins 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000011146 sterile filtration Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 230000000975 bioactive effect Effects 0.000 claims description 6
- 238000005262 decarbonization Methods 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000008213 purified water Substances 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 230000008719 thickening Effects 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 108090000145 Bacillolysin Proteins 0.000 claims description 3
- 102000035092 Neutral proteases Human genes 0.000 claims description 3
- 108091005507 Neutral proteases Proteins 0.000 claims description 3
- 108091005804 Peptidases Proteins 0.000 claims description 3
- 239000004365 Protease Substances 0.000 claims description 3
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 102000035101 Aspartic proteases Human genes 0.000 claims description 2
- 108091005502 Aspartic proteases Proteins 0.000 claims description 2
- 235000021050 feed intake Nutrition 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 102000005158 Subtilisins Human genes 0.000 claims 1
- 108010056079 Subtilisins Proteins 0.000 claims 1
- 235000019658 bitter taste Nutrition 0.000 abstract description 4
- 238000010306 acid treatment Methods 0.000 abstract description 2
- 239000003513 alkali Substances 0.000 abstract description 2
- 239000002440 industrial waste Substances 0.000 abstract description 2
- 238000006386 neutralization reaction Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 238000009835 boiling Methods 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 10
- 108090000765 processed proteins & peptides Proteins 0.000 description 5
- 102000004169 proteins and genes Human genes 0.000 description 4
- 108090000623 proteins and genes Proteins 0.000 description 4
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 3
- 238000005904 alkaline hydrolysis reaction Methods 0.000 description 3
- 239000003245 coal Substances 0.000 description 3
- 238000010025 steaming Methods 0.000 description 3
- 241001465754 Metazoa Species 0.000 description 2
- 210000000988 bone and bone Anatomy 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical class [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000010612 desalination reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 210000002435 tendon Anatomy 0.000 description 2
- 239000004471 Glycine Substances 0.000 description 1
- ONIBWKKTOPOVIA-UHFFFAOYSA-N Proline Natural products OC(=O)C1CCCN1 ONIBWKKTOPOVIA-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 150000007516 brønsted-lowry acids Chemical class 0.000 description 1
- 150000007528 brønsted-lowry bases Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 210000003041 ligament Anatomy 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 210000002826 placenta Anatomy 0.000 description 1
- 210000003491 skin Anatomy 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
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- Peptides Or Proteins (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Meat, Egg Or Seafood Products (AREA)
Abstract
The present invention discloses a producing technique for fish scale collagen. The fish scale collagen is obtained through twice acid treatment, alkali neutralization, boiling, enzymolysis, exchange adsorption, concentration, filtration, drying and spraying. The present invention provides a producing technique for fish scale collagen, which fully uses a fish scale of an industrial waste to change waste into valuable, and has simple and safe technique step and easy operation. A product produced has the characteristics of low and stable molecular weight, no fishy smell and bitterness, very low ash content, high productive efficiency and thorough enzymolysis fish scale.
Description
One, technical field
The invention belongs to the biological extraction technical field, especially relate to a kind of Fishscale collagen production process.
Two, background technology
Collagen protein (collagen) be collagen again, is a kind of sugar-protein that contains, and is extensive in distributed in nature, mainly is distributed in the mammiferous reticular tissue, as the constituent material of skin, bone, tendon, ligament, blood vessel; Have about 16% to be protein in the human body component, collagen protein accounts for 30～40% of body internal protein total amount, is the maximum protein of people's in-vivo content; The amino acid of collagen is formed very special, and wherein glycine (Gly) accounts for 30%, and proline(Pro) (Pro) and oxyproline (Hyp) account for about 25% altogether.
Collagen peptide comes from collagen protein, is widely used in food, makeup, and beverage and health products trade, the collagen peptide of traditional technology mainly comes from the skin of Lu Sheng with animal, bone, tendon and placenta; But, make the source of collagen product limited owing to the influence of the extremely strong mad cow disease of infectivity and the needs of protection of animal; Contain rich in protein in the fish scale, its proteinic main moiety is a collagen protein, but the nutritive ingredient of fish scale was ignored by people in the past always, especially at home, be regarded as rubbish in the processing of aquatic products industry, its value of not only not being fully used, but also contaminate environment.
The utilization of fish scale in recent years begins to cause concern, takes up the extraction of collagen peptide, mainly by steaming and decocting under high pressure, and acidolysis, alkaline hydrolysis, four kinds of methods of enzymolysis; Steaming and decocting under high pressure, acidolysis, alkaline hydrolysis, be traditional extracting method, the problem that the steaming and decocting under high pressure method exists is that power consumption is high, is unfavorable for safety in production under the condition of High Temperature High Pressure, and the molecular weight product height that obtains, the unfavorable and absorption by human body of the collagen peptide of this explained hereafter; Acidolysis, the alkaline hydrolysis method need add a large amount of bronsted lowry acids and bases bronsted lowries, and seriously polluted to environment introduces a large amount of inorganic salt and increased the pressure of desalination in the follow-up work, and the molecular weight of product is wayward.
Enzymolysis is a kind of novel method, and scientific research field is crossed correlative study, but has following some deficiency: one, how the pre-treatment of fish scale alternately soaks with hydrochloric acid and saturated limewater with duration before the enzymolysis; Two, the enzyme amount of Jia Ruing is big, and majority thinks that best enzyme amount is 3%-5%; Three, make the thorough enzymolysis of fish scale, generally surpass 5 hours, enzymolysis time is long; Below all be unfavorable for actual production; Four, the product of producing has fishy smell, bitter taste, the ash content of coal height.
Three, summary of the invention
The objective of the invention is to improve the deficiency of prior art and provide a kind of and made full use of that the industrial waste fish scale is turned waste into wealth, the molecular weight product of the simple and safe easy handling of processing step, production is low and stable, product does not have that fishy smell bitter taste, the ash content of coal are extremely low, production efficiency is high, the thorough Fishscale collagen production process of enzymolysis of fish scale.
The object of the present invention is achieved like this, and a kind of Fishscale collagen production process is characterized in that this technology may further comprise the steps:
A, fish scale is dropped in the retort, add the weight 2-10 water doubly that drops into fish scale, add the technical-grade hydrochloric acid of the weight 50%-70% that drops into fish scale, stirring reaction 8-16 hour, control pH value was below 2.0, behind specific time, sour water is put into the pond, wash fish scale with water;
B, with the water in the fish scale put clean after, add the weight 2-10 water doubly that drops into fish scale again, add the hydrochloric acid of fish scale charging capacity 5%-20%, after stirring reaction 2-12 hour, sour water is put into the pond, wash fish scale with water;
Add entry in the fish scale after c, the washing, transfer pH7.0-7.5, wash with NaOH solution;
Add the weight 1.5-10 purified water doubly that drops into fish scale in d, the clean fish scale, the washing fish scale, intensification was boiled 30 minutes;
E, cool the temperature to 55-65 ℃, control pH6.5 adds the feed intake bioactive enzyme of weight 0.1%-1% of fish scale, and enzymolysis 1-4 hour, enzymolysis was warming up to 70-90 ℃ after finishing, and is incubated 30 minutes;
F, solution is cooled to 50-55 ℃, leaves standstill 30 minutes after-filtration, remove a small amount of residue fish scale;
G, the clear liquid that will obtain after the f step filters adsorb with Zeo-karb, anionite-exchange resin;
The pH value of h, regulator solution is between 5.0-7.5;
I, concentrated, 50-70 ℃ of control thickening temperature, vapor pressure remains on 0.03-0.05Mpa when concentrating, and being concentrated into solid content is 20%-50%;
J, in concentrated solution, add to drop into the gac of fish scale weight 3%-10%, temperature 55-70 ℃ following whip attachment 10-30 minute;
K, decarbonization filtering are taken off the gac in the solution;
L, sterile filtration are carried out sterile filtration with solution with the millipore filtration that the stainless steel sheet frame presss from both sides film filter plate and 0.22 μ m;
M, spraying drying are carried out spraying drying with the filtrate after the sterile filtration, obtain the collagen protein work in-process, 160-230 ℃ of control inlet temperature, 40-85 ℃ of temperature out control.
N, spraying drying finish, and promptly obtain fish scale collagen.
The employed enzyme of enzymolysis be in Sumizyme MP, neutral protease, aspartic protease, the compound protease one or both and above mix arbitrarily.
Employed bioactive enzyme pH value scope is 4.0-9.5,40 ℃-70 ℃ of temperature ranges.
The preferred NovoCor ABG of the employed enzyme of enzymolysis, Neutrase0.8L, Alcalase3.0T, Alcalase2.4L, Flavorzyme500L, trypsinase, papoid, bromeline.
Compared with the prior art the present invention has following distinguishing feature and positively effect:
1, fish scale pre-treatment step of the present invention is only used twice acid treatment, after the alkali neutralization is soaked without saturated limewater, reaches the effect of desalination degreasing, has shortened the production time, has guaranteed the complete enzymolysis of fish scale, and has reduced the pollution to environment;
2, increased the step that heats up and boil before enzymolysis, make fish scale expanded, the connection between albumen is loose, has reduced the enzyme amount of enzymolysis step, has shortened enzymolysis time.
3, lower than prior art enzyme concentration during enzymolysis, be 0.1%-1% with the enzyme amount, enzymolysis＜4 hour, the time spent is short, and enzymolysis is abundant, has not only reduced production cost, has shortened the production time, has also solved because add organized enzyme to make product that the problem of peculiar smell be arranged.
4, the collagen peptide that goes out of this explained hereafter is compared with the product that prior art is produced, no fishy smell bitter taste, and the ash content of coal extremely low＜1%, molecular weight is low and stable.
Four, specific embodiments:
Embodiment 1, and a kind of Fishscale collagen production process is that fish scale 100kg is dropped in the retort, the water that adds 1000kg adds the 70kg technical-grade hydrochloric acid, stirring reaction 8-16 hour, control pH value behind specific time, is put into the pond with sour water below 2.0, wash fish scale with water, with the water in the fish scale put clean after, add the water of 1000kg again, the hydrochloric acid that adds 20kg, after stirring reaction 2-12 hour, sour water is put into the pond, wash fish scale with water; Add entry in the fish scale after the washing, transfer pH7.0-7.5, wash with NaOH solution; The purified water that adds 1000kg in the fish scale of cleaning, the washing fish scale heats up and boiled 30 minutes; Cool the temperature to 55-65 ℃, control pH6.5, add the 1kg bioactive enzyme, employed bioactive enzyme pH value scope is 4.0-9.5,40 ℃-70 ℃ of temperature ranges, that present embodiment uses is neutral protease Neutrase0.8L, enzymolysis 1-4 hour, enzymolysis is warming up to 70-90 ℃ after finishing, and is incubated 30 minutes; Solution is cooled to 50-55 ℃, leaves standstill 30 minutes after-filtration, remove a small amount of residue fish scale; Liquid after filtering is adsorbed with Zeo-karb, anionite-exchange resin; The pH value of regulator solution is between 5.0-7.5; Concentrate, 50-70 ℃ of control thickening temperature, vapor pressure remains on 0.03-0.05Mpa when concentrating, and being concentrated into solid content is 20%-50%; The gac that in concentrated solution, adds 10kg, temperature 55-70 ℃ following whip attachment 10-30 minute; Decarbonization filtering is taken off the gac in the solution; Sterile filtration is carried out sterile filtration with solution with the millipore filtration that the stainless steel sheet frame presss from both sides film filter plate and 0.22 μ m; Spraying drying is carried out spraying drying with the filtrate after the sterile filtration, obtains the collagen protein work in-process, 160-230 ℃ of control inlet temperature, 40-85 ℃ of temperature out control; Spraying drying finishes, and promptly obtains fish scale collagen.
Embodiment 2, and a kind of Fishscale collagen production process is that fish scale 100kg is dropped in the retort, the water that adds 200kg adds the 50kg technical-grade hydrochloric acid, stirring reaction 8-16 hour, control pH value behind specific time, is put into the pond with sour water below 2.0, wash fish scale with water, with the water in the fish scale put clean after, add the water of 200kg again, the hydrochloric acid that adds 5kg, after stirring reaction 2-12 hour, sour water is put into the pond, wash fish scale with water; Add entry in the fish scale after the washing, transfer pH7.0-7.5, wash with NaOH solution; The purified water that adds 150kg in the fish scale of cleaning, the washing fish scale heats up and boiled 30 minutes; Cool the temperature to 55-65 ℃, control pH6.5 adds 0.1kg compound protease Flavorzyme500L, and enzymolysis 1-4 hour, enzymolysis was warming up to 70-90 ℃ after finishing, and is incubated 30 minutes; Solution is cooled to 50-55 ℃, leaves standstill 30 minutes after-filtration, remove a small amount of residue fish scale; Liquid after filtering is adsorbed with Zeo-karb, anionite-exchange resin respectively; The pH value of regulator solution is between 5.0-7.5; Concentrate, 50-70 ℃ of control thickening temperature, vapor pressure remains on 0.03-0.05Mpa when concentrating, and being concentrated into solid content is 20%-50%; The gac that in concentrated solution, adds 3kg, temperature 55-70 ℃ following whip attachment 10-30 minute; Decarbonization filtering is taken off the gac in the solution; Sterile filtration is carried out sterile filtration with solution with the millipore filtration that the stainless steel sheet frame presss from both sides film filter plate and 0.22 μ m; Spraying drying is carried out spraying drying with the filtrate after the sterile filtration, obtains the collagen protein work in-process, 160-230 ℃ of control inlet temperature, 40-85 ℃ of temperature out control; Spraying drying finishes, and promptly obtains fish scale collagen.
Claims (3)
1. Fishscale collagen production process is characterized in that this technology may further comprise the steps:
A, fish scale is dropped in the retort, add the weight 2-10 water doubly that drops into fish scale, add the technical-grade hydrochloric acid of the weight 50%-70% that drops into fish scale, stirring reaction 8-16 hour, control pH value was below 2.0, behind specific time, sour water is put into the pond, wash fish scale with water;
B, with the water in the fish scale put clean after, add the weight 2-10 water doubly that drops into fish scale again, add the hydrochloric acid of fish scale charging capacity 5%-20%, after stirring reaction 2-12 hour, sour water is put into the pond, wash fish scale with water;
Add entry in the fish scale after c, the washing, transfer pH7.0-7.5, wash with NaOH solution;
Add the weight 1.5-10 purified water doubly that drops into fish scale in d, the clean fish scale, the washing fish scale, intensification was boiled 30 minutes;
E, cool the temperature to 55-65 ℃, control pH6.5, add the feed intake bioactive enzyme of weight 0.1%-1% of fish scale, enzymolysis 1-4 hour, enzymolysis is warming up to 70-90 ℃ after finishing, be incubated 30 minutes, the employed enzyme of enzymolysis be in Sumizyme MP, neutral protease, aspartic protease, the compound protease one or both and above mix arbitrarily;
F, solution is cooled to 50-55 ℃, leaves standstill 30 minutes after-filtration, remove a small amount of residue fish scale;
G, the clear liquid that will obtain after the f step filters adsorb with Zeo-karb, anionite-exchange resin;
The pH value of h, regulator solution is between 5.0-7.5;
I, concentrated, 50-70 ℃ of control thickening temperature, vapor pressure remains on 0.03-0.05Mpa when concentrating, and being concentrated into solid content is 20%-50%;
J, in concentrated solution, add to drop into the gac of fish scale weight 3%-10%, temperature 55-70 ℃ following whip attachment 10-30 minute;
K, decarbonization filtering are taken off the gac in the solution;
L, sterile filtration are carried out sterile filtration with solution with the millipore filtration that the stainless steel sheet frame presss from both sides film filter plate and 0.22 μ m;
M, spraying drying are carried out spraying drying with the filtrate after the sterile filtration, obtain the collagen protein work in-process, 160-230 ℃ of control inlet temperature, 40-85 ℃ of temperature out control;
N, spraying drying finish, and promptly obtain fish scale collagen.
2. a kind of Fishscale collagen production process of stating according to claim 1 is characterized in that employed bioactive enzyme pH value scope is 4.0-9.5,40 ℃-70 ℃ of temperature ranges.
3. a kind of Fishscale collagen production process of stating according to claim 1 or 2 is characterized in that the preferred NovoCor ABG of the employed enzyme of enzymolysis, Neutrase0.8L, Alcalase3.0T, Alcalase 2.4L, Flavorzyme500L, trypsinase, papoid, bromeline.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100449168A CN100370033C (en) | 2005-10-19 | 2005-10-19 | Fishscale collagen production process |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100449168A CN100370033C (en) | 2005-10-19 | 2005-10-19 | Fishscale collagen production process |
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| CN1775950A CN1775950A (en) | 2006-05-24 |
| CN100370033C true CN100370033C (en) | 2008-02-20 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102066435B1 (en) * | 2018-10-11 | 2020-02-11 | 주식회사 골드레벤 | Method for manufacturing collagen using olive and olive collagen manufactured by using the same and cosmetic compositions comprising the olive collagen |
| RU2789341C1 (en) * | 2021-11-15 | 2023-02-01 | Людмила Михайловна Коколова | Method for producing collagen from the scales of the carassius carassius jacuticus carp |
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| JP5127194B2 (en) * | 2006-09-29 | 2013-01-23 | 辻製油株式会社 | Collagen peptide powder, method for producing the same and polyphenol-containing product |
| CN100381528C (en) * | 2006-11-06 | 2008-04-16 | 四川大学 | Preparation method of undenatured fish scale collagen |
| JP4369969B2 (en) * | 2007-10-26 | 2009-11-25 | 株式会社アールビーエス | Biocompatible material and method for producing the same |
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| CN102321719A (en) * | 2011-09-28 | 2012-01-18 | 山东天久生物技术有限公司 | Industrial production method for preparing collagen from fish scale by enzyme method |
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| CN1775950A (en) | 2006-05-24 |
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