CN103421871A - Preparation method of tuna bone collagen peptide - Google Patents
Preparation method of tuna bone collagen peptide Download PDFInfo
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- CN103421871A CN103421871A CN2012101730337A CN201210173033A CN103421871A CN 103421871 A CN103421871 A CN 103421871A CN 2012101730337 A CN2012101730337 A CN 2012101730337A CN 201210173033 A CN201210173033 A CN 201210173033A CN 103421871 A CN103421871 A CN 103421871A
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- tuna bone
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- 102000008186 Collagen Human genes 0.000 title claims abstract description 25
- 108010035532 Collagen Proteins 0.000 title claims abstract description 25
- 210000000988 Bone and Bones Anatomy 0.000 title claims abstract description 19
- 229920001436 collagen Polymers 0.000 title claims abstract description 13
- 229960005188 collagen Drugs 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000012528 membrane Substances 0.000 claims abstract description 19
- QTBSBXVTEAMEQO-UHFFFAOYSA-N acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000001728 nano-filtration Methods 0.000 claims abstract description 7
- 230000035484 reaction time Effects 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 239000000047 product Substances 0.000 claims abstract 6
- 239000006228 supernatant Substances 0.000 claims abstract 5
- 238000000034 method Methods 0.000 claims description 17
- 238000007792 addition Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000010298 pulverizing process Methods 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 102000020504 Collagenase family Human genes 0.000 claims description 4
- 108060005980 Collagenase family Proteins 0.000 claims description 4
- 229960002424 collagenase Drugs 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims 2
- 235000013601 eggs Nutrition 0.000 claims 1
- 102000004196 processed proteins & peptides Human genes 0.000 claims 1
- 108090000765 processed proteins & peptides Proteins 0.000 claims 1
- 102000004190 Enzymes Human genes 0.000 abstract description 9
- 108090000790 Enzymes Proteins 0.000 abstract description 9
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 4
- 239000002244 precipitate Substances 0.000 abstract 4
- 238000005119 centrifugation Methods 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000009833 condensation Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- 238000007654 immersion Methods 0.000 abstract 1
- 238000001694 spray drying Methods 0.000 abstract 1
- 229940088598 Enzyme Drugs 0.000 description 7
- 102000004169 proteins and genes Human genes 0.000 description 7
- 108090000623 proteins and genes Proteins 0.000 description 7
- 239000002253 acid Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 238000010612 desalination reaction Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229920001184 polypeptide Polymers 0.000 description 3
- 235000014347 soups Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- -1 sodium-chlor Chemical compound 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003809 water extraction Methods 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 102000035336 Aspartic proteases Human genes 0.000 description 1
- 108091005540 Aspartic proteases Proteins 0.000 description 1
- 229940110715 ENZYMES FOR TREATMENT OF WOUNDS AND ULCERS Drugs 0.000 description 1
- 102000035348 Neutral proteases Human genes 0.000 description 1
- 108091005544 Neutral proteases Proteins 0.000 description 1
- 210000002784 Stomach Anatomy 0.000 description 1
- 238000005296 abrasive Methods 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 238000005039 chemical industry Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002255 enzymatic Effects 0.000 description 1
- 238000006911 enzymatic reaction Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000751 protein extraction Methods 0.000 description 1
- 235000014102 seafood Nutrition 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Abstract
The invention discloses a preparation method of a tuna bone collagen peptide. The preparation method comprises the following steps of carrying out immersion and cleaning of tuna bone, crushing the tuna bone by a crusher, uniformly mixing the crushed tuna bone and water having the volume 4-8 times volume of the crushed tuna bone, feeding the mixture into a centrifugal machine, carrying out continuous centrifugal separation at a rotation rate of 8000-12000r/min for 30min, removing a supernatant, carrying out decalcification of the precipitates with an edible acetic acid aqueous solution having content of 4-8% and the volume 2-4 times volume of the precipitates for 30-50min, carrying out centrifugation for another 30min, adding the precipitates into water having the volume 3-6 times that of the precipitates, adding the mixture into a biological enzymolysis tank, carrying out enzymolysis, wherein in the enzymolysis, the amount of a compound enzyme is 0.1-2% that of the raw materials and reaction conditions comprise a temperature of 37-65 DEG C, a PH value of 6.5-8.0 and reaction time of 4-8h, treating the enzymolysis products by a 30KD ultrafiltration membrane, and carrying out nanofiltration membrane condensation and spray drying of the enzymolysis products having the molecular weight less than 30KD.
Description
Technical field
The invention belongs to a kind of method that sea-food extracts, specifically a kind of extraction preparation method of fish-bone collagen peptide.
Technical background
At present, the tuna bone is as the tankage of the tuna course of processing, as waste or production low value feed, economic worth is lower, and tuna is as a kind of high-quality marine economy fish, and market demand is huge, the tuna bone quantity produced is large, wherein is rich in the high-quality active collagen.Collagen protein, as a kind of important bio-tissue structural protein, more and more causes people's concern and rise, and market potential is huge, economic worth is higher, particularly the collagen protein micromolecule active polypeptide, be widely used in medicine, beauty and health care and food service industry.The traditional technology that collagen protein extracts can be divided into five classes, i.e. acid system, alkaline process, enzyme process, salt method and hot water extraction etc.Its ultimate principle is all the characteristic according to collagen protein, changes the external environment of protein, and collagen protein is separated from other protein.Acid system and alkaline process are that collagen protein is extracted under acid and alkaline environment, and acid system is applied more extensive in the extraction process of collagen protein, and the alkaline process report seldom.The salt method is that raw material is always extracted at certain density salts solution, and the main salt used has sodium-chlor, Repone K and sodium acetate.Although above three kinds of method techniques are simple, cost is also low belongs to the high energy consumption industry owing in leaching process, can using a large amount of fresh water and acid-alkali salt, and the acid-alkali salt of discharge will produce certain ecological impact to surrounding environment.Do not meet green sustainability Economic Development Mode.The hot water extraction need to be used a large amount of fresh water and the energy, does not meet the main flow of country and development of world economy.
Biological enzyme is to utilize the gentle high efficiency of enzyme reaction collagen protein to be mentioned out from different raw materials under certain envrionment conditions, and the most frequently used enzyme has stomach en-, trypsinase, aspartic protease, Sumizyme MP, neutral protease and papoid at present.Along with the development of Enzymes Industry and constantly widening of Application Areas, zymin output increases rapidly, and market competition advantage constantly increases.The membrane separation concentration purification technique be the film that utilizes different pore size by target product according to its molecular size separated, the concentrated novel method of mentioning that is further purified, in production efficiency, energy consumption and aspect of performance have obvious advantage, in biological medicine, chemical industry and food service industry, be widely used, the film industrialization development is rapid at present in addition, auxiliary products are complete, and cost constantly reduces, and are the optimal selections of technique upgrading.
Summary of the invention
The present invention is directed to tuna collagen material characteristics, by biological enzymolysis technology and scientific and reasonable being integrated of membrane technique, adopt the industry mill to carry out the pulverization process in early stage to raw material, by large flux high-speed and continuous centrifugal separation equipment, water-soluble noncollagen protein is separated, contain the precipitation of collagen protein after compound bio enzymolysis technology is hydrolyzed to the active small molecular polypeptide, after the film of special pore size distribution is separated concentrated the purification, obtain certain density active small molecular polypeptide slurries, obtain the high purity molecular weight and be less than 30KD collagen active peptide white powder finally by crossing the ultra micro drying of dusting.
The technical solution adopted for the present invention to solve the technical problems is: after raw material tuna bone is carried out to soaking and washing, at first use pulverizer to its carry out pulverization process for the fluid soup compound after, enter industrial abrasive dust and be broken to 300～500 microns left and right of particle diameter, with enter 8000～12000 rev/mins of continuously centrifugeds of supercentrifuge after 4～8 times of volume water mix and separate the water-soluble substances of removing noncollagen protein in 30 minutes, containing the throw out of collagen protein and the 4%-8% alimentary acetic acid aqueous solution decalcification of 2～4 times of volumes processed after 30-50 minute, recentrifuge was processed after 30 minutes, add after 3-6 times of volume water and enter the biological enzymolysis tank and carry out the complex enzyme hydrolysis processing.The prozyme chief component is trypsinase and Collagenase, addition is 0.1～2% of raw material, reaction conditions is 37～65 ℃ of temperature, PH 6.5～8.0,4～8 hours reaction times, enzymatic vessel outlet is connected with membrane separation apparatus, ultra-filtration membrane through molecular weight, be 30KD, molecular weight be less than 30KD pass through after ultra-filtration membrane directly enter nanofiltration membrane and carry out after the desalination and concentration processing being dusted drying.
The invention has the beneficial effects as follows: utilize to greatest extent enzyme and raw material to be worth, further reduce production costs, this technique invention has improved collagen protein extraction yield and purity, and wherein a large amount of water resources recycle, reduce production energy consumption.
Specific embodiments
Example 1: after raw material tuna bone is carried out to soaking and washing, at first use pulverizer to its carry out pulverization process for the fluid soup compound after, enter technical grade colloidal mill micronizing to 300 microns left and right of particle diameter, with enter 12000 rev/mins of continuously centrifugeds of supercentrifuge after 8 times of volume water mix and separate the water-soluble substances of removing noncollagen protein in 30 minutes, process after 30 minutes after recentrifuge removal moisture containing the throw out of collagen protein and 4% alimentary acetic acid aqueous solution decalcification of 4 times of volumes, add after 3 times of volume water to enter the biological enzymolysis tank and carry out the complex enzyme hydrolysis processing.The prozyme chief component is trypsinase and Collagenase, and addition is raw material 0.1%, and reaction conditions is 37 ℃ of temperature, PH8.0,4 hours reaction times.Enzymolysis product is processed with ultrafiltration apparatus, and the molecular weight that sees through of ultra-filtration membrane is 30KD, molecular weight be less than 30KD pass through after ultra-filtration membrane directly enter nanofiltration membrane and carry out after desalination and concentration being dusted drying, be finished product.
Example 2: after raw material tuna bone is carried out to soaking and washing, at first use pulverizer to its carry out pulverization process for the fluid soup compound after, enter technical grade colloidal mill micronizing to 500 microns left and right of particle diameter, with enter 8000 rev/mins of continuously centrifugeds of supercentrifuge after 4 times of volume water mix and separate the water-soluble substances of removing noncollagen protein in 30 minutes, containing the throw out of collagen protein and 8% alimentary acetic acid aqueous solution decalcification of 2 times of volumes processed after 50 minutes, recentrifuge adds 6 times of volume water to enter the biological enzymolysis tank and carries out the complex enzyme hydrolysis processing after removing moisture.The prozyme chief component is trypsinase and Collagenase, and addition is raw material 2%, and reaction conditions is 65 ℃ of temperature, PH6.5,8 hours reaction times.Enzymolysis product is processed with ultrafiltration apparatus, and the molecular weight that sees through of ultra-filtration membrane is 30KD, molecular weight be less than 30KD pass through after ultra-filtration membrane directly enter nanofiltration membrane and carry out after desalination and concentration being dusted drying, be finished product.
Claims (4)
1. the preparation method of a tuna osso-albumin egg peptide, it is characterized in that the method includes the steps of: after raw material tuna bone is carried out to soaking and washing, at first after using pulverizer to its pulverization process with enter 8000～12000 rev/mins of continuously centrifugeds of whizzer after 4～8 times of volume water mix and separate and within 30 minutes, remove supernatant, the 4%--8% alimentary acetic acid decalcification of throw out and 2～4 times of volumes was processed after 30-50 minute, 8000-12000 rev/min of continuously centrifuged of recentrifuge machine removed supernatant in 30 minutes, with enter the biological enzymolysis tank after 3-6 times of water mixes and carry out enzymolysis processing, the prozyme addition is 0.1～2% of raw material, reaction conditions is 37～65 ℃ of temperature, PH 6.5～8.0, 4～8 hours reaction times, enzymolysis product 30KD ultrafiltration membrane treatment, permeation parts is concentrated through nanofiltration membrane, spraying drying is tuna bone collagen peptide finished product.
2. a kind of preparation method of tuna bone collagen peptide as claimed in claim 1, it is characterized in that the method includes the steps of: after raw material tuna bone is carried out to soaking and washing, at first use pulverizer it is carried out after pulverization process and enter 9000～10000 rev/mins of continuously centrifugeds of whizzer after 4～8 times of volume water mix and separate and within 30 minutes, remove supernatant, in the 4.5%-7.5% alimentary acetic acid aqueous solution of throw out and 2.5～3.5 times of volumes, decalcification was processed after 30-50 minute, 8000-12000 rev/min of continuously centrifuged of recentrifuge machine removed supernatant in 30 minutes, with enter the biological enzymolysis tank after 3-6 times of water mixes and carry out enzymolysis processing, the prozyme addition is 0.1～2% of raw material, reaction conditions is 37～65 ℃ of temperature, PH6.5～8.0, enter the biological enzymolysis tank and carry out enzymolysis processing, the prozyme addition is 1～1.5% of raw material, reaction conditions is 45～55 ℃ of temperature, PH7.～8.0, 4.5～7.5 hours reaction times, enzymolysis product 30KD ultrafiltration membrane treatment, permeation parts is concentrated through nanofiltration membrane, spraying drying is tuna bone collagen peptide finished product.
3. a kind of preparation method of tuna bone collagen peptide as claimed in claim 1, is characterized in that described prozyme chief component is trypsinase and Collagenase.
4. a kind of preparation method of tuna bone collagen small-molecular peptides as claimed in claim 1, it is characterized in that described nanofiltration membrane to see through molecular weight be 380D.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101730337A CN103421871A (en) | 2012-05-14 | 2012-05-14 | Preparation method of tuna bone collagen peptide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101730337A CN103421871A (en) | 2012-05-14 | 2012-05-14 | Preparation method of tuna bone collagen peptide |
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| CN103421871A true CN103421871A (en) | 2013-12-04 |
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| CN2012101730337A Pending CN103421871A (en) | 2012-05-14 | 2012-05-14 | Preparation method of tuna bone collagen peptide |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103798845A (en) * | 2014-03-05 | 2014-05-21 | 青岛金海源食品有限公司 | Method for developing nano-calcium collagen by utilizing cod bones |
| CN104164468B (en) * | 2014-04-24 | 2017-01-11 | 吉林金梓源生物科技股份有限公司 | Method for preparing collagen peptide from animal cardiac tube |
| CN106337074A (en) * | 2016-10-24 | 2017-01-18 | 广东工业大学 | Cirrhinus molitorella bone collagen extracting method |
| CN108752466A (en) * | 2018-06-19 | 2018-11-06 | 浙江兴业集团有限公司 | A kind of chelated calcium preparation method of tuna bone collagen peptide |
| CN111329043A (en) * | 2020-03-18 | 2020-06-26 | 福建紫山食品科技有限公司 | Tremella can with effects of maintaining beauty and keeping young and production method thereof |
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| CN101061827A (en) * | 2006-04-30 | 2007-10-31 | 中国食品发酵工业研究院 | Industry method of producing fish collagen peptide from fish skin and bone by an enzyme method |
| CN101397581A (en) * | 2008-10-15 | 2009-04-01 | 青岛贝尔特生物科技有限公司 | Method for extracting fishskin collagen polypeptide from fish wastes |
-
2012
- 2012-05-14 CN CN2012101730337A patent/CN103421871A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101061827A (en) * | 2006-04-30 | 2007-10-31 | 中国食品发酵工业研究院 | Industry method of producing fish collagen peptide from fish skin and bone by an enzyme method |
| CN101397581A (en) * | 2008-10-15 | 2009-04-01 | 青岛贝尔特生物科技有限公司 | Method for extracting fishskin collagen polypeptide from fish wastes |
Non-Patent Citations (3)
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| 辛建美: "酶解金枪鱼碎肉制备活性肽及其分离的研究", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103798845A (en) * | 2014-03-05 | 2014-05-21 | 青岛金海源食品有限公司 | Method for developing nano-calcium collagen by utilizing cod bones |
| CN104164468B (en) * | 2014-04-24 | 2017-01-11 | 吉林金梓源生物科技股份有限公司 | Method for preparing collagen peptide from animal cardiac tube |
| CN106337074A (en) * | 2016-10-24 | 2017-01-18 | 广东工业大学 | Cirrhinus molitorella bone collagen extracting method |
| CN108752466A (en) * | 2018-06-19 | 2018-11-06 | 浙江兴业集团有限公司 | A kind of chelated calcium preparation method of tuna bone collagen peptide |
| CN111329043A (en) * | 2020-03-18 | 2020-06-26 | 福建紫山食品科技有限公司 | Tremella can with effects of maintaining beauty and keeping young and production method thereof |
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Application publication date: 20131204 |
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