CN104774257A - Method for extracting collagen from Mahi-mahi leftovers - Google Patents
Method for extracting collagen from Mahi-mahi leftovers Download PDFInfo
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- CN104774257A CN104774257A CN201510162420.4A CN201510162420A CN104774257A CN 104774257 A CN104774257 A CN 104774257A CN 201510162420 A CN201510162420 A CN 201510162420A CN 104774257 A CN104774257 A CN 104774257A
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- 102000008186 Collagen Human genes 0.000 title claims abstract description 47
- 108010035532 Collagen Proteins 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 30
- 229920001436 collagen Polymers 0.000 title abstract description 13
- 235000021190 leftovers Nutrition 0.000 title abstract 4
- 239000002994 raw material Substances 0.000 claims abstract description 33
- 239000002002 slurry Substances 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000000605 extraction Methods 0.000 claims abstract description 18
- 230000008014 freezing Effects 0.000 claims abstract description 13
- 238000007710 freezing Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 4
- 241000252185 Cobitidae Species 0.000 claims description 26
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 238000002525 ultrasonication Methods 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 16
- 238000010298 pulverizing process Methods 0.000 claims description 13
- 238000010612 desalination reaction Methods 0.000 claims description 11
- 239000012528 membrane Substances 0.000 claims description 5
- 238000001728 nano-filtration Methods 0.000 claims description 5
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 claims description 3
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 3
- 241000251468 Actinopterygii Species 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000009210 therapy by ultrasound Methods 0.000 abstract 2
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 230000029087 digestion Effects 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 230000020477 pH reduction Effects 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 12
- 239000000284 extract Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 210000001519 tissue Anatomy 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- 230000001133 acceleration Effects 0.000 description 4
- 238000004945 emulsification Methods 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 230000035515 penetration Effects 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 230000008961 swelling Effects 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- 206010053262 Skin swelling Diseases 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 239000003925 fat Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 235000013372 meat Nutrition 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 238000000751 protein extraction Methods 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 238000003809 water extraction Methods 0.000 description 2
- PMMYEEVYMWASQN-DMTCNVIQSA-N Hydroxyproline Chemical compound O[C@H]1CN[C@H](C(O)=O)C1 PMMYEEVYMWASQN-DMTCNVIQSA-N 0.000 description 1
- 102000011782 Keratins Human genes 0.000 description 1
- 108010076876 Keratins Proteins 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 210000000845 cartilage Anatomy 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- PMMYEEVYMWASQN-UHFFFAOYSA-N dl-hydroxyproline Natural products OC1C[NH2+]C(C([O-])=O)C1 PMMYEEVYMWASQN-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000004833 fish glue Substances 0.000 description 1
- 229960002591 hydroxyproline Drugs 0.000 description 1
- 210000002435 tendon Anatomy 0.000 description 1
- FGMPLJWBKKVCDB-UHFFFAOYSA-N trans-L-hydroxy-proline Natural products ON1CCCC1C(O)=O FGMPLJWBKKVCDB-UHFFFAOYSA-N 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]
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Biochemistry (AREA)
- Gastroenterology & Hepatology (AREA)
- Zoology (AREA)
- Biophysics (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Medicinal Chemistry (AREA)
- Molecular Biology (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Toxicology (AREA)
- Peptides Or Proteins (AREA)
Abstract
The invention relates to a method for extracting collagen, and in particular to a method for extracting collagen from Mahi-mahi leftovers. According to the technical scheme, the method for extracting collagen from Mahi-mahi leftovers comprises the following steps: with fish skin, fishbone and fins of Mahi-mahi as raw materials, a, crushing the raw materials with a special device, and mixing the crushed raw materials with water to obtain slurry; b, adding an acidic material to the slurry, and carrying out acidification; c, carrying out ultrasonic treatment on the acidified slurry; d, carrying out digestion on the slurry subjected to ultrasonic treatment; e, filtering; f, desalinating; g, freezing; and h, drying. With adoption of the technical scheme, the provided method for extracting collagen from Mahi-mahi leftovers has the advantages of high material utilization rate, improved product extraction rate as well as little pollution and environmental friendliness in extraction processes.
Description
Technical field
The present invention relates to a kind of collagen protein extracting method, particularly a kind of extracting method of Mahi loach fish corner material collagen protein.
Background technology
Collagen protein is the protein forming collagen fabric, for forming sustentacular tissue and the conjunctive tissue of animal, is mainly present in the skin of animal, bone, cartilage, blood vessel, tendon etc., and the positions such as fish squama, fin, fish glue are also containing collagen.
Collagen content in fish-skin is higher, the highlyest accounts for more than 80% of its total protein, then much higher compared with other positions of fish body.And the position work in-processes such as fish-skin, fish phosphorus and fin are often by the waste as converted products, producing level is not high.Documents and materials both at home and abroad about collagen protein extraction in fish-skin are more, and the fingerling class related to is also more, integrates and mainly contains acid-base method, enzyme process and Hot water extraction.Its object is all make fish-skin swelling by process in early stage, removes residual meat, fat and pigment, extracts collagen.Different skin tissue structure is different, and soak time is also different, and some immersion reaches several days time, and production efficiency reduces greatly, and long immersion also requires to be in for a long time in low temperature environment to delay molten the going bad of fish-skin.Production cycle is long, and power consumption is large.Be the tissues such as the corner flesh of fish, fish-skin, fin in Mahi loach processing scrap stock, fish-skin, fin and fish phosphorus account for the overwhelming majority.Mahi loach fish-skin has special structure, and fish-skin is covered by the round phosphorus of tiny difficult drop-off, is bonded in keratin skin, and the method selecting traditional collagen protein to extract requires to extract extremely for a long time, and the production time is long, and product yield is also low.And mainly contain acid-base method, enzyme process and Hot water extraction at present.Its object is all make fish-skin swelling by process in early stage, removes residual meat, fat and pigment, extracts collagen.Different skin tissue structure is different, and soak time is also different, and some immersion reaches several days time, and production efficiency reduces greatly, and long immersion also requires to be in for a long time in low temperature environment to delay molten the going bad of fish-skin.Production cycle is long, and power consumption is large.
Summary of the invention
For the deficiency that prior art exists, the invention provides a kind of utilization of materials high, improve product extraction yield, the extracting method of Mahi loach fish corner material collagen protein that leaching process pollutes little, environmental protection.
For achieving the above object, the invention provides following technical scheme: a kind of extracting method of Mahi loach fish corner material collagen protein, it is characterized in that: extraction step is as follows: with fish-skin, fish-bone and fin in Mahi loach fish for raw material, a, adopt specific equipment to pulverize raw material; Raw material after pulverizing is watered, makes it to become slurries; B, to add in slurries acid material implement acidolysis; C, to after acidolysis slurries implement ultrasonication; D, slurries implement lixiviate after ultrasonication; E, filtration; F, desalination; G, freezing; H, drying.
Wherein, the specific equipment in step a is pulverizer; Being blended into the water pulverized in raw material in step b is 3-8:1 with the ratio of pulverizing raw material; In step c, the time of ultrasonication is 0.5-3h; The time of lixiviate is 3-8h; Acid material in steps d is citric acid; Filtration in step e adopts strainer, the upper strata oil layer in slurries and sedimentable matter is implemented to filter, forms the acid solution containing collagen protein; Desalination in step f is by the acid solution containing collagen protein, respectively by purpose ceramic-film filter and nanofiltration membrane desalination; Freezing temp in step g is subzero 30 DEG C; Temperature dry in step h is 8-15 DEG C.
Adopt technique scheme, the fish-skin of Mahi loach fish, fish-bone and fin is adopted to be raw material, the waste material of Mahi loach fish is effectively utilized, energy-conservation, ultrasonication is carried out to the slurries after acidolysis, the strong cavitation effect utilizing Ultrasonic Radiation pressure to produce, mechanical vibration, disturbance effect, high acceleration, emulsification, spread, smash and the multistage effects such as stirring action, increase molecular motion of material frequency and speed, increase solvent penetration power, thus accelerate being separated of the swelling and impurity of fish-skin, promote the carrying out that collagen protein extracts; And adopt the slurries after ultrasonication only to need lixiviate 3-8h, substantially reduce the extraction time of collagen protein, improve the speed of extraction, make the extraction efficiency of product be improved, output also improves simultaneously thereupon; Adopt ultrasonication to pollute little, greatly can reduce the pollution to environment, environmental protection and energy saving.
The present invention is set to further: raw material, before pulverizing, adopts cutter to be cut to segment.
Adopt technique scheme, be conducive to after operation like this implementing to pulverize to raw material, make the raw material of pulverizing more tiny, thus for convenience of providing place mat to the extraction of collagen protein.
The present invention is further set to: in Mahi loach fish, fish-skin, fish-bone and fin are freezing raw material.
Adopt technique scheme, arranging like this is in order to a large amount of enforcement is produced, and conveniently implements to assemble to a large amount of raw materials, then implements on a large scale to produce, not only can reduce production cost, and facilitate processing.
Embodiment
An extracting method for Mahi loach fish corner material collagen protein, its corner material is other material of removing flesh of fish part, and extraction step is as follows: with fish-skin, fish-bone and fin in Mahi loach fish for raw material, a, adopts specific equipment to pulverize raw material; Raw material after pulverizing is watered, makes it to become slurries; B, to add in slurries acid material implement acidolysis; C, to after acidolysis slurries implement ultrasonication; D, slurries implement lixiviate after ultrasonication; E, filtration; F, desalination; G, freezing; H, drying.Specific equipment in step a is pulverizer; Being blended into the water pulverized in raw material in step b is 3-8:1 with the ratio of pulverizing raw material; In step c, the time of ultrasonication is 0.5-3h; The time of lixiviate is 3-8h; Acid material in steps d is citric acid; Filtration in step e adopts strainer, the upper strata oil layer in slurries and sedimentable matter is implemented to filter, forms the acid solution containing collagen protein; Desalination in step f is by the acid solution containing collagen protein, respectively by purpose ceramic-film filter and nanofiltration membrane desalination; Freezing temp in step g is subzero 30 DEG C; Temperature dry in step h is 8-15 DEG C.The fish-skin of Mahi loach fish, fish-bone and fin is adopted to be raw material, the waste material of Mahi loach fish is effectively utilized, energy-conservation, ultrasonication is carried out to the slurries after acidolysis, the strong cavitation effect utilizing Ultrasonic Radiation pressure to produce, mechanical vibration, disturbance effect, high acceleration, emulsification, spread, smash and the multistage effects such as stirring action, increase molecular motion of material frequency and speed, increase solvent penetration power, thus accelerate being separated of the swelling and impurity of fish-skin, promote the carrying out that collagen protein extracts; And adopt the slurries after ultrasonication only to need lixiviate 3-8h, substantially reduce the extraction time of collagen protein, improve the speed of extraction, make the extraction efficiency of product be improved, output also improves simultaneously thereupon; Adopt ultrasonication to pollute little, greatly can reduce the pollution to environment, environmental protection and energy saving.
In order to make the raw material of pulverizing more tiny, ensure the extraction completely of collagen protein, raw material, before pulverizing, adopts cutter to be cut to segment.In order to a large amount of enforcement is produced, convenient to a large amount of raw materials enforcement gathering, then implement on a large scale to produce, in Mahi loach fish, fish-skin, fish-bone and fin are freezing raw material, so not only can reduce production cost, and facilitate processing.
In the embodiment of the present invention 1, by freezing Mahi loach fish waste, cut into pieces, put into crusher for crushing, after pulverizing, the ratio of adding water is fish-skin: water is 1:5, slurry enters in acidolysis cylinder, citric acid is added in slurry, the content of citric acid in slurry is made to be 0.3M, be that 150w carries out assisted extraction 1h at ultrasonic power, keep slurry temperature lower than 40 DEG C in leaching process, utilize the strong cavitation effect that Ultrasonic Radiation pressure produces, mechanical vibration, disturbance effect, high acceleration, emulsification, diffusion, smash and the multistage effects such as stirring action, increase molecular motion of material frequency and speed, increase solvent penetration power, thus accelerate being separated of the swelling and impurity of fish-skin, promote the carrying out that collagen protein extracts.Lixiviate 6h again after ultrasonication, the slurries after extraction carry out centrifuging, and removing upper strata oil layer and sedimentable matter, be the acid solution containing collagen protein.Neutralization is containing the acid solution of collagen protein, and respectively by purpose ceramic-film filter and nanofiltration membrane desalination, filtered liquid lyophilize, obtains collagen protein.
In the embodiment of the present invention 2, by freezing Mahi loach fish waste, cut into pieces, put into crusher for crushing, after pulverizing, the ratio of adding water is fish-skin: water is 1:3, slurry enters in acidolysis cylinder, citric acid is added in slurry, the content of citric acid in slurry is made to be 0.5M, be that 180w carries out assisted extraction 1h at ultrasonic power, keep slurry temperature lower than 40 DEG C in leaching process, utilize the strong cavitation effect that Ultrasonic Radiation pressure produces, mechanical vibration, disturbance effect, high acceleration, emulsification, diffusion, smash and the multistage effects such as stirring action, increase molecular motion of material frequency and speed, increase solvent penetration power, thus accelerate being separated of the swelling and impurity of fish-skin, promote the carrying out that collagen protein extracts.Lixiviate 6h again after ultrasonication, the slurries after extraction carry out centrifuging, and removing upper strata oil layer and sedimentable matter, be the acid solution containing collagen protein.Neutralization is containing the acid solution of collagen protein, and respectively by purpose ceramic-film filter and nanofiltration membrane desalination, filtered liquid lyophilize, obtains collagen protein.
Following chart is the collagen content that the embodiment of the present invention 1 and 2 is produced.
| Batch | Embodiment one | Embodiment two |
| Mahi loach fish skin raw material quality (g) | 100±0.01 | 100±0.01 |
| Extract quality product (g) | 20.762 | 16.106 |
| Product hydroxyproline content (%) | 3.3370 | 2.3676 |
| Product collagen protein purity mean value (%) | 92.37 | 91.25 |
| Collagen protein extraction yield (%) | 20.76 | 16.11 |
Claims (5)
1. an extracting method for Mahi loach fish corner material collagen protein, is characterized in that: extraction step is as follows: with fish-skin, fish-bone and fin in Mahi loach fish for raw material, a, adopts specific equipment to pulverize raw material; Raw material after pulverizing is watered, makes it to become slurries; B, to add in slurries acid material implement acidolysis; C, to after acidolysis slurries implement ultrasonication; D, slurries implement lixiviate after ultrasonication; E, filtration; F, desalination; G, freezing; H, drying.
2. the extracting method of Mahi loach fish corner material collagen protein according to claim 1, is characterized in that: the specific equipment in step a is pulverizer; Being blended into the water pulverized in raw material in step b is 3-8:1 with the ratio of pulverizing raw material; In step c, the time of ultrasonication is 0.5-3h; The time of lixiviate is 3-8h; Acid material in steps d is citric acid; Filtration in step e adopts strainer, the upper strata oil layer in slurries and sedimentable matter is implemented to filter, forms the acid solution containing collagen protein; Desalination in step f is by the acid solution containing collagen protein, respectively by purpose ceramic-film filter and nanofiltration membrane desalination; Freezing temp in step g is subzero 30 DEG C; Temperature dry in step h is 8-15 DEG C.
3. the extracting method of Mahi loach fish corner material collagen protein according to claim 1 and 2, is characterized in that: described raw material, before pulverizing, adopts cutter to be cut to segment.
4. the extracting method of Mahi loach fish corner material collagen protein according to claim 1 and 2, is characterized in that: in described Mahi loach fish, fish-skin, fish-bone and fin are freezing raw material.
5. the extracting method of Mahi loach fish corner material collagen protein according to claim 3, is characterized in that: in described Mahi loach fish, fish-skin, fish-bone and fin are freezing raw material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510162420.4A CN104774257A (en) | 2015-04-08 | 2015-04-08 | Method for extracting collagen from Mahi-mahi leftovers |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510162420.4A CN104774257A (en) | 2015-04-08 | 2015-04-08 | Method for extracting collagen from Mahi-mahi leftovers |
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| CN104774257A true CN104774257A (en) | 2015-07-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201510162420.4A Pending CN104774257A (en) | 2015-04-08 | 2015-04-08 | Method for extracting collagen from Mahi-mahi leftovers |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108208847A (en) * | 2018-01-17 | 2018-06-29 | 温州科技职业学院 | The preparation method of the compound calcium powder of ocean source amino acid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101735304A (en) * | 2008-11-26 | 2010-06-16 | 大连隆合海洋生物工程技术有限公司 | Method for preparing water-based collagen of codfish skin by ultrasound wave extraction |
| CN102690853A (en) * | 2012-03-22 | 2012-09-26 | 浙江省海洋开发研究院 | Preparation method of sleeve-fish skin low-molecular-weight collagen peptide |
| CN103627761A (en) * | 2013-10-22 | 2014-03-12 | 浙江省海洋开发研究院 | Method for preparing collagen peptide rich in hydroxyproline |
-
2015
- 2015-04-08 CN CN201510162420.4A patent/CN104774257A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101735304A (en) * | 2008-11-26 | 2010-06-16 | 大连隆合海洋生物工程技术有限公司 | Method for preparing water-based collagen of codfish skin by ultrasound wave extraction |
| CN102690853A (en) * | 2012-03-22 | 2012-09-26 | 浙江省海洋开发研究院 | Preparation method of sleeve-fish skin low-molecular-weight collagen peptide |
| CN103627761A (en) * | 2013-10-22 | 2014-03-12 | 浙江省海洋开发研究院 | Method for preparing collagen peptide rich in hydroxyproline |
Non-Patent Citations (1)
| Title |
|---|
| 任俊凤等: "河豚鱼皮胶原蛋白肽的提取及其抗氧化活性的研究", 《中国食品学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108208847A (en) * | 2018-01-17 | 2018-06-29 | 温州科技职业学院 | The preparation method of the compound calcium powder of ocean source amino acid |
| CN108208847B (en) * | 2018-01-17 | 2021-02-26 | 温州科技职业学院 | Preparation method of marine-source amino acid compound calcium powder |
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Address after: 325000 Wenzhou science and Technology Park incubator, No. 38, Dongfang South Road, Ouhai, Zhejiang, China Applicant after: Wenzhou Vocational College of Science and Technology Address before: 325000 Hongqiao Road, Ouhai District, Zhejiang, No. six, No. 1000, No. Applicant before: Wenzhou Vocational College of Science and Technology |
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Application publication date: 20150715 |