CN104498568A - Method for preparing fish-skin collagen powder by use of fresh fish skin - Google Patents
Method for preparing fish-skin collagen powder by use of fresh fish skin Download PDFInfo
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Abstract
The invention relates to a method for preparing a fish-skin collagen powder by the use of fresh fish skin. The method comprises the following steps: fresh fish skin is selected as a raw material and is immersed in sodium hydroxide, the fresh skin is washed with water to neutral pH after fat and impure protein on the surface of the fish skin are removed, and crushing is carried out; drinking water and edible vinegar are added to the crushed fish skin and uniform agitation is carried out, ultrasonication and deodorization treatments are carried out, and papain is added to carry out controlled-enzymatic hydrolysis so as to obtain a fish-skin enzymatic hydrolysate; active carbon is added for decarburization clarification after enzyme deactivation, filtration is carried out, and a filtrate undergoes concentration and spray drying so as to obtain the fish-skin collagen powder. By ultrasonication of the fish skin, active ingredients in acetic acid are activated to react with fishy smell substances in the fish skin so as to remove the fishy smell. By adding active carbon into the enzymatic hydrolysate to carry out decarburization clarification for fishy smell elimination and decoloration, the prepared fish-skin collagen powder has no fishy smell. The method provided by the invention has advantages of advanced technology, reasonable process and controllable operation, and is suitable for large-scale production.
Description
Technical field
The present invention relates to the preparation of protein, especially a kind of method utilizing fresh fish leather to get collagen of fish skin powder.
Background technology
We know, the raw materials of collagen protein, mainly from mammiferous bone, skin etc., due to pestilence in animal in recent years, brings very large threat to the mankind, as mad cow disease, foot and mouth disease, bird flu etc., causes people to the fear of collagen product.Thus, the marine organisms collagen from ocean is popular in vain.
At present, the research of extracting collagen protein from fish-skin is a lot, and general technology all includes the processing steps such as process to raw material, enzymolysis, filtration, concentrated and spraying dry.Such as, disclosed 200910131265.4, No. 201310064690.2 applications for a patent for invention.But containing a large amount of bad smell material in fish-skin, its Producing reason is organic chemicals methylamine because fish exists with it and homologue dimethylamine, Trimethylamine 99 etc., and traditional production technique is difficult to remove methylamine and homologue dimethylamine, Trimethylamine 99.These materials are not removed in leaching process, can have a strong impact on local flavor and the purity of final collagen product.
How to solve the bad smell in collagen of fish skin, the quality improving collagen product is a problem demanding prompt solution.
Summary of the invention
In order to overcome the bad smell material that contains in fish-skin in prior art and cause the deficiency of the smell difference of collagen product, the invention provides a kind of technique advanced person, the operation fresh fish leather that utilizes that is reasonable, easy controlled operation gets the method for collagen of fish skin powder, the collagen of fish skin powder that employing the method is produced is without bad smell.
The technical solution adopted for the present invention to solve the technical problems is: a kind of method utilizing fresh fish leather to get collagen of fish skin powder, is characterized in that: through following process steps:
(1), the choosing and process of raw material
Choosing free of contamination fresh fish skin is raw material, for subsequent use;
(2), the removal of impurities of alkali bubble, break process
The fresh fish skin chosen in step (1) is sent into stirred pot, adds calcium hydroxide while stirring and regulate PH to be 10 ~ 14, soak 3 ~ 5 days, remove fat and the foreign protein on fish-skin surface; Then will remove the fish-skin clear water soaking flushing of fat and foreign protein, be washed till pH value for neutral, then carry out break process;
(3), ultrasonic wave, except raw meat process
Fish-skin after break process in step (2) is added tap water, edible vinegar, mixture is carried out ultrasonication, remove the fishy smell of fish-skin; Wherein, the consumption of described tap water is 3 ~ 8 times of fresh fish tare weight amount; The add-on of described edible vinegar is 0.5 ~ 1.5% of fresh fish tare weight amount; Described hyperacoustic intensity control is at 700 ~ 800 watts/liter, and described hyperacoustic treatment time is 10 ~ 90 minutes;
(4), enzymolysis
By middle for step (3) ultrasonic wave, except the fish-skin feeding enzymatic vessel after raw meat process, regulate Ph value 5.0 ~ 8.0, control temperature 40 DEG C ~ 60 DEG C, adds papoid, constant temperature enzymolysis 1 ~ 10 hour, obtained fish-skin enzymolysis solution; Wherein, the use enzyme amount of described papoid is 1 ~ 5% of fresh fish tare weight amount;
(5) go out enzyme
Fish-skin enzymolysis solution obtained in step (4) is heated to 80 ~ 100 DEG C, is incubated 10 ~ 45 minutes, carries out going out ferment treatment, obtain the fish-skin enzymolysis solution of enzyme-deactivating;
(6) carbon takes off, filters
Fish-skin enzymolysis solution after the enzyme-deactivating of gained in step (5) is sent into carbon and takes off tank, add the gac of its weight 1 ~ 5%, be warming up to 80 ~ 90 DEG C, be incubated 30 ~ 60 minutes, carry out the de-clarification of carbon, filter, obtain collagen of fish skin filtered liquid;
(7) concentrated, spraying dry
The collagen of fish skin filtered liquid obtained in step (6) is concentrated, then sends in spray-dryer and carry out spraying dry, obtain collagen of fish skin powder.
Described edible vinegar is one or more in Shanxi mature vinegar, zhenjiang vinegar, Sichuan bran vinegar, Zhejiang rose vinegar.
Described sodium hydroxide is food grade sodium hydroxide.
Filter-cloth filtering or centrifuging is filtered into after described collagen of fish skin clear liquid carbon takes off clarification.
Described centrifuging is the rotating speed of control whizzer is 4000rpm ~ 20000rpm, and centrifugation time is 5 ~ 15 minutes.
Described spray-dired working conditions is: inlet temperature is 200 ~ 230 DEG C, and temperature out is 82 ~ 85 DEG C, and atomizing disk rotating speed is located at 48Hz, and in tower, negative pressure is at 8 ~ 10Pa.
The present invention is that to choose free of contamination fresh fish skin be raw material, and by soaking with sodium hydroxide, after the fat removing fish-skin surface and foreign protein, it is neutral for being washed till pH value with clear water, broken; After fish-skin after fragmentation adds tap water, edible vinegar, carry out ultrasonic wave, except raw meat process; Ultrasonic wave carries out control enzyme enzymolysis except the fish-skin after raw meat process adds papoid, obtains fish-skin enzymolysis solution; Enzymolysis solution goes out and adds gac after enzyme and carry out the de-clarification of carbon, filters, obtains collagen of fish skin filtered liquid; Collagen of fish skin filtered liquid, through concentrated, spraying dry, obtains collagen of fish skin powder.The present invention adopts ultrasonic technology and biological enzyme control degradation technology to carry out Combined Processing to the fish-skin after removal foreign protein, wherein, when ultrasonic wave is propagated in media as well, heat effect can be produced, mechanical effect or cavitation effect, utilize ultrasonication effect can break up tissue and the cytolemma of decomposition fish-skin, excite fishy smell material methylamine and homologue dimethylamine thereof in effective constituent in acetic acid and fish-skin, Trimethylamine 99 reacts, remove the fishy smell in fish-skin, make fish-skin albumen fully come out simultaneously, namely biological enzyme and protein contacts is conducive to, thus raising enzymolysis efficiency, the dipping pretreatment time of fish-skin can be shortened again, and the degraded of biological enzyme to fish-skin albumen has selectivity and the specificity of height, action condition is gentle, and reaction easily controls, and can retain the nutritive ingredient in raw material well, rich in protein in fish-skin is converted into the collagen protein of human body absorption easy to digest, add the de-clarification of carbon that gac carries out de-raw meat, decolouring in fish-skin enzymolysis solution, eliminate the bad smell in fish-skin enzymolysis solution further.Present invention process is advanced, and operation is reasonable, and operate controlled, be suitable for large-scale production, the collagen of fish skin powder produced, without bad smell, expands the scope of application.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
embodiment 1
Fresh fish leather is utilized to get a method for collagen of fish skin powder, through following process steps:
(1), the choosing and process of raw material
Choosing free of contamination fresh fish skin is raw material, for subsequent use;
Choose commercially available qualified Shanxi mature vinegar, food grade sodium hydroxide, for subsequent use;
(2), the removal of impurities of alkali bubble, break process
Send the fresh fish skin chosen in step (1) to stirred pot, add while stirring in step (1) and choose food-grade calcium hydroxide and regulate pH value to be 12, soaks 4 days, the removal fat on fish-skin surface and foreign protein; Then the fish-skin clear water removing fat and foreign protein is soaked, rinses, be washed till pH value for neutral, then carry out break process;
(3), ultrasonic wave is except raw meat process
Fish-skin after break process in step (2) is added Shanxi mature vinegar selected in the tap water of fresh fish tare weight amount 5 times, step (1), mixture is carried out ultrasonication 50 minutes, by fish-skin sonolysis, break up tissue and the cytolemma of fish-skin, and to excite in the effective constituent in acetic acid and fish-skin fishy smell material methylamine and homologue dimethylamine thereof, Trimethylamine 99 reacts, and removes the fishy smell in fish-skin; Wherein, the add-on of Shanxi mature vinegar is 1% of fresh fish tare weight amount; Ultrasonic intensity controls at 750 watts/liter;
(4), enzymolysis
By ultrasonic wave in step (3) except the fish-skin after raw meat process sends into enzymatic vessel, regulate Ph value 6.5, control temperature 50 DEG C, adds the papoid of fresh fish tare weight amount 3%, constant temperature enzymolysis 5 hours, obtained fish-skin enzymolysis solution;
(5) go out enzyme
Fish-skin enzymolysis solution obtained in step (4) is heated to 90 DEG C, is incubated 30 minutes, carries out going out ferment treatment, obtain the fish-skin enzymolysis solution of enzyme-deactivating;
(6) carbon takes off, filters
Fish-skin enzymolysis solution after the enzyme-deactivating of gained in step (5) is sent into carbon and takes off tank, add the gac of its weight 3%, be warming up to 85 DEG C, be incubated and within 45 minutes, carry out the de-clarification of carbon, the rotating speed entering centrifugal filter control whizzer is 4000rpm, filter 15 minutes, obtain collagen of fish skin filtered liquid;
(7) concentrated, spraying dry
The collagen of fish skin filtered liquid obtained in step (6) is concentrated, then sends in spray-dryer and carry out spraying dry, obtain collagen of fish skin powder; Spray-dired working conditions is: inlet temperature is 215 DEG C, and temperature out is 83 DEG C, and atomizing disk rotating speed is located at 48Hz, and in tower, negative pressure is at 9Pa.
What the present embodiment provided utilizes fresh fish leather to get in the method for collagen of fish skin powder, removing the fish-skin after foreign protein adopts ultrasonic wave and bio-enzyme degradation technology to carry out Combined Processing, the tissue of sonolysis fish-skin and cytolemma, and excite fishy smell material methylamine and homologue dimethylamine thereof in effective constituent in acetic acid and fish-skin, Trimethylamine 99 reacts, remove the fishy smell in fish-skin, make fish-skin albumen fully come out simultaneously, be beneficial to biological enzyme and protein contacts, improve enzymolysis efficiency, in fish-skin, rich in protein is converted into the collagen protein of human body absorption easy to digest, add the de-clarification of carbon that gac carries out de-raw meat, decolouring in fish-skin enzymolysis solution, eliminate the bad smell in fish-skin enzymolysis solution further.Its technique is advanced, and operation is reasonable, and operate controlled, be suitable for large-scale production, the collagen of fish skin powder produced, without bad smell, expands the scope of application.
embodiment 2
Fresh fish leather is utilized to get a method for collagen of fish skin powder, through following process steps:
(1), the choosing and process of raw material
Choosing free of contamination fresh fish skin is raw material, for subsequent use;
Choose commercially available qualified zhenjiang vinegar, Sichuan bran vinegar, in 1 ︰ 1 ratio mixing; Choose food grade sodium hydroxide, for subsequent use;
(2), the removal of impurities of alkali bubble, break process
The fresh fish skin chosen in step (1) is sent into stirred pot, adds while stirring in step (1) and choose food-grade calcium hydroxide and regulate pH value to be 10, soaks 5 days, the fat on removal fish-skin surface and foreign protein; Then will remove the fish-skin clear water soaking flushing of fat and foreign protein, be washed till pH value for neutral, then carry out break process;
(3), ultrasonic wave is except raw meat process
Fish-skin after break process in step (2) is added the mixed edible vinegar produced in the tap water of fresh fish tare weight amount 8 times, step (1), mixture is carried out ultrasonication 10 minutes, by fish-skin while carrying out sonolysis, to excite in the effective constituent in acetic acid and fish-skin fishy smell material methylamine and homologue dimethylamine thereof, Trimethylamine 99 reacts, remove the fishy smell of fish-skin; Wherein, edible vinegar add that total amount is fresh fish tare weight amount 1.5%; Ultrasonic intensity controls at 800 watts/liter;
(4), enzymolysis
By ultrasonic wave in step (3) except the fish-skin after raw meat process sends into enzymatic vessel, regulate Ph value 5.0, control temperature 60 DEG C, adds the papoid of fresh fish tare weight amount 5%, constant temperature enzymolysis 1 hour, obtained fish-skin enzymolysis solution;
(5) go out enzyme
Fish-skin enzymolysis solution obtained in step (4) is heated to 80 DEG C, is incubated 45 minutes, carries out going out ferment treatment, obtain the fish-skin enzymolysis solution of enzyme-deactivating;
(6) carbon takes off, filters
Fish-skin enzymolysis solution after the enzyme-deactivating of gained in step (5) is sent into carbon and takes off tank, add the gac of its weight 1%, be warming up to 90 DEG C, be incubated and within 60 minutes, carry out the de-clarification of carbon, filter-cloth filtering, obtains collagen of fish skin filtered liquid;
(7) concentrated, spraying dry
The collagen of fish skin filtered liquid obtained in step (6) is concentrated, then sends in spray-dryer and carry out spraying dry, obtain collagen of fish skin powder; Spray-dired working conditions is: inlet temperature is 200 DEG C, and temperature out is 85 DEG C, and atomizing disk rotating speed is located at 48Hz, and in tower, negative pressure is at 8Pa.
What the present embodiment provided utilizes fresh fish leather to get in the method for collagen of fish skin powder, when carrying out super ripple process to fish-skin, to excite in the effective constituent in edible vinegar and fish-skin fishy smell material methylamine and homologue dimethylamine thereof, Trimethylamine 99 reacts, remove the fishy smell in fish-skin; Add the de-clarification of carbon that gac carries out de-raw meat, decolouring in fish-skin enzymolysis solution, eliminate the bad smell in fish-skin enzymolysis solution further, make the collagen of fish skin powder produced without bad smell.Fish-skin is after carrying out ultrasonication, and fish-skin albumen fully comes out, and is beneficial to biological enzyme and protein contacts, improves enzymolysis efficiency.The preparation method technique that the present embodiment provides is advanced, and operation is reasonable, operates controlled, is suitable for large-scale production.
embodiment 3
Fresh fish leather is utilized to get a method for collagen of fish skin powder, through following process steps:
(1), the choosing and process of raw material
Choosing free of contamination fresh fish skin is raw material, for subsequent use;
Select commercially available qualified Zhejiang rose vinegar, food grade sodium hydroxide, for subsequent use;
(2), the removal of impurities of alkali bubble, break process
The fresh fish skin chosen in step (1) is sent into stirred pot, adds the food-grade calcium hydroxide chosen in step (1) while stirring and regulate pH value to be 14, soak 3 days, remove fat and the foreign protein on fish-skin surface; Then the fish-skin clear water removing fat and foreign protein is soaked, rinses, be washed till pH value for neutral, then carry out break process;
(3), ultrasonic wave is except raw meat process
Fish-skin after break process in step (2) is added Zhejiang rose vinegar selected in the tap water of fresh fish tare weight amount 3 times, step (1), mixture is carried out ultrasonication 90 minutes, by fish-skin while carrying out sonolysis, remove the fishy smell of fish-skin; Wherein, Zhejiang rose vinegar add that total amount is fresh fish tare weight amount 0.5%; Ultrasonic intensity controls at 700 watts/liter;
(4), enzymolysis
By ultrasonic wave in step (3) except the fish-skin after raw meat process sends into enzymatic vessel, regulate Ph value 8.0, control temperature 40 DEG C, adds the papoid of fresh fish tare weight amount 1%, constant temperature enzymolysis 10 hours, obtained fish-skin enzymolysis solution;
(5) go out enzyme
Fish-skin enzymolysis solution obtained in step (4) is heated to 100 DEG C, is incubated 10 minutes, the ferment treatment that carries out going out obtains the fish-skin enzymolysis solution of enzyme-deactivating;
(6) carbon takes off, filters
Fish-skin enzymolysis solution after the enzyme-deactivating of gained in step (5) is sent into carbon and takes off tank, add the gac of its weight 5%, be warming up to 80 DEG C, be incubated and within 30 minutes, carry out the de-clarification of carbon, the rotating speed entering centrifugal filter control whizzer is 20000rpm, filter 5 minutes, obtain collagen of fish skin filtered liquid;
(7) concentrated, spraying dry
The collagen of fish skin filtered liquid obtained in step (6) is concentrated, then sends in spray-dryer and carry out spraying dry, obtain collagen of fish skin powder; Spray-dired working conditions is: inlet temperature is 230 DEG C, and temperature out is 82 DEG C, and atomizing disk rotating speed is located at 48Hz, and in tower, negative pressure is at 10Pa.
What the present embodiment provided utilizes fresh fish leather to get the method for collagen of fish skin powder, and in the effective constituent of fish-skin in ultrasonic excitation acetic acid and fish-skin, fishy smell material reacts, and removes fishy smell; Add the de-clarification of carbon that gac carries out de-raw meat, decolouring in its enzymolysis solution, the collagen of fish skin powder produced is without bad smell.Its preparation method technique is advanced, and operation is reasonable, operates controlled, is suitable for large-scale production.
Claims (6)
1. utilize fresh fish leather to get a method for collagen of fish skin powder, it is characterized in that: through following process steps:
(1), the choosing and process of raw material
Choosing free of contamination fresh fish skin is raw material, for subsequent use;
(2), the removal of impurities of alkali bubble, break process
The fresh fish skin chosen in step (1) is sent into stirred pot, adds calcium hydroxide while stirring and regulate PH to be 10 ~ 14, soak 3 ~ 5 days, remove fat and the foreign protein on fish-skin surface; Then will remove the fish-skin clear water soaking flushing of fat and foreign protein, be washed till pH value for neutral, then carry out break process;
(3), ultrasonic wave, except raw meat process
Fish-skin after break process in step (2) is added tap water, edible vinegar, mixture is carried out ultrasonication, remove the fishy smell of fish-skin; Wherein, the consumption of described tap water is 3 ~ 8 times of fresh fish tare weight amount; The add-on of described edible vinegar is 0.5 ~ 1.5% of fresh fish tare weight amount; Described hyperacoustic intensity control is at 700 ~ 800 watts/liter, and described hyperacoustic treatment time is 10 ~ 90 minutes;
(4), enzymolysis
By middle for step (3) ultrasonic wave, except the fish-skin feeding enzymatic vessel after raw meat process, regulate Ph value 5.0 ~ 8.0, control temperature 40 DEG C ~ 60 DEG C, adds papoid, constant temperature enzymolysis 1 ~ 10 hour, obtained fish-skin enzymolysis solution; Wherein, the use enzyme amount of described papoid is 1 ~ 5% of fresh fish tare weight amount;
(5) go out enzyme
Fish-skin enzymolysis solution obtained in step (4) is heated to 80 ~ 100 DEG C, is incubated 10 ~ 45 minutes, carries out going out ferment treatment, obtain the fish-skin enzymolysis solution of enzyme-deactivating;
(6) carbon takes off, filters
Fish-skin enzymolysis solution after the enzyme-deactivating of gained in step (5) is sent into carbon and takes off tank, add the gac of its weight 1 ~ 5%, be warming up to 80 ~ 90 DEG C, be incubated 30 ~ 60 minutes, carry out the de-clarification of carbon, filter, obtain collagen of fish skin filtered liquid;
(7) concentrated, spraying dry
The collagen of fish skin filtered liquid obtained in step (6) is concentrated, then sends in spray-dryer and carry out spraying dry, obtain collagen of fish skin powder.
2. a kind of method utilizing fresh fish leather to get collagen of fish skin powder according to claim 1, is characterized in that: described edible vinegar is one or more in Shanxi mature vinegar, zhenjiang vinegar, Sichuan bran vinegar, Zhejiang rose vinegar.
3. a kind of method utilizing fresh fish leather to get collagen of fish skin powder according to claim 1, is characterized in that: described sodium hydroxide is food grade sodium hydroxide.
4. a kind of method utilizing fresh fish leather to get collagen of fish skin powder according to claim 1, is characterized in that: be filtered into filter-cloth filtering or centrifuging after described collagen of fish skin clear liquid carbon takes off clarification.
5. a kind of method utilizing fresh fish leather to get collagen of fish skin powder according to claim 4, is characterized in that: described centrifuging is the rotating speed of control whizzer is 4000rpm ~ 20000rpm, and centrifugation time is 5 ~ 15 minutes.
6. a kind of method utilizing fresh fish leather to get collagen of fish skin powder according to claim 1, it is characterized in that: described spray-dired working conditions is: inlet temperature is 200 ~ 230 DEG C, temperature out is 82 ~ 85 DEG C, and atomizing disk rotating speed is located at 48Hz, and in tower, negative pressure is at 8 ~ 10Pa.
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CN110564796A (en) * | 2019-07-13 | 2019-12-13 | 德州蓝力生物技术有限公司 | Production process of hydrolyzed collagen |
CN110236083A (en) * | 2019-07-25 | 2019-09-17 | 湛江千护宝生物有限公司 | A kind of preparation method rich in the instant fish-skin of collagen |
CN113201064A (en) * | 2020-10-09 | 2021-08-03 | 海南翔泰生物科技有限公司 | Method for preparing fish skin collagen powder from fresh fish skin |
WO2023040084A1 (en) * | 2021-09-16 | 2023-03-23 | 海南三元星生物科技股份有限公司 | Method for extracting collagen tripeptide and prepared collagen tripeptide |
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