CN116640519A - Fish skin gelatin extraction method - Google Patents

Fish skin gelatin extraction method Download PDF

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Publication number
CN116640519A
CN116640519A CN202310481350.3A CN202310481350A CN116640519A CN 116640519 A CN116640519 A CN 116640519A CN 202310481350 A CN202310481350 A CN 202310481350A CN 116640519 A CN116640519 A CN 116640519A
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China
Prior art keywords
fish skin
gelatin
skin
solution
concentration
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CN202310481350.3A
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Inventor
马华威
潘传燕
罗旭
吕敏
张文敏
阮秋凤
陈伟介
王维生
杨琼
王园园
王卉
高雪梅
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Guangxi Xiaoyanren Biotechnology Co ltd
Guangxi Academy of Fishery Sciences
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Guangxi Xiaoyanren Biotechnology Co ltd
Guangxi Academy of Fishery Sciences
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Priority to CN202310481350.3A priority Critical patent/CN116640519A/en
Publication of CN116640519A publication Critical patent/CN116640519A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09HPREPARATION OF GLUE OR GELATINE
    • C09H1/00Pretreatment of collagen-containing raw materials for the manufacture of glue
    • C09H1/04Pretreatment of collagen-containing raw materials for the manufacture of glue of hides, hoofs, or leather scrap
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09HPREPARATION OF GLUE OR GELATINE
    • C09H3/00Isolation of glue or gelatine from raw materials, e.g. by extracting, by heating

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Meat, Egg Or Seafood Products (AREA)
  • Peptides Or Proteins (AREA)

Abstract

The invention discloses a method for extracting fishskin gelatin, which comprises the steps of cleaning fresh fishskin, draining water, soaking for 10-15h by using NaOH solution, and expanding for 3h by using glacial acetic acid; soaking the fish skin for 3-5h by adopting a tannin solution; placing the fish skin in a microwave digestion instrument for treatment; adding fish skin, salt water and citric acid into an enzymolysis tank, heating to 40-45 ℃, regulating the pH of the solution to 2.0-3.0, adding pepsin, and stirring for 1-1.5h for homogenizing; adding distilled water into the fish skin, homogenizing in water bath at 50-55deg.C for 5-6 hr; pouring the slurry into a container, decocting for 30-60min, and standing at 0-4deg.C for 8-10 hr to obtain gelatin product. The fish skin gelatin extracted by the extraction method disclosed by the invention is subjected to enzymolysis and heat treatment after microwave digestion, so that the gelatin micro-network structure prepared from the fish skin can be changed, the surface pore size is uniform, the crosslinking degree is good, the arrangement is compact, and the problem of low gelatin yield caused by excessive hydrolysis is solved.

Description

Fish skin gelatin extraction method
Technical Field
The invention relates to the technical field of biological extraction, in particular to a method for extracting fishskin gelatin.
Background
Gelatin is a denatured product of collagen partial hydrolysis, fish skin is an important source of gelatin, fish gelatin has the technical problems of poor quality, poor rheological property and poor gel property and the like compared with mammalian gelatin, because the content of amino acids (proline and hydroxyproline) in the fish skin is obviously lower than that of mammals, the difference of thermal stability, gel strength, viscosity, emulsifying property and the like of the fish skin gelatin and terrestrial animal gelatin is caused, and the extraction of gelatin from the fish skin is a good way for reutilizing aquatic byproducts and developing high-value gelatin products.
Common methods for extracting fish skin gelatin include thermal extraction, acid extraction, salt extraction, protease extraction, etc. The extraction process affects the mechanism of gelatin formation. The heat extraction process disrupts the stability of the triple helix structure, causing the helix to turn into a coil and form soluble gelatin by disrupting hydrogen and covalent bonds. The acid breaks the triple helix structure of collagen by breaking the acid-proof cross-linking and triple helix amide bond of the terminal peptide region and the intramolecular and intermolecular non-covalent bond, and the gelatin obtained by the acid method has low purity and poor quality. The degradation of gelatin can be reduced by trypsin extraction of salmon skin gelatin, the hydrolysis degree is difficult to control in the process, the emulsifying property and the gel strength of the obtained gelatin cannot reach the expected effect, the production cost is high, and the industrial production is difficult to popularize.
Disclosure of Invention
The invention provides an extraction method of fishskin gelatin for solving the technical problems.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the extraction method of the fishskin gelatin is characterized by comprising the following steps of:
(1) Pretreatment: cleaning fresh fish skin, draining, soaking in NaOH solution for 10-15 hr, and expanding with glacial acetic acid for 3 hr;
(2) Soaking the fishskin in the step (1) for 3-5h by adopting a tannin solution; placing the fish skin in a microwave digestion instrument for treatment;
(3) Adding the fish skin treated in the step (2), brine and citric acid into an enzymolysis tank, heating to 40-45 ℃, regulating the pH value of the solution to 2.0-3.0, adding pepsin, and stirring for 1-1.5h for homogenization;
(4) Adding distilled water into the fish skin obtained in the step (3), and homogenizing in a water bath at 50-55 ℃ for 5-6h;
(5) Pouring the slurry into a container, decocting for 30-60min, and placing at 0-4deg.C for 8-10 hr to obtain gelatin product.
Preferably, in step (1), the concentration of NaOH solution is 1% -3% and the glacial acetic acid concentration is 0.6% -1%.
Preferably, the concentration of the tannin solution is 1% -2%, and the mass ratio of the tannin solution to the fish skin is 1:1-3.
Preferably, in the step (2), the control condition of the microwave digestion instrument is that the power is 500-600W, the temperature is kept at 70 ℃ and 3-5min, the temperature is raised to 80 ℃ and kept at 8-10min, and then the pressure is relieved and cooled to 40 ℃.
Preferably, in the step (3), the mass ratio of the fish skin, the brine and the citric acid is 1:2:2, the concentration of the brine is 1-3%, the concentration of the citric acid is 1%, and acetic acid or NaOH is adopted for regulating the pH value of the solution.
Preferably, the concentration of the pepsin is 3000U/mg, and the mass ratio of the pepsin to the fish skin is 1-3:200-400.
Preferably, in step (4), the speed of rotation of the homogenate is 1400-1600rpm.
Preferably, the brine is an aqueous solution of sodium chloride.
Preferably, the fish skin is one or more than two of tilapia skin, grass carp skin and sea bass skin.
The invention also provides a fish skin gelatin extracted by the method.
In summary, the invention adopts the technical scheme, and has the following technical effects:
1. the fish skin gelatin extracted by the extraction method disclosed by the invention is subjected to enzymolysis and heat treatment after microwave digestion, so that the gelatin micro-network structure prepared from the fish skin can be changed, the surface pore size is uniform, the crosslinking degree is good, the arrangement is compact, and the problem of low gelatin yield caused by excessive hydrolysis is solved.
2. The fish skin gelatin of the invention improves the gel strength of the gelatin by adding the tannin and the salt, and enhances the gel strength of the gelatin by the action of the tannin and the salt, thereby improving the water holding capacity and the water absorption rate of the gelatin.
3. The invention provides proper enzymolysis environment through comprehensive treatment of brine, citric acid and pepsin, maintains the fiber network structure of gelatin while ensuring enzymolysis efficiency, and enhances intermolecular force of gelatin through sodium ion concentration.
4. According to the invention, through combination of enzymolysis and heat treatment, gelatin is extracted from fish skin, so that the gelatin has a spongy porous net structure and longer and higher fibers, maintains a good triple helix conformational state, and has good viscosity, emulsification characteristics, oxidation resistance and other functional characteristics.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail by referring to preferred embodiments. It should be noted, however, that many of the details set forth in the description are merely provided to provide a thorough understanding of one or more aspects of the invention, and that these aspects of the invention may be practiced without these specific details.
The extraction method of the fishskin gelatin is characterized by comprising the following steps of:
(1) Pretreatment: cleaning fresh fish skin, draining, soaking in NaOH solution for 10-15 hr, and expanding with glacial acetic acid for 3 hr;
(2) Soaking the fishskin in the step (1) for 3-5h by adopting a tannin solution; placing the fish skin in a microwave digestion instrument for treatment;
(3) Adding the fish skin treated in the step (2), brine and citric acid into an enzymolysis tank, heating to 40-45 ℃, regulating the pH value of the solution to 2.0-3.0, adding pepsin, and stirring for 1-1.5h for homogenization;
(4) Adding distilled water into the fish skin obtained in the step (3), and homogenizing in a water bath at 50-55 ℃ for 5-6h;
(5) Pouring the slurry into a container, decocting for 30-60min, and placing at 0-4deg.C for 8-10 hr to obtain gelatin product.
Preferably, in step (1), the concentration of NaOH solution is 1% -3% and the glacial acetic acid concentration is 0.6% -1%.
Preferably, the concentration of the tannin solution is 1% -2%, and the mass ratio of the tannin solution to the fish skin is 1:1-3.
Preferably, in the step (2), the control condition of the microwave digestion instrument is that the power is 500-600W, the temperature is kept at 70 ℃ and 3-5min, the temperature is raised to 80 ℃ and kept at 8-10min, and then the pressure is relieved and cooled to 40 ℃.
Preferably, in the step (3), the mass ratio of the fish skin, the brine and the citric acid is 1:1:1, the concentration of the brine is 1-3%, the concentration of the citric acid is 1%, and acetic acid or NaOH is adopted for regulating the pH value of the solution.
Preferably, the concentration of the pepsin is 3000U/mg, and the mass ratio of the pepsin to the fish skin is 1-3:200-400.
Preferably, in step (4), the speed of rotation of the homogenate is 1400-1600rpm.
Preferably, the brine is an aqueous solution of sodium chloride.
Preferably, the fish skin is one or more than two of tilapia skin, grass carp skin and sea bass skin.
The invention also provides a fish skin gelatin extracted by the method.
Example 1
The extraction method of the fishskin gelatin is characterized by comprising the following steps of:
(1) Pretreatment: respectively cleaning 200g of fresh fish skin (tilapia skin, grass carp skin and sea bass skin), draining, soaking in 500mL 1% NaOH solution for 10-15h, and expanding with 500m l glacial acetic acid with concentration of 0.6% for 3h;
(2) Soaking the fish skin in the step (1) for 3-5h by adopting a tannin solution with the concentration of 500m l being 1% -2%; placing the fish skin in a microwave digestion instrument for treatment; the control conditions of the microwave digestion instrument are that the power is 500-600W, the temperature is kept at 70 ℃ for 3-5min, the temperature is increased to 80 ℃ for 8-10min, and then the pressure is relieved and cooled to 40 ℃;
(3) Adding the fish skin treated in the step (2), 1% saline with the concentration of 400m l and 1% citric acid with the concentration of 400m l into an enzymolysis tank, heating to 40-45 ℃, regulating the pH of the solution to 2.0-3.0 by adopting acetic acid or NaOH, adding 3g of pepsin with the concentration of 3000U/mg, and stirring for 1-1.5h for homogenization;
(4) Adding distilled water into the fish skin obtained in the step (3), and homogenizing in a water bath at 50-55 ℃ for 5-6h; the rotating speed is 1400-1600rpm;
(5) Pouring the slurry into a container, decocting for 30-60min, and placing at 0-4deg.C for 8-10 hr to obtain gelatin product.
Example 2
The extraction method of the fishskin gelatin is characterized by comprising the following steps of:
(1) Pretreatment: cleaning 300g fresh fish skin (tilapia skin, grass carp skin and sea bass skin), draining, soaking in 500mL 3% NaOH solution for 10-15h, and swelling with 600m l concentration 1% glacial acetic acid for 3h;
(2) Soaking the fish skin in the step (1) for 3-5h by adopting 600m l concentration 1% -2% tannin solution; (3) Adding the fish skin treated in the step (2), 3% saline with the concentration of 600m l and 1% ningming acid with the concentration of 600m l into an enzymolysis tank, heating to 40-45 ℃, regulating the pH of the solution to 2.0-3.0 by adopting acetic acid or NaOH, adding 4g of pepsin with the concentration of 3000U/mg, and stirring for 1-1.5h for homogenate;
(4) Adding distilled water into the fish skin obtained in the step (3), and homogenizing in a water bath at 50-55 ℃ for 5-6h; the rotating speed is 1400-1600rpm;
(5) Pouring the slurry into a container, decocting for 30-60min, and placing at 0-4deg.C for 8-10 hr to obtain gelatin product.
Example 3
The extraction method of the fishskin gelatin is characterized by comprising the following steps of:
(1) Pretreatment: respectively cleaning 500g of fresh fish skin (tilapia skin, grass carp skin and sea bass skin), draining, soaking in 800mL 2% NaOH solution for 10-15h, and expanding with 800m l concentration 1% glacial acetic acid for 3h;
(2) Placing the fish skin in a microwave digestion instrument for treatment; the control conditions of the microwave digestion instrument are that the power is 500-600W, the temperature is kept at 70 ℃ for 3-5min, the temperature is increased to 80 ℃ for 8-10min, and then the pressure is relieved and cooled to 40 ℃;
(3) Adding the fish skin treated in the step (2), 1000ml of 2% saline water and 1000ml of 1% citric acid into an enzymolysis tank, heating to 40-45 ℃, regulating the pH of the solution to 2.0-3.0 by adopting acetic acid or NaOH, and adding 5g of 3000U/mg
Stirring for 1-1.5h after pepsin is stirred;
(4) Adding distilled water into the fish skin obtained in the step (3), and homogenizing in a water bath at 50-55 ℃ for 5-6h; rotational speed is 1400-1600rpm
(5) Pouring the slurry into a container, decocting for 30-60min, and placing at 0-4deg.C for 8-10 hr to obtain gelatin product.
Example 4
The extraction method of the fishskin gelatin is characterized by comprising the following steps of:
(1) Pretreatment: cleaning 300g of fresh fish skin (tilapia skin, grass carp skin and sea bass skin), draining, soaking in 600mL of 1% NaOH solution for 10-15h, and swelling with 800mL of 0.6% glacial acetic acid for 3h;
(2) Soaking the fish skin in the step (1) for 3-5h by adopting 900ml of tannin solution with the concentration of 1% -2%; placing the fish skin in a microwave digestion instrument for treatment; the control conditions of the microwave digestion instrument are that the power is 500-600W, the temperature is kept at 70 ℃ for 3-5min, the temperature is increased to 80 ℃ for 8-10min, and then the pressure is relieved and cooled to 40 ℃;
(3) Adding the fish skin treated in the step (2) into an enzymolysis tank, heating to 40-45 ℃, regulating the pH of the solution to 2.0-3.0 by adopting acetic acid or NaOH, adding 3g of pepsin with the concentration of 3000U/mg, and stirring for 1-1.5h for homogenating;
(4) Adding distilled water into the fish skin obtained in the step (3), and homogenizing in a water bath at 50-55 ℃ for 5-6h; the rotating speed is 1400-1600rpm;
(5) Pouring the slurry into a container, decocting for 30-60min, and placing at 0-4deg.C for 8-10 hr to obtain gelatin product.
Example 5
The extraction method of the fishskin gelatin is characterized by comprising the following steps of:
(1) Pretreatment: respectively cleaning 400g of fresh fish skin (tilapia skin, grass carp skin and sea bass skin), draining, soaking in 900mL of 1% NaOH solution for 10-15h, and expanding with 800mL of glacial acetic acid with concentration of 0.6% for 3h;
(2) Soaking the fish skin in the step (1) for 3-5h by adopting 900ml of tannin solution with the concentration of 1% -2%; placing the fish skin in a microwave digestion instrument for treatment; the control conditions of the microwave digestion instrument are that the power is 500-600W, the temperature is kept at 70 ℃ for 3-5min, the temperature is increased to 80 ℃ for 8-10min, and then the pressure is relieved and cooled to 40 ℃;
(3) Adding the fish skin treated in the step (2), 400ml of 1% saline water and 400ml of 1% citric acid into an enzymolysis tank, heating to 40-45 ℃ and regulating the pH of the solution to 2.0-3.0 by adopting acetic acid or NaOH, and stirring for 1-1.5h for homogenization;
(4) Adding distilled water into the fish skin obtained in the step (3), and homogenizing in a water bath at 50-55 ℃ for 5-6h; the rotating speed is 1400-1600rpm;
(5) Pouring the slurry into a container, decocting for 30-60min, and placing at 0-4deg.C for 8-10 hr to obtain gelatin product.
Test example 1
Gelatin samples obtained by extracting tilapia skin, grass carp skin and sea bass skin obtained in examples 1-5 were tested for gel strength and emulsifying property, and the results are shown in table 1.
The results show that the samples extracted by the method of the invention, whether tilapia skin, grass carp skin or sea bass skin, have stronger gel strength and stronger emulsifying property than other examples which do not completely follow the method of the invention. And after microwave digestion treatment and brine and citric acid treatment are combined, the emulsifying property of the water-soluble polymer is greatly improved.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (10)

1. The extraction method of the fishskin gelatin is characterized by comprising the following steps of:
(1) Pretreatment: cleaning fresh fish skin, draining, soaking in NaOH solution for 10-15 hr, and expanding with glacial acetic acid for 3 hr;
(2) Soaking the fishskin in the step (1) for 3-5h by adopting a tannin solution; placing the fish skin in a microwave digestion instrument for treatment;
(3) Adding the fish skin treated in the step (2), brine and citric acid into an enzymolysis tank, heating to 40-45 ℃, regulating the pH value of the solution to 2.0-3.0, adding pepsin, and stirring for 1-1.5h for homogenization;
(4) Adding distilled water into the fish skin obtained in the step (3), and homogenizing in a water bath at 50-55 ℃ for 5-6h;
(5) Pouring the slurry into a container, decocting for 30-60min, and standing at 0-4deg.C for 8-10 hr to obtain gelatin product.
2. The method according to claim 1, wherein in the step (1), the concentration of the NaOH solution is 1% -3% and the concentration of the glacial acetic acid is 0.6% -1%.
3. The method for extracting fishskin gelatin of claim 1, wherein the concentration of the tannin solution is 1% -2%, and the mass ratio of the tannin solution to the fishskin is 1:1-3.
4. The method according to claim 1, wherein in the step (2), the control conditions of the microwave digestion instrument are controlled, the power is 500-600W, the temperature is 70 ℃ for 3-5min, the temperature is raised to 80 ℃ for 8-10min, and then the pressure is released and cooled to 40 ℃.
5. The method according to claim 1, wherein in the step (3), the mass ratio of the fish skin, the brine and the citric acid is 1:2:2, the concentration of the brine is 1-3%, the concentration of the citric acid is 1%, and acetic acid or NaOH is adopted for regulating the pH value of the solution.
6. The method for extracting fishskin gelatin of claim 1 wherein the pepsin concentration is 3000U/mg and the mass ratio of pepsin to fishskin is 1-3:200-400.
7. The method according to claim 1, wherein in the step (4), the rotation speed of the homogenate is 1400-1600rpm.
8. The method of claim 1, wherein the brine is an aqueous solution of sodium chloride.
9. The method for extracting gelatin from fish skin of claim 1, wherein the fish skin is one or more of tilapia skin, grass carp skin and sea bass skin.
10. A fish skin gelatin extracted by the method of any one of claims 1-9.
CN202310481350.3A 2023-04-28 2023-04-28 Fish skin gelatin extraction method Pending CN116640519A (en)

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