Fish collagen peptide enzymolysis process

Abstract

The invention discloses a fish collagen peptide enzymolysis process, and relates to the technical field of fish collagen production, and the technical scheme is as follows: the fish collagen peptide enzymolysis process specifically comprises the following steps: S1, cleaning, cutting and freezing pretreated raw materials, mincing meat and degreasing; s2, extracting; s3, performing enzymolysis catalysis; s4, carrying out inactivation; s5, removing fishy smell and smell; s6, filtering; s7, performing concentration; the fish collagen peptide enzymolysis process has the beneficial effects that impurities and undesirable components in the raw materials are effectively removed through the fine pretreatment step, so that the purity and the quality of the final product are improved, the condition is strictly controlled in the enzymolysis process, collagen is ensured to be uniformly and efficiently decomposed into small molecule peptide fragments, and the enzymolysis quality of the fish collagen peptide is improved. The method has the advantages that the method is favorable for improving the solubility and the bioavailability of the product, the enzymolysis efficiency of the collagen is improved by optimizing the freezing temperature, the extraction temperature and the enzymolysis conditions, the higher hydrolysis degree is obtained, and the production efficiency is high.

Description

Technical Field

[0001] The invention relates to the technical field of fish collagen production, and in particular to a fish collagen peptide enzymatic hydrolysis process. Background Art

[0002] Fish collagen is widely used in food, cosmetics, health care products and medical fields due to its good biocompatibility, low antigenicity and easy absorption.

[0003] The existing fish collagen extraction and enzymatic hydrolysis processes have the disadvantages of low hydrolysis degree, unstable product quality and low production efficiency. Summary of the invention

[0004] To this end, the present invention provides a fish collagen peptide enzymatic hydrolysis process to solve the problems of low hydrolysis degree and unstable product quality in the fish collagen extraction and enzymatic hydrolysis processes.

[0005] In order to achieve the above object, the present invention provides the following technical solution: a fish collagen peptide enzymatic hydrolysis process, the specific steps are as follows:

[0006] S1. Preprocessing:

[0007] ①Raw material cleaning: ensure the cleanliness of the raw materials and remove surface dirt and internal impurities;

[0008] ② Cutting and freezing: Cut the fish into small pieces along with the meat, scales and bones, and freeze them quickly to lock in the protein structure and nutrients, which helps to maintain the freshness and nutritional value of the raw materials;

[0009] ③ Mincing and defatting: Use a meat grinder to mince the fish pieces, and then defatted with sodium hydroxide solution to remove excess fat.

[0010] Decalcification and cleaning: The defatted fish paste needs to be decalcified. Add 10% citric acid solution, mix it with the fish paste thoroughly, and let it stand for a while to allow the citric acid to combine with the calcium ions in the fish to form soluble calcium citrate, thereby removing the calcium in the fish. After decalcification, rinse the fish paste with clean water to remove the residual citric acid and impurities, in preparation for the subsequent extraction steps;

[0011] S2, extraction: add the defatted fish paste into water three times the volume of the fish paste for extraction and boiling. After boiling, filter out impurities and leave only the suspension;

[0012] S3, enzymatic hydrolysis catalysis: after the suspension extract is cooled, a composite protease consisting of hydrolytic protease, neutral protease and flavor protease is added for enzymatic hydrolysis to obtain an enzymatic hydrolyzate;

[0013] S4, inactivation: after the enzymatic hydrolysis is completed, the enzymatic hydrolyzate is heated and inactivated;

[0014] S5. Deodorization: After the enzymatic hydrolysate is filtered through multiple stages, activated carbon and filter aid are added to perform decarbonization treatment for 30 minutes to obtain a clear and transparent enzymatic hydrolysate;

[0015] S6. Filtration: remove impurities and mycelium through multi-stage biofilm filtration and separation at room temperature;

[0016] S7, concentration: using a double-effect concentrator to concentrate the fish collagen peptide liquid;

[0017] S8, centrifugal spray: centrifugal spray drying to obtain fish collagen peptide powder.

[0018] Preferably, in step S1, the freezing temperature is selected to be -2 to -10°C.

[0019] Preferably, in step S1, the degreasing temperature is 20-25°C.

[0020] Preferably, in step S2, the temperature during the extraction process is controlled at 95-100° C. and the boiling time is 1 hour.

[0021] Preferably, in step S3, the enzymolysis temperature is 50-55° C., the pH during enzymolysis is controlled at about 7.5-8.5, and the enzymolysis time is 4 hours.

[0022] Preferably, in step S4, the inactivation temperature is 90-100° C. and the inactivation time is 20-30 min.

[0023] Preferably, in step S5, continuous stirring is required during the decarbonization process.

[0024] The embodiments of the present invention have the following advantages:

[0025] Through sophisticated pretreatment steps, impurities and undesirable components in the raw materials are effectively removed, thereby improving the purity and quality of the final product. Strictly controlled conditions during the enzymatic hydrolysis process ensure that collagen is evenly and efficiently broken down into small molecule peptides, which helps to improve the solubility and bioavailability of the product. By optimizing the freezing temperature, extraction temperature and enzymatic hydrolysis conditions, the enzymatic hydrolysis efficiency of collagen is improved, a higher degree of hydrolysis is obtained, and high production efficiency. DETAILED DESCRIPTION

[0026] The following is a description of the implementation of the present invention by specific embodiments. People familiar with the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0027] Embodiment 1:

[0028] The present invention provides a fish collagen peptide enzymatic hydrolysis process, the specific steps are as follows:

[0029] S1. Preprocessing:

[0030] ①Raw material cleaning: ensure the cleanliness of the raw materials and remove surface dirt and internal impurities;

[0031] ② Cutting and freezing: Cut the fish together with the fish meat, fish scales and fish bones into small pieces and freeze them quickly to lock in the protein structure and nutrients. The freezing temperature of -2°C helps to maintain the freshness and nutritional value of the raw materials;

[0032] ③ Mincing and defatting: Use a meat grinder to mince the fish pieces, and then defatting with sodium hydroxide solution at a temperature of 20-25°C for 1 hour to remove excess fat.

[0033] Decalcification and cleaning: The defatted fish paste needs to be decalcified. Add 10% citric acid solution, mix it with the fish paste thoroughly, and let it stand for a while to allow the citric acid to combine with the calcium ions in the fish to form soluble calcium citrate, thereby removing the calcium in the fish. After decalcification, rinse the fish paste with clean water to remove the residual citric acid and impurities, in preparation for the subsequent extraction steps;

[0034] S2. Extraction: Add the defatted fish paste into water three times the volume of the fish paste for extraction. During the extraction process, the temperature is controlled at 95°C and the boiling time is 1 hour. During the period, stirring is required to prevent the bottom from sticking and burning. After the boiling is completed, the impurities and undissolved substances are removed by filtering equipment, leaving only the suspension containing collagen;

[0035] S3, enzymatic hydrolysis catalysis: after the suspension is cooled to a suitable temperature, a composite protease consisting of hydrolytic protease, neutral protease and flavor protease is added for enzymatic hydrolysis. The purpose of enzymatic hydrolysis is to decompose collagen into small molecular peptides to improve the solubility and bioavailability of the product. During the enzymatic hydrolysis process, the enzymatic hydrolysis temperature (50-55°C), pH value (7.5-8.5) and enzymatic hydrolysis time (4 hours) need to be strictly controlled. At the same time, regular stirring is required to ensure uniform enzymatic hydrolysis;

[0036] S4, inactivation: After the enzymatic hydrolysis is completed, the enzymatic hydrolyzate is heated to 90-100℃ for inactivation. The purpose of inactivation is to kill the residual enzymes and microorganisms to ensure the safety and stability of the product. The inactivation time is 20-30 minutes, and the temperature must be kept uniform during this period to avoid protein denaturation caused by local overheating;

[0037] S5. Deodorization: After the enzymatic hydrolysate is filtered through multiple stages, activated carbon and filter aids are added for decarbonization. Activated carbon has a strong adsorption capacity and can adsorb and remove the fishy and odorous components in the enzymatic hydrolysate. The decarbonization treatment time is 30 minutes, during which it is necessary to stir regularly to ensure sufficient contact between the activated carbon and the enzymatic hydrolysate.

[0038] S6. Filtration: Remove impurities and mycelium through multi-stage biofilm filtration separation at room temperature. Multi-stage biofilm filtration separation technology has the advantages of high efficiency, energy saving, and environmental protection, and can ensure the purity and safety of the product;

[0039] S7, Concentration: Use a double-effect concentrator to concentrate the fish collagen peptide liquid. During the concentration process, the temperature and pressure must be controlled to avoid protein denaturation and loss;

[0040] S8. Centrifugal spray: The concentrated fish collagen peptide liquid is sent to the centrifugal spray dryer for drying. The centrifugal spray dryer can quickly atomize the peptide liquid into tiny droplets and quickly dry it into a powdered product at high temperature. The dried fish collagen peptide powder has good solubility, stability and bioavailability, and is easy to store and transport.

[0041] Embodiment 2:

[0042] The present invention provides a fish collagen peptide enzymatic hydrolysis process, the specific steps are as follows:

[0043] S1. Preprocessing:

[0044] ①Raw material cleaning: ensure the cleanliness of the raw materials and remove surface dirt and internal impurities;

[0045] ② Cutting and freezing: Cut the fish together with the fish meat, fish scales and fish bones into small pieces and freeze them quickly to lock in the protein structure and nutrients. The freezing temperature of -6°C helps to maintain the freshness and nutritional value of the raw materials;

[0046] ③ Mincing and defatting: Use a meat grinder to mince the fish pieces, and then defatting with sodium hydroxide solution at a temperature of 20-25°C for 1 hour to remove excess fat.

[0047] Decalcification and cleaning: The defatted fish paste needs to be decalcified. Add 10% citric acid solution, mix it with the fish paste thoroughly, and let it stand for a while to allow the citric acid to combine with the calcium ions in the fish to form soluble calcium citrate, thereby removing the calcium in the fish. After decalcification, rinse the fish paste with clean water to remove the residual citric acid and impurities, in preparation for the subsequent extraction steps;

[0048] S2. Extraction: Add the defatted fish paste into water three times the volume of the fish paste for extraction. During the extraction process, the temperature is controlled at 97°C and the boiling time is 1 hour. During the period, stirring is required to prevent the bottom from sticking and burning. After the boiling is completed, the impurities and undissolved substances are removed by filtering equipment, leaving only the suspension containing collagen;

[0049] S3, enzymatic hydrolysis catalysis: after the suspension is cooled to a suitable temperature, a composite protease consisting of hydrolytic protease, neutral protease and flavor protease is added for enzymatic hydrolysis. The purpose of enzymatic hydrolysis is to decompose collagen into small molecular peptides to improve the solubility and bioavailability of the product. During the enzymatic hydrolysis process, the enzymatic hydrolysis temperature (50-55°C), pH value (7.5-8.5) and enzymatic hydrolysis time (4 hours) need to be strictly controlled. At the same time, regular stirring is required to ensure uniform enzymatic hydrolysis;

[0050] S4, inactivation: After the enzymatic hydrolysis is completed, the enzymatic hydrolyzate is heated to 90-100℃ for inactivation. The purpose of inactivation is to kill the residual enzymes and microorganisms to ensure the safety and stability of the product. The inactivation time is 20-30 minutes, and the temperature must be kept uniform during this period to avoid protein denaturation caused by local overheating;

[0051] S5. Deodorization: After the enzymatic hydrolysate is filtered through multiple stages, activated carbon and filter aids are added for decarbonization. Activated carbon has a strong adsorption capacity and can adsorb and remove the fishy and odorous components in the enzymatic hydrolysate. The decarbonization treatment time is 30 minutes, during which it is necessary to stir regularly to ensure sufficient contact between the activated carbon and the enzymatic hydrolysate.

[0052] S6. Filtration: Remove impurities and mycelium through multi-stage biofilm filtration separation at room temperature. Multi-stage biofilm filtration separation technology has the advantages of high efficiency, energy saving, and environmental protection, and can ensure the purity and safety of the product;

[0053] S7, Concentration: Use a double-effect concentrator to concentrate the fish collagen peptide liquid. During the concentration process, the temperature and pressure must be controlled to avoid protein denaturation and loss;

[0054] S8. Centrifugal spray: The concentrated fish collagen peptide liquid is sent to the centrifugal spray dryer for drying. The centrifugal spray dryer can quickly atomize the peptide liquid into tiny droplets and quickly dry it into a powdered product at high temperature. The dried fish collagen peptide powder has good solubility, stability and bioavailability, and is easy to store and transport.

[0055] Embodiment 3:

[0056] The present invention provides a fish collagen peptide enzymatic hydrolysis process, the specific steps are as follows:

[0057] S1. Preprocessing:

[0058] ①Raw material cleaning: ensure the cleanliness of the raw materials and remove surface dirt and internal impurities;

[0059] ② Cutting and freezing: Cut the fish together with the fish meat, fish scales and fish bones into small pieces and freeze them quickly to lock in the protein structure and nutrients. The freezing temperature of -8℃ helps to maintain the freshness and nutritional value of the raw materials;

[0060] ③ Mincing and defatting: Use a meat grinder to mince the fish pieces, and then defatting with sodium hydroxide solution at a temperature of 20-25°C for 1 hour to remove excess fat.

[0061] Decalcification and cleaning: The defatted fish paste needs to be decalcified. Add 10% citric acid solution, mix it with the fish paste thoroughly, and let it stand for a while to allow the citric acid to combine with the calcium ions in the fish to form soluble calcium citrate, thereby removing the calcium in the fish. After decalcification, rinse the fish paste with clean water to remove the residual citric acid and impurities, in preparation for the subsequent extraction steps;

[0062] S2. Extraction: Add the defatted fish paste into water three times the volume of the fish paste for extraction. During the extraction process, the temperature is controlled at 100°C and the boiling time is 1 hour. During the period, stirring is required to prevent the bottom from sticking and burning. After the boiling is completed, the impurities and undissolved substances are removed by filtering equipment, leaving only the suspension containing collagen;

[0063] S3, enzymatic hydrolysis catalysis: after the suspension is cooled to a suitable temperature, a composite protease consisting of hydrolytic protease, neutral protease and flavor protease is added for enzymatic hydrolysis. The purpose of enzymatic hydrolysis is to decompose collagen into small molecular peptides to improve the solubility and bioavailability of the product. During the enzymatic hydrolysis process, the enzymatic hydrolysis temperature (50-55°C), pH value (7.5-8.5) and enzymatic hydrolysis time (4 hours) need to be strictly controlled. At the same time, regular stirring is required to ensure uniform enzymatic hydrolysis;

[0064] S4, inactivation: After the enzymatic hydrolysis is completed, the enzymatic hydrolyzate is heated to 90-100℃ for inactivation. The purpose of inactivation is to kill the residual enzymes and microorganisms to ensure the safety and stability of the product. The inactivation time is 20-30 minutes, and the temperature must be kept uniform during this period to avoid protein denaturation caused by local overheating;

[0065] S5. Deodorization: After the enzymatic hydrolysate is filtered through multiple stages, activated carbon and filter aids are added for decarbonization. Activated carbon has a strong adsorption capacity and can adsorb and remove the fishy and odorous components in the enzymatic hydrolysate. The decarbonization treatment time is 30 minutes, during which it is necessary to stir regularly to ensure sufficient contact between the activated carbon and the enzymatic hydrolysate.

[0066] S6. Filtration: Remove impurities and mycelium through multi-stage biofilm filtration separation at room temperature. Multi-stage biofilm filtration separation technology has the advantages of high efficiency, energy saving, and environmental protection, and can ensure the purity and safety of the product;

[0067] S7, Concentration: Use a double-effect concentrator to concentrate the fish collagen peptide liquid. During the concentration process, the temperature and pressure must be controlled to avoid protein denaturation and loss;

[0068] S8. Centrifugal spray: The concentrated fish collagen peptide liquid is sent to the centrifugal spray dryer for drying. The centrifugal spray dryer can quickly atomize the peptide liquid into tiny droplets and quickly dry it into a powdered product at high temperature. The dried fish collagen peptide powder has good solubility, stability and bioavailability, and is easy to store and transport.

[0069] Based on the data provided in Examples 1, 2 and 3 above, the degree of hydrolysis of fish collagen peptide enzymatic hydrolysis process at different freezing temperatures and extraction temperatures was tested and the following data were obtained:

[0070]

[0071] 1. Effect of freezing temperature on hydrolysis degree:

[0072] When the extraction temperature was maintained at 95 °C, the freezing temperature was reduced from -2 °C to -10 °C, and the degree of hydrolysis was increased from 37.42% to 40.23%.

[0073] When the extraction temperature was increased to 97°C, the freezing temperature was reduced from -2°C to -10°C, and the degree of hydrolysis was increased from 38.69% to 41.48%.

[0074] When the extraction temperature reached 100°C, the freezing temperature decreased from -2°C to -10°C, and the degree of hydrolysis increased from 39.45% to 42.58%.

[0075] It can be seen that as the freezing temperature decreases, the degree of hydrolysis tends to gradually increase. A lower freezing temperature helps to better maintain the freshness and nutritional value of the raw materials, and is also beneficial to the subsequent enzymatic hydrolysis process.

[0076] 2. Effect of extraction temperature on hydrolysis degree:

[0077] Under the condition of freezing temperature of -2℃, the extraction temperature increased from 95℃ to 100℃, and the hydrolysis degree increased from 37.42% to 39.45%.

[0078] Under the condition of freezing temperature of -6℃, the extraction temperature increased from 95℃ to 100℃, and the hydrolysis degree increased from 39.21% to 41.23%.

[0079] Under the condition of freezing temperature of -10℃, the extraction temperature increased from 95℃ to 100℃, and the hydrolysis degree increased from 40.23% to 42.58%.

[0080] This shows that with the increase of extraction temperature, the degree of hydrolysis also tends to gradually increase. Higher extraction temperature is conducive to the dissolution of collagen and the enzymatic hydrolysis reaction, thereby increasing the degree of hydrolysis.

[0081] The fish collagen peptide enzymatic hydrolysis process of Example 3 (freezing temperature is -10°C, extraction temperature is 100°C) achieved the highest hydrolysis degree of 42.58%, and the fish collagen peptidase production efficiency was high.

[0082] The above is only a preferred embodiment of the present invention. Any person skilled in the art may modify the present invention by using the above technical solution or modify it into an equivalent technical solution. Therefore, any simple modification or equivalent replacement made according to the technical solution of the present invention shall fall within the scope of protection claimed by the present invention.

Claims

1. A fish collagen peptide enzymatic hydrolysis process, characterized in that: The specific steps are as follows: S1. Preprocessing: ①Raw material cleaning: ensure the cleanliness of the raw materials and remove surface dirt and internal impurities; ② Cutting and freezing: Cut the fish into small pieces along with the meat, scales and bones, and freeze them quickly to lock in the protein structure and nutrients, which helps to maintain the freshness and nutritional value of the raw materials; ③ Mincing and defatting: Use a meat grinder to mince the fish pieces, and then defatted with sodium hydroxide solution to remove excess fat. Decalcification and cleaning: The defatted fish paste needs to be decalcified. Add 10% citric acid solution, mix it with the fish paste thoroughly, and let it stand for a while to allow the citric acid to combine with the calcium ions in the fish to form soluble calcium citrate, thereby removing the calcium in the fish. After decalcification, rinse the fish paste with clean water to remove the residual citric acid and impurities, in preparation for the subsequent extraction steps; S2, extraction: add the defatted fish paste into water three times the volume of the fish paste for extraction and boiling. After boiling, filter out impurities and leave only the suspension; S3, enzymatic hydrolysis catalysis: after the suspension extract is cooled, a composite protease consisting of hydrolytic protease, neutral protease and flavor protease is added for enzymatic hydrolysis to obtain an enzymatic hydrolyzate; S4, inactivation: after the enzymatic hydrolysis is completed, the enzymatic hydrolyzate is heated and inactivated; S5. Deodorization: After the enzymatic hydrolysate is filtered through multiple stages, activated carbon and filter aid are added to perform decarbonization treatment for 30 minutes to obtain a clear and transparent enzymatic hydrolysate; S6. Filtration: remove impurities and mycelium through multi-stage biofilm filtration and separation at room temperature; S7, concentration: using a double-effect concentrator to concentrate the fish collagen peptide liquid; S8, centrifugal spray: centrifugal spray drying to obtain fish collagen peptide powder.

2. The process for enzymatic hydrolysis of fish collagen peptide according to claim 1, characterized in that: In step S1, the freezing temperature is selected to be -2 to -10°C.

3. The fish collagen peptide enzymatic hydrolysis process according to claim 1, characterized in that: In the step S1, the degreasing temperature is 20-25°C.

4. The process for enzymatic hydrolysis of fish collagen peptide according to claim 1, characterized in that: In step S2, the temperature is controlled at 95-100° C. during the extraction process, and the boiling time is 1 hour.

5. The process for enzymatic hydrolysis of fish collagen peptide according to claim 1, characterized in that: In step S3, the enzymolysis temperature is 50-55° C., the pH during enzymolysis is controlled at about 7.5-8.5, and the enzymolysis time is 4 hours.

6. The process for enzymatic hydrolysis of fish collagen peptide according to claim 1, characterized in that: In step S4, the inactivation temperature is 90-100° C. and the inactivation time is 20-30 min.

7. The process for enzymatic hydrolysis of fish collagen peptide according to claim 1, characterized in that: In the step S5, continuous stirring is required during the decarbonization process.

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