CN109182432A - The preparation method of fish collagen oligopeptide - Google Patents
The preparation method of fish collagen oligopeptide Download PDFInfo
- Publication number
- CN109182432A CN109182432A CN201811093580.8A CN201811093580A CN109182432A CN 109182432 A CN109182432 A CN 109182432A CN 201811093580 A CN201811093580 A CN 201811093580A CN 109182432 A CN109182432 A CN 109182432A
- Authority
- CN
- China
- Prior art keywords
- fish collagen
- collagen oligopeptide
- fish
- preparation
- protease
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/14—Extraction; Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/14—Extraction; Separation; Purification
- C07K1/34—Extraction; Separation; Purification by filtration, ultrafiltration or reverse osmosis
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P21/00—Preparation of peptides or proteins
- C12P21/06—Preparation of peptides or proteins produced by the hydrolysis of a peptide bond, e.g. hydrolysate products
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Genetics & Genomics (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Analytical Chemistry (AREA)
- Biophysics (AREA)
- Zoology (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Wood Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Water Supply & Treatment (AREA)
- Biotechnology (AREA)
- General Chemical & Material Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Microbiology (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention discloses a kind of preparation methods of fish collagen oligopeptide, using ocean fish-skin as raw material, by the processing such as enzymatic hydrolysis, it is prepared into the product that oligomeric peptide content is higher than 96%, contain L MALIC ACID sodium and trimethylglycine in the protease that enzymolysis process uses, it can promote collagen hydrolysate, improve the yield of small molecule fish collagen oligopeptide；The fish collagen oligopeptide can be widely applied to the wine industry, drink industry, flavouring industry, healthcare industry, the functional foods such as oral solution, tablet, capsule and medicine trade field.It has the beneficial effect that fish collagen oligopeptide prepared by the present invention is the small molecule mixing peptides that molecular weight concentrates on 300-1000Da, is easy to directly be absorbed by small intestine, human skin etc., reduces the waste of nutritional ingredient；And content of beary metal is small, quality is more excellent.
Description
Technical field
The present invention relates to oligopeptide preparation technical fields, more particularly, to a kind of preparation method of fish collagen oligopeptide.
Background technique
Collagen is widely present in the connective tissues such as skin, bone, tendon, the film of animal, is the main of composition connective tissue
Ingredient.Previous production collagen mainly utilizes resourceful terrestrial animal, such as ox, the skin of pig, bone to add as raw material
Work production.Though the collagen of fish already by human knowledge, such as tortoise-shell glue, yellow croaker glue, fails as a kind of important work
Industry application material is used, this mainly relies on the product of marine fishing, and source is unstable, lacks scale.In recent years, by
It is influenced in terrestrial animal by many factors such as environment, infection diseases, the safety of protein is under suspicion, and aquaculture
Industry and fish processing industry have a great development, the aquatic resources steady sources such as fish-skin, fish-bone, fish scale, and without dangerous worry,
Therefore, the application, exploitation of Isin glue collagen just become hot spot concerned by people.
Collagen molecules amount wider distribution, the big collagen human body of molecular weight are difficult to be absorbed and utilized, suitable for steady
Determine agent, emulsifier, clarifying agent etc..The lesser collagen of molecular weight, generally by 10~100 Amino acid profiles, molecular weight
Less than 1000 dalton, this collagen is also referred to as collagen peptide, and because its molecular weight is smaller, human body is easy to absorb, in nutrition
Using more in health food, there is higher demand in the market to the collagen.In the relatively small collagen of molecular weight
In, fish collagen oligopeptide is a kind of deep processed product of common Isin glue collagen, relatively small with pollution-free or pollution
Fish-skin, bone are raw material, and purification is process, they are mostly made of 2-6 amino acid, molecular weight concentrates on 200-
The small molecule of 1000 dalton mixes peptides, can directly be absorbed by small intestine, human skin etc., has powerful nutritive peculiarity,
Application is extensive, is the ingredient of novel nutritious and healthy food, has its unique advantage in nutrition and application aspect.
The method for extracting fish collagen oligopeptide mainly has Hot water extraction, acid system, alkaline process, salt method and enzyme process etc., activity
The preparation method of peptide, which then has, to be extracted from native organism, by chemical method and recombinant DNA technology synthesis, extracorporeal hydrolysis albumen
Matter etc..With the fast development of Enzymes Industry, enzymatic hydrolysis is more mild, safe, more single-minded than traditional acid system, alkaline process, no
Only degradation time is short, and product nutrition loss is less, and non-environmental-pollution.Currently, enzymatic hydrolysis marine collagen albumen mainly has single enzyme
Method and multi-enzyme method, multi-enzyme method are divided into mixed enzyme solution and stepwise discretization method again.The condition of enzymolysis and extraction active peptide is typically considered as
Requirement of institute's development to molecular weight, the lesser product of molecular weight preferably use multi-enzyme method.
The prior art such as Authorization Notice No. is the Chinese invention patent of 102286589 B of CN, and it is oligomeric to disclose a kind of soft-shelled turtle
The extracting method of peptide, after being digested as raw material with alkali protease using soft-shelled turtle, then with flavor protease it is circumscribed and adjust flavor, enzymatic hydrolysis
Liquid carries out ultrafiltration, and alkali protease additional amount is the 0.2-5% of raw material soft-shelled turtle weight, and flavor protease additional amount is raw material soft-shelled turtle
The 0.1-2% of weight, retaining molecular weight are that the ultrafiltration membrane of 0.5-30 ten thousand dalton carries out ultrafiltration, and film concentrated spray is dry
To turtle oligopeptide；This method is easy to operate, in good taste, at low cost, environment-friendly high-efficiency, but the oligomeric peptide molecule that this method is extracted
It measures distributed more widely, is not easy to be absorbed and utilized, and content of beary metal is higher in product, food-grade requirement cannot be reached.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of fish collagen oligopeptide, obtain collagen using enzymatic isolation method
The small molecule fish collagen oligopeptide that content is high, molecular weight is concentrated, content of beary metal is low.
The present invention in view of the above technology in the problem of mentioning, the technical solution taken are as follows:
The preparation method of fish collagen oligopeptide, including following production technology:
Raw material cleans → mentions glue → enzymatic hydrolysis → remove except metal → decoloration, deodorization and desalination → film filtering → nanofiltration → concentration →
Bacterium filtering → spray drying.
The preparation method of fish collagen oligopeptide, specifically includes the following steps:
Cleaning: by the sodium hydroxide and salt of fish-skin food-grade 0.1%-0.3%, according to the ratio of solid-liquid ratio 1:3-4
Cleaning 2-4h exhausts water, then clean 5-8 time with tap water, and it is bright colourless for cleaning to water, and pH is spare in 8-9；
It mentions glue: high-temperature water is added according to production ordering after feeding intake, mentions glue；
Enzymatic hydrolysis: pH to 8.0-8.5 is adjusted, 50-55 DEG C of temperature, carries out enzyme with the protease of fish-skin dosage 0.02-1.0%
It solves, heat up enzyme deactivation after enzymatic hydrolysis 1-4h；
Except metal: starch xanthate and mulberry leaf polysaccharide is added in enzymatic hydrolysis solution, is sufficiently mixed, after reacting 20-24h, warp
Diatomite filtering, obtains fish collagen oligopeptide clear liquid, and filter pressure is controlled in 0.2-0.6MP；
Decoloration, deodorization and desalination: the fish collagen oligopeptide clear liquid filtered passes sequentially through macroporous absorbent resin-cation and hands over
It changes resin-anion exchange resin to be adsorbed, removes color, peculiar smell and the salt in clear liquid, carried out after absorption with eluent
Elution；
Film filtering: filter pressure is controlled in 0.15MPa, and flow control is in 6-8m3/h；
Nanofiltration: nanofiltration operating pressure is controlled in 1.2-1.3MPa, and material concentration is concentrated into 20-25% and stops nanofiltration；
Concentration: vacuum falling film concentration, at 30-60 DEG C, vacuum degree control is concentrated -0.06 to -0.08MPa for temperature control
It is 35-45% discharging to concentration；
Aseptic filtration: guarantee the microbiological indicator of product by 0.22-0.45 microns of sterilization film low temperature degermings；
Spray drying: the product after aseptic filtration is spray-dried.
Preferably, adhesive tape part is mentioned are as follows: adjust pH6.0-6.5,70-75 DEG C mentions glue.
Preferably, protease is preferably compound fertilizer production, papain, neutral proteinase, appointing in alkali protease
It anticipates one kind.
Preferably, the L MALIC ACID sodium and 0.3-0.8% trimethylglycine for being 1-5% containing quality in protease, L-
Natrium malicum and trimethylglycine have gain effect, on the one hand can promote protease by the peptide chain of Isin glue collagen from interior
Portion disconnects, and the amino acid of active site of protein is exposed, and further cuts off the hydrophobic amino acid of peptide termini, releases
Come, while increase small molecule amino acid dissociates degree, moreover it is possible to effectively reduce the bitter taste of peptide, improve mouthfeel；On the other hand, by
It is preferable in its dissolubility, be conducive to enzyme and preferably contacted with Isin glue collagen, promotes the progress of hydrolysis, molecular weight finally can be improved
The yield of the small molecule fish collagen oligopeptide of concentration.
Preferably, except in metal process, the content of the starch xanthate of addition is the 2-10% of enzymolysis liquid, mulberry leaf polysaccharide
Content be enzymolysis liquid 1-2%；The special presence of starch xanthate and mulberry leaf polysaccharide can break a huge sum of money in enzymatic hydrolysis solution
Belong to the coordination structure of complex compound, destroy the complexation equilibrium state of complex ion and heavy metal ion, make polar group in its molecule with
It digests the heavy metal ion in solution and bond ion transfer occurs, is i.e. starch xanthate and mulberry leaf polysaccharide is by the polarity in molecule
The heavy metal ion that base location gives in enzymatic hydrolysis solution forms stable heavy metallic salt precipitating, the solubility of these heavy metallic salts precipitating
Product much smaller than other precipitatings that heavy metal ion is formed solubility product, so that heavy metal ion is in the form that precipitates from enzymatic hydrolysis solution
In separate, can finally reduce heavy metal to the pollution and toxic hazard of fish collagen oligopeptide product；Meanwhile starch xanthate and mulberry
Leaf polyose stability with higher, preparation is simple, low in cost, removal of heavy metal ions rate with higher.
Preferably, eluent is room temperature deionised water, flow velocity 2-3BV/h.
Preferably, spray drying condition are as follows: feed pressure 3.0-5.0MPa is spray-dried 80-95 DEG C of leaving air temp.
The present invention also provides a kind of fish collagen oligopeptide powder that method as above is prepared, the fish collagen oligopeptide powder with
Butt meter: oligomeric peptide content >=96.6%, ash content < 0.4%, molecular weight 300-1000Da, average molecular weight 650Da, weight
Lead (mg/kg)≤0.15 in metal salt, cadmium (mg/kg)≤0.05, inorganic arsenic (mg/kg)≤0.1, methyl mercury (mg/kg)≤
0.2。
Compared with the prior art, the advantages of the present invention are as follows: (1) in of the invention fish collagen oligopeptide oligomeric peptide content high
Peptides are mixed up to 96% or more, and for the small molecule that molecular weight concentrates on 300-1000Da, are easy to straight by small intestine, human skin etc.
Absorption is connect, the waste of nutritional ingredient is reduced；(2) in extraction process, by removing the methods of metal, film filtering, nanofiltration, effectively
The fishy smell and heavy metal for eliminating albumen peptide product not only meet food-grade requirement, while improving the quality of product.
Specific embodiment
The present invention program is described further below by embodiment:
Embodiment 1:
The preparation method of fish collagen oligopeptide, including following production technology:
Raw material cleans → mentions glue → enzymatic hydrolysis → remove except metal → decoloration, deodorization and desalination → film filtering → nanofiltration → concentration →
Bacterium filtering → spray drying.
The preparation method of fish collagen oligopeptide, specifically includes the following steps:
(1) it cleans: by the sodium hydroxide and salt of fish-skin food-grade 0.1%, cleaning 2h according to the ratio of solid-liquid ratio 1:3
Water is exhausted, is then cleaned 5 times with tap water, cleaning to water is bright colourless, pH 8, spare；
(2) it mentions glue: high-temperature water is added according to production ordering after feeding intake, adjust pH6.0,70 DEG C mention glue；
(3) it digests: adjusting pH to 8.0, temperature 50 C carries out enzyme with the compound fertilizer production of fish-skin dosage 0.02%
It solves, heat up enzyme deactivation after enzymatic hydrolysis 1h；Contain 1% L MALIC ACID sodium and 0.3% trimethylglycine, L- apple in compound fertilizer production
Tartaric acid sodium and trimethylglycine have gain effect, on the one hand can promote protease by the peptide chain of Isin glue collagen from inside
It disconnects, the amino acid of active site of protein is exposed, and further the hydrophobic amino acid of peptide termini is cut off, is released
Come, while increase small molecule amino acid dissociates degree, moreover it is possible to effectively reduce the bitter taste of peptide, improve mouthfeel；On the other hand, by
It is preferable in its dissolubility, be conducive to enzyme and preferably contacted with Isin glue collagen, promotes the progress of hydrolysis, molecular weight finally can be improved
The yield of the small molecule fish collagen oligopeptide of concentration；
(4) it removes metal: the starch xanthate of enzymolysis liquid 2% and 1% mulberry leaf polysaccharide is added in enzymatic hydrolysis solution, it is sufficiently mixed
It closes, after reacting 20h, is filtered through diatomite, obtain fish collagen oligopeptide clear liquid, filter pressure is controlled in 0.2MP；
The special presence of starch xanthate and mulberry leaf polysaccharide can break the coordination of heavy metal complex in enzymatic hydrolysis solution
Structure destroys the complexation equilibrium state of complex ion and heavy metal ion, makes the weight in the polar group and enzymatic hydrolysis solution in its molecule
Bond ion transfer occurs for metal ion, i.e., starch xanthate and mulberry leaf polysaccharide give the polarity base location in molecule to enzymatic hydrolysis
Heavy metal ion in solution forms stable heavy metallic salt precipitating, and the solubility product of these heavy metallic salts precipitating is much smaller than heavy metal
The solubility product for other precipitatings that ion is formed, so that heavy metal ion is separated from enzymatic hydrolysis solution in the form precipitated, most
Heavy metal can be reduced eventually to the pollution and toxic hazard of fish collagen oligopeptide product；Meanwhile starch xanthate and mulberry leaf polysaccharide have compared with
High stability, preparation is simple, low in cost, removal of heavy metal ions rate with higher；
(5) decolourize, deodorize and desalination: the fish collagen oligopeptide clear liquid filtered pass sequentially through macroporous absorbent resin-sun from
Sub-exchange resin-anion exchange resin is adsorbed, and is removed color, peculiar smell and salt in clear liquid, is used eluent after absorption
It is eluted；Eluent is room temperature deionised water, flow velocity 2BV/h；
(6) film filters: filter pressure is controlled in 0.15MPa, and flow control is in 6m3/h；
(7) nanofiltration: nanofiltration operating pressure is controlled in 1.2MPa, and material concentration is concentrated into 20% stopping nanofiltration；
(8) be concentrated: vacuum falling film concentration, temperature are controlled at 30 DEG C, and in -0.06MPa, be concentrated into concentration is vacuum degree control
35% discharging；
(9) aseptic filtration: guarantee the microbiological indicator of product by 0.22 micron of sterilization film low temperature degerming；
(10) it is spray-dried: the product after aseptic filtration is spray-dried；Feed pressure 3.0MPa, is spray-dried out
80 DEG C of air temperature.
Embodiment 2:
The preparation method of fish collagen oligopeptide, including following production technology:
Raw material cleans → mentions glue → enzymatic hydrolysis → remove except metal → decoloration, deodorization and desalination → film filtering → nanofiltration → concentration →
Bacterium filtering → spray drying.
The preparation method of fish collagen oligopeptide, specifically includes the following steps:
(1) it cleans: by the sodium hydroxide and salt of fish-skin food-grade 0.2%, cleaning 3h according to the ratio of solid-liquid ratio 1:3
Water is exhausted, is then cleaned 6 times with tap water, cleaning to water is bright colourless, pH 8, spare；
(2) it mentions glue: high-temperature water is added according to production ordering after feeding intake, adjust pH6.2,72 DEG C mention glue；
(3) it digests: adjusting pH to 8.3,52 DEG C of temperature, carry out enzyme with the compound fertilizer production of fish-skin dosage 0.05%
It solves, heat up enzyme deactivation after enzymatic hydrolysis 2h；Contain 3% L MALIC ACID sodium and 0.5% trimethylglycine, L- apple in compound fertilizer production
Tartaric acid sodium and trimethylglycine have gain effect, on the one hand can promote protease by the peptide chain of Isin glue collagen from inside
It disconnects, the amino acid of active site of protein is exposed, and further the hydrophobic amino acid of peptide termini is cut off, is released
Come, while increase small molecule amino acid dissociates degree, moreover it is possible to effectively reduce the bitter taste of peptide, improve mouthfeel；On the other hand, by
It is preferable in its dissolubility, be conducive to enzyme and preferably contacted with Isin glue collagen, promotes the progress of hydrolysis, molecular weight finally can be improved
The yield of the small molecule fish collagen oligopeptide of concentration；
(4) it removes metal: the starch xanthate of enzymolysis liquid 6% and 1% mulberry leaf polysaccharide is added in enzymatic hydrolysis solution, it is sufficiently mixed
It closes, after reacting 22h, is filtered through diatomite, obtain fish collagen oligopeptide clear liquid, filter pressure is controlled in 0.4MP；
The special presence of starch xanthate and mulberry leaf polysaccharide can break the coordination of heavy metal complex in enzymatic hydrolysis solution
Structure destroys the complexation equilibrium state of complex ion and heavy metal ion, makes the weight in the polar group and enzymatic hydrolysis solution in its molecule
Bond ion transfer occurs for metal ion, i.e., starch xanthate and mulberry leaf polysaccharide give the polarity base location in molecule to enzymatic hydrolysis
Heavy metal ion in solution forms stable heavy metallic salt precipitating, and the solubility product of these heavy metallic salts precipitating is much smaller than heavy metal
The solubility product for other precipitatings that ion is formed, so that heavy metal ion is separated from enzymatic hydrolysis solution in the form precipitated, most
Heavy metal can be reduced eventually to the pollution and toxic hazard of fish collagen oligopeptide product；Meanwhile starch xanthate and mulberry leaf polysaccharide have compared with
High stability, preparation is simple, low in cost, removal of heavy metal ions rate with higher；
(5) decolourize, deodorize and desalination: the fish collagen oligopeptide clear liquid filtered pass sequentially through macroporous absorbent resin-sun from
Sub-exchange resin-anion exchange resin is adsorbed, and is removed color, peculiar smell and salt in clear liquid, is used eluent after absorption
It is eluted；Eluent is room temperature deionised water, flow velocity 3BV/h；
(6) film filters: filter pressure is controlled in 0.18MPa, and flow control is in 7m3/h；
(7) nanofiltration: nanofiltration operating pressure is controlled in 1.2MPa, and material concentration is concentrated into 22% stopping nanofiltration；
(8) be concentrated: vacuum falling film concentration, temperature are controlled at 50 DEG C, and in -0.07MPa, be concentrated into concentration is vacuum degree control
40% discharging；
(9) aseptic filtration: guarantee the microbiological indicator of product by 0.40 micron of sterilization film low temperature degerming；
(10) it is spray-dried: the product after aseptic filtration is spray-dried；Feed pressure 4.0MPa, is spray-dried out
85 DEG C of air temperature.
Embodiment 3:
The preparation method of fish collagen oligopeptide, including following production technology:
Raw material cleans → mentions glue → enzymatic hydrolysis → remove except metal → decoloration, deodorization and desalination → film filtering → nanofiltration → concentration →
Bacterium filtering → spray drying.
The preparation method of fish collagen oligopeptide, specifically includes the following steps:
(1) it cleans: by the sodium hydroxide and salt of fish-skin food-grade 0.3%, cleaning 4h according to the ratio of solid-liquid ratio 1:4
Water is exhausted, is then cleaned 8 times with tap water, cleaning to water is bright colourless, pH 9, spare；
(2) it mentions glue: high-temperature water is added according to production ordering after feeding intake, adjust pH6.5,75 DEG C mention glue；
(3) it digests: adjusting pH to 8.5,55 DEG C of temperature, digested with the compound fertilizer production of fish-skin dosage 1.0%,
Heat up enzyme deactivation after enzymatic hydrolysis 4h；Contain 5% L MALIC ACID sodium and 0.8% trimethylglycine, L- apple in compound fertilizer production
Sour sodium and trimethylglycine have gain effect, on the one hand can promote protease that the peptide chain of Isin glue collagen is disconnected from inside
It opens, the amino acid of active site of protein is exposed, and further the hydrophobic amino acid of peptide termini is cut off, is released,
While increase small molecule amino acid dissociates degree, moreover it is possible to effectively reduce the bitter taste of peptide, improve mouthfeel；On the other hand, due to
Its dissolubility is preferable, is conducive to enzyme and preferably contacts with Isin glue collagen, promotes the progress of hydrolysis, molecule quantity set finally can be improved
In small molecule fish collagen oligopeptide yield；
(4) it removes metal: the starch xanthate of enzymolysis liquid 10% and 2% mulberry leaf polysaccharide is added in enzymatic hydrolysis solution, sufficiently
Mixing is filtered after reaction for 24 hours through diatomite, and fish collagen oligopeptide clear liquid is obtained, and filter pressure is controlled in 0.6MP；
The special presence of starch xanthate and mulberry leaf polysaccharide can break the coordination of heavy metal complex in enzymatic hydrolysis solution
Structure destroys the complexation equilibrium state of complex ion and heavy metal ion, makes the weight in the polar group and enzymatic hydrolysis solution in its molecule
Bond ion transfer occurs for metal ion, i.e., starch xanthate and mulberry leaf polysaccharide give the polarity base location in molecule to enzymatic hydrolysis
Heavy metal ion in solution forms stable heavy metallic salt precipitating, and the solubility product of these heavy metallic salts precipitating is much smaller than heavy metal
The solubility product for other precipitatings that ion is formed, so that heavy metal ion is separated from enzymatic hydrolysis solution in the form precipitated, most
Heavy metal can be reduced eventually to the pollution and toxic hazard of fish collagen oligopeptide product；Meanwhile starch xanthate and mulberry leaf polysaccharide have compared with
High stability, preparation is simple, low in cost, removal of heavy metal ions rate with higher；
(5) decolourize, deodorize and desalination: the fish collagen oligopeptide clear liquid filtered pass sequentially through macroporous absorbent resin-sun from
Sub-exchange resin-anion exchange resin is adsorbed, and is removed color, peculiar smell and salt in clear liquid, is used eluent after absorption
It is eluted；Eluent is room temperature deionised water, flow velocity 3BV/h；
(6) film filters: filter pressure is controlled in 0.20MPa, and flow control is in 8m3/h；
(7) nanofiltration: nanofiltration operating pressure is controlled in 1.3MPa, and material concentration is concentrated into 25% stopping nanofiltration；
(8) be concentrated: vacuum falling film concentration, temperature are controlled at 60 DEG C, and in -0.08MPa, be concentrated into concentration is vacuum degree control
45% discharging；
(9) aseptic filtration: guarantee the microbiological indicator of product by 0.45 micron of sterilization film low temperature degerming；
(10) it is spray-dried: the product after aseptic filtration is spray-dried；Feed pressure 5.0MPa, is spray-dried out
95 DEG C of air temperature.
Comparative example 1:
L MALIC ACID sodium and trimethylglycine, rest part and embodiment 2 complete one are free of in compound fertilizer production
It causes.
Comparative example 2:
It is not added with starch xanthate and mulberry leaf polysaccharide in enzymatic hydrolysis solution, rest part and embodiment 2 are completely the same.
Embodiment 4:
Embodiment 2 is set as test group, comparative example 1, comparative example 2 are set to control group 1, control group 2.
Using the standard and detection method of defined in the fish oligopeptide powder GB/T22729-2008 of ocean to test group and right
It is detected and is evaluated according to the molecular weight of fish collagen oligopeptide, heavy metallic salt content in group 1 and 2, the results are shown in Table 1.
1 measurement result of table
| Test group | Control group 1 | Control group 2 | |
| Molecular weight is less than 1000Da | 96.7% | 87% | 96.3% |
| Lead (in terms of Pb)/(mg/kg) | ≤0.15 | ≤0.15 | ≤0.5 |
| Cadmium (in terms of Cd)/(mg/kg) | ≤0.05 | ≤0.05 | ≤0.1 |
| Inorganic arsenic/(mg/kg) | ≤0.1 | ≤0.1 | ≤1.0 |
| Methyl mercury/(mg/kg) | ≤0.2 | ≤0.2 | ≤0.5 |
As shown in Table 1, the fish collagen oligopeptide that test group is prepared, molecular weight less than 1000Da ratio be higher than pair
According to group 1, illustrate that the addition of L MALIC ACID sodium and trimethylglycine may advantageously facilitate protease and play a role, improves small molecule fish
The yield of collagen oligopeptide；And the fish collagen oligopeptide that test group is prepared, content of beary metal are significantly lower than control group 2, say
Bright starch xanthate and mulberry leaf polysaccharide have gain effect, can be improved the removal rate of heavy metal ion in enzymolysis liquid.
Routine operation in operating procedure of the invention is well known to those skilled in the art, herein without repeating.
Technical solution of the present invention is described in detail in embodiment described above, it should be understood that the above is only
For specific embodiments of the present invention, it is not intended to restrict the invention, all any modifications made in spirit of the invention,
Supplement or similar fashion substitution etc., should all be included in the protection scope of the present invention.
Claims (9)
1. the preparation method of fish collagen oligopeptide, including raw material clean, mention glue, enzymatic hydrolysis, except metal, decoloration, deodorization and desalination, film
Filtering, nanofiltration, concentration, aseptic filtration, spray drying, it is characterised in that: contain L- in the protease that the enzymolysis process uses
Natrium malicum and trimethylglycine.
2. the preparation method of fish collagen oligopeptide according to claim 1, it is characterised in that: L- apple in the protease
The content of sour sodium is 1-5%, and the content of trimethylglycine is 0.3-0.8%.
3. the preparation method of fish collagen oligopeptide according to claim 1 or 2, it is characterised in that: the protease is multiple
Close flavor protease or papain or neutral proteinase or alkali protease.
4. the preparation method of fish collagen oligopeptide according to claim 1, it is characterised in that: described specific step is as follows:
(1) it cleans: the sodium hydroxide and salt of fish-skin food-grade 0.1-0.3% is cleaned according to the ratio of solid-liquid ratio 1:3-4
2-4h exhausts water, is then cleaned 5-8 times with tap water, cleaning to water be it is bright colourless, pH is spare in 8-9；
(2) it mentions glue: high-temperature water is added according to production ordering after feeding intake, mentions glue；
(3) it digests: adjusting pH to 8.0-8.5,50-55 DEG C of temperature, digested with the protease of fish-skin dosage 0.02-1.0%,
Heat up enzyme deactivation after enzymatic hydrolysis 1-4h；
(4) it removes metal: starch xanthate and mulberry leaf polysaccharide is added in enzymatic hydrolysis solution, is sufficiently mixed, after reacting 20-24h, warp
Diatomite filtering, obtains fish collagen oligopeptide clear liquid, and filter pressure is controlled in 0.2-0.6MP；
(5) decoloration, deodorization and desalination: the fish collagen oligopeptide clear liquid filtered passes sequentially through macroporous absorbent resin-cation and hands over
It changes resin-anion exchange resin to be adsorbed, removes color, peculiar smell and the salt in clear liquid, carried out after absorption with eluent
Elution；
(6) film filters: filter pressure is controlled in 0.15-0.20MPa, and flow control is in 6-8m3/h；
(7) nanofiltration: nanofiltration operating pressure is controlled in 1.2-1.3MPa, and material concentration is concentrated into 20-25% and stops nanofiltration；
(8) be concentrated: vacuum falling film concentration, temperature are controlled at 30-60 DEG C, and vacuum degree control is concentrated into -0.06 to -0.08MPa
Concentration is 35-45% discharging；
(9) aseptic filtration: guarantee the microbiological indicator of product by 0.22-0.45 microns of sterilization film low temperature degermings；
(10) it is spray-dried.
5. the preparation method of fish collagen oligopeptide according to claim 4, it is characterised in that: the condition for mentioning glue is
PH6.0-6.5,70-75 DEG C of temperature mentions glue.
6. the preparation method of fish collagen oligopeptide according to claim 4, it is characterised in that: described remove in metal process adds
The content of the starch xanthate entered is the 2-10% of enzymolysis liquid, and the content of mulberry leaf polysaccharide is the 1-2% of enzymolysis liquid.
7. the preparation method of fish collagen oligopeptide according to claim 4, it is characterised in that: the eluent is room temperature
Deionised water, flow velocity 2-3BV/h.
8. the preparation method of fish collagen oligopeptide according to claim 4, it is characterised in that: the condition of the spray drying
Are as follows: feed pressure 3.0-5.0MPa is spray-dried 80-95 DEG C of leaving air temp.
9. the preparation method of fish collagen oligopeptide according to claim 1, it is characterised in that: the fish collagen oligopeptide
It can be made into fish collagen oligopeptide powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811093580.8A CN109182432A (en) | 2018-09-19 | 2018-09-19 | The preparation method of fish collagen oligopeptide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811093580.8A CN109182432A (en) | 2018-09-19 | 2018-09-19 | The preparation method of fish collagen oligopeptide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109182432A true CN109182432A (en) | 2019-01-11 |
Family
ID=64908359
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811093580.8A Withdrawn CN109182432A (en) | 2018-09-19 | 2018-09-19 | The preparation method of fish collagen oligopeptide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109182432A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108821899A (en) * | 2018-09-28 | 2018-11-16 | 广州市云凌贸易有限公司 | It is a kind of to promote fish protein fertilizer of plant growth and preparation method thereof |
| CN110577975A (en) * | 2019-09-24 | 2019-12-17 | 福州海锐黎思生物科技有限责任公司 | Method for extracting and preparing swimming bladder collagen oligopeptide |
| CN111826411A (en) * | 2019-04-15 | 2020-10-27 | 罗士柱 | Method for preparing puffer fish collagen oligopeptide powder |
| CN114736288A (en) * | 2022-04-26 | 2022-07-12 | 河北昊鹿翔生物科技有限公司 | Collagen oligopeptide and extraction process thereof |
| CN115428912A (en) * | 2021-06-04 | 2022-12-06 | 烟台大学 | Normal-temperature instant sea cucumber and functional seasoning thereof |
-
2018
- 2018-09-19 CN CN201811093580.8A patent/CN109182432A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108821899A (en) * | 2018-09-28 | 2018-11-16 | 广州市云凌贸易有限公司 | It is a kind of to promote fish protein fertilizer of plant growth and preparation method thereof |
| CN111826411A (en) * | 2019-04-15 | 2020-10-27 | 罗士柱 | Method for preparing puffer fish collagen oligopeptide powder |
| CN110577975A (en) * | 2019-09-24 | 2019-12-17 | 福州海锐黎思生物科技有限责任公司 | Method for extracting and preparing swimming bladder collagen oligopeptide |
| CN115428912A (en) * | 2021-06-04 | 2022-12-06 | 烟台大学 | Normal-temperature instant sea cucumber and functional seasoning thereof |
| CN114736288A (en) * | 2022-04-26 | 2022-07-12 | 河北昊鹿翔生物科技有限公司 | Collagen oligopeptide and extraction process thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109182432A (en) | The preparation method of fish collagen oligopeptide | |
| US10414795B2 (en) | Techniques of preparing collagen active peptides | |
| US20230118351A1 (en) | Method for producing clam active peptide | |
| CN108103131A (en) | A kind of preparation process of ocean fish collagen oligopeptide powder and its application | |
| CN109845876A (en) | Highly purified soybean oligopeptide and preparation method and application with unique solubility for high energy | |
| CN110240626A (en) | A kind of quinoa polysaccharide polypeptide production method | |
| CN103014108A (en) | Preparation method of corn oligopeptide | |
| CN109486889A (en) | A kind of moringa seeds micromolecule polypeptide and its preparation process | |
| CN106359839A (en) | Extraction method of oyster peptides | |
| CN102228125B (en) | Preparation method of algal active peptide | |
| CN110029140A (en) | A kind of preparation method of wheat active peptide and the wheat active peptide of preparation | |
| CN109907327A (en) | A kind of abalone peptide and its production method | |
| CN107647385A (en) | A kind of fishbone dust and the preparation method of protein peptide mixture chewable tablets | |
| CN108517343A (en) | A kind of preparation method of the anti-oxidant protein peptides of Porphyra yezoensis | |
| CN101633947A (en) | New method for preparing sunflower seed meal proteolytic peptide and application of sunflower seed meal proteolytic peptide | |
| CN109293766A (en) | The method of collagen polypeptide is extracted from fish scale | |
| CN108588053B (en) | Enzyme special for animal protein hydrolysis and preparation method thereof | |
| CN109757601B (en) | Sea cucumber peptide and production method thereof | |
| CN106260551A (en) | Chelating calcium mixed feed and preparation method thereof | |
| CN110897059A (en) | Method for preparing plant hydrolyzed protein beverage by using wheat germs | |
| CN102277403B (en) | Production technology of yellow wine lees proteins by enzymatic extraction | |
| CN109777850A (en) | A kind of abalone tripe peptide and its production method and application | |
| CN107893095A (en) | A kind of method that marine source albumen prepares high F value oligopeptide | |
| CN105154505A (en) | Preparation method of feed grade ocean fish oligopeptide meal | |
| CN109369775A (en) | Low purine marine fishes oligopeptide and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20190111 |