CN108103131A - A kind of preparation process of ocean fish collagen oligopeptide powder and its application - Google Patents
A kind of preparation process of ocean fish collagen oligopeptide powder and its application Download PDFInfo
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- 102000008186 Collagen Human genes 0.000 title claims abstract description 62
- 108010035532 Collagen Proteins 0.000 title claims abstract description 62
- 229920001436 collagen Polymers 0.000 title claims abstract description 60
- 239000000843 powder Substances 0.000 title claims abstract description 44
- 108010038807 Oligopeptides Proteins 0.000 title claims abstract description 42
- 102000015636 Oligopeptides Human genes 0.000 title claims abstract description 42
- 241000251468 Actinopterygii Species 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 35
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 108090000765 processed proteins & peptides Proteins 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 10
- MVORZMQFXBLMHM-QWRGUYRKSA-N Gly-His-Lys Chemical compound NCCCC[C@@H](C(O)=O)NC(=O)[C@@H](NC(=O)CN)CC1=CN=CN1 MVORZMQFXBLMHM-QWRGUYRKSA-N 0.000 claims abstract description 7
- 108010038983 glycyl-histidyl-lysine Proteins 0.000 claims abstract description 7
- 239000003814 drug Substances 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims description 61
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 39
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 23
- 239000003292 glue Substances 0.000 claims description 23
- 239000000047 product Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 229940088598 enzyme Drugs 0.000 claims description 18
- 238000012856 packing Methods 0.000 claims description 16
- 102000004190 Enzymes Human genes 0.000 claims description 15
- 108090000790 Enzymes Proteins 0.000 claims description 15
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- 238000001514 detection method Methods 0.000 claims description 13
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- 235000013305 food Nutrition 0.000 claims description 8
- 238000005516 engineering process Methods 0.000 claims description 7
- 238000005374 membrane filtration Methods 0.000 claims description 7
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- 108091005804 Peptidases Proteins 0.000 claims description 5
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 claims description 5
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- 230000009849 deactivation Effects 0.000 claims description 5
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- 235000019419 proteases Nutrition 0.000 claims description 5
- 229920000742 Cotton Polymers 0.000 claims description 4
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- 239000007787 solid Substances 0.000 claims description 4
- 230000001954 sterilising effect Effects 0.000 claims description 4
- 238000004659 sterilization and disinfection Methods 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
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- 235000020679 tap water Nutrition 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 3
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- 239000002131 composite material Substances 0.000 claims description 3
- 229940079593 drug Drugs 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
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- 108091005508 Acid proteases Proteins 0.000 claims description 2
- 108010004032 Bromelains Proteins 0.000 claims description 2
- JJWSNOOGIUMOEE-UHFFFAOYSA-N Monomethylmercury Chemical compound [Hg]C JJWSNOOGIUMOEE-UHFFFAOYSA-N 0.000 claims description 2
- 108090000526 Papain Proteins 0.000 claims description 2
- 101000693530 Staphylococcus aureus Staphylokinase Proteins 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 229910052785 arsenic Inorganic materials 0.000 claims description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 2
- 235000019835 bromelain Nutrition 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
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- 244000248349 Citrus limon Species 0.000 claims 1
- 235000005979 Citrus limon Nutrition 0.000 claims 1
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- 230000002906 microbiologic effect Effects 0.000 claims 1
- -1 trypsase Proteins 0.000 claims 1
- 238000002156 mixing Methods 0.000 abstract description 4
- 239000002775 capsule Substances 0.000 abstract 1
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- 239000003826 tablet Substances 0.000 abstract 1
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- 102000004196 processed proteins & peptides Human genes 0.000 description 3
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- 230000004308 accommodation Effects 0.000 description 2
- 230000003712 anti-aging effect Effects 0.000 description 2
- 230000002929 anti-fatigue Effects 0.000 description 2
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- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical class [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
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Classifications
-
- 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
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/17—Amino acids, peptides or proteins
- A23L33/18—Peptides; Protein hydrolysates
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Abstract
The present invention provides a kind of ocean fish collagen oligopeptide powder, preparation method thereof and its applications, using ocean fish-skin as raw material, by the method for acidolysis, enzymolysis mixing, prepare the oligomeric Gly-His-Lys that oligomeric peptide content is higher than 96%.It can be widely applied to the wine industry, drink industry, flavouring industry, healthcare industry, the functional foods such as oral liquid, tablet, capsule and medicine trade field.
Description
Technical field
The invention belongs to food processing technology field more particularly to a kind of preparation method of ocean fish collagen oligopeptide powder and
Using.
Background technology
Collagen molecules amount wider distribution, the big collagen human body of molecular weight are difficult to absorb, and are suitable for steady
Determine agent, emulsifier, fining agent etc..The smaller 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 easily absorbs, 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, ocean fish collagen oligopeptide is a kind of deep processed product of common ocean Isin glue collagen, with pollution-free or pollution phase
It is raw material to smaller fish-skin, bone, refined to be process, they are mostly be made of 2-6 amino acid, molecule quantity set
In in the small molecule of 200-1000 dalton mix peptides, can directly be absorbed by small intestine, human skin etc., with powerful battalion
Characteristic is supported, application is extensive, is the dispensing of new nutritious and healthy food, has its unique advantage in nutrition and application aspect.
Ocean fish oligopeptide main function has following several respects：1st, it can effectively solve the problem that skin and the reduction of muscle moisture are asked
Topic, supplements collagen peptide in due course, and skin can be made to keep young.2nd, make it is calcareous combine closely with osteocyte, will not be lost in or degenerate.3、
Cornea can be made to keep moistening transparent, increase eyes transparency.4th, promote muscle cell tight union, make it have elasticity and light
Pool.5th, endocrine, protection are adjusted and strengthens viscera function.6th, binding domain-immunoglobulin increases immunity.Based on ocean collagen
The advantage broadly above that oligopeptide has, using ocean fish collagen oligopeptide as the cosmetics of raw material and additive, food
It is welcomed by the people.Due to its unique nutritive value, containing various bioactivators, on the one hand with land raw material
On the other hand not available free of contamination characteristic provides an effective approach for the deep processing and utilization of fish.So
And in China, active material is extracted from marine organisms using modern means of science and technology, is developed as drug, the work of health food
Still it is in the stage for being badly in need of development.
The method of extraction ocean fish 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, is synthesized by chemical method and recombinant DNA technology, 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 leak is less, and non-environmental-pollution.At present, enzymolysis marine collagen albumen mainly has single enzyme
Method and multi-enzyme method, multi-enzyme method are divided into as mixed enzyme solution and stepwise discretization method.The condition of enzymolysis and extraction active peptide is typically considered as
Requirement of institute's development to molecular weight, the smaller product of molecular weight preferably use multi-enzyme method.Chinese patent literature CN107365824A
A kind of preparation method for hydrolyzing Isin glue collagen Gly-His-Lys is disclosed, mainly includes alkaline process ozone air-float except raw meat degreasing, filtering removal
Filtrate, the aspergillus oryzae Qushui River solution, filtrate through enzyme deactivation, concentrate, be dried to obtain hydrolysis fish collagen protein powder the step of.Fish is hydrolyzed in extraction
The early period of collagen peptide is removed in raw meat, skimming processes, using lye ozone air-float fulling, is simplified production technology, is especially existed
Using bent method zymolysis technique in Isin glue collagen extraction process, production cost is greatly reduced, although extraction process is quick and convenient,
Isin glue collagen peptide output capacity is high, and impurity is few, however, enzymolysis process raw material and condition are uncontrollable, causes enzymolysis product property not
Stablize.Chinese patent literature CN 103540635A disclose a kind of preparation process of fish scale collagen, and the technique by locating in advance
Reason, colloidal sol, enzymolysis, filtration drying and etc. be prepared for collagen protein powder, fish scale is made to turn waste into wealth, realizes the abundant profit of resource
With, but the method raw material fish scale source is limited, and complex technical process, it is impossible to large-scale production, and the glue that Optimization of Low Value Fish is intrinsic
Former protein peptides antibacterial effect is weak, and medical value is limited, and reduces the economic value of product.Chinese patent literature CN103388017A
A kind of method that two steps enzymatic isolation method prepares fish skin collagen oligopeptide is disclosed, step includes pretreatment, two steps digest, it is dense to purify
Contracting, rapid draing, collagen yield are more than 85%, and for white or pale yellow powder, purity is more than 90%, and molecular weight is small
In 1000Da, the above-mentioned method safety for preparing collagen oligopeptide is easy, but the oligopeptides sample protein content prepared is low, molecular weight distribution
It is relatively wide, it is not easy to absorb.In addition, pH value, the production processed are adjusted using technical-grade hydrochloric acid and sodium hydroxide in hydrolytic process
Product final quality cannot reach food-grade requirement or since the fishy smell of fish-skin itself causes the albumen peptide product fishy smell prepared
Weight, content of beary metal is high or even cannot meet collagen content height simultaneously, the micromolecular collagen oligopeptide that molecular weight is concentrated
Requirement.
The content of the invention
In order to solve the above problem in the prior art, the stock of fish is made full use of, nutritional ingredient is solved and wastes serious ask
Topic, the present invention provide a kind of preparation method of ocean fish collagen oligopeptide powder, although using acid-base accommodation pH value in preparation process,
But not the processing quality of product is influenced, while fish-skin itself fishy smell and heavy metal can be effectively removed, and obtains collagen
The oligomeric Gly-His-Lys of small molecule collagen that content is high, molecular weight is concentrated.
The present invention is achieved through the following technical solutions：
A kind of preparation method of ocean fish collagen oligopeptide powder, including following production technology：
Raw material → cleaning → carry glue → filtering and standing → cottonseed cake filtering → enzymolysis → decoloration → plate-frame filtering → membrane filtration →
Nanofiltration → concentration → aseptic filtration → spray drying → receipts powder inner packing → metal detection outer packing.
The preparation method of ocean as described above fish collagen oligopeptide powder, specifically includes following steps：
(1) clean：By the food sodium hydroxide and salt of fish-skin food-grade 0.1%-0.3%, according to solid-liquid ratio 1：3
Ratio cleaning 2-4h water is exhausted, then clean 8 times or so with tap water, it is bright colourless to clean to water, pH 9 or so,
It is spare；
(2) glue is carried：High-temperature water is added according to production ordering after feeding intake, carries glue；
(3) filtering and standing：The complete feed liquid of glue will be put forward and stand 2-4h in settling tank again after the filtering of triangle sieves, treated point
Discharge filtering after layer；
(4) cottonseed cake filters：Supernatant is filtered by cotton cake filtering machine, entire filter pressure is controlled in 0.2MPa,
The turbidity of feed liquid is controlled within 100NTU；
(5) digest：After filtering, Ph to 8.0 or so, 50-55 DEG C of temperature, with the albumen of fish-skin dosage 0.02-1.0% are adjusted
Enzyme is digested, and heat up enzyme deactivation after enzymolysis 1-4h；
(6) decolourize：Activated carbon of the material liquid volume than 0.1-0.3% is added in, is discharged after keeping the temperature 40min；
(7) plate-frame filtering：Decoloration terminates laggard such as plate-frame filtering, and the pressure of plate-frame filtering is controlled within 0.4MPa, material
Liquid is into being ejected feed liquid in sheet frame with purified water after complete, until filtering terminates when solid content is 0；
(8) membrane filtration：Filter pressure is controlled in 0.15MPa, and flow control is in 6-8m3/h；
(9) nanofiltration：Nanofiltration operating pressure is controlled in 1.2-1.3MPa, and material concentration is concentrated into 20-25% and stops nanofiltration；
(10) concentrate：Vacuum falling film concentrates, and temperature is controlled within 60 DEG C, vacuum degree control -0.06 to -0.08MPa,
Concentration is concentrated into discharge for 35-45%；
(11) aseptic filtration：The microorganism for ensureing product by 0.45 micron and 0.22 micron of sterilization film low temperature degerming refers to
Mark；
(12) it is spray-dried：Product after aseptic filtration is spray-dried；
(13) powder inner packing is received：It is spray-dried out after powder crosses the vibrating screen of 20 mesh and is packaged into 5kg/ bags or 10kg/ bags；
(14) metal detection outer packing：It is without exception by metal detector (sus2.5mm, Fe2.0mm) after detection is qualified
After carry out outer packing.
Preferably, step (2) carries glue and adjusts pH6, and 75 DEG C carry glue；
Preferably, the discarded part after step (3), step (4) filtering adds in citric acid solution, 2- after fully shaking mixing
5 it is small when after discharge, further with step (6) in discharging together with enter step (7) plate-frame filtering the step of.
Preferably, the concentration of citric acid is preferably 0.5-1.5mol/L in above-mentioned steps, more preferably 1mol/L；Citric acid
Additional proportion is preferably discarded part：Citric acid is 1：5-10 (volume ratio), more preferably discarded part：Citric acid is 1：8 (bodies
Product ratio)；It is preferred that when stirring 5 is small.
Preferably, step (5) protease be preferably albumen composite hydrolytic enzyme, papain, neutral proteinase, trypsase,
Any one in acid protease, bromelain, alkali protease.
Preferably, step (12) is spray-dried：Feed pressure 3.0-5.0MPa is spray-dried 80-95 DEG C of leaving air temp；It is excellent
Select 80 DEG C.
The present invention also provides the ocean fish collagen oligopeptide powder that a kind of as above method is prepared, the collagen is oligomeric
Gly-His-Lys are in terms of butt：Oligomeric peptide content >=96.5%, ash content ＜ 0.5%, molecular weight 300-850Dalton, average molecular weight
For 550Dalton, lead (mg/kg)≤0.2 in heavy metallic salt, cadmium (mg/kg)≤0.06, inorganic arsenic (mg/kg)≤0.1, methyl
Mercury (mg/kg)≤0.2.
The present invention also provides a kind of purposes for the ocean fish collagen oligopeptide powder that as above method is prepared, as food
Product, drug or health products active ingredient or additive use.
In ocean fish collagen oligopeptide powder in the present invention more than 96%, and ash content are up to rich in oligopeptide, content
Less than 0.5%, impurity is substantially free of.Molecular weight concentrate on 300-850 dalton small molecule mixing peptides, can by small intestine,
Human skin etc. directly absorbs.Average molecular weight is 550 dalton, and dissolubility is good, can dissolve water under room temperature rapidly, is formed equal
Even scattered solution.
There is moisturizing and nourishing, strengthen rich in amino acid, absorption easy to digest in ocean fish collagen oligopeptide powder in the present invention
Immunity of organisms, anti-aging, antifatigue, beauty, anti-oxidant and other effects.
The beneficial effects are mainly as follows the following aspects：
(1) compared with prior art, fish collagen oligopeptide powder in ocean of the present invention, using traditional enzymolysis and extraction skill
Art, the effective collagen extracted in fish-skin；The method preferably combined simultaneously using zymohydrolysis extracting method with sour formulation, to part
Extraction waste part is extracted again, has given full play to the sour technical advantage put forward with enzymatic isolation method, by the more thorough of fish-skin extraction.
(2) fish collagen oligopeptide powder in ocean of the present invention contains oligopeptide, has moisturizing and nourishing, strengthens immunity of organism
Power, anti-aging, antifatigue, beauty, anti-oxidant and other effects, human body can directly absorb, and reduce the waste of nutritional ingredient.
(3) in fish collagen oligopeptide powder extraction process in ocean of the present invention, although employing sodium hydroxide and salt
The method for adjusting pH value, pollution problem caused by still avoiding when using a large amount of soda acids, and due to rear and employ acid
Extraction method, be effectively reduced sodium hydroxide and salt adjust the product final quality that pH is brought decline, environmental pollution the problem of.
(4) in fish collagen oligopeptide powder extraction process in ocean of the present invention, by plate-frame filtering, → membrane filtration → is received
The problem of the methods of filter effectively avoids albumen peptide product fishy smell weight, and content of beary metal is high, effectively eliminates fish-skin itself
Fishy smell and heavy metal.
(5) in fish collagen oligopeptide powder extraction process in ocean of the present invention, extracted again by adding in citric acid
Method obtains collagen content height, the oligomeric Gly-His-Lys of small molecule collagen that molecular weight is concentrated.
(6) raw material sources of the invention are extensive, and extracting method is simply controllable, and product quality is stablized, beneficial to production application.
Specific embodiment
With reference to embodiment, present disclosure is further illustrated.It should be appreciated that the implementation of the present invention is not limited to
In the following examples, the accommodation in any form and/or change made to the present invention fall within the scope of the present invention.
In the present invention, if not refering in particular to, all parts, percentage are unit of weight, and all equipment and raw material etc. are equal
It is commercially available or the industry is common.Method in following embodiments is the routine of this field unless otherwise instructed
Method.
Embodiment 1
Ocean fish collagen oligopeptide powder, prepares according to following steps：
(1) clean：By the food sodium hydroxide and salt of fish-skin food-grade 0.1%-0.3%, according to solid-liquid ratio 1：3
Ratio cleaning 2-4h water is exhausted, then clean 8 times or so with tap water, it is bright colourless to clean to water, pH 9 or so,
It is spare；
(2) glue is carried：High-temperature water is added according to production ordering after feeding intake, adjusts pH6,75 DEG C carry glue；
(3) filtering and standing：The complete feed liquid of glue will be put forward and stand 2-4h in settling tank again after the filtering of triangle sieves, treated point
Discharge filtering after layer；
(4) cottonseed cake filters：Supernatant is filtered by cotton cake filtering machine, entire filter pressure is controlled in 0.2MPa,
The turbidity of feed liquid is controlled within 100NUT；
(5) digest：After filtering, pH is adjusted 8.0 or so, 50-55 DEG C of temperature, with albumen composite hydrolytic enzyme, albumen enzyme amount
0.02-1.0% is digested, and heat up enzyme deactivation after enzymolysis 1-4h；
(6) decolourize：Activated carbon of the material liquid volume than 0.1-0.3% is added in, is discharged after keeping the temperature 40min；
(7) plate-frame filtering：Decoloration terminates laggard such as plate-frame filtering, and the pressure of plate-frame filtering is controlled within 0.4MPa, material
Liquid is into being ejected feed liquid in sheet frame with purified water after complete, until filtering terminates when solid content is 0；
(8) membrane filtration：Filter pressure is controlled in 0.15MPa, and flow control is in 6-8 cubes/h；
(9) nanofiltration：Nanofiltration operating pressure is controlled in 1.2-1.3MPa, and material concentration is concentrated into 20-25% and stops nanofiltration；
(10) concentrate：Vacuum falling film concentrate, temperature control within 60 degrees Celsius, vacuum degree control -0.06 to -
0.08MPa is concentrated into concentration and discharges for 35-45%；
(11) aseptic filtration：The microorganism for ensureing product by 0.45 micron and 0.22 micron of sterilization film low temperature degerming refers to
Mark；
(12) it is spray-dried：Product after aseptic filtration is spray-dried；Feed pressure 3.0-5.0MPa, spraying are dry
Dry 80 DEG C of leaving air temp；
(13) powder inner packing is received：It is spray-dried out after powder crosses the vibrating screen of 20 mesh and is packaged into 5kg/ bags or 10kg/ bags；
(14) metal detection outer packing：It is without exception by metal detector (sus2.5mm, Fe2.0mm) after detection is qualified
After carry out outer packing.
Embodiment 2
Preferably, fish collagen oligopeptide powder in ocean of the present invention, prepares according to following steps：
(1) clean：By the food sodium hydroxide and salt of fish-skin food-grade 0.1%-0.3%, according to solid-liquid ratio 1：3
Ratio cleaning 2-4h water is exhausted, then clean 8 times or so with tap water, it is bright colourless to clean to water, pH 9 or so,
It is spare；
(2) glue is carried：High-temperature water is added according to production ordering after feeding intake, adjusts pH6,75 DEG C carry glue；
(3) filtering and standing：The complete feed liquid of glue will be put forward and stand 2-4h in settling tank again after the filtering of triangle sieves, treated point
Discharge filtering after layer；
(4) cottonseed cake filters：Supernatant is filtered by cotton cake filtering machine, entire filter pressure is controlled in 0.2MPa,
The turbidity of feed liquid is controlled within 100NUT；
Discarded part after step (3), step (4) filtering adds in 1mol/L citric acid solutions, and citric acid additional proportion is excellent
Elect discarded part as：Citric acid is 1：8 (volume ratios)；Fully shaking mixing after 5 it is small when after discharge, further with following step
(6) the step of discharging enters step (7) plate-frame filtering together in.
(5) digest：After filtering, pH is adjusted 8.0 or so, 50-55 DEG C of temperature, with trypsase, tryptose enzyme amount 0.02-
1.0% is digested, and heat up enzyme deactivation after enzymolysis 1-4h；
(6) decolourize：Activated carbon of the material liquid volume than 0.1-0.3% is added in, is discharged after keeping the temperature 40min；
(7) plate-frame filtering：Decoloration terminates laggard such as plate-frame filtering, and the pressure of plate-frame filtering is controlled within 0.4MPa, material
Liquid is into being ejected feed liquid in sheet frame with purified water after complete, until filtering terminates when solid content is 0；
(8) membrane filtration：Filter pressure is controlled in 0.15MPa, and flow control is in 6-8 cubes/h；
(9) nanofiltration：Nanofiltration operating pressure is controlled in 1.2-1.3MPa, and material concentration is concentrated into 20-25% and stops nanofiltration；
(10) concentrate：Vacuum falling film concentrate, temperature control within 60 degrees Celsius, vacuum degree control -0.06 to -
0.08MPa is concentrated into concentration and discharges for 35-45%；
(11) aseptic filtration：The microorganism for ensureing product by 0.45 micron and 0.22 micron of sterilization film low temperature degerming refers to
Mark；
(12) it is spray-dried：Product after aseptic filtration is spray-dried；Feed pressure 3.0-5.0MPa, spraying are dry
Dry 80 DEG C of leaving air temp；
(13) powder inner packing is received：It is spray-dried out after powder crosses the vibrating screen of 20 mesh and is packaged into 5kg/ bags or 10kg/ bags；
(14) metal detection outer packing：It is without exception by metal detector (sus2.5mm, Fe2.0mm) after detection is qualified
After carry out outer packing.
Ocean fish collagen oligopeptide powder described in above-described embodiment 1-2, using ocean fish oligopeptide powder GB/T22729-
The standard of defined and detection method are (clear to the sense organ, molecular weight, transmittance of the oligomeric Gly-His-Lys of collagen in above-described embodiment in 2008
Clear degree), heavy metallic salt content be detected and evaluate, wherein taking sample 20g, be placed in the glass plate of clean water white transparency, in
Natural light or the interior for being equivalent to natural light differentiate its structural state with tactile, depending on its color and luster, impurity, smell its smell, its taste of product
Taste carries out organoleptic examination.Other detections are measured according to method as defined in coherent detection.After testing, it the results are shown in Table 1.
The requirement of 1 standard of table and the testing result of embodiment 1-2 compare
From the point of view of table 1, the white powder of ocean fish collagen oligopeptide powder of the present invention, soluble easily in water, the peculiar smell such as no fishy smell,
And its heavy metallic salt content is low, hence it is evident that less than the requirement in standard.Molecular weight contains less than the oligopeptide in 300-850 dalton
Amount >=96%, ash content≤0.5%.
Although inventor has done technical scheme more detailed elaboration and has enumerated, it should be understood that right
For the those skilled in the art of this field one, modification is made to above-described embodiment or uses equivalent alternative solution, this
It is it is clear that these made without departing from theon the basis of the spirit of the present invention are changed or changed to those skilled in the art
Into belonging to the scope of protection of present invention.
Claims (9)
1. a kind of preparation method of ocean fish collagen oligopeptide powder, including following production technology：
Raw material → cleaning → proposes glue → filtering and standing → cottonseed cake filtering → enzymolysis → decoloration → plate-frame filtering → membrane filtration → nanofiltration
→ concentration → aseptic filtration → spray drying → receipts powder inner packing → metal detection outer packing.
2. the preparation method of fish collagen oligopeptide powder in ocean according to claim 1, which is characterized in that specifically include following
Step：
(1) clean：By fish-skin with 1:The food sodium hydroxide and saline solution of the 0.1-0.3% of 3 ratios is cleaned, after 2-4h
Water is exhausted, is then cleaned 8 times or so with tap water, is cleaned to water to be bright colourless, pH is spare 9 or so；
(2) glue is carried：High-temperature water is added according to production ordering after feeding intake, carries glue；
(3) filtering and standing：The complete feed liquid of glue will be put forward, 2-4h is stood in settling tank after the filtering of triangle sieves, after being layered
Discharging filtering；
(4) cottonseed cake filters：Supernatant is filtered by cotton cake filtering machine, entire filter pressure is controlled in 0.1-0.3MPa,
The turbidity of feed liquid is controlled within 100NTU；
(5) digest：After filtering, adjust pH to 8.0 or so, 50-55 DEG C of temperature, with the protease of fish-skin weight 0.02-1.0% into
Row digests, and heat up enzyme deactivation after enzymolysis 1-4h；
(6) decolourize：Activated carbon stirring of the material liquid volume than 0.1-0.3% is added in, is discharged after keeping the temperature 40min；
(7) plate-frame filtering：Into plate-frame filtering after decoloration, the pressure of plate-frame filtering is controlled within 0.4MPa, feed liquid into
Feed liquid in sheet frame is ejected with purified water after complete, until filtering terminates when solid content is 0%；
(8) membrane filtration：Filter pressure is controlled in 0.15MPa, and flow control is in 6-8m3/h；
(9) nanofiltration：Nanofiltration operating pressure is controlled in 1.2-1.3MPa, and material concentration is concentrated into 20-25% and stops nanofiltration；
(10) concentrate：Vacuum falling film concentrates, and temperature is controlled within 60 DEG C, and vacuum degree control is -0.06 to -0.08MPa, concentration
It discharges to concentration for 35-45%；
(11) aseptic filtration：Ensure the microbiological indicator of product by 0.45 micron and 0.22 micron of sterilization film low temperature degerming；
(12) it is spray-dried：Product after aseptic filtration is spray-dried；
(13) powder inner packing is received：It is spray-dried out after powder crosses the vibrating screen of 20 mesh and packs；
(14) metal detection outer packing：It is without exception laggard by metal detector (sus2.5mm, Fe2.0mm) after detection is qualified
Row outer packing.
3. according to the preparation method of claim 1-2 any one of them ocean fish collagen oligopeptide powder, which is characterized in that step
(2) carry glue and adjust pH6,75 DEG C carry glue.
4. according to the preparation method of claim 1-3 any one of them ocean fish collagen oligopeptide powder, which is characterized in that step
(3), step (4) filtering after discarded part add in citric acid solution, be sufficiently stirred rear 2-5 it is small when after discharge, further with step
Suddenly the step of discharging enters step (7) plate-frame filtering together in (6).
5. according to the preparation method of claim 1-4 any one of them ocean fish collagen oligopeptide powder, lemon in above-mentioned steps
The concentration of acid is preferably 0.5-1.5mol/L, more preferably 1mol/L；Citric acid additional proportion is preferably discarded part：Citric acid
For 1：5-10 (volume ratio), more preferably discarded part：Citric acid is 1：8 (volume ratios)；It is preferred that when stirring 5 is small.
6. according to the preparation method of claim 1-5 any one of them ocean fish collagen oligopeptide powder, step (5) protease is excellent
It elects as in albumen composite hydrolytic enzyme, papain, neutral proteinase, trypsase, acid protease, bromelain, alkali protease
Any one.
7. according to the preparation method of claim 1-6 any one of them ocean fish collagen oligopeptide powder, step (12) spraying is dry
It is dry：Feed pressure 3.0-5.0MPa is spray-dried 80-95 DEG C of leaving air temp；It is preferred that 80 DEG C.
8. a kind of ocean fish collagen oligopeptide powder being prepared such as any one of claim 1-7 method, the collagen are oligomeric
Gly-His-Lys are in terms of butt：Oligomeric peptide content >=96.5%, ash content ＜ 0.5%, molecular weight 300-850Dalton, average molecular weight
For 550Dalton, lead (mg/kg)≤0.2 in heavy metallic salt, cadmium (mg/kg)≤0.06, inorganic arsenic (mg/kg)≤0.1, methyl
Mercury (mg/kg)≤0.2.
9. a kind of purposes of the ocean fish collagen oligopeptide powder described in claim 8, as food, drug or health products activity into
Divide or additive uses.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109811026A (en) * | 2019-03-08 | 2019-05-28 | 福建康是美生物科技有限公司 | A kind of extracting method of collagen |
| CN109832536A (en) * | 2018-09-28 | 2019-06-04 | 北京姿美堂生物技术有限公司 | A kind of taste collagen solid beverage and preparation method thereof |
| 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 |
| WO2020087857A1 (en) * | 2018-10-31 | 2020-05-07 | 广东兴亿海洋生物工程股份有限公司 | Low-purine marine fish oligopeptide and preparation method therefor |
| CN111165649A (en) * | 2020-01-14 | 2020-05-19 | 潘志杰 | Equipment and processing technology for preparing ocean fish oligopeptide powder |
| CN111826411A (en) * | 2019-04-15 | 2020-10-27 | 罗士柱 | Method for preparing puffer fish collagen oligopeptide powder |
| CN115581300A (en) * | 2018-08-20 | 2023-01-10 | 北京姿美堂生物技术有限公司 | Composition for relieving fatigue and enhancing immunity and preparation method thereof |
| CN117736307A (en) * | 2024-02-19 | 2024-03-22 | 北京盛美诺生物技术有限公司 | III type small molecule collagen peptide capable of promoting III type and IV type collagen secretion and preparation method thereof |
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| CN115581300A (en) * | 2018-08-20 | 2023-01-10 | 北京姿美堂生物技术有限公司 | Composition for relieving fatigue and enhancing immunity and preparation method thereof |
| CN109832536A (en) * | 2018-09-28 | 2019-06-04 | 北京姿美堂生物技术有限公司 | A kind of taste collagen solid beverage and preparation method thereof |
| WO2020087857A1 (en) * | 2018-10-31 | 2020-05-07 | 广东兴亿海洋生物工程股份有限公司 | Low-purine marine fish oligopeptide and preparation method therefor |
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| CN111826411A (en) * | 2019-04-15 | 2020-10-27 | 罗士柱 | Method for preparing puffer fish collagen oligopeptide powder |
| 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 |
| CN111165649A (en) * | 2020-01-14 | 2020-05-19 | 潘志杰 | Equipment and processing technology for preparing ocean fish oligopeptide powder |
| CN117736307A (en) * | 2024-02-19 | 2024-03-22 | 北京盛美诺生物技术有限公司 | III type small molecule collagen peptide capable of promoting III type and IV type collagen secretion and preparation method thereof |
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