CN105063153B - A kind of preparation method of food-grade low salt ocean fish oligopeptide powder - Google Patents
A kind of preparation method of food-grade low salt ocean fish oligopeptide powder Download PDFInfo
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Abstract
The present invention provides a kind of preparation methods of food-grade low salt ocean fish oligopeptide powder, using food-grade ocean low fat fish meal as raw material, grind, digest by washing pro desalting, colloid mill, UF membrane, concentration and spray drying are made.The present invention carries out washing pro desalting to raw material fish meal, remove most salinities in raw material fish meal, alleviate the pressure of subsequent nano-filtration film desalination, it is digested using food-grade industrialization protease preparation, enzymolysis liquid is detached by 1000~10000Da ultrafiltration membranes, it is stripped of molecular weight larger pigment and peptide, reuse the free amino acid in 150~500Da NF membranes removing enzymolysis liquid and remaining salinity, with high salt point of oligomeric peptide content is few in the fish oligopeptide powder of food-grade low salt obtained ocean, it can be widely applied for food service industry, it is suitble to large-scale industrial production.
Description
Technical field
This patent belongs to the preparation field of marine fish active peptide, and in particular to molecular weight is less than or equal to the food-grade of 1000Da
The preparation of low salt ocean fish oligopeptide.
Background technology
Oligopeptide refers to that one kind is made of 2~10 amino acid, the functional bioactive of 180~1000Da of molecular weight
Peptide.Research shows that oligopeptide has very strong bioactivity, including：Adjust hormone in vivo level；Improve minerals and micro member
Element absorbs；Resist bacterium and virus；Improve immunity；Inhibit and destroy tumour cell；Anti-oxidant and removing free radical etc..
China marine site is vast, and marine fish resource is abundant, with the fast development of Marine Fishing Industry, the low value fish of fishing
Ascendant trend is presented in yield, accounts for 60% of marine capture production or so.Due to rich in protein, low value fish mainly by with
It is processed into fish meal, as fodder protein additive, results in the loss of a large amount of protein resources in this way, it is low in economic efficiency.
If carrying out further deep processing to marine low-value fish meal, ocean fish oligopeptide is produced, marine low-value is not only can effectively improve
The availability of fish protein resource, moreover it is possible to improve value-added content of product, realize the substantially increment of economic benefit.
The salt content of usual ocean fish meal adjusts pH value in 2~5%, enzymolysis process can bring some salinities into again, these salt
The overwhelming majority is divided to be enriched in final Gly-His-Lys so that the salt content of Gly-His-Lys is up to 10~25%, and carrys out desalination by UF membrane merely
Effect is general, and energy consumption is of high cost greatly.It is a primary object of the present invention to overcome the deficiencies in the prior art, propose a kind of washing
Desalination is carried out in conjunction with the method for UF membrane, is digested using high-quality protease preparation, prepares food-grade low salt marine fish
Oligomeric Gly-His-Lys, lay a solid foundation for large-scale industrial production.
Invention content
The present invention industrializes protease preparation to food-grade ocean low fat made of marine low-value fish using food-grade
Fish meal is hydrolyzed, to obtain food-grade low salt ocean fish oligopeptide powder.Preparation method of the present invention includes washing
Pro desalting, colloid mill are ground, enzymolysis, UF membrane, concentrate and be spray-dried and etc..It is as follows：
（1）Pro desalting is washed, i.e., according to material water quality than 1:2~15 that food-grade ocean is added in pro desalting blending tank is low
5~50 DEG C, 40~100r/min of speed of agitator of temperature is arranged in fatty fish meal and pure water, washes 5~60min, then by 40~
The membrane pressure filter press filtration of 200 mesh obtains pro desalting fish meal.
（2）Colloid mill is ground, i.e., pro desalting fish meal is delivered in enzymolysis premix tank by screw conveyor, and
According to material water quality than 1:4~15 injection pure water, colloid mill is pumped into after stirring and evenly mixing by screw pump, will be pre- de- using colloid mill
Salt fish meal particulate abrasive is crushed to 40~80 mesh, increases the surface area of fish meal particle, convenient for being contacted with enzyme.
（3）Protease is added in enzymolysis, adjustment pH value to 6.0~10.0, and the mass ratio of control albumen enzyme-to-substrate is 0.1
~5%, 3~6h is digested at 40~65 DEG C；Enzymolysis terminates to be warming up to 80~99 DEG C, 10~25min of enzyme deactivation；Lead to respectively after cooling
The bag type filtering machine of the membrane pressure filter and 100~400 mesh of crossing 40~200 mesh carries out pressure-filtering deslagging together and two and crosses and filter out
Slag obtains enzymolysis liquid.
（4）UF membrane first uses first of 1000~10000Da ultrafiltration membranes to retain macromolecular peptide and color in enzymolysis liquid
Element then carries out being separated off free amino acid and residual salts using 150~500Da of second NF membranes pair, one of film permeate
Point, obtain the oligopeptide liquid that molecular weight is less than or equal to 1000Da, 20~60 DEG C, 0.4~1.2MPa of pressure of separation temperature, time 30
~180min.
（5）Concentration and spray drying, i.e., first use triple effect external circulation vacuum concentrator by the solid content of oligopeptide liquid
10~30% are concentrated into, it is 160~200 DEG C to reuse spray drying tower control inlet air temperature, and leaving air temp is 80~100 DEG C, right
Oligopeptide liquid is dried, and obtains food-grade low salt ocean fish oligopeptide powder, color be it is faint yellow or white, yield 10~
35%, oligomeric peptide content >=85%, protein hydrolysate proportion >=90% of the relative molecular mass less than 1000Da, salinity≤
4%, moisture≤6%, ash content≤5%.
As a kind of preferred embodiment of food-grade low salt of the present invention ocean fish oligopeptide powder, preparation method thereof, wherein：
The step（1）In preferably food-grade ocean low fat fish meal crude protein content 70-75%, moisture≤8.0%, crude fat≤
2.5%, protein content few hydrolysis result high in fat is good.It is preferred that material water quality is than 1:10, temperature 50 C, speed of agitator 100r/
Min washes 30min, removes the salinity in raw material fish meal as possible.
As a kind of preferred embodiment of food-grade low salt of the present invention ocean fish oligopeptide powder, preparation method thereof, wherein：
The step（2）In preferably expect water quality than 1:Pro desalting fish meal particulate abrasive is crushed to 80 mesh by 6, time 20min, is increased
The surface area that fish meal particle is contacted with enzyme.
As a kind of preferred embodiment of food-grade low salt of the present invention ocean fish oligopeptide powder, preparation method thereof, wherein：
The step（3）Middle preferred protease is the mixture of alkali protease and neutral proteinase, alkali protease such as NS 37071
（Novozymes Company of Denmark）, neutral proteinase such as Neutrase 0.8L（Novozymes Company of Denmark）, the additive amount of two kinds of protease
It is the 1% of substrate quality, optimal pH is respectively 8.5 and 7.5,55 DEG C of temperature, enzymolysis time 5h.The condition is conducive to alkalinity
Protease and neutral proteinase are fully hydrolyzed fish meal protein.
As a kind of preferred embodiment of food-grade low salt of the present invention ocean fish oligopeptide powder, preparation method thereof, wherein：
The step（4）In preferably molecular cut off 10000Da ultrafiltration membranes detached, 45 DEG C, pressure 1.2MPa of separation temperature, the time
40min removes the high molecular weight protein of 10000Da or more, and flux is big, and separative efficiency is high, avoids causing because disengaging time is long
Peptide liquid microbial contamination is smelly.It is preferred that molecular cut off 150Da NF membranes removing free amino acid and remaining salinity, separation temperature
40 DEG C, pressure 0.8MPa, time 60min of degree ensures to retain oligopeptide as possible while the most of salinity of removing and amino acid.
As a kind of preferred embodiment of food-grade low salt of the present invention ocean fish oligopeptide powder, preparation method thereof, wherein：
The step（5）In preferably oligopeptide liquid solid content be concentrated into 30%, convenient for spray drying.It is preferred that air inlet and the outlet temperature
Respectively 180 and 90 DEG C, Gly-His-Lys moisture is reduced as possible, is convenient for preservation.
The advantage of the invention is that：1）Washing pro desalting processing is carried out to fish meal raw material, is removed exhausted big in raw material fish meal
Part salinity alleviates the pressure of follow-up separating desalination；2）It is digested using high-quality protease, enzymolysis site is wide, item
Part is mild；3）Enzymolysis liquid is refined using advanced membrane separation technique, improves the quality of oligopeptide.
The present invention takes full advantage of the abundant low value stock of fish in China marine site, with high salt point of the oligomeric peptide content of Gly-His-Lys of preparation
It is few, food service industry is can be widely applied for, heavy industrialization continuous production is suitble to, for opening for China's marine low-value fish protein
Hair utilizes and opens new approach.
Specific implementation mode
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that real
It applies content described in example and is merely to illustrate the present invention, without sheet described in detail in claims should will not be limited
Invention.
Embodiment 1
Food-grade ocean low fat fish meal is through weighing balance precise, according to material water quality than 1:5 with pure water in pro desalting
It is mixed in blending tank, 25 DEG C, speed of agitator 60r/min of temperature is set, wash 10min, then the membrane pressure filter by 100 mesh
Press filtration obtains pro desalting fish meal, salt rejection rate 86.2%；Pro desalting fish meal is delivered to enzymolysis premix tank by screw conveyor
In, according to material water quality than 1:8 injection pure water, 60r/min by screw pump are pumped into colloid mill after stirring and evenly mixing, utilize colloid mill
Pro desalting fish meal particulate abrasive is crushed to 60 mesh, then is delivered in enzymatic vessel by screw pump and prepares to digest；Control temperature 50
DEG C, pH9.0, Novi letter alkali protease NS 37071 is added according to the 0.5% of substrate quality, it is defeated by screw pump after digesting 4h
It send into enzyme deactivation device and is warming up to 90 DEG C of enzyme deactivation 20min, obtained enzymolysis liquid is utilized respectively the membrane pressure filter and 200 of 100 mesh
Purpose bag type filtering machine carries out de- slag, the enzymolysis liquid to be removed the gred；The enzymolysis liquid of slagging-off enters after Pasteurizer sterilizes
Film separation system first detaches enzymolysis liquid using the membrane separator of molecular cut off 5000Da, separating pressure 0.6MPa, temperature
40 DEG C of degree, time 1.5h, the membrane separator that permeate reuses molecular cut off 300Da is detached, separating pressure 0.8MPa,
30 DEG C of temperature, time 2h obtain oligopeptide liquid；Oligopeptide liquid is concentrated into solid content by triple effect external circulation vacuum concentrator
It is spray-dried after 15%, drying condition is 165 DEG C of inlet temperature, and it is oligomeric to obtain food-grade low salt marine fish for 85 DEG C of outlet temperature
Gly-His-Lys.
After measured, food-grade low salt ocean fish oligopeptide powder, yield 20.74%, oligomeric peptide content made from the present embodiment
86.25%, 1000Da protein hydrolysate 90.30% below, salinity 3.44%, moisture 5.78%, ash content 4.26%.
Embodiment 2
Food-grade ocean low fat fish meal is through weighing balance precise, according to material water quality than 1:6 with pure water in pro desalting
It is mixed in blending tank, 30 DEG C, speed of agitator 60r/min of temperature is set, wash 20min, then the membrane pressure filter by 100 mesh
Press filtration obtains pro desalting fish meal, salt rejection rate 89.8%；Pro desalting fish meal is delivered to enzymolysis premix tank by screw conveyor
In, according to material water quality than 1:10 injection pure water, 60r/min by screw pump are pumped into colloid mill after stirring and evenly mixing, utilize colloid
Pro desalting fish meal particulate abrasive is crushed to 80 mesh by mill, then is delivered in enzymatic vessel by screw pump and is prepared to digest；Control temperature
55 DEG C, pH7.5 are added Novi according to the 0.8% of substrate quality and believe neutral proteinase Neutrase 0.8L, after digesting 6h, pass through
Screw pump, which is delivered in enzyme deactivation device, is warming up to 95 DEG C of enzyme deactivation 15min, and obtained enzymolysis liquid is utilized respectively the diaphragm type press filtration of 100 mesh
The bag type filtering machine of machine and 200 mesh carries out de- slag, the enzymolysis liquid to be removed the gred；The enzymolysis liquid of slagging-off sterilizes by Pasteurizer
Enter film separation system afterwards, first enzymolysis liquid is detached using the membrane separator of molecular cut off 3500Da, separating pressure
0.8MPa, temperature 50 C, time 2h, the membrane separator that permeate reuses molecular cut off 500Da are detached, separating pressure
30 DEG C of 0.8MPa, temperature, time 2h obtain oligopeptide liquid；Oligopeptide liquid is concentrated into solid by triple effect external circulation vacuum concentrator
It is spray-dried after shape object content 20%, drying condition is 170 DEG C of inlet temperature, and 90 DEG C of outlet temperature obtains food-grade low salt sea
Foreign fish oligopeptide powder.
After measured, food-grade low salt ocean fish oligopeptide powder, yield 15.34%, oligomeric peptide content made from the present embodiment
88.71%, 1000Da protolysate 90.83% below, salinity 2.45%, moisture 5.26%, ash content 3.17%.
Embodiment 3
Food-grade ocean low fat fish meal is through weighing balance precise, according to material water quality than 1:10 with pure water in pro desalting
It is mixed in blending tank, temperature 50 C is set, speed of agitator 60r/min washes 30min, then the membrane pressure filter by 100 mesh
Press filtration obtains pro desalting fish meal, salt rejection rate 94.8%；Pro desalting fish meal is delivered to enzymolysis premix tank by screw conveyor
In, according to material water quality than 1:6 injection pure water, 60r/min by screw pump are pumped into colloid mill after stirring and evenly mixing, utilize colloid mill
Pro desalting fish meal particulate abrasive is crushed to 100 mesh, then is delivered in enzymatic vessel by screw pump and prepares to digest；Control temperature 55
DEG C, pH8.5, be added Novi letter alkali protease NS 37071 according to the 1% of substrate quality, enzymolysis 0.5h waits for that pH is down to 7.0, then
1% Novi letter neutrality protease N eutrase 0.8L are added, continue to digest 4.5h；Obtained enzymolysis liquid is conveyed by screw pump
To 98 DEG C of enzyme deactivation 10min are warming up in enzyme deactivation device, it is utilized respectively the bag type filtering machine of the membrane pressure filter and 200 mesh of 100 mesh
Carry out de- slag, the enzymolysis liquid to be removed the gred；The enzymolysis liquid of slagging-off enters film separation system after Pasteurizer sterilizes, and first makes
Enzymolysis liquid is detached with the membrane separator of molecular cut off 10000Da, separating pressure 1.2MPa, temperature 45 C, time 1h,
The membrane separator that permeate reuses molecular cut off 150Da is detached, separating pressure 0.8MPa, temperature 45 C, time 2h,
Obtain oligopeptide liquid；Oligopeptide liquid is spray-dried after triple effect external circulation vacuum concentrator is concentrated into solid content 30%, is done
Dry condition is 180 DEG C of inlet temperature, and 90 DEG C of outlet temperature obtains food-grade low salt ocean fish oligopeptide powder.
After measured, food-grade low salt ocean fish oligopeptide powder, yield 25.74%, oligomeric peptide content made from the present embodiment
90.51%, 1000Da protein hydrolysate 92.63% below, salinity 3.88%, moisture 4.83%, ash content 4.82%.
Embodiment 4
Food-grade ocean low fat fish meal is through weighing balance precise, according to material water quality than 1:2 with pure water in pro desalting
It is mixed in blending tank, 5 DEG C, speed of agitator 40r/min of temperature is set, wash 5min, then the membrane pressure filter pressure for passing through 40 mesh
Filter obtains pro desalting fish meal, salt rejection rate 94.8%；Pro desalting fish meal is delivered in enzymolysis premix tank by screw conveyor,
According to material water quality than 1:4 injection pure water, 60r/min by screw pump are pumped into colloid mill after stirring and evenly mixing, utilize colloid mill will
Pro desalting fish meal particulate abrasive is crushed to 40 mesh, then is delivered in enzymatic vessel by screw pump and prepares to digest；40 DEG C of temperature of control,
Novi letter alkali protease NS 37071 is added according to the 0.1% of substrate quality in pH8.5, and enzymolysis 0.5h waits for that pH is down to 7.0, then adds
Add 1% Novi to believe neutrality protease N eutrase 0.8L, continues to digest 2.5h；Obtained enzymolysis liquid is delivered to by screw pump
80 DEG C of enzyme deactivation 10min are warming up in enzyme deactivation device, the bag type filtering machine of the membrane pressure filter and 100 mesh that are utilized respectively 40 mesh carries out
De- slag, the enzymolysis liquid to be removed the gred；The enzymolysis liquid of slagging-off enters film separation system after Pasteurizer sterilizes, and first uses and cuts
The membrane separator of molecular weight 1000Da is stayed to detach enzymolysis liquid, 20 DEG C, time 30min of separating pressure 0.4MPa, temperature, thoroughly
It crosses liquid and reuses the membrane separator of molecular cut off 150Da and detached, separating pressure 1.2MPa, temperature 60 C, the time
180min obtains oligopeptide liquid；Oligopeptide liquid is sprayed after triple effect external circulation vacuum concentrator is concentrated into solid content 10%
Dry, drying condition is 160 DEG C of inlet temperature, and 80 DEG C of outlet temperature obtains food-grade low salt ocean fish oligopeptide powder.
After measured, food-grade low salt ocean fish oligopeptide powder, yield 23.95%, oligomeric peptide content made from the present embodiment
88.45%, 1000Da protein hydrolysate 91.12% below, salinity 3.95%, moisture 4.97%, ash content 4.82%.
Embodiment 5
Food-grade ocean low fat fish meal is through weighing balance precise, according to material water quality than 1:15 with pure water in pro desalting
It is mixed in blending tank, temperature 50 C is set, speed of agitator 100r/min washes 60min, then the diaphragm type press filtration for passing through 200 mesh
Machine press filtration obtains pro desalting fish meal, salt rejection rate 94.8%；Pro desalting fish meal is delivered to enzymolysis premix tank by screw conveyor
In, according to material water quality than 1:15 injection pure water, 60r/min by screw pump are pumped into colloid mill after stirring and evenly mixing, utilize colloid
Pro desalting fish meal particulate abrasive is crushed to 80 mesh by mill, then is delivered in enzymatic vessel by screw pump and is prepared to digest；Control temperature
Novi letter alkali protease NS 37071 is added according to the 5% of substrate quality in 65 DEG C, pH8.5, and enzymolysis 2h waits for that pH is down to 7.0, then
5% Novi letter neutrality protease N eutrase 0.8L are added, continue to digest 4h；Obtained enzymolysis liquid is delivered to by screw pump
99 DEG C of enzyme deactivation 25min are warming up in enzyme deactivation device, be utilized respectively 200 mesh membrane pressure filter and 400 mesh bag type filtering machine into
The de- slag of row, the enzymolysis liquid to be removed the gred；The enzymolysis liquid of slagging-off enters film separation system after Pasteurizer sterilizes, and first uses
The membrane separator of molecular cut off 10000Da detaches enzymolysis liquid, 20 DEG C of separating pressure 0.4MPa, temperature, the time
30min, the membrane separator that permeate reuses molecular cut off 500Da are detached, separating pressure 1.2MPa, temperature 60 C,
Time 180min obtains oligopeptide liquid；Oligopeptide liquid is after triple effect external circulation vacuum concentrator is concentrated into solid content 10%
Spray drying, drying condition are 200 DEG C of inlet temperature, and 100 DEG C of outlet temperature obtains food-grade low salt ocean fish oligopeptide
Powder.
After measured, food-grade low salt ocean fish oligopeptide powder, yield 16.04%, oligomeric peptide content made from the present embodiment
89.22%, 1000Da protolysate 91.05% below, salinity 2.34%, moisture 4.99%, ash content 3.25%.
Claims (3)
1. a kind of preparation method of food-grade low salt ocean fish oligopeptide powder, which is characterized in that include the following steps：
（1）Pro desalting is washed, i.e., according to material water quality than 1:10 are added food-grade ocean low fat fish in pro desalting blending tank
Powder and pure water, are arranged temperature 50 C, and 40~100r/min of speed of agitator washes 20min, then the diaphragm type by 40~200 mesh
Filter press press filtration obtains pro desalting fish meal；The food-grade ocean low fat fish meal is marine low-value fish through low made of degreasing
Fatty fish protein powder, crude protein content 55-75%, moisture≤10.0%, crude fat≤4.0%；
（2）Colloid mill is ground, i.e., pro desalting fish meal is delivered in enzymolysis premix tank by screw conveyor, and according to
Expect water quality than 1:6 injection pure water, 20min by screw pump are pumped into colloid mill after stirring and evenly mixing, using colloid mill by pro desalting
Fish meal particulate abrasive is crushed to 80 mesh, increases the surface area of fish meal particle, convenient for being contacted with enzyme；
（3）Enzymolysis, 55 DEG C of temperature of control, pH8.5 are added alkali protease enzymolysis according to the 1% of substrate quality, wait for that pH is down to
7.5, then add 1% neutrality protease and continue to digest, digest total time 5h；Enzymolysis terminates to be warming up to 80~99 DEG C, and enzyme deactivation 10~
25min；It is pressed together by the bag type filtering machine of the membrane pressure filter of 40~200 mesh and 100~400 mesh respectively after cooling
It filters out bis- filtering and removing slag of Zha He and obtains enzymolysis liquid；
（4）UF membrane first uses first of 1000~10000Da ultrafiltration membranes to retain macromolecular peptide and pigment in enzymolysis liquid,
Then it carries out being separated off free amino acid and remaining salinity using 150~500Da of second NF membranes pair, one of film permeate,
Obtain molecular weight be less than or equal to 1000Da oligopeptide liquid, 20~60 DEG C, 0.4~1.2MPa of pressure of separation temperature, the time 30~
180min；
（5）Concentration and spray drying, i.e., first use triple effect external circulation vacuum concentrator to concentrate the solid content of oligopeptide liquid
To 10~30%, it is 160~200 DEG C to reuse spray drying tower control inlet air temperature, and leaving air temp is 80~100 DEG C, to oligomeric
Peptide liquid is dried, and obtains food-grade low salt ocean fish oligopeptide powder.
2. the preparation method of food-grade low salt according to claim 1 ocean fish oligopeptide powder, which is characterized in that step
（4）Described in UF membrane, used first of ultrafiltration membrane is the rolled membrane module that molecular cut off is 10000Da, separation
Temperature 45 C, pressure 1.2MPa, time 40min；The molecular cut off of second NF membrane is the rolled membrane module of 150Da, point
40 DEG C from temperature, pressure 0.8MPa, time 60min.
3. the preparation method of food-grade low salt according to claim 1 ocean fish oligopeptide powder, which is characterized in that step
（5）It is middle that oligopeptide liquid is concentrated into solid content 30%, the inlet air temperature of spray drying using triple effect external circulation vacuum concentrator
It it is 180 DEG C, leaving air temp is 90 DEG C.
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| CN106119328A (en) * | 2016-06-29 | 2016-11-16 | 大连深蓝肽科技研发有限公司 | A kind of high-quality shrimp oligopeptide powder, preparation method thereof of applicable industrialized production |
| CN106805252A (en) * | 2017-01-22 | 2017-06-09 | 福州大学 | A kind of fish small peptide and its application in nutrition fortifier |
| CN107893098A (en) * | 2018-01-12 | 2018-04-10 | 广州欧普康特医食品有限公司 | A kind of ocean fish oligopeptide and its preparation method and application |
| CN110074377B (en) * | 2019-05-23 | 2022-10-25 | 华南理工大学 | Flavor development peptide and preparation method and application thereof |
| CN112251485A (en) * | 2020-11-19 | 2021-01-22 | 南通途美机电设备有限公司 | Device for extracting active peptide from fresh marine fish and preparation method thereof |
| CN112544849A (en) * | 2020-12-08 | 2021-03-26 | 舟山市寂静水产有限公司 | Biological peptide preservation method |
| CN113512108B (en) * | 2021-03-23 | 2022-03-25 | 广州天启生物科技有限公司 | Marine fish skin collagen oligopeptide and preparation method and application thereof |
| CN113136409B (en) * | 2021-03-23 | 2022-03-29 | 广州天启生物科技有限公司 | Preparation method of food-grade low-salinity ocean fish oligopeptide |
| CN113174420B (en) * | 2021-04-23 | 2022-10-21 | 中海海洋科技股份有限公司 | Preparation method of high-yield marine fish oligopeptide product |
| CN113136330B (en) * | 2021-05-15 | 2022-09-23 | 德州蓝力生物技术有限公司 | Production and treatment device and process of cod skin collagen peptide |
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