CN113980110A - Method for preparing protein peptide by using euphausia superba shelling wastewater - Google Patents
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
- C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
- C07K14/43504—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates
- C07K14/43509—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans from invertebrates from crustaceans
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- 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
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- 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
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- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- C12N9/00—Enzymes; Proenzymes; Compositions thereof; Processes for preparing, activating, inhibiting, separating or purifying enzymes
- C12N9/0004—Oxidoreductases (1.)
- C12N9/0006—Oxidoreductases (1.) acting on CH-OH groups as donors (1.1)
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention relates to the field of efficient utilization of marine biological resources, and particularly relates to a method for preparing protein peptide by using euphausia superba shelling wastewater. The method comprises the following steps: recovering shelling waste water; concentrating the recovered solution to obtain a concentrated solution; heating the concentrated solution to obtain thermal condensate and enzymolysis solution; primary separation; defluorination; secondary separation; membrane separation; spray drying to obtain the final product. According to the invention, the antarctic krill protein peptide is obtained by recovering the antarctic krill shelling wastewater for concentration and further deep processing, so that the effective utilization rate of the antarctic krill biological resources is improved.
Description
The technical field is as follows:
the invention relates to the field of efficient utilization of marine biological resources, and particularly relates to a method for preparing protein peptide by using euphausia superba shelling wastewater.
Background art:
antarctic krill is a crustacean living in sea areas around the continents of Antarctica, and the biomass of the crustacean is huge, and with the development of the ocean fishing industry, the fishing of Antarctic krill becomes a new growing point of the ocean fishing industry. At present, after being captured for a plurality of times, antarctic krill are directly processed into frozen products or dried into shrimp meal on an antarctic krill capturing ship, and a few of antarctic krill are processed into shrimp meat. With consumer awareness of antarctic krill, market demand for shrimp meat is increasing. The problem is that the shipborne shelled shrimps are low in processing efficiency and cannot meet a large amount of consumption requirements; the ground-based processing of the euphausia superba kernels is limited by the fact that the euphausia superba kernels are thawed after being frozen, krill protein autolysis is caused, the yield of the euphausia superba kernels is influenced, and the economic cost is high.
In the aspect of shelling antarctic krill, shelling devices are developed by domestic and foreign research institutions, for example, the antarctic krill shelling equipment disclosed by the invention patent CN201410674568.1 in China comprises a discharge device, a homogenizing device arranged at one end of the discharge device and a shelling device arranged at the other end of the discharge device.
The invention discloses a bionic-based material distribution device for euphausia superba shelling, which is disclosed by Chinese patent CN201710560120.0 and comprises a power source, a transmission mechanism, a conveyor belt and a scraper plate; the scraper is perpendicular to the rollers of the antarctic krill shelling equipment and is fixed on the conveyor belt, and the shape of the scraper is profiled with the space between the adjacent rollers; when the power source works, the lower belt body of the transmission belt moves backwards, the upper belt body moves forwards, the scraper is close to but not in contact with the roller when running to the lower belt body along with the transmission belt, and the scraper is separated from the roller when running to the upper belt body along with the transmission belt. The invention provides a material distributing device from the perspective of bionics, which realizes the function of automatically scraping and conveying shrimps accumulated on a roller backwards in a single direction; the scraper can freely swing below the conveyer belt in a hinged mode, and prawn can be scraped backwards by utilizing the gravity of the scraper.
The most basic principle of all existing shelling equipment is that shrimp shells or shrimp limbs of Antarctic krill are clamped through mechanical rotation, then shrimp meat is separated from the shells through extrusion, and the separation of the shrimp meat and the shrimp shells is realized through auxiliary water flow impact. In the process, tissue liquid between the shell and the kernel of the Antarctic krill enters water, visceral tissue and digestive juice in the shell of the head of the Antarctic krill are also brought into the water together, the digestive juice further hydrolyzes the meat of the Antarctic krill, and formed water-soluble components are further dissolved in the water, so that the process causes the reduction of the shelling yield of the Antarctic krill and the loss of a large amount of water-soluble protein components. There is also a loss of lipids that accompanies this process. Therefore, how to recover and utilize the part of the water-soluble component has great economic benefits.
The invention content is as follows:
the technical problems to be solved by the invention are that the existing antarctic krill shelling process causes the reduction of antarctic krill shelling yield, the loss of a large amount of water-soluble protein components and the loss of lipid accompanying the process. Therefore, how to recover and utilize the part of the water-soluble component has great economic benefits.
In order to solve the problems, the invention provides a method for preparing protein peptide by using the antarctic krill shelling wastewater, which is characterized in that the antarctic krill shelling wastewater is recovered and concentrated, and further deep processing is carried out to obtain the antarctic krill protein peptide, so that the effective utilization rate of the antarctic krill biological resources is improved.
In order to achieve the purpose, the invention is realized by the following technical scheme: a method for preparing protein peptide by using euphausia superba shelling wastewater comprises the following steps:
(1) recovering shelling waste water; the shelling wastewater is 1-15 parts by mass of washing water generated by 3 parts by mass of antarctic krill in the mechanical shelling process, and the source of the washing water is tap water or purified water;
(2) concentrating the recovered solution to obtain a concentrated solution;
(3) heating the concentrated solution to obtain thermal condensate and concentrated solution; by heating, the protein with large molecular weight is heated and denatured, the hydrophobic groups are exposed to form a thermopolymer, and solid matters in the liquid are primarily recovered while the thermopolymer is formed, so that the content of the solid matters in the liquid is reduced.
(4) Primary separation; separating the hot polymer and the concentrated solution to obtain a mixture of protein and lipid.
(5) Defluorination;
(6) secondary separation; the second separation is to add defluorinating agent into the concentrated solution to form floccule, and to separate the fluorine-containing component through centrifugal separation.
(7) Membrane separation; the membrane separation is to further carry out membrane separation on the defluorinated small molecular protein liquid, adopt membranes with different molecular weights, separate the small molecular proteins according to different molecular weights by using ultrafiltration and nanofiltration modes, and remove salt by nanofiltration.
(8) Spray drying to obtain a finished product;
furthermore, filtering and collecting rinsing water for shelling antarctic krill in the shelling wastewater recovery process in the step (1), and recycling the rinsing water for rinsing, wherein in the recycling rinsing process, the water temperature is less than or equal to 15 ℃ (the temperature is too high, so that the autolysis degree of the shrimps is improved, the solid loss is serious), and the solid content in the obtained shelling wastewater is 2-10%.
Further, the temperature is maintained at 30-70 ℃ in the concentration process of the recovery liquid in the step (2), and the solid content of the obtained concentrated liquid is 2-30%.
Further, the temperature of the concentrated solution in the step (3) is not less than 90 ℃ (the protein molecules in the concentrated solution can be subjected to thermal agglutination only when the temperature is higher than the temperature), and a rotary scraped surface heat exchanger is adopted for heating.
Further, the step (4) adopts a horizontal spiral centrifuge for separation, and the water content of the separated solid phase is less than or equal to 65 percent, which is a water content range when the separation degree of the horizontal spiral centrifuge is better when the biomass and the liquid are separated.
Further, defluorination in the step (5) is carried out by adopting defluorination resin or inorganic matters containing calcium ions, wherein the inorganic matters containing the calcium ions are one or more of calcium chloride, calcium hydroxide or calcium sulfate.
Further, step (6) adopts a centrifugal separation mode.
Further, the membrane separation in the step (7) comprises ceramic membrane filtration, ultrafiltration and nanofiltration. The ceramic membrane filtration, ultrafiltration and nanofiltration are sequentially carried out, and the functions of the ceramic membrane filtration, ultrafiltration and nanofiltration are respectively separating small particles which are not centrifuged down, intercepting macromolecules with the molecular weight of more than 3000-10000, and permeating sodium ions, chloride ions and the like with the molecular weight of less than 150-300.
Further, the temperature of the spray drying in the step (8) is 180-220 ℃ of inlet air temperature, and the outlet air temperature is less than or equal to 80 ℃.
The proteins in the processing solution are mainly water-soluble proteins, and are mostly derived from proteins such as actin, histone, and phosphate dehydrogenase. The processing method has a certain selection function on peptide segments in the protein, the pore diameter of the nanofiltration membrane is small, only substances below 150Da are allowed to pass through, the polypeptide in the processing stock solution can be well reserved, the ultrafiltration membrane has a good protein separation function, the polypeptide in a target molecular weight region can be reserved in a targeted manner, the pore diameter of the ultrafiltration membrane is large (the cut-off molecular weight is 3500Da), and part of the peptide with small molecular weight is lost in the ultrafiltration process.
The nutrition evaluation of amino acid shows that the protein source for human for a long time does not cause deletion of certain amino acid in view of the proportion of essential amino acid. The peptide powder has high nutrition evaluation in terms of the combination of EAAI and F value, and is a good protein supplement.
The invention has the beneficial effects that:
wastewater generated in the antarctic krill shelling process is recycled to obtain the antarctic krill protein peptide, so that the effective utilization rate of the antarctic krill biological resources is improved.
Drawings
FIG. 1 shows the variation of the composition of the respective product involved in the recovery process (dry basis).
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a method for preparing protein peptide by using euphausia superba shelling wastewater comprises the following steps:
(1) recovering shelling waste water; the shelling wastewater is 5 tons of flushing water produced by 3 tons of antarctic krill in the mechanical shelling process, and the source of the flushing water is tap water or purified water;
(2) concentrating the recovered solution to obtain a concentrated solution;
(3) heating the concentrated solution to obtain thermal condensate and enzymolysis solution;
(4) primary separation;
(5) defluorination;
(6) secondary separation;
(7) membrane separation;
(8) spray drying to obtain a finished product;
filtering and collecting rinsing water for shelling antarctic krill in the shelling wastewater recovery process in the step (1), and circularly using the rinsing water for rinsing, wherein the water temperature is less than or equal to 15 ℃ in the circular rinsing process, and the solid content in the obtained shelling wastewater is 2-10%.
And (3) in the concentration process of the recovered solution in the step (2), the temperature is maintained at 30-70 ℃, and the solid content of the obtained concentrated solution is 2-30%.
And (3) heating the concentrated solution in the step (3) at a temperature of more than or equal to 90 ℃, steaming at a high temperature for 10min, and heating by adopting a rotary scraped surface heat exchanger.
And (4) separating by adopting a horizontal spiral centrifuge, or roughly separating protein fat flocculent aggregates by using 100-mesh filter cloth, then separating suspended matters in the liquid by using a disc centrifuge 16000r/s, collecting precipitates after centrifugation, wherein the water content of the separated solid phase is less than or equal to 65%.
And (5) defluorinating by adopting defluorinating resin or inorganic matters containing calcium ions, wherein the inorganic matters containing the calcium ions are one or more of calcium chloride, calcium hydroxide or calcium sulfate.
And (6) adopting a centrifugal separation mode.
And (7) membrane separation comprises ceramic membrane filtration, ultrafiltration and nanofiltration. The ceramic membrane filtration, ultrafiltration and nanofiltration are sequentially carried out, and the functions of the ceramic membrane filtration, ultrafiltration and nanofiltration are respectively separating small particles which are not centrifuged down, intercepting macromolecules with the molecular weight of more than 3000-10000, and permeating sodium ions, chloride ions and the like with the molecular weight of less than 150-300.
The temperature of the spray drying in the step (8) is 180-220 ℃ of the inlet air temperature, and the outlet air temperature is less than or equal to 80 ℃.
The invention also improves the antarctic krill shucking machine, realizes the recycling of water resources in the shucking process, and carries out reprocessing on the shucking rinsing water to recover protein substances. Heating the rinsing liquid stock solution to 90 ℃, cooking at high temperature for 10min, roughly separating protein fat flocculent aggregates by using 100-mesh filter cloth, then separating suspended matters in the liquid by using a disc centrifuge 16000r/s, collecting precipitates after centrifugation, performing membrane concentration on the supernatant, and determining the operation conditions of the membrane concentration according to the previous experiment: the nanofiltration (150Da) temperature is 25 ℃, the operating pressure is 4.0MPa, and the concentration multiple is 10 times; the ultrafiltration (3500Da) temperature is 25 ℃, the operating pressure is 3.0MPa, and the concentration multiple is 12 times, so that the solid content of the two membrane concentrated trapped fluids is basically kept consistent. Selecting euphausia superba (YX), shelled shrimp meat (QK), shelled processing stock solution (YY), stewing centrifugal precipitation (CD), nanofiltration trapped fluid (NL), ultrafiltration trapped fluid (CL) to be freeze-dried to be tested and common euphausia superba peptide (LX), and analyzing the change of each component. As can be seen from the analysis of figure 1, the protein content of the shrimp meat is obviously increased after the shells are removed, and the total sugar content almost disappears along with the removal of the shrimp shells. The stock solution mainly contains protein substances (61.24g/100g), the protein substances are remarkably increased after heating, mainly because macromolecular protein and fat are flocculated and precipitated after heating, the fat content in the precipitate (CD) after centrifugal separation is up to 46.23g/100g, and the protein substances are effectively removed. The ultrafiltration nanofiltration membrane is concentrated into the concentration of protein in the feed liquid in one step, the change of the protein content in the concentration process of the two membranes is different, the molecular weight of a substance permeable by the nanofiltration membrane (NL) is extremely small, the supernatant component after cooking centrifugation is hardly influenced, the difference between the protein content and the processing liquid stock solution is not large (69.31g/100g), and the desalting effect is also realized in the process; the ultrafiltration membrane (CL) has larger membrane pore diameter and mainly plays a role in intercepting macromolecular proteins and polypeptides, so the protein content is higher (76.09g/100 g).
The NL concentrated solution has the fat content of 18.26 percent and is not greatly different from the YY of the processing solution, because the pore diameter of the nanofiltration membrane is small, organic matters such as protein, fat and the like can be well reserved, but desalination is performed, so that the ash content is greatly reduced, the protein is greatly improved, and the fat content is reduced but the degreasing effect is not obvious; the fat content of the CL concentrate is significantly reduced because the pore size of the membrane is large, only larger molecules can be retained, the protein retention rate is high, but other substances can permeate, the ash content is 13.46%, and the fat content is only 8.65%, so that the CL concentrate has higher protein content compared with NL. The results of later experiments also show that the membrane concentration also effectively reduces the content of fluorine and heavy metal elements.
In general, the Antarctic krill peptide extracted from the shelling liquid has a great recovery value.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, so that any person skilled in the art can change or modify the above technical content into an equivalent embodiment with equivalent changes. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (9)
1. A method for preparing protein peptide by using euphausia superba shelling wastewater is characterized by comprising the following steps:
(1) recovering shelling waste water;
(2) concentrating the recovered solution to obtain a concentrated solution;
(3) heating the concentrated solution to obtain thermal condensate and enzymolysis solution;
(4) primary separation;
(5) defluorination;
(6) secondary separation;
(7) membrane separation;
(8) spray drying to obtain the final product.
2. A method of producing a protein peptide according to claim 1, wherein: filtering and collecting rinsing water for shelling antarctic krill in the shelling wastewater recovery process in the step (1), and circularly using the rinsing water for rinsing, wherein the water temperature is less than or equal to 15 ℃ in the circular rinsing process, and the solid content in the obtained shelling wastewater is 2-10%.
3. A method of producing a protein peptide according to claim 1, wherein: and (3) in the concentration process of the recovered solution in the step (2), the temperature is maintained at 30-70 ℃, and the solid content of the obtained concentrated solution is 2-30%.
4. A method of producing a protein peptide according to claim 1, wherein: and (4) heating the concentrated solution in the step (3) at a temperature of more than or equal to 90 ℃, and heating by adopting a rotary scraped surface heat exchanger.
5. A method of producing a protein peptide according to claim 1, wherein: and (4) separating by adopting a horizontal spiral centrifuge, wherein the water content of the separated solid phase is less than or equal to 65 percent.
6. A method of producing a protein peptide according to claim 1, wherein: and (5) defluorinating by adopting defluorinating resin or inorganic matters containing calcium ions, wherein the inorganic matters containing the calcium ions are one or more of calcium chloride, calcium hydroxide or calcium sulfate.
7. A method of producing a protein peptide according to claim 1, wherein: and (6) adopting a centrifugal separation mode.
8. A method of producing a protein peptide according to claim 1, wherein: and (7) membrane separation comprises ceramic membrane filtration, ultrafiltration and nanofiltration.
9. A method of producing a protein peptide according to claim 1, wherein: the temperature of the spray drying in the step (8) is 180-220 ℃ of the inlet air temperature, and the outlet air temperature is less than or equal to 80 ℃.
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