Manufacturing method of krill oil

Abstract

The present invention relates to a method for manufacturing krill oil, and more specifically, to a method for manufacturing krill oil that is easy to encapsulate by removing impurities (proteins, salts, etc.) through a series of extraction and purification processes to lower the acid value, maximize the phospholipid content, and increase fluidity (lower viscosity).

Description

Technology Field

[0001] The present invention relates to a method for manufacturing krill oil, and more specifically, to a method for manufacturing krill oil that is easy to encapsulate by removing impurities (proteins, salts, etc.) through a series of extraction and purification processes to lower the acid value, maximize the phospholipid content, and increase fluidity (lower viscosity). Background Technology

[0002] Krill oil refers to oil extracted and refined from krill, and krill is a type of crustacean similar to shrimp that inhabits only the pristine waters of the Antarctic Ocean.

[0003] Although krill are sometimes called 'krill shrimp' because they resemble shrimp in appearance, they are crustaceans belonging to the order Euphoridae and are a type of plankton, so they are taxonomically unrelated to shrimp.

[0004] Krill oil is rich in omega-3 fatty acids EPA and DHA, which are known as essential nutrients that are necessary for bodily functions but cannot be synthesized in the body and must be obtained only through food.

[0005] In particular, DHA is an essential nutrient for the brain and nervous system, and a deficiency is reported to lead to degenerative diseases such as dementia and depression. Furthermore, krill oil contains astaxanthin, which has anti-inflammatory and antioxidant effects, and is known to help boost immunity, prevent heart disease, and protect eyesight.

[0006] Processes for extracting oil or active ingredients from krill include solvent extraction, fractionation, high concentration, enzymatic extraction, and supercritical extraction. Solvent extraction is a process that extracts oil components using organic solvents such as ethanol or acetone.

[0007] In addition to the basic extraction process, the krill oil manufacturing process is being researched and developed in combination with auxiliary processes, such as increasing the content of the active ingredient phospholipids or removing proteins or impurities.

[0008] Technical points requiring continuous development include high phospholipid content, low acid value, and low impurity content (protein, etc.); further research in these areas is required to enhance utilization in health functional foods and the like.

[0009] The matters described in the background technology above are intended to aid in understanding the background of the invention and may include matters that are not prior art already known to those skilled in the art to which this technology belongs. The problem to be solved

[0010] Accordingly, in order to solve the above-mentioned problems, the present invention aims to provide a method for manufacturing krill oil that is easy to encapsulate by removing impurities (proteins, salts, etc.) through a series of purification processes (salt treatment, liquid / liquid phase separation, ion exchange resin treatment, etc.) performed on extracted, filtered, and concentrated krill oil, thereby lowering the acid value, maximizing the phospholipid content, and increasing fluidity (lowering viscosity). means of solving the problem

[0011] The method for producing krill oil according to the present invention for achieving the above objectives may include processes of adding an acidic salt to a krill oil concentrate extracted, filtered, and concentrated from dried krill, stirring and filtering, then neutralizing it by treating it with a basic salt, and further concentrating and drying.

[0012] At this time, various types of acidic salts such as sodium citrate, sodium acetate, and phosphate can be used.

[0013] In addition, the method for producing krill oil according to the present invention may include processes for adding an aqueous organic solvent solution (such as an aqueous ethanol solution) to the krill oil concentrate after secondary concentration, stirring, and then allowing it to stand to obtain an organic solvent layer through liquid / liquid phase separation, followed by concentration and drying.

[0014] In addition, the method for producing krill oil according to the present invention may include processes such as adding an aqueous organic solvent solution to the krill oil concentrate after secondary concentration, stirring, and allowing it to stand to obtain an organic solvent layer through liquid / liquid phase separation, adding an ion exchange resin and stirring, and filtration, concentration, and drying.

[0015] At this time, the added ion exchange resin may be a mixed exchange resin in which a cation exchange resin and an anion exchange resin are mixed, and it is preferable that the mixing ratio of the cation exchange resin is high, and it is even more preferable that the mixing ratio of the cation exchange resin and the anion exchange resin is at the 2:1 level.

[0016] Meanwhile, the krill oil manufacturing method of the present invention may be a composite process in which two or more of the various embodiments described above are fused. Effects of the invention

[0017] The method for producing krill oil according to the present invention as described above has the effect of lowering the acid value and maximizing the phospholipid content by removing impurities (protein, salt, heavy metals, etc.).

[0018] In addition, as high molecular weight organic substances such as proteins and heavy metals are removed, viscosity is lowered, which increases fluidity. This facilitates post-processing steps for product manufacturing, such as encapsulation, and has the effect of improving yield. Specific details for implementing the invention

[0019] Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings to fully understand the present invention. Embodiments of the present invention may be modified in various forms, and the scope of the present invention should not be interpreted as being limited to the embodiments described in detail below. These embodiments are provided to more completely explain the present invention to those with average knowledge in the art. Accordingly, the shapes of elements in the drawings may be exaggerated to emphasize clearer explanations. It should be noted that in each drawing, identical components may be depicted with the same reference numerals. Detailed descriptions of known functions and configurations that are deemed to unnecessarily obscure the essence of the present invention are omitted.

[0021] The krill oil manufacturing method of the present invention basically comprises the following first process.

[0022] 1) Drying stage of krill raw material or preparation stage of dried krill;

[0023] 2) A step of extracting krill oil from dried krill using a solvent;

[0024] 3) A step of filtering the extracted krill oil to remove the krill meal;

[0025] 4) A step of concentrating the filtrate to prepare a primary concentrate;

[0026] 5) a step of preparing a secondary concentrate through additional concentration; and

[0027] 6) Step of drying the secondary concentrate.

[0029] At this time, the extraction step of step 2) above may use an organic solvent such as ethanol or alcohol, and it is preferable to control the temperature to 40 to 60°C. The extraction time is preferably 30 minutes to 2 hours, and it is preferable to ensure that stirring is performed during the extraction process.

[0030] The first concentration step of step 4) above is a process in which concentration is achieved to a level of approximately 50 to 80% compared to before concentration, and it is preferable to perform this under a vacuum of 0 to 10 torr and to control the temperature to 50 to 70℃.

[0031] It is preferable that the secondary concentration step of step 5) above be performed under a vacuum state of 0.2 to 1 torr.

[0032] The phospholipid content of the krill oil obtained through the first process described above is 30–38% by weight, the protein content is 15–20% by weight, and the acid value is 35–40.

[0034] The present invention includes a second process that performs the following process after step 4) of the first process as described above, that is, the first concentration step.

[0035] 4-10) Step of adding an acidic salt to the primary concentrate;

[0036] 4-11) A step of filtering the acid salt-treated primary concentrate;

[0037] 4-12) A step of neutralizing by treating with a basic salt;

[0038] 4-13) A step of filtering the primary concentrate treated with basic salt;

[0039] 5) a step of preparing a secondary concentrate through additional concentration; and

[0040] 6) Step of drying the secondary concentrate.

[0042] At this time, steps 4-10) to 4-13) are salt treatment steps, characterized by sequentially treating an acidic salt and a basic salt, and stirring and filtration in between.

[0043] The method may include the step of adding an acidic salt to a krill oil concentrate extracted, filtered, and concentrated from dried krill, stirring and filtering, then treating it with a basic salt to neutralize it, and then filtering.

[0044] At this time, the acidic salt used may be any one selected from sodium citrate, sodium acetate, and phosphate, or a mixture of two or more.

[0045] The phospholipid content of the krill oil obtained through the second process described above is 40–45% by weight, the protein content is 8–10% by weight, and the acid value is 26–29.

[0047] The present invention includes a third process that performs the following process after step 4) of the first process as described above, that is, the first concentration step.

[0048] 4-20) A step of further concentrating the primary concentrate to remove the solvent;

[0049] 4-21) A step of adding an aqueous organic solvent solution, stirring, and then letting it stand;

[0050] 4-22) A step of separating and obtaining an organic solvent layer when liquid / liquid phase separation occurs;

[0051] 5) a step of preparing a secondary concentrate through additional concentration; and

[0052] 6) Step of drying the secondary concentrate.

[0054] At this time, steps 4-20) to 4-22) are characterized by performing an additional purification / separation process by adding an aqueous organic solvent solution (such as an aqueous ethanol solution), stirring, and then allowing it to stand to obtain an organic solvent layer through liquid / liquid phase separation.

[0055] The additional concentration process in step 4-20) above is a process of further removing the solvent before adding an aqueous organic solvent solution to the primary concentrate, and it is recommended to concentrate it to about half the volume of the primary concentrate.

[0056] Various organic solvents, such as ethanol, can be used as the aqueous organic solvent added in step 4-21) above, and it is preferable that the mixing ratio of the organic solvent to water be 1:1 by volume.

[0057] The phospholipid content of the krill oil obtained through the above third process is 40–45% by weight, the protein content is 9–12% by weight, and the acid value is 23–26.

[0059] The present invention includes a fourth process that performs the following process after step 4) of the first process as described above, that is, the first concentration step.

[0060] 4-30) A step of further concentrating the primary concentrate to remove the solvent;

[0061] 4-31) A step of adding an aqueous organic solvent solution, stirring, and then letting it stand;

[0062] 4-32) A step of separating and obtaining an organic solvent layer when liquid / liquid phase separation occurs;

[0063] 4-33) A step of adding an ion exchange resin to the obtained organic solvent layer and stirring;

[0064] 4-34) A step of removing the added ion exchange resin by filtration;

[0065] 5) a step of preparing a secondary concentrate through additional concentration; and

[0066] 6) Step of drying the secondary concentrate.

[0068] At this time, steps 4-30) to 4-34) are characterized by adding an aqueous organic solvent solution (such as an aqueous ethanol solution), stirring, and then allowing it to stand to obtain an organic solvent layer through liquid / liquid phase separation, and then performing a complex purification / separation process by additionally treating the obtained organic solvent layer with an ion exchange resin.

[0069] Steps 4-30) to 4-32) above are performed in the same or similar manner as the third process described above.

[0070] The ion exchange resin added in step 4-33) above may be a mixed exchange resin in which a cation exchange resin and an anion exchange resin are mixed, and it is preferable that the mixing ratio of the cation exchange resin is higher than that of the anion exchange resin, and more preferably, the mixing ratio of the cation exchange resin and the anion exchange resin may be at the level of 2:1.

[0071] After adding the ion exchange resin in step 4-33) above, it is preferable to stir for 70 to 100 minutes to induce the removal of impurities in the organic solvent layer through the ion exchange reaction.

[0072] The phospholipid content of the krill oil obtained through the above fourth process is 43–47% by weight, the protein content is 7–10% by weight, and the acid value is 25–27.

[0073] Meanwhile, the krill oil manufacturing method of the present invention may be a composite process in which two or more of the first to fourth processes described above are performed in a fused form, either in series or in parallel.

[0075] [Example 1] First Process

[0076] 100g of dried krill was prepared, and 600ml of extract was obtained by stirring with 90% ethanol at a temperature of 50℃ for 1 hour. The obtained extract was filtered to remove the krill meal, and the remaining filtrate was concentrated at a temperature of 60℃ under vacuum conditions of 0 to 10 torr to obtain 100ml of primary concentrate.

[0077] The obtained primary concentrate was filtered and further concentrated to obtain a secondary concentrate, which was then vacuum dried under vacuum conditions of 0.2 to 1 torr to finally obtain the Example 1 product having a weight-based phospholipid content of 35%, a protein content of 15%, and an acid value of 37.

[0079] [Example 2] Second process

[0080] 1.5 g of sodium citrate was added to 100 ml of the primary concentrate obtained in the same manner as in Example 1, and the mixture was stirred for 30 minutes under conditions of 50°C. After filtration, 0.5 g of 1 M sodium hydroxide (NaOH) was added and stirred to neutralize the mixture. After further filtration, the mixture was concentrated a second time and vacuum dried to finally obtain the Example 2 product, which had a phospholipid content of 43% by weight, a protein content of 9.8%, and an acid value of 28.

[0082] [Example 3] Third process

[0083] 100 ml of the primary concentrate obtained in the same manner as in Example 1 was further concentrated to about half the volume, 50 ml, to remove the solvent, then 100 ml of an aqueous ethanol solution (ethanol:water = 1:1, volume ratio) was added and stirred, followed by standing. When liquid / liquid phase separation occurred and separated into an ethanol layer and a water layer, the ethanol layer was separated and obtained, then concentrated a second time and vacuum dried to finally obtain the Example 3 product, which has a weight-based phospholipid content of 42%, a protein content of 10.5%, and an acid value of 25.

[0085] [Example 4] 4th Process

[0086] After separating and obtaining the ethanol layer in the same manner as in Example 3 above, 3 to 5 g of a mixed exchange resin of cation and anion (cation exchange resin:anion exchange resin = 2:1, weight ratio) was added and stirred for 80 minutes.

[0087] After the ion exchange reaction was sufficiently carried out, the added ion exchange resin was removed by filtration, and after secondary concentration, vacuum drying was performed to finally obtain the product of Example 4, which had a phospholipid content of 44% by weight, a protein content of 9%, and an acid value of 26.

[0089] division Phospholipid content (wt%) Protein content (wt%) Sanga Example 1 35 15.4 37 Example 2 43 9.8 28 Example 3 42 10.5 25 Example 4 44 9 26

[0091] The embodiments of the method for manufacturing krill oil according to the present invention are merely preferred embodiments that enable a person skilled in the art with ordinary knowledge in the technical field to which the present invention belongs to easily implement the present invention, and are not limited to the aforementioned embodiments and attached drawings; therefore, the scope of the rights of the present invention is not limited by this.

[0092] Therefore, the true scope of technical protection of the present invention should be determined by the technical concept of the appended claims. Furthermore, it will be obvious to those skilled in the art that various substitutions, modifications, and changes are possible within the scope of the technical concept of the present invention, and it is self-evident that parts easily modifiable by those skilled in the art are also included within the scope of rights of the present invention.

Claims

Claim 1 A method for producing purified krill oil comprising: a step of extracting krill oil from dried krill using an aqueous ethanol solution; a step of concentrating the extracted krill oil to produce a krill oil concentrate; and a step of first adding an acidic salt to the krill oil concentrate and then sequentially adding a basic salt; wherein the step of adding the acidic salt is characterized by stirring at 50°C for 30 minutes, and the amount of the basic salt added is an amount capable of neutralizing the krill oil concentrate acidified by the acidic salt added first. Claim 2 A method for producing refined krill oil according to claim 1, wherein the acid salt is one selected from sodium citrate, sodium acetate, and phosphate, or a mixture of two or more. Claim 3 A method for producing purified krill oil according to claim 1, further comprising: a step of adding the acidic salt first and then adding the basic salt sequentially, followed by a step of further concentrating the salt-treated krill oil concentrate by reducing the pressure to a range of 0.2 to 1 torr; and a step of drying the further concentrated krill oil concentrate. Claim 4 delete Claim 5 A method for producing purified krill oil, comprising the steps of: extracting krill oil from dried krill using an aqueous ethanol solution; concentrating the extracted krill oil to produce a krill oil concentrate; adding an aqueous ethanol solution to the krill oil concentrate, stirring, and then allowing it to stand; separating and obtaining an ethanol layer when liquid / liquid phase separation occurs; and adding a mixed exchange resin, comprising a mixture of a cation exchange resin and an anion exchange resin, to the obtained ethanol layer as an ion exchange resin; wherein the mixing ratio of the cation exchange resin and the anion exchange resin is 2:1 by weight. Claim 6 A method for producing purified krill oil according to claim 5, characterized in that the organic solvent applied to the krill oil concentrate is an aqueous ethanol solution mixed with ethanol and water in a 1:1 volume ratio. Claim 7 A method for producing purified krill oil according to claim 5, further comprising the step of additionally concentrating the krill oil concentrate prior to the step of adding the ethanol aqueous solution, stirring, and then letting it stand. Claim 8 A method for producing purified krill oil according to claim 5, further comprising, after the step of separating and obtaining the ethanol layer, a step of further concentrating the obtained ethanol layer by reducing the pressure to a range of 0.2 to 1 torr; and a step of drying the further concentrated ethanol layer. Claim 9 delete Claim 10 delete Claim 11 delete

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