Phosphorus shrimp oil microcapsule powder, and preparation method and application thereof

Abstract

The application discloses phosphorus shrimp oil microcapsule powder and a preparation method and application thereof, and relates to the field of food technology. The preparation method comprises the following steps: S1, preparing a wall material into an aqueous solution, then adding phosphorus shrimp oil, stirring uniformly, and obtaining a phosphorus shrimp oil-wall material emulsion; S2, spray freezing: atomizing the phosphorus shrimp oil-wall material emulsion, and freezing the mist droplets in liquid nitrogen to form spherical ice crystals; S3, freeze drying: freeze drying the spherical ice crystals under the condition that the cold trap temperature is below-80 DEG C and the cavity heating temperature is 32-37 DEG C, and obtaining the phosphorus shrimp oil microcapsule powder. The preparation method is simple and efficient, can better retain heat-sensitive active ingredients, and improves the oxidation stability of the product, and has good application potential in the field of functional food.

Description

Technical Field

[0001] This invention relates to the field of food technology, specifically to a krill oil microcapsule powder, its preparation method, and its application. Background Technology

[0002] Krill oil is rich in phosphatidylcholine (PC), phosphatidylethanolamine (PE), Omega-3 polyunsaturated fatty acids, astaxanthin, and other bioactive components, possessing significant nutritional and health benefits. To broaden the application of krill oil in various common foods and dietary supplements such as solid beverages, milk powder, and tablets, industrially it is often prepared into microencapsulated powders that are easy to store, transport, and reconstitute. Currently, spray drying has become the mainstream technology for preparing such microencapsulated powders due to its simplicity, low cost, and suitability for continuous large-scale production.

[0003] However, the core functional components of krill oil (including phosphatidylcholine and phosphatidylethanolamine) are extremely sensitive to high temperatures and oxygen. Traditional spray drying processes typically require temperatures between 150°C and 200°C, which can easily lead to thermal degradation and oxidation of these heat-sensitive active ingredients. This not only results in a loss of nutritional value but also severely affects the flavor, quality stability, and shelf life of the final product.

[0004] Therefore, there is an urgent need to develop a microencapsulation preparation technology that can retain the heat-sensitive active ingredients in krill oil to the maximum extent. Summary of the Invention

[0005] To address the problems existing in the prior art, the present invention aims to provide a krill oil microcapsule powder, its preparation method, and its application. The preparation method of the krill oil microcapsule powder of the present invention is simple, can effectively avoid the damage of active ingredients to high temperatures, and is beneficial to protecting the structural and functional integrity of heat-sensitive components such as PC and PE in krill oil, thus having good application prospects.

[0006] This invention provides the following technical solution: This invention provides a method for preparing krill oil microcapsule powder using spray freeze-drying, comprising the following steps: S1. Prepare the wall material into an aqueous solution with a mass concentration of 10%~50%, then add 5%~50% krill oil by mass of the wall material, stir evenly, and obtain a krill oil-wall material emulsion. S2. Spray freezing: After atomizing the krill oil-wall material emulsion, the droplets are frozen in liquid nitrogen to form spherical ice crystals; S3. Freeze-drying: The spherical ice crystals are freeze-dried at a cold trap temperature below -80°C and a cavity heating temperature of 32~37°C to obtain krill oil microcapsule powder.

[0007] Furthermore, the wall material is octenyl succinic acid starch (OSA-starch).

[0008] Further, in step S1, the mixing is specifically performed by: high-speed shearing dispersion at a speed of 8000-15000 rpm for 2-10 minutes at room temperature.

[0009] Preferably, in step S2, the atomization is achieved by a spraying device having a nozzle with a diameter of 1.0 mm and / or 2.0 mm.

[0010] Preferably, in step S2, the flow rate of the krill oil-wall material emulsion atomization is 10~65 mL / min.

[0011] Preferably, in step S2, the pressure of atomizing the krill oil-wall material emulsion is 0.05-0.25 MPa.

[0012] The atomization flow rate is controlled by the pressure.

[0013] Preferably, in step S2, the volume ratio of liquid nitrogen to krill oil-wall material emulsion is (5-20):1.

[0014] Preferably, the freeze-drying is carried out under vacuum conditions, and the freeze-drying time is 3 to 12 hours.

[0015] Secondly, the present invention also discloses a krill oil microcapsule powder, which is prepared by the above-mentioned method for preparing krill oil microcapsule powder.

[0016] Thirdly, the present invention also discloses the application of the above-mentioned krill oil microcapsule powder in the food field.

[0017] Through the above design, the present invention has the following effects: This invention effectively avoids the damage to heat-sensitive components caused by high temperatures by freezing the atomized droplets of krill oil-wall material emulsion and then sublimating and drying them under vacuum conditions. This better preserves the functional properties and oxidative stability of krill oil. Throughout the process, the temperature is consistently controlled below 37°C, effectively preventing damage to active ingredients and protecting the structural and functional integrity of heat-sensitive components such as PC and PE in the krill oil. This method shows promising application prospects. Attached Figure Description

[0018] To more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the following description of the embodiments will be briefly introduced. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0019] Figure 1 This is a schematic diagram showing the comparison of phospholipid retention rates provided by the present invention. Detailed Implementation

[0020] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0021] It should be understood that, when used in this specification and the appended claims, the terms “comprising” and “including” indicate the presence of the described features, integrals, steps, operations, elements and / or components, but do not exclude the presence or addition of one or more other features, integrals, steps, operations, elements, components and / or collections thereof.

[0022] It should also be understood that the terminology used in this specification is for the purpose of describing particular embodiments only and is not intended to limit the invention. As used in this specification and the appended claims, the singular forms “a,” “an,” and “the” are intended to include the plural forms unless the context clearly indicates otherwise.

[0023] Example 1 A method for preparing krill oil microcapsule powder includes the following steps: S1. Prepare an aqueous solution of octenyl succinic acid starch with a mass concentration of 25%, then add krill oil accounting for 25% of the mass of octenyl succinic acid starch, and disperse it at room temperature (25℃) by high-speed shearing at 12000 rpm for 5 minutes to make it uniform, and obtain krill oil-wall material emulsion. S2. Spray freezing: A spray device is used to control the spray pressure at 0.10 MPa. The krill oil-wall material emulsion is atomized through a nozzle with a diameter of 1.0 mm at a flow rate of 30 mL / min and sprayed into a cavity containing liquid nitrogen, so that the droplets freeze rapidly to form tiny spherical ice crystals; wherein, the volume ratio of liquid nitrogen to krill oil-wall material emulsion is 10:1. S3. Freeze-drying: Start the vacuum and freeze-dry the spherical ice crystals for 8 hours at a cold trap temperature of -80℃ and a cavity heating temperature of 35℃ to obtain krill oil microcapsule powder.

[0024] Example 2 A method for preparing krill oil microcapsule powder includes the following steps: S1. Prepare an aqueous solution of octenyl succinic acid starch with a mass concentration of 10%, then add 5% krill oil (by mass of octenyl succinic acid starch), and disperse it at room temperature (25°C) by high-speed shearing at 8000 rpm for 10 minutes to make it uniform, thus obtaining a krill oil-wall material emulsion. S2. Spray freezing: A spray device is used to control the spray pressure at 0.05 MPa. The krill oil-wall material emulsion is atomized through a nozzle with a diameter of 1.0 mm at a flow rate of 10 mL / min and sprayed into a cavity containing liquid nitrogen, so that the droplets freeze rapidly to form tiny spherical ice crystals; wherein, the volume ratio of liquid nitrogen to krill oil-wall material emulsion is 5:1. S3. Freeze-drying: Start the vacuum and freeze-dry the spherical ice crystals for 12 hours at a cold trap temperature of -90℃ and a cavity heating temperature of 37℃ to obtain krill oil microcapsule powder.

[0025] Example 3 A method for preparing krill oil microcapsule powder includes the following steps: S1. Prepare an aqueous solution of octenyl succinic acid starch with a mass concentration of 30%, then add krill oil accounting for 50% of the mass of octenyl succinic acid starch, and disperse it at room temperature (25℃) by high-speed shearing at 10000 rpm for 8 minutes to make it uniform, and obtain krill oil-wall material emulsion. S2. Spray freezing: A spray device is used to control the spray pressure at 0.08 MPa. The krill oil-wall material emulsion is atomized through a nozzle with a diameter of 1.0 mm at a flow rate of 25 mL / min and sprayed into a cavity containing liquid nitrogen, so that the droplets freeze rapidly to form tiny spherical ice crystals; wherein, the volume ratio of liquid nitrogen to krill oil-wall material emulsion is 15:1. S3. Freeze-drying: Start the vacuum and freeze-dry the spherical ice crystals for 5 hours at a cold trap temperature of -85℃ and a cavity heating temperature of 33℃ to obtain krill oil microcapsule powder.

[0026] Example 4 A method for preparing krill oil microcapsule powder includes the following steps: S1. Prepare an aqueous solution of octenyl succinic acid starch with a mass concentration of 50%, then add krill oil accounting for 35% of the mass of octenyl succinic acid starch, and disperse it at room temperature (25℃) by high-speed shearing at 15000 rpm for 2 minutes to make it uniform, and obtain krill oil-wall material emulsion. S2. Spray freezing: A spray device is used to control the spray pressure at 0.25 MPa. The krill oil-wall material emulsion is atomized through a nozzle with a diameter of 2.0 mm at a flow rate of 65 mL / min and sprayed into a cavity containing liquid nitrogen, so that the droplets freeze rapidly to form tiny spherical ice crystals; wherein, the volume ratio of liquid nitrogen to krill oil-wall material emulsion is 20:1. S3. Freeze-drying: Start the vacuum and freeze-dry the spherical ice crystals for 3 hours at a cold trap temperature of -90℃ and a cavity heating temperature of 37℃ to obtain krill oil microcapsule powder.

[0027] Comparative Example 1 A method for preparing krill oil microcapsule powder using a traditional spray drying process includes the following steps: S1. Prepare an aqueous solution of octenyl succinic acid starch with a mass concentration of 25%, then add krill oil accounting for 25% of the mass of octenyl succinic acid starch, and disperse it at room temperature (25℃) by high-speed shearing at 12000 rpm for 5 minutes to make it uniform, and obtain krill oil-wall material emulsion. S2. Spray drying: A centrifugal spray dryer is used for drying, with the following control parameters: inlet air temperature 180℃, outlet air temperature 85℃, feed flow rate 30 mL / min, and atomizer speed 20000 r / min; the powder at the bottom of the drying tower is collected to obtain spray-dried krill oil microcapsule powder.

[0028] Comparative Example 2 A method for preparing krill oil microcapsule powder using a traditional freeze-drying process includes the following steps: S1. Prepare an aqueous solution of octenyl succinic acid starch with a mass concentration of 25%, then add krill oil accounting for 25% of the mass of octenyl succinic acid starch, and disperse it at room temperature (25℃) by high-speed shearing at 12000 rpm for 5 minutes to make it uniform, and obtain krill oil-wall material emulsion. S2. Spread the krill oil-wall material emulsion evenly in a freeze-drying tray and pre-freeze it in a -40℃ freezer for 12 hours to form a solid ice layer.

[0029] S3. Transfer the pre-frozen sample to a freeze dryer. Drying conditions: cold trap temperature -80℃, chamber pressure 10Pa, chamber partition heating temperature 35℃, drying time 36 hours.

[0030] S4. The dried block product is mechanically pulverized (ball milling, 300 rpm, 5 minutes) and passed through a 100-mesh sieve to obtain traditional freeze-dried krill oil microcapsule powder.

[0031] Comparative Example 3 A method for preparing krill oil microcapsule powder includes the following steps: S1. Prepare an aqueous solution of octenyl succinic acid starch with a mass concentration of 25%, then add krill oil accounting for 25% of the mass of octenyl succinic acid starch, and disperse it at room temperature (25℃) by high-speed shearing at 12000 rpm for 5 minutes to make it uniform, and obtain krill oil-wall material emulsion. S2. Spray freezing: A spray device is used to control the spray pressure at 0.10 MPa. The krill oil-wall material emulsion is atomized through a nozzle with a diameter of 1.0 mm at a flow rate of 30 mL / min and sprayed into a cavity containing liquid nitrogen, so that the droplets freeze rapidly to form tiny spherical ice crystals; wherein, the volume ratio of liquid nitrogen to krill oil-wall material emulsion is 10:1. S3. Freeze-drying: Start the vacuum and freeze-dry the spherical ice crystals for 8 hours at a cold trap temperature of -80℃ and a cavity heating temperature of 55℃ to obtain krill oil microcapsule powder.

[0032] Comparative Example 4 A method for preparing krill oil microcapsule powder includes the following steps: S1. Prepare an aqueous solution of octenyl succinic acid starch with a mass concentration of 25%, then add krill oil accounting for 25% of the mass of octenyl succinic acid starch, and disperse it at room temperature (25℃) by high-speed shearing at 12000 rpm for 5 minutes to make it uniform, and obtain krill oil-wall material emulsion. S2. Spray freezing: A spray device is used to control the spray pressure at 0.10 MPa. The krill oil-wall material emulsion is atomized through a nozzle with a diameter of 1.0 mm at a flow rate of 30 mL / min and sprayed into a cavity containing liquid nitrogen, so that the droplets freeze rapidly to form tiny spherical ice crystals; wherein, the volume ratio of liquid nitrogen to krill oil-wall material emulsion is 10:1. S3. Freeze-drying: Start the vacuum and freeze-dry the spherical ice crystals for 8 hours at a cold trap temperature of -70℃ and a cavity heating temperature of 55℃ to obtain krill oil microcapsule powder.

[0033] To verify the technical effect of the present invention, the phospholipid retention rate of the krill oil microcapsule powder prepared in the above embodiments and comparative examples was tested. The test results are shown in Table 1 below. Figure 1 As shown: Table 1. Test results of phospholipid retention rate of krill oil microcapsule powder in the examples and comparative examples. As shown in Table 1 and Figure 1As shown, the embodiments of the present invention have a short process cycle, and the phospholipid retention rate of the prepared krill oil microcapsule powder is significantly higher than that of the comparative examples, with the phospholipid retention rate of the product in Example 1 reaching as high as 87.1%. In contrast, Comparative Example 1 uses a traditional spray drying process to prepare krill oil microcapsule powder. Although the drying time is short and the drying efficiency is higher, the drying temperature (180°C) is high, leading to phospholipid oxidation and decomposition. Comparative Example 2 uses a traditional freeze-drying process to prepare krill oil microcapsule powder. Although its phospholipid retention rate is high, its process cycle is too long, and there is still a risk of phospholipid oxidation during the long-term drying process. At the same time, traditional drying requires mechanical pulverization, which may damage the microcapsule structure and cause some phospholipid exposure and loss. Comparative Examples 3 and 4 use the same spray-freeze process as Example 1, but the drying chamber is heated to an excessively high temperature, resulting in thermal damage to the phospholipids and a significant reduction in the phospholipid retention rate. In particular, Comparative Example 4, due to insufficient cold trap temperature, further aggravates phospholipid oxidation. Therefore, this invention achieves efficient microencapsulation of krill oil under low-temperature conditions throughout the entire process through spray freeze-drying technology. This avoids the high-temperature heat damage of traditional spray drying and overcomes the defects of traditional freeze-drying, such as long cycle and loss of phospholipids due to pulverization.

[0034] In summary, the preparation process of this invention can efficiently prepare krill oil microcapsule powder while better preserving its heat-sensitive active ingredients and improving the oxidative stability of the product, thus showing good application potential in the field of functional foods.

[0035] The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any person skilled in the art can easily conceive of various equivalent modifications or substitutions within the technical scope disclosed in the present invention, and these modifications or substitutions should all be covered within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. A method for preparing krill oil microcapsule powder, characterized in that, Includes the following steps: S1. Prepare the wall material into an aqueous solution with a mass concentration of 10%~50%, then add 5%~50% krill oil by mass of the wall material, stir evenly, and obtain a krill oil-wall material emulsion. S2. Spray freezing: After atomizing the krill oil-wall material emulsion, the droplets are frozen in liquid nitrogen to form spherical ice crystals; S3. Freeze-drying: The spherical ice crystals are freeze-dried at a cold trap temperature below -80°C and a cavity heating temperature of 32~37°C to obtain krill oil microcapsule powder.

2. The method for preparing krill oil microcapsule powder as described in claim 1, characterized in that, The wall material is octenyl succinic starch.

3. The method for preparing krill oil microcapsule powder as described in claim 1, characterized in that, In step S1, the mixing process specifically involves: high-speed shearing dispersion at a speed of 8000-15000 rpm for 2-10 minutes at room temperature.

4. The method for preparing krill oil microcapsule powder as described in claim 1, characterized in that, In step S2, the atomization is achieved by a spraying device having a nozzle with a diameter of 1.0 mm and / or 2.0 mm.

5. The method for preparing krill oil microcapsule powder as described in claim 1, characterized in that, In step S2, the flow rate of the krill oil-wall material emulsion atomization is 10~65 mL / min.

6. The method for preparing krill oil microcapsule powder as described in claim 1, characterized in that, In step S2, the pressure for atomizing the krill oil-wall material emulsion is 0.05-0.25 MPa.

7. The method for preparing krill oil microcapsule powder as described in claim 1, characterized in that, In step S2, the volume ratio of liquid nitrogen to krill oil-wall material emulsion is (5-20):

1.

8. The method for preparing krill oil microcapsule powder as described in claim 1, characterized in that, The freeze-drying is carried out under vacuum conditions for 3 to 12 hours.

9. A krill oil microcapsule powder, characterized in that, It is prepared by the method for preparing krill oil microcapsule powder according to any one of claims 1-8.

10. The application of the krill oil microcapsule powder as described in claim 9 in the food industry.

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