Composite vegetable oil microcapsule powder and preparation method thereof

Abstract

The invention relates to composite vegetable oil microcapsule powder and a preparation method thereof, and belongs to the technical field of biology. The composite vegetable oil microcapsule powder provided by the invention is prepared from an oil phase, a water phase and auxiliary materials. The preparation method comprises the following steps: preparing an oil phase and a water phase, emulsifying, homogenizing, drying and mixing to obtain the composite vegetable oil microcapsule powder. By optimizing emulsification parameters, an oil phase and a water phase are fully mixed to obtain a more stable emulsion, so that grease is better embedded in a wall material, and the microencapsulation effect is improved; a spray drying technology is adopted, and parameters are reasonably set, so that the drying efficiency is improved, and grease oxidation and wall material deformation are avoided; by reasonably setting mixing parameters, the components are uniformly mixed, so that the stability of the product is ensured, and the quality of the product is improved; the process provided by the invention improves the stability and encapsulation efficiency of the product, prolongs the shelf life of the product, and has better market competitiveness.

Description

Technical Field

[0001] The present invention belongs to the field of biotechnology, and particularly relates to a compound vegetable oil microcapsule powder and a preparation method thereof. Background Art

[0002] Microcapsule powder is a powdery substance formed by encapsulating solid, liquid or gaseous substances with high-quality wall materials using microencapsulation technology. It can improve the stability of products, prevent mutual interference between various components, and is more easily absorbed and utilized by the human body, being favored by consumers. Compound vegetable oil microcapsule powder is a product prepared by combining multiple vegetable oils with wall materials through microencapsulation technology, having good stability and wide application. However, when preparing microcapsule powder by existing production processes, the emulsification effect is often unstable, the drying efficiency is low, and the mixing is uneven, resulting in low encapsulation rate, unstable products, short shelf life, too large particle size, and poor absorption and utilization effect by the human body, seriously affecting the quality and performance of the products. Therefore, an improved production process is urgently needed to improve the production efficiency and product quality of compound vegetable oil microcapsule powder. Summary of the Invention

[0003] In view of this, the purpose of the present invention is to provide a compound vegetable oil microcapsule powder and a preparation method thereof, to prepare a product with high encapsulation rate and stable storage, and at the same time improve the production efficiency of the product.

[0004] The present invention provides a compound vegetable oil microcapsule powder, which is prepared from an oil phase, an aqueous phase and auxiliary materials;

[0005] The oil phase comprises raw materials in the following weight parts: 12 - 18 parts of coconut oil, 8 - 12 parts of linseed oil, and 6 - 12 parts of safflower oil;

[0006] The aqueous phase comprises raw materials in the following weight parts: 15 - 22 parts of resistant dextrin, 8 - 14 parts of maltitol, 8 - 12 parts of casein, and 6 - 10 parts of isomaltooligosaccharide;

[0007] The auxiliary materials comprise raw materials in the following weight parts: 1 - 2 parts of emulsifier, 2 - 4 parts of microcapsule wall material, 0.5 - 1.5 parts of antioxidant, and 1 - 2 parts of glidant.

[0008] Preferably, the coconut oil, linseed oil and safflower oil are refined coconut oil, linseed oil and safflower oil;

[0009] The refining includes steps of degumming, deacidification, decolorization and deodorization.

[0010] Preferably, the emulsifier includes monoglyceride and diglyceride fatty acid esters, lecithin or gum arabic.

[0011] Preferably, the microcapsule wall material includes sodium octenyl succinate starch, maltodextrin or chitosan.

[0012] Preferably, the antioxidant includes sodium ascorbate and / or potassium citrate.

[0013] Preferably, the glidant includes silicon dioxide.

[0014] The present invention also provides a method for preparing the composite vegetable oil microcapsule powder, comprising the following steps:

[0015] Mix coconut oil, linseed oil and safflower oil to obtain an oil phase; mix resistant dextrin, maltitol oligosaccharide, casein and isomaltooligosaccharide, add water, and stir until completely dissolved to obtain an aqueous phase; add the oil phase to the aqueous phase, and perform shear emulsification at 50°C to 60°C, with a shear speed of 8000 rpm to 12000 rpm and an emulsification time of 10 minutes to 15 minutes to form a primary emulsion; homogenize the primary emulsion to obtain microcapsule emulsion 1; mix microcapsule emulsion 1 with an emulsifier and a microcapsule wall material to obtain microcapsule emulsion 2; perform spray drying on microcapsule emulsion 2 to obtain microcapsule powder; the inlet air temperature of the spray drying is 150°C to 180°C, and the outlet air temperature is 80°C to 90°C; mix the microcapsule powder with an antioxidant and a glidant to obtain the composite vegetable oil microcapsule powder.

[0016] Preferably, the particle sizes of the resistant dextrin, maltitol oligosaccharide, casein and isomaltooligosaccharide are 40 to 80 mesh; the particle sizes of the emulsifier, antioxidant, microcapsule wall material and glidant are 80 to 120 mesh.

[0017] Preferably, the pressure of the homogenization is 30 MPa to 50 MPa, and the number of times is 3 to 5 times.

[0018] Preferably, the mixing speed of the microcapsule powder with the antioxidant and the glidant is 500 rpm to 800 rpm, and the time is 15 minutes to 30 minutes.

[0019] Advantages of the present invention:

[0020] The composite vegetable oil microcapsule powder provided by the present invention has the advantages of high encapsulation rate and storage stability. By optimizing the emulsification parameters, the present invention enables the oil phase and the aqueous phase to be fully mixed, obtains a more stable emulsion, better embeds the oil in the wall material, and improves the microencapsulation effect; by adopting the spray drying technology and reasonably setting its parameters, the drying efficiency is improved and the oxidation of the oil and the deformation of the wall material are avoided; by reasonably setting the mixing parameters, the components are uniformly mixed, the stability of the product is ensured, and the product quality is improved; through the overall process of the present invention, the stability and encapsulation rate of the product are improved, the shelf life of the product is extended, and it has better market competitiveness. Description of the Drawings

[0021] Figure 1Results of the determination of the particle size and Zeta potential of the composite vegetable oil microcapsule powder; among them, A is the result of particle size determination; B is the result of Zeta potential determination.

[0022] Figure 2 Scanning electron microscope images of the composite vegetable oil microcapsule powder at different magnifications; among them, A is the scanning electron microscope image at 400×, B is the scanning electron microscope image at 1000×, and C is the scanning electron microscope image at 4000×.

[0023] Figure 3 TGA curve of the thermogravimetric analysis of the composite vegetable oil microcapsule powder.

[0024] Figure 4 Fourier transform infrared spectroscopy analysis diagram of the composite vegetable oil microcapsule powder.

[0025] Figure 5 X-ray diffraction pattern of the composite vegetable oil microcapsule powder. Detailed implementation methods

[0026] The present invention provides a composite vegetable oil microcapsule powder, which is prepared from an oil phase, an aqueous phase and excipients;

[0027] The oil phase includes the following raw materials in parts by weight: 12-18 parts of coconut oil, 8-12 parts of linseed oil, and 6-12 parts of safflower oil; preferably: 14-16 parts of coconut oil, 9-11 parts of linseed oil, and 7-11 parts of safflower oil; more preferably: 15 parts of coconut oil, 10 parts of linseed oil, and 8 parts of safflower oil;

[0028] The aqueous phase includes the following raw materials in parts by weight: 15-22 parts of resistant dextrin, 8-14 parts of maltodextrin, 8-12 parts of casein, and 6-10 parts of isomaltooligosaccharide; preferably: 18-21 parts of resistant dextrin, 10-13 parts of maltodextrin, 9-11 parts of casein, and 7-9 parts of isomaltooligosaccharide; more preferably: 20 parts of resistant dextrin, 12 parts of maltodextrin, 10 parts of casein, and 8 parts of isomaltooligosaccharide;

[0029] The excipients include the following raw materials in parts by weight: 1-2 parts of emulsifier, 2-4 parts of microcapsule wall material, 0.5-1.5 parts of antioxidant, and 1-2 parts of glidant; preferably: 1.2-1.8 parts of emulsifier, 2.5-3.5 parts of microcapsule wall material, 0.8-1.2 parts of antioxidant, and 1.2-1.8 parts of glidant; more preferably: 1.5 parts of emulsifier, 3 parts of microcapsule wall material, 1 part of antioxidant, and 1.5 parts of glidant.

[0030] The present invention has no special limitation on the sources of the oil phase, the aqueous phase and the excipients, and conventional commercially available products in the art can be used.

[0031] In the present invention, the oil-phase raw materials, namely coconut oil, linseed oil and safflower oil, are preferably refined coconut oil, linseed oil and safflower oil. In the present invention, the refining preferably includes steps of degumming, deacidification, decolorization and deodorization. The present invention has no special limitation on the methods of degumming, deacidification, decolorization and deodorization, and the conventional degumming, deacidification, decolorization and deodorization methods in the art can be used for treatment. In one embodiment, the method of degumming can be: heating coconut oil, linseed oil and safflower oil at 60°C to 80°C (such as 60°C, 70°C or 80°C), adding 0.1% to 0.3% (such as 0.1%, 0.2% or 0.3%) of phosphoric acid or citric acid, stirring for 10 minutes to 15 minutes (such as 10 minutes, 12.5 minutes, 14 minutes or 15 minutes) to hydrolyze the colloidal substances, and then removing the colloids. The present invention has no special limitation on the way of removing the colloids, and the colloids can be removed by means of static sedimentation or centrifugation to obtain the degummed oil. In one embodiment, the method of deacidification can be: adding 0.1% to 0.3% (such as 0.1%, 0.2% or 0.3%) of sodium hydroxide or sodium carbonate, stirring for 10 minutes to 15 minutes (such as 10 minutes, 12.5 minutes, 14 minutes or 15 minutes) to neutralize the free fatty acids to form soapstock, and then removing the soapstock. The present invention has no special limitation on the way of removing the soapstock, and the soapstock can be removed by means of static sedimentation or centrifugation to obtain the deacidified oil. In one embodiment, the method of decolorization can be: adding 0.5% to 1.0% (such as 0.5%, 0.75%, 0.9% or 1.0%) of activated carbon or clay, stirring for 20 minutes to 30 minutes (such as 20 minutes, 25 minutes or 30 minutes) to adsorb the pigments and odor substances in the oil, and then removing the adsorbent. The present invention has no special limitation on the way of removing the adsorbent, and the adsorbent can be removed by filtration to obtain the decolorized oil. In one embodiment, the method of deodorization can be: carrying out vacuum distillation at 180°C to 200°C (such as 180°C, 190°C or 200°C), with a vacuum degree of 0.1 MPa to 0.3 MPa (such as 0.1 MPa, 0.2 MPa or 0.3 MPa) and a time of 20 to 40 minutes (such as 20 minutes, 25 minutes, 30 minutes, 35 minutes or 40 minutes) to remove the odor substances in the oil and obtain refined coconut oil, linseed oil and safflower oil.

[0032] In the present invention, the emulsifier preferably includes mono- and diglycerol fatty acid esters, lecithin or gum arabic. The microcapsule wall material preferably includes sodium octenyl succinate starch, maltodextrin or chitosan. The antioxidant preferably includes sodium ascorbate and / or potassium citrate. When the antioxidant is sodium ascorbate and potassium citrate, the mass ratio of sodium ascorbate to potassium citrate is preferably (0.25 to 0.75):(0.25 to 0.75), more preferably (0.45 to 0.55):(0.45 to 0.55), and further preferably 0.5:0.5. The glidant preferably includes silicon dioxide.

[0033] The present invention also provides a method for preparing the composite vegetable oil microcapsule powder, comprising the following steps:

[0034] Preparation of the oil phase: Mix coconut oil, linseed oil and safflower oil to obtain the oil phase; the mixing method is preferably stirring and mixing after heating, and the heating is preferably heating to 50°C to 60°C. In one embodiment, 50°C, 52°C, 55°C, 58°C or 60°C can be selected; the stirring speed is preferably 500 rpm to 800 rpm. In one embodiment, 500 rpm, 600 rpm, 650 rpm, 700 rpm or 800 rpm can be selected; the stirring time is 10 to 15 minutes. In one embodiment, 10 minutes, 11 minutes, 12.5 minutes or 15 minutes can be selected.

[0035] Preparation of the water phase: Mix resistant dextrin, maltitol oligosaccharide, casein and isomaltooligosaccharide, add to water, and stir until completely dissolved to obtain the water phase; the stirring is preferably stirring after heating, and the heating is preferably heating to 60°C to 70°C. In one embodiment, 60°C, 62°C, 65°C, 68°C or 70°C can be selected; the stirring speed is preferably 1000 rpm to 1500 rpm. In one embodiment, 1000 rpm, 1200 rpm, 1250 rpm, 1400 rpm or 1500 rpm can be selected; the stirring time is preferably 30 to 45 minutes. In one embodiment, 30 minutes, 37.5 minutes, 40 minutes or 45 minutes can be selected.

[0036] Primary emulsification: Add the oil phase to the water phase, and perform shear emulsification at 50°C to 60°C, with a shear speed of 8000 rpm to 12000 rpm and an emulsification time of 10 minutes to 15 minutes to form a primary emulsion; when adding the oil phase to the water phase, it is preferably added slowly; the temperature of the shear emulsification is preferably 50°C, 52°C, 55°C, 58°C or 60°C; the shear speed is preferably 8000 rpm, 9000 rpm, 10000 rpm, 11000 rpm or 12000 rpm; the emulsification time is preferably 10 minutes, 11 minutes, 12.5 minutes or 15 minutes.

[0037] Homogenization: Homogenize the primary emulsion to obtain microcapsule emulsion 1; the pressure of the homogenization is preferably 30 MPa to 50 MPa, and in one embodiment, 30 MPa, 35 MPa, 40 MPa, 45 MPa or 50 MPa can be selected. The number of times of homogenization is preferably 3 to 5 times, and in one embodiment, 3 times, 4 times or 5 times can be selected to ensure the stability of the emulsion and obtain uniform microcapsule emulsion 1.

[0038] Add emulsifier and microcapsule wall material: Mix microcapsule emulsion 1 with an emulsifier and a microcapsule wall material to obtain microcapsule emulsion 2; the mixing is stirring mixing, and the rotation speed of the stirring is preferably 500 rpm to 800 rpm. In one embodiment, 500 rpm, 600 rpm, 650 rpm, 700 rpm or 800 rpm can be selected; the stirring time is 10 to 15 minutes, and in one embodiment, 10 minutes, 12.5 minutes, 14 minutes or 15 minutes can be selected to further improve the stability of the emulsion and the microencapsulation effect.

[0039] Drying: Spray-dry microcapsule emulsion 2 to obtain microcapsule powder; the inlet air temperature of the spray drying is 150 °C to 180 °C, preferably 150 °C, 160 °C, 165 °C, 170 °C or 180 °C; the outlet air temperature is 80 °C to 90 °C, preferably 80 °C, 83 °C, 85 °C, 88 °C or 90 °C. The atomization pressure is preferably 25 to 30 MPa, and in one embodiment, 25 MPa, 26 MPa, 28 MPa or 30 MPa can be selected; after the spray drying, it is preferred to collect the dried microcapsule powder. For the microcapsule powder that cannot be completely collected, it is preferred to use a bag filter for further collection to ensure the purity and yield of the product. After detection, the loss rate of the microcapsule powder after spray drying is 5% to 8%.

[0040] Mixing: Mix the microcapsule powder obtained by spray drying with an antioxidant and a glidant; the mixing speed is preferably 500 rpm to 800 rpm, and in one embodiment, 500 rpm, 600 rpm, 650 rpm, 700 rpm or 800 rpm can be selected; the mixing time is preferably 15 minutes to 30 minutes, and in one embodiment, 15 minutes, 18 minutes, 20 minutes, 22.5 minutes, 28 minutes or 30 minutes can be selected to ensure that each component is fully and evenly mixed, so that the antioxidant and the glidant are evenly distributed in the microcapsule powder to obtain composite vegetable oil microcapsule powder. The present invention has no special limitation on the mixing equipment, and conventional mixing equipment in the art can be used. According to the production scale and product characteristics, a horizontal mixer or a conical mixer can be selected.

[0041] In the present invention, the sizes of the resistant dextrin, maltitol oligosaccharide, casein, and isomaltooligosaccharide are preferably 40 to 80 mesh, and in one embodiment, 40 mesh, 50 mesh, 60 mesh, 70 mesh, or 80 mesh can be selected; the sizes of the emulsifier, antioxidant, microcapsule wall material, and glidant are preferably 80 to 120 mesh, and in one embodiment, 80 mesh, 90 mesh, 100 mesh, 110 mesh, or 120 mesh can be selected; the present invention has no special limitation on the method for controlling the sizes of the above raw materials, and the conventional methods in the art for controlling the sizes of raw materials can be used. In one embodiment, sieving can be selected.

[0042] The technical solutions provided by the present invention will be described in detail below in conjunction with embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0043] In the following embodiments, unless otherwise specified, all are conventional methods.

[0044] In the following embodiments, the materials, reagents, etc. used, unless otherwise specified, can be obtained from commercial channels.

[0045] The equipment and models used in the following embodiments are: hydration tank, model LYY120; alkali refining tank, model 1730; decolorization tank, model JL-2-500; deodorization tank, model JL-2-500; centrifuge, model ZYDB21SJ-34.

[0046] Example 1

[0047] A composite vegetable oil microcapsule powder is prepared from an oil phase, a water phase, and auxiliary materials. The oil phase, water phase, and auxiliary materials include the following raw materials:

[0048] Oil phase: 15 kg of refined coconut oil, 10 kg of refined linseed oil, 8 kg of refined safflower oil; water phase: 20 kg of resistant dextrin, 12 kg of maltitol oligosaccharide; auxiliary materials: 10 kg of casein, 8 kg of isomaltooligosaccharide, 1.5 kg of mono- and diglycerol fatty acid esters, 3 kg of octenyl succinic anhydride starch sodium, 0.5 kg of potassium citrate, 0.5 kg of sodium ascorbate, 1.5 kg of silicon dioxide.

[0049] The preparation method of the composite vegetable oil microcapsule powder includes the following steps:

[0050] 1. Pretreatment

[0051] 1.1 The refining processes of the refined coconut oil, refined linseed oil, and refined safflower oil are as follows:

[0052] The coconut oil, linseed oil, and safflower oil are respectively fed into a degumming device (hydration tank), heated at 70 °C, 0.2% phosphoric acid is added, stirred for 12.5 minutes, and then allowed to stand and settle for 4.5 h to remove the colloid, obtaining the degummed oil;

[0053] Feed the degummed oil into a deacidification device (caustic refining tank), add 0.2% sodium hydroxide, stir for 12.5 minutes, then let it stand and settle for 7 hours to remove soapstock, obtaining the deacidified oil;

[0054] Feed the deacidified oil into a decolorization device (decolorization tank), add 0.75% activated carbon, stir for 25 minutes, then use a filtration device to filter and remove the adsorbent (activated carbon), obtaining the decolorized oil;

[0055] Feed the decolorized oil into a deodorization device (deodorization tank), carry out vacuum distillation at 190 °C, with a vacuum degree of 0.2 MPa and a time of 30 minutes, obtaining refined coconut oil, linseed oil and safflower oil.

[0056] 1.2 Sieving of raw materials

[0057] Put resistant dextrin, maltitol oligosaccharide, casein, and isomaltooligosaccharide into a vibrating screen respectively, adjust the screen aperture to 60 mesh, the vibration frequency to 75 Hz, and the amplitude to 3.5 mm, and carry out sieving to remove large particles and impurities, obtaining treated resistant dextrin, maltitol oligosaccharide, casein, and isomaltooligosaccharide;

[0058] Put potassium citrate, mono- and diglycerol fatty acid esters, sodium starch octenyl succinate, sodium ascorbate, and silicon dioxide into a gyratory vibrating screen respectively, adjust the screen aperture to 100 mesh, and the rotation speed to 1500 rpm, and carry out sieving to ensure that the particles are small and uniform, obtaining treated potassium citrate, mono- and diglycerol fatty acid esters, sodium starch octenyl succinate, sodium ascorbate, and silicon dioxide, which is convenient for subsequent mixing and dispersion.

[0059] 2. Microencapsulation:

[0060] Weigh the raw materials obtained in step 1 of this example according to the following weights:

[0061] Oil phase: 15 kg of refined coconut oil, 10 kg of refined linseed oil, 8 kg of refined safflower oil; aqueous phase: 20 kg of resistant dextrin, 12 kg of maltitol oligosaccharide, 10 kg of casein, 8 kg of isomaltooligosaccharide; auxiliary materials: 1.5 kg of mono- and diglycerol fatty acid esters, 3 kg of sodium starch octenyl succinate, 0.5 kg of potassium citrate, 0.5 kg of sodium ascorbate, 1.5 kg of silicon dioxide.

[0062] (1) Preparation of oil phase: Mix the refined coconut oil, linseed oil and safflower oil, heat to 55 °C in a stirring tank, and use a high-speed shear stirrer to stir evenly at a speed of 650 rpm for 12.5 minutes.

[0063] (2) Preparation of aqueous phase: Mix the treated resistant dextrin, maltitol oligosaccharide, casein, and isomaltooligosaccharide, add them to 22.5 L of water, heat to 65 °C in a stirring tank, stir at a speed of 1250 rpm using a high-speed shear stirrer for 37.5 minutes until completely dissolved to obtain the aqueous phase.

[0064] (3) Primary emulsification: Slowly add the oil phase to the aqueous phase in a high-shear emulsifier, perform high-speed shear emulsification at 55 °C, with a shear speed of 10000 rpm and an emulsification time of 12.5 minutes to form a primary emulsion.

[0065] (4) Homogenization: Feed the primary emulsion into a homogenizing emulsifier for high-pressure homogenization. The homogenization pressure is 40 MPa and the number of homogenization times is 4 times to form microcapsule emulsion 1.

[0066] (5) Adding emulsifier and microcapsule wall material: In a stirring tank, mix microcapsule emulsion 1 with mono- and diglycerol fatty acid esters and sodium starch octenyl succinate, stir at a speed of 650 rpm using a high-speed shear stirrer for 12.5 minutes to obtain microcapsule emulsion 2.

[0067] (6) Spray drying: Feed microcapsule emulsion 2 into a spray drying tower, atomize the emulsion into uniform fine droplets through a centrifugal atomizer, control the inlet air temperature at 165 °C, the outlet air temperature at 85 °C, and the atomization pressure at 28 MPa to quickly evaporate the water in the emulsion and form microcapsule powder;

[0068] Use a cyclone separator to collect the dried microcapsule powder to improve the product yield and purity;

[0069] For the microcapsule powder that cannot be completely collected, use a bag filter for further collection to ensure the product purity;

[0070] (7) Mixing: Mix the microcapsule powder obtained by spray drying with potassium citrate, sodium ascorbate, and silicon dioxide in a mixer at a mixing speed of 650 rpm for 22.5 minutes to obtain the composite vegetable oil microcapsule powder.

[0071] Example 2

[0072] A composite vegetable oil microcapsule powder is prepared from an oil phase, an aqueous phase, and auxiliary materials. The oil phase, aqueous phase, and auxiliary materials include the following raw materials:

[0073] Oil phase: 12 kg of refined coconut oil, 8 kg of refined linseed oil, 6 kg of refined safflower oil; Aqueous phase: 15 kg of resistant dextrin, 8 kg of maltitol oligosaccharide, 8 kg of casein, 6 kg of isomaltooligosaccharide; Auxiliary materials: 1 kg of lecithin, 2 kg of maltodextrin, 0.25 kg of potassium citrate, 0.25 kg of sodium ascorbate, 1 kg of silicon dioxide.

[0074] The preparation method of the composite vegetable oil microcapsule powder comprises the following steps:

[0075] 1. Pretreatment

[0076] 1.1 The refining processes of the refined coconut oil, refined linseed oil and refined safflower oil are as follows:

[0077] Respectively feed the coconut oil, linseed oil and safflower oil into a degumming device (hydration tank), heat at 60 °C, add 0.1% citric acid, stir for 10 minutes, and then use a centrifuge at a rotation speed of 5000 rpm for 45 minutes to remove colloids, obtaining degummed oil;

[0078] Feed the degummed oil into a deacidification device (caustic refining tank), add 0.1% sodium hydroxide, stir for 10 minutes, and then let it stand for sedimentation for 8 hours to remove soapstock, obtaining deacidified oil;

[0079] Feed the deacidified oil into a decolorization device (decolorization tank), add 0.5% activated carbon, stir for 20 minutes, and then use a filtration device to filter out the adsorbent (activated carbon), obtaining decolorized oil;

[0080] Feed the decolorized oil into a deodorization device (deodorization tank), carry out vacuum distillation at 180 °C, with a vacuum degree of 0.1 MPa and a time of 20 minutes, obtaining refined coconut oil, linseed oil and safflower oil.

[0081] 1.2 Sieving of raw materials

[0082] Respectively put resistant dextrin, maltitol, casein, isomaltooligosaccharide into a vibrating sieve, adjust the sieve mesh aperture to 40 meshes, the vibration frequency to 50 Hz, and the amplitude to 2 mm for sieving to remove large particles and impurities, obtaining treated resistant dextrin, maltitol, casein, isomaltooligosaccharide;

[0083] Respectively put potassium citrate, lecithin, maltodextrin, sodium ascorbate, silicon dioxide into a rotary vibrating sieve, adjust the sieve mesh aperture to 80 meshes, and the rotation speed to 1000 rpm for sieving to ensure that the particles are small and uniform, obtaining treated potassium citrate, lecithin, maltodextrin, sodium ascorbate, silicon dioxide, which is convenient for subsequent mixing and dispersion.

[0084] 2. Microencapsulation:

[0085] Weigh the raw materials obtained in step 1 of this example according to the following weights:

[0086] Oil phase: 12 kg of refined coconut oil, 8 kg of refined linseed oil, 6 kg of refined safflower oil; aqueous phase: 15 kg of resistant dextrin, 8 kg of maltitol, 8 kg of casein, 6 kg of isomaltooligosaccharide; excipients: 1 kg of lecithin, 2 kg of maltodextrin, 0.25 kg of potassium citrate, 0.25 kg of sodium ascorbate, 1 kg of silicon dioxide.

[0087] (1) Preparation of oil phase: Mix the refined coconut oil, linseed oil and safflower oil, heat to 50 °C in a stirring tank, and stir evenly at a speed of 500 rpm using a high-speed shear stirrer for 10 minutes.

[0088] (2) Preparation of aqueous phase: Mix the treated resistant dextrin, maltitol, casein, and isomaltooligosaccharide, add 11.1 L of water, heat to 60 °C in a stirring tank, and stir at a speed of 1000 rpm using a high-speed shear stirrer for 30 minutes until completely dissolved to obtain the aqueous phase.

[0089] (3) Primary emulsification: Slowly add the oil phase to the aqueous phase in a high-shear emulsifier, perform high-speed shear emulsification at 50 °C, with a shear speed of 8000 rpm and an emulsification time of 10 minutes to form a primary emulsion.

[0090] (4) Homogenization: Feed the primary emulsion into a homogenizing emulsifier for high-pressure homogenization, with a homogenization pressure of 30 MPa and 3 homogenization times to form microcapsule emulsion 1.

[0091] (5) Add emulsifier and microcapsule wall material: In a stirring tank, mix microcapsule emulsion 1 with lecithin and maltodextrin, and stir at a speed of 500 rpm using a high-speed shear stirrer for 10 minutes to obtain microcapsule emulsion 2.

[0092] (6) Spray drying: Feed microcapsule emulsion 2 into a spray drying tower, atomize the emulsion into uniform and fine droplets through a centrifugal atomizer, control the inlet air temperature at 150 °C, the outlet air temperature at 80 °C, and the atomization pressure at 25 MPa to quickly evaporate the water in the emulsion to form microcapsule powder;

[0093] Use a cyclone separator to collect the dried microcapsule powder to improve the yield and purity of the product;

[0094] For the microcapsule powder that cannot be completely collected, use a bag filter for further collection to ensure the purity of the product;

[0095] (7) Mixing: Mix the microcapsule powder obtained by spray drying with potassium citrate, sodium ascorbate and silicon dioxide in a mixer at a mixing speed of 500 rpm for 15 minutes to obtain the composite vegetable oil microcapsule powder.

[0096] Example 3

[0097] A compound vegetable oil microcapsule powder is prepared from an oil phase, an aqueous phase and excipients. The oil phase, aqueous phase and excipients include the following raw materials:

[0098] Oil phase: 18 kg of refined coconut oil, 12 kg of refined linseed oil, 12 kg of refined safflower oil; Aqueous phase: 22 kg of resistant dextrin, 14 kg of maltitol oligosaccharide, 12 kg of casein, 10 kg of isomaltooligosaccharide; Excipients: 2 kg of arabic gum, 4 kg of chitosan, 0.75 kg of potassium citrate, 0.75 kg of sodium ascorbate, 2 kg of silicon dioxide.

[0099] The preparation method of the compound vegetable oil microcapsule powder includes the following steps:

[0100] 1. Pretreatment:

[0101] 1.1 The refining process of the refined coconut oil, refined linseed oil and refined safflower oil is as follows:

[0102] Respectively send coconut oil, linseed oil and safflower oil into a degumming device (hydration tank), heat at 80 °C, add 0.3% phosphoric acid, stir for 15 minutes, and then use a centrifuge at a speed of 6000 r / min for 60 minutes to remove colloid, obtaining degummed oil;

[0103] Send the degummed oil into a deacidification device (caustic refining tank), add 0.3% sodium carbonate, stir for 15 minutes, and then use a centrifuge at a speed of 6000 r / min for 60 minutes to remove soapstock, obtaining deacidified oil;

[0104] Send the deacidified oil into a decolorization device (decolorization tank), add 1.0% clay, stir for 30 minutes, and then use a filtration device to filter and remove the adsorbent (clay), obtaining decolorized oil;

[0105] Send the decolorized oil into a deodorization device (deodorization tank), perform vacuum distillation at 200 °C, with a vacuum degree of 0.3 MPa and a time of 40 minutes, obtaining refined coconut oil, linseed oil and safflower oil.

[0106] 1.2 Sieving of raw materials

[0107] Respectively put resistant dextrin, maltitol oligosaccharide, casein, isomaltooligosaccharide into a vibrating sieve, adjust the sieve mesh aperture to 80 mesh, the vibration frequency to 100 Hz, and the amplitude to 5 mm for sieving to remove large particles and impurities, obtaining treated resistant dextrin, maltitol oligosaccharide, casein, isomaltooligosaccharide;

[0108] Put potassium citrate, gum arabic, chitosan, sodium ascorbate, and silicon dioxide into a vibratory sieve respectively. Adjust the sieve aperture to 120 mesh and the rotation speed to 2000 rpm for sieving to ensure that the particles are fine and uniform, obtaining the treated potassium citrate, gum arabic, chitosan, sodium ascorbate, and silicon dioxide, which are convenient for subsequent mixing and dispersion.

[0109] 2. Microencapsulation:

[0110] Weigh the raw materials obtained in step 1 of this example according to the following weights:

[0111] Oil phase: 18 kg of refined coconut oil, 12 kg of refined linseed oil, 12 kg of refined safflower oil; aqueous phase: 22 kg of resistant dextrin, 14 kg of maltitol oligosaccharide, 12 kg of casein, 10 kg of isomaltooligosaccharide; auxiliary materials: 2 kg of gum arabic, 4 kg of chitosan, 0.75 kg of potassium citrate, 0.75 kg of sodium ascorbate, 2 kg of silicon dioxide.

[0112] (1) Preparation of oil phase: Mix the refined coconut oil, linseed oil, and safflower oil, heat them to 60 °C in a stirring tank, and stir evenly at a speed of 800 rpm using a high-speed shear stirrer for 15 minutes.

[0113] (2) Preparation of aqueous phase: Mix the treated resistant dextrin, maltitol oligosaccharide, casein, and isomaltooligosaccharide, add 34.8 L of water, heat them to 70 °C in a stirring tank, and stir at a speed of 1500 rpm using a high-speed shear stirrer for 45 minutes until completely dissolved to obtain the aqueous phase.

[0114] (3) Primary emulsification: Slowly add the oil phase to the aqueous phase in a high-shear emulsifier, perform high-speed shear emulsification at 60 °C, with a shear speed of 12000 rpm and an emulsification time of 15 minutes to form a primary emulsion.

[0115] (4) Homogenization: Feed the primary emulsion into a homogenizing emulsifier for high-pressure homogenization, with a homogenization pressure of 50 MPa and a homogenization times of 5 times to form microcapsule emulsion 1.

[0116] (5) Add emulsifier and microcapsule wall material: In a stirring tank, mix microcapsule emulsion 1 with gum arabic and chitosan, and stir at a speed of 800 rpm using a high-speed shear stirrer for 15 minutes to obtain microcapsule emulsion 2.

[0117] (6) Spray drying: Feed microcapsule emulsion 2 into a spray drying tower, atomize the emulsion into uniform and fine droplets through a centrifugal atomizer, control the inlet air temperature at 180 °C, the outlet air temperature at 90 °C, and the atomization pressure at 30 MPa to rapidly evaporate the water in the emulsion and form microcapsule powder;

[0118] Use a cyclone separator to collect the dried microcapsule powder, improving the product yield and purity;

[0119] For the microcapsule powder that could not be fully collected, use a bag filter for further collection to ensure the product purity;

[0120] (7) Mixing: Mix the microcapsule powder obtained by spray drying with potassium citrate, sodium ascorbate, and silicon dioxide in a mixer at a mixing speed of 800 rpm for 30 minutes to obtain the composite vegetable oil microcapsule powder.

[0121] Test Example 1

[0122] Perform the following tests on the composite vegetable oil microcapsule powder (hereinafter referred to as microcapsule powder) prepared in Example 1:

[0123] 1. Stability of the microcapsule powder

[0124] Determine the stability of the microcapsule powder according to GB / T 21121-2024 "Determination of Oxidation Stability of Animal and Vegetable Oils (Accelerated Oxidation Test)".

[0125] Accelerated oxidation test results: After an induction period of 6 - 24 hours, the peroxide value is 0.15 - 0.52 mmol / kg, and the acid value is 0.11 - 0.23 mg KOH / g, indicating that the microcapsule powder of the present invention has good oxidation stability.

[0126] 2. Encapsulation efficiency of the microcapsule powder

[0127] Use the solvent extraction method (according to the method for determining the encapsulation efficiency in the reference "Xu Yafu et al. Preparation and Performance Analysis of Antarctic Krill Oil Microcapsule Powder [J]. China Oils and Fats. 2022, 47(02): 70 - 73.") to determine the encapsulation efficiency of the microcapsule powder of the present invention. The results show that the encapsulation efficiency of the microcapsule powder of the present invention is 91.2 - 95.3%.

[0128] 3. Shelf life

[0129] According to the method of the "Guideline for Stability Testing of Health Foods", use the accelerated test at 65 °C. The results show that: the normal temperature shelf life of the microcapsule powder of the present invention is 1.5 - 2 years, indicating that the product quality of the microcapsule powder of the present invention is stable.

[0130] Test Example 2

[0131] Structural characterization of the vegetable oil microcapsule powder (hereinafter referred to as microcapsule powder or CFP) prepared in Example 1

[0132] 1. Determination of microcapsule powder particle size and Zeta potential

[0133] An appropriate amount of microcapsule powder was dissolved in ethanol to prepare a solution with a concentration of 0.1 mg / mL, and its particle size distribution and Zeta potential were detected using a laser nanometer particle size analyzer (Litesizer 500). Each sample was measured 3 times repeatedly.

[0134] The measurement results of the particle size and Zeta potential of the microcapsule powder are as Figure 1 shown. As shown in Figure 1 A, the measured particle size results of the microcapsule powder were 582.19 nm, 499.77 nm, and 582.56 nm respectively, and the PDI (polymer dispersity index) values were 0.2067, 0.2094, and 0.1215 respectively. All PDI values were less than 0.3, indicating that the particle size distribution of this system was uniform, with good stability and dispersibility. Zeta potential is one of the indicators used to evaluate the stability of nanoparticles. Nanoparticles with higher Zeta potential values are relatively more stable. As shown in Figure 1 B, the Zeta potential values of the microcapsule powder after detection were -15.87 mV, -15.80 mV, and -14.28 mV respectively. The Zeta potential data results indicated that the sample particles might undergo a certain degree of agglomeration, but it was not easy to attract each other and agglomerate in large quantities, and the particle stability of the microcapsule powder was relatively good.

[0135] 2. Scanning electron microscopy analysis

[0136] The CFP sample powder was fixed on the sample copper stage, and the excess powder was gently blown away. After sputtering with gold, the microscopic morphological characteristics of CFP were observed using a scanning electron microscope (SEM), and the acceleration voltage was set at 5 kV.

[0137] The morphology of the microcapsule powder was analyzed by SEM, as shown in Figure 2 . Figure 2 A, B, and C in Figure 2 respectively represent the scanning electron microscope images of CFP at different magnifications. As can be seen from

[0138]

[0139] 4.4690 mg of microcapsule powder was accurately weighed using an analytical balance and placed in an alumina crucible, which was then placed in the sample chamber of the instrument. The baseline was adjusted, the temperature range was set to 30 - 600 °C, the gas flow rate was 50 mL / min, the experimental gas was nitrogen, and a thermogravimetric analyzer (NETZSCH TGA209F3, Germany) was used to perform thermogravimetric analysis on the microcapsule powder at a heating rate of 10 K / min.

[0140] Figure 3 The thermogravimetric analysis results of CFP are shown in Figure 3 . As can be seen from Figure 3It can be seen that the TGA heating range is 30 - 600 °C. As the temperature increases, the sample mass gradually decreases. The TGA curve of CFP can be divided into three stages: The first stage is from 30 - 180 °C, where the weight loss curve is flat and the weight loss rate of the sample is 2.5663%. The second stage is from 180 - 420 °C, with a weight loss rate of 85.3675%, and it starts to change rapidly around 300 °C, indicating that the sample begins to thermally decompose. Finally, in the temperature range of 420 - 600 °C, the curve tends to be stable, and the thermal decomposition of the microcapsule powder is basically completed, and the weight change gradually stabilizes.

[0141] 4. Fourier Transform Infrared Spectroscopy (FT-IR)

[0142] An appropriate amount of microcapsule powder was measured using a Fourier transform infrared spectrometer, and the scanning spectral range was set to 500 - 4000 cm -1 , the resolution was 4.000, the number of scans was 32, and the infrared absorption spectrum of the microcapsule powder was collected.

[0143] The Fourier transform infrared spectroscopy measurement results of the microcapsule powder are as Figure 4 shown. It can be seen from Figure 4 that CFP has a very strong and broad characteristic peak at 3383.53 cm -1 , which is the stretching vibration of the characteristic peak caused by -OH. The peak at 2923.56 cm -1 is related to the asymmetric stretching of the C-H bond, that is, the stretching of the free amino acid NH 3 band. The absorption peak at 2854.11 cm -1 is the stretching vibration caused by C-H. The absorption peaks at 1743.88 cm -1 and 1657.35 cm -1 are the stretching vibrations of the characteristic peaks caused by C=O. The absorption peak at 1464.79 cm -1 is the in-plane bending vibration absorption peak of C-H. The absorption peak at 1380.06 cm -1 is the deformation vibration of C-O, and 1234.43 cm -1 is the CH 2 bending vibration. At the same time, at 1173.77 cm -1 it is caused by the in-plane bending vibration of C-H, 1103.67 cm -1 is the C-O-H stretching vibration, and 723.78 cm -1 is the C-C stretching vibration.

[0144] 5. X-ray Diffraction (XRD)

[0145] The CFP was tested using an X-ray diffractometer (Rigaku Ultima IV, Japan). The test conditions were Cu-Kα radiation, a tube voltage of 40 kV, a tube current of 40 mA, a step size of 0.02°, and a scanning range of 5° to 90°. The diffraction spectrum of the sample was recorded.

[0146] XRD can be used to characterize the structural features of a sample, such as its crystalline, amorphous structure, and lattice parameters. It has the advantages of simple sample preparation and non-destructiveness to the sample. The XRD results of the microcapsule powder are as Figure 5 shown. A broad peak was observed at around 2θ = 20°, indicating that the CFP mainly exists in the form of an amorphous polymer.

[0147] The above are only the preferred embodiments of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and refinements can be made, and these improvements and refinements should also be regarded as the protection scope of the present invention.

Claims

1. A composite vegetable oil microcapsule powder, characterized in that: It is prepared from an oil phase, an aqueous phase and auxiliary materials; The oil phase comprises the following raw materials in parts by weight: 12 to 18 parts of coconut oil, 8 to 12 parts of linseed oil and 6 to 12 parts of safflower oil; The aqueous phase comprises the following raw materials in parts by weight: 15-22 parts of resistant dextrin, 8-14 parts of maltooligosaccharide, 8-12 parts of casein, and 6-10 parts of isomaltooligosaccharide; The auxiliary materials include the following raw materials in parts by weight: 1-2 parts of emulsifier, 2-4 parts of microcapsule wall material, 0.5-1.5 parts of antioxidant and 1-2 parts of glidant.

2. The composite vegetable oil microcapsule powder according to claim 1, characterized in that: The coconut oil, linseed oil and safflower oil are refined coconut oil, linseed oil and safflower oil; The refining includes degumming, deacidification, decolorization and deodorization steps.

3. The composite vegetable oil microcapsule powder according to claim 1, characterized in that: The emulsifier includes mono- and di-glycerol fatty acid esters, lecithin or gum arabic.

4. The composite vegetable oil microcapsule powder according to claim 1, characterized in that: The microcapsule wall material includes sodium starch octenylsuccinate, maltodextrin or chitosan.

5. The composite vegetable oil microcapsule powder according to claim 1, characterized in that: The antioxidants include sodium ascorbate and / or potassium citrate.

6. The composite vegetable oil microcapsule powder according to claim 1, characterized in that: The glidant includes silicon dioxide.

7. The method for preparing the composite vegetable oil microcapsule powder according to any one of claims 1 to 6, characterized in that: The following steps are involved: Coconut oil, linseed oil and safflower seed oil are mixed to obtain an oil phase; resistant dextrin, oligomaltose, casein and oligomaltose are mixed, added into water, and stirred until completely dissolved to obtain an aqueous phase; the oil phase is added into the aqueous phase, and shear emulsified at 50°C to 60°C, with a shear rate of 8000rpm to 12000rpm and an emulsification time of 10 minutes to 15 minutes to form a primary emulsion; the primary emulsion is homogenized to obtain a microcapsule emulsion 1; the microcapsule emulsion 1 is mixed with an emulsifier and a microcapsule wall material to obtain a microcapsule emulsion 2; the microcapsule emulsion 2 is spray-dried to obtain a microcapsule powder; the inlet air temperature of the spray drying is 150°C to 180°C, and the outlet air temperature is 80°C to 90°C; the microcapsule powder is mixed with an antioxidant and a flow aid to obtain a composite vegetable oil microcapsule powder.

8. The preparation method according to claim 7, characterized in that: The sizes of the resistant dextrin, maltooligosaccharide, casein and isomaltooligosaccharide are 40-80 meshes; the sizes of the emulsifier, antioxidant, microcapsule wall material and flow aid are 80-120 meshes.

9. The preparation method according to claim 7, characterized in that: The homogenization pressure is 30MPa to 50MPa, and the number of times is 3 to 5 times.

10. The preparation method according to claim 7, characterized in that: The microcapsule powder is mixed with the antioxidant and the glidant at a speed of 500 rpm to 800 rpm for 15 to 30 minutes.

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