High-stability microcapsules of zophobius morio oil, and preparation method and application thereof

Abstract

The application discloses a kind of high-stability pentatomidae oil microcapsules and its preparation method and application, belong to microcapsule technical field.The microcapsule uses pentatomidae oil as core material, maltodextrin, arabic gum and gelatin as wall material, and the mass ratio of core material and wall material is 1:2~1:4;Preparation method includes that maltodextrin, arabic gum and gelatin are added to water and heated to be dissolved to obtain wall material solution, pentatomidae oil is added and emulsified by high shear to obtain emulsion, then by spray drying or freeze drying treatment, pentatomidae oil microcapsule is obtained.The application realizes the efficient embedding of pentatomidae oil by optimizing the composition of wall material and core wall ratio, and the embedding rate can reach more than 95%, the obtained microcapsule particle size is uniform, oxidation stability is significantly improved, and can effectively mask the fishy smell of pentatomidae oil itself.

Description

Technical Field

[0001] This invention relates to the field of microcapsule technology, specifically to a highly stable grain insect oil microcapsule, its preparation method, and its application. Background Technology

[0002] Five-grain insect oil is rich in various unsaturated fatty acids and has high nutritional and medicinal value. However, in practical applications, due to its highly unsaturated chemical structure, five-grain insect oil is extremely sensitive to light, heat, and oxygen, and is very prone to oxidative rancidity. This not only produces a strong odor but also generates harmful substances, resulting in extremely poor product stability. On the other hand, its strong fishy smell and low sensory acceptance severely limit its widespread application in the food, health product, and cosmetic fields.

[0003] Microencapsulation technology is an effective means to solve the above problems. By encapsulating the oil in a protective wall material, it can effectively isolate the influence of the external environment, improve oxidation stability, and mask unpleasant odors. In the prior art, such as patent CN121892048A, a method for masking the odor of Antarctic krill oil using OSA starch and sodium alginate as wall materials is disclosed. However, its wall material system is complex and depends on pH-responsive crosslinking, and the process conditions are relatively harsh.

[0004] Despite the existence of various microencapsulation technologies, problems remain, including low encapsulation efficiency, limited improvement in oxidative stability, and cumbersome preparation processes. Therefore, there is an urgent need to develop a microcapsule with high encapsulation efficiency, that can significantly improve the oxidative stability of millet insect oil and effectively mask its fishy odor, and whose preparation process is simple and easy to implement. Summary of the Invention

[0005] In view of this, the present invention provides a highly stable grain insect oil microcapsule, its preparation method and application, to solve the problems of grain insect oil being easily oxidized and rancid, having a strong fishy smell, poor stability, low encapsulation efficiency and complex process.

[0006] The technical solution provided by this invention is as follows: In a first aspect, the present invention provides a method for preparing highly stable grain insect oil microcapsules, comprising the following steps: S1. Wall material dissolution Add maltodextrin, gum arabic, and gelatin to water, heat and stir until completely dissolved to obtain a wall material solution; S2. Emulsification Five grain insect oil is added to the wall material solution obtained in step S1, and emulsion is obtained by high shear emulsification; S3. Drying The emulsion obtained in step S2 is dried to obtain five grain insect oil microcapsules.

[0007] Furthermore, in step S1, the mass ratio of maltodextrin, gum arabic, and gelatin is (3~5):(2~4):(1~3); the solid content of the wall material solution is 10~20%.

[0008] Furthermore, in step S1, the mass ratio of maltodextrin, gum arabic, and gelatin is 4:3:2.

[0009] Furthermore, in step S2, the high-shear emulsification speed is 8000~15000 rpm, and the time is 5~15 min.

[0010] Furthermore, the drying process in step S3 is either spray drying or freeze drying.

[0011] Furthermore, the spray drying conditions are an inlet air temperature of 150~180℃ and an outlet air temperature of 70~85℃; the freeze drying conditions are drying at -35~-10℃ for 40~50 hours.

[0012] Secondly, the present invention provides a method for preparing highly stable grain insect oil microcapsules as described in any of the preceding claims.

[0013] Furthermore, the five-grain insect oil microcapsules use five-grain insect oil as the core material and maltodextrin, gum arabic, and gelatin as the wall material, wherein the mass ratio of the core material to the wall material is 1:(2~4).

[0014] Furthermore, the particle size of the five-grain insect oil microcapsules is 10~50μm, and the encapsulation rate is ≥95%.

[0015] Thirdly, the present invention provides the application of a grain insect oil microcapsule as described in any of the preceding claims in pharmaceuticals, food, health products or cosmetics.

[0016] The beneficial effects of this invention are as follows: This invention utilizes a composite wall material made from maltodextrin, gum arabic, and gelatin. By optimizing the ratio of these three components and the core-to-wall ratio, highly efficient encapsulation of *Corydalis esculenta* oil is achieved. The resulting microcapsules exhibit high encapsulation efficiency and low surface oil content, significantly reducing core material leakage and loss during storage. The synergistic effect of maltodextrin, gum arabic, and gelatin forms a dense, continuous, and complete wall film on the oil droplet surface, effectively blocking oxygen intrusion, significantly delaying the oxidative rancidity of *Corydalis esculenta* oil, and greatly improving its oxidative stability. Simultaneously, the wall material completely encapsulates the *Corydalis esculenta* oil, effectively masking its inherent fishy odor and significantly improving sensory quality. This allows it to be used as a high-quality functional ingredient in food, health product, and cosmetic fields with stringent flavor and taste requirements. Detailed Implementation

[0017] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be clearly and completely described below in conjunction with the embodiments of this invention. Obviously, the described embodiments are only a part of the embodiments of this invention, not all of them. Based on the embodiments of this invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this invention. Experimental methods in the following embodiments that do not specify specific conditions are generally performed under conventional conditions or as recommended by the manufacturer. Unless otherwise stated, percentages and parts are weight percentages and parts by weight.

[0018] Unless otherwise specified, the technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains. It should be noted that the terms used herein are for the purpose of describing particular embodiments only and are not intended to limit the exemplary embodiments of this application.

[0019] Preparation Example A method for preparing five-grain insect oil includes the following steps: After the dried grain insects were crushed and passed through a 40-mesh sieve, the crushed insects were placed in a supercritical extraction vessel. The extraction pressure was set to 25 MPa, the extraction temperature to 43℃, and the CO2 flow rate to 20 L / h. The extraction was carried out for 3 hours, and the extract was collected to obtain crude oil from the grain insects. According to the test results from PONY Testing Group (report number: B1G205033B1F10I3053), the total amount of unsaturated fatty acids in Wugu Worm Oil is 49.1g / 100g, of which the content of EPA is 2.16g / 100g and the content of nervonic acid is 0.0104g / 100g. Example

[0020] This embodiment provides a method for preparing highly stable grain insect oil microcapsules, including the following steps: S1. Wall material dissolution Weigh 40 g of maltodextrin, 30 g of gum arabic, and 20 g of gelatin, add them to 350 mL of deionized water, heat to 60°C and stir continuously until all wall materials are completely dissolved, to obtain a wall material solution with a solid content of 20%. S2. Emulsification After the wall material solution cooled to room temperature, 25 g of the five grain insect oil obtained from the preparation example was added, and the mixture was sheared at 10,000 rpm for 10 min using a high shear dispersion emulsifier to form a uniform and stable emulsion. S3. Spray drying The emulsion obtained in step S2 was fed into a spray dryer by a peristaltic pump for drying. The spray drying parameters were set as follows: inlet air temperature 170℃, outlet air temperature 80℃, and feed rate 25 mL / min. After drying, the five grain insect oil microcapsules were collected. Example

[0021] This embodiment provides a method for preparing highly stable grain insect oil microcapsules, including the following steps: S1. Wall material dissolution Weigh out 40 g of maltodextrin, 30 g of gum arabic and 20 g of gelatin, add them to 350 mL of deionized water, heat to 60°C and stir continuously until all wall materials are completely dissolved to obtain a wall material solution. S2. Emulsification After the wall material solution cooled to room temperature, 45 g of the five grain insect oil obtained from the preparation example was added, and the mixture was sheared at 10,000 rpm for 10 min using a high shear dispersion emulsifier to form a uniform and stable emulsion. S3. Spray drying The emulsion obtained in step S2 was transferred to a stainless steel tray for freeze drying and pre-frozen in a refrigerator at -40°C for 12 hours to allow the emulsion to solidify completely. The pre-frozen solid was then quickly transferred to a vacuum freeze dryer and vacuum dried at -10°C for 45 hours. After drying, the five grain insect oil microcapsules were collected. Example

[0022] This embodiment provides a method for preparing highly stable grain insect oil microcapsules, including the following steps: S1. Wall material dissolution Weigh 40 g of maltodextrin, 30 g of gum arabic, and 20 g of gelatin, add them to 350 mL of deionized water, heat to 60°C and stir continuously until all wall materials are completely dissolved, to obtain a wall material solution with a solid content of 20%. S2. Emulsification After the wall material solution cooled to room temperature, 30 g of the five grain insect oil obtained from the preparation example was added, and the mixture was sheared at 12,000 rpm for 8 min using a high shear dispersion emulsifier to form a uniform and stable emulsion. S3. Spray drying The emulsion obtained in step S2 was fed into a spray dryer by a peristaltic pump for drying. The spray drying parameters were set as follows: inlet air temperature 165℃, outlet air temperature 78℃, and feed rate 20 mL / min. After drying, the five grain insect oil microcapsules were collected.

[0023] Comparative Example 1 A method for preparing highly stable grain insect oil microcapsules includes the following steps: S1. Wall material dissolution Weigh 90 g of gum arabic, add it to 350 mL of deionized water, heat to 60°C and stir continuously until the gum arabic is completely dissolved to obtain the wall material solution. S2. Emulsification After the wall material solution cooled to room temperature, 25 g of the five grain insect oil obtained from the preparation example was added, and the mixture was sheared at 10,000 rpm for 10 min using a high shear dispersion emulsifier to form a uniform and stable emulsion. S3. Spray drying The emulsion obtained in step S2 was fed into a spray dryer by a peristaltic pump for drying. The spray drying parameters were set as follows: inlet air temperature 170℃, outlet air temperature 80℃, and feed rate 25 mL / min. After drying, the five grain insect oil microcapsules were collected.

[0024] The difference between this comparative example and Example 1 lies in the composition of the wall material; the wall material in this comparative example is only gum arabic.

[0025] Comparative Example 2 A method for preparing highly stable grain insect oil microcapsules includes the following steps: S1. Wall material dissolution Weigh 50 g of gum arabic and 40 g of gelatin, add them to 350 mL of deionized water, heat to 60°C and stir continuously until all wall materials are completely dissolved to obtain a wall material solution. S2. Emulsification After the wall material solution cooled to room temperature, 25 g of the five grain insect oil obtained from the preparation example was added, and the mixture was sheared at 10,000 rpm for 10 min using a high shear dispersion emulsifier to form a uniform and stable emulsion. S3. Spray drying The emulsion obtained in step S2 was fed into a spray dryer by a peristaltic pump for drying. The spray drying parameters were set as follows: inlet air temperature 170℃, outlet air temperature 80℃, and feed rate 25 mL / min. After drying, the five grain insect oil microcapsules were collected.

[0026] The difference between this comparative example and Example 1 lies in the composition of the wall material. The wall material of this comparative example is gum arabic and gelatin.

[0027] Comparative Example 3 A method for preparing highly stable grain insect oil microcapsules includes the following steps: S1. Wall material dissolution Weigh out 50 g of maltodextrin and 40 g of gum arabic, add them to 350 mL of deionized water, heat to 60°C and stir continuously until all wall materials are completely dissolved to obtain a wall material solution. S2. Emulsification After the wall material solution cooled to room temperature, 25 g of the five grain insect oil obtained from the preparation example was added, and the mixture was sheared at 10,000 rpm for 10 min using a high shear dispersion emulsifier to form a uniform and stable emulsion. S3. Spray drying The emulsion obtained in step S2 was fed into a spray dryer by a peristaltic pump for drying. The spray drying parameters were set as follows: inlet air temperature 170℃, outlet air temperature 80℃, and feed rate 25 mL / min. After drying, the five grain insect oil microcapsules were collected.

[0028] The difference between this comparative example and Example 1 lies in the composition of the wall material. The wall material of this comparative example is maltodextrin and gum arabic.

[0029] Comparative Example 4 A method for preparing highly stable grain insect oil microcapsules includes the following steps: S1. Wall material dissolution Weigh 40 g of maltodextrin, 30 g of gum arabic, and 20 g of gelatin, add them to 350 mL of deionized water, heat to 60°C and stir continuously until all wall materials are completely dissolved, to obtain a wall material solution with a solid content of 20%. S2. Emulsification After the wall material solution cooled to room temperature, 90 g of the five grain insect oil obtained from the preparation example was added, and the mixture was sheared at 10,000 rpm for 10 min using a high shear dispersion emulsifier to form a uniform and stable emulsion. S3. Spray drying The emulsion obtained in step S2 was fed into a spray dryer by a peristaltic pump for drying. The spray drying parameters were set as follows: inlet air temperature 170℃, outlet air temperature 80℃, and feed rate 25 mL / min. After drying, the five grain insect oil microcapsules were collected.

[0030] The difference between this comparative example and Example 1 lies in the ratio of core material to wall material. The mass ratio of core material to wall material in this comparative example is 1:1.

[0031] Comparative Example 5 A method for preparing highly stable grain insect oil microcapsules includes the following steps: S1. Wall material dissolution Weigh out 20 g of maltodextrin, 60 g of gum arabic and 10 g of gelatin, add them to 350 mL of deionized water, heat to 60°C and stir continuously until all wall materials are completely dissolved to obtain a wall material solution. S2. Emulsification After the wall material solution cooled to room temperature, 25 g of the five grain insect oil obtained from the preparation example was added, and the mixture was sheared at 10,000 rpm for 10 min using a high shear dispersion emulsifier to form a uniform and stable emulsion. S3. Spray drying The emulsion obtained in step S2 was fed into a spray dryer by a peristaltic pump for drying. The spray drying parameters were set as follows: inlet air temperature 170℃, outlet air temperature 80℃, and feed rate 25 mL / min. After drying, the five grain insect oil microcapsules were collected.

[0032] Compared to Example 1, the proportion of gum arabic in the wall material of this comparative example is too high.

[0033] Comparative Example 6 A method for preparing highly stable grain insect oil microcapsules includes the following steps: S1. Wall material dissolution Weigh out 70 g of maltodextrin, 10 g of gum arabic and 10 g of gelatin, add them to 350 mL of deionized water, heat to 60°C and stir continuously until all wall materials are completely dissolved to obtain a wall material solution. S2. Emulsification After the wall material solution cooled to room temperature, 25 g of the five grain insect oil obtained from the preparation example was added, and the mixture was sheared at 10,000 rpm for 10 min using a high shear dispersion emulsifier to form a uniform and stable emulsion. S3. Spray drying The emulsion obtained in step S2 was fed into a spray dryer by a peristaltic pump for drying. The spray drying parameters were set as follows: inlet air temperature 170℃, outlet air temperature 80℃, and feed rate 25 mL / min. After drying, the five grain insect oil microcapsules were collected.

[0034] Compared to Example 1, the proportion of maltodextrin in the wall material of this comparative example is too high.

[0035] Comparative Example 7 A method for preparing highly stable grain insect oil microcapsules includes the following steps: S1. Wall material dissolution Weigh out 30 g of maltodextrin, 20 g of gum arabic, and 40 g of gelatin, add them to 350 mL of deionized water, heat to 60°C and stir continuously until all wall materials are completely dissolved, to obtain a wall material solution with a solid content of 20%. S2. Emulsification After the wall material solution cooled to room temperature, 25 g of the five grain insect oil obtained from the preparation example was added, and the mixture was sheared at 10,000 rpm for 10 min using a high shear dispersion emulsifier to form a uniform and stable emulsion. S3. Spray drying The emulsion obtained in step S2 was fed into a spray dryer by a peristaltic pump for drying. The spray drying parameters were set as follows: inlet air temperature 170℃, outlet air temperature 80℃, and feed rate 25 mL / min. After drying, the five grain insect oil microcapsules were collected.

[0036] Compared to Example 1, the proportion of gelatin in the wall material of this comparative example is too high.

[0037] Performance testing 1. Particle size determination The particle size of the microcapsules was determined using a laser particle size analyzer.

[0038] 2. Encapsulation rate determination Weigh 1.0 g of the microcapsule products prepared in each example and comparative example, denoted as M. First, determine the surface oil content of the microcapsules: Place the sample in a 50 mL centrifuge tube, add 12 mL of petroleum ether, gently extract for about 5 min, then centrifuge at 5000 r / min for 8 min, and collect the supernatant; repeat the extraction with 8 mL of petroleum ether once more, centrifuge, and combine the two supernatants. Add 12 mL of isopropanol and 6 mL of deionized water to the combined supernatant, mix well, centrifuge at 4000 r / min for 5 min, transfer the upper organic phase to a pre-weighed rotary evaporator flask (mass denoted as M0), and rotary evaporate at 50℃ until the organic solvent is completely evaporated. Then, dry in a 50℃ oven to constant weight, and weigh the rotary evaporator flask at this point, denoted as M1. The surface oil content is calculated using the following formula: Surface oil content (%) = (M1 - M0) / M × 100%.

[0039] Take 1.0 g of the microcapsule product prepared in each example and comparative example, denoted as M, and place it in a 50 mL centrifuge tube. Add 35 mL of 80 mM sodium citrate solution, and gently shake to fully dissolve the microcapsules. Divide the dissolved liquid into two centrifuge tubes, and add 8 mL of n-hexane and 12 mL of isopropanol to each tube respectively. After vigorous shaking and mixing, centrifuge at 3500 r / min for 8 min. Transfer the upper organic phase to a pre-weighed rotary evaporator flask (denoted as M0'), and rotary evaporate at 50°C until the organic solvent is completely evaporated. Dry the flask in a 50°C oven to constant weight, and weigh the flask at this point, denoted as M1'. The total oil content is calculated using the following formula: Total oil content (%) = (M1' - M1') / M × 100%.

[0040] Encapsulation rate (%) = (1 - surface oil content / total oil content) × 100%.

[0041] Each sample was measured in triplicate, and the average value of the results was taken.

[0042] 3. Oxidative stability determination The samples were placed in an open chamber at 40℃ and 75% relative humidity, and samples were taken every 5 days to determine the peroxide value.

[0043] The peroxide value was determined according to the indicator titration method in GB 5009.227-2023 "Determination of Peroxide Value in Food".

[0044] 4. Test Results Table 1 Performance test results of different grain insect oil microcapsules

[0045] As shown in Table 1, the microcapsules of *Polygonum multiflorum* oil prepared in this invention are significantly superior to unencapsulated *Polygonum multiflorum* oil and the comparative products in terms of particle size, encapsulation efficiency, and oxidative stability. Compared with unencapsulated *Polygonum multiflorum* oil, the microcapsules of this invention exhibit a significantly reduced oxidation rate, an extremely slow increase in peroxide value, and a substantial improvement in antioxidant stability. Test results indicate that this invention utilizes a specific ratio of maltodextrin, gum arabic, and gelatin, which synergistically form a dense and complete wall structure, achieving efficient encapsulation and excellent antioxidant protection of *Polygonum multiflorum* oil.

[0046] The above descriptions are merely embodiments of the present invention, and common knowledge such as specific technical solutions and / or characteristics are not described in detail here. It should be noted that those skilled in the art can make various modifications and improvements without departing from the technical solutions of the present invention, and these should also be considered within the scope of protection of the present invention. These modifications and improvements will not affect the effectiveness of the implementation of the present invention or the practicality of the patent. The scope of protection claimed in this application should be determined by the content of its claims, and the specific embodiments described in the specification can be used to interpret the content of the claims.

Claims

1. A method for preparing highly stable grain insect oil microcapsules, characterized in that, Includes the following steps: S1. Wall material dissolution Add maltodextrin, gum arabic, and gelatin to water, heat and stir until completely dissolved to obtain a wall material solution; S2. Emulsification Five grain insect oil is added to the wall material solution obtained in step S1, and emulsion is obtained by high shear emulsification; S3. Drying The emulsion obtained in step S2 is dried to obtain five grain insect oil microcapsules.

2. The method for preparing a highly stable grain insect oil microcapsule according to claim 1, characterized in that, In step S1, the mass ratio of maltodextrin, gum arabic, and gelatin is (3~5):(2~4):(1~3); the solid content of the wall material solution is 10~20%.

3. The method for preparing a highly stable grain insect oil microcapsule according to claim 2, characterized in that, In step S1, the mass ratio of maltodextrin, gum arabic, and gelatin is 4:3:

2.

4. The method for preparing a highly stable grain insect oil microcapsule according to claim 1, characterized in that, In step S2, the high-shear emulsification speed is 8000~15000 rpm, and the time is 5~15 min.

5. The method for preparing a highly stable grain insect oil microcapsule according to claim 1, characterized in that, The drying process in step S3 is either spray drying or freeze drying.

6. The method for preparing a highly stable grain insect oil microcapsule according to claim 5, characterized in that, The conditions for spray drying are an inlet air temperature of 150~180℃ and an outlet air temperature of 70~85℃; the conditions for freeze drying are drying at -35~-10℃ for 40~50 hours.

7. The grain insect oil microcapsules prepared by the method for preparing a highly stable grain insect oil microcapsule according to any one of claims 1-6.

8. The five-grain insect oil microcapsule according to claim 7, characterized in that, The five-grain insect oil microcapsules use five-grain insect oil as the core material and maltodextrin, gum arabic, and gelatin as the wall material, wherein the mass ratio of the core material to the wall material is 1:(2~4).

9. The five-grain insect oil microcapsule according to claim 7, characterized in that, The microcapsules of Wugu insect oil have a particle size of 10~50μm and an encapsulation rate of ≥95%.

10. The application of the five-grain insect oil microcapsule as described in any one of claims 7-9 in pharmaceuticals, food, health products or cosmetics.

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