Squalene-tea oil microcapsule powder with high resolubility and gelatinization
By using heat-denaturated whey protein isolate, natural whey protein isolate and maltodextrin as wall materials, tea oil and squalene were encapsulated and spray-dried, and tea oil microcapsules powder with high resolubleness and gelation characteristics was prepared, which solved the problem that tea oil microcapsules were difficult to achieve high resolubleness and gelation at the same time, and achieved the efficient resolubleness and gelation effects of tea oil microcapsules.
Patent Information
- Application Number
- CN202411981540.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-31
- Publication Date
- 2025-04-11
AI Technical Summary
The prior art has failed to achieve the high resolubility and gelation properties of tea oil microcapsules simultaneously.
Thermal denatured whey protein isolate, natural whey protein isolate and maltodextrin are used as wall materials to encapsulate tea oil and squalene to form an oil-in-water emulsion. Then, microcapsule powder with high resolubleness and gelation characteristics was prepared by spray drying.
The resolving performance and gel characteristics of tea oil microcapsules are significantly improved, so that they can form gels after micro-heating treatment, and have good storage stability and release effects of functional components.
Smart Images

Figure CN119791274A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to a squalene-tea oil microcapsule powder with high solubility and gelability, belonging to the technical field of food processing. Background Art
[0002] Tea oil is rich in 85% to 97% unsaturated fatty acids and active substances such as squalene and vitamin E. Compared with edible oils such as soybean oil and rapeseed oil, the content of squalene in tea oil is higher. Squalene has biological activities such as antioxidant, antibacterial and immune-enhancing. Increasing the content of squalene will help improve the nutritional properties of tea oil. Oily substances have high viscosity and poor fluidity, which greatly limits their application areas. Emulsifying liquid oils and spray-drying them into microcapsule powders is conducive to expanding the application scenarios of tea oil.
[0003] Resolubility is the property of a substance to maintain or restore its solubility after solidification. It is important in food, medicine and cosmetics. Highly resolubility powder in food can improve the dissolution effect of solid beverages, seasonings and baked products. Resolubility is a key indicator for the application of tea oil microcapsules.
[0004] Protein emulsion gel has the dual properties of emulsion and gel. Usually, the gel property of protein is used to denature the protein, use the denatured protein to stabilize the emulsion, and then cross-link to form a gel. This emulsion gel formation process is relatively complicated. If the protein-stabilized oil microcapsule powder can be used to directly dissolve to form a gel network, it will be beneficial to the application of emulsion gel and may expand its application in food shaping or 3D printing. However, research in this area has not been reported.
[0005] The solubility of oil microcapsule powder depends on the hydrophilicity of the particle surface, while gelation depends on the interaction between particles. Therefore, it is difficult to prepare an oil microcapsule with both high solubility and gelation properties. Summary of the invention
[0006] [Technical issues]
[0007] Currently, there is no literature mentioning how to make tea oil microcapsules have both high solubility and gelation properties.
[0008] [Technical solution]
[0009] In order to solve the above problems, the present invention uses heat-denatured whey protein isolate, natural whey protein isolate, and maltodextrin as wall materials to encapsulate tea oil and squalene to obtain an oil-in-water emulsion; and then spray drying is used to prepare a microcapsule powder with high solubility and gelation properties. The microcapsule powder prepared by the present invention can obtain a gel after a slight heating treatment. The method of the present invention greatly improves the solubility and convenient gelation properties of tea oil microcapsules.
[0010] The first object of the present invention is to provide a method for preparing a squalene-tea oil microcapsule powder having high solubility and gelability, comprising the following steps:
[0011] (1) mixing squalene and tea oil uniformly to obtain a tea oil-squalene mixture;
[0012] (2) adding the heat-denatured whey protein isolate solution to the tea oil-squalene mixture to form an oil-in-water emulsion; then adding the natural whey protein isolate solution and mixing evenly, and then adding the maltodextrin solution and mixing evenly to obtain a squalene-tea oil emulsion;
[0013] (3) The squalene-tea oil emulsion is spray-dried to obtain a squalene-tea oil microcapsule powder having high solubility and gelability.
[0014] In one embodiment of the present invention, in step (1), squalene and tea oil are evenly mixed, which reduces the dielectric constant of the tea oil and increases the hydrophobicity of the tea oil.
[0015] In one embodiment of the present invention, the step (1) of uniformly mixing squalene and tea oil may be performed by adding squalene to tea oil and mixing them uniformly.
[0016] In one embodiment of the present invention, the mass ratio of tea oil to squalene in step (1) is 0-100:0-100; more preferably 0-50:50-100.
[0017] In one embodiment of the present invention, in step (2), the mass ratio of the tea oil-squalene mixture, the heat-denatured whey protein isolate, the natural whey protein isolate, and the maltodextrin is 10-30:0-30:20-50:10-25, but not 0; more preferably 30:20:30:20.
[0018] In one embodiment of the present invention, in step (2), the mass concentration of the heat-denatured whey protein isolate solution is 8-12%, the mass concentration of the natural whey protein isolate solution is 20-30%, the mass concentration of the maltodextrin solution is 20-40%, and the solvent is water.
[0019] In one embodiment of the present invention, the heat-denatured whey protein isolate solution in step (2) is obtained by subjecting the heat-denatured whey protein isolate solution to heat treatment at a temperature of 65-90° C. for a time of 20-40 min.
[0020] In one embodiment of the present invention, the preparation conditions for forming the oil-in-water emulsion in step (2) are: high-speed shearing at 14000-16000 rpm to obtain a crude emulsion, and homogenizing at 40-50 MPa for 2-4 times.
[0021] In one embodiment of the present invention, the mixing conditions for adding the natural whey protein isolate solution in step (2) are: high-speed shearing at 14000-16000 rpm to obtain a crude emulsion, and homogenizing at 40-50 MPa for 2-4 times.
[0022] In one embodiment of the present invention, the conditions for uniform mixing of the maltodextrin solution added in step (2) are: high-speed shearing at 14000-16000 rpm to obtain a crude emulsion, and homogenizing at 40-50 MPa for 2-4 times.
[0023] In one embodiment of the present invention, the conditions for spray drying in step (2) are:
[0024] The inlet temperature is 160-170°C, the feed rate is 8-10 mL / min, the outlet temperature is 80-85°C, and the air flow rate is 500-600 L / h.
[0025] The second object of the present invention is to obtain the squalene-tea oil microcapsule powder with high solubility and gelability prepared by the method of the present invention.
[0026] In one embodiment of the present invention, the squalene-tea oil microcapsule powder having both high solubility and gelability is rich in squalene.
[0027] In one embodiment of the present invention, the mass ratio of tea oil-squalene mixture, heat-denatured whey protein isolate, natural whey protein isolate, and maltodextrin in the squalene-tea oil microcapsule powder with high solubility and gelability is 10-30:0-30:20-50:10-25, but not 0; further preferably 30:20:30:20; the mass ratio of tea oil and squalene in the tea oil-squalene mixture is 0-100:0-100; further preferably 0-50:50-100.
[0028] The third object of the present invention is to use the squalene-tea oil microcapsule powder with high solubility and gelability in the field of food, medicine or cosmetics.
[0029] The fourth object of the present invention is to provide a method for improving the embedding efficiency, solubility, stability and gelation performance of squalene-tea oil microcapsule powder, comprising the following steps:
[0030] (1) mixing squalene and tea oil uniformly to obtain a tea oil-squalene mixture;
[0031] (2) adding the heat-denatured whey protein isolate solution to the tea oil-squalene mixture to form an oil-in-water emulsion; then adding the natural whey protein isolate solution and mixing evenly, and then adding the maltodextrin solution and mixing evenly to obtain a squalene-tea oil emulsion;
[0032] (3) The squalene-tea oil emulsion is spray-dried to obtain a squalene-tea oil microcapsule powder with high embedding rate, high solubility, high stability and gelability.
[0033] [Beneficial Effects]
[0034] (1) The present invention improves the embedding rate of tea oil microcapsule powder by increasing the content of squalene rich in tea oil. The high embedding rate has a good protective effect on the functional ingredients, and the addition of active ingredients also gives the microcapsule a higher nutritional value.
[0035] (2) The squalene-tea oil microcapsule powder of the present invention can be dispersed in water in a short time to form a uniform white emulsion; the particle size distribution after redissolution is very close to that of the initial emulsion, and the particle size is small and uniform, which is conducive to the release of internal functional components and human absorption.
[0036] (3) The squalene-tea oil microcapsule powder of the present invention has good storage stability.
[0037] (4) The squalene-tea oil microcapsule powder of the present invention has a resolubilization and gelling effect and can be used for the development of direct shaping products. BRIEF DESCRIPTION OF THE DRAWINGS
[0038] Figure 1 The effects of different squalene contents on the surface oil and embedding efficiency of microcapsule powder in Examples 1-4 are shown.
[0039] Figure 2 The figure shows the effect of different squalene contents on the dielectric constant of the tea oil-squalene mixture in Examples 1-3.
[0040] Figure 3 These are SEM images of tea oil microcapsules (Example 1), tea oil-squalene (Example 2) microcapsules, and squalene microcapsules (Example 4).
[0041] Figure 4 The changes in the hydroperoxide content of the tea oil-squalene mixture (A) and the tea oil-squalene microcapsule powder (B) in Examples 1-4 after different storage times.
[0042] Figure 5 The figure is a comparison of the particle size distribution of the initial emulsion and the reconstituted emulsion prepared in Examples 1-4.
[0043] Figure 6 These are laser confocal images of the tea oil microcapsule reconstituted emulsion in Example 1 at different stirring times.
[0044] Figure 7 These are the performance test results of the surface oil and embedding rate of the microcapsule powder in Example 1 and Comparative Examples 1-4.
[0045] Figure 8 It is a comparison chart of the particle size distribution of the reconstituted emulsions of Examples 1 and 2 and Comparative Examples 1 and 4.
[0046] Fig. 9 The dissolution and gelation effects of the microcapsule powders in Examples 1, 2, 4 and Comparative Examples 1-4 are shown.
[0047] Fig.10 The plasticity effect of the reconstituted gels prepared in Example 1, Example 2 and Comparative Example 4. DETAILED DESCRIPTION
[0048] The preferred embodiments of the present invention are described below. It should be understood that the embodiments are for better explaining the present invention and are not used to limit the present invention.
[0049] Test method:
[0050] 1. Test methods for particle size and potential:
[0051] NanoBrook Omni particle size analyzer and potentiometer (Brookhaven Instruments, USA) were used to measure the particle size and light intensity distribution of the samples.
[0052] The sample was diluted 500 times and balanced at 25°C for 1 min before measurement. The laser diffraction angle was 90°, the refractive index of water was 1.33, and the particle size distribution of the sample was calculated using the NNLS model.
[0053] 2. Test methods for surface oil and embedding rate:
[0054] Dry a 25 mL beaker at 105°C for 1 hour, cool it in a desiccator for 0.5 hour, and weigh its mass, recorded as m. 1 Take 1g (recorded as m) of microcapsule powder, add 20mL of petroleum ether, mix thoroughly and shake for 50s, filter the sample and collect the filtrate in a beaker, rinse the remaining sample with 5mL of petroleum ether, evaporate the petroleum ether in a 60℃ water bath, place the beaker at 105℃ for 1h, take it out, cool it in a desiccator for 0.5h, and weigh its mass, recorded as m. 2 .
[0055] Dry a 25 mL beaker at 105°C for 1 hour, cool it in a desiccator for 0.5 hour, and weigh its mass, recorded as M. 1Take 1g (denoted as M) of microcapsule powder; add 1mL of ammonia water and 7.5mL of methanol, vortex and oscillate for 2min; then add 17mL of ether, vortex and oscillate for 2min; finally, add 17mL of petroleum ether, vortex and oscillate for 2min, filter the sample with a funnel and collect the filtrate into a constant weight beaker, rinse the remaining sample with 5mL of petroleum ether, evaporate the filtrate in a 60℃ water bath, place the beaker at 105℃ for 1h, take it out, cool it in a desiccator for 0.5h, and weigh its mass, denoted as M 2 .
[0056] The surface oil, total oil and embedding rate of the sample were calculated according to formulas (1), (2) and (3):
[0057]
[0058]
[0059] 3. Laser confocal test method
[0060] 5 mL of 1 mg / mL Nile red-ethanol solution was added to 100 g of the initial emulsion to prepare a Nile red emulsion. The Nile red emulsion was spray dried under the following drying conditions: inlet temperature of 170°C, feed rate of 8 mL / min, outlet temperature of 85°C, and air flow rate of 600 L / h to prepare a dyed microcapsule powder. The dyed microcapsule powder was mixed with water at a powder-water mass ratio of 1:3, stirred at 500 r / min for 0.25-12 h, and the oil droplet distribution of the reconstituted emulsion was observed using a laser confocal microscope.
[0061] 4. Microstructure testing method:
[0062] The microstructure of the microcapsule powder was observed using a Hitachi SU8100 (Regulus8100) cold field emission scanning electron microscope.
[0063] Take a small amount of microcapsule powder sample and spread it on the conductive glue. Use an ear-cleaning bulb to carefully blow away the loose sample. Spray gold on the sample and observe the microstructure of the microcapsule powder.
[0064] 5. Test method for oxidation stability:
[0065] The microcapsule powder and its core material were placed in a 45°C thermostat for 42 days. At different time points, 0.1 g of microcapsule powder was added to 0.3 g of deionized water and stirred at room temperature for 2 h at 500 rpm. 0.4 g of the reconstituted emulsion (corresponding to 0.03 g of core material) was added to 1.5 mL of isooctane-isopropanol (3:1, v / v) solution, vortexed for 1 min, and then centrifuged (3000 rpm, 5 min). Take 0.2 mL of the upper organic phase and place it in 2.8 mL of methanol-n-butanol (2:1, v / v) solution, and add 15 μL of ferrous ion solution (0.132 M barium chloride solution and 0.144 M ferrous sulfate solution are mixed in a 1:1 volume ratio under acidic conditions) and 15 μL of ammonium thiocyanate solution (3.94 M). After vortexing for 30 seconds, protect from light and react for 20 minutes. Measure the absorbance at 510 nm and substitute it into the isopropylbenzene hydroperoxide standard curve to calculate the concentration of hydroperoxide.
[0066] 6. Test method for dielectric properties:
[0067] Squalene and tea oil were mixed in a mass ratio of 0:100, 10:90, 20:80, 30:70, 40:60, 50:50 and 100:0, 45 mL of the oil phase was taken into a 50 mL centrifuge tube, placed in a room, and after reaching room temperature, the dielectric constant was measured using a 870 liquid dielectric constant meter (Brookhaven Instruments, USA) at a gear of 1-20. Raw materials used in the embodiment:
[0068] Natural whey protein isolate: Agropur, BiPRO9500, purity ~94%, purchased from Shanghai Hengyu Investment Co., Ltd.;
[0069] Camellia oil: purchased from Zhejiang Jiusheng Camellia Oil Technology Co., Ltd.;
[0070] Squalene: purity ~80%, purchased from Yichun Sea Turtle Life Science Co., Ltd.;
[0071] a-Tocopherol acetate: purity 99.2%, purchased from Zhejiang Medicine Co., Ltd.;
[0072] Maltodextrin: DE value: 16.5-19.5, purchased from Sigma-Aldrich.
[0073] The solutions mentioned in the examples without specifying the solvent are water; the % mentioned without specifying the meaning refers to the mass percentage; the reaction temperature not mentioned is room temperature 20-30°C.
[0074] The spray drying parameters were set as follows:
[0075] Spray drying was performed using a BUCHI Mini Spray Dryer B-290 laboratory spray drying apparatus at an inlet temperature of 170°C, a feed rate of 8-10 mL / min, an outlet temperature of 85°C, and an air flow rate of 600 L / h.
[0076] Example 1
[0077] A method for preparing squalene-tea oil microcapsule powder with high solubility and gelability comprises the following steps:
[0078] (1) dissolving natural whey protein isolate in water to obtain a natural whey protein isolate solution with a mass concentration of 10%; heating the whey protein isolate solution in a water bath at 85° C. for 30 min to denature the protein, and cooling to room temperature to obtain a heat-denatured whey protein isolate solution with a mass concentration of 10%;
[0079] Dissolving natural whey protein isolate in water to obtain a natural whey protein isolate solution with a mass concentration of 25%;
[0080] Dispersing maltodextrin in water to obtain a maltodextrin solution with a mass concentration of 40%;
[0081] (2) 15 g of tea oil was added to 100 g of heat-denatured whey protein isolate solution, mixed, high-speed shearing at 16000 rpm to obtain a crude emulsion, and homogenized at 50 MPa for 3 times to obtain an oil-in-water emulsion; 60 g of whey protein isolate solution was added to 115 g of oil-in-water emulsion, mixed, high-speed shearing at 16000 rpm to obtain a crude emulsion, and homogenized at 50 MPa for 3 times; 25 g of maltodextrin solution was added, mixed, high-speed shearing at 16000 rpm to obtain a crude emulsion, and homogenized at 50 MPa for 3 times to obtain an initial emulsion;
[0082] The content of heat-denatured whey protein isolate in the initial emulsion is 5%, the content of whey protein isolate is 7.5%, the concentration of maltodextrin is 5%, the content of tea oil is 7.5%, and the content of water is 75%.
[0083] (3) The emulsion is spray-dried to obtain squalene-tea oil microcapsule powder (100% tea oil) with high solubility and gelability.
[0084] Example 2
[0085] The "15 g tea oil" in step (2) of Example 1 was adjusted to "7.5 g tea oil and 7.5 g squalene" so that the mass ratio of tea oil to squalene was 50:50, and the mass percentage of squalene was 50%; the rest was consistent with Example 1, and squalene-tea oil microcapsule powder (50% tea oil + 50% squalene) was obtained.
[0086] Example 3
[0087] The "15 g tea oil" in step (2) of Example 1 was adjusted to "13.5 g tea oil and 1.5 g squalene", "12.0 g tea oil and 3.0 g squalene", "10.5 g tea oil and 4.5 g squalene", "9.0 g tea oil and 6.0 g squalene" so that the mass ratios of tea oil and squalene were 90:10, 80:20, 70:30, and 60:40, and the mass percentages of squalene were 10%, 20%, 30%, and 40%; the rest were kept consistent with Example 1 to obtain squalene-tea oil microcapsule powder.
[0088] Example 4
[0089] The "15 g tea oil" in step (2) of Example 1 was adjusted to "0 g tea oil and 15.0 g squalene" so that the mass ratio of tea oil to squalene was 0:100 and the mass percentage of squalene was 100%; the rest was consistent with Example 1 to obtain squalene microcapsule powder (100% squalene).
[0090] Example 5
[0091] The reconstituted emulsion was prepared using the microcapsule powder prepared in Examples 1-4, as follows:
[0092] Accurately weigh 0.1 g of microcapsule powder, add 0.3 g of ultrapure water according to the same solid content as the initial emulsion, stir at 500 rpm for different time (0.5-12 h) to obtain a reconstituted emulsion. The reconstituted emulsion is tested for particle size.
[0093] 0.12 g of microcapsule powder was accurately weighed, 0.28 g of ultrapure water was added, and the mixture was stirred at 500 rpm for 2 h to obtain a reconstituted emulsion having a solid content of 30%. The reconstituted emulsion was subjected to a gel forming test.
[0094] 0.04 g of microcapsule powder was accurately weighed, 0.36 g of ultrapure water was added, and the mixture was stirred at 500 rpm for 2 h to obtain a reconstituted emulsion having a solid content of 10%. The reconstituted emulsion was subjected to a gel forming test.
[0095] Accurately weigh 0.15 g of microcapsule powder, add 0.45 g of ultrapure water according to the same solid content as the initial emulsion, stir at 500 rpm and 60°C for 20 min to obtain a reconstituted emulsion, place it at 60°C for 8 h, and then perform a gel plasticity test on the reconstituted emulsion.
[0096] The obtained tea oil microcapsule powder, initial emulsion and reconstituted emulsion were subjected to performance tests, and the test results are as follows:
[0097] Figure 1The effects of different squalene contents on the surface oil and embedding efficiency of microcapsule powder in Examples 1-4 are shown in FIG. Figure 1 It can be seen that: when a higher proportion of squalene is added (>30%), the embedding rate of the microcapsule powder is significantly improved, and the microcapsule embedding rate increases with the increase of squalene content. When the squalene content is 100%, the microcapsule embedding rate reaches 94.9%; when the squalene content is 0%, the surface oil of tea oil microcapsules is 3.4% and the embedding rate is 83.4%.
[0098] Figure 2 The effect of different squalene contents on the dielectric constant of tea oil-squalene mixture in Examples 1-3. Figure 2 It can be seen that the dielectric constant of tea oil is ~3.1, and the dielectric constant of squalene is ~2.4. Squalene is more hydrophobic than tea oil. As the amount of squalene added increases, the dielectric constant decreases proportionally.
[0099] Figure 3 The SEM images of tea oil microcapsules (Example 1), tea oil-squalene (Example 2) microcapsules and squalene microcapsules (Example 4) are shown in FIG. Figure 3 It can be seen that all the microcapsule powder particles are approximately spherical, with a smooth surface and some dents. The particles are complete in shape, with almost no cracks and breaks. They can isolate the internal tea oil and air, and have a good protective effect.
[0100] Figure 4 The changes in the content of hydroperoxide in the tea oil-squalene mixture (A) and tea oil-squalene microcapsule powder (B) in Examples 1-4 after different storage times. Figure 4 It can be seen that after 42 days of storage, the content of hydrogen peroxide in the tea oil-squalene microcapsule powder was below 2 mmol / kg, and the microcapsules inhibited the oxidation of the internal core material.
[0101] Figure 5 The figure is a comparison of the particle size distribution of the initial emulsion and the reconstituted emulsion prepared in Examples 1-4. Figure 5 It can be seen that the particle size of all initial emulsions presents a unimodal distribution. With the increase of squalene addition, the initial emulsion particle size shows a decreasing trend. The peak of tea oil emulsion is ~325nm, and the particle size of squalene emulsion is ~240nm. The peak shape is narrow and the droplet distribution is uniform. All microcapsule powders form a unimodal distribution after stirring for 8 hours. The initial emulsion particle size peaks of 0%, 10%, 50% and 100% squalene addition are at 324, 324, 266 and 241nm respectively. After re-dissolution, the particle size peaks shift to 394, 394, 357 and 324nm respectively. The particle size of the emulsion before and after re-dissolution is similar.
[0102] Figure 6This is the laser confocal image of tea oil microcapsule reconstituted emulsion under different stirring times in Example 1. Figure 6 It can be seen that: when the stirring time is short (0.5-2h), there is aggregation between the oil droplets in the reconstituted emulsion; as the reconstitution time increases, the aggregation of the oil droplets in the reconstituted emulsion completely disappears at 6h.
[0103] Comparative Example 1
[0104] The "15 g tea oil" in step (1) of Example 1 was adjusted to "7.5 g tea oil and 7.5 g vitamin E" and the rest was kept consistent with Example 1 to obtain tea oil microcapsule powder (50% tea oil + 50% squalene).
[0105] Comparative Example 2
[0106] In step (1) of Example 1, "15 g tea oil" was changed to "15 g vitamin E" and the rest was kept the same as Example 1 to obtain microcapsule powder (100% VE).
[0107] Comparative Example 3
[0108] The “15 g tea oil” in step (1) of Example 1 was adjusted to “7.5 g squalene and 7.5 g vitamin E”, and the rest was kept the same as Example 1 to obtain microcapsule powder (50% VE + 50% squalene).
[0109] Comparative Example 4
[0110] The “15 g tea oil” in step (1) of Example 1 was adjusted to “7.5 g tea oil, 3.75 g squalene and 3.75 g vitamin E”, and the rest was kept consistent with Example 1 to obtain microcapsule powder (25% VE + 25% squalene + 50% tea oil).
[0111] Comparative Example 5
[0112] The “100 g 10% heat-denatured whey protein isolate solution” and “60 g 25% whey protein isolate solution” in step (2) of Example 1 were adjusted to “100 g 25% whey protein isolate solution”, and the rest was kept consistent with Example 1 to obtain microcapsule powder.
[0113] The obtained microcapsule powder was used to prepare a reconstituted emulsion according to the method of Example 5, and the performance test was performed. The test results are as follows:
[0114] Figure 7 These are the performance test results of the surface oil and embedding rate of the microcapsule powder in Example 1 and Comparative Examples 1-4. Figure 8 : is a comparison chart of the particle size distribution of the reconstituted emulsions of Examples 1 and 2 and Comparative Examples 1 and 4. Figure 7 and Figure 8It can be seen that: the particle size of the reconstituted emulsion of Example 1 presents a unimodal distribution, the surface oil is 3.4%, and the embedding efficiency is 83.4%; the reconstituted emulsion of Comparative Example 1 presents a bimodal distribution, the surface oil is 5.7%, the embedding efficiency is 74.7%, and the addition of vitamin E reduces the embedding efficiency of tea oil microcapsules; the surface oil of the microcapsule powder of Comparative Example 2 is 8.6%, the embedding efficiency is 58.5%, and the embedding efficiency of vitamin E microcapsules is poor; the surface oil of the microcapsule powder of Comparative Example 3 is 1.7%, and the embedding efficiency is 92.3%, and the addition of squalene can improve the embedding efficiency of vitamin E; the particle size of Comparative Example 4 presents a unimodal distribution, the surface oil of the microcapsules is 1.7%, and the embedding efficiency is 92.4%, and the microcapsules co-embedded with tea oil, squalene and vitamin E have a higher embedding efficiency.
[0115] Fig. 9 The resolubilization and gelation effects of the microcapsule powders in Examples 1, 2, 4 and Comparative Examples 1-4. Fig. 9 It can be seen that the microcapsule powders of Examples 1, 2 and 4 can form gels at 60°C, 2h and 45°C, 8h in the reconstituted emulsion with a solid content of 30%, but only the reconstituted emulsion with 100% squalene can form gels at a solid content of 30%, 37°C, and 8h; when the solid content is 10%, the other samples except Comparative Example 5 form gels at 37°C, 18h; all samples cannot form gels at 25°C, 18h. At a solid content of 30%, a temperature of 45°C, and a temperature of 8h, Comparative Example 1 cannot form a gel, and the addition of vitamin E reduces the gelling property of the tea oil reconstituted emulsion; Comparative Example 2 cannot form a gel, and the gelling property of the vitamin E reconstituted emulsion is poor; Comparative Example 3 can form a gel, and the addition of squalene can improve the gelling property of the vitamin E reconstituted emulsion; Comparative Example 4 is in a semi-gelled state, and compared with the tea oil-squalene co-embedded sample, the gelling property of the reconstituted emulsion co-embedded with tea oil, squalene and vitamin E is poor; No matter what the conditions are, Comparative Example 5 cannot form a gel, indicating that the addition of heat-denatured whey protein isolate is beneficial to the gelation of the reconstituted emulsion.
[0116] Fig.10 The plasticity effect of the reconstituted gel prepared in Example 1, Example 2 and Comparative Example 4. Fig.10 It can be seen that Example 1, Example 2 and Comparative Example 4 have good gel plasticity.
[0117] Although the present invention has been disclosed as above in the form of a preferred embodiment, it is not intended to limit the present invention. Anyone familiar with this technology can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention should be based on the definition of the claims.
Claims
1. A method for preparing squalene-tea oil microcapsule powder with high solubility and gelability, characterized in that: The steps include: (1) mixing squalene and tea oil uniformly to obtain a tea oil-squalene mixture; (2) adding the heat-denatured whey protein isolate solution to the tea oil-squalene mixture to form an oil-in-water emulsion; then adding the natural whey protein isolate solution and mixing evenly, and then adding the maltodextrin solution and mixing evenly to obtain a squalene-tea oil emulsion; (3) The squalene-tea oil emulsion is spray-dried to obtain a squalene-tea oil microcapsule powder having high solubility and gelability.
2. The method according to claim 1, characterized in that In step (1), the mass ratio of tea oil to squalene is 0-100:0-100; more preferably 0-50:50-100.
3. The method according to claim 1, characterized in that In step (2), the mass ratio of the tea oil-squalene mixture, the heat-denatured whey protein isolate, the natural whey protein isolate and the maltodextrin is 10-30:0-30:20-50:10-25, but not 0; more preferably 30:20:30:
20.
4. The method according to claim 1, characterized in that: The heat-denatured whey protein isolate solution in step (2) is obtained by subjecting the heat-denatured whey protein isolate solution to heat treatment at a temperature of 65-90° C. for a time of 20-40 min.
5. The method according to claim 1, characterized in that In step (2), the mass concentration of the heat-denatured whey protein isolate solution is 8-12%, the mass concentration of the natural whey protein isolate solution is 20-30%, the mass concentration of the maltodextrin solution is 20-40%, and the solvent is water.
6. The method according to claim 1, characterized in that The preparation conditions for forming the oil-in-water emulsion in step (2) are: high-speed shearing at 14000-16000 rpm to obtain a crude emulsion, and homogenizing at 20-30° C. and 40-50 MPa for 2-4 times.
7. The method according to claim 1, characterized in that The conditions for spray drying are: The inlet temperature is 160-170°C, the feed rate is 8-10 mL / min, the outlet temperature is 80-85°C, and the air flow rate is 500-600 L / h.
8. The squalene-tea oil microcapsule powder having high solubility and gelability prepared by the method according to any one of claims 1 to 7.
9. Use of the squalene-tea oil microcapsule powder with high solubility and gelability as claimed in claim 8 in the fields of food, medicine or cosmetics.
10. A method for improving the embedding efficiency, solubility, stability and gelling performance of squalene-tea oil microcapsule powder, characterized in that: The steps include: (1) mixing squalene and tea oil uniformly to obtain a tea oil-squalene mixture; (2) adding the heat-denatured whey protein isolate solution to the tea oil-squalene mixture to form an oil-in-water emulsion; then adding the natural whey protein isolate solution and mixing evenly, and then adding the maltodextrin solution and mixing evenly to obtain a squalene-tea oil emulsion; (3) The squalene-tea oil emulsion is spray-dried to obtain a squalene-tea oil microcapsule powder with high embedding rate, high solubility, high stability and gelability.