A microgranule embedding a high-load amount of a fat-soluble vitamin, a method for preparing the same, and use thereof

Abstract

The application discloses embedding high-load fat-soluble vitamin microparticles, a preparation method and application thereof. The microparticles are composed of 50-85 parts of fat-soluble vitamins, 10-35 parts of wall materials, 0.1-5 parts of stabilizers and 1-10 parts of drying aids, and have high oil load, high stability and pressure resistance. Compared with the prior art, the microparticle product of the application can still maintain high stability at an oil load of up to 85%, the three-month accelerated retention rate is more than 97%, and the stability of the tablet product is more than 98%. In addition, the microparticle product has low surface oil (less than 10%) and tablet oil permeation rate (less than 5%), and has good pressure resistance (tablet hardness is more than 200N). In the preparation process, no solvent that may produce toxic side effects is used, ensuring the safety and environmental protection of the process. Therefore, the microparticle preparation of the application has wide application prospects in the fields of food, health food and the like.

Description

Technical Field

[0001] This invention relates to the field of vitamin preparation technology, specifically to a method for preparing and applying microparticles encapsulated with high loading capacity of fat-soluble vitamins. Background Technology

[0002] Vitamins are a class of substances that play a vital role in regulating metabolism and maintaining normal physiological functions in the human body; they are essential nutrients. Vitamins A, E, and K are all fat-soluble vitamins. Vitamin A is crucial for maintaining vision and promoting growth and development. It is an important component of the retina and plays a key role in night vision and adapting to changes in light. In addition, vitamin A helps maintain healthy skin and mucous membranes and supports the function of the immune system. Vitamin E is an antioxidant that helps protect cells from damage caused by free radicals. It is very important for maintaining healthy skin and protecting the function of the eyes and nervous system. Furthermore, vitamin E can promote the normal function of the reproductive system. Vitamin K is essential for blood clotting. It participates in the synthesis of clotting proteins, which helps with wound healing and the normal clotting process. In addition, vitamin K may also play a role in bone health.

[0003] The above fat-soluble vitamins are viscous liquids or solids that are insoluble in water at room temperature. They are inconvenient to transport and use, and are also easily affected by oxidation, which affects their effectiveness. In order to improve the stability of vitamins and make them easier to use, many methods have been developed at home and abroad to prepare fat-soluble vitamins into solid products.

[0004] Existing technologies record several research findings on vitamin E preparations: CN200610095069.2 A pressure-resistant vitamin E microcapsule and its preparation method. It describes the preparation of an aqueous phase using a wall material, octenyl succinate starch, auxiliary wall material, and a flow aid. Vitamin E is injected into the aqueous phase wall material, followed by stirring, emulsification, homogenization, and spray drying to obtain the product. The product has an oil loading capacity of up to 70%, good flowability, and certain pressure resistance. CN202211263141.3 A vitamin E granule and its preparation method and application. It describes a method for obtaining vitamin E granules by stirring vitamin E with a solid adsorbent material, the solid adsorbent material including: porous calcium silicate, colloidal silica, or mica. CN202010299430.3 A method for preparing fat-soluble vitamin granules that can be used in beverages. It describes the preparation of vitamin D, vitamin E, or a mixture of both granules using a solvent method with raspberry glycoside as an adjuvant. A clear and transparent solution is obtained by dissolving raspberry glycoside in a solvent and stirring. A fat-soluble vitamin is dispersed in the solvent to obtain a uniformly dispersed suspension. The suspension is slowly added to the solution while stirring, and the solution is dried to obtain a white solid. The white solid is ground and sieved to obtain a powder, which is a fat-soluble vitamin granule suitable for use in beverages. CN201680070628.6 Vitamin Preparation. This relates to a method for preparing granules containing at least one fat-soluble vitamin. The granule composition includes at least one fat-soluble vitamin, at least one emulsifier, and at least one non-reducing sugar. Specifically, the emulsifier and non-reducing sugar are added to an aqueous phase at 65°C, cooled to 50-55°C and degassed for one hour. Fat-soluble vitamin oil containing antioxidants is added to a matrix and emulsified. The emulsion is sprayed onto a spray pan containing corn starch using a rotating nozzle. The starch is removed by sieving to obtain the product granules. CN202011198275.2 A high-oil-load-bearing, pressure-resistant microparticle formulation and its preparation method. Preparation method: (1) Mix the embedding material 1 with the oil phase and stir at 75-85℃ for 15-30 min to obtain an oil phase composition; (2) Dissolve the gelatin raw material in water, add acid to adjust the pH to 2.5-3.5 for hydrolysis, adjust to neutral, and then add transglutaminase for crosslinking to obtain gelatin with a freezing strength of 50-180 Bloom g; (3) Add the oil phase composition obtained in step 1) to the gelatin obtained in step 2), stir, and homogenize and disperse; (4) Add a dispersant during the drying process to obtain a high oil-loaded pressure-resistant microparticle formulation.

[0005] While currently available technical preparation methods can produce fat-soluble vitamin microcapsule powders or microparticles, the products produced suffer from problems such as complex preparation processes, low oil loading, and poor particle pressure resistance. There is no product that can solve all of these problems simultaneously. Summary of the Invention

[0006] To address the pressing technical problems in the background art, this invention discloses an encapsulated high-content fat-soluble vitamin microparticle formulation with high oil loading capacity, high stability, and pressure resistance. Its production process does not use solvents that may produce toxic side effects, facilitating practical application and ensuring the stability of the production process and processing, thus possessing excellent prospects for industrial application.

[0007] A microparticle encapsulating a high-loading fat-soluble vitamin, wherein the raw material of the microparticle comprises the following components in parts by weight:

[0008]

[0009] For the technical solution described above, in a further preferred embodiment, a higher proportion of the oil-carrying component is formed by weight:

[0010]

[0011] In a further preferred embodiment of the above-described technical solution, the fat-soluble vitamin may be selected from at least one of vitamin A acetate, vitamin A palmitate, d-α-tocopherol, dl-α-tocopherol, d-α-tocopherol acetate, dl-α-tocopherol acetate concentrate, d-α-tocopherol acetate concentrate, mixed tocopherol concentrate, vitamin K1, and vitamin K2.

[0012] In a further preferred embodiment of the technical solution described above, the wall material is selected from at least one of gum arabic, gelatin, guar gum, and carrageenan; gelatin is preferred.

[0013] In a further preferred embodiment of the above-described technical solution, the wall material has a gel strength (6.67%) of 180-250 Bloom g (i.e., the gel strength of the wall material at a concentration of 6.67% is 180 to 250 Bloom g); a viscosity (6.67%, 60°C) of 10-30 mPa·s (the viscosity of the wall material at a concentration of 6.67% and a temperature of 60°C is 10 to 30 mPa·s); preferably 10-20 mPa·s; a transmittance of not less than 60% under light with a wavelength of 450 nm; and a transmittance of not less than 80% under light with a wavelength of 620 nm.

[0014] In a further preferred embodiment of the above-described technical solution, the aqueous solution prepared during the use of the wall material needs to be adjusted to a pH of 5.5-6.8.

[0015] In a further preferred embodiment of the above-described technical solution, the drying agent may be selected from at least one of calcium silicate, silicon dioxide, tricalcium phosphate, talc, and corn starch; preferably silicon dioxide.

[0016] In a further preferred embodiment of the above-described technical solution, the specific gravity of the drying agent is 0.05-0.15, and the particle size is 13 micrometers < D90 < 22 micrometers; preferably, the particle size is 15 micrometers < D90 < 17 micrometers; the particle size is 25 micrometers < D99 < 36 micrometers, and more preferably, 27 micrometers < D99 < 34 micrometers.

[0017] In a further preferred embodiment of the above-described technical solution, the stabilizer is preferably agar;

[0018] In a further preferred embodiment of the technical solution described above, the stabilizer gel strength (1.5% solution, 20℃) is 1200-1600 g / cm³. 2 The preferred gel strength (1.5% solution, 20℃) is 1300-1500 g / cm³. 2 ;

[0019] In a further preferred embodiment of the technical solution described above, the weight ratio of the stabilizer to the wall material is 0.01-0.1:1; more preferably, it is 0.01-0.07:1.

[0020] A second aspect of the present invention relates to a method for preparing microparticles encapsulated with high loading of fat-soluble vitamins, comprising the following steps:

[0021] (1) Take 10-35 parts by weight of wall material and put it into room temperature water. After it absorbs water and swells, heat it to dissolve it completely and adjust the pH to between 5.5 and 6.8.

[0022] (2) Take 60-85 parts by weight of fat-soluble vitamins and heat them under light-protected and nitrogen-protected conditions to obtain a free-flowing oily liquid;

[0023] (3) Add step (2) to step (1), emulsify and homogenize twice under light-proof and nitrogen protection conditions, and control the emulsion viscosity at 1500-2500 MPa.s;

[0024] (4) Disperse the stabilizer completely in water, heat until completely dissolved, and then cool.

[0025] (5) Add step (4) to step (3), stir evenly, and spray the emulsion into an environment with a drying agent to obtain dried granules.

[0026] In a further preferred embodiment of the technical solution described above, the heating temperature in step (1) is 45-70°C, more preferably 65-70°C.

[0027] In a further preferred embodiment of the technical solution described above, the heating temperature in step (2) is 60-65℃.

[0028] In a further preferred embodiment of the above-described technical solution, the homogenization conditions in step (3) are a primary homogenization pressure of 20-25 MPa and a secondary homogenization pressure of 45-55 MPa.

[0029] In a further preferred embodiment of the above-described technical solution, the emulsion viscosity in step (3) is 1000-3000 MPa, more preferably 1500-2500 MPa.s, and even more preferably 1800-2400 MPa.s.

[0030] In a further preferred embodiment of the above-described technical solution, the heating temperature in step (4) is 95-98℃.

[0031] In a further preferred embodiment of the technical solution described above, the cooling temperature in step (4) is 60-65℃.

[0032] A third aspect of the present invention is to protect the application of a method for encapsulating high-load fat-soluble vitamin microparticles in the fields of food, health food powders, granules, capsules, tablets, and tablet candies.

[0033] Compared with the prior art, the present invention has the following beneficial effects:

[0034] The fat-soluble vitamin microparticle product of this invention can achieve an oil loading of up to 85%. Even with such a high oil loading, it still maintains high product stability (accelerated retention rate exceeding 97% after three months), high tablet product stability (accelerated retention rate exceeding 98% after three months), low surface oil content (below 10%), low tablet oil leakage rate (below 5%), and good compressive strength (tablet hardness above 200N). The product preparation process is simple, does not use toxic solvents, and is green and safe. It has excellent application prospects in the fields of food and health food powders, granules, capsules, tablets, and tablet candies. Detailed Implementation

[0035] The present invention will be further described below with reference to the embodiments, but it should be understood that the scope of protection of the present invention is not limited to the embodiments.

[0036] In this invention, unless otherwise explicitly stated, percentages and contents are all by mass. Unless otherwise specified, the experimental methods used are conventional methods, and the materials and reagents used are commercially available.

[0037] 1. In the embodiment, the product performance of the samples is evaluated by first sampling and packaging each sample into several parallel samples. In order to ensure the scientificity and credibility of the product performance evaluation, the same number of sub-samples are randomly selected for each product, and the same test conditions and measurement techniques are used for evaluation. The performance is quantified and compared by statistical analysis of the obtained data (calculating the average value).

[0038] 2. Standard test method for gel strength (6.67%) in the examples:

[0039] Accurately weigh a certain amount of sample and dissolve it in water under specified conditions to prepare a solution with a concentration of 6.67%.

[0040] The strength of the gel is measured using a Bloom Gelometer or a similar device. This device typically includes a standard probe that is pressed into the gel surface to a specific depth and the force required is recorded.

[0041] The gel strength is calculated based on the measured force value and the standard curve.

[0042] 3. Standard test method for viscosity (6.67%, 60°C) in the examples:

[0043] Accurately weigh a certain amount of sample and dissolve it in water under specified conditions to prepare a solution with a concentration of 6.67%. Place the solution in a water bath and control the water bath temperature at 60℃.

[0044] The viscosity of a solution is measured using a viscometer (such as a Brookfield viscometer). The rotor is immersed in the sample and rotated at a constant speed; the viscosity is determined by measuring the torque.

[0045] 4. The standard detection method in this embodiment, where the transmittance is not less than 60% under light with a wavelength of 450 nanometers:

[0046] Measurements were performed using a UV-Vis spectrophotometer.

[0047] Prepare the sample solution under specified conditions, place the sample solution in the optical path, set the wavelength to 450 nanometers, and measure the absorbance of the sample.

[0048] Calculate the transmittance using absorbance and ensure it is not less than 60%.

[0049] 4. The standard detection method in this embodiment, where the transmittance is not less than 80% under light with a wavelength of 620 nm:

[0050] The measurements were also performed using a UV-Vis spectrophotometer.

[0051] The wavelength was set to 620 nm to measure the absorbance transmitted through the sample solution.

[0052] Calculate the transmittance using absorbance and ensure it is not less than 80%.

[0053] 5. Standard method for detecting specific gravity in the examples: The specific gravity of the sample is measured using the specific gravity bottle method or the buoyancy method.

[0054] 6. Standard testing methods for particle sizes D90 and D99 in the examples:

[0055] The particle size distribution of the sample is measured using a particle size analyzer (such as a laser diffraction particle size analyzer or a dynamic light scattering particle size analyzer).

[0056] 6. Standard test method for gel strength (1.5% solution, 20°C) in the examples:

[0057] Accurately weigh a certain amount of sample and dissolve it in water at 20℃ to achieve a solution concentration of 1.5%.

[0058] Use a Bloom Gelometer or other similar device to measure and calculate the gel strength, following the steps outlined above.

[0059] 7. Standard detection method for vitamin E content in the examples:

[0060] The tests were conducted according to the methods described in GB 5009.82-2016 National Food Safety Standard for the Determination of Vitamins A, D, and E in Food.

[0061] Example 1

[0062] (1) Accurately weigh 150g of gelatin (gel strength (6.67%) is 213 Bloom g, viscosity (6.67%, 60℃) is 14 MPa.s, transmittance is 78.16% under light with a wavelength of 450 nm and 90.99% under light with a wavelength of 620 nm) and place it in a beaker. Add 520ml of water and let it soak at room temperature until the gelatin absorbs water and swells for 2 hours. Then transfer the beaker to a water bath, heat the water bath to 68℃, and start stirring to completely dissolve the gelatin. Adjust the pH of the solution to 5.8 with a pH adjuster.

[0063] (2) Accurately weigh 720g of dl-α-tocopherol acetate into a beaker, transfer the beaker to a water bath, and heat the water bath to 60°C under light-proof and nitrogen-protected conditions. Turn on the stirring to obtain a free-flowing oily liquid.

[0064] (3) Add the liquid obtained in step (2) to the wall material solution in step (1), stir and emulsify for 40 minutes under light-proof and nitrogen protection conditions, homogenize the emulsion twice, the homogenization pressure of the first homogenization is 22 MPa, the homogenization pressure of the second homogenization is 48 MPa, and the viscosity of the emulsion is 1870 MPa.s.

[0065] (4) Accurately weigh 1.8g of agar (gel strength 1300g / cm). 2 Disperse the agar in 88.2 ml of water, heat to 96°C while stirring, and cool down to 60°C after the agar is completely dissolved.

[0066] (5) Add the solution from step (4) to the emulsion from step (3), stir well, and spray the emulsion into a drying tower containing silica to obtain dried particles. The silica used is 45.4 g, with a specific gravity of 0.08, a particle size D90 of 16.7 μm, and a D99 of 32.4 μm. This sample is designated as Sample 1.

[0067] Example 2

[0068] (1) Accurately weigh 500g of gelatin (gel strength (6.67%) is 185 Bloom g, viscosity (6.67%, 60℃) is 11 MPa.s, transmittance is 78.34% under light with a wavelength of 450 nm and 91.62% under light with a wavelength of 620 nm) and put it into a beaker. Add 1800ml of water and soak at room temperature for 2 hours. Transfer the beaker to a water bath and heat the water bath to 66℃. Start stirring to completely dissolve the gelatin. Adjust the pH of the solution to 6.5 with a pH adjuster.

[0069] (2) Accurately weigh 2600g of d-α-tocopherol acetate into a beaker, transfer the beaker to a water bath, and heat the water bath to 64°C under light-proof and nitrogen-protected conditions. Start stirring to obtain a free-flowing oily liquid.

[0070] (3) Add the liquid obtained in step (2) to the wall material solution in step (1), stir and emulsify for 40 minutes under light-proof and nitrogen protection conditions, homogenize the emulsion twice, the homogenization pressure of the first homogenization is 23 MPa, the homogenization pressure of the second homogenization is 52 MPa, and the viscosity of the emulsion is 2230 MPa.s.

[0071] (4) Accurately weigh 20.6g of agar (gel strength 1400g / cm). 2 Disperse the agar in 500 ml of water, heat to 98°C while stirring, and cool down to 63°C after the agar is completely dissolved.

[0072] (5) Add the solution from step (4) to the emulsion from step (3), stir until homogeneous, and spray the emulsion into a silica drying tower to obtain dried particles. The silica used was 77.4 g, with a specific gravity of 0.12, a particle size D90 of 15.4 μm, and a D99 of 29.8 μm. This sample is designated as sample 2.

[0073] Example 3

[0074] (1) Accurately weigh 1600g of gelatin (gel strength (6.67%) is 225 Bloom g, viscosity (6.67%, 60℃) is 15 MPa.s, transmittance is 83.51% under light with a wavelength of 450 nm and 92.38% under light with a wavelength of 620 nm) and put it into a beaker. Add 4500ml of water and soak at room temperature for 2 hours. Transfer the beaker to a water bath and heat the water bath to 66℃. Start stirring to completely dissolve the gelatin. Adjust the pH of the solution to 6.0 with a pH adjuster.

[0075] (2) Accurately weigh 6800g of mixed tocopherol concentrate into a beaker, transfer the beaker to a water bath, and heat the water bath to 61°C under light-proof and nitrogen-protected conditions. Turn on the stirring to obtain a free-flowing oily liquid.

[0076] (3) Add the liquid obtained in step (2) to the wall material solution in step (1), stir and emulsify for 40 minutes under light-proof and nitrogen protection conditions, homogenize the emulsion twice, the homogenization pressure of the first homogenization is 25 MPa, the homogenization pressure of the second homogenization is 50 MPa, and the viscosity of the emulsion is 2340 MPa.s.

[0077] (4) Accurately weigh 105g of agar (gel strength 1500g / cm). 2 Disperse the agar in 2000ml of water, heat to 97℃ while stirring, and cool down to 65℃ after the agar is completely dissolved.

[0078] (5) Add the solution from step (4) to the emulsion from step (3), stir well, and spray the emulsion into a silica drying tower to obtain dried particles. 280.5 g of silica was used, with a specific gravity of 0.13, a particle size D90 of 16.1 micrometers, and a D99 of 28.6 micrometers. This sample is designated as Sample 3.

[0079] Example 4 (Comparison between the product of this invention and the patented product)

[0080] The content and physicochemical properties of samples 1, 2, 3, 4 (prepared using the method described in patent CN200610095069.2), 5 (prepared using the method described in patent CN202211263141.3), and 6 (prepared as particles using the method described in patent CN202011198275.2) were tested, and the results are shown in Table 1.

[0081] Table 1

[0082]

[0083]

[0084] The surface oil content reflects the encapsulation effect of the product; the lower the surface oil content, the better the encapsulation effect. The detection method involves taking an appropriate amount of sample in a container, adding petroleum ether, and shaking on a shaker to extract the surface oil. The extract is then filtered and collected. This process is repeated three times, with 30 ml, 20 ml, and 20 ml of petroleum ether added respectively. The extracts are combined, the solvent is evaporated to constant weight, and the product is weighed. The ratio of the surface oil content to the particle weight is calculated. In practical applications of this product, according to the formulation of this invention, performance is excellent when the surface oil content is less than 10%; average when the surface oil content is between 10% and 20%; and poor when the surface oil content exceeds 20%.

[0085] Compared with samples 4 and 5, the product obtained by this invention has lower surface oil and higher loading; compared with sample 6, the particle preparation process is easier to control, does not require hydrolysis and cross-linking, and is more conducive to large-scale production.

[0086] Example 5 (Destructive testing results of the product of this invention)

[0087] When conducting the experiments in Tables 2-1 to 2-5, samples 1, 2, 3, 4, 5, and 6 from the same batch were divided into different small packages, with each small package containing the same amount of sample, and it was ensured that the same batch of samples was used each time.

[0088] The packaged samples were placed in a 60℃ accelerated drying oven, and samples were taken for testing at each time point. After testing, the samples were not returned. The samples were then subjected to a 20-day destructive accelerated drying test for evaluation. The results are shown in Tables 2-1 to 2-5:

[0089] Table 2-1

[0090]

[0091] Table 2-2

[0092]

[0093] Table 2-3

[0094]

[0095] Table 2-4

[0096]

[0097] Table 2-5

[0098]

[0099] The 20-day destructive accelerated test showed that after 20 days of accelerated treatment at 60℃, the fat-soluble vitamin product obtained by the process disclosed in this invention did not show significant changes in any of its physicochemical indicators and had a high product retention rate.

[0100] Example 6 (Comparison of accelerated test results for the product of this invention)

[0101] When conducting the experiments in Tables 3-1 to 3-4, samples 1, 2, 3, 4, 5, and 6 from the same batch were divided into different small packages, with each small package containing the same amount of sample, and it was ensured that the same batch of samples was used each time.

[0102] The packaged samples were placed in an accelerated drying oven at 40℃ and 75% RH. Samples were taken and tested at each time point. After testing, the samples were not returned. The accelerated stability test was carried out on each group of samples for 3 months. The results are shown in Tables 3-1 to 3-4:

[0103] Table 3-1

[0104]

[0105] Table 3-2

[0106]

[0107] Table 3-3

[0108]

[0109] Table 3-4

[0110]

[0111] The accelerated stability test at 40℃ and 75%RH shows that after three months of acceleration, the various physicochemical indicators of the fat-soluble vitamin products obtained by the process disclosed in this invention did not change significantly, and the content retention rate was high, with all retention rates above 97%.

[0112] Example 7 (Comparison of Evaluation Results of Tableting Application of the Product of the Invention)

[0113] Samples 1, 2, 3, 4, 5, and 6 were subjected to tableting application tests using the same formulation (the tableting formulation, by weight, consisted of: 15 parts of sample 1, 2, 3, 4, 5, and 6, 20 parts of microcrystalline cellulose, 25 parts of mannitol, 38.5 parts of lactose, and 1.5 parts of magnesium stearate). The results are shown in Table 4. The oil penetration rate reflects the breakage of the product during the tableting process; a lower oil penetration rate indicates less particle breakage. The detection method involves taking an appropriate amount of compressed tablets in a container, adding petroleum ether, shaking on a shaker to extract the surface oil, filtering and collecting the extract. This step is repeated twice, adding 50 ml and 50 ml of petroleum ether respectively. The extracts are combined, the solvent is evaporated to constant weight, and the weight is calculated. The ratio of the oil content to the particle oil content is then calculated. In practical applications of this product, according to the formulation of this invention, performance is excellent when the oil penetration rate does not exceed 5%; average when the oil penetration rate is between 5-10%; and poor when the oil penetration rate exceeds 10%. Tablet hardness reflects the product's compressibility. Tableting is performed using the same formulation, dosage, and compression parameters, and the tablet hardness is tested. Higher tablet hardness indicates stronger compressibility. In practical applications of this product, according to the formulation of this invention, performance is excellent when the tablet hardness exceeds 160N; average when the tablet hardness is between 120N and 160N; and poor when the tablet hardness is below 120N.

[0114] Table 4

[0115]

[0116] The tableting application evaluation experiment shows that the fat-soluble vitamin products obtained by the process disclosed in this invention have smooth tablet surfaces, intact particles, no breakage, and good compression resistance. After three months of accelerated processing, the vitamin content retention rate in the tablets is high, with retention rates all above 98%.

[0117] Example 8 (*wall material, stabilizer and combination)

[0118] Based on the process parameters of Example 1, the effects of wall materials and stabilizers on the product were investigated in detail, and the results are shown in Table 5:

[0119] Table 5

[0120]

[0121] The results show that when different wall materials are used to prepare products, it is impossible to prepare products or the quality of the products obtained is very poor and unusable when the wall material is used alone to encapsulate high vitamin loads. When different wall materials are used with agar, or different wall materials are used with different stabilizers, only the combination described in the patent can produce qualified products.

[0122] Example 9 (*Selection of gelatin gel strength)

[0123] Based on the process of Example 1, the gelling strength of the gelatin was changed while other conditions remained unchanged. The main focus was on investigating the effect of the gelling strength of the wall material gelatin on the product performance. The results are shown in Table 6:

[0124] Table 6

[0125]

[0126] The results show that the gelatin gel strength in Example 1 of this invention has a significant impact on product preparation and final quality. Products with a gelatin gel strength of 180-250 Bloom g exhibit better emulsification, resulting in rounded particles with less surface oil and lower oil penetration. When the gelatin gel strength is below 180 Bloom g or above 250 Bloom g, the emulsification effect is poor, leading to incomplete emulsification or poor particle formation, which affects the product's encapsulation rate and breakage.

[0127] Example 10 (*Agar gel strength selection)

[0128] Based on the process of Example 1, the gel strength of the agar was changed while other conditions remained unchanged; the focus was on investigating the effect of the gel strength of the stabilizer agar in the invention on the product performance: the results are shown in Table 7:

[0129] Table 7

[0130]

[0131] The results show that the agar gel strength in Example 1 of this invention has a significant impact on product preparation and final quality. An agar gel strength of 1200-1600 g / cm³ was used. 2 The product emulsion emulsification effect is good, resulting in round particles with less surface oil and high tablet hardness. The agar gel strength is below 1200 g / cm³. 2 or higher than 1600g / cm 2 At this time, the emulsion emulsification effect of the product is poor, and there are problems such as incomplete emulsification or poor particle formation, which will affect the encapsulation rate and pressure resistance of the product.

[0132] Example 11 (*Selection of stabilizer to wall material ratio)

[0133] Based on the process of Example 1, the ratio of stabilizer to wall material was changed while other conditions remained unchanged; the focus was on investigating the effect of the stabilizer to wall material ratio on product performance: the results are shown in Table 8:

[0134] Table 8

[0135]

[0136] The results show that the ratio of stabilizer to wall material in Example 1 of this invention has a significant impact on product preparation and final quality. A stabilizer-to-wall material ratio of 0.01-0.1:1 results in better emulsification of the product emulsion, producing round particles with less surface oil and lower oil penetration. When the stabilizer-to-wall material ratio is below 0.01:1 or above 0.1:1, the emulsification effect is poor, leading to incomplete emulsification or poor particle formation, which affects the product's encapsulation rate and oil penetration rate.

[0137] Example 12 (*Selection of silica specific gravity)

[0138] Based on the process of Example 1, the specific gravity of silica was changed while other conditions remained unchanged. The main focus was on investigating the effect of the specific gravity of silica, the drying agent in the invention, on product performance. The results are shown in Table 9.

[0139] Table 9

[0140]

[0141] The results show that the specific gravity of silica in Example 1 of this invention has a significant impact on product preparation and final quality. Using silica with a specific gravity of 0.05-0.15 yields better preparation results, resulting in well-formed particles, high and stable content, and high tablet hardness. When the specific gravity of silica is below 0.05 or above 0.15, the product preparation process is not smooth, particle formation is poor, and the product content and pressure resistance are affected.

[0142] Example 13 (*Selection of silica particle size)

[0143] Based on the process of Example 1, the particle size of silica was changed while other conditions remained unchanged. The influence of the particle size of the silica drying agent in the invention on the product performance was investigated in detail. The results are shown in Table 10:

[0144] Table 10

[0145]

[0146]

[0147] The results show that the silica particle size in Example 1 of this invention has a significant impact on product preparation and final quality. Using silica particles with a D90 of 13-22 micrometers and a D99 of 25-36 micrometers resulted in better product preparation, producing well-formed particles with high and stable content, and high tablet hardness. When the silica particle size D90 was below 13 micrometers or D99 was above 36 micrometers, the product preparation process was not smooth, particle formation was poor, and the product content and compressive strength were affected.

[0148] Example 14 (*Solution pH selection)

[0149] Based on the process of Example 1, the pH of the solution was changed while other conditions remained unchanged. The effect of the pH of the wall material solution on the product was investigated in detail. The results are shown in Table 9:

[0150] Table 11

[0151]

[0152] The results show that the pH of the wall material solution in Example 1 of this invention has a significant impact on product preparation and final quality. When the pH of the wall material emulsion is between 5.5 and 6.8, the viscosity of the product wall material solution is moderate, resulting in well-formed particles with high and stable content and good stability. When the pH of the wall material emulsion is below 5.5 or above 6.8, the viscosity of the product wall material solution is unsuitable for particle preparation, resulting in poor particle formation and affecting the product content and stability.

[0153] Example 15 (*Emulsion viscosity)

[0154] Based on the process of Example 1, the emulsion viscosity was changed while other conditions remained unchanged. The effect of the wall material solution viscosity on the product was investigated in detail, and the results are shown in Table 12:

[0155] Table 12

[0156]

[0157] The results show that the emulsion viscosity in Example 1 of this invention has a significant impact on product preparation and final quality. A wall material emulsion viscosity between 1500-2500 MPa.s indicates a suitable product with good particle formation, low surface oil content, and high tablet hardness. Conversely, wall material emulsion viscosities below 1500 MPa.s or above 2500 MPa.s are unsuitable for particle preparation, resulting in poor particle formation and negatively affecting surface oil content and pressure resistance.

[0158] Example 16 (*Effect of different core materials in the preparation of fat-soluble vitamins)

[0159] Based on the process of Example 1, the fat-soluble vitamin was changed while other conditions remained unchanged. The focus was on the application effects of other fat-soluble vitamin products. The results are shown in Table 13:

[0160] The results show that, based on the process of Example 1 of this invention, a variety of fat-soluble vitamin products can be prepared, and all product indicators are qualified. All listed fat-soluble vitamins (including vitamin A acetate, vitamin A palmitate, dl-α-tocopherol, mixed tocopherol concentrate, vitamin K1, and vitamin K2) exist as free-flowing yellow or yellowish-brown particles. They exhibit fairly high vitamin loadings of 78.1%, 78.4%, 78.6%, 78.3%, 78.3%, and 78.2%, respectively. All fat-soluble vitamins have low surface oil content, with vitamin K1 having the lowest at 7.63% and dl-α-tocopherol the highest at 9.15%. Except for vitamin A acetate, whose tablet hardness is 235N, the tablet hardness of the other five fat-soluble vitamins is between 219N and 229N. Regarding oil penetration, except for the mixed tocopherol concentrate, which has a slightly higher penetration rate of 3.4%, the oil penetration rates of the other fat-soluble vitamins are between 2.2% and 3.1%. These fat-soluble vitamin microparticles maintain high stability, low surface oil content, and good pressure resistance while having a high oil loading capacity, making them suitable for various food and health product applications.

[0161] Table 13

[0162]

[0163] The above description is merely a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. A method for encapsulating high-loading fat-soluble vitamin microparticles, characterized in that: The raw material for the microparticles comprises the following components in parts by weight: Fat-soluble vitamins: 50-85 servings Wall material: 10-35 parts Stabilizer: 0.1-5 parts Drying agent: 1-10 parts; The wall material is selected from at least one of gum arabic and gelatin; the gel strength of the wall material measured in an aqueous solution with a mass fraction of 6.67% is 180-250 Bloom g; and the viscosity measured in an aqueous solution with a mass fraction of 6.67% at a temperature of 60°C is 10-30 mPa·s. The stabilizer is agar; the gel strength of the stabilizer in an aqueous solution with a mass fraction of 1.5% at a temperature of 20°C is 1200-1600 g / cm³. 2 The weight ratio of the stabilizer to the wall material is 0.01-0.1:

1. The drying agent is selected from at least one of calcium silicate, silicon dioxide, tricalcium phosphate, talc, and corn starch; the specific gravity of the drying agent is 0.05-0.

15. Its preparation method includes the following steps: (1) Take 10-35 parts by weight of wall material and put it into room temperature water. After it absorbs water and swells, heat it to dissolve it completely and adjust the pH to between 5.5 and 6.

8. (2) Take 60-85 parts by weight of fat-soluble vitamins and heat them under light-protected and nitrogen-protected conditions to obtain a free-flowing oily liquid; (3) Add step (2) to step (1), emulsify and homogenize twice under light-proof and nitrogen-protected conditions, and control the emulsion viscosity at 1500-2500 mPa.s; (4) Disperse the stabilizer completely in water, heat until completely dissolved, and then cool. (5) Add step (4) to step (3), stir evenly, and spray the emulsion into the environment with the drying agent to obtain dried granules.

2. The microparticles according to claim 1, characterized in that: The raw material for the microparticles comprises the following components in parts by weight: Fat-soluble vitamins: 65-85 servings Wall material: 15-20 parts Stabilizer: 0.15-2 parts Drying agent: 2-5 parts.

3. The microparticles according to claim 1, characterized in that: The fat-soluble vitamin is selected from at least one of vitamin A acetate, vitamin A palmitate, d-α-tocopherol, dl-α-tocopherol, d-α-tocopherol acetate, dl-α-tocopherol acetate, vitamin K1, and vitamin K2.

4. The microparticles according to claim 1, characterized in that: The fat-soluble vitamin is a tocopherol d-α-acetate concentrate or a mixed tocopherol concentrate.

5. The microparticles according to claim 1, characterized in that: When the drying agent is silicon dioxide, its particle size is 13 micrometers < D90 < 22 micrometers; and its particle size is 25 micrometers < D99 < 36 micrometers.

6. The microparticle according to claim 1, characterized in that: The wall material has a transmittance of not less than 60% under light with a wavelength of 450 nanometers.

7. The microparticles according to claim 1, characterized in that: The wall material has a transmittance of not less than 80% under light with a wavelength of 620 nanometers.

8. The method for preparing high-loading fat-soluble vitamin microparticles as described in claim 1, characterized in that: Includes the following steps: (1) Take 10-35 parts by weight of wall material and put it into room temperature water. After it absorbs water and swells, heat it to dissolve it completely and adjust the pH to between 5.5 and 6.

8. (2) Take 60-85 parts by weight of fat-soluble vitamins and heat them under light-protected and nitrogen-protected conditions to obtain a free-flowing oily liquid; (3) Add step (2) to step (1), emulsify and homogenize twice under light-proof and nitrogen-protected conditions, and control the emulsion viscosity at 1500-2500 mPa.s; (4) Disperse the stabilizer completely in water, heat until completely dissolved, and then cool. (5) Add step (4) to step (3), stir evenly, and spray the emulsion into the environment with the drying agent to obtain dried granules.

9. The method according to claim 8, characterized in that: The temperature of step (1) is 45-70℃, the temperature of step (2) is 60-65℃, the heating temperature of step (4) is 95-98℃, the cooling temperature of step (4) is 60-65℃, and the homogenization conditions of step (3) are a primary homogenization pressure of 20-25MPa and a secondary homogenization pressure of 45-55MPa.

10. The application of the encapsulation of high-loading fat-soluble vitamin microparticles as described in claim 1, characterized in that, The application area is food.

11. The application of encapsulating high-loading fat-soluble vitamin microparticles as described in claim 1, characterized in that, The application area is health food.

12. The application according to any one of claims 10 or 11, characterized in that, Dosage forms include powders, granules, capsules, or tablets.

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