Vitamin A microcapsule and preparation method thereof

Abstract

The invention relates to the technical field of vitamin A micro-capsule production, in particular to a vitamin A micro-capsule and a preparation method thereof. Research finds that the roundness of the vitamin A micro-capsule prepared by the emulsion through a spray drying process can be controlled by controlling the size of a relational expression 0.88 * ln (Q) + 0.12 * e (-0.002 mu) * (N / 1000) 0.18-0.05 * Te-120 + 0.1 * (epsilon / 2.4) 0.5, the relational expression obtained through parameter calculation of the spray drying process is controlled to be 50% or above, the vitamin A micro-capsule with the roundness being 50% or above can be obtained, and the vitamin A micro-capsule with the roundness being 50% or above can be used for preparing the vitamin A micro-capsule with the roundness being 50% or above. The roundness of the vitamin A micro-capsule is remarkably improved, so that the situation that the micro-capsule is released too early in gastric juice is improved, the intestinal targeting property is improved, meanwhile, the situation that the micro-capsule is degraded in the storage period is improved, and the stability of the micro-capsule is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of vitamin A microcapsule production, and in particular to a vitamin A microcapsule and a preparation method thereof. Background Art

[0002] Vitamin A is a fat-soluble vitamin derivative with core physiological functions, including maintaining visual function, promoting epithelial tissue health, enhancing immunity, and supporting bone development. It is widely used in food, health supplements, pharmaceuticals, and feed. In the food industry, it is added as a nutritional supplement to infant formula, dairy products, and beverages; in pharmaceuticals, it is used to treat vitamin A deficiency and in skin repair preparations; and in animal feed, it is used as a growth promoter. Vitamin A is not a single compound, but rather a series of retinol derivatives, including retinol, retinaldehyde, retinoic acid, retinyl acetate, and retinyl palmitate. However, these substances are chemically unstable and easily degraded by factors such as light, oxygen, and heat, resulting in loss of activity. Traditionally, vitamin A acetate, due to its oily form, is difficult to evenly disperse, requiring microencapsulation to improve its water solubility and stability, thereby expanding its application.

[0003] The roundness of microcapsules (also called microcapsules) is a key indicator that determines their performance. In the existing technology, microcapsules with insufficient roundness are prone to surface defects (such as depressions or wrinkles), leading to the following problems: (1) Decreased stability: irregular shapes increase the specific surface area, accelerate oxygen penetration, and trigger the oxidative degradation of vitamin A. The monthly degradation rate in the 37°C accelerated test can exceed 5%; (2) Poor mixing uniformity: downstream customers (such as food or feed manufacturers) need to mix microcapsules with other powders. Uneven shapes can easily lead to stratification or agglomeration, affecting the quality of the final product; (3) Deterioration of controlled release performance: low roundness may destroy the integrity of the wall material, leading to premature release in gastric fluid (>10%) and reduced intestinal targeting efficiency. Therefore, improving roundness is crucial for the commercial application of products. Summary of the Invention

[0004] Therefore, the technical problem to be solved by the present invention is to overcome the defect of low roundness of vitamin A microcapsules in the prior art, thereby providing a vitamin A microcapsule and a preparation method thereof.

[0005] To this end, the present application provides a method for preparing vitamin A microcapsules, comprising spray drying an emulsion containing vitamin A to prepare vitamin A microcapsules; wherein, during the spray drying process, the atomizer speed N rpm, the emulsion viscosity μmPa·s, the inlet air temperature Te°C, the inlet air speed εm / s, and the motion coefficient Q satisfy the following relationship:

[0006] 0.88×ln(Q)+0.12×e^(-0.002μ)×(N / 1000)^0.18-0.05×|Te-120|+0.1×(ε / 2.4)^0.5≥50% (e.g., 50%-100%, 50%-98%, 60%-99%, or 70%-99.9%);

[0007] The kinetic coefficient Q is calculated by the emulsion density ρg / mL, the feed rate υmL / min, and the atomizer aperture αmm according to the following formula: Q=ρ×υ / α.

[0008] The emulsion viscosity refers to the viscosity measured by a viscometer at the feed temperature.

[0009] |Te-120| represents the absolute value of Te-120.

[0010] Furthermore, the feed temperature of the emulsion is 50°C-80°C.

[0011] Furthermore, 18000≤N≤25000, 50≤μ≤1000, 100≤Te≤140, 1.5≤ε≤3.0, 1.8≤Q≤3.2; preferably, 18000≤N≤23000, 50≤μ≤200, 120≤Te≤130, 1.8≤ε≤2.5, 2.2≤Q≤3.0.

[0012] Further,

[0013] 80%≤0.88×ln(Q)+0.12×e^(-0.002μ)×(N / 1000)^0.18-0.05×|Te-120|+

[0014] 0.1×(ε / 2.4)^0.5≤100%, preferably

[0015] 95%≤0.88×ln(Q)+0.12×e^(-0.002μ)×(N / 1000)^0.18-0.05×|Te-120|+

[0016] 0.1×(ε / 2.4)^0.5≤99.8%.

[0017] Furthermore, 0.5≤υ≤1.5, 0.4≤α≤2.0, 0.5≤ρ≤1.5; preferably, 1.1≤υ≤1.5, 0.5≤α≤1.2, 0.9≤ρ≤1.2.

[0018] Furthermore, the vitamin A is selected from one or more of retinol, retinoic acid, retinyl esters or retinal; optionally, the retinyl esters include vitamin A acetate.

[0019] Furthermore, the preparation method of the vitamin A-containing emulsion comprises:

[0020] Step S1: dissolving the wall material in water to obtain an aqueous phase; heating vitamin A to obtain an oil phase;

[0021] Step S2: Mix the water phase and the oil phase to form an emulsion containing vitamin A.

[0022] Furthermore, the wall material includes protein. Optionally, the wall material includes one or more of zein, prolamin, rice gluten, gliadin, hordein, kafirin, and vicilin.

[0023] Furthermore, in step S1, the aqueous phase is prepared by dissolving the antioxidant enzyme and the wall material in water simultaneously or successively to obtain the aqueous phase; and / or, the step of mixing an oil-soluble antioxidant with vitamin A before the vitamin A is heated is also included;

[0024] Furthermore, the antioxidant enzyme includes one or more of superoxide dismutase, catalase, and glutathione peroxidase.

[0025] Furthermore, the mass ratio of antioxidant enzyme to vitamin A is 0.2-0.8:20-65.5.

[0026] Furthermore, the oil-soluble antioxidant includes one or more of purple sweet potato proanthocyanidins, phycocyanin, and carnosic acid;

[0027] Furthermore, the mass ratio of the oil-soluble antioxidant to vitamin A is 10-40:20-65.5.

[0028] Furthermore, in the vitamin A microcapsule, the mass ratio of the wall material to vitamin A is 20-50:20-65.5.

[0029] Furthermore, in step S1, the step of dissolving the antioxidant enzyme and the wall material in water simultaneously or successively to prepare the aqueous phase also includes the step of mixing the oil-soluble antioxidant with the vitamin A before the vitamin A is heated.

[0030] Furthermore, in step S1, the mass ratio of water to vitamin A is 1200-1500:20-65.5.

[0031] Furthermore, the wall material is zein, the antioxidant enzyme is superoxide dismutase, and the oil-soluble antioxidant is phycocyanin.

[0032] Furthermore, the preparation method of the vitamin A-containing emulsion comprises:

[0033] Step S1: dissolving zein and superoxide dismutase in water to obtain an aqueous phase; mixing vitamin A and phycocyanin, and heating to obtain an oil phase;

[0034] Step S2: Mix the water phase and the oil phase to form an emulsion containing vitamin A.

[0035] Furthermore, the vitamin A microcapsules include, by weight, 30-40 parts of zein, 20-30 parts of vitamin A acetate, 0.3-0.5 parts of superoxide dismutase and 30-40 parts of phycocyanin.

[0036] Furthermore, the dissolution temperature during the preparation of the aqueous phase is 20°C-75°C; and / or, the heating treatment temperature during the preparation of the oil phase is 50°C-80°C; and / or, in step S2, the mixing temperature of the aqueous phase and the oil phase is 50°C-80°C, and the stirring rate is 800-1500 rpm.

[0037] The present invention also provides vitamin A microcapsules prepared by any of the above-mentioned methods for preparing vitamin A microcapsules.

[0038] The present invention also provides a food or feed composition comprising the vitamin A microcapsules prepared by any of the above-mentioned methods for preparing the vitamin A microcapsules.

[0039] The technical solution of the present invention has the following advantages:

[0040] 1. The present invention provides a method for preparing vitamin A microcapsules, comprising spray-drying an emulsion containing vitamin A to prepare the vitamin A microcapsules; wherein, during the spray-drying process, the atomizer speed N rpm, the emulsion viscosity μmPa·s, the inlet air temperature Te°C, the inlet air speed εm / s, and the kinetic coefficient Q satisfy the following relationship: 0.88×ln(Q)+0.12×e^(-0.002μ)×(N / 1000)^0.18-0.05×|Te-120|+0.1×(ε / 2.4)^0.5≥50%; wherein the kinetic coefficient Q is calculated using the emulsion density ρg / mL, the feed rate υmL / min, and the atomizer aperture αmm according to the following formula: Q=ρ×υ / α. The study found that by controlling the size of the relationship 0.88×ln(Q)+0.12×e^(-0.002μ)×(N / 1000)^0.18-0.05×|Te-120|+0.1×(ε / 2.4)^0.5, it can be used to control the roundness of vitamin A microcapsules prepared by the spray drying process of the emulsion. The above relationship obtained by calculating the parameters of the spray drying process can obtain vitamin A microcapsules with a roundness of more than 50%, which significantly improves the roundness of the vitamin A microcapsules, thereby improving the premature release of the microcapsules in gastric juice, improving intestinal targeting, and at the same time improving the degradation of the microcapsules during storage, thereby improving their stability. In addition, it is convenient for vitamin A microcapsules to mix well when compounded with other materials, and it is not easy to stratify or agglomerate, thereby ensuring the quality of food or feed products.

[0041] 2. The preparation method of vitamin A microcapsules provided by the present invention can further improve the roundness of the microcapsules by controlling 18000≤N≤25000, 50≤μ≤1000, 100≤Te≤140, 1.5≤ε≤3.0, 1.8≤Q≤3.2; in particular, 18000≤N≤23000, 50≤μ≤200, 120≤Te≤130, 1.8≤ε≤2.5, 2.2≤Q≤3.0.

[0042] By controlling 0.5≤υ≤1.5, 0.4≤α≤2.0, 0.5≤ρ≤1.5; especially controlling 1.1≤υ≤1.5, 0.5≤α≤1.2, 0.9≤ρ≤1.2, the motion coefficient Q can be better controlled to obtain vitamin A microcapsules with higher roundness.

[0043] 3. The preparation method of vitamin A microcapsules provided by the present invention, wherein the wall material includes protein, and in step S1, the preparation of the aqueous phase is a step of dissolving the antioxidant enzyme and the wall material in water simultaneously or successively to obtain the aqueous phase; and / or, before the vitamin A is heated, the step of mixing an oil-soluble antioxidant with the vitamin A is also included; by using a protein wall material, combining the antioxidant enzyme to form a hydrogen bond antioxidant network and using an oil-soluble antioxidant in the oil phase, and combining the relationship (I) obtained by controlling various parameters in the spray drying process to be controlled to above 50%, the degradation rate of the vitamin A microcapsules is further reduced, and its stability and intestinal targeting are improved.

[0044] 4. The preparation method of vitamin A microcapsules provided by the present invention, which uses zein, superoxide dismutase and phycocyanin in combination to prepare vitamin A microcapsules with significantly improved stability and intestinal targeting.

[0045] 5. The present invention provides a method for preparing vitamin A microcapsules. The vitamin A microcapsules include, by weight, 30-40 parts of zein, 20-30 parts of vitamin A acetate, 0.3-0.5 parts of antioxidant enzymes, and 30-40 parts of oil-soluble antioxidants. The vitamin A microcapsules prepared by using zein, superoxide dismutase, and phycocyanin in a specific ratio not only have a significantly improved encapsulation efficiency, but also can better adapt to the control of various parameters in the spray drying process, solving the problem of balancing the roundness and encapsulation efficiency of vitamin A microcapsules. The vitamin A microcapsules are particularly suitable for the efficient encapsulation and intestinal targeted delivery of heat-sensitive active ingredients, and have significant prospects for industrial application. DETAILED DESCRIPTION

[0046] The following examples are provided for a better understanding of the present invention and are not intended to limit the best mode of implementation. They do not limit the content and scope of protection of the present invention. Any product identical or similar to the present invention obtained by anyone under the guidance of the present invention or by combining the features of the present invention with other prior arts shall fall within the scope of protection of the present invention.

[0047] If no specific experimental steps or conditions are specified in the examples, the conventional experimental steps or conditions described in the literature in this field can be used. If the manufacturer of the reagents or instruments is not specified, they are all commercially available conventional reagents.

[0048] Examples 1 to 18

[0049] (1) Example 1 provides a method for preparing vitamin A microcapsules, comprising the following steps:

[0050] 1) Aqueous phase preparation: Weigh 356 g of zein and 5 g of superoxide dismutase, dissolve in 1200 g of water, and heat in a water bath at 28 ± 2°C while stirring to dissolve the solids for 50 min.

[0051] 2) Oil phase preparation step: Place 265 g of vitamin A acetate crystals and 374 g of phycocyanin in a three-well flask and heat to dissolve in a 62°C oil bath for 50 min.

[0052] 3) Emulsion preparation step: The aqueous phase and the oil phase were stirred and mixed using a stirrer at a temperature of 62° C., a stirring speed of 1200 rpm, and a mixing time of 50 min;

[0053] 4) Spray drying step: The spray drying parameters were set according to Table 1: the emulsion was kept at 62°C, water was added to the emulsion to adjust the viscosity of the emulsion at 62°C to 50 mPa·s, and the emulsion density was measured to be 0.91 g / mL; the atomization speed was 18,000 rpm, the feed flow rate was 1 mL / min, the inlet air velocity was 1.8 m / s, an atomizer with a pore size of 0.5 mm was selected, the inlet air temperature was 120°C, the emulsion was fed through a peristaltic pump while being kept at 62°C, and spray dried to obtain vitamin A microcapsules, which were recorded as Sample 1.

[0054] Examples 2 to 18 respectively used the above method to prepare the remaining 17 batches of vitamin A microcapsules according to the parameters in Table 1. The only difference was the parameters of the spray drying step, which were recorded as samples 2 to 18. During the preparation of samples 1 to 18, the parameters of the spray drying step were shown in Table 1.

[0055] Table 1 Spray drying parameters

[0056] Sample number N μ υ α ε Te Q ρ 1 18,000 50 1 0.5 1.8 120 1.8 0.89 2 18,000 150 1.1 0.5 2.2 120 2 0.92 3 18,000 200 1.2 0.5 2.5 120 2.3 0.97 4 22,000 50 1 0.45 2.5 125 2 0.88 5 22,000 150 1.1 0.45 1.8 125 2.3 0.96 6 22,000 200 1.2 0.45 2.2 125 2.6 0.99 7 25,000 50 1.1 0.44 2.2 130 2.3 0.90 8 25,000 150 1.2 0.44 2.5 130 2.6 0.94 9 25,000 200 1 0.44 1.8 130 2.3 0.99 10 18,000 50 1.2 0.5 1.8 120 2.2 0.91 11 18,000 150 1 0.5 2.2 120 1.9 0.95 12 18,000 200 1.1 0.5 2.5 120 2.2 0.99 13 22,000 50 1.1 0.45 1.8 125 2.2 0.90 14 22,000 150 1.2 0.45 2.5 125 2.6 0.96 15 22,000 200 1 0.45 2.2 125 2.2 1 16 25,000 50 1.2 0.44 2.2 130 2.4 0.88 17 25,000 150 1 0.44 2.5 130 2.2 0.95 18 25,000 200 1.1 0.44 1.8 130 2.5 0.98

[0057] (2) Test roundness

[0058] The roundness test was performed on the above samples 1 to 18 respectively. The test method is as follows:

[0059] Sample preparation: Take the spray-dried microcapsule sample and disperse it on a glass slide to avoid particle overlap. Use a scanning electron microscope (SEM) to take clear images of at least 100 microcapsules.

[0060] Image processing: Import the image into image analysis software (such as ImageJ), extract the microcapsule outline by grayscale threshold segmentation, and calculate the projected area (A) and perimeter (P) of each particle.

[0061] Sphericity calculation: The sphericity index is calculated according to the formula SI = 4πA / P2. The closer the SI value is to 1, the closer the particle is to an ideal sphere.

[0062] Data verification: Each group of samples was tested three times and the average value was taken as the final result to ensure that the test error was ≤1%.

[0063] Calculation of the measured value of roundness ω: The measured value of roundness was calculated according to the formula ω = sphericity × 100%. The results are shown in Table 2.

[0064] Calculate the ω measured for samples 1-18 and the calculated The relative deviation is shown in Table 2 below.

[0065] Table 2 Relative deviation results

[0066]

[0067]

[0068] (3) Calculation of roundness

[0069] Based on 18 sets of experimental data and multiple nonlinear regression, a preliminary Mathematical relationship with Q, N, μ, Te, ε: The interaction term (e^(cμ)×(N / d)^e) is introduced to describe the coupling effect between N and μ. The prediction equation obtained by least squares fitting is: R2≥0.95. The predicted value of roundness was calculated based on this formula, and the results are shown in Table 2.

[0070] (4) Relative deviation

[0071] The relative deviation between the predicted value of roundness and the measured value of roundness is calculated. The results are shown in Table 2. The roundness actually tested is basically consistent with the result calculated by the method of the present invention, with a relative deviation of <5%.

[0072] From the results, it can be seen that compared with other samples, the roundness of the microcapsules prepared from samples 3, 10 and 12 reaches more than 90%, especially in the preparation process of sample 3, the roundness is higher by limiting each parameter within the preferred range.

[0073] Example 19

[0074] This embodiment provides a method for preparing vitamin A microcapsules, comprising the following steps:

[0075] (1) Preparation of aqueous phase: Weigh 392 g of zein and 3 g of superoxide dismutase, dissolve in 1500 g of water, keep the water warm in a water bath at 50 ± 2 °C, and dissolve by stirring for 45 min;

[0076] (2) Oil phase preparation step: Place 300 g of vitamin A acetate crystals and 305 g of phycocyanin in a three-well plate and heat in a 75°C oil bath to dissolve for approximately 45 min.

[0077] (3) Emulsion preparation step: The aqueous phase and the oil phase were mixed using a stirrer at 62°C, with a stirring speed of 1000 rpm and a mixing time of 40 min;

[0078] (4) Spray drying step: The spray drying parameters were the same as those used in the preparation of sample 10.

[0079] Example 20

[0080] This example provides a method for preparing vitamin A microcapsules, which is basically the same as that of Example 3, except that the same mass of catalase is used instead of superoxide dismutase.

[0081] Example 21

[0082] This embodiment provides a method for preparing vitamin A microcapsules, which is basically the same as that of Example 3, except that the same mass of carnosic acid is used instead of phycocyanin.

[0083] Example 22

[0084] This example provides a method for preparing vitamin A microcapsules, which is basically the same as Example 3, except that the amounts of certain raw materials are different. Specifically, in this example, the amount of zein is adjusted to 200 g, the amount of superoxide dismutase is adjusted to 2 g, and the amount of vitamin A acetate crystals is adjusted to 400 g; the remaining operations and process conditions are the same as Example 3.

[0085] Example 23

[0086] This example provides a method for preparing vitamin A microcapsules, which is basically the same as that of Example 3, except that superoxide dismutase is not added in step (1).

[0087] Example 24

[0088] This embodiment provides a method for preparing vitamin A microcapsules, which is basically the same as that of Example 3, except that phycocyanin is not added in step (2).

[0089] Experimental Example 1 Test Encapsulation Efficiency

[0090] 1. The roundness of the vitamin A microcapsules prepared in Examples 19-24 was tested separately using the same testing method as item (2) of Example 1, and the results were compared with those of Samples 1-3 and Samples 10-13.

[0091] 2. The encapsulation efficiency of the vitamin A microcapsules prepared from samples 1-3, samples 10-13, and examples 19-24 was tested using the following method:

[0092] Sample treatment: Take 0.5 g of microcapsule sample, extract it with 50 mL of ethanol, and take the supernatant to obtain the test solution 1.

[0093] Take 0.5 g of microcapsule sample, add 25 mL of purified water to dissolve, then add 25 mL of ethanol and mix well to obtain test solution 2;

[0094] Content determination: Take test solution 1 and test solution 2, respectively, and use high performance liquid chromatography (HPLC) to determine the content of vitamin A acetate (respectively recorded as C1 and C2). Chromatographic conditions: C18 column, mobile phase methanol-water (volume ratio of 90:10), detection wavelength of 325nm, column temperature: 27℃, flow rate of 0.5mL / min.

[0095] Encapsulation efficiency calculation: Encapsulation efficiency was calculated using the following formula: Encapsulation efficiency = (C2 - C1 / C2) × 100%. Repeat verification: Each group of samples was tested three times in parallel, and the average value was taken to ensure that the error was ≤ 1%.

[0096] Table 3 Encapsulation efficiency results

[0097] project ω(%) Encapsulation efficiency (%) Sample 1 77.6 90.1 Sample 2 84.3 91.3 Sample 3 99.8 98.7 Sample 10 95.2 98.7 Sample 11 85.2 91.2 Sample 12 90.1 91.5 Sample 13 71.3 96.4 Example 19 95.5 99.1 Example 20 99.7 98.5 Example 21 99.3 98.5 Example 22 99.7 97.7 Example 23 99.5 97.1 Example 24 99.3 98.4

[0098] As can be seen from the results in Table 3, the vitamin A microcapsule samples prepared in the present invention have high roundness and good encapsulation efficiency, with the encapsulation efficiency reaching more than 90%. In particular, the vitamin A microcapsules prepared in Sample 3 and Examples 20-24 have a roundness of more than 99% and an encapsulation efficiency of more than 97%.

[0099] Experimental Example 2

[0100] Sample 3 obtained in Example 3 and the microcapsules prepared in Examples 19-24 were tested with commercially available products A and B as follows:

[0101] 1. pH-responsive release characteristics

[0102] Gastric digestive fluid: Take 16.4 mL of concentrated hydrochloric acid, add 800 mL of water, mix evenly with 10 g of pepsin, and dilute to 1000 mL to obtain gastric digestive fluid;

[0103] Intestinal digestive fluid: Take 6.8 g of potassium dihydrogen phosphate, add 500 mL of water to dissolve it, and adjust the pH value to 6.8 with 0.1 mol / L sodium hydroxide solution; take another 10 g of pancreatic enzyme, add 100 mL of water to dissolve it, mix the two liquids and dilute with water to 1000 mL.

[0104] The content of vitamin A acetate in the vitamin A acetate microcapsules was tested using high performance liquid chromatography. 0.5 g of the sample was weighed and dissolved in 50 mL of 50% by volume ethanol aqueous solution. The mixture was mixed and tested after homogeneity. The chromatographic conditions were the same as those in Experimental Example 1. The content of vitamin A acetate in the initial microcapsules was obtained, and the mass of vitamin A acetate in 10 g of the initial microcapsules was calculated.

[0105] Take 10 g of the microcapsule sample, add 100 mL of the prepared gastric digestive fluid, place it in a shaker at 37°C and shake for 2 hours. After digestion is complete, centrifuge the sample at a centrifugal speed of 5000 r / min, remove the supernatant, add 100 mL of intestinal digestive fluid to the lower layer of chyme, place it in a shaker at 37°C and shake for 45 minutes. After digestion is complete, centrifuge the sample at a centrifugal speed of 5000 r / min, remove the supernatant, and dissolve the chyme in 100 mL of 50% volume ethanol aqueous solution. Use high performance liquid chromatography to test the content of vitamin A acetate in the sample. The chromatographic conditions are the same as those in Experimental Example 1. Calculate the total mass of vitamin A acetate in the chyme.

[0106] Digestibility = (mass of vitamin A acetate in the initial microcapsules - mass of vitamin A acetate in the chyme) / mass of vitamin A acetate in the initial microcapsules × 100%.

[0107] 2. Stability

[0108] The microcapsule samples to be tested were stored at 40°C / 75% RH for 3 months. The content of vitamin A microcapsules in the microcapsules before and after storage was tested, and the retention rate was calculated according to the following formula: retention rate = content of vitamin A acetate in the microcapsules after 3 months of storage / content of vitamin A acetate in the microcapsules before 3 months of storage × 100%.

[0109] The results are shown in Table 4 below.

[0110] Table 4 Release characteristics and stability results

[0111] project Release rate in intestinal fluid 45min / % Retention rate / % Example 3 96.5 97.5 Example 19 93.3 94.0 Example 20 96.2 96.4 Example 21 96.3 96.9 Example 22 95.6 94.4 Example 23 96.5 93.8 Example 24 96.1 94.0 Commercially available product A 87.5 86.5 Commercially available product B 88.4 93.3

[0112] The results showed that compared with commercially available products, the intestinal release rate and retention rate of the microcapsules prepared in each embodiment of the present invention were significantly improved. Compared with Example 19, Example 3 improved the intestinal targeting ability and stability by improving the roundness. Compared with Examples 19-24, Example 3 further improved the intestinal targeting ability and stability by optimizing the formula composition of the vitamin A microcapsules.

[0113] Obviously, the above embodiments are merely examples for clarity of explanation and are not intended to limit the implementation methods. Those skilled in the art will readily appreciate that other variations or modifications based on the above descriptions are possible. It is not necessary and impossible to enumerate all implementation methods here. Obvious variations or modifications arising therefrom remain within the scope of protection of the present invention.

Claims

1. A method for preparing vitamin A microcapsules, characterized in that: The method comprises spray drying an emulsion containing vitamin A to prepare vitamin A microcapsules; wherein, during the spray drying process, the following relationship is satisfied between the atomizer speed N rpm, the emulsion viscosity μmPa·s, the inlet air temperature Te°C, the inlet air speed εm / s and the motion coefficient Q: 0.88×ln(Q)+0.12×e^(-0.002μ)×(N / 1000)^0.18-0.05×|Te-120|+0.1×(ε / 2.4)^0.5≥50%; The kinetic coefficient Q is calculated by the emulsion density ρg / mL, the feed rate υmL / min, and the atomizer aperture αmm according to the following formula: Q=ρ×υ / α.

2. The method for preparing vitamin A microcapsules according to claim 1, wherein 18000≤N≤25000, 50≤μ≤1000, 100≤Te≤140, 1.5≤ε≤3.0, 1.8≤Q≤3.2; preferably, 18000≤N≤23000, 50≤μ≤200, 120≤Te≤130, 1.8≤ε≤2.5, 2.2≤Q≤3.

0.

3. The method for preparing vitamin A microcapsules according to claim 1, wherein 80%≤0.88×ln(Q)+0.12×e^(-0.002μ)×(N / 1000)^0.18-0.05×|Te-120|+0.1×(ε / 2.4)^0.5≤100%, excellent Choose 95%≤0.88×ln(Q)+0.12×e^(-0.002μ)×(N / 1000)^0.18-0.05×|Te-120|+0.1×(ε / 2.4)^0.5≤99.8%.

4. The method for preparing vitamin A microcapsules according to claim 1, wherein 0.5≤υ≤1.5, 0.4≤α≤2.0, 0.5≤ρ≤1.5; preferably, 1.1≤υ≤1.5, 0.5≤α≤1.2, 0.9≤ρ≤1.

2.

5. The method for preparing vitamin A microcapsules according to any one of claims 1 to 4, characterized in that: The vitamin A is selected from one or more of retinol, retinoic acid, retinyl esters or retinal; optionally, the retinyl esters include vitamin A acetate.

6. The method for preparing vitamin A microcapsules according to any one of claims 1 to 5, characterized in that: The preparation method of the vitamin A-containing emulsion comprises: Step S1: dissolving the wall material in water to obtain an aqueous phase; heating vitamin A to obtain an oil phase; Step S2: mixing the aqueous phase and the oil phase to obtain an emulsion containing vitamin A; preferably, the preparation method further satisfies one or more of the following conditions A to D: A. The wall material comprises protein. Optionally, the wall material is selected from one or more of zein, prolamin, rice gluten, gliadin, hordein, kafirin, and vicilin; In steps B and S1, the aqueous phase is prepared by dissolving the antioxidant enzyme and the wall material in water simultaneously or successively to obtain the aqueous phase; and / or, the step of mixing an oil-soluble antioxidant with the vitamin A before the vitamin A is heated is also included; Optionally, the antioxidant enzyme includes one or more of superoxide dismutase, catalase, and glutathione peroxidase; Optionally, the mass ratio of antioxidant enzyme to vitamin A is 0.2-0.8:20-65.5; Optionally, the oil-soluble antioxidant includes one or more of purple sweet potato proanthocyanidins, phycocyanin, and carnosic acid; Optionally, the mass ratio of the oil-soluble antioxidant to vitamin A is 10-40:20-65.5; C. In vitamin A microcapsules, the mass ratio of wall material to vitamin A is 20-50:20-65.5; D. In step S1, the mass ratio of water to vitamin A is 1200-1500:20-65.

5.

7. The method for preparing vitamin A microcapsules according to claim 6, characterized in that: The wall material is zein, the antioxidant enzyme is superoxide dismutase, and the oil-soluble antioxidant is phycocyanin; preferably, based on weight, the vitamin A microcapsules include 30-40 parts of zein, 20-30 parts of vitamin A acetate, 0.3-0.5 parts of antioxidant enzyme and 30-40 parts of oil-soluble antioxidant.

8. The method for preparing vitamin A microcapsules according to claim 6 or 7, characterized in that: The dissolution temperature during the preparation of the aqueous phase is 20°C-75°C; and / or, the heating temperature during the preparation of the oil phase is 50°C-80°C; and / or, in step S2, the temperature of mixing the aqueous phase and the oil phase is 50°C-80°C, and the stirring rate is 800-1500 rpm.

9. Vitamin A microcapsules prepared by the method for preparing vitamin A microcapsules according to any one of claims 1 to 8.

10. A food or feed composition, characterized in that The vitamin A microcapsules are prepared by the method for preparing the vitamin A microcapsules according to any one of claims 1 to 8.

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