Vitamin premix and preparation process thereof

Abstract

The present invention provides a vitamin premix and a preparation process thereof, and belongs to the technical field of food additives, the preparation process is as follows: fat-soluble vitamin mixed particles, mixed water-soluble vitamins and mixed minerals are added into a mixer for mixing, then vitamin C, magnesium taurate, amino acids and tricalcium phosphate are added for continuous mixing, and sieving is performed to obtain the vitamin premix. Wherein the fat-soluble vitamin mixed particles comprise the following raw materials: vitamin A, vitamin E acetate, vitamin D3, vitamin K2, Arabic gum, modified protein and beta-cyclodextrin; the mixed water-soluble vitamins comprise the following raw materials: vitamin B1, vitamin B2, vitamin B5, vitamin B12, folic acid and nicotinamide; the mixed mineral substance comprises the following raw materials: ferrous glycinate, calcium citrate, magnesium citrate and zinc glycinate. The vitamin premix prepared by the invention can be used as a nutritional supplement in various foods, is convenient to use, and has good stability and mixing uniformity.

Description

Technical Field

[0001] The present invention belongs to the technical field of food additives, and particularly relates to a vitamin premix and a preparation process thereof. Background Art

[0002] A vitamin premix is a food additive that precisely mixes and evenly blends various vitamins, minerals, amino acids and other nutritional amino acids in scientific proportions, aiming to provide comprehensive nutritional support for foods or nutritional supplements. With the development of the modern food industry, people's demand for nutritional balance is increasing day by day, and the problem of nutrient loss caused by processing, cooking or partial eating in traditional diets is becoming more and more prominent. The emergence of vitamin premixes effectively solves the cumbersome process of adding single nutrients in food processing, helps food producers simplify production processes, and at the same time ensures the stability and consistency of nutritional components. Its core advantage lies in the ability to accurately control the addition amount of micronutrients, avoiding over - addition or under - addition. Especially in the fields of formula milk powder, fortified foods and nutritional supplements, vitamin premixes can significantly improve the nutritional value and market competitiveness of products. In addition, its standardized production mode reduces the complexity of raw material procurement and storage, and reduces the quality risks caused by improper operation, becoming an indispensable key technical support for the modern healthy food industry.

[0003] Currently, the preparation of vitamin premixes mainly relies on traditional processes such as physical mixing, granulation and microencapsulation. Among them, the physical mixing method is the most common means, which directly mixes raw material powders. However, due to the significant differences in the particle size, density and electrostatic properties of different components, it is easy to cause uneven mixing. Especially for active ingredients with extremely low contents (such as fat - soluble vitamins) or moisture - absorbing minerals (such as iron and zinc), local enrichment or stratification phenomena are very likely to occur, affecting the uniformity and stability of the final product. Although granulation technology can improve fluidity and dispersibility, the high - temperature and high - humidity environment may damage the activity of heat - sensitive vitamins (such as vitamin C), and uneven particle sizes will still reduce the absorption efficiency. In addition, although microencapsulation technology can encapsulate nutrients to improve stability, the process is complex, costly, and the release rate is difficult to accurately control. These technical bottlenecks make vitamin premixes still face problems such as quality fluctuations, low bioavailability and poor taste in practical applications, restricting their further development in the field of high - end nutritional products.

[0004] In view of the deficiencies of traditional processes, attempts have been made to improve the performance of premixes through means such as new carrier technologies, nano-dispersion, and intelligent encapsulation. For example, using high-fat carriers as stable carriers for vitamins can effectively protect fat-soluble components and improve taste; nano-particle technology enhances dispersion by reducing particle size; layered encapsulation technology can achieve gradient release of components and improve utilization. However, these improvements also have limitations: high-fat carriers may affect the release of water-soluble vitamins, nano-particle technology may pose risks of aggregation or oxidation due to excessive surface activity, and the stability of layered encapsulation still needs to be verified during storage. It is difficult for these technologies to simultaneously achieve uniformity, bioavailability, and sensory quality. Therefore, there is an urgent need to develop a new vitamin premix and its preparation process to achieve breakthroughs in the uniformity, stability, and functionality of vitamin premixes, meeting the market demand for highly efficient, stable, and palatable nutritional products. Summary of the Invention

[0005] The object of the present invention is to provide a preparation process for a vitamin premix. By adding fat-soluble vitamin mixed particles prepared by a specific method, and mixing with mixed water-soluble vitamins, mixed minerals, vitamin C, magnesium taurate, amino acids, etc., a vitamin premix is made, significantly improving its stability, mixing uniformity, and fluidity.

[0006] To achieve the above object, the present invention provides the following technical solutions:

[0007] The present invention provides a preparation process for a vitamin premix, comprising the following steps:

[0008] By weight, 10 - 30 parts of fat-soluble vitamin mixed particles, 5 - 15 parts of mixed water-soluble vitamins, and 2 - 7 parts of mixed minerals are added to a mixer for mixing, and then 40 - 120 parts of vitamin C, 5 - 15 parts of magnesium taurate, 2 - 7 parts of amino acids, and 0.8 - 2.4 parts of tricalcium phosphate are added for continuous mixing, and then sieved to obtain the vitamin premix.

[0009] Preferably, a preparation process for a vitamin premix comprises the following steps:

[0010] (1) By weight, 0.2 - 0.8 parts of vitamin B1, 1 - 2 parts of vitamin B2, 1 - 3 parts of vitamin B5, 0.03 - 0.08 parts of vitamin B12, 0.05 - 0.09 parts of folic acid, 2 - 6 parts of nicotinamide, 10 - 20 parts of maltodextrin, and 20 - 40 parts of microcrystalline cellulose are added to a mixer for mixing to obtain mixed water-soluble vitamins;

[0011] (2) By weight, 3 - 8 parts of ferrous glycinate, 3 - 8 parts of calcium citrate, 1 - 5 parts of magnesium citrate, 1 - 5 parts of zinc glycinate, and 0.3 - 0.6 parts of ascorbyl palmitate are added to a mixer for mixing to obtain mixed minerals;

[0012] (3) Mix 10 - 30 parts by weight of fat-soluble vitamin mixed microparticles, 5 - 15 parts of mixed water-soluble vitamins, and 2 - 7 parts of mixed minerals in a mixer, then add 40 - 120 parts of vitamin C, 5 - 15 parts of magnesium taurinate, 2 - 7 parts of amino acids, and 0.8 - 2.4 parts of tricalcium phosphate and continue mixing, then sieve to obtain the vitamin premix.

[0013] Preferably, the amino acids are composed of γ-aminobutyric acid and L-theanine, and the weight ratio of γ-aminobutyric acid to L-theanine is 3:1 - 3.

[0014] Preferably, in step (1), the rotation speed of the mixer is 30 - 40 r / min, and the mixing time is 7 - 15 min.

[0015] Preferably, in step (2), the rotation speed of the mixer is 30 - 40 r / min, and the mixing time is 10 - 20 min.

[0016] Preferably, in step (3), the rotation speed of the mixer is 25 - 35 r / min, the mixing time is 3 - 8 min, and the continuous mixing time is 7 - 15 min.

[0017] Preferably, the sieve mesh used for sieving in step (3) is 200 - 270 meshes.

[0018] The preparation process of the vitamin premix of the present invention effectively improves the comprehensive properties such as the mixing uniformity, fluidity, and stability of the premix through multi-stage mixing and component synergy.

[0019] Among them, the premixing of water-soluble vitamins with microcrystalline cellulose and maltodextrin dilutes the adhesiveness of vitamins by utilizing the high fluidity characteristics of the carriers (the needle-like crystal structure of microcrystalline cellulose and the powder fluidity of maltodextrin), avoiding agglomeration caused by surface tension differences; the separate mixing of minerals achieves preliminary dispersion through particle differences (such as the crystalline powder of magnesium citrate and the hydrophobicity of ascorbyl palmitate); the components such as fat-soluble vitamin mixed microparticles, vitamin C, magnesium taurinate, and tricalcium phosphate added in the final mixing stage further improve the overall fluidity through the complementarity of different particle sizes and morphologies (such as the synergy of micron-sized microparticles and nano-sized modified protein particles).

[0020] In addition, as a fat-soluble antioxidant, the ester group and ascorbic acid moiety in the molecular structure of ascorbyl palmitate can effectively capture free radicals and inhibit the oxidation chain reaction initiated by metal ions in the mineral mixture, thereby protecting fat-soluble vitamins and water-soluble vitamins from oxidative degradation. Its fat-soluble property enables it to preferentially penetrate to the surface of mineral particles, form a protective film, reduce the contact between metal ions and oxygen and moisture, and significantly improve the antioxidant stability of the premix, especially delaying the oxidative rancidity of oils and fats and the loss of vitamin activity during high temperature or storage. In addition, ascorbyl palmitate can also form chelates with metal ions in minerals, reduce the catalytic activity of metal ions, and further reduce the oxidation risk.

[0021] The microcrystalline structure of tricalcium phosphate has a high specific surface area, can adsorb trace moisture in the premix, reduce the overall water activity, inhibit the growth of microorganisms and caking phenomenon, and significantly improve the fluidity and storage stability of the premix; in addition, the weak alkaline buffering property of tricalcium phosphate neutralizes acidic substances (such as vitamin decomposition products or environmental pollutants) generated during the mixing process, maintains the stability of the system pH value, and avoids component denaturation or precipitation caused by acid-base imbalance. Its particle morphology can also act as a physical barrier to disperse and fix fat-soluble vitamin microparticles and mineral particles, prevent local aggregation, and improve the mixing uniformity. At the same time, tricalcium phosphate and ascorbyl palmitate form a synergistic effect: the calcium ions of tricalcium phosphate can combine with ascorbyl palmitate to enhance its adsorption stability on the mineral surface, while the antioxidant effect of ascorbyl palmitate can inhibit the potential oxidation reaction between tricalcium phosphate and metal ions, jointly maintaining the functional properties of the premix during long-term storage.

[0022] Preferably, the preparation method of the fat-soluble vitamin mixed microparticles includes the following steps:

[0023] Mix pea protein, carrageenan and phosphate buffer solution, heat and stir, then add neutral protease, enzymatically hydrolyze, inactivate the enzyme, cool to obtain a partially enzymolyzed solution; subject the partially enzymolyzed solution to high-voltage pulsed electric field treatment first, then to dynamic high-pressure microfluidic circulation treatment, reduce pressure and concentrate, and freeze-dry to obtain a modified protein.

[0024] Mix vitamin A, vitamin E acetate, vitamin D3, vitamin K2 with absolute ethanol to obtain material A; mix gum arabic, modified protein, β-cyclodextrin with water to obtain material B; mix the above material A and material B, shear at high speed, spray dry, and sieve to obtain fat-soluble vitamin mixed microparticles.

[0025] In the preparation process of the above-mentioned fat-soluble vitamin mixed microparticles, after pea protein is locally enzymatically hydrolyzed by neutral protease, macromolecular proteins are cleaved into small peptides and amino acids, exposing more active groups. Subsequently, through high-voltage pulsed electric field and dynamic high-pressure microfluidization cyclic treatment, the tertiary structure of protein molecules is further destroyed, forming highly dispersed nanoparticles. This modification significantly improves the surface activity and emulsifying ability of the protein, enabling it to better combine with gum arabic and β-cyclodextrin. The hydrophobic region of the modified protein can physically entrap the fat-soluble vitamin, while the hydrophilic region forms a composite network structure with gum arabic and β-cyclodextrin, thus stabilizing the internal structure of the microparticles. As a cyclic molecule, β-cyclodextrin can encapsulate the fat-soluble vitamin in its hydrophobic inner cavity through molecular inclusion, reducing its contact with oxygen and moisture, delaying oxidation and photolysis, and simultaneously forming a composite colloid network with gum arabic: As a natural polymer emulsifier, gum arabic binds to the modified protein through electrostatic interaction and hydrogen bond, forming a stable emulsifying skeleton, and β-cyclodextrin fills in the gaps of the skeleton through intermolecular interaction, further enhancing the mechanical strength and antioxidant barrier of the system. This synergistic effect significantly improves the dispersibility and mixing uniformity of the fat-soluble vitamin, avoiding the problem of local oxidation hot spots caused by vitamin aggregation in traditional microparticle preparation.

[0026] Preferably, the weight ratio of the pea protein to the carrageenan is 2-6:0.2-1.5.

[0027] Preferably, the weight ratio of the neutral protease to the pea protein is 0.01-0.05:2-6.

[0028] Preferably, the weight ratio of vitamin A, vitamin E acetate, vitamin D3, and vitamin K2 is 5-10:2-8:1-5:0.5-3.

[0029] Preferably, the weight ratio of the gum arabic, the modified protein, and the β-cyclodextrin is 20-40:3-10:4-6.

[0030] Preferably, the preparation method of the fat-soluble vitamin mixed microparticles comprises the following steps:

[0031] Mix 2-6 parts by weight of pea protein, 0.2-1.5 parts by weight of carrageenan with 100-300 parts by weight of phosphate buffer solution, stir at 35-45 °C and 80-150 r / min for 1-3 h, then add 0.01-0.05 parts by weight of neutral protease, enzymatically hydrolyze for 20-30 min, inactivate the enzyme, cool to room temperature to obtain a locally enzymolyzed solution; first treat the locally enzymolyzed solution by high-voltage pulsed electric field for 20-40 s, then perform dynamic high-pressure microfluidization cyclic treatment for 3-5 times, reduce pressure and concentrate, and freeze-dry to obtain the modified protein;

[0032] Mix 5 - 10 parts by weight of vitamin A, 2 - 8 parts by weight of vitamin E acetate, 1 - 5 parts by weight of vitamin D3, 0.5 - 3 parts by weight of vitamin K2 with 70 - 100 parts by weight of absolute ethanol to obtain material A; mix 20 - 40 parts by weight of gum arabic, 3 - 10 parts by weight of modified protein, 4 - 6 parts by weight of β - cyclodextrin with 100 - 200 parts by weight of water to obtain material B; mix the above - mentioned material A and material B, perform high - speed shearing for 3 - 10 min, spray - dry, and pass through a 200 - 270 - mesh sieve to obtain fat - soluble vitamin mixed microparticles.

[0033] Preferably, the concentration of the phosphate buffer solution is 0.1 - 0.3 M and the pH is 6.8 - 7.4.

[0034] Preferably, the enzyme activity of the neutral protease is 30 - 70 U / mg.

[0035] Preferably, the temperature of the enzymatic hydrolysis is 50 - 60 °C.

[0036] Preferably, the temperature for inactivating the enzyme is 80 - 90 °C and the time is 7 - 15 min.

[0037] Preferably, the field strength of the high - voltage pulsed electric field is 10 - 20 kV / cm, the number of pulses is 40 - 60 times, and the pulse width is 100 - 300 μs.

[0038] Preferably, the pressure of the dynamic high - pressure microfluidization is 80 - 120 MPa and the temperature is 25 - 35 °C.

[0039] Preferably, the rotation speed of the high - speed shearing is 10000 - 15000 r / min.

[0040] Preferably, the conditions for spray - drying are: inlet temperature is 90 - 100 °C, outlet temperature is 55 - 65 °C, and feed rate is 7 - 10 g / min.

[0041] Preferably, the mixed water - soluble vitamins include the following raw materials: vitamin B1, vitamin B2, vitamin B5, vitamin B12, folic acid, and nicotinamide.

[0042] Preferably, the mixed minerals include the following raw materials: ferrous glycinate, calcium citrate, magnesium citrate, and zinc glycinate.

[0043] The present invention also provides a vitamin premix prepared by the above - mentioned preparation process.

[0044] Compared with the prior art, the advantages and beneficial effects of the present invention are:

[0045] 1. The present invention provides a vitamin premix and a preparation process thereof. The vitamin premix further improves functionality, stability and mixing uniformity by adding fat-soluble vitamin mixed particles prepared by high-speed shearing and spray drying of vitamin A, vitamin E acetate, vitamin D3, vitamin K2, gum arabic, modified protein, β-cyclodextrin, etc., and synergizing with mixed water-soluble vitamins, mixed minerals, vitamin C, magnesium taurine, amino acids and other components. The vitamin premix can be directly used in a variety of foods as a nutritional supplement and is easy to use.

[0046] 2. In the process of preparing the fat-soluble vitamin mixed microparticles of the present invention, the modified protein can combine with the hydrophobic region of gum arabic through hydrophobic interaction, and form multi-point anchoring with the hydroxyl groups and other groups of gum arabic by means of hydrogen bonds, thereby constructing a stable protein-polysaccharide composite interface layer. This interface layer is further compressed and densified during the dynamic high-pressure microfluidization process, and the composite forms a continuous membrane structure at the oil-water interface, which effectively inhibits the aggregation of lipid droplets and improves the dispersibility; β-cyclodextrin includes vitamins through its hydrophobic cavity, and directionally anchors the fat-soluble molecules in the hydrophobic core of the composite, while the linear polysaccharide chain of gum arabic maintains the minimum spacing between particles through the steric hindrance effect, so that the potential of the particles is stable, and the dispersion system dominated by Brownian motion significantly improves the fluidity.

[0047] 3. The present invention also adds ascorbyl palmitate during the preparation of mixed minerals, which can inhibit the oxidation chain reaction caused by metal ions in the minerals, thereby protecting fat-soluble vitamins and water-soluble vitamins from oxidative degradation. Its fat-soluble properties enable it to preferentially penetrate into the surface of mineral particles to form a protective film, reduce the contact of metal ions with oxygen and water, and significantly improve the antioxidant stability of the premix. Tricalcium phosphate is also added in the final mixing stage to absorb trace moisture in the premix, reduce the overall water activity, inhibit microbial growth and agglomeration, and significantly improve the fluidity and storage stability of the premix. Its particle shape can also serve as a physical barrier to disperse and fix fat-soluble vitamin particles and mineral particles, prevent local aggregation, and improve mixing uniformity. DETAILED DESCRIPTION

[0048] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0049] Some of the raw materials of the embodiments and comparative examples are as follows:

[0050] Maltodextrin was purchased from Shandong Xiwang Sugar Co., Ltd. and was food grade.

[0051] Microcrystalline cellulose was purchased from Linghu Xinwang Chemical Co., Ltd., Huzhou City, food grade.

[0052] Pea protein was purchased from Linyi Yuwang Vegetable Protein Co., Ltd., food grade.

[0053] Carrageenan was purchased from Green New (Fujian) Food Co., Ltd., food grade.

[0054] Arabic gum was purchased from Taizhou Dingli Glue Industry Co., Ltd., food grade.

[0055] β-Cyclodextrin was purchased from Hefei Shengrun Bioproducts Co., Ltd., food grade.

[0056] Neutral protease was purchased from Shanghai Yuanye Bio-Technology Co., Ltd., enzyme activity 50 u / mg.

[0057] Example 1

[0058] This example provides a preparation process of a vitamin premix, including the following steps:

[0059] (1) Add 0.5 parts by weight of vitamin B1, 1.5 parts by weight of vitamin B2, 2 parts by weight of vitamin B5, 0.06 parts by weight of vitamin B12, 0.07 parts by weight of folic acid, 4 parts by weight of nicotinamide, 15 parts by weight of maltodextrin and 30 parts by weight of microcrystalline cellulose into a mixer and mix for 10 min at a rotation speed of 35 r / min to obtain a mixed water-soluble vitamin;

[0060] (2) Add 5 parts by weight of ferrous glycinate, 5 parts by weight of calcium citrate, 3 parts by weight of magnesium citrate, 3 parts by weight of zinc glycinate and 0.5 parts by weight of ascorbyl palmitate into a mixer and mix for 15 min at a rotation speed of 35 r / min to obtain a mixed mineral;

[0061] (3) Add 20 parts by weight of mixed fat-soluble vitamin particles, 10 parts by weight of mixed water-soluble vitamin and 5 parts by weight of mixed mineral into a mixer and mix for 5 min at a rotation speed of 30 r / min, then add 80 parts by weight of vitamin C, 10 parts by weight of magnesium taurate, 5 parts by weight of amino acids and 1.5 parts by weight of tricalcium phosphate and continue to mix for 10 min, and pass through a 250-mesh sieve to obtain the vitamin premix. The amino acids are composed of γ-aminobutyric acid and L-theanine in a weight ratio of 3:2.

[0062] The preparation method of the mixed fat-soluble vitamin particles includes the following steps:

[0063] Mix 4.2 parts by weight of pea protein, 0.8 parts by weight of carrageenan with 200 parts by weight of 0.2 M phosphate buffer (pH 7.2), stir at 40 °C and 100 r / min for 2 h, then add 0.03 parts by weight of neutral protease, enzymatically hydrolyze at 55 °C for 25 min, raise the temperature to 85 °C to inactivate the enzyme for 10 min, cool to room temperature to obtain a partially enzymatically hydrolyzed solution; subject the partially enzymatically hydrolyzed solution to high-voltage pulsed electric field treatment for 30 s, with the field strength of the high-voltage pulsed electric field being 15 kV / cm, the number of pulses being 50 times, and the pulse width being 200 μs, then perform dynamic high-pressure microfluidization circulation treatment 4 times, with the pressure of the dynamic high-pressure microfluidization being 100 MPa and the temperature being 30 °C, reduce the pressure and concentrate, and freeze-dry to obtain a modified protein;

[0064] Mix 8 parts by weight of vitamin A, 5 parts by weight of vitamin E acetate, 3 parts by weight of vitamin D3, 2 parts by weight of vitamin K2 with 82 parts by weight of absolute ethanol to obtain Material A; mix 30 parts by weight of gum arabic, 6 parts by weight of modified protein, 5 parts by weight of β-cyclodextrin with 160 parts by weight of water to obtain Material B; mix the above Material A and Material B, perform high-speed shearing at 12000 r / min for 5 min, spray-dry, and pass through a 250-mesh sieve to obtain fat-soluble vitamin mixed microparticles. Among them, the conditions for spray drying are: inlet temperature 95 °C, outlet temperature 60 °C, and feeding rate 8.5 g / min.

[0065] Example 2

[0066] This example provides a preparation process for a vitamin premix, including the following steps:

[0067] (1) Add 0.2 parts by weight of vitamin B1, 1 part by weight of vitamin B2, 1 part by weight of vitamin B5, 0.03 parts by weight of vitamin B12, 0.05 parts by weight of folic acid, 2 parts by weight of nicotinamide, 10 parts by weight of maltodextrin and 20 parts by weight of microcrystalline cellulose into a mixer and mix for 7 min at a rotation speed of 40 r / min to obtain a mixed water-soluble vitamin;

[0068] (2) Add 3 parts by weight of ferrous glycinate, 3 parts by weight of calcium citrate, 1 part by weight of magnesium citrate, 1 part by weight of zinc glycinate and 0.3 parts by weight of ascorbyl palmitate into a mixer and mix for 10 min at a rotation speed of 40 r / min to obtain a mixed mineral;

[0069] (3) Add 10 parts by weight of fat-soluble vitamin mixed microparticles, 5 parts by weight of mixed water-soluble vitamins, and 2 parts by weight of mixed minerals into a mixer and mix for 3 min at a rotation speed of 35 r / min. Then add 40 parts by weight of vitamin C, 5 parts by weight of magnesium taurinate, 2 parts by weight of amino acids, and 0.8 parts by weight of tricalcium phosphate and continue to mix for 7 min. Pass through a 200-mesh sieve to obtain the vitamin premix. The amino acids are composed of γ-aminobutyric acid and L-theanine in a weight ratio of 3:1.

[0070] The preparation method of the fat-soluble vitamin mixed microparticles is the same as that in Example 1.

[0071] Example 3

[0072] This example provides a preparation process of a vitamin premix, including the following steps:

[0073] (1) Add 0.8 parts by weight of vitamin B1, 2 parts by weight of vitamin B2, 3 parts by weight of vitamin B5, 0.08 parts by weight of vitamin B12, 0.09 parts by weight of folic acid, 6 parts by weight of nicotinamide, 20 parts by weight of maltodextrin, and 40 parts by weight of microcrystalline cellulose into a mixer and mix for 15 min at a rotation speed of 30 r / min to obtain mixed water-soluble vitamins;

[0074] (2) Add 8 parts by weight of ferrous glycinate, 8 parts by weight of calcium citrate, 5 parts by weight of magnesium citrate, 5 parts by weight of zinc glycinate, and 0.6 parts by weight of ascorbyl palmitate into a mixer and mix for 20 min at a rotation speed of 30 r / min to obtain mixed minerals;

[0075] (3) Add 30 parts by weight of fat-soluble vitamin mixed microparticles, 15 parts by weight of mixed water-soluble vitamins, and 7 parts by weight of mixed minerals into a mixer and mix for 8 min at a rotation speed of 25 r / min. Then add 120 parts by weight of vitamin C, 15 parts by weight of magnesium taurinate, 7 parts by weight of amino acids, and 2.4 parts by weight of tricalcium phosphate and continue to mix for 15 min. Pass through a 270-mesh sieve to obtain the vitamin premix. The amino acids are composed of γ-aminobutyric acid and L-theanine in a weight ratio of 3:3.

[0076] The preparation method of the fat-soluble vitamin mixed microparticles is the same as that in Example 1.

[0077] Comparative Example 1

[0078] The difference between this comparative example and Example 1 is that the preparation method of the fat-soluble vitamin mixed microparticles is different. Specifically, the preparation method of the fat-soluble vitamin mixed microparticles includes the following steps:

[0079] Mix 4.2 parts by weight of pea protein, 0.8 part by weight of carrageenan with 200 parts by weight of 0.2 M phosphate buffer (pH 7.2), stir at 40 °C and 100 r / min for 2 h, then add 0.03 part by weight of neutral protease, enzymatically hydrolyze at 55 °C for 25 min, raise the temperature to 85 °C to inactivate the enzyme for 10 min, cool to room temperature to obtain a partially hydrolyzed solution, concentrate under reduced pressure and freeze-dry to obtain a modified protein;

[0080] Mix 8 parts by weight of vitamin A, 5 parts by weight of vitamin E acetate, 3 parts by weight of vitamin D3, 2 parts by weight of vitamin K2 with 82 parts by weight of absolute ethanol to obtain Material A; mix 30 parts by weight of gum arabic, 6 parts by weight of modified protein, 5 parts by weight of β-cyclodextrin with 160 parts by weight of water to obtain Material B; mix the above Material A and Material B, perform high-speed shearing at 12000 r / min for 5 min, spray-dry, and pass through a 250-mesh sieve to obtain fat-soluble vitamin mixed microparticles. Among them, the conditions for spray-drying are: inlet temperature 95 °C, outlet temperature 60 °C, and feeding rate 8.5 g / min.

[0081] Comparative Example 2

[0082] The difference between this comparative example and Example 1 is: the preparation method of the fat-soluble vitamin mixed microparticles is different, specifically as follows: the preparation method of the fat-soluble vitamin mixed microparticles includes the following steps:

[0083] Mix 4.2 parts by weight of pea protein with 200 parts by weight of 0.2 M phosphate buffer (pH 7.2) to obtain a pea protein solution; first treat the pea protein solution with high-voltage pulsed electric field for 30 s, the field strength of the high-voltage pulsed electric field is 15 kV / cm, the number of pulses is 50 times, and the pulse width is 200 μs, then perform dynamic high-pressure microfluidization cyclic treatment 4 times, the pressure of the dynamic high-pressure microfluidization is 100 MPa, and the temperature is 30 °C, concentrate under reduced pressure and freeze-dry to obtain a modified protein;

[0084] Mix 8 parts by weight of vitamin A, 5 parts by weight of vitamin E acetate, 3 parts by weight of vitamin D3, 2 parts by weight of vitamin K2 with 82 parts by weight of absolute ethanol to obtain Material A; mix 30 parts by weight of gum arabic, 6 parts by weight of modified protein, 5 parts by weight of β-cyclodextrin with 160 parts by weight of water to obtain Material B; mix the above Material A and Material B, perform high-speed shearing at 12000 r / min for 5 min, spray-dry, and pass through a 250-mesh sieve to obtain fat-soluble vitamin mixed microparticles. Among them, the conditions for spray-drying are: inlet temperature 95 °C, outlet temperature 60 °C, and feeding rate 8.5 g / min.

[0085] Comparative Example 3

[0086] The difference between this comparative example and Example 1 is as follows: The preparation method of the fat-soluble vitamin mixed microparticles is different, specifically as follows: The preparation method of the fat-soluble vitamin mixed microparticles includes the following steps:

[0087] Mix 8 parts by weight of vitamin A, 5 parts by weight of vitamin E acetate, 3 parts by weight of vitamin D3, 2 parts by weight of vitamin K2 with 82 parts by weight of absolute ethanol to obtain Material A; mix 30 parts by weight of gum arabic, 5 parts by weight of β-cyclodextrin with 160 parts by weight of water to obtain Material B; mix the above Material A and Material B, perform high-speed shearing at 12000 r / min for 5 min, spray dry, and pass through a 250-mesh sieve to obtain fat-soluble vitamin mixed microparticles. Among them, the conditions for spray drying are: inlet temperature 95°C, outlet temperature 60°C, and feed rate 8.5 g / min.

[0088] Comparative Example 4

[0089] The difference between this comparative example and Example 1 is as follows: The preparation method of the fat-soluble vitamin mixed microparticles is different, specifically as follows: The preparation method of the fat-soluble vitamin mixed microparticles includes the following steps:

[0090] Mix 4.2 parts by weight of pea protein, 0.8 parts by weight of carrageenan with 200 parts by weight of 0.2 M phosphate buffer solution (pH 7.2), stir at 40°C and 100 r / min for 2 h, then add 0.03 parts by weight of neutral protease, perform enzymatic hydrolysis at 55°C for 25 min, raise the temperature to 85°C to inactivate the enzyme for 10 min, and cool to room temperature to obtain a partially enzymolyzed solution; subject the partially enzymolyzed solution to high-voltage pulsed electric field treatment for 30 s, the field strength of the high-voltage pulsed electric field is 15 kV / cm, the number of pulses is 50 times, and the pulse width is 200 μs, then perform dynamic high-pressure microfluidization circulation treatment 4 times, the pressure of the dynamic high-pressure microfluidization is 100 MPa, and the temperature is 30°C, perform vacuum concentration and freeze drying to obtain a modified protein;

[0091] Mix 8 parts by weight of vitamin A, 5 parts by weight of vitamin E acetate, 3 parts by weight of vitamin D3, 2 parts by weight of vitamin K2 with 82 parts by weight of absolute ethanol to obtain Material A; mix 30 parts by weight of gum arabic, 6 parts by weight of the modified protein with 160 parts by weight of water to obtain Material B; mix the above Material A and Material B, perform high-speed shearing at 12000 r / min for 5 min, spray dry, and pass through a 250-mesh sieve to obtain fat-soluble vitamin mixed microparticles. Among them, the conditions for spray drying are: inlet temperature 95°C, outlet temperature 60°C, and feed rate 8.5 g / min.

[0092] Comparative Example 5

[0093] The difference between this comparative example and Example 1 is that ascorbyl palmitate was not added in step (2).

[0094] Comparative Example 6

[0095] The difference between this comparative example and Example 1 is that tricalcium phosphate was not added in step (3).

[0096] Performance Test

[0097] The following performance determinations were carried out on the vitamin premixes prepared in Examples 1-3 and Comparative Examples 1-6. Among them, the method for determining the mixing uniformity was as follows: 10 random samples were taken from the vitamin premixes prepared in each example, the content of vitamin A in the samples was detected (refer to the standard GB 5009.82-2016), and the RSD was calculated to characterize the mixing uniformity. RSD = standard deviation / mean × 100%; the smaller the value, the more uniform the mixing. The test method for fluidity was as follows: The vitamin premixes prepared in each example were taken and placed in a 100 mL plastic graduated cylinder to measure the loose volume of the premix. Then, the plastic graduated cylinder containing the premix was placed in a rotary shaker for compaction, and the compacted volume of the premix was measured. The compressibility was calculated to characterize the fluidity. Compressibility = (loose volume - compacted volume) / loose volume × 100%; the smaller the value, the better the fluidity. The test method for antioxidant stability was as follows: The vitamin premixes prepared in each example were taken and placed in an oven at 60 °C for 2 weeks for an accelerated oxidation experiment. The peroxide value of the premix before and after the experiment was measured (refer to the standard GB 5009.227-2023), and the oxidation rate was calculated to characterize the stability. Oxidation rate = (peroxide value after the experiment - initial peroxide value) / initial peroxide value × 100%; the smaller the value, the better the stability. The results of each performance test are shown in Table 1.

[0098] Table 1: Results of various performance tests of vitamin premixes

[0099]

[0100] It can be seen from the above test results that the vitamin premixes prepared in Examples 1-3 have excellent mixing uniformity, fluidity and stability. In particular, the vitamin premix prepared in Example 1 has the best comprehensive performance. This is because in the present invention, by adding the fat-soluble vitamin mixed microparticles prepared by a specific method and acting together with the mixed water-soluble vitamins, mixed minerals, vitamin C, tricalcium phosphate, etc., the mixing uniformity, fluidity and stability of the premix are further improved. Compared with Example 1, in Comparative Examples 1-4, the specific self-made fat-soluble vitamin mixed microparticles were not used; in Comparative Example 5, ascorbyl palmitate was not used in the mixed minerals; in Comparative Example 6, tricalcium phosphate was not used in the final mixing stage. It can be seen from the comparison of the above test results that the comprehensive performance of the prepared vitamin premixes all decreased to varying degrees. The comparison of the above test results further proves the importance of the technical solutions corresponding to Examples 1-3 of the present invention for their technical effects.

[0101] The above is the preferred embodiment of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the principle described in the present invention, several improvements and refinements can be made, and these improvements and refinements should also be regarded as the protection scope of the present invention.

Claims

1. A preparation process of a vitamin premix, characterized in that, It includes the following steps: By weight, 10 - 30 parts of fat-soluble vitamin mixed microparticles, 5 - 15 parts of mixed water-soluble vitamins and 2 - 7 parts of mixed minerals are added to a mixer for mixing, then 40 - 120 parts of vitamin C, 5 - 15 parts of magnesium taurate, 2 - 7 parts of amino acids and 0.8 - 2.4 parts of tricalcium phosphate are added and mixed continuously, and then sieved to obtain the vitamin premix.

2. The preparation process of the vitamin premix according to claim 1, characterized in that, The preparation method of the fat-soluble vitamin mixed microparticles includes the following steps: Mix pea protein, carrageenan and phosphate buffer solution, heat and stir, then add neutral protease for enzymatic hydrolysis, inactivate the enzyme, and cool to obtain a partially enzymolyzed solution; the partially enzymolyzed solution is first treated by high-voltage pulsed electric field and then by dynamic high-pressure microfluidic circulation treatment, concentrated under reduced pressure, and freeze-dried to obtain modified protein; Mix vitamin A, vitamin E acetate, vitamin D3, vitamin K2 and absolute ethanol to obtain material A; mix arabic gum, modified protein, β-cyclodextrin and water to obtain material B; mix the above material A and material B, shear at high speed, spray dry, and sieve to obtain fat-soluble vitamin mixed microparticles.

3. The preparation process of the vitamin premix according to claim 2, wherein, The weight ratio of the pea protein to the carrageenan is 2 - 6:0.2 - 1.5; the weight ratio of the neutral protease to the pea protein is 0.01 - 0.05:2 - 6.

4. The preparation process of the vitamin premix according to claim 2, characterized in that, The weight ratio of vitamin A, vitamin E acetate, vitamin D3, vitamin K2 is 5 - 10:2 - 8:1 - 5:0.5 - 3; the weight ratio of arabic gum, modified protein, β-cyclodextrin is 20 - 40:3 - 10:4 - 6.

5. The preparation process of the vitamin premix according to claim 2, characterized in that, The field strength of the high-voltage pulsed electric field is 10 - 20 kV / cm, the number of pulses is 40 - 60 times, and the pulse width is 100 - 300 μs.

6. The preparation process of the vitamin premix according to claim 2, characterized in that, The pressure of the dynamic high-pressure microfluidics is 80 - 120 MPa, and the temperature is 25 - 35 °C.

7. The preparation process of the vitamin premix according to claim 1, characterized in that, The mixed water-soluble vitamins include the following raw materials: Vitamin B1, vitamin B2, vitamin B5, vitamin B12, folic acid, nicotinamide.

8. The preparation process of the vitamin premix according to claim 1, characterized in that, The mixed minerals include the following raw materials: ferrous glycinate, calcium citrate, magnesium citrate, zinc glycinate.

9. The preparation process of the vitamin premix according to claim 1, characterized in that, The amino acids are composed of γ-aminobutyric acid and L-theanine.

10. A vitamin premix, characterized in that, Prepared by the preparation process according to any one of claims 1 - 9.

Images