A vitamin premix and a preparation process thereof

Abstract

The application provides a vitamin premix and a preparation process thereof, and belongs to the technical field of food additives, and the preparation process is as follows: adding mixed microparticles of fat-soluble vitamins, mixed water-soluble vitamins and mixed minerals into a mixer and mixing, then adding vitamin C, magnesium taurate, amino acids and tricalcium phosphate and continuing to mix, and sieving to obtain the vitamin premix. The raw materials of the mixed microparticles of fat-soluble vitamins include vitamin A, vitamin E acetate, vitamin D3, vitamin K2, acacia, modified protein and beta-cyclodextrin; the raw materials of the mixed water-soluble vitamins include vitamin B1, vitamin B2, vitamin B5, vitamin B12, folic acid and nicotinamide; and the raw materials of the mixed minerals include ferrous glycinate, calcium citrate, magnesium citrate and zinc glycinate. The vitamin premix prepared by the application can be used in various foods as a nutritional supplement, is convenient to use, and has good stability and mixing uniformity.

Description

TECHNICAL FIELD

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

[0002] The vitamin premix is a kind of food additive that precisely proportionally mixes various vitamins, minerals, amino acids and other nutrients according to scientific ratios, aiming to provide comprehensive nutritional support for food or nutritional supplements. With the development of modern food industry, people's demand for balanced nutrition is increasing, and the problem of nutrient loss caused by processing, cooking or food preferences in traditional diets is becoming increasingly prominent. The emergence of vitamin premix effectively solves the cumbersome process of single nutrient addition in food processing, helps food manufacturers simplify production links, and at the same time ensures the stability and consistency of nutritional ingredients. Its core advantage lies in the precise control of the addition amount of micronutrients, avoiding excessive or insufficient, especially in the field of formula milk powder, fortified food and nutritional supplements, vitamin premix 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, reduces the quality risk caused by improper operation, and becomes an indispensable key technology support for modern health food industry.

[0003] At present, the preparation of vitamin premix 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 the raw material powder, but due to the significant differences in particle size, density and electrostatic properties of different components, it is easy to cause uneven mixing, especially for active ingredients with extremely low content (such as fat-soluble vitamins) or moisture-absorbing minerals (such as iron and zinc), which are prone to local enrichment or stratification, affecting the uniformity and stability of the final product. Although the granulation technology can improve the flowability and dispersibility, the high temperature and humidity environment may damage the activity of heat-sensitive vitamins (such as vitamin C), and uneven particle size may also reduce the absorption efficiency. In addition, although the microencapsulation technology can wrap nutrients to improve stability, the process is complex, the cost is high, and the release speed is difficult to accurately control. These technical bottlenecks make the vitamin premix still face problems such as quality fluctuation, low bioavailability and poor taste in actual application, which restricts its further development in the field of high-end nutritional products.

[0004] In view of the shortcomings of the traditional process, people try to improve the performance of premix through new carrier technology, nano dispersion and intelligent embedding means. For example, high-fat carriers are used as stable carriers for vitamins, which can effectively protect fat-soluble ingredients and improve the taste; nano particle technology enhances the dispersibility by reducing the particle size; layered embedding technology can achieve gradient release of ingredients and improve the utilization. However, these improvements also have limitations: high-fat carriers may affect the release of water-soluble vitamins, nano particle technology may cause agglomeration or oxidation risk due to high surface activity, and the stability of layered embedding still needs to be verified during storage. These technologies are difficult to balance uniformity, bioavailability and sensory quality at the same time. Therefore, it is urgent to develop a new vitamin premix and its preparation process, in order to realize the breakthrough of uniformity, stability and functionality of vitamin premix, and meet the market demand for efficient, stable and palatable nutritional products. SUMMARY

[0005] The purpose of the present application is to provide a preparation process of vitamin premix, by adding fat-soluble vitamin mixed microparticles prepared by a specific method, mixed water-soluble vitamins, mixed minerals, vitamin C, magnesium taurate, amino acids, etc. to form vitamin premix, so that its stability, mixing uniformity and flowability are significantly improved.

[0006] In order to achieve the above purpose, the present application provides the following technical solutions:

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

[0008] According to weight parts, 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 for further mixing, sieving, to obtain the vitamin premix.

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

[0010] (1) According to weight parts, 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 malt dextrin and 20-40 parts of microcrystalline cellulose are added to a mixer for mixing, to obtain mixed water-soluble vitamins;

[0011] (2) According to weight parts, 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 ascorbic acid palmitate are added to a mixer for mixing, to obtain mixed minerals;

[0012] (3) adding 10-30 parts of the mixed fat-soluble vitamin microparticles, 5-15 parts of the mixed water-soluble vitamin, and 2-7 parts of the mixed mineral into a mixer, mixing, then adding 40-120 parts of vitamin C, 5-15 parts of magnesium taurate, 2-7 parts of amino acid, and 0.8-2.4 parts of tricalcium phosphate, continuing to mix, sieving, to obtain the vitamin premix.

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

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

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

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

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

[0018] The preparation process of the vitamin premix effectively improves the comprehensive performance of the premix, such as mixing uniformity, fluidity, and stability, through multi-stage mixing and synergistic effect of the components.

[0019] Pre-mixing of the water-soluble vitamin with the microcrystalline cellulose and the malt dextrin dilutes the adhesion of the vitamin by using the high fluidity characteristics (the needle-shaped crystalline structure of the microcrystalline cellulose and the powder fluidity of the malt dextrin) of the carrier, and avoids agglomeration caused by differences in surface tension; separate mixing of the mineral realizes preliminary dispersion through particle differences (such as the crystalline powder of magnesium citrate and the hydrophobicity of ascorbic acid palmitate); and the mixed fat-soluble vitamin microparticles, vitamin C, magnesium taurate, tricalcium phosphate, and other components added in the final mixing stage further improve the overall fluidity through complementation of different particle sizes and forms (such as the synergy of micrometer-level microparticles and nanometer-level modified protein particles).

[0020] In addition, as a fat-soluble antioxidant, ascorbyl palmitate can effectively capture free radicals and inhibit the oxidation chain reaction caused by metal ions in the mineral mixture, thereby protecting fat-soluble vitamins and water-soluble vitamins from oxidative degradation. Its fat-soluble properties enable it to preferentially penetrate the surface of mineral particles, forming a protective film that reduces the contact between metal ions and oxygen and moisture, significantly improving the antioxidant stability of the premix, especially delaying the oxidation of oil and the loss of vitamin activity during high-temperature or storage processes. In addition, ascorbyl palmitate can also form chelates with metal ions in minerals, reducing the catalytic activity of metal ions and further reducing the risk of oxidation.

[0021] The microcrystalline structure of tricalcium phosphate has a high specific surface area, which can adsorb trace amounts of moisture in the premix, reduce the overall water activity, inhibit the growth of microorganisms and caking, and significantly improve the flowability and storage stability of the premix. In addition, the weak alkaline buffering performance of tricalcium phosphate can neutralize acidic substances produced during the mixing process, such as vitamin decomposition products or environmental pollutants, maintaining the stability of the system pH value and avoiding the denaturation or precipitation of ingredients caused by acid-base imbalance. Its particle morphology can also act as a physical barrier to disperse and fix fat-soluble vitamin particles and mineral particles, preventing local aggregation and improving mixing uniformity. At the same time, tricalcium phosphate and ascorbyl palmitate form a synergistic effect: the calcium ions of tricalcium phosphate can bind with ascorbyl palmitate, enhancing 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, together maintaining the functional properties of the premix during long-term storage.

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

[0023] Mix pea protein, carrageenan, and phosphate buffer, heat and stir, then add neutral protease, enzymatic hydrolysis, enzyme inactivation, cooling, to obtain a partial enzymatic hydrolysate; the partial enzymatic hydrolysate is first treated by high-pressure pulsed electric field, then treated by dynamic high-pressure microjet circulation, reduced pressure concentration, freeze-drying to obtain modified protein;

[0024] Mix vitamin A, vitamin E acetate, vitamin D3, and vitamin K2 with anhydrous ethanol to obtain material A; mix gum arabic, modified protein, and β-cyclodextrin with water to obtain material B; mix the above-mentioned material A and material B, high-speed shearing, spray drying, sieving to obtain fat-soluble vitamin mixed microparticles.

[0025] In the preparation process of the above-mentioned fat-soluble vitamin mixed microparticles, the pea protein is partially enzymolyzed by neutral protease, and the macromolecular protein is cut into small molecular peptides and amino acids, exposing more active groups. Subsequently, the tertiary structure of the protein molecules is further destroyed by high-voltage pulse electric field and dynamic high-pressure microfluidization cycle treatment, forming highly dispersed nanoscale particles. This modification significantly improves the surface activity and emulsifying capacity of the protein, enabling it to better combine with gum arabic and β-cyclodextrin. The hydrophobic region of the modified protein can form physical embedding with fat-soluble vitamins, while the hydrophilic region forms a complex network structure with gum arabic and β-cyclodextrin, thereby stabilizing the internal structure of the microparticles. As a cyclic molecule, β-cyclodextrin has a hydrophobic internal cavity that can encapsulate fat-soluble vitamins within the ring through molecular embedding, reducing their contact with oxygen and water, delaying oxidation and photolysis, and forming a complex colloidal network with gum arabic. Gum arabic, as a natural high-molecular emulsifier, combines with the modified protein through electrostatic interaction and hydrogen bonding to form a stable emulsification framework, and β-cyclodextrin fills the gaps between the framework through intermolecular interaction, further enhancing the mechanical strength and antioxidant barrier of the system. This synergistic effect significantly improves the dispersibility and uniformity of fat-soluble vitamins, avoiding the problem of local oxidation hotspots caused by vitamin aggregation in traditional microparticle preparation.

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

[0027] Preferably, the weight ratio of the neutral protease and 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 gum arabic, modified protein, and 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, and 100-300 parts by weight of phosphate buffer, 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, enzymolyze for 20-30 min, inactivate the enzyme, and cool to room temperature to obtain a partial enzymolysis solution; the partial enzymolysis solution is first treated by high-voltage pulse electric field for 20-40 s, then treated by dynamic high-pressure microfluidization cycle for 3-5 times, reduced pressure concentration, freeze-drying to obtain modified protein;

[0032] Mixing 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 anhydrous ethanol to obtain material A; mixing 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; mixing the above material A with material B, high-speed shearing for 3-10 min, spray drying, and passing through a 200-270 mesh screen to obtain fat-soluble vitamin mixed microparticles.

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

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

[0035] Preferably, the temperature of the enzymolysis is 50-60℃.

[0036] Preferably, the temperature of the enzyme inactivation is 80-90℃, and the time is 7-15 min.

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

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

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

[0040] Preferably, the conditions of the spray drying are as follows: the inlet temperature is 90-100℃, the outlet temperature is 55-65℃, and the feeding rate is 7-10g / 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 application also provides a vitamin premix prepared by the above preparation process.

[0044] Compared with the prior art, the application has the following advantages and beneficial effects:

[0045] 1. The present application provides a kind of vitamin premix and its preparation process, by adding by vitamin A, vitamin E acetate, vitamin D3, vitamin K2, gum arabic, modified protein, β-cyclodextrin etc. The mixed microparticles of fat-soluble vitamin prepared by high-speed shearing and spray drying, synergistic effect with mixed water-soluble vitamin, mixed mineral, vitamin C, magnesium taurine, amino acid etc. Component, further improve the functionality, stability and mixing uniformity of vitamin premix, can be directly used in a variety of food as nutritional supplement, convenient to use.

[0046] 2, in the process of preparing the mixed microparticles of fat-soluble vitamin in the present application, the modified protein can be combined with the hydrophobic region of gum arabic through hydrophobic interaction, and form multi-point anchoring with the hydroxyl group of gum arabic by hydrogen bond, so as to construct a stable protein-polysaccharide complex interface layer, which is further compressed and densified in the process of dynamic high pressure microfluidization, and the complex forms a continuous membrane structure at the oil-water interface, effectively inhibiting the coalescence of lipid droplets and improving the dispersibility; β-cyclodextrin can form inclusion with vitamin through its hydrophobic cavity, and the fat-soluble molecules are anchored in the hydrophobic core of the complex, and the linear polysaccharide chain of gum arabic maintains the minimum distance between particles through steric hindrance effect, so that the zeta potential is stable, and the dispersion system dominated by Brownian motion significantly improves the fluidity.

[0047] 3, in the preparation of mixed minerals in the present application, ascorbic acid palmitate is also added, which can inhibit the oxidation chain reaction caused by metal ions in the minerals, thereby protecting the fat-soluble vitamins and water-soluble vitamins from oxidative degradation, and its fat-soluble characteristics enable it to preferentially penetrate the surface of mineral particles to form a protective film, reducing the contact of metal ions with oxygen and moisture, and significantly improving the antioxidant stability of the premix; In the final mixing stage, tricalcium phosphate is also added, which can adsorb trace amounts of moisture in the premix, reduce the overall water activity, inhibit the growth of microorganisms and caking, and significantly improve the fluidity and storage stability of the premix. 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 mixing uniformity. DETAILED DESCRIPTION

[0048] The technical solutions in the embodiments of the present application will be described clearly and completely below. Obviously, the described embodiments are only a part of the embodiments of the present application, not all. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor belong to the scope of protection of the present application.

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

[0050] Maltodextrin is purchased from Shandong Xiwang Sugar Industry Co., Ltd., food grade.

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

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

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

[0054] Gum arabic was purchased from Taizhou Dingli Gum Industry Co., Ltd., food grade.

[0055] Beta-cyclodextrin was purchased from Hefei Shengrun Biological Products Co., Ltd., food grade.

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

[0057] Example 1

[0058] The present embodiment provides a preparation process of a vitamin premix, comprising the following steps:

[0059] (1) 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 malt dextrin and 30 parts by weight of microcrystalline cellulose were added into a mixer and mixed for 10 min at a speed of 35 r / min to obtain mixed water-soluble vitamins;

[0060] (2) 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 ascorbic acid palmitate were added into a mixer and mixed for 15 min at a speed of 35 r / min to obtain mixed minerals;

[0061] (3) 20 parts by weight of fat-soluble vitamin mixed particles, 10 parts by weight of mixed water-soluble vitamins and 5 parts by weight of mixed minerals were added into a mixer and mixed for 5 min at a speed of 30 r / min, then 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 were added and mixed for 10 min, and then passed through a 250 mesh screen to obtain the vitamin premix. The amino acids were composed of γ-aminobutyric acid and L-theanine at a weight ratio of 3:2.

[0062] The preparation method of the fat-soluble vitamin mixed particles comprises 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 0.2M phosphate buffer (pH 7.2), stir at 40℃ and 100r / min for 2h, then add 0.03 parts by weight of neutral protease, enzymolysis at 55℃ for 25min, raise the temperature to 85℃ to inactivate the enzyme for 10min, cool to room temperature to obtain a partial enzymolysis liquor; the partial enzymolysis liquor is first treated by high-voltage pulsed electric field for 30s, the field strength of the high-voltage pulsed electric field is 15kV / cm, the pulse number is 50 times, and the pulse width is 200μs, then it is treated by dynamic high-pressure microfluidization for 4 times, the pressure of the dynamic high-pressure microfluidization is 100MPa, and the temperature is 30℃, then it is concentrated under reduced pressure, freeze-dried to obtain 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 anhydrous 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, high-speed shear at 12000r / min for 5min, spray drying, pass through a 250 mesh screen to obtain fat-soluble vitamin mixed microparticles. Among them, the conditions for spray drying are: inlet temperature 95℃, outlet temperature 60℃, feeding rate 8.5g / min.

[0065] Example 2

[0066] The present embodiment provides a preparation process of vitamin premix, which comprises 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 malt dextrin and 20 parts by weight of microcrystalline cellulose into a mixer and mix for 7min at a speed of 40r / min to obtain mixed water-soluble vitamins;

[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 ascorbic acid palmitate into a mixer and mix for 10min at a speed of 40r / min to obtain mixed minerals;

[0069] (3) 10 parts by weight of the mixed microparticles of fat-soluble vitamins, 5 parts by weight of the mixed water-soluble vitamins, and 2 parts by weight of the mixed minerals were added into a mixer and mixed for 3 min at a speed of 35 r / min, then 40 parts by weight of vitamin C, 5 parts by weight of magnesium taurate, 2 parts by weight of amino acids, and 0.8 parts by weight of tricalcium phosphate were added and mixed for another 7 min, and the mixture was sieved through a 200-mesh screen to obtain the vitamin premix. The amino acids were composed of γ-aminobutyric acid and L-theanine at a weight ratio of 3:1.

[0070] The preparation method of the mixed microparticles of fat-soluble vitamins was the same as that in Embodiment 1.

[0071] Embodiment 3

[0072] The embodiment provides a preparation process of a vitamin premix, which comprises the following steps:

[0073] (1) 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 malt dextrin, and 40 parts by weight of microcrystalline cellulose were added into a mixer and mixed for 15 min at a speed of 30 r / min to obtain the mixed water-soluble vitamins.

[0074] (2) 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 ascorbic acid palmitate were added into a mixer and mixed for 20 min at a speed of 30 r / min to obtain the mixed minerals.

[0075] (3) 30 parts by weight of the mixed microparticles of fat-soluble vitamins, 15 parts by weight of the mixed water-soluble vitamins, and 7 parts by weight of the mixed minerals were added into a mixer and mixed for 8 min at a speed of 25 r / min, then 120 parts by weight of vitamin C, 15 parts by weight of magnesium taurate, 7 parts by weight of amino acids, and 2.4 parts by weight of tricalcium phosphate were added and mixed for another 15 min, and the mixture was sieved through a 270-mesh screen to obtain the vitamin premix. The amino acids were composed of γ-aminobutyric acid and L-theanine at a weight ratio of 3:3.

[0076] The preparation method of the mixed microparticles of fat-soluble vitamins was the same as that in Embodiment 1.

[0077] Comparative Example 1

[0078] The difference between the comparative example and Embodiment 1 is that the preparation method of the mixed microparticles of fat-soluble vitamins is different, and specifically as follows: the preparation method of the mixed microparticles of fat-soluble vitamins comprises the following steps:

[0079] Mix 4.2 parts by weight of pea protein, 0.8 parts by weight of carrageenan with 200 parts by weight of 0.2M phosphate buffer (pH 7.2), stir at 40℃, 100r / min for 2h, then add 0.03 parts by weight of neutral protease, enzymatic hydrolysis at 55℃ for 25min, raise the temperature to 85℃ to inactivate the enzyme for 10min, cool to room temperature, obtain a partially hydrolyzed liquid, concentrate under reduced pressure, freeze-drying to obtain 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 anhydrous 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, high speed shearing at 12000r / min for 5min, spray drying, pass through a 250 mesh screen to obtain fat-soluble vitamin mixed microparticles. The spray drying conditions are: inlet temperature 95℃, outlet temperature 60℃, feeding rate 8.5g / min.

[0081] Comparative Example 2

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

[0083] Mix 4.2 parts by weight of pea protein with 200 parts by weight of 0.2M phosphate buffer (pH 7.2) to obtain a pea protein solution; first treat the pea protein solution by high-voltage pulsed electric field for 30s, the field strength of the high-voltage pulsed electric field is 15kV / cm, the pulse number is 50 times, and the pulse width is 200μs, then treat the pea protein solution by dynamic high-pressure microjet circulation for 4 times, the pressure of the dynamic high-pressure microjet is 100MPa, and the temperature is 30℃, concentrate under reduced pressure, and freeze-drying to obtain 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 anhydrous 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, high speed shearing at 12000r / min for 5min, spray drying, pass through a 250 mesh screen to obtain fat-soluble vitamin mixed microparticles. The spray drying conditions are: inlet temperature 95℃, outlet temperature 60℃, feeding rate 8.5g / min.

[0085] Comparative Example 3

[0086] The difference between the present comparative example and example 1 is that the preparation method of the mixed microparticles of fat-soluble vitamins is different, which is specifically as follows: the preparation method of the mixed microparticles of fat-soluble vitamins comprises the following steps:

[0087] 8 parts by weight of vitamin A, 5 parts by weight of vitamin E acetate, 3 parts by weight of vitamin D3, and 2 parts by weight of vitamin K2 are mixed with 82 parts by weight of anhydrous ethanol to obtain material A; 30 parts by weight of gum arabic and 5 parts by weight of β-cyclodextrin are mixed with 160 parts by weight of water to obtain material B; the above-mentioned material A and material B are mixed, high-speed sheared at 12000 r / min for 5 min, spray dried, and sieved through a 250-mesh screen to obtain the mixed microparticles of fat-soluble vitamins. The spray drying conditions are: inlet temperature 95℃, outlet temperature 60℃, and feeding rate 8.5 g / min.

[0088] Comparative Example 4

[0089] The difference between the present comparative example and example 1 is that the preparation method of the mixed microparticles of fat-soluble vitamins is different, which is specifically as follows: the preparation method of the mixed microparticles of fat-soluble vitamins comprises the following steps:

[0090] 4.2 parts by weight of pea protein and 0.8 parts by weight of carrageenan are mixed with 200 parts by weight of 0.2M phosphate buffer (pH 7.2) and stirred at 40℃ and 100 r / min for 2h, then 0.03 parts by weight of neutral protease is added and enzymolysis is carried out at 55℃ for 25 min, the enzyme is inactivated by increasing the temperature to 85℃ for 10 min, and then the temperature is cooled to room temperature to obtain a partial enzymolysis liquid; the partial enzymolysis liquid is first treated by high-voltage pulsed electric field for 30 s, and then treated by dynamic high-pressure microfluidization for 4 times, wherein the high-voltage pulsed electric field has a field strength of 15 kV / cm and a pulse number of 50 times with a pulse width of 200 μs, and the dynamic high-pressure microfluidization has a pressure of 100 MPa and a temperature of 30℃; the mixture is concentrated under reduced pressure and freeze-dried to obtain a modified protein.

[0091] 8 parts by weight of vitamin A, 5 parts by weight of vitamin E acetate, 3 parts by weight of vitamin D3, and 2 parts by weight of vitamin K2 are mixed with 82 parts by weight of anhydrous ethanol to obtain material A; 30 parts by weight of gum arabic, 6 parts by weight of modified protein, and 160 parts by weight of water are mixed to obtain material B; the above-mentioned material A and material B are mixed, high-speed sheared at 12000 r / min for 5 min, spray dried, and sieved through a 250-mesh screen to obtain the mixed microparticles of fat-soluble vitamins. The spray drying conditions are: inlet temperature 95℃, outlet temperature 60℃, and feeding rate 8.5 g / min.

[0092] Comparative Example 5

[0093] The difference between the present comparative example and example 1 is that ascorbic acid palmitate is not added in step (2).

[0094] Comparative Example 6

[0095] The difference between this comparative example and Example 1 is that no tricalcium phosphate is added in step (3).

[0096] Performance test

[0097] The following performance tests were conducted on the vitamin premixes prepared in Examples 1-3 and Comparative Examples 1-6. The method for testing the mixing uniformity was as follows: 10 samples of each of the vitamin premixes prepared were randomly taken, the content of vitamin A in the samples was detected (reference standard GB 5009.82-2016), and the RSD was calculated to represent the mixing uniformity, RSD = standard deviation / average value x 100%; the smaller the value, the more uniform the mixing. The method for testing the flowability was as follows: each of the vitamin premixes prepared was taken and placed in a 100 mL plastic measuring cylinder, the bulk volume of the premix was measured, then the plastic measuring cylinder containing the premix was placed in a rotary shaker for tamping, the tapped volume of the premix was measured, and the compression degree was calculated to represent the flowability, compression degree = (bulk volume-tapped volume) / bulk volume x 100%; the smaller the value, the better the flowability. The method for testing the antioxidant stability was as follows: each of the vitamin premixes prepared was taken and placed in a 60°C oven for 2 weeks for accelerated oxidation experiment, the peroxide value of the premix before and after the experiment was measured (reference standard GB 5009.227-2023), and the oxidation rate was calculated to represent the stability, oxidation rate = (peroxide value after the experiment-initial peroxide value) / initial peroxide value x 100%; the smaller the value, the better the stability. The results of the performance tests are shown in Table 1.

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

[0099]

[0100] From the test results, it can be seen that the vitamin premixes prepared in Examples 1-3 have excellent mixing uniformity, fluidity and stability, especially the vitamin premix prepared in Example 1 has the best comprehensive performance, because the present application adds the self-prepared fat-soluble vitamin mixed microparticles prepared by the specific method, which further improves the mixing uniformity, fluidity and stability of the premix by the combined action of the mixed water-soluble vitamins, mixed minerals, vitamin C, tricalcium phosphate and the like. Compared with Example 1, the specific self-prepared fat-soluble vitamin mixed microparticles are not used in Comparative Examples 1-4, ascorbic acid palmitate is not used in the mixed minerals of Comparative Example 5, and tricalcium phosphate is not used in the final mixing stage of Comparative Example 6, and from the comparison of the above test results, it can be seen that the comprehensive performance of the prepared vitamin premixes all appears different degrees of decline. The above test results further prove the importance of the technical solutions in Examples 1-3 of the present application to the technical effects.

[0101] The above is the preferred embodiment of the present application, it should be pointed out that for the ordinary skilled in the art, without departing from the principles of the present application, can also make a number of improvements and refinements, these improvements and refinements should also be considered as the protection scope of the present application.

Claims

1. A process for the preparation of a vitamin premix, characterized in that, The preparation process comprises the following steps: (1) adding 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 malt dextrin and 20-40 parts of microcrystalline cellulose into a mixer to mix, to obtain mixed water-soluble vitamins; (2) adding 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 ascorbic acid palmitate into the mixer to mix, to obtain mixed minerals; (3) adding 10-30 parts of fat-soluble vitamin mixed microparticles, 5-15 parts of mixed water-soluble vitamins and 2-7 parts of mixed minerals into the mixer to mix, then adding 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 to continue mixing, and sieving, to obtain the vitamin premix; The preparation method of the fat-soluble vitamin mixed microparticles comprises the following steps: mixing pea protein, carrageenan and phosphate buffer, heating and stirring, then adding neutral protease, enzymolysis, enzyme inactivation, cooling, to obtain a partial enzymolysis liquid; subjecting the partial enzymolysis liquid to high-voltage pulsed electric field treatment first, then to dynamic high-pressure microjet circulation treatment, reducing pressure concentration, freeze-drying, to obtain modified protein; mixing vitamin A, vitamin E acetate, vitamin D3, vitamin K2 and anhydrous ethanol to obtain material A; mixing gum arabic, modified protein and β-cyclodextrin with water to obtain material B; mixing the above material A and material B, high-speed shearing, spray drying, sieving, to obtain fat-soluble vitamin mixed microparticles; the weight ratio of pea protein to carrageenan is 2-6:0.2-1.5; the weight ratio of neutral protease to pea protein is 0.01-0.05:2-6; the weight ratio of vitamin A to vitamin E acetate to vitamin D3 to vitamin K2 is 5-10:2-8:1-5:0.5-3; the weight ratio of gum arabic to modified protein to β-cyclodextrin is 20-40:3-10:4-6; the field strength of the high-voltage pulsed electric field is 10-20 kV / cm, the pulse number is 40-60 times, and the pulse width is 100-300 μs; the pressure of the dynamic high-pressure microjet is 80-120 MPa, and the temperature is 25-35 °C.

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

3. A vitamin premix, characterized in that, Prepared according to the preparation process in any one of claims 1-2. Prepared according to the preparation process in any one of claims 1-2.

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