A method for preparing VA microcapsule particles

Abstract

The application discloses a preparation method of VA microcapsule particles, and mainly forms a composite wall material through electrostatic interaction between gum arabic and plant polypeptides, and embeds VA essential oil by compounding with reducing sugar, and obtains the VA microcapsule particles after fluidized bed granulation, and in a specific temperature and humidity range, the reducing sugar in the VA microcapsule particles and the protein in the gum arabic / plant polypeptide composite wall material occur the Maillard reaction to obtain the final product. The VA microcapsule particles obtained by the application will be applied in tabletting products, and effectively improve the pressure resistance and storage stability of the products.

Description

Technical Field

[0001] This invention relates to a process for preparing VA microcapsules, and more particularly to a process for preparing VA microcapsules for gum arabic / plant polypeptide composite wall materials by high-temperature crosslinking after VA emulsion granulation. Background Technology

[0002] Vitamin A (VA) is a pale yellow, fat-soluble vitamin, primarily found in retinyl acetate and retinyl palmitate. Vitamin A plays a crucial role in human vision development, gene expression, and embryonic development and growth. Since the human body cannot synthesize vitamin A, it must be obtained through a regular diet. However, vitamin A has an unstable chemical structure and poor dispersibility in water. Therefore, it is typically encapsulated in water-soluble polymers to form microcapsules for addition to feed and food. Microencapsulation improves the dispersibility of vitamin A in water, increases its stability, and enhances its bioavailability.

[0003] Microencapsulation refers to the process of encapsulating solids, liquids, or gases in tiny, sealed capsules. Preparation typically involves emulsion formation and drying. An emulsion is a colloidal dispersion system consisting of small droplets of one fluid dispersed in another immiscible fluid. The dispersed fluid is called the dispersed phase, and the fluid being dispersed is called the continuous phase. Emulsion drying mainly includes spray drying and fluidized bed granulation. Spray drying is suitable for preparing water-soluble microcapsule powders, while fluidized bed granulation is suitable for microparticles. Microparticle products have better pressure resistance and storage stability than dry powder products.

[0004] The macromolecular emulsifiers used in the preparation of microparticle products mainly include gum arabic, gelatin, and modified starch. Gelatin products have stronger tableting stability than gum arabic and modified starch products, while modified starch has stronger emulsifying properties than both gum arabic and gelatin products. However, gelatin, as a wall material for fat-soluble vitamin preparations, poses a risk of animal-derived diseases, while modified starch microparticle products have poor pressure resistance. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to provide a method for preparing VA microcapsule particles, wherein the VA microcapsule particles obtained by the preparation method have high encapsulation efficiency and hardness, low surface oil content, and high tableting stability.

[0006] The technical solution of the present invention is as follows:

[0007] A method for preparing VA microcapsule particles includes the following steps:

[0008] (1) Dissolve gum arabic in hot water to obtain a gum arabic aqueous solution;

[0009] (2) Dissolve the plant polypeptide in hot water to obtain an aqueous solution of the plant polypeptide, and then add acid to acidify it to obtain an acidic aqueous solution of the plant polypeptide;

[0010] (3) Add the gum arabic aqueous solution obtained in step (1) to the acidic aqueous solution of plant polypeptide obtained in step (2), heat and stir evenly, then add reducing sugar, heat and stir evenly to obtain the wall material aqueous solution;

[0011] (4) Heat and melt the VA essential oil, then add the wall material aqueous solution obtained in step (3), and shear at high speed to obtain VA primary emulsion. Then add alkali to adjust the pH value to 5-6 to obtain VA emulsion.

[0012] (5) The VA emulsion obtained in step (4) is subjected to fluidized bed granulation to obtain VA microparticles, and then subjected to a further Maillard reaction to obtain the VA microcapsule microparticles.

[0013] In this invention, gum arabic and plant peptides form a soluble electrostatic complex, which effectively enhances the emulsifying properties of gum arabic, thereby improving the encapsulation effect and reducing surface oil in the microcapsules. At the same time, the gum arabic / plant peptide complex in the microparticles can undergo a hydroxylamine condensation reaction with reducing sugars, i.e., the Maillard reaction, thereby increasing the density of the wall material and improving the tableting stability of the product.

[0014] Preferably, the mass ratio of gum arabic to plant polypeptides is 3:3 to 5, and the mass ratio of gum arabic to reducing sugar is 3:2 to 4; most preferably, the mass ratio of gum arabic to plant polypeptides is 3:4, and the mass ratio of gum arabic to reducing sugar is 3:3.

[0015] Preferably, the VA essential oil comprises 35-45% of the total mass of gum arabic, plant polypeptides, and reducing sugars; more preferably, the VA essential oil comprises 40% of the total mass of gum arabic, plant polypeptides, and reducing sugars.

[0016] Preferably, in step (1), the temperature of the hot water is 55-65°C, and the mass percentage concentration of the gum arabic aqueous solution is 20-30%, more preferably 26.5%.

[0017] Preferably, in step (2), the plant polypeptide is any one or a mixture of several of soybean peptides, corn peptides and pea peptides in any proportion.

[0018] The temperature of the hot water used is 55-65℃, and the mass percentage concentration of the plant polypeptide aqueous solution is 30-35%; more preferably 32.4%.

[0019] The acid is selected from one or more of hydrochloric acid, sulfuric acid, and nitric acid; hydrochloric acid is preferred; the concentration of the hydrochloric acid is 10-14 mol / L, more preferably 12 mol / L; the pH value of the acidic aqueous solution of the plant polypeptide is 2-2.5, which is conducive to the formation of soluble electrostatic complexes and can effectively improve the emulsifying properties of gum arabic.

[0020] Preferably, in step (3), the heating and stirring temperature is 55-65°C and the stirring speed is 3-3.5 m / s, more preferably 3.14 m / s.

[0021] Preferably, in step (3), the reducing sugar is any one or a mixture of several of glucose, fructose, galactose, lactose, and maltose in any proportion.

[0022] Preferably, in step (4), the VA essential oil is heated to a temperature of 55-65°C;

[0023] The high-speed shearing speed is 9-10 m / s, more preferably 9.42 m / s; the high-speed shearing time is 20-30 min, more preferably 20 min.

[0024] Preferably, in step (4), the alkali is selected from one or more of sodium hydroxide and potassium hydroxide, with a concentration of 10-14 mol / L; the alkali is further preferably an aqueous solution of sodium hydroxide with a concentration of 10-14 mol / L, and even more preferably 12 mol / L.

[0025] Preferably, in step (5), the VA particles are 40-80 mesh in size and the weight loss of the VA particles is 8-12%.

[0026] Preferably, in step (5), the temperature of the fluidized bed is 25-30°C, the fluidization time is 10-15 min, and the weight loss of the VA particles is controlled to be 8-12%.

[0027] Preferably, in step (5), the Maillard reaction is carried out at a temperature of 70-80°C and the crosslinking time is 3-5 hours.

[0028] Compared with the prior art, the present invention has the following technical effects:

[0029] (1) The present invention uses plant polypeptides and gum arabic to form a soluble electrostatic complex under specific pH conditions, which effectively improves the emulsifying properties of gum arabic.

[0030] (2) The plant polypeptides used in this invention are plant-derived and do not pose a risk of animal-derived diseases compared to animal-derived proteins.

[0031] (3) The present invention is that the arabin / plant polypeptide complex in the microparticles undergoes a hydroxylamine condensation reaction with reducing sugar within a specific moisture content and temperature range, namely the Maillard reaction, which can effectively improve the pressure resistance and storage stability of the product.

[0032] (4) No chemical cross-linking curing agents, such as formaldehyde and glutaraldehyde, are used in this invention, making it green and safe. Detailed Implementation

[0033] Example 1

[0034] (1) Weigh out gum arabic and soybean peptides respectively and dissolve them in water at 60±5℃ to prepare a 26.5wt% gum arabic aqueous solution and a 32.4wt% soybean peptide aqueous solution, wherein the mass ratio of gum arabic: soybean peptide: glucose is 3:4:3;

[0035] (2) Weigh VA essential oil to 40% of the total mass of gum arabic, soybean peptides and glucose, heat it to 60℃±5℃ to melt it, and keep it warm;

[0036] (3) Add 12 mol / L hydrochloric acid to the soybean peptide aqueous solution in step (1) and adjust the pH to 2;

[0037] (4) The gum arabic aqueous solution from step (1) is added to the acidic aqueous solution of soybean peptides prepared in step (3), and stirred evenly at 60±5℃ with a stirring speed of 3.14m / s.

[0038] (5) Weigh out glucose and add it to the solution prepared in step (4), and stir until well mixed;

[0039] (6) Add the VA essential oil that has been kept warm in step (2) to the solution prepared in step (5), start high-speed shearing for 30 minutes, and stir at a speed of 9.42 m / s to obtain VA primary emulsion;

[0040] (7) Adjust the pH of the VA emulsion to 5-6 using a 12mol / L NaOH aqueous solution to obtain the VA emulsion;

[0041] (8) The VA emulsion prepared in step (7) is subjected to fluidized bed granulation to obtain VA microparticles, which are then sieved through a 40-80 mesh screen. The weight loss of the VA microparticles is 8%.

[0042] (9) Place the VA microparticles in a rotary evaporator and carry out the Maillard reaction at 70°C. After 5 hours, the VA microcapsule microparticle product is obtained.

[0043] Example 2

[0044] (1) Weigh out gum arabic and pea peptides respectively and dissolve them in water at 60±5℃ to prepare a 20.0wt% gum arabic aqueous solution and a 30.0wt% pea peptide aqueous solution, wherein the mass ratio of gum arabic:pea peptide:lactose is 3:3:2;

[0045] (2) Weigh VA essential oil to 35% of the total mass of gum arabic, pea peptides and lactose, heat it to 60±5℃ to melt it, and keep it warm;

[0046] (3) Add 12 mol / L hydrochloric acid to the pea peptide aqueous solution in step (1) and adjust the pH to 2;

[0047] (4) The gum arabic aqueous solution from step (1) is added to the pea peptide acidic aqueous solution prepared in step (3), and stirred evenly at 60±5℃ with a stirring speed of 3.50m / s.

[0048] (5) Weigh out lactose and add it to the solution prepared in step (4), and stir until well mixed;

[0049] (6) Add the VA essential oil that has been kept warm in step (2) to the solution prepared in step (5), start high-speed shearing for 20 minutes, and stir at a speed of 9.0 m / s to obtain VA primary emulsion;

[0050] (7) Adjust the pH of the VA emulsion to 5-6 using a 12mol / L NaOH aqueous solution to obtain the VA emulsion;

[0051] (8) The VA emulsion prepared in step (7) is subjected to fluidized bed granulation to obtain VA microparticles, which are then sieved through a 40-80 mesh screen. The weight loss of the VA microparticles is 8%.

[0052] (9) Place the VA microparticles in a rotary evaporator and allow the Maillard reaction to occur at 80°C. After 3 hours, the VA microcapsule microparticle product is obtained.

[0053] Example 3

[0054] (1) Weigh out gum arabic and corn peptide respectively and dissolve them in water at 60±5℃ to prepare a 30.0wt% gum arabic aqueous solution and a 35.0wt% corn peptide aqueous solution, wherein the mass ratio of gum arabic: corn peptide: glucose is 3:5:4;

[0055] (2) Weigh VA essential oil to 45% of the total mass of gum arabic, corn peptide and glucose, heat and melt it at 60±5℃ and keep it warm;

[0056] (3) Add 12 mol / L hydrochloric acid to the corn peptide aqueous solution in step (1) and adjust the pH to 2.5;

[0057] (4) The gum arabic aqueous solution from step (1) is added to the corn peptide aqueous solution prepared in step (3), and stirred evenly at 60±5℃ with a stirring speed of 3.0m / s.

[0058] (5) Weigh out glucose and add it to the solution prepared in step (4), and stir until well mixed;

[0059] (6) Add the VA essential oil that has been kept warm in step (2) to the solution prepared in step (5), start high-speed shearing for 30 minutes, and stir at a speed of 10.0 m / s to obtain VA primary emulsion;

[0060] (7) Adjust the pH of the VA emulsion to 5-6 using a 12mol / L NaOH aqueous solution to obtain the VA emulsion;

[0061] (8) The VA emulsion prepared in step (7) is subjected to fluidized bed granulation to obtain VA microparticles, which are then sieved through a 40-80 mesh screen. The weight loss of the VA microparticles is 12%.

[0062] (9) Place the VA microparticles in a rotary evaporator and carry out the Maillard reaction at 70°C. After 5 hours, the VA microcapsule microparticle product is obtained.

[0063] Example 4

[0064] (1) Weigh out gum arabic and soybean peptides respectively and dissolve them in water at 60±5℃ to prepare a 26.5wt% gum arabic aqueous solution and a 32.4wt% soybean peptide aqueous solution, wherein the mass ratio of gum arabic: soybean peptide: glucose is 3:4:3;

[0065] (2) Weigh VA essential oil to 40% of the total mass of gum arabic, soybean peptides and glucose, heat it to 60±5℃ to melt it, and keep it warm;

[0066] (3) Add 12 mol / L hydrochloric acid to the soybean peptide aqueous solution in step (1) and adjust the pH to 2.5;

[0067] (4) The gum arabic aqueous solution from step (1) is added to the acidic soybean peptide aqueous solution prepared in step (3), and stirred evenly at 60±5℃ with a stirring speed of 3.0m / s.

[0068] (5) Weigh out glucose and add it to the solution prepared in step (4), and stir until well mixed;

[0069] (6) Add the VA essential oil that has been kept warm in step (2) to the solution prepared in step (5), start high-speed shearing for 30 minutes, and stir at a speed of 9.0 m / s to obtain VA primary emulsion;

[0070] (7) Adjust the pH of the VA emulsion to 5-6 using a 12mol / L NaOH aqueous solution to obtain the VA emulsion;

[0071] (8) The VA emulsion prepared in step (7) is subjected to fluidized bed granulation to obtain VA microparticles, which are then sieved through a 40-80 mesh screen. The weight loss of the VA microparticles is 8%.

[0072] (9) Place the VA microparticles in a rotary evaporator and carry out the Maillard reaction at 70°C. After 5 hours, the VA microcapsule microparticle product is obtained.

[0073] Example 5

[0074] (1) Weigh out gum arabic and soybean peptides respectively and dissolve them in water at 60±5℃ to prepare a 26.5wt% gum arabic aqueous solution and a 32.4wt% soybean peptide aqueous solution, wherein the mass ratio of gum arabic: soybean peptide: glucose is 3:4:3;

[0075] (2) Weigh VA essential oil to 40% of the total mass of gum arabic, soybean peptides and glucose, heat it to 60±5℃ to melt it, and keep it warm;

[0076] (3) Add 12 mol / L hydrochloric acid to the soybean peptide aqueous solution in step (1) and adjust the pH to 2.3;

[0077] (4) The gum arabic aqueous solution from step (1) is added to the acidic soybean peptide aqueous solution prepared in step (3), and stirred evenly at 60±5℃ with a stirring speed of 3.0m / s.

[0078] (5) Weigh out glucose and add it to the solution prepared in step (4), and stir until well mixed;

[0079] (6) Add the VA essential oil that has been kept warm in step (2) to the solution prepared in step (5), start high-speed shearing for 30 minutes, and stir at a speed of 9.0 m / s to obtain VA primary emulsion;

[0080] (7) Adjust the pH of the VA emulsion to 5-6 using a 12mol / L NaOH aqueous solution to obtain the VA emulsion;

[0081] (8) The VA emulsion prepared in step (7) is subjected to fluidized bed granulation to obtain VA microparticles, which are then sieved through a 40-80 mesh screen. The weight loss of the VA microparticles is 8%.

[0082] (9) Place the VA microparticles in a rotary evaporator and carry out the Maillard reaction at 70°C. After 5 hours, the VA microcapsule microparticle product is obtained.

[0083] Example 6

[0084] (1) Weigh out gum arabic and soybean peptides respectively and dissolve them in water at 60±5℃ to prepare a 26.5wt% gum arabic aqueous solution and a 32.4wt% soybean peptide aqueous solution, wherein the mass ratio of gum arabic: soybean peptide: glucose is 3:4:2;

[0085] (2) Weigh VA essential oil to 40% of the total mass of gum arabic, soybean peptides and glucose, heat it to 60±5℃ to melt it, and keep it warm;

[0086] (3) Add 12 mol / L hydrochloric acid to the soybean peptide aqueous solution in step (1) and adjust the pH to 2.0;

[0087] (4) The gum arabic aqueous solution from step (1) is added to the acidic soybean peptide aqueous solution prepared in step (3), and stirred evenly at 60±5℃ with a stirring speed of 3.0m / s.

[0088] (5) Weigh out glucose and add it to the solution prepared in step (4), and stir until well mixed;

[0089] (6) Add the VA essential oil that has been kept warm in step (2) to the solution prepared in step (5), start high-speed shearing for 30 minutes, and stir at a speed of 9.0 m / s to obtain VA primary emulsion;

[0090] (7) Adjust the pH of the VA emulsion to 5-6 using a 12mol / L NaOH aqueous solution to obtain the VA emulsion;

[0091] (8) The VA emulsion prepared in step (7) is subjected to fluidized bed granulation to obtain VA microparticles, which are then sieved through a 40-80 mesh screen. The weight loss of the VA microparticles is 8%.

[0092] (9) Place the VA microparticles in a rotary evaporator and carry out the Maillard reaction at 70°C. After 5 hours, the VA microcapsule microparticle product is obtained.

[0093] Example 7

[0094] (1) Weigh out gum arabic and soybean peptides respectively and dissolve them in water at 60±5℃ to prepare a 26.5wt% gum arabic aqueous solution and a 32.4wt% soybean peptide aqueous solution, wherein the mass ratio of gum arabic: soybean peptide: glucose is 3:4:3.5;

[0095] (2) Weigh VA essential oil to 40% of the total mass of gum arabic, soybean peptides and glucose, heat it to 60±5℃ to melt it, and keep it warm;

[0096] (3) Add 12 mol / L hydrochloric acid to the soybean peptide aqueous solution in step (1) and adjust the pH to 2.0;

[0097] (4) The gum arabic aqueous solution from step (1) is added to the acidic soybean peptide aqueous solution prepared in step (3), and stirred evenly at 60±5℃ with a stirring speed of 3.0m / s.

[0098] (5) Weigh out glucose and add it to the solution prepared in step (4), and stir until well mixed;

[0099] (6) Add the VA essential oil that has been kept warm in step (2) to the solution prepared in step (5), start high-speed shearing for 30 minutes, and stir at a speed of 9.0 m / s to obtain VA primary emulsion;

[0100] (7) Adjust the pH of the VA emulsion to 5-6 using a 12mol / L NaOH aqueous solution to obtain the VA emulsion;

[0101] (8) The VA emulsion prepared in step (7) is subjected to fluidized bed granulation to obtain VA microparticles, which are then sieved through a 40-80 mesh screen. The weight loss of the VA microparticles is 8%.

[0102] (9) Place the VA microparticles in a rotary evaporator and carry out the Maillard reaction at 70°C. After 5 hours, the VA microcapsule microparticle product is obtained.

[0103] Example 8

[0104] (1) Weigh out gum arabic and soybean peptides respectively and dissolve them in water at 60±5℃ to prepare a 26.5wt% gum arabic aqueous solution and a 32.4wt% soybean peptide aqueous solution, wherein the mass ratio of gum arabic: soybean peptide: glucose is 3:4:4;

[0105] (2) Weigh VA essential oil to 40% of the total mass of gum arabic, soybean peptides and glucose, heat it to 60±5℃ to melt it, and keep it warm;

[0106] (3) Add 12 mol / L hydrochloric acid to the soybean peptide aqueous solution in step (1) and adjust the pH to 2.0;

[0107] (4) The gum arabic aqueous solution from step (1) is added to the acidic soybean peptide aqueous solution prepared in step (3), and stirred evenly at 60±5℃ with a stirring speed of 3.0m / s.

[0108] (5) Weigh out glucose and add it to the solution prepared in step (4), and stir until well mixed;

[0109] (6) Add the VA essential oil that has been kept warm in step (2) to the solution prepared in step (5), start high-speed shearing for 30 minutes, and stir at a speed of 9.0 m / s to obtain VA primary emulsion;

[0110] (7) Adjust the pH of the VA emulsion to 5-6 using a 12mol / L NaOH aqueous solution to obtain the VA emulsion;

[0111] (8) The VA emulsion prepared in step (7) is subjected to fluidized bed granulation to obtain VA microparticles, which are then sieved through a 40-80 mesh screen. The weight loss of the VA microparticles is 8%.

[0112] (9) Place the VA microparticles in a rotary evaporator and carry out the Maillard reaction at 70°C. After 5 hours, the VA microcapsule microparticle product is obtained.

[0113] Example 9

[0114] (1) Weigh out gum arabic and soybean peptides respectively and dissolve them in water at 60±5℃ to prepare a 26.5wt% gum arabic aqueous solution and a 32.4wt% soybean peptide aqueous solution, wherein the mass ratio of gum arabic: soybean peptide: glucose is 3:4:3;

[0115] (2) Weigh VA essential oil to 40% of the total mass of gum arabic, soybean peptides and glucose, heat it to 60±5℃ to melt it, and keep it warm;

[0116] (3) Add 12 mol / L hydrochloric acid to the soybean peptide aqueous solution in step (1) and adjust the pH to 2.0;

[0117] (4) The gum arabic aqueous solution from step (1) is added to the acidic soybean peptide aqueous solution prepared in step (3), and stirred evenly at 60±5℃ with a stirring speed of 3.0m / s.

[0118] (5) Weigh out glucose and add it to the solution prepared in step (4), and stir until well mixed;

[0119] (6) Add the VA essential oil that has been kept warm in step (2) to the solution prepared in step (5), start high-speed shearing for 30 minutes, and stir at a speed of 9.0 m / s to obtain VA primary emulsion;

[0120] (7) Adjust the pH of the VA emulsion to 5-6 using a 12mol / L NaOH aqueous solution to obtain the VA emulsion;

[0121] (8) The VA emulsion prepared in step (7) is subjected to fluidized bed granulation to obtain VA microparticles, which are then sieved through a 40-80 mesh screen. The weight loss of the VA microparticles is 9%.

[0122] (9) Place the VA microparticles in a rotary evaporator and carry out the Maillard reaction at 70°C. After 5 hours, the VA microcapsule microparticle product is obtained.

[0123] Example 10

[0124] (1) Weigh out gum arabic and soybean peptides respectively and dissolve them in water at 60±5℃ to prepare a 26.5wt% gum arabic aqueous solution and a 32.4wt% soybean peptide aqueous solution, wherein the mass ratio of gum arabic: soybean peptide: glucose is 3:4:3;

[0125] (2) Weigh VA essential oil to 40% of the total mass of gum arabic, soybean peptides and glucose, heat it to 60±5℃ to melt it, and keep it warm;

[0126] (3) Add 12 mol / L hydrochloric acid to the soybean peptide aqueous solution in step (1) and adjust the pH to 2.0;

[0127] (4) The gum arabic aqueous solution from step (1) is added to the acidic soybean peptide aqueous solution prepared in step (3), and stirred evenly at 60±5℃ with a stirring speed of 3.0m / s.

[0128] (5) Weigh out glucose and add it to the solution prepared in step (4), and stir until well mixed;

[0129] (6) Add the VA essential oil that has been kept warm in step (2) to the solution prepared in step (5), start high-speed shearing for 30 minutes, and stir at a speed of 9.0 m / s to obtain VA primary emulsion;

[0130] (7) Adjust the pH of the VA emulsion to 5-6 using a 12mol / L NaOH aqueous solution to obtain the VA emulsion;

[0131] (8) The VA emulsion prepared in step (7) is subjected to fluidized bed granulation to obtain VA microparticles, which are then sieved through a 40-80 mesh screen. The weight loss of the VA microparticles is 11%.

[0132] (9) Place the VA microparticles in a rotary evaporator and carry out the Maillard reaction at 70°C. After 5 hours, the VA microcapsule microparticle product is obtained.

[0133] Comparative Example 1

[0134] (1) Weigh out gum arabic and glucose in a mass ratio of 3:7, dissolve them in water at 60±5℃, and prepare a 37.5wt% aqueous solution;

[0135] (2) Weigh VA essential oil to 40% of the total mass of gum arabic and glucose, heat it to 60±5℃ to melt it, and keep it warm;

[0136] (3) Add the VA essential oil that has been kept warm in step (2) to the solution prepared in step (1), and start high-speed shearing for 20 minutes to obtain VA primary emulsion;

[0137] (4) The VA emulsion prepared in step (3) is subjected to fluidized bed granulation to obtain VA microparticles, which are then sieved through a 40-80 mesh screen.

[0138] Comparative Example 2

[0139] (1) Weigh out gum arabic and glucose in a mass ratio of 3:7, dissolve them in water at 60±5℃, and prepare a 37.5wt% aqueous solution;

[0140] (2) Weigh VA essential oil to 40% of the total mass of gum arabic and glucose, heat it to 60±5℃ to melt it, and keep it warm;

[0141] (3) Add the VA essential oil that has been kept warm in step (2) to the solution prepared in step (1), and start high-speed shearing for 20 minutes to obtain VA primary emulsion;

[0142] (4) The VA emulsion prepared in step (3) is subjected to fluidized bed granulation to obtain VA microparticles, which are then sieved through a 40-80 mesh screen.

[0143] (5) Place the VA microparticles in a rotary evaporator and allow the Maillard reaction to occur at 75±5℃. After 5 hours, VA microcapsule microparticles are obtained.

[0144] Comparative Example 3

[0145] (1) Weigh out gum arabic and soybean peptides respectively and dissolve them in water at 60±5℃ to prepare a 26.5wt% gum arabic aqueous solution and a 32.4wt% soybean peptide aqueous solution, wherein the mass ratio of gum arabic: soybean peptide: glucose is 3:4:3;

[0146] (2) Weigh VA essential oil to 40% of the total mass of gum arabic, soybean peptides and glucose, heat it to 60±5℃ to melt it, and keep it warm;

[0147] (3) Add 12 mol / L hydrochloric acid to the soybean peptide aqueous solution in step (1) and adjust the pH to 2;

[0148] (4) Add the gum arabic aqueous solution from step (1) to the soybean peptide aqueous solution prepared in step (3) and stir evenly at 60±5℃;

[0149] (5) Weigh out glucose and add it to the solution prepared in step (4), and stir until well mixed;

[0150] (6) Add the VA essential oil that has been kept warm in step (2) to the solution prepared in step (5), and start high-speed shearing for 20 minutes to obtain VA primary emulsion;

[0151] (7) Adjust the pH of the VA emulsion to 5-6 using a 12mol / L NaOH aqueous solution to obtain the VA emulsion;

[0152] (8) The VA emulsion prepared in step (7) is subjected to fluidized bed granulation to obtain VA microparticles, which are then sieved through a 40-80 mesh screen.

[0153] Comparative Example 4

[0154] (1) Weigh out gum arabic and soybean peptides respectively and dissolve them in water at 60±5℃ to prepare a 26.5wt% gum arabic aqueous solution and a 32.4wt% soybean peptide aqueous solution, wherein the mass ratio of gum arabic: soybean peptide: glucose is 3:4:3;

[0155] (2) Weigh VA essential oil to 40% of the total mass of gum arabic, soybean peptides and glucose, heat it to 60℃±5℃ to melt it, and keep it warm;

[0156] (3) Add 12 mol / L hydrochloric acid to the soybean peptide aqueous solution in step (1) and adjust the pH to 3;

[0157] (4) The gum arabic aqueous solution from step (1) is added to the acid soybean peptide aqueous solution prepared in step (3), and stirred evenly at 60±5℃ with a stirring speed of 3m / s.

[0158] (5) Weigh out glucose and add it to the solution prepared in step (4), and stir until well mixed;

[0159] (6) Add the VA essential oil that has been kept warm in step (2) to the solution prepared in step (5), start high-speed shearing for 30 minutes, and stir at a speed of 9 m / s to obtain VA primary emulsion;

[0160] (7) Adjust the pH of the VA emulsion to 5-6 using NaOH aqueous solution to obtain the VA emulsion;

[0161] (8) The VA emulsion prepared in step (7) is subjected to fluidized bed granulation to obtain VA microparticles, which are then sieved through a 40-80 mesh screen. The weight loss of the VA microparticles is 8%.

[0162] (9) Place the VA microparticles in a rotary evaporator and carry out the Maillard reaction at 70°C. After 5 hours, the VA microcapsule microparticle product is obtained.

[0163] Comparative Example 5

[0164] (1) Weigh out gum arabic and soybean peptides respectively and dissolve them in water at 60±5℃ to prepare a 26.5wt% gum arabic aqueous solution and a 32.4wt% soybean peptide aqueous solution, wherein the mass ratio of gum arabic: soybean peptide: glucose is 3:4:3;

[0165] (2) Weigh VA essential oil to 40% of the total mass of gum arabic, soybean peptides and glucose, heat it to 60℃±5℃ to melt it, and keep it warm;

[0166] (3) Add hydrochloric acid to the soybean peptide aqueous solution from step (1) and adjust the pH to 2;

[0167] (4) The gum arabic aqueous solution from step (1) is added to the acid soybean peptide aqueous solution prepared in step (3), and stirred evenly at 60±5℃ with a stirring speed of 3m / s.

[0168] (5) Weigh out glucose and add it to the solution prepared in step (4), and stir until well mixed;

[0169] (6) Add the VA essential oil that has been kept warm in step (2) to the solution prepared in step (5), start high-speed shearing for 30 minutes, and stir at a speed of 9 m / s to obtain VA primary emulsion;

[0170] (7) Adjust the pH of the VA emulsion to 5-6 using a 12mol / L NaOH aqueous solution to obtain the VA emulsion;

[0171] (8) The VA emulsion prepared in step (7) is subjected to fluidized bed granulation to obtain VA microparticles, which are then sieved through a 40-80 mesh screen. The weight loss of the VA microparticles is 15%.

[0172] (9) Place the VA microparticles in a rotary evaporator and carry out the Maillard reaction at 70°C. After 5 hours, the VA microcapsule microparticle product is obtained.

[0173] Example 11

[0174] (1) Weigh out gum arabic and soybean peptides respectively and dissolve them in water at 60±5℃ to prepare a 26.5wt% gum arabic aqueous solution and a 32.4wt% soybean peptide aqueous solution, wherein the mass ratio of gum arabic: soybean peptide: glucose is 3:4:3;

[0175] (2) Weigh VA essential oil to 40% of the total mass of gum arabic, soybean peptides and glucose, heat it to 60℃±5℃ to melt it, and keep it warm;

[0176] (3) Add 12 mol / L hydrochloric acid to the soybean peptide aqueous solution in step (1) and adjust the pH to 2;

[0177] (4) The gum arabic aqueous solution from step (1) is added to the acidic soybean peptide aqueous solution prepared in step (3), and stirred evenly at 60±5℃ with a stirring speed of 3m / s.

[0178] (5) Weigh out glucose and add it to the solution prepared in step (4), and stir until well mixed;

[0179] (6) Add the VA essential oil that has been kept warm in step (2) to the solution prepared in step (5), start high-speed shearing for 30 minutes, and stir at a speed of 9 m / s to obtain VA primary emulsion;

[0180] (7) Adjust the pH of the VA emulsion to 5-6 using a 12mol / L NaOH aqueous solution to obtain the VA emulsion;

[0181] (8) The VA emulsion prepared in step (7) is subjected to fluidized bed granulation to obtain VA microparticles, which are then sieved through a 40-80 mesh screen. The weight loss of the VA microparticles is 8%.

[0182] (9) Place the VA microparticles in a rotary evaporator and carry out the Maillard reaction at 70°C. After 6 hours, the VA microcapsule microparticle product is obtained.

[0183] Table 1 shows the encapsulation efficiency, surface oil content, hardness, and tablet retention rate of the VA microcapsules obtained in Examples 1-11 and Comparative Examples 1-5.

[0184] Table 1

[0185]

[0186]

[0187] The results of Comparative Example 4 show that, with other conditions unchanged, an excessively high pH value in the acidic aqueous solution of plant polypeptides can also lead to a decrease in the encapsulation efficiency, surface oil content, hardness, and other properties of VA microcapsules. The results of Comparative Example 5 show that excessive weight loss during fluidized bed granulation can also lead to a decrease in various properties of VA microcapsules.

[0188] The test methods involved in Table 1 are as follows:

[0189] Methods for measuring surface oil and embedding rate using ultraviolet spectrophotometry:

[0190] 1. Standard curve preparation: Weigh VA standard into a 100mL volumetric flask, add cyclohexane and sonicate to dissolve, then cool and dilute to volume. Transfer 5mL to a 50mL volumetric flask and dilute to volume with isopropanol. Measure the absorbance at 294nm wavelength and plot a standard curve of concentration versus absorbance.

[0191] 2. Sample Preparation: Weigh 0.5g of sample into a centrifuge tube, add 50mL of cyclohexane to the sample using a graduated cylinder, shake and extract for 10min. Filter the extract using a 0.45μm filter to obtain the filtrate. Transfer 10mL of the filtrate to a 50mL volumetric flask, dilute to volume with isopropanol, and measure the absorbance at 294nm. Calculate the VA concentration based on the standard curve of concentration versus absorbance.

[0192] Calculation formula:

[0193]

[0194]

[0195] Method for testing the hardness of VA samples using a texture analyzer:

[0196] Test procedure: TPA-25N

[0197] Parameter settings: Time: 2s

[0198] Measuring range: 25N

[0199] Probe recovery height: 30mm

[0200] Deformation: 100%

[0201] Detection speed: 60mm / min

[0202] Starting force: 0.05N

[0203] After setting the above parameters, the VA sample is tested, and the hardness index can be obtained directly.

Claims

1. A method for preparing VA microcapsule particles, characterized in that, Includes the following steps: (1) Dissolve gum arabic in hot water to obtain a gum arabic aqueous solution; (2) Dissolve the plant polypeptide in hot water to obtain an aqueous solution of the plant polypeptide, and then add acid to acidify it to obtain an acidic aqueous solution of the plant polypeptide; The acid is selected from one or more of hydrochloric acid, sulfuric acid, and nitric acid, and the hydrogen ion concentration is 10-14 mol / L; The pH value of the acidic aqueous solution of the plant polypeptide is 2 to 2.5; (3) Add the gum arabic aqueous solution obtained in step (1) to the acidic aqueous solution of plant polypeptide obtained in step (2), heat and stir evenly, then add reducing sugar, heat and stir evenly to obtain the wall material aqueous solution; The mass ratio of gum arabic to plant polypeptides is 3:3-5; (4) Heat and melt the VA essential oil, then add the wall material aqueous solution obtained in step (3), and shear at high speed to obtain VA primary emulsion. Then add alkali to adjust the pH value to 5-6 to obtain VA emulsion. (5) The VA emulsion obtained in step (4) is subjected to fluidized bed granulation to obtain VA microparticles, and then subjected to a further Maillard reaction to obtain the VA microcapsule microparticles. In step (5), the VA particles are 40-80 mesh in size and the weight loss of the VA particles is 8-12%. In step (5), the Maillard reaction is carried out at a temperature of 70-80°C and the crosslinking time is 3-5 hours.

2. The method for preparing VA microcapsule particles according to claim 1, characterized in that, The mass ratio of gum arabic to reducing sugar is 3:2-4; The VA essential oil comprises 35-45% of the total mass of gum arabic, plant polypeptides, and reducing sugars.

3. The method for preparing VA microcapsule particles according to claim 1, characterized in that, In step (1), the temperature of the hot water is 55-65°C, and the mass percentage concentration of the gum arabic aqueous solution is 20-30%.

4. The method for preparing VA microcapsule particles according to claim 1, characterized in that, In step (2), the plant polypeptide is any one or a mixture of several of soybean peptides, corn peptides and pea peptides in any proportion; The temperature of the hot water used is 55-65℃, and the mass percentage concentration of the plant polypeptide aqueous solution is 30-35%. The acid is hydrochloric acid, and the concentration of the hydrochloric acid is 10-14 mol / L.

5. The method for preparing VA microcapsule particles according to claim 1, characterized in that, In step (3), the heating and stirring temperature is 55-65℃ and the stirring speed is 3-3.5m / s.

6. The method for preparing VA microcapsule particles according to claim 1, characterized in that, In step (3), the reducing sugar is any one or a mixture of several of glucose, fructose, galactose, lactose and maltose in any proportion.

7. The method for preparing VA microcapsule particles according to claim 1, characterized in that, In step (4), the VA essential oil is heated to a temperature of 55-65℃; The high-speed shearing speed is 9–10 m / s, and the high-speed shearing time is 20–30 min.

8. The method for preparing VA microcapsule particles according to claim 1, characterized in that, In step (4), the alkali is selected from one or more of sodium hydroxide and potassium hydroxide, and the concentration is 10-14 mol / L.

9. The method for preparing VA microcapsule particles according to claim 1, characterized in that, In step (4), the alkali is an aqueous solution of sodium hydroxide with a concentration of 10-14 mol / L.

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