CN110693848B - Vitamin A microcapsule preparation without antioxidant and preparation method thereof - Google Patents

Vitamin A microcapsule preparation without antioxidant and preparation method thereof Download PDF

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CN110693848B
CN110693848B CN201911026965.7A CN201911026965A CN110693848B CN 110693848 B CN110693848 B CN 110693848B CN 201911026965 A CN201911026965 A CN 201911026965A CN 110693848 B CN110693848 B CN 110693848B
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vitamin
preparation
parts
sodium
starch
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CN110693848A (en
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任翔
徐玉涛
田中乐
吴文忠
陈剑彬
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Innobio Corp ltd
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/5005—Wall or coating material
    • A61K9/5021—Organic macromolecular compounds
    • A61K9/5052—Proteins, e.g. albumin
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/10—Organic substances
    • A23K20/174—Vitamins
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K40/00—Shaping or working-up of animal feeding-stuffs
    • A23K40/30—Shaping or working-up of animal feeding-stuffs by encapsulating; by coating
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/15—Vitamins
    • A23L33/155—Vitamins A or D
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/30—Encapsulation of particles, e.g. foodstuff additives
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00—Medicinal preparations containing organic active ingredients
    • A61K31/045—Hydroxy compounds, e.g. alcohols; Salts thereof, e.g. alcoholates
    • A61K31/07—Retinol compounds, e.g. vitamin A
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/5005—Wall or coating material
    • A61K9/5021—Organic macromolecular compounds
    • A61K9/5036—Polysaccharides, e.g. gums, alginate; Cyclodextrin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P3/00—Drugs for disorders of the metabolism
    • A61P3/02—Nutrients, e.g. vitamins, minerals
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

Abstract

The preparation method comprises the steps of raw material preparation, water phase preparation, oil phase preparation, emulsion preparation, spray drying and the like, wherein the raw materials comprise the following components in parts by mass: 50-70 parts of vitamin A, 5-25 parts of sodium starch octenyl succinate, 5-20 parts of Arabic gum, 1-5 parts of vitamin E polyethylene glycol succinate, 0.1-2 parts of acidity regulator, 0.1-1 part of glucose oxidase and 0-1.5 parts of anticaking agent. The invention adopts microencapsulation technology to embed vitamin A, and obtains vitamin A microcapsule powder with no antioxidant, high oil loading, high embedding rate, high bioavailability and high stability by spray drying.

Description

Vitamin A microcapsule preparation without antioxidant and preparation method thereof
Technical Field
The invention belongs to the technical field of microcapsules, and particularly relates to a preparation method of an antioxidant-free high-bioavailability high-stability vitamin A microcapsule preparation.
Background
Vitamin a was the first discovery and is also an extremely important, highly deficient, fat-soluble vitamin essential for maintaining normal metabolism and function in humans. Vitamin a is not a single compound but a series of retinol derivatives including retinol, retinal, retinoic acid, retinol acetate, retinol palmitate and the like.
Vitamin a belongs to fat-soluble vitamins, and can be dissolved in most organic solvents to different degrees, but is not dissolved in water. Vitamin a and its derivatives are readily oxidized and isomerized, especially when exposed to light (especially uv), oxygen, reactive metals, and high temperature environments, which can accelerate such oxidative destruction. But generally the cooking process does not cause too much damage to the vitamin a in the food. Under ideal conditions, such as low temperature freezing, the retinoid remains stable in serum, tissue or crystalline form for a long period of time. Retinal is relatively stable to base under anaerobic conditions, but is unstable in acid and can undergo dehydrogenation or rearrangement of double bonds. During the rancidity process, the vitamin A and carotene contained in the oil can be seriously damaged.
Therefore, many enterprises, scientific research institutions, and the like research and develop steady-state preparations of vitamin a, and it is desired to make vitamin a more stable.
CN201010101199.9 discloses a method for preparing a continuous stable vitamin A microcapsule, which comprises the steps of continuously adding vitamin A crystals and an antioxidant into a crystallization melter in proportion under the protection of nitrogen to prepare antioxidant-containing vitamin A molten oil; then the melted oil is sent into a supergravity rotating packed bed emulsifier with a liquid distributor by a pump, and simultaneously the aqueous solution containing the modified starch capable of being gelatinized is sent into the supergravity rotating packed bed emulsifier by the pump after being deoxidized, and vitamin A emulsion is obtained at an outlet; continuously atomizing the emulsion, spraying the emulsion into a cooled starch bed for granulation, and then carrying out fluidized drying and gelation treatment in a fluidized bed with nitrogen as a drying medium to obtain the stable vitamin A microcapsule. The present invention has the advantages of continuous production, good embedding effect and high product storing stability.
CN201110142580.4 discloses a preparation method of a vitamin A microcapsule nutrition enhancer for beverages, which mainly adopts sodium caseinate as a main wall material to embed VA palmitate, and adopts micromolecular maltodextrin and white granulated sugar to fill, and mainly emphasizes the oxygen-free production process, the filling of protective gas and the stability of products.
CN201710637373.3 discloses a fat-soluble nutrient microcapsule and a preparation method thereof, the preparation method of the fat-soluble nutrient microcapsule comprises emulsification and granulation processes, wherein the emulsification is performed in a cavitation emulsifier, and the preparation method can reduce the loss of nutrient active substances of the fat-soluble nutrient microcapsule and has high stability.
CN201811312455.1 discloses octenyl succinic acid starch ester, fat-soluble nutrient microcapsules, a preparation method and application thereof, wherein the preparation method of the octenyl succinic acid starch ester comprises the following steps: and carrying out esterification reaction on gelatinized starch and octenyl succinic anhydride in the cavitation emulsification process to obtain the octenyl succinic acid starch ester. The preparation method promotes and strengthens esterification reaction through a cavitation emulsification process, so that starch and octenyl succinic anhydride in a gelatinized state are remarkably substituted in a crystalline region and an amorphous region of the starch due to aggravation of molecular collision, and the esterification rate of the prepared octenyl succinic acid starch ester is further improved, thereby greatly improving the emulsification performance. The method is rapid and efficient, a hydrolysis step is not needed after esterification, the problems that molecular chains are damaged to different degrees due to hydrolysis, the chain length and the content of amylose are obviously reduced, and further the density of the formed film of the octenyl succinic acid starch ester is reduced, and the formed film is easy to absorb moisture, crisp and heat-conducting are solved, and the application performance of the method is improved.
CN 109452467A discloses a vitamin A microcapsule and a preparation method and application thereof, wherein ascorbic acid palmitate and carnosic acid are used as an antioxidant after choline and/or choline derivatives are pretreated, and unexpected synergistic effect is achieved among the components on the stability of vitamin A in feed or feed premix. It is also found that the vitamin A can maintain the optimal stability when the pH value is between 6.0 and 7.5, therefore, the invention can provide the optimal storage environment for the vitamin A by controlling the pH value of the vitamin A emulsion to be between 6.0 and 7.5 in the preparation process of the vitamin A microcapsule.
There are also many prior art studies that disclose microencapsulation of vitamin A, but these prior art techniques have relied on antioxidants to improve the stability of vitamin A. Also, although vitamin a stability after microencapsulation is improved, no prior art discloses data relating to its bioavailability. Embedding stability is the goal of our pursuit, but whether excessive embedding will affect vitamin A metabolism in vivo is also a concern.
Disclosure of Invention
The present invention aims to provide a vitamin microcapsule formulation stably embedded and having excellent release metabolism characteristics, and it is expected to realize stabilization treatment of the formulation by means of component optimization instead of using an antioxidant. Therefore, the invention firstly provides a preparation method of an antioxidant-free vitamin A microcapsule preparation, which comprises the following steps:
(1) preparing a raw material, wherein the raw material comprises the following components in parts by mass:
Figure BDA0002248962390000021
Figure BDA0002248962390000031
(2) sequentially dispersing modified starch and Arabic gum in water at 60-80 deg.C, stirring to dissolve completely, and cooling to 30-40 deg.C;
(3) adding an acidity regulator into the system obtained in the step (2), controlling the pH value to be 6-8, uniformly stirring, and adding glucose oxidase to obtain a water phase;
(4) adding vitamin E polyethylene glycol succinate into vitamin A, heating to melt at 60-80 deg.C, stirring, mixing, and cooling to 30-40 deg.C to obtain oil phase;
(5) slowly adding the oil phase into the water phase, and stirring at 30-40 ℃ until the oil phase and the water phase are uniformly mixed;
(6) shearing and emulsifying the mixture obtained in the step (5) for 0.5-1h, and then homogenizing for 2 times at 40-70MPa to obtain emulsion;
(7) and (3) spray drying the emulsion prepared in the step (6): the air inlet temperature is 80-210 ℃, and the air outlet temperature is 70-120 ℃; the product is sieved and then is uniformly mixed with an anticaking agent.
The invention adopts a microencapsulation process to embed the vitamin A, and obtains a vitamin A microcapsule powder product without antioxidant, with high oil loading, high embedding rate, high bioavailability and high stability through specific material combination and preparation process. Can be widely applied to the fields of feed, dietary supplement, daily chemical, medicine and the like.
Detailed Description
The invention provides a high-bioavailability high-vitamin A microcapsule preparation which realizes high stability independent of an antioxidant. The selection and combination of raw materials and the operation scheme adapted to the raw materials are the core technical means for realizing the technical effect of the invention. In the preparation method of the microcapsule preparation product, the raw materials comprise, by mass, 50-70 parts of vitamin A, 5-25 parts of modified starch, 5-20 parts of Arabic gum, 1-5 parts of vitamin E succinic acid polyethylene glycol ester, 0.1-1 part of glucose oxidase, 0.1-2 parts of acidity regulator and 0-1.5 parts of anticaking agent.
The vitamin a in the feed is typically crystalline and is selected from vitamin a acetate, vitamin a palmitate or mixtures thereof.
The modified starch in the raw material is selected from one or a mixture of more of sodium starch octenylsuccinate, acetylated distarch, carboxyl starch and phosphorylated starch. Sodium starch octenylsuccinate and phosphorylated starches are preferred.
The acidity regulator in the raw material is selected from one or a mixture of more of sodium bicarbonate, sodium hydroxide, sodium carbonate, calcium hydroxide and potassium hydroxide. Preferably selected from sodium bicarbonate, calcium hydroxide and sodium hydroxide.
The anticaking agent in the starting material is selected from the group consisting of silica, calcium silicate and tricalcium phosphate.
It will be readily understood that the above preferred technical features may be combined to constitute a preferred embodiment of the invention, and as demonstrated in the examples, the interaction of sodium starch octenyl succinate and gum arabic with polyethylene glycol vitamin E succinate may result in a product of high entrapment rate, high stability and high bioavailability as described in the present invention.
The following non-limiting examples further illustrate the technical solutions and effects of the present invention, and should not be construed as limiting the present invention in any way. Unless otherwise specified, all percentages in this specification mean mass percentages.
Example 1
409g of water is weighed into a 1000mL beaker, the water temperature is 62 ℃, 125g of sodium starch octenyl succinate and 100g of Arabic gum are added into the beaker, the mixture is stirred until the starch sodium octenyl succinate and the Arabic gum are completely dissolved, and the temperature is reduced to 35 ℃ for standby. Adding 6g of sodium bicarbonate into the water phase, controlling the pH value to be 6.8-7.1, and then adding 4g of glucose oxidase. Mixing 7.5g of vitamin E succinic acid polyethylene glycol ester and 252.5g of vitamin A acetic ester, melting in a water bath at 75 ℃, uniformly stirring, and cooling to 35 ℃ to obtain an oil phase. Slowly pouring the oil phase into the water phase, shearing and emulsifying at 35 deg.C for 0.5h, homogenizing at 40MPa for 2 times, and spray drying at air inlet temperature of 170 deg.C and air outlet temperature of 84 deg.C. Sieving, and adding silicon dioxide to obtain vitamin A acetate microcapsule powder, which is recorded as sample 1.
Example 2
1000g of water are weighed into a 2000mL beaker, the water temperature is 65 ℃, 200g of sodium starch octenyl succinate and 150g of Arabic gum are added into the beaker, the mixture is stirred until the starch sodium octenyl succinate and the Arabic gum are completely dissolved, and the temperature is reduced to 38 ℃ for standby. Adding 5g of calcium hydroxide into the water phase, controlling the pH value to be 6.9-7.5, and then adding 10g of glucose oxidase. Mixing 20g of vitamin E succinic acid polyethylene glycol ester and 605g of vitamin A acetic ester, melting in a water bath at 80 ℃, uniformly stirring, and cooling to 38 ℃ to obtain an oil phase. Slowly pouring the oil phase into the water phase, shearing and emulsifying at 38 deg.C for 0.5h, homogenizing at 55MPa for 2 times, and spray drying at air inlet temperature of 180 deg.C and air outlet temperature of 90 deg.C. Sieving, and adding silicon dioxide to obtain vitamin A acetate microcapsule powder, which is recorded as sample 2.
Example 3
2000g of water are weighed into a 3000mL beaker, the water temperature is 75 ℃, 240g of phosphorylated starch and 260g of acacia gum are added, the mixture is stirred until the phosphorylated starch and the acacia gum are completely dissolved, and the temperature is reduced to 40 ℃ for standby. Adding 4g of sodium hydroxide into the water phase, controlling the pH value to be 7.0-7.3, and then adding 16g of glucose oxidase. Mixing 60g of vitamin E succinic acid polyethylene glycol ester and 1400g of vitamin A palmitate, putting into a water bath with the temperature of 69 ℃ for melting, stirring uniformly, and cooling to 40 ℃ to obtain an oil phase. Slowly pouring the oil phase into the water phase, shearing and emulsifying at 40 ℃ for 1h, homogenizing at 50MPa for 2 times, and then performing spray drying, wherein the air inlet temperature is 175 ℃ and the air outlet temperature is 87 ℃. Sieving, adding silicon dioxide to obtain vitamin A acetate microcapsule powder, and recording as sample 3.
Example 4
Product performance evaluations were performed on sample 1, sample 2, and sample 3, with the results shown in table 1:
TABLE 1
Name (R) Appearance of the product Smell of nourishing Embedding rate Bulk density Particle size Reconstitution property
Sample 1 Orange yellow powder Inherent smell 99.2％ 0.43g/ml Sieving with 40 mesh sieve at a rate of not less than 95% Emulsion homogeneity
Sample 2 Orange powder Inherent smell 98.9％ 0.40g/ml Sieving with 40 mesh sieve at a rate of not less than 95% Emulsion homogeneity
Sample 3 Orange powder Inherent smell 99.3％ 0.38g/ml Sieving with 40 mesh sieve at a rate of not less than 95% Emulsion homogeneity
The results show that the vitamin A microcapsule powder obtained by the process disclosed by the patent has high product embedding rate, good reconstitution property and appropriate bulk density and granularity, and the property indexes show that the product has excellent characteristics and can be widely applied to the fields of feeds, dietary supplements, daily chemicals, medicines and the like.
Example 5
Sample 1, sample 2 and sample 3 were placed in an accelerated oven at 40 ℃ and 75% humidity for three months for product stability evaluation, with the results shown in table 2:
TABLE 2
Figure BDA0002248962390000051
Figure BDA0002248962390000061
The accelerated stability experiment shows that the appearance, the taste and the smell of the three samples, the embedding rate and the reconstitution property of the three samples are not changed after the three-month acceleration, the retention rate of the vitamin A is slightly reduced, but the product with the retention rate more than or equal to 90 percent after the three-month acceleration is generally considered to be qualified. It can be seen that the vitamin A microcapsule powder prepared by the process disclosed by the patent has excellent stability.
Example 6
Bioavailability was evaluated at the cellular level for samples 1-3 as follows:
TABLE 3
Name (R) Bioavailability of
Vitamin A raw material 5.63％
Sample 1 46.73％
Sample 2 45.60％
Sample 3 50.11％
The results show that the bioavailability of the vitamin A raw material is only 5.63 percent, and the bioavailability of the vitamin A microcapsule powder prepared by the formula and the process disclosed by the patent is 8-9 times of that of the raw material, so that the bioavailability is greatly improved.
Example 7
Referring to the formulation and process parameters of example 2, only sodium starch octenyl succinate and acacia gum were replaced by other wall materials of different types, and the effect of the combination of different wall materials and vitamin E polyethylene glycol succinate on the stability and bioavailability of the product was examined, with the following results:
TABLE 4
Figure BDA0002248962390000071
From the results, it can be seen that only sodium starch octenyl succinate and acacia gum act together with vitamin E polyethylene glycol succinate to obtain a product with high embedding rate, high stability and high bioavailability. While other wall material combinations do not have this effect.
Example 8
Referring to the formulation and process parameters of example 2, the vitamin E polyethylene glycol succinate alone was removed to yield a product with an entrapment rate of 98.1%, a 3-month accelerated retention rate of 93.2% at 40 ℃, and a cellular level bioavailability of 14.7%. Therefore, the combination of the vitamin E succinic acid polyethylene glycol ester and the wall material ensures the stability and bioavailability of the product, and is not indispensable.

Claims (6)

1. The preparation method of the vitamin A microcapsule preparation without the antioxidant comprises the following steps:
(1) preparing a raw material, wherein the raw material comprises the following components in parts by mass:
Figure FDA0003252196210000011
wherein the modified starch is selected from sodium starch octenylsuccinate and phosphorylated starch;
(2) sequentially dispersing modified starch and Arabic gum in water at 60-80 deg.C, stirring to dissolve completely, and cooling to 30-40 deg.C;
(3) adding an acidity regulator into the system obtained in the step (2), controlling the pH value to be 6-8, uniformly stirring, and adding glucose oxidase to obtain a water phase;
(4) adding vitamin E polyethylene glycol succinate into vitamin A, heating to melt at 60-80 deg.C, stirring, mixing, and cooling to 30-40 deg.C to obtain oil phase;
(5) slowly adding the oil phase into the water phase, and stirring at 30-40 ℃ until the oil phase and the water phase are uniformly mixed;
(6) shearing and emulsifying the mixture obtained in the step (5) for 0.5-1h, and then homogenizing for 2 times at 40-70MPa to obtain emulsion;
(7) and (3) spray drying the emulsion prepared in the step (6): the air inlet temperature is 80-210 ℃, and the air outlet temperature is 70-120 ℃; the product is sieved and then is uniformly mixed with an anticaking agent.
2. The method of claim 1, wherein the vitamin a is selected from the group consisting of vitamin a acetate, vitamin a palmitate, and mixtures thereof.
3. The method according to claim 1, wherein the acidity regulator is selected from one or more of sodium bicarbonate, sodium hydroxide, sodium carbonate, calcium hydroxide and potassium hydroxide.
4. The method of claim 3, wherein the acidity regulator is selected from the group consisting of sodium bicarbonate, calcium hydroxide, and sodium hydroxide.
5. The method of claim 1, wherein said anticaking agent is selected from the group consisting of silica, calcium silicate and tricalcium phosphate.
6. An antioxidant-free vitamin a microcapsule formulation prepared by the process of claim 1.
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