Fat-soluble nutrient microcapsule as well as preparation method and application thereof

Abstract

The invention relates to a fat-soluble nutrient microcapsule as well as a preparation method and application thereof. The invention provides a fat-soluble nutrient microcapsule. The fat-soluble nutrient microcapsule comprises the following components: fat-soluble nutrients, hydrophilic colloid, a co-emulsifier and starch, wherein the hydrophilic colloid comprises gelatin with the freezing and congealing degree of 125 to 270 Bloom g; the co-emulsifier comprises glycerol and / or sorbitol. The fat-soluble nutrient microcapsule provided by the invention has good pressure resistance and stability, can meet tabletting requirements, and can be stored for a long time. Meanwhile, the invention further provides a preparation method of the fat-soluble nutrient microcapsule, and the fat-soluble nutrient microcapsule which is compact in internal structure, free of holes and good in pressure resistance and stability can be prepared.

Description

Technical Field

[0001] The present invention belongs to the field of food and health product additives, and particularly relates to lipid-soluble nutrient microcapsules, a preparation method thereof and an application thereof. More specifically, it relates to a pressure-resistant lipid-soluble nutrient microcapsule, a preparation method thereof and an application thereof. Background Art

[0002] The lipid-soluble nutrients described in the present invention mainly include lipid-soluble vitamins, carotenoids and coenzyme Q10 (CoQ10). Vitamins are a class of trace organic regulatory substances that humans and animals must obtain from food to maintain normal physiological functions, and play an important role in the growth, metabolism and development of the body. Carotenoids are a general term for a class of important natural pigments, which can improve the reproductive ability and immune function of animals, and have various physiological functions such as antioxidant, coloring and enhancing the communication between cells. Coenzyme Q10 is a lipid-soluble quinone compound that can activate human cells and plays a key role in cell energy production. It has functions such as improving human immunity, enhancing antioxidant capacity, delaying aging and enhancing human vitality. It is widely used in the adjuvant treatment of cardiovascular system diseases in medicine, and is widely used as a nutritional health product and food additive at home and abroad.

[0003] Since lipid-soluble vitamins, carotenoids and coenzyme Q10 are all very unstable substances, extremely sensitive to light, heat and oxygen, they are not suitable for direct addition to foods and health products. Therefore, researchers and related enterprises have developed a variety of methods for stabilizing these lipid-soluble nutrients. The common practice is to prepare these lipid-soluble nutrients into microcapsules and then use them as additives.

[0004] The preparation method of lipid-soluble nutrient microcapsules usually involves dissolving the nutrient and other lipid-soluble core materials in oil or organic solvents to form an oil phase, then mixing it with an aqueous phase containing a water-soluble wall material, and using methods such as high-pressure homogenization, high-speed shearing, high-speed jet, ultrasonic cavitation, and grinding for emulsification, and then performing spray granulation and drying to obtain microcapsules. Since the lipid-soluble nutrients are encapsulated in tiny capsules formed by a continuous wall material, direct contact with the environment is avoided, thereby maintaining their stability during storage, transportation and use. However, it has been found that when the microcapsules are directly used in the preparation of tablets, the capsules are likely to rupture due to low mechanical strength. During stability studies, it was found that the nutrient content decreased, indicating that the lipid-soluble nutrients oxidized and deteriorated after the capsules ruptured.

[0005] To improve the stability of fat-soluble nutrient microcapsules, technicians usually make improvements in aspects such as the selection of the wall material, oil phase or other excipients of the microcapsules, the addition of a support structure, and the optimization of the preparation process, so as to enhance the pressure resistance of the microcapsules and thus improve the application stability of the microcapsules. For example, CN101873848B improved the wall material of the microcapsules. It disclosed a preparation of a lipophilic health component, which includes a lipophilic health component and a protective colloid, wherein the protective colloid is a modified starch with emulsifying ability, and the lipophilic health component is selected from the group consisting of vitamin A, CoQ10 and their esters; CN103549157B disclosed a preparation method of a water-repellent vitamin microcapsule, which includes the following steps: adding a protein active enzyme to a vitamin emulsion formed by emulsifying and homogenizing a wall material and a core material, regranulating, performing a cross-linking reaction and then drying to obtain a water-repellent vitamin microcapsule; US8685446B2 disclosed a microcapsule with a multi-layer wall material, which uses multiple protective colloids for embedding.

[0006] To improve the pressure resistance of fat-soluble nutrient microcapsules during the emulsification process of the microcapsule preparation technology, the common practice in the prior art is to compound multiple wall materials or specific embedding materials and dispersants. For example, CN106074462B compounded gelatin and gum arabic to wrap lycopene, and then homogenized it through a high-pressure homogenizer. The homogenized emulsion was put into a temporary storage tank, evacuated, stirred, and the emulsion was granulated in one step by spray-starch fluidized bed drying method to obtain lycopene microcapsules. CN112189846A adopted specific embedding materials and dispersants. Through the selection of different embedding wall materials and the combined use and synergistic effect of dispersants, the inherent defects of oil and fat-soluble functional ingredient raw materials in application were overcome by the microencapsulation technology, and problems such as oil leakage and unstable exudation of fat-soluble functional ingredients during the tabletting process were solved. The mechanical strength and stability of high-oil-loading microparticles were improved, and it was pressure-resistant and did not leak oil. Therefore, it has good application prospects in the preparation of tablet or capsule products. However, emulsification methods such as high-speed shearing and high-pressure homogenization have the following problems: 1) The emulsification process needs to be carried out batch by batch and in an open environment. The single-batch emulsification time is long, and a large number of air bubbles are easily introduced, causing the fat-soluble nutrients to deteriorate; 2) The internal structure of the prepared microparticle samples is not dense enough, and there are a large number of cavities, which affects the pressure resistance of the products. Due to these influencing factors, part of the fat-soluble nutrient microcapsule products are lost during the preparation process and are easily broken during the tabletting process, and the fat-soluble nutrients are directly in contact with the internal environment and excipients of the tablets, thus affecting the stability of the fat-soluble nutrients during the storage of the tablets. Summary of the Invention

[0007] Problems to be Solved by the Invention

[0008] In view of the problems of poor pressure resistance and instability of fat-soluble nutrient microcapsules in the actual application process in the prior art, the present invention aims to provide a pressure-resistant fat-soluble nutrient microcapsule, its preparation method and application.

[0009] Solutions for Solving the Problems

[0010] To solve the above technical problems, the present invention provides the following technical solutions:

[0011] [1]. A fat-soluble nutrient microcapsule, wherein the fat-soluble nutrient microcapsule contains the following components: fat-soluble nutrients, hydrophilic colloids, co-emulsifiers and starch; wherein,

[0012] The hydrophilic colloid contains gelatin with a bloom gel strength of 125-270 Bloom g;

[0013] The co-emulsifier contains glycerol and / or sorbitol.

[0014] [2]. The fat-soluble nutrient microcapsule according to [1], wherein, based on the total dry weight of the fat-soluble nutrient microcapsule, the fat-soluble nutrient microcapsule contains 30-60% by mass of hydrophilic colloid and 1-5% by mass of co-emulsifier.

[0015] [3]. The fat-soluble nutrient microcapsule according to [1] or [2], wherein the fat-soluble nutrient contains any one or more of vitamin A, vitamin A ester, vitamin E, vitamin E ester, vitamin D2, vitamin D3, vitamin K, coenzyme Q10, curcumin, β-carotene, lutein, canthaxanthin, lutein ester, lycopene, astaxanthin and polyunsaturated fatty acids.

[0016] [4]. The fat-soluble nutrient microcapsule according to any one of [1] to [3], wherein, based on the total dry weight of the fat-soluble nutrient microcapsule, the fat-soluble nutrient microcapsule contains 10-30% by mass of fat-soluble nutrients.

[0017] [5]. The fat-soluble nutrient microcapsule according to any one of [1] to [4], wherein the starch contains any one or more of potato starch, corn starch, waxy corn starch, wheat starch, barley starch, rye starch, rice starch, sorghum starch, sweet potato starch, cassava starch, sweet potato starch and legume starch.

[0018] [6]. The fat-soluble nutrient microcapsule according to any one of [1] to [5], wherein, based on the total dry weight of the fat-soluble nutrient microcapsule, the fat-soluble nutrient microcapsule contains 15-25% by mass of starch.

[0019] [7]. The fat-soluble nutrient microcapsule according to any one of [1] to [6], wherein the fat-soluble nutrient microcapsule further contains a filler; the filler includes any one or more of maltodextrin, glucose, granulated sugar, crystalline fructose, maltose, fiber sugar, and xylitol; and / or, based on the total dry weight of the fat-soluble nutrient microcapsule, the fat-soluble nutrient microcapsule contains 5 to 20% by mass of the filler;

[0020] [8]. The fat-soluble nutrient microcapsule according to any one of [1] to [7], wherein the fat-soluble nutrient microcapsule further contains an antioxidant; the antioxidant includes any one or more of tocopherol, dibutylhydroxytoluene, butylhydroxyanisole, tea polyphenols, propyl gallate, rosemary extract, glycyrrhizin antioxidant, phytic acid, ascorbic acid, sodium ascorbate, D-isoascorbic acid, sodium D-isoascorbate, ascorbyl palmitate, and lecithin; and / or, based on the total dry weight of the fat-soluble nutrient microcapsule, the fat-soluble nutrient microcapsule contains 0.1 to 10% by mass of the antioxidant.

[0021] [9]. The fat-soluble nutrient microcapsule according to any one of [1] to [8], wherein the fat-soluble nutrient microcapsule further contains water less than or equal to 5% by mass.

[0022]

[10] . The method for preparing the fat-soluble nutrient microcapsule according to any one of [1] to [9], characterized in that the preparation method includes the following steps:

[0023] S1: Mix the fat-soluble nutrient, hydrophilic colloid, co-emulsifier, optional filler, and optional antioxidant with water, evacuate and stir simultaneously to obtain a coarse emulsion;

[0024] S2: Continue to shear the coarse emulsion while evacuating to obtain an emulsion or dispersion;

[0025] S3: Granulate the emulsion or dispersion in one step by spray-fluidized bed drying method to obtain the fat-soluble nutrient microcapsule.

[0026]

[11] . The preparation method according to

[10] , wherein in the step S1, the stirring speed is 1.0 to 1.5 m / s; and / or, the stirring temperature is 60 to 70 °C; and / or, the stirring time is 30 - 60 min.

[0027]

[12] . The preparation method according to

[10] or

[11] , wherein in the step S2, the shearing speed is greater than or equal to 19.6 m / s; and / or, the shearing temperature is 60 to 65 °C; and / or, the shearing time is 20 to 40 min.

[0028]

[13] . According to the preparation method described in any one of

[10] to

[12] , wherein, in the step S3, when the emulsion or dispersion is granulated in one step by spray-starch fluidized bed drying method, the fluidized drying is carried out in stages. The temperature of the first stage is 18 - 40 °C, the time of the first stage is 10 - 20 min, the temperature of the second stage is 40 - 60 °C, and the time of the second stage is 40 - 60 min.

[0029]

[14] . Use of the fat-soluble nutrient microcapsule described in any one of [1] to [9] and / or the fat-soluble nutrient microcapsule prepared by the preparation method described in any one of

[10] to

[13] in the preparation of food or health products.

[0030] Effects of the Invention

[0031] By implementing the above technical solutions, the present invention has achieved the following beneficial effects:

[0032] First of all, the present invention provides a fat-soluble nutrient microcapsule, which has good pressure resistance and stability. Experimental data shows that the fat-soluble nutrient microcapsule provided by the present invention deforms 100% under the action of a 25N pressure and can remain intact without rupture; after being placed for 12 months at 25 °C and RH75%, the retention rate of the fat-soluble nutrient content is greater than 95%; after direct tableting and being placed for 12 months at 25 °C and RH75%, the retention rate of the fat-soluble nutrient content is still greater than 95%, which is sufficient to meet the tableting requirements.

[0033] At the same time, the present invention also provides a preparation method for the fat-soluble nutrient microcapsule. The preparation method has a simple process, is suitable for large-scale production, and the preparation method provided by the present invention can prepare a fat-soluble nutrient microcapsule with a dense internal structure without cavities and having good pressure resistance and stability.

[0034] Due to the good pressure resistance and stability, the fat-soluble nutrient microcapsule provided by the present invention can also be used as a raw material and further applied to the processing of food or health products, especially can be used for the preparation of health food in tablet form. Description of the Drawings

[0035] Figure 1 : Test results of the pressure resistance of vitamin A microcapsules in Example 1.

[0036] Figure 2 : Test results of the pressure resistance of vitamin A microcapsules in Example 2.

[0037] Figure 3 : Test results of the pressure resistance of vitamin A microcapsules in Comparative Example 1.

[0038] Figure 4 : Results of the pressure resistance test of vitamin A microcapsules in Comparative Example 2.

[0039] Figure 5 : Results of the pressure resistance test of vitamin A microcapsules in Comparative Example 3. Detailed implementation manners

[0040] The following describes the implementation manners of the present invention, but the present invention is not limited thereto. The present invention is not limited to the various components described below. Various changes can be made within the scope of the invention claimed, and the implementation manners and embodiments obtained by appropriately combining the technical means respectively disclosed in different implementation manners and embodiments are also included in the technical scope of the present invention.

[0041] In the present invention, the terms "comprise", "have", "include" or "contain" may mean inclusive or open-ended, and do not exclude additional, unrecited elements or method steps. At the same time, "comprise", "have", "include" or "contain" may also mean closed-ended, excluding additional, unrecited elements or method steps.

[0042] In the present invention, the meaning expressed by "can" includes both the meaning of performing a certain process and the meaning of not performing a certain process.

[0043] In the present invention, "optional" or "optionally" means that certain substances, components, execution steps, applied conditions and other factors are used or not used.

[0044] In the present invention, the numerical ranges expressed by "numerical value A to numerical value B", "numerical value A - numerical value B", "numerical value A or more / less" refer to the ranges including the endpoint numerical values A and B.

[0045] In the present invention, the term "about" is used to define that the numerical ranges and parameters of the present invention are approximate numerical values, and the relevant numerical values in the specific embodiments have been presented as precisely as possible here. Unless otherwise clearly stated, it should be understood that all ranges, quantities, numerical values and percentages used in the present invention are modified by "about". Here, "about" generally means that the actual numerical value is within ±5%, ±3%, ±1% or ±0.5% of a certain specific numerical value or range. And the numerical values and numerical ranges appearing in the present invention should be understood to include the systematic errors inevitable in industrial production.

[0046] In the present invention, the "some specific / preferred embodiments", "other specific / preferred embodiments", "embodiments", etc. mentioned refer to the specific elements (e.g., features, structures, properties, and / or characteristics) related to the embodiment, which are included in at least one of the embodiments described herein, and may or may not be present in other embodiments. Additionally, it should be understood that the elements can be combined in various embodiments in any suitable manner.

[0047] In the present invention, the unit names used are all international standard unit names, and if not otherwise specified, the "%" used represents weight or mass percentage content.

[0048] Unless otherwise defined, other technical and scientific terms used in the present invention have the same meaning as commonly understood by those of ordinary skill in the technical field to which the present invention pertains.

[0049] I. First aspect

[0050] The first aspect of the present invention provides a fat-soluble nutrient microcapsule, which comprises the following components: a fat-soluble nutrient, a hydrophilic colloid, a co-emulsifier, and starch.

[0051] In some embodiments, the fat-soluble nutrient microcapsule further comprises a filler.

[0052] In some embodiments, the fat-soluble nutrient microcapsule further comprises an antioxidant.

[0053] In some embodiments, the fat-soluble nutrient microcapsule further comprises water.

[0054] In some embodiments, the fat-soluble nutrient microcapsule consists of the following components: a fat-soluble nutrient, a hydrophilic colloid, a co-emulsifier, a filler, an antioxidant, and starch.

[0055] In some embodiments, the fat-soluble nutrient microcapsule consists of the following components: a fat-soluble nutrient, a hydrophilic colloid, a co-emulsifier, a filler, an antioxidant, starch, and water.

[0056] Fat-soluble Nutrients

[0057] The fat-soluble nutrient referred to in the present invention means a substance that is insoluble or substantially insoluble in water under normal temperature (about 25°C) and normal pressure (about 101.325 kPa) and has beneficial effects on life and health.

[0058] In some embodiments, the fat-soluble nutrient comprises any one or more of vitamin A, vitamin A esters (such as retinol acetate, retinol palmitate, retinol linoleate, retinol propionate, etc.), vitamin E, vitamin E esters (such as tocopherol acetate, tocopherol succinate, tocopherol nicotinate, tocopherol linoleate, tocopherol palmitate, etc.), vitamin D2, vitamin D3, vitamin K, coenzyme Q10, curcumin, β-carotene, lutein, canthaxanthin, lutein esters (such as lutein dipalmitate, etc.), lycopene, astaxanthin, and polyunsaturated fatty acids (such as eicosapentaenoic acid EPA, docosahexaenoic acid DHA, arachidonic acid ARA, gamma-linolenic acid GLA, etc.).

[0059] In some embodiments, the fat-soluble nutrient is vitamin A, vitamin A ester, vitamin E, vitamin E ester, vitamin D2, vitamin D3, vitamin K, coenzyme Q10, curcumin, β-carotene, lutein, canthaxanthin, lutein ester, lycopene, astaxanthin, or polyunsaturated fatty acid; preferably vitamin A.

[0060] In some embodiments, based on the total dry weight of the fat-soluble nutrient microcapsules, the fat-soluble nutrient microcapsules contain 10-30% by mass of the fat-soluble nutrient; for example, the fat-soluble nutrient microcapsules may contain 10% by mass, 11% by mass, 12% by mass, 13% by mass, 14% by mass, 15% by mass, 16% by mass, 17% by mass, 18% by mass, 19% by mass, 20% by mass, 21% by mass, 22% by mass, 23% by mass, 24% by mass, 25% by mass, 26% by mass, 27% by mass, 28% by mass, 29% by mass, or 30% by mass, etc. of the fat-soluble nutrient; preferably, the fat-soluble nutrient microcapsules contain 15-20% by mass or 18-22% by mass of the fat-soluble nutrient.

[0061] Hydrophilic Colloids

[0062] The hydrophilic colloid described in the present invention refers to a high-molecular substance that can interact with water molecules and form a colloidal solution.

[0063] In some embodiments, the hydrophilic colloid comprises gelatin.

[0064] In some embodiments, the hydrophilic colloid is gelatin. The gelatin described in the present invention is mainly a protein substance obtained by denaturing and degrading the collagen of animal skins or bones. The present invention does not particularly limit the preparation method of gelatin. For example, it can be obtained through the following process: cleaning to remove impurities and fats on animal skins or bones, using hot water or organic solvents (such as ethanol) to remove residual fats, rinsing with water after acid or alkali treatment, heating the treated raw materials in hot water (for example, 60 - 100 °C) to hydrolyze collagen into gelatin.

[0065] In some embodiments, the gelatin includes any one or more of porcine gelatin, bovine bone gelatin, and fish gelatin. In some embodiments, the gelatin is porcine gelatin, bovine bone gelatin, or fish gelatin; preferably, the gelatin is porcine gelatin.

[0066] In some embodiments, the gel strength of the gelatin is 125 - 275 Bloom g; for example, the gel strength of the gelatin can be 125 Bloom g, 130 Bloom g, 135 Bloom g, 140 Bloom g, 145 Bloom g, 150 Bloom g, 155 Bloom g, 160 Bloom g, 165 Bloom g, 170 Bloom g, 175 Bloom g, 180 Bloom g, 185 Bloom g, 190 Bloom g, 195 Bloom g, 200 Bloom g, 205 Bloom g, 210 Bloom g, 215 Bloom g, 220 Bloom g, 225 Bloom g, 230 Bloom g, 235 Bloom g, 240 Bloom g, 245 Bloom g, 250 Bloom g, 255 Bloom g, 260 Bloom g, 265 Bloom g, 270 Bloom g, or 275 Bloom g, etc.; preferably, the gel strength of the gelatin is 200 - 250 Bloom g.

[0067] In some embodiments, based on the total dry weight of the fat-soluble nutrient microcapsules, the fat-soluble nutrient microcapsules contain 30 to 60% by mass of a hydrophilic colloid; for example, the fat-soluble nutrient microcapsules may contain 30% by mass, 31% by mass, 32% by mass, 33% by mass, 34% by mass, 35% by mass, 36% by mass, 37% by mass, 38% by mass, 39% by mass, 40% by mass, 41% by mass, 42% by mass, 43% by mass, 44% by mass, 45% by mass, 46% by mass, 47% by mass, 48% by mass, 49% by mass, 50% by mass, 51% by mass, 52% by mass, 53% by mass, 54% by mass, 55% by mass, 56% by mass, 57% by mass, 58% by mass, 59% by mass or 60% by mass, etc. of the hydrophilic colloid; preferably, the fat-soluble nutrient microcapsules contain 35 to 50% by mass of the hydrophilic colloid; more preferably, the fat-soluble nutrient microcapsules contain 38 to 44% by mass of the hydrophilic colloid.

[0068] Co-emulsifiers

[0069] The co-emulsifier described in the present invention refers to a compound that can mix two immiscible substances to form an emulsion liquid, and it mainly improves the stability of the emulsion by adjusting the fluidity or strength of the interfacial film, and the viscosity or rheology of the emulsion.

[0070] In some embodiments, the co-emulsifier comprises glycerol and / or sorbitol; preferably, the co-emulsifier is glycerol and / or sorbitol; more preferably, the co-emulsifier is glycerol or sorbitol; even more preferably, the co-emulsifier is glycerol. The present invention has found that an appropriate co-emulsifier (such as glycerol or sorbitol, especially glycerol) can combine with gelatin to form a three-dimensional network structure, increase the toughness and shrinkage force of the microcapsules, and promote the microcapsules to have good properties of withstanding pressure without rupture.

[0071] In some embodiments, based on the total dry weight of the fat-soluble nutrient microcapsules, the fat-soluble nutrient microcapsules contain 1 to 5% by mass of the co-emulsifier; for example, the fat-soluble nutrient microcapsules may contain 1% by mass, 2% by mass, 3% by mass, 4% by mass or 5% by mass, etc. of the co-emulsifier; preferably, the fat-soluble nutrient microcapsules contain 1 to 5% by mass of the co-emulsifier; more preferably, the fat-soluble nutrient microcapsules contain 2 to 4% by mass of the co-emulsifier.

[0072] Fillers

[0073] The filler described in the present invention refers to a substance used to fill materials or increase the volume of materials, and it can be used to fill the voids in the microcapsules, especially the voids in the microcapsule walls.

[0074] In some embodiments, the filler comprises any one or more of maltodextrin, glucose, granulated sugar, crystalline fructose, maltose, cellobiose, and xylitol.

[0075] In some embodiments, the filler is maltodextrin, glucose, granulated sugar, crystalline fructose, maltose, cellobiose, or xylitol; preferably, the filler is granulated sugar or crystalline fructose; more preferably, the filler is fructose. The filler selected in the present invention can fill the voids in the three-dimensional spatial structure formed by the macromolecular material gelatin and the co-emulsifier, achieving a dense and cavity-free internal structure, and further improving the pressure resistance of the microcapsules.

[0076] In some embodiments, based on the total dry weight of the fat-soluble nutrient microcapsules, the fat-soluble nutrient microcapsules contain 5-20% by mass of the filler; for example, the fat-soluble nutrient microcapsules may contain 5% by mass, 6% by mass, 7% by mass, 8% by mass, 9% by mass, 10% by mass, 11% by mass, 12% by mass, 13% by mass, 14% by mass, 15% by mass, 16% by mass, 17% by mass, 18% by mass, 19% by mass, or 20% by mass, etc. of the filler; preferably, the fat-soluble nutrient microcapsules contain 10-18% by mass of the filler; more preferably, the fat-soluble nutrient microcapsules contain 14-16% by mass of the filler.

[0077] Antioxidants

[0078] The antioxidant referred to in the present invention means a substance that can delay or prevent an oxidation reaction.

[0079] In some embodiments, the antioxidant comprises any one or more of tocopherol, dibutylhydroxytoluene (BHT), butylhydroxyanisole (BHA), tea polyphenols, propyl gallate, rosemary extract, glycyrrhizin antioxidant, phytic acid, ascorbic acid, sodium ascorbate, D-isoascorbic acid, sodium D-isoascorbate, ascorbyl palmitate, and lecithin.

[0080] In some embodiments, the antioxidant comprises an oil-phase antioxidant and a water-phase antioxidant. The oil-phase antioxidant is BHT or tocopherol, and the water-phase antioxidant is sodium ascorbate or sodium D-isoascorbate; preferably, the oil-phase antioxidant is BHT, and the water-phase antioxidant is sodium ascorbate.

[0081] In some embodiments, based on the total dry weight of the fat-soluble nutrient microcapsules, the fat-soluble nutrient microcapsules contain 0.1 to 10% by mass of an antioxidant; for example, the fat-soluble nutrient microcapsules may contain 0.1% by mass, 0.3% by mass, 0.5% by mass, 0.7% by mass, 0.9% by mass, 1% by mass, 1.5% by mass, 2% by mass, 2.5% by mass, 3% by mass, 3.5% by mass, 4% by mass, 4.5% by mass, 5% by mass, 5.5% by mass, 6% by mass, 6.5% by mass, 7% by mass, 7.5% by mass, 8% by mass, 8.5% by mass, 9% by mass, 9.5% by mass or 10% by mass, etc. of the antioxidant; preferably, the fat-soluble nutrient microcapsules contain 0.1 to 1% by mass of an oil-phase antioxidant and 1 to 5% by mass of an aqueous-phase antioxidant.

[0082] Starch

[0083] The starch referred to in the present invention means a natural polysaccharide that has not been modified by physical, chemical or enzymatic methods, etc.

[0084] In some embodiments, the starch comprises any one or more of potato starch, corn starch, waxy corn starch, wheat starch, barley starch, rye starch, rice starch, sorghum starch, sweet potato starch, tapioca starch, sweet potato starch and legume starch.

[0085] In some embodiments, the starch is potato starch, corn starch, waxy corn starch, wheat starch, barley starch, rye starch, rice starch, sorghum starch, sweet potato starch, tapioca starch, sweet potato starch or legume starch; preferably corn starch.

[0086] In some embodiments, based on the total dry weight of the fat-soluble nutrient microcapsules, the fat-soluble nutrient microcapsules contain 15 to 25% by mass of starch; for example, the fat-soluble nutrient microcapsules may contain 15% by mass, 16% by mass, 17% by mass, 18% by mass, 19% by mass, 20% by mass, 21% by mass, 22% by mass, 23% by mass, 24% by mass or 25% by mass of starch; preferably, the fat-soluble nutrient microcapsules contain 16 to 24% by mass of starch; more preferably, the fat-soluble nutrient microcapsules contain 18 to 22% by mass of starch.

[0087] Water

[0088] The fat-soluble nutrient microcapsules of the present invention may contain a small amount of water, and the water content does not exceed 5% by mass of the total mass of the fat-soluble nutrient microcapsules, and preferably the water content is less than or equal to 3% by mass.

[0089] II. Second aspect

[0090] The second aspect of the present invention provides a method for preparing the fat-soluble nutrient microcapsules described in the first aspect, which comprises the following steps:

[0091] S1: Mix the fat-soluble nutrient, hydrophilic colloid, co-emulsifier, optional filler, optional antioxidant and water, evacuate the air while stirring to obtain a coarse emulsion;

[0092] S2: Continue to shear the coarse emulsion while evacuating the air to obtain an emulsion or dispersion;

[0093] S3: Granulate the emulsion or dispersion in one step by spray-starch fluidized bed drying method to obtain the fat-soluble nutrient microcapsules.

[0094] By stirring and shearing while evacuating the air, the air bubbles in the emulsion are greatly reduced, and the cavities inside the microcapsules obtained by spray granulation can be greatly reduced, improving the compactness of the internal structure of the fat-soluble nutrient microcapsules. In some embodiments, the vacuum degree of the whole system is greater than or equal to 0.07 Mpa when evacuating the air.

[0095] In some embodiments, in the step S1, the stirring speed is 1.0-1.5 m / s (for example, it can be 1.0 m / s, 1.1 m / s, 1.2 m / s, 1.3 m / s, 1.4 m / s or 1.5 m / s, etc.), and / or the stirring temperature is 60-70 °C (for example, it can be 60 °C, 61 °C, 62 °C, 63 °C, 64 °C, 65 °C, 66 °C, 67 °C, 68 °C, 69 °C or 70 °C, etc.), and / or the stirring time is 30-60 min (for example, it can be 30 min, 32 min, 34 min, 36 min, 38 min, 40 min, 42 min, 44 min, 46 min, 48 min, 50 min, 52 min, 54 min, 56 min, 58 min or 60 min, etc.).

[0096] In some embodiments, in the step S2, the shearing speed is greater than or equal to 19.6 m / s (for example, it can be 19.6 m / s or 20 m / s, etc.), and / or the shearing temperature is 60-65 °C (for example, it can be 60 °C, 61 °C, 62 °C, 63 °C, 64 °C or 65 °C, etc.), and / or the shearing time is 20-40 min (for example, it can be 20 min, 22 min, 24 min, 26 min, 28 min, 30 min, 32 min, 34 min, 36 min, 38 min or 40 min, etc.).

[0097] In some embodiments, in the step S2, the particle size Dv(90) of the emulsion or dispersion is 1.0 - 3.0 μm.

[0098] In some embodiments, in the step S3, when the emulsion or dispersion is granulated in one step by spray - starch fluidized bed drying method, the fluidized drying is carried out in sections. The temperature of the first section is 18 - 40 °C (for example, it can be 18 °C, 20 °C, 22 °C, 24 °C, 26 °C, 28 °C, 30 °C, 32 °C, 34 °C, 36 °C, 38 °C or 40 °C, etc.), the time of the first section is 10 - 20 min (for example, it can be 10 min, 12 min, 14 min, 16 min, 18 min or 20 min, etc.), the temperature of the second section is 40 - 60 °C (for example, it can be 40 °C, 42 °C, 44 °C, 46 °C, 48 °C, 50 °C, 52 °C, 54 °C, 56 °C, 58 °C or 60 °C, etc.), and the time of the second section is 40 - 60 min (for example, it can be 40 min, 42 min, 44 min, 46 min, 48 min, 50 min, 52 min, 54 min, 56 min, 58 min or 60 min, etc.).

[0099] In some embodiments, in the step S3, the particle size distribution of the obtained fat - soluble nutrient microcapsules is 40 - 80 mesh.

[0100] III. The third aspect

[0101] The third aspect of the present invention provides the application of the fat - soluble nutrient microcapsules described in the first aspect and / or the fat - soluble nutrient microcapsules prepared by the preparation method described in the second aspect in the preparation of foods or health products.

[0102] In some embodiments, the health product is a tablet.

[0103] Examples

[0104] The embodiments of the present invention will be described in detail below in conjunction with examples. However, those skilled in the art will understand that the following examples are only used to illustrate the present invention and should not be regarded as limiting the scope of the present invention. For those not specified in the examples, the conventional conditions or the conditions recommended by the manufacturer are followed. Unless otherwise specified, the materials or instruments used are all conventional products that can be obtained through commercial purchase.

[0105] In the present invention, the pressure resistance test is carried out by the following method: Place a single micro - capsule particle on the tray of a texture analyzer (Yingtai Technology, accuracy d = 0.001 g), select a pressure of 25 N, apply a vertical pressure to the capsule with a probe until the capsule undergoes 100% deformation. Observe the morphology of the micro - capsule under a microscope.

[0106] In the present invention, the test method for the gel strength of gelatin is the method for determining the gel strength of gelatin specified in the national standard GB6783-2013.

[0107] Example 1

[0108] 1. Add 96 g of vitamin A (VA) crystals, 5 g of dibutylhydroxytoluene (BHT), 196 g of porcine gelatin (250 Bloom g), 87 g of fructose, 6 g of glycerol, and 10 g of sodium ascorbate to 500 g of pure water. Stir at 65 °C while evacuating for 30 min at a stirring speed of 1.2 m / s to prepare a crude emulsion.

[0109] 2. While continuing to evacuate, start high-speed shearing. The vacuum degree is 0.075 Mpa, the shearing speed is 19.6 m / s, and the emulsification time is 25 min to prepare an emulsion.

[0110] 3. Granulate the emulsion in one step by spray - starch fluidized bed drying. The fluidized drying is carried out in stages. The temperature in the first stage is 22 °C and the time is 15 min. The temperature in the second stage is 56 °C and the time is 50 min to obtain vitamin A microcapsules with a weight loss of less than 5% and a particle size of 40 - 80 mesh.

[0111] Perform a pressure resistance test on the above microcapsules. The test result is that the microcapsules remain intact without rupture, as Figure 1 shown.

[0112] Example 2

[0113] 1. Add 96 g of vitamin A (VA) crystals, 5 g of dibutylhydroxytoluene (BHT), 196 g of porcine gelatin (250 Bloom g), 87 g of fructose, 6 g of sorbitol, and 10 g of sodium ascorbate to 500 g of pure water. Stir at 65 °C while evacuating for 30 min at a stirring speed of 1.2 m / s to prepare a crude emulsion.

[0114] 2. While continuing to evacuate, start high-speed shearing. The vacuum degree is 0.075 Mpa, the shearing speed is 19.6 m / s, and the emulsification time is 25 min to prepare an emulsion.

[0115] 3. Granulate the emulsion in one step by spray - starch fluidized bed drying. The fluidized drying is carried out in stages. The temperature in the first stage is 22 °C and the time is 15 min. The temperature in the second stage is 56 °C and the time is 50 min to obtain vitamin A microcapsules with a weight loss of less than 5% and a particle size of 40 - 80 mesh.

[0116] Perform a pressure resistance test on the above microcapsules. The test result is that some of the microcapsules are slightly ruptured, as Figure 2 shown.

[0117] Comparative Example 1

[0118] 1. Add 96 g of vitamin A (VA) crystals, 5 g of dibutylhydroxytoluene (BHT), 196 g of porcine gelatin (100 Bloom g), 87 g of fructose, 6 g of glycerol, and 10 g of sodium ascorbate to 500 g of pure water. Stir at 65 °C while evacuating the vacuum for 30 min at a stirring speed of 1.2 m / s to prepare a crude emulsion;

[0119] 2. While continuing to evacuate the vacuum, start high-speed shearing. The vacuum degree is 0.075 Mpa, the shearing speed is 19.6 m / s, and the emulsification time is 25 min to prepare an emulsion;

[0120] 3. Granulate the emulsion in one step by spray-starch fluidized bed drying. The fluidized drying is carried out in stages. The temperature in the first stage is 22 °C and the time is 15 min. The temperature in the second stage is 56 °C and the time is 50 min to obtain vitamin A microcapsules with a weight loss of less than 5% and a particle size of 40 - 80 mesh.

[0121] Perform a pressure resistance test on the above microcapsules. The test result is that the microcapsules are severely ruptured, as Figure 3 shown.

[0122] Comparative Example 2

[0123] 1. Add 96 g of vitamin A (VA) crystals, 5 g of dibutylhydroxytoluene (BHT), 196 g of gum arabic, 87 g of fructose, 6 g of glycerol, and 10 g of sodium ascorbate to 400 g of pure water. Stir at 65 °C while evacuating the vacuum for 30 min at a stirring speed of 1.2 m / s to prepare a crude emulsion;

[0124] 2. While continuing to evacuate the vacuum, start high-speed shearing. The vacuum degree is 0.075 Mpa, the shearing speed is 19.6 m / s, and the emulsification time is 25 min to prepare an emulsion;

[0125] 3. Granulate the emulsion in one step by spray-starch fluidized bed drying. The fluidized drying is carried out in stages. The temperature in the first stage is 22 °C and the time is 15 min. The temperature in the second stage is 56 °C and the time is 50 min to obtain vitamin A microcapsules with a weight loss of less than 5% and a particle size of 40 - 80 mesh.

[0126] Perform a pressure resistance test on the above microcapsules. The test result is that the microcapsules are ruptured, as Figure 4 shown.

[0127] Comparative Example 3

[0128] 1. Add 96 g of vitamin A (VA) crystals, 5 g of dibutylhydroxytoluene (BHT), 196 g of porcine gelatin (250 Bloom g), 87 g of fructose, 6 g of polyethylene glycol 400, and 10 g of sodium ascorbate to 500 g of pure water. Stir at 65 °C while evacuating the vacuum for 30 min at a stirring speed of 1.2 m / s to prepare a crude emulsion;

[0129] 2. While continuing to evacuate, start high-speed shearing. The degree of vacuum is 0.075 Mpa, the shearing speed is 19.6 m / s, and the emulsification time is 25 min to prepare an emulsion.

[0130] 3. Granulate the emulsion in one step by spray-starch fluidized bed drying. The fluidized drying is carried out in sections. The temperature of the first section is 22 °C and the time is 15 min. The temperature of the second section is 56 °C and the time is 50 min to obtain vitamin A microcapsules with a weight loss of less than 5% and a particle size of 40 - 80 mesh.

[0131] Perform a pressure resistance test on the above microcapsules. The test result is that the microcapsules rupture, as Figure 5 shown.

[0132] Test Example 1

[0133] Directly place the vitamin A microcapsules prepared in Examples 1 and 2 and Comparative Examples 1 and 2 at 25 °C and RH 75% for 12 months. At the same time, directly tablet the vitamin A microcapsules prepared in Examples 1 and 2 and Comparative Examples 1 and 2 and place them at 25 °C and RH 75% for 12 months, and detect the retention rate of vitamin A content. The obtained results are shown in Table 1 below.

[0134] Table 1 Detection results of vitamin A content retention rate

[0135]

[0136] According to the results in Table 1, the retention rate of vitamin A content in the vitamin A microcapsules prepared in Examples 1 and 2 is greater than 95% after being placed at 25 °C and RH 75% for 12 months; the retention rate of vitamin A content is still greater than 95% after being directly tableted and placed at 25 °C and RH 75% for 12 months, which is sufficient to meet the tableting requirements.

Claims

1. A fat-soluble nutrient microcapsule, characterized in that: The fat-soluble nutrient microcapsules contain the following components: fat-soluble nutrients, hydrophilic colloids, emulsifiers and starch; wherein, The hydrophilic colloid comprises gelatin having a freezing degree of 125 to 270 Bloom g; The co-emulsifier comprises glycerol and / or sorbitol.

2. The fat-soluble nutrient microcapsule according to claim 1, characterized in that: Based on the total dry weight of the fat-soluble nutrient microcapsules, the fat-soluble nutrient microcapsules contain 30-60% by mass of a hydrophilic colloid and 1-5% by mass of an auxiliary emulsifier.

3. The fat-soluble nutrient microcapsule according to claim 1 or 2, characterized in that: The fat-soluble nutrients include any one or more of vitamin A, vitamin A ester, vitamin E, vitamin E ester, vitamin D2, vitamin D3, vitamin K, coenzyme Q10, curcumin, β-carotene, lutein, canthaxanthin, lutein ester, lycopene, astaxanthin and polyunsaturated fatty acids; And / or, based on the total dry weight of the fat-soluble nutrient microcapsules, the fat-soluble nutrient microcapsules contain 10 to 30 mass % of fat-soluble nutrients.

4. The fat-soluble nutrient microcapsule according to any one of claims 1 to 3, characterized in that: The starch comprises any one or more of potato starch, corn starch, waxy corn starch, wheat starch, barley starch, rye starch, rice starch, sorghum starch, sweet potato starch, cassava starch, sweet potato starch and bean starch; And / or, based on the total dry weight of the fat-soluble nutrient microcapsules, the fat-soluble nutrient microcapsules contain 15 to 25 mass % of starch.

5. The fat-soluble nutrient microcapsule according to any one of claims 1 to 4, characterized in that: The fat-soluble nutrient microcapsules further contain a filler; the filler contains any one or more of maltodextrin, glucose, white sugar, crystalline fructose, maltose, cellulose and xylitol; and / or, based on the total dry weight of the fat-soluble nutrient microcapsules, the fat-soluble nutrient microcapsules contain 5 to 20% by mass of the filler; and / or, The fat-soluble nutrient microcapsules also contain antioxidants; the antioxidants include any one or more of tocopherol, butylated hydroxytoluene, butylated hydroxyanisole, tea polyphenols, propyl gallate, rosemary extract, licorice antioxidants, phytic acid, ascorbic acid, sodium ascorbate, D-isoascorbic acid, sodium D-isoascorbate, ascorbyl palmitate, and lecithin; and / or, based on the total dry weight of the fat-soluble nutrient microcapsules, the fat-soluble nutrient microcapsules contain 0.1 to 10 mass% of antioxidants.

6. The fat-soluble nutrient microcapsule according to any one of claims 1 to 5, characterized in that: The fat-soluble nutrient microcapsules also contain less than or equal to 5% by mass of water.

7. The method for preparing the fat-soluble nutrient microcapsules according to any one of claims 1 to 6, characterized in that: The preparation method comprises the following steps: S1: mixing fat-soluble nutrients, hydrophilic colloid, co-emulsifier, optional filler and optional antioxidant with water, evacuating and stirring to obtain a crude emulsion; S2: continuing to shear the crude emulsion while evacuating the vacuum to obtain an emulsion or a dispersion; S3: The emulsion or dispersion is granulated in one step by a spray-starch fluidized bed drying method to obtain the fat-soluble nutrient microcapsules.

8. The preparation method according to claim 7, characterized in that: In step S1, the stirring speed is 1.0-1.5 m / s; and / or, the stirring temperature is 60-70° C.; and / or, the stirring time is 30-60 min; and / or, In the step S2, the shearing speed is greater than or equal to 19.6 m / s; and / or the shearing temperature is 60-65° C.; and / or the shearing time is 20-40 min.

9. The preparation method according to claim 7 or 8, characterized in that: In step S3, when the emulsion or dispersion is granulated in one step by spray-starch fluidized bed drying method, fluidized drying is carried out in stages, the temperature of the first stage is 18-40°C, the first time period is 10-20 minutes, the temperature of the second stage is 40-60°C, and the second time period is 40-60 minutes.

10. Use of the fat-soluble nutrient microcapsules according to any one of claims 1 to 6 and / or the fat-soluble nutrient microcapsules prepared by the preparation method according to any one of claims 7 to 9 in the preparation of food or health products.

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