CN114521656B - Multilayer coated heat-sensitive nutrient microcapsule and preparation method thereof - Google Patents

Multilayer coated heat-sensitive nutrient microcapsule and preparation method thereof Download PDF

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CN114521656B
CN114521656B CN202210134263.6A CN202210134263A CN114521656B CN 114521656 B CN114521656 B CN 114521656B CN 202210134263 A CN202210134263 A CN 202210134263A CN 114521656 B CN114521656 B CN 114521656B
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nutrient
oil
particles
wax
vitamin
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CN114521656A (en
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李建东
陈志荣
张其磊
严宏岳
刘香
朱小勇
王桂来
戚丽丹
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Xinchang Xinhecheng Vitamin Co ltd
Zhejiang University ZJU
Zhejiang NHU Co Ltd
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Xinchang Xinhecheng Vitamin Co ltd
Zhejiang University ZJU
Zhejiang NHU Co Ltd
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    • 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
    • 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
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/03—Organic compounds
    • A23L29/035—Organic compounds containing oxygen as heteroatom
    • 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
    • A23L33/105—Plant extracts, their artificial duplicates or their derivatives
    • 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
    • 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
    • A23P20/00—Coating of foodstuffs; Coatings therefor; Making laminated, multi-layered, stuffed or hollow foodstuffs
    • A23P20/10—Coating with edible coatings, e.g. with oils or fats
    • A23P20/15—Apparatus or processes for coating with liquid or semi-liquid products
    • A23P20/18—Apparatus or processes for coating with liquid or semi-liquid products by spray-coating, fluidised-bed coating or coating by casting
    • 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
    • A23P20/00—Coating of foodstuffs; Coatings therefor; Making laminated, multi-layered, stuffed or hollow foodstuffs
    • A23P20/20—Making of laminated, multi-layered, stuffed or hollow foodstuffs, e.g. by wrapping in preformed edible dough sheets or in edible food containers
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
    • Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics

Abstract

The application discloses a multilayer-coated heat-sensitive nutrient microcapsule and a preparation method thereof, wherein the nutrient microcapsule comprises: nutrient microparticles; the packaging material is filled in the inner pore canal of the nutrient particle and wraps the surface of the nutrient particle; the outer wall material is wrapped outside the nutrient particles and the packaging material; wherein the nutrient microparticles comprise: nutrients, inner wall material and oil. The interior of the nutrient particle is filled with the packaging material, so that the microcapsule is not easy to absorb water and deteriorate, has good stability, long shelf life and good rigidity, and is not easy to damage, deform and the like in the subsequent processing process.

Description

Multilayer coated heat-sensitive nutrient microcapsule and preparation method thereof
Technical Field
The application relates to the technical field of pharmaceutical chemicals, in particular to a multilayer-coated heat-sensitive nutrient microcapsule and a preparation method thereof.
Background
Nutrients are chemical components in food that provide energy, body constituents, and tissue repair and physiological regulation functions to the human body. Modern medical research shows that the nutrients needed by human body are not hundreds, some of them can be made by self-synthesis, but can not be made by self-synthesis, and there are more than 40 kinds which must be taken by external world, after fine division, seven major nutrients can be summarized: the essential nutrients for human body include 7 kinds such as protein, fat, sugar, inorganic salt (mineral), vitamin, water and cellulose.
Fat-soluble vitamins, carotenoids, coenzyme Q10, polyunsaturated fatty acids and other nutrients are basically insoluble in water, and are difficult to be added uniformly to feeds or foods, so the application range is limited. And these nutrients are extremely sensitive to light, heat and oxygen due to the particularity of their structure, and are therefore also called heat-sensitive nutrients. In order to improve the stability and bioavailability of these heat-sensitive nutrients, they are often prepared as microcapsules for use.
As spray drying with mature technology and low cost, it is widely used in the production of nutrient microcapsules. CN109452467A takes a mixture of proteins and carbohydrates as a wall material, and is mixed and emulsified with vitamin A to obtain a vitamin A emulsion, and spray drying is carried out after pH and oil drop particle size are regulated. CN102224934B, mixing and emulsifying the vitamin A palmitate oil and the sodium caseinate solution, homogenizing, and performing hot air spray drying to obtain the vitamin A microcapsule. CN101703243B uses maltodextrin and gelatin as wall materials, and adds emulsifiers such as glyceryl monostearate and sucrose ester to embed vitamin E oil, and vitamin E powder is obtained by spray drying.
However, the spray drying has inevitable limitations, for example, when researchers apply the vitamin A dry powder prepared by spray drying to the vitamin complex tablets in the document 'stability influence factor of vitamin A in vitamin complex tablets', after the vitamin A dry powder is prepared into the tablets by tabletting, after the vitamin A dry powder is stored for 16 weeks under the conditions of 40 ℃ plus or minus 2 ℃ and 75% plus or minus 5% of relative humidity, the content of the vitamin A is reduced by 37 to 58 percent; in the study on the stability of vitamin D in infant formula milk powder, researchers have found that vitamin D is not a very important factor in the study 3 When the vitamin D complex is applied to infant formula milk powder, after the milk powder is stored for 5 months at 50 DEG C 3 The content of (A) is reduced by 24 to 38 percent; when researchers study the stability of effective components of the compound premix in the storage process, the vitamin A content of the premix is reduced by 35-38% after the premix is stored for 6 months at 50 ℃. The great reduction of the nutrient content may be caused by a spray drying process, and after a long time of high-temperature fluidized drying, the nutrient components are damaged, so that the yield loss is large, and the microcapsules are easy to collapse and form irregular shapes, so that the microcapsules are easy to damage when being mixed with other products for processing.
Spray freeze drying techniques are therefore used instead of spray drying. For example, in the prior art, "a process for preparing polyunsaturated fatty acid oil microcapsules by spray freeze drying", atomized liquid droplets are frozen into solid particles in spray drying equipment, and the solid particles are coated with maltodextrin, and then the solid particles are transferred to vacuum drying equipment, and the drying temperature is gradually increased for drying, so that the polyunsaturated fatty acid oil microcapsules are obtained. Mixing soybean oil, fat-soluble flavor substances and alpha-lactalbumin to obtain a mixture; shearing and homogenizing the mixture at a high speed to obtain an emulsion; atomizing the emulsion into small droplets and spraying the droplets into liquid nitrogen; and (3) carrying out vacuum freeze drying on the frozen particles to obtain the alpha-lactalbumin flavor powder microcapsule.
Although the spray freeze drying technology well relieves the damage loss of hot air to nutrients and protects heat-sensitive nutrients to a greater extent, a large number of holes are formed in the particles due to rapid sublimation of moisture in the drying process, so that the rigidity of the product is insufficient, and the pressure resistance of the product is poor.
When the nutrient is applied to feed and dietary supplements, the temperature and pressure in the processing process are higher and higher, and the change of process conditions in the processing process puts higher requirements on the stability and the pressure resistance of products.
In summary, the existing nutrient microcapsules still have certain structural defects, so that the application stability and the pressure resistance of the microcapsules in feed and food still have a large space for improving.
Disclosure of Invention
In order to solve the above-mentioned disadvantages in the art, the present application aims to provide a multi-coated heat-sensitive nutrient microcapsule and a method for preparing the same.
According to one aspect of the present application, there is provided a multi-layered coated heat-sensitive nutrient microcapsule comprising:
nutrient microparticles;
the packaging material is filled in the inner pore canal of the nutrient particle and wraps the surface of the nutrient particle;
the outer wall material is wrapped outside the nutrient particles and the packaging material;
wherein the nutrient microparticles comprise: nutrients, inner wall material and oil.
According to some embodiments of the present application,said nutrient is selected from vitamin A, vitamin A ester, vitamin E ester, and vitamin D 2 Vitamin D 3 One or more of vitamin K, biotin, coenzyme Q10, curcumin, beta-carotene, lutein, canthaxanthin, lutein esters, lycopene, astaxanthin and polyunsaturated fatty acids.
According to some embodiments of the present application, the oil is selected from one or more of corn oil, soybean oil, sunflower oil, olive oil, coconut oil, rapeseed oil, cottonseed oil, aloe oil.
According to some embodiments of the application, the inner wall material is selected from one or more of maltodextrin, cyclodextrin, glucose, syrup, white granulated sugar, fructose, sucrose, glycerol, gum arabic, gelatin, starch octenyl succinate.
According to some embodiments of the present application, the encapsulating material is selected from one or more of a wax fat, a vegetable oil, and a hydrogenated vegetable oil;
further, the wax fat is selected from one or more of beeswax, carnauba wax, candelilla wax, microcrystalline wax, montanate wax, rice germ oil wax, spermaceti wax, lanolin wax, ximedwood wax, sasol wax, food grade paraffin wax and japan wax;
the vegetable oil is selected from one or more of palm oil, palm stearin and cocoa butter;
the hydrogenated vegetable oil is selected from one or more of hydrogenated cottonseed oil, hydrogenated palm oil, hydrogenated soybean oil and hydrogenated sunflower oil.
According to some embodiments of the present application, the outer wall material is selected from one or more of cellulose derivatives, acrylics, shellac, propolis, rosin, chitosan, chemically modified polysaccharides, prolamins, and crosslinked proteins.
Further, the outer wall material is selected from prolamin, ethyl cellulose, hydroxypropyl methylcellulose and polyacrylic resin IV
According to some embodiments of the present application, the nutrient microparticles further comprise an antioxidant;
further, the antioxidant is selected from one or more of vitamin E, ethoxyquinoline, BHT, BHA and TBHQ, tea polyphenol, propyl gallate, dilauryl thiodipropionate, rosemary extract, glycyrrhiza antioxidant, phytic acid, ascorbic acid, sodium ascorbate, D-erythorbic acid, D-sodium erythorbate, ascorbyl palmitate and lecithin.
According to some embodiments of the present application, the ratio of nutrient microparticles to encapsulating material is 20: (1-8); the weight of the outer wall material is increased by no more than 5 percent of the total weight.
According to another aspect of the present application, there is also provided a method for preparing the above-mentioned nutrient microcapsule, comprising:
(1) Dissolving the inner wall material in water, uniformly mixing with grease and nutrients, and shearing to obtain emulsion;
(2) Carrying out spray freeze drying on the emulsion to prepare nutrient particles;
(3) Filling an encapsulating material into the inner pore canal of the nutrient particle in a vacuum impregnation or vacuum spraying mode, and wrapping the surface of the nutrient particle to form a first coating layer;
(4) Suspending the packaged particles in fluidized air, and spraying the outer wall material to the surface of the particles to form a second coating layer.
According to some embodiments of the present application, the spraying pressure in the step (2) is 0.2 to 0.5MPa, the freezing temperature is less than or equal to-15 ℃, the vacuum drying temperature is 35 to 60 ℃, and the vacuum degree is 20 to 80KPa.
According to some embodiments of the present application, the filling of the encapsulation material into the inner pores of the nutrient microparticles and the wrapping of the encapsulation material on the surface of the nutrient microparticles by means of vacuum impregnation comprises: and immersing the nutrient particles into the packaging material under the conditions of preset vacuum degree, preset temperature and preset stirring speed, gradually relieving pressure and standing until normal pressure after stirring for preset time, so that the packaging material is filled into the internal pore channels of the nutrient particles and wraps the surface of the nutrient particles to form a first coating layer.
Further, the predetermined vacuum degree of the vacuum impregnation is: 0.1 to 0.2MPa, the preset temperature is 35 to 55 ℃, and the preset time is 0.5 to 1 hour.
According to some embodiments of the application, the packaging material is filled into the inner pores of the nutrient particles by means of vacuum spraying, and is wrapped on the surfaces of the nutrient particles to form a first coating layer.
According to some embodiments of the present application, suspending the encapsulated particles in fluidized air, spraying an outer wall material onto the surface thereof, comprises: the atomization pressure is 0.15-0.20 MPa, the air inlet temperature is 60-80 ℃, and the spraying flow rate is 3-5 g/min.
The present application provides a multi-layered coated heat-sensitive nutrient microcapsule comprising: nutrient microparticles; the nutrient particles are filled with the nutrient particles, the nutrient particles are wrapped with the packaging material, and the nutrient particles and the packaging material are wrapped with the outer wall material. The interior of the nutrient particle is filled with the packaging material, so that the microcapsule is not easy to absorb water and deteriorate, has good stability, long shelf life and good rigidity, and is not easy to damage, deform and the like in the subsequent processing process. Meanwhile, a protective layer is added after the packaging material is filled, and the inner-layer compact structure is combined with the protective layer of the outer-layer wall material to form a multilayer coating layer, so that the stability of the microcapsule is further enhanced, the high-temperature and high-humidity resistance of the microcapsule is improved, and the shelf life of the product is prolonged.
The nutrient particles comprise nutrients, inner wall materials and grease, wherein the nutrients are dissolved in the grease, so that the uniformity of the nutrients in the particles can be improved, and the stability of the nutrients can also be improved; the fats and oils herein are optional physiologically acceptable fats and oils, preferably liquid oils;
according to the multilayer coated heat-sensitive nutrient microcapsule, high-melting-point grease and/or wax grease are selected as packaging materials to fill pore channels of particles, and a first coating layer is formed on the surfaces of the particles: on one hand, air in the pore passage inside the particle is replaced, the oxidation speed is slowed down, air and moisture are isolated, the stability of the particle is effectively improved, on the other hand, the structure of the particle is more compact, the compression resistance is greatly improved, the bulk density of the particle is improved, and the dispersibility of the particle in the premix is improved;
the application also provides a preparation method of the multilayer-coated heat-sensitive nutrient microcapsule, which comprises the steps of firstly selecting a spray freezing granulation technology, retaining nutrient components to the maximum extent, forming porous particles which are more approximate to a spherical shape, then filling pore channels in the particles in a vacuum impregnation or vacuum grease spraying mode, forming a first coating layer on the surfaces of the particles, and finally coating a protective layer. The compact and crack-free double-layer protection and the honeycomb structure filled with the encapsulating material inside endow the microcapsule with the capability of better bearing mechanical stress, thereby overcoming the problem of microcapsule damage easily caused in tablet tabletting in the feed processing process.
The application combines the spray freezing granulation technology with the vacuum impregnation technology, can improve the retention rate of the heat-sensitive nutrients to the maximum extent, and realizes integrated and continuous operation.
Drawings
Fig. 1 is a schematic structural view of a multi-layer coated heat-sensitive nutrient microcapsule of the present application.
Detailed Description
As mentioned above, the current nutrient microcapsule products are porous granules, which cannot effectively isolate oxygen and moisture, and are prone to moisture absorption and deterioration during storage and transportation, and meanwhile, due to the porous structure, the product has insufficient rigidity, and is limited in feed processing and tablet application. In view of the above problems, the present application provides a multi-layer coated heat-sensitive nutrient microcapsule and a method for preparing the same.
The technical solutions of the present application will be described clearly and completely in conjunction with the embodiments of the present application, and it is obvious that the described embodiments are some, but not all, of the embodiments of the present application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It is specifically noted that similar alternatives and modifications will be apparent to those skilled in the art for the present application, which are all considered to be included in the present application. It will be apparent to those skilled in the art that modifications or appropriate variations and combinations of the methods and applications described herein can be made to implement and use the techniques of this application without departing from the spirit and scope of the disclosure. It is to be understood that the embodiments described are only a few embodiments of the present application and not all embodiments.
If the specific conditions are not indicated, the method is carried out according to the conventional conditions or the conditions suggested by the manufacturer, and the raw material medicines or auxiliary materials and the reagents or instruments used by the method are conventional products which can be obtained commercially.
According to the technical concept of the present application, there is provided a multi-layered coated heat-sensitive nutrient microcapsule and a method for preparing the same.
The preparation method of the microcapsule comprises the following steps:
1) Dissolving the inner wall material in water, mixing with oil and nutrients, and shearing to obtain emulsion;
2) Pumping the emulsion into an integrated spray freeze drying device, controlling the spray pressure to be 0.2-0.5MPa and the freezing temperature to be less than or equal to-15 ℃, and performing vacuum drying until the water content of the material is 5-8% to obtain nutrient particles;
3) Adjusting the vacuum degree and the temperature, immediately adding an encapsulating material solution for dipping or spraying to ensure that the encapsulating material completely fills the pore passages inside the nutrient particles, forming a first coating layer on the surfaces of the nutrient particles, and filtering and drying to obtain the nutrient microcapsules filled and coated with the encapsulating material;
4) Collecting the nutrient microcapsule containing the packaging material, completely suspending the nutrient microcapsule in fluidized air, spraying the outer-layer wall material solution onto the surface of the nutrient microcapsule, and drying to obtain the multilayer-coated nutrient microcapsule.
Wherein, the proportion relation among the nutrients, the inner wall material and the grease is adjusted according to different types of the nutrients.
The oil is selected from one or more of soybean oil, oleum Maydis, oleum Arachidis Hypogaeae, oleum Cocois, oleum Sesami, oleum Olivarum, oleum Rapae, rice bran oil, and oleum Helianthi.
Further, an antioxidant can be further included in the step (1).
The antioxidant is selected from one or more of vitamin E, ethoxyquinoline, BHT, BHA and TBHQ, tea polyphenols, propyl gallate, dilauryl thiodipropionate, herba Rosmarini officinalis extract, glycyrrhrizae radix antioxidant, phytic acid, ascorbic acid, sodium ascorbate, D-isoascorbic acid, ascorbyl palmitate, and lecithin;
according to the preparation method, in the step 3), the packaging material is heated and melted in a constant-temperature water bath box and then is sent into a drying chamber of an integrated spray freezing system by a peristaltic pump;
according to some embodiments of the present application, the packaging material may be dissolved in an organic solvent to form a packaging material solution, and then the packaging material solution is pumped into a drying chamber of the integrated spray freezing system by a peristaltic pump for filling;
wherein the organic solvent comprises dichloromethane, ethyl acetate, isobutyl acetate, acetone, ethanol, butanone, tetrahydrofuran, isobutanol, isopropanol and the like.
In order to improve the stability and pressure resistance of the freeze-dried product, the invention adopts a vacuum impregnation/vacuum spraying mode to inject the packaging material into the inner pore path of the microcapsule, and finally, the microcapsule coating outer wall material filled with the packaging material is protected.
The present application will be described in detail with reference to specific examples.
Example 1 vitamin A microcapsules and preparation thereof
The raw materials comprise:
inner wall material 220.8g of starch sodium octenyl succinate; 286g of maltodextrin
Nutrient Vitamin A acetate crystal 180g
Oil and fat Corn oil 150g
Antioxidant agent Ethoxyquinoline 40g
Packaging material Palm stearin
Outer wall material Alcohol soluble protein solution
(1) Crystallizing vitamin A acetate, and shearing corn oil and ethoxyquin at 60-70 deg.C for 30min to obtain oil phase;
dissolving sodium starch octenyl succinate and maltodextrin in water, keeping the temperature at 85 ℃ for 30min, and performing low-speed shearing at 550r/min to obtain a water phase;
mixing the oil phase and the water phase, and fully emulsifying to obtain an emulsion;
(2) Spraying the emulsion into a vacuum spray freeze drying device by a peristaltic pump, controlling the spray pressure to be 0.2MPa, the freezing temperature to be less than or equal to minus 15 ℃, the vacuum drying temperature to be 35-60 ℃ and the vacuum degree to be 20-80 KPa, and drying until the water content of the material is 5-8% to prepare vitamin A acetate particles;
(3) Vacuum impregnation: adjusting the vacuum degree of a drying chamber to 0.1-0.2 MPa, the temperature to 35-55 ℃, heating and melting palm stearin in a constant-temperature water bath box, then conveying the palm stearin into the vacuum drying chamber by a peristaltic pump, stirring for 5-10min, standing, gradually releasing pressure, standing for 0.5-1 h, keeping for 10min after normal pressure, completely filling the palm stearin into pore channels inside vitamin A acetate particles, and forming a first coating layer on the surfaces of the nutrient particles;
(4) Directly introducing the particles obtained in the step (3) into a fluidized bed, spraying a prolamin solution, and embedding the microcapsules filled with the grease, wherein the atomization pressure is 0.15-0.20 MPa, the air inlet temperature is 60-80 ℃, and the spraying flow rate is 3-5 g/min;
(5) The microcapsules obtained after drying were collected and the vitamin a acetate retention in the production process was calculated to be 99.7%.
Example 2 beta-Carotene microcapsules and their preparation
The raw materials comprise:
inner wall material Gelatin 400g
Nutrient Beta-carotene Crystal 70g
Oil and fat Olive oil 290g
Antioxidant agent Ascorbyl palmitate 27g
Organic solvent Acetone 8kg
Packaging material Food grade paraffin wax
Outer wall material Ethyl cellulose solution
(1) Mixing beta-carotene crystal, ascorbyl palmitate and olive oil, and heating to 55 ℃ to prepare a beta-carotene solution to prepare an oil phase;
dissolving gelatin in water, keeping the temperature at 60-70 ℃ for 30min, and preparing a water phase at a low-speed shearing speed of 550 r/min;
mixing the oil phase and the water phase, emulsifying, and homogenizing at 800bar under high pressure for 20min to obtain emulsion;
(2) Spraying the emulsion into a vacuum spray freeze drying device by a peristaltic pump, controlling the spray pressure to be 0.5MPa, the freezing temperature to be less than or equal to minus 15 ℃, the vacuum drying temperature to be 35-60 ℃ and the vacuum degree to be 20-80 KPa, and drying until the water content of the material is 5-8% to prepare beta-carotene particles;
(3) Vacuum spraying: collecting the beta-carotene particles obtained in the step (2), putting the beta-carotene particles into vacuum spraying equipment, heating and melting food-grade paraffin in acetone, and then conveying the molten food-grade paraffin into the vacuum spraying equipment by a peristaltic pump to ensure that the paraffin completely fills the inner pore channels of the beta-carotene particles and forms a first coating layer on the surfaces of the nutrient particles;
(4) Directly introducing the particles obtained in the step (3) into a fluidized bed, spraying ethyl cellulose solution, embedding the microcapsules filled with the grease, wherein the atomization pressure is 0.15-0.20 MPa, the air inlet temperature is 60-80 ℃, and the spraying flow rate is 3-5 g/min;
(5) The microcapsules obtained after drying were collected and the retention of beta-carotene in the production process was calculated to be 97.1%.
Example 3
The raw materials comprise:
inner wall material 223g of starch sodium octenyl succinate; maltodextrin 270g
Nutrient 185g of vitamin A acetate crystal
Oil and fat 152g of sunflower seed oil
Antioxidant agent Ethoxyquinoline 41g
Packaging material Beeswax (Cera flava)
Outer wall material Chitosan
(1) Carrying out high-speed shearing on the vitamin A acetate crystal, the ethoxyquinoline and the sunflower seed oil for 30min at the temperature of 60-70 ℃ to prepare an oil phase;
dissolving sodium starch octenylsuccinate and maltodextrin in water, keeping the temperature at 85 ℃ for 30min, and performing low-speed shearing at 550r/min to obtain a water phase;
mixing the oil phase and the water phase, and fully emulsifying to obtain an emulsion;
(2) Spraying the emulsion into a vacuum spray freeze drying device by a peristaltic pump, controlling the spray pressure to be 0.5MPa, the freezing temperature to be less than or equal to minus 15 ℃, the vacuum drying temperature to be 35-60 ℃ and the vacuum degree to be 20-80 KPa, and drying until the water content of the material is 5-8% to obtain vitamin A acetate particles;
(3) Adjusting the vacuum degree of a drying chamber to 35-50 KPa and the temperature to 0-30 ℃, heating and melting beeswax in a constant temperature water bath box, then sending the beeswax into the vacuum drying chamber by a peristaltic pump, stirring for 5min, standing, gradually releasing pressure, standing until the pressure is normal, keeping for 10min, completely filling pores inside vitamin A acetate particles with beeswax, and forming a first coating layer on the surface of the nutrient particles;
(4) Directly introducing the particles obtained in the step (3) into a fluidized bed, spraying chitosan, embedding the microcapsules filled with the grease, wherein the atomization pressure is 0.15-0.20 MPa, the air inlet temperature is 60-80 ℃, and the spraying flow rate is 3-5 g/min;
(5) The microcapsules obtained after drying were collected and the vitamin a acetate retention in the production process was calculated to be 97.8%.
Comparative example 1 microcapsules prepared by a conventional spray-drying method
Weighing 220.8g of octenyl succinic acid starch sodium, 286g of maltodextrin, 578g of water, preserving heat for 30min at 85 ℃, and dissolving at a low-speed shearing speed of 550r/min to prepare a water phase; after the water phase is completely dissolved, adding an oil phase core material under the condition of high-speed shearing, wherein the oil phase core material consists of 180g of vitamin A acetate crystals and 40g of ethoxyquinoline, shearing for 30min, carrying out spray drying, and collecting and drying the microcapsule.
Comparative example 2 vacuum impregnation was not carried out
The raw materials comprise:
Figure BDA0003503765890000111
Figure BDA0003503765890000121
(1) Carrying out high-speed shearing on the vitamin A acetate crystals, ethoxyquin and corn oil at the temperature of 60-70 ℃ for 30min to prepare an oil phase core material;
dissolving sodium starch octenyl succinate and maltodextrin in water, keeping the temperature at 85 ℃ for 30min, and performing low-speed shearing at 550r/min to obtain a water phase;
mixing and shearing the oil phase core material and the water phase wall material, and fully emulsifying to obtain an emulsion;
(2) Spraying the emulsion into a vacuum spray freeze drying device by a peristaltic pump, controlling the spray pressure to be 0.2MPa, the freezing temperature to be less than or equal to minus 15 ℃, the vacuum drying temperature to be 35-60 ℃ and the vacuum degree to be 20-80 KPa, and drying until the water content of the material is 5-8% to obtain vitamin A acetate particles;
(3) Directly introducing the particles obtained in the step (2) into a fluidized bed, spraying alcohol soluble protein solution, embedding the microcapsules filled with the oil, wherein the atomization pressure is 0.15-0.20 MPa, the air inlet temperature is 60-80 ℃, and the spraying flow rate is 3-5 g/min;
(4) The microcapsules obtained after drying were collected.
Test examples
The products of the above examples 1-3 and comparative examples 1-2 were tested by the following specific methods:
(1) And (3) microcapsule product stability detection:
and (3) respectively sealing the products by using plastic bags and aluminum foil bags, and detecting the liquid phase content under the stability test conditions of 40 +/-2 ℃ and 75% +/-5% humidity in the test period of 1, 2 and 3 months (external standard method). The results are shown in Table 1:
TABLE 1 stability test results
Figure BDA0003503765890000122
Figure BDA0003503765890000131
As calculated from the data in the table above, the retention of vitamin a acetate in example 1 after 3 months was 97.9%; the retention of beta-carotene after 3 months in example 2 was 95.7%; the vitamin a acetate of example 3 has a retention of 85.7% after 3 months. Whereas the vitamin a acetate of comparative example 1 and comparative example 2 had a retention after 3 months of only 57.1% and 62.0%, respectively.
The stability of the nutrient microcapsule product can be obviously improved by adopting the technologies of spray freeze drying, grease filling and outer wall protective film.
(2) After the microcapsule is applied to the compound vitamin tablet, the stability of the microcapsule is detected:
multivitamin mineral tablets having about 1500IU of vitamin a acetate per tablet were prepared. And (3) tabletting environmental conditions: the environmental humidity is about 45 percent, the environmental temperature is 18-25 ℃, and the pressure of the tablet press is 30-40 KN. After pressing, the liquid phase content is detected under the stability test conditions of 40 +/-2 ℃ and 75% +/-5% humidity according to a commercial package under the test period of 1, 2 and 3 months (external standard method). The results are shown in Table 2:
TABLE 2 stability test results
Figure BDA0003503765890000132
According to the data calculation in the table, when the nutrient microcapsule is applied to the multivitamin tablet, the stability of the nutrient in the tablet can be obviously improved by adopting the technologies of spray freeze drying, grease filling and outer wall protection film. The retention of vitamin a acetate in example 1 after 3 months was 85.9%; the retention of the nutrient of comparative example 1 after 3 months was 58.5%; comparative example 2 was only 64.1%.
(3) And (3) texture determination:
the hardness of the examples, comparative examples and control were measured using a texture analyzer.
The measurement was carried out in a TMS-PRO type texture analyzer (Food Technology, U.S.A.) TPA format, and each sample was measured in 3 replicates and averaged.
Measurement parameters are as follows: the measurement results of the operating program (YPA-25N addition recoverability), the sensor range (25N), the probe height (20 mm), the deformation amount (100%), the probe operating rate (60 mm/min), and the initial force (0.005N) are shown in Table 3:
TABLE 3 texture test results
Microcapsules Hardness of Toughness of
Example 1 8.637N When the deformation is 89%, the crushing peak is generated
Example 2 8.532N Has a breaking peak when the deformation is 92%
Example 3 8.023N When the deformation is 60 percent, the crushing peak is generated
Comparative example 1 7.877N When the deformation is 50 percent, the crushing peak is generated
Comparative example 2 7.378N Has a breaking peak when the deformation is 45 percent
As can be seen from the data in table 3, compared to comparative examples 1 and 2, hardness and toughness of examples 1, 2 and 3 are significantly increased, which shows that the microcapsules subjected to the techniques of spray freeze drying, oil filling and outer wall protection can enhance pressure resistance, and allow the nutrient microcapsules to be applied in downstream products in a wider range, and have a better elastic change range in the face of variable process conditions.
The above description of the embodiments is only intended to help understand the method of the present application and its core ideas. It should be noted that, for those skilled in the art, it is possible to make several improvements and modifications to the present application without departing from the principle of the present application, and such improvements and modifications also fall within the scope of the claims of the present application.

Claims (15)

1. A multi-layer coated heat-sensitive nutrient microcapsule, comprising:
nutrient microparticles;
the packaging material is filled in the inner pore canal of the nutrient particle and wraps the surface of the nutrient particle;
the outer wall material is wrapped outside the nutrient particles and the packaging material;
wherein the nutrient microparticles comprise: nutrients, inner wall materials and grease;
the mass ratio of the nutrient particles to the packaging material is 20: (1-8);
the weight of the outer wall material is increased by no more than 5 percent of the total weight;
the preparation method of the microcapsule comprises the following steps:
(1) Dissolving the inner wall material in water, uniformly mixing with grease and nutrients, and shearing to obtain emulsion;
(2) Carrying out spray freeze drying on the emulsion to prepare nutrient particles;
(3) Filling an encapsulating material into the inner pore canal of the nutrient particle in a vacuum impregnation or vacuum spraying mode, and wrapping the surface of the nutrient particle to form a first coating layer;
(4) And suspending the packaged particles in fluidized air, and spraying the outer-layer wall material to the surface of the particles to form a second coating layer.
2. The nutrient microcapsule according to claim 1, wherein the nutrient is selected from the group consisting of vitamin A, vitamin A esters, vitamin E esters, vitamin D 2 Vitamin D 3 One or more of vitamin K, biotin, coenzyme Q10, curcumin, beta-carotene, lutein, canthaxanthin, lutein esters, lycopene, astaxanthin and polyunsaturated fatty acids.
3. The nutrient microcapsule according to claim 1, wherein the oil is selected from one or more of corn oil, soybean oil, sunflower oil, olive oil, coconut oil, rapeseed oil, cottonseed oil, and aloe oil.
4. The nutrient microcapsule of claim 1, wherein the inner wall material is selected from one or more of maltodextrin, cyclodextrin, glucose, syrup, white granulated sugar, fructose, sucrose, glycerol, gum arabic, gelatin, starch octenyl succinate.
5. The nutrient microcapsule according to claim 1, wherein the encapsulating material is selected from one or more of wax fat, vegetable oil and hydrogenated vegetable oil.
6. The nutrient microcapsule according to claim 5, wherein the wax fat is selected from one or more of beeswax, carnauba wax, candelilla wax, microcrystalline wax, montanate wax, rice germ oil wax, spermaceti wax, lanolin wax, simmental wax, sasol wax, food grade paraffin wax, and Japan wax;
the vegetable oil is selected from one or more of palm oil, palm stearin and cocoa butter;
the hydrogenated vegetable oil is selected from one or more of hydrogenated cottonseed oil, hydrogenated palm oil, hydrogenated soybean oil and hydrogenated sunflower oil.
7. The nutrient microcapsule according to claim 1, wherein the outer wall material is selected from one or more of cellulose derivatives, acrylics, shellac, propolis, rosin, chitosan, chemically modified polysaccharides, prolamin, and cross-linked protein.
8. The nutrient microcapsule according to claim 1, wherein the outer wall material is selected from prolamin, ethylcellulose, hypromellose, and polyacrylic resin No. IV.
9. The nutrient microcapsule of claim 1, further comprising an antioxidant in the nutrient microparticles.
10. The nutrient microcapsule according to claim 9, wherein the antioxidant is selected from one or more of vitamin E, ethoxyquin, BHT, BHA and TBHQ, tea polyphenol, propyl gallate, dilauryl thiodipropionate, rosemary extract, glycyrrhiza antioxidant, phytic acid, ascorbic acid, sodium ascorbate, D-erythorbic acid, sodium D-erythorbate, ascorbyl palmitate, lecithin.
11. A process for the preparation of a nutrient microcapsule according to any one of claims 1 to 10 comprising:
(1) Dissolving the inner wall material in water, uniformly mixing with grease and nutrients, and shearing to obtain emulsion;
(2) Carrying out spray freeze drying on the emulsion to prepare nutrient particles;
(3) Filling an encapsulating material into the inner pore canal of the nutrient particle in a vacuum impregnation or vacuum spraying mode, and wrapping the surface of the nutrient particle to form a first coating layer;
(4) Suspending the packaged particles in fluidized air, and spraying the outer wall material to the surface of the particles to form a second coating layer.
12. The preparation method according to claim 11, wherein the spraying pressure in the step (2) is 0.2 to 0.5MPa, the freezing temperature is less than or equal to-15 ℃, the vacuum drying temperature is 35 to 60 ℃, and the vacuum degree is 20 to 80KPa.
13. The method according to claim 11, wherein the vacuum impregnation process in the step (3) comprises: and immersing the nutrient particles into the packaging material, stirring for a preset time, gradually relieving pressure, standing until normal pressure is reached, filling the packaging material into the inner pore channels of the nutrient particles, and wrapping the surface of the nutrient particles to form a first coating layer.
14. The method according to claim 13, wherein the vacuum degree of the vacuum impregnation is 0.1 to 0.2MPa, the temperature is 35 to 55 ℃, and the time is 0.5 to 1h.
15. The process according to claim 11, wherein the atomization pressure in the step (4) is 0.15 to 0.20MPa, the temperature of the air supply is 60 to 80 ℃, and the spraying flow rate is 3 to 5g/min.
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