CN108392635B - Essence microcapsule and preparation method and application thereof - Google Patents

Essence microcapsule and preparation method and application thereof Download PDF

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Publication number
CN108392635B
CN108392635B CN201810069890.XA CN201810069890A CN108392635B CN 108392635 B CN108392635 B CN 108392635B CN 201810069890 A CN201810069890 A CN 201810069890A CN 108392635 B CN108392635 B CN 108392635B
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release layer
essence
capsule core
slow release
aroma substance
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CN108392635A (en
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邓晶晶
彭姣凤
刘娟
刘能
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Botton Spices Co ltd
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Dongguan Boton Flavors & Fragrances Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
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    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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Abstract

The invention relates to an essence microcapsule and a preparation method and application thereof. The essence microcapsule comprises a capsule core, a slow release layer and a quick release layer, wherein the slow release layer and the quick release layer are sequentially coated on the capsule core, the capsule core is made of a first aromatic substance, the slow release layer is made of at least one of Arabic gum, hydroxypropyl methyl cellulose, chitosan, polyvinyl alcohol, polyethylene glycol, ethyl cellulose, konjac glucomannan, gelatin and pullulan, the quick release layer is made of a second aromatic substance, and the fragrance of the second aromatic substance is consistent with that of the first aromatic substance. The essence microcapsule has long fragrance duration, strong fragrance intensity and good fragrance outbreak.

Description

Essence microcapsule and preparation method and application thereof
Technical Field
The invention relates to the field of essence and flavor, and particularly relates to an essence microcapsule and a preparation method and application thereof.
Background
The essence is prepared by mixing various fragrant raw materials, and the physical and chemical properties of the components may have large difference, so that some components are easy to volatilize or easy to deteriorate under the influence of external environment, and the essence has the defects of short fragrance duration, short shelf life of products and the like when being applied to downstream fragrant products. In order to protect the essence, prevent the essence from volatilizing, prolong the fragrance release time, and achieve the effects of slow release and even controlled release, the microencapsulation technology is usually adopted to achieve the above purposes, however, some microcapsule essences achieve a certain slow release effect, but the slow release effect is not ideal, the fragrance duration time is still short, and the problems of insufficient fragrance intensity and weak explosiveness generally exist in the application of the microcapsule essences.
Disclosure of Invention
Therefore, there is a need for providing a perfume microcapsule with long fragrance duration, strong fragrance intensity and good fragrance burst.
In addition, a preparation method and application of the essence microcapsule are also provided.
An essence microcapsule comprises a capsule core, a slow release layer and a quick release layer, wherein the slow release layer and the quick release layer are sequentially coated on the capsule core, the capsule core is made of a first aromatic substance, the slow release layer is made of at least one of acacia, hydroxypropyl methyl cellulose, chitosan, polyvinyl alcohol, polyethylene glycol, ethyl cellulose, konjac glucomannan, gelatin and pullulan, the quick release layer is made of a second aromatic substance, and the fragrance of the second aromatic substance is consistent with that of the first aromatic substance.
The surface of the capsule core containing the first aroma substance is coated with the slow release layer of the material, so that the volatilization of the aroma of the first aroma substance can be effectively reduced, the effect of prolonging the aroma release time of the capsule core is achieved, the aroma of the essence microcapsule can last for a relatively strong time, and the problems of weakened aroma intensity and insufficient explosiveness caused by the embedding of the capsule core by the slow release layer can be solved by coating the surface of the slow release layer with the quick release layer containing the second aroma substance with the aroma consistent with the aroma of the first aroma substance.
In one embodiment, the capsule core comprises the following materials in percentage by mass: 0.1-20% of the first aroma substance, 0.1-30% of an adsorbent, 50-98% of a filler and 0-1% of a first binder.
In one embodiment, the adsorbent is a porous material.
In one embodiment, the filler is selected from at least one of starch, starch derivatives, carbohydrates, cellulose, and cellulose derivatives.
In one embodiment, the first aroma is selected from at least one of a fragrance, a flavor, and a plant extract; the second aroma substance is at least one of essence, spice and plant extract.
In one embodiment, the mass ratio of the sustained-release layer to the capsule core is 1: 100-15: 100.
In one embodiment, the material of the quick release layer comprises, by mass percent: 0.1-40% of the second aroma substance, 60-99.8% of the second binder, 0-5% of the disintegrating agent, 0-8% of the emulsifier and 0-0.5% of the pigment.
In one embodiment, the emulsifier is selected from at least one of glyceryl monostearate, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyglycerol fatty acid ester, sucrose fatty acid ester, polyoxyethylene hydrogenated castor oil, xylitol anhydride monostearate, phospholipid and modified soybean phospholipid; and/or the disintegrating agent is selected from at least one of hydroxypropyl methylcellulose, croscarmellose sodium, sodium carboxymethyl starch and crospovidone, and/or the second binder is selected from at least one of starch, starch derivatives, acacia, gelatin, shellac, agar, oligosaccharide, sodium alginate, polyvinyl alcohol and cellulose.
In one embodiment, the ratio of the sum of the mass of the capsule core and the mass of the slow release layer to the mass of the quick release layer is (70-99) to (1-30).
A preparation method of essence microcapsules comprises the following steps:
coating a slow release material on the surface of the capsule core to form a slow release layer, wherein the material of the capsule core comprises a first aroma substance, and the slow release material is selected from at least one of Arabic gum, hydroxypropyl methyl cellulose, chitosan, polyvinyl alcohol, polyethylene glycol, ethyl cellulose, konjac glucomannan, gelatin and pullulan; and
forming a quick release layer on the outer surface of the slow release layer so that the quick release layer is coated on the outer surface of the slow release layer to obtain the essence microcapsule, wherein the material of the quick release layer comprises a second aroma substance, and the aroma of the second aroma substance is consistent with that of the first aroma substance.
In one embodiment, before the step of coating the surface of the capsule core with the sustained-release material, the method further comprises the step of preparing the capsule core:
weighing raw materials according to mass percentage, wherein the raw materials comprise: 0.1-20% of the first aroma substance, 0.1-30% of an adsorbent, 50-98% of a filler and 0-1% of a first binder;
mixing the raw materials with a first solvent to obtain a mixture;
forming the mixed material to obtain a pill;
drying the pellets to remove the first solvent, resulting in the caplets.
In one embodiment, the step of coating the sustained-release material on the surface of the capsule core comprises the following steps: dissolving the slow-release material in a second solvent to obtain slurry; coating the slurry on the surface of the capsule core.
In one embodiment, the step of forming the immediate release layer on the outer surface of the sustained release layer is:
weighing the following components in percentage by mass: 0.1-40% of the second aroma substance, 60-99.8% of the second binder, 0-5% of a disintegrating agent, 0-8% of an emulsifying agent and 0-0.5% of a pigment;
mixing the components with water to form an emulsion;
coating the emulsion on the outer surface of the slow release layer to form the quick release layer.
The essence microcapsule is applied to food, daily chemical products, medicine preparation, health products or tobacco products.
Drawings
Fig. 1 is a schematic structural diagram of a perfume microcapsule according to an embodiment;
fig. 2 is a flow chart of a method of making perfume microcapsules according to one embodiment;
fig. 3 is a flow chart of the core preparation steps in the preparation method of the perfume microcapsule shown in fig. 2;
fig. 4 is a flowchart of the preparation steps of the immediate release layer in the method of preparing the microcapsule with fragrance shown in fig. 2.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
As shown in fig. 1, an essence microcapsule 100 according to an embodiment includes a core 110, and a sustained-release layer 120 and a quick-release layer 130 sequentially coated on the core 110.
The material of the core 110 includes a first aroma substance. Specifically, the material of the capsule core 110 includes, by mass: 0.1-20% of first aroma substance, 0.1-30% of adsorbent, 50-98% of filler and 0-1% of first binder.
The first aroma substance is at least one selected from essence, perfume and plant extract. Wherein the essence is selected from one of peppermint essence, fruit essence, flower essence, milk essence, coffee essence, chocolate essence, nut essence, baking essence, green essence, grass essence, costustoot essence and wine essence; the perfume is selected from one of daily chemical perfume, edible perfume and tobacco perfume. The plant extract may be, but not limited to, tea extract, aloe extract, honeysuckle extract, pueraria extract, peppermint extract, ginseng extract, angelica extract, licorice extract, peony extract, calendula extract, etc., rose extract, etc.
The adsorbent is a porous material, can be a natural porous material, and can also be a synthetic porous material. The first aroma substance is adsorbed in the porous structure of the adsorbent.
Specifically, the adsorbent is selected from at least one of porous starch, silica, activated carbon, and organic porous polymer. Specifically, the organic porous polymer may be, but is not limited to, super crosslinked polystyrene, polysulfone, polyarylate, borate ester, and the like.
Further, the adsorbent consists of porous starch and silicon dioxide in a mass ratio of 1: 0.2-1: 0.5. The application of the adsorbent can enable the essence microcapsule to have wider application range and be used in food, daily chemicals and tobacco.
The filler is at least one selected from starch, starch derivatives, saccharides, cellulose and cellulose derivatives. Wherein the starch derivative is selected from at least one of maltodextrin, malto-oligosaccharide, beta-cyclodextrin, sodium starch octenylsuccinate and hydroxypropyl starch. The saccharide compound is at least one selected from glucose, fructose, lactose, sucrose, oligosaccharide, chitosan, carrageenan and konjac gum. The cellulose derivative is at least one selected from microcrystalline cellulose, cellulose acetate butyrate, methyl cellulose, carboxymethyl cellulose, ethyl cellulose, hydroxyethyl cellulose and hydroxypropyl cellulose.
Furthermore, the filler comprises microcrystalline cellulose, maltodextrin and lactose in a mass ratio of (0.5-1) to (0.5-1).
It should be noted that the starch referred to herein is a normal starch, i.e., a starch that has not been subjected to modification or denaturation treatment; starch derivatives refer to derivatives of starch raw materials produced by biochemical reactions.
The first binder is at least one selected from hydroxypropyl methylcellulose, polyvinylpyrrolidone, sodium carboxymethylcellulose, xanthan gum and sodium alginate. Further, the first binder is selected from one of hydroxypropyl methylcellulose and sodium carboxymethyl cellulose.
Specifically, the core 110 is a pellet-like structure. The common essence microcapsule is usually in a powder type, so dust is easily generated in the production process, when the common essence microcapsule is applied, particularly in a product with a granular final shape, the compatibility of the powder essence and the granular product is poor, the essence is unevenly distributed in the product, even the essence is separated from the product, and the delamination causes adverse effects on the shape and the quality of the product, and the capsule core 110 is made into a pill-shaped structure with a certain granularity, and the first aroma substance is adsorbed in the adsorbent, so that the problem of dust generated in the production process of the powder essence can be effectively solved, and the problems of poor compatibility of the powder essence and the granular product, uneven distribution of the essence and delamination of the essence and the product are caused in the application process.
The material of the sustained-release layer 120 is at least one selected from gum arabic, hydroxypropyl methylcellulose, chitosan, polyvinyl alcohol, polyethylene glycol, ethyl cellulose, konjac gum, gelatin, and pullulan. These materials have good film-forming properties and can slowly release the fragrance of the capsule core. Further, the material of the sustained-release layer 120 is at least one selected from gum arabic, pullulan, and polyvinyl alcohol. The material of the sustained-release layer 120 has good film-forming property, and can form a semipermeable membrane on the surface of the capsule core 110 to control the release of the first aroma substance in the capsule core 110, so that the sustained-release layer has better sustained-release effect.
Specifically, the mass ratio of the sustained-release layer 120 to the capsule core 110 is 1: 100-15: 100. The mass ratio can enable the slow release layer 120 to have a proper thickness so as to ensure that the fragrance of the essence in the capsule core 110 can be slowly released, and the fragrance of the essence microcapsule 100 can last for a long time. Further, the mass ratio of the sustained-release layer 120 to the capsule core 110 is 1: 100-8: 100.
The material of the immediate release layer 130 includes a second aroma. Specifically, the material of the quick release layer 130 includes, by mass percent: 0.1-40% of second aroma substance, 60-99.8% of second binder, 0-5% of disintegrating agent, 0-8% of emulsifier and 0-0.5% of pigment.
The second aroma substance is at least one selected from essence, perfume and plant extract. Wherein, in the second aroma substance, the essence is selected from one of peppermint essence, fruit essence, flower essence, milk essence, coffee essence, chocolate essence, nut essence, baking essence, green essence, grass essence, costustoot essence and wine essence; the perfume is selected from one of daily chemical perfume, edible perfume and tobacco perfume. The plant extract may be, but not limited to, tea extract, aloe extract, honeysuckle extract, pueraria extract, peppermint extract, ginseng extract, angelica extract, licorice extract, peony extract, calendula extract, etc., rose extract, etc.
In particular, the second aroma is in accordance with the note of the first aroma to ensure that the second aroma has the same aroma as the first aroma.
The second binder is at least one selected from starch, starch derivatives, acacia, gelatin, shellac, agar, sodium alginate, polyvinyl alcohol and cellulose. Specifically, the starch derivative is at least one selected from maltodextrin, maltooligosaccharide, beta-cyclodextrin, sodium starch octenylsuccinate and hydroxypropyl starch. The second binder has certain emulsifiability, film-forming property and adhesiveness, so that the second aroma substance can be adhered to the surface of the slow-release layer 120.
Further, the second binder is composed of sodium starch octenyl succinate, Arabic gum and maltodextrin in a mass ratio of 1:1 (5-10).
The disintegrant is at least one selected from hydroxypropyl methylcellulose, croscarmellose sodium, sodium carboxymethyl starch, and crospovidone. The disintegrant accelerates disintegration and diffusion of the immediate release layer 130.
The emulsifier is at least one selected from glyceryl monostearate, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyglycerol fatty acid ester, sucrose fatty acid ester, polyoxyethylene hydrogenated castor oil, xylitol anhydride monostearate, soybean phospholipid and modified soybean phospholipid.
The pigment may be natural pigment or synthetic pigment.
Specifically, the grain size of the essence microcapsule 100 is 6-80 meshes, and the essence microcapsule 100 with the grain size can effectively solve the problem that powder essence generates dust in the production process and solve the problems that the powder essence is not good in compatibility with granular products, the essence is not uniformly distributed and the essence is separated from the products and layered. Further, the grain diameter of the essence microcapsule 100 is 20-80 meshes. The ratio of the sum of the mass of the capsule core 110 and the mass of the slow release layer 120 to the mass of the quick release layer 130 is (70-99): (1-30), and the ratio not only can ensure that the essence microcapsule 100 has proper fragrance, but also can ensure that the quick release layer 130 is well adhered to the slow release layer 120. Furthermore, the ratio of the sum of the mass of the capsule core 110 and the sustained-release layer 120 to the mass of the quick-release layer 130 is (80-92): 8-20.
The essence microcapsule 100 has at least the following advantages:
(1) because the surface of the capsule core 110 containing the first aroma substance in the essence microcapsule 100 is coated with the slow release layer 120 made of the material, the slow release layer 120 made of the material can effectively reduce the volatilization of the aroma of the first aroma substance, so that the effect of prolonging the aroma release time of the capsule core 110 is achieved, and the aroma of the essence microcapsule 100 can last for a relatively long time, and the problem of low aroma intensity and insufficient explosiveness caused by the fact that the capsule core 110 is embedded by the slow release layer 120 can be solved by coating the slow release layer 130 containing the second aroma substance with the same aroma note as the first aroma substance on the surface of the slow release layer 120, so that the essence microcapsule 100 can meet the requirement of relatively long aroma duration time, and still has relatively high aroma intensity and relatively good aroma explosiveness.
Meanwhile, the capsule core comprises 0.1-20% of first aroma substances, 0.1-30% of adsorbent, 50-98% of filler and 0-1% of first binder in percentage by mass, the adsorbent is a porous material, and the first aroma substances are embedded in the porous structure of the adsorbent and embedded in the whole capsule core 110, so that the aroma release speed can be slowed down more effectively, and the aroma release time of the capsule core 110 is further prolonged.
(2) The common essence microcapsule is usually in a powder type, so dust is easily generated in the production process, when the common essence microcapsule is applied, particularly in a product with a granular final shape, the compatibility of the powder essence and the granular product is poor, the essence is unevenly distributed in the product, even the essence is separated from the product to be layered, and adverse effects are caused on the shape and the quality of the product.
The essence microcapsule 100 can be applied to food, daily chemical products, medicine preparation, health products or tobacco products. Specifically, the food can be chewing gum, candy, solid beverage, biscuit, snack food, etc.; the daily chemical product can be toothpaste, skin care product, cleaning product, etc.
As shown in fig. 2, a method for preparing the essence microcapsule 100 according to an embodiment is a method for preparing the essence microcapsule 100, and the method includes the following steps:
step S210: the caplet 110 is prepared.
Referring to fig. 3, the process of preparing the core 110 is as follows:
step S212: weighing the raw materials according to the mass percentage, wherein the raw materials comprise: 0.1-20% of first aroma substance, 0.1-30% of adsorbent, 50-98% of filler and 0-1% of first binder.
The first aroma substance is at least one selected from essence, perfume and plant extract. Wherein the essence is selected from one of peppermint essence, fruit essence, flower essence, milk essence, coffee essence, chocolate essence, nut essence, baking essence, green essence, grass essence, costustoot essence and wine essence; the perfume is selected from one of daily chemical perfume, edible perfume and tobacco perfume. The plant extract may be, but not limited to, tea extract, aloe extract, honeysuckle extract, pueraria extract, peppermint extract, ginseng extract, angelica extract, licorice extract, peony extract, calendula extract, etc., rose extract, etc.
The adsorbent is a porous material, can be a natural porous material, and can also be a synthetic porous material. The perfume is adsorbed in the adsorbent. Specifically, the adsorbent is selected from at least one of porous starch, silica, activated carbon, and organic porous polymer. Further, the adsorbent consists of porous starch and silicon dioxide in a mass ratio of 1: 0.2-1: 0.5.
The filler is at least one selected from starch, starch derivatives, saccharides, cellulose and cellulose derivatives. Wherein the starch derivative is selected from at least one of maltodextrin, malto-oligosaccharide, beta-cyclodextrin, sodium starch octenylsuccinate and hydroxypropyl starch. The saccharide compound is at least one selected from monosaccharide, oligosaccharide, chitosan, carrageenan, lactose and konjac gum. The cellulose derivative is at least one selected from microcrystalline cellulose, cellulose acetate butyrate, methyl cellulose, carboxymethyl cellulose, ethyl cellulose, hydroxyethyl cellulose and hydroxypropyl cellulose.
Furthermore, the filler comprises microcrystalline cellulose, maltodextrin and lactose in a mass ratio of (0.5-1) to (0.5-1). The filler adopting the combination can not only ensure the subsequent molding of the capsule core, but also can not influence the smooth release of the fragrance in the later period.
The first binder is at least one selected from hydroxypropyl methylcellulose, polyvinylpyrrolidone, sodium carboxymethylcellulose, xanthan gum and sodium alginate. Further, the first binder is selected from one of hydroxypropyl methylcellulose and sodium carboxymethyl cellulose.
Step S214: mixing the raw materials and the first solvent to obtain a mixture.
Specifically, the step of forming the mixture of the raw materials and the first solvent mixture is as follows: mixing a first aroma substance and an adsorbent to adsorb the first aroma substance into the adsorbent, and then adding a filler and a first binder to obtain a mixture; and mixing the mixture with a first solvent to obtain a mixed material. The first aroma substance and the adsorbent are mixed firstly, and then the filler and the first binder are added, so that the first aroma substance can be adsorbed into the porous structure of the adsorbent more fully. Wherein the solvent is water or ethanol water solution. Specifically, the mass percentage content of the ethanol aqueous solution is below 30%.
Step S216: and forming the mixed material to obtain the pellet.
Specifically, the blend is prepared into pellets by an extrusion spheronization apparatus.
Step S218: the pellet is dried to remove the first solvent, resulting in a caplet 110.
Specifically, the pellets are dried at 35 ℃ to 50 ℃ to remove the solvent.
Step S220: the surface of the capsule core 110 is coated with a sustained-release material to form a sustained-release layer 120.
The slow release material is selected from at least one of acacia, hydroxypropyl methylcellulose, chitosan, polyvinyl alcohol, polyethylene glycol, ethyl cellulose, konjac gum, gelatin and pullulan. Further, the material of the sustained-release layer 120 is at least one selected from gum arabic, pullulan, and polyvinyl alcohol.
Specifically, the mass ratio of the sustained-release layer 120 to the capsule core 110 is 1: 100-15: 100. Further, the mass ratio of the sustained-release layer 120 to the capsule core 110 is 1: 100-8: 100.
Specifically, the step of coating the sustained-release material on the surface of the capsule core 110 is as follows: dissolving the slow-release material in a second solvent to obtain slurry; the slurry is coated on the surface of the caplet 110. Wherein the second solvent is water or an aqueous solution of ethanol. Specifically, the mass percentage content of the ethanol aqueous solution is below 30%. More specifically, the mass percentage concentration of the slow-release material in the slurry is 1-20%; the step of coating the surface of the caplet 110 with the slurry is achieved by using a coating machine.
Step S230: forming a quick release layer 130 on the outer surface of the sustained release layer 120, so that the quick release layer 130 is coated on the outer surface of the sustained release layer 120, thereby obtaining the essence microcapsule 100.
Referring to fig. 4, the step of forming the quick release layer 130 on the outer surface of the sustained release layer 120 includes:
step S232: weighing the following components in percentage by mass: 0.1-40% of second aroma substance, 60-99.8% of second binder, 0-5% of disintegrating agent, 0-8% of emulsifier and 0-0.5% of pigment.
The second aroma substance is at least one selected from essence, perfume and plant extract. Wherein, in the second aroma substance, the essence is selected from one of peppermint essence, fruit essence, flower essence, milk essence, coffee essence, chocolate essence, nut essence, baking essence, green essence, grass essence, costustoot essence and wine essence; the perfume is selected from one of daily chemical perfume, edible perfume and tobacco perfume. The plant extract may be, but not limited to, tea extract, aloe extract, honeysuckle extract, pueraria extract, peppermint extract, ginseng extract, angelica extract, licorice extract, peony extract, calendula extract, etc., rose extract, etc.
In particular, the second aroma substance is in accordance with the note of the first aroma substance.
The second binder is at least one selected from starch, starch derivatives, acacia, gelatin, shellac, agar, sodium alginate, polyvinyl alcohol and cellulose. These substances have certain emulsifying property, film forming property and adhesion property, and can make the second aroma substance adhere to the surface of the slow release layer 120 well. Specifically, the starch derivative is at least one selected from maltodextrin, maltooligosaccharide, beta-cyclodextrin, sodium starch octenylsuccinate and hydroxypropyl starch.
Further, the second binder is composed of sodium starch octenyl succinate, Arabic gum and maltodextrin in a mass ratio of 1:1 (5-10).
The disintegrant is at least one selected from hydroxypropyl methylcellulose, croscarmellose sodium, sodium carboxymethyl starch, and crospovidone. The disintegrant accelerates disintegration and diffusion of the immediate release layer 130.
The emulsifier is at least one selected from glyceryl monostearate, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyglycerol fatty acid ester, sucrose fatty acid ester, polyoxyethylene hydrogenated castor oil, xylitol anhydride monostearate, phospholipid and modified soybean phospholipid. Further, the emulsifier is polyoxyethylene sorbitan fatty acid ester.
The pigment may be natural pigment or synthetic pigment.
Step S234: the components are mixed with water to form an emulsion.
Specifically, the step of mixing each component with water is: dissolving the second binder and the disintegrant in water, and adding the emulsifier, the second aroma substance and the pigment to obtain the emulsion.
Step S236: the emulsion is coated on the outer surface of the sustained-release layer 120 to form the immediate-release layer 130.
Specifically, the method of applying the emulsion on the outer surface of the sustained-release layer 120 is spraying.
Specifically, step S236 is performed at 30 ℃ to 90 ℃.
Further, a step of sieving the pellets is further included before the step of forming the immediate release layer 130 on the outer surface of the sustained-release layer 120.
Further, the grain diameter of the essence microcapsule 100 is 6 meshes to 80 meshes; further, the grain diameter of the essence microcapsule 100 is 20-80 meshes. The ratio of the sum of the mass of the capsule core 110 and the sustained-release layer 120 to the mass of the quick-release layer 130 is (70-99): 1-30; furthermore, the ratio of the sum of the mass of the capsule core 110 and the sustained-release layer 120 to the mass of the quick-release layer 130 is (80-92): 8-20.
The preparation method of the essence microcapsule 100 is simple to operate and easy for industrial production.
The following is part of the examples (the following examples take the example of a mixture of mint-type flavour and cooling agent as the first aroma substance, mint-type flavour as the second aroma substance, wherein the cooling agent is a flavourant, and the following examples contain no other explicitly indicated components except unavoidable impurities unless otherwise specified):
examples 1 to 10
The preparation process of the essence microcapsules of examples 1 to 10 is as follows:
(1) preparing a capsule core: weighing the raw materials of the capsule core according to the mass percentage in the table 1; mixing a first aroma substance and an adsorbent to adsorb the first aroma substance into the adsorbent, then adding a filler and a first binder, and uniformly mixing to obtain a mixture; uniformly stirring and mixing the mixture and water to obtain a mixture; preparing the mixture into a pill by adopting an extrusion rounding device, and drying the pill at 50 ℃ to remove water in the pill to obtain the capsule core.
(2) Dissolving the slow-release material in water to obtain slurry with the mass percentage concentration of 10%; coating the pulp on the surface of the capsule core by using a coating machine to form a slow release layer on the surface of the capsule core. Wherein, the weight of the slow release layer is the weight of the slow release material, the mass ratio of the slow release layer to the capsule core is shown in table 2, the slow release material is shown in table 2, and the obtained capsule core coated with the slow release layer is screened for standby application as required.
(3) Preparation of the quick release layer: weighing the components according to the mass percentage content in the table 3; dissolving a second binder and a disintegrating agent in water, adding an emulsifier, a second aroma substance and a pigment, and stirring and homogenizing to obtain an emulsion; and (3) spraying the emulsion on the outer surface of the slow release layer by adopting coating equipment at the temperature of 60 ℃ according to the required amount of the quick release layer in the table 3 to form the quick release layer, and sieving to obtain the essence microcapsule with the particle size of 20-80 meshes. Wherein the mass of the quick-release layer is substantially the sum of the masses of the components.
TABLE 1
Figure BDA0001557846500000121
Figure BDA0001557846500000131
TABLE 2
Figure BDA0001557846500000132
Figure BDA0001557846500000141
TABLE 3
Figure BDA0001557846500000142
Figure BDA0001557846500000151
Figure BDA0001557846500000161
Comparative example 1
The perfume microcapsule of comparative example 1 was prepared in substantially the same process as in example 1 except that comparative example 1 did not prepare a quick release layer, i.e., no quick release layer was provided on the sustained release layer of the perfume microcapsule of comparative example 1.
Comparative example 2
Comparative example 2 is a mint flavor.
Evaluation:
the essence microcapsules of the examples 1-10 and the essence with the mint flavor of the comparative example 1 and the essence with the mint flavor of the comparative example 2 are respectively prepared into chewing gum according to the conventional preparation process of the chewing gum, and in each chewing gum, the total content of the active ingredients of the mint flavor is the same, and the mass percentage content is 0.5%.
The test method comprises the following steps: the aroma intensity and persistence of each chewing gum was scored by 10 flavor and fragrance professionals as evaluators, and the results are shown in table 4. Wherein, the evaluation of the aroma intensity mainly evaluates the aroma intensity of the chewing gum when the chewing gum is just eaten; the aroma persistence was evaluated as the difference in intensity of the aroma ten minutes after chewing the gum. Evaluating the intensity of the aroma by 0-10 points: the fragrance is strong or very remarkable by 9-10; the fragrance is moderate for 6-8; the fragrance is light, but 3-5 can be obviously identified; the fragrance is almost no or very weak 0-2. Wherein, the scoring data in table 4 is the average value of the evaluation scores of 10 flavor and fragrance professional practitioners on the aroma intensity and the persistence of each chewing gum, and the detailed description is given.
TABLE 4
Figure BDA0001557846500000162
Figure BDA0001557846500000171
Figure BDA0001557846500000181
As can be seen from table 4, the chewing gum containing the mint-flavor essence of comparative example 2 was strong in flavor and good in cool burst, but was also very irritating and poor in taste. While the chewing gum using the essence microcapsule of comparative example 1, which has only a sustained release layer and no quick release layer, has slightly weak fragrance intensity and cool feeling when being put into the mouth, the essence microcapsules of examples 1 to 10 reconcile the contradiction, have strong fragrance intensity and comfortable cool feeling, reduce irritation, and in the aspect of fragrance persistence, the chewing gum directly added with the mint-flavor essence of comparative example 2 has very weak fragrance after being chewed for ten minutes, while the chewing gum of the essence microcapsule of comparative example 1 and examples 1 to 10 can still feel obvious characteristic fragrance and cool feeling.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (14)

1. The essence microcapsule is characterized by comprising a capsule core, a slow release layer and a quick release layer, wherein the slow release layer and the quick release layer are sequentially coated on the capsule core, the capsule core is made of a first aroma substance, the slow release layer is made of at least one of acacia, hydroxypropyl methyl cellulose, chitosan, polyvinyl alcohol, polyethylene glycol, ethyl cellulose, konjac glucomannan, gelatin and pullulan, the quick release layer is made of a second aroma substance, and the aroma of the second aroma substance is consistent with that of the first aroma substance;
the capsule core comprises the following materials in percentage by mass: 0.1-20% of the first aroma substance, 0.1-30% of an adsorbent, 50-98% of a filler and 0-1% of a first binder;
the quick release layer comprises the following materials in percentage by mass: 0.1-40% of the second aroma substance, 60-99.8% of the second binder, 0-5% of a disintegrating agent, 0-8% of an emulsifying agent and 0-0.5% of a pigment; the second binder is at least one selected from starch, starch derivatives, Arabic gum, gelatin, shellac, agar, oligosaccharide, sodium alginate, polyvinyl alcohol and cellulose;
the mass ratio of the slow release layer to the capsule core is 1: 100-15: 100; the mass ratio of the sum of the capsule core and the mass of the slow release layer to the mass of the quick release layer is (70-99): 1-30.
2. The perfume microcapsule according to claim 1, wherein the adsorbent is a porous material.
3. The flavor microcapsule according to claim 1, wherein the filler is at least one selected from the group consisting of starch, starch derivatives, saccharides, cellulose, and cellulose derivatives.
4. The flavor microcapsule according to claim 1, wherein the first aroma substance is selected from at least one of flavors, fragrances, and plant extracts; the second aroma substance is at least one of essence, spice and plant extract.
5. The flavor microcapsule of claim 1, wherein the first binder is selected from at least one of hydroxypropyl methylcellulose, polyvinylpyrrolidone, sodium carboxymethylcellulose, xanthan gum, and sodium alginate.
6. The essence microcapsule according to claim 1, wherein the second binder comprises sodium starch octenyl succinate, gum arabic and maltodextrin in a mass ratio of 1:1 (5-10).
7. The essence microcapsule according to claim 1, wherein the mass ratio of the slow release layer to the capsule core is 1: 100-8: 100.
8. The essence microcapsule according to claim 1, wherein the mass ratio of the sum of the capsule core and the sustained release layer to the quick release layer is (80-92) to (8-20).
9. The flavor microcapsule according to claim 1, wherein the emulsifier is at least one selected from the group consisting of glycerol monostearate, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyglycerol fatty acid ester, sucrose fatty acid ester, polyoxyethylene hydrogenated castor oil, xylitol anhydride monostearate, soybean phospholipid and modified soybean phospholipid; and/or the disintegrating agent is selected from at least one of hydroxypropyl methyl cellulose, croscarmellose sodium, sodium carboxymethyl starch and crospovidone.
10. The preparation method of the essence microcapsule is characterized by comprising the following steps:
coating a slow release material on the surface of the capsule core to form a slow release layer, wherein the material of the capsule core comprises a first aroma substance, and the slow release material is selected from at least one of Arabic gum, hydroxypropyl methyl cellulose, chitosan, polyvinyl alcohol, polyethylene glycol, ethyl cellulose, konjac glucomannan, gelatin and pullulan; and
forming a quick release layer on the outer surface of the slow release layer so that the quick release layer is coated on the outer surface of the slow release layer to obtain the essence microcapsules, wherein the material of the quick release layer comprises a second aroma substance, and the second aroma substance has the same aroma with the first aroma substance;
the capsule core comprises the following materials in percentage by mass: 0.1-20% of the first aroma substance, 0.1-30% of an adsorbent, 50-98% of a filler and 0-1% of a first binder;
the quick release layer comprises the following materials in percentage by mass: 0.1-40% of the second aroma substance, 60-99.8% of the second binder, 0-5% of a disintegrating agent, 0-8% of an emulsifying agent and 0-0.5% of a pigment; the second binder is at least one selected from starch, starch derivatives, Arabic gum, gelatin, shellac, agar, oligosaccharide, sodium alginate, polyvinyl alcohol and cellulose;
the mass ratio of the slow release layer to the capsule core is 1: 100-15: 100; the mass ratio of the sum of the capsule core and the mass of the slow release layer to the mass of the quick release layer is (70-99): 1-30.
11. The method for preparing essence microcapsule according to claim 10, wherein the step of coating the surface of the core with the sustained-release material is preceded by the step of preparing the core:
weighing raw materials according to the components of the capsule core;
mixing the raw materials with a first solvent to obtain a mixture;
forming the mixture to obtain a pellet;
drying the pellets to remove the first solvent, resulting in the caplets.
12. The preparation method of the essence microcapsule according to claim 10, wherein the step of coating the slow release material on the surface of the capsule core comprises: dissolving the slow-release material in a second solvent to obtain slurry; coating the slurry on the surface of the capsule core.
13. The method for preparing the essence microcapsule according to claim 10, wherein the step of forming the quick release layer on the outer surface of the slow release layer comprises:
weighing the components according to the components of the quick release layer;
mixing the components with water to form an emulsion;
coating the emulsion on the outer surface of the slow release layer to form the quick release layer.
14. Use of the flavour microcapsule of any one of claims 1 to 9 in the preparation of food, daily chemical products, pharmaceuticals, health products or tobacco products.
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Address after: No. 8, Xixi Road, Liaobu Town, Dongguan City, Guangdong Province, 523000

Patentee after: Botton Spices Co.,Ltd.

Address before: 523411 First Floor, Wealth Building, Liaobu Town, Dongguan City, Guangdong Province

Patentee before: DONGGUAN BOTON FLAVORS & FRAGRANCES Co.,Ltd.

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