CN113081999A - Microcapsule wall material for embedding plant extract and preparation thereof - Google Patents

Microcapsule wall material for embedding plant extract and preparation thereof Download PDF

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Publication number
CN113081999A
CN113081999A CN202110458028.XA CN202110458028A CN113081999A CN 113081999 A CN113081999 A CN 113081999A CN 202110458028 A CN202110458028 A CN 202110458028A CN 113081999 A CN113081999 A CN 113081999A
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wall material
molecular weight
peg
microcapsule
polyacrylic resin
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CN113081999B (en
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张开良
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Anhui Qingbutang Biotechnology Co ltd
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/5005—Wall or coating material
    • A61K9/5021—Organic macromolecular compounds
    • A61K9/5052—Proteins, e.g. albumin
    • A61K9/5057—Gelatin
    • 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
    • A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/52—Adding ingredients
    • 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
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/03—Organic compounds
    • A23L29/045—Organic compounds containing nitrogen 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
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
    • 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
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/232—Angelica
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/236—Ligusticum (licorice-root)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/25—Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
    • A61K36/258—Panax (ginseng)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/50—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates
    • A61K47/69—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit
    • A61K47/6949—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit inclusion complexes, e.g. clathrates, cavitates or fullerenes
    • A61K47/6951—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit inclusion complexes, e.g. clathrates, cavitates or fullerenes using cyclodextrin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/5005—Wall or coating material
    • A61K9/5021—Organic macromolecular compounds
    • A61K9/5026—Organic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyvinyl pyrrolidone, poly(meth)acrylates
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/5005—Wall or coating material
    • A61K9/5021—Organic macromolecular compounds
    • A61K9/5031—Organic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyethylene glycol, poly(lactide-co-glycolide)
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/5005—Wall or coating material
    • A61K9/5021—Organic macromolecular compounds
    • A61K9/5036—Polysaccharides, e.g. gums, alginate; Cyclodextrin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/5089—Processes
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    • 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
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Abstract

The invention provides a high-temperature-resistant and water-soluble-resistant microcapsule wall material capable of shielding pungent odor and poor taste of plant extract components. Wherein the inner wall material is gelatin/low molecular weight PEG-based wall material, and is prepared from gelatin, deionized water, glycerol, low molecular weight PEG, diluent and polymethyl methacrylate/polyvinylpyrrolidone polymer compound. The outer wall material is prepared from chitosan dispersion solution, polylysine, a high molecular weight composite PEG mixture containing propylene glycol and polyacrylic resin. The microcapsule wall material provided by the invention can effectively shield the bad smell and taste of the plant extract component, and has the properties of high temperature resistance and water solubility resistance.

Description

Microcapsule wall material for embedding plant extract and preparation thereof
Technical Field
The invention relates to a semi-colloid microcapsule wall material for embedding a plant extract and a preparation method thereof, in particular to a high-temperature-resistant semi-colloid microcapsule wall material capable of reducing pungent odor or taste of the plant extract and a preparation method thereof, belonging to the technical field of capsule preparation.
Background
With the development of natural medicinal chemistry and health care product research and development, more and more plant extract products enter the life of people; not only as a medicine, but also various health products and health products are increasingly focused on the use of extracts, rather than directly using natural plant roots and stems for brewing and soaking. Compared with direct soaking, the extract (powder/paste) extracted by using water or ethanol and other organic solvents usually contains higher content of beneficial components, so that the utilization rate is improved, and the waste of materials is avoided.
However, most plant extracts have an unpleasant pungent taste, either taste or smell. For example, ginseng, due to the peculiar taste of its saponins, is often not pleasantly acceptable for infusion or for use as an additive in skin care or hair washing products.
In order to mask the pungent odor of plant extracts, a capsule preparation or microcapsule preparation is currently generally used. The microcapsule preparation has the advantages of taste masking and active ingredient isolation effects close to those of conventional capsule preparations, small particle size (millimeter or even micron), wide application in the fields of medicines and foods, direct eating, and capability of being used as a food processing additive, and is more easily accepted by people.
However, most of the current edible extract products still adopt the conventional capsule form, for example, CN104784386A discloses a ginkgo slimming capsule, which is composed of a capsule shell and contents such as ginkgo leaf, lotus leaf extract, tuckahoe extract, rhizoma alismatis extract and the like sealed in the capsule shell.
CN101181254A discloses a capsule containing natural capsaicin, which comprises natural capsaicin; volatile oil or extract of fructus Zanthoxyli, Cuminum celery, rhizoma Zingiberis recens, fructus Foeniculi or flos Caryophylli; pericarpium Citri Tangerinae or fructus crataegi extract; inulin, cellopolysaccharide or glucomannan; folium Ginkgo or radix Acanthopanacis Senticosi extract; the preparation method comprises dissolving natural capsaicin in emulsifier, mixing with edible oil and adjuvants, and making into capsule or soft capsule.
However, most of the products involving plant extracts are generally conventional soft/hard capsule formulations for the purpose of masking odors and isolating active ingredients, resulting in limited applications thereof; for example, it is not a convenient food additive component in food processing. In a few microcapsule preparations, the odor-masking effect is poor, and the granules are hard granules which easily disintegrate in water to release the active extract component, resulting in poor use effects when taken with water or when food is thermally processed with water.
Therefore, in order to improve or improve the smell and taste of the plant extract product, it is necessary to improve the microcapsule wall material, so that the product embedding the extract component not only has improved taste and smell, but also can avoid rapid disintegration or swelling when mixed with hot water, i.e. can inhibit the disintegration or swelling speed within a certain time, and can be used for hot water drinking or short food thermal processing process.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a high-temperature-resistant water-soluble-resistant microcapsule wall material capable of shielding the unpleasant odor and taste of plant extract components and a preparation method thereof.
Specifically, the present invention mainly relates to the following aspects.
In a first aspect, the invention provides a high-temperature-resistant and water-soluble-resistant microcapsule wall material capable of shielding pungent odor and poor taste of plant extract components, wherein the microcapsule wall material is divided into two layers, including an inner layer wall material and an outer layer wall material.
Wherein the inner wall material is gelatin/low molecular weight PEG-based wall material, and is prepared from gelatin, deionized water, glycerol, low molecular weight PEG, diluent and polymethyl methacrylate/polyvinylpyrrolidone polymer compound. Wherein the mass ratio of the polymethyl methacrylate to the polyvinylpyrrolidone in the polymethyl methacrylate/polyvinylpyrrolidone polymer compound is 1: 0.5-1.
Wherein, the outer wall material is prepared from chitosan dispersion solution, polylysine, a high molecular weight composite PEG mixture containing propylene glycol and polyacrylic resin. Among them, polyacrylic acid resin IV is preferable.
According to the invention, by combining the wall materials with different matrixes, compared with direct mixing use, the obtained wall material and microcapsule have obviously improved high temperature resistance (thermodynamic stability) and water solubility resistance. Wherein said elevated temperature refers to a temperature above 50 ℃, but generally not exceeding 121 ℃, preferably not exceeding 100 ℃, more preferably not exceeding 90 ℃.
The high temperature resistance and water solubility resistance of the invention generally refer to the swelling/dissolving performance under the high temperature water resistance condition.
In a second aspect, the present invention provides a method for preparing high temperature resistant water-soluble microcapsules capable of masking pungent odor and unpleasant taste of plant extract components, the method comprising the steps of:
(1) preparing a core material comprising one or more plant extract components:
mixing powder or paste of one or more plant extracts and an embedding material at least comprising beta-cyclodextrin in deionized water containing an organic solvent, uniformly mixing, drying, and crushing to obtain core material particles; wherein the content of the plant extract in the core material is not more than 50%, preferably not more than 20%, more preferably not more than 10% by weight;
wherein the organic solvent is absolute ethyl alcohol or methanol, and preferably ethyl alcohol.
(2) Preparing inner-layer wall material slurry A:
preparing the gelatin/low molecular weight PEG-based inner wall material raw material according to the following components and contents: 1 part of gelatin, 1-3 parts of deionized water, 0.5-0.8 part of glycerol and 0.1-0.2 part of low molecular weight PEG; swelling gelatin with deionized water, sequentially adding glycerol and low molecular weight PEG, mixing, adding 0.5-1 times of diluent and 0.05-0.1 part of polymethyl methacrylate/polyvinylpyrrolidone polymer compound, and homogenizing; thereby obtaining inner wall material slurry A.
Wherein, preferably, an acetic acid solution (with the mass concentration of 1-2%) containing 1-3wt% of chitosan is used as a diluent;
wherein, the low molecular weight PEG is PEG200-PEG800, such as PEG400 and PEG 600; PEG600 is preferred.
(3) Preparing outer-layer wall material slurry B:
preparing the raw materials of the outer-layer wall material slurry according to the following weight ratio: chitosan dispersion solution: polylysine: high molecular weight complex PEG mixture with propylene glycol = 10-15: 1-2: 0.5-1, and proper amount of polyacrylic resin (preferably 1-3 times of the high molecular weight composite PEG mixture); and uniformly mixing the raw materials in the chitosan dispersion solution to obtain a suspension as outer-layer wall material slurry B.
Wherein the chitosan dispersion solution is a chitosan-acetic acid solution, wherein the mass fraction of the chitosan is 3-5%, and the acetic acid concentration of the acetic acid solution is 1-2 wt%. Chitosan is not readily soluble in water, but is soluble in acidic solutions; the acetic acid is a nontoxic acid solution, is basically volatilized in the subsequent process, and has little residue and no toxic or side effect.
Wherein the high molecular weight composite PEG is a PEG4000 and PEG6000 composite with the mass ratio of 1-3: 1; wherein the mass ratio of PEG4000 to PEG6000 is preferably 2-3: 1.
Wherein, in the high molecular weight composite PEG containing propylene glycol, the mass content of the propylene glycol is 5-10%.
Among them, polylysine preferably has a molecular weight of 1500 or more.
When the polyacrylic resin powder is used, it is dissolved by slightly heating with ethanol (for example, heating to 40 to 50 ℃).
(4) Taking the inner-layer wall material slurry A as a binder, carrying out wet mixing granulation on the core material, drying by an oven or a boiling machine, and then finishing granules to obtain preformed semi-colloidal microcapsule particles;
wherein the particle size after finishing is 0.1-5mm, preferably 0.1-3 mm.
The amount of the core material is determined according to the actual conditions such as odor irritation strength, and may be, for example, 5% to 50% by mass of the inner wall material slurry a.
Compared with the method for preparing the microcapsule with smaller grain diameter in the prior art, the method for preparing the microcapsule with smaller grain diameter has the advantages that the grain diameter of the microcapsule is larger, the method is suitable for wet granulation, the preparation method is simple and convenient, the cost is lower, and the method is suitable for industrial production.
(5) Preparing microcapsule particles: and (3) rapidly dispersing the preformed microcapsule particles in the outer-layer wall material slurry B to form a suspension with a proper concentration, and performing spray drying granulation to obtain the microcapsule particles.
The outer wall material slurry B is preferably used in a concentration suitable for spray drying, for example, so that the mass concentration of the preformed microcapsule particles in the suspension is 30 to 60%.
Among them, it is preferable that the dispersion time is short, for example, not more than 1min, or not more than 0.5min, preferably not more than 15s, in order to prevent the microcapsule particles from being partially dissolved in the outer wall material slurry B.
Preferably, the microcapsule particles in the step (5) are further coated with an ethanol solution spraying method of polyacrylic resin to form an outer protective film, so as to increase the quality stability and shelf life of the microcapsule.
In the preparation method of the microcapsule and the wall material, the raw materials are all commercially available or prepared according to a general method in the field.
In a third aspect, the invention provides a microcapsule wall material prepared by the above preparation method and a microcapsule preparation containing the wall material.
In a fourth aspect, the present invention relates to the use of a wall material comprising the above-described microcapsules for use in a hot environment or process treatment; such as hot water infusion or thermal processing as a food additive.
The invention provides a microcapsule wall material with obviously improved high temperature resistance (high thermodynamic stability) and water solubility resistance through specific wall material component selection and a composite structure, and the microcapsule wall material is particularly suitable for taste masking application and heat-resistant processing treatment, such as masking unpleasant odor and taste of plant extracts.
In addition, the capsule preparation has a specific particle size range, is simple in preparation process, does not need a complex microencapsulation process, and is easy to realize large-scale production.
Detailed Description
The present invention will be described in detail with reference to specific production examples and examples, but these examples are only illustrative of the present invention, and do not limit the actual scope of the present invention.
Example 1
Preparation of microcapsules containing composite wall Material 1
(1) Stirring and mixing light brown Ginseng radix extract powder (containing ginsenoside as main component) and beta-cyclodextrin at a mass ratio of 1:9 in deionized water containing 20% ethanol for 1 hr, fully embedding, evaporating, concentrating, drying, and pulverizing to obtain core material granule.
(2) Preparing the gelatin/low molecular weight PEG-based inner wall material raw material according to the following components and contents: according to parts by weight, 10 parts of gelatin, 20 parts of deionized water, 5 parts of glycerol and 1 part of PEG 6001; fully swelling gelatin with deionized water, sequentially adding glycerol and PEG400, uniformly mixing, adding 20 parts by weight of diluent (acetic acid solution containing 2wt% of chitosan) and 1 part of polymethyl methacrylate/polyvinylpyrrolidone polymer compound (mixed in equal mass ratio), and stirring at high speed under a water bath condition for full homogenization; thereby obtaining inner wall material slurry A.
(3) Preparing outer wall material slurry according to the following weight ratio: 10 parts of chitosan dispersion solution, 1 part of polylysine, 1 part of high molecular weight composite PEG mixture containing 5% propylene glycol, and 2 parts of polyacrylic resin (which is dissolved by adding a proper amount of ethanol and heating slightly when in use); and adding the corresponding raw materials into the chitosan dispersion solution, and uniformly mixing to obtain a suspension as outer-layer wall material slurry B.
Wherein the chitosan dispersion solution contains 4% of chitosan by mass and 1wt% of acetic acid.
Wherein the high molecular weight composite PEG is a PEG4000 and PEG6000 composite with the mass ratio of 2: 1; polylysine has a molecular weight of about 2000 Da.
(4) Taking the prepared inner wall material slurry A as a binder and a proper amount of deionized water as a wetting agent of a core material, carrying out wet mixing granulation on the core material in a granulator, drying in an oven, and then finishing granules to obtain preformed microcapsule granules; wherein the particle size after size stabilization is about 1 mm.
(5) And (3) rapidly dispersing the preformed microcapsule particles in the outer-layer wall material slurry B, rapidly stirring for 15-20s to form a homogeneous suspension with the particle mass concentration of about 40%, and performing spray drying granulation to obtain the microcapsule particles 1 with the composite wall material.
Example 2
Preparation of microcapsules containing composite wall Material 2
(1) Mixing the paste mixed extract of rhizoma Ligustici Chuanxiong and radix Angelicae sinensis with beta-cyclodextrin at a mass ratio of 1:15 in 4.5 times of deionized water containing 40% ethanol by volume, stirring and mixing for 1h, evaporating, concentrating, drying, and pulverizing to obtain core material granule.
(2) Weighing 10 parts of gelatin, 25 parts of deionized water, 6 parts of glycerol and 6001.5 parts of PEG; fully swelling gelatin with deionized water, sequentially adding glycerol and PEG600, uniformly mixing, adding 30 parts by weight of diluent (acetic acid solution containing 1.5wt% of chitosan) and 0.8 part of polymethyl methacrylate/polyvinylpyrrolidone polymer compound (mixed in equal mass ratio), and stirring at high speed under a water bath condition for full homogenization; thereby obtaining inner wall material slurry A.
(3) Taking 15 parts of chitosan dispersion solution, 1 part of polylysine, 1 part of high molecular weight composite PEG mixture containing 6% propylene glycol and 2.5 parts of polyacrylic resin (when in use, a proper amount of ethanol is added for dissolving by slight heating); and adding the raw materials except the chitosan dispersion solution into the chitosan dispersion solution, uniformly mixing to obtain a suspension, and preparing to obtain outer-layer wall material slurry B.
Wherein the chitosan dispersion solution contains 5 percent of chitosan by mass and 1.5 percent of acetic acid by weight.
Wherein the high molecular weight composite PEG is a PEG4000 and PEG6000 composite with the mass ratio of 2.5: 1; polylysine has a molecular weight of about 2000 Da.
(4) Taking the prepared inner wall material slurry A as a binder and a proper amount of deionized water as a wetting agent of a core material, carrying out wet mixing granulation on the core material in a granulator, drying in an oven, and then finishing granules to obtain preformed microcapsule granules; wherein the particle size after finishing is 0.5-1 mm.
(5) And (2) rapidly dispersing the preformed microcapsule particles in the outer-layer wall material slurry B, rapidly stirring for 15-20s to form a homogeneous solution with the particle mass concentration of about 45%, performing spray drying granulation, and further uniformly coating the microcapsule particles with an ethanol solution (12 wt%) of polyacrylic resin by adopting a spray method after drying to form a polyacrylic resin outer-layer protective film, thereby preparing the microcapsule particles 2 with the composite wall material.
Comparative example 1
Step (1) same as example 1; core material particles are prepared.
Weighing the following components in parts by weight: 10 parts of gelatin, 20 parts of deionized water, 5 parts of glycerol and 1 part of PEG 6001; fully swelling gelatin with deionized water, sequentially adding glycerol and PEG400, uniformly mixing, adding 20 parts by weight of diluent (acetic acid solution containing 2wt% of chitosan) and 1 part of polymethyl methacrylate/polyvinylpyrrolidone polymer compound (mixed in equal mass ratio), and stirring at high speed under a water bath condition for full homogenization; thereby obtaining slurry a.
Slurry B was formulated with the same components and proportions as in example 1, namely: weighing 10 parts of chitosan dispersion solution, 1 part of polylysine, 1 part of high molecular weight composite PEG mixture containing 5% of propylene glycol and 2 parts of polyacrylic resin; and adding the corresponding raw materials into the chitosan dispersion solution, and uniformly mixing to obtain a suspension, thereby obtaining slurry B. And mixing the slurry A and the slurry B to obtain mixed coating slurry.
And (4) suspending the core material particles through a fluidized bed by adopting an air suspension method, spraying the mixed coating slurry with proper viscosity on the surfaces of the core material particles through a high-pressure nozzle, and increasing the air flow temperature to volatilize the solvent so as to obtain the comparative microcapsule particles D1.
Comparative example 2
Comparative example 2 was conducted with the same steps and conditions except for the differences in the steps (2) to (3), to obtain comparative microcapsule particles D2. Wherein, the steps (2) to (3) in this comparative example are as follows:
weighing 10 parts of gelatin, 20 parts of deionized water and 5 parts of glycerol according to parts by weight; fully swelling gelatin with deionized water, adding glycerol, uniformly mixing, adding 20 parts by weight of diluent (acetic acid solution containing 2wt% of chitosan), and stirring at high speed under a water bath condition for full homogenization; thereby obtaining inner wall material slurry A.
Step (3) weighing 10 parts of chitosan dispersion solution (the composition is the same as that in example 1) and 1 part of polylysine; and adding the corresponding raw materials into the chitosan dispersion solution, and uniformly mixing to obtain a suspension as outer-layer wall material slurry B.
Effect embodiment: high temperature resistance and water solubility resistance test
The microcapsule granules of examples 1-2 and comparative examples 1-2 were divided into 4 groups of 3 replicates each of example 1, example 2, control 1 and control 2, and the values were averaged.
The test method comprises the following steps: the microcapsule particles are added into a beaker under the condition of water bath at the temperature of 95 +/-2 ℃ according to the proportion of 1g/ml, and the beaker contains 100ml of preheated deionized water. The solution was stirred slowly during the test. And (3) starting timing when the microcapsule particles are added, stopping timing when the capsule particles are all swelled, the particles disappear and a gelatinization-like phenomenon (the particles are swelled into mutually bonded pasty liquid, and basically no particles exist), and calculating the average value of the anti-water-solubility time of each group.
The results are as follows:
TABLE 1 results of microcapsule granule resistance to high temperature and water solubility
Group of Water dissolution resistant time (seconds)
Example 1 98s
Example 2 106s
Comparative example 1 72s
Comparative example 2 47s
As can be seen from the above table, the high temperature resistance and water solubility of the capsule of the comparative example group are significantly reduced, and the high temperature resistance and water solubility resistance of the comparative example 2 using only the chitosan outer layer are significantly reduced.
The invention discovers that even if the form of the composite wall material is adopted, when the components and the content of the wall material are different, the effects of high temperature resistance and water solubility resistance are also greatly different. For a single wall material and a composite wall material, even if the same components are adopted, the composite wall material has more excellent high temperature resistance and water solubility resistance. The high-temperature-resistant and water-soluble-resistant components are reasonably distributed, and even if the outer wall material swells, the inner wall material still has certain swelling resistance, so that the microcapsule has excellent technical effects in the aspects of high temperature resistance and water solubility resistance.
It is well known in the art that the better the resistance to high temperature and water solubility, the more suitable it is for hot water-based applications, and as a food additive for food thermal processing; without the microcapsule swelling that would tend to cause the escape of the plant extract embedded inside, which in turn would lead to the loss of the active ingredient, to the destruction by heating and to the corresponding development of unpleasant taste or odor.
It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should also be understood that various alterations, modifications and/or variations can be made to the present invention by those skilled in the art after reading the technical content of the present invention, and all such equivalents fall within the protective scope defined by the claims of the present application.

Claims (9)

1. The microcapsule wall material is divided into two layers, including an inner layer wall material and an outer layer wall material; the inner wall material is gelatin/low molecular weight PEG-based wall material, and is prepared from gelatin, deionized water, glycerol, low molecular weight PEG, diluent and polymethyl methacrylate/polyvinylpyrrolidone high molecular compound; wherein the mass ratio of the polymethyl methacrylate to the polyvinylpyrrolidone in the polymethyl methacrylate/polyvinylpyrrolidone polymer compound is 1: 0.5 to 1;
the outer wall material is prepared from chitosan dispersion solution, polylysine, a high molecular weight composite PEG mixture containing propylene glycol and polyacrylic resin; wherein, the polyacrylic resin is preferably polyacrylic resin IV;
further, the surface of the outer wall material is also coated with a polyacrylic resin film.
2. A method for preparing high temperature resistant, water soluble resistant microcapsules that mask the pungent odor and unpleasant taste of plant extract components, comprising the steps of:
(1) preparing a core material comprising one or more plant extract components:
mixing powder or paste of one or more plant extracts and an embedding material at least comprising beta-cyclodextrin in deionized water containing an organic solvent, uniformly mixing, drying, and crushing to obtain core material particles; wherein the content of the plant extract in the core material is not more than 50% by weight;
preparing inner-layer wall material slurry A:
preparing the gelatin/low molecular weight PEG-based inner wall material raw material according to the following components and contents: 1 part of gelatin, 1-3 parts of deionized water, 0.5-0.8 part of glycerol and 0.1-0.2 part of low molecular weight PEG; swelling gelatin with deionized water, sequentially adding glycerol and low molecular weight PEG, mixing, adding 0.5-1 times of diluent and 0.05-0.1 part of polymethyl methacrylate/polyvinylpyrrolidone polymer compound, and homogenizing; thereby obtaining inner layer wall material slurry A;
preparing outer-layer wall material slurry B:
preparing an outer layer wall material slurry raw material and a chitosan dispersion solution according to the following weight ratio: polylysine: high molecular weight complex PEG mixture with propylene glycol = 10-15: 1-2: 0.5-1, and proper amount of polyacrylic resin; uniformly mixing the raw materials in a chitosan dispersion solution to obtain a suspension as outer-layer wall material slurry B;
wherein the chitosan dispersion solution is a chitosan-acetic acid solution, wherein the mass fraction of chitosan is 3-5%; the high molecular weight composite PEG is a PEG4000 and PEG6000 composite with the mass ratio of 1-3: 1;
taking the inner-layer wall material slurry A as a binder, carrying out wet mixing granulation on the core material, drying by an oven or a boiling machine, and then carrying out granulation to obtain preformed microcapsule particles;
and (3) rapidly dispersing the preformed microcapsule particles in the outer-layer wall material slurry B to form a suspension with a proper concentration, and performing spray drying granulation to obtain the microcapsule particles.
3. The method of claim 2, wherein: the method further comprises further spraying the microcapsule particles of step (5) with an ethanol solution of polyacrylic resin to form a protective film.
4. The method of claim 2, wherein: wherein in the step (1), the organic solvent is absolute ethyl alcohol or methanol, preferably ethyl alcohol.
5. The method of claim 2, wherein: in the step (2), an acetic acid solution containing 1-3wt% of chitosan is used as a diluent; wherein, the low molecular weight PEG is PEG200-800, preferably PEG 600.
6. The method of claim 2, wherein: in the step (3), the mass ratio of PEG4000 to PEG6000 is 2-3: 1;
wherein, in the high molecular weight composite PEG containing propylene glycol, the mass content of the propylene glycol is 5-10%;
wherein, the molecular weight of the polylysine is more than 1500.
7. The method of claim 2, wherein: wherein, when the polyacrylic resin powder is used, ethanol is added and slightly heated to just dissolve the polyacrylic resin powder.
8. Microcapsule formulations obtainable by a process according to any one of claims 1 to 7.
9. Use of the microcapsule formulation of claim 8 for thermal environment or thermal processing treatment.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040108608A1 (en) * 2002-11-25 2004-06-10 Amorepacific Corporation Method for stabilizing active components using polyol/polymer microcapsule, and cosmetic composition containing the microcapsule
CN1633999A (en) * 2004-11-19 2005-07-06 中国海洋大学 Allicin microcapsule and its preparation method
WO2014084423A1 (en) * 2012-11-30 2014-06-05 (주)케이피티 Pressure sensitive destructible microcapsule containing scrubbing agents, preparation method therefor, and use therefor
CN107281158A (en) * 2016-04-12 2017-10-24 王玉万 Capsule core material and its micro-capsule containing tylosin are prepared with tylosin anti-stripping agent
CN107362154A (en) * 2006-06-05 2017-11-21 帝斯曼营养品股份公司 With the microcapsules for improving shell
CN107510050A (en) * 2017-09-19 2017-12-26 太仓市林港农场专业合作社 A kind of alliin compound microcapsule and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040108608A1 (en) * 2002-11-25 2004-06-10 Amorepacific Corporation Method for stabilizing active components using polyol/polymer microcapsule, and cosmetic composition containing the microcapsule
CN1633999A (en) * 2004-11-19 2005-07-06 中国海洋大学 Allicin microcapsule and its preparation method
CN107362154A (en) * 2006-06-05 2017-11-21 帝斯曼营养品股份公司 With the microcapsules for improving shell
WO2014084423A1 (en) * 2012-11-30 2014-06-05 (주)케이피티 Pressure sensitive destructible microcapsule containing scrubbing agents, preparation method therefor, and use therefor
CN107281158A (en) * 2016-04-12 2017-10-24 王玉万 Capsule core material and its micro-capsule containing tylosin are prepared with tylosin anti-stripping agent
CN107510050A (en) * 2017-09-19 2017-12-26 太仓市林港农场专业合作社 A kind of alliin compound microcapsule and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张韵等: "复凝聚法和食用油双层微胶囊化香兰素研究", 《食品工业科技》 *

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