CN106852726A - A kind of OPC microcapsules and preparation method thereof - Google Patents

A kind of OPC microcapsules and preparation method thereof Download PDF

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Publication number
CN106852726A
CN106852726A CN201710035742.1A CN201710035742A CN106852726A CN 106852726 A CN106852726 A CN 106852726A CN 201710035742 A CN201710035742 A CN 201710035742A CN 106852726 A CN106852726 A CN 106852726A
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opc
microcapsules
solution
prepared
acid
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张婉萍
赵晓伟
李玲玉
朱海洋
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Shanghai Institute of Technology
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Shanghai Institute of Technology
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/4973—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
    • A61K8/498—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom having 6-membered rings or their condensed derivatives, e.g. coumarin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00—Medicinal preparations containing organic active ingredients
    • A61K31/33—Heterocyclic compounds
    • A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
    • A61K31/35—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom
    • A61K31/352—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom condensed with carbocyclic rings, e.g. methantheline 
    • 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
    • A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
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    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
    • A61K47/10—Alcohols; Phenols; Salts thereof, e.g. glycerol; Polyethylene glycols [PEG]; Poloxamers; PEG/POE alkyl ethers
    • 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
    • A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
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    • A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
    • A61K47/14—Esters of carboxylic acids, e.g. fatty acid monoglycerides, medium-chain triglycerides, parabens or PEG fatty acid esters
    • 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
    • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/11—Encapsulated compositions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36—Carboxylic acids; Salts or anhydrides thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37—Esters of carboxylic acids
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73—Polysaccharides
    • A61K8/736—Chitin; Chitosan; Derivatives thereof
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/86—Polyethers
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    • A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/4816—Wall or shell material
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    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/08—Anti-ageing preparations
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/56—Compounds, absorbed onto or entrapped into a solid carrier, e.g. encapsulated perfumes, inclusion compounds, sustained release forms

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Abstract

A kind of OPC microcapsules, by OPC, 1~30% lipophilic emulsifier that mass percent concentration is 0.1~5%, 1~10% shitosan, 1~10% glacial acetic acid, 1~30% water, 0.005~0.1% glutaraldehyde and the liquid fat of surplus are prepared from.The preparation method of above-mentioned microcapsules is additionally provided, by OPC, shitosan, glacial acetic acid heating for dissolving in water, water phase components is obtained；By lipophilic emulsifier, liquid fat Hybrid Heating and it is uniformly dispersed, oil phase component is obtained；Under stirring, water phase components are slowly added into oil phase component, uniform emulsion is obtained；Solidify during glutaraldehyde is added into emulsion, then sequentially pass through centrifugation, ethanol, petroleum ether, acetone dispersion air-dry to obtain OPC microcapsules.OPC microcapsules of the invention, can be such that OPC separates with external environment, effectively prevent strong destruction of the external environments such as periods of direct sunlight to OPC.

Description

A kind of OPC microcapsules and preparation method thereof
Technical field
The invention belongs to field of fine chemical, be related to a kind of microcapsules, specifically a kind of OPC microcapsules and Its preparation method.
Background technology
OPC belongs to condensed tannin, is that the one kind at the position such as core, skin or seed for being widely present in various plants is more Phenolic compounds.
OPC is widely used in the fields such as food, medicine and cosmetics.
In field of medicaments, because OPC has active anticancer and the cardiovascular function of protection, and by as anti-cancer, preventing and treating The active ingredient of cardiovascular disease medicine.
In field of food, OPC is used as a kind of natural preservative, the shelf life for extending food；It is external extensive For in the health food such as lowering blood pressure and blood fat, antitumor, brain tonic；The dispensing or additive of ordinary food are also used for, to increase The alimentary health-care function of food.
In cosmetic field, because OPC has anti-oxidant, Scavenging ability, also with elastase inhibitor activity It is active with microcirculation is improved, so the skin care item containing OPC, can improve scytitis, prevent melanism, anti-aging.
However, the research to OPC stability shows, under high temperature easily there is thermal degradation, periods of direct sunlight pair in OPC OPC has strong destruction.
Shitosan is the unique alkaline polysaccharide in natural polysaccharide, with unique physicochemical characteristics and biology work( Energy.Shitosan and its catabolite are nontoxic, with biocompatibility, biodegradability, security and good moulding property etc. Premium properties, and have certain anti-inflammation, promote the effect such as wound healing.Because shitosan has above superperformance and work With, applied in the middle of cosmetics, both protect coated material, it is ensured that its structural intergrity and stability, can carry again The utilization rate of coating high, makes it be absorbed to greatest extent.And the microcapsules prepared with shitosan have with obvious control The release of effect thing and the effect of extension working substance curative effect.
In recent years, research of the various active materials in terms of dermatology and cosmeceutical is coated to be vigorously developed, it is poly- containing shell The cosmetics of sugar have the unrivaled advantage of Traditional makeup, and it has good biocompatibility, security, slow release, Cosmetics will be made to high-quality, high-grade development.
The content of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of OPC microcapsules and its preparation side Method, described this OPC microcapsules and preparation method thereof will solve capsulated OPC of the prior art and exist Easily there is thermal degradation under high temperature, the technical problem of strong destruction is vulnerable under periods of direct sunlight.
The invention provides a kind of OPC microcapsules, it is prepared from by the raw material of following mass percent：
Described lipophilic emulsifier is ceteareth -6, ceteareth -25, the poly- second two of cetyl Alcohol/the dimethyl siloxane of polypropylene glycol -10/1, the polyricinoleate of polyglycereol -3, the isostearate of polyglycereol -2, polyglycereol -2 Double isostearates, the isostearate of polyglycereol -2 three, the pentaerythritol tetraisostearate of polyglycereol -2, sorbitan monooleate, dehydration Sorbitan stearate, sorbitan sesquioleate, sorbitan trioleate, polyoxyethylene (2) oleyl alcohol ether, polyoxy One or more mixtures for being constituted in ethene (10) oleyl alcohol ether；
Described liquid fat is caprylic capric glyceryl ester, isopropyl myristate, myristyl myristate, palm Isopropyl propionate, isobutyl palmitate, ethylhexyl palmitate, isoamyl laurate, isostearic acid, isooctadecanol, pentaerythrite Four isostearic acids, isostearic acid glyceryl ester, isopropyl isostearate, the pungent decylate of trimethylolpropane tris, neopentyl glycol two In isostearic acid, cetearyl stearate, n-nonanoic acid cetearyl alcohol ester, PEG-7 cocounut oil acid glyceride, three isooctyl acid glyceride One or more mixtures for being constituted.
Present invention also offers a kind of preparation method of above-mentioned OPC microcapsules, comprise the following steps：
1) OPC, lipophilic emulsifier, shitosan, glacial acetic acid, water, glutaraldehyde, liquid are weighed according to mass percent State grease；
2) acetum is made by glacial acetic acid is soluble in water；
3) add chitosan into step 2) in prepared acetum, 30~60 DEG C are heated to being completely dissolved, quiet Chitosan-acetic acid solution is obtained after putting removing bubble；
4) OPC is added to step 3) in prepared solution, 25~50 DEG C stir after it is first molten Liquid；
5) lipophilic emulsifier is added in liquid fat, second is obtained after being stirred in 25~60 DEG C of waters bath with thermostatic control molten Liquid；
6) in 25~60 DEG C of solution of heated at constant temperature second, second is stirred under the stir speed (S.S.) of 150rpm~1000rpm molten Liquid, while the first solution is slowly dropped into in the second solution, emulsifies 0.5~4 hour；
7) in step 6) it is added dropwise in glutaraldehyde in the prepared system for completing, continue 150rpm~1000rpm's Stirred 0.5~4 hour under stir speed (S.S.)；
8) by step 7) prepared by reactant be fully transferred in centrifuge tube, under the rotating speed of 10000~40000rpm Centrifugation, obtains sediment；
9) by step 8) in gained sediment use absolute ethyl alcohol and petroleum ether, washed product natural after being disperseed with acetone respectively Volatilize, obtain OPC microcapsules.
The present invention is used as microcapsules by using lipophilic emulsifier, shitosan, glacial acetic acid, water, glutaraldehyde, liquid fat Wall material, OPC is wrapped in the middle of wall material as core, first OPC, shitosan, glacial acetic acid heating for dissolving are existed In water, water phase components are obtained；By lipophilic emulsifier, liquid fat Hybrid Heating and it is uniformly dispersed, oil phase component is obtained；Stirring Under, water phase components are slowly added into oil phase component, uniform emulsion is obtained；Solidify during glutaraldehyde is added into emulsion, Centrifugation is sequentially passed through again, and ethanol, petroleum ether, acetone dispersion air-dry to obtain OPC microcapsules.Meanwhile, wall material used, shell The good biocompatibility of glycan, can promote absorption of the OPC on skin to permeate, and then improve the utilization of OPC Efficiency, is conducive to it in the more wide application of ordinary food, health food, medicine, cosmetic field.
A kind of cladding OPC microcapsules of the invention, employ the shitosan with good biocompatibility as wall Material coats OPC, and OPC microcapsules are prepared for by emulsion-crosslinking method using lipophilic emulsifier, liquid fat etc., Preparation process is simple, energy consumption are low, obtained microcapsules good sphericity, and size controlling is in nanometer range.
The present invention is compared with prior art, and its technological progress is significant.Prepared OPC microcapsules are for original The problem that anthocyanidin is easily destroyed by external environments such as periods of direct sunlight, for the cladding of OPC provides suitable carrier, by original Anthocyanidin separates with external environment, protects the structural intergrity and stability of OPC, and then improves OPC Active utilization rate, promotion is developed with functionality is strong, the good penetrability cosmetics containing OPC active matter.
The present invention is mainly used in cosmetic technical field using OPC microcapsules prepared by emulsion-crosslinking method.
Brief description of the drawings
Fig. 1 is the microphotograph before OPC microcapsules centrifugation prepared by embodiment 1.
Specific embodiment
The invention will be further elaborated by the following examples, but is not intended to limit the present invention.
It is former containing 1% obtained by the OPC microcapsules of the gained of embodiments of the invention 1 and the comparative examples of embodiment 1 Anthocyanidin aqueous solution permeability data assay method is as follows：
1. instrument：The high performance liquid chromatographs of Agilent 1260, TP-6 intelligence penetrating absorption instrument.
2. operating procedure：
(1) reception liquid is configured：40% absolute ethyl alcohol of PBS cushioning liquid+60%.
(2) external osmotic deffusion experiment
1. weighed respectively with assay balance 10g or so containing 1% OPC microcapsules and containing the 1% OPC aqueous solution In small beaker, it is transferred to completely in 100mL volumetric flasks, 100mL is settled to deionized water, rocks uniform, will raw sample It is diluted to 0.1% OPC microcapsules and the 0.1% OPC aqueous solution；It is standby.
2. load stirrer in reception tank, and fill reception liquid, by artificial skin be fixed on diffusion cell supply pool and Between reception tank (bright to face supply pool, dark face towards reception tank), skin is set to be immersed in solution below.
3. 3mL is pipetted containing 0.1% OPC microcapsules in supply pool with 1mL liquid-transfering guns, same method pipettes 3mL Containing the 0.1% OPC aqueous solution in supply pool, as supply liquid.
4. set recirculated water temperature be 37 DEG C, rotating speed is 400r/min, respectively 1h, 2h, 4h, 6h, 8h, 10h, 12h, 1mL reception liquids are extracted with 1mL medical aseptics syringe when 24h, 36h, while supplementing the fresh reception liquid of same volume.Sample passes through After 0.22 μm of filtering membrane filtration, the concentration of filtrate procyanidins is surveyed with efficient liquid phase.
Experimental result：
Wherein, Cn：Reception liquid drug concentration, μ g/mL when n-th is sampled；
V：Reception liquid volume in receiving chamber, 17mL；
Ci：Reception liquid drug concentration, μ g/mL when i ＆ lt is sampled；
1.0：Each sample volume, mL；
S：Effective infiltrating area, 1cm2；
Q：Permeability, μ g/cm2。
Embodiment 1：
In terms of 1000g formula materials, OPC 1g, lipophilic emulsifier 10g, shitosan 10g, glacial acetic acid 10g, water are taken 10g, glutaraldehyde 0.05g, liquid fat 958.95g.
Described lipophilic emulsifier is ceteareth -6；
Described liquid fat is caprylic capric glyceryl ester；
The step of preparation method, is as follows：
1) acetum is made by glacial acetic acid is soluble in water；
2) add chitosan into step 1) in prepared acetum, 30 DEG C are heated to being completely dissolved, and standing is removed Chitosan-acetic acid solution is obtained after removing bubble；
3) OPC is added to step 2) in prepared solution, 25 DEG C stir after solution a；
4) lipophilic emulsifier is added in liquid fat, solution b is obtained after being stirred in 25 DEG C of waters bath with thermostatic control；
5) in 25 DEG C of heated at constant temperature solution b, the agitating solution b under the stir speed (S.S.) of 200rpm, while solution a is slowly dripped Enter in solution b, emulsify 1.5 hours；
6) in step 5) glutaraldehyde is added dropwise in the prepared system for completing, continuation is stirred under the stir speed (S.S.) of 200rpm Mix 1.5 hours；
7) by step 6) prepared by reactant be fully transferred in centrifuge tube, under the rotating speed of 10000rpm centrifugation point From obtaining sediment.
8) by step 7) in gained sediment respectively with absolute ethanol washing once, petroleum ether three times.Washed product Volatilized naturally after being disperseed with proper amount of acetone, obtain OPC microcapsules.
The case of comparative examples of embodiment 1：
Configure the 1% OPC aqueous solution.
OPC microcapsules to the gained of above-described embodiment 1 and being spent containing 1% original obtained by the comparative examples of embodiment 1 Blue or green element aqueous solution permeability data is determined, and as a result be see the table below：
Embodiment 2：
In terms of 1000g formula materials, OPC 50g, lipophilic emulsifier 300g, shitosan 100g, glacial acetic acid are taken 100g, water 300g, glutaraldehyde 1g, liquid fat 149g.
Described lipophilic emulsifier is ceteareth -25；
Described liquid fat is isopropyl myristate；
The step of preparation method, is as follows：
1) acetum is made by glacial acetic acid is soluble in water；
2) add chitosan into step 1) in prepared acetum, 60 DEG C are heated to being completely dissolved, and standing is removed Chitosan-acetic acid solution is obtained after removing bubble；
3) OPC is added to step 2) in prepared solution, 50 DEG C stir after solution a；
4) lipophilic emulsifier is added in liquid fat, solution b is obtained after being stirred in 60 DEG C of waters bath with thermostatic control；
5) in 60 DEG C of heated at constant temperature solution b, the agitating solution b under the stir speed (S.S.) of 1000rpm, while solution a is slow It is added dropwise in solution b, emulsifies 4 hours；
6) in step 5) glutaraldehyde of 1g is added dropwise in the prepared system for completing, continue the stirring speed in 1000rpm Stirred 4 hours under rate；
7) by step 6) prepared by reactant be fully transferred in centrifuge tube, under the rotating speed of 40000rpm centrifugation point From obtaining sediment.
8) by step 7) in gained sediment respectively with absolute ethanol washing once, petroleum ether three times.Washed product Volatilized naturally after being disperseed with proper amount of acetone, obtain OPC microcapsules.
Embodiment 3：
In terms of 1000g formula materials, OPC 25g, lipophilic emulsifier 150g, shitosan 50g, glacial acetic acid 50g are taken, Water 150g, glutaraldehyde 0.5g, liquid fat 574.5g.
Described lipophilic emulsifier is the isostearate of polyglycereol -2 three；
Described liquid fat is isopropyl palmitate；
The step of preparation method, is as follows：
1) acetum is made by glacial acetic acid is soluble in water；
2) add chitosan into step 1) in prepared acetum, 45 DEG C are heated to being completely dissolved, and standing is removed Chitosan-acetic acid solution is obtained after removing bubble；
3) OPC is added to step 2) in prepared solution, 40 DEG C stir after solution a；
4) lipophilic emulsifier is added in liquid fat, solution b is obtained after being stirred in 40 DEG C of waters bath with thermostatic control；
5) in 40 DEG C of heated at constant temperature solution b, the agitating solution b under the stir speed (S.S.) of 500rpm, while solution a is slowly dripped Enter in solution b, emulsify 2.5 hours；
6) in step 5) glutaraldehyde is added dropwise in the prepared system for completing, continuation is stirred under the stir speed (S.S.) of 500rpm Mix 2.5 hours；
7) by step 6) prepared by reactant be fully transferred in centrifuge tube, under the rotating speed of 25000rpm centrifugation point From obtaining sediment.
8) by step 7) in gained sediment respectively with absolute ethanol washing once, petroleum ether three times.Washed product Volatilized naturally after being disperseed with proper amount of acetone, obtain OPC microcapsules.
Above said content is only the basic explanation under present inventive concept, and according to appointing that technical scheme is made What equivalent transformation, all should belong to protection scope of the present invention.

Claims (3)

1. a kind of OPC microcapsules, it is characterised in that be prepared from by the raw material of following mass percent：
OPC 0.1~5%,
Lipophilic emulsifier 1~30%,
Shitosan 1~10%,
Glacial acetic acid 1~10%,
Water 1~30%,
Glutaraldehyde 0.005~0.1%,
Liquid fat surplus；
Described lipophilic emulsifier is ceteareth -6, ceteareth -25, cetyl polyethylene glycol/poly- The dimethyl siloxane of propane diols -10/1, the polyricinoleate of polyglycereol -3, the isostearate of polyglycereol -2, polyglycereol -2 pairs are different Stearate, the isostearate of polyglycereol -2 three, the pentaerythritol tetraisostearate of polyglycereol -2, sorbitan monooleate, Sorbitan Alcohol stearate, sorbitan sesquioleate, sorbitan trioleate, polyoxyethylene（2）Oleyl alcohol ether, polyoxyethylene （10）One or more mixtures for being constituted in oleyl alcohol ether；
Described liquid fat is different caprylic capric glyceryl ester, isopropyl myristate, myristyl myristate, palmitic acid Propyl ester, isobutyl palmitate, ethylhexyl palmitate, isoamyl laurate, isostearic acid, isooctadecanol, pentaerythrite four are different Stearic acid, isostearic acid glyceryl ester, isopropyl isostearate, the pungent decylate of trimethylolpropane tris, neopentyl glycol two are different hard One kind in resin acid, cetearyl stearate, n-nonanoic acid cetearyl alcohol ester, PEG-7 cocounut oil acid glyceride, three isooctyl acid glyceride Or two or more constituted mixtures.
2. the preparation method of a kind of OPC microcapsules described in claim 1, it is characterised in that comprise the following steps：
1）OPC, lipophilic emulsifier, shitosan, glacial acetic acid, water, glutaraldehyde, fluid oil are weighed according to mass percent Fat；
2）Acetum is made by glacial acetic acid is soluble in water；
3）Add chitosan into step 2) in prepared acetum, 30~60 DEG C are heated to being completely dissolved, and standing is removed Chitosan-acetic acid solution is obtained after removing bubble；
4）OPC is added to step 3) in prepared solution, 25~50 DEG C stir after the first solution；
5）Lipophilic emulsifier is added in liquid fat, the second solution is obtained after being stirred in 25~60 DEG C of waters bath with thermostatic control；
6）In 25~60 DEG C of solution of heated at constant temperature second, the second solution is stirred under the stir speed (S.S.) of 150rpm~1000rpm, together When the first solution is slowly dropped into in the second solution, emulsify 0.5~4 hour；
7）In step 6) it is added dropwise in glutaraldehyde in the prepared system for completing, continue the stirring in 150rpm~1000rpm Stirred 0.5~4 hour under speed；
8）By step 7) prepared by reactant be fully transferred in centrifuge tube, under the rotating speed of 10000~40000rpm be centrifuged Separate, obtain sediment；
9）By step 8) in gained sediment respectively use absolute ethyl alcohol and petroleum ether, washed product acetone dispersion after wave naturally It is dry, obtain OPC microcapsules.
3. application of the OPC microcapsules described in claim 1 in food, health food, medicine or cosmetics.
CN201710035742.1A 2017-01-17 2017-01-17 A kind of OPC microcapsules and preparation method thereof Pending CN106852726A (en)

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CN108402464A (en) * 2018-04-04 2018-08-17 江南大学 One kind is rich in wild cherry certain kind of berries anthocyanidin microcapsules and preparation method thereof
CN108403574A (en) * 2018-06-08 2018-08-17 桃源县兴隆米业科技开发有限公司 A kind of preparation method based on purple rice extracting solution whitening moisturizing face masque
CN109259234A (en) * 2018-11-19 2019-01-25 福建农林大学 It is a kind of using resistant starch as the procyanidine microcapsules and preparation method of wall material
CN109999767A (en) * 2019-04-17 2019-07-12 江苏师范大学 A kind of method of glutaraldehyde modification of chitosan resin adsorption separation purple sweet potato anthocyanin
CN110664705A (en) * 2019-10-30 2020-01-10 广东省农业科学院蚕业与农产品加工研究所 Preparation method of sweet potato anthocyanin eye shadow
CN111840115A (en) * 2020-08-17 2020-10-30 蓝科恒业医疗科技(长春)有限公司 Procyanidine oligomer-based facial hormone-dependent dermatitis treatment liquid and preparation method thereof
CN114698844A (en) * 2022-04-11 2022-07-05 湖北工业大学 Application of chitosan procyanidin composition in inhibiting formation of gastrointestinal pentostatin
CN114794479A (en) * 2022-05-20 2022-07-29 中国计量大学 Preparation method of procyanidine-chitosan microgel

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108402464A (en) * 2018-04-04 2018-08-17 江南大学 One kind is rich in wild cherry certain kind of berries anthocyanidin microcapsules and preparation method thereof
CN108403574A (en) * 2018-06-08 2018-08-17 桃源县兴隆米业科技开发有限公司 A kind of preparation method based on purple rice extracting solution whitening moisturizing face masque
CN109259234A (en) * 2018-11-19 2019-01-25 福建农林大学 It is a kind of using resistant starch as the procyanidine microcapsules and preparation method of wall material
CN109999767A (en) * 2019-04-17 2019-07-12 江苏师范大学 A kind of method of glutaraldehyde modification of chitosan resin adsorption separation purple sweet potato anthocyanin
CN110664705A (en) * 2019-10-30 2020-01-10 广东省农业科学院蚕业与农产品加工研究所 Preparation method of sweet potato anthocyanin eye shadow
CN111840115A (en) * 2020-08-17 2020-10-30 蓝科恒业医疗科技(长春)有限公司 Procyanidine oligomer-based facial hormone-dependent dermatitis treatment liquid and preparation method thereof
CN114698844A (en) * 2022-04-11 2022-07-05 湖北工业大学 Application of chitosan procyanidin composition in inhibiting formation of gastrointestinal pentostatin
CN114794479A (en) * 2022-05-20 2022-07-29 中国计量大学 Preparation method of procyanidine-chitosan microgel

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