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CN111358703B - Fullerene-containing microcapsule and composition thereof - Google Patents

Fullerene-containing microcapsule and composition thereof Download PDF

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Publication number
CN111358703B
CN111358703B CN202010184155.0A CN202010184155A CN111358703B CN 111358703 B CN111358703 B CN 111358703B CN 202010184155 A CN202010184155 A CN 202010184155A CN 111358703 B CN111358703 B CN 111358703B
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fullerene
parts
microcapsule
essence
composition
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CN111358703A (en
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张婧芳
朱常锋
韩鄂宁
刘雅玲
王颖
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Xiamen Fuci Biotechnology Co ltd
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Xiamen Fuci Biotechnology Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/11Encapsulated compositions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/35Ketones, e.g. benzophenone
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/64Proteins; Peptides; Derivatives or degradation products thereof
    • A61K8/65Collagen; Gelatin; Keratin; Derivatives or degradation products thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/67Vitamins
    • A61K8/673Vitamin B group
    • A61K8/675Vitamin B3 or vitamin B3 active, e.g. nicotinamide, nicotinic acid, nicotinyl aldehyde
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/733Alginic acid; Salts thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/735Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/736Chitin; Chitosan; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8141Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • A61K8/8147Homopolymers or copolymers of acids; Metal or ammonium salts thereof, e.g. crotonic acid, (meth)acrylic acid; Compositions of derivatives of such polymers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/817Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Compositions or derivatives of such polymers, e.g. vinylimidazol, vinylcaprolactame, allylamines (Polyquaternium 6)
    • A61K8/8176Homopolymers of N-vinyl-pyrrolidones. Compositions of derivatives of such polymers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/86Polyethers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/02Preparations for care of the skin for chemically bleaching or whitening the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions

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  • Inorganic Chemistry (AREA)
  • Cosmetics (AREA)

Abstract

The invention relates to a fullerene-containing microcapsule and a composition thereof, wherein the fullerene-containing microcapsule comprises the following components in parts by weight: 36-52 parts of gel materials, 8-16 parts of water-soluble film forming materials, 5-15 parts of functional components, 45-95 parts of deionized water and 0-5 parts of pigments, wherein the functional components consist of fullerene, astaxanthin and nicotinamide. The composition comprises the fullerene containing microcapsule. The fullerene-containing microcapsule has the advantages of good embedding effect, high embedding rate, good embedding capacity for active ingredients, effective protection of the activity of a compound, good antioxidant, anti-aging and whitening effects, safe performance and no generation of the problems of skin tightness, pruritus and redness.

Description

Fullerene-containing microcapsule and composition thereof
Technical Field
The invention relates to the technical field of cosmetics, in particular to a fullerene-containing microcapsule and a composition thereof.
Background
Whether neutral skin, mixed skin or oily skin, whether young skin, mature skin or aged skin, can be subjected to external free radicals in life to interfere keratin oxidation and further aging. Moreover, if the skin is aged, the increase of metabolites can cause pore blockage, increase of grease secretion and overgrowth of pox; in the same period, the fibers on the bottom layer of the skin are aged and collapsed to form furrows, and a large number of wrinkles are generated, so that the facial appearance is more old.
The existing anti-aging and anti-oxidation products mainly use vitamin C, vitamin E and related extracts and derivatives thereof, although the substances can prevent skin cells from being oxidized through the oxidation effect of the substances, the effects are short and difficult to store, and the allergy phenomena of tightness, redness and swelling and the like can be generated when some extracts are used. The cage-like football structure of fullerene makes it stable and not easy to decompose, and it can keep the functions of anti-oxidation and free radical removal in skin cells for a long time, and the anti-oxidation function prolongs the anti-oxidation capability of the skin cells from the aspect of timeliness, and can achieve the purpose of fundamentally long-acting anti-aging. However, the fullerene is a water-insoluble substance, and how to modify, package and protect the fullerene to prepare the anti-aging and anti-oxidation product has a very profound significance.
Disclosure of Invention
The invention aims to overcome the technical problems that the existing fullerene is difficult to be prepared into an anti-aging and anti-oxidation product and the health care effect of the product is exerted, and provides a microcapsule containing fullerene; on the other hand, the compound containing fullerene is embedded in the microcapsule by utilizing the wrapping of the saccule, so that the compound is not interfered by external environment factors, and the stable antioxidant activity of the functional components is kept.
The invention also protects the composition containing the fullerene-containing microcapsule, and the fullerene-containing microcapsule is dispersed in essence for convenient use.
The invention also provides a preparation method of the composition, which adopts a dropping method to prepare the composition, and when the fullerene-containing microcapsule falls into the essence, the appearance state of the microcapsule is unchanged.
The microcapsule containing fullerene comprises functional components, namely fullerene, astaxanthin and nicotinamide, wherein the astaxanthin is an excellent antioxidant, can enhance the immunity of the organism and has a coloring effect; nicotinamide is the vitamin B group, which acts as a precursor for NADH and NADPH by regulating the equilibrium of the two levels in vivo. High levels of NADPH exert a powerful antioxidant effect, preventing spontaneous glycosylation of proteins and sugars. Preferably, the mass ratio of the fullerene, the astaxanthin and the nicotinamide is 1-3:1-3:4-5, more preferably, the mass ratio of the fullerene, the astaxanthin and the nicotinamide is 2:2:5, and the advantages of adopting the mixture ratio are as follows: the most efficient antioxidation and whitening effects are achieved through the antioxidation and whitening action mechanisms of the three components at different cell levels.
The astaxanthin, the nicotinamide and the fullerene are compounded, so that the astaxanthin, the nicotinamide and the fullerene have an unexpected technical effect, and the compound of the astaxanthin, the nicotinamide and the fullerene can stably form uniform fluid and form uniform, mellow and light red microcapsules under the support of sodium alginate under the action of calcium ions, so that the astaxanthin, the nicotinamide and the fullerene are attractive in appearance, the effects of moisturizing, whitening, moisturizing and resisting oxidation can be realized by applying the compound on the surface of human skin, the molecular weight is small, the compound is easy to absorb by the skin, and no side effect is caused.
The fullerene-containing microcapsule further comprises a gel material and a water-soluble film-forming material, wherein the gel material and the water-soluble film-forming material are one of keys for forming the microcapsule and maintaining a specific form, the gel material plays a role in integral forming and supporting from the inside of the microcapsule, and the water-soluble film-forming material is the key for forming an encapsulating layer structure. Preferably, the gel material is 36-52 parts, the water-soluble film-forming material is 8-16 parts, more preferably, the gel material is 40-50 parts, the water-soluble film-forming material is 10-15 parts, for example, the gel material is 42 parts, the water-soluble film-forming material is 14 parts; or 46 parts of gel material and 12 parts of water-soluble film-forming material; or 48 parts of gel material and 11 parts of water-soluble film-forming material.
In the invention, the fullerene comprises fullerene C60 and C70 and fullerene derivatives, wherein the fullerene derivatives comprise C2m, fullerene metal derivatives, fullerene oxygen-containing derivatives and organic compound modified or included fullerene, oxygen atoms in the fullerene oxygen-containing derivatives are connected with carbon atoms on a fullerene skeleton or are bonded with an alkylene chain, organic compounds in the organic compound modified or included fullerene are cyclodextrin and/or crown ether, and m is more than or equal to 30 and less than or equal to 60;
Preferably, the fullerene and the derivative thereof can be expressed by any one of C2M, M @ C2M, M2@ C2M, MA @ C2M, M3N @ C2M, M2C2@ C2M, M2S @ C2M, M2O @ C2M and MXA3-XN @ C2M, wherein M is more than or equal to 30 and less than or equal to 60, M and A are both any one metal element selected from Sc, Y and lanthanide elements, and @ is a connecting group or a metal.
The fullerene and the fullerene derivative may be water-soluble or oily, and the water-soluble film-forming material of the present invention may be one that dissolves the water-soluble fullerene and the fullerene derivative or one that forms a coating structure with the oil-soluble fullerene and the fullerene derivative. For example, when PVP is used as the water-soluble film-forming material, PVP-coated water-soluble fullerenes can be formed.
In the fullerene containing microcapsule of the present invention, deionized water is 45 to 95 parts, preferably 50 to 80 parts, more preferably 60 to 75 parts, for example 62 parts, for example 65 parts, for example 70 parts. Deionized water is used for dispersing and dissolving other materials to form liquid with certain viscosity, the dosage of the deionized water is lower than 45 parts, so that the microcapsules are too hard and cannot be extruded and formed, and the dosage of the deionized water is higher than 95 parts, so that the microcapsules are loose in structure and cannot be extruded and formed.
The microcapsule containing fullerene can also contain pigment, so that the product presents different color systems from transparent orange red to yellow, and the product is endowed with beautiful appearance.
The fullerene-containing microcapsule can be independently used as a product, is light in weight, high in stability and convenient to carry, and can meet the requirements of carrying and supplementing with people; the composition can also be added into products requiring fullerene introduction, such as essence to form a composition, and the cosmetic with antioxidant and anti-aging effects can be formed.
In the composition, the essence preferably comprises the following components: 2-5 parts of gel material, 4-8 parts of moisturizing material, 0.05-0.6 part of acid-base regulator, 0.05-1.5 parts of preservative and 0-0.5 part of essence. More preferably comprises the following components: 3-4 parts of gel material, 5-7 parts of moisture retention material, 0.1-0.5 part of acid-base regulator, 0.5-1.0 part of preservative and 0-0.5 part of essence. The formula of the essence has the advantages of preventing functional components in the microcapsules from exuding before being applied to skin, promoting skin absorption, keeping moisture and keeping the appearance attractive.
The essence containing the fullerene microcapsule is used as cosmetics, and transparent or non-transparent pearl-shaped microspheres are uniformly distributed in the colloidal essence; the microcapsules are transparent orange-red to yellow regular round small balls, the colloidal essence liquid is transparent and semi-liquid, and the microcapsules can be uniformly dispersed on the upper layer, the middle layer and the lower layer of the container and cannot move under the action of common external shearing force by controlling the density, the mechanical property and other factors of the essence liquid and the microcapsules. The composition realizes the repair and stability maintenance of skin keratin cells through the relatively independent physical barrier effect of essence and micro-capsule balls, retains skin moisture to a great extent, relieves damaged keratin cells, releases fullerene through the wall breaking of the microspheres, realizes the antioxidation effect, achieves the anti-aging effect, has safe performance, and does not cause the problems of tightness, pruritus and redness and swelling of the skin.
In the preparation method of the composition, the first raw material is used for preparing the fullerene-containing microcapsule, and comprises a gel material, a water-soluble film-forming material, an effective component, deionized water and a pigment (optional). The second raw material is used for preparing the essence, and comprises gel materials, moisture-keeping materials, pH regulator, antiseptic and essence (optional). In the step 3, the material A flows out at a constant speed by using a constant-temperature dripper, the constant temperature is favorable for uniformly emulsifying the mixed liquid and assisting in promoting the stable forming of the microcapsule at the later stage; the constant flow rate is used for controlling the liquid to uniformly flow out, so that the microcapsules are uniform in size, attractive in appearance and complete in coating. The invention cuts off the liquid column by a cutter to form a series of liquid drops, preferably the diameter of the liquid drops is 3-8mm, more preferably the diameter of the liquid drops is 4-7mm, such as 5mm or 6mm, and the liquid drops are uniform spherical, have rich coating functional components and uniform color and luster, do not deform under slight shearing force and have better performance. When the microspheres (i.e., the fullerene-containing microcapsules) fall into the essence, the appearance of the microspheres is unchanged, mainly because the film-forming material of the microspheres coats the inner components thereof and is not fused with the external liquid. The appearance of the microsphere is not changed, so that the appearance is ensured, and meanwhile, the coating functional components are not influenced by the outside.
Compared with the traditional method for encapsulating fullerene by using hard or soft capsules, the preparation process provided by the invention realizes one-time stable encapsulation by adopting an integral forming technology, and ensures the stability of the amount of fullerene, astaxanthin and nicotinamide contained in each microcapsule through the stable mixing time, temperature, fluid speed and control on the diameter of liquid drops. The capsule shell and the content are integrated and the micro-capsule is soaked in the isotonic solution (essence) for a long time without rupture and content overflow, and the micro-capsule is ruptured by extrusion of a pump head and can be fused with the essence to form uniform emulsion.
The specific scheme is as follows:
a fullerene containing microcapsule comprising the following components in parts by weight: 36-52 parts of gel materials, 8-16 parts of water-soluble film-forming materials, 5-15 parts of functional components, 20-50 parts of deionized water and 0-5 parts of pigments, wherein the functional components comprise fullerene, astaxanthin and nicotinamide, and the fullerene comprises at least one of C60, C70 or fullerene derivatives.
Further, the gel material is at least one of polymethyl cellulose, gellan gum, gelatin, agar, sodium hyaluronate or carbomer;
Optionally, the fullerene derivative comprises at least one of a fullerene metal derivative, a fullerene oxygen-containing derivative, and fullerene modified or included by an organic compound; preferably, the oxygen atom in the fullerene oxygen-containing derivative is connected with a carbon atom on a fullerene skeleton or bonded with an alkylene chain, and the organic compound in the fullerene modified or included by the organic compound is cyclodextrin and/or crown ether;
preferably, the chemical formula of the fullerene derivative is C2M, M @ C2M, M2@ C2M, MA @ C2M, M3N @ C2M, M2C2@ C2M, M2S @ C2M, M2O @ C2M or MXA3-XN @ C2M, wherein 30 ≦ M ≦ 60, M and A are both selected from any one of Sc, Y and lanthanide elements, and @isa connecting group or a representation method of a metal;
optionally, the water-soluble film forming material is at least one of PEG400, sodium polyacrylate, sodium alginate, hydroxyethyl cellulose, PVP, or chitosan.
Further, the mass ratio of the fullerene, the astaxanthin and the nicotinamide in the effective components is 1-3:1-3: 4-5;
optionally, the fullerene containing microcapsule comprises the following components in parts by weight: 40-50 parts of gel materials, 10-15 parts of water-soluble film forming materials, 8-12 parts of functional components, 25-45 parts of deionized water and 0-5 parts of pigments.
Further, the microcapsule containing fullerene has a pearl appearance in the form of a droplet having a diameter of 3-8 mm.
The invention also protects a composition comprising the fullerene containing microcapsule.
Further, the composition also comprises essence, wherein the fullerene-containing microcapsule is dispersed in the essence.
Further, the essence comprises the following components in parts by weight: 2-5 parts of gel material, 4-8 parts of moisture retention material, 0.05-0.6 part of acid-base regulator, 0.05-1.5 parts of preservative and 0-0.5 part of essence;
preferably, the essence comprises the following components in parts by weight: 3-4 parts of gel material, 5-7 parts of moisture retention material, 0.1-0.5 part of acid-base regulator, 0.5-1.0 part of preservative and 0-0.5 part of essence.
Further, the gel material is at least one of polymethyl cellulose, gellan gum, gelatin, agar, sodium hyaluronate or carbomer;
optionally, the moisture retaining material is at least one of betaine, trehalose, PCA-Na, hyaluronic acid, butylene glycol, squalane, or glycerol;
optionally, the pH regulator is at least one of citric acid, triethylamine or sodium hydroxide.
The invention also provides a preparation method of the composition, which comprises the following steps:
Step 1: weighing the first raw material for preparing the fullerene-containing microcapsule according to the weight parts, mixing the first raw material, heating, stirring uniformly and homogenizing to obtain a material A;
and 2, step: : weighing the second raw materials for preparing the essence according to the parts by weight, and uniformly mixing the second raw materials to obtain a material B;
and 3, step 3: and (3) using a constant-temperature dripper to flow out the material A at a constant speed, and then cutting off a liquid column by using a cutter to form a series of liquid drops, so that the liquid drops fall into the material B, and the shape of the liquid drops is not changed to prepare the composition.
Further, the mass ratio of the material A to the material B is as follows: 5-45: 95-55;
optionally, the heating temperature in the step 1 is 60-85 ℃, and the homogenization time is 3-8 min;
optionally, the constant temperature in step 3 is 60-85 deg.C, the constant rate is 2-5 drops/s, and the diameter of the drop is 3-8 mm.
Has the advantages that:
the fullerene-containing microcapsule provided by the invention can keep a stable form by formula design, the appearance of the microcapsule is similar to that of a pearl or a roe, the microcapsule is transparent, orange red and spherical, the microcapsule is glittering and translucent like a champagne pearl in vision, and the content of the microcapsule is rich in nutrition like a roe.
Moreover, the fullerene-containing microcapsule provided by the invention realizes the addition of high-content fullerene, the highest addition amount of the fullerene and derivatives thereof can reach 0.1-15% of the total weight of the fullerene-containing microcapsule, and due to the slow release effect of the microcapsule, effective components permeate from the skin surface layer to the skin bottom layer to achieve the anti-oxidation effect from inside to outside, so that the performance is safe, and the skin cannot be tensed and red and swollen; in addition, the compound containing the fullerene is embedded in the microcapsule, so that the compound is not interfered by external environmental factors, and the stable antioxidant activity is kept.
Furthermore, the microcapsule containing fullerene provided by the invention is light in weight, high in stability, convenient to carry, capable of meeting the requirements of carrying and supplementing, and has a wider application level.
Finally, the preparation method of the fullerene-containing microcapsule and the fullerene-containing composition provided by the invention has the advantages that the price of the preparation raw materials is low, the preparation method is suitable for industrial mass production, and the immeasurable market prospect is realized; the preparation raw materials can be completely replaced by edible raw materials, is suitable for the food processing industry, and can be converted into a health food preparation technology; the preparation method is simple and quick, and can prepare the hydrogel microspheres with uniform size and quality by controlling the speed of the liquid flow and the cutting rate, thereby facilitating the quality control.
Drawings
In order to more clearly illustrate the technical solution of the present invention, the drawings will be briefly introduced, and it is apparent that the drawings in the following description relate only to some embodiments of the present invention and are not limiting to the present invention.
FIG. 1 is a graph showing the results of the antioxidant activity assay according to an embodiment of the present invention.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein. Those skilled in the art will recognize that the specific techniques or conditions, not specified in the examples, are according to the techniques or conditions described in the literature of the art or according to the product specification. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available. In the following examples, "%" means weight percent, unless otherwise specified.
The following examples to prepare
Example 1:
preparing a microcapsule containing fullerene, weighing a first raw material (distributed according to 100 parts by weight of the total amount), wherein the dosage of each raw material is shown in table 1, a gel material adopts 36 parts of gellan gum, a water-soluble film-forming material adopts agar, and the functional components are as follows: 2.5 parts of nicotinamide, 1 part of astaxanthin and 1 part of fullerene. Mixing the first raw materials, heating at 85 deg.C, stirring, and homogenizing at 55mPa for 5min to obtain material A.
Preparing essence, weighing the second raw material (distributed according to the total amount of 100 parts by weight), wherein the dosage of each raw material is shown in table 2, wherein: the gel material is as follows: 2 parts of carbomer 940, 3 parts of hyaluronic acid, and moisturizing materials: 2 parts of betaine, 1 part of trehalose, 2 parts of PCA-Na, 3 parts of glycerol, triethylamine as an acid-base regulator and phenoxyethanol as a preservative, and uniformly mixing the second raw material to obtain a material B.
TABLE 1 first ingredient amount/part by weight
Components Example 1 Example 2 Example 3 Example 4 Example 5 Example 6
Gel-like material 36 38 50 52 40 45
Water-soluble film-forming material 12 8 10 15 16 14
Functional ingredient 4.5 8 15 12 16 6
Deionized water 47 45 25 21 28 35
Pigment 0.5 1 0 0 0 0
Total up to 100 100 100 100 100 100
TABLE 2 second raw materials used in amount/part by weight
Components Example 1 Example 2 Example 3 Example 4 Example 5 Example 6
Gel-like material 5 4 2 3 2.5 3.5
Moisture-retaining material 8 4 6 5 7 5.5
Acid-base regulator 0.5 0.1 0.2 0.3 0.6 0.4
Preservative 1 1.5 0.5 1.2 0.9 0.6
Essence 0.5 0.4 0.3 0.5 0 0
Deionized water 85 90 91 90 89 90
Total up to 100 100 100 100 100 100
Preparing the material A into microcapsule containing fullerene by using a dropping method, uniformly flowing out the homogenized mixed solution in a cylindrical shape from a constant-temperature (85 ℃) dropping head at a uniform speed, and cutting the liquid column by using a cutter to form the microcapsule with the diameter of 5 mm. The microcapsules fell into the material B (25 deg.C) and the appearance was unchanged.
Experiments prove that the fullerene-containing microcapsule with the antioxidant and anti-aging effects, prepared by the embodiment, has a good embedding effect, the embedding rate is as high as 90% (the embedding rate refers to the percentage content of the total addition amount of the effective components in the first raw material in the microcapsule), the microcapsule has good embedding capacity on the active components, and the activity of a compound can be effectively protected. In the embodiment, the compound of the fullerene, the astaxanthin and the nicotinamide is cooperatively matched, so that excellent antioxidant, anti-aging and whitening effects are realized.
At a concentration of 0.4g/cm on the skin2The composition containing the fullerene microcapsule and the essence is applied, the moisture of the skin after the composition is obviously improved, the oil output is reduced, the skin is compact, moist and glossy, and the fullerene microcapsule with the antioxidant and anti-aging effects is fully proved to be capable of filling the skin from the skin basal layer, supplementing the collagen vitality and fundamentally achieving the anti-aging and anti-oxidation effects.
Example 2:
preparing a fullerene-containing microcapsule, weighing a first raw material (distributed according to the total amount of 100 parts by weight), wherein the dosage of each raw material is shown in table 1, and the gel material adopts the following components: 12 parts of gelatin, 20 parts of carbomer 940, 6 parts of sodium hyaluronate, 5 parts of sodium alginate, 2 parts of hydroxyethyl cellulose and 1 part of PEG400 serving as a water-soluble film forming material, and the water-soluble film forming material comprises the following functional components: 4 parts of nicotinamide, 3 parts of astaxanthin and 1 part of fullerene. Mixing the first raw materials, heating at 75 deg.C, stirring, and homogenizing at 55mPa for 5min to obtain material A.
Preparing essence, weighing a second raw material (distributed according to the total amount of 100 parts by weight), wherein the use amount of each raw material is shown in table 2, wherein: the gel material is carbomer 940, and the moisturizing material is as follows: 2 parts of butanediol, 2 parts of squalane, triethylamine as an acid-base regulator and phenoxyethanol as a preservative, and uniformly mixing the second raw material to obtain a material B.
Preparing the material A into microcapsules containing fullerene by using a dropping method, uniformly flowing out the homogenized mixed solution in a cylindrical shape from a constant-temperature (75 ℃) dropping head at a uniform speed, and cutting off a liquid column by using a cutter to form the microcapsules with the diameter of 5 mm. The microcapsules fell into the material B (25 deg.C) and the appearance was unchanged.
Experiments prove that the hydrogel microspheres with the antioxidant and anti-aging effects prepared by the embodiment have good embedding effect, the embedding rate is up to 90%, the hydrogel microspheres have good embedding capacity on active ingredients, and the activity of a compound can be effectively protected. In the embodiment, through the synergistic cooperation of the compound of the fullerene and the astaxanthin, the excellent antioxidant, anti-aging and whitening effects are realized, and in addition, the compound of the embodiment also has the effects of resisting inflammation, sterilizing, promoting wound healing and maintaining water-oil balance, so that the hydrogel microsphere has the multi-dimensional biological efficacy of antioxidant, anti-aging and moisturizing effects.
At a concentration of 0.4g/cm on the skin2The hydrogel microspheres and the essence mixture are applied, so that the water content of the skin after the hydrogel microspheres and the essence mixture are obviously improved, the oil output is reduced, the skin is compact, moist and glossy, and the hydrogel microspheres with the antioxidant and anti-aging effects fully fill the skin from the skin basal layer, supplement the collagen activity, and fundamentally achieve the anti-aging and anti-oxidation effects.
Example 3
Preparing a fullerene-containing microcapsule, weighing a first raw material (distributed according to the total amount of 100 parts by weight), wherein the dosage of each raw material is shown in table 1, a gel material adopts gellan gum, a water-soluble film-forming material adopts sodium alginate, and the functional components are as follows: 10 parts of nicotinamide, 2.5 parts of astaxanthin and 2.5 parts of fullerene. Mixing the first raw materials, heating at 65 deg.C, stirring, and homogenizing at 55mPa for 5min to obtain material A.
Preparing essence, weighing the second raw material (distributed according to the total amount of 100 parts by weight), wherein the dosage of each raw material is shown in table 2, wherein: the gel material is sodium hyaluronate, the moisture retention material is butanediol, the acid-base regulator is triethylamine, and the preservative is phenoxyethanol, and the second raw material is uniformly mixed to obtain the material B.
Preparing the material A into microcapsule containing fullerene by using a dropping method, uniformly flowing out the homogenized mixed solution in a cylindrical shape from a constant-temperature (65 ℃) dropping head at a uniform speed, and cutting the liquid column by using a cutter to form the microcapsule with the diameter of 5 mm. The microcapsules fell into the material B (25 deg.C) and the appearance was unchanged.
Example 4
Preparing a microcapsule containing fullerene, weighing a first raw material (distributed according to the total amount of 100 parts by weight), wherein the dosage of each raw material is shown in table 1, a gel material adopts gellan gum, a water-soluble film-forming material adopts chitosan, and the functional components are as follows: 6 parts of nicotinamide, 3 parts of astaxanthin and 3 parts of fullerene. Mixing the first raw materials, heating at 60 deg.C, stirring, and homogenizing at 55mPa for 5min to obtain material A.
Preparing essence, weighing a second raw material (distributed according to the total amount of 100 parts by weight), wherein the use amount of each raw material is shown in table 2, wherein: the gel material is agar, the moisture retention material is glycerol, the acid-base regulator is triethylamine, and the preservative is phenoxyethanol, and the second raw material is uniformly mixed to obtain the material B.
Preparing the material A into microcapsule containing fullerene by using a dropping method, uniformly flowing out the homogenized mixed solution in a cylindrical shape from a constant-temperature (60 ℃) dropping head at a uniform speed, and cutting the liquid column by using a cutter to form the microcapsule with the diameter of 5 mm. The microcapsules fell into the material B (25 deg.C) and the appearance was unchanged.
Example 5
Preparing a microcapsule containing fullerene, weighing a first raw material (distributed according to the total amount of 100 parts by weight), wherein the dosage of each raw material is shown in table 1, a gel material adopts gellan gum, a water-soluble film-forming material adopts PEG400, and the functional components are as follows: 10 parts of nicotinamide, 4 parts of astaxanthin and 2 parts of fullerene. Mixing the first raw materials, heating at 80 deg.C, stirring, and homogenizing at 55mPa for 5min to obtain material A.
Preparing essence, weighing a second raw material (distributed according to the total amount of 100 parts by weight), wherein the use amount of each raw material is shown in table 2, wherein: the gel material is gellan gum, the moisture retention material is hyaluronic acid, the acid-base regulator is triethylamine, and the preservative is phenoxyethanol, and the second raw material is uniformly mixed to obtain the material B.
Preparing the material A into microcapsules containing fullerene by using a dropping method, uniformly flowing out the homogenized mixed solution in a cylindrical shape from a constant-temperature (80 ℃) dropping head at a uniform speed, and cutting off a liquid column by using a cutter to form the microcapsules with the diameter of 5 mm. The microcapsules fell into the material B (25 deg.C) and the appearance was unchanged.
Example 6
Preparing a microcapsule containing fullerene, weighing a first raw material (distributed according to the total amount of 100 parts by weight), wherein the dosage of each raw material is shown in table 1, a gel material adopts carbomer, a water-soluble film-forming material adopts sodium polyacrylate, and the microcapsule comprises the following functional components: 10 parts of nicotinamide, 1 part of astaxanthin and 3 parts of fullerene. Mixing the first raw materials, heating at 70 deg.C, stirring, and homogenizing at 55mPa for 5min to obtain material A.
Preparing essence, weighing a second raw material (distributed according to the total amount of 100 parts by weight), wherein the use amount of each raw material is shown in table 2, wherein: the gel material is carbomer, the moisture retention material is butanediol, the acid-base regulator is citric acid, and the preservative is phenoxyethanol, and the second raw material is uniformly mixed to obtain the material B.
Preparing the material A into microcapsule containing fullerene by using a dropping method, uniformly flowing out the homogenized mixed solution in a cylindrical shape from a constant-temperature (70 ℃) dropping head at a uniform speed, and cutting the liquid column by using a cutter to form the microcapsule with the diameter of 5 mm. The microcapsules fell into the material B (25 deg.C) and the appearance was unchanged.
Detection of antioxidant Activity
Preparing functional components of fullerene and fullerene respectively: the mass ratio of astaxanthin is 3: 1. fullerene: the mass ratio of astaxanthin is 1: 1, keeping the rest components all the time, adding the three microcapsules into the same essence according to different mass contents, and measuring the oxidation resistance rate within 2 hours according to a beta-carotene bleaching method for 2 hours, wherein the experimental result is shown in 1.
The abscissa in fig. 1 denotes the labeled fullerene/fullerene: astaxanthin (3: 1)/fullerene: the content of astaxanthin (1: 1) is 0-50 wt%, and the ordinate indicates antioxidant activity.
As can be seen from figure 1, the antioxidant effect of the fullerene and astaxanthin compounded is superior to that of single fullerene.
In addition, the compound of the embodiment also has the effects of resisting inflammation, sterilizing, promoting wound healing and maintaining water-oil balance, and the compound of the embodiment has the biological effects of oxidation resistance, ageing resistance and moisture retention and contains multiple dimensions of the microcapsule containing the fullerene.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various features described in the foregoing embodiments may be combined in any suitable manner without contradiction. The invention is not described in detail in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.

Claims (12)

1. A fullerene containing microcapsule characterized by: the microcapsule containing fullerene comprises the following components in parts by weight: 36-52 parts of gel materials, 8-16 parts of water-soluble film-forming materials, 5-15 parts of functional components, 20-50 parts of deionized water and 0-5 parts of pigments, wherein the functional components comprise fullerene, astaxanthin and nicotinamide, and the fullerene comprises at least one of C60, C70 or fullerene derivatives; the mass ratio of the fullerene, the astaxanthin and the nicotinamide in the effective components is 1-3:1-3: 4-5; the microcapsule containing fullerene has the appearance of a droplet with the diameter of 3-8 mm and the appearance of a pearl.
2. A fullerene containing microcapsule according to claim 1, wherein: the gel material is at least one of polymethyl cellulose, gellan gum, gelatin, agar, sodium hyaluronate or carbomer;
Optionally, the fullerene derivative comprises at least one of a fullerene metal derivative, a fullerene oxygen-containing derivative, and a fullerene modified or included with an organic compound.
3. A fullerene containing microcapsule according to claim 2, wherein: the oxygen atom in the fullerene oxygen-containing derivative is connected with the carbon atom on the fullerene skeleton or bonded with an alkylene chain, and the organic compound in the fullerene modified or included by the organic compound is cyclodextrin and/or crown ether.
4. A fullerene containing microcapsule according to claim 2, wherein: the chemical formula of the fullerene derivative is C2M, M @ C2M, M2@ C2M, MA @ C2M, M3N @ C2M, M2C2@ C2M, M2S @ C2M, M2O @ C2M or MXA3-XN @ C2M, wherein M is more than or equal to 30 and less than or equal to 60, M and A are any one metal element selected from Sc, Y and lanthanide elements, and @ is a connecting group or a metal representation method;
optionally, the water-soluble film-forming material is at least one of PEG400, sodium polyacrylate, sodium alginate, hydroxyethyl cellulose, PVP, or chitosan.
5. A fullerene containing microcapsule according to claim 1, wherein: the microcapsule containing fullerene comprises the following components in parts by weight: 40-50 parts of gel materials, 10-15 parts of water-soluble film forming materials, 8-12 parts of functional components, 25-45 parts of deionized water and 0-5 parts of pigments.
6. A composition comprising a fullerene containing microcapsule according to any one of claims 1 to 5.
7. The composition of claim 6, wherein: the composition further comprises essence, wherein the fullerene-containing microcapsules are dispersed in the essence.
8. The composition of claim 7, wherein: the essence comprises the following components in parts by weight: 2-5 parts of gel material, 4-8 parts of moisture retention material, 0.05-0.6 part of acid-base regulator, 0.05-1.5 parts of preservative and 0-0.5 part of essence.
9. The composition of claim 8, wherein: the essence comprises the following components in parts by weight: 3-4 parts of gel material, 5-7 parts of moisture retention material, 0.1-0.5 part of acid-base regulator, 0.5-1.0 part of preservative and 0-0.5 part of essence.
10. The composition of claim 8, wherein: the gel material is at least one of polymethyl cellulose, gellan gum, gelatin, agar, sodium hyaluronate or carbomer;
optionally, the moisture retaining material is at least one of betaine, trehalose, PCA-Na, hyaluronic acid, butylene glycol, squalane, or glycerol;
optionally, the pH regulator is at least one of citric acid, triethylamine or sodium hydroxide.
11. A method of preparing a composition according to any one of claims 7 to 10, wherein: the method comprises the following steps:
step 1: weighing the first raw material for preparing the fullerene-containing microcapsule according to the weight parts, mixing the first raw material, heating, stirring uniformly and homogenizing to obtain a material A;
and 2, step: weighing a second raw material for preparing the essence according to the weight parts, and uniformly mixing the second raw material to obtain a material B;
and 3, step 3: and (3) using a constant-temperature dripper to flow out the material A at a constant speed, and then cutting off a liquid column by using a cutter to form a series of liquid drops, so that the liquid drops fall into the material B, and the shape of the liquid drops is not changed to prepare the composition.
12. A process for preparing a composition according to claim 11, characterized in that: the mass ratio of the material A to the material B is as follows: 5-45: 95-55;
optionally, the heating temperature in the step 1 is 60-85 ℃, and the homogenization time is 3-8 min;
optionally, the constant temperature in step 3 is 60-85 deg.C, the constant rate is 2-5 drops/s, and the diameter of the drop is 3-8 mm.
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