CN109394585B - Antioxidant and moisturizing liquid crystal composition and preparation method and application thereof - Google Patents
Antioxidant and moisturizing liquid crystal composition and preparation method and application thereof Download PDFInfo
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
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- A—HUMAN NECESSITIES
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- 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
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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
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Abstract
The invention relates to the technical field of daily chemical products, and discloses an antioxidant and moisturizing liquid crystal composition and a preparation method and application thereof. The liquid crystal composition comprises 0.01-5% of ophiopogonpolysaccharide, 0.5-15% of silybum marianum seed oil, 1-20% of emulsifier, 1-20% of co-emulsifier, 5-35% of liquid grease, 0.01-5% of thickener, 0.1-10% of preservative and the balance of water. According to the invention, the silybum marianum seed oil and the ophiopogonpolysaccharide are encapsulated in the liquid crystal structure prepared by special material combination, so that the overall stability is high, and the liquid crystal structure is complete; can form a good closed system on the skin, enhance the hydration of the skin, have obvious moisturizing performance and antioxidant effect and have good application prospect in the field of cosmetics.
Description
Technical Field
The invention relates to the technical field of daily chemical products, in particular to an antioxidant and moisturizing liquid crystal composition and a preparation method and application thereof.
Background
In daily skin care, moisture retention and oxidation resistance are important conditions for ensuring skin health and delaying aging. In recent years, due to the doubts about the toxicity and irritation of chemical cosmetics, more and more scientific researchers tend to search for safe and efficient moisturizing antioxidant active ingredients from natural plants. The ophiopogonpolysaccharide is natural plant polysaccharide extracted from radix Ophiopogonis, has effects of retaining youthful looks, moistening skin, building body, blackening hair, resisting aging, absorbing water from atmosphere to keep skin moist, and absorbing water from skin deep layer to achieve moisture keeping effect. The silybum marianum seed oil is prepared from Silybum marianum (L.) Gaertn of CompositaeSilybum marianum Gaertn) The fruit is refined by the processes of cold frying, filtering and the like. The silybum marianum seed oil is rich in vitamin E and its derivatives and phytosterol, and has the effects of improving immunity, resisting against tumor, and improving immunityScavenging free radicals, resisting oxidation, increasing skin elasticity and water retention, and keeping skin moisture. Silybum marianum seed oil is an active ingredient commonly used in high-end cosmetics at present.
At present, the carrier technology related to the silybum marianum seed oil and the ophiopogon japonicus polysaccharide is less in patents, and how to improve the active ingredients of the silybum marianum seed oil and the ophiopogon japonicus polysaccharide and keep the integral stability of the product is the research focus of a novel carrier technology.
Disclosure of Invention
In view of the above, the present invention is directed to an antioxidant and moisturizing liquid crystal composition and a preparation method thereof, so that the liquid crystal composition has high stability at low temperature, light, high temperature and normal temperature;
another object of the present invention is to provide an antioxidant and moisturizing liquid crystal composition and a method for preparing the same, such that the liquid crystal composition has higher moisturizing performance and antioxidant effect than a product with the same active ingredients;
another object of the present invention is to provide the related application of the liquid crystal composition in the preparation of daily chemical products.
In order to achieve the above purpose, the invention provides the following technical scheme:
an antioxidant and moisturizing liquid crystal composition comprises 0.01-5% of ophiopogonpolysaccharide, 0.5-15% of silybum marianum seed oil, 1-20% of an emulsifier, 1-20% of an auxiliary emulsifier, 5-35% of liquid grease, 0.01-5% of a thickener, 0.1-10% of a preservative and the balance of water; the percentage is mass percent.
Wherein the preferable mass percentage of the ophiopogonpolysaccharide is 0.05-4%, more preferable mass percentage is 0.1-2%, and further preferable mass percentage is 0.5-1%; in a specific embodiment of the present invention, the ophiopogonpolysaccharide is 0.01%, 0.02%, 0.05%, 0.1%, 0.5%, 0.8%, 1%, 2%, 3%, 4% or 5% by mass;
the mass percentage of the silybum marianum seed oil is preferably 1% -12%, more preferably 2% -10%, and further preferably 4% -8%; in a specific embodiment of the invention, the silybum marianum seed oil is 0.5%, 1%, 2%, 4%, 5%, 6%, 7%, 8%, 10%, 12% or 15% by mass;
the mass percentage of the emulsifier is preferably 3% -18%, more preferably 5% -15%, and further preferably 8% -12%; in a specific embodiment of the invention, the mass percentage of the emulsifier is 3%, 7%, 20%, 5%, 8%, 15%, 9%, 8.5%, 4% or 6%;
the emulsifier is one or a mixture of more than two of PEG-20 methyl glucose sesquistearate, steareth-21, steareth-2, polyglycerol-6 distearate, polyglycerol-3 beeswax ester, C14-22 alcohol/C12-20 alkyl glucoside, arachidyl alcohol glucoside, cetostearyl alcohol and cetostearyl glucoside, eicosyl docosyl alcohol and eicosyl glucoside, cocoyl glucoside and cocoyl alcohol, cetostearyl alcohol and cocoyl glucoside, and hydrogenated lecithin. When the emulsifier is a mixture of a plurality of substances, the proportion of each component in the mixture is not particularly limited; in a specific embodiment of the invention, the emulsifier is selected from one, two or three of the above emulsifiers; for example:
c14-22 alcohol/C12-20 alkyl glucoside + hydrogenated lecithin;
coco glucoside and coco alcohol + arachidyl glucoside + hydrogenated lecithin;
eicosyl docosyl alcohol and icosyl glucoside + PEG-20 methyl glucose sesquistearate + cetostearyl alcohol and coco glucoside;
steareth-21 + steareth-2;
cetostearyl alcohol and cetostearyl glycoside + arachidyl behenyl alcohol and arachidyl glucoside;
polyglyceryl-6 distearate + eicosyl docosyl alcohol and eicosyl glucoside + C14-22 alcohol/C12-20 alkyl glucoside;
cetostearyl alcohol and cetostearyl glycoside + polyglycerol-3 beeswax + hydrogenated lecithin;
eicosyl docosyl alcohol and icosyl glucoside + cetostearyl alcohol and cetostearyl glucoside;
c14-22 alcohol/C12-20 alkyl glucoside + eicosyl docosyl alcohol and eicosyl glucoside;
hydrogenated lecithin + arachidonol glucoside;
the mass percentage of the co-emulsifier is preferably 2-18%, more preferably 5-13%, and further preferably 6-10%; in a specific embodiment of the present invention, the mass percentage of the emulsifier is 1%, 5%, 2%, 12%, 20%, 10%, 13%, 18% or 7%;
the auxiliary emulsifier is one or more of ceteareth-6, cetostearyl alcohol, cetyl alcohol, stearyl alcohol, behenyl alcohol and PEG-100 stearate. When the coemulsifier is a mixture of a plurality of substances, the proportion of each component in the mixture is not particularly limited by the invention; in a specific embodiment of the invention, the co-emulsifier is selected from one, two or three of the above-mentioned co-emulsifiers; for example:
behenyl alcohol + PEG-100 stearate; stearyl alcohol + PEG-100 stearate; cetostearyl alcohol + behenyl alcohol; cetostearyl alcohol + PEG-100 stearate; cetostearyl alcohol + behenyl alcohol + PEG-100 stearate; cetyl alcohol + cetostearyl alcohol + behenyl alcohol; ceteareth-6 + PEG-100 stearate + behenyl alcohol;
the mass percentage of the liquid oil is preferably 8-30%, more preferably 10-25%, and further preferably 12-20%; in a specific embodiment of the present invention, the liquid oil is 10%, 11%, 25%, 7%, 19%, 5%, 8%, 12%, 13%, 30% or 35% by mass;
the liquid oil is one or a mixture of more than two of caprylic/capric glyceride, isopropyl myristate, simethicone, vitamin E, ethyl oleate, mineral oil, polycyclopentadimethylsiloxane, caprylic/capric cocoa butter, isononyl isononanoate, isohexadecane, soybean oil, propylene glycol dicaprylate, octyl butanol salicylate, sunflower seed oil and squalane. When the liquid grease is a mixture of a plurality of substances, the proportion of each component in the mixture is not particularly limited; in a specific embodiment of the invention, the liquid oil is one, two, three or four of the liquid oils; for example:
dimethicone + caprylic/capric glyceride + isononyl isononanoate; mineral oil + polycyclopentadimethylsiloxane + caprylic/capric cocoa butter; squalane + octylbutanol salicylate + cocoa butter octyldecanoate; isononyl isononanoate, simethicone and vitamin E; isohexadecane + mineral oil + ethyl oleate; isopropyl myristate + dimethicone; simethicone plus soybean oil; dimethicone + isopropyl myristate + isononyl isononanoate; sunflower seed oil, squalane and simethicone; propylene glycol dicaprylate decanoate + caprylic/capric glyceride + dimethicone; simethicone plus mineral oil; mineral oil + squalane + isopropyl myristate + polycyclopentadimethylsiloxane; isononyl isononanoate + isohexadecane + simethicone + squalane;
the mass percentage of the thickening agent is preferably 0.05-4.5%, more preferably 0.1-0.4%, and further preferably 0.2-0.3%; in a specific embodiment of the invention, the thickener is present in an amount of 0.3%, 1.01%, 0.62%, 5%, 2.1%, 0.01%, 0.2%, 0.1%, 0.05%, 0.4%, 0.7% or 4.5% by mass;
the thickener is one or more of xanthan gum, hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer, polyacrylamide/C13-14 isoparaffin/lauryl alcohol ether-7, polyvinylpyrrolidone, hydroxypropyl methylcellulose, polyacrylate cross-linked polymer-6, gelatin, acacia and carbomer. When the thickener is a mixture of a plurality of substances, the present invention is not particularly limited to the ratio of the components in the mixture; in a specific embodiment of the invention, the thickener is selected from one, two, three or four of the above thickeners; for example:
polyacrylamide/C13-14 isoparaffin/lauryl alcohol ether-7 + gelatin; hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer + hydroxypropyl methylcellulose; polyacrylate crosspolymer-6 + carbomer; polyvinylpyrrolidone + hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer; gum arabic + polyacrylamide/C13-14 isoparaffin/lauryl alcohol ether-7 + polyacrylate crosspolymer-6; hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer and polyacrylate cross-linked polymer-6; polyacrylamide/C13-14 isoparaffin/laureth-7 + carbomer; hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer, xanthan gum and carbomer; polyvinylpyrrolidone + polyacrylamide/C13-14 isoparaffin/laureth-7 + gum arabic;
the preservative is preferably 0.2-9 wt%, more preferably 1-8 wt%, and even more preferably 3-6 wt%; in a specific embodiment of the invention, the preservative is 0.5%, 3%, 3.5%, 9%, 1.3%, 8%, 0.2%, 6%, 1%, 0.1% or 2% by mass;
the antiseptic is one or more of phenoxyethanol, 1, 2-hexanediol, 1, 2-pentanediol, methyl hydroxybenzoate, ethylparaben, ethylhexyl glycerol, caprylyl hydroximic acid, and p-hydroxyacetophenone. When the preservative is a mixture of a plurality of substances, the present invention is not particularly limited to the ratio of each component in the mixture; in a specific embodiment of the invention, the preservative is selected from one, two, three or four of the above preservatives; for example:
1, 2-hexanediol +1, 2-pentanediol; p-hydroxyacetophenone +1, 2-pentanediol; ethylhexyl glycerol + caprylyl hydroxamic acid +1, 2-hexanediol; methylparaben + ethylparaben; ethylhexyl glycerol + caprylyl hydroxamic acid + p-hydroxyacetophenone; phenoxyethanol + caprylyl hydroxamic acid + p-hydroxyacetophenone; phenoxyethanol + ethylhexylglycerin; phenoxyethanol +1, 2-hexanediol;
in addition, the invention also provides a preparation method of the liquid crystal composition, which comprises the following steps:
mixing and stirring silybum marianum seed oil, an emulsifier, an auxiliary emulsifier and liquid oil to obtain a uniform oil phase; mixing and stirring ophiopogonpolysaccharide, a thickening agent and the balance water to obtain a uniform water phase;
the oil phase is rapidly added into the water phase, and the liquid crystal colostrum is obtained after shearing and emulsification treatment;
and cooling the liquid crystal colostrum, adding a preservative, and stirring to obtain the liquid crystal composition.
More specifically, the mixing and stirring temperature of the silybum marianum seed oil, the emulsifier, the co-emulsifier and the liquid oil is preferably 35-80 ℃, more preferably 40-75 ℃, and further preferably 50-70 ℃; the mixing and stirring time is preferably 10-40 min, more preferably 12-35 min, and further preferably 15-30 min; the mixing and stirring speed is preferably 100 to 600 rpm, more preferably 150 to 550 rpm, and further preferably 200 to 500 rpm.
The mixing and stirring temperature of the ophiopogonpolysaccharide, the thickening agent and the balance water is preferably 35-80 ℃, more preferably 40-75 ℃, and further preferably 50-70 ℃; the mixing and stirring time is preferably 10-40 min, more preferably 12-35 min, and further preferably 15-30 min; the mixing and stirring speed is preferably 100 to 600 rpm, more preferably 150 to 550 rpm, and further preferably 200 to 500 rpm.
The rotation speed of the shearing emulsification treatment is preferably 2000-15000 rpm, more preferably 4000-12000 rpm, and further preferably 8000-10000 rpm; the time for the shearing emulsification treatment is preferably 1 to 30 min, more preferably 5 to 25 min, and still more preferably 10 to 20 min.
The temperature of the liquid crystal colostrum is preferably reduced to 20-60 ℃, more preferably to 25-50 ℃, and further preferably to 30-45 ℃; the stirring time is preferably 10-40 min, more preferably 12-35 min, and further preferably 15-30 min; the rotation speed of the stirring is preferably 100-600 rpm, more preferably 150-550 rpm, and further preferably 200-500 rpm.
In the invention, the emulsifier and the co-emulsifier are matched, so that the skin care composition has good penetration promoting effect, and can effectively convey and penetrate the active components into the stratum corneum layer, so that the active components effectively act on deep cells of the skin to effectively exert skin efficacy; compared with the common product with the same content of silybum marianum seed oil and ophiopogon japonicus polysaccharide, the skin feeling comprehensive evaluation is better, and the product has better appearance, spreadability and after-use feeling; has stronger moisture retention capacity and oxidation resistance;
meanwhile, the components synergistically increase the stability of the liquid crystal composition; compared with the liquid crystal structure just prepared, the liquid crystal composition has no obvious change in the liquid crystal structure and number after being placed under the conditions of 45 ℃, 4 ℃, illumination and room temperature for 2 months.
Based on the technical effects, the invention provides the application of the liquid crystal composition or the liquid crystal composition prepared by the preparation method in the preparation of daily chemical products. Preferably, the daily chemical product is a cosmetic, a shower gel or a hair washing and caring product, wherein the cosmetic includes but is not limited to skin care products; the daily chemical product form preferably comprises cream and emulsion.
According to the technical scheme, the silybum marianum seed oil and the ophiopogonpolysaccharide are wrapped in the liquid crystal structure prepared by special material combination, so that the whole stability is high, and the liquid crystal structure is complete; can form a good closed system on the skin, enhance the hydration of the skin, have obvious moisturizing performance and antioxidant effect and have good application prospect in the field of cosmetics.
Drawings
FIG. 1 is a view showing the liquid crystal structure of the liquid crystal composition immediately after preparation in example 7;
FIG. 2 is a structural diagram of a liquid crystal composition of example 7 of the present invention after being exposed to 45 deg.C, 4 deg.C, light and room temperature for 2 months;
FIG. 3 is a view showing the liquid crystal composition liquid crystal structure of the liquid crystal composition immediately after preparation in example 11;
FIG. 4 is a structural diagram of a liquid crystal composition of example 11 of the present invention after being exposed to 45 deg.C, 4 deg.C, light and room temperature for 2 months;
FIG. 5 is a polarization microscope photograph of the liquid crystal cream C1;
FIG. 6 is a polarization microscope photograph of the liquid crystal cream C2;
FIG. 7 shows a skin feel test radar plot;
fig. 8 is a bar graph showing the moisture retention performance test.
Detailed Description
The invention discloses an antioxidant and moisturizing liquid crystal composition, and a preparation method and application thereof. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. The liquid crystal composition, the preparation method and the application thereof of the present invention have been described by way of example, and it is obvious to those skilled in the art that the technology of the present invention can be implemented and applied by modifying or appropriately changing and combining the liquid crystal composition, the preparation method and the application thereof without departing from the content, spirit and scope of the present invention.
In the specific embodiment of the invention, the comparison test is involved, and the test environment, the raw materials and the like are consistent except for the difference of each test group.
The antioxidant and moisturizing liquid crystal composition provided by the invention, and the preparation method and application thereof are further described below.
Example 1: preparation of the liquid Crystal composition of the invention
Stirring and mixing 0.5% of silybum marianum seed oil, 2% of C14-22 alcohol/C12-20 alkyl glucoside, 1% of hydrogenated lecithin, 1% of ceteareth-6, 5% of dimethyl silicone oil, 2% of caprylic/capric glyceride and 3% of isononyl isononanoate at the stirring speed of 300 rpm in a water bath condition of 35 ℃ for 25 min to obtain a uniform oil phase;
mixing 0.01% of ophiopogonpolysaccharide, 0.1% of polyacrylamide/C13-14 isoparaffin/lauryl alcohol ether-7, 0.2% of gelatin and the balance of water, and stirring and mixing at a stirring speed of 300 rpm for 25 min under a water bath condition of 35 ℃ to obtain a uniform water phase;
rapidly adding the oil phase into the water phase, and shearing at 4000 rpm for 5 min to obtain liquid crystal colostrum;
cooling the liquid crystal colostrum to 25 deg.C, adding 0.5% phenoxyethanol, stirring and mixing at 550 rpm for 10 min to obtain antioxidant and moisturizing liquid crystal composition.
Example 2: preparation of the liquid Crystal composition of the invention
Stirring and mixing 8% of silybum marianum seed oil, 4% of coco glucoside and coco alcohol, 2% of arachidyl alcohol glucoside, 1% of hydrogenated lecithin, 5% of ceteareth-6, 1% of mineral oil, 5% of polycyclopentadimethylsiloxane and 5% of cocoa butter octadecanoate at a stirring speed of 200 rpm for 30 min under a water bath condition of 65 ℃ to obtain a uniform oil phase;
mixing 3% of ophiopogonpolysaccharide, 1% of hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer, 0.01% of hydroxypropyl methylcellulose and the balance of water, and stirring and mixing for 30 min at a stirring speed of 200 rpm under a water bath condition of 65 ℃ to obtain a uniform water phase;
rapidly adding the oil phase into the water phase, and shearing at 2000 rpm for 20 min to obtain liquid crystal colostrum;
cooling the liquid crystal colostrum to 45 ℃, adding 1.5% of 1, 2-hexanediol and 1.5% of 1, 2-pentanediol, and stirring and mixing for 30 min at a stirring speed of 100 rpm to obtain the antioxidant and moisturizing liquid crystal composition.
Example 3: preparation of the liquid Crystal composition of the invention
Stirring and mixing 1% of silybum marianum seed oil, 6% of eicosyl docosyl alcohol and eicosyl glucoside, 2% of PEG-20 methyl glucose sesquistearate, 12% of cetostearyl alcohol and coco glucoside, 2% of cetostearyl alcohol, 10% of squalane, 10% of octyl butanol salicylate and 5% of cocoa butter octadecanoate at a stirring speed of 500 rpm for 20 min under a water bath condition of 75 ℃ to obtain a uniform oil phase;
mixing 0.1% of ophiopogonpolysaccharide, 0.6% of polyacrylate cross-linked polymer-6, 0.02% of carbomer and the balance of water, and stirring and mixing for 20 min at a stirring speed of 500 rpm under the condition of a water bath at 75 ℃ to obtain a uniform water phase;
rapidly adding the oil phase into the water phase, and shearing at 6000 rpm for 2 min to obtain liquid crystal colostrum;
cooling the liquid crystal colostrum to 40 ℃, adding 2% of p-hydroxyacetophenone and 1.5% of 1, 2-pentanediol, and stirring and mixing for 10 min at the stirring speed of 300 rpm to obtain the antioxidant and moisturizing liquid crystal composition.
Example 4: preparation of the liquid Crystal composition of the invention
Stirring and mixing 10% of silybum marianum seed oil, 2% of steareth-21, 3% of steareth-2, 9% of behenyl alcohol, 3% of PEG-100 stearate, 4% of isononyl isononanoate, 1% of dimethyl silicone oil and 2% of vitamin E for 30 min at a stirring speed of 400 rpm under a water bath condition of 80 ℃ to obtain a uniform oil phase;
mixing 0.01% of ophiopogonpolysaccharide, 2% of polyvinylpyrrolidone, 3% of hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer and the balance of water, and stirring and mixing for 30 min at a stirring speed of 400 rpm under a water bath condition of 80 ℃ to obtain a uniform water phase;
rapidly adding the oil phase into the water phase, and shearing at 12000 rpm for 1 min to obtain liquid crystal colostrum;
cooling the liquid crystal colostrum to 35 ℃, adding 6% of ethylhexyl glycerol, 1.5% of caprylyl hydroximic acid and 1.5% of 1, 2-hexanediol, and stirring and mixing for 15 min at a stirring speed of 500 rpm to obtain the antioxidant and moisturizing liquid crystal composition.
Example 5: preparation of the liquid Crystal composition of the invention
Stirring and mixing 2% of silybum marianum seed oil, 5% of hexadecyl octadecyl alcohol and hexadecyl octadecyl glycoside, 3% of eicosyl docosyl alcohol and eicosyl glucoside, 12% of octadecyl alcohol, 8% of PEG-100 stearate, 6% of isohexadecane, 8% of mineral oil and 5% of ethyl oleate for 40 min at a stirring speed of 100 rpm under a water bath condition of 60 ℃ to obtain a uniform oil phase;
mixing 0.02% of ophiopogonpolysaccharide, 1% of Arabic gum, 1% of polyacrylamide/C13-14 isoparaffin/lauryl alcohol ether-7, 0.1% of polyacrylate cross-linked polymer-6 and the balance of water, and stirring and mixing at a stirring speed of 100 rpm for 40 min under a water bath condition of 60 ℃ to obtain a uniform water phase;
rapidly adding the oil phase into the water phase, and shearing at 10000 rpm for 3 min to obtain liquid crystal colostrum;
cooling the liquid crystal colostrum to 45 deg.C, adding 0.5% methyl hydroxybenzoate and 0.8% ethyl hydroxybenzoate, stirring and mixing at 300 rpm for 10 min to obtain antioxidant and moisture keeping liquid crystal composition.
Example 6: preparation of the liquid Crystal composition of the invention
Stirring and mixing 12% of silybum marianum seed oil, 3% of polyglycerol-6 distearate, 6% of eicosyl docosyl alcohol and eicosyl glucoside, 6% of C14-22 alcohol/C12-20 alkyl glucoside, 1% of cetostearyl alcohol, 2% of isopropyl myristate and 3% of dimethyl silicone oil for 40 min at a stirring speed of 550 rpm under a water bath condition of 70 ℃ to obtain a uniform oil phase;
mixing 5% of ophiopogonpolysaccharide, 0.01% of hydroxypropyl methylcellulose and the balance of water, and stirring and mixing for 30 min at a stirring speed of 550 rpm under a water bath condition of 70 ℃ to obtain a uniform water phase;
rapidly adding the oil phase into the water phase, and shearing at 8000 rpm for 25 min to obtain liquid crystal colostrum;
cooling the liquid crystal colostrum to 50 ℃, adding 1% of ethylhexyl glycerol, 1% of caprylyl hydroximic acid and 1% of p-hydroxyacetophenone, stirring and mixing at the stirring speed of 600 rpm for 18 min to obtain the antioxidant and moisturizing liquid crystal composition.
Example 7: preparation of the liquid Crystal composition of the invention
Stirring and mixing 15% of silybum marianum seed oil, 2% of cetostearyl alcohol and cetostearyl glycoside, 6% of polyglycerol-3 beeswax ester, 1% of hydrogenated lecithin, 3% of cetostearyl alcohol, 2% of behenyl alcohol, 1% of dimethyl silicone oil and 4% of soybean oil at a stirring speed of 600 rpm for 35 min under a water bath condition of 50 ℃ to obtain a uniform oil phase;
mixing 2% of ophiopogonpolysaccharide, 0.1% of hydroxyethyl acrylate/acryloyl dimethyl taurate copolymer, 0.1% of polyacrylate cross-linked polymer-6 and the balance of water, and stirring and mixing for 10 min at a stirring speed of 600 rpm under a water bath condition of 50 ℃ to obtain a uniform water phase;
rapidly adding the oil phase into the water phase, and shearing at 6000 rpm for 12 min to obtain liquid crystal colostrum;
cooling the liquid crystal colostrum to 40 deg.C, adding 2% phenoxyethanol, 3% caprylyl hydroximic acid, and 3% p-hydroxyacetophenone, stirring and mixing at 200 rpm for 12 min to obtain antioxidant and moisturizing liquid crystal composition.
Example 8: preparation of the liquid Crystal composition of the invention
Stirring and mixing 4 mass percent of silybum marianum seed oil, 1 mass percent of polyglycerol-6 distearate, 7 mass percent of eicosyl docosyl alcohol and eicosyl glucoside, 0.5 mass percent of C14-22 alcohol/C12-20 alkyl glucoside, 5 mass percent of cetostearyl alcohol, 5 mass percent of PEG-100 stearate, 1 mass percent of dimethyl silicone oil, 3 mass percent of isopropyl myristate and 4 mass percent of isononyl isononanoate at a stirring speed of 500 rpm under the condition of a water bath at 40 ℃ for 15 min to obtain a uniform oil phase;
mixing 1% of ophiopogonpolysaccharide, 0.1% of hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer and the balance of water, and stirring and mixing at a stirring speed of 500 rpm for 15 min under a water bath condition of 40 ℃ to obtain a uniform water phase;
rapidly adding the oil phase into the water phase, and shearing at 9000 rpm for 10 min to obtain liquid crystal colostrum;
cooling the liquid crystal colostrum to 20 ℃, adding 0.2% of p-hydroxyacetophenone, stirring and mixing for 40 min at the stirring speed of 100 rpm, and obtaining the antioxidant and moisturizing liquid crystal composition.
Example 9: preparation of the liquid Crystal composition of the invention
Stirring and mixing 5% of silybum marianum seed oil, 2% of eicosyl docosyl alcohol and eicosyl glucoside, 1% of hexadecyl octadecyl alcohol and hexadecyl octadecyl glucoside, 5% of hexadecyl octadecyl alcohol, 5% of behenyl alcohol, 3% of PEG-100 stearate, 2% of sunflower seed oil, 5% of squalane and 5% of dimethyl silicone oil at a stirring speed of 400 rpm for 40 min under a water bath condition of 75 ℃ to obtain a uniform oil phase;
mixing 0.5% of ophiopogonpolysaccharide, 0.05% of polyacrylamide/C13-14 isoparaffin/lauryl alcohol ether-7 and the balance of water, and stirring and mixing at a stirring speed of 400 rpm for 40 min under a water bath condition of 75 ℃ to obtain a uniform water phase;
rapidly adding the oil phase into the water phase, and shearing at 2000 rpm for 30 min to obtain liquid crystal colostrum;
cooling the liquid crystal colostrum to 30 ℃, adding 3% of 1, 2-pentanediol and 3% of 1, 2-hexanediol, stirring and mixing for 40 min at a stirring speed of 100 rpm, and obtaining the antioxidant and moisturizing liquid crystal composition.
Example 10: preparation of the liquid Crystal composition of the invention
Stirring and mixing 7% of silybum marianum seed oil, 3% of C14-22 alcohol/C12-20 alkyl glucoside, 1% of eicosyl docosyl alcohol and eicosyl glucoside, 3% of cetyl alcohol, 5% of cetostearyl alcohol, 5% of behenyl alcohol, 3% of propylene glycol dioctanoate decanoate, 5% of caprylic/capric glyceride and 5% of dimethyl silicone oil at a stirring speed of 500 rpm for 30 min under a water bath condition of 65 ℃ to obtain a uniform oil phase;
mixing 0.8% of ophiopogonpolysaccharide, 0.2% of hydroxyethyl acrylate/acryloyl dimethyl taurate copolymer, 0.2% of polyacrylate cross-linked polymer-6 and the balance of water, and stirring and mixing for 30 min at a stirring speed of 500 rpm under a water bath condition of 65 ℃ to obtain a uniform water phase;
rapidly adding the oil phase into the water phase, and shearing at 8000 rpm for 10 min to obtain liquid crystal colostrum;
cooling the liquid crystal colostrum to 40 deg.C, adding 0.5% phenoxyethanol and 0.5% ethylhexyl glycerol, stirring and mixing at 300 rpm for 20 min to obtain antioxidant and moisturizing liquid crystal composition.
Example 11: preparation of the liquid Crystal composition of the invention
Stirring and mixing 4% of silybum marianum seed oil, 3% of steareth-21, 3% of steareth-2, 7% of ceteareth-6, 5% of PEG-100 stearate, 6% of behenyl alcohol, 4% of dimethicone and 3% of mineral oil in water bath condition at 80 ℃ at a stirring speed of 400 rpm for 10 min to obtain uniform oil phase;
mixing 1% of ophiopogonpolysaccharide, 0.1% of polyacrylamide/C13-14 isoparaffin/lauryl alcohol ether-7, 0.1% of carbomer and the balance of water, and stirring and mixing at a stirring speed of 150 rpm for 12 min under a water bath condition of 35 ℃ to obtain a uniform water phase;
rapidly adding the oil phase into the water phase, and shearing at 15000 rpm for 2 min to obtain liquid crystal colostrum;
cooling the liquid crystal colostrum to 20 deg.C, adding 0.1% p-hydroxyacetophenone, stirring at 150 rpm, and mixing for 35 min to obtain antioxidant and moisture keeping liquid crystal composition.
Example 12: preparation of the liquid Crystal composition of the invention
Stirring and mixing 6% of silybum marianum seed oil, 1% of hydrogenated lecithin, 4% of arachidonoyl glucoside, 7% of cetostearyl alcohol, 4% of mineral oil, 8% of squalane, 6% of isopropyl myristate and 12% of polycyclopentadimethyl siloxane at a stirring speed of 150 rpm for 12 min under a water bath condition of 70 ℃ to obtain a uniform oil phase;
mixing 4% of ophiopogonpolysaccharide, 0.5% of hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer, 0.1% of xanthan gum, 0.1% of carbomer and the balance of water, and stirring and mixing for 35 min at a stirring speed of 200 rpm under a water bath condition of 70 ℃ to obtain a uniform water phase;
rapidly adding the oil phase into the water phase, and shearing at 15000 rpm for 2 min to obtain liquid crystal colostrum;
cooling the liquid crystal colostrum to 60 ℃, adding 1% of 1, 2-hexanediol and 2% of 1, 2-pentanediol, and stirring and mixing for 15 min at a stirring speed of 200 rpm to obtain the antioxidant and moisturizing liquid crystal composition.
Example 13: preparation of the liquid Crystal composition of the invention
Stirring and mixing 2% of silybum marianum seed oil, 3% of hexadecyl alcohol and coco glucoside, 2% of octadecyl alcohol, 10% of isononyl isononanoate, 8% of isohexadecane, 10% of dimethyl silicone oil and 7% of squalane at a stirring speed of 600 rpm for 15 min under a water bath condition of 60 ℃ to obtain a uniform oil phase;
mixing 0.05% of ophiopogonpolysaccharide, 2% of polyvinylpyrrolidone, 0.5% of polyacrylamide/C13-14 isoparaffin/lauryl alcohol ether-7, 2% of acacia gum and the balance of water, and stirring and mixing at a stirring speed of 600 rpm for 20 min under a water bath condition of 60 ℃ to obtain a uniform water phase;
rapidly adding the oil phase into the water phase, and shearing at 6000 rpm for 10 min to obtain liquid crystal colostrum;
cooling the liquid crystal colostrum to 40 deg.C, adding 0.5% phenoxyethanol and 1.5%1, 2-hexanediol, stirring and mixing at 200 rpm for 15 min to obtain antioxidant and moisture keeping liquid crystal composition.
Example 14: stability test
The stability test was performed using examples 7 and 11 as test samples. The oxidation-resistant and moisture-retaining liquid crystal compositions obtained in example 7 and example 11 were subjected to 45 ℃, 4 ℃, light and room temperature conditions, respectively, and then observed for stability, whether they were precipitated and separated into layers or not at 1 week, 1 month and 2 months, respectively, and the crystal morphology stability was observed under a polarization microscope, and the results are shown in table 1.
TABLE 1 stability of antioxidant and moisturizing liquid crystal compositions
As shown in fig. 1 and 2, the polarization microscope images of the oxidation-resistant and moisture-retaining liquid crystal composition taken in the stability test of example 7 are magnified 100 times. FIG. 1 is a structural view of a liquid crystal composition as prepared, and FIG. 2 is a structural view of a liquid crystal composition after the liquid crystal composition is left at 45 ℃ under 4 ℃ under light and at room temperature for 2 months. Comparing fig. 1 and fig. 2, it is found that the number of the liquid crystal is the same as that of fig. 1, the size is uniform, no obvious change occurs, and the liquid crystal composition does not separate and delaminate.
As shown in fig. 3 and 4, the polarization microscope images of the oxidation-resistant and moisture-retaining liquid crystal composition taken in the stability test of example 11 are magnified 100 times. FIG. 3 is a structural view of a liquid crystal composition immediately after preparation, and FIG. 4 is a structural view of a liquid crystal composition after the liquid crystal composition is left at 45 ℃ under 4 ℃ under light irradiation and at room temperature for 2 months. Comparing fig. 3 and fig. 4, it is found that the number of the liquid crystal is the same as that of fig. 3, the size is uniform, no obvious change occurs, and the liquid crystal composition does not separate and delaminate.
Example 15: skin feel test
1. Preparation of common cream
Melting 2.0% of PEC-10 polydimethylsiloxane, 1.0% of sucrose stearate, 1.0% of stearyl alcohol, 4.5% of glyceryl monostearate and 3.0% of jojoba oil in a water bath at 75 ℃ according to mass percentage to obtain an oil phase;
dissolving 5.0% glycerol, 5.0% propylene glycol, 0.3% triethanolamine, 0.2% carbomer 2020 and 77.0% purified water in 75 deg.C water bath to obtain water phase; mixing the oil phase and the water phase under stirring, and emulsifying to obtain common cream.
2. Preparation of liquid Crystal creams C1 and C2
The common cream is mixed with the antioxidant and moisturizing liquid crystal composition of example 7 according to a ratio of 1:1 to obtain the cream of the antioxidant and moisturizing liquid crystal composition with a mass fraction of 50.0%, wherein the cream contains 1% of ophiopogonpolysaccharide and 7.5% of silybum marianum seed oil in percentage by mass.
The prepared C1 liquid crystal cream is magnified by 100 times under a polarization microscope to obtain a polarization microscope image as shown in FIG. 5, the liquid crystal of the antioxidant and moisturizing cream is uniform in size as shown in FIG. 5, and the effective components are coated in the liquid crystal structure.
The common cream is mixed with the antioxidant and moisturizing liquid crystal composition of example 11 according to a ratio of 1:1 to obtain a cream of the antioxidant and moisturizing liquid crystal composition with a mass fraction of 50.0%, wherein the cream contains 0.5% of ophiopogon polysaccharides and 2% of silybum marianum seed oil in percentage by mass.
The prepared C2 liquid crystal cream was magnified 100 times under a polarization microscope to obtain a polarization microscope image as shown in fig. 6, and as shown in fig. 6, the liquid crystal of the antioxidant and moisturizing cream was uniform in size, and the effective ingredients were coated in the liquid crystal structure.
3. Preparation of comparative creams D1 and D2
Comparative creams D1 and D2 without liquid crystal structure were prepared according to the formulation and method in 1:
according to the mass percentage, 1% of ophiopogonpolysaccharide, 7.5% of silybum marianum seed oil, 2.0% of PEC-10 polydimethylsiloxane, 1.0% of sucrose stearate, 1.0% of stearyl alcohol, 4.5% of glyceryl monostearate and 3.0% of jojoba oil are melted in a water bath at 75 ℃ to obtain an oil phase;
dissolving 5.0% glycerol, 5.0% propylene glycol, 0.3% triethanolamine, 0.2% carbomer 2020 and 69.5% purified water in 75 deg.C water bath to obtain water phase; and stirring and mixing the oil phase and the water phase, and emulsifying to obtain the antioxidant and moisturizing comparative cream D1 without a liquid crystal structure.
The content of ophiopogonin and silybum marianum seed oil in the comparison cream is the same as that of the liquid crystal cream C1, and the same basic cream components as those in the comparison cream 1 are adopted, except that the ophiopogonin and the silybum marianum seed oil are not encapsulated by a liquid crystal structure.
According to the mass percentage, 0.5% of ophiopogonpolysaccharide, 2% of silybum marianum seed oil, 2.0% of PEC-10 polydimethylsiloxane, 1.0% of sucrose stearate, 1.0% of stearyl alcohol, 4.5% of glyceryl monostearate and 3.0% of jojoba oil are melted in a water bath at 75 ℃ to obtain an oil phase;
dissolving 5.0% glycerol, 5.0% propylene glycol, 0.3% triethanolamine, 0.2% carbomer 2020 and 75.5% purified water in 75 deg.C water bath to obtain water phase; and stirring and mixing the oil phase and the water phase, and emulsifying to obtain the antioxidant and moisturizing comparative cream D2 without a liquid crystal structure.
The content of ophiopogonin and silybum marianum seed oil in the comparison cream is the same as that of the liquid crystal cream C2, and the same basic cream components as those in the comparison cream 1 are adopted, except that the ophiopogonin and the silybum marianum seed oil are not encapsulated by a liquid crystal structure.
4. Skin feel test
The skin feel of the above liquid crystal creams and the comparative creams was tested to compare the skin feel differences of the antioxidant and moisturizing creams without and with the liquid crystal composition of the present invention.
Selecting 20 sensory evaluators, wherein the age is between 20 and 50 years.
I. Preparation of sensory evaluator
(1) The panelists' hands and faces did not use any skin care product for the 5 h prior to the test.
(2) The panelists sat still for 30 min in an environment with humidity of (50. + -.10)% and temperature of (22. + -.1). The time familiar with sensory scoring criteria and evaluation questionnaires. Sensory evaluation scoring criteria are shown in table 2.
II. Sensory evaluation procedure
(1) The evaluator washed the arms and the face with a moderate amount of mild and non-fragrant amino acid facial cleanser, wherein the arms were rinsed for 1 min, the hands were 3cm away from the faucet, and after rinsing, the moisture on the face and the hands was wiped off with a non-fragrant paper towel.
(2) Uniformly entering a sensory evaluation laboratory, and marking the positions 5 cm away from the wrist on the inner sides of the two arms of an evaluator by using caliper positioning plates 5 cm multiplied by 5 cm after 2 min.
(3) After 2 min, the skin care product was started and 0.2 mL of sample was applied to the marked area on the inside of the arm using a syringe (needle removed).
(4) And (3) coating the finger belly in a circling way at the speed of 1-2 r/min, and evaluating and scoring the sensory feeling of the coated sample after 3 circles of coating.
(5) After 11 circles of smearing, paste absorption is promoted by beating, and after absorption, relative performance is evaluated by comparing with a reference sample.
TABLE 2 summary of sensory evaluation indices for cosmetic products
TABLE 3 sensory evaluation record sheet
By plotting a radar chart according to the sensory evaluation results in table 3, it is clear from the skin-feel radar chart in fig. 7 that the comprehensive evaluation of the skin-feel of the antioxidant and moisturizing cream containing the liquid crystal composition of the present invention is better than that containing no liquid crystal composition of the present invention, and has better appearance, spreadability and after-use feel.
Example 16: test for moisture retention
The liquid crystal cream of example 15 and the comparative cream were used as test samples to compare the difference in moisturizing performance between the antioxidant and moisturizing creams containing the liquid crystal composition of the present invention and the liquid crystal composition of the present invention.
The capacitance method is used for measuring the moisture content of the human skin stratum corneum, and is based on the obvious difference of dielectric constants of water and other substances, the capacitance values of the measured skin are different according to the moisture content of the skin stratum corneum, and the parameters can represent the moisture content of the skin.
30 testers are selected, and the test environment temperature is 19.0 ℃ and the test environment humidity is 44.5%. Selecting the part of the left and right arm of the subject 5 cm away from the palm base as the test part with the test area of 3 × 3cm2Test specimenThe sample amount is 0.05 mL, samples are evenly smeared on the inner test parts of the left arm and the right arm of each subject, smearing time is recorded, the moisture content is tested by a skin moisture content tester CM825 produced by Germany CK company for 15 min, 30 min, 1 h, 2 h, 4 h and 6 h after the samples are smeared, the measurement is carried out 3 times in parallel, and an average value is taken. Counting the value of each test part of the tested subject and analyzing the change rule of the moisture content.
As can be seen from FIG. 8, the skin moisture content of the liquid crystal cream is obviously higher than that of the comparative cream within 6 h, which indicates that the cream containing the liquid crystal composition has stronger moisturizing capability and can exert the functions of ophiopogon japonicus polysaccharide and silybum marianum seed oil better than the cream without the liquid crystal composition.
Example 17: test for Oxidation resistance
The liquid crystal cream and the comparative cream in example 15 were used as test samples to conduct an antioxidant effect test.
The method for eliminating DPPH free radicals is used for evaluating the in-vitro antioxidant performance of a sample, when a free radical scavenger exists, the free radical scavenger is paired with electrons of the sample, so that the ultraviolet absorption intensity is weakened or even disappears, and the fading degree is in direct proportion to the quantity of the received electrons. Therefore, the antioxidant activity of the sample can be evaluated by measuring the change in absorbance.
Adding 4.0 mL (0.02 mg/mL) of an absolute ethanol solution of DPPH and 2.0 mL (3 mg/mL) of an absolute ethanol diluent of each test sample into a 10 mL colorimetric tube in sequence, adding absolute ethanol to the scale, uniformly mixing, immediately measuring an absorbance (A) at a wavelength of 517 nm in a 1cm cuvette, marking the absorbance as Ai, measuring the absorbance after storing for 30 min in a dark place at room temperature, marking as Aj, and marking the absorbance as Ac in a contrast test, wherein the absorbance is an ethanol solution only added with DPPH. The radical clearance (K) was calculated as follows:
taking liquid crystal cream and comparison cream as experimental groups, detecting the clearance rate of free radicals, measuring for three times, taking an average value, and obtaining the following test results:
TABLE 4 Oxidation resistance efficacy experiments
Sample (I) | K(%) |
Liquid crystal cream C1 | 75.8 |
Comparative cream D1 | 63.2 |
Liquid crystal cream C2 | 74.3 |
Comparative cream D2 | 61.5 |
As can be seen from table 4, the cream of the antioxidant and moisturizing liquid crystal composition provided by the invention has a high radical scavenging rate, has a more significant effect of resisting radicals than the antioxidant and moisturizing cream without the liquid crystal composition, is increased by more than 12%, and can exert the functions of ophiopogon japonicus polysaccharide and silybum marianum seed oil.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. An antioxidant and moisturizing liquid crystal composition is characterized by comprising 0.01-5% of ophiopogonpolysaccharide, 0.5-15% of silybum marianum seed oil, 1-20% of an emulsifier, 1-20% of a co-emulsifier, 5-35% of liquid grease, 0.01-5% of a thickener, 0.1-10% of a preservative and the balance of water; the emulsifier and the co-emulsifier are combined as follows:
when the emulsifier is cetyl stearyl alcohol, cetyl stearyl glucoside, polyglycerol-3 beeswax ester and hydrogenated lecithin, the auxiliary emulsifier is cetyl stearyl alcohol and behenyl alcohol;
when the emulsifier is steareth-21 and steareth-2, the co-emulsifier is ceteareth-6, PEG-100 stearate and behenyl alcohol.
2. The liquid crystal composition of claim 1, which comprises 0.05-4% of ophiopogonpolysaccharide, 1-12% of silybum marianum seed oil, 3-18% of emulsifier, 2-18% of co-emulsifier, 8-30% of liquid grease, 0.05-4.5% of thickener, 0.2-9% of preservative and the balance of water.
3. The liquid crystal composition of claim 2, which comprises 0.1-2% of ophiopogonpolysaccharide, 2-10% of silybum marianum seed oil, 5-15% of emulsifier, 5-13% of co-emulsifier, 10-25% of liquid grease, 0.1-0.4% of thickener, 1-8% of preservative and the balance of water.
4. The liquid crystal composition according to any one of claims 1 to 3, wherein the liquid oil is one or a mixture of two or more of caprylic/capric glyceride, isopropyl myristate, dimethicone, vitamin E, ethyl oleate, mineral oil, polycyclo-dimethicone, cocoa butter octadecanoate, isononyl isononanoate, isohexadecane, soybean oil, propylene glycol dicaprylate, octyl butanol salicylate, sunflower seed oil, and squalane.
5. The liquid crystal composition according to any one of claims 1 to 3, wherein the thickener is one or a mixture of two or more of xanthan gum, hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer, polyacrylamide/C13-14 isoparaffin/lauryl alcohol ether-7, polyvinylpyrrolidone, hydroxypropyl methylcellulose, polyacrylate crosspolymer-6, gelatin, acacia, and carbomer.
6. The liquid crystal composition of any one of claims 1 to 3, wherein the preservative is one or a mixture of two or more of phenoxyethanol, 1, 2-hexanediol, 1, 2-pentanediol, methylparaben, ethylparaben, ethylhexylglycerin, caprylyl hydroxamic acid, and p-hydroxyacetophenone.
7. A method for producing a liquid crystal composition according to claim 1, comprising:
mixing and stirring silybum marianum seed oil, an emulsifier, an auxiliary emulsifier and liquid oil to obtain a uniform oil phase; mixing and stirring ophiopogonpolysaccharide, a thickening agent and the balance water to obtain a uniform water phase;
the oil phase is rapidly added into the water phase, and the liquid crystal colostrum is obtained after shearing and emulsification treatment;
and cooling the liquid crystal colostrum, adding a preservative, and stirring to obtain the liquid crystal composition.
8. Use of the liquid crystal composition according to any one of claims 1 to 6 or the liquid crystal composition prepared by the preparation method according to claim 7 for preparing daily chemical products.
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