CN113730303B - Method for preparing multiple emulsion by using single type emulsifier and repairing ice crystal cream after sun - Google Patents

Method for preparing multiple emulsion by using single type emulsifier and repairing ice crystal cream after sun Download PDF

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CN113730303B
CN113730303B CN202111096074.6A CN202111096074A CN113730303B CN 113730303 B CN113730303 B CN 113730303B CN 202111096074 A CN202111096074 A CN 202111096074A CN 113730303 B CN113730303 B CN 113730303B
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emulsifier
multiple emulsion
single type
sun
peg
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CN113730303A (en
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李玲玉
孙琦
孙方卉
霍刚
方兆华
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Osmun Biological Co ltd
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Osmun Biological 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
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • 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
    • A61K8/04Dispersions; Emulsions
    • A61K8/06Emulsions
    • A61K8/066Multiple emulsions, e.g. water-in-oil-in-water
    • 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
    • A61K8/37Esters of carboxylic acids
    • 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
    • A61K8/37Esters of carboxylic acids
    • A61K8/375Esters of carboxylic acids the alcohol moiety containing more than one hydroxy group
    • 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
    • A61K8/58Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing atoms other than carbon, hydrogen, halogen, oxygen, nitrogen, sulfur or phosphorus
    • A61K8/585Organosilicon compounds
    • 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
    • A61K8/731Cellulose; Quaternized cellulose derivatives
    • 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
    • A61K8/8141Compositions 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
    • A61K8/8152Homopolymers or copolymers of esters, e.g. (meth)acrylic acid esters; 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
    • A61K8/89Polysiloxanes
    • A61K8/891Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • 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
    • A61K8/89Polysiloxanes
    • A61K8/891Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • A61K8/894Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone modified by a polyoxyalkylene group, e.g. cetyl dimethicone copolyol
    • 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
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/004Aftersun 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
    • A61K2800/52Stabilizers
    • A61K2800/524Preservatives

Abstract

A method for preparing multiple emulsion by using single type emulsifier relates to the technical field of emulsion preparation, which is prepared by mixing main components such as lipophilic emulsifier, emollient, thickener and the like according to a specific proportion. Under the matching use of the components, a special multiple emulsifying system can be formed, and the multiple emulsifying system can achieve good stabilizing effect on the active ingredients added into the internal water phase and keep the active ingredients from deteriorating for a long time. In addition, the embodiment of the invention also provides the after-sun repair ice crystal cream, which is characterized in that the tea extract is added as an active component in the inner water phase of the formed multiple emulsion system, so that the active component in the tea extract is well stabilized under the action of the multiple emulsion system, the effect of the active component is well exerted, and the better after-sun repair effect is achieved.

Description

Method for preparing multiple emulsion by using single type emulsifier and repairing ice crystal cream after sun
Technical Field
The invention relates to the technical field of emulsion preparation, in particular to a method for preparing multiple emulsion by using a single type of emulsifier and repair ice crystal cream after sun.
Background
In the open air in hot summer, even rigorous sun protection can not completely avoid the damage of sunlight. Ultraviolet rays in sunlight can influence the skin cuticle and dermis layers, and the ultraviolet rays generate a large amount of free radicals and active oxygen inside and outside epidermis cells, so that abnormal cell activities are caused, and skin aging is promoted; the barrier function of the skin is weakened after sun drying, the water loss is serious, and the skin is dry and water-deficient; ultraviolet rays induce skin cells to release various inflammatory mediators, excite skin inflammatory reaction, and cause skin stinging, erythema, desquamation and the like; the ultraviolet rays activate tyrosinase expression, so that melanocytes can accelerate synthesis of melanin, and skin pigmentation is caused. Therefore, it is necessary to repair the skin after sun in time. Post-sun repair is mainly performed by several aspects: the antioxidant and the free radical scavenger are used for effectively scavenging and reducing a large amount of free radicals generated by ultraviolet irradiation; calm and relieve the skin, reduce skin irritation, thus relieve the symptoms such as redness, fever, even allergy, inflammation, etc.; repairing skin barrier function and moisturizing; inhibiting tyrosinase activity of melanocyte, and reducing excessive secretion of melanin.
Among the known natural plant extracts, there are a number of natural active ingredients that have a restorative effect on the skin after sun. For example, tea polyphenols are one of the natural active ingredients that have been demonstrated. Specifically, tea polyphenol is a generic name of polyphenols in tea, and comprises flavanols, anthocyanins, flavonoids, flavonols, phenolic acids and the like, and the difference of the ultraviolet light absorption of the tea polyphenol can be utilized to obtain a broad-spectrum sun-proof natural ultraviolet absorbent, so that the tea polyphenol has the effects of reducing the formation of skin melanin and preventing skin aging. The tea extract has remarkable wrinkle formation inhibiting effect, and can inhibit collagenase and elastase, prevent elastin content from decreasing or denaturing, and maintain skin elasticity and wrinkle preventing effect. The tea extract has good effects of resisting aging, resisting oxidation and inhibiting melanin synthesis and transfer in vitro.
However, such natural active ingredients, including tea polyphenols, have a common characteristic of being susceptible to instability by light and heat, not only reducing or even losing activity, but also causing discoloration and off-taste to the product, resulting in limited use. In order to solve the above problems, in the prior art, the stability of the active ingredient is improved by adopting a manner of wrapping ingredients, microcapsules and the like, but the manner is easy to cause unstable emulsifying system of the product or cause that the product is not easy to be uniformly coated on the skin, the requirement on the manufacturing process of the product is high, the manufacturing cost is improved, and the extra added substances of wrapping agents and microcapsule ingredients can cause unnecessary burden to the skin.
Disclosure of Invention
The first object of the present invention is to provide a method for preparing multiple emulsion with a single type of emulsifier, which is simple and convenient to operate, can rapidly and efficiently form multiple emulsion systems, and the obtained multiple emulsion systems have better stability.
The invention provides a crystal frost for repairing after sun-curing, which has scientific formula and reasonable collocation, and can form a special multiple emulsifying system, thereby improving the stability of active ingredients and fully reflecting the sun-curing and repairing capabilities of the active ingredients. In addition, the product has fresh skin feel and good body feel effect.
Embodiments of the present invention are implemented as follows:
a method of preparing a multiple emulsion with a single type of emulsifier comprising:
mixing lipophilic emulsifier and emollient to obtain oil phase;
mixing the oil phase with the inner water phase to obtain a mixed phase;
mixing the mixed phase with an external water phase containing a thickener to obtain a multiple emulsion;
wherein, the use level of the lipophilic emulsifier is 0.5 to 3 weight percent, the use level of the emollient is 3 to 10 weight percent, and the use level of the thickener is 0.1 to 2 weight percent; the lipophilic emulsifier is polyether modified siloxane emulsifier.
An after-sun repair ice crystal cream comprising multiple emulsions prepared according to the above method of preparing multiple emulsions with a single type of emulsifier, wherein 0.01-5 wt% of tea extract is added into the inner aqueous phase of the multiple emulsions.
The embodiment of the invention has the beneficial effects that:
the embodiment of the invention provides a method for preparing multiple emulsion by using a single type of emulsifier, which is prepared by mixing main components such as a lipophilic emulsifier, an emollient, a thickener and the like according to a specific proportion. Under the matching use of the components, a special multiple emulsifying system can be formed, and the multiple emulsifying system can achieve good stabilizing effect on the active ingredients added into the internal water phase and keep the active ingredients from deteriorating for a long time. In addition, the embodiment of the invention also provides the after-sun repair ice crystal cream, which is characterized in that the tea extract is added as an active component in the inner water phase of the formed multiple emulsion system, so that the active component in the tea extract is well stabilized under the action of the multiple emulsion system, the effect of the active component is well exerted, and the better after-sun repair effect is achieved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a comparison of the free radical scavenging effect of the after-sun repair ice cream provided in example 1, example 2 and comparative example 1 of the present invention after 1 day;
FIG. 2 is a comparison of the free radical scavenging effect of the after-sun restoration crystal creams provided in example 1, example 2 and comparative example 1 of the present invention after 30 days;
FIG. 3 is a graph showing the stability test results of the after-sun restoration crystal frost according to example 1 of the present invention;
FIG. 4 is a graph showing the stability test results of the after-sun restoration crystal frost provided in comparative example 1 of the present invention;
FIG. 5 is a graph showing the stability of the after-sun restoration crystal creams provided in example 1 and comparative example 1 of the present invention stored at room temperature for 6 months, wherein the left side of the graph is comparative example 1, and the right side is example 1;
fig. 6 is a photograph of comparative pictures of the after-sun restoration crystal cream provided in example 1 and comparative example 1 of the present invention under a microscope, wherein the left side of the photograph is comparative example 1, and the right side of the photograph is example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The following is a detailed description of a method for preparing multiple emulsions with a single type of emulsifier and repairing ice crystal cream after sun exposure.
Embodiments of the present invention provide a method of preparing multiple emulsions with a single type of emulsifier, comprising:
s1, mixing a lipophilic emulsifier and an emollient to prepare an oil phase;
s2, mixing the oil phase with the inner water phase to prepare a mixed phase;
s3, mixing the mixed phase with an external water phase containing a thickening agent to prepare the multiple emulsion;
wherein the use level of the lipophilic emulsifier is 0.5-3 wt%, the use level of the emollient is 3-10 wt%, and the use level of the thickener is 0.1-2 wt%; the lipophilic emulsifier is polyether modified siloxane emulsifier.
Multiple emulsion systems, generally referred to as water-in-oil-in-water (W/O/W) structures, are composed of an inner aqueous phase, an oil phase and an outer aqueous phase, and are commonly used in the fields of skin care products, cosmetics and the like, and some active substances which can achieve specific functions but have poor stability are wrapped in the inner aqueous phase, so that the protection effect on the active substances can be achieved. In the prior art, the choice of emulsifier as an intermediate reservoir is critical to the formation of multiple emulsion systems. The lipophilic emulsifier and the hydrophilic emulsifier are usually mixed according to a specific proportion to form a stable oil phase, and the requirements on the collocation and proportion of the lipophilic emulsifier and the hydrophilic emulsifier are high, so that the operation difficulty is high for a preparation staff. The method has huge practical value if a method for quickly and stably forming multiple emulsions under a single emulsion system can be developed.
Based on this, the inventors have found through long-term practical work that when an emulsifier common in the prior art is employed, neither a hydrophilic emulsifier nor a lipophilic emulsifier is used alone, but a stable oil layer is not formed. The use of hydrophilic emulsifiers can be dispensed with only in the case of specific concentrations of specific types of lipophilic emulsifiers, i.e. polyether-modified silicone emulsifiers, so that the difficulty in the preparation of multiple emulsion systems is greatly reduced. Meanwhile, the multiple emulsion system obtained by the method can show better stability in the attempt of protecting various active substances, hardly has conflict phenomenon with each active substance, and has better use prospect.
Further, the lipophilic emulsifier comprises at least one of cetyl PEG/PPG-10/1 dimethicone, bis-PEG/PPG-14/14 dimethicone, PEG-3 dimethicone, PEG-10 dimethicone, PEG-9 dimethicone ethyl dimethicone, lauryl PEG-9 dimethicone ethyl dimethicone, and dimethicone/dimethicone PEG-10/15 cross polymer. In the present invention, "not" or "means the ratio of each monomer in the polymer. The polyether modified polysiloxane emulsifier is a commercialized emulsifier and has a wider source.
Optionally, the thickener comprises at least one of polyacrylate crosslinked polymer-6, acrylic acid (ester) based/C10-30 alkanol acrylate crosslinked polymer, acrylic acid (ester)/behenyl alcohol polyether-25 methacrylate copolymer, acrylic acid (ester) based copolymer sodium, sodium polyacrylate, carbomer, sodium acrylate/sodium acryloyldimethyl taurate copolymer, hydroxyethyl cellulose, ammonium acryloyldimethyl taurate/VP copolymer. The thickener is used for increasing the viscosity of the product and keeping the product in a uniform emulsion state. The inventors have found that if some thickener having hydrophilic properties is used in the outer aqueous phase, it can contribute to the stability of the multiple emulsion system. It should be emphasized that the hydrophilic thickener is not equivalent to the hydrophilic emulsifier, which is in a state of dynamic balance on the oil-water interface, but the thickener of the present invention has a certain emulsification effect, but is in an external water phase, and the mechanism of action of the two is not the same, mainly by steric hindrance to stabilize the multiple emulsion system.
The emollient comprises at least one of stearyl heptanoate, cyclopentadimethicone, isononyl isononanoate, caprylic/capric triglyceride, hydrogenated polydecene, isodecyl pivalate, dioctyl carbonate, white pool seed oil, squalane, isopropyl myristate, and dimethicone. Emollients are the major constituent of the oil phase and are also carriers for lipophilic emulsifiers. Meanwhile, the emollient has certain lipophilic property, and can improve the lubrication effect of the product.
In addition, the internal water phase also comprises 4 to 6 weight percent of humectant; the humectant comprises at least one of glycerol, butanediol, 1, 3-propylene glycol, dipropylene glycol, bis-PEG-18 methyl ether dimethyl silane, PEG/PPG-17/6 copolymer, allantoin, betaine, trehalose, panthenol, glycereth-26, polyethylene glycol-32, and PEG/PPG/polytetramethylene glycol-8/5/3 glycerol. The humectant has certain hydrophilic property, can retain moisture, and can improve the moisturizing effect of the product.
The inner water phase/outer water phase also comprises 0.5 to 2 weight percent of preservative; the preservative comprises at least one of p-hydroxyacetophenone, 1, 2-hexanediol, octanediol, glycerol octanoate, and o-cymene-5-ol. The preservative plays a role in inhibiting bacteria in the product, so that the product can be stored for a longer time. When mixing, a small amount of preservative can be mixed into the inner water phase, and a large amount of preservative can be mixed into the outer water phase, so that a better preservative effect can be achieved.
Further, the inner water phase/outer water phase also comprises 0.1 to 0.5 weight percent of auxiliary materials; the auxiliary materials comprise at least one of magnesium sulfate, sodium chloride, triethanolamine and aminomethyl propanol. The auxiliary materials are not essential components in the scheme of the invention, and are mainly used for regulating and controlling the flow property, the uniformity and the like of the product according to the final properties of the product, and the content of the auxiliary materials is preferably not more than 0.5wt percent, otherwise, the stability of the emulsion is influenced.
The embodiment of the invention also provides an after-sun repair ice crystal cream, which comprises multiple emulsion prepared by the method for preparing multiple emulsion by using a single type of emulsifier, wherein 0.01-5 wt% of tea extract is added into an internal water phase of the multiple emulsion.
Optionally, the after-sun repair ice crystal cream comprises, in weight percent:
0.01 to 5 weight percent of tea extract, 0.5 to 3 weight percent of lipophilic emulsifier, 0 to 6 weight percent of humectant, 3 to 10 weight percent of emollient, 0.1 to 2 weight percent of thickener, 0 to 2 weight percent of preservative, 0 to 0.5 weight percent of auxiliary material, 0 to 2 weight percent of skin conditioner and the balance of water.
The tea extract comprises at least one of purple bamboo tea extract, black tea extract, herba Clerodendranthi Spicati extract, tea oil extract, and palmitoyl tea extract. The polyphenols in the tea can be used as natural ultraviolet absorbent to reduce skin melanin formation and prevent skin aging. Meanwhile, the tea extract also has remarkable wrinkle formation inhibiting effect, has inhibiting effect on collagenase and elastase, can prevent elastin content from decreasing or denaturing, and maintains skin elasticity and wrinkle preventing effect. The tea extract has good effects of resisting aging, resisting oxidation and inhibiting melanin synthesis and transfer in vitro.
Optionally, the tea extract of the present invention is prepared by extracting tea leaves with water, organic solvent or supercritical CO 2 Extracting to obtain liquid or solid component. Wherein the tea polyphenol content of the tea extract is 5-10wt%. Proper content of tea polyphenol is a guarantee for realizing the repairing effect of the product. When the tea extract prepared by self-extraction is adoptedWhen taking the material, the tea polyphenol content is relatively low, so that the usage amount can be properly increased to 1-5wt% when the material is used for repairing ice crystal cream after sun drying in order to ensure the effect, and the production cost is low. In addition, commercial tea extracts or even pure tea polyphenols can be used, in which case the amount of tea extract in the after-sun restoration crystal cream can be reduced to below 1wt% and even to 0.01wt% in the case of pure tea polyphenols.
In addition, the invention also finds another benefit in formulating the post-sun repair ice cream with one such multiple emulsion system. The advantage of this multiple emulsion system is even more pronounced in the case of no addition of active ingredient or of the addition of the majority of the other active ingredients, and the use of hydrophilic emulsifiers can be dispensed with for the simplification of the operating process. However, when adding tea extract, the inventors found that if a mixed system of a lipophilic emulsifier and a hydrophilic emulsifier is used, a stable oil layer cannot be formed, and even if too many hydrophilic groups exist in the lipophilic emulsifier, the stability of the oil layer is deteriorated. Only polyether modified polysiloxane type emulsifier with proper hydrophobic effect and hydrophilic effect can form stable oil layer. The reason for this is probably because a large amount of phenolic hydroxyl groups in the tea polyphenols and hydrophilic groups in the emulsifier have strong hydrogen bonding action, and the action force damages the stability of the oil layer. Meanwhile, the hydrogen bonding effect also has a certain influence on the repairing effect of the tea polyphenol. It is anticipated that similar effects may exist when other polyhydroxy actives are employed. On this basis, the inventors have further found that when the mass ratio of tea extract to lipophilic emulsifier is 1:0.7 to 0.9, and the obtained product has better stability.
Optionally, the oil/inner water phase further comprises 0.1 to 2wt% of a skin conditioning agent; the skin conditioner comprises at least one of pearl extract, 4-tert-butylcyclohexanol, menthol lactate, bisabolol, and rhizoma Zingiberis recens root extract. Skin conditioning agents are not essential ingredients of the present regimen, and are primarily used to introduce additional skin care benefits into the product, such as whitening, spot-lightening, cooling, anti-inflammatory, soothing, etc. The amount of skin conditioning agent is preferably not too much, preferably not more than 2% by weight, and may be selected to be incorporated into the internal aqueous or oil phase depending on the particular hydrophobic and hydrophilic properties of the skin conditioning agent selected for use.
The preparation method of the after-sun repair crystal cream can be carried out in the following way:
s1, mixing a lipophilic emulsifier, an emollient and a skin conditioner to obtain a mixed component A, namely an oil phase;
s2, mixing the tea extract, the humectant, part of auxiliary materials and part of preservative to obtain a mixed component B, namely an inner water phase;
s3, mixing the thickener, the humectant, the rest auxiliary materials and the rest preservative to obtain a mixed component C, namely an external water phase;
s4, uniformly mixing the mixed component A and the mixed component B to obtain a mixed component AB, namely a mixed phase;
s5, mixing the mixed component AB with the mixed component C to obtain the composite material.
The steps S1 to S3 are not strictly limited in order, and may be performed simultaneously or separately.
In step S4, the mixed component B may be optionally added slowly to the mixed component a, with sufficient stirring to form a stable water-in-oil (W/O) structure. The mixed component AB was then added to the mixed component C, and a W/O/W multiple emulsified structure was formed with sufficient stirring.
The features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
The embodiment provides a repair crystal cream after sun, the composition of which is shown in the following table:
the preparation method comprises the following steps:
s1, mixing a lipophilic emulsifier, an emollient and a skin conditioner to obtain a mixed component A;
s2, mixing the tea extract, the humectant, part of auxiliary materials and part of preservative to obtain a mixed component B;
s3, mixing the thickener, the humectant, the rest auxiliary materials and the rest preservative to obtain a mixed component C;
s4, uniformly mixing the mixed component A and the mixed component B to obtain a mixed component AB;
s5, mixing the mixed component AB with the mixed component C.
Example 2
The embodiment provides a repair crystal cream after sun, the composition of which is shown in the following table:
the preparation method is described in example 1.
Example 3
The embodiment provides a repair crystal cream after sun, the composition of which is shown in the following table:
the preparation method is described in example 1.
Example 4
The embodiment provides a repair crystal cream after sun, the composition of which is shown in the following table:
the preparation method is described in example 1.
Example 5
The embodiment provides a repair crystal cream after sun, the composition of which is shown in the following table:
the preparation method is described in example 1.
Example 6
This example provides a method for preparing multiple emulsions with a single type of emulsifier using the following materials:
the preparation method is described in example 1, wherein the tea extract is replaced with water of equal quality.
The multiple emulsion obtained by the method is stored for 6 months at room temperature, does not change color or deteriorate, and still presents stable emulsion morphology.
Example 7
This example provides a method for preparing multiple emulsions with a single type of emulsifier using the following materials:
the preparation method is described in example 1, wherein the tea extract is replaced by equivalent amount of bamboo extract.
The multiple emulsion obtained by the method is stored for 6 months at room temperature, does not change color or deteriorate, and still presents stable emulsion morphology. It is shown that the addition of the active ingredient (bamboo extract) does not destroy the stability of the multiple emulsion.
Comparative example 1
This comparative example provides an after sun repair ice cream having substantially the same main ingredients and preparation as in example 1, except that the emulsifier is replaced by cetyl PEG/PPG-10/1 polydimethylsiloxane with glyceryl stearate/PEG-100 stearate.
Comparative example 2
This comparative example provides an after sun repair ice cream having essentially the same principal ingredients and preparation as in example 1, except that the emulsifier is replaced by sorbitan isostearate by cetyl PEG/PPG-10/1 polydimethylsiloxane.
Comparative example 3
The present comparative example provides an after-sun repair ice cream having substantially the same main components and preparation method as in example 1, except that the content of the extract of purple bamboo tea was increased to 10wt% and the content of the lipophilic emulsifier was increased to 6wt%.
Comparative example 4
This comparative example provides an after-sun repair ice cream having substantially the same main ingredients and preparation method as in example 1, except that the amount of humectant was reduced to 2wt% and the amount of emollient was reduced to 2wt%.
Test example 1
The test examples were prepared by using the after-sun repair ice crystal creams provided in examples 1 to 5 and comparative examples 1 to 4, and the radical scavenging effect was tested, and each test sample was tested 2 times, and after 1 day of sample storage, and after 30 days of sample storage, respectively. The specific method for testing is as follows:
the test samples were prepared into solutions with concentrations of 0.01%, 0.1%, 1% and 10%, respectively, and DPPH radical scavenging experiments were performed, and the test results are shown in Table 1.
TABLE 1 free radical scavenging Effect test results
As can be seen from Table 1, the after-sun repair ice crystal cream provided in examples 1 to 5 of the present invention has a small difference between the effect of scavenging free radicals after 1 day of storage and the effect of scavenging free radicals after 30 days of storage, which indicates that the ice crystal cream has better stability. In comparative example 1, after the emulsifier is replaced by the lipophilic emulsifier with hydrophilic groups, the effect of scavenging free radicals after 1 day is obviously reduced compared with the embodiment of the invention, the emulsifying system is stable, the active ingredients of the tea extract are not damaged by illumination, heat and other conditions, and the effect of the hydrophilic groups of the emulsifier on the activity of the tea extract can be reasonably estimated (example 1vs, example 2vs, comparative example 1 can be seen in the attached figures 1-2). Comparative example 2, in which the emulsifier was replaced with a hydrophilic emulsifier, failed to form a stable emulsion system, the active material was largely destroyed after 1 day, which exhibited significantly poorer free radical scavenging effect than comparative example 1, and after 30 days, substantially no active material remained. Comparative examples 3 and 4, which changed the amounts of tea extract/emulsifier, emollient/humectant, respectively, still formed an emulsified system, it was seen that the effect of scavenging free radicals was not much worse than in the examples after 1 day of testing (also demonstrated that the hydrophilic groups in comparative example 1 did have an effect on the activity of the tea extract), but thus the emulsified system was unstable in the long term and the effect of scavenging free radicals was greatly reduced in the 30 day after testing.
It should be noted that the restoration of skin by tea extract is mainly dependent on its antioxidant capacity, i.e. its scavenging effect on free radicals. Therefore, the effect of the product on repairing the skin after sun exposure can be reflected to a certain extent by testing the free radical scavenging effect of the product.
Test example 2
The test example adopts the after-sun repair ice crystal cream prepared in the example 1 and the comparative example 1, and the stability test of light shading, heat resistance, low temperature, illumination and the like at normal temperature is carried out on the ice crystal cream.
Wherein, the heat-resistant test conditions are: 45+/-1 ℃ and keeping the temperature away from light. The illumination test conditions are as follows: illumination constant temperature and humidity test box (1.47 x 10) 6 Lux·hr). The low-temperature performance test conditions are as follows: 4+/-1 ℃ and keeping the temperature away from light. The test results are shown in FIGS. 3 to 4.
The tea extract is stable under low temperature, and has serious discoloration under normal temperature light-proof and illumination conditions, and the most serious discoloration under heat-resistant conditions. As can be seen from fig. 3 and 4, the color change degree of the after-sun repair ice crystal cream a prepared in example 1 is obviously lower than that of the common cream prepared in comparative example 1 under the same treatment conditions, which shows that the technical scheme of the invention greatly reduces the color change degree of the tea extract and has better product stability. In addition, fig. 5 shows a comparison of example 1 with comparative example 1 after 6 months of storage at room temperature, and it can also be seen that the after-sun repair ice crystal cream of comparative example 1 shows a significant discoloration (see left graph in fig. 5), while the after-sun repair ice crystal cream of example 1 shows a better stability (see right graph in fig. 5).
Test example 3
The post-sun repair ice crystal creams prepared in example 1 and comparative example 1 were taken under a microscope (see fig. 6), and it can be seen from the figure that the post-sun repair ice crystal cream provided in example 1 of the present application is uniform and glossy under the microscope, and has a large number of multiple emulsion structures (see right diagram in fig. 6), whereas the post-sun repair ice crystal cream prepared in comparative example 1 is darker in color and less obvious in multiple emulsion phenomenon.
In summary, the embodiment of the invention provides a method for preparing multiple emulsion by using a single type of emulsifier, which is prepared by mixing main components such as lipophilic emulsifier, emollient, thickener and the like according to a specific proportion. Under the matching use of the components, a special multiple emulsifying system can be formed, and the multiple emulsifying system can achieve good stabilizing effect on the active ingredients added into the internal water phase and keep the active ingredients from deteriorating for a long time. In addition, the embodiment of the invention also provides the after-sun repair ice crystal cream, which is characterized in that the tea extract is added as an active component in the inner water phase of the formed multiple emulsion system, so that the active component in the tea extract is well stabilized under the action of the multiple emulsion system, the effect of the active component is well exerted, and the better after-sun repair effect is achieved.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A method of preparing a multiple emulsion with a single type of emulsifier comprising:
mixing lipophilic emulsifier and emollient to obtain oil phase; the oil phase is free of thickener;
mixing the oil phase with the inner water phase to prepare a mixed phase;
mixing the mixed phase with an external water phase comprising a thickener to produce the multiple emulsion;
wherein the dosage of the lipophilic emulsifier is 0.5-wt% -3-wt%, the dosage of the emollient is 3-wt% -10 wt%, and the dosage of the thickener is 0.1-wt% -2-wt%;
the lipophilic emulsifier is at least one of cetyl PEG/PPG-10/1 polydimethylsiloxane, bis-PEG/PPG-14/14 polydimethylsiloxane, PEG-3 polydimethylsiloxane, PEG-10 polydimethylsiloxane and polydimethylsiloxane PEG-10/15 crosslinked polymer;
the thickener is at least one of polyacrylate crosslinked polymer-6, acrylic acid (ester)/C10-30 alkanol acrylate crosslinked polymer, acrylic acid (ester)/behenyl alcohol polyether-25 methacrylate copolymer, acrylic acid (ester) copolymer sodium, sodium polyacrylate, carbomer, sodium acrylate/sodium acryloyldimethyl taurate copolymer, hydroxyethyl cellulose and acryloyldimethyl taurate ammonium/VP copolymer;
the emollient is at least one of stearyl heptanoate, cyclopentadimethicone, isononyl isononanoate, caprylic/capric triglyceride, hydrogenated polydecene, isodecyl pivalate, dioctyl carbonate, white pool seed oil, squalane, isopropyl myristate, and dimethicone.
2. The method of preparing a multiple emulsion with a single type of emulsifier of claim 1 wherein the inner aqueous phase further comprises 4wt% -6 wt% humectant; the humectant is at least one of glycerin, butanediol, 1, 3-propylene glycol, dipropylene glycol, di-PEG-18 methyl ether dimethyl silane, PEG/PPG-17/6 copolymer, allantoin, betaine, trehalose, panthenol, glycerin polyether-26, polyethylene glycol-32, and PEG/PPG/polybutylene glycol-8/5/3 glycerin.
3. The method of preparing a multiple emulsion with a single type of emulsifier according to claim 1, wherein the internal aqueous phase further comprises 0.5wt% -2 wt% preservative; the preservative is at least one of p-hydroxyacetophenone, 1, 2-hexanediol/octanediol, glycerol caprylate and o-cymene-5-ol.
4. The method of preparing a multiple emulsion with a single type of emulsifier according to claim 1, wherein the outer aqueous phase further comprises 0.5wt% -2 wt% preservative; the preservative is at least one of p-hydroxyacetophenone, 1, 2-hexanediol/octanediol, glycerol caprylate and o-cymene-5-ol.
5. The method of preparing multiple emulsions with a single type of emulsifier according to claim 1, wherein the inner aqueous phase further comprises 0.1% -wt% to 0.5% -wt% of adjuvants; the auxiliary materials are at least one of magnesium sulfate, sodium chloride, triethanolamine and aminomethyl propanol/water.
6. The method of preparing multiple emulsions with a single type of emulsifier according to claim 1, wherein the outer aqueous phase further comprises 0.1% -wt% to 0.5% -wt% of adjuvants; the auxiliary materials are at least one of magnesium sulfate, sodium chloride, triethanolamine and aminomethyl propanol/water.
7. The after-sun repair crystal cream is characterized by comprising multiple emulsion prepared by the method for preparing multiple emulsion by using a single type of emulsifier according to any one of claims 1-6, wherein 0.01wt% -5 wt% of tea extract is added into an inner water phase of the multiple emulsion.
8. The after sun repair ice cream of claim 7, wherein the tea extract comprises at least one of a purple bamboo shoot tea extract, a black tea extract, a clerodendranthus spicatus extract, a camellia oleifera extract, and a palmitoyl tea extract.
9. The after-sun repair ice cream of claim 7, wherein the oil phase further comprises 0.1wt% to 2wt% of a skin conditioning agent; the skin conditioner comprises at least one of pearl extract, 4-tert-butylcyclohexanol, menthol lactate, bisabolol, and ginger root extract.
10. The after-sun repair ice cream of claim 7, wherein the inner aqueous phase further comprises 0.1wt% to 2wt% of a skin conditioning agent; the skin conditioner comprises at least one of pearl extract, 4-tert-butylcyclohexanol, menthol lactate, bisabolol, and ginger root extract.
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