CN113730303A - Method for preparing multiple emulsions by using single type emulsifier and ice crystal cream for repairing after-sun - Google Patents

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

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CN113730303A
CN113730303A CN202111096074.6A CN202111096074A CN113730303A CN 113730303 A CN113730303 A CN 113730303A CN 202111096074 A CN202111096074 A CN 202111096074A CN 113730303 A CN113730303 A CN 113730303A
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emulsifier
peg
single type
tea extract
dimethicone
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CN113730303B (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 emulsions by using a single type of emulsifier relates to the technical field of emulsion preparation, and 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 emulsification system can be formed, and the multiple emulsification system can achieve good stabilizing effect on the active components added into the internal water phase and keep the active components from deteriorating for a long time. In addition, the embodiment of the invention also provides the after-sun repair ice cream, which is characterized in that the tea extract is added into the internal water phase of the formed multiple emulsion system to serve as an active component, so that under the action of the multiple emulsion system, the active component in the tea extract is well stabilized, the effect of the active component is fully exerted, and a better after-sun repair effect is achieved.

Description

Method for preparing multiple emulsions by using single type emulsifier and ice crystal cream for repairing after-sun
Technical Field
The invention relates to the technical field of emulsion preparation, in particular to a method for preparing multiple emulsions by using a single type emulsifier and a post-basking repair ice crystal cream.
Background
In hot summer outdoors, even if the sun is strictly protected, the damage of sunlight cannot be completely avoided. Ultraviolet rays in sunlight can affect the stratum corneum and the dermis of skin, and the ultraviolet rays generate a large amount of free radicals and active oxygen inside and outside epidermal cells to cause abnormal cell activities and promote skin aging; after the sun is dried, the barrier function of the skin is weakened, the water loss is serious, and the skin is dry and lacks water; ultraviolet rays induce skin cells to release various inflammatory mediators, so that inflammatory reaction of the skin is stimulated, and phenomena of skin stabbing pain, erythema, desquamation and the like appear; ultraviolet light activates tyrosinase expression, which accelerates the synthesis of melanin by melanocytes, causing skin pigmentation. Therefore, it is very necessary to repair the skin after sunburn in time. Post-basking repair is mainly performed by several aspects: a large amount of free radicals generated by ultraviolet irradiation are effectively eliminated and reduced through an antioxidant and a free radical scavenger; calming and relieving skin, and reducing skin irritation, thereby relieving symptoms such as skin redness, fever, 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 many natural active ingredients having a repairing effect on the skin after sunburn. For example, tea polyphenols are one of the natural active ingredients that have been identified. Specifically, tea polyphenol is a general term of polyphenol substances in tea, comprises flavanols, anthocyanins, flavonoids, flavonols, phenolic acids and the like, and can be used for obtaining a broad-spectrum sunscreen natural ultraviolet absorbent by utilizing the difference of the absorption of ultraviolet regions, thereby having the effects of reducing the formation of skin melanin and preventing skin aging. The tea extract has remarkable wrinkle formation inhibiting effect, and has collagenase and elastase inhibiting effect, and can prevent elastin content from decreasing or denaturing, and maintain skin elasticity and wrinkle resistance. The tea extract has good effects of resisting aging and oxidation, and inhibiting melanin synthesis and transfer in vitro.
However, such natural active ingredients including tea polyphenol have a common characteristic of being easily affected by light and heat and unstable, so that not only is the activity reduced and even lost, but also the product is discolored and smells, and the application of the natural active ingredients is limited. In order to solve the problems, the prior art mostly adopts a coating component, a microcapsule and the like to improve the stability of the active component, but the method easily causes the instability of an emulsion system of the product or causes the product not to be easily and uniformly coated on the skin, has high requirements on the product manufacturing process and increases the manufacturing cost, and the extra substances such as the coating agent and the microcapsule component also cause unnecessary burden on the skin.
Disclosure of Invention
The first objective of the present invention is to provide a method for preparing multiple emulsions with a single type of emulsifier, which is simple and convenient to operate, can rapidly and efficiently form multiple emulsion systems, and can obtain multiple emulsion systems with better stability.
The second purpose of the invention is to provide the after-sun repair ice cream which is scientific in formula, reasonable in collocation and capable of forming a special multiple emulsification system, so that the stability of active ingredients is improved, and the sun-proof repair capability of the active ingredients is fully embodied. In addition, the product has fresh skin feeling and good body feeling effect.
The embodiment of the invention is realized by the following steps:
a method of preparing multiple emulsions with a single type of emulsifier comprising:
mixing lipophilic emulsifier and emollient to obtain oil phase;
mixing the oil phase and the internal water phase to obtain a mixed phase;
mixing the mixed phase with an external water phase containing a thickening agent to prepare a multiple emulsion;
wherein, the dosage of the lipophilic emulsifier is 0.5 to 3 weight percent, the dosage of the emollient is 3 to 10 weight percent, and the dosage of the thickener is 0.1 to 2 weight percent; the lipophilic emulsifier is polyether modified siloxane emulsifier.
A post-basking repair ice cream comprising a multiple emulsion prepared according to the above method for preparing multiple emulsions with a single type of emulsifier, wherein 0.01-5 wt% of tea extract is added to an internal aqueous phase of the multiple emulsion.
The embodiment of the invention has the beneficial effects that:
the embodiment of the invention provides a method for preparing multiple emulsions 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 ratio. Under the matching use of the components, a special multiple emulsification system can be formed, and the multiple emulsification system can achieve good stabilizing effect on the active components added into the internal water phase and keep the active components from deteriorating for a long time. In addition, the embodiment of the invention also provides the after-sun repair ice cream, which is characterized in that the tea extract is added into the internal water phase of the formed multiple emulsion system to serve as an active component, so that under the action of the multiple emulsion system, the active component in the tea extract is well stabilized, the effect of the active component is fully exerted, and a 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 needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a comparison of the radical scavenging effect of the post-basking repair cryocreams provided in examples 1 and 2 of the present invention and comparative example 1 after 1 day;
FIG. 2 is a comparison of the radical scavenging effect of the after-sun repair ice creams provided by 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 repair ice cream provided in example 1 of the present invention;
FIG. 4 is a graph showing the results of a stability test of the post-basking repair ice cream provided in comparative example 1 of the present invention;
FIG. 5 is a graph comparing the stability of the post-basking repair ice creams provided in example 1 of the present invention and comparative example 1 stored at room temperature for 6 months, wherein comparative example 1 is on the left and example 1 is on the right;
FIG. 6 is a photograph under a microscope comparing photographs of the post-basking repair ice creams provided by example 1 and comparative example 1 of the present invention, wherein the left side of the drawing is comparative example 1 and the right side is example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following is a detailed description of a method of preparing multiple emulsions with a single type of emulsifier and a post-basking repair ice cream according to embodiments of the present invention.
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 internal 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 dosage of the lipophilic emulsifier is 0.5-3 wt%, the dosage of the emollient is 3-10 wt%, and the dosage of the thickener is 0.1-2 wt%; the lipophilic emulsifier is polyether modified siloxane emulsifier.
The multiple emulsification system generally refers to a water-in-oil-in-water (W/O/W) structure, which consists of an inner water phase, an oil phase and an outer water phase, and is commonly used in the fields of skin care products, cosmetics and the like, and active substances which can realize specific functions but have poor stability are wrapped in the inner water phase, so that the protection effect on the active substances can be achieved. In the prior art, the selection of an emulsifier as the intermediate oil layer is critical to the formation of multiple emulsion systems. The lipophilic emulsifier and the hydrophilic emulsifier are usually required to be mixed according to a specific ratio for use to form a stable oil phase, and the requirements on the matching and the ratio of the lipophilic emulsifier and the hydrophilic emulsifier are high, so that the operation difficulty is high for a formulator. It would be of great practical value if a method could be developed for the rapid and stable formation of multiple emulsions in a single emulsion system.
Based on this, the inventors have found through long-term practical work that when emulsifiers commonly used in the prior art are used, neither hydrophilic emulsifiers nor lipophilic emulsifiers are used alone, and a stable oil layer cannot be formed. Only under the condition of adopting a specific kind of lipophilic emulsifier with specific concentration, namely polyether modified siloxane emulsifier, the use of hydrophilic emulsifier can be omitted, thereby greatly reducing the preparation difficulty of a multiple emulsification system. Meanwhile, the multiple emulsification system obtained by the method can show better stability in the attempt of protecting various active substances, almost has no conflict phenomenon with each active substance, and has better application 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 dimethiconoethyl dimethicone, lauryl PEG-9 dimethiconoethyl dimethicone, and dimethicone/dimethicone PEG-10/15 crosspolymer. In the present invention, "/" does not mean "or", and indicates the ratio of each monomer in the polymer. The various polyether modified polysiloxane emulsifiers are commercialized emulsifiers and have wide sources.
Optionally, the thickener comprises at least one of polyacrylate crosspolymer-6, acrylic acid/C10-30 alkanol acrylate crosspolymer, acrylic acid/beheneth-25 methacrylate copolymer, sodium acrylic acid copolymer, sodium polyacrylate, carbomer, sodium acrylate/sodium acryloyldimethyl taurate copolymer, hydroxyethyl cellulose, ammonium acryloyldimethyl taurate/VP copolymer. The thickener is used to increase the viscosity of the product and maintain the product in a uniform emulsion state. The inventors have found that the stability of multiple emulsion systems can be promoted by using thickeners with hydrophilic properties in the external aqueous phase. It is emphasized that the thickener with hydrophilic property is not equal to the hydrophilic emulsifier, which is in a dynamic equilibrium state at the interface of oil and water, but the thickener of the present invention has a certain emulsification effect, but is in an external water phase, and mainly stabilizes the multiple emulsion system through steric hindrance, and the two have different mechanisms of action.
The emollient comprises at least one of stearyl heptanoate, cyclopentyldimethicone, isononyl isononanoate, caprylic/capric triglyceride, hydrogenated polydecene, isodecyl pivalate, dioctyl carbonate, meadowfoam seed oil, squalane, isopropyl myristate, and dimethicone. Emollients are the main constituents of the oil phase and are also carriers for lipophilic emulsifiers. Meanwhile, the emollient has certain lipophilic property, and can improve the lubricating 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 glycerin, butylene glycol, 1, 3-propylene glycol, dipropylene glycol, bis-PEG-18 methyl ether dimethylsilane, PEG/PPG-17/6 copolymer, allantoin, betaine, trehalose, panthenol, glyceryl polyether-26, polyethylene glycol-32, and PEG/PPG/polytetramethylene glycol-8/5/3 glycerin. The humectant has certain hydrophilic property, can retain water, and improves the moisturizing effect of the product.
The inner water phase/the outer water phase also comprises 0.5 to 2 weight percent of preservative; the antiseptic comprises at least one of p-hydroxyacetophenone, phenoxyethanol, 1, 2-hexanediol, caprylic glycol, glyceryl caprylate, and o-cymene-5-ol. The preservative plays a bacteriostatic role in the product, so that the product can be stored for a longer time. During mixing, a small amount of preservative can be mixed into the inner water phase, and a large amount of preservative is mixed into the outer water phase, so that a better preservative effect is achieved.
Furthermore, the inner water phase/the outer water phase also comprises 0.1 wt% -0.5 wt% of auxiliary materials; the adjuvants include at least one of magnesium sulfate, sodium chloride, triethanolamine, and aminomethyl propanol. The auxiliary materials are not essential components of the scheme of the invention, 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 0.5 wt%, otherwise, the auxiliary materials can influence the stability of the emulsion.
The embodiment of the invention also provides a post-basking repair ice crystal cream, which comprises multiple emulsion prepared by the method for preparing multiple emulsion by using the single type emulsifier, wherein 0.01-5 wt% of tea extract is added into the internal water phase of the multiple emulsion.
Optionally, the post-basking repair ice cream comprises, in weight percent:
0.01-5 wt% of tea extract, 0.5-3 wt% of lipophilic emulsifier, 0-6 wt% of humectant, 3-10 wt% of emollient, 0.1-2 wt% of thickener, 0-2 wt% of preservative, 0-0.5 wt% of auxiliary material, 0-2 wt% of skin conditioner and the balance of water.
The tea extract comprises at least one of Zisun bamboo shoot tea extract, black tea extract, Clerodendranthus spicatus extract, Camellia oleifera extract, and palmitoyl tea extract. The polyphenol substances in the tea can be used as natural ultraviolet absorbent, and can reduce the formation of skin melanin and prevent skin aging. Meanwhile, the tea extract also has the effects of remarkably inhibiting wrinkle formation, inhibiting collagenase and elastase, preventing the content reduction or denaturation of elastin, and maintaining skin elasticity and anti-wrinkle effect. The tea extract has good effects of resisting aging and oxidation, and inhibiting melanin synthesis and transfer in vitro.
Optionally, the tea extract of the invention is obtained by subjecting tea leaves to water extraction, organic solvent extraction or supercritical CO extraction2Extracting the obtained liquid or solid component. Wherein the tea polyphenol content of the tea extract is 5 wt% -10 wt%. The tea polyphenol with proper content is the guarantee for realizing the product repairing effect. It should be noted that, when the tea extract prepared by the above self-extraction is adopted, because the content of tea polyphenol is relatively low, in order to ensure the effect, the dosage can be properly increased to 1 wt% -5 wt% when the tea extract is used for repairing ice cream after being dried, which has the advantage of low production cost. Furthermore, commercially available tea extracts may be used, even pure tea polyphenols, in which case the amount of tea extract in the post-sun repair ice cream may be reduced to below 1 wt%, or even up to 0.01 wt% in the case of pure tea polyphenols.
In addition, the invention has found another benefit of the multiple emulsion system in formulating the post-basking repair cryocream. The advantage of the multiple emulsion system is further increased by the simplification of the process, which can be achieved without the use of hydrophilic emulsifiers, in the case of no or most of the other active ingredients. When the tea extract is added, the inventor finds that a stable oil layer cannot be formed if a mixed system of a lipophilic emulsifier and a hydrophilic emulsifier is adopted, 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 emulsifiers with appropriate hydrophobic and hydrophilic effects can form a 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 breaks the stability of the oil layer. Meanwhile, the hydrogen bonding effect also has certain influence on the repair effect of the tea polyphenol. It is anticipated that similar effects may exist when other polyhydroxy actives are employed. On the basis, the inventor further finds that when the mass ratio of the tea extract to the lipophilic emulsifier is 1: 0.7-0.9, the obtained product has better stability.
Optionally, the oil phase/internal water phase also comprises 0.1-2 wt% of skin conditioning agent; the skin conditioner comprises at least one of Margarita extract, 4-tert-butylcyclohexanol, menthol lactate, bisabolol, and ginger root extract. Skin conditioners are not essential ingredients of the present regimen and are primarily used to introduce additional skin care benefits in the product, such as whitening, lightening, cooling, anti-inflammatory, soothing, etc. The skin conditioning agent is also preferably used in an amount of not more than about 2% by weight, and may be optionally blended into the internal aqueous phase or the oil phase at the time of use, depending on the particular hydrophobic and hydrophilic properties of the selected skin conditioning agent.
The preparation method of the ice crystal cream for repairing after sun exposure can be carried out by adopting the following steps:
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 the auxiliary materials and part of the preservative to obtain a mixed component B, namely an internal water phase;
s3, mixing the thickening agent, 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;
and 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, mixing component B may be added slowly to mixing component a, optionally with sufficient agitation to form a stable water-in-oil (W/O) structure. Subsequently, the mixed component AB is added to the mixed component C, and under sufficient stirring, a multiple emulsified structure of W/O/W is formed.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a after-sun repair ice cream, which comprises the following components in percentage by weight:
Figure BDA0003268698330000111
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 the auxiliary materials and part of the preservative to obtain a mixed component B;
s3, mixing the thickening agent, 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;
and S5, mixing the mixed component AB with the mixed component C.
Example 2
The embodiment provides a after-sun repair ice cream, which comprises the following components in percentage by weight:
Figure BDA0003268698330000121
Figure BDA0003268698330000131
the preparation process is as in example 1.
Example 3
The embodiment provides a after-sun repair ice cream, which comprises the following components in percentage by weight:
Figure BDA0003268698330000132
the preparation process is as in example 1.
Example 4
The embodiment provides a after-sun repair ice cream, which comprises the following components in percentage by weight:
Figure BDA0003268698330000141
the preparation process is as in example 1.
Example 5
The embodiment provides a after-sun repair ice cream, which comprises the following components in percentage by weight:
Figure BDA0003268698330000142
Figure BDA0003268698330000151
the preparation process is as in example 1.
Example 6
This example provides a method for preparing multiple emulsions with a single type of emulsifier using the following raw materials as shown in the table:
Figure BDA0003268698330000152
the preparation method was carried out by replacing the tea extract with water of equal mass, according to example 1.
The multiple emulsion obtained by the method is stored at room temperature for 6 months, does not change color or deteriorate, and still presents a stable emulsion form.
Example 7
This example provides a method for preparing multiple emulsions with a single type of emulsifier using the following raw materials as shown in the table:
Figure BDA0003268698330000161
the preparation method was carried out by replacing the tea extract with an equal amount of bamboo extract, according to example 1.
The multiple emulsion obtained by the method is stored at room temperature for 6 months, does not change color or deteriorate, and still presents a stable emulsion form. It is stated 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 a post-basking repair ice cream having the main ingredients and preparation method substantially the same as example 1, except that the emulsifier was replaced with cetyl PEG/PPG-10/1 dimethicone by glyceryl stearate/PEG-100 stearate.
Comparative example 2
This comparative example provides a post-basking repair ice cream having essentially the same main ingredients and preparation method as in example 1, except that the emulsifier was replaced by sorbitan isostearate from cetyl PEG/PPG-10/1 dimethicone.
Comparative example 3
This comparative example provides a post-basking repair ice cream having the main components and preparation method substantially the same as example 1, except that the content of the purple bamboo shoot tea extract was increased to 10 wt%, and the content of the lipophilic emulsifier was increased to 6 wt%.
Comparative example 4
This comparative example provides a post-basking repair ice cream having the main components and preparation method substantially the same as example 1, except that the amount of humectant was reduced to 2 wt% and the amount of emollient was reduced to 2 wt%.
Test example 1
In the experimental example, the after-sun repair ice cream provided in examples 1 to 5 and comparative examples 1 to 4 was used to test the free radical scavenging effect, and each experimental sample was tested 2 times, and the samples were respectively stored for 1 day and sampled and tested 30 days later. The specific method of testing is as follows:
samples to be tested are respectively prepared into solutions to be tested with the concentrations of 0.01%, 0.1%, 1% and 10% to be subjected to DPPH free radical scavenging experiments, and the test results are shown in Table 1.
TABLE 1 free radical scavenging Effect test results
Figure BDA0003268698330000181
As can be seen from table 1, the effects of removing free radicals after 1 day of storage and 30 days of storage of the ice cream repaired after sun exposure provided in embodiments 1 to 5 of the present invention are not very different, which indicates that the ice cream has better stability. In contrast, 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 that in the embodiment of the invention, the emulsifying system is relatively stable, the active ingredients of the tea extract are not damaged by light, heat and other conditions, and the hydrophilic groups of the emulsifier can be reasonably presumed to have certain influence on the activity of the tea extract (in example 1vs, example 2vs, comparative example 1 can be seen in attached figures 1-2). Comparative example 2 replacement of the emulsifier with a hydrophilic emulsifier failed to form a stable emulsion system, and after 1 day the active substance was largely destroyed, which exhibited a radical scavenging effect significantly worse than comparative example 1, and after 30 days, substantially no active substance remained. Comparative example 3 and comparative example 4, which changed the amounts of tea extract/emulsifier, emollient/humectant, respectively, still allowed the formation of an emulsified system, it can be seen that the scavenging effect of free radicals was not much inferior to that of the examples after 1 day of testing (it is also demonstrated that the hydrophilic group in comparative example 1 indeed has an effect on the activity of tea extract), but the emulsified system was not stable in the long term and the scavenging effect of free radicals was greatly reduced after 30 days of testing.
It should be noted that the repair of skin by tea extract is mainly dependent on its antioxidant capacity, i.e. its scavenging effect on free radicals. Therefore, the repairing effect of the product on the skin after the sun can be reflected to a certain extent by testing the free radical removing effect of the product.
Test example 2
In the test example, the after-sun repair ice cream prepared in example 1 and comparative example 1 was used, and stability tests such as normal temperature light-proof, heat resistance, low temperature, and light irradiation were performed on the after-sun repair ice cream.
Wherein, the heat resistance test conditions are as follows: keeping the temperature at 45 +/-1 ℃ and keeping out of the sun. The illumination test conditions were: illumination constant temperature and humidity test box (1.47X 10)6Lux · 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 at low temperature, and has severe color change under the conditions of normal temperature, light and heat resistance. As can be seen from fig. 3 and 4, the crystal cream a prepared in example 1 has a lower degree of color change than the common cream prepared in comparative example 1, and the technical scheme of the present invention greatly reduces the degree of color change of the tea extract, and the product stability is better. Furthermore, fig. 5 shows the comparison of example 1 with comparative example 1 after 6 months of storage at room temperature, it can also be seen that the post-sun repair ice cream of comparative example 1 shows a significant discoloration (see left panel in fig. 5), whereas the post-sun repair ice cream of example 1 shows a better stability (see right panel in fig. 5).
Test example 3
In contrast, the after-sun repair ice cream prepared in comparative example 1 is darker in color and less obvious in multiple emulsification phenomenon, and the after-sun repair ice cream prepared in example 1 is photographed under a microscope (see fig. 6).
In summary, the present invention provides a method for preparing multiple emulsions with a single type of emulsifier, which is prepared by mixing lipophilic emulsifiers, emollients, thickeners, etc. in specific proportions. Under the matching use of the components, a special multiple emulsification system can be formed, and the multiple emulsification system can achieve good stabilizing effect on the active components added into the internal water phase and keep the active components from deteriorating for a long time. In addition, the embodiment of the invention also provides the after-sun repair ice cream, which is characterized in that the tea extract is added into the internal water phase of the formed multiple emulsion system to serve as an active component, so that under the action of the multiple emulsion system, the active component in the tea extract is well stabilized, the effect of the active component is fully exerted, and a better after-sun repair effect is achieved.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement 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 multiple emulsions with a single type of emulsifier, comprising:
mixing lipophilic emulsifier and emollient to obtain oil phase;
mixing the oil phase and the internal water phase to prepare a mixed phase;
mixing the mixed phase with an external aqueous phase comprising a thickener to make the multiple emulsion;
wherein the dosage of the lipophilic emulsifier is 0.5-3 wt%, the dosage of the emollient is 3-10 wt%, and the dosage of the thickener is 0.1-2 wt%; the lipophilic emulsifier is polyether modified siloxane emulsifier.
2. The method of preparing multiple emulsions with a single type of emulsifier according to claim 1, wherein 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 dimethiconoethyl dimethicone, lauryl PEG-9 dimethiconoethyl dimethicone, and dimethicone/dimethicone PEG-10/15 crosspolymer.
3. The method of preparing multiple emulsions with a single type of emulsifier according to claim 1, wherein the thickener comprises at least one of polyacrylate crosspolymer-6, acrylic acid/C10-30 alkanol acrylate crosspolymer, acrylic acid/beheneth-25 methacrylate copolymer, sodium acrylate copolymer, sodium polyacrylate, carbomer, sodium acrylate/sodium acryloyldimethyl taurate copolymer, hydroxyethyl cellulose, ammonium acryloyldimethyl taurate/VP copolymer.
4. The method of preparing multiple emulsions with a single type of emulsifier according to claim 1 wherein the emollient comprises at least one of stearyl heptanoate, cyclopentadimethylsiloxane, isononyl isononanoate, caprylic/capric triglyceride, hydrogenated polydecene, isodecyl neopentanoate, dioctyl carbonate, meadowfoam oil, squalane, isopropyl myristate, and polydimethylsiloxane.
5. The method for preparing multiple emulsions with a single type of emulsifier according to claim 1, wherein the internal aqueous phase further comprises 4-6 wt% of a humectant; the humectant comprises at least one of glycerin, butylene glycol, 1, 3-propylene glycol, dipropylene glycol, bis-PEG-18 methyl ether dimethylsilane, PEG/PPG-17/6 copolymer, allantoin, betaine, trehalose, panthenol, glyceryl polyether-26, polyethylene glycol-32, and PEG/PPG/polytetramethylene glycol-8/5/3 glycerin.
6. The method for preparing multiple emulsions with a single type of emulsifier according to claim 1, wherein the internal/external aqueous phases further comprise 0.5 to 2 wt% of a preservative; the antiseptic comprises at least one of p-hydroxyacetophenone, phenoxyethanol, 1, 2-hexanediol/caprylyl glycol, glyceryl caprylate, and o-cymene-5-ol.
7. The method for preparing multiple emulsions with a single type of emulsifier according to claim 1, wherein the inner/outer aqueous phase further comprises 0.1 to 0.5 wt% of an adjuvant; the auxiliary materials comprise at least one of magnesium sulfate, sodium chloride, triethanolamine and aminomethyl propanol/water.
8. The after-sun repair ice cream is characterized by comprising the multiple emulsion prepared by the method for preparing the multiple emulsion by using the single-type emulsifier according to any one of claims 1 to 7, wherein 0.01-5 wt% of tea extract is added into an internal water phase of the multiple emulsion.
9. The post-basking repair ice cream of claim 8, wherein the tea extract comprises at least one of a Phyllostachys Pubescens tea extract, a Black tea extract, a Clerodendranthus spicatus extract, a Camellia oleifera extract, and a palmitoyl tea extract.
10. The post-basking repair ice cream of claim 8, further comprising 0.1-2 wt% of a skin conditioning agent in the oil/internal water phase; the skin conditioner comprises at least one of pearl extract, 4-tert-butylcyclohexanol, menthol lactate, bisabolol, and ginger root extract.
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