CN115844739A - Microbeads for cosmetics and use thereof - Google Patents

Microbeads for cosmetics and use thereof Download PDF

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Publication number
CN115844739A
CN115844739A CN202211424386.XA CN202211424386A CN115844739A CN 115844739 A CN115844739 A CN 115844739A CN 202211424386 A CN202211424386 A CN 202211424386A CN 115844739 A CN115844739 A CN 115844739A
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China
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phase
oil
oil phase
aqueous phase
channel
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CN202211424386.XA
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Chinese (zh)
Inventor
张亚
巫雨婷
刘喆
陈衍玲
程易
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Beijing Huaxi Haiyu Technology Co ltd
Tsinghua University
Bloomage Biotech Co Ltd
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Beijing Huaxi Haiyu Technology Co ltd
Tsinghua University
Bloomage Biotech Co Ltd
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Priority to CN202211424386.XA priority Critical patent/CN115844739A/en
Publication of CN115844739A publication Critical patent/CN115844739A/en
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Abstract

The application discloses a microballon and application for cosmetics, the microballon contains oil phase and aqueous phase, the aqueous phase is located the inside of oil phase, the oil phase wraps up completely the aqueous phase, the microballon skin is the oil phase, and the inlayer is the aqueous phase, and in cosmetics goods, this microballon suspends in cosmetics goods. When the consumer applies the microbeads, the oil phase breaks down first and spreads on the skin surface, and then the aqueous phase containing the active ingredient slowly permeates through the oil layer to exert its effect. Thus, the concentration of the active ingredient in contact with the skin can be effectively reduced, and the irritation can be reduced.

Description

Microbeads for cosmetics and use thereof
Technical Field
The invention relates to the technical field of cosmetics, in particular to a microbead and application thereof.
Background
For example, GABA (gamma-aminobutyric acid) is an inhibitory neurotransmitter, and when the GABA is applied to a cosmetic formula, skin wrinkles can be effectively weakened, because the GABA can trigger hyperpolarization of a neuron cell membrane, a chloride ion channel is opened, and potential difference inside and outside cells is neutralized, so that neuron cell excitation can be inhibited, and muscle contraction at the wrinkle part can be effectively reduced; however, because GABA acts on neuronal cells, consumers can generate certain irritation when using cosmetics containing GABA, which seriously affects the use experience of the cosmetics.
In order to reduce the irritation of such active ingredients, they may be encapsulated, for example by means of microcapsules or liposomes, which in turn affect the release of the active ingredient and the skin-care effect.
Disclosure of Invention
Aiming at the technical problems that the stimulation feeling of the active ingredients is generated when the skin care effect of the active ingredients is effectively exerted, and the release and the skin care effect of the active ingredients are influenced when the stimulation feeling of the active ingredients is reduced in the prior art, the application provides the micro-beads, and the micro-beads do not influence the active ingredients to exert the skin care effect while the stimulation feeling of the active ingredients is reduced.
The specific technical scheme of the invention is as follows:
1. a microbead, wherein the microbead comprises an oil phase and an aqueous phase, the aqueous phase being located inside the oil phase, and the oil phase completely enveloping the aqueous phase.
2. The microbead according to claim 1, wherein the mass ratio of the oil phase to the aqueous phase is 2-5.
3. The microbead according to item 1 or 2, wherein the oil phase comprises a thickener and an oleoester, preferably, the thickener is 0.5-50% and the oleoester is 50-99.5% in mass percentage of the oil phase.
4. The microbead according to item 3, wherein the thickener comprises a weakly polar polymer that can form a 3D space network structure encapsulating oil esters and has thermodynamic reversibility,
preferably, the thickener comprises one or more than two of castor oil/IPDI copolymer, glyceryl behenate/eicosanedioate, styrene/butadiene copolymer, dextrin palmitate and dibutyl ethylhexanoyl glutamine.
5. The microbead according to item 3 or 4, wherein the oil ester comprises one or more of a glyceride, a hydrocarbon or an ester wax,
preferably, the glyceride comprises one or more of triglyceride, diglyceride and monoglyceride, the hydrocarbon is selected from hydrocarbon derived from petroleum component, synthetic hydrocarbon or hydrocarbon of animal and vegetable origin, the ester wax comprises monoester of fatty acid and fatty alcohol,
more preferably, the oil ester comprises one or more of caprylic/capric triglyceride, meadowfoam seed oil, shea butter, tocopheryl acetate, isopropyl palmitate, hydrogenated polyisobutene, squalane, oleic acid, dioctyl carbonate.
6. The microbead according to any of claims 1-5, wherein the aqueous phase contains an active ingredient, preferably comprising an active ingredient with a stimulating sensation;
preferably, the content of the active ingredient is 0.1-10% by mass percentage in the water phase.
7. The microbead according to any of the items 1-6, wherein the aqueous phase also contains other ingredients in the cosmetic, preferably 0.01-5% by mass of the other ingredients in the aqueous phase.
8. The microbead according to any of claims 1-7, wherein the particle size of the microbead is in the range of 0.1-10mm.
9. Use of the microbead according to any of items 1-8 in cosmetics.
10. The use according to item 9, the microbeads being for delivery of a skin care ingredient.
11. Use of the microbead according to any of items 1-8 to reduce the irritation of an active ingredient.
12. A cosmetic preparation comprising the microbead according to any of claims 1-8.
13. The cosmetic preparation of claim 12, wherein the cosmetic preparation is a lotion, emulsion, gel, or cream;
preferably, the micro-beads account for 0.1-100% by mass of the cosmetic preparation.
ADVANTAGEOUS EFFECTS OF INVENTION
The micro-beads provided by the invention can well reduce the irritation of the active ingredients and do not influence the release of the active ingredients and the skin care effect.
Drawings
FIG. 1 is a schematic view of an apparatus for preparing microbeads.
FIG. 2 is a partially enlarged view of a microchannel device in an apparatus for preparing microbeads.
FIG. 3 is a schematic view of the resulting beads prepared in example 1.
1-oil phase storage tank, 2-water phase storage tank, 3-oil phase pump, 4-water phase pump, 5-micro-channel device, 6-collecting pipe, 7-oil phase, 8-water phase, 9-channel A, 10-channel B, 11-channel C
Detailed Description
The present invention is described in detail in the following description in conjunction with the embodiments illustrated in the figures, wherein like numerals indicate like features throughout. While specific embodiments of the invention are shown in the drawings, it should be understood that the invention may be embodied in various forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
It should be noted that certain terms are used throughout the description and claims to refer to particular components. As one skilled in the art will appreciate, various names may be used to refer to a component. This specification and claims do not intend to distinguish between components that differ in name but not function. In the following description and in the claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. The description which follows is a preferred embodiment of the invention, however, the description is given for the purpose of illustrating the general principles of the invention and not for the purpose of limiting the scope of the invention. The scope of the present invention is defined by the appended claims.
The invention provides a micro-bead for cosmetics, wherein the micro-bead comprises an oil phase and a water phase, the water phase is positioned in the oil phase, and the oil phase completely wraps the water phase.
The micro-bead that this application provided, because the aqueous phase is located the inside of oil phase, the oil phase wraps up the aqueous phase completely, and the consumer is when using to paint the micro-bead, and the oil phase can break earlier, spreads on the skin surface, and then the aqueous phase that contains active ingredient is in slowly permeating oil layer performance efficiency, can effectively reduce the active ingredient in the aqueous phase and the concentration of skin contact like this, weakens its irritability.
In the present application, the oil phase is gelatinous and the aqueous phase is an aqueous solution or hydrogel.
In some embodiments, the mass ratio of the oil phase to the aqueous phase is from 2 to 5.
For example, the mass ratio (m) of the oil phase and the water phase Oil phase :m Aqueous phase ) 1, 3.
In the present application, the mass ratio of the oil phase to the water phase is controlled by controlling the pump speed of the oil phase and the water phase, and the mass ratio of the oil phase to the water phase in the microbeads is determined by a conventional method, for example, the prepared microbeads are crushed by a teflon container and then the mass ratio of the oil phase to the water phase is calculated by TGA thermal weight loss method.
The mass ratio of the oil phase to the water phase in the microbeads is set within a specific range, so that the permeation speed of the active ingredients can be well controlled, and the effect of the active ingredients is not influenced.
In some embodiments, the oil phase comprises a thickener and an oil ester, preferably, the thickener is 0.5-50% and the oil ester is 50-99.5% by mass of the oil phase. For example, the thickener is 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 25%, 30%, 35%, 40%, 45%; the oleyl ester is 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, 99%.
In some embodiments, the oil phase further comprises an oil soluble active.
In some embodiments, the thickener comprises a weakly polar polymer that can form a 3D space network structure encapsulating oil esters and has thermodynamic reversibility, preferably, the thickener comprises one or more of castor oil/IPDI copolymer, glyceryl behenate/eicosanedioate, styrene/butadiene copolymer, dextrin palmitate, and dibutyl ethylhexanoyl glutamine.
In some embodiments, the oil ester comprises one or more of a glyceride, a hydrocarbon, or an ester wax. Preferably, the glyceride comprises one or more of triglyceride, diglyceride and monoglyceride, the hydrocarbon is selected from hydrocarbon derived from petroleum component, synthetic hydrocarbon or hydrocarbon of animal and plant origin, and the ester wax is selected from monoester of fatty acid and fatty alcohol. More preferably, the oil ester comprises one or more of caprylic/capric triglyceride, meadowfoam seed oil, shea butter, tocopheryl acetate, isopropyl palmitate, hydrogenated polyisobutene, squalane, oleic acid, dioctyl carbonate.
In some embodiments, the oil soluble actives include, but are not limited to, ceramides, sphingosines, plant essential oils, oil soluble antioxidants, fragrances, and the like.
In some embodiments, the aqueous phase contains an active ingredient, preferably the active ingredient comprises a stinging active ingredient, preferably the stinging active ingredient comprises one or more of aminobutyric acid, ascorbic acid, niacinamide, and a-hydroxycarboxylic acid; preferably, the active ingredient is 0.1-10% by mass in the aqueous phase, for example, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, etc.
In some embodiments, the aqueous phase may also contain other ingredients in the cosmetic including, but not limited to, preservatives, other active ingredients, and the like, preferably 0.01 to 5% by mass of the aqueous phase, for example, 0.01%, 0.05%, 0.1%, 0.5%, 1%, 2%, 3%, 4%, 5%, and the like.
In some embodiments, the preservative includes, but is not limited to, propylene glycol, butylene glycol, pentylene glycol, caprylyl hydroxamic acid, phenoxyethanol, or the like. The other active ingredients include, but are not limited to, hyaluronic acid or salts thereof, ectoin, oligopeptides, amino acids, vitamins and/or plant extracts, and the like. The oligopeptide may be, for example, carnosine, tripeptide-1 copper, acetyl hexapeptide-3, palmitoyl pentapeptide-3, palmitoyl tripeptide-5, and the like.
In some embodiments, the beads have a particle size in the range of 0.1 to 10mm, e.g., 0.5mm, 1mm, 2mm, 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm, 10mm, and the like.
In the present application, the particle size of the microbeads is determined by a method that is conventional in the art, such as taking a photograph with a microscope and then measuring the diameter, preferably taking a photograph of the microbeads with a graduated scale and then measuring the diameter of the microbeads in the photograph with software that is commonly used in the art, preferably measuring the diameter of the microbeads in the photograph with ImageJ or equivalent commercially available measurement software.
In the present application, the method for preparing the microbeads is not limited in any way, and the microbeads can be prepared by a method conventional in the art, for example, by mixing an oil phase and an aqueous phase.
Fig. 1 is a schematic diagram of an apparatus for preparing microbeads according to an embodiment of the present invention, and as shown in fig. 1, the apparatus for preparing microbeads includes an oil phase storage tank 1, a water phase storage tank 2, an oil phase pump 3, a water phase pump 4, a microchannel apparatus 5 and a collecting pipe 6, an outlet of the oil phase storage tank 1 is connected to an inlet of the oil phase pump 3, an outlet of the water phase storage tank 2 is connected to an inlet of the water phase pump 4, an inlet of the oil phase pump 3 and an inlet of the water phase pump 4 are both connected to an inlet of the microchannel apparatus 5 to prepare microbeads, and an outlet of the microchannel apparatus 5 is connected to an inlet of the collecting pipe 6 to collect the microbeads obtained by preparation.
FIG. 2 is an enlarged schematic view of microchannel device 5, where microchannel device 5 includes channel A9, channel B10, and channel C11, where channel A9 is connected to channel C11, where channel B10 is connected to channel A9 and perpendicular to channel A9, and where channel B10 is connected to channel C11 and perpendicular to channel C11.
In fig. 2 the oil phase 7 is mixed with the water phase 8 from the channel A9 via the channel B10 into the channel C11 and is thus collected by the collection tube 6.
In the present application, the solvent contained in the collection tube 6 is not limited in any way, and may be a solvent commonly used in the art, for example, water.
When preparing the microbeads, the oil phase solution and the water phase solution are respectively placed in an oil phase storage tank 1 and a water phase storage tank 2, enter a channel A and a channel B in a micro-channel device 5 under the action of an oil phase pump 3 and a water phase pump 4, and enter a collecting pipe 6 through a channel C11 to collect the microbeads.
Those skilled in the art will appreciate that the method for preparing microbeads described above in connection with fig. 1 is only an exemplary method, and the microbeads of the present application can be obtained by controlling the relevant parameters such as the inner diameter, flow rate, etc. of the oil phase and water phase pipelines, for example, the microbeads with the oil phase wrapped around the water phase can be prepared in the form of microchannels, including but not limited to "hydrodynamic focusing manner", such as "cross" or "Y" microchannels; or "T-cut" and the like.
During the preparation of the micro-bead, the shape and the size of the micro-bead can be controlled by controlling the inner diameter of the micro-channel, the Reynolds number of the fluid and the shearing momentum ratio of the fluid.
In some embodiments, the temperature of the oil phase storage tank 1 and the water phase storage tank 2 is not particularly limited as long as the oil phase is in a dissolved state, and may be, for example, 80 to 95 ℃.
In some embodiments, the flow rate of the oil phase at the tank pump 3 is 2-50ml/h, for example, the flow rate of the oil phase at the tank pump 3 may be 2ml/h, 5ml/h, 10ml/h, 15ml/h, 20ml/h, 25ml/h, 30ml/h, 35ml/h, 40ml/h, 45ml/h, 50ml/h, etc.
In some embodiments, the flow rate of the aqueous phase at the aqueous phase pump 4 is 1 to 20ml/h, for example, the flow rate of the aqueous phase at the aqueous phase pump 4 can be 1ml/h, 2ml/h, 3ml/h, 4ml/h, 5ml/h, 6ml/h, 7ml/h, 8ml/h, 9ml/h, 10ml/h, 11ml/h, 12ml/h, 13ml/h, 14ml/h, 15ml/h, 16ml/h, 17ml/h, 18ml/h, 19ml/h, 20ml/h, and the like.
In some embodiments, the channel A9 has a dimension of 0.1-6.0mm, e.g., a dimension of 0.1mm, 0.2mm, 0.3mm, 0.4mm, 0.5mm, 1mm, 1.5mm, 2.0mm, 2.5mm, 3.0mm, 3.5mm, 4.0mm, 4.5mm, 5.0mm, 5.5mm, 6.0mm. The channel C11 has a dimension of 0.1-7.0mm, for example, a dimension of 1mm, 1.5mm, 2.0mm, 2.5mm, 3.0mm, 3.5mm, 4.0mm, 4.5mm, 5.0mm, 5.5mm, 6.0mm, 6.5mm, 7.0mm.
In some embodiments, the dimension of the channel B10 is 0.5-6.0mm, e.g., 0.5mm, 1.0mm, 1.5mm, 2.0mm, 2.5mm, 3.0mm, 3.5mm, 4.0mm, 4.5mm, 5.0mm, 5.5mm, 6.0mm. In some embodiments, the temperature of the collection tube 6 is 10-50 ℃, preferably 20 ℃.
In some embodiments, the temperature of the collection tube 6 may be 10-50 ℃, e.g., 10 ℃, 20 ℃, 30 ℃, 40 ℃, 50 ℃, etc.
The application provides the application of the micro-beads in cosmetics.
Further, the beads are used to deliver skin care ingredients.
The application also provides the application of the microbeads in reducing the irritation of active ingredients. The present application provides a cosmetic preparation comprising the above-described microbeads.
In some embodiments, the cosmetic preparation is a lotion, emulsion, gel, or cream.
In some embodiments, the microbeads range from 0.1 to 100% by mass of the cosmetic preparation. For example, the amount of the beads is 0.1%, 0.5%, 1%, 5%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 100%, or the like, in mass percentage based on the cosmetic preparation.
In some embodiments, the cosmetic preparation may comprise other ingredients commonly used in cosmetics in addition to the microbeads. In the present application, as for other ingredients commonly used, the present application is not limited in any way, and it may be ingredients conventional in the art, for example, preservatives, thickeners, perfumes, efficacy ingredients, and the like.
Examples
The invention is described generally and/or specifically for the materials used in the tests and the test methods, in the following examples,% means wt%, i.e. percent by weight, unless otherwise specified. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products commercially available, wherein Table 1 is a table of raw materials and equipment sources used in examples and comparative example 1.
TABLE 1 table of sources of raw materials and equipments used in examples and comparative examples
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Example 1
As shown in fig. 1 and 2, an oil phase solution and a water phase solution are respectively placed in an oil phase storage tank 1 and a water phase storage tank 2, the temperatures of the oil phase storage tank 1 and the water phase storage tank 2 are both 85 ℃, the oil phase solution and the water phase solution are respectively sent into a micro-channel device 5 under the action of an oil phase pump 3 and a water phase pump 4, microbeads enter a collecting pipe 6 through a channel C, the liquid in the collecting pipe 6 is deionized water, the temperature is 20 ℃, after the microbeads are solidified, the microbeads are obtained by filtering with a filter screen, wherein the water phase is 5% of GABA and 95% of water, the flow rate of the water phase is 4mL/h, and the inner diameter of the channel A is 0.6mm; the oil phase is 10% of castor oil/IPDI copolymer and 90% of caprylic/capric triglyceride, the flow rate of the oil phase is 4mL/h, and the inner diameter of the channel B is 0.6mm; the inner diameter of the channel C is 1.1mm. The mass ratio of the oil phase to the water phase is 1:1, the bead size is 1.52mm.
The beads prepared in example 1 are shown in FIG. 3.
The method for measuring the mass ratio of the oil phase to the water phase in the prepared microbeads is as follows: and (3) smashing the prepared microbeads by a polytetrafluoroethylene container, and then calculating the mass ratio of the oil phase to the water phase by a TGA heating weight loss method.
The method for measuring the size of the bead is as follows: the diameter of the microbeads in the pictures was measured using ImageJ or equivalent commercial measurement software.
Examples 2 to 22
Examples 2-22 were prepared in the same manner as example 1, wherein:
example 2 aqueous phase 5% GABA and 95% water, flow rate of aqueous phase 4mL/h, channel A inner diameter 0.6mm; the oil phase is 10% of castor oil/IPDI copolymer and 90% of caprylic/capric triglyceride, the flow rate of the oil phase is 6mL/h, and the inner diameter of the channel B is 0.6mm; the inner diameter of the channel C is 1.1mm. The mass ratio of the oil phase to the water phase is 1.5:1, the bead size is 1.93mm.
Example 3 aqueous phase 5% GABA and 95% water, flow rate of aqueous phase 4mL/h, channel A inner diameter 0.6mm; the oil phase is 10% of castor oil/IPDI copolymer and 90% of caprylic/capric triglyceride, the flow rate of the oil phase is 8mL/h, and the inner diameter of the channel B is 0.6mm; the inner diameter of the channel C is 1.1mm. The mass ratio of the oil phase to the water phase is 2:1, the bead size is 2.01mm.
Example 4 aqueous phase 5% GABA and 95% water, flow rate of aqueous phase 4mL/h, inner diameter of channel A0.6 mm; the oil phase is 10% of castor oil/IPDI copolymer and 90% of caprylic/capric triglyceride, the flow rate of the oil phase is 14mL/h, and the inner diameter of the channel B is 0.6mm; the inner diameter of the channel C is 1.1mm. The mass ratio of the oil phase to the water phase is 3.5:1, the bead size is 2.09mm.
Example 5 aqueous phase 5% GABA and 95% water, flow rate of aqueous phase 4mL/h, inner diameter of channel A0.6 mm; the oil phase is 10% of castor oil/IPDI copolymer and 90% of caprylic/capric triglyceride, the flow rate of the oil phase is 16mL/h, and the inner diameter of the channel B is 0.6mm; the inner diameter of the channel C is 1.1mm. The mass ratio of the oil phase to the water phase is 4:1, the bead size is 2.18mm.
Example 6 aqueous phase 5% GABA and 95% water, flow rate of aqueous phase 4mL/h, channel A inner diameter 0.6mm; the oil phase is 10% of castor oil/IPDI copolymer and 90% of caprylic/capric triglyceride, the flow rate of the oil phase is 18mL/h, and the inner diameter of the channel B is 0.6mm; the inner diameter of the channel C is 1.1mm. The mass ratio of the oil phase to the water phase is 4.5:1, bead size 2.43mm.
Example 7 aqueous phase 5% GABA and 95% water, aqueous phase flow rate of 4mL/h, channel A internal diameter of 0.6mm; the oil phase is 10% of castor oil/IPDI copolymer and 90% of caprylic/capric triglyceride, the flow rate of the oil phase is 22mL/h, and the inner diameter of the channel B is 0.6mm; the inner diameter of the channel C is 1.1mm. The mass ratio of the oil phase to the water phase is 5.5:1, bead size 2.52mm.
Example 8 aqueous phase 5% GABA and 95% water, aqueous phase flow rate of 4mL/h, channel A internal diameter of 0.7mm; the oil phase is 10% of castor oil/IPDI copolymer and 90% of caprylic/capric triglyceride, the flow rate of the oil phase is 24mL/h, and the inner diameter of the channel B is 0.7mm; the inner diameter of the channel C is 1.5mm. The mass ratio of the oil phase to the water phase is 6:1, the bead size is 2.83mm.
Example 9 aqueous phase 5% GABA and 95% water, aqueous phase flow rate of 4mL/h, channel A inner diameter of 3.0mm; the oil phase is 10% of castor oil/IPDI copolymer and 90% of caprylic/capric triglyceride, the flow rate of the oil phase is 40mL/h, and the inner diameter of the channel B is 3.0mm; the inner diameter of the channel C is 6.5mm. The mass ratio of the oil phase to the water phase is 10:1, the bead size is 8.45mm.
Example 10 aqueous phase 5% GABA and 95% water, flow rate of aqueous phase 4mL/h, inner diameter of channel A1.5 mm; the oil phase is 10% of castor oil/IPDI copolymer and 90% of caprylic/capric triglyceride, the flow rate of the oil phase is 12mL/h, and the inner diameter of the channel B is 1.5mm; the inner diameter of the channel C is 2.8mm. The mass ratio of the oil phase to the water phase is 3:1, bead size 4.58mm.
Example 11 aqueous phase 5% GABA and 95% water, flow rate of aqueous phase 4mL/h, inner diameter of channel A1.7 mm; the oil phase is 10% of castor oil/IPDI copolymer and 90% of caprylic/capric triglyceride, the flow rate of the oil phase is 12mL/h, and the inner diameter of the channel B is 1.7mm; the inner diameter of the channel C is 3.5mm. The mass ratio of the oil phase to the water phase is 3:1, the bead size is 6.75mm.
Example 12 aqueous phase 5% GABA and 95% water, aqueous phase flow rate of 4mL/h, channel A inner diameter of 3.0mm; the oil phase is 10% of castor oil/IPDI copolymer and 90% of caprylic/capric triglyceride, the flow rate of the oil phase is 12mL/h, and the inner diameter of the channel B is 3.0mm; the inner diameter of the channel C is 6.5mm. The mass ratio of the oil phase to the water phase is 3:1, bead size 9.38mm.
Example 13 aqueous phase 5% GABA and 95% water, flow rate of aqueous phase 4mL/h, channel A inner diameter 0.6mm; the oil phase is 10% of castor oil/IPD copolymer, 56% of caprylic/capric triglyceride and 34% of meadowfoam seed oil, the flow rate of the oil phase is 12mL/h, and the inner diameter of the channel B is 0.6mm; the inner diameter of the channel C is 1.1mm. The mass ratio of the oil phase to the water phase is 3:1, the bead size is 2.35mm.
Example 14 aqueous phase 5% GABA and 95% water, aqueous phase flow rate of 4mL/h, channel A inner diameter of 0.6mm; the oil phase is 10% of castor oil/IPD copolymer, 53% of caprylic/capric triglyceride, 34% of white Potentilla seed oil and 3% of shea butter, the flow rate of the oil phase is 12mL/h, and the inner diameter of the channel B is 0.6mm; the inner diameter of the channel C is 1.1mm. The mass ratio of the oil phase to the water phase is 3:1, the bead size is 2.04mm.
Example 15 aqueous phase 5% GABA and 95% water, flow rate of aqueous phase 4mL/h, inner diameter of channel A0.6 mm; the oil phase is 10% of castor oil/IPDI copolymer, 40% of dioctyl carbonate, 30% of white pond flower seed oil, 10% of squalane, 5% of shea butter and 5% of tocopherol acetate, the flow rate of the oil phase is 12mL/h, and the inner diameter of the channel B is 0.6mm; the inner diameter of the channel C is 1.1mm. The mass ratio of the oil phase to the water phase is 3:1, the bead size is 2.39mm.
Example 16 aqueous phase 5% GABA and 95% water, flow rate of aqueous phase 4mL/h, channel A inner diameter 1.5mm; the oil phase is 10% of castor oil/IPDI copolymer, 40% of dioctyl carbonate, 30% of hydrogenated polyisobutene, 10% of squalane, 5% of oleic acid and 5% of isopropyl palmitate, the flow rate of the oil phase is 12mL/h, and the inner diameter of the channel B is 1.5mm; the inner diameter of the channel C is 2.8mm. The mass ratio of the oil phase to the water phase is 3:1, the bead size is 4.91mm.
Example 17 the aqueous phase was 5% GABA and 95% water, the flow rate of the aqueous phase was 4mL/h, and the inner diameter of channel A was 0.6mm; the oil phase is 3% of glyceryl behenate/eicosanedioate, 40% of caprylic acid/capric acid triglyceride, 30% of dioctyl carbonate, 20% of hydrogenated polyisobutene and 7% of squalane, the flow rate of the oil phase is 12mL/h, and the inner diameter of the channel B is 0.6mm; the inner diameter of the channel C is 1.1mm. The mass ratio of the oil phase to the water phase is 3:1, the bead size is 2.35mm.
Example 18 aqueous phase 5% GABA and 95% water, aqueous phase flow rate of 4mL/h, channel A inner diameter of 0.6mm; the oil phase is 3% dextrin palmitate, 50% dioctyl carbonate, 40% caprylic/capric triglyceride and 7% isopropyl palmitate, the flow rate of the oil phase is 12mL/h, and the inner diameter of the channel B is 0.6mm; the inner diameter of the channel C is 1.1mm. The mass ratio of the oil phase to the water phase is 3:1, the bead size is 2.02mm.
Example 19 the aqueous phase was 5% GABA and 95% water, the flow rate of the aqueous phase was 4mL/h, and the inner diameter of channel A was 0.6mm; the oil phase is 0.2% of castor oil/IPDI copolymer and 99.8% of caprylic acid/capric acid triglyceride, the flow rate of the oil phase is 12mL/h, and the inner diameter of the channel B is 0.6mm; the inner diameter of the channel C is 1.1mm. The mass ratio of the oil phase to the water phase is 3:1, bead size 2.52mm.
Example 20 aqueous phase 5% GABA and 95% water, flow rate of aqueous phase 4mL/h, inner diameter of channel A0.6 mm; the oil phase is 0.2% of castor oil/IPDI copolymer, 90% of caprylic/capric triglyceride and 9.8% of dioctyl carbonate, the flow rate of the oil phase is 12mL/h, and the inner diameter of the channel B is 0.6mm; the inner diameter of the channel C is 1.1mm. The mass ratio of the oil phase to the water phase is 3:1, bead size 2.51mm.
Example 21 aqueous phase 5% GABA and 95% water, aqueous phase flow rate of 4mL/h, channel A internal diameter of 0.7mm; the oil phase is 55% of castor oil/IPDI copolymer and 45% of caprylic/capric triglyceride, the flow rate of the oil phase is 12mL/h, and the inner diameter of the channel B is 0.7mm; the inner diameter of the channel C is 1.5mm. The mass ratio of the oil phase to the water phase is 3:1, bead size 2.86mm.
Example 22 the aqueous phase was 10% ascorbic acid and 90% water, the flow rate of the aqueous phase was 4mL/h, and the internal diameter of channel A was 0.7mm; the oil phase is 90% caprylic acid/capric acid triglyceride, the flow rate of the oil phase is 12mL/h, and the inner diameter of the channel B is 0.7mm; the inner diameter of the channel C is 1.5mm. The mass ratio of the oil phase to the water phase is 3:1, the bead size is 2.85mm.
Comparative example 1
Comparative example 1 is different from example 11 in that comparative example 1 is a physical mixture of oil gel particles and an aqueous phase solution, wherein the mass ratios of the aqueous phase component, the oil gel particle component (oil phase component), the oil gel particles and the aqueous phase are shown in table 2.
Comparative example 2
Comparative example 2 is different from example 11 in that comparative example 2 is a physical mixture of a liquid oil phase and an aqueous phase solution, wherein the mass ratios of the aqueous phase component, the liquid oil phase component and the aqueous phase are shown in table 2.
Comparative example 3
Comparative example 3 is different from example 11 in that comparative example 3 is a physical mixture of oil gel particles and an aqueous phase solution, wherein the mass ratios of the aqueous phase component, the oil gel particle component (oil phase component), the oil gel particles and the aqueous phase are shown in table 2.
TABLE 2 reaction condition tables of examples and comparative examples
Figure BDA0003944219800000121
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Figure BDA0003944219800000131
Experimental example 1 evaluation of irritation and wrinkle evaluation after Using GABA
A. Evaluation of irritation
(1) The evaluation method comprises the following steps: the method comprises the steps of objectively evaluating the irritation strength and irritation difference of different samples, screening GABA sensitive people by using a 3% GABA aqueous solution, setting the score to be 1-5, firstly training a subject to respectively sense the irritation of 1 point and 5 points, and secondly evaluating the irritation brought by the actual samples by the subject according to the criterion.
The GABA sensitive population screening method comprises the following steps:
sucking 20 μ L of solution, applying to the periphery of eyes of the subject, respectively applying physiological saline and 3% GABA aqueous solution to the left and right sides, reacting for about 1min, and inquiring about the pain of the subject; selecting subjects who responded to 3% GABA samples (felt a tingling sensation); finally, 10 subjects sensitive to GABA were screened, of which 3 men, 7 women, office white collar between the ages of 27 and 40, with an average age of 33 years.
The irritation scoring criteria were:
the score was set to 1-5 points, wherein the stimulation by 5% GABA aqueous solution was defined as 1 point, the stimulation by physiological saline was defined as 5 points, and the specific evaluation criteria are shown in Table 3.
TABLE 3 irritation evaluation criteria
1 The stabbing pain is severe and totally unacceptable
2 The stabbing pain is strong and not received well
3 A tingle is perceived and accepted
4 Slight tingling sensation, acceptable
5 Has no irritation and is acceptable
(2) And (3) sample testing:
negative control and positive control: wherein 0.6% NaCl solution is used as a negative control, and 5% GABA solution is used as a positive control; the method comprises sucking 20 μ L of 0.6% NaCl solution, uniformly applying to canthus of subject, reacting for about 1min, inquiring irritation of subject, and informing subject that the irritation is 1 point. Subsequently, 20. Mu.L of a 5% GABA aqueous solution was aspirated and applied uniformly to the canthus of the subject, and the subject was asked for irritation in response to about 1min, and was informed to define the irritation as 5 points.
b, sample testing: the wet tissue was wiped around the eyes and recovered for 10-15min, and then a sample test was performed, in which 10 beads prepared in examples 1-21 were placed on fingertips, pressed one by one and applied to the canthus, massaged up and down back and forth for 20 min to complete absorption, reacted for about 1-2 min, the subject was asked about the tingling of the face and described, and the degree of the intensity of the irritation was scored, and the results are shown in table 5.
c: physical mixing of oleogel particles with aqueous GABA solution samples test: wiping the periphery of eyes with a wet tissue, recovering for 10-15min, and then carrying out sample test by taking 10 oleogel microbeads and placing the oleogel microbeads at the corners of the eyes, raising the head of a subject slightly to keep the microbeads staying at the corners of the eyes, quickly sucking 10 mu LGABA aqueous solution to the corners of the eyes, quickly smearing the oleogel and GABA aqueous solution at the same time, massaging the eyes up and down to complete absorption, reacting for about 1-2 min, inquiring and describing the stabbing pain of the face of the subject, and scoring the strength of the stimulation, wherein the results are shown in Table 5.
d, physically mixing a liquid oil phase with a GABA aqueous solution to test: wiping the periphery of eyes with a wet paper towel, recovering for 10-15min, then performing sample test, sucking 40 μ L of mixed emulsion, placing at the corner of eyes, massaging up and down back and forth for 20 min till complete absorption, reacting for about 1-2 min, inquiring and describing the stabbing pain of the face of a subject, and scoring the strength of the stimulation, wherein the results are shown in table 5.
B. Wrinkle evaluation
(1) Wrinkle evaluation method: the method objectively evaluates the wrinkle-removing effect of different samples, and gives a comprehensive score by comparing the other half face before smearing and without any component. The score was set at 1-5 points, with 5 points representing very significant wrinkle reduction and 1 point representing no wrinkle reduction. The subjects were enrolled on a total of 10, 3 men, 7 women, age 27 to 40 years, mean age 33 years, wrinkle rating 3-5.
The score was set to 1-5 points, with 1 point representing no wrinkle-removing effect and 5 points representing very significant wrinkle-removing effect, and the specific scoring criteria are shown in table 4.
TABLE 4 wrinkle scoring criteria
Figure BDA0003944219800000141
Figure BDA0003944219800000151
The wrinkle length measuring method comprises the following steps:
the canthus position is selected, the lengths of the wrinkles before and after smearing are recorded by using a Visia equipment imaging system respectively, and the change condition of the wrinkle length is calculated.
(2) And (3) sample testing:
a, sample testing: wiping canthus with a wet tissue, recovering for 10-15min, observing the wrinkle degree before applying, placing 10 beads prepared in examples 1-21 on the finger tips, pressing and applying to canthus, massaging back and forth up and down for 20 min until completely absorbing, after 10min of reaction, slightly wiping off the excess oil in canthus with a paper towel, observing the wrinkle condition before applying and on the other canthus, and scoring, the results are shown in Table 5.
b: oleogel microbeads and GABA aqueous samples tested: wiping canthus with a wet tissue, recovering for 10-15min, observing wrinkle degree before smearing, and then performing sample test, wherein the addition amount of oil phase and GABA aqueous solution is consistent with the addition amount of water in oil gel, the method is that 10 oil gel microspheres are taken and placed at the canthus, a subject is required to slightly raise the head to keep the microspheres to stay at the canthus, then 10 mu LGABA aqueous solution is quickly sucked to the canthus, the oil gel and the GABA aqueous solution are quickly smeared at the same time, massaging back and forth up and down for 20 min till complete absorption, after reacting for 10min, slightly wiping off surface grease with the tissue, observing wrinkles of the canthus before smearing and on the other side and scoring, and the result is shown in Table 5.
c, testing an oil-water homogeneous mixed liquid sample: wiping the canthus with a wet paper towel, recovering for 10-15min, observing the wrinkle degree before smearing, performing sample test, sucking 40 μ L of mixed emulsion, placing at the canthus, and after smearing, scoring irritation by the subject. Massaging the eyes up and down back and forth for 20 minutes until the eyes are completely absorbed, after 10 minutes of reaction, lightly wiping off the surface oil esters with a paper towel, and observing and scoring the wrinkles before smearing and on the other side of the eyes, wherein the results are shown in Table 5.
TABLE 5 irritation score and wrinkle score results
Figure BDA0003944219800000152
Figure BDA0003944219800000161
Experimental example 2 irritation test after use of ascorbic acid
The samples obtained in example 22 and comparative example 3 were applied to the curved side of the forearm of a subject (the subject was a female 25 to 35 years old, worked on a paper in the office, worn with a thin long-sleeved garment during the test to avoid excessive UV irradiation, and no skin care product or sunscreen product was applied to the forearm during the test), continuously applied for 10 days, 2 times a day, and the L, a, and b values of the applied area were measured after 10 days using an NS800 spectrophotometer (3 nh sanen), wherein L represents a white-black value, a represents a red-green value, and b represents a yellow-blue value, respectively.
Wherein, when the L value increased by 5% and the b value decreased by 6% after 10 days, the subject using the sample of example 22 had no irritation, while the subject using the sample of comparative example 3 had a significant irritation, indicating that the microbeads were able to reduce the irritation of ascorbic acid.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention will still fall within the protection scope of the technical solution of the present invention.

Claims (10)

1. A microbead, wherein the microbead comprises an oil phase and an aqueous phase, the aqueous phase is located inside the oil phase, and the oil phase completely surrounds the aqueous phase.
2. The microbead according to claim 1, wherein the mass ratio of the oil phase and the aqueous phase is 2-5.
3. The microbead according to claim 1 or 2, wherein the oil phase comprises a thickener and an oleoester, preferably the thickener is 0.5-50% and the oleoester is 50-99.5% by mass of the oil phase.
4. The microbead according to claim 3, wherein the thickener comprises a weakly polar polymer that can form a 3D space network structure encapsulating oil esters and is thermodynamically reversible,
preferably, the thickener comprises one or more than two of castor oil/IPDI copolymer, glyceryl behenate/eicosanedioate, styrene/butadiene copolymer, dextrin palmitate and dibutyl ethylhexanoyl glutamine.
5. The microbead according to claim 3 or 4, wherein the oil ester comprises one or more of a glyceride, a hydrocarbon or an ester wax,
preferably, the glyceride comprises one or more of triglyceride, diglyceride and monoglyceride, the hydrocarbon is selected from hydrocarbon derived from petroleum component, synthetic hydrocarbon or hydrocarbon of animal and vegetable origin, the ester wax comprises monoester of fatty acid and fatty alcohol,
more preferably, the oil ester comprises one or more of caprylic/capric triglyceride, meadowfoam seed oil, shea butter, tocopheryl acetate, isopropyl palmitate, hydrogenated polyisobutene, squalane, oleic acid, dioctyl carbonate.
6. The microbead according to any of claims 1-5, wherein the aqueous phase contains an active ingredient, preferably the active ingredient comprises an active ingredient with a stinging sensation;
preferably, the content of the active ingredient is 0.1-10% by mass percentage in the water phase.
7. The microbead according to any of claims 1-6, wherein the aqueous phase also contains other ingredients in the cosmetic, preferably 0.01-5% by mass of the other ingredients in the aqueous phase;
preferably, the particle size of the microbeads ranges from 0.1 to 10mm.
8. Use of the microbead according to any of claims 1-7 in cosmetics;
preferably, the microbeads are used to deliver skin care ingredients.
9. Use of a microbead according to any of claims 1-7 to reduce the irritation of an active ingredient.
10. A cosmetic preparation comprising the microbead of any of claims 1-7;
preferably, the cosmetic preparation is a water, lotion, gel or cream;
preferably, the micro-beads account for 0.1-100% by mass of the cosmetic preparation.
CN202211424386.XA 2022-11-15 2022-11-15 Microbeads for cosmetics and use thereof Pending CN115844739A (en)

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