CN115998648A

CN115998648A - Composition with pore-shrinking effect, nano microemulsion, preparation method and application thereof

Info

Publication number: CN115998648A
Application number: CN202211559583.2A
Authority: CN
Inventors: 杨帆; 郭苗; 周正; 胡雅文; 周紫燕
Original assignee: Mcgill Biotechnology Co ltd
Current assignee: Mcgill Biotechnology Co ltd
Priority date: 2022-12-06
Filing date: 2022-12-06
Publication date: 2023-04-25

Abstract

The invention relates to a composition with a pore-refining effect, a nano-microemulsion, a preparation method and an application thereof, wherein the composition with the pore-refining effect comprises a fucus seradix extract, dipalmitoyl hydroxyproline and dipeptide diamino Ding Xianbian-based amide diacetate. Wherein the Fucus vesiculosus extract balances skin grease and plays a role in shrinking pores from root sources; dipalmitoyl hydroxyproline is an important raw material for synthesizing collagen, and supplements collagen to support pores; the dipeptide diamino Ding Xianbian-based amide diacetate can smooth skin, and the dipeptide diamino Ding Xianbian-based amide diacetate and the dipeptide diamino diacetate have a synergistic effect which is unexpected by a person skilled in the art on the efficacy of pore-shrinking, so that the skin can be smoothed more effectively and the pores can be shrunk. The invention also utilizes the microemulsion technology to carry out encapsulation on the composition to obtain a nano microemulsion product, which can improve the stability of the composition, help the composition to stay and permeate in pores, improve the permeability and the sebaceous gland enrichment, and slowly release and take effect for a long time.

Description

Composition with pore-shrinking effect, nano microemulsion, preparation method and application thereof

Technical Field

The invention belongs to the technical field of cosmetics, relates to a composition with a pore-shrinking effect, nano-microemulsion and a preparation method and application thereof, and in particular relates to a composition with a pore-shrinking effect, nano-microemulsion with a pore-shrinking effect and a preparation method thereof, and essence emulsion with a pore-shrinking effect and a preparation method thereof.

Background

The enlarged pores of the face are one of the common skin problems, and are an important expression of skin aging, and the reason of the enlarged pores is probably related to hypersecretion of skin grease, skin inflammation and skin aging, with the increase of the age, the elasticity around the pores is reduced, the hair follicle volume is increased, collagen is lost, the support around the pores is lost, and the structural integrity of the skin is damaged, so that the skin aging often leads to the enlarged pores.

Most of the existing products for refining pores are astringent, exfoliating and exfoliating cosmetics, and the like, and basically solve the problem of pores from the surface. The astringent cosmetics mainly use organic acid to coagulate proteins, so that the effect of temporarily shrinking pores is achieved, but the problem of large pores cannot be fundamentally solved; the corner plugs are removed by dissolving the oil and fat by using similar compatibility, but the oil and fat secretion can not be regulated and controlled, the corner plugs can be regenerated quickly, and if the oil and fat secretion is not regulated and controlled, the pores can be bigger; the cosmetics for removing cutin mostly contain salicylic acid, fruit acid and the like, and dissolve, soften and remove dead skin accumulated on the surface of skin to dredge and block pores, but the cosmetics have great skin irritation and are easy to damage sensitive skin. In addition, in the existing products for refining pores, the active ingredients are single and do not have synergistic effect.

For example, CN103932954a discloses a cosmetic for whitening and tendering skin and refining pores and a method for producing the same, comprising: adding VC ethyl ether, tranexamic acid, arbutin and mulberry extract into water, heating to 70 ℃ for dissolution to form aqueous phase liquid; mixing licoflavone, phenethyl resorcinol, propylene glycol and glycerol, heating to 85deg.C for dissolving to form oil phase solution; mixing the water phase liquid and the oil phase liquid, stirring uniformly, putting into a fermentation tank, adding kojic acid and glucose, and fermenting at 30 ℃ for 3 days to prepare a base liquid; respectively oven drying folium Vaccinii Vitis-idaeae, glycyrrhrizae radix, ginseng radix and herba Saussureae Involueratae, grinding into powder, adding endothelin antagonist, and mixing completely to obtain medicinal powder; and uniformly scattering the medicinal powder into the base solution to obtain the cosmetic. However, the endothelin antagonist adopted by the invention is easy to produce adverse reactions such as edema and the like, and the safety aspect is to be verified.

The natural components with the pore-shrinking effect can better overcome the defects, but the natural components are mostly sensitive and are easily decomposed under the influence of light and heat, and the stability is poor, so that the original functions are lost. The microemulsion technology has good loading capacity and stability for hydrophilic and hydrophobic components, acts on the stratum corneum of the skin, can strengthen the mobility of lipid bilayer of the stratum corneum, and weakens the skin barrier effect, thereby effectively improving the percutaneous permeability of substances. Meanwhile, the microemulsion and the nanoemulsion have good fluidity, adjustable viscosity and pleasant skin feel, and are easy to be accepted by consumers.

Disclosure of Invention

Aiming at the defects of the prior art, the invention aims to provide a composition with the effect of pore refinement, nano-microemulsion and a preparation method and application thereof, and in particular provides a composition with the effect of pore refinement, nano-microemulsion with the effect of pore refinement and a preparation method thereof, and essence emulsion with the effect of pore refinement and a preparation method thereof.

In order to achieve the aim of the invention, the invention adopts the following technical scheme:

in a first aspect, the present invention provides a composition having pore-refining efficacy comprising a fucus seradix extract, dipalmitoyl hydroxyproline, and dipeptidediamino Ding Xianbian-based amide diacetate.

The invention creatively discovers that the composition consisting of three components of the fucus seradix extract, the dipalmitoyl hydroxyproline and the dipeptide diamino Ding Xianbian-based amide diacetate can interact and positively influence each other, wherein the fucus seradix extract balances skin grease and plays a role in shrinking pores from root sources; wherein dipalmitoyl hydroxyproline is an important raw material for synthesizing collagen, and supplements collagen to support pores; the dipeptide diamino Ding Xianbian-based amide diacetate can smooth skin, and the dipeptide diamino Ding Xianbian-based amide diacetate and the dipeptide diamino diacetate have synergistic effect which is unexpected by the person skilled in the art on the efficacy of pore refinement, so that the dipeptide diamino Ding Xianbian-based amide diacetate can more effectively smooth skin and shrink pores. The composition is very suitable for skin care products, is mild and non-irritating, is suitable for sensitive skin, and has good stability.

Preferably, the composition with pore-refining effect comprises, by mass, 5-20 parts of a fucus seradix extract, 2-10 parts of dipalmitoyl hydroxyproline and 2-10 parts of dipeptide diamino Ding Xianbian-based amide diacetate.

When the three components are combined in a specific mass ratio, the effects of refining pores are more remarkable and mutually promoted.

The mass fraction of the fucus serrulata extract can be 5 parts, 7 parts, 8 parts, 10 parts, 12 parts, 14 parts, 16 parts, 18 parts, 20 parts and the like.

The mass parts of the dipalmitoyl hydroxyproline can be selected from 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts and the like.

The mass parts of the dipeptide diamino Ding Xianbian-based amide diacetate can be 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts and the like.

Other specific point values in the numerical ranges are selectable, and will not be described in detail herein.

In a second aspect, the present invention provides a nano-microemulsion having pore-shrinking effect, wherein the nano-microemulsion having pore-shrinking effect is prepared from the composition having pore-shrinking effect, the surfactant, the polyol and the water according to the first aspect.

The invention creatively utilizes the microemulsion technology to encapsulate the composition, can improve the stability of the composition, helps the composition to stay and permeate in pores, improves the permeability and sebaceous gland enrichment, and is slowly released and takes effect for a long time.

Preferably, the nano-microemulsion with pore-shrinking effect is prepared from, by mass, 10-30 parts of the composition with pore-shrinking effect, 15-30 parts of a surfactant, 5-15 parts of a polyol and 30-70 parts of water.

When the composition, the surfactant, the polyol and the water are combined in the specific mass ratio relationship, the system is more stable on the basis of ensuring the optimized efficacy of the nano-microemulsion.

The mass fraction of the composition can be 10 parts, 12 parts, 14 parts, 16 parts, 18 parts, 20 parts, 22 parts, 24 parts, 26 parts, 28 parts, 30 parts, etc.

The mass parts of the surfactant can be 15 parts, 17 parts, 18 parts, 20 parts, 22 parts, 24 parts, 25 parts, 26 parts, 28 parts, 29 parts, 30 parts and the like.

The mass parts of the polyol may be selected from 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, etc.

The water may be selected from 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, 65 parts, 70 parts, etc.

Preferably, the surfactant includes a nonionic surfactant and an anionic surfactant.

The nonionic surfactant is selected from any one or a combination of at least two of tween, span, polyglycerol oleate, castor oil polyoxyethylene ether or polyoxyethylene ether hydrogenated castor oil.

The anionic surfactant is selected from any one or a combination of at least two of sodium stearyl glutamate, sodium stearyl lactate, potassium cetyl phosphate or sodium N-stearyl-N-methyl taurate.

Preferably, the surfactant comprises tween, span and sodium stearyl lactate.

The surfactant in the nano-microemulsion product is more preferably a combination of tween, span and sodium stearyl lactate, because the surfactant in the combination mode can ensure that the nano-microemulsion system is longer and more effective and stable, thereby maintaining the stability and the considerable permeability of the efficacy composition.

Preferably, the polyol comprises any one or a combination of at least two of glycerol, 1, 3-butanediol, polyethylene glycol, propylene glycol, hexylene glycol or polypropylene glycol.

In a third aspect, the present invention provides a method for preparing the nano-microemulsion having pore-shrinking effect according to the second aspect, the method comprising:

mixing and dissolving dipalmitoyl hydroxyproline and a surfactant to obtain a solution A; mixing and dissolving the Fucus vesiculosus extract, dipeptide diamino Ding Xianbian-base amide diacetate, polyalcohol and water to obtain solution B; and mixing and homogenizing the solution A and the solution B to obtain the nano-microemulsion with the effect of refining pores.

The preparation method of the nano-microemulsion is simple and easy to implement, and is very suitable for industrial scale-up production. The prepared nano-microemulsion has small liquid drops, can overcome unstable factors in some emulsion systems, can improve the stability of the composition, helps the composition to stay and permeate in pores, improves the permeability, enriches sebaceous glands, and slowly releases and takes effect for a long time.

Preferably, the mixing and dissolving of dipalmitoyl hydroxyproline with the surfactant is performed at 45-60 ℃, for example, 45 ℃, 50 ℃, 55 ℃, 60 ℃, etc.

Preferably, the mixing and dissolving of the Fucus vesiculosus extract, the dipeptide diamino Ding Xianbian-yl amide diacetate, the polyol and the water is performed at 15-40 ℃, for example 15 ℃, 20 ℃, 25 ℃,30 ℃, 35 ℃, 40 ℃, etc.

Preferably, the mixing and homogenizing are performed at 15-40deg.C (e.g., 15deg.C, 20deg.C, 25deg.C, 30deg.C, 35deg.C, 40deg.C, etc.) for 5-15min (e.g., 5min, 8min, 10min, 12min, 15min, etc.).

The preparation method of the nano-microemulsion with pore-shrinking effect specifically comprises the following steps:

heating dipalmitoyl hydroxyproline, tween-65, sodium stearyl lactate and span 80 to dissolve at 45-55deg.C, and performing vortex oscillation with vortex oscillator until the materials are mixed uniformly to obtain solution A; dissolving Fucus vesiculosus extract, dipeptide diamino Ding Xianbian-base amide diacetate and propylene glycol in water, and mixing at 15-40deg.C to obtain solution B; mixing the solution A and the solution B, mixing at 15-40deg.C, and oscillating with turbine for 5-15min to obtain the final product.

In a fourth aspect, the invention provides the composition with pore-shrinking effect of the first aspect or the application of the nano-microemulsion with pore-shrinking effect of the second aspect in preparation of cosmetics.

The composition or the nano-microemulsion with the pore-shrinking effect can be suitable for cosmetics with various effects and various dosage forms, such as toning lotion, emulsion, facial mask, facial cleaning product, makeup removing product and the like. Other commonly used functional components such as whitening component (nicotinamide, glutathione, etc.), antioxidant component (such as coenzyme Q10, vitamin E, tocopherol acetate, etc.), and moisturizing component (hyaluronic acid, sodium hyaluronate, hydrolyzed collagen, etc.) can be added into the cosmetics according to actual needs.

In a fifth aspect, the invention provides an essence emulsion with pore-shrinking effect, which is prepared from the nano microemulsion with pore-shrinking effect, an emulsifying agent, a thickening agent, an emollient, a pH regulator and water.

Preferably, the raw materials for preparing the essence milk with pore-refining effect further comprise any one or a combination of at least two of a filler, a preservative, a fragrance and an antioxidant.

Such as diatomaceous earth, titanium dioxide, and the like. Such as sodium benzoate, phenoxyethanol, and the like. Such as various fragrances and the like. Such as lactic acid, arginine, and the like. Such as tocopheryl acetate, and the like.

Preferably, the emollient comprises any one or a combination of at least two of glycerin, butylene glycol, squalane, ethyl nonanoate, caprylic capric triglyceride, dimethiconol, or stearyl alcohol.

Preferably, the thickener comprises any one or a combination of at least two of carbomers, hydroxyethyl cellulose, tara gum, sclerotium gum, pectin, ammonium acrylodimethyltaurate/behenate polyether-25 methacrylate cross-linked polymer or acrylic acid (ester) class/C10-30 alkanol acrylate cross-linked polymer.

Preferably, the emulsifier comprises any one or a combination of at least two of dipalmitin, glycerol stearate, C12-20 alkyl glucosides, coco glucoside, sucrose stearate or hydrogenated lecithin.

In a sixth aspect, the present invention provides a method for preparing the essence milk with pore-shrinking effect according to the fifth aspect, the method comprising:

dispersing the thickener in water, mixing with the emollient and the pH regulator, homogenizing, mixing with the emulsifier, emulsifying, and mixing with the nanometer microemulsion to obtain the essence emulsion with pore-refining effect.

The preparation method of the essence emulsion is simple and easy to implement and is very suitable for industrial scale-up production.

Preferably, the preparation raw material for carrying out the mixing and homogenizing further comprises any one or a combination of at least two of a filler, a preservative, a fragrance and an antioxidant.

Compared with the prior art, the invention has the following beneficial effects:

The invention also creatively utilizes the microemulsion technology to carry out encapsulation on the composition to obtain a nano microemulsion product, which can improve the stability of the composition, help the composition to stay and permeate in pores, improve the permeability and sebaceous gland enrichment, and slowly release and take effect for a long time.

The composition or the nano-microemulsion with the effect of refining pores can be suitable for cosmetics with various effects and various dosage forms, is mild and non-irritating, and has good stability.

Drawings

FIG. 1 is a statistical plot of the effect of application example 1 samples on skin pore feature count;

FIG. 2 is a statistical plot of the effect of application example 1 samples on skin pore scores;

FIG. 3 is a statistical plot of the effect of application example 1 samples on skin pore percentile;

FIG. 4 is a statistical plot of the effect of application example 1 samples on the number of skin pores;

FIG. 5 is a statistical plot of the effect of application example 1 samples on the average area of skin pores;

FIG. 6 is a statistical plot of the effect of application example 1 samples on skin pore area ratio;

fig. 7 is a graph showing improvement of facial pores of the subject before and after the sample was used in application example 1.

Detailed Description

In order to further describe the technical means adopted by the present invention and the effects thereof, the following describes the technical scheme of the present invention in combination with the preferred embodiments of the present invention, but the present invention is not limited to the scope of the embodiments.

The sources of the functional components contained in the products related to the following examples, comparative examples, application examples and comparative application examples are as follows (only the functional components are represented, and the essential auxiliary material components contained in other commercial raw materials are not described in detail):

dipalmitoyl hydroxyproline is derived from a product commercially available from Kang Disi chemical industry (Hubei) limited under the trade name dipalmitoyl hydroxyproline;

the Fucus vesiculosus extract is derived from a product purchased from Majia trade company, calif. in Guangzhou, under the trade name Fucus vesiculosus extract;

dipeptide diamino Ding Xianbian-yl amide diacetate is available from the Wohan der waals biotechnology Co., ltd under the trade name dipeptide diamino Ding Xianbian-yl amide diacetate;

the acrylate/C10-30 alkyl acrylate crosslinked polymer was obtained from a product available from Guangzhou macroengineering biotechnology Co., ltd under the trade name acrylate/C10-30 alkyl acrylate crosslinked polymer;

hydroxyethyl cellulose is derived from a product available under the trade name hydroxyethyl cellulose from Shanghai Ming chemical Co., ltd;

the dimethiconol is derived from a product available from south Beijing Bemula Biotechnology Co., ltd under the trade name dimethiconol;

caprylic capric triglyceride is derived from a product commercially available from Shanghai source streams biotechnology Co.

Example 1

The embodiment provides a nano microemulsion with pore-shrinking effect, and the preparation method comprises the following steps:

(1) Mixing and dissolving 5 parts of dipalmitoyl hydroxyproline, 12 parts of tween-65, 8 parts of sodium stearyl lactate and 80 parts of span at 50 ℃, and carrying out vortex oscillation by a vortex oscillator after dissolving until the raw materials are uniformly mixed to obtain solution A;

(2) Mixing 10 parts of Fucus vesiculosus extract, 5 parts of dipeptide diamino Ding Xianbian-base amide diacetate, 9 parts of propylene glycol and 48 parts of water at 35 ℃ for dissolving to obtain solution B;

(3) Mixing the solution A and the solution B, and carrying out turbine oscillation for 10min at 35 ℃ to obtain the nano-microemulsion with pore-refining effect.

Example 2

(1) Mixing 2 parts of dipalmitoyl hydroxyproline with 8 parts of tween-80, 10 parts of sodium stearyl lactate and 80 parts of span at 50 ℃ for dissolution, and carrying out vortex oscillation by a vortex oscillator after dissolution until the raw materials are uniformly mixed to obtain solution A;

(2) Mixing 15 parts of Fucus vesiculosus extract, 3 parts of dipeptide diamino Ding Xianbian-base amide diacetate, 12 parts of 1, 3-butanediol and 45 parts of water at 35 ℃ for dissolving to obtain solution B;

Example 3

(1) 8 parts of dipalmitoyl hydroxyproline, 12 parts of tween-65, 8 parts of sodium stearoyl glutamate and 80 parts of span are mixed and dissolved at 50 ℃, and vortex oscillation is carried out by a vortex oscillator after dissolution until the raw materials are uniformly mixed, so as to obtain solution A;

(2) 8 parts of a fucus serrulata extract, 4 parts of dipeptide diamino Ding Xianbian-base amide diacetate, 10 parts of hexanediol and 47 parts of water are mixed and dissolved at 35 ℃ to obtain a solution B;

Example 4

The present example provides a nano microemulsion having pore-shrinking effect, and the preparation method is different from that of example 1 only in that the formulation of the surfactant is different, and 12 parts of tween-65, 8 parts of sodium stearyl lactate and 80 parts of span are replaced by 15 parts of tween-65 and 8 parts of sodium stearyl lactate. The other components remained unchanged, and the preparation method is described in example 1.

Example 5

The present example provides a nano microemulsion having pore-shrinking effect, and the preparation method is different from that of example 1 only in that the formulation of the surfactant is different, and 12 parts of tween-65, 8 parts of sodium stearyl lactate and 80 parts of span are replaced by 80 15 parts of span and 8 parts of sodium stearyl lactate. The other components remained unchanged, and the preparation method is described in example 1.

Example 6

The present example provides a nano microemulsion having pore-shrinking effect, and the preparation method is different from that of example 1 only in that the formulation of the surfactant is different, and 12 parts of tween-65, 8 parts of sodium stearyl lactate and 80 parts of span are replaced by 18 parts of tween-65 and 80 parts of span. The other components remained unchanged, and the preparation method is described in example 1.

Comparative example 1

The comparative example provides a nano-microemulsion, the preparation method of which is different from that of example 1 only in that dipalmitoyl hydroxyproline is not contained in the preparation raw materials, and the mass parts of the dipalmitoyl hydroxyproline are distributed to the mass parts of the fucus seradix extract and the dipeptide diamino Ding Xianbian-based amide diacetate, and the nano-microemulsion is specifically as follows:

(1) Mixing and dissolving 12 parts of tween-65, 8 parts of sodium stearyl lactate and 80 parts of span at 50 ℃, and carrying out vortex oscillation by a vortex oscillator after dissolving until the raw materials are uniformly mixed to obtain solution A;

(2) Mixing and dissolving 13.5 parts of Fucus vesiculosus extract, 6.5 parts of dipeptide diamino Ding Xianbian-base amide diacetate, 9 parts of propylene glycol and 48 parts of water at 35 ℃ to obtain solution B;

Comparative example 2

The comparative example provides a nano-microemulsion, the preparation method of which is different from that of example 1 only in that the preparation raw material does not contain the fucus extract of the edge of tooth, and the mass parts of the fucus extract are distributed to the mass parts of dipalmitoyl hydroxyproline and dipeptide diamino Ding Xianbian-base amide diacetate, and the nano-microemulsion is specifically as follows:

(1) 10 parts of dipalmitoyl hydroxyproline, 12 parts of tween-65, 8 parts of sodium stearyl lactate and 80 parts of span are mixed and dissolved at 50 ℃, and vortex oscillation is carried out by a vortex oscillator after dissolution until the raw materials are uniformly mixed, so as to obtain solution A;

(2) Mixing and dissolving 10 parts of dipeptide diamino Ding Xianbian-base amide diacetate, 9 parts of propylene glycol and 48 parts of water at 35 ℃ to obtain a solution B;

Comparative example 3

The comparative example provides a nano-microemulsion, the preparation method of which is different from that of example 1 only in that the preparation raw material does not contain dipeptide diamino Ding Xianbian-based amide diacetate, and the mass parts of the dipeptide diamino Ding Xianbian-based amide diacetate are distributed on the mass of dipalmitoyl hydroxyproline and the fucus seradix extract, and the nano-microemulsion is specifically as follows:

(1) Mixing and dissolving 6.5 parts of dipalmitoyl hydroxyproline, 65 parts of tween-65, 8 parts of sodium stearyl lactate and 80 parts of span at 50 ℃, and carrying out vortex oscillation by a vortex oscillator after dissolving until the raw materials are uniformly mixed to obtain solution A;

(2) Mixing and dissolving 13.5 parts of Fucus vesiculosus extract, 9 parts of propylene glycol and 48 parts of water at 35 ℃ to obtain solution B;

Application example 1

The application example provides essence emulsion with pore-shrinking effect, which comprises the following formula:

the preparation method comprises the following steps:

wetting and dispersing the thickener in water completely to obtain a mixed solution; then adding an emollient, a filler and a pH regulator into the mixed solution, heating to 65 ℃, homogenizing for 3min at 3000r/min to ensure that the mixture is completely dispersed; adding emulsifier, homogenizing at 3000r/min for 3min to completely emulsify, stirring, cooling to 30deg.C, and adding nanometer microemulsion.

Application examples 2 to 6

The present application example provides five kinds of essence emulsions having pore-refining effect, and the formulation is different from that of application example 1 only in that the nano-microemulsion of example 1 is replaced by the nano-microemulsion of examples 2 to 6 in equal amount. The other components remained unchanged, and the preparation method is described in application example 1.

Comparative application examples 1 to 3

The present comparative application example provides three kinds of essence emulsions, and the formulation thereof is different from that of application example 1 only in that the nano-microemulsion of example 1 is replaced with the nano-microemulsion of comparative examples 1 to 3 in equal amount. The other components remained unchanged, and the preparation method is described in application example 1.

Comparative application example 4

The present comparative application example provides an emulsion whose formulation differs from application example 1 only in that the nanoemulsion of example 1 is absent, the reduction being made up by water.

Test example 1

Skin safety test:

placing the products prepared in application examples 1-6 in a patch tester, attaching the patch tester with the test object to the forearm flexor side of the tested person (33), and uniformly applying the patch to skin by lightly pressing the palm for 24 hours; skin irritation and sensitization were observed according to table 1 (skin response grading standard of skin seal patch test) 30min, 24 hr, and 48 hr after removal of the subject patch tester, respectively, and the observation results were recorded.

TABLE 1

The results show that the products of application examples 1-6 have scoring grades of 0 at 30min, 24 h and 48 h, and have no adverse skin reaction, which indicates that the composition, the nano-microemulsion and the essence emulsion products related to the invention have no irritation to skin.

Test example 2

Pore improvement effect evaluation:

the subjects were 90 Chinese healthy sensitive myofemales aged between 27 and 48 years, with an average age of 36.90 + -5.24 years, randomized into 9 groups of 10 individuals each, using the products of application examples 1-6 and comparative application examples 1-3, respectively. The subjects gave written consent with informed. The subject would like to coordinate and understand the necessity and duration of control in order to follow the protocol established by the clinical trial center. Half-face experiments were performed with controls of the blank group (comparative application example 4), once a day each morning and evening, the usage method and usage amount were consistent, and the subjects filled in self-evaluation questionnaires by taking a picture of the VISIA, primos CR at D0, D14 and D28, respectively, for 28 consecutive days. The data is counted by adopting SPSS 28.0, normal distribution inspection is carried out on the test data, and if the test data is normal distribution, a T inspection method is adopted for statistical analysis; and if the test data are in non-normal distribution, analyzing and counting by adopting a rank sum test method. Rank sum test is used for statistical analysis of the rank data. Statistical method significance level p < 0.05.

(1) Skin pores (VISIA) (cheek):

and acquiring and photo-analyzing the facial image information by using the VISIA. The feature count means that the feature parameters are counted, the size and the intensity of the feature parameters are not calculated, the value is small, and the skin is good; the score represents the evaluation of the size, area and intensity of the characteristic parameters, and the score is smaller, which indicates that the skin is better. The statistical results are shown in Table 2, wherein statistical graphs of the effects of the application example 1 sample on the skin pore characteristic count, the skin pore score, and the skin pore percentile are shown in FIGS. 1-3, respectively.

TABLE 2

As can be seen from the data in table 2: after 14 days of using the essence emulsion of application example 1, the characteristic count of skin pores of the cheek is reduced by 3.26%, the score of skin pores is reduced by 6.11%, and the percentile of skin pores is reduced by 2.20%; after 28 days of use of the sample, the characteristic count of skin pores of the cheek was reduced by 3.93%, the score of skin pores was reduced by 13.40%, and the percentile of skin pores was reduced by 7.98% without significance. The effect is obviously better than that of a comparative application example, and the effects of the Fucus vesiculosus extract, the dipalmitoyl hydroxyproline and the dipeptide diamino Ding Xianbian-based amide diacetate have the synergistic effect which is unexpected by the technicians in the field on the efficacy of refining pores, so that the skin is smoothed more effectively and the pores are shrunk.

(2) Skin pore (VISIA & IPP) (cheek)

The VISIA was used for facial Image acquisition and photo analysis in combination with Image-pro skin analysis software. The smaller skin pore analysis value indicates an improvement in skin pores, and the statistical results are shown in table 3 (average rate of decrease of 10 persons per group). Statistical graphs of the effects of the application example 1 sample on the number of skin pores, the average area of the skin pores and the ratio of the area of the skin pores are shown in fig. 4 to 6, respectively.

TABLE 3 Table 3

As can be seen from the data in table 3: the nano-microemulsion and the essence emulsion prepared from the nano-microemulsion have excellent pore-refining effect, and the data of comparative application examples 1 and 1-3 show that three components of the edge of tooth Fucus vesiculosus extract, the dipalmitoyl hydroxyproline and the dipeptide diamino Ding Xianbian-based amide diacetate have synergistic promotion effect on pore-improving effect.

(3) Randomly selecting a subject of application example 1, observing and comparing pore conditions of the face on about 0 day, 14 day and 28 day of the test, wherein black spots are marked pores, as shown in fig. 7, a left face uses an application example 1 sample, a right face uses a blank group sample, the black marks of the left face are reduced after 14 days, and the black marks of the left face are obviously reduced after 28 days; the right face has no obvious change.

Test example 3

Stability test:

(1) Centrifugal experiment: the samples of examples 1 to 6 were subjected to centrifugation at 25℃for 30min at 3000r/min, respectively, and the samples were observed for delamination.

(2) Thermal stability experiments: samples of examples 1 to 6 were placed in a constant temperature environment of (50.+ -. 1) ℃ for 30 days, and the phenomenon of the samples was observed.

The results are shown in Table 4:

TABLE 4 Table 4

Group of	Centrifugal test	Thermal stability test
			Example 1	Normal state	No abnormality
Example 2	Normal state	No abnormality
			Example 3	Normal state	No abnormality
Example 4	Precipitation is achieved, and shaking can be uniformly carried outPowder medicine	Precipitation and uniform dispersion by shaking
			Example 5	Precipitation and uniform dispersion by shaking	Precipitation and uniform dispersion by shaking
Example 6	Precipitation and uniform dispersion by shaking	Precipitation and uniform dispersion by shaking

From the results shown in table 4, the nano-microemulsion and the essence emulsion prepared from the nano-microemulsion have good stability through the optimized selection of the surfactant, and the centrifugal experiment and the thermal stability experiment are free from abnormalities, so that the nano-microemulsion system is longer and more effective and stable, and the stability and the considerable permeability of the efficacy composition can be maintained.

The applicant states that the present invention is illustrated by the above examples as a composition, nanoemulsion, and method of preparation and application thereof having pore-shrinking effect, but the present invention is not limited to the above examples, i.e. it does not mean that the present invention must be practiced by the above examples. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.

The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.

In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.

Claims

1. A composition having pore-shrinking effect, wherein the composition comprises a fucus seradix extract, dipalmitoyl hydroxyproline, and dipeptidediamino Ding Xianbian-based amide diacetate.

2. The composition with pore-shrinking effect according to claim 1, wherein the composition with pore-shrinking effect comprises, in parts by mass, 5-20 parts of a fucus seradix extract, 2-10 parts of dipalmitoyl hydroxyproline and 2-10 parts of dipeptidyl diamino Ding Xianbian-ylamide diacetate.

3. A nano-microemulsion having pore-enlarging effect, wherein the raw materials for preparing the nano-microemulsion having pore-enlarging effect comprise the composition having pore-enlarging effect, according to claim 1 or 2, a surfactant, a polyol and water;

preferably, the nano-microemulsion with pore-refining effect is prepared from the raw materials of 10-30 parts by mass of the composition with pore-refining effect of claim 1 or 2, 15-30 parts by mass of surfactant, 5-15 parts by mass of polyol and 30-70 parts by mass of water.

4. The nano-microemulsion having pore-refining efficacy according to claim 3, wherein said surfactant comprises a nonionic surfactant and an anionic surfactant;

the nonionic surfactant is selected from any one or a combination of at least two of tween, span, polyglycerol oleate, castor oil polyoxyethylene ether or polyoxyethylene ether hydrogenated castor oil;

the anionic surfactant is selected from any one or a combination of at least two of sodium stearyl glutamate, sodium stearyl lactate, potassium cetyl phosphate or sodium N-stearyl-N-methyl taurate;

preferably, the surfactant comprises tween, span and sodium stearyl lactate;

5. The method for preparing nano-microemulsion having pore-shrinking effect according to claim 3 or 4, wherein said method comprises:

6. The method for preparing a nano-microemulsion having pore-refining effect according to claim 5, wherein said mixing and dissolving dipalmitoyl hydroxyproline with a surfactant is carried out at 45-60 ℃;

preferably, the mixing and dissolving of the fucus serrulata extract, the dipeptide diamino Ding Xianbian-yl amide diacetate, the polyalcohol and the water is carried out at 15-40 ℃;

preferably, the mixing and homogenizing is carried out at 15-40deg.C for 5-15min.

7. Use of the composition with pore-shrinking effect of claim 1 or 2 or the nano-microemulsion with pore-shrinking effect of claim 3 or 4 in the preparation of cosmetics.

8. The essence emulsion with pore-shrinking effect is characterized in that the preparation raw materials of the essence emulsion with pore-shrinking effect comprise the nano microemulsion with pore-shrinking effect, an emulsifying agent, a thickening agent, an emollient, a pH regulator and water according to claim 3 or 4.

9. The essence emulsion with pore-shrinking effect according to claim 8, wherein the raw materials for preparing the essence emulsion with pore-shrinking effect further comprise any one or a combination of at least two of a filler, a preservative, a fragrance and an antioxidant;

preferably, the emollient comprises any one or a combination of at least two of glycerin, butylene glycol, squalane, ethyl nonanoate, caprylic capric triglyceride, dimethiconol, or stearyl alcohol;

preferably, the thickener comprises any one or a combination of at least two of carbomers, hydroxyethyl cellulose, tara gum, sclerotium gum, pectin, ammonium acryloyldimethyl taurate/behenate-25 methacrylate cross-linked polymer or acrylic acid (ester) class/C10-30 alkanol acrylate cross-linked polymer;

10. The method for preparing the essence cream with pore-shrinking effect according to claim 8 or 9, wherein the method comprises the following steps:

dispersing a thickening agent in water, mixing with an emollient and a pH regulator, homogenizing, mixing with an emulsifying agent, emulsifying, and mixing with nano microemulsion to obtain the essence emulsion with the effect of refining pores;