CN112870108A

CN112870108A - Composition with anti-aging and moisturizing effects and preparation method and application thereof

Info

Publication number: CN112870108A
Application number: CN202110169720.0A
Authority: CN
Inventors: 孟庆洋; 李基西; 林贞翔; 罗丹; 周秋娜; 胡霞云; 金荣熙; 金延埈
Original assignee: Shanghai Baiqueling Biotechnology Co ltd; Cosmax China Cosmetics Co Ltd
Current assignee: Shanghai Baiqueling Biotechnology Co ltd; Cosmax China Cosmetics Co Ltd; Cosmax China Inc
Priority date: 2021-02-07
Filing date: 2021-02-07
Publication date: 2021-06-01

Abstract

The invention provides a composition with anti-aging and moisturizing effects, and a preparation method and application thereof. The composition consists of hyaluronic acid microcapsules and active matter liposomes, the active matter is wrapped by the microcapsules and the liposomes, the active matter is slowly released, the utilization rate of the active matter is improved, and the stability of the microcapsules and the liposomes is improved. By adjusting the proportion of the hyaluronic acid microcapsules and the active substance liposome, better anti-aging and moisturizing effects are achieved. Through the microcapsule and the liposome, the composition has better functions of moisturizing the surface layer, supplementing sodium hyaluronate deeply and promoting the synthesis of collagen, and finally achieves the aims of resisting aging and moisturizing.

Description

Composition with anti-aging and moisturizing effects and preparation method and application thereof

Technical Field

The invention belongs to the field of cosmetics, and particularly relates to a composition with anti-aging and moisturizing effects, and a preparation method and application thereof.

Background

With the development of the human society, the aging of the population is accelerated, and the aging problem becomes a relatively concerned problem in the whole society. With age, the morphological structure and physiological function of the skin change. Skin aging is the result of multiple factors, and stress, strain, injury, infection, malnutrition, metabolic disorders, and drug abuse can affect skin condition. Healthy skin is smooth, moist and elastic, free radicals destroy collagen and active substances in normal cell membrane tissues to form fine lines and wrinkles, and dry lines are formed when the skin is evaporated, lacks water and loses elasticity.

The anti-aging products on the market mainly use active substances with the efficacy of repairing damaged skin to reduce fine lines and wrinkles and omit dry lines, and a penetration enhancer is used for accelerating the absorption of active ingredients by the skin. Penetration enhancers do not selectively promote the absorption of active ingredients by the skin and may also promote the entry of some irritating ingredients into the skin causing skin irritation.

As a common means for wrapping active substances in cosmetics in recent years, the liposome and the microcapsule have the problems of no high temperature resistance, no color change, no leakage and no good storage while improving the utilization rate of the active substances, so that the liposome and the microcapsule cannot be applied to more cosmetics.

Disclosure of Invention

In order to solve the problem that anti-aging active substances effectively enter skin and simultaneously reduce irritation and dry lines in the prior art, the invention provides an anti-aging and moisturizing composition, hyaluronic acid microcapsules and active substance liposomes with different proportions, so that irritation is reduced, absorption of the skin on the composition is improved, sodium hyaluronate is supplemented to the skin, collagen is promoted to be generated, a damaged skin barrier is repaired, the generation of dry lines and fine lines is reduced, and the anti-aging and moisturizing purpose is achieved. At the same time, the anti-aging composition improves the stability of the microcapsules and the active substance liposome, and can stably exist in the cosmetic formula

The technical scheme of the invention is as follows:

the invention provides a composition with anti-aging and moisturizing effects, which comprises the following components in parts by weight, namely hyaluronic acid microcapsules, wherein active liposome is (1-5) to (1-5);

the hyaluronic acid microcapsule is a microcapsule wrapping hyaluronic acid derivatives;

the active substance liposome is a liposome which wraps the active substance;

the hyaluronic acid derivative comprises one or more of hyaluronic acid, hyaluronate and other hyaluronic acid derivatives;

the active matter comprises rutting pavilion-based disodium sulfate, hydroxyproline, magnesium ascorbyl phosphate and peptides, wherein the ratio of the rutting pavilion-based disodium sulfate to the hydroxyproline to the magnesium ascorbyl phosphate is 1:1: 0.1: 0.1;

the peptides are preferably selected from one or more of palmitoyl pentapeptide-4, acetyl hexapeptide-8, carnosine, palmitoyl tripeptide-5, palmitoyl tripeptide-1, palmitoyl tetrapeptide-7, tripeptide-1, acetyl tetrapeptide-3, dipeptide-2 and acetyl octapeptide-3.

Preferably, the composition comprises the following components in parts by weight, namely the hyaluronic acid microcapsules, wherein the active liposome is (1-5) to (1-3).

Preferably, the composition comprises the following components in parts by weight: the active liposome is 3:1 or 5: 2.

In another aspect, the present invention provides a method for preparing a composition, comprising the steps of:

1) adding 1-3 parts of glycerol and 1-3 parts of water into the active substance liposome according to a proportion, homogenizing for 1-2 minutes at a homogenizing speed of 6000-;

2) adding 0.05-0.1 part of thickening agent and 4-5 parts of water into the hyaluronic acid microcapsule according to the proportion, and uniformly mixing for later use;

3) slowly adding the materials obtained in the step 1) into the mixture obtained in the step 2) while stirring, uniformly mixing, homogenizing the obtained materials for 1-2 minutes by using a high-pressure homogenizer, and filtering by using a 1-micron filter to obtain the composition, wherein the components are in parts by weight.

Preferably, the preparation of the hyaluronic acid microcapsule comprises the following steps:

1) adding 0.6 part of hyaluronic acid derivative into 20-25 parts of water, and uniformly stirring to obtain a first component for heat preservation for later use;

2) adding 20-30 parts of surfactant into 40-45 parts of water, and uniformly stirring at 60-80 ℃ to obtain a second component for heat preservation and standby;

3) slowly dripping the first component into the second component, and adjusting pH with citric acid to obtain hyaluronic acid microcapsule.

Preferably, the preparation method of the active substance liposome comprises the following steps:

1) stirring 3 parts of lecithin and 40-60 parts of ethanol to obtain a third component, and evaporating the ethanol on a rotary evaporator to form a transparent film;

2) ultrasonically stirring water and active substances uniformly according to the proportion of 80:1, and keeping the temperature for later use;

3) hydrating the substance obtained in step 2) on a rotary evaporator to make the film completely fall off, and performing ultrasonic treatment for 5-10min to obtain active substance liposome with ultrafiltration membrane pore diameter of 0.01-0.05 μm.

Preferably, the thickener is one or more of xanthan gum, sodium acrylate/sodium acryloyldimethyl taurate copolymer, sodium polyacrylate and ammonium acryloyldimethyl taurate/VP copolymer.

Preferably, the thickener is a sodium acrylate/sodium acryloyldimethyl taurate copolymer.

Preferably, the surfactant is a mixture of surfactants in a weight ratio of 17.5: 7.5 sucrose palmitate with glyceryl linoleate.

The invention also provides an application of the composition, and the composition is applied to the cosmetic field including but not limited to water, essence, emulsion, spray, cream, facial mask, foundation fluid and the like.

With age, the epidermis becomes thinner, the papilla of the dermis decreases, the nucleus shrinks, and apoptotic bodies appear in the cell. The fibrin positive structure is remarkably lost, so that the connection between the epidermis and the dermis of the skin is loosened, the synthesis rate of glycosaminoglycan (namely sodium hyaluronate) is lower than the degradation rate, the water retention capacity of the skin is reduced while wrinkles are caused to appear, the water content of the stratum corneum is reduced, and dry lines and fine lines are caused to appear. At the same time, free radicals and protein have saccharification reaction to produce AGEs as the end product of saccharification, which denatures collagen, makes skin hard, dark yellow and lose elasticity, and accelerates aging.

Therefore, the hyaluronic acid microcapsule and the active substance liposome are preferably used as the anti-aging moisturizing composition and act on the epidermal layer and the dermal layer, so that the anti-aging moisturizing composition brings multi-dimensional anti-aging moisturizing effect to the skin and has good stability. The hyaluronic acid microcapsule permeates skin through layer-by-layer slow release, and the sodium hyaluronate permeates the bottom of the skin to fill the skin while locking water and keeping moisture on the surface layer of the skin. The active substance liposome can enter skin through three ways of intercellular permeation, cell permeation and hair follicle permeation, the liposome membrane has a structure similar to that of human skin, and can easily penetrate skin, provide fatty acid for skin cell membrane, release linoleic acid from fatty acid, promote synthesis of skin ceramide, protect skin barrier, and improve skin moisture-retaining and water-locking capacity. The polypeptide encapsulated by the liposome can penetrate the deep layer of the skin, acetyl hexapeptide-8 simulates botulinum toxin, the release of neurotransmitter (Ach) is inhibited, excessive muscle contraction and tension are reduced, palmitoyl pentapeptide-4 can promote the generation of collagen, carnosine can effectively reduce the occurrence of saccharification reaction, the collagen and other structural proteins are protected from degradation, and the generation of wrinkles is reduced.

Drawings

FIG. 1 is a graph showing a statistic of wrinkle change rate in Experimental example 4.

Detailed Description

Embodiments of the present application will be described in detail by examples, so that how to apply technical means to solve technical problems and achieve technical effects of the present application can be fully understood and implemented.

The raw materials and equipment used in the present application are all common raw materials and equipment in the field, and are all from commercially available products, unless otherwise specified. The methods used in this application are conventional in the art unless otherwise indicated.

The preparation method of the anti-aging moisturizing composition comprises the following steps:

1) adding 3 parts of glycerol and 1 part of water into the active matter liposome according to the proportion, homogenizing for 2 minutes at the homogenizing speed of 6000-;

2) adding 0.08 part of sodium acrylate/sodium acryloyldimethyl taurate copolymer and 4 parts of water into the hyaluronic acid microcapsules according to the proportion, and uniformly mixing for later use;

3) slowly adding the materials obtained in the step 1) into the mixture obtained in the step 2) while stirring, uniformly mixing, homogenizing the obtained materials for 1 minute by using a high-pressure homogenizer, and filtering by using a 1-micron filter to obtain the composition, wherein the components are all in parts by weight.

The preparation method of the hyaluronic acid microcapsule comprises the following steps:

1) adding 0.6 part of hyaluronic acid derivative into 25 parts of water, and uniformly stirring to obtain a first component for heat preservation and standby;

2) adding 17.5 parts of sucrose palmitate and 7.5 parts of glycerol linoleate into 45 parts of water, and uniformly stirring at the temperature of 60-80 ℃ to obtain a second component, and keeping the temperature for later use;

The preparation method of the active substance liposome comprises the following steps:

1) stirring 3 parts of lecithin and 50 parts of ethanol to obtain a third component, and evaporating the ethanol on a rotary evaporator to form a transparent film;

The anti-aging and moisturizing compositions were tested for anti-aging, moisturizing effects, and comparative examples 1-3 and compositions 1-11 were prepared according to the following table 1 for stability and efficacy testing.

TABLE 1

Compositions containing active ingredients only, not containing liposomes and microencapsulation

The composition without liposome and microcapsule structure is prepared specifically as follows:

1) adding 0.6 part of hyaluronic acid derivative into 25 parts of water, uniformly stirring, and keeping the temperature for later use;

3) uniformly mixing the materials obtained in the steps 1) and 2), adding 3 parts of glycerol and 5 parts of water, and uniformly stirring for later use;

4) to the material obtained in 3) was added 0.08 part of a thickener, and the mixture was stirred uniformly and filtered through a 1 μm filter to obtain the composition used in comparative example 3.

Experimental example 1. cytotoxicity evaluation test: for testing the safety of the composition

MTT assay is an experimental method widely used for detecting cytotoxicity or cell proliferation by measuring the number of living cells, and the detection principle is that succinate dehydrogenase in mitochondria of the living cells can reduce water-soluble yellow salt MTT (3- (4, 5-dimethylthiazole-2) -2, 5-diphenyl tetrazolium bromide) into water-insoluble blue formazan and deposit the blue formazan in the cells, but dead cells do not have the function. The generated crystalline formazan is generally added with DMSO (dimethyl sulfoxide), and the absorbance is measured after dissolution. The specific experimental method is that the test solution is prepared according to the specification of 1X10 in a 96-well plate⁴Each of the cells was inoculated at a density of 100. mu.l each with DMEM medium containing 10% bovine serum and keratinocytes (HaCaT), and the medium was changed to serum-free medium after 24 hours of culture. The culture was carried out for 24 hours after the treatment by adding the compositions at different concentrations to serum-free medium, respectively. Thereafter, the medium was removed, treated with 20. mu.l of MTT solution, and allowed to react at 37 ℃ for 2 hours. The cell viability was calculated by adding 200 μ l of isopropanol to the cells from which the MTT solution was removed, gently shaking for 30min to completely dissolve the crystalline formazan, measuring the absorbance at 570nm, and calculating the cell viability according to the following equation.

The cytotoxicity results of the compositions 1 to 11 and the compositions obtained in comparative examples 1 to 3 are shown in Table 2.

TABLE 2

The cell viability as shown in Table 2 indicates that the components are not significantly cytotoxic.

EXAMPLE 2 Hyaluronidase inhibition experiment

Compositions 1 to 7 comparative examples 1 to 3 were each prepared as a 1% aqueous solution as a sample liquid. Adding into a test tube0.1mL 0.25mmol/L CaCl₂Mixing the solution with 0.5mL of hyaluronidase solution, and culturing at 37 deg.C for 20 min; adding 0.5mL of sample solution, and carrying out heat preservation culture at 37 ℃ for 20 min; adding 0.5mL of sodium hyaluronate solution, and keeping the temperature at 37 ℃ for 30 min; then standing for 5min at normal temperature, adding 0.1ml of 0.4mol/L NAOH solution and 0.5ml of acetylacetone solution, heating in a boiling water bath for reaction for 15min, and immediately carrying out ice bath for 5 min; then adding 1.0mL of Ellisib reagent, diluting with 3.0mL of absolute ethyl alcohol, standing for 20min, developing, measuring the absorbance value, and substituting into the following formula to calculate the inhibition rate.

Hyaluronidase inhibition (%) - (A-B) - (C-D) ]/(A-B) × 100%

In the formula: a is the absorbance value of the control solution (the sample solution is replaced by acetic acid buffer solution); b is the absorbance value of the blank control solution (acetic acid buffer solution is used for replacing the sample solution and the enzyme solution); c is the absorbance value of the tested sample solution; d is the absorbance value of the blank solution (the enzyme solution is replaced by acetic acid buffer solution)

The results of the hyaluronidase inhibition experiments are shown in table 3.

TABLE 3

The experimental results of table 3 show that:

(1) the hyaluronic acid microcapsule and the active substance liposome have more obvious inhibition effect on hyaluronidase than the combination of pure active substances, which shows that the hyaluronic acid microcapsule and the active substance liposome can improve the utilization rate of active ingredients;

(2) the inhibition rate of the hyaluronic acid microcapsule and the active substance liposome is higher than that of a single component on the hyaluronidase, which indicates that the hyaluronic acid microcapsule and the active substance liposome have a synergistic effect;

(3) the compositions with different proportions have different effects on the inhibition rate of the hyaluronidase, the compositions 3 and 7 have the most obvious effect on the inhibition rate of the hyaluronidase, the effect of reducing the decomposition rate of glycosaminoglycan in skin is better, and meanwhile, the compositions have good anti-inflammatory effect.

Experimental example 3 stability test was carried out on the compositions 3 and 7 and the comparative examples 1 and 2 to examine the stability of the compositions

The test method comprises the following steps: 50ml of each of the compositions 3 and 7 and comparative examples 1 and 2 was stored in a thermostat at a temperature of (-18, -7, 4, 25, 37, 45, 50 ℃), and after 30 days, it was observed whether or not there was any change in stability factors such as delamination, flocculation, precipitation, discoloration, unevenness, and the like.

And (4) conclusion: the stability test results are shown in table 4, after 30-day stability test, the compositions 3 and 7 do not find the occurrence of layering, flocculation, color change and nonuniformity, the comparative example 1 only contains hyaluronic acid microcapsules and finds that the low-temperature has slight flocculation and agglomeration phenomena, and the comparative example 2 only contains active liposome and has obvious color change at 37, 45 and 50 ℃, which indicates that the anti-aging composition has good stability.

TABLE 4

Experimental example 4.

Compositions 3 and 7 and comparative example 3 are respectively and correspondingly applied to the following examples 1, 2 and 3, and the specific formula is shown in table 5, and the specific formula is weight percentage.

TABLE 5

4.1 safety testing

Taking the essence milk obtained in the examples 1, 2 and 3, and placing the essence milk in a spot tester, wherein a control hole is a blank control; the spot tester with the tested object is attached to the bent side of the forearm of the tested person, and the tested person is lightly pressed by the palm to be uniformly attached to the skin for 24 hours; and observing the skin irritation and sensitization according to the skin reaction grading standard of the skin closed patch test in the table 6 after 30min, 24 hours and 48 hours after the test object patch tester is removed, and recording the observation results.

TABLE 6

The experimental results are as follows: the essential milks obtained in examples 1, 2 and 3 were subjected to a human skin patch test, and the results are shown in Table 7. The result of a human body skin patch test shows that 30 people have no skin adverse reaction, which shows that the essence milk prepared by the composition is safe, mild and free of irritation.

TABLE 7

4.28 h moisture test

Selecting the measurement area of forearm curvature of the subject to be 2 x 2cm²Smearing the essence milk prepared from 8 μ L of the product (examples 1 and 2, and blank control group) on the area to be detected, and patting with finger cot to absorb; measurements were performed using a Corneometer (CK, Germany) before use, 0h, 2h, 4h and 8h after use, respectively, and the same spot was averaged 3 times.

The experimental results are as follows: referring to table 8, the experimental results show that compared to example 3, the essential emulsions prepared in examples 1 and 2 of the present invention have very excellent instant moisturizing effect and can maintain higher moisture content after 8 hours, and at the same time, the hyaluronic acid microcapsules and the active liposome can provide moisturizing power to the epidermis and simultaneously permeate into the dermis, promote the synthesis of collagen glycosaminoglycan, and provide more excellent moisturizing effect.

TABLE 8

4.3.1 volunteer self-evaluation 4 weeks after using the product of example 1

31 female volunteers with various skin types were selected and evaluated in 28 days by using the product example 1 once in the morning and at night as shown in the following table 9, and after 28 days, 97% of the patients considered that their skin became moist, 87% of the patients considered that their fishtail lines appeared to be smoothed, and 85% of the patients considered that their fine lines on their faces were reduced, thereby indicating that the product of example 1 had significant anti-aging and moisturizing effects.

TABLE 9

4.3.2 instrumental analysis

31 female volunteers, face using product example 1, once in the morning and once in the evening, cured to replicate the skin texture using tacky and curable silicone gels with added catalyst, wrinkle area, length, depth were measured at D0 and D28. The results are shown in fig. 1, and show that the product of example 1 has the effect of obviously reducing the area, length and depth of wrinkles by applying twice a day and continuously applying for 28 days.

There are many other possible embodiments of the present invention, which are not listed here, and the embodiments claimed in the claims of the present invention can be implemented.

The details not described in the specification of the present application belong to the common general knowledge of those skilled in the art.

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. "substantially" means within an acceptable error range, and a person skilled in the art can solve the technical problem within a certain error range to substantially achieve the technical effect.

It is also noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a good or system that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such good or system. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a commodity or system that includes the element.

The foregoing description shows and describes several preferred embodiments of the present application, but as aforementioned, it is to be understood that the application is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as expressed herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the application, which is to be protected by the claims appended hereto.

Claims

1. A composition with anti-aging and moisturizing effects is characterized by comprising hyaluronic acid microcapsules, wherein the hyaluronic acid microcapsules comprise (1-5) active liposome and (1-5);

the active substance liposome is a liposome which wraps the active substance;

2. The composition of claim 1, wherein the composition comprises the following components in parts by weight, the hyaluronic acid microcapsules, the active liposome is (1-5) to (1-3).

3. The composition according to claim 2, wherein the composition comprises the following components in parts by weight, hyaluronic acid microcapsules: the active liposome is 3:1 or 5: 2.

4. A method of preparing the composition of claim 1, comprising the steps of:

3) slowly adding the materials obtained in the step 1) and stirring while adding the materials obtained in the step 2), uniformly mixing, homogenizing the obtained materials for 1-2 minutes by using a high-pressure homogenizer, and filtering by using a 1-micron filter to obtain the composition.

5. The method according to claim 4, wherein the hyaluronic acid microcapsules are prepared by the steps of:

6. The method of claim 4, wherein the method of preparing the liposome active agent comprises the steps of:

7. The preparation method of claim 4, wherein the thickener is one or more of xanthan gum, sodium acrylate/sodium acryloyldimethyl taurate copolymer, sodium polyacrylate and ammonium acryloyldimethyl taurate/VP copolymer.

8. The method of claim 7, wherein the thickener is preferably a sodium acrylate/sodium acryloyldimethyl taurate copolymer.

9. The method according to claim 4, wherein the surfactant is a mixture of surfactants in a weight ratio of 17.5: 7.5 sucrose palmitate with glyceryl linoleate.

10. Use of the composition of claim 1 for cosmetic applications including but not limited to water, serum, lotion, spray, cream, mask, foundation.