CN112870122A

CN112870122A - High-stability nano emulsion with light protection effect and preparation method thereof

Info

Publication number: CN112870122A
Application number: CN202110125375.0A
Authority: CN
Inventors: 施丽娟; 周春亚; 周秋娜; 金荣熙; 刘攀攀; 申彦晟; 金延埈
Original assignee: Cosmax China Cosmetics Co Ltd
Current assignee: Cosmax China Cosmetics Co Ltd
Priority date: 2021-01-29
Filing date: 2021-01-29
Publication date: 2021-06-01
Anticipated expiration: 2041-01-29
Also published as: CN112870122B

Abstract

The invention discloses a high-stability nano emulsion with a light protection effect and a preparation method thereof. According to the invention, by means of the nano emulsion carrier and the combination of four natural extracts of the echinacea purpurea extract, the mirabilis jalapa extract, the alkanna tinctoria root extract and the medicago sativa extract, on one hand, the plant extract with the photoprotection can better permeate into the skin, the efficacy of active substances is exerted to the maximum extent, and the problem of low bioavailability of the active substances in the traditional preparation is solved; on the other hand, the stability of the natural extract can be improved. The nano emulsion provided by the invention is simple and convenient in preparation method, good in stability, excellent in moisturizing effect, mild and non-irritant, and can provide better light protection for skin.

Description

High-stability nano emulsion with light protection effect and preparation method thereof

Technical Field

The invention belongs to the field of daily cosmetics, and relates to a high-stability nano emulsion with a photoprotective effect and a preparation method thereof.

Background

Ultraviolet irradiation can not only tan and sunburn skin, but also generate excessive active oxygen, so that the skin loses elasticity, wrinkles appear and skin aging is accelerated; compared with ultraviolet rays, the blue light has stronger penetrating power and can reach subcutaneous tissues, and besides solar radiation, the blue light comes from various lighting and electronic equipment, so that the damage of the blue light to the skin cannot be ignored.

At present, natural extracts have been widely used in photoprotection, and examples thereof include Echinacea purpurea (Echinacea purpurea) extract, Mirabilis jalapa L (Mirabilis jalapa L.) extract, Lithospermum erythrorhizon sieb.et Zucc (Lithospermum erythrorhizon) root extract, and Medicago sativa L (Medicago sativa L.) extract, each of which is used in photoprotection products, but the effects thereof are not superior when used alone.

The echinacea purpurea extract contains various active ingredients, has high medicinal value, can be used for treating snake and insect bites and skin diseases by external application, and can be used for treating headache, brain heat, cold, fever, respiratory tract and digestive tract infection by oral administration, and can enhance the immune system. The Echinacea purpurea extract contains triterpenes, and can inhibit skin induced allergy and treat dermatitis; can inhibit capillary permeability to achieve antiinflammatory effect; contains polyphenols and polysaccharides, and can scavenge free radicals in vivo and protect organism from damage of excessive free radicals generated by internal or external factors; the compound has obvious absorption peaks in UVA and UVB wave band ranges, can effectively inhibit inflammation caused by UVB irradiation, reduces redness, and improves the restoring force of cells under pressure conditions.

The Mirabilis jalapa extract contains active ingredients such as protein, amino acid, polysaccharide, etc., and cell membranes of the active ingredients are in a double-phospholipid structure, so that the active ingredients are protected, and the active ingredients are facilitated to permeate into skin stratum corneum to strengthen skin barriers. Mirabilis jalapa extract has effects of scavenging free radicals, inhibiting tyrosinase, inhibiting elastase activity, promoting synthesis of collagen in dermis layer, and increasing expression of anti-aging protein in human fibroblast, so as to reduce photoaging and pigmentation caused by UV irradiation.

Alkannin in the alkannin root extract belongs to naphthoquinone compounds, and has wide biological activity, such as anti-inflammatory, antivirus, antioxidation, blood sugar reduction, etc.

The purple alfalfa generates a large amount of secondary metabolites such as flavonoid compounds when stressed by a large amount of radiation, drought or other severe environments, so as to adapt to the environment and maintain the growth. The ultraviolet-visible light spectrum of the alfalfa extract has an absorption peak at 400-500nm, which shows that the alfalfa extract has the characteristic of absorbing blue light and can protect the blue light; the alfalfa extract can also scavenge free radicals and has antioxidant effects, thus also repairing the damage caused by blue light.

In addition, although the common photoprotective products contain natural extracts, the problem of poor stability of the natural extracts is not solved. Therefore, there is a need for a more effective and stable photoprotective article.

Disclosure of Invention

In order to overcome the defects of poor photoprotection effect, incapability of realizing synergistic cooperation of all components, low bioavailability and poor stability of the traditional photoprotection product in the prior art, the invention provides the nano emulsion prepared by combining the echinacea purpurea extract, the mirabilis jalapa extract, the alkanna tinctoria root extract and the medicago sativa extract, so that the bioavailability of active substances is improved, and the nano emulsion is simple and convenient in preparation method and good in stability.

The application is realized by the following technical scheme:

the invention provides a high-stability nano emulsion with a photoprotection effect, which comprises the following components: 70-95 parts of phase A; 0.1-3 parts of phase B; 1-10 parts of a phase C; 1-6.5 parts of phase D; wherein, the phase A consists of water, a humectant, a skin conditioner and a pH regulator; phase B is a thickening agent; phase C comprises emollient, emulsifier, and solvent; the phase D consists of the following components in proportion: the echinacea purpurea extract comprises a mirabilis jalapa extract, a radix Arnebiae extract, a medicago sativa extract, wherein the purple medic extract comprises (1-6.5), (1-6.5) and (1-6.5);

the parts and proportions are by weight.

Preferably, the ratio of the echinacea purpurea extract to the mirabilis jalapa extract to the alkanna tinctoria root extract to the medicago sativa extract is preferably (1-4) to (1-4).

Preferably, the ratio of the echinacea purpurea extract to the mirabilis jalapa extract to the alkanna tinctoria root extract to the medicago sativa extract is 3:2:1:3 or 2:4:2:3 or 2:3:3:4 or 1:3:2: 2.

In certain specific embodiments:

the phase A consists of 70-85 parts of water, 10-15 parts of humectant, 0.01-5 parts of skin conditioner and 0.1-3 parts of pH regulator.

Preferably, the humectant is selected from one or more of glycerol, butanediol, 1, 2-pentanediol, 1, 2-hexanediol, dipropylene glycol and sorbitol;

the skin conditioning agent is one or more selected from panthenol, sodium hyaluronate, allantoin, raffinose, dipotassium glycyrrhizinate, nicotinamide, adenosine, and caprylyl glycol;

the pH regulator is selected from one or more of arginine, tromethamine and aminomethyl propylene glycol.

In certain specific embodiments:

phase C comprises 1-10 parts of emollient, 0.1-5 parts of emulsifier and 0.1-5 parts of solvent.

Preferably, the emollient is selected from one or more of caprylic/capric triglyceride, meadowfoam seed oil, macadamia integrifolia seed oil, shea butter, squalane;

the emulsifier is one or more selected from glycerol stearate, polyglycerol-3-methyl glucose distearate, hydrogenated lecithin, cetearyl glucoside and sorbitan sesquioleate;

the solvent is one or more selected from water, 1, 2-hexanediol, butanediol and dipropylene glycol.

Preferably, the thickening agent is selected from one or more of acrylic acid (ester)/C10-30 alkanol acrylate crosspolymer, sodium acrylate/sodium acryloyldimethyl taurate copolymer, carbomer, ammonium acryloyldimethyl taurate/VP copolymer, hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer and vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane crosspolymer.

The invention also provides a preparation method of the nano emulsion, which comprises the following steps:

mixing water, humectant, skin conditioner, and pH regulator, heating to 70-80 deg.C to dissolve to obtain phase A, and keeping the temperature; mixing emollient, emulsifier and solvent, heating to 80-85 deg.C, homogenizing for 3 min, and cooling to 30 deg.C or below to obtain phase C; mixing Echinacea purpurea extract, Mirabilis jalapa extract, radix Arnebiae extract, and herba Medicaginis extract, and stirring to obtain phase D; adding the thickener as phase B into phase A, homogenizing for 3 min, controlling the temperature at 70-80 deg.C, cooling the obtained content to 40-45 deg.C, sequentially adding phase C and phase D, homogenizing for 3 min, and mixing to obtain the final product.

The phases are arranged in the proportions described above.

The nanoemulsion prepared according to the above method has a blue opalescent appearance.

Preferably, the phase B thickener is dispersed in advance before the phase A is added.

Compared with the prior art, the application can obtain the following technical effects:

the invention combines the plant extracts of the echinacea purpurea extract, the mirabilis jalapa extract, the alkanna tinctoria root extract and the alfalfa extract by means of a nano emulsion carrier, and has the following advantages: on one hand, the components in the composition are matched with each other, so that the composition can better permeate into the skin, furthest exerts the effect of the active substance, overcomes the problem of low bioavailability of the active substance in the traditional dosage form, and has better photoprotective effect than that of a single natural component with the same weight; on the other hand, the nano emulsion is applied to a light protection product, the preparation method is simple and convenient, and the stability of the product, especially the stability of the natural extract is improved. In addition, the nano emulsion has excellent moisturizing effect, is mild and non-irritant, and can provide better light protection for skin.

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.

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 preparation method of the nano emulsion comprises the following steps: mixing water, humectant, skin conditioner, and pH regulator, heating to 70-80 deg.C to dissolve to obtain phase A, and keeping the temperature; pre-weighing or pre-dispersing the phase B for later use; mixing emollient, emulsifier and solvent, heating to 80-85 deg.C, homogenizing for 3 min, and cooling to 30 deg.C or below to obtain phase C; weighing Echinacea purpurea extract, Mirabilis jalapa extract, radix Arnebiae extract, and herba Medicaginis extract at a certain ratio, mixing, and stirring to obtain phase D; adding phase B into phase A, homogenizing for 3 min, controlling temperature at 70-80 deg.C, cooling the obtained content to 40-45 deg.C, sequentially adding phase C and phase D, homogenizing for 3 min, and mixing to obtain emulsion.

In one embodiment, the components of the high stability nanoemulsion with photoprotective efficacy are substantially within the following ranges (in parts and proportions):

70-95 parts of phase A; 0.1-3 parts of phase B; 1-10 parts of a phase C; and 1-6.5 parts of a phase D. Wherein, the phase A consists of 70 to 85 parts of water, 10 to 15 parts of humectant, 0.01 to 5 parts of skin conditioner and 0.1 to 3 parts of pH regulator; phase B is a thickening agent; phase C comprises 1-10 parts of emollient, 0.1-5 parts of emulsifier and 0.1-5 parts of solvent; the phase D comprises the following components in proportion of (1-6.5) purple jasmine extract, (1-6.5) purple alfalfa extract, (1-6.5) purple coneflower extract and (1-6.5) purple alfalfa extract; preferably, the echinacea purpurea extract comprises a mirabilis jalapa extract, a alkanna tinctoria root extract, a medicago sativa extract, wherein the medicago sativa extract comprises (1-4) to (1-4); more preferably, the echinacea purpurea extract, mirabilis jalapa extract, alkanna tinctoria root extract, medicago sativa extract, is 3:2:1:3 or 2:4:2:3 or 2:3:3:4 or 1:3:2: 2.

In a specific implementation, the humectant can be one or more selected from glycerol, butanediol, 1, 2-pentanediol, 1, 2-hexanediol, dipropylene glycol and sorbitol.

In a specific embodiment, the skin conditioning agent may be selected from one or more of panthenol, sodium hyaluronate, allantoin, raffinose, dipotassium glycyrrhizinate, nicotinamide, adenosine, and caprylyl glycol.

In specific implementation, the pH regulator can be one or more selected from arginine, tromethamine and aminomethyl propylene glycol.

In a specific implementation, the thickening agent can be one or more selected from acrylic acid (ester)/C10-30 alkanol acrylate crosspolymer, sodium acrylate/sodium acryloyldimethyl taurate copolymer, carbomer, ammonium acryloyldimethyl taurate/VP copolymer, hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer and vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane crosspolymer; .

In a specific implementation, the emollient may be selected from one or more of caprylic/capric triglyceride, meadowfoam seed oil, macadamia ternifolia seed oil, shea butter, squalane.

In a specific implementation, the emulsifier can be selected from one or more of glycerol stearate, polyglycerol-3-methylglucdistearate, hydrogenated lecithin, cetearyl glucoside and sorbitan sesquioleate.

In a specific implementation, the solvent can be one or more selected from water, 1, 2-hexanediol, butanediol and dipropylene glycol.

In examples 1 to 20 and comparative examples 1 to 4, the compositions and the compounding ratios of the A phase, the B phase, the C phase and the D phase are shown in tables 1 and 2. Wherein Table 1 shows the compositions of phase A, phase B and phase C, and the total weight of phase D, and Table 2 shows the specific proportions of phase D.

The nano-emulsions of examples 1 to 20 and comparative examples 1 to 4 were prepared according to the above-described preparation methods of nano-emulsions, respectively. Wherein, the specific compositions of A, B, C phases in examples 1-20 and comparative examples 1-4, and the total parts of phase D are shown in Table 1; the specific composition of phase D is shown in table 2.

TABLE 1

TABLE 2

In addition, a general emulsion not using the nano emulsion preparation process was prepared, and its formulation is shown in table 3, and the preparation method is as follows.

TABLE 3

Mixing water, glycerol, 1, 2-pentanediol, 1, 2-hexanediol, dipotassium glycyrrhizinate, sodium hyaluronate and aminomethyl propylene glycol, heating to 70-80 deg.C to dissolve to obtain water phase, and keeping the temperature for later use; mixing white Potentilla seed oil and polyglycerol-3 methyl glucose distearate, heating to 70-80 deg.C to dissolve to obtain oil phase, and keeping the temperature; dispersing carbomer in advance for later use; weighing Echinacea purpurea extract, Mirabilis jalapa extract, Boragina officinalis root extract and Medicago sativa extract according to the proportion of the composition in example 12, namely 3:2:1:3, mixing, and stirring uniformly to obtain a composition for later use; adding the oil phase into the water phase, homogenizing for 5 min, adding pre-dispersed carbomer, homogenizing for 3 min, cooling the obtained content to 40-45 deg.C, adding the composition, homogenizing for 3 min, and mixing to obtain the common emulsion.

Experimental example 1: instant, 8h moisture test

Selecting the measurement area of forearm curvature of the subject to be 2 x 2cm²Applying 8 μ L of the product (nanoemulsion and ordinary emulsion prepared in example 12) to the area to be detected, and patting with finger cot to absorb; the moisture content of the stratum corneum was measured using a Corneometer (CK, Germany) at 0h, 2h, 4h and 8h before use, respectively, the same point was measured 5 times, and the average of 3 times after the maximum and minimum values were excluded was recorded.

The experimental results are shown in table 4, and after comparing the nano emulsion prepared in example 12 of the present invention with the conventional emulsion, it was found that the nano emulsion of the present invention has very excellent instant moisturizing effect and can maintain a high moisture content even after 8 hours.

(remark: horny layer moisture loss rate (product used rear horny layer moisture content-used front horny layer moisture content) ÷ product used front horny layer moisture content × 100%)

TABLE 4

Experimental example 2: determination of Reactive Oxygen Species (ROS)

In humans, keratinocytes and fibroblasts continue to produce reactive oxygen species which are then rapidly scavenged by non-enzymatic and enzymatic antioxidants. When the skin is subjected to external stimulation, such as ultraviolet irradiation or blue light radiation, excessive active oxygen is generated, and the skin aging is accelerated through a series of conversion processes, so that the health is damaged. In this experiment, a molecular fluorescent probe 2 ', 7' -dichlorodihydrofluorescein diethyl ester H was used₂DCFDA (2 ', 7' -Dichlorodihydrofluorescein diacetate) determined the inhibitory effect of the nanoemulsion prepared by the present invention on hydrogen peroxide-induced ROS in Human Dermal Fibroblasts (HDFs). H₂DCFDA itself has no fluorescence, and upon intracellular interaction with ROS, it can produce dichlorofluorescein (DCF,2 ', 7' -dichlorfluoroscein), the stronger the fluorescence intensity, the higher the intracellular ROS content.

The results are shown in Table 5, and the fluorescence intensity of each example is lower than that of the comparative example, so that it can be seen that H can be inhibited by the nano-emulsion prepared in each example₂O₂Induced ROS content in HDFs, whereas the inhibitory effect of the comparative examples is limited.

TABLE 5

Experimental example 3: security patch test

Taking the nano-emulsion obtained in the examples 12, 15, 17 and 18 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; the skin irritation and sensitization were observed as in table 6 after 30min, 24 hours, and 48 hours, respectively, after removal of the test article plaque test device, and the observation results were recorded.

TABLE 6

The experimental results are as follows: the results of the human skin patch tests on examples 12, 15, 17, 18 are shown in Table 7. The result of the skin patch test of the human body shows that 30 people have no adverse reaction to the skin.

TABLE 7

Experimental example 4: skin barrier repair test

40 volunteers aged 18-60 years (except pregnant or lactating women) with impaired facial skin barrier were selected and divided into 8 groups of 5 persons, each group using the nanoemulsion prepared in examples 12, 15, 17, 18 and comparative examples 1-4, respectively, once a day, morning and evening, and the transepidermal water loss rate of the face was measured using a transepidermal water loss rate measuring probe Tewameter (CK, Germany) before use and after continuous use for 4 weeks, respectively, 5 times at the same point, and 3 average records were taken after excluding the maximum and minimum. Trans Epidermal Water Loss (TEWL), which reflects the barrier function of the stratum corneum, can be used to evaluate the ability of cosmetics to repair the skin barrier. Under the test condition, the higher the TEWL value obtained, the more the transepidermal water loss per unit time and unit cross-sectional area is, the poorer the skin barrier function is, otherwise, the better the skin barrier function is, i.e. the more the TEWL value is reduced, the stronger the repair capability of the product on the skin barrier is.

The rate of change in Tewl value (Tewl value after 4 weeks use of the product-before Tewl value) divided by before Tewl value × 100%.

The experimental results are as follows: the results are shown in table 8, where the examples and comparative examples are effective, but the comparative examples have limited ability to repair the skin barrier.

TABLE 8

Experimental example 5: stability test

The test method comprises the following steps: the nano emulsion and the ordinary emulsion obtained in example 12 were stored in thermostats at different temperatures (-18, -7,4,25,37,45,50 ℃), and the change in stability factors such as appearance and odor was observed at different time periods.

And (4) conclusion: the test results are shown in table 9, and after 3 months of stability test, the stability of the nano emulsion prepared in example 12 at various temperatures has no obvious change, no delamination, no transparency, no odor change and excellent stability; when the common emulsion is tested for 1 month, the common emulsion is obviously layered and transparent at high temperature (37,45 and 50 ℃), has obvious peculiar smell and poor stability.

TABLE 9

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 high-stability nano emulsion with photoprotective efficacy is characterized by comprising the following components: 70-95 parts of phase A; 0.1-3 parts of phase B; 1-10 parts of a phase C; 1-6.5 parts of phase D; wherein, the phase A consists of water, a humectant, a skin conditioner and a pH regulator; phase B is a thickening agent; phase C comprises emollient, emulsifier, and solvent; the phase D consists of the following components in proportion: the echinacea purpurea extract comprises a mirabilis jalapa extract, a radix Arnebiae extract, a medicago sativa extract, wherein the purple medic extract comprises (1-6.5), (1-6.5) and (1-6.5); the parts and proportions are by weight.

2. The nanoemulsion of claim 1, wherein the ratio of echinacea purpurea extract to mirabilis jalapa extract to salvia miltiorrhiza extract to medicago sativa extract is preferably (1-4): 1-4.

3. The nanoemulsion of claim 2, wherein the ratio of echinacea purpurea extract to mirabilis jalapa extract to salvia miltiorrhiza extract to medicago sativa extract is preferably 3:2:1:3 or 2:4:2:3 or 2:3:3:4 or 1:3:2: 2.

4. The nanoemulsion of any of claims 1-3, wherein:

5. The nanoemulsion of claim 4, wherein:

the humectant is selected from one or more of glycerol, butanediol, 1, 2-pentanediol, 1, 2-hexanediol, dipropylene glycol and sorbitol;

6. The nanoemulsion of any of claims 1-3, wherein:

7. The nanoemulsion of claim 6, wherein:

the emollient is one or more selected from caprylic/capric triglyceride, meadowfoam seed oil, macadamia ternifolia seed oil, shea butter and squalane;

8. The nanoemulsion of any of claims 1-3, wherein:

the thickening agent is selected from one or more of acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, sodium acrylate/sodium acryloyldimethyl taurate copolymer, carbomer, ammonium acryloyldimethyl taurate/VP copolymer, hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer and vinyl polydimethylsiloxane/polymethylsiloxane silsesquioxane cross-linked polymer.

9. A method of preparing the nanoemulsion of claim 1, comprising the steps of:

10. The process according to claim 9, wherein the thickener as phase B is subjected to a preliminary dispersion treatment before being added to phase A.