An emulsion and a method for preparing the same

Abstract

The application belongs to the technical field of daily chemical industry, and particularly relates to an emulsion and a preparation method thereof. The emulsion provided in the application comprises an emulsifier, glycerol, oil-phase active substance, pentaerythritol tetra(ethylhexanoate) and water; the emulsifier is a lipopeptide; the weight percentage of the lipopeptide and the glycerol is not less than 3%; the weight ratio of the oil-phase active substance and the pentaerythritol tetra(ethylhexanoate) is 1:3-10; the ratio of the sum of the weights of the lipopeptide and the glycerol to the sum of the weights of the oil-phase active substance and the pentaerythritol tetra(ethylhexanoate) is 1:3-10; and the ratio of the sum of the weights of the lipopeptide, the glycerol, the oil-phase active substance and the pentaerythritol tetra(ethylhexanoate) to the weight of the water is 1:1-4. The emulsion is prepared by using sodium bacillomycin, glycerol and pentaerythritol tetra(ethylhexanoate), can effectively inhibit the diffusion of the oil-phase active substance at the interface of the emulsion, reduce the oxidative degradation of the oil-phase active substance, and greatly prolong the effective action time of the oil-phase active substance in the emulsion.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of daily chemical industry, and particularly relates to an emulsion and a preparation method thereof. BACKGROUND

[0002] For a long time, the stabilization of oil-phase active substances is a research hotspot in the development of cosmetics. Long-chain conjugated molecules represented by retinol, phenolic molecules represented by equol, and polyhydroxy alcohol molecules represented by vitamin C palmitate are very susceptible to degradation, discoloration, and metamorphosis due to light and heat in the daily environment, which has brought great challenges to their application in cosmetics. The current stabilization strategy for oil-phase active substances in cosmetics mainly focuses on obtaining liposomes, aqueous gels, microemulsions, and emulsions and other encapsulating bodies based on the self-assembly phenomenon of various surfactants, so as to inhibit the consumption of oxidants to oil-phase active substances through the tight surfactant interface film, thereby achieving the effect of active substance stabilization.

[0003] Lipopeptide is a secondary metabolite (usually a mixture) produced in the microbial fermentation process, which is usually composed of a β-amino or β-hydroxy fatty acid (lipophilic group) and a peptide chain or a peptide ring (hydrophilic group). It is a kind of biological surfactant. Sodium subtilipetide is a kind of lipopeptide biological surfactant, also known as surfactin, which is produced by fermentation of Bacillus subtilis strains. The hydrophilic group of its molecule is composed of a cyclic peptide. The cyclic peptide composed of 7 amino acids has rich hydrogen bond acceptors and donors, and is a biological-based anionic surfactant. Lipopeptide has the advantages of greenness and safety, and is a research hotspot in the current surfactant research. At present, lipopeptide has been applied in the preparation of emulsions and gels in the field of daily chemical industry. However, there are few related researches on the application of lipopeptide to protect oil-phase active substances from rapid degradation over time in the prior art. Moreover, the protective effect of lipopeptide on oil-phase active substances is related to other components, and the influencing factors are complex. Therefore, it is necessary to provide a product that utilizes lipopeptide to achieve good antioxidant protection of oil-phase active substances, and to solve the problems of complex preparation process and poor universality of various encapsulating bodies in the prior art. SUMMARY

[0004] In order to solve the above problems, an emulsion and a preparation method thereof are provided. The emulsion provided by the present application utilizes sodium subtilipetide and glycerol, pentaerythritol tetra (ethylhexanoate) ester in combination to prepare an emulsion containing oil-phase active substances. The addition of sodium subtilipetide can effectively inhibit the diffusion of oil-phase active substances at the interface of the emulsion, thereby reducing the oxidative degradation of oil-phase active substances and prolonging the effective action time of oil-phase active substances in the emulsion. Moreover, the preparation process is simple, and the problems of complex preparation process and poor universality of the existing technology in dealing with the easy degradation of oil-phase active substances are solved.

[0005] According to one aspect of the present application, an emulsion is provided, comprising an emulsifier, glycerol, an oil phase active, pentaerythritol tetra (ethylhexanoate) and water;

[0006] The emulsifier is a lipopeptide;

[0007] The weight percentage of the lipopeptide and glycerol is not less than 3%;

[0008] The weight ratio of the oil phase active and pentaerythritol tetra (ethylhexanoate) is 1:3-10;

[0009] The ratio of the sum of the weights of the lipopeptide and glycerol to the sum of the weights of the oil phase active and pentaerythritol tetra (ethylhexanoate) is 1:3-10;

[0010] The ratio of the sum of the weights of the lipopeptide, glycerol, oil phase active and pentaerythritol tetra (ethylhexanoate) to the weight of water is 1:1-4.

[0011] Further, the weight percentage of the lipopeptide and glycerol is selected from 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19% or 20% and any percentage therebetween.

[0012] Further, the weight ratio of the oil phase active and pentaerythritol tetra (ethylhexanoate) is selected from 1:4, 1:5, 1:6, 1:7, 1:8 or 1:9 and any value therebetween.

[0013] Further, the ratio of the sum of the weights of the lipopeptide and glycerol to the sum of the weights of the oil phase active and pentaerythritol tetra (ethylhexanoate) is selected from 1:4, 1:5, 1:6, 1:7, 1:8 or 1:9 and any value therebetween.

[0014] Further, the ratio of the sum of the weights of the lipopeptide, glycerol, oil phase active and pentaerythritol tetra (ethylhexanoate) to the weight of water is selected from 1:1.5, 1:2, 1:2.5, 1:3 or 1:3.5 and any value therebetween.

[0015] The emulsion provided by the present application adopts the above components and is compounded in a specific ratio, which can form a microemulsion gel, and further form an oil-in-water emulsion in the dilution process. The emulsion has the performance advantages of small particle size and high stability. Since the lipopeptide has a large hydrophilic head group, hydrogen bonds can be formed between cyclic peptides to hinder the diffusion of oxidizing species in the water phase to the oil phase, thereby achieving the protection and stabilization effect of the active in the oil phase, and inhibiting the oxidative deterioration and degradation thereof.

[0016] Optionally, the weight percentage of the lipopeptide and glycerol is not less than 5%, and is further preferably 5%-10%; and / or,

[0017] The weight ratio of the oil phase active substance to pentaerythritol tetra (ethylhexanoate) is 1:5-8.

[0018] Optionally, the lipopeptide is bacitracin sodium.

[0019] Optionally, the oil phase active substance comprises one or more of retinol, retinyl acetate, retinyl propionate, retinyl palmitate, bakuchiol, equol, nervonic acid, ascorbyl palmitate, ascorbyl tetrapalmitate.

[0020] According to another aspect of the present application, a method for preparing any of the above emulsions is provided, the method comprising the following steps:

[0021] 1) Dissolve the lipopeptide in glycerol, heat and stir to obtain solution A;

[0022] 2) Dissolve the oil phase active substance in pentaerythritol tetra (ethylhexanoate), stir to obtain solution B;

[0023] 3) Under constant temperature water bath and stirring conditions, add solution A to solution B to obtain an oil gel;

[0024] 4) Under stirring conditions, add the water phase to the oil gel and mix thoroughly to obtain the emulsion containing the lipopeptide.

[0025] Optionally, the lipopeptide in step 1) is bacitracin sodium.

[0026] Optionally, the temperature for heating and stirring in step 1) is 75-85°C.

[0027] Optionally, the temperature of the constant temperature water bath in step 3) is 45-55°C.

[0028] Optionally, the stirring speed in step 3) is not less than 600 rpm.

[0029] Optionally, the stirring temperature in step 4) is 20-30°C. After the formation of the oil gel, since the mixing of solutions A and B is already relatively uniform during the dilution process in step 4), slight heating or normal temperature conditions can be used at this time, with normal temperature being preferred, as normal temperature is more conducive to the preservation of the oil phase active substance.

[0030] Optionally, in step 3), solution B is added to solution A in batches and slowly; further optionally, solution B is further added after each addition of solution B is fully emulsified.

[0031] According to a final aspect of the present application, any of the above emulsions is provided for use in cosmetics.

[0032] The beneficial effects of the present application include, but are not limited to:

[0033] 1. The emulsion according to the present application has the advantages of small particle size and high stability, and does not have the problem of demulsification after high-temperature storage, cold-hot cycle, shear test, etc.

[0034] 2. The emulsion according to the present application can effectively protect the oil phase active substance from oxidative degradation, can inhibit the degradation and discoloration of retinyl propionate and other oil phase active ingredients, and can significantly improve the retention rate of the oil phase active substance in the emulsion over time.

[0035] 3. The emulsion according to the present application has the characteristics of simple preparation process and low equipment requirement, so that the production cost is low and easy to operate. The preparation of the emulsion does not require complex equipment such as high-pressure homogenization, but only needs simple stirring and mixing to prepare an emulsion with excellent antioxidant activity of the oil phase active substance.

[0036] 4. The emulsion according to the present application has the characteristics of simple composition, mild raw materials and low irritation, which meets the trend of green and safe raw materials in the daily chemical industry. BRIEF DESCRIPTION OF DRAWINGS

[0037] The drawings described herein are used to provide further understanding of the present application, and form a part of the present application. The schematic embodiments of the present application and their descriptions are used to explain the present application, and do not constitute an improper limitation on the present application. In the drawings:

[0038] Figure 1 is a schematic diagram of the molecular structure of sodium mycobacillus lipopeptide;

[0039] Figure 2 is a schematic diagram of the oil phase gel photo results of Examples 1-3 of the present application (in the figure, the numbers 1, 2 and 3 correspond to Examples 1, 2 and 3, respectively);

[0040] Figure 3 is a schematic diagram of the emulsion photo results of Examples 1-3 of the present application (in the figure, the numbers 1 and 2 correspond to Examples 1 and 2, respectively);

[0041] Figure 4 is a schematic diagram of the stability results of Example 1 and Comparative Example 2 of the present application (in the figure, the numbers 1 and D2 correspond to Example 1 and Comparative Example 2, respectively);

[0042] Figure 5 is a schematic diagram of the stability results of Example 2 and Comparative Example 4 of the present application (in the figure, the numbers 2 and D4 correspond to Example 2 and Comparative Example 4, respectively);

[0043] Figure 6 is a schematic diagram of the photo results of Comparative Example 1 and Comparative Example 3 of the present application (in the figure, the numbers D1 and D3 correspond to Comparative Example 1 and Comparative Example 3, respectively);

[0044] Figure 7This is a schematic diagram of the photographic result of Comparative Example 7 of this application (the number D7 in the figure corresponds to Comparative Example 7). Detailed Implementation

[0045] The present application is described in detail below with reference to the embodiments, but the present application is not limited to these embodiments. Unless otherwise specified, the raw materials and catalysts used in the embodiments of the present application were purchased commercially.

[0046] like Figure 1 The diagram shows the molecular structure of sodium subtilisin. In the prior art, sodium subtilisin has been reported as an emulsifier in the preparation of daily necessities such as gels or emulsions. The main function of adding sodium subtilisin in the prior art is to act as an emulsifier, enabling a mixture of two or more immiscible components to form a stable emulsion. In this application, the inventors, during their research on applying sodium subtilisin to emulsion preparation, discovered that when sodium subtilisin is used in combination with glycerol and pentaerythritol tetra(ethylhexanoate), the addition of sodium subtilisin to the emulsion containing oil-phase active ingredients effectively inhibits the diffusion of oil-phase active ingredients at the emulsion interface, thereby reducing the oxidative degradation of the oil-phase active ingredients and prolonging their effective action time in the emulsion.

[0047] Further experimental research by the inventors revealed that the protective effect of sodium subtilisin against oxidation of active oil phase substances is closely related to the selection of compatible components and the proportion of corresponding components added. For example, the use of oleic acid, GTCC, etc., which are commonly used in emulsion preparation, cannot achieve good synergistic effects, or even form an emulsion, thus limiting their compatibility with sodium subtilisin.

[0048] In this application, the inventors explored the effects of suitable components and addition ratios in combination with sodium subtilisin to improve the retention rate of active oil phases over time, based on the application of sodium subtilisin to improve the retention rate of active oil phases over time. They obtained an emulsion scheme that can significantly improve the retention rate of active oil phases over time, greatly improving the preservation effect of active oil phases. The following specific examples, comparative examples, and test cases further illustrate the scheme of this application.

[0049] Example 1

[0050] An emulsion comprising phase A, phase B and phase C, wherein phase A comprises the following raw materials in parts by weight: 1g of sodium subtilis lipopeptide and 20g of glycerin; phase B comprises the following raw materials in parts by weight: 15g of retinyl propionate and 75g of pentaerythritol tetra(ethylhexyl) ester; and phase C comprises 160g of water.

[0051] It is prepared according to the following method:

[0052] Take 1 g of bacillus subtilis lipopeptide sodium dissolved in 20 g of glycerol, heated and stirred at 80 ℃ for 20 min to obtain a clear and stable D phase (A); take 15 g of retinol propionate dissolved in 75 g of liquid oil phase pentaerythritol tetra (ethylhexyl) ester to obtain an oil phase containing active substances (B);

[0053] D phase (A) and oil phase (B) are incubated at 50 ℃ in a water bath;

[0054] Under the condition of stirring D phase (A) at 600 rpm in a 50 ℃ constant temperature water bath, slowly add oil phase (B), ensure that each added oil phase is completely emulsified and dissolved, and then further add oil phase, to obtain an oil gel containing active substances. With the increase of oil phase content, the viscosity of the system gradually increases, and finally an oil gel containing active substances is obtained;

[0055] Under the condition of stirring the oil gel at 500 rpm, add 160 g of water phase (C) and stir for 10 min until the oil gel is completely dissolved, to obtain an oil-in-water (o / w) emulsion containing retinol propionate.

[0056] The oil phase gel photo results prepared in Example 1 are shown in Figure 2 The emulsion photo results are shown in Figure 3 The emulsion photo results are shown in

[0057] Example 2

[0058] An emulsion comprising A phase, B phase and C phase, wherein A phase comprises the following raw materials in parts by weight: 1 g of bacillus subtilis lipopeptide sodium, 20 g of glycerol; B phase comprises the following raw materials in parts by weight: 15 g of psoralen, 75 g of pentaerythritol tetra (ethylhexyl) ester; C phase is water 160 g.

[0059] It is prepared by the following method:

[0060] Take 1 g of bacillus subtilis lipopeptide sodium dissolved in 20 g of glycerol, heated and stirred at 80 ℃ for 20 min to obtain a clear and stable D phase (A); take 15 g of retinol propionate dissolved in 75 g of liquid oil phase pentaerythritol tetra (ethylhexyl) ester to obtain an oil phase containing active substances (B);

[0061] D phase (A) and oil phase (B) are incubated at 50 ℃ in a water bath;

[0062] Under the condition of stirring D phase (A) at 600 rpm in a 50 ℃ constant temperature water bath, slowly add oil phase (B), ensure that each added oil phase is completely emulsified and dissolved, and then further add oil phase, to obtain an oil gel containing active substances. With the increase of oil phase content, the viscosity of the system gradually increases, and finally an oil gel containing active substances is obtained;

[0063] 160 g water phase (C) was added under the condition of stirring the oil gel at 500 rpm, and stirring for 10 min until the oil gel was completely dissolved, to obtain an oil-in-water (o / w) emulsion containing bakuchiol.

[0064] The results of the oil phase gel prepared in Example 2 are shown in Figure 2 The results of the emulsion are shown in Figure 3 The results of the emulsion are shown in

[0065] Example 3

[0066] An emulsion comprising A phase, B phase and C phase, wherein the A phase comprises the following raw materials in parts by weight: 1 g of trichosanthin lipopeptide sodium, 20 g of glycerol; the B phase comprises the following raw materials in parts by weight: 15 g of ascorbic acid tetrapalmitate, 75 g of pentaerythritol tetra (ethylhexyl) ester; and the C phase is water 160 g.

[0067] It is prepared by the following method:

[0068] 1 g of trichosanthin lipopeptide sodium is dissolved in 20 g of glycerol, heated and stirred at 80°C for 20 min to obtain a clear and stable D phase (A); 15 g of ascorbic acid tetrapalmitate is dissolved in 75 g of liquid oil phase pentaerythritol tetra (ethylhexyl) ester to obtain an oil phase containing active substances (B);

[0069] The D phase (A) and the oil phase (B) are incubated at 50°C in a water bath;

[0070] The oil phase (B) is slowly added under the condition of stirring the D phase (A) at 600 rpm in a 50°C constant temperature water bath, ensuring that each added oil phase is completely emulsified and dissolved, and then further adding the oil phase, to obtain an oil gel containing active substances. As the content of the oil phase increases, the viscosity of the system gradually increases, and finally an oil gel containing active substances is obtained;

[0071] 160 g water phase (C) is added under the condition of stirring the oil gel at 500 rpm, and stirring for 10 min until the oil gel is completely dissolved, to obtain an oil-in-water (o / w) emulsion containing ascorbic acid tetrapalmitate.

[0072] The results of the oil phase gel prepared in Example 3 are shown in Figure 2 The results of the emulsion are shown in

[0073] Example 4

[0074] An emulsion comprising A phase, B phase and C phase, wherein the A phase comprises the following raw materials in parts by weight: 1 g of trichosanthin lipopeptide sodium, 20 g of glycerol; the B phase comprises the following raw materials in parts by weight: 15 g of ascorbic acid tetrapalmitate, 75 g of pentaerythritol tetra (ethylhexyl) ester; and the C phase is water 160 g.

[0075] It is prepared by the following method:

[0076] Take 1 g of bacillus subtilis lipopeptide sodium and dissolve it in 20 g of glycerol, heat and stir at 80℃ for 20 min to obtain a clear and stable D phase (A); take 15 g of retinol propionate and dissolve it in 75 g of liquid oil phase pentaerythritol tetra (ethylhexyl) ester to obtain an oil phase containing active substances (B);

[0077] D phase (A) and oil phase (B) are incubated in a water bath at 50℃;

[0078] Under the condition of stirring D phase (A) at 600 rpm in a constant temperature water bath at 50℃, slowly add oil phase (B), make sure that each added oil phase is completely emulsified and dissolved, then further add oil phase, thus obtaining an oil gel containing active substances. With the increase of oil phase content, the viscosity of the system gradually increases, and finally an oil gel containing active substances is obtained;

[0079] Under the condition of stirring the oil gel at 500 rpm, add 111 g of water phase (C) and stir for 10 min until the oil gel is completely dissolved, thus obtaining an oil-in-water (o / w) emulsion containing retinol propionate.

[0080] Example 5

[0081] An emulsion comprising A phase, B phase and C phase, wherein A phase comprises the following raw materials in parts by weight: bacillus subtilis lipopeptide sodium 1 g, glycerol 20 g; B phase comprises the following raw materials in parts by weight: retinol propionate 15 g, pentaerythritol tetra (ethylhexyl) ester 75 g; C phase is water 444 g.

[0082] It is prepared by the following method:

[0083] Take 1 g of bacillus subtilis lipopeptide sodium and dissolve it in 20 g of glycerol, heat and stir at 80℃ for 20 min to obtain a clear and stable D phase (A); take 15 g of retinol propionate and dissolve it in 75 g of liquid oil phase pentaerythritol tetra (ethylhexyl) ester to obtain an oil phase containing active substances (B);

[0084] D phase (A) and oil phase (B) are incubated in a water bath at 50℃;

[0085] Under the condition of stirring D phase (A) at 600 rpm in a constant temperature water bath at 50℃, slowly add oil phase (B), make sure that each added oil phase is completely emulsified and dissolved, then further add oil phase, thus obtaining an oil gel containing active substances. With the increase of oil phase content, the viscosity of the system gradually increases, and finally an oil gel containing active substances is obtained;

[0086] Add 444 g of the aqueous phase (C) to the oil gel under stirring at 500 rpm, and stir for 10 min until the oil gel is completely dissolved, to obtain an oil-in-water (o / w) emulsion containing retinyl propionate.

[0087] Example 6

[0088] An emulsion comprising an A phase, a B phase and a C phase, wherein the A phase comprises the following raw materials in parts by weight: 1 g of sodium subtilipet, 20 g of glycerol; the B phase comprises the following raw materials in parts by weight: 10 g of retinyl propionate, 80 g of pentaerythritol tetra (ethylhexyl) ester; and the C phase is 160 g of water.

[0089] It is prepared by the following method:

[0090] Dissolve 1 g of sodium subtilipet in 20 g of glycerol, and heat and stir at 80 °C for 20 min to obtain a clear and stable D phase (A); dissolve 10 g of retinyl propionate in 80 g of liquid oil phase pentaerythritol tetra (ethylhexyl) ester to obtain an oil phase (B) containing active substances;

[0091] Incubate the D phase (A) and the oil phase (B) at 50 °C in a water bath;

[0092] Slowly add the oil phase (B) to the D phase (A) under stirring at 600 rpm in a 50 °C constant temperature water bath, ensure that each addition of the oil phase is completely emulsified and dissolved, and then further add the oil phase, to obtain an oil gel containing active substances. As the content of the oil phase increases, the viscosity of the system gradually increases, and finally an oil gel containing active substances is obtained;

[0093] Add 160 g of the aqueous phase (C) to the oil gel under stirring at 500 rpm, and stir for 10 min until the oil gel is completely dissolved, to obtain an oil-in-water (o / w) emulsion containing retinyl propionate.

[0094] Example 7

[0095] An emulsion comprising an A phase, a B phase and a C phase, wherein the A phase comprises the following raw materials in parts by weight: 0.45 g of sodium subtilipet, 8.55 g of glycerol; the B phase comprises the following raw materials in parts by weight: 15 g of retinyl propionate, 75 g of pentaerythritol tetra (ethylhexyl) ester; and the C phase is 160 g of water.

[0096] It is prepared by the following method:

[0097] Dissolve 0.45 g of sodium subtilipet in 8.55 g of glycerol, and heat and stir at 80 °C for 20 min to obtain a clear and stable D phase (A); dissolve 15 g of retinyl propionate in 75 g of liquid oil phase pentaerythritol tetra (ethylhexyl) ester to obtain an oil phase (B) containing active substances;

[0098] The D phase (A) and the oil phase (B) are incubated in a water bath at 50 °C;

[0099] The oil phase (B) is slowly added under stirring of the D phase (A) at 600 rpm in a constant temperature water bath at 50 °C, ensuring that each added oil phase is completely emulsified and dissolved before further addition of the oil phase, to obtain an oil gel containing active substances. With the increase of the content of the oil phase, the viscosity of the system gradually increases, and finally an oil gel containing active substances is obtained.

[0100] The water phase (C) is added to the oil gel under stirring at 500 rpm, and the oil gel is completely dissolved after stirring for 10 min, to obtain an oil-in-water (o / w) emulsion containing retinyl propionate.

[0101] Example 8

[0102] An emulsion comprising A phase, B phase and C phase, wherein the A phase comprises the following raw materials in parts by weight: 1.5 g of sodium subtilipetrolipetide, 28.5 g of glycerol; the B phase comprises the following raw materials in parts by weight: 15 g of retinyl propionate, 75 g of pentaerythritol tetra (ethylhexyl) ester; and the C phase is water 200 g.

[0103] It is prepared by the following method:

[0104] 1.5 g of sodium subtilipetrolipetide is dissolved in 28.5 g of glycerol, heated and stirred at 80 °C for 20 min to obtain a clear and stable D phase (A); 15 g of retinyl propionate is dissolved in 75 g of liquid oil phase pentaerythritol tetra (ethylhexyl) ester to obtain an oil phase (B) containing active substances.

[0105] The D phase (A) and the oil phase (B) are incubated in a water bath at 50 °C;

[0106] The oil phase (B) is slowly added under stirring of the D phase (A) at 600 rpm in a constant temperature water bath at 50 °C, ensuring that each added oil phase is completely emulsified and dissolved before further addition of the oil phase, to obtain an oil gel containing active substances. With the increase of the content of the oil phase, the viscosity of the system gradually increases, and finally an oil gel containing active substances is obtained.

[0107] The water phase (C) is added to the oil gel under stirring at 500 rpm, and the oil gel is completely dissolved after stirring for 10 min, to obtain an oil-in-water (o / w) emulsion containing retinyl propionate.

[0108] Comparative Example 1

[0109] An emulsion comprising A phase, B phase and C phase, wherein the A phase comprises the following raw materials in parts by weight: 1 g of bacillus subtilis lipopeptide sodium, 20 g of glycerol; the B phase comprises the following raw materials in parts by weight: 15 g of retinol propionate, 75 g of oleic acid; and the C phase is 160 g of water.

[0110] It is prepared by the following method:

[0111] 1 g of bacillus subtilis lipopeptide sodium is dissolved in 20 g of glycerol, heated and stirred at 80 DEG C for 20 min to obtain a clear and stable D phase (A); 15 g of retinol propionate is dissolved in 75 g of liquid oil phase oleic acid to obtain an oil phase containing active substances (B);

[0112] The D phase (A) and the oil phase (B) are incubated at 50 DEG C in a water bath.

[0113] The oil phase (B) is slowly added under the condition of stirring the D phase (A) at 600 rpm in a 50 DEG C constant temperature water bath, and it is found that the two phases cannot be mutually soluble or emulsified, and the results are shown in Figure 6 D1 picture in the example.

[0114] Comparative example 2

[0115] An emulsion comprising A phase, B phase and C phase, wherein the A phase comprises the following raw materials in parts by weight: 1 g of bacillus subtilis lipopeptide sodium, 20 g of glycerol; the B phase comprises the following raw materials in parts by weight: 15 g of retinol propionate, 75 g of GTCC; and the C phase is 160 g of water.

[0116] It is prepared by the following method:

[0117] 1 g of bacillus subtilis lipopeptide sodium is dissolved in 20 g of glycerol, heated and stirred at 80 DEG C for 20 min to obtain a clear and stable D phase (A); 15 g of retinol propionate is dissolved in 75 g of liquid oil phase GTCC to obtain an oil phase containing active substances (B);

[0118] The D phase (A) and the oil phase (B) are incubated at 50 DEG C in a water bath.

[0119] The oil phase (B) is slowly added under the condition of stirring the D phase (A) at 600 rpm in a 50 DEG C constant temperature water bath, and it is ensured that the oil phase is completely emulsified and dissolved each time, and then the oil phase is further added, that is, an oil gel containing active substances is obtained, and with the increase of the content of the oil phase, the viscosity of the system gradually increases, and finally an oil gel containing active substances is obtained;

[0120] 160 g of water phase (C) is added under the condition of stirring the oil gel at 500 rpm, and the oil gel is completely dissolved after stirring for 10 min, that is, an oil-in-water (o / w) type emulsion containing retinol propionate is obtained.

[0121] The results are shown inFigure 4 The results show that the emulsion is not stable in storage and can cause problems such as separation and discoloration, as shown in the middle D2 picture.

[0122] Comparative Example 3

[0123] An emulsion comprising A phase, B phase and C phase, wherein the A phase comprises the following raw materials in parts by weight: 1 g of sodium subtilipetrolide, 20 g of butanediol; the B phase comprises the following raw materials in parts by weight: 15 g of xanthophyll propionate, 75 g of pentaerythritol tetra (ethylhexyl) ester; and the C phase is 160 g of water.

[0124] It is prepared by the following method:

[0125] 1 g of sodium subtilipetrolide is dissolved in 20 g of butanediol, heated and stirred at 80°C for 20 min, but a clear and stable D phase (A) cannot be obtained; 15 g of xanthotoxol is dissolved in 75 g of liquid oil phase pentaerythritol tetraethylhexyl ester to obtain an oil phase containing active substances (B);

[0126] The D phase (A) and the oil phase (B) are incubated at 50°C in a water bath;

[0127] Under the condition of stirring the D phase (A) at 600 rpm in a 50°C constant temperature water bath, the oil phase (B) is slowly added, but the oil phase gel cannot be formed, and the results are as follows Figure 6 as shown in the middle D3 picture.

[0128] Comparative Example 4

[0129] An emulsion comprising A phase, B phase and C phase, wherein the A phase comprises the following raw materials in parts by weight: 1 g of sodium subtilipetrolide, 20 g of butanediol; the B phase comprises the following raw materials in parts by weight: 15 g of xanthophyll propionate, 75 g of pentaerythritol tetra (ethylhexyl) ester; and the C phase is 160 g of water.

[0130] It is prepared by the following method:

[0131] 1 g of sodium subtilipetrolide is dissolved in 20 g of butanediol, heated and stirred at 80°C for 20 min, but a clear and stable D phase (A) cannot be obtained; 15 g of xanthotoxol is dissolved in 75 g of liquid oil phase pentaerythritol tetraethylhexyl ester to obtain an oil phase containing active substances (B);

[0132] The D phase (A) and the oil phase (B) are incubated at 50°C in a water bath;

[0133] Under the condition of stirring the D phase (A) at 600 rpm in a 50°C constant temperature water bath, the oil phase (B) is slowly added, but the oil phase gel cannot be formed, and the results are as follows

[0134] 160 g of the aqueous phase (C) was added to the oil gel under stirring at 500 rpm, and stirring was continued for 10 min until the oil gel was completely dissolved, thereby obtaining an oil-in-water (o / w) emulsion containing bakuchiol.

[0135] The results are shown in Table D4. Figure 5 The results show that the emulsion is not storage stable and can cause problems such as separation and discoloration.

[0136] Comparative Example 5

[0137] An emulsion comprising an A phase, a B phase and a C phase, wherein the A phase comprises the following raw materials in parts by weight: 1 g of trichosanthin lipopeptide sodium, 20 g of glycerol; the B phase comprises the following raw materials in parts by weight: 15 g of retinol propionate, 75 g of pentaerythritol tetra(ethylhexyl) ester; and the C phase is 100 g of water.

[0138] It is prepared by the following method:

[0139] 1 g of trichosanthin lipopeptide sodium was dissolved in 20 g of glycerol, and stirring was performed at 80°C for 20 min to obtain a clear and stable D phase (A); 15 g of retinol propionate was dissolved in 75 g of liquid oil phase pentaerythritol tetra(ethylhexyl) ester to obtain an oil phase (B) containing active substances;

[0140] The D phase (A) and the oil phase (B) were incubated at 50°C in a water bath;

[0141] The oil phase (B) was slowly added under stirring of the D phase (A) at 600 rpm in a 50°C constant temperature water bath, and it was ensured that each addition of the oil phase was completely emulsified and dissolved, and then further oil phase was added, thereby obtaining an oil gel containing active substances. With the increase of the content of the oil phase, the viscosity of the system gradually increased, and finally an oil gel containing active substances was obtained;

[0142] 100 g of the aqueous phase (C) was added to the oil gel under stirring at 500 rpm, and stirring was continued for 10 min, but the oil gel could not be completely dissolved, thereby obtaining a mixture with large viscosity and opacity, which does not belong to the category of emulsion.

[0143] Comparative Example 6

[0144] An emulsion comprising an A phase, a B phase and a C phase, wherein the A phase comprises the following raw materials in parts by weight: 0.5 g of trichosanthin lipopeptide sodium, 20.5 g of glycerol; the B phase comprises the following raw materials in parts by weight: 15 g of retinol propionate, 75 g of pentaerythritol tetra(ethylhexyl) ester; and the C phase is 160 g of water.

[0145] It is prepared by the following method:

[0146] Take 0.5 g of bacillus subtilis lipopeptide sodium and dissolve it in 20.5 g of glycerol, heat and stir at 80 ℃ for 20 min to obtain a clear and stable D phase (A); take 15 g of retinol propionate and dissolve it in 75 g of liquid oil phase pentaerythritol tetra (ethylhexyl) ester to obtain an oil phase containing active substances (B);

[0147] Incubate the D phase (A) and the oil phase (B) in a water bath at 50 ℃;

[0148] Slowly add the oil phase (B) under the condition of stirring the D phase (A) at 600 rpm in a constant temperature water bath at 50 ℃, and it is found that the oil phase cannot be completely emulsified or dissolved in the D phase, and free oil phase always exists, indicating that the ratio of lipopeptide to glycerol is too low to form an oil phase gel, resulting in the failure to form an emulsion.

[0149] Comparative Example 7

[0150] An emulsion comprising A phase, B phase and C phase, wherein the A phase comprises the following raw materials in parts by weight: bacillus subtilis lipopeptide sodium 0.4 g, glycerol 8 g; the B phase comprises the following raw materials in parts by weight: retinol propionate 15 g, pentaerythritol tetra (ethylhexyl) ester 75 g; and the C phase is water 138 g.

[0151] It is prepared by the following method:

[0152] Take 0.4 g of bacillus subtilis lipopeptide sodium and dissolve it in 8 g of glycerol, heat and stir at 80 ℃ for 20 min to obtain a clear and stable D phase (A); take 15 g of retinol propionate and dissolve it in 75 g of liquid oil phase pentaerythritol tetra (ethylhexyl) ester to obtain an oil phase containing active substances (B);

[0153] Incubate the D phase (A) and the oil phase (B) in a water bath at 50 ℃;

[0154] Slowly add the oil phase (B) under the condition of stirring the D phase (A) at 600 rpm in a constant temperature water bath at 50 ℃, and it is found that the oil phase cannot be completely emulsified or dissolved in the D phase, and free oil phase always exists, indicating that the ratio of A to B is too low to form an oil phase gel, and therefore an emulsion cannot be formed, and the results are shown in Figure 7 D7 picture in the middle.

[0155] Comparative Example 8

[0156] An emulsion comprising A phase, B phase and C phase, wherein the A phase comprises the following raw materials in parts by weight: bacillus subtilis lipopeptide sodium 1 g, glycerol 20 g; the B phase comprises the following raw materials in parts by weight: retinol propionate 30 g, pentaerythritol tetra (ethylhexyl) ester 60 g; and the C phase is water 160 g.

[0157] It is prepared by the following method:

[0158] Take 1 g of sodium mycobacterial lipopeptide and dissolve it in 20 g of glycerol, heat and stir at 80 ℃ for 20 min to obtain a clear and stable D phase (A); take 30 g of retinyl propionate and dissolve it in 60 g of liquid oil phase pentaerythritol tetra (ethylhexyl) ester to obtain an oil phase containing active substances (B);

[0159] Incubate the D phase (A) and the oil phase (B) in a water bath at 50 ℃;

[0160] Slowly add the oil phase (B) to the D phase (A) under stirring at 600 rpm in a constant temperature water bath at 50 ℃, ensure that each addition of the oil phase is completely emulsified and dissolved, and then further add the oil phase, to obtain an oil gel containing active substances. As the content of the oil phase increases, the viscosity of the system gradually increases, and finally an oil gel containing active substances is obtained;

[0161] Add 160 g of an aqueous phase (C) to the oil gel under stirring at 500 rpm, and stir for 10 min until the oil gel is completely dissolved, to obtain an oil-in-water (o / w) emulsion containing retinyl propionate.

[0162] Test Example 1

[0163] Active substance degradation rate determination experiment method: The degradation rate of active substances such as retinyl propionate and bakuchiol was determined by high performance liquid chromatography-ultraviolet detector. Specifically, the prepared examples 1-8, comparative examples 2, 4 and 8 were placed in a constant temperature oven at 50 ℃, and every 7 d, 15 d and 28 d, the emulsion was dissolved in methanol, and the degradation rate was determined by high performance liquid chromatography. The specific high performance liquid chromatography conditions are as follows: the chromatographic column is a C18 reversed phase chromatographic column (250*4.6mm, 5um), the mobile phase composition is 98vol% methanol and 2vol% water, the flow rate of the mobile phase is 1ml / min, the detection wavelength is 325nm, and the external standard method is used for quantitative detection.

[0164] Table 1 is the component ratio of the emulsion of examples 1-8 and comparative examples 1-8, and table 2 is the results of the active substance degradation rate determination experiment in test example 1.

[0165] Table 1 Component ratio of emulsion

[0166]

[0167] Table 2 Results of active substance degradation rate determination experiment

[0168]

[0169] According to the results in Table 2, the emulsion of the present application example has a higher retention rate over time than Comparative Examples 2 and 4, and the oil phase component pentaerythritol tetra(ethylhexyl) ester in the present application has a better compatibility effect with other components than GTCC, and can still maintain a high retention rate after 28 days, while Comparative Examples 2 and 4 have precipitation problems after 28 days.

[0170] In addition, according to the experimental results described in Examples 1-8 and Comparative Examples 1-8 and the experimental results in the Figures 2-7 It can be seen that when the components of the emulsion in the present application are properly matched in the appropriate proportions, the emulsion product can be successfully prepared and obtained while having excellent protective effects on the oil phase active substance, while using other components for matching or inappropriate matching proportions, there are problems such as easy precipitation, inability to form an emulsion, inability to form an oil gel, and large color change. Among them, from the Figure 5 It can be seen that the emulsion of Comparative Example 4 is broken after storage, retinyl propionate is precipitated in large quantities, and the color change is severe; from the Figure 6 It can be seen that the color change of Comparative Example 3 is large after storage, and in Comparative Example 1, the oil and lipopeptide, glycerol are mixed to form an oil gel, but there is a phenomenon of stratification; from the Figure 7 It can be seen that the quality of the oil gel in Comparative Example 7 is not good, and there is free oil.

[0171] The present application example scheme introduces sodium lipopeptide, and preferably glycerol and pentaerythritol tetra(ethylhexyl) ester for matching with the oil phase active substance, and the matching proportion, so that the example scheme has a very good protective effect on the oil phase active substance, and can still maintain a retention rate of 90% or more of the oil phase active substance after 28 days, and can effectively reduce the degradation of the oil phase active substance.

[0172] The above is only an embodiment of the present application, and the protection scope of the present application is not limited by these specific embodiments, but is determined by the claims of the present application. The present application can have various changes and variations for those skilled in the art. Any modification, equivalent replacement, improvement, etc. within the technical idea and principle of the present application shall be included in the protection scope of the present application.

Claims

1. An oleogel, characterized in that, It contains emulsifiers, glycerin, oil phase actives, and pentaerythritol tetra(ethylhexanoate); The emulsifier is sodium subtilisin; The weight percentage of glycerol in the sodium subtilis lipopeptide is not less than 3%. The weight ratio of the oil phase active material to pentaerythritol tetra(ethylhexanoate) ester is 1:3~10; The ratio of the sum of the weights of the subtilis lipopeptide sodium and glycerol to the sum of the weights of the oil phase active material and pentaerythritol tetra(ethylhexanoate) ester is 1:3~10.

2. The oleogel according to claim 1, characterized in that, The weight percentage of the sodium subtilis lipopeptide to glycerol is not less than 5%; and / or, The weight ratio of the oil phase active material to pentaerythritol tetra(ethylhexanoate) ester is 1:5~8.

3. The oleogel according to claim 2, characterized in that, The weight percentage of the sodium subtilis lipopeptide and glycerol is 5% to 10%.

4. The oleogel according to claim 1, characterized in that, The oil-phase active ingredient comprises one or more of retinol, retinyl acetate, retinyl propionate, retinyl palmitate, psoralen, equol, nervonic acid, ascorbyl palmitate, and ascorbyl tetrapalmitate.

5. An emulsion, characterized in that, It comprises the oleogel according to any one of claims 1-4 and water.

6. The emulsion according to claim 5, characterized in that, The weight ratio of the sum of the components of the subtilis lipopeptide sodium, glycerol, oil phase active material and pentaerythritol tetra(ethylhexanoate) ester to the weight of water is 1:1 to 4.

7. The method for preparing the oleogel according to any one of claims 1 to 4, characterized in that, The method includes the following steps: 1) Dissolve sodium subtilis lipopeptide in glycerol, heat and stir to obtain solution A; 2) Dissolve the active substance in the oil phase in pentaerythritol tetra(ethylhexanoate) ester and stir to obtain solution B; 3) Under constant temperature water bath and stirring conditions, solution A is added to solution B to obtain oleogel.

8. The method for preparing the emulsion according to claim 5 or 6, characterized in that, It also includes adding an aqueous phase to the oleogel under stirring conditions to mix it thoroughly, thereby obtaining the emulsion containing sodium subtilisin.

9. The use of the oleogel as described in any one of claims 1 to 4 or the emulsion as described in claim 5 or 6 in the preparation of cosmetics.

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