Emulsion and method for preparing the same
The emulsion stabilizes oil-phase active substances in cosmetics by using glycerin, pentaerythritol tetra(2-ethylhexanoic acid) ester, and lipopeptide surfactants to form a stable water-in-oil emulsion, addressing decomposition issues and simplifying the preparation process.
Patent Information
- Application Number
- JP2026510165
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2023-08-21
- Filing Date
- 2024-08-20
- Publication Date
- 2026-08-26
AI Technical Summary
Existing technologies face challenges in stabilizing oil-phase active substances in cosmetics due to their susceptibility to decomposition and discoloration from light and heat, and the preparation processes are complex and lack versatility.
An emulsion is formulated using glycerin, pentaerythritol tetra(2-ethylhexanoic acid) ester, and a lipopeptide surfactant, such as surfactin sodium, to create a microemulsion gel that forms a water-in-oil emulsion, stabilizing the active substances by inhibiting oxidative decomposition through hydrogen bonding.
The emulsion achieves high stability with small particle sizes, prevents oxidative decomposition of oil-phase active substances, and simplifies the preparation process, reducing equipment requirements and production costs while ensuring environmental safety.
Smart Images
Figure 2026528991000001_ABST
Abstract
Description
Technical Field
[0004] ,
[0001] This application belongs to the technical field of daily chemical industry, and specifically relates to emulsions and their preparation methods.
[0002] This application claims the priority of a Chinese patent application filed on August 21, 2023, with an application number of 202311056263.X and an invention title of "Emulsion and Its Preparation Method", and the entire content thereof is incorporated herein by reference.
Background Art
[0003] For many years, the stabilization of oil-phase active substances has been a research hotspot in cosmetics development. Long-chain conjugated molecules represented by retinol, phenolic molecules represented by equol, polyhydric alcohol-based molecules represented by ascorbyl palmitate, etc. are easily decomposed, discolored, and deteriorated by light and heat in the daily environment, which poses a great challenge to their application in cosmetics. The current stabilization strategies for oil-phase active substances in cosmetics mainly focus on obtaining encapsulation bodies such as liposomes, aqueous gels, microemulsions, and emulsions based on the self-assembly phenomenon of various surfactants. Thereby, the consumption of oil-phase active substances by oxides can be suppressed through the dense interfacial film of surfactants, and thus the stabilizing effect of the active substances can be exerted.
[0004] Lipopeptides are secondary metabolites (usually mixtures) produced during microbial fermentation processes and are a type of biosurfactant typically composed of β-amino acids or β-hydroxy fatty acids (lipophilic groups) and peptide chains or peptide rings (hydrophilic groups). Sodium surfactin is a lipopeptide-based biosurfactant, also known as surfactin, and is produced by the fermentation of Bacillus subtilis strains. The hydrophilic group of its molecule is composed of a cyclic peptide, and this cyclic peptide, consisting of seven amino acids, has abundant hydrogen bond acceptors and donors, making it a bio-derived anionic surfactant. Lipopeptides have advantages such as being environmentally friendly and highly safe, and are currently a hot spot in surfactant research. Currently, lipopeptides are already being applied in the daily chemical industry, such as in the preparation of emulsions and gels, but there is little related research on using lipopeptides to protect oil-phase active substances and avoid excessive degradation over time in conventional technology. Furthermore, the protective effect of lipopeptides on oil-phase active substances is related to other components in the formulation, and the influencing factors are relatively complex. Therefore, it is necessary to provide a product that utilizes lipopeptides to exhibit excellent antioxidant protective effects on oil-phase active substances, and at the same time, it is necessary to solve the problems of complexity and low versatility of the preparation process that are universally present in various encapsulated products in conventional technology. [Overview of the project] [Problems that the invention aims to solve]
[0005] To solve the above problems, this application provides an emulsion and a method for preparing the same. The emulsion provided by this application contains an oil-phase active substance prepared by combining glycerin and pentaerythritol tetra(2-ethylhexanoic acid) ester with surfactant sodium. The addition of surfactant sodium effectively suppresses the diffusion of the oil-phase active substance at the emulsion interface, thereby reducing the oxidative decomposition of the oil-phase active substance and extending the effective action time of the oil-phase active substance in the emulsion. Furthermore, the preparation process is simple, solving the common problems of complexity and low versatility in the preparation process when dealing with the problem of easy decomposition of oil-phase active substances in the prior art. [Means for solving the problem]
[0006] In one embodiment of the present application, an emulsion containing an emulsifier, glycerin, an oil-phase active substance, pentaerythritol tetra(2-ethylhexanoic acid) ester, and water is provided. The emulsifier is a lipopeptide. The weight percentage of the lipopeptide and the glycerin is 3% or more. The weight ratio of the oil phase active substance to the pentaerythritol tetra(2-ethylhexanoic acid) ester is 1:3 to 13. The ratio of the total weight of the lipopeptide and glycerin to the total weight of the oil phase active substance and pentaerythritol tetra(2-ethylhexanoic acid) ester is 1:3 to 10. The ratio of the total weight of the lipopeptide, glycerin, oil phase active substance, and pentaerythritol tetra(2-ethylhexanoic acid) ester to the weight of water is 1:1 to 4.
[0007] Furthermore, the weight percentages of the lipopeptide and glycerin are selected from 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, and any percentage between these values.
[0008] Furthermore, the weight ratio of the oil phase active substance to the pentaerythritol tetra(2-ethylhexanoic acid) ester is selected from 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, 1:12, and any value between these numbers.
[0009] Furthermore, the ratio of the total weight of the lipopeptide and glycerin to the total weight of the oil phase active substance and pentaerythritol tetra(2-ethylhexanoic acid) ester is selected from 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, and any value between these numbers.
[0010] Furthermore, the ratio of the total weight of the lipopeptide, glycerin, oil phase active substance, and pentaerythritol tetra(2-ethylhexanoic acid) ester to the weight of water is selected from 1:1.5, 1:2, 1:2.5, 1:3, 1:3.5, and any value between these numbers.
[0011] The emulsion provided in this application, by employing the above-mentioned components and blending them in specific proportions, forms a microemulsion gel, and subsequently forms a water-in-oil emulsion during the dilution process. This emulsion has the advantage of small particle size and high stability, and because the hydrophilic head portion of the lipopeptide is large, hydrogen bonds are formed between the cyclic peptides, inhibiting the diffusion of oxidized species in the aqueous phase into the oil phase, thereby achieving a protective and stabilizing effect on the active substance in the oil phase, and suppressing its oxidative alteration and decomposition.
[0012] Optionally, the weight percentage of the lipopeptide and the glycerin is 5% or more, and further optionally 5% to 12%, and / or The weight ratio of the oil phase active substance to the pentaerythritol tetra(2-ethylhexanoic acid) ester is 1:5 to 11.
[0013] Optionally, the lipopeptide may contain one or more of the following: surfactant sodium, iturine, fenzi, phongi, daptomycin, polymyxin, batirasidine L, phospholipidase inhibitor peptide, and batirasidine D.
[0014] Optionally, the oil-phase active substance may include one or more of the following: retinol, retinol acetate, retinol propionate, retinol palmitate, boswellianol, equol, nerve acid, ascorbic acid palmitate, ascorbic acid tetrapalmitate, and phenylethyl resorcinol.
[0015] In other embodiments of this application, a method for preparing any of the above emulsions is provided, 1) Dissolve the lipopeptide in glycerin, heat and stir to obtain solution A, 2) Dissolve the oil-phase active substance in pentaerythritol tetra(2-ethylhexanoic acid) ester and stir to obtain solution B. 3) Add solution A to solution B under constant temperature water bath and stirring conditions to obtain an oil gel. 4) The method includes adding an aqueous phase to an oil gel under stirring conditions and mixing thoroughly to obtain a lipopeptide-containing emulsion.
[0016] Optionally, in step 1), the lipopeptide may include one or more of surfactin sodium, iturine, fenzi, phongidin, daptomycin, polymyxin, batirasidine L, phospholipidase inhibitor peptide, and batirasidine D.
[0017] Optionally, in step 2), the heating and stirring temperature is 75-85°C.
[0018] Optionally, in step 3) above, the temperature of the constant-temperature water bath is 45-55°C.
[0019] Optionally, in step 3) above, the stirring speed is 600 rpm or higher.
[0020] Optionally, in the step 4), the stirring temperature is 20-30°C. After forming the oil gel, in the step 4), since the mixing of liquid A and liquid B is already relatively uniform in the stirring and dilution process, at this time, mild heating or normal temperature conditions can be adopted, and normal temperature can be selected, which is more favorable for the preservation of the oil-phase active substance.
[0021] Optionally, in the step 3), liquid B is added to liquid A slowly in multiple portions, and further optionally, after each addition of liquid B is sufficiently emulsified, liquid B is added again.
[0022] In the last aspect of the present application, the application of any of the above emulsions to cosmetics is provided.
Advantages of the Invention
[0023] The beneficial effects of the present application include, but are not limited to, the following technical effects.
[0024] 1.1. The emulsion of the present application has the advantages of small particle size and high stability, and no creaming out occurs even under conditions such as high-temperature storage, thermal cycling, and shear test.
[0025] 2. The emulsion of the present application can effectively prevent the oxidative decomposition of the oil-phase active substance, suppress the decomposition and discoloration of the oil-phase active substance components such as retinol propionate, and significantly improve the residual rate of the oil-phase active substance in the emulsion over time.
[0026] 3. The emulsion of the present application has the characteristics of a simple preparation process and low requirements for equipment, so the production cost is low and the operation is easy. For the preparation of this emulsion, there is no need to use complex equipment such as a high-pressure homogenizer, and an emulsion with excellent antioxidant action on the oil-phase active substance can be prepared by simple stirring and mixing.
[0027] 4. The emulsion of this invention has simple components, mild raw materials, and low irritancy, and is in line with the trend towards environmentally friendly and safe raw materials in the daily chemical industry. [Brief explanation of the drawing]
[0028] The drawings provided herein are intended to provide a further understanding of the present application and constitute part of it. The schematic embodiments and descriptions thereof are for interpretive purposes and do not constitute an unreasonable limitation of the present application. [Figure 1] This is a schematic diagram showing the molecular structure of surfactant sodium. [Figure 2] This is a schematic diagram showing the photographic results of the oil gels according to Examples 1 to 3 of the present invention (reference numerals 1, 2, and 3 in the figure correspond to Examples 1, 2, and 3, respectively). [Figure 3] This is a schematic diagram showing the photographic results of the emulsions according to Examples 1 to 3 of the present invention (reference numerals 1 and 2 in the figure correspond to Examples 1 and 2, respectively). [Figure 4] This is a schematic diagram showing the stability results for Example 1 and Comparative Example 2 of the present application (reference numerals 1 and D2 in the figure correspond to Example 1 and Comparative Example 2, respectively). [Figure 5] This is a schematic diagram showing the stability results for Example 2 and Comparative Example 4 of the present application (reference numerals 2 and D4 in the figure correspond to Example 2 and Comparative Example 4, respectively). [Figure 6] This is a schematic diagram showing photographic results for Comparative Example 1 and Comparative Example 3 of the present application (the symbols D1 and D3 in the figure correspond to Comparative Example 1 and Comparative Example 3, respectively). [Figure 7] This is a schematic diagram showing the photographic results related to Comparative Example 7 of the present invention (the symbol D7 in the figure corresponds to Comparative Example 7). [Figure 8] This is a schematic diagram showing the stability results for Example 9 of the present invention (reference numeral 9 in the figure corresponds to Example 9). [Figure 9] This is a schematic diagram showing the stability results for Comparative Example 9 of the present application (the symbol D9 in the figure corresponds to Comparative Example 9). [Modes for carrying out the invention]
[0029] The present application will be described in detail below by combining examples, but the present application is not limited to these examples. Unless otherwise specified, the raw materials and catalysts used in the examples of the present application were all purchased through commercial channels.
[0030] Figure 1 shows a schematic diagram of the molecular structure of surfactant sodium. In the prior art, there are correlation reports that surfactant sodium has been applied as an emulsifier in the preparation of everyday products such as gels and emulsions. In the prior art, the addition of surfactant sodium mainly acts as an emulsifier, forming a stable emulsion in a mixture of two or more immiscible components. In the present application, in the process of research on applying surfactant sodium to emulsion preparation, the inventors discovered that in an emulsion containing an oil-phase active substance prepared by combining surfactant sodium with glycerin and pentaerythritol tetra(2-ethylhexanoic acid) ester, the addition of surfactant sodium effectively suppresses the diffusion of the oil-phase active substance at the emulsion interface, thereby reducing the oxidative decomposition of the oil-phase active substance and extending the effective action time of the oil-phase active substance in the emulsion.
[0031] Through further experimental research, the inventors discovered that the antioxidant and protective effect of surfactant sodium on oil-phase active substances is closely related to the selection of components it is combined with and the proportion of those components added. For example, when commonly used in emulsion preparation processes, such as oleic acid and GTCC, a good synergistic effect cannot be obtained, and in severe cases, emulsion formation is not possible, thus limiting its use in combination with surfactant sodium.
[0032] In this application, the inventors, based on the idea of improving the time-dependent retention rate of oil-phase active substances by applying sodium surfactant, explored the effects of suitable components and addition ratios for formulation with sodium surfactant, and obtained an emulsion scheme that significantly improves the time-dependent retention rate of oil-phase active substances. This greatly improves the preservation effect of oil-phase active substances, and the scheme of this application will be further explained below through specific examples, comparative examples, and test examples.
[0033] Example 1 The emulsion contains phases A, B, and C. Phase A contains 1 g of sodium surfactant and 20 g of glycerin (parts by weight), Phase B contains 15 g of retinol propionate and 75 g of pentaerythritol tetra(2-ethylhexanoic acid) (parts by weight), and Phase C contains 160 g of water (parts by weight).
[0034] It is prepared according to the following method.
[0035] Dissolve 1 g of sodium surfactin in 20 g of glycerin, heat at 80°C for 20 minutes, and stir to obtain a clear and stable D phase (A). Dissolve 15 g of retinol propionate in 75 g of pentaerythritol tetra(2-ethylhexanoic acid) ester in the liquid oil phase to obtain an active substance-containing oil phase (B).
[0036] Phase D (A) and oil phase (B) are kept warm in a 50°C water bath.
[0037] In a 50°C constant temperature water bath, phase D (A) is stirred at 600 rpm while oil phase (B) is slowly added. After confirming that the added oil phase is completely emulsified and dissolved each time, the oil phase is further added to obtain an active substance-containing oil gel. As the oil phase content increases, the viscosity of the system gradually increases, and then an active substance-containing oil gel is obtained.
[0038] While stirring the oil gel at 500 rpm, 160 g of aqueous phase (C) is added and stirred for 10 minutes to completely dissolve the oil gel and obtain a retinol propionate-containing water-in-oil (O / W) emulsion.
[0039] The photographic results of the oil gel prepared in this Example 1 are shown at reference numeral 1 in Figure 2, and the photographic results of the emulsion are shown at reference numeral 1 in Figure 3.
[0040] Example 2 The emulsion contains phases A, B, and C. Phase A contains 1 g of sodium surfactant and 20 g of glycerin (parts by weight), Phase B contains 15 g of boswellianol and 75 g of pentaerythritol tetra(2-ethylhexanoic acid) ester (parts by weight), and Phase C contains 160 g of water (parts by weight).
[0041] It is prepared according to the following method.
[0042] Dissolve 1 g of surfactant sodium in 20 g of glycerin, heat at 80°C for 20 minutes, and stir to obtain a clear and stable D phase (A). Dissolve 15 g of boswellianol in 75 g of pentaerythritol tetra(2-ethylhexanoic acid) ester in the liquid oil phase to obtain an active substance-containing oil phase (B).
[0043] Phase D (A) and oil phase (B) are kept warm in a 50°C water bath.
[0044] In a 50°C constant temperature water bath, phase D (A) is stirred at 600 rpm while oil phase (B) is slowly added. After confirming that the added oil phase is completely emulsified and dissolved each time, the oil phase is further added to obtain an active substance-containing oil gel. As the oil phase content increases, the viscosity of the system gradually increases, and then an active substance-containing oil gel is obtained.
[0045] While stirring the oil gel at 500 rpm, 160 g of aqueous phase (C) is added and stirred for 10 minutes to completely dissolve the oil gel and obtain a boswellianol-containing water-in-oil (O / W) emulsion.
[0046] The photographic results of the oil gel prepared in this Example 2 are shown at reference numeral 2 in Figure 2, and the photographic results of the emulsion are shown at reference numeral 2 in Figure 3.
[0047] Example 3 The emulsion contains phases A, B, and C. Phase A contains 1 g of sodium surfactant and 20 g of glycerin (parts by weight), Phase B contains 15 g of tetrapalmitate ascorbic acid and 75 g of pentaerythritol tetra(2-ethylhexanoic acid) (parts by weight), and Phase C contains 160 g of water (parts by weight).
[0048] It is prepared according to the following method.
[0049] Dissolve 1 g of sodium surfactin in 20 g of glycerin, heat at 80°C for 20 minutes, and stir to obtain a clear and stable phase D (A). Dissolve 15 g of tetrapalmitate ascorbic acid in 75 g of pentaerythritol tetra(2-ethylhexanoic acid) ester in the liquid oil phase to obtain an active substance-containing oil phase (B).
[0050] Phase D (A) and oil phase (B) are kept warm in a 50°C water bath.
[0051] In a 50°C constant temperature water bath, phase D (A) is stirred at 600 rpm while oil phase (B) is slowly added. After confirming that the added oil phase is completely emulsified and dissolved each time, the oil phase is further added to obtain an active substance-containing oil gel. As the oil phase content increases, the viscosity of the system gradually increases, and then an active substance-containing oil gel is obtained.
[0052] While stirring the oil gel at 500 rpm, 160 g of aqueous phase (C) is added and stirred for 10 minutes to completely dissolve the oil gel and obtain an ascorbic acid tetrapalmitate-containing water-in-oil (O / W) emulsion.
[0053] The photographic results of the oil gel prepared in this Example 3 are shown by reference numeral 3 in Figure 2.
[0054] Example 4 The emulsion contains phases A, B, and C. Phase A contains 1 g of sodium surfactant and 20 g of glycerin (parts by weight), Phase B contains 15 g of retinol propionate and 75 g of pentaerythritol tetra(2-ethylhexanoic acid) (parts by weight), and Phase C contains 111 g of water (parts by weight).
[0055] It is prepared according to the following method.
[0056] Dissolve 1 g of sodium surfactin in 20 g of glycerin, heat at 80°C for 20 minutes, and stir to obtain a clear and stable D phase (A). Dissolve 15 g of retinol propionate in 75 g of pentaerythritol tetra(2-ethylhexanoic acid) ester in the liquid oil phase to obtain an active substance-containing oil phase (B).
[0057] Phase D (A) and oil phase (B) are kept warm in a 50°C water bath.
[0058] In a 50°C constant temperature water bath, phase D (A) is stirred at 600 rpm while oil phase (B) is slowly added. After confirming that the added oil phase is completely emulsified and dissolved each time, the oil phase is further added to obtain an active substance-containing oil gel. As the oil phase content increases, the viscosity of the system gradually increases, and then an active substance-containing oil gel is obtained.
[0059] While stirring the oil gel at 500 rpm, 111 g of aqueous phase (C) is added and stirred for 10 minutes to completely dissolve the oil gel and obtain a retinol propionate-containing water-in-oil (O / W) emulsion.
[0060] Example 5 The emulsion contains phases A, B, and C. Phase A contains 1 g of sodium surfactant and 20 g of glycerin (parts by weight), Phase B contains 15 g of retinol propionate and 75 g of pentaerythritol tetra(2-ethylhexanoic acid) (parts by weight), and Phase C contains 444 g of water (parts by weight).
[0061] It is prepared according to the following method.
[0062] Dissolve 1 g of sodium surfactin in 20 g of glycerin, heat at 80°C for 20 minutes, and stir to obtain a clear and stable D phase (A). Dissolve 15 g of retinol propionate in 75 g of pentaerythritol tetra(2-ethylhexanoic acid) ester in the liquid oil phase to obtain an active substance-containing oil phase (B).
[0063] Phase D (A) and oil phase (B) are kept warm in a 50°C water bath.
[0064] In a 50°C constant temperature water bath, phase D (A) is stirred at 600 rpm while oil phase (B) is slowly added. After confirming that the added oil phase is completely emulsified and dissolved each time, the oil phase is further added to obtain an active substance-containing oil gel. As the oil phase content increases, the viscosity of the system gradually increases, and then an active substance-containing oil gel is obtained.
[0065] While stirring the oil gel at 500 rpm, 444 g of aqueous phase (C) is added and stirred for 10 minutes to completely dissolve the oil gel and obtain a retinol propionate-containing water-in-oil (O / W) emulsion.
[0066] Example 6 The emulsion contains phases A, B, and C. Phase A contains 1 g of sodium surfactant and 20 g of glycerin (parts by weight), Phase B contains 10 g of retinol propionate and 80 g of pentaerythritol tetra(2-ethylhexanoic acid) (parts by weight), and Phase C contains 160 g of water (parts by weight).
[0067] It is prepared according to the following method.
[0068] Dissolve 1 g of sodium surfactin in 20 g of glycerin, heat at 80°C for 20 minutes, and stir to obtain a clear and stable phase D (A). Dissolve 10 g of retinol propionate in 80 g of pentaerythritol tetra(2-ethylhexanoic acid) ester in the liquid oil phase to obtain an active substance-containing oil phase (B).
[0069] Phase D (A) and oil phase (B) are kept warm in a 50°C water bath.
[0070] In a 50°C constant temperature water bath, phase D (A) is stirred at 600 rpm while oil phase (B) is slowly added. After confirming that the added oil phase is completely emulsified and dissolved each time, the oil phase is further added to obtain an active substance-containing oil gel. As the oil phase content increases, the viscosity of the system gradually increases, and then an active substance-containing oil gel is obtained.
[0071] While stirring the oil gel at 500 rpm, 160 g of aqueous phase (C) is added and stirred for 10 minutes to completely dissolve the oil gel and obtain a retinol propionate-containing water-in-oil (O / W) emulsion.
[0072] Example 7 The emulsion contains phases A, B, and C. Phase A contains 0.45 g of sodium surfactant and 8.55 g of glycerin (parts by weight), Phase B contains 15 g of retinol propionate and 75 g of pentaerythritol tetra(2-ethylhexanoic acid) (parts by weight), and Phase C contains 160 g of water (parts by weight).
[0073] It is prepared according to the following method.
[0074] Dissolve 0.45 g of sodium surfactin in 8.55 g of glycerin, heat at 80°C for 20 minutes, and stir to obtain a clear and stable phase D (A). Dissolve 15 g of retinol propionate in 75 g of pentaerythritol tetra(2-ethylhexanoic acid) ester in the liquid oil phase to obtain an active substance-containing oil phase (B).
[0075] Phase D (A) and oil phase (B) are kept warm in a 50°C water bath.
[0076] In a 50°C constant temperature water bath, phase D (A) is stirred at 600 rpm while oil phase (B) is slowly added. After confirming that the added oil phase is completely emulsified and dissolved each time, the oil phase is further added to obtain an active substance-containing oil gel. As the oil phase content increases, the viscosity of the system gradually increases, and then an active substance-containing oil gel is obtained.
[0077] While stirring the oil gel at 500 rpm, 160 g of aqueous phase (C) is added and stirred for 10 minutes to completely dissolve the oil gel and obtain a retinol propionate-containing water-in-oil (O / W) emulsion.
[0078] Example 8 The emulsion contains phases A, B, and C. Phase A contains 1.5 g of sodium surfactant and 28.5 g of glycerin (parts by weight), Phase B contains 15 g of retinol propionate and 75 g of pentaerythritol tetra(2-ethylhexanoic acid) (parts by weight), and Phase C contains 200 g of water (parts by weight).
[0079] It is prepared according to the following method.
[0080] Dissolve 1.5 g of sodium surfactin in 28.5 g of glycerin, heat at 80°C for 20 minutes, and stir to obtain a clear and stable phase D (A). Dissolve 15 g of retinol propionate in 75 g of pentaerythritol tetra(2-ethylhexanoic acid) ester in the liquid oil phase to obtain an active substance-containing oil phase (B).
[0081] Phase D (A) and oil phase (B) are kept warm in a 50°C water bath.
[0082] In a 50°C constant temperature water bath, phase D (A) is stirred at 600 rpm while oil phase (B) is slowly added. After confirming that the added oil phase is completely emulsified and dissolved each time, the oil phase is further added to obtain an active substance-containing oil gel. As the oil phase content increases, the viscosity of the system gradually increases, and then an active substance-containing oil gel is obtained.
[0083] While stirring the oil gel at 500 rpm, 200 g of aqueous phase (C) is added and stirred for 10 minutes to completely dissolve the oil gel and obtain a retinol propionate-containing water-in-oil (O / W) emulsion.
[0084] Example 9 The emulsion contains phases A, B, and C. Phase A contains 0.75 g of sodium surfactant and 6.75 g of glycerin (parts by weight), Phase B contains 2 g of phenylethyl resorcinol and 20.5 g of pentaerythritol tetra(2-ethylhexanoic acid) ester (parts by weight), and Phase C contains 70 g of water (parts by weight).
[0085] It is prepared according to the following method.
[0086] Dissolve 0.75 g of surfactant sodium in 6.75 g of glycerin, heat at 80°C for 20 minutes, and stir to obtain a clear and stable D phase (A). Dissolve 2 g of phenylethyl resorcinol in 20.5 g of pentaerythritol tetra(2-ethylhexanoic acid) ester in the liquid oil phase to obtain an active substance-containing oil phase (B).
[0087] Phase D (A) and oil phase (B) are kept warm in a 50°C water bath.
[0088] In a 50°C constant temperature water bath, phase D (A) is stirred at 600 rpm while oil phase (B) is slowly added. After confirming that the added oil phase is completely emulsified and dissolved each time, the oil phase is further added to obtain an active substance-containing oil gel. As the oil phase content increases, the viscosity of the system gradually increases, and then an active substance-containing oil gel is obtained.
[0089] While stirring the oil gel at 500 rpm, 70 g of aqueous phase (C) was added and stirred for 10 minutes to completely dissolve the oil gel and obtain a phenylethyl resorcinol-containing water-in-oil (O / W) emulsion. The stability results are shown by reference numeral 9 in Figure 8.
[0090] Comparative Example 1 The emulsion contains phases A, B, and C. Phase A contains 1 g of sodium surfactant and 20 g of glycerin (parts by weight), Phase B contains 15 g of retinol propionate and 75 g of oleic acid (parts by weight), and Phase C contains 160 g of water (parts by weight).
[0091] It is prepared according to the following method.
[0092] Dissolve 1 g of sodium surfactin in 20 g of glycerin, heat at 80°C for 20 minutes, and stir to obtain a clear and stable D phase (A). Dissolve 15 g of retinol propionate in 75 g of oleic acid in the liquid oil phase to obtain an active substance-containing oil phase (B).
[0093] Phase D (A) and oil phase (B) are kept warm in a 50°C water bath.
[0094] When the oil phase (B) was slowly added while stirring phase D (A) at 600 rpm in a 50°C constant temperature water bath, it was confirmed that the two phases could not be mixed or emulsified, and the result is shown as indicated by the symbol D1 in Figure 6.
[0095] Comparative Example 2 The emulsion contains phases A, B, and C. Phase A contains 1 g of sodium surfactant and 20 g of glycerin (parts by weight), Phase B contains 15 g of retinol propionate and 75 g of GTCC (parts by weight), and Phase C contains 160 g of water (parts by weight).
[0096] It is prepared according to the following method.
[0097] Dissolve 1 g of sodium surfactin in 20 g of glycerin, heat at 80°C for 20 minutes, and stir to obtain a clear and stable D phase (A). Dissolve 15 g of retinol propionate in 75 g of GTCC liquid oil phase to obtain an active substance-containing oil phase (B).
[0098] Phase D (A) and oil phase (B) are kept warm in a 50°C water bath.
[0099] In a 50°C constant temperature water bath, phase D (A) is stirred at 600 rpm while oil phase (B) is slowly added. After confirming that the added oil phase is completely emulsified and dissolved each time, the oil phase is further added to obtain an active substance-containing oil gel. As the oil phase content increases, the viscosity of the system gradually increases, and then an active substance-containing oil gel is obtained.
[0100] While stirring the oil gel at 500 rpm, 160 g of aqueous phase (C) is added and stirred for 10 minutes to completely dissolve the oil gel and obtain a retinol propionate-containing water-in-oil (O / W) emulsion.
[0101] The results are shown in Figure 4, labeled D2, indicating that this emulsion has poor storage stability and can cause problems such as precipitation and discoloration.
[0102] Comparative Example 3 The emulsion contains phases A, B, and C. Phase A contains 1 g of sodium surfactant and 20 g of butylene glycol (parts by weight), Phase B contains 15 g of retinol propionate and 75 g of pentaerythritol tetra(2-ethylhexanoic acid) (parts by weight), and Phase C contains 160 g of water (parts by weight).
[0103] It is prepared according to the following method.
[0104] Dissolve 1 g of surfactant sodium in 20 g of butylene glycol and heat at 80°C for 20 minutes with stirring, but a clear and stable D phase (A) could not be obtained. Dissolve 15 g of boswellianol in 75 g of pentaerythritol tetra(2-ethylhexanoic acid) ester in the liquid oil phase to obtain the active substance-containing oil phase (B).
[0105] Phase D (A) and oil phase (B) are kept warm in a 50°C water bath.
[0106] When the oil phase (B) was slowly added while stirring phase D (A) at 600 rpm in a 50°C constant temperature water bath, it was confirmed that an oil gel could not be formed, and the result is shown as indicated by the symbol D3 in Figure 6.
[0107] Comparative Example 4 The emulsion contains phases A, B, and C. Phase A contains 1 g of sodium surfactant and 20 g of glycerin (parts by weight), Phase B contains 15 g of boswellianol and 75 g of GTCC (parts by weight), and Phase C contains 160 g of water (parts by weight).
[0108] It is prepared according to the following method.
[0109] Dissolve 1 g of surfactant sodium in 20 g of glycerin, heat at 80°C for 20 minutes, and stir to obtain a clear and stable D phase (A). Dissolve 15 g of boswellianol in 75 g of liquid GTCC to obtain an active substance-containing oil phase (B).
[0110] Phase D (A) and oil phase (B) are kept warm in a 50°C water bath.
[0111] In a 50°C constant temperature water bath, phase D (A) is stirred at 600 rpm while oil phase (B) is slowly added. After confirming that the added oil phase is completely emulsified and dissolved each time, the oil phase is further added to obtain an active substance-containing oil gel. As the oil phase content increases, the viscosity of the system gradually increases, and then an active substance-containing oil gel is obtained.
[0112] While stirring the oil gel at 500 rpm, 160 g of aqueous phase (C) is added and stirred for 10 minutes to completely dissolve the oil gel and obtain a boswellianol-containing water-in-oil (O / W) emulsion.
[0113] The results are shown in Figure 5, labeled D4, indicating that this emulsion has poor storage stability and can cause problems such as precipitation and discoloration.
[0114] Comparative Example 5 The emulsion contains phases A, B, and C. Phase A contains 1 g of sodium surfactant and 20 g of glycerin (parts by weight), Phase B contains 15 g of retinol propionate and 75 g of pentaerythritol tetra(2-ethylhexanoic acid) (parts by weight), and Phase C contains 100 g of water (parts by weight).
[0115] It is prepared according to the following method.
[0116] Dissolve 1 g of sodium surfactin in 20 g of glycerin, heat at 80°C for 20 minutes, and stir to obtain a clear and stable D phase (A). Dissolve 15 g of retinol propionate in 75 g of pentaerythritol tetra(2-ethylhexanoic acid) ester in the liquid oil phase to obtain an active substance-containing oil phase (B).
[0117] Phase D (A) and oil phase (B) are kept warm in a 50°C water bath.
[0118] In a 50°C constant temperature water bath, phase D (A) is stirred at 600 rpm while oil phase (B) is slowly added. After confirming that the added oil phase is completely emulsified and dissolved each time, the oil phase is further added to obtain an active substance-containing oil gel. As the oil phase content increases, the viscosity of the system gradually increases, and then an active substance-containing oil gel is obtained.
[0119] When 100g of aqueous phase (C) was added to the oil gel while stirring at 500 rpm and stirred for 10 minutes, the oil gel could not be completely dissolved, resulting in a highly viscous and opaque mixture that does not fall under the category of emulsion.
[0120] Comparative Example 6 The emulsion contains phases A, B, and C. Phase A contains 0.5 g of sodium surfactant and 20.5 g of glycerin (parts by weight), Phase B contains 15 g of retinol propionate and 75 g of pentaerythritol tetra(2-ethylhexanoic acid) (parts by weight), and Phase C contains 160 g of water (parts by weight).
[0121] It is prepared according to the following method.
[0122] Dissolve 0.5 g of surfactant sodium in 20.5 g of glycerin, heat at 80°C for 20 minutes, and stir to obtain a clear and stable D phase (A). Dissolve 15 g of retinol propionate in 75 g of pentaerythritol tetra(2-ethylhexanoic acid) ester in the liquid oil phase to obtain an active substance-containing oil phase (B).
[0123] Phase D (A) and oil phase (B) are kept warm in a 50°C water bath.
[0124] When oil phase (B) was gradually added to phase D (A) in a constant temperature water bath at 50°C while stirring at 600 rpm, the oil phase could not be completely emulsified or dissolved in phase D, and free oil phase always remained. This explains that the ratio of lipopeptide to glycerin was too low, preventing the formation of an oil phase gel and thus an emulsion.
[0125] Comparative Example 7 The emulsion contains phases A, B, and C. Phase A contains 0.4 g of sodium surfactant and 8 g of glycerin (parts by weight), Phase B contains 15 g of retinol propionate and 75 g of pentaerythritol tetra(2-ethylhexanoic acid) (parts by weight), and Phase C contains 138 g of water (parts by weight).
[0126] It is prepared according to the following method.
[0127] Dissolve 0.4 g of surfactant sodium in 8 g of glycerin, heat at 80°C for 20 minutes, and stir to obtain a clear and stable phase D (A). Dissolve 15 g of retinol propionate in 75 g of pentaerythritol tetra(2-ethylhexanoic acid) ester in the liquid oil phase to obtain an active substance-containing oil phase (B).
[0128] Phase D (A) and oil phase (B) are kept warm in a 50°C water bath.
[0129] When the oil phase (B) was slowly added to the D phase (A) while stirring at 600 rpm in a 50°C constant temperature water bath, it was confirmed that the oil phase could not be completely emulsified or dissolved in the D phase, and that free oil phase always remained. This is because the A:B ratio was too small to form an oil phase gel, and therefore an emulsion could not be formed, as shown in D7 in Figure 7.
[0130] Comparative Example 8 The emulsion contains phases A, B, and C. Phase A contains 1 g of sodium surfactant and 20 g of glycerin (parts by weight), Phase B contains 30 g of retinol propionate and 60 g of pentaerythritol tetra(2-ethylhexanoic acid) (parts by weight), and Phase C contains 160 g of water (parts by weight).
[0131] It is prepared according to the following method.
[0132] Dissolve 1 g of sodium surfactin in 20 g of glycerin, heat at 80°C for 20 minutes, and stir to obtain a clear and stable phase D (A). Dissolve 30 g of retinol propionate in 60 g of pentaerythritol tetra(2-ethylhexanoic acid) ester in the liquid oil phase to obtain an active substance-containing oil phase (B).
[0133] Phase D (A) and oil phase (B) are kept warm in a 50°C water bath.
[0134] In a 50°C constant temperature water bath, phase D (A) is stirred at 600 rpm while oil phase (B) is slowly added. After confirming that the added oil phase is completely emulsified and dissolved each time, the oil phase is further added to obtain an active substance-containing oil gel. As the oil phase content increases, the viscosity of the system gradually increases, and then an active substance-containing oil gel is obtained.
[0135] While stirring the oil gel at 500 rpm, 160 g of aqueous phase (C) is added and stirred for 10 minutes to completely dissolve the oil gel and obtain a retinol propionate-containing water-in-oil (O / W) emulsion.
[0136] Comparative Example 9 The emulsion contains phases A, B, and C. Phase A contains 0.4 g of sodium surfactant and 7.1 g of glycerin (parts by weight), Phase B contains 2 g of phenylethyl resorcinol and 28 g of pentaerythritol tetra(2-ethylhexanoic acid) ester (parts by weight), and Phase C contains 62.5 g of water (parts by weight).
[0137] It is prepared according to the following method.
[0138] Dissolve 0.4 g of surfactant sodium in 7.1 g of glycerin, heat at 80°C for 20 minutes, and stir to obtain a clear and stable D phase (A). Dissolve 2 g of phenylethyl resorcinol in 28 g of pentaerythritol tetra(2-ethylhexanoic acid) ester in the liquid oil phase to obtain an active substance-containing oil phase (B).
[0139] Phase D (A) and oil phase (B) are kept warm in a 50°C water bath.
[0140] In a 50°C constant temperature water bath, phase D (A) is stirred at 600 rpm while oil phase (B) is slowly added. After confirming that the added oil phase is completely emulsified and dissolved each time, the oil phase is further added to obtain an active substance-containing oil gel. As the oil phase content increases, the viscosity of the system gradually increases, and then an active substance-containing oil gel is obtained.
[0141] While stirring the oil gel at 500 rpm, 62.5 g of aqueous phase (C) was added and stirred for 10 minutes to completely dissolve the oil gel and obtain a phenylethyl resorcinol-containing water-in-oil (O / W) emulsion. The stability results are shown by reference numeral 9 in Figure 9.
[0142] Test Example 1 Method for measuring the decomposition rate of active substances: The decomposition rate of active substances such as retinol propionate, boswellianol, and phenylethyl resorcinol will be measured using high-performance liquid chromatography (HCM) with an ultraviolet detector. Specifically, emulsions of Examples 1-9, Comparative Examples 2, 4, and 8 will be left in a 50°C constant temperature bath, and the emulsions will be dissolved in methanol every 7, 15, and 28 days, and the decomposition rate will be measured by HCM. Specifically, the HCM measurement conditions are as follows: Chromatography column: C18 reversed-phase chromatography column (250 × 4.6 mm, 5 μm) Mobile phase components: methanol 98 vol%, water 2 vol%, Mobile phase flow rate: 1mL / min, Detection wavelength: 325nm, Quantification method: external standard method.
[0143] Table 1 shows the proportions of components in the emulsions of Examples 1-9 and Comparative Examples 1-9, and Table 2 shows the results of the active substance degradation rate measurement test in Test Example 1.
[0144] Table 1: Emulsion component ratios [Table 1] TIFF2026528991000003.tif228170 TIFF2026528991000004.tif92170 Table 2 Results of the measurement test of the degradation rate of active substances [Table 2] The results in Table 2 clearly show that the emulsions according to the examples of the present application have a significantly higher retention rate over time compared to Comparative Examples 2 and 4. Pentaerythritol tetra(2-ethylhexanoic acid) ester, the oil phase component in the present application, exhibits excellent blending effects with other components for GTCC, maintaining a high retention rate even after 28 days, whereas Comparative Examples 2 and 4 experienced precipitation problems after 28 days.
[0145] Furthermore, from the experimental results described in Examples 1-9 and Comparative Examples 1-9, and the experimental results in Figures 2-9, it became clear that when the components of the emulsion in the present invention are blended in appropriate proportions, an excellent protective effect against the oil phase active substance is observed, and the emulsion product can be successfully prepared and obtained. On the other hand, when other components are blended or the blending ratio is inappropriate, problems such as precipitation, inability to form an emulsion, inability to form an oil gel, and significant discoloration occur. From Figure 5, it can be seen that the emulsion of Comparative Example 4 underwent creaming out after storage, with a large amount of retinol propionate ester precipitation and significant discoloration. From Figure 6, it can be seen that the emulsion of Comparative Example 3 underwent significant discoloration after storage, and in Comparative Example 1, it was seen that the mixture of the oil phase, lipopeptide, and glycerin did not form an oil gel and underwent layer separation. From Figure 7, it can be seen that the quality of the oil gel in Comparative Example 7 was poor and that a free oil phase was present. From Figure 9, it can be seen that the emulsion of Comparative Example 9 underwent clear layer separation, indicating poor emulsion stability.
[0146] In contrast, the embodiment of the present application introduces surfactant sodium and optimizes the glycerin and pentaerythritol tetra(2-ethylhexanoic acid) ester blended with the oil phase active substance, as well as their blending ratio, thereby exhibiting an extremely excellent protective effect on the oil phase active substance. This allows the remaining rate of the oil phase active substance to be maintained at 90% or more even after 28 days, effectively reducing the decomposition of the oil phase active substance.
[0147] The above are merely embodiments of the present application, and the scope of protection of the present application is not limited to these specific embodiments, but is determined by the claims of the present application. Those skilled in the art can make various changes and modifications to the present application. Any modifications, substitutions with equivalents, improvements, etc., made within the scope of the technical idea and principles of the present application shall all be included in the scope of protection of the present application.
Claims
1. It is an oil gel, (a) at least one lipopeptide, (b) Glycerin and (c) Pentaerythritol tetra(2-ethylhexanoic acid) ester and (d) An oil gel characterized by containing at least one oil-phase active substance.
2. The oil gel according to claim 1, characterized in that the weight percentage of the lipopeptide and the glycerin is 3% or more.
3. The oil gel according to claim 1, characterized in that the weight ratio of the oil phase active substance to the pentaerythritol tetra(2-ethylhexanoic acid) ester is 1:3 to 13.
4. The oil gel according to claim 1, characterized in that the ratio of the total weight of the lipopeptide and the glycerin to the total weight of the oil phase active substance and the pentaerythritol tetra(2-ethylhexanoic acid) ester is 1:3 to 10.
5. The oil gel according to claim 2, characterized in that the weight percentage of the lipopeptide and the glycerin is 5% or more.
6. The oil gel according to claim 5, characterized in that the weight percentage of the lipopeptide and the glycerin is 5% to 12%.
7. The oil gel according to claim 3, characterized in that the weight ratio of the oil phase active substance to the pentaerythritol tetra(2-ethylhexanoic acid) ester is 1:5 to 11.
8. The oil gel according to claim 1, characterized in that the lipopeptide contains one or more of surfactin sodium, iturine, fenzi, phongidin, daptomycin, polymyxin, batrasilidine L, phospholipidase inhibitor peptide, and batrasilidine D.
9. The oil gel according to claim 1, characterized in that the oil phase active substance contains one or more of the following: retinol, retinol acetate, retinol propionate, retinol palmitate, boswellianol, equol, nerve acid, ascorbic acid palmitate, ascorbic acid tetrapalmitate, and phenylethyl resorcinol.
10. It is an emulsion. An emulsion comprising a nozzle assembly according to any one of claims 1 to 9.
11. The emulsion according to claim 10, characterized in that the ratio of the total weight of the lipopeptide, the glycerin, the oil phase active substance, and the pentaerythritol tetra(2-ethylhexanoic acid) ester to the weight of water is 1:1 to 4.
12. 1) Dissolve the lipopeptide in glycerin, heat and stir to obtain solution A, 2) Dissolve the oil-phase active substance in pentaerythritol tetra(2-ethylhexanoic acid) ester and stir to obtain solution B, 3) A method for preparing an oil gel according to any one of claims 1 to 9, characterized by comprising adding solution A to solution B under constant temperature water bath and stirring conditions to obtain an oil gel.
13. The method for preparing an emulsion according to claim 10 or 11, further comprising the step of adding an aqueous phase to an oil gel under stirring conditions and mixing thoroughly to obtain a lipopeptide-containing emulsion.
14. The use is characterized in that the oil gel according to any one of claims 1 to 9, or the emulsion according to claim 10 or claim 11, is used in cosmetics.