Water-in-silicone oil self-emulsifying composition, essence water and preparation method and application thereof
By spontaneously forming an emulsion under low shear force by the water-in-silicone self-emulsification composition of silicone oil, the problem of low transdermal absorption of water-soluble active substances is solved by utilizing the sealing and polarity characteristics of phenyl silicone oil, and stable transdermal absorption and industrial application are achieved.
Patent Information
- Application Number
- CN202510403709.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-01
- Publication Date
- 2025-07-04
AI Technical Summary
The prior art is difficult to effectively improve the transdermal absorption rate of water-soluble actives, and traditional permeability-promoting methods may damage the skin or cannot be applied on a large scale.
A water-in-silicone self-emulsification composition is employed, comprising an aqueous phase and an oily phase, wherein the aqueous phase comprises a polyol and the oily phase comprises a phenyl silicone oil, and the emulsion is formed spontaneously by low shear force, enhancing transdermal absorption of the active substance using the enclosing and polar properties of the phenyl silicone oil.
Spontaneously form a stable emulsion under low-strength mechanical force, extending the residence time of the active substance on the skin, improving transdermal absorption, and is suitable for large-scale industrial production.
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Figure CN120241534A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of cosmetics, and particularly relates to a water-in-silicone self-emulsifying composition, essence water, and their preparation methods and applications. Background Art
[0002] There is a natural barrier on the skin surface, which is composed of closely arranged keratinocytes and lipids, thus forming a stable "brick-wall structure" to protect the skin from external conditions. Among them, the lipid barrier is mainly composed of substances such as ceramides, cholesterol, and free fatty acids. They are highly hydrophobic and have a natural hindrance to the penetration of water-soluble substances, making most water-soluble active substances can only stay on the skin surface or rely on special mechanisms to enter the deep layer of the skin. Therefore, a major problem of water-based products with extremely high water content (such as toner, spray, etc.) is how to make more water-soluble active substances penetrate through the stratum corneum to the skin.
[0003] Currently, the common penetration enhancement methods on the market are divided into chemical penetration enhancement technology, physical penetration enhancement technology, biological penetration enhancement technology, and pharmaceutical penetration enhancement technology.
[0004] Chemical penetration enhancement technology changes the interaction of stratum corneum lipids by using compounds to achieve the purpose of enhancing permeability. The most common compounds are substances such as ethanol and menthol, but these substances usually cause damage to the skin barrier.
[0005] Physical penetration enhancement technology enhances penetration by physically changing the stratum corneum structure. Common ones include ultrasonic introduction and microneedles. Such methods are usually used in beauty salons, cannot be widely used in daily life, and may cause skin damage.
[0006] Pharmaceutical penetration enhancement technology is the fastest-developing and most widely used transdermal penetration enhancement technology in the cosmetics industry. Common ones include liposome, microcapsule, and microemulsion technologies. It can not only protect active ingredients and enhance their stability, but also expand their transdermal absorption. Especially liposome technology, relying on the phospholipid bilayer structure similar to the cell membrane, directly transports the encapsulated active substances to the target cells.
[0007] The patent application with the application number 202411585675.7 discloses a rhamnolipid self-emulsifying skin care lotion, a preparation method and an application thereof. Specifically, the application of rhamnolipid in maintaining skin pH, skin moisturization or promoting penetration is disclosed, and a rhamnolipid self-emulsifying skin care lotion is disclosed. Its raw materials include an aqueous phase and an oil phase. An acid or a base may be contained in the aqueous phase, and the mass percentage of rhamnolipid in the skin care lotion is ≥0.2%; the pH value of the skin care lotion is 5.0 - 6.0. The skin care lotion of this invention not only has high moisturizing property, high stability and high penetration ability, but also has the advantage of maintaining skin pH for a long time. However, rhamnolipid belongs to a natural surfactant, and its emulsifying property is known. At the same time, the formula added with rhamnolipid needs to keep the formula pH stable within 5.0 - 6.0, otherwise problems such as thinning of the lotion, demulsification and precipitation may occur.
[0008] Therefore, it has become a problem to be solved at present to provide a lotion that can improve skin permeability and expand the transdermal absorption degree of active ingredients. Summary of the Invention
[0009] Based on the above technical background, the main object of the present invention is to provide a water-in-silicone oil self-emulsifying composition, essence water and their preparation methods and applications to overcome the deficiencies in the prior art.
[0010] To achieve the foregoing invention object, the technical solutions adopted by the present invention include:
[0011] In the first aspect of the present invention, a water-in-silicone oil self-emulsifying composition is provided. The water-in-silicone oil self-emulsifying composition includes an aqueous phase and an oil phase;
[0012] The aqueous phase includes water and polyols;
[0013] The oil phase includes phenyl silicone oil.
[0014] Preferably, the polyol is selected from one or more of glycerol, butanediol, propylene glycol, pentanediol and hexanediol.
[0015] Preferably, the polyol accounts for 1 - 70% of the total mass of the aqueous phase
[0016] Preferably, the phenyl silicone oil is selected from one or more of trimethylpentaphenyltrisiloxane, diphenylhexamethylsiloxane, tetramethyltetraphenyltrisiloxane, phenylpolydimethylsiloxane and diphenylpolydimethylsiloxane.
[0017] Preferably, the aqueous phase further includes an emulsification stabilizer;
[0018] The emulsification stabilizer is selected from one or more of betaine, erythritol, inulin, mannitol, niacinamide, panthenol, allantoin, metal chloride salts.
[0019] Preferably, the oil phase further comprises a polar oil compatible with phenyl silicone oil;
[0020] The polar oil compatible with phenyl silicone oil is selected from one or more of pentaerythritol tetra(ethylhexanoate), isononyl isononanoate, dicaprylyl carbonate, and tocopheryl acetate.
[0021] More preferably, the polar oil compatible with phenyl silicone oil accounts for 1-50% of the total mass of the oil phase.
[0022] A second aspect of the present invention lies in providing a method for preparing the water-in-silicone oil self-emulsifying composition described in the first aspect of the present invention, and the preparation method includes the following steps:
[0023] Step 1: Mix water and polyol, heat up to 65-75 °C, and stir evenly to obtain an aqueous phase;
[0024] Step 2: Heat the phenyl silicone oil to 35-45 °C and stir evenly to obtain an oil phase.
[0025] A third aspect of the present invention lies in providing an application of the water-in-silicone oil self-emulsifying composition described in the first aspect of the present invention in the preparation of cosmetics.
[0026] A fourth aspect of the present invention lies in providing an essence water, and the essence water is prepared from raw materials including the water-in-silicone oil self-emulsifying composition described in the first aspect of the present invention.
[0027] In the essence water, the mass ratio of the aqueous phase to the oil phase in the water-in-silicone oil self-emulsifying composition is (90-99):(1-10).
[0028] The beneficial effects of the present invention:
[0029] (1) The water-in-silicone oil self-emulsifying composition of the present invention includes an aqueous phase and an oil phase. The aqueous phase includes polyol, and the oil phase includes phenyl silicone oil. The composition of the present invention uses phenyl silicone oil as the continuous phase. This composition can undergo a phase transformation on the face, and by undergoing phase inversion emulsification on the face, an instant water-in-silicone oil emulsion can be obtained. At the same time, by utilizing the strong sealing property of phenyl silicone oil, the residence time of water-soluble active substances on the skin can be extended.
[0030] (2) The water-in-silicone oil self-emulsifying composition of the present invention is a penetration-enhancing composition made with phenyl silicone oil as the continuous phase. Without traditional emulsifiers, this composition can spontaneously form an emulsion under low-intensity mechanical force, enhancing the transdermal absorption of active substances or functional ingredients and effectively improving the problem of low penetration rate of active substances in aqueous products. In addition, the introduction of phenyl groups in phenyl silicone oil enhances the polarity of the silicone oil, enabling it to reduce the interfacial tension between water and oil, thereby promoting the formation of smaller and more stable water droplets in the phenyl silicone oil. This makes the composition not only have self-emulsifying properties but also form a more stable emulsifying system.
[0031] (3) The polyol added in the present invention plays a role in regulating the interfacial tension between water and oil in the water-in-silicone oil self-emulsifying composition. Part of the polyol molecule dissolves in the aqueous phase, and the other part accumulates at the water-oil interface, acting as a "bridge". The addition of polyol not only helps in the formation of the self-emulsifying system but also contributes to the formation of a more stable self-emulsifying system.
[0032] (4) The preparation method of the water-in-silicone oil self-emulsifying composition of the present invention is simple and fully adaptable to large-scale industrial production. Cosmetics containing the composition of the present invention can enhance the penetration rate of water-soluble active substances and the efficacy of cosmetics. The composition of the present invention has good application prospects in the cosmetics industry. Description of the Drawings
[0033] Figure 1 Pictures showing the compositions prepared in Example 2, Comparative Example 1, and Comparative Example 2 before shaking;
[0034] Figure 2 Pictures showing the compositions prepared in Example 2, Comparative Example 1, and Comparative Example 2 after shaking;
[0035] Figure 3 Micrographs showing the compositions prepared in Example 2, Comparative Example 1, and Comparative Example 2 after emulsification;
[0036] Figure 4 Pictures showing the compositions prepared in Examples 2 to 5 before shaking;
[0037] Figure 5 Pictures showing the compositions prepared in Examples 2 to 5 after shaking;
[0038] Figure 6 Test results showing the penetration amounts of the essence waters prepared in Examples 6 to 7 and Comparative Examples 3 to 4. Detailed Description of the Invention
[0039] The present invention will be described in detail below, and its features and advantages will become clearer and more distinct with these descriptions.
[0040] The first aspect of the present invention is to provide a water-in-silicone oil self-emulsifying composition, and the water-in-silicone oil self-emulsifying composition comprises an aqueous phase and an oil phase.
[0041] The aqueous phase comprises water and a polyol.
[0042] Preferably, the aqueous phase further comprises an emulsification stabilizer.
[0043] The oil phase comprises a phenyl silicone oil.
[0044] Preferably, the oil phase further comprises a polar oil compatible with the phenyl silicone oil. The compatibility between the polar oil and the phenyl silicone oil is good.
[0045] The polyol is selected from one or more of glycerol, butanediol, propylene glycol, pentanediol and hexanediol.
[0046] Preferably, the polyol is selected from one or more of glycerol, 1,2-pentanediol, 1,3-propylene glycol, 1,2-hexanediol and 1,3-butanediol.
[0047] The polyol accounts for 1-70% of the total mass of the aqueous phase, preferably 3-12% of the total mass of the aqueous phase.
[0048] The emulsification stabilizer is selected from one or more of betaine, erythritol, inulin, mannitol, niacinamide, panthenol, allantoin and metal chlorides.
[0049] Preferably, the solid humectant is selected from one or more of betaine, panthenol, allantoin and sodium chloride.
[0050] The aqueous phase further comprises a preservative, and the preservative is preferably p-hydroxyacetophenone.
[0051] The phenyl silicone oil is selected from one or more of trimethylpentaphenyltrisiloxane, diphenylhexamethylsiloxane, tetramethyltetraphenyltrisiloxane, phenylpolydimethylsiloxane and diphenylpolydimethylsiloxane.
[0052] Preferably, the phenyl silicone oil is trimethylpentaphenyltrisiloxane and diphenylpolydimethylsiloxane.
[0053] The polar oil compatible with the phenyl silicone oil is selected from one or more of pentaerythritol tetra(ethylhexanoate), isononyl isononanoate, dicaprylyl carbonate and tocopheryl acetate.
[0054] Preferably, the polar oil compatible with the phenyl silicone oil is one or more of pentaerythritol tetra(ethylhexanoate), isononyl isononanoate or tocopheryl acetate.
[0055] The polar oil compatible with the phenyl silicone oil accounts for 1-50% of the total mass of the oil phase, preferably 10-30% of the total mass of the oil phase.
[0056] Optionally, the aqueous phase further comprises ascorbyl ethyl ether or niacinamide.
[0057] The composition of the present invention is a penetration-enhancing composition prepared with phenyl silicone oil as the continuous phase. Without traditional emulsifiers, this composition can spontaneously form an emulsion under low shear force, enhancing the transdermal absorption of active ingredients or functional components.
[0058] The second aspect of the present invention is to provide a method for preparing the water-in-silicone oil self-emulsifying composition according to the first aspect of the present invention. The preparation method comprises the following steps:
[0059] Step 1: Mix water and polyol, heat to 65 - 75°C, stir evenly to obtain an aqueous phase.
[0060] Step 2: Heat phenyl silicone oil to 35 - 45°C, stir evenly to obtain an oil phase.
[0061] Preferably, in Step 1, mix water and polyol, then add one or several of preservatives and emulsification stabilizers, heat to 70°C after mixing, stir evenly, and then cool to obtain an aqueous phase.
[0062] Preferably, in Step 2, add polar oil to phenyl silicone oil, heat to 40°C after mixing, stir evenly, and then cool to obtain an oil phase.
[0063] The third aspect of the present invention is to provide an application of the water-in-silicone oil self-emulsifying composition according to the first aspect of the present invention in the preparation of cosmetics.
[0064] The cosmetics include water-based products without emulsifiers, sprays, facial masks, essence liquids, etc.
[0065] Based on 100% of the mass of the cosmetics, the oil phase accounts for 1 - 10%, and the aqueous phase accounts for 90 - 99%.
[0066] Preferably, based on 100% of the mass of the cosmetics, the oil phase accounts for 1 - 5%, and the aqueous phase accounts for 95 - 99%.
[0067] The fourth aspect of the present invention is to provide an essence water, which is prepared from raw materials including the water-in-silicone oil self-emulsifying composition according to the first aspect of the present invention.
[0068] In the essence water, the mass ratio of the aqueous phase to the oil phase in the water-in-silicone oil self-emulsifying composition is (90 - 99) : (1 - 10).
[0069] Preferably, in the essence water, the mass ratio of the aqueous phase to the oil phase in the water-in-silicone oil self-emulsifying composition is 99 : 1.
[0070] The preparation raw materials of the essence water further include functional ingredients, and the functional ingredients are vitamin C ethyl ether or niacinamide.
[0071] The essence water is prepared through the following steps:
[0072] Add the functional ingredients to the water phase of the water-in-silicone oil self-emulsifying composition, mix evenly, and then mix evenly with the oil phase to obtain the essence water.
[0073] Examples
[0074] The present invention will be further described below through specific examples. These examples are only for illustrating the present invention and are not used to limit the scope of the present invention. The raw materials used in the examples of the present invention are all commercially available.
[0075] Example 1
[0076] A water-in-silicone oil self-emulsifying composition includes an oil phase and a water phase.
[0077] Weigh each raw material according to the following mass percentages: In the oil phase: trimethylpentaphenyltrisiloxane 1.0%, diphenylpolydimethylsiloxane 0.5%, tocopheryl acetate 0.2%, pentaerythritol tetra(ethylhexanoate) 0.3%; in the water phase: weigh 1,3-butanediol 5.0%, glycerol 3.0%, 1,2-pentanediol 2.0%, betaine 0.5%, sodium chloride 0.8%, p-hydroxyacetophenone 0.3%, allantoin 0.12%, and the rest is water.
[0078] A preparation method of a water-in-silicone oil self-emulsifying composition, the preparation method includes:
[0079] Add the weighed water, 1,3-butanediol, glycerol, 1,2-pentanediol, betaine, sodium chloride, p-hydroxyacetophenone, and allantoin to a preparation pot, heat the preparation pot to 70°C, stir evenly and then start to cool to obtain the water phase.
[0080] Add the weighed trimethylpentaphenyltrisiloxane, diphenylpolydimethylsiloxane, tocopheryl acetate, and pentaerythritol tetra(ethylhexanoate) to the preparation pot, heat the preparation pot to 40°C, stir evenly and then cool to obtain the oil phase.
[0081] Example 2
[0082] A water-in-silicone oil self-emulsifying composition includes an oil phase and a water phase.
[0083] Weigh each raw material according to the following mass percentages: In the oil phase: trimethyl pentaphenyl trisiloxane 60.0%, diphenyl polydimethylsiloxane 5.0%, tocopheryl acetate 2.0%, isononyl isononanoate 3.0%; in the aqueous phase: 1,2-pentanediol 20.0%, betaine 1.0%, sodium chloride 1.6%, and the balance is water (7.4%).
[0084] A method for preparing a water-in-silicone oil self-emulsifying composition, the preparation method comprising:
[0085] Add the weighed water, 1,2-pentanediol, betaine, and sodium chloride to a preparation pot, heat the preparation pot to 70°C, stir evenly and then start to cool to obtain an aqueous phase.
[0086] Add the weighed trimethyl pentaphenyl trisiloxane, diphenyl polydimethylsiloxane, tocopheryl acetate, and isononyl isononanoate to a preparation pot, heat the preparation pot to 40°C, stir evenly and then cool to obtain an oil phase.
[0087] Example 3
[0088] A water-in-silicone oil self-emulsifying composition, comprising an oil phase and an aqueous phase.
[0089] Weigh each raw material according to the following mass percentages: In the oil phase: trimethyl pentaphenyl trisiloxane 60.0%, diphenyl polydimethylsiloxane 5.0%, tocopheryl acetate 2.0%, isononyl isononanoate 3.0%; in the aqueous phase: 1,3-propanediol 20.0%, betaine 1.0%, sodium chloride 1.6%, and the balance is water (7.4%).
[0090] A method for preparing a water-in-silicone oil self-emulsifying composition, the preparation method comprising:
[0091] Add the weighed water, 1,3-propanediol, betaine, and sodium chloride to a preparation pot, heat the preparation pot to 70°C, stir evenly and then start to cool to obtain an aqueous phase.
[0092] Add the weighed trimethyl pentaphenyl trisiloxane, diphenyl polydimethylsiloxane, tocopheryl acetate, and isononyl isononanoate to a preparation pot, heat the preparation pot to 40°C, stir evenly and then cool to obtain an oil phase.
[0093] Example 4
[0094] A water-in-silicone oil self-emulsifying composition, comprising an oil phase and an aqueous phase.
[0095] Weigh each raw material according to the following mass percentages: In the oil phase: 60.0% of trimethylpentaphenyltrisiloxane, 5.0% of diphenylpolydimethylsiloxane, 2.0% of tocopheryl acetate, 3.0% of isononyl isononanoate; in the aqueous phase: 20.0% of 1,2 - hexanediol, 1.0% of betaine, 1.6% of sodium chloride, and the rest is water (7.4%).
[0096] A preparation method of a water - in - silicone - oil self - emulsifying composition, the preparation method comprising:
[0097] Add the weighed water, 1,2 - hexanediol, betaine, and sodium chloride into a preparation pot, heat the preparation pot to 70 °C, stir evenly and then start to cool to obtain an aqueous phase.
[0098] Add the weighed trimethylpentaphenyltrisiloxane, diphenylpolydimethylsiloxane, tocopheryl acetate, and isononyl isononanoate into a preparation pot, heat the preparation pot to 40 °C, stir evenly and then cool to obtain an oil phase.
[0099] Example 5
[0100] A water - in - silicone - oil self - emulsifying composition, comprising an oil phase and an aqueous phase.
[0101] Weigh each raw material according to the following mass percentages: In the oil phase: 60.0% of trimethylpentaphenyltrisiloxane, 5.0% of diphenylpolydimethylsiloxane, 2.0% of tocopheryl acetate, 3.0% of isononyl isononanoate; in the aqueous phase: 20.0% of glycerol, 1.0% of betaine, 1.6% of sodium chloride, and the rest is water (7.4%).
[0102] A preparation method of a water - in - silicone - oil self - emulsifying composition, the preparation method comprising:
[0103] Add the weighed water, glycerol, betaine, and sodium chloride into a preparation pot, heat the preparation pot to 70 °C, stir evenly and then start to cool to obtain an aqueous phase.
[0104] Add the weighed trimethylpentaphenyltrisiloxane, diphenylpolydimethylsiloxane, tocopheryl acetate, and isononyl isononanoate into a preparation pot, heat the preparation pot to 40 °C, stir evenly and then cool to obtain an oil phase.
[0105] Example 6
[0106] A water - in - silicone - oil self - emulsifying composition, comprising an oil phase and an aqueous phase.
[0107] Weigh each raw material according to the following mass percentages: In the oil phase: trimethylpentaphenyltrisiloxane 1.0%, diphenylpolydimethylsiloxane 0.5%, tocopheryl acetate 0.2%, pentaerythritol tetra(ethylhexanoate) 0.3%; In the aqueous phase: 1,3-butanediol 5.0%, glycerol 3.0%, 1,2-pentanediol 2.0%, betaine 0.5%, sodium chloride 0.8%, p-hydroxyacetophenone 0.3%, allantoin 0.12%, panthenol 0.7%, niacinamide 0.1%, and the rest is water.
[0108] A method for preparing a water-in-silicone oil self-emulsifying composition, the preparation method comprising:
[0109] Add the weighed water, 1,3-butanediol, glycerol, 1,2-pentanediol, betaine, sodium chloride, p-hydroxyacetophenone, allantoin, and panthenol to a preparation pot, heat the preparation pot to 70°C, stir evenly and then start to cool, and then add niacinamide and mix evenly to obtain an aqueous phase.
[0110] Add the weighed trimethylpentaphenyltrisiloxane, diphenylpolydimethylsiloxane, tocopheryl acetate, and pentaerythritol tetra(ethylhexanoate) to a preparation pot, heat the preparation pot to 40°C, stir evenly and then cool to obtain an oil phase.
[0111] A method for preparing essence water, comprising the following steps:
[0112] Mix and fill according to the mass ratio of aqueous phase:oil phase = 99:1 to obtain essence water.
[0113] Example 7
[0114] A water-in-silicone oil self-emulsifying composition, comprising an oil phase and an aqueous phase.
[0115] Weigh each raw material according to the following mass percentages: In the oil phase: trimethylpentaphenyltrisiloxane 1.0%, diphenylpolydimethylsiloxane 0.5%, tocopheryl acetate 0.2%, pentaerythritol tetra(ethylhexanoate) 0.3%; In the aqueous phase: 1,3-butanediol 5.0%, glycerol 3.0%, 1,2-pentanediol 2.0%, betaine 0.5%, sodium chloride 0.8%, p-hydroxyacetophenone 0.3%, allantoin 0.12%, panthenol 0.7%, vitamin C ethyl ether 0.1%, and the rest is water.
[0116] A method for preparing a water-in-silicone oil self-emulsifying composition, the preparation method comprising:
[0117] Add the weighed water, 1,3-butanediol, glycerol, 1,2-pentanediol, betaine, sodium chloride, p-hydroxyacetophenone, allantoin, and panthenol to a preparation pot, heat the preparation pot to 70°C, stir evenly and then start to cool, and then add vitamin C ethyl ether and mix evenly to obtain an aqueous phase.
[0118] Add the weighed trimethylpentaphenyltrisiloxane, diphenylpolydimethylsiloxane, tocopheryl acetate, and pentaerythritol tetra(ethylhexanoate) to a preparation pot. Heat the preparation pot to 40 °C, stir evenly, and then cool to obtain an oil phase.
[0119] A method for preparing essence water, comprising the following steps:
[0120] Mix and fill according to the mass ratio of water phase:oil phase = 99:1 to obtain essence water.
[0121] Comparative example
[0122] Comparative example 1
[0123] An oil-in-water self-emulsifying composition, comprising an oil phase and a water phase.
[0124] Weigh each raw material according to the following mass percentages: in the oil phase: polydimethylsiloxane (viscosity 2 cst) 60.0%, diphenylpolydimethylsiloxane 5.0%, tocopheryl acetate 2.0%, isononyl isononanoate 3.0%; in the water phase: 1,2-pentanediol 20.0%, betaine 1.0%, sodium chloride 1.6%, and the rest is water (7.4%).
[0125] A method for preparing an oil-in-water self-emulsifying composition, the preparation method comprising:
[0126] Add the weighed water, 1,2-pentanediol, betaine, and sodium chloride to a preparation pot. Heat the preparation pot to 65 - 75 °C, stir evenly, and then start to cool to obtain a water phase.
[0127] Add the weighed polydimethylsiloxane (viscosity 2 cst), diphenylpolydimethylsiloxane, tocopheryl acetate, and isononyl isononanoate to a preparation pot. Heat the preparation pot to 35 - 45 °C, stir evenly, and then cool to obtain an oil phase.
[0128] Comparative example 2
[0129] An oil-in-water self-emulsifying composition, comprising an oil phase and a water phase.
[0130] Weigh each raw material according to the following mass percentages: in the oil phase: polydimethylsiloxane (viscosity 350 cst) 60.0%, diphenylpolydimethylsiloxane 5.0%, tocopheryl acetate 2.0%, isononyl isononanoate 3.0%; in the water phase: 1,2-pentanediol 20.0%, betaine 1.0%, sodium chloride 1.6%, and the rest is water (7.4%).
[0131] A method for preparing an oil-in-water self-emulsifying composition, the preparation method comprising:
[0132] Add the weighed water, 1,2-pentanediol, betaine, and sodium chloride to a preparation pot. Heat the preparation pot to 65 - 75 °C, and after stirring evenly, start cooling to obtain an aqueous phase.
[0133] Add the weighed polydimethylsiloxane (viscosity 350 cst), diphenylpolydimethylsiloxane, tocopheryl acetate, and isononyl isononanoate to a preparation pot. Heat the preparation pot to 35 - 45 °C, and after stirring evenly, cool to obtain an oil phase.
[0134] Comparative Example 3
[0135] Weigh each raw material according to the following mass percentages: 1,3-butanediol 5.0%, glycerol 3.0%, 1,2-pentanediol 2.0%, betaine 0.5%, sodium chloride 0.8%, p-hydroxyacetophenone 0.3%, allantoin 0.12%, panthenol 0.7%, niacinamide 0.1%, and the rest is water.
[0136] Add the weighed water, 1,3-butanediol, glycerol, 1,2-pentanediol, betaine, sodium chloride, p-hydroxyacetophenone, allantoin, and panthenol to a preparation pot. Heat the preparation pot to 65 - 75 °C, and after stirring evenly, start cooling, then add niacinamide and mix evenly to obtain essence water.
[0137] Comparative Example 4
[0138] Weigh each raw material according to the following mass percentages: 1,3-butanediol 5.0%, glycerol 3.0%, 1,2-pentanediol 2.0%, betaine 0.5%, sodium chloride 0.8%, p-hydroxyacetophenone 0.3%, allantoin 0.12%, panthenol 0.7%, vitamin C ethyl ether 0.1%, and the rest is water.
[0139] Add the weighed water, 1,3-butanediol, glycerol, 1,2-pentanediol, betaine, sodium chloride, p-hydroxyacetophenone, allantoin, and panthenol to a preparation pot. Heat the preparation pot to 65 - 75 °C, and after stirring evenly, start cooling, then add vitamin C ethyl ether and mix evenly to obtain essence water.
[0140] Experimental Example
[0141] Conductivity Test of Experimental Example 1
[0142] Conductivity is a physical parameter representing the electrical conductivity of a substance. When the composition is an O / W (oil-in-water) system with water as the continuous phase, the composition has electrical conductivity, and the higher the proportion of water, the greater the conductivity; conversely, the less water, the smaller the conductivity. When the conductivity is zero, it proves that the system has changed from O / W to W / O (water-in-oil) system at this time. The change trend of conductivity can be used to judge whether phase inversion occurs and at which ratio phase inversion occurs.
[0143] Take 10 parts of the aqueous phase prepared in Example 1, and then add the oil phase prepared in Example 1 to the aqueous phase for mixing. When the addition amounts of the oil phase are 2 parts, 6 parts, 10 parts, 14 parts, 18 parts, 22 parts, 26 parts, 30 parts, 34 parts, 38 parts, and 40 parts respectively, measure the conductivity of the mixture of the aqueous phase and the oil phase. The test results are shown in Table 1.
[0144] Table 1 Conductivity test data of the aqueous phase and the oil phase at different ratios
[0145]
[0146]
[0147] It can be seen from Table 1 that the conductivity becomes 0 when the addition amount of the oil phase reaches 38 parts, indicating that at this time, the system has become a W / O (water-in-oil) system and the phase inversion is completed. Therefore, as the addition amount of the oil phase prepared in Example 1 gradually increases, the phenomenon of transformation from an O / W system to a W / O system occurs.
[0148] This experiment simulates the change in the conductivity of the composition when the composition of the present invention is used on the face. It shows that when the composition of the present invention is applied on the face, as the water evaporates, the proportion of the silicone oil phase becomes larger and larger. When the water-oil ratio required for phase inversion is reached, the composition will help the skin care product to undergo phase inversion on the face.
[0149] Experimental Example 2 Emulsification test
[0150] Perform emulsification tests on the compositions prepared in Example 2, Comparative Example 1, and Comparative Example 2 respectively. The test process is as follows: Mix the prepared aqueous phase and oil phase in a ratio of 1:1.
[0151] Pictures of the compositions prepared in Example 2, Comparative Example 1, and Comparative Example 2 before shaking are as shown in Figure 1 shown, and pictures of the compositions prepared in Example 2, Comparative Example 1, and Comparative Example 2 after shaking are as shown in Figure 2 shown. Comparing Example 2, Comparative Example 1, and Comparative Example 2, the only difference is the silicone used. Among them, the viscosity of the polydimethylsiloxane (350 cst) used in Comparative Example 2 is similar to the viscosity of the trimethylpentaphenyltrisiloxane used in Example 2. Figure 3 Show the micrographs of the compositions prepared in Example 2, Comparative Example 1, and Comparative Example 2 after shaking.
[0152] Compare Figure 1 and Figure 2, it can be seen that the 2 cst polydimethylsiloxane used in Comparative Example 1 was completely unable to form an emulsion, and the aqueous phase was only dispersed in the oil phase under shaking. The 350 cst polydimethylsiloxane used in Comparative Example 2 was similar in viscosity to trimethylpentaphenyltrisiloxane, but still did not exhibit emulsifying properties. The liquid could not present an emulsion state after shaking, while a uniform emulsion was formed after shaking in Example 2.
[0153] The above results show that the trimethylpentaphenyltrisiloxane used in the present invention can help emulsify, make the liquid form finer emulsions, and make the liquid present an emulsion state. The main reason for this difference is due to the structure of phenyl silicone oil itself. Compared with polydimethylsiloxane, the introduction of phenyl changes the overall polarity of the siloxane, enhancing its hydrophilicity. Therefore, phenyl silicone oil has stronger wettability to water than polydimethylsiloxane. The introduction of phenyl groups enhances the polarity of phenyl silicone oil, enabling it to reduce the interfacial tension between water and oil, thereby promoting the formation of finer and more stable water droplets in phenyl silicone oil.
[0154] From Figure 3 it can be seen that the product prepared in Example 2 (using trimethylpentaphenyltrisiloxane) formed stable and optically distinct water droplets after shaking (emulsification), while the products prepared in Comparative Example 1 and Comparative Example 2 only dispersed water after shaking (using two different viscosities of polydimethylsiloxane), and the droplets would quickly coalesce, and the system was very unstable. The above results show that phenyl silicone oil can form a stable self-emulsifying system.
[0155] Experimental Example 3 Emulsification Test
[0156] To verify whether different polyols have an impact on this self-emulsifying system, the water-in-silicone oil self-emulsifying compositions prepared in Examples 2 to 5 were respectively subjected to emulsification tests. The test process was as follows: The prepared aqueous phase and oil phase were mixed in a ratio of 1:1. The pictures before shaking are as Figure 4 shown, and the pictures after shaking are as Figure 5 shown.
[0157] Comparing Figure 4 and Figure 5 it can be seen that polyols improve the stability of the self-emulsifying system by adjusting the interfacial tension between water and oil and affecting the droplet distribution. However, different polyols have different contributions to the self-emulsifying system. Judging from the whiteness of the emulsion, when 1,2-pentanediol and 1,2-hexanediol were used, the emulsification effect of the prepared composition was the best.
[0158] The above results indicate that adding polyols to the water-in-silicone oil self-emulsifying composition described in the present invention contributes to the formation of a self-emulsifying system. Polyols play a role in regulating the interfacial tension between water and oil in the composition of the present invention. Part of the molecule of the polyol dissolves in the aqueous phase, while the other part accumulates at the water-oil interface, acting as a "bridge", which helps to form a more stable self-emulsifying system. The reason for the differences among different polyols is mainly due to the polarity of the polyols themselves. Among them, glycerol has the strongest polarity, and the experimental data also show that the whiteness of the emulsion of the self-emulsifying system involving glycerol is relatively the lowest. Due to its strong polarity, it is more inclined to stay in the aqueous phase in terms of phase distribution rather than aggregating at the interface to reduce the surface tension, resulting in larger particle sizes of the emulsion droplets and a decrease in the light scattering ability, and thus the lowest whiteness of the emulsion. The polarity of 1,3-propanediol is between that of glycerol and 1,2-pentanediol and 1,2-hexanediol. It can partially reduce the surface tension and improve the dispersibility, so the whiteness of the emulsion shown is also in the middle among the three. 1,2-Pentanediol and 1,2-hexanediol have the lowest polarity and the best emulsifying effect, and the formed emulsifying system is also more stable.
[0159] Experimental Example 4 Permeability Test
[0160] The transdermal absorption of cosmetics refers to the process in which the active ingredients in cosmetics act on the skin surface or enter the epidermis or dermis according to the effectiveness of the product, and accumulate and play a role at this site. Cosmetics are products that act on the human body surface, and the skin on the human body surface has physical and chemical barrier functions for the absorption and transmission of exogenous substances. For the efficacy evaluation and safety evaluation of cosmetics, transdermal absorption research is an essential link.
[0161] The present invention uses the in-vivo tape stripping method for permeability testing. By setting up a control group (Comparative Examples 3-4) and a sample group (Examples 6-7), after the prepared essence water is brought into contact with the skin for a certain period of time, the penetration of niacinamide and vitamin C ethyl ether in the stratum corneum of different layers in the essence water is investigated.
[0162] Sampling method:
[0163] (1) Clean the inner sides of the left and right anterior arms of the subject and dry them, and then sit quietly in a constant temperature and humidity room for 1 h.
[0164] (2) During the test, the inner sides of the left and right anterior arms of the subject are segmented into a sample group and a control group. There are 3 areas in each group, and the area of each area is 3 cm × 3 cm. The intervals between multiple areas on the same arm are at least 1 cm or more. In the sample group area, use the sample (the essence water prepared in Examples 6-7), and the usage amount is 2 mg / cm 2 , and after fully absorbing by circular rubbing, use a skin keratin patch to remove the active ingredients on the skin surface for testing 30 minutes later.
[0165] (3) The skin keratin patch will be continuously applied in 11 layers (the first layer is discarded) within a fixed area, placed in a centrifuge tube, added with a 1:1 methanol aqueous solution, ultrasonically extracted for 30 min, and then filtered through a 0.22-μm filter membrane for measurement. The 2nd - 11th layers and the 2nd - 10th layers are combined into one layer to measure the contents of niacinamide and vitamin C ethyl ether.
[0166] (4) Calculate the penetration amount according to the calculation formula. The test results of the penetration amount are shown in Table 2 and Figure 6 as follows.
[0167] Penetration amount: Q = C × V;
[0168] Penetration amount increase multiple: G = Q s ÷Q b ×100%;
[0169] In the formula:
[0170] Q = Penetration amount;
[0171] C = Concentration of the target substance in the extract;
[0172] V = Volume fixed, mL;
[0173] Q s = Penetration amount of the sample group;
[0174] Q b = Penetration amount of the control group.
[0175] Table 2 Test results of the penetration amount
[0176]
[0177]
[0178] It can be seen from Table 2 and Figure 6 that through the transdermal absorption test, the penetration amount of niacinamide at 30 min in Comparative Example 3 (0.1% niacinamide) is 0.781 μg / cm 2 , and the penetration amount of vitamin C ethyl ether at 30 min in Comparative Example 4 (0.1% vitamin C ethyl ether) is 0.362 μg / cm 2 ; the penetration amount of niacinamide at 30 min in the essence water prepared in Example 6 is 1.233 μg / cm 2 , and the penetration amount of vitamin C ethyl ether at 30 min in the essence water prepared in Example 7 is 0.613 μg / cm 2 . The penetration amount of Example 6 is increased by 1.58 times compared with Comparative Example 3, and the penetration amount of Example 7 is increased by 1.69 times compared with using only Comparative Example 4. The above results show that after using the water-in-silicone self-emulsifying composition of the present invention, the permeability of niacinamide or vitamin C ethyl ether in the aqueous product can be promoted.
[0179] The present invention has been described in detail above in connection with specific embodiments and exemplary examples, but these descriptions should not be construed as limiting the present invention. Those skilled in the art understand that, without departing from the spirit and scope of the present invention, various equivalent substitutions, modifications or improvements can be made to the technical solutions and their implementation manners of the present invention, and all of these fall within the scope of the present invention. The protection scope of the present invention shall be subject to the appended claims.
Claims
1. A water-in-silicone oil self-emulsifying composition, characterized in that, The water-in-silicone oil self-emulsifying composition comprises an aqueous phase and an oil phase; The aqueous phase comprises water and polyols; The oil phase comprises phenyl silicone oil.
2. The water-in-silicone oil self-emulsifying composition according to claim 1, wherein The polyols are selected from one or more of glycerol, butanediol, propylene glycol, pentanediol and hexanediol.
3. The water-in-silicone oil self-emulsifying composition according to claim 1, wherein The polyols account for 1-70% of the total mass of the aqueous phase.
4. The water-in-silicone oil self-emulsifying composition according to claim 1, wherein The phenyl silicone oil is selected from one or more of trimethylpentaphenyltrisiloxane, diphenylhexamethylsiloxane, tetramethyltetraphenyltrisiloxane, phenylpolydimethylsiloxane and diphenylpolydimethylsiloxane.
5. The water-in-silicone oil self-emulsifying composition according to claim 1, wherein The aqueous phase further comprises an emulsification stabilizer; The emulsification stabilizer is selected from one or more of betaine, erythritol, inulin, mannitol, niacinamide, panthenol, allantoin and metal chlorides.
6. The water-in-silicone oil self-emulsifying composition according to claim 1, wherein The oil phase further comprises a polar oil compatible with the phenyl silicone oil; The polar oil compatible with the phenyl silicone oil is selected from one or more of pentaerythritol tetra(ethylhexanoate), isononyl isononanoate, dicaprylyl carbonate and tocopheryl acetate.
7. The water-in-silicone oil self-emulsifying composition according to claim 6, wherein The polar oil compatible with the phenyl silicone oil accounts for 1-50% of the total mass of the oil phase.
8. A method for preparing the water-in-silicone oil self-emulsifying composition according to any one of claims 1 to 7, characterized in that, The preparation method comprises the following steps: Step 1: Mix water and polyols, heat up to 65-75 °C, and stir evenly to obtain an aqueous phase; Step 2: Heat up the phenyl silicone oil to 35-45 °C and stir evenly to obtain an oil phase.
9. Use of the water-in-silicone oil self-emulsifying composition according to any one of claims 1 to 7 in the preparation of cosmetics.
10. An essence water, characterized in that, The essence water is prepared from raw materials comprising the water-in-silicone oil self-emulsifying composition according to any one of claims 1 to 7; In the essence water, the mass ratio of the aqueous phase to the oil phase in the water-in-silicone oil self-emulsifying composition is (90-99):(1-10).
Citation Information
Patent Citations
Rhamnolipid self-emulsifying skin care emulsion, preparation method and application
CN119424241A