Low-viscosity multi-type emulsion composition

A non-amphiphilic nanoparticle-based multiple emulsion composition addresses thermodynamic instability and skin irritation issues in conventional emulsions, providing stable, low-viscosity formulations with improved sensory experience and reduced heat damage.

JP2025178148APending Publication Date: 2025-12-05AMOREPACIFIC CORP

Patent Information

Application Number
JP2025079898
Authority / Receiving Office
JP · JP
Patent Type
Applications
Current Assignee / Owner
Priority Date
2024-05-22
Filing Date
2025-05-12
Publication Date
2025-12-05

AI Technical Summary

Technical Problem

Conventional multiple emulsion compositions, particularly w/o/w formulations, suffer from thermodynamic instability due to internal pressure imbalances, leading to formulation instability and the use of PEG surfactants that can cause skin irritation, necessitating the development of a stable, low-viscosity emulsion without these drawbacks.

Method used

A multiple emulsion composition is formed by mixing water and an oil component, where the water component includes a dispersion of non-amphiphilic nanoparticles, and the oil component includes an emulsion with an external phase, surrounded by these nanoparticles, allowing for a continuous phase and dispersed phase without the need for additional surfactants, and can be prepared at room temperature.

Benefits of technology

The composition achieves improved emulsion stability, reduces skin irritation risks, and allows for low-viscosity formulations without the use of PEG surfactants, while maintaining a unique sensory experience and protecting heat-sensitive ingredients.

✦ Generated by Eureka AI based on patent content.

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Abstract

To provide a multi-type emulsion composition and a preparation method thereof.SOLUTION: Disclosed herein are a multi-type emulsion composition and a preparation method thereof. The emulsion composition is a composition in which a water part and an oil part are mixed and emulsified, the water part includes a non-amphipathic nanoparticle dispersion, the oil part includes an emulsion and the emulsion includes an oil phase or silicone phase as an external phase, the emulsion composition includes the water part as a continuous phase and the oil part as a dispersed phase, and the dispersed phase is surrounded by the non-amphipathic nanoparticles.SELECTED DRAWING: Figure 1
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Description

[Technical Field]

[0001] The present disclosure provides a multiple emulsion composition and a method for producing the same. [Background technology]

[0002] W / o / w complex formulations are typically obtained by preparing a w / o emulsion in the first step, an o / w emulsion in the second step, and finally a w / o / w formulation. Complex formulations themselves are thermodynamically unstable because the internal pressure of the w / o emulsion is higher than that of the continuous (external) phase, causing the liquid inside to migrate outward, resulting in formulation instability. To overcome or delay this phenomenon, research has been conducted to prevent the internal particles from escaping by adjusting osmotic pressure, forming a lamellar structure, or increasing hardness, but the stability of complex formulations remains insufficient. To address this formulation stability issue, conventional techniques have typically used PEG surfactants with high HLB values, which have excellent emulsifying power, or by increasing the viscosity and hardness of the formulation. However, PEG generates harmful substances such as ethylene oxide and 1,4-dioxane during the manufacturing process, which can cause skin irritation and hives, leading to active research into replacing PEG with other surfactants. [Prior art documents] [Patent documents]

[0003] [Patent Document 1] Korean Patent Publication No. 10-2015-0070920 Summary of the Invention [Problem to be solved by the invention]

[0004] In one aspect, the present disclosure aims to provide a multiple emulsion composition.

[0005] In another aspect, the present disclosure aims to provide a method for producing the emulsion composition. [Means for solving the problem]

[0006] In one aspect, the present disclosure relates to a multiple emulsion composition, the emulsion composition being formed by mixing and emulsifying water and an oil component, the water component comprising a dispersion of non-amphiphilic nanoparticles, the oil component comprising an emulsion, the emulsion comprising an oil phase portion or a silicone portion as an external phase, the emulsion composition comprising the water component as a continuous phase and the oil component as a dispersed phase, and the dispersed phase being surrounded by non-amphiphilic nanoparticles.

[0007] In one exemplary implementation, the non-amphiphilic nanoparticles may have an average size of 10 nm or more and less than 1 μm.

[0008] In one exemplary implementation, the non-amphiphilic nanoparticles may be selected from the group consisting of nanoemulsion particles, solid lipid nanoparticles (SLN), liposomes, and polymersomes.

[0009] In one exemplary implementation, the dispersion of non-amphiphilic nanoparticles may be immiscible with the oil and / or immiscible with the oil phase portion or the silicone portion.

[0010] In one exemplary implementation, the emulsion may include an aqueous phase as the internal phase.

[0011] In one exemplary implementation, the non-amphiphilic nanoparticle dispersion and emulsion may be included in a weight ratio greater than 1:1.

[0012] In one exemplary implementation, the dispersion of non-amphiphilic nanoparticles may be included in an amount of less than 25% by weight based on the total weight of the emulsion composition.

[0013] In one exemplary implementation, the emulsion may be present in an amount of less than 15% by weight based on the total weight of the emulsion composition.

[0014] In one exemplary implementation, the average size of the dispersed phase may be 1 to 50 μm.

[0015] In one exemplary implementation, the emulsion composition may further include a surfactant.

[0016] In one exemplary implementation, the emulsion composition may be PEG-free.

[0017] In one exemplary implementation, the viscosity of the emulsion composition may be 4,000 to 14,000 cps.

[0018] In one exemplary implementation, the emulsion composition may be formed by mixing and emulsifying water and oil at room temperature.

[0019] In one exemplary implementation, the formulation of the emulsion composition may be w / o / w or w / s / w.

[0020] In another aspect, the present disclosure relates to a method for producing the composite emulsion composition, the method comprising the steps of producing a dispersion of non-amphiphilic nanoparticles, producing an emulsion containing an oil phase or a silicone phase as an external phase, producing water containing the dispersion of the non-amphiphilic nanoparticles, producing an oil containing emulsion, and mixing the water and oil. [Effects of the Invention]

[0021] In one aspect, the technology disclosed in the present disclosure has the effect of providing a multiple emulsion composition.

[0022] In another aspect, the technology disclosed in the present disclosure has the effect of providing a method for producing the emulsion composition.

[0023] Conventional multiple emulsion technologies include methods for improving stability by adjusting the selection and ratio of surfactants, methods for reducing the fluidity of emulsion particles by adding oil gelling agents, and / or methods for controlling fluidity by using thickeners to prevent coalescence. While these methods can produce multiple emulsions, they have the drawback of leaving a distinctive residual feeling depending on the use of surfactants, oil gelling agents, and / or thickeners. Another drawback is that the surfactant content must be increased to improve stability. The present disclosure has the effect of improving the usability of multiple formulations and forming multiple formulations, particularly low-viscosity multiple formulations, without or with minimal surfactant use. [Brief explanation of the drawings]

[0024] [Figure 1] 1 shows photographs of the emulsion compositions of Examples 1 to 4 taken with an optical microscope (DSX110, OLYMPUS) (scale bar 20 μm). [Figure 2] 1 shows photographs of the emulsion compositions of Examples 1 to 4 taken with an optical microscope (DSX110, OLYMPUS) (scale bar 5 μm). [Figure 3] 1 shows photographs of the emulsion compositions of Examples 1 to 4 taken at different storage temperatures to confirm the formulation stability of the emulsion compositions. [Figure 4] 1 shows photographs of emulsion compositions taken at different storage temperatures to confirm the formulation stability of the emulsion compositions of Comparative Examples 1 to 6. [Figure 5] 3 shows photographs of the emulsion compositions of Comparative Examples 1 to 6 taken at different angles. DETAILED DESCRIPTION OF THE INVENTION

[0025] The present disclosure will be described in detail below.

[0026] In one aspect, the present disclosure relates to a multiple emulsion composition, wherein water and an oil component are mixed and emulsified, the water component comprises a dispersion of non-amphiphilic nanoparticles, the oil component comprises an emulsion, the emulsion comprises an oil phase portion or a silicone phase portion as an external phase, the emulsion composition comprises the water component as a continuous phase and the oil component as a dispersed phase, and the dispersed phase is surrounded by non-amphiphilic nanoparticles.

[0027] In one exemplary implementation, the water and oil may be mixed in a weight ratio of 70-90:10-30, 72-88:12-28, 76-88:12-24, or 78-86:14-22.

[0028] The continuous phase means a phase that continues in a continuous state, and the dispersed phase means a phase that is dispersed within the continuous phase.

[0029] The non-amphiphilic nanoparticles refer to nanoparticles that are not amphiphilic, meaning that the physical properties of the nanoparticles are not amphiphilic, having both hydrophilic and hydrophobic moieties. For example, the non-amphiphilic nanoparticles according to the present disclosure can be formed using an amphiphilic substance such as a phospholipid, but the physical properties of the formed nanoparticles themselves do not have amphiphilic properties. Therefore, there is no need to modify the physical properties to have a Janus structure, which is different from conventional Pickering emulsion compositions that use Janus-structured powders.

[0030] In one exemplary implementation, the dispersion of non-amphiphilic nanoparticles may be an aqueous dispersion in which non-amphiphilic nanoparticles are dispersed.

[0031] In one exemplary embodiment, the concentration of the non-amphiphilic nanoparticles in the dispersion may be 15% or less (w / w) or 5 to 15% (w / w). The concentration may be adjusted depending on the oil content within the range. In another exemplary embodiment, to achieve a low-viscosity composite formulation and improve the emulsion stability of the composite formulation, the concentration of the non-amphiphilic nanoparticles in the dispersion may be 1% or more, 2% or more, 3% or more, 4% or more, 5% or more, 6% or more, 7% or more, 8% or more, 9% or more, 10% or more, 11% or more, 12% or more, 13% or more, or 14% or more (w / w). Alternatively, the concentration may be 15% or less, 14% or less, 13% or less, 12% or less, 11% or less, 10% or less, 9% or less, 8% or less, 7% or less, or 6% or less (w / w).

[0032] In one exemplary implementation, the non-amphiphilic nanoparticles may be nanosized.

[0033] In one exemplary implementation, the non-amphiphilic nanoparticles may have an average size of 10 nm or more and less than 1 μm.

[0034] In another exemplary embodiment, the average size of the non-amphiphilic nanoparticles may be 10 nm or more, 50 nm or more, or 100 nm or more, or may be less than 1 μm, 900 nm or less, 800 nm or less, 700 nm or less, 600 nm or less, 500 nm or less, 400 nm or less, 300 nm or less, or 200 nm or less. For example, the average size of the non-amphiphilic nanoparticles may be 10 to 700 nm or 10 to 500 nm.

[0035] In another exemplary implementation, the average size of the non-amphiphilic nanoparticles may be 500 nm or less, or 150-300 nm.

[0036] In one exemplary implementation, the size refers to the particle size.

[0037] In one exemplary implementation, the diameter refers to the longest diameter.

[0038] In one exemplary embodiment, the non-amphiphilic nanoparticles may be selected from the group consisting of nanoemulsion particles, solid lipid nanoparticles (SLN), liposomes, and polymersomes. The nanoemulsion particles, solid lipid nanoparticles, liposomes, and polymersomes may be prepared and used by conventional preparation methods known in the art.

[0039] Generally, emulsions are divided into three types: microemulsions, nanoemulsions, and macroemulsions, depending on the average size of the internal phase. A nanoemulsion is a mixture of at least two immiscible liquids, one of which is dispersed in the other in the form of small particles, with the particle size being in the nanometer range. The nanoemulsion particles refer to the internal phase of a nanoemulsion, i.e., the emulsion particles.

[0040] Solid lipid nanoparticles are known as one of the drug delivery systems proposed to overcome the drawbacks of conventional colloidal carriers, and their size may be determined by various factors such as the type and amount of lipid used and the type and amount of surfactant.

[0041] The liposome is a spherical or ellipsoidal structure formed from lipids, characterized by having an internal space separated from the outside by at least one bilayer membrane, and has a bilayer membrane structure that spontaneously aligns due to the interaction of molecules that have both lipophilic and hydrophilic properties, such as phospholipids.

[0042] The polymersome has a structure similar to that of a liposome, with a membrane surrounding an internal fluid, which may contain a polymer, for example, a molecular bilayer membrane formed by the self-association of amphiphilic copolymers similar to phospholipids.

[0043] In one exemplary implementation, the non-amphiphilic nanoparticles may include an effective ingredient (also referred to as an active ingredient).

[0044] The active ingredient is, for example, an oil-soluble active ingredient, such as vitamin A, for example, retinol, vitamin E, carotene, coenzyme Q10, resveratrol, beta-carotene, bakuchiol, and lycopene.

[0045] In one exemplary implementation, the non-amphiphilic nanoparticles may have no inner and outer layer or at least two layered structures.

[0046] In one exemplary embodiment, the active ingredient may be supported by non-amphiphilic nanoparticles. That is, when the non-amphiphilic nanoparticles have at least two layered structures, the inner layer may support an active ingredient such as whitening, anti-wrinkle, or antioxidant. In one exemplary embodiment, the non-amphiphilic nanoparticles support a water-soluble or lipid-soluble active ingredient.

[0047] In one exemplary implementation, the non-amphiphilic nanoparticles may be amorphous, spherical, or ellipsoid in shape.

[0048] In one exemplary implementation, the dispersion of non-amphiphilic nanoparticles may be immiscible with the oil and / or immiscible with the oil phase portion or the silicone portion.

[0049] In one exemplary implementation, the emulsion may include an aqueous phase as the internal phase.

[0050] In one exemplary embodiment, the emulsion formulation may be w / o or w / s. The composite emulsion composition of the present disclosure according to one aspect has the effect of significantly improving the emulsion stability of the composite formulation by first preparing a w / o or w / s emulsion, then adding it to an oil component, and then mixing and emulsifying the oil component with water to which a dispersion of non-amphiphilic nanoparticles has been added.

[0051] In one exemplary implementation, the emulsion formulation is w / o and the emulsion composition formulation is w / o / w.

[0052] In an exemplary embodiment, the emulsion formulation is w / s, and the emulsion composition formulation is w / s / w. In this case, the oil may be a silicone component. In this specification, the oil may refer to a silicone component. For example, the oil may include elastomer, silicone oil, etc. In one exemplary implementation, the elastomer may include at least one selected from the group consisting of vinyl dimethicone / methicone silsesquioxane crosspolymer, polysilicone-11, polysilicone-13, diphenyl dimethicone / vinyl diphenyl dimethicone / silsesquioxane crosspolymer, dimethicone / vinyl dimethicone crosspolymer, dimethicone / phenyl vinyl dimethicone crosspolymer, and polymethylsilsesquioxane. In one exemplary implementation, the silicone oil may include at least one selected from the group consisting of methicone-based silicone oil, dimethicone-based silicone oil, cyclomethicone-based silicone oil, and phenyl trimethicone-based silicone oil.

[0053] In one exemplary implementation, the dispersion of non-amphiphilic nanoparticles and the emulsion may be comprised in a weight ratio of greater than 1:1, greater than 1 to 8:1, greater than 1 to 7.5:1, greater than 1 to 7:1, greater than 1 to 6.5:1, greater than 1 to 6:1, greater than 1 to 5.5:1, greater than 1 to 5:1, greater than 1 to 4.5:1, greater than 1 to 4:1, greater than 1 to 3.5:1, or greater than 1 to 3:1.

[0054] In another exemplary implementation, the non-amphiphilic nanoparticle dispersion and emulsion may be contained in a weight ratio of 1.5 or more:1, a weight ratio of 1.5 to 8:1, a weight ratio of 1.5 to 7.5:1, a weight ratio of 1.5 to 7:1, a weight ratio of 1.5 to 6.5:1, a weight ratio of 1.5 to 6:1, a weight ratio of 1.5 to 5.5:1, a weight ratio of 1.5 to 5:1, a weight ratio of 1.5 to 4.5:1, a weight ratio of 1.5 to 4:1, a weight ratio of 1.5 to 3.5:1, or a weight ratio of 1.5 to 3:1.

[0055] In one exemplary embodiment, the non-amphiphilic nanoparticle dispersion may be present in an amount of less than 25 wt %, 24 wt % or less, 23 wt % or less, 22 wt % or less, 21 wt % or less, 20 wt % or less, 19 wt % or less, 18 wt % or less, 17 wt % or less, 16 wt % or less, or 15 wt % or less, based on the total weight of the emulsion composition. In another exemplary embodiment, the non-amphiphilic nanoparticle dispersion may be present in an amount of 5 wt % or more, 6 wt % or more, 7 wt % or more, 8 wt % or more, 9 wt % or more, or 10 wt % or more, based on the total weight of the emulsion composition. If the content of the non-amphiphilic nanoparticle dispersion is low, the emulsion stability of the composite formulation may be reduced. If the content of the non-amphiphilic nanoparticle dispersion is high, the emulsion stability may be improved, but it may be difficult to form a low-viscosity composite formulation. Therefore, the dispersion of the non-amphiphilic nanoparticles is preferably contained in an amount of 5% by weight or more but less than 25% by weight, 5 to 24% by weight, 5 to 23% by weight, 5 to 22% by weight, 5 to 21% by weight, or 5 to 20% by weight, based on the total weight of the emulsion composition.

[0056] In one exemplary embodiment, the emulsion may be contained in an amount of less than 15 wt %, 14 wt % or less, 13 wt % or less, 12 wt % or less, 11 wt % or less, 10 wt % or less, 9 wt % or less, 8 wt % or less, 7 wt % or less, 6 wt % or less, 5 wt % or less, or 4 wt % or less, based on the total weight of the emulsion composition. In another exemplary embodiment, the emulsion may be contained in an amount of more than 3 wt %, 4 wt % or more, 5 wt % or more, 6 wt % or more, 7 wt % or more, 8 wt % or more, 9 wt % or more, or 10 wt % or more, based on the total weight of the emulsion composition. If the emulsion content is low, it may be difficult to provide the unique feel of a composite formulation, while if the emulsion content is high, the emulsion stability of the composite formulation may be reduced, resulting in a heavy and sticky feel when used. Therefore, the emulsion is preferably contained in an amount of more than 3 wt % and less than 15 wt %, 4 to 14 wt %, 5 to 13 wt %, or 5 to 10 wt % relative to the total weight of the emulsion composition.

[0057] In one exemplary embodiment, the dispersion and emulsion of the non-amphiphilic nanoparticles may be included in an amount of 5% by weight or more but less than 25% by weight and more than 3% by weight or more but less than 15% by weight, respectively, based on the total weight of the emulsion composition, in order to improve the emulsion stability of the composite formulation and provide the composite formulation with a desired feel and low viscosity.

[0058] In one exemplary implementation, the average size of the dispersed phase may be 1 to 50 μm.

[0059] In another example embodiment, the average size of the dispersed phase may be 1 μm or more, 2 μm or more, 3 μm or more, 4 μm or more, 5 μm or more, 6 μm or more, 7 μm or more, 8 μm or more, 9 μm or more, or 10 μm or more, or 50 μm or less, 45 μm or less, 40 μm or less, 35 μm or less, 30 μm or less, 25 μm or less, 20 μm or less, 15 μm or less, 10 μm or less, or 5 μm or less. For example, the average size of the dispersed phase is 1 to 30 μm, 5 to 30 μm, 10 to 40 μm, or 10 to 30 μm.

[0060] In one exemplary implementation, the size refers to the particle size.

[0061] In one exemplary implementation, the diameter refers to the longest diameter.

[0062] Generally, the size of the dispersed phase formed by emulsification with a surfactant is small, about 1 to 2 μm, and has the drawback of causing fusion between dispersed phases. While Pickering emulsion compositions can form dispersed phases with a size of about 10 to 20 μm, they have the drawback of being difficult to formulate into stable formulations. In one aspect, the multiple emulsion composition according to the present disclosure overcomes the drawbacks of conventional Pickering emulsion compositions, which have low emulsion stability, while having the advantage of being able to have dispersed phases with large sizes like Pickering emulsion compositions and not causing fusion between dispersed phases.

[0063] In conventional emulsion compositions, the dispersed phase is generally made small and uniform in size to improve formulation stability and prevent fusion of the dispersed phase. In contrast, the multiple emulsion composition according to one embodiment of the present disclosure has the advantage of exhibiting excellent formulation stability even when the dispersed phase is large in size.

[0064] In one exemplary implementation, the dispersed phase may be surrounded by non-amphiphilic nanoparticles, with the non-amphiphilic nanoparticles attached to each other on the surface of the dispersed phase.

[0065] In a composite emulsion composition according to one embodiment of the present disclosure, the sizes of the dispersed phase and the non-amphiphilic nanoparticles may be adjusted so that the difference in size causes the non-amphiphilic nanoparticles to be located on the surface of the dispersed phase and form an interface between the dispersed phase and the continuous phase. The non-amphiphilic nanoparticles, which have a particle size smaller than that of the dispersed phase, are attracted to the surface of the dispersed phase and form an interface between the dispersed phase and the continuous phase, while the small particle size non-amphiphilic nanoparticles adhere to each other due to the attractive forces between the non-amphiphilic nanoparticles and surround the surface of the dispersed phase to form an interface.

[0066] In one embodiment of the multiple emulsion composition of the present disclosure, water-dispersed non-amphiphilic nanoparticles contained in water gather on the surface of the dispersed phase during the emulsification process, adhere to each other, and form an interface surrounding the dispersed phase. Because the non-amphiphilic nanoparticle dispersion is immiscible with oil, the non-amphiphilic nanoparticles surround the dispersed phase. Therefore, unlike conventional Pickering emulsion compositions, the multiple emulsion composition of the present disclosure can be used without surface-treating the nanoparticles to form a Janus structure. This allows for a stable emulsified system to be achieved without adding any additional surfactants other than those used in producing the non-amphiphilic nanoparticle dispersion and / or emulsion.

[0067] In one exemplary implementation, the emulsion composition may not contain any additional surfactants for emulsifying the multiple emulsion composition other than the surfactants used to prepare the dispersion of non-amphiphilic nanoparticles and the emulsion.

[0068] In one exemplary embodiment, the emulsion composition may further include an additional surfactant for emulsifying the composite emulsion composition in addition to the surfactant used in preparing the dispersion of non-amphiphilic nanoparticles and the emulsion.

[0069] The surfactant means a substance having two different properties that allows mixing of at least two liquids that are not miscible with each other, for example, an oil phase and a water phase.

[0070] In one exemplary embodiment, the emulsion composition may be PEG-free. The present disclosure has the advantage of being able to form a low-viscosity complex formulation without using a PEG surfactant.

[0071] In one exemplary embodiment, the viscosity of the emulsion composition may be 4,000 to 14,000 cps at room temperature. Conventionally, there has been a technical limitation in that it is difficult to form a composite formulation with a low viscosity of 10,000 cps or less, or 4,000 to 6,000 cps. Due to the low stability of composite formulations, the realization of composite formulations has been limited to high-hardness creams in order to control the fluidity of w / o or w / s particles. On the other hand, the emulsion composition of the present disclosure has the advantage of being able to form a low-viscosity composite formulation without using, or with a minimum use of, surfactants, oil gelling agents, and / or thickeners when forming the composite formulation.

[0072] In another exemplary implementation, the viscosity of the emulsion composition may be 4,000 cps or more, 4,500 cps or more, 5,000 cps or more, 5,500 cps or more, 6,000 cps or more, 6,500 cps or more, 7,000 cps or more, 7,500 cps or more, or 8,000 cps or more, and may be 14,000 cps or less, 13,000 cps or less, 12,000 cps or less, 11,000 cps or less, 10,000 cps or less, 9,000 cps or less, 8,000 cps or less, 7,000 cps or less, 6,000 cps or less, 5,500 cps or less, 5,000 cps or less, or 4,500 cps or less.

[0073] In another exemplary embodiment, when the emulsion composition is a w / o / w formulation, the viscosity may be 4,000 to 10,000 cps.

[0074] In another exemplary embodiment, when the emulsion composition is a w / s / w formulation, the viscosity may be 8,000 to 14,000 cps.

[0075] In one exemplary implementation, the emulsion composition may be prepared by mixing and emulsifying water and oil at room temperature.

[0076] In one exemplary implementation, the room temperature may be 1 to 35°C, 10 to 30°C, or 15 to 25°C.

[0077] In conventional w / o / w complex formulations, the o / w portion is typically prepared by emulsifying at high temperatures (70–80°C) using an oil phase component, a solid phase component (e.g., butter, wax, higher alcohol), and / or an emulsifier. The w / o / w complex formulation is formed by preparing and mixing the oil and water components, followed by adding the w / o component (internal phase) and heating. While it is possible to arbitrarily use ingredients that do not require high-temperature dissolution (i.e., components that are liquid at room temperature) to prepare a complex formulation, this approach leaves room for the monotonous experience, fails to provide the unique experience of a complex formulation, and severely limits the types of emulsifiers that can be used. While a lamellar structure can be used to improve the stability of the complex structure, the components required to create the lamellar structure must also be dissolved at high temperatures. In contrast, the complex emulsion composition of the present disclosure can be prepared by room-temperature emulsification, as the water and oil components are mixed and emulsified at room temperature. Warm emulsification is also available as needed. Therefore, the present disclosure has the effect of significantly reducing heat damage to heat-sensitive active ingredients such as retinol, since the complex formulation can be finally emulsified at room temperature when produced.

[0078] In one exemplary implementation, the formulation of the emulsion composition may be w / o / w or w / s / w.

[0079] In one exemplary implementation, the emulsion composition may be a cosmetic composition.

[0080] In one exemplary implementation, the cosmetic composition may be a formulation such as a mist, spray, toner, serum, gel, emulsion, cream, pack, foam cleanser, makeup base, or foundation.

[0081] In one exemplary embodiment, the emulsion composition may be a topical skin composition. The topical skin composition is intended to be applied to the outer skin, and may include, for example, various pharmaceutical formulations. In one exemplary embodiment, the topical skin composition may be in the form of a mist, spray, suspension, emulsion, gel, lotion, ointment, or the like.

[0082] In another aspect, the present disclosure relates to a method for producing the composite emulsion composition, the method comprising the steps of producing a dispersion of non-amphiphilic nanoparticles, producing an emulsion containing an oil phase or a silicone phase as an external phase, producing water containing the dispersion of the non-amphiphilic nanoparticles, producing an oil containing emulsion, and mixing the water and oil.

[0083] In the above preparation method, the order of preparing the dispersion and emulsion of non-amphiphilic nanoparticles and / or the order of preparing the water and oil components can be freely selected by those skilled in the art.

[0084] In one exemplary implementation, the manufacturing method may further include adding a surfactant during the process of mixing the water and oil.

[0085] In one exemplary implementation, the manufacturing method may include mixing and emulsifying the water and oil at room temperature.

[0086] The present disclosure will be described in more detail below with reference to examples. It will be obvious to those skilled in the art that these examples are merely for the purpose of illustrating the present disclosure and are not intended to limit the scope of the present disclosure in any way.

[0087] [Manufacturing Example 1] Preparation of dispersions of non-amphiphilic nanoparticles An aqueous dispersion containing nanoemulsion particles as non-amphiphilic nanoparticles was prepared according to the composition in Table 1 below. The oil phase was heated to 70°C to dissolve, and then dispersed using a homogenizer to produce a lipophilic mixture. The aqueous phase was heated to 70°C in a separate container to dissolve, and the lipophilic mixture prepared above was then slowly added to the aqueous phase, and water-dispersed nanoparticles were formed using a homogenizer at 70°C. The nanoparticle size was adjusted using an ultrasonic / high-pressure homogenizer.

[0088] [Table 1]

[0089] An aqueous dispersion containing solid lipid nanoparticles as non-amphiphilic nanoparticles was prepared according to the composition in Table 2 below. The oil phase was heated to 70°C to dissolve, and then dispersed using a homogenizer to produce a lipophilic mixture. The aqueous phase was heated to 70°C in a separate container to dissolve, and the lipophilic mixture prepared above was then slowly added to the aqueous phase, and water-dispersed nanoparticles were formed using a homogenizer at 70°C. When cooled, the lipids recrystallized, forming nanoparticles. The nanoparticle size was adjusted using an ultrasonic / high-pressure homogenizer.

[0090] [Table 2]

[0091] An aqueous dispersion containing liposomes as non-amphiphilic nanoparticles was prepared according to the composition in Table 3 below. A 100% hydrogenated oleoyl-palmitoyl / oleoyl-stearylphosphatidylcholine mixture (Lipoid S100-3) and cholesterol were dissolved in ethanol by heating to prepare a mixture. The mixture was added to water at 60°C, and then mixed and stirred in a homogenizer at 5,000 rpm for 5 minutes. Water-dispersible nanoparticles were then prepared using a high-pressure homogenizer (1,000 bar, 3 cycles). The remaining ethanol solution was removed using a rotary evaporator to prepare liposomes composed of lipids and cholesterol.

[0092] [Table 3]

[0093] An aqueous dispersion containing polymersomes as non-amphiphilic nanoparticles was prepared according to the composition in Table 4 below. Poly(methacrylic acid-co-stearyl methacrylate) copolymer, 100% hydrogenated oleoyl-palmitoyl / oleoyl-stearylphosphatidylcholine mixture (Lipoid S100-3), and cholesterol were dissolved in ethanol at 60°C to prepare a mixture. The mixture was added to water at 60°C and then mixed and stirred in a homogenizer at 5,000 rpm for 5 minutes to prepare a primary dispersed polymer-liposome complex. Water-dispersed nanoparticles were then prepared using a high-pressure homogenizer (1,000 bar, 3 cycles). The remaining ethanol solution was removed using a rotary evaporator to prepare a polymer-liposome nanocomplex using an acidity-sensitive polymer.

[0094] [Table 4]

[0095] [Manufacturing Example 2] Emulsion production A w / o emulsion was prepared according to the composition in Table 5 below. An oil phase was prepared and uniformly dispersed in an aji mixer at 70°C. An aqueous phase was prepared and heated to 70°C and stirred. The aqueous phase was added to the oil phase, and emulsified in a homogenizer at 4,000 rpm for 5 minutes, and then cooled.

[0096] [Table 5]

[0097] A w / o emulsion was prepared according to the composition in Table 6 below. An oil phase was prepared and uniformly dispersed using an aji mixer at 70°C. An aqueous phase was prepared and heated to 70°C while stirring. The aqueous phase was added to the oil phase, and emulsified using a homogenizer at 4,000 rpm for 5 minutes, followed by cooling.

[0098] [Table 6]

[0099] A w / s emulsion was produced according to the composition in Table 7 below. A silicone phase was prepared and uniformly dispersed at room temperature using an aji mixer. An aqueous phase was prepared and uniformly dissolved and dispersed using an aji mixer. The aqueous phase was added to the silicone phase, and emulsified using a homogenizer at 2,000 rpm for 5 minutes.

[0100] [Table 7]

[0101] [Example 1] Preparation of w / o / w complex emulsion composition W / o / w composite emulsion compositions were prepared by emulsifying at room temperature the compositions (wt%) shown in Tables 8 to 10 below. Water, excluding the non-amphiphilic nanoparticle aqueous dispersion, was prepared and stirred in a homogenizer at 8,000 rpm for 3 minutes to thoroughly disperse at room temperature. The non-amphiphilic nanoparticle aqueous dispersion was added to the dispersed water, and the mixture was thoroughly stirred in an agitator to produce a water mixture containing the non-amphiphilic nanoparticle aqueous dispersion. Furthermore, the oil component excluding the emulsion was uniformly mixed at room temperature, and then the prepared emulsion was added to produce an oil component containing the emulsion. The oil component was then added to the water, and the mixture was emulsified in a homogenizer at 2,000 rpm for 3 to 5 minutes at room temperature to produce a composite emulsion composition.

[0102] The viscosity of the emulsion compositions of Examples 1-1 to 1-15 was measured at room temperature and found to be in the range of 6500±500 cps (measuring device: Viscometer, LVDV-II+Pro, Brookfield, USA).

[0103] Furthermore, each emulsion composition was stored at room temperature, 37°C, 45°C, 60°C, under cycling conditions (a method in which the temperature was changed from 45°C to -15°C or from -15°C to 45°C in a 12-hour cycle), refrigerated (5°C), and frozen (-15°C) conditions, and the emulsion stability was visually evaluated after 4 weeks.The emulsion compositions of Examples 1-1 to 1-15 were found to have formulation stability with no separation of oil and water.The evaluation criteria are as follows: ◎: The interface between water and oil is well maintained under all temperature conditions, and no oil separation is observed. △: When the interface between water and oil becomes partially unstable under temperature conditions of 1 or higher. When the interface between water and oil is destroyed under temperature conditions of X;1 or higher, and oil separation occurs.

[0104] [Table 8]

[0105] [Table 9]

[0106] [Table 10]

[0107] As confirmed above, the present disclosure provides composite emulsion compositions formed by mixing and emulsifying an oil-containing emulsion with a water-containing dispersion of non-amphiphilic nanoparticles. The emulsion compositions of Examples 1-1 to 1-15, in which the emulsion content was less than 15 wt % relative to the total weight of the emulsion composition and the non-amphiphilic nanoparticle dispersion was contained at a weight ratio of greater than 1 relative to the emulsion content, were confirmed to significantly improve the stability of thermodynamically unstable composite formulations. Furthermore, it was confirmed that both emulsions containing and not containing PEG formed composite emulsion compositions with excellent formulation stability.

[0108] Meanwhile, when a heat-sensitive ingredient (e.g., retinol) is added to a conventional complex formulation, there is a technical limitation in that there is no way to prevent heat exposure. This is because the outer o / w portion is created through a heating process to produce the final w / o / w complex formulation. In contrast, the present disclosure has been confirmed to enable emulsification at room temperature during the production of a complex formulation, thereby significantly reducing heat damage to the heat-sensitive retinol ingredient.

[0109] [Example 2] Preparation of w / s / w complex emulsion composition According to the method described in Example 1, w / s / w complex emulsion compositions were prepared with the compositions (wt %) shown in Table 11 below, and the viscosity and emulsion stability were evaluated.

[0110] The viscosity of the emulsion compositions of Examples 2-1 and 2-2 was measured and found to be in the range of 11,000±2,000 cps.

[0111] It was also confirmed that by mixing and emulsifying an oil containing a w / s emulsion with water containing a dispersion of non-amphiphilic nanoparticles, a w / s / w complex emulsion composition with excellent formulation stability can be formed.

[0112] [Table 11]

[0113] [Comparative Example 1] Preparation of w / o / w complex emulsion composition According to the method described in Example 1, w / o / w complex emulsion compositions were produced with the compositions (wt %) shown in Tables 12 and 13 below, and the viscosity and emulsion stability were evaluated.

[0114] When the viscosities of the emulsion compositions of Comparative Examples 1-1 to 1-9 were measured, it was confirmed that the viscosities of the emulsion compositions of Comparative Examples 1-1 to 1-8 were in the range of 6500±500 cps, and that the viscosity of the emulsion composition of Comparative Example 1-9 exceeded 14,000 cps.

[0115] The emulsion compositions of Comparative Examples 1-1 to 1-4, in which the emulsion content was less than 15 wt % relative to the total weight of the emulsion composition and the weight ratio of the dispersion of non-amphiphilic nanoparticles to the emulsion content was greater than 1, were confirmed to exhibit excellent formulation stability. However, because the emulsion compositions of Comparative Examples 1-1 to 1-4 contained an emulsion content of 3 wt % or less, they were found to be unable to provide the sensation of use characteristic of composite formulations. Composite formulations are characterized by the fact that as the emulsion particles burst, the outermost water phase, the middle oil particles, and the innermost water phase are perceived in that order, providing a diverse sensation of use. Therefore, it was confirmed that, in forming the composite emulsion composition according to the present disclosure, it is preferable to use an emulsion content of greater than 3 wt %.

[0116] The emulsion compositions of Comparative Examples 1-5 to 1-8 contained a high emulsion content of 15% by weight, and were found to have a heavy, sticky feel when used. Furthermore, the emulsion compositions of Comparative Examples 1-5 to 1-8 contained an emulsion and a dispersion of non-amphiphilic nanoparticles at a weight ratio of 1:1, and therefore contained a low content of the dispersion of non-amphiphilic nanoparticles, resulting in a decrease in the emulsion stability of the composite preparation.

[0117] The emulsion compositions of Comparative Examples 1 to 9, in which the emulsion content was less than 15 wt % relative to the total weight of the emulsion composition and the weight ratio of the non-amphiphilic nanoparticle dispersion to the emulsion content was greater than 1, exhibited excellent formulation stability. However, the emulsion compositions of Comparative Examples 1 to 9, in which the content of the non-amphiphilic nanoparticle dispersion was 25 wt %, had viscosities exceeding 14,000 cps and were unable to form low-viscosity w / o / w formulations. Therefore, it was confirmed that, in forming the low-viscosity composite emulsion composition according to the present disclosure, it is preferable to use less than 25 wt % of the non-amphiphilic nanoparticle dispersion.

[0118] [Table 12]

[0119] [Table 13]

[0120] Although certain parts of the present disclosure have been described in detail above, it will be apparent to those skilled in the art that such specific descriptions are merely preferred embodiments and are not intended to limit the scope of the present disclosure. Therefore, the true scope of the present disclosure should be defined by the appended claims and their equivalents.

Claims

1. A multiple emulsion composition comprising: The emulsion composition is a mixture and emulsified of water and oil, the water comprises a dispersion of non-amphiphilic nanoparticles; The oil component contains an emulsion, and the emulsion contains an oil phase portion or a silicone phase portion as an external phase, The emulsion composition contains the water as a continuous phase and the oil as a dispersed phase, A multiple emulsion composition, wherein the dispersed phase is surrounded by non-amphiphilic nanoparticles.

2. 2. The multiple emulsion composition according to claim 1, wherein the average size of the non-amphiphilic nanoparticles is 10 nm or more and less than 1 μm.

3. 2. The multiple emulsion composition according to claim 1, wherein the non-amphiphilic nanoparticles are selected from the group consisting of nanoemulsion particles, solid lipid nanoparticles (SLN), liposomes, and polymersomes.

4. The multiple emulsion composition according to claim 1 , wherein the dispersion of the non-amphiphilic nanoparticles is immiscible with the oil component and / or is immiscible with the oil phase portion or silicone portion.

5. The multiple emulsion composition according to claim 1 , wherein the emulsion comprises an aqueous phase as an internal phase.

6. The multiple emulsion composition according to claim 1 , wherein the dispersion of non-amphiphilic nanoparticles and the emulsion are contained in a weight ratio of greater than 1:

1.

7. 2. The multiple emulsion composition according to claim 1, wherein the dispersion of non-amphiphilic nanoparticles is contained in an amount of less than 25% by weight based on the total weight of the emulsion composition.

8. 2. The multiple emulsion composition according to claim 1, wherein the emulsion is contained in an amount of less than 15% by weight based on the total weight of the emulsion composition.

9. 2. The multiple emulsion composition according to claim 1, wherein the average size of the dispersed phase is 1 to 50 μm.

10. The multiple emulsion composition according to claim 1 , wherein the emulsion composition further comprises a surfactant.

11. The multiple emulsion composition according to claim 1 , wherein the emulsion composition is PEG-free.

12. 2. The multiple emulsion composition according to claim 1, wherein the viscosity of the emulsion composition is 4,000 to 14,000 cps.

13. The multiple emulsion composition according to claim 1 , wherein the emulsion composition is obtained by mixing and emulsifying water and oil at room temperature.

14. 2. The multiple emulsion composition according to claim 1, wherein the emulsion composition is formulated as w / o / w or w / s / w.

15. A method for producing the multiple emulsion composition according to any one of claims 1 to 14, comprising the steps of: preparing a dispersion of non-amphiphilic nanoparticles; preparing an emulsion comprising an oil phase or a silicone phase as an external phase; preparing a water containing dispersion of the non-amphiphilic nanoparticles; producing the oil containing emulsion; and mixing the water and oil.

Citation Information

Patent Citations

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    KR1020150070920A

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