阅读说明：本技术 形成乳化颗粒的纳米胶囊及包含其的乳化组合物 (Nanocapsule forming emulsified particle and emulsified composition comprising the same ) 是由 黄允均 安知惠 李多情 金荣宣 朴胜寒 蔡秉根 崔桐沅 于 2019-08-28 设计创作，主要内容包括：本说明书中公开了一种形成乳化颗粒的纳米胶囊及包含其的乳化组合物。所述乳化组合物包含水相；以及油相,其中,在所述水相与油相的界面处设有多个非两亲性纳米胶囊,并且包含被所述多个非两亲性纳米胶囊包围的乳化颗粒。所述乳化组合物可以在水包油型乳化组合物中形成乳化颗粒,而无需使用表面活性剂。(Disclosed herein are nanocapsules forming emulsified particles and an emulsified composition comprising the same. The emulsified composition comprises an aqueous phase; and an oil phase, wherein a plurality of non-amphiphilic nanocapsules are disposed at an interface of the water phase and the oil phase, and comprise emulsified particles surrounded by the plurality of non-amphiphilic nanocapsules. The emulsion composition can form emulsion particles in an oil-in-water emulsion composition without using a surfactant.)

1. An emulsified composition comprising: an aqueous phase; and an oil phase, wherein,

wherein a plurality of non-amphiphilic nanocapsules are arranged at an interface between the water phase and the oil phase, and emulsified particles surrounded by the plurality of non-amphiphilic nanocapsules are formed.

2. The emulsified composition as claimed in claim 1, wherein the emulsified composition is an oil-in-water type composition.

3. The emulsion composition according to claim 1, wherein no oil separation occurs when the emulsion composition is frozen at a temperature of-60 ℃ or lower, sublimed by pressure reduction, and removed of water to prepare a dry substance.

4. The emulsified composition as claimed in claim 1, wherein the non-amphiphilic nanocapsules have an average particle size of 10nm to 1 μm.

5. The emulsified composition as claimed in claim 1, wherein the emulsified particles have an average particle size of 1 μm to 30 μm.

6. The emulsified composition as claimed in claim 1, wherein the non-amphiphilic nanocapsule is one or more selected from the group consisting of liposomes, polymersomes, nanoemulsion particles, and solid lipid nanoparticles.

7. The emulsified composition as claimed in claim 1, wherein the non-amphiphilic nanocapsules comprise one or more substances selected from the group consisting of phospholipids, waxes, lipids and ceramides.

8. The emulsified composition as claimed in claim 1, wherein the non-amphiphilic nanocapsule is contained in the aqueous phase of the emulsified composition in a form dispersed in an aqueous dispersion.

9. The emulsified composition as claimed in claim 8, wherein the oil phase and the aqueous dispersion containing the non-amphiphilic nanocapsules are mixed in a weight ratio of 1: 0.4 to 3.

10. The emulsified composition as claimed in claim 8, wherein the aqueous dispersion comprising the non-amphiphilic nanocapsules comprises water, a polyol and a lipid.

11. The emulsified composition as claimed in claim 10, wherein the lipid is one or more selected from the group consisting of phospholipids, waxes, oils and ceramides.

12. A method of preparing an emulsified composition according to any one of claims 1 to 11 comprising:

mixing an aqueous phase containing water-dispersible non-amphiphilic nanocapsules and an oil phase; and

a step of forming emulsified particles surrounded by the non-amphiphilic nanocapsules.

Technical Field

Disclosed herein are nanocapsules forming emulsified particles and an emulsified composition comprising the same.

Background

In general emulsification techniques, in addition to a method using a surfactant, a typical known method is to stabilize a particle having a bernoulli (Janus) structure, which has both hydrophilicity and lipophilicity, at an interface by adjusting physical properties of powder particles such as silica or partial powder particles. However, this method has disadvantages in that the stability of the dosage form under freezing and thawing is poor, and the feeling of use is limited due to a characteristic tailing feeling brought about by the characteristics of the powder particles used. Furthermore, there are still many technical limitations to the mass production of bernoulli-structured powders.

Among the existing emulsification techniques, there is a technique using a polyoxyethylene hydrogenated castor oil derivative, which has both hydrophilic and lipophilic properties by using Polyethylene glycol (PEG), thereby being stably located at the interface between water and oil. However, in recent years, attention to harmful ingredients in cosmetics has been increasing, and PEG is known to cause skin problems or urticaria by stimulating skin mucosa, so that more and more consumers select cosmetics not containing PEG, and thus the use of PEG in cosmetics is rapidly decreasing.

[ Prior art documents ]

[ patent document ]

(patent document 1) korean patent No. 10-1547528B 1.

Disclosure of Invention

Technical problem

In one aspect, the present invention aims to provide an emulsion composition that forms emulsion particles by water-dispersible non-amphiphilic nanocapsules without using a surfactant. Although Pickering (Pickering) emulsion is a form of emulsification using powder, it is required to modify physical properties of powder to be amphiphilic, and the water dispersion type non-amphiphilic nanocapsule according to the present specification is not required to be subjected to other physical property treatment and stably exists at an interface of water and oil to form emulsified particles.

In another aspect, the present description aims to provide a process for the preparation of said emulsified composition.

Technical scheme

In one aspect, the technology disclosed in this specification provides an emulsified composition comprising an aqueous phase; and an oil phase, wherein a plurality of non-amphiphilic nanocapsules are arranged at an interface between the water phase and the oil phase, and emulsified particles surrounded by the plurality of non-amphiphilic nanocapsules are formed.

In one exemplary embodiment, the emulsified composition may be an oil-in-water type composition.

In an exemplary embodiment, when the emulsion composition is prepared as a dry material by sublimating and removing water by reducing pressure after freezing at a temperature of-60 ℃ or less, oil separation may not occur.

In one exemplary embodiment, the non-amphiphilic nanocapsule may have an average particle size of 10nm to 1 μm.

In one exemplary embodiment, the emulsified particles may have an average particle size of 1 μm to 30 μm.

In one exemplary embodiment, the non-amphiphilic nanocapsule may be one or more selected from the group consisting of a Liposome (Liposome), a Polymersome (Polymersome), a Nanoemulsion Particle (Nanoemulsion Particle), and a Solid Lipid Nanoparticle (SLN).

In one exemplary embodiment, the non-amphiphilic nanocapsule may comprise one or more substances selected from the group consisting of phospholipids, waxes, greases (buttons), and ceramides.

In one exemplary embodiment, the non-amphiphilic nanocapsules may be included in the aqueous phase of the emulsion composition in a form dispersed in an aqueous dispersion.

In one exemplary embodiment, the mixing weight ratio of the oil phase in the emulsified composition to the aqueous dispersion comprising the non-amphiphilic nanocapsules may be 1: 0.4 to 3.

In one exemplary embodiment, the aqueous dispersion comprising the non-amphiphilic nanocapsules may comprise water, a polyol, and a lipid.

In one exemplary embodiment, the lipid may be one or more selected from the group consisting of phospholipids, waxes, oils, and ceramides.

In another aspect, the technology disclosed in this specification provides a method of preparing an emulsified composition comprising: mixing an aqueous phase containing water-dispersible non-amphiphilic nanocapsules and an oil phase; and a step of forming emulsified particles surrounded by the non-amphiphilic nanocapsules.

Advantageous effects

In one aspect, the technical effect disclosed in the present specification is to provide an emulsion composition that forms emulsion particles by water-dispersible non-amphiphilic nanocapsules without using a surfactant. The existing water dispersion type nanocapsules are mainly used for the purpose of skin transfer or stabilization of functional ingredients, but in the emulsion composition according to the present specification, the water dispersion type nanocapsules are used for the emulsification use of the emulsion composition without additional physical property modification, thereby forming emulsion particles. The emulsion composition according to the present specification can form emulsion particles in an oil-in-water type emulsion composition without using a surfactant.

In another aspect, the technical effect disclosed in the present specification is to provide a method for preparing the emulsified composition.

Drawings

Fig. 1a shows a polarization microscope image of an emulsified composition according to one embodiment of the present description.

Fig. 1b shows a confocal microscope image of an emulsified composition according to one embodiment of the present description.

Fig. 2 shows the results of comparing the rheological properties of the emulsified composition according to one embodiment of the present specification, the existing O/W type emulsion and the pickering emulsion. The chart shows, in order from top to bottom, a pickering emulsion, an O/W emulsion, the composition of example 11 and the composition of example 2.

Fig. 3 shows the result of confirming the change in skin texture when the emulsified composition according to one embodiment of the present specification is applied to the skin.

Fig. 4 shows a moisture content change rate (%) displayed by confirming a change in the moisture content of the skin when the emulsion composition according to one embodiment of the present specification is applied to the skin.

Fig. 5 shows the results of confirming the dosage form stability of the emulsified composition according to one embodiment of the present specification and the existing O/W type emulsion after freeze-drying.

Fig. 6 shows a result of confirming a change in dosage form stability with temperature of an emulsified composition according to one embodiment of the present specification. The results of storage under the conditions of (a) room temperature, (b)37 ℃, (c)45 ℃, (d) cold storage, and (e) cycle for 4 weeks are shown.

Fig. 7 shows the comparison result of the effect of delivering the efficacy ingredient according to one experimental example of the present specification.

Fig. 8 shows the results of comparing the skin absorption amounts of the efficacy ingredients according to one experimental example of the present specification.

Fig. 9a to 9d show results of confirming skin changes in a dry environment after applying a composition according to one embodiment of the present specification to the skin. FIG. 9a shows the change in skin moisture content; FIG. 9b shows the variation in skin tenderness around the eye; fig. 9c shows the variation of skin elasticity (R5) around the eyes; and fig. 9d shows the change in wrinkles (Ra) around the eyes.

Detailed Description

Hereinafter, the technology disclosed in the present specification will be described in detail.

In one aspect, the technology disclosed in the present specification provides an emulsified composition comprising emulsified particles formed from non-amphiphilic nanocapsules.

In another aspect, the technology disclosed in the present specification provides an emulsifier composition for forming emulsified particles, comprising a non-amphiphilic nanocapsule as an effective ingredient.

In yet another aspect, the technology disclosed in the present specification provides a non-amphiphilic nanocapsule for preparing an emulsified composition.

In yet another aspect, the technology disclosed in this specification provides for the use of non-amphiphilic nanocapsules in the preparation of an emulsified composition.

In yet another aspect, the technology disclosed in this specification provides a non-amphiphilic nanocapsule for forming emulsified particles.

In yet another aspect, the technology disclosed in this specification provides for the use of non-amphiphilic nanocapsules in forming emulsified particles.

In yet another aspect, the technology disclosed in this specification provides an emulsification method comprising the step of forming emulsified particles using non-amphiphilic nanocapsules.

In one exemplary embodiment, the emulsified composition may comprise emulsified particles.

In one exemplary embodiment, the emulsified particles may be surrounded by a plurality of non-amphiphilic nanocapsules.

In one exemplary embodiment, the emulsified composition comprises an aqueous phase; and an oil phase, wherein a plurality of non-amphiphilic nanocapsules of 2 or more are provided at an interface of the water phase and the oil phase, and emulsified particles surrounded by the plurality of non-amphiphilic nanocapsules are formed.

In one exemplary embodiment, the emulsification method may include: a step of disposing a plurality of non-amphiphilic nanocapsules at an interface of the aqueous phase and the oil phase; and a step of forming emulsified particles surrounded by the non-amphiphilic nanocapsules.

In one exemplary embodiment, the emulsifier composition is an aqueous dispersion composition, and may be an aqueous dispersion comprising non-amphiphilic nanocapsules.

In one exemplary embodiment, the emulsified composition may be a composition that is not emulsified with a surfactant.

In one exemplary embodiment, the plurality of non-amphiphilic nanocapsules may be attached to each other at an interface of the water phase and the oil phase to form emulsified particles.

In the present specification, a non-amphiphilic nanocapsule refers to a nanocapsule that is not amphiphilic, which means that the physical properties of the nanocapsule are not amphiphilic having both hydrophilicity and hydrophobicity. For example, the nanocapsule according to the present specification may be formed of an amphiphilic substance, such as phospholipid, but the physical properties of the formed nanocapsule itself do not have the amphiphilic property. Therefore, physical property modification for having the bernoulli structure is not required, and unlike the emulsifying composition using the bernoulli-structured powder, there may be no limitation by the physical properties of the oil phase. In addition, since the nanocapsule according to the present specification does not use polyethylene glycol (PEG), safety to the skin may be improved.

In the present specification, the nanocapsule refers to particles having a nano unit size, and the nanocapsule may have no distinction between an inner layer and an outer layer therein, or may have a layered structure of 2 layers or more. When the inner layer has a layered structure of 2 layers or more, the inner layer can be loaded with effective components for whitening, oxidation resistance and the like.

In one exemplary embodiment, the non-amphiphilic nanocapsule may have an amorphous, spherical or ellipsoidal shape.

In one exemplary embodiment, the emulsified composition may be an oil-in-water type composition.

The emulsion composition according to the present specification does not exhibit oil separation upon freeze-drying, and exhibits very excellent formulation stability.

In an exemplary embodiment, when the emulsion composition is prepared as a dry substance by sublimating and removing water by reducing pressure after freezing at a temperature of-60 ℃ or less, or-120 ℃ to-60 ℃, oil separation phenomenon may not occur upon visual confirmation.

In an exemplary embodiment, the temperature of the freeze-drying conditions may be from-120 ℃ to-100 ℃, or from-120 ℃ to-110 ℃.

In an exemplary embodiment, the pressure of the freeze-drying conditions can be 1mTorr to 100mTorr, 1mTorr to 50mTorr, 10mTorr to 80mTorr, or 20mTorr to 40 mTorr.

In one exemplary embodiment, the non-amphiphilic nanocapsule may have an average particle size of 10nm to 1 μm. In one exemplary embodiment, the non-amphiphilic nanocapsules may have an average particle size of 500nm or less.

In one exemplary embodiment, the non-amphiphilic nanocapsule may have an average particle size of 10nm to 500 nm.

In one exemplary embodiment, the emulsified particles may have an average particle size of 1 μm to 30 μm. In another exemplary embodiment, the average particle size of the emulsified particles 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, 10 μm or more, 11 μm or more, 12 μm or more, 13 μm or more, 14 μm or more, or 15 μm or more, and 30 μm or less, 29 μm or less, 28 μm or less, 27 μm or less, 26 μm or less, 25 μm or less, 24 μm or less, 23 μm or less, 22 μm or less, 21 μm or less, 20 μm or less, 19 μm or less, 18 μm or less, 17 μm or less, 16 μm or less, 15 μm or less, 14 μm or less, 13 μm or less, 12 μm or less, 11 μm or less, or 10 μm or less. For example, the emulsified particles may have an average particle diameter of 2 μm to 30 μm, 5 μm to 30 μm, 2 μm to 20 μm, 5 μm to 20 μm, 2 μm to 10 μm, 5 μm to 10 μm, or 2 μm to 15 μm.

The emulsified particles using the existing surfactant have a size of about 1 to 2 μm and coalescence between the emulsified particles occurs, whereas the emulsified particles according to the present specification are distinguished in that they may have a size of 2 μm or more and coalescence between the emulsified particles does not occur.

In one exemplary embodiment, the particle size of the non-amphiphilic nanocapsule or the particle size of the emulsified particles may refer to the diameter of the particles.

In one exemplary embodiment, the diameter may refer to the longest diameter.

In one exemplary embodiment, the non-amphiphilic nanocapsule may be one or more selected from the group consisting of a Liposome (Liposome), a Polymersome (Polymersome), a Nanoemulsion Particle (Nanoemulsion Particle), and a Solid Lipid Nanoparticle (SLN). The liposomes, polymersomes, nanoemulsion particles and solid lipid nanoparticles can be prepared and used according to conventional preparation methods known in the art.

In one exemplary embodiment, the non-amphiphilic nanocapsule is a nano emulsion particle whose effect includes that an effect ingredient can be loaded, and the skin delivery function of the effect ingredient is very excellent.

In an exemplary embodiment, the non-amphiphilic nanocapsule may comprise one or more substances selected from the group consisting of phospholipids, waxes, greases (buttons) and ceramides, thereby enabling the use of nanocapsules for forming emulsified particles without physical property modification.

In one exemplary embodiment, the phospholipid may be one or more selected from the group consisting of hydrogenated lecithin, hydrogenated phosphatidylcholine, soybean phospholipid, hydrogenated lysophosphatidylcholine, hydrogenated lysolecithin, and unsaturated lecithin.

In one exemplary embodiment, the wax may be one or more selected from the group consisting of vegetable wax, animal wax, mineral wax, and synthetic wax.

In one exemplary embodiment, the wax may be one or more selected from candelilla wax, carnauba wax, Ozokerite (Ozokerite), ceresin, montan wax, microcrystalline wax, methyl behenate, glyceryl dibehenate, glyceryl tribehenate, stearyl behenate, and trihydroxystearin.

In an exemplary embodiment, the grease may be one or more selected from shea Butter, cocoa Butter, almond grease, apricot grease, peach grease, Cupuacu Butter (Cupuacu Butter), pistachio Butter, olive Butter, aloe Butter, vanilla grease, illipe Butter, camellia Butter, babassu Butter, avocado Butter, jojoba grease, kokum Butter, cocoa Butter, mango Butter, soybean Butter, grape seed grease, kokum Butter, star palm grease (Murumuru Butter), and Macadamia nut seed grease (Macadamia seed Butter).

In an exemplary embodiment, the ceramide may be a natural ceramide, a synthetic ceramide, or a ceramide-like.

The ceramide is similar in structure to natural ceramide, is a synthetic substance having characteristics such as skin protection and moisturizing ability similar to natural ceramide, and is not limited in kind, and may be, for example, hydroxypropyl dipalmitoamide MEA.

In one exemplary embodiment, the non-amphiphilic nanocapsules may be included in the aqueous phase of the emulsion composition in a form dispersed in an aqueous dispersion.

In one exemplary embodiment, the aqueous phase comprises: an aqueous dispersion comprising non-amphiphilic nanocapsules, and the non-amphiphilic nanocapsules may be located at an interface of an aqueous phase and an oil phase of an emulsified composition to form emulsified particles.

In one exemplary embodiment, the non-amphiphilic nanocapsule may be a water-dispersed non-amphiphilic nanocapsule. Thus, the emulsifying composition according to the present description may comprise: an aqueous phase comprising water-dispersible non-amphiphilic nanocapsules; and an oil phase, wherein the plurality of non-amphiphilic nanocapsules form emulsified particles.

In the present specification, the non-amphiphilic nanocapsule of the water dispersion type refers to a non-amphiphilic nanocapsule existing in a dispersed form in a water phase, and the non-amphiphilic nanocapsule of the water dispersion type may refer to an aqueous dispersion including the non-amphiphilic nanocapsule.

In one exemplary embodiment, the emulsion composition may comprise a weight ratio of 1: an oil phase of 0.4 to 3 and an aqueous dispersion comprising non-amphiphilic nanocapsules. The effect includes preventing the problem of the decrease of the formulation stability caused by the too small content of the water dispersible non-amphiphilic nanocapsules. In addition, the problem that the use feeling such as extensibility, spreadability, and absorption feeling is reduced due to the excessively high content of the water-dispersible non-amphiphilic nanocapsule is prevented.

In an exemplary embodiment, the non-amphiphilic nanocapsules of the water dispersion type (i.e., the water dispersion containing the non-amphiphilic nanocapsules) added and mixed in the water phase of the emulsified composition may include water, a polyol, and a lipid.

In one exemplary embodiment, the non-amphiphilic nanocapsules of the aqueous dispersion type (i.e., the aqueous dispersion comprising the non-amphiphilic nanocapsules) added and mixed in the aqueous phase of the emulsion composition may comprise an aqueous phase portion of 45 to 90 wt%, based on the total weight of the aqueous dispersion; and 1 to 55 wt% of an oil phase comprising a lipid.

In one exemplary embodiment, the lipid may be contained in an amount of 1 to 30% by weight, based on the total weight of the aqueous dispersion. In another exemplary embodiment, the lipid may be present in an amount of 1 wt% or more, 3 wt% or more, 5 wt% or more, 7 wt% or more, 9 wt% or more, 11 wt% or more, 13 wt% or more, or 15 wt% or more, and 30 wt% or less, 28 wt% or less, 26 wt% or less, 24 wt% or less, 22 wt% or less, or 20 wt% or less, based on the total weight of the aqueous dispersion.

In one exemplary embodiment, the aqueous phase portion may include a polyol.

In one exemplary embodiment, the oil phase may comprise one or more materials selected from polyols, emulsifiers, and oils.

In one exemplary embodiment, the non-amphiphilic nanocapsules of the aqueous dispersion type (i.e., the aqueous dispersion comprising the non-amphiphilic nanocapsules) added and mixed in the aqueous phase of the emulsion composition may comprise an aqueous phase portion of 45 to 75 wt%; and 25 to 55 wt% of an oil phase comprising a polyol, a lipid, and an emulsifier.

In one exemplary embodiment, the polyol, the lipid, and the emulsifier are preferably added in amounts of 40 to 55 wt%, 30 to 50 wt%, and 10 to 20 wt%, respectively, based on the total weight of the oil phase part, in consideration of the formation of the emulsified particles.

In one exemplary embodiment, the lipid includes a phospholipid and a wax, and the mixing weight ratio of the phospholipid and the wax may preferably be 1: 9 to 18.

In one exemplary embodiment, the lipid further includes ceramide, and the mixed weight ratio of ceramide to phospholipid may be 1: 3 to 3: 1.

in one exemplary embodiment, the non-amphiphilic nanocapsules of the aqueous dispersion type (i.e., the aqueous dispersion containing the non-amphiphilic nanocapsules) added and mixed in the aqueous phase of the emulsified composition may comprise: 70 to 90 wt% of an aqueous phase portion comprising a polyol; and 10 to 30 wt% of an oil phase comprising an oil and a lipid.

In one exemplary embodiment, the lipid may be one or more selected from the group consisting of phospholipids, waxes, oils, and ceramides.

In one exemplary embodiment, the polyol may be one or more selected from the group consisting of butylene glycol, propylene glycol, glycerin, pentylene glycol, dipropylene glycol, and diglycerin.

In one exemplary embodiment, the emulsifier may be one or more selected from sorbitan sesquioleate, glyceryl stearate, polysorbate 60, polysorbate 80, sorbitan stearate, PEG-20 glyceryl isostearate, polyglyceryl-2 diisostearate, cetostearyl alcohol, polyglyceryl-3 methylglucose distearate, PEG-100 stearate, sorbitan isostearate, lauryl glucoside, disodium cocoamphodiacetate, cocofatty acid diethanolamide, and cocamidopropyl betaine.

In an exemplary embodiment, the oil may be one or more selected from the group consisting of vegetable oil, silicone oil, ester oil, and hydrocarbon oil.

In one exemplary embodiment, the vegetable Oil may be one or more selected from the group consisting of olive Oil, camellia Oil, castor Oil, jojoba Oil, almond Oil, grape seed Oil, vanilla Oil (Herb Oil), rose Oil, coconut Oil, avocado Oil, macadamia nut Oil, moringa Oil, rice bran Oil, apricot seed Oil, sunflower seed Oil, meadowfoam seed Oil, and crambe Abyssinian Oil.

In one exemplary embodiment, the silicone oil may be one or more selected from the group consisting of polydimethylsiloxane (Dimethyl polysiloxane), methylphenylpolysiloxane, Decamethylcyclopentasiloxane (Decamethylcyclopentasiloxane), methylpolytrimethicone, phenylpolytrimethicone, cyclomethicone, and Dimethicone (Dimethicone).

In an exemplary embodiment, the ester oil may be one or more selected from isopropyl palmitate, 2-octyldodecanol myristate, isopropyl myristate, butyl octanol salicylate, cetearyl octanoate, cetyl octyl hexanoate (cetyl hexanoate), coco octanoate/decanoate, decyl cocoate, isostearyl isostearate, pentaerythritol tetracaprylate, dioctyl carbonate.

In one exemplary embodiment, the hydrocarbon oil may be one or more selected from the group consisting of n-octane, n-nonane, n-decane, n-undecane, n-dodecane, n-tridecane, n-tetradecane, n-pentadecane, n-hexadecane, n-heptadecane, n-octadecane, vaseline, paraffin, ceresin, hydrogenated polydecene, hydrogenated polyisobutene, and squalane.

In another aspect, the technology disclosed in the present specification provides a method for preparing the water-dispersible non-amphiphilic nanocapsule, comprising: a step of mixing and dissolving the aqueous phase; mixing and dissolving the oil phase; and a step of adding the oil phase part to the water phase part, dispersing the oil phase part with a homogenizer, and then cooling the resulting dispersion.

The homogenizer may use any method without limitation so long as it provides sufficient energy required to disperse the molten lipophilic mixed phase to produce nanocapsules having a particle size of 10nm to 1 μm. In particular, ultrasonic and high-pressure homogenizers may be preferred for the formation of lipid nanocapsule particles.

The emulsion composition does not use an additional surfactant for emulsifying the emulsion composition, other than the surfactant for preparing the nanocapsule. Therefore, Switching (Switching) with the surfactant present in the outer phase of the emulsion composition does not occur, and the stability of the nanocapsule and the stability of the emulsified particle structure in the dosage form can be maintained for a longer time. Therefore, the emulsion composition is excellent in formulation stability under freeze-thaw. Also, since the water dispersion type non-amphiphilic nanocapsule is easily mass-produced, it is possible to improve the disadvantages of the conventional emulsification method of stabilizing powder at the interface.

When the emulsion composition is applied to the skin, nanocapsules present at the interface are accumulated (packing) on the skin surface to improve roughness of the skin, and evaporation of moisture can be suppressed by a blocking effect (occlusive effect), thereby maintaining a high skin moisture content. In addition, when the functional ingredient is loaded in the non-amphiphilic nanocapsule, the skin permeability of the functional ingredient can be improved. The nanocapsule according to the present specification may be variously designed according to the intended purpose such as use feeling, efficacy, and the like.

In another aspect, the technology disclosed in this specification provides a method of preparing an emulsified composition comprising: mixing an aqueous phase containing water-dispersible non-amphiphilic nanocapsules and an oil phase; and a step of forming emulsified particles surrounded by the non-amphiphilic nanocapsules by attaching the non-amphiphilic nanocapsules to each other.

[ examples ] A method for producing a compound

Hereinafter, the present disclosure is described in more detail by way of examples. It will be understood by those skilled in the art that these examples are only for illustrating the present disclosure, and the scope of the present invention is not limited by these examples.

[ examples 1-1 and 1-2 ] preparation of Water-dispersible non-amphiphilic nanocapsules

In this example, water-dispersible non-amphiphilic nanocapsules were prepared according to the compositions (wt%) of tables 1 and 2 below. Specifically, the oil phase was heated and dissolved at 70 ℃, and then dispersed using a homogenizer to prepare a lipophilic mixture. The aqueous phase was heated and dissolved at 70 ℃ in another vessel, and the prepared lipophilic mixture was then slowly added to the aqueous phase and formed into capsule particles by a homogenizer at 70 ℃. Upon cooling, lipid recrystallization occurs and nanocapsule particles are formed. The size of the nanocapsule was prepared to a particle size of 10nm to 1 μm by using a homogenizer of an ultrasonic wave and a high pressure homogenizer, thereby preparing water dispersible non-amphiphilic nanocapsules in the form of solid lipid nanoparticles (example 1-1) and nanoemulsion particles (example 1-2).

[ TABLE 1 ]

[ TABLE 2 ]

[ examples 2 to 10, and comparative example 1 ] preparation of emulsified compositions

An emulsified composition was prepared according to the composition (wt%) of table 3 below, as described below.

1) Heating, mixing and dissolving an aqueous phase comprising water, water-dispersible non-amphiphilic nanocapsules, 1, 2-hexanediol, ethylhexylglycerin, carbomer, and tromethamine at 50-75 deg.C.

2) Heating the rest oil phase at 50-75 deg.C, mixing, and dissolving.

3) While maintaining the temperature at 50 to 75 ℃, the oil phase part was added to the dissolution tank of the water phase part, and an emulsified composition was prepared by a homogenizer.

[ TABLE 3 ]

[ Experimental example 1 ]

The prepared emulsion composition was evaluated for spreadability upon application, moisture retention durability, absorption feeling, and formulation stability, and is shown in table 4.

[ TABLE 4 ]

Very good: the quality is excellent; o: good; and (delta): difference (D)

From the comparison of examples 2, 4 to 6, it was confirmed that emulsification using the non-amphiphilic nanocapsule was possible regardless of the type of oil or polarity of the oil, and the formulation stability was excellent. Thus, it was confirmed that the water dispersion type non-amphiphilic nanocapsule according to the present specification can be used to form emulsified particles without being limited by an oil phase.

Further, in examples 2, 3, and 7 and comparative example 1, the stability of the formulation according to the content of the non-amphiphilic nanocapsules of the water dispersion type and the oil content was confirmed, and as a result, it was preferable in terms of the stability of the formulation that the content of the non-amphiphilic nanocapsules located at the interface of water and oil increased as the oil content increased. In example 7, the moisture retention duration and the absorption feeling were not good because the contents of the oil and the non-amphiphilic nanocapsule were relatively low.

Further, from comparison of examples 2, 8 to 10, it was confirmed that the feeling of use can be adjusted by adjusting the content of the non-amphiphilic nanocapsules, because the content of the water dispersion type non-amphiphilic nanocapsules affects the extensibility and spreadability at the initial coating.

[ Experimental example 2 ]

A fluorescent dye (nile red, 515-560nm excitation; >590nm emission) was added at the time of preparing the nanocapsule, and the water dispersion type non-amphiphilic nanocapsule was prepared in the same manner as in example 1-1, an emulsified composition was formed in the same manner as in example 2, and then observed under a microscope to confirm the emulsified particle structure of the emulsified composition.

FIG. 1a shows an image observed with a Polarizing Microscope (LV 100 POL); fig. 1b shows an image observed with a Laser Confocal Microscope (VIVASCOPE 1500). It can be observed that the nanocapsules loaded with fluorescent dye are located at the interface of the emulsified particles. It was confirmed that the emulsion composition according to the present specification can stabilize nanocapsules at the interface of an aqueous phase and an oil phase without using a surfactant, thereby forming emulsion particles.

[ Experimental example 3 ]

The rheological properties of the emulsified compositions using nanocapsules according to examples 2 and 11 of the present specification, the O/W type emulsion and the pickering emulsion as conventional emulsified compositions (measuring apparatus: rheometer (AR2000), measurement conditions: osc. stress (Pa)0.1 to [email protected] frequency 50Hz) were measured and compared, and as a result, it was found that the emulsified compositions according to examples 2 and 11 of the present specification had Yield stress (Yield stress) values (see fig. 2). This means that, unlike other dosage forms, the burst sensation at the initial use, that is, the water burst sensation at the initial use can be felt. In addition, the latter section exhibits a viscosity increase phenomenon similar to a shear-thickening (shear-thickening) phenomenon. This is because the characteristics of the nanocapsule are expressed at the rear stage. The emulsion composition according to the present specification shows a smooth ending feeling of the nanocapsule particles due to the coating of the nanocapsules due to the application, and shows the effect of improving skin roughness and moisture retention.

From the above, it was confirmed that the compositions of example 2 and example 11 have different characteristics in structure and feeling in use as compared with the conventional emulsion dosage forms. The O/W type emulsion and Pickering emulsion were prepared and used in the experiments as follows.

Preparation of O/W type emulsion

An O/W type emulsion was prepared according to the following composition (wt%) of Table 5 in accordance with a conventional method.

[ TABLE 5 ]

Preparation of pickering emulsion

Pickering emulsions were prepared according to the conventional method according to the composition (% by weight) of Table 6 below.

[ TABLE 6 ]

[ Experimental example 4 ]

The prepared emulsion composition of example 2 was applied to the skin to observe the change rate of texture and moisture content.

As shown in fig. 3, the results of the texture change experiment confirmed that the emulsion composition of example 2, when applied to the skin, had a 14.4% reduction in skin roughness as compared to that before application. Further, as shown in fig. 4, it was confirmed from the results of the rate of change of the moisture content that the skin retained moisture longer when the emulsion composition of example 2 was applied to the skin than when it was not applied and the O/W emulsion of the experimental example 3. This is because the nanocapsules forming the emulsified particles burst and are accumulated on the surface of the skin when being applied to the skin, thereby preventing water loss and smoothing the texture.

[ Experimental example 5 ]

The prepared emulsion composition of example 2 and the O/W type emulsion of experimental example 3 were freeze-dried to compare their formulation stability.

Freeze-drying refers to a drying process in which a substance is frozen and the dry substance is prepared by direct sublimation of ice into steam by reducing the partial pressure of water vapor (water vapor). First, the emulsion composition of example 2 and the O/W type emulsion of Experimental example 3 were frozen at a temperature of-80 ℃ or below using a refrigerator, and then transferred to a dryer for sublimation, thereby obtaining freeze-dried samples as shown in FIG. 5 (left: O/W type emulsion of Experimental example 3, right: emulsion composition of example 2).

Such freeze-drying is advantageous in that it can stabilize functional ingredients according to the desired purpose and be applied to various forms of cosmetics by being re-processed into powder and rehydrated (rehydration) at the use stage. In contrast to ordinary emulsions such as the O/W emulsion of experimental example 3, which did not undergo freeze-drying because of the phenomenon of oil exudation due to the deformation of the appearance caused by shrinkage during freeze-drying, the emulsion composition of example 2 maintained a good emulsion particle structure during freeze-drying, did not undergo oil separation, and had excellent formulation stability. In the case of ordinary emulsions, additional effort is required to maintain a good emulsified particle structure, and therefore, an unexpected feeling in use may occur. However, when the nanocapsule according to the present specification is used, since the emulsified particles are well-maintained in their structure by being encapsulated by the nanocapsule, excellent dosage form stability and feeling in use can be achieved without using additional other materials.

[ Experimental example 6 ]

The formulation stability of the prepared emulsified composition of example 2 was observed as a function of temperature and is shown in fig. 6. As a result, it was confirmed that the stability of the formulation was good after storage at room temperature, 37 ℃ and 45 ℃ for 4 weeks under refrigeration. Further, the storage was carried out in cycles of 12 hours and 4 weeks by changing the temperature from 40 ℃ to-10 ℃ or-10 ℃ to 40 ℃ over 12 hours, and as a result, it was confirmed that the stability of the dosage form was good and no oil separation occurred.

Further, the formulation stability of the emulsion composition of example 2 prepared as described was observed by viscosity measurement with time and is shown in fig. 7. The viscosity of a sample stored at 30 ℃ was measured using a Viscometer (Brookfield Viscometer, LVDV-2+ P) (measurement conditions: S64 spindle, 12rpm, measurement for 2 minutes).

[ TABLE 7 ]

[ Experimental example 7 ]

The delivery effect of tocopherol as a functional ingredient in the manufactured nanocapsule of the emulsion composition of example 11 was confirmed and is shown in fig. 7. The O/W type emulsion prepared by adding 0.5 wt% of tocopherol to the O/W type emulsion of experimental example 3 was used to compare the effect of delivering the efficacy ingredient.

In order to confirm the effect of delivering the functional components, each composition was applied to the skin for 3 hours, and then the remaining composition on the surface was wiped off and 10 pieces of a release tape (D-square striping Discs D101, cuperm) for collecting the skin stratum corneum were attached (taping) to prepare samples. The skin penetration was confirmed by imaging the functional component tocopherol attached to the tape using DESI-MS (instrument: QTOF-MS (Q-time of flight mass spectrometer)) imaging technique.

As a result, it was confirmed that the emulsion composition of example 11 allows the functional ingredient to be delivered deeper into the skin than the O/W type emulsion of experimental example 3 to which tocopherol is added. The bright yellow portion in fig. 7 represents the efficacy ingredient.

[ Experimental example 8 ]

The skin absorption amount of tocopherol as a functional ingredient in the manufactured nanocapsule of the emulsion composition of example 11 was confirmed and is shown in fig. 8. The O/W type emulsion prepared by adding 0.5 wt% of tocopherol to the O/W type emulsion of experimental example 3 was used to compare the skin absorption amount of the effect ingredient.

In order to confirm the skin absorption amount of the functional components, each composition was applied to the skin for 3 hours, and then the remaining composition on the surface was wiped off, and 10 pieces of a release tape (D-square striping Discs D101, cuperm) for collecting the skin stratum corneum were attached (taping) to prepare samples. Tocopherol as an effective ingredient attached to the tape was analyzed by HPLC analysis to confirm skin absorption (analytical equipment Waters 2695, column SunFire slide (4.6 × 250mm × 5 μm), hexane: isopropanol 99: 1, flow rate 0.7mL/min, 325 nm).

As a result, it was confirmed that the skin absorption amount of tocopherol in the emulsion composition of example 11 was higher than that of the O/W type emulsion of experimental example 3 to which tocopherol was added. In fig. 8, tapes 1 to 5, 6 to 10, and 1 to 10 represent the average value of tapes No. 1 to 5, 6 to 10, and 1 to 10, respectively, and the y-axis represents the measured absorption amount (%).

[ Experimental example 9 ]

After the prepared emulsion composition of example 11 was applied to the skin, the moisture content of the skin, the softness of the skin around the eyes, the elasticity of the skin around the eyes, and the change of wrinkles around the eyes were confirmed in a dry environment, and are shown in fig. 9a to 9 d. Wait for 1 hour under the condition that the relative humidity is less than 35 percent to form a dry environment.

As a result, it was confirmed that the emulsified composition of example 11 had the effects of increasing the moisture content of the skin, the softness of the skin around the eyes, the elasticity of the skin around the eyes, and preventing wrinkles around the eyes even under a dry environment, unlike the experimental group not coated with the composition.

As described above, having described certain portions of the present disclosure in detail, it should be understood by those skilled in the art that these specific techniques are only preferred embodiments and the scope of the present invention is not limited thereto. Therefore, the scope of the invention is to be defined by the appended claims and equivalents thereof.