WO2017057873A1 - High ceramide content nano emulsion with improved transparency, cosmetic composition containing same, and preparation method therefor - Google Patents

Abstract

The present invention relates to a high ceramide content nano emulsion with improved transparency, a cosmetic composition containing the same, and a preparation method therefor and, more specifically, to a high ceramide content nano emulsion, a cosmetic composition containing the same, and a preparation method therefor, the nano emulsion comprising a ceramide, an ionic surfactant, and a polyol, and prepared by additionally adding silicone oil in a proper mixing ratio and emulsifying the mixture under high pressure. According to the high ceramide content nano emulsion with improved transparency, of the present invention, emulsified particles having a nano size of 10-30 nm are prepared such that a high amount, up to 10 wt%, of ceramide can be contained, and gelation is prevented such that stability can be improved when the emulsion is applied to cosmetics. In addition, transparency is improved such that the ceramide, having been restrictively applied to conventional liquid-type cosmetics, can be widely applied as a transparent toner type or a cream type.

Description

High content ceramide nanoemulsion with improved transparency, cosmetic composition containing the same and preparation method thereof

This application claims the benefit of priority based on Korean Patent Application No. 10-2015-0137335 filed on September 30, 2015, and all the contents disclosed in the literature of that Korean patent application are incorporated as part of this specification.

The present invention relates to a high content ceramide nanoemulsion with improved transparency, a cosmetic composition containing the same and a method for preparing the same, and more specifically, to prepare a ceramide, an ionic surfactant, a polyol and a silicone oil by high-pressure emulsification in an appropriate blending ratio It relates to a high content ceramide nano emulsion, a cosmetic composition containing the same and a method for producing the same.

The surface of human skin consists of keratinocytes that have differentiated from the basal layer and have matured keratinocytes. These keratinocytes are bound by the double-chain lamellar structure of ceramide, which is present in large amounts in the stratum corneum, thus maintaining a smooth and elastic skin.

Ceramides are poorly soluble and are prepared as fine particles when contained in a large amount in a cosmetic formulation. In this case, the formulation is less stable and gelation occurs. If the particle size is small, the surface energy between the particles increases, and the attraction force is large. Since the interaction between the ceramides is increased and not completely dispersed in the oil phase, the gelation occurs due to the binding between the ceramides which come out somewhat in the water phase.

In order to solve this problem, a technique of inducing ceramide stabilization by making granules (grains) from ceramide, stearic acid and cholesterol, and adding them to the last step in preparing an emulsion is applied. In other words, by using a method of making granules that stabilized ceramide externally first and then dispersing them in an emulsion, a method of implementing stability by removing fluidity from solid ceramides made of solids is used. Korean Patent Application No. 2008-0072355 discloses a technique related to ceramide on a nucleating agent using a solidification shell.

However, this method also reduces the amount that can be used in the actual cosmetics due to the large amount of encapsulating agent used in the encapsulation process of ceramide. In addition, in the feeling of use as an essential component of the cosmetic composition, a saccharide-based or polymer-based encapsulating agent has a disadvantage in that it impairs the feeling of use of the original cosmetic.

[Preceding technical literature]

Republic of Korea Patent Publication No. 0837558 "Emulsion composition containing double stabilized ceramide nanocapsule, preparation method thereof and skin cosmetic composition using the same"

Ceramide, which prevents the loss of moisture in skin tissues for people with dry skin and acts as a barrier to foreign substances on the skin surface, is easy to crystallize in cosmetic formulations due to its structural specificity, and when contained in a high content of the formulation, layer Separation or precipitation occurs.

Therefore, the ceramides contained in the current cosmetic formulations are usually about 2% by weight, and these cosmetic formulations are not applicable to the skin type, which is a transparent formulation because of the significant drop in transparency and turbidity. The situation is being manufactured. In addition, when left for a long time, the formulation stability is lowered and gelation occurs.

Accordingly, an object of the present invention is to prepare a ceramide nanoemulsion having excellent formulation stability capable of maintaining transparency while containing a high content of ceramide.

The present invention has been made to achieve the above object, and provides a high content ceramide nanoemulsion with improved transparency, including ceramide, ionic surfactant, polyol and ethanol. The nanoemulsion may further comprise a silicone oil. At this time, the composition is 1 to 10% by weight of ceramide; 1 to 1.5 weight percent of ionic surfactant; 20 to 40 weight percent polyol; And 1 to 5% by weight of ethanol; It is preferably contained in a composition of 15 to 30% by weight of silicone oil, and the particle size of the high content ceramide nanoemulsion thus prepared is preferably 10 to 30 nm.

The present invention provides a method for producing a ceramide emulsion, comprising the steps of: i) mixing a ceramide-dissolved oil phase solution and a surfactant-dissolved aqueous phase solution to prepare a primary dispersion; ii) preparing a secondary oil dispersion by adding silicone oil and ethanol to the primary mixed solution; iii) emulsifying the secondary mixed solution at high speed to prepare a primary emulsion; iv) preparing a secondary emulsion by high pressure emulsifying the primary emulsion, wherein the solvent of the oil phase solution in step i) is a polyol, and the surfactant of the aqueous phase solution is an ionic surfactant. It provides a method for producing a ceramide emulsion improved transparency. At this time, the high speed emulsification of step iii) may be emulsified at 5000 to 10000 rpm using a homomixer for 1 to 20 minutes, and the high pressure emulsification of step iv) is performed using a microfludizer to 12000. It can emulsify 1 to 5 cycles at ~ 18000 psi.

According to the high content ceramide nanoemulsion with improved transparency of the present invention, by preparing a nano-size emulsified particles of 10 to 30 nm, it can contain a ceramide in a high content up to 10% by weight, and prevents gelation when applied to cosmetics Stability can be improved. In addition, since the transparency is improved, it is possible to apply the ceramide, which was conventionally applied to cosmetics of the latex type in a wide range, to a transparent skin type or a cream type.

1 is an image of a comparative example comparing transparency of a high content ceramide nanoemulsion as an embodiment of the present invention.

Figure 2 is a flow chart of the ceramide emulsion production method improved transparency of the present invention.

The present invention relates to a high content ceramide nanoemulsion with improved transparency, to a cosmetic composition containing the same and a method for preparing the same, and more particularly to a ceramide, an ionic surfactant, a polyol, and additionally adding silicone oil in an appropriate blending ratio It relates to a high content ceramide nanoemulsion prepared by high-pressure emulsification, a cosmetic composition containing the same and a preparation method thereof. Hereinafter, the present invention will be described in detail.

The ceramide is preferably contained 1 to 10% by weight based on the total weight of the emulsion. If it is included in less than 1% by weight when applied as a cosmetic formulation is ineffective, if contained in more than 10% by weight it will cause the gelation to reduce the formulation stability.

The ionic surfactant is potassium cesyl phosphate, sodium stearoyl glutamate, glyceryl stearate citrate, distearyl dimonium chloride, distearyl dimonium chloride β-branched monohexadecyl phosphate arginine (Hexadecyl) may be used alone or in combination of two or more selected, more preferably potassium cetyl phosphate (Potassium Cetyl Phosphate) or sodium stearoyl glutamate (Sodium Stearoyl Glutamate) Can be used.

Such ionic surfactant is preferably contained 1 to 1.5% by weight based on the total weight of the emulsion. When it is included in less than 1% by weight, the gelation occurs due to the stabilization effect is insufficient when applied as a cosmetic formulation, and when it exceeds 1.5% by weight it is preferable to adjust appropriately within the above range.

The polyol is to improve the transparency and improve the moisturizing power by adjusting the refractive index of the formulation, glycerin (Glycerine), 1,3-butylene glycol (1,3-Butylene Glycol; BG), propylene glycol (Propylene Glycol; PG) And dipropylene glycol (Dipropylene Glycol; DPG) can be used alone or two or more selected from the group consisting of, it is preferably contained within 20 to 40% by weight relative to the total weight of the emulsion. When included in less than 20% by weight is limited to solubilization of high content ceramide, when exceeding 40% by weight there is a problem that the feeling of use on the skin is lowered.

The silicone oil is to replace the wax part that can form a conventional lamellar structure to adjust the feeling of use and suspension, and to apply a dimethicone-based, cyclopentasiloxane (Cyclopentasiloxane) similar to the refractive index of the wax Can be. Such silicone oil is preferably contained within the range of 15 to 30% by weight based on the total weight of the emulsion, when the content is less than 15% by weight, the transparency is lowered, and when more than 30% by weight, the interface for emulsifying the silicone oil There arises a problem that the content of the active agent exceeds the appropriate value.

The particle size of the high content ceramide nanoemulsion according to the present invention is preferably 10 to 30 nm. If it is less than 10 nm it is difficult to achieve due to the manufacturing process, if it is more than 30 nm it is because the transparency is lowered and gelation is caused to reduce the formulation stability.

On the other hand, high content ceramide nanoemulsion with improved transparency can be contained as a cosmetic composition by diluting or adding a thickener, which is skin, lotion, cream, serum, essence, powder, foundation, spray, mask pack, sheet pack, It may be formulated in the form of one of a sleeping pack, a washoff pack and a peeloff pack.

Thickeners added as the cosmetic composition may be known, and include dextrin palmitate, dextrin palmitate / ethylhexanoate, cyclopentasiloxane, and PEG / PPG-19 / 19. Dimethicone (Cyclopentasiloxane and PEG / PPG-19 / 19 Dimethicone), Polysilicone-11, Dimethicone Crosspolymer, Quaternium-18 Hectorite, Stearal Cornium hectorite (Stearalkonium Hectorite) and disteardimonium hectorite (Disteardimonium Hectorite) It can be used alone or two or more selected from the group consisting of.

Furthermore, the present invention provides a method for preparing ceramide emulsion, comprising the steps of: i) mixing the oil phase solution in which ceramide is dissolved and the aqueous solution in which surfactant is dissolved to prepare a primary oil dispersion; ii) preparing a secondary oil dispersion by adding silicone oil and ethanol to the primary mixed solution; iii) emulsifying the secondary mixed solution at high speed to prepare a primary emulsion; iv) preparing a secondary emulsion by high pressure emulsifying the primary emulsion, wherein the solvent of the oil phase solution in step i) is a polyol, and the surfactant of the aqueous phase solution is an ionic surfactant. It provides a method for producing a ceramide emulsion improved transparency.

At this time, the high speed emulsification of step iii) may be emulsified at 5000 to 10000 rpm using a homomixer for 1 to 20 minutes, and the high pressure emulsification of step iv) is performed using a microfludizer to 12000. It can emulsify 1 to 5 cycles at ~ 18000 psi.

According to the grant High content  Ceramide nano emulsion  Produce

Ceramide-102 (Hydroxypropyl Bislauramide MEA) and Ceramide-104 (Hydroxypropyl Bispalmitamide MEA) were used as ceramides, Eumulgin SG (Sodium Stearoyl Glutamate) as an ionic surfactant, Glycerine as a polyol, and dimethicone as a silicone oil. Nanoemulsion was prepared according to the composition ratios of Examples 1 to 6 of Table 1 using (Dimethicone).

The preparation process of the nanoemulsion of Examples 1 to 6 was carried out as follows.

step 1) After adding Ceramide-102 or Ceramide-104 to Glycerine, the mixture is stirred and heated to 80 ° C. for oil dispersion.

step 2) Eumulgin SG is added to the water and dispersed in oil while heating up to 80 ° C.

step 3) The mixture of step 2) is slowly added while homomixing the mixture of step 1).

step 4) After confirming the appearance of the mixture of step 3), dimethicone and ethanol were further added, and primary emulsification was performed at 8500 rpm for 5 minutes.

step 5) The primary emulsified mixture is subjected to 3 cycles (10 minutes based on 500 ml) at 15000 psi using a Microfludizer.

Composition	Example 1	Example 2	Example 3	Example 4	Example 5	Example 6
Ceramide-102	5%	5%	-	-	-	-
Ceramide-104	-	-	5%	5%	5%	5%
Eumulgin SG	1.5%	1.5%	1.5%	1.5%	1.5%	1.5%
Glycerin	30%	30%	20%	30%	30%	30%
Dimethicone	16%	16%	16%	16%	16%	16%
Ethanol	3%	0%	3%	3%	9%	12%
Water	To 100	To 100	To 100	To 100	To 100	To 100

High content  Ceramide nano Emulsion  Itemized Test

Table 2 below shows the results of the samples of the prepared Examples 1 to 6 to evaluate the items of particle size, stability and turbidity. The 4-week stability test was evaluated for stabilization through crystallization or layer separation after 4 weeks at a temperature of 45 ° C., and the suspension was carried out to satisfy the particle size range of 10 to 30 nm in the samples of Examples 1 to 6. The results are based on the Nephelometry Turbidity Unit (NTU) by Nephelometry, which measures the scattering degree by the suspended particles by selecting Examples 1, 2, 5, and 6.

test item	Example 1	Example 2	Example 3	Example 4	Example 5	Example 6
Particle size	18nm	22 nm	32nm	58 nm	29 nm	25 nm
4 weeks stability (cold)	Good	Good	Good	Good	Good	Separation
Turbidity (NTU)	32	43	-	-	89	153

According to the test results of [Table 2], Ceramide-102 of the two ceramides was found to form smaller nanoemulsion particles at the same composition ratio than Ceramide-104. In addition, when comparing Examples 1 and 2 and Examples 4 to 6, respectively, it was found that the fine particles were formed as the ethanol content was increased. It was confirmed that the small size does not necessarily mean high stability.

Preparation of High Content Ceramide Nanoemulsion According to Surfactant Type

The nanoemulsion was prepared by varying the type of surfactant according to Examples 7 to 10 in Table 3 below, according to the kind of surfactant. Ceramide adopts Ceramide-104, and surfactants include TA-100 (Distearyl Dimonium Dhloride), Amphisol K (Potassium Cetyl Phosphate), Dracorin CE (Glyceryl Stearate Citrate), and Phopure LC (β-branched monohexadecyl phosphate arginine) Four species were each added.

Since the manufacturing process of the nanoemulsion according to Examples 7 to 10 of Table 3 is the same as the method for preparing the nanoemulsion of Examples 1 to 6, a detailed description thereof will be omitted.

Creation costs	Example 7	Example 8	Example 9	Example 10
Ceramide-104	5%	5%	5%	5%
TA-100	1.5%	-	-	-
Amphisol K	-	1.5%	-	-
Dracorin CE	-	-	1.5%	-
Phopure LC	-	-	-	1.5%
Glycerin	30%	30%	30%	30%
Dimethicone	16%	16%	16%	16%
Ethanol	3%	3%	3%	3%
Water	To 100	To 100	To 100	To 100

Itemized Testing of High Content Ceramide Nanoemulsions

Since the item-specific test method of the nano-emulsion according to Examples 7 to 10 of Table 4 is the same as the item-specific test method of the nano-emulsion of Examples 1 to 6 it will not be described in detail.

test item	Example 7	Example 8	Example 9	Example 10
Particle size	More than 100nm	22 nm	58.5 nm	43 nm
4 weeks stability (cold)	decision	Good	Particulate Identification	Good

The results of the test in Table 4 indicate that the particle size of the cationic surfactant TA-100 (Example 7) exceeded the nano range, and that the particle size of the relatively bulk Dracorin CE (Example 9) was large. Can be. Amphisol K (Example 8) also showed similar particle size and stability as Eumulgin SG (Examples 1 to 6).

Claims (15)

1. High content ceramide nanoemulsion with improved transparency, including ceramides, ionic surfactants, polyols and ethanol.
2. The method of claim 1,

   The ceramide nano emulsion is a high content ceramide nano emulsion with improved transparency, characterized in that it further comprises a silicone oil.
3. The method of claim 1,

   100% by weight of the ceramide nano emulsion, 1 ~ 10% by weight of ceramide; 1 to 1.5 weight percent of ionic surfactant; 20 to 40 weight percent polyol; And 1 to 5% by weight of ethanol; high content ceramide nanoemulsion with improved transparency.
4. The method of claim 2,

   The silicone oil is a high content ceramide nanoemulsion with improved transparency, characterized in that contained in 15 to 30% by weight.
5. The method of claim 1,

   The particle size of the emulsion is a high content ceramide nanoemulsion with improved transparency, characterized in that 10 ~ 30 nm.
6. The method of claim 1,

   The ionic surfactant is selected from the group consisting of potassium cesyl phosphate, sodium stearoyl glutamate, glyceryl stearate citrate, distearyl dimonium chloride, β-branched monohexahexadecyl phosphate arginine alone or two or more A high content ceramide nanoemulsion with improved transparency.
7. The method of claim 1,

   The ionic surfactant is potassium cesyl phosphate or sodium stearoyl glutamate high transparency ceramide nanoemulsion with improved transparency.
8. The method of claim 1,

   The polyol is a high content ceramide nanoemulsion with improved transparency, characterized in that selected from the group consisting of glycerin, 1,3-butylene glycol, propylene glycol, and dipropylene glycol alone or two or more.
9. The method of claim 2,

   The silicone oil is dimethicone series or cyclopentasiloxane, characterized in that the improved high content ceramide nanoemulsion of transparency.
10. Cosmetic composition containing the high content ceramide nanoemulsion of any one of Claims 1-9.
11. The method of claim 10,

    The cosmetic composition is a cosmetic composition, characterized in that it further comprises a thickener.
12. The method of claim 10,

    The cosmetic composition is formulated in the form of any one of skin, lotion, cream, serum, essence, powder, foundation, spray, mask pack, sheet pack, sleep pack, wash off pack and peel off pack Composition.
13. In the method for preparing ceramide emulsion,

    i) mixing the oil phase solution in which ceramide is dissolved and the aqueous phase solution in which a surfactant is dissolved to prepare a primary oil dispersion;

    ii) preparing a secondary oil dispersion by adding silicone oil and ethanol to the primary mixed solution;

    iii) emulsifying the secondary mixed solution at high speed to prepare a primary emulsion;

    iv) high pressure emulsifying the primary emulsion to prepare a secondary emulsion;

    In step i), the solvent of the oily solution is a polyol, and the surfactant of the aqueous solution is an ionic surfactant.
14. The method of claim 13,

    The high-speed emulsification of step iii) is a method for producing a ceramide emulsion having improved transparency, characterized in that emulsification at 5000 ~ 10000 rpm for 1 to 20 minutes using a homo mixer.
15. The method of claim 13,

    The high pressure emulsification of step iv) is a 1 to 5 cycle emulsification using a microfluidizer 1 ~ 5 cycle emulsified improved ceramide emulsion production method.

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