TWI709414B - Nano emulsion having a high ceramide content and improved transparency, cosmetic composition containing the same, and preparation method of the same - Google Patents

Abstract

The invention relates to a nano emulsion having a high ceramide content and improved transparency, a cosmetic composition containing the same, and a preparation method of the same. In detail, the nano emulsion having a high ceramide content is prepared by using a ceramide, an ionic surfactant and a polyol formulated at a suitable ratio, and by further adding a silicone oil thereto and performing high pressure emulsification thereon. The invention further relates to a cosmetic composition containing the nano emulsion and a preparation method of the nano emulsion. The nano emulsion is obtained by preparing nanosized emulsion particles having a size of 10 to 30 nm and has a high content of up to 10% by weight of the ceramide, which prevents gelation and improves stability in application of the nano emulsion in cosmetics. Since transparency is improved, the ceramide whose use was limited to emulsion type cosmetics can be widely applied in transparent lotion type or cream type cosmetics.

Description

Nanoemulsion with improved transparency and high content of ceramide Liquid, cosmetic composition including the same and preparation method thereof

The present invention relates to a high-content ceramide nanoemulsion with improved transparency, a cosmetic composition containing the same, and a preparation method thereof. In more detail, it relates to a method for comparing ceramide and ion with an appropriate blending ratio. A high-content ceramide nanoemulsion prepared by high-pressure emulsification of a surfactant, polyol and silicone oil, a cosmetic composition containing the same, and a preparation method thereof.

The surface of human skin includes keratinocytes degenerated from mature keratinocytes differentiated from the basal layer. These keratinocytes are combined by the double-stranded layered structure of ceramide, which is abundant in the stratum corneum, so as to maintain smooth and elastic skin.

Ceramides are poorly soluble, so they need to be prepared in the form of microparticles to provide them in a large amount in cosmetic formulations. However, this leads to the stability of the formulation Decrease, and gelation (Gelation) occurs. If the particle size is smaller, the surface energy between the particles is larger and the effect of gravity is larger. The interaction between the ceramides is increased and cannot be completely dispersed on the oil, so the gelation occurs due to the bond between the ceramides which is slightly in the water phase.

In order to solve the above-mentioned problems, the technique of stabilizing ceramide in the following way is applied: preparing granules (particles) with ceramide, stearic acid, cholesterol, etc., when preparing an emulsion, adding the aforementioned particles (particles) in the final step . That is, a method of achieving stability in a way that ceramide eliminates fluidity is used. The above-mentioned ceramide is a hard solid prepared by the following steps: firstly, particles stabilizing the ceramide are prepared externally; then, the above-mentioned particles are dispersed into an emulsion. Korean Patent Application No. 2008-0072355 discloses a related technology using ceramide on a nucleating agent of a solid shell.

However, this method will also reduce the content of ceramide that can be actually used in cosmetics due to the large amount of encapsulating agent used in the encapsulation process of ceramide. In addition, in terms of the feeling of use, the encapsulating agent of sugar or polymer, which is an essential component of the cosmetic composition, has the disadvantage of destroying the inherent feeling of use of the cosmetic.

The prior art documents include Korean Registered Patent Publication No. 0837558 "Emulsion composition including dual-stable ceramide nanocapsules, its preparation method, and skin cosmetic composition using the same."

For people with dry skin, Ceramide, which prevents moisture loss in skin tissues and exerts a barrier function of foreign bodies on the skin surface, is easy to crystallize in cosmetic formulations due to its structural properties, and therefore contains a higher content of In this case, layer separation or separation phenomenon occurs.

Therefore, the current ceramide contained in cosmetic formulations is usually about 2% by weight. Moreover, the transparency of this cosmetic formulation is significantly reduced and turbidity also occurs. Therefore, it cannot be applied to transparent formulations of lotions. At present, it is only limited It can be used to prepare low viscosity emulsions. In addition, when left unused for a long time, the stability of the dosage form decreases and gelation occurs.

Therefore, the purpose of the present invention is to prepare a ceramide nanoemulsion that contains ceramide in a high content and maintains transparency in a dosage form with excellent stability.

The present invention is proposed in order to achieve the above-mentioned object, and provides a high-content ceramide nanoemulsion containing ceramide, an ionic surfactant, a polyol, and ethanol with improved transparency. The aforementioned nanoemulsion may further include silicone oil. At this time, the above composition preferably contains 1% to 10% by weight of Ceramide, 1% to 1.5% by weight of ionic surfactant, 20% to 40% by weight of polyol, 1% by weight To 5% by weight of ethanol and 15% to 30% by weight of silicone oil, the particle size of the high-content ceramide nanoemulsion prepared in this way is preferably 10nm to 30nm.

The invention provides a preparation of ceramide emulsion with improved transparency The preparation method is characterized in that it comprises the following steps: i) mixing the oil phase solution in which ceramide is dissolved and the water phase solution in which the surfactant is dissolved to prepare a primary oil dispersion; ii) adding to the above primary oil dispersion The step of preparing a secondary oil dispersion with silicone oil and ethanol; iii) the step of emulsifying the above-mentioned secondary oil dispersion at a high speed to prepare a primary emulsion; and iv) the step of emulsifying the above-mentioned primary emulsion at high pressure to prepare a secondary emulsion And in step i) above, the solvent of the oil phase solution is a polyol, and the surfactant of the water phase solution is an ionic surfactant. At this time, the high-speed emulsification in step iii) can be emulsified at 5000 rpm to 10000 rpm for 1 minute to 20 minutes using a homomixer, and the high-pressure emulsification in step iv) can be emulsified at 12000 psi to 18000 psi using a Microfluidizer. Perform emulsification from 1 cycle to 5 cycles.

The high-content ceramide nanoemulsion with improved transparency according to the present invention can contain ceramide at a high content of up to 10% by weight by preparing 10nm to 30nm nano-sized emulsified particles, which can prevent coagulation. Gelation to improve stability when applied to cosmetics. In addition, since the transparency has been improved, ceramide, which was previously restrictedly used in emulsion cosmetics, can be widely used in transparent lotions or creams.

s10, s20, s30, s40: steps

Figure 1 is a comparison of the high-content ceramide nanoemulsion of an embodiment of the present invention The transparency of the image is relatively compared.

2 is a flow chart of the preparation method of the high-content ceramide nanoemulsion with improved transparency of the present invention.

The present invention relates to a high-content ceramide nanoemulsion with improved transparency, a cosmetic composition containing the same, and a preparation method thereof. More specifically, it relates to a ceramide, ionic surfactant, and Polyol is prepared by adding silicone oil according to an appropriate mixing ratio and high-pressure emulsification to prepare a high-content ceramide nanoemulsion, 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 in 1% to 10% by weight relative to the total weight of the emulsion. In the case of less than 1% by weight, the effect is very small when applied to cosmetic formulations, and in the case of more than 10% by weight, gelation is initiated and the stability of the dosage form decreases.

The above-mentioned ionic surfactant can be used alone selected from the group consisting of Potassium Cetyl Phosphate, Sodium Stearoyl Glutamate, Glyceryl Stearate Citrate, Distearyl Dimonium Chloride (Distearyl Dimonium Chloride), β-branched monohexadecyl (Hexadecyl) arginine phosphate group consisting of one, or two or more selected and used, more preferably Potassium Cetyl Phosphate or sodium stearyl glutamate can be used (Sodium Stearoyl Glutamate).

It is preferable that such an ionic surfactant contains 1 weight% to 1.5 weight% with respect to the whole weight of an emulsion. When it is less than 1% by weight, the stabilizing effect is very small and gelation occurs when applied to cosmetic formulations. When it is more than 1.5% by weight, it will cause skin irritation, so it is preferably within the above range.地调。 Ground adjustment.

The above polyols are used to adjust the refractive index of the dosage form to improve transparency and moisturizing power. It can be used alone selected from glycerine (Glycerine), 1,3-butylene glycol (1,3-Butylene Glycol: BG), and propylene glycol (Propylene Glycol: PG) and dipropylene glycol (Dipropylene Glycol: DPG) constitute one, or select two or more of them to be used. Preferably, the polyol is contained in the range of 20% to 40% by weight relative to the total weight of the emulsion. When it is less than 20% by weight, the solubilization of the high content of ceramide is limited, and when it is more than 40% by weight, there is a problem that the feeling of use of the skin decreases.

The above silicone oil is used to replace the previous wax that can form a layered structure to adjust the feeling of use and turbidity. Dimethicone and Cyclopentasiloxane with similar refractive index and wax can be used. )Wait. It is preferable to contain such silicone oil in the range of 15% to 30% by weight relative to the total weight of the emulsion. When it is less than 15% by weight, the transparency decreases, and when it is more than 30% by weight, it is used The problem that the content of the surfactant for emulsifying silicone oil exceeds the appropriate value.

The particle size of the high-content ceramide nanoemulsion of the present invention is better It is 10nm to 30nm. The reason is that when it is less than 10 nm, it is difficult to perform the preparation process, and when it is greater than 30 nm, the transparency decreases, gelation is initiated, and the stability of the dosage form decreases.

On the other hand, a high-content ceramide nanoemulsion with improved transparency can be used as a cosmetic composition by diluting or adding a thickening agent. The above cosmetic composition can be used as a lotion, lotion, cream, and essence. Any form of liquid, essence, powder, foundation, spray, mask, patch mask, sleeping mask, wash mask and tear-off mask can be formulated.

As the tackifier added as the above cosmetic composition, a known tackifier can be used, and it can be used alone selected from Dextrin Palmitate and Dextrin Palmitate/Ethylhexanoate. , Cyclopentasiloxane and PEG/PPG-19/19 Dimethicone (PEG/PPG-19/19 Dimethicone), Polysilicone-11 (Polysilicone-11), Dimethicone Dimethicone Crosspolymer, Quaternium-18 Magnesium Lithium Silicate (Quaternium-18 Hectorite), Stearalkonium Hectorite and Disteardimonium Hectorite ) Is used in one or two or more groups.

Furthermore, the present invention provides a method for preparing a ceramide emulsion with improved transparency. Fig. 2 is a flow chart of a preparation method of ceramide emulsion with improved transparency. Referring to Figure 2, the preparation method of the ceramide emulsion with improved transparency includes: i) mixing the oil phase solution in which ceramide is dissolved with the dissolved boundary The step of preparing a primary oil dispersion from the aqueous phase solution of the surfactant (step s10); ii) the step of preparing a secondary oil dispersion by adding silicone oil and ethanol to the above-mentioned primary oil dispersion (step s20); iii) The step of emulsifying the above-mentioned secondary oil dispersion at high speed to prepare a primary emulsion (step s30); and iv) the step of emulsifying the above-mentioned primary emulsion at high pressure to prepare a secondary emulsion (step s40); and in the above step s10 , The solvent of the oil phase solution is a polyol, and the surfactant of the water phase solution is an ionic surfactant.

At this time, the high-speed emulsification in the above step s30 can be emulsified with a homomixer at 5000rpm to 10000rpm for 1 minute to 20 minutes, and the high-pressure emulsification in the step s40 can be carried out from 1 to 5 cycles with a microjet homogenizer at 12000psi to 18000psi Of emulsification.

Preparation of nano emulsion with high content of ceramide according to the composition ratio

Ceramide-102 (Hydroxypropyl Bislauramide MEA (Hydroxypropyl Bislauramide MEA)) and Ceramide-104 (Hydroxypropyl Bispalmitamide MEA) are used as ceramide, and Eumulgin SG (hard Sodium Stearoyl Glutamate (Sodium Stearoyl Glutamate) is used as an ionic surfactant, Glycerine is used as a polyol, and Dimethicone is used as a silicone oil, according to the following table 1 The composition ratio of Example 1 to Example 6 was used to prepare nanoemulsion.

The preparation process of the nanoemulsion of the following Examples 1 to 6 was implemented as described below.

Step 1), after adding Ceramide-102 or Ceramide-104 to glycerin, the temperature is raised to 80°C while stirring to perform oil dispersion.

Step 2), add Eumulgin SG to the water, while heating up to 80°C, while dispersing the oil.

Step 3), while homogenously stirring the mixture of the above step 1), slowly add the mixture of the above step 2).

In step 4), after confirming the appearance of the mixture of the above step 3), dimethicone and ethanol were additionally added, and emulsification was performed once at 8500 rpm for 5 minutes.

Step 5), using a micro-jet homogenizer to emulsify the mixture obtained by performing the above-mentioned primary emulsification at 15000 psi for 3 cycles (for 10 minutes on a 500 ml basis).

Various tests of nano emulsion with high content of ceramide

The following Table 2 is the result of obtaining the prepared samples of the aforementioned Examples 1 to 6 and evaluating the items such as particle size, stability, and turbidity. Please refer to Figure 1, which compares Example 1, Example 5 and Example 6 Relative transparency. The 4-week stability test is to evaluate the stability according to whether crystallization or layer separation occurs after being placed at a temperature of 45°C for 4 weeks. The turbidity is selected from the samples of Examples 1 to 6 above. Example 1, Example 2, Example 5, and Example 6 in the range of 10 nm to 30 nm are used to measure the scattering degree formed by suspended particles. The Nephelometry Turbidity Unit (Nephelometry Turbidity Unit: NTU) is the result expressed as a benchmark.

According to the test results in Table 2 above, among the two ceramides, compared to Ceramide-104, Ceramide-102 forms smaller nano-emulsion particles at the same composition ratio. Furthermore, comparing Example 1 and Example 2, Example 4 to Example 6 respectively, the increase in ethanol content resulted in the formation of fine particles, but according to the stability test results of Example 6, it was confirmed that layer separation occurred Therefore, it was confirmed that higher stability is not achieved as long as the particle size is small.

Preparation of high-content ceramide nanoemulsion based on surfactants

Hereinafter, according to Examples 7 to 10 in Table 3 below, a nanoemulsion was prepared by changing the type of surfactant. Use Ceramide-104 as Ceramide, add TA-100 (Distearyl Dimonium Chloride), Amphisol K (Potassium Cetyl Phosphate)), Dracorin CE (Glyceryl Stearate Citrate), Phopure LC (β-branched monohexadecyl arginine phosphate) as surfactants.

The preparation process of the nanoemulsions of Examples 7 to 10 in Table 3 below is the same as the preparation method of the nanoemulsions of Examples 1 to 6 described above, so the detailed description is omitted.

Various tests of nano emulsion with high content of ceramide

The test methods of the nanoemulsions of Examples 7 to 10 in Table 4 below are the same as the test methods of the nanoemulsions of Examples 1 to 6 described above, so detailed descriptions are omitted. With further reference to FIG. 1, compared with Example 10, the relative transparency of the prepared Example 1, Example 5 and Example 6 can be seen.

According to the test results in Table 4 above, it can be seen that in the case of TA-100 as a cationic surfactant (Example 7), the particle size exceeds the nanometer range, which is better for the relatively large Dracorin CE (Example 9). In this case, a larger particle size is formed. In addition, in the case of Amphisol K (Example 8), the particle size and stability were similar to those of Eumulgin SG (Example 1 to Example 6).

Claims (11)

A high-content nanoemulsion of ceramide with improved transparency, comprising ceramide, ionic surfactant, polyol, ethanol and silicone oil, wherein the nanoemulsion is 100% by weight. The nanoemulsion comprises 1% to 10% by weight of the ceramide, 1% to 1.5% by weight of the ionic surfactant, 20% to 40% by weight of the polyol, 1% by weight % To 5% by weight of the ethanol and 15% to 30% by weight of the silicone oil, and the particle size of the nanoemulsion is 10 nm to 30 nm. As described in item 1 of the scope of the patent application, the transparency of the high-content nanoemulsion of ceramide is improved, wherein the ionic surfactant is selected from the group consisting of potassium cetyl phosphate, sodium stearyl glutamate, One or two or more of the group consisting of glyceryl stearate citrate, distearyl dimethyl ammonium chloride, and β-branched monohexadecyl arginine phosphate. The high-content nanoemulsion of ceramide with improved transparency as described in item 1 of the scope of patent application, wherein the ionic surfactant is potassium cetyl phosphate or sodium stearyl glutamate. The high-content ceramide nanoemulsion with improved transparency as described in item 1 of the scope of patent application, wherein the polyol is selected from the group consisting of glycerin, 1,3-butanediol, propylene glycol and dipropylene glycol One or two or more of them. The high-content ceramide nanoemulsion with improved transparency as described in item 1 of the scope of the patent application, wherein the silicone oil is dimethicone or cyclopentasiloxane. A cosmetic composition comprising a nanoemulsion with a high content of ceramide with improved transparency as described in any one of items 1 to 5 of the scope of patent application. The cosmetic composition described in item 6 of the scope of patent application further includes a thickening agent. Such as the cosmetic composition described in item 6 of the scope of patent application, which is based on lotion, lotion, cream, essence, essence, powder, foundation, spray, facial mask, patch mask, sleeping mask, and washing facial mask And take-off mask in any form. A method for preparing a high-content ceramide nanoemulsion with improved transparency as described in item 1 of the scope of the patent application, which comprises the following steps: i) mixing the oil phase solution in which ceramide is dissolved with the dissolved interfacial activity The step of preparing a primary oil dispersion liquid from the aqueous phase solution of the agent; ii) the step of adding silicone oil and ethanol to the primary oil dispersion liquid to prepare a secondary oil dispersion liquid; iii) the secondary oil dispersion liquid Emulsifying to prepare a primary emulsion; and iv) emulsifying the above-mentioned primary emulsion under high pressure to prepare a secondary emulsion; and in the step i), the solvent of the oil phase solution is a polyol, and The surfactant of the aqueous solution is an ionic surfactant. Nerves with improved transparency as described in item 9 of the scope of patent application The method for preparing an amide emulsion, wherein the high-speed emulsification in step iii) is emulsification using a homomixer at 5000 rpm to 10000 rpm for 1 to 20 minutes. The method for preparing a ceramide emulsion with improved transparency as described in item 9 of the scope of patent application, wherein the high-pressure emulsification in step iv) is performed by 1 to 5 cycles of emulsification at 12,000 psi to 18,000 psi using a microjet homogenizer.

Images