KR20170107128A - Manufacturing method of multi-lamellar structured transparent liquid crystal composition - Google Patents

Abstract

The present invention relates to a method for manufacturing a multi-layer transparent liquid crystal composition, which comprises the following steps: mixing a composition comprising lecithin and mannosylerythritol lipid (MEL); heating and dissolving the composition to manufacture an oil phase part; dissolving polyol and a water-soluble active ingredient in water to manufacture a water phase part; mixing and stirring the water phase part with a homogenizer to manufacture a primary emulsion; adding the primary emulsion into a high-pressure emulsifier and emulsifying the primary emulsion with high pressure for refinement; cooling and filtering the refined composition. According to the present invention, the transparent multilayer liquid crystal composition manufactured by the manufacturing method has a multi-layered structure to increase the amount of usable components contained in the structure, and the multi-layered structure is not easily broken and stable to maintain the multi-layered structure. In addition, the liquid crystal composition manufactured thereby has very little irritation to the skin and has a soft feeling and an excellent moisture-retaining ability.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a transparent multi-layer liquid crystal composition,

More particularly, the present invention relates to a method for producing a transparent multi-layer liquid crystal composition, which comprises mixing a composition containing lecithin and Mannosylerythritol Lipid (MEL), heating and dissolving the mixture to prepare an oily portion, And a water-soluble active ingredient are dissolved in water to prepare an aqueous phase. The primary phase and the aqueous phase are mixed and stirred with a homogenizer to prepare a primary emulsion. The primary emulsion is introduced into a high-pressure emulsifier and emulsified by high- And filtering the liquid crystal composition.

The stratum corneum, which is located at the outermost part of the skin and is in direct contact with the outside, plays an important role in skin barrier function. The stratum corneum consists of several layers of flat keratinocytes to prevent the loss of water and electrolytes inside the skin and to function as a barrier to protect the body from the external environment. (J. Invest. Dermatol., 69: 535-546, 1977). In addition, the intercellular quality is approximately 50% for ceramide, 20-25% for cholesterol, 20-25% for free fatty acid, 10% for cholesterol ester, 1 to 2% Cholesterol sulfate and small amounts of phospholipids.

In order to enhance the skin barrier function by using the characteristics of intercellular quality, the liquid crystal cosmetics which contains the intercellular lipid components such as ceramides and cholesterol and simulates the multi-lamellar structure of the stratum corneum The same formulations were developed. However, since ceramides and cholesterol are hardly soluble, they are difficult to be contained in the formulations stably and are difficult to be contained in the emulsified formulations in large quantities because of problems such as precipitation. Especially, they are difficult to use for solubilization formulations of skins and toners.

To solve this problem, the researchers fabricated a liposome-like structure using self-assembly of phospholipids and conducted studies to effectively transfer physiologically active substances into the skin. Phospholipids have the property of increasing the permeability of physiologically active substances by increasing the fluidity of the horny layer lipids (Biochem. Biophys. Acta, 1237 (1995): 176-182). However, the liposome has a double layer bilayer structure, so that the amount of the usable substance contained in the liposome is relatively small, and it is easily broken due to the structural weakness of the double layer, so that the internal usable substance can be precipitated.

Accordingly, the inventors of the present invention have found that, in order to prepare a liquid crystal composition which can stably contain a large amount of intercellular quality of existing intercellular lipids rather than existing liposomes due to its multi-layered structure, the present inventors have found that mannosylerythritol lipid (MEL) To prepare multilayer liquid crystal compositions. MEL is a natural biosurfactant made by yeast, a glycolipid composed of mannose, sugar alcohols and fatty acids. Since MEL is an amphipathic structure with two properties of hydrophobicity derived from the properties of lipids and hydrophilic derived from the properties of sugars, it has a structure similar to that of ceramides forming human membranes. Due to this property, MEL can form a lamellar structure and can act as an effective ingredient for skin roughness (Japanese Patent PCT / JP2006 / 323239).

In order to miniaturize and clarify the intercellular components as described above, the present inventors manufactured a liquid crystal composition using a high pressure homogenizer. With the general solubilization method, hydrophobic components such as ceramides, cholesterol, and phospholipids can be solubilized only in the core space of the solubilizer, so that the solubilization space is relatively inadequate. That is, by using a general solubilization method, such poorly soluble components are difficult to be solubilized and it is very difficult to keep the composition stable. Therefore, methods for finely dispersing emulsified particles using a high-pressure emulsifier and stabilizing poorly soluble materials are widely used in the cosmetics industry.

Thus, the present inventors used MEL and lecithin to simulate the structure of the stratum corneum multilayer structure, stabilize ceramide and cholesterol, which are intercellular lipid components that can help the skin barrier function of the human body, To develop a multi-layer liquid crystal composition.

As a result of intensive research efforts by the present inventors in order to overcome the problems of the prior art, the present inventors have found that a composition comprising lecithin and Mannosylerythritol Lipid (MEL) is mixed, heated and dissolved to prepare an oily portion, And a water-soluble active ingredient are dissolved in water to prepare an aqueous phase. The primary phase and the aqueous phase are mixed and stirred with a homogenizer to prepare a primary emulsion. The primary emulsion is introduced into a high-pressure emulsifier and emulsified by high- And filtering the liquid crystal composition to form a transparent multilayer liquid crystal composition. In the case of the transparent multilayer liquid crystal composition prepared by the present production method, since the multilayer structure is formed, the amount of the usable component contained in the structure can be increased, and since the multilayer structure is not easily broken and stable, Can be maintained. Further, it was confirmed that the liquid crystal composition thus produced exhibits a soft feeling and a good moisture-retaining ability with very little skin irritation, and thus completed the present invention.

JP 2006-323239 A

Accordingly, it is a main object of the present invention to provide a transparent multi-layered multi-layer liquid crystal display device which can increase the amount of the usable component contained in the liquid crystal of the multilayer structure and stably maintain the usable component, Layer liquid crystal composition of the present invention.

It is another object of the present invention to provide a transparent multilayer liquid crystal composition using the transparent multilayer liquid crystal composition.

It is another object of the present invention to provide a cosmetic composition for skin moisturizing using the transparent multi-layer liquid crystal composition.

According to one aspect of the present invention, the present invention provides a method for producing a transparent multilayer liquid crystal composition.

(a) mixing a composition comprising lecithin and Mannosylerythritol Lipid (MEL), followed by heating and dissolving to prepare an oily portion;

(b) dissolving the polyol and the water-soluble potentiation component in water to prepare a water-containing part;

(c) mixing the oil phase of step (a) and the water phase of step (b) with a homogenizer to prepare a first emulsion;

(d) charging the primary emulsion of step (c) into a high-pressure emulsifier and emulsifying it by high-pressure emulsification; And

(d) cooling and filtering the composition of step (d).

The term " transparent multi-layer liquid crystal composition " of the present invention means that the outer appearance is transparent and the oil layer and the water phase layer are formed in a stacked structure of 3 to 10 layers in order.

The transparency of the outer surface means that the liquid is clear so as to be shrunk to the inside, and the degree of transparency can be measured depending on how clearly the letters behind the container containing the liquid are clearly visible, as in the present invention. Further, the degree of transparency can be measured according to the size of the liquid crystal composition. The transparent multi-layer liquid crystal composition of the present invention has relatively small size and high transparency by using lecithin and MEL.

According to the experimental example of the present invention, in the case of Comparative Example 1 which does not contain lecithin and MEL, Example 1 which contains only lecithin, and Example 2 which contains only MEL, the particle size 200-500 nm and an opaque or translucent emulsion was prepared, but it was confirmed that a highly transparent liquid crystal composition in the range of 100-120 nm was prepared in Example 3 including both lecithin and MEL (see Experimental Example 1-2) ).

According to the experimental example of the present invention, the structure of Example 3 was observed by a freezing scanning electron microscope. As a result, it was confirmed that the multilayer structure in which several layers were stacked was actually formed (see Experimental Example 3).

In the present invention, the water-soluble potent component of step (b) may be any water-soluble active ingredient as long as it can be dissolved in water to form a water-soluble part, for example, a wrinkle-reducing functional ingredient, a whitening functional ingredient and a natural extract.

Examples of the wrinkle-improving functional raw material include adenosine, and whitening functional raw materials include arbutin and niacinamide. The natural extracts include natural extracts of plants, animals, or minerals extracted from aloe, green tea, citrus fruits, and gingko leaves, and the above water-soluble potentiation components are not limited to the above-mentioned kinds.

In the present invention, the oily phase of the step (a) may further comprise ceramide or a derivative thereof, cholesterol, a nonionic surfactant and a polyol, and the oily components may include caprylic / capryl triglyceride, squalane, Free, olive oil, sunflower oil, macadamia nut oil, octyldodecanol, and the like.

The non-ionic surfactant is selected from the group consisting of PEG-40 hydrogenated castor oil, octyldodeces, polysorbate 60, phage-40 stearate, ceteareth-20, phage-20 glyceryl isostearate, polyglyceryl -3 methyl glucose distearate, polyglyceryl-10 stearate, and cholester, and the content thereof is preferably 0.1 to 3% by weight.

The polyol used in the present invention may also be a polyol such as glycerin, diglycerin, propylene glycol, dipropylene glycol, 1,3-butyleneglycol, ethylhexyl glycerin, polyglycerin, caprylyl glycol, And 1,2-hexanediol, and the content thereof is preferably 5 to 60% by weight.

In the present invention, the oily portion of the step (a) is contained in an amount of 5 to 15% by weight based on the total weight of the composition. If the amount of the oil phase in the above range is large, the emulsified particles become large and the viscosity becomes high due to the ratio of the inner phase to the outer phase, which may make it difficult to carry out the high-pressure emulsification.

In the present invention, the water phase of step (b) comprises 75 to 95% by weight based on the total weight of the composition. If the amount of the water phase is less than the above range, the emulsified particles become large, and the viscosity becomes high due to the ratio between the inner and outer surfaces, thereby making it difficult to carry out high-pressure emulsification.

In the present invention, the primary emulsion in the step (c) has a particle size of 200 to 500 nm. If the particle size of the primary emulsion is too large beyond the above range, even if high-pressure emulsification is performed, it may be difficult to obtain a result of a transparent level.

In the present invention, the high-pressure emulsification of the step (d) is characterized in that the emulsion is passed 1 to 5 times at a pressure of 500 to 1500 bar. Since the size of the particles does not decrease as the pressure of the high-pressure emulsifier is high and the number of times of communication is high, the ratio of lecithin and MEL, the pressure of the high-pressure emulsifier and the number of times of passage of the high-pressure emulsifier should be appropriately set, It is preferable to emulsify at a high pressure in the same range as described above.

According to another aspect of the present invention, there is provided a transparent multi-layer liquid crystal composition produced by the above method.

In the present invention, the multilayer transparent liquid crystal composition is formed to have a structure of 3 to 10 layers and has a transparent appearance.

The term " transparent multi-layer liquid crystal composition " of the present invention means that the outer appearance is transparent and the oil layer and the water phase layer are formed in a stacked structure of 3 to 10 layers in order.

According to another aspect of the present invention, there is provided a skin moisturizing cosmetic composition containing a transparent multilayer liquid crystal composition.

According to the experimental example of the present invention, the skin moisturizing power of the cosmetic composition containing the transparent multi-layer liquid crystal composition prepared by the production method of the present invention was confirmed, and it was confirmed that the skin moisturizing power was superior to the non-mordant group. From these results, it can be seen that the transparent multi-layer liquid crystal composition of the present invention is not only suitable for use in formulations requiring transparency because the outer appearance is transparent, but also is excellent in moisture retention, making it suitable as a cosmetic composition (see Experimental Example 4 ).

In the present invention, the cosmetic composition may be at least one selected from the group consisting of a skin lotion, a skin softener, a skin toner, an astringent, a lotion, a milk lotion, a moisturizer, a nutrient lotion, a massage cream, a nutritional cream, a moisturizer cream, a hand cream, And a single formulation selected from the group consisting of a pack, a soap, a cleansing foam, a cleansing lotion, a cleansing cream, a body lotion and a body cleanser.

In addition, the cosmetic composition comprising the multilayered transparent liquid crystal composition prepared in the present invention is not particularly limited in its formulation. However, considering the appearance of transparent and advantages in use, skin, toner, solution, suspension, emulsion, paste , Gels, creams, lotions, powders, powder foundations, emulsion foundation, sunscreens, packs, mask sheets, lipsticks, mist and the like.

Hereinafter, the present invention will be described more specifically.

In order for the transparent liquid crystal composition of the present invention to form a multilayer structure, phospholipids and MEL's role is important. Lecithin, which is one of phospholipids, can be self-emulsified when mixed with a sufficient aqueous medium to form bilayer or multilayer lamellar structures have. The lamellar structure of the multilayered lamellar structure has a lamellar structure in which a lamellar structure of a valve structure composed of phospholipids is stacked in order of an oil layer and an aqueous phase layer. In addition to lecithin, the formation of a lamellar structure was facilitated by using a MEL having a structure similar to that of a human ceramide.

In the present invention, when preparing a transparent multi-layer liquid crystal composition, a high-pressure emulsification method was used to miniaturize the particle size to about 100 nm. The high-pressure emulsification method is an emulsification method using a high-pressure homogenizer, and generally refers to a process in which a primary emulsified emulsion with a homogenizer is passed through a high-pressure emulsifier to perform secondary emulsification. The process of atomization of oil particles at high pressure is 500 ~ 2,000 bar. The process of atomization of high-pressure fluid passes through a small gap at the valve at high speed, and cavitation, turbulence and shear force It is cleaved into fine particles and the levitation force is reduced, making the components of the liquid completely homogeneous.

The preferred pressure in the present invention is suitably 500 to 1,500 bar for passing the emulsion one or more times. Here, the most preferable size distribution of the emulsified particles is that the mean particle size of the first emulsified particles with a general homogenizer is about 200 to 500 nm, and when the first emulsification with a general homo mixer is followed by a second emulsification with a high pressure emulsifier, Is reduced to 50 to 150 nm to form a transparent to semi-transparent state.

INDUSTRIAL APPLICABILITY As described above, the multilayered transparent liquid crystal composition prepared by the method of the present invention has an advantage that the active ingredient can be contained in a greater amount through the multilayer structure simulating the skin lipid structure and the stability can be improved I have. Further, since the outer appearance is transparent, it is not only suitable for use in formulations requiring transparency, but also has a very soft feeling and a good moisture-retaining ability with little irritation to the skin.

Fig. 1 is an external view of Comparative Example 1 and Examples 1 to 3 produced according to the present invention.
2 is a graph of particle size distribution measured by Dynamic Light Scattering (DLS) of Example 3 prepared according to the present invention.
3 is an image of a Cryo-Transmission Electron Microscopy (Cryo-TEM) of Example 3 prepared according to the present invention.

Hereinafter, the present invention will be described in more detail with reference to Examples. These embodiments are only for illustrating the present invention, and thus the scope of the present invention is not construed as being limited by these embodiments.

Example 1: Preparation of Comparative Examples and Examples

The multi-layered liquid crystal composition of the present invention is characterized by including MEL, lecithin and polyol in order to solubilize poorly soluble materials such as ceramides and cholesterol.

Here, the MEL may be represented by the following formula (1).

[Chemical Formula 1]

The MEL may be represented by Candida bombicola / glucose / methyl rapeseedate ferment, olea europaea (olive) fruit oil.

Experiments were conducted with the compositions shown in the following Table 1 in order to prepare multilayer liquid crystal compositions having an apparently transparent appearance stabilizing the intercellular quality of the present invention. At this time, the A phase was dissolved by heating at 80 to 100 ° C, and the mixture was put into a phase B heated to 70 to 90 ° C and stirred homogenously at 5,000 rpm for 5 minutes using a homogenizer to homogeneously emulsify. In this way, the composition in which the primary emulsification proceeded was introduced into the high-pressure emulsifier, and the high-pressure emulsification was repeated three times at a pressure of 1,000 bar. The high pressure emulsified composition was cooled to room temperature, filtered and stored.

ingredient Comparative Example 1 Example 1 Example 2 Example 3 A Ceramide 0.1 0.1 0.1 0.1 cholesterol 0.1 0.1 0.1 0.1 lecithin 0 One 0 One Erythritol lipid 0 0 One One PIGGY-40 Hydrogenated Castor Oil One One One One Polyol 5 5 5 5 B Polyol 40 40 40 40 additive q.s. q.s. q.s. q.s. Distilled water to 100 to 100 to 100 to 100

It was confirmed whether or not the composition prepared in Comparative Example 1 and Examples 1 to 3 was made of a transparent or opaque milky white composition after high-pressure emulsification. The appearance of the composition was observed in Table 2, same. In Table 2, an opaque formulation is indicated as X, a translucent formulation as?, And a transparent formulation as?.

Composition Exterior Comparative Example 1 X Example 1 △ Example 2 △ Example 3 ○

As shown in Table 2 and FIG. 1, when the lecithin and the MEL were not included, an opaque appearance formulation was prepared, and when the lecithin or MEL was not included, a translucent formulation was prepared. The semitransparent appearance is obtained because the particle size is greater than 100 nm, and ceramide and cholesterol are stabilized by lecithin or MEL, but this formulation is disadvantageous for use in formulations requiring transparency, such as toner and skin . However, when lecithin and MEL are contained simultaneously as in Example 3, ceramides and cholesterol are stably present in particles having a particle size of about 100 nm, so transparency can be maintained. Therefore, when the transparent cosmetic preparation is prepared, It is possible to effectively use the composition without any limitation on the amount of the composition used.

Experimental Example 2: Measurement of Particle Size of Multilayer Transparent Liquid Crystal Composition

The particle size distribution of the multi-layered transparent liquid crystal composition of the present invention was measured using Dynamic Light Scattering (DLS). As a result, as shown in FIG. 2, the particle distribution of Example 3 is about 113 nm in terms of intensity.

In addition, the results of measuring the sizes of the respective examples were measured at 257.6 nm for Comparative Example 1, 187.6 nm for Example 1, and 162.2 nm for Example 2, respectively.

Experimental Example 3: Structural observation of transparent liquid crystal composition of multiple layers

The structure of the multilayered transparent liquid crystal composition of the present invention was observed using a Cryo-Transmission Electron Microscopy (Cryo-TEM). As a result, as shown in FIG. 3, it can be seen that Example 3 uniformly forms multi-layered particles of about 100 nm. As a result, it can be confirmed that the particle size similar to the result of the particle size analysis using DLS of Experimental Example 2 was also shown.

Preparation Example 1: Cosmetic preparation using a multilayer transparent liquid crystal composition

In Production Example 1, as shown in Table 3 below, the multilayered transparent liquid crystal composition containing ceramide and cholesterol prepared in Example 3 was added to purified water to finally produce a cosmetic containing ceramide and cholesterol stably. The preparation of the present cosmetics is one of the examples using a multilayered transparent liquid crystal composition and does not limit the selection and manufacturing method of the formulations in applying the multilayered transparent liquid crystal composition to cosmetics.

ingredient Weight Percentage (%) Multi-layer transparent liquid crystal composition 5 glycerin 8 Octyldodec-16 0.3 ethanol 2 incense q.s. antiseptic q.s. Purified water to 100

As a result of the particle size distribution measurement using DLS, 71 nm was confirmed and the zeta potential was found to be stable at 78.5 mV.

Experimental Example 4: Moisture resistance test of transparent liquid crystal composition of multiple layers

Five healthy female subjects were made a toner containing 5% of a transparent liquid crystal composition in a multilayer. After 2 hours of application, 4 hours after application, and 8 hours after application, a toner containing 5% Were tested.

Instrumental analysis using a corneometer analysis showed that the toners containing the multilayered transparent liquid crystal composition were 18.4%, 14.3% and 8.4% higher after 2 hours, 4 hours and 8 hours, respectively. Therefore, it was found that the multi-layered transparent liquid crystal composition has a moisturizing effect due to the intercellular components contained therein.

The cosmetic composition comprising the multilayered transparent liquid crystal composition is not particularly limited in its formulation, but may be in the form of a skin, a toner, a solution, a suspension, an emulsion, a paste, a gel, a cream, , Powder, powder foundation, emulsion foundation, sunscreen, pack, mask sheet, lipstick, mist, and the like.

Claims (10)

Method of preparing transparent multi-layer liquid crystal composition:
(a) mixing a composition comprising lecithin and Mannosylerythritol Lipid (MEL), followed by heating and dissolving to prepare an oily portion;
(b) dissolving the polyol and the water-soluble potentiation component in water to prepare a water-containing part;
(c) mixing the oil phase of step (a) and the water phase of step (b) with a homogenizer to prepare a first emulsion;
(d) charging the primary emulsion of step (c) into a high-pressure emulsifier and emulsifying it by high-pressure emulsification; And
(d) cooling and filtering the composition of step (d).
The method of claim 1, wherein the oily phase of step (a) further comprises a ceramide or derivative thereof, cholesterol, a nonionic surfactant, and a polyol.
The method of claim 1, wherein the oily phase of step (a) comprises 5 to 15 wt% of the total weight of the composition.
The process for preparing a transparent multi-layer liquid crystal composition according to claim 1, wherein the step (b) comprises 75 to 95% by weight based on the total weight of the composition.
The method according to claim 1, wherein the primary emulsion in the step (c) has a particle size of 200 to 300 nm. a
The method of claim 1, wherein the high-pressure emulsion is passed through the emulsion at a pressure of 500 to 1500 bar 1 to 5 times.
A transparent multi-layer liquid crystal composition produced by the manufacturing method of any one of claims 1 to 6.
The transparent multi-layer liquid crystal composition according to claim 7, wherein the multi-layer transparent liquid crystal composition has a structure of 3 to 10 layers and has a transparent appearance.
A cosmetic composition for moisturizing skin containing the transparent multilayer liquid crystal composition of claim 7.
The cosmetic composition according to claim 9, wherein the cosmetic composition is at least one selected from the group consisting of a skin lotion, a skin softener, a skin toner, an astringent, a lotion, a milk lotion, a moisturizing lotion, a nutrition lotion, a massage cream, a nutritive cream, a moisturizer cream, a hand cream, , A pack, a soap, a cleansing foam, a cleansing lotion, a cleansing cream, a body lotion and a body cleanser.

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