KR102199766B1 - Manufacturing method of multi-lamellar structured transparent liquid crystal composition - Google Patents

Abstract

The present invention prepares an oil phase by mixing a composition containing lecithin and Mannosylerythritol Lipid (MEL), heating and dissolving it, and dissolving a polyol and a water-soluble active ingredient in water to prepare an aqueous phase. A method for producing a transparent multilayer liquid crystal composition comprising the step of mixing and stirring the aqueous phase with a homogenizer to prepare a primary emulsion, and then introducing the primary emulsion into a high-pressure emulsifier and cooling and filtering the micronized composition by high-pressure emulsification It is about.
According to the present invention, in the case of the transparent multilayer liquid crystal composition prepared by the above manufacturing method, since it forms a multilayer structure, the amount of oil-soluble components that can be contained in the structure can be increased, and the multilayer structure is not easily broken and is stable. Therefore, the oil-soluble component can be maintained. In addition, the liquid crystal composition thus produced has very little skin irritation, a soft feeling of use and excellent moisturizing power.

Description

Manufacturing method of multi-lamellar structured transparent liquid crystal composition

The present invention relates to a method of manufacturing a transparent multilayer liquid crystal composition, and more specifically, after mixing a composition containing lecithin and Mannosylerythritol Lipid (MEL), heating and dissolving to prepare an oil phase part, polyol And water-soluble active ingredients are dissolved in water to prepare an aqueous phase, mixed and stirred with a homogenizer to prepare a primary emulsion, and then put the primary emulsion into a high-pressure emulsifier and high-pressure emulsifying to cool the micronized composition. And it relates to a method for producing a transparent multi-layer liquid crystal composition comprising the step of filtering.

The stratum corneum, which is located on the outermost part of the skin and in direct contact with the outside, plays an important role of the skin barrier function. The stratum corneum consists of several layers of flat-shaped keratinocytes, preventing the loss of moisture and electrolytes inside the skin, and acting as a barrier to protect the human body from the external environment. (J. Invest. Dermatol. 69: 535-546, 1977). In addition, although there are differences depending on the experimental method and the location of the skin tissue, intercellular lipids are approximately 50% ceramide, 20 to 25% cholesterol, 20 to 25% free fatty acids, and about 10% cholesterol ester, 1 to 2%. It is known to consist of cholesterol sulfate and a small amount of phospholipids.

In order to help strengthen the skin barrier function by using the characteristics of these intercellular lipids, liquid crystal cosmetics that contain intercellular lipid components such as ceramide and cholesterol, and that simulate the multi-lamellar structure of the stratum corneum of the skin. The same formulations were developed. However, since ceramide and cholesterol are poorly soluble, it is difficult to stably contain in the formulation, and because of problems such as precipitation, it is difficult to contain a large amount in an emulsion formulation, and in particular, it has a disadvantage that it is difficult to use in solubilizing formulations such as skins and toners.

In order to solve such a problem, researchers have prepared structures such as liposomes using self-assembly of phospholipids, and conducted research to effectively deliver physiologically active substances into the skin. Phospholipids have properties that can increase the skin permeability of physiologically active substances by increasing the fluidity of lipids in the stratum corneum of the skin (Biochem. Biophys. Acta, 1237(1995): 176-182). However, since the liposome has a bilayer structure, the amount of useful substances that can be contained in the liposome is relatively small, and due to the structural weakness of the double layer, it is easily broken and the useful substances inside can be precipitated.

Accordingly, the present inventors used Mannosylerythritol Lipid (MEL) and lecithin to prepare a liquid crystal composition capable of stably containing a large amount of intercellular lipids than conventional liposomes due to the multilayer structure of intercellular lipids. To prepare a multilayered liquid crystal composition. MEL is a natural biosurfactant made by yeast, and is a glycolipid composed of mannose, sugar alcohol and fatty acids. MEL is an amphiphilic structure that has two properties: hydrophobicity derived from the properties of lipids and hydrophilicity derived from the properties of sugars, so it has a structure similar to that of ceramides that form human sebum. Due to such properties, MEL can form a lamellar structure, and it is known that it can act as an effective ingredient for skin roughness [Japanese Patent PCT/JP2006/323239].

In addition, the present inventors prepared a liquid crystal composition using a high pressure homogenizer in order to refine and make the intercellular lipid components as described above. When a general solubilization method is used, components having high hydrophobicity such as ceramide, cholesterol, and phospholipids can be solubilized only in the core space of the solubilizing agent, so there is relatively little space for solubilization. That is, when a general solubilization method is used, such poorly soluble components are difficult to solubilize and it is very difficult to stably maintain the composition. Therefore, methods of miniaturizing emulsified particles and stabilizing poorly soluble substances using a high-pressure emulsifier are widely used in the cosmetic industry.

In this way, the present inventors use MEL and lecithin to simulate a multilayered structure, which is the structure of the stratum corneum, and stabilize ceramide and cholesterol, which are intercellular lipid components that can help the skin barrier function of the human body, so that it can be easily applied in cosmetic formulations. To develop a multilayer liquid crystal composition.

Accordingly, as a result of the present inventors' intensive research efforts to overcome the problems of the prior art, after mixing a composition containing lecithin and Mannosylerythritol Lipid (MEL), heating and dissolving to prepare an oily part, polyol And water-soluble active ingredients are dissolved in water to prepare an aqueous phase, and the oil phase and the aqueous phase are mixed and stirred with a homogenizer to prepare a primary emulsion, and then the primary emulsion is introduced into a high pressure emulsifier, and the micronized composition is cooled by high pressure emulsification. And a transparent multi-layer liquid crystal composition was prepared by a manufacturing method comprising the step of filtering. In the case of the transparent multilayer liquid crystal composition prepared by this manufacturing method, since it forms a multilayer structure, the amount of oil-soluble components that can be contained in the structure can be increased. Can be maintained. In addition, it was confirmed that the liquid crystal composition thus produced exhibits a soft feeling of use and excellent moisturizing power with very little skin irritation, and the present invention was completed.

JP 2006-323239 A

Therefore, the main object of the present invention is not only to increase the amount of oil-soluble components contained in the liquid crystal of a multilayer structure, but also to stably maintain the oil-soluble components, and to have a soft feeling of use and excellent moisturizing power with very little skin irritation. It is to provide a method for producing a layered liquid crystal composition.

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

Another object of the present invention is to provide a cosmetic composition for moisturizing skin using the transparent multilayer liquid crystal composition.

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

(a) mixing a composition containing lecithin and Mannosylerythritol Lipid (MEL), heating and dissolving to prepare an oil phase;

(b) dissolving a polyol and a water-soluble active ingredient in water to prepare an aqueous phase;

(c) preparing a primary emulsion by mixing and stirring the oil phase part of step (a) and the water phase part of step (b) with a homogenizer;

(d) injecting the primary emulsion of step (c) into a high-pressure emulsifier and high-pressure emulsification to refine it; And

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

The term "transparent multilayer liquid crystal composition" of the present invention means that the external appearance is transparent, and the oil layer and the water phase layer are sequentially stacked in 3 to 10 layers.

The transparent appearance means that the liquid is transparent to the inside. As shown in FIG. 1 of the present invention, the degree of transparency can be measured according to how clearly the letters behind the container containing the liquid are clearly visible. In addition, the degree of transparency can be measured according to the size of the liquid crystal composition, and the transparent multilayer liquid crystal composition of the present invention has a 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 not containing lecithin and MEL, Example 1 containing only lecithin, and Example 2 containing only MEL, the size of the particles when manufactured under the same conditions as the present invention 200-500 nm and an opaque or translucent emulsion was prepared, but in the case of Example 3 containing both lecithin and MEL, it was confirmed that a very transparent liquid crystal composition in the range of 100-120 nm was prepared (see Experimental Example 1-2. ).

In addition, according to the experimental example of the present invention, as a result of observing the structure of Example 3 with a freezing scanning electron microscope, it was confirmed that the structure of Example 3 was actually formed as a multi-layer stacked in layers (see Experimental Example 3).

In the present invention, any water-soluble active ingredient in the step (b) may be used as long as it is dissolved in water to form an aqueous phase, such as a wrinkle-improving functional ingredient, a whitening functional ingredient, and a natural extract.

The wrinkle-improving functional raw material includes adenosine, and the whitening functional raw material includes arbutin and niacinamide. In addition, natural extracts include natural extracts of plants, animals, or minerals extracted from aloe, green tea, tangerines, ginkgo leaves, and the like, and the water-soluble component is not limited to the above types.

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

Singi nonionic surfactants are PEG-40 hydrogenated castor oil, octyldodeces, polysorbate 60, PEG-40 stearate, ceteareth-20, PEG-20 glyceryl isostearate, and polyglyceryl. -3 It may contain at least one selected from the group consisting of methyl glucose distearate, polyglyceryl-10 stearate, and choles, and the content is preferably 0.1 to 3% by weight.

In addition, the polyol used in the present invention is glycerin, diglycerin, propylene glycol, dipropylene glycol, 1,3-butylene glycol, ethylhexyl glycerin, polyglycerin, caprylyl glycol, pentylene glycol It may contain at least one selected from the group consisting of Cole and 1,2-hexanediol, and the content is preferably 5 to 60% by weight.

In the present invention, the oil phase portion of the step (a) is characterized in that it contains 5 to 15% by weight based on the total weight of the composition. If there are many oil phases in the above range, the emulsified particles become large and viscosity is generated due to the ratio of the inner wound to the outer wound, which may cause a problem in that it is difficult to perform high pressure emulsification.

In the present invention, the aqueous portion of the step (b) is characterized in that it contains 75 to 95% by weight based on the total weight of the composition. In the above range, if the water phase is small, the emulsified particles become larger and viscosity is generated due to the ratio of the inner and outer wounds, and thus, it is difficult to perform high pressure emulsification.

In the present invention, the particle size of the first emulsion in step (c) is 200 to 500 nm. If the particle size of the primary emulsion is too large outside the above range, there may be a problem in that it is difficult to obtain a transparent result even when high pressure emulsification is performed.

In the present invention, the high-pressure emulsification of step (d) is characterized in that passing 1 to 5 times at a pressure of 500 to 1500 bar. The high pressure of the high pressure emulsifier does not mean that the particle size keeps getting smaller because the number of calls is high, so the ratio of lecithin and MEL, the pressure of the high pressure emulsifier, and the number of passes of the high pressure emulsifier must be specified in an appropriate range. Since the composition can be prepared, it is preferable to perform high pressure emulsification within the above range.

According to another aspect of the present invention, the present invention provides a transparent multilayer liquid crystal composition prepared by the above manufacturing method.

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

The term "transparent multilayer liquid crystal composition" of the present invention means that the external appearance is transparent, and the oil layer and the water phase layer are sequentially stacked in 3 to 10 layers.

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

According to the experimental example of the present invention, as a result of confirming the skin moisturizing power of the cosmetic composition containing the transparent multilayer liquid crystal composition prepared by the manufacturing method of the present invention, it was confirmed that the skin moisturizing power was superior to that of the non-application group. From these results, it can be seen that the transparent multilayer liquid crystal composition of the present invention has a transparent appearance and is not only suitable for use in a formulation requiring transparency, but also has excellent moisturizing power and is very suitable as a cosmetic composition (see Experimental Example 4). ).

In the present invention, the cosmetic composition is a skin lotion, skin softener, skin toner, astringent, lotion, milk lotion, moisture lotion, nutrition lotion, massage cream, nutrition cream, moisture cream, hand cream, foundation, essence, nutrition essence, It is characterized by having one formulation selected from the group consisting of a pack, soap, cleansing foam, cleansing lotion, cleansing cream, body lotion, and body cleanser.

In addition, the cosmetic composition including the multi-layered transparent liquid crystal composition prepared in the present invention is not particularly limited in its formulation, but considering its transparent appearance and advantages in use, skins, toners, solutions, suspensions, emulsions, pastes , Gel, cream, lotion, powder, powder foundation, emulsion foundation, sun cream, pack, mask sheet, lipstick, mist, and other formulations can be used.

Hereinafter, the present invention will be described in more detail.

In order for the transparent liquid crystal composition of the present invention to form a multilayer structure, the roles of phospholipids and MEL are important. Lecithin, one of the phospholipids, is self-emulsifying when mixed with a sufficient aqueous medium to form a double-layer or multi-layer lamellar structure. have. The composition for forming a multi-layered lamella structure forms a multi-layered structure in which an oil layer and an aqueous phase layer are sequentially stacked in a kind of valve structure consisting of phospholipids. In addition, in addition to lecithin, the formation of a lamella structure was facilitated by using MEL, which has a structure similar to that of ceramide in the human body.

In the present invention, when preparing a transparent multilayer liquid crystal composition, it was used to refine the size of the particles to about 100 nm by using a high pressure emulsification method. The high pressure emulsification method is an emulsification method using a high pressure homogenizer, and generally refers to secondary emulsification by passing the emulsion first emulsified with a homogenizer through a high pressure emulsifier. Pressure is generally high-pressure emulsification at 500 ~ 2,000 bar, and the process of atomization of oil particles is nano-sized due to cavitation, turbulence, and shear force due to a rapid drop in pressure while high-pressure fluid passes through a small gap in the valve at high speed. As it is split into fine particles, the levitation force is reduced, and the composition of the liquid is made completely uniform.

In the present invention, it is suitable to pass the emulsion at least once at 500 to 1,500 bar. The most preferable size distribution of emulsified particles here is that the average particle size of the first emulsified particles with a general homogenizer is about 200 to 500 nm, and if the second emulsification is performed with a high pressure emulsifier after the first emulsification with a general homomixer, the average particle size Is reduced to 50 ~ 150 nm to form a transparent ~ translucent property.

As described above, the multi-layered transparent liquid crystal composition prepared by the manufacturing method of the present invention can contain more active ingredients through a multi-layered structure that simulates the skin lipid structure, and has the advantage of improving stability. Have. In addition, since the external appearance is transparent, it is not only suitable for use in formulations requiring transparency, but also has a soft feeling of use and excellent moisturizing power with very little skin irritation.

1 is a photograph of the appearance of Comparative Example 1 and Examples 1 to 3 prepared according to the present invention.
2 is a graph of particle size distribution measured by a dynamic light scattering (DLS) device of Example 3 manufactured according to the present invention.
3 is an image of a cryo-transmission electron microscope (Cryo-TEM) of Example 3 prepared according to the present invention.

Hereinafter, the present invention will be described in more detail through examples. Since these examples are for illustrative purposes only, the scope of the present invention is not to be construed as being limited by these examples.

Example 1: Preparation of Comparative Examples and Examples

The multilayered liquid crystal composition of the present invention is characterized in that it contains MEL, lecithin, and polyol to solubilize poorly soluble substances such as ceramide and cholesterol.

Here, the MEL may be represented by the following Formula 1.

[Formula 1]

The MEL may be expressed as Candidia bombicola/glucose/methyl rapeseedate ferment, olea europaea(olive)fruit oil.

In order to prepare a multilayered liquid crystal composition having a transparent appearance stabilizing intercellular lipids of the present invention, an experiment was conducted with the composition shown in Table 1 below. At this time, the A phase was dissolved by heating at 80 to 100°C, and then added to the B phase heated at 70 to 90°C, and the mixture was uniformly emulsified by stirring for 5 minutes at 5,000 rpm with a homogenizer. In this way, the firstly emulsified composition was put into a high-pressure emulsifier, and the high-pressure emulsification was performed by repeating three times at a pressure of 1,000 bar. The composition after high pressure emulsification 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 Mannosylerythritol Lipid 0 0 One One PEG-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

After high pressure emulsification of the compositions of Comparative Example 1 and Examples 1 to 3, it was confirmed whether or not the composition was prepared as a transparent or opaque milky white composition. same. In Table 2, the opaque formulation is indicated as X, the translucent formulation as △, and the transparent formulation as ○.

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

As shown in the results of Table 2 and FIG. 1, when lecithin and MEL were not included, a formulation having an opaque appearance was prepared, and when lecithin or MEL was not included, a translucent formulation was prepared. The translucent appearance is obtained because the size of the particles is 100 nm or more, and ceramide and cholesterol are stabilized by lecithin or MEL, but these formulations have a disadvantage that they are not suitable for use in formulations requiring transparency such as toners and skins. . However, when lecithin and MEL are simultaneously contained as in Example 3, ceramide and cholesterol are stably present in particles of about 100 nm to maintain transparency, and therefore, when preparing a transparent cosmetic, the input of this composition is the appearance of the cosmetic. Since it does not affect the composition, it can be effectively used without limitation on the amount of the composition.

Experimental Example 2: Measurement of particle size of multi-layered transparent liquid crystal composition

The particle size distribution of the multilayer transparent liquid crystal composition of the present invention was measured using a dynamic light scattering (DLS). As a result, as shown in FIG. 2, it can be seen that the particle distribution of Example 3 is about 113 nm based on intensity.

In addition, as a result of measuring the size of each of the examples, Comparative Example 1 was 257.6 nm, Example 1 was 187.6 nm, Example 2 was measured to be 162.2 nm.

Experimental Example 3: Structure observation of a multi-layered transparent liquid crystal composition

The structure of the multi-layered 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 was found that Example 3 uniformly formed multilayer particles of about 100 nm. As a result, it can be seen that the size was similar to that of the particle size analysis result using DLS of Experimental Example 2.

Preparation Example 1: Preparation of a cosmetic using a multi-layered transparent liquid crystal composition

In Preparation Example 1, as shown in Table 3 below, a multi-layered transparent liquid crystal composition containing ceramide and cholesterol prepared in Example 3 was added to purified water to finally prepare a cosmetic composition stably containing ceramide and cholesterol. The preparation of this cosmetic is one of examples using a multi-layered transparent liquid crystal composition, and when applying a multi-layered transparent liquid crystal composition to a cosmetic, the selection of a formulation and a method of manufacturing are not limited.

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

As a result of measuring the particle size distribution using DLS, 71 nm was confirmed and the zeta potential was ?78.5 mV, indicating a stable distribution.

Experimental Example 4: Moisturizing power test of multi-layered transparent liquid crystal composition

For 5 healthy female subjects, a toner containing 5% of a multi-layered transparent liquid crystal composition was prepared, using a corneometer before sample application, 2 hours after application, 4 hours after application, and 8 hours after application. The moisturizing power test was conducted.

As a result of analyzing the changes in the measured values of the instrument analysis using a Corneometer, the toner containing the multi-layered transparent liquid crystal composition obtained 18.4%, 14.3%, and 8.4% higher results, respectively, 2 hours, 4 hours, and 8 hours after application. Therefore, it was found that there is a moisturizing effect due to the intercellular lipid components contained in the multilayer transparent liquid crystal composition.

The cosmetic composition including the multi-layered transparent liquid crystal composition is not particularly limited in its formulation, but considering its transparent appearance and advantages in use, skin, toner, solution, suspension, emulsion, paste, gel, cream, lotion , Powder, powder foundation, emulsion foundation, sun cream, pack, mask sheet, lipstick, mist, etc. can be widely applied.

Claims (10)

A method for preparing a transparent multilayer liquid crystal composition comprising the following steps and does not contain an anti-inflammatory agent:
(a) mixing a composition containing lecithin and Mannosylerythritol Lipid (MEL), heating and dissolving to prepare an oil phase;
(b) preparing an aqueous phase by dissolving a polyol and a water-soluble active ingredient in water;
(c) preparing a primary emulsion by mixing and stirring the oil phase part of step (a) and the water phase part of step (b) with a homogenizer;
(d) introducing the primary emulsion of step (c) into a high-pressure emulsifier and high-pressure emulsification to refine it; And
(d) cooling and filtering the composition of step (d).
The method of claim 1, wherein the oil phase part of the step (a) further comprises ceramide or a derivative thereof, cholesterol, a nonionic surfactant, and a polyol.
The method of claim 1, wherein the oil phase part of the step (a) comprises 5 to 15% by weight based on the total weight of the composition.
The method of claim 1, wherein the (b) water phase comprises 75 to 95% by weight based on the total weight of the composition.
The method of claim 1, wherein the particle size of the first emulsion in step (c) is 200 to 300 nm. a
The method of claim 1, wherein the high-pressure emulsification is passed 1 to 5 times at a pressure of 500 to 1500 bar.
A transparent multilayer liquid crystal composition prepared by the manufacturing method of any one of claims 1 to 6.
The transparent multilayer liquid crystal composition according to claim 7, wherein the transparent multilayer 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 method of claim 9, wherein the cosmetic composition is a skin lotion, skin softener, skin toner, astringent, lotion, milk lotion, moisture lotion, nutrition lotion, massage cream, nutrition cream, moisture cream, hand cream, foundation, essence, nutrition essence , Pack, soap, cleansing foam, cleansing lotion, cleansing cream, body lotion, and a cosmetic composition for skin moisturizing, characterized in that it has one formulation selected from the group consisting of a body cleanser.

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