KR102266174B1 - Nano emulsion composition comprising nano-cellulose and producing method thereof - Google Patents

Abstract

The present invention relates to a nanoemulsion emulsion cosmetic composition containing nanocellulose and a method for preparing the same, and the nanoemulsion of the present invention has a small and homogeneous particle size, excellent skin penetration ability, and improved formulation stability. In addition, when the emulsion composition of the present invention is formulated as a cosmetic or external application for skin, the delivery power of the active ingredient is improved, so that a product with excellent effect can be manufactured.

Description

Nano-emulsion composition comprising nano-cellulose and its manufacturing method {Nano emulsion composition comprising nano-cellulose and producing method thereof}

The present invention relates to a nanoemulsion emulsion cosmetic composition using nanocellulose and a method for preparing the same, and the nanoemulsion of the present invention has a small and homogeneous particle size, excellent skin penetration ability, and improved formulation stability. In addition, the emulsion composition of the present invention can be used as a cosmetic or external preparation for skin.

Cosmetics are generally formulated by combining ingredients that do not dissolve in each other, such as water-soluble and fat-soluble ingredients. In order to combine the above components, an emulsifier or surfactant is used to prepare an emulsion formulation in which the two components are combined, that is, an emulsion.

The size of the emulsion affects the stability of the phase and the ability to deliver the active substance, and the smaller the size of the emulsion, the better the stability and the ability to deliver the active substance. The size of the emulsion can also influence the phase stability in the formulation. Therefore, as a method to solve this problem, a nano-emulsifying formulation having an emulsion particle size of several hundred nm was developed. Various methods are known for the nano-emulsion production method, but among them, a method using a high-pressure homogenizer and a method using interfacial chemical properties such as an inversion temperature emulsification method and a D-phase emulsification method are widely used. The method using the interfacial chemical properties has a limitation in that a limited emulsifier must be used, such as polyoxyethylene (POE)-based. The fact that PEG-based compounds with ethylene oxide added are the main emulsifiers used in the preparation of nanoemulsions so far, but the fact that a trace amount of dioxin may be contained in the recent process of polymerization of ethylene glycol may cause irritation to the skin are reported, and according to the recent trend of consumers who value safety and well-being, there is a need for a method to avoid the use of emulsifiers with concerns about irritation.

On the other hand, the high pressure homogenizer has disadvantages of equipment cost, location, and long time. However, the manufacturing method is a mechanical method, and unlike the interfacial chemical method, it is free from problems due to side effects and has the advantage that continuous manufacturing is possible.

In the present invention, a nanoemulsion was prepared with a high pressure homogenizer among the above techniques, and nanocellulose was added thereto to reduce the size of the emulsion, thereby greatly increasing the effect of delivering an active substance to the human body.

Republic of Korea Patent Registration No. 10-1259452 Republic of Korea Patent Publication No. 10-2017-0103628

An object of the present invention is to provide a nano-emulsion emulsion cosmetic composition comprising nano-cellulose particles.

Another object of the present invention is to provide a skin external preparation or cosmetic comprising a nano-emulsion emulsion composition containing nano-cellulose particles.

In order to solve the above problems, the present invention provides a nanoemulsion emulsion composition comprising nanocellulose particles, wherein the nanocellulose particles are dispersed and included in the composition.

In one embodiment of the present invention, the nanocellulose particles are included in an amount of 0.1 to 10% by weight based on the total weight of the composition.

In one embodiment of the present invention, the size of the nanocellulose particles is characterized in that the average is less than 30nm.

In one embodiment of the present invention, the nano-cellulose is kraft paper or sulfite pulp derived from various wood, powdered cellulose obtained by pulverizing them with a high-pressure homogenizer or mill, or these acids Microcrystalline cellulose powder purified by chemical treatment such as hydrolysis, cellulose derived from bacteria, or those derived from plants such as kenaf, hemp, rice, bacchus, and bamboo may be used, but not limited thereto.

In addition, in one embodiment of the present invention, the nanoemulsion is characterized in that the average particle size is 8 to 30 nm, more preferably 12 to 18 nm.

In another aspect, the present invention provides a cosmetic comprising a nanoemulsion emulsion composition comprising nanocellulose particles.

In another aspect, the present invention provides an external preparation for skin comprising a nanoemulsion emulsion composition containing nanocellulose particles.

As another aspect, the present invention comprises the steps of (a) preparing an aqueous phase and an oil phase; (b) adding an oil phase to the aqueous phase, adding nanocellulose and stirring; and (c) providing a method for producing a nanoemulsion cosmetic composition comprising the step of homogenizing the composition of step (b) under high pressure .

In an embodiment of the present invention, the high-pressure homogenization step is performed at 300 to 800 psi, but is not limited thereto.

In another embodiment of the present invention, the high-pressure homogenization process is characterized by repeating 1 to 6 times, and more preferably repeating 4 to 5 times, but is not limited thereto.

The nanoemulsion emulsion composition containing the nano-cellulose particles of the present invention is characterized in that the particle size is smaller than that of the conventional nano-emulsion, and it is homogeneous to ensure emulsion stability, and the particle size is small so that it is used for cosmetics or external use for skin. When used as a skincare product, it has the characteristics of more effectively delivering the active ingredient into the skin.

1 shows the results obtained by measuring the particle size of a nano-emulsion to which nanocellulose is added.
Figure 2 shows the results obtained by measuring the particle size of the nano-emulsion to which nanocellulose is not added.
3 is a result showing the skin moisture content when the nanoemulsion composition of the present invention contains a moisturizing active ingredient.
FIG. 4 is a result showing the increase in skin moisture content confirmed through FIG. 3 by comparison.

The present inventors found that, in the emulsion composition of the nanoemulsion formulation, in order to make the size of the emulsion particles smaller and more homogeneous, when nanocellulose particles are included in the formulation, the size of the emulsion particles becomes smaller, and completed the present invention did.

That is, the present invention relates to an emulsion composition comprising a nanoemulsion, characterized in that it comprises dispersed nanocellulose in a particulate state, and to a nanoemulsion emulsion composition.

In the present invention, the term 'nanoemulsion' refers to an emulsion formulation in which an aqueous phase and an oil phase are mixed, and the size of the emulsified particles ranges from several tens of nm to several hundreds of nm. When the size of the emulsified particles is larger than the skin lipid gap, the active ingredient contained in the composition has a disadvantage that it is difficult to penetrate into the skin, so making the emulsified particles small is a very important technique in a formulation such as the present invention.

The nanoemulsion particles of the present invention have an average particle size of 8 to 30 nm, more preferably 12 to 18 nm. Although not limited thereto, in an embodiment of the present invention, a nanoemulsion having an average particle size of 16 nm was prepared. The particle size in the conventional general nanoemulsion formulation generally has a size of several tens to several hundreds of nm, so there is a limitation in delivering the active ingredient into the skin. The nano-emulsion of the present invention has a feature of maintaining a smaller particle size including nanocellulose, and due to this property, it has a more improved effect in penetrating the active ingredient into the skin.

As used herein, the term “average particle size” refers to the average diameter of particles in a liquid-liquid dispersion system, and since the particles are three-dimensional objects, the particle size calculated using the concept of equivalent sphere to measure the diameter when it is not a perfect sphere will include For example, a sphere of the same maximum length, a sphere of the same minimum length, a sphere of the same mass, a sphere of the same volume, a sphere of the same surface area, a sphere passing through the same sieve aperture, a sphere having the same sedimentation rate, etc. The particle size can be calculated from the diameter of the equivalent spherical shape by converting it into an equivalent spherical shape having the same characteristics, and the average particle size can be regarded as an average value calculated for these particle sizes of the particles. The average particle size also includes a particle size measured by a dynamic light scattering (DLS) method. The dynamic light scattering method includes a method of determining the particle size by Brownian motion of particles, and a method of determining the particle size by reading the wavelength intensity of scattered light that changes at regular time intervals. The light used in the method may include a laser. A formula for determining the particle size may be generally used, and the formula includes a Stoke-Einstein relational expression for a diffusion coefficient.

The 'emulsification' formulation can be broadly divided into an O/W (oil in water) formulation in which the oil phase component is emulsified in the aqueous phase, and a W/O (water in oil) formulation in which the aqueous phase component is emulsified among the oil phase components. and recently, a W/O/W type emulsifier type incorporating a multi-liquid crystal film emulsification technology has been developed. The nanoemulsion emulsion formulation of the present invention may include all of the above types, and more preferably, may be a water-in-oil (W/O) formulation, but is not limited thereto.

The "nanocellulose" of the present invention is a cellulose-based raw material made into nanoparticles, and the cellulose is craft paper or sulfurous acid pulp derived from various wood, and these are pulverized with a high-pressure homogenizer or mill. Powdered cellulose, microcrystalline cellulose powder purified by chemical treatment such as acid hydrolysis, cellulose derived from bacteria, etc. may be used. In addition, plants such as kenaf, hemp, rice, bacchus, and bamboo may be used. In an embodiment of the present invention, nano-cellulose was prepared using cellulose derived from wood, particularly pulp, cotton, or bamboo, but is not limited thereto.

The number average diameter of the 'nanocellulose' according to the present invention is 1-200 nm, preferably 1-150 nm, more preferably 1-100 nm, most preferably about 1-30 nm. In one embodiment of the present invention, nano-cellulose having a diameter of 20 nm or less was used. The nanocellulose may exist in the form of single microfibrils or in the form in which nanofibers are entangled with each other, but is not particularly limited. However, it is characterized in that it exists in a dispersed form in the formulation.

The nanocellulose may be included in a powdery or water-dispersed form in the composition of the present invention, and more preferably, may be included in an aqueous-dispersed form. Although not limited thereto, it may be included in an amount of 0.1 to 10% by weight in the total composition, and more preferably, may be included in an amount of 1 to 5% by weight. When the nanocellulose is included in an amount of less than 0.1% by weight, the effect on the particle size of the nanoemulsion is insignificant, and when it is included in an amount of 10% by weight or more, the properties of the composition may be affected. In an embodiment of the present invention, a nanoemulsion composition comprising the nanocellulose in an amount of 3% by weight was prepared, and efficacy was evaluated.

In addition, in the case of the nanoemulsion emulsion composition of the present invention, it may be included in cosmetics, and the cosmetic may be prepared in any formulation conventionally prepared in the art, for example, a solution, suspension, emulsion, paste, It may be formulated as a gel, cream, lotion, powder, soap, surfactant-containing cleansing, oil, powder foundation, emulsion foundation, wax foundation and spray, but is not limited thereto. More specifically, flexible lotion, astringent lotion, nourishing lotion, nourishing cream, massage cream, moisture cream, moisturizing gel cream, lotion, gel, essence, eye cream, peel-off mask pack, cleansing cream, cleansing foam, cleansing water, It can be prepared in the form of packs, ointments, sticks, patches, sprays or powders.

In particular, the composition of the present invention may be included in functional cosmetics or general cosmetics, and 'functional cosmetics' is a cosmetic that has a professional therapeutic function introduced into it, so that unlike general cosmetics, it provides professional functionality emphasizing physiologically active efficacy and effect. It refers to cosmetics prescribed by Ordinance of the Ministry of Health and Welfare, such as products that help skin whitening, products that help improve skin wrinkles, products that help burn skin finely or protect the skin from UV rays do. In an embodiment of the present invention, a cosmetic composition including a moisturizing active ingredient (hyaluronic acid) was prepared as an embodiment, but is not limited thereto.

When the composition of the present invention is used as a cosmetic, auxiliary agents commonly used in the cosmetic field, for example, fatty substances, organic solvents, solubilizers, thickeners, gelling agents, emollients, antioxidants, suspending agents, stabilizers, foaming agents ( foaming agent), fragrance, surfactant, water, ionic or nonionic emulsifier, filler, sequestering agent, chelating agent, preservative, vitamin, blocker, wetting agent, essential oil, dye, pigment, hydrophilic or lipophilic active agent , lipid vesicles, as well as any other ingredients commonly used in cosmetics, together with adjuvants commonly used in the field of cosmetology or dermatology, as a component of general cosmetics or functional cosmetics.

In another aspect, the nanoemulsion emulsion composition of the present invention may be used as an external preparation for skin. The topical skin preparation is a concept that includes quasi-drugs intended to be applied to the skin, and quasi-drugs are those used for the purpose of treating, alleviating, treating or preventing diseases of humans or animals, or having a weak action on the human body. It refers to articles that do not act directly on the human body, are not instruments or machines, and the like, and products that are used for sterilization, insecticide, and similar purposes to prevent infection.

The skin external preparation refers to a solid, semi-solid, or liquid external preparation that can be easily applied to the skin by mixing drugs with various bases such as oils and fats, petrolatum, lanolin, and glycerol. Formulation for external use is not particularly limited, but may include, for example, powder, patch, gel, ointment, cream, liquid or aerosol formulation.

In addition, the present invention is a method for producing a nanoemulsion emulsion composition comprising nanocellulose particles,

(a) preparing an aqueous phase and an oil phase; (b) adding an oil phase to the aqueous phase, adding nanocellulose and stirring; and (c) providing a method for producing a nanoemulsion cosmetic composition comprising the step of homogenizing the composition of step (b) under high pressure .

In the present invention, the step of high-pressure homogenization after adding the aqueous phase part, oil phase part and nanocellulose is characterized in that it is performed at a pressure of 300-800 psi. The pressure range is a condition in which nanocellulose can be homogeneously mixed in the emulsion composition, and the emulsion particles can be prepared in nano size. In addition, although not limited thereto, the high-pressure homogenization is characterized in that it is repeated 1 to 6 times, more preferably 3 to 6 times.

Hereinafter, the present invention will be described in more detail by way of Examples. These examples are merely for illustrating the present invention in more detail, and it will be apparent to those skilled in the art that the scope of the present invention is not limited to these examples.

< Example >

Nanocellulose containing particles Nanoemulsion Preparation of the composition

An emulsion was prepared with the composition shown in Table 1 below. First, a water-soluble component, a moisturizing agent, and purified water are stirred and dissolved by heating (65-75°C) to prepare an aqueous phase part. Then, the oil-soluble component, emulsifier, and oil are stirred and heated to dissolve them to prepare the oil phase. An emulsion composition of Example 1 was prepared by adding the oil phase to the aqueous phase and sufficiently stirring using a homomixer, which was then treated with a high-pressure homogenizer to prepare an emulsion composition of Example 2.

The nanoemulsion composition of Example 3 was prepared by adding 3% by weight of nanocellulose having a diameter of 20 nm or less to the emulsion of Example 1, and the nanoemulsion composition of Example 4 was prepared by passing through a high pressure homogenizer in the same manner. The high-pressure homogenizer was treated 4 to 5 times at 300 to 800 psi, and was equally applied to all examples.

name Example 1 (wt%) Example 3
(weight%) One Purified water to 100 to 100 2 Nanocellulose 0 3.0 1% hyaluronic acid 2.0 2.0 2 glycerine 5.0 5.0 4 glycereth-26 2.0 2.0 5 Carbomer 941 (25%)
(sodium polyacrylate 941) 10.0 10.0 6 Phenoxyethanol 0.4 0.4 7 TRIETHANOL AMINE 0.5 0.5 8 coconut oil 0.05 0.05 9 Polyoxyethylene(5) Oleyl Ether 1.0 1.0 total amount 100 100

The particle size analysis of the nanoemulsion to which nanocellulose was added and the nanoemulsion without the addition of nanocellulose prepared as described above was analyzed, and the average particle size was measured using a Dynamic Light Scattering Spectrophotometer (DLS-7000, Otsuka Electronics, Japan) as the particle size analysis equipment. measured.

As a result, as shown in Figure 1, in the case of the nano-emulsion to which nano-cellulose is added, the particle size corresponds to the range of 8 to 30 nm and the average particle size was measured to be 16 nm, but in the case of the nano-emulsion to which nano-cellulose is not added, It was measured to have a particle size of 65 to 300 nm.

That is, in the case of the nano-emulsion containing nano cellulose, it was confirmed that the particle size and homogeneity of the emulsion were very high.

<Experimental example>

Evaluation of moisturizing power of a cosmetic composition containing a nanoemulsion

(1) Evaluation of skin moisture content

In order to evaluate the skin delivery power of the nanoemulsion containing nanocellulose prepared in the above example, an experiment was conducted to measure the transdermal delivery rate of the skin moisturizing component. For women aged 18 to 55, the emulsion of Examples 1 to 4 was applied to the inner part of the lower arm in the morning and evening for 2 weeks, before use (0 W), after 1 week (1 W), 2 After a week (2 W), each skin moisture content was measured. In order to reduce measurement error, each measurement was performed by the same tester, and skin measurement was performed after taking skin stability for at least 30 minutes under constant temperature and humidity conditions (23±1℃, 50±2% RH) without air movement and direct sunlight. did.

Skin moisture content was measured using Skin-O-Mat® (Cosmomed inc, Germany). The measured value is displayed as a value between 0.0 and 125.0 (AU: Arbitrary Unit), and the higher the moisture content in the skin, the higher the measured value. In this experiment, the skin surface at the same location was repeatedly measured three times for each measurement period, and the average value was evaluated.

The measured values for the skin moisture content are shown in Table 2 and FIG. 3 below. In the case of a general nanoemulsion, the water content was only slightly increased for 2 weeks, but in the case of the nanoemulsion containing nanocellulose as in Examples 3 and 4, the water content after 2 weeks was significantly increased. improvement could be seen.

0 Week 1 Week 2 weeks Example 1 25.1±5.73 31.0±4.81 ^a 32.8±5.30 ^a Example 2 26.1±6.14 34.0±3.15 ^ab 33.1±4.52 ^a Example 3 27.0±6.49 34.9±3.91 ^ab 36.1±3.93 ^ae Example 4 26.7±6.78 37.6±2.98 ^abcd 39.2±4.29 ^aef

a: 0w vs. 1w, 2w, ANOVA, significant : p<0.05

b: 1w, Example 1 vs. Example 2, Example 3, Example 4, ANOVA, significant: p<0.05

c: 1w, Example 2 vs. Example 4, ANOVA, significant: p<0.05

d: 1w, Example 3 vs. Example 4, ANOVA, significant: p<0.05

e: 2w, Example 1 vs. Example 3, Example 4, ANOVA, significant: p<0.05

f: 2w, Example 2 vs. Example 4, ANOVA, significant: p<0.05

(2) skin moisture content rate of increase ( % ) evaluation

Using the skin moisture content data measured using Skin-O-Mat® (Cosmomed inc, Germany), the increase/decrease rate (%) of the skin moisture content over time was calculated. The increase/decrease rate of skin moisture content after 1 week (1w) and 2 weeks (2w) after using the product was compared with that before using the product. The skin moisture content increase/decrease rate was calculated using the following formula.

All measurements were repeated three times to obtain an average value. Statistical analysis results were checked for significance at the 95% confidence interval, and normality verification of the results was performed using the Kolmogorov-Smirnov and Shapiro-Wilk methods. One-way ANOVA was performed for statistical analysis of skin moisture content before and after product use and changes in skin moisture content increase/decrease rate. As a statistical analysis program, SPSS 23.0 (IBM SPSS Statistics, USA) was used.

The increase/decrease rate of the skin moisture content measured as described above is shown in Table 3 and FIG. 4 below. In the case of the nanoemulsion containing the nanocellulose of the present invention (Examples 3 and 4), it was confirmed that the increase rate of the skin moisture content was higher than that of the general nanoemulsion.

1 week 2 weeks Example 1 28.2±7.59 35.5±11.08 Example 2 35.5±7.72 30.4±7.32 Example 3 33.3±5.30 36.9±5.83 Example 4 46.8±7.16 51.4±8.16

So far, with respect to the present invention, the preferred embodiments have been looked at. Those of ordinary skill in the art to which the present invention pertains will understand that the present invention can be implemented in a modified form without departing from the essential characteristics of the present invention. Therefore, the disclosed embodiments are to be considered in an illustrative rather than a restrictive sense. The scope of the present invention is indicated in the claims rather than the foregoing description, and all differences within the scope equivalent thereto should be construed as being included in the present invention.

Claims (12)

It is a nano-emulsion consisting of hyaluronic acid, glycerin, glycereth, carbomer, phenoxyethanol, triethanolamine, coconut oil, polyoxyethylene and purified water as nanocellulose particles and skin moisturizing ingredients,
The nanoemulsion is mixed with glycerin, glycereth, carbomer, phenoxyethanol, triethanolamine, coconut oil, polyoxyethylene and purified water while heating, and then nanocellulose and hyaluronic acid are added and stirred, and the stirred composition is prepared A nano-emulsion was prepared by high-pressure homogenization repeated 4 to 5 times at a pressure of 300-800 psi,
Nanoemulsion emulsion cosmetic composition for skin moisturizing, characterized in that the average particle size of the nanoemulsion particles is 8 to 30nm, and increases the skin moisture content. According to claim 1,
The nano-cellulosic particles are dispersed in the composition and contained in the nano-emulsion emulsion cosmetic composition. According to claim 1,
The nano-cellulosic particles are contained in 0.1 to 10% by weight based on the total weight of the composition nanoemulsion emulsion cosmetic composition. According to claim 1,
The nano-emulsion emulsion cosmetic composition of which the size of the nano-cellulose particles is an average of 30 nm or less. According to claim 1,
The nanocellulose is craft paper or sulfite pulp derived from various wood, powdered cellulose pulverized by a high-pressure homogenizer or mill, etc., or these are purified by chemical treatment such as acid hydrolysis. Microcrystalline cellulose powder, cellulose derived from bacteria or derived from plants such as kenaf, hemp, rice, bacchus, and bamboo, nanoemulsion emulsion cosmetic composition. delete delete It is a nano-emulsion consisting of hyaluronic acid, glycerin, glycereth, carbomer, phenoxyethanol, triethanolamine, coconut oil, polyoxyethylene and purified water as nanocellulose particles and skin moisturizing ingredients,
The nanoemulsion is mixed with glycerin, glycereth, carbomer, phenoxyethanol, triethanolamine, coconut oil, polyoxyethylene and purified water while heating, nanocellulose and hyaluronic acid are added and stirred, and the stirred composition is prepared A nanoemulsion was prepared by high-pressure homogenization repeated 4 to 5 times at a pressure of 300-800 psi,
The average particle size of the nanoemulsion particles is 8 to 30 nm, and an external preparation for skin moisturizing, characterized in that it increases the skin moisture content. 9. The method of claim 8,
The external preparation for skin is one or more selected from powder, patch, gel, ointment, cream, liquid or aerosol. delete delete delete

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