KR100488220B1 - Polyoxypropylene-polyoxyeth-yethylene vitamin e-containing novel nanoemulsion compositions for skin-protecting and skin-curing and preparation thereof - Google Patents

Abstract

The present invention relates to a stable and safe oil-in-water type nanoemulsion cosmetic composition and a method for producing the emulsifier is polyoxypropylene-polyoxyethylene (POP-POE) vitamin E represented by the following formula (1).

<Formula 1>

In the above formula,

R ₁ is — (O—CH ₂ CH ₂ ) _m , m is an integer from 0 to 250, R ₂ is H (OCH (CH ₃ ) CH ₂ ) _n −, n is an integer from 1 to 200, A is , B is CH _{3 at} the 5-, 7- or 8- position of vitamin E, and p is 1 or 3.

Description

Nano-emulsion cosmetic composition containing polyoxypropylene-polyoxyethylene (POP-POE) vitamin E and preparation method thereof }

       The present invention relates to a stable and safe nano-emulsion cosmetic composition for the skin protection agent and skin treatment using an emulsifier consisting of polyoxypropylene-polyoxyethylene (POP-POE) vitamin E and a method for producing the same.

The emulsion composition is a formulation in which one phase is stably dispersed in another phase using an emulsifier that significantly lowers the interfacial tension in order to uniformly mix oily and aqueous components that are not mixed with each other. It has been widely used in cosmetics and external medicines because of the relatively excellent skin absorption and penetration properties of drug components effective for skin treatment. However, conventional emulsion composition (macroemulsion) until now has a relatively large particle [usually 0.5-100 micron (μm)] thermodynamic instability disadvantages and also has the disadvantage of limited skin absorption of the active ingredient. Therefore, to improve the stability of the emulsion composition, to add an electrolyte, to adjust the ratio of oil and aqueous components, to use a higher fatty alcohol, wax or the like in the oil phase to increase the viscosity of the composition or to the carboxyvinyl polymer in the water phase Thickeners such as, cellulose derivatives, bentonite, etc. or anionic emulsifiers with nonionic emulsifiers and mixtures of emulsifiers with different HLB (hydrophile-liphophile balance) values. There have been attempts to use the lights together. However, the emulsified compositions prepared by these methods are also difficult to reduce the particle size and the limit of the lowering of the interfacial tension, so that the thermodynamic instability is not fundamentally improved, and the large emulsion particles are significantly small enough to absorb skin well. There are disadvantages that cannot be made and problems such as deterioration of skin safety when using a large amount of surfactant.

Therefore, the present inventors have continued to study how to solve these problems, the composition of the nano-emulsion formulation of the medium size of the emulsion (macroemulsion) and solubilization, the size of the emulsion particles of the general emulsion composition Since it is much smaller than the particles and much larger surface area per unit volume, it has been found that the thermodynamic stability is significantly improved and the skin absorption of the active ingredient is significantly improved than the general emulsion composition.

Nanoemulsion can be defined as oil-in-water emulsification, in which particles have an average diameter of 50 to 1000 nm, generally 100 to 500 nm. More specifically, one of the reasons nano emulation is of interest is the active ingredient of skin protection products. The efficiency of the delivery system is good. Nano-Emulsions help the skin penetrate the active ingredients, similar to liposomes, and increase their concentration in the skin. In general, nanoemulsion is a system of small particles with a large surface area, which greatly improves the stability of the nanoemulsion and also enables the effective ingredient to be efficiently delivered into the skin. In addition, these small particles can evenly warm the skin's surface and penetrate through the rough tissue of the skin's surface. Nanoemulsions are more suitable than liposomes for the delivery of lipophilic compounds because their internal particles are hydrophobic. In addition, nanoemulsion is attracting more and more attention due to its bioactive effect.

In general, two methods are known for making nanoemulsions. The first and most commonly used method is to create nanoemulsions using a high pressure homogenizer, such as phospholipids, or a co-surfactant with a suitable surfactant. The second method is to use the phase transition temperature principle. The interfacial tension near the phase transition temperature is very low, so if emulsification is made and rapidly cooled at temperatures near the phase transition temperature, nanoemulsions are produced (see Science and Technology of Emulsions- from Nanoemulsions to Multiple Emulsions, TF Tadros.21st IFSCC Berlin Congress Proceedings PP 442-458

The problem with the first method is that it must be manufactured while contacting the water phase and the oil phase through the thin nozzle while maintaining the machine at high pressure (e.g. 800 atm). Nanoemulsions of viscosity are made. If the viscosity is high, the fluidity of the phase is bad, and therefore the mixing is bad, which may be a manufacturing problem. The problem with the second method is that it is difficult to manufacture at the phase transition temperature in the mass production process, and in particular, it is more difficult to rapidly cool the mass produced product. Therefore, in spite of the problems mentioned above, when it is inevitable to manufacture nanoemulsion products, almost 5% or more of phospholipids, which are surfactants that can make vesicles and nanoemulsions, are used at high pressure. Using Niger, the company creates low viscosity nanoemulsions. In general, it is very difficult to produce small particles such as nanoemulsions. Therefore, a lot of energy and surfactants are required to manufacture nanoemulsions, and these difficulties have always been obstacles to the application of nanoemulsion technology to actual products such as cosmetics, pharmaceuticals, and food industry, and sometimes easy skin penetration. This raises concerns about skin side effects. Even though the nanoemulsion, which has emerged as an alternative to the general emulsion composition, has excellent properties, it can be seen that it is not widely used due to the problems listed above.

On the other hand, the present inventors have developed a POP-POE vitamin E of the formula (1) having excellent surface activity, such as the formation of vesicles, and the patent application No. 1998-20705 (Korean Patent Publication No. 2000-840) Filed an international patent (PCT / KR99 / 100270) to obtain a US patent (Patent No. 6,355,811 B1) and found its use as an antioxidant for POP-POE vitamin E and filed a patent application No. 2000-13818. Antioxidant cosmetic composition containing POP-POE vitamin E (patent application KR 00-13838), novel emulsion composition with oxidation stability (patent application KR-0027779, KR 00-71700), low viscosity We have filed an oil-in-water emulsion cosmetic (patent application KR01-3-110).

<Formula 1>

In the above formula,

R ₁ is — (O—CH ₂ CH ₂ ) _m , m is an integer from 0 to 250, R ₂ is H (OCH (CH ₃ ) CH ₂ ) _n −, n is an integer from 1 to 200, A is , B is CH _{3 at} the 5-, 7- or 8- position of vitamin E, and p is 1 or 3.

delete

In this POP-POE vitamin E, hydrophobicity is improved without disturbing the excellent orientation of tocopherol, thereby improving skin safety, and having excellent antioxidant activity and surfactant activity.

On the other hand, the inventors found that POP-POE vitamin E amphiphilic substance has excellent physical properties such as excellent in vivo antioxidant properties and vesicle formation through continuous and intensive studies. Were published at the 21st IFSCC Congress (Berlin 2000) and presented again at the 21st IFSCC Congress (Berlin 2000) .These papers were entitled "Polyoxypropylene-polyoxyethylene tocopheryl ether: A series of Novel Amphiphiles from Tocopherol for Functional Cosmetics". IFSCC Magazine PP 269-276 Vol. 4, No. 4 A paper titled "Novel nanoemulsions of POP-POE tocopheryl ether", published in 2001 and related to the composition and method of preparing nanoemulsions for skin protection and skin treatments using POP-POE vitamin E of the present application. The paper was presented on April 27, 2002 by Kim Young-dae and three others at the 22nd International Conference on Cosmetics and Chemistry of Edenburgh, UK.

The present inventors recognize the importance of nanoemulsion and based on the results of the above research, phospholipids that form vesicles by repeating research on nanoemulsion, which is a formulation that can be most widely used in cosmetics, medicine, food, etc. The fact that it is used in the manufacture of emulsification and the use of surfactants with excellent properties to form vesicles such as POP-POE vitamin E can be difficult to process using the homogenizer at high pressure or using the phase transition temperature principle. In addition to the use of agitators or homogenizers at normal pressure, which is a simpler process rather than a low productivity method, the nanoemulsion composition for high viscosity creamy skin protectors and skin treatments, as well as low viscosity products in a more efficient and economical way. Knowing that it can be prepared to complete the present invention.

Accordingly, it is an object of the present invention to provide a nano-emulsion composition for oil-in-water type skin protectors and skin treatments with excellent stability and low skin side effects and a method of manufacturing the same.

The present invention provides an oil-in-water type nanoemulsion cosmetic composition containing an emulsifier consisting of POP-POE vitamin E represented by the following Chemical Formula 1, and prepared by a two-phase complex emulsification method.

<Formula 1>

In the above formula,

R ₁ is — (O—CH ₂ CH ₂ ) _m , m is an integer from 0 to 250, R ₂ is H (OCH (CH ₃ ) CH ₂ ) _n −, n is an integer from 1 to 200, A is , B is CH _{3 at} the 5-, 7- or 8- position of vitamin E, and p is 1 or 3.

delete

Hereinafter, the nano-emulsion cosmetic composition of the present invention and its manufacturing process will be described in detail. The emulsifier for nanoemulsion constituting the nano-emulsion cosmetic composition of the present invention is preferably in the range of m to 20 to 150 and n is 10 to 120 in the POP-POE vitamin E of the general formula (1), more preferably m ranges from 30 to 100 and n ranges from 5 to 90.

POP-POE vitamin E of formula (1) can be prepared by the method described in Korean Patent Publication No. 2000-840.

POP-POE Vitamin E has a structure with one hydrophilic group between two lipophilic groups, similar to the phospholipids that make vesicles and nanoemulsions. It is excellent in forming a uniform thin film on the skin, showing excellent emollient effect, and also having antioxidant activity. Therefore, when POP-POE vitamin E is included in the skin protection and skin treatment composition of nanoemulsion, it improves the stability, less skin irritation, improves skin luster and flexibility, increases skin penetration of active ingredients, and It prevents or delays oxidizing and aging.

POP-POE vitamin E may be used in an amount of 0.1 to 60% by weight, preferably 1 to 50% by weight, in the skin protection and skin treatment composition of the nanoemulsion of the present invention.

In addition to the POP-POE vitamin E in the skin protection agent and skin treatment composition of the nano-emulsion of the present invention, as a component commonly used, it is useful for forming a formulation and skin protection widely used in skin protection and skin treatment products. Components and water-soluble components can be used, and representative oil-soluble components include hydrocarbons such as paraffin oil, squalane and squalene; Synthetic triglycerides obtained by reacting with a natural product such as capric capric triglyceride; Synthetic ester oils such as cetyloctanoate, octyl dodecanol and isopropyl palmitate; Vegetable oils such as jojoba oil, olive oil, soybean oil, moon soybean oil, sancho oil, sesame oil and perilla oil; Animal oils such as mink oil; Fat-soluble vitamins such as vitamins A, E, and F, and derivatives thereof, and the like; as the water-soluble component, polyols such as propylene glycol, butylene glycol, glycerin, and polyethylene glycol; Mucopolysaccharides such as hyaluronic acid, chondroitin sulfate, and glucosamine; Water-soluble vitamins such as vitamin C and panthenol and derivatives thereof; Benzophenone derivative ultraviolet absorbers including homomenthyl salicylate benzophenone, 2-hydroxy benzophenone, 4-methoxy benzophenone; Cinnamic acid derivatives such as ethylhexyl-p-methoxycinnamate and octylmethoxycinnamate; Ultraviolet absorbers such as butylmethoxydibenzoylmethane, albutin, gojiksan, and bilberry extracts, which have skin whitening effects, and alpha hydroxy acids, pancreses, and allantoin and amino acids, which promote skin circulation. Additives such as protein, flavonoids, milk, honey and extracts such as Angelica, Cheongung, Ginseng, Bellflower, Marigold, Green Tea and Wild Chrysanthemum, which are effective for skin protection, and dihydroxyacetone with skin pigmentation And zinc oxide, which has a soothing effect on the skin. In addition, as an ingredient of the skin protection agent and skin treatment composition of the nano-emulsion of the present invention, an active ingredient used for the treatment of the skin may be used. For example, the skin bleach hydroquinone and acne treatment products promote the circulation of keratin skin. Salicylic acid, alpha hydroxy acid, sulfur, pancrese as an enzyme, hydrocortisone as a component of corticosteroids for treating skin diseases, and the like can be used. The above-listed ingredients are ingredients that can be used in the present invention without particular limitation, and thus, the use of ingredients that can be used in skin protectants and skin treatments other than these is not limited.

Nano-emulsion composition for skin protection and skin treatment of the present invention by using POP-POE vitamin E as an emulsifier, the liquid crystal is easily formed, the emulsifier is well adsorbed on the interface between the oil-soluble and water-soluble phase and stabilize the dispersion of the oil phase more finely Emulsification is more stable, smooth and rich in use, and it moisturizes the skin and promotes skin absorption of the ingredients effective for skin protection and skin treatment. In particular, the nano-emulsion composition for the skin protection agent and skin treatment of the present invention can be prepared by a high pressure homogenizer or an ultrasonic syringe, but more efficiently by simply using a homogenizer at atmospheric pressure or by stirring as a high speed propeller stirrer. It can also emulsify. In other words, the economic emulsification method newly developed by the inventor of the present invention called "two-phase composite emulsification method" in which the oil-soluble phase and the water-soluble phase are heated and mixed in advance to form a high viscosity oil-soluble phase and a water-soluble phase complex and then emulsified with a high speed propeller stirrer Stable nanoemulsions can be prepared (Ref. 22) IFSCC Congress Proceedings, Novel nanoemulsions of POP-POE tocopheryl ether, Young-Dae Kim et al. This is a new, more efficient emulsification method that can produce nanoemulsions that are completely distinct from the methods of using homogenizers under the high pressure (for example, about 800 atm), which is a conventional general nanoemulsion preparation method, and those using the phase temperature principle. . In addition, since the emulsifier is a polymer, the nanoemulsion composition for the skin protection agent and the skin treatment of the present invention is safe without excessive skin penetration of the surfactant, and the composition is more stable and effective because the emulsified particle is a nanoemulsion formulation made finer. Since the skin permeability of is better, the contained skin protection ingredient and skin treatment ingredient may exhibit more improved skin protection effect and skin treatment effect than the composition of the general emulsifier type.

The skin protection agent and skin treatment nanoemulsion composition of the present invention is a skin cream, lotion, essence, body lotion, emulsified body oil and baby oil, sunscreen cream and lotion, sun tanning cream and lotion, emulsion self-tanning oil, etc. Dispersion products such as emulsified products, emulsified foundation creams, makeup bases, emulsified skin treatment products such as emulsified creams and lotion formulations in external medicines, wrinkle improvement products, acne treatment products, adrenal cortex hormone products, etc. Can be used.

The skin protection agent and skin treatment nanoemulsion composition of the present invention is a lipophilic component paraffin oil, squalane, squalene, capriccapric triglyceride, cetyloctanoenite, octyldodecanol, isopropyl palmitate, jojoba oil, Olive oil, soybean oil, walnut oil, olive oil, seaweed oil, sesame oil, perilla oil, mink oil, pasol 1789, parabenzoic acid propyl, methyl parabenzoate mixed with an emulsifier and heated, and some or all of the purified water (about 30-100%), propylene glycol, butylene glycol, glycerin, polyethylene glycol, allantoin, hyaluronic acid, chondroitin sulfate, glucosamine, etc. are added to dissolve the hydrophilic components, which are melted. After emulsifying with a stirrer or homogenizer, flavorings and vitamins are relatively heat-stable additives , Plant extracts, milk, hormones, enzymes, hormones, etc. may be added and emulsified again and cooled to obtain a skin protector and skin treatment composition of the oil-in-water type nanoemulsion. In particular, it may be prepared using a homogenizer or agitator in the emulsification step, but when the viscosity of the oil-soluble and water-soluble complex formed before emulsification is high, it is difficult to homogenize the homogenizer, so it is easier to use a propeller stirrer. It is preferable to use a stirrer because a nanoemulsion can be produced.

Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the following examples are only for illustrating the present invention, and the scope of the present invention is not limited thereto.

POP (20) -POE (50) Vitamin E, POP (30) -POE (70) Vitamin E, POP (25) -POE (55) Vitamin E, POP (15) -POE ( 50) Vitamin E, POP (25) -POE (60) and POP (18) -POE (55) Vitamin E and the like are prepared according to the method described in Korean Patent Laid-Open No. 2000-840.

Examples 1-3 and Comparative Examples 1-3: Oil-in-water Base Nanoemulsion Cosmetic Composition

Nanoemulsions to be used in skin protection products and skin treatment products can be prepared by adding skin protection agents and skin treatment agents to nanoemulsion compositions containing only conventional oil-soluble ingredients, water-soluble ingredients, and emulsifiers. It is necessary to confirm that the emulsifier POP-POE vitamin E used in the examples of the present invention using only the phase component and the emulsifier has the ability to make stable and safe nanoemulsions. Therefore, the experiment of manufacturing the base nanoemulsion with the composition of Examples 1-3. Table 1 shows the formulation of the composition using the other emulsifiers of Comparative Examples 1-3 for comparison with the oil-in-water base nanoemulsion composition for skin protectants and skin treatments of Examples 1-3 of the present invention using POP-POE vitamin E. have. The emulsifiers chosen for the comparative examples are commonly used surfactants having a hydrophilic-hydrophobic balance (HLB) similar to the emulsifiers of the examples. According to the composition of Table 1, the oil-soluble phase (part A) and the surfactant (part B) are injected into a tank and heated to 70 ° C., which is 30-100% purified water and an aqueous solution of propylene glycol heated to 70 ° C. Add phase (part C) and stir the mixture slowly with a propeller stirrer to form a high viscosity composite, add the remaining purified water and again emulsify by rotating the stirrer at high speed (about 1,000-2,500 RPM) and cool to room temperature Base nanoemulsion compositions were prepared at atmospheric pressure. For comparison, the compositions of Comparative Examples 1-3 of Table 1 were prepared in the same manner.

Experimental Example 1 Nano-Emulsion by Measuring Particle Size and Particle Size

Stability evaluation

In order to confirm that the oil-in-water base nanoemulsion compositions for skin protectants and skin treatments obtained in Examples 1-3 are actual nanoemulsions and these nanoemulsions are changed in particle size during long-term storage at high temperature (40 ° C.). In order to evaluate the stability by measuring the particle size of the composition of Example 1-3 and the composition of Comparative Example 1-3 was measured as follows.

Table 1. Oil-in-water base nano-emulsion cosmetic composition (unit: weight%)

  function  Ingredient To conduct Comparative example One 2 3 One 2 3  A: Usability  Paraffin oil 50 50 30 50 50 50  Squalane 10 10 6 10 10 10  Methylparaben 0.1 0.1 0.1 0.1 0.1 0.1  B: emulsifier  POP (20) -POE (50) Vitamin E 5 - 1.5 - - -  POP (30) -POE (70) Vitamin E - 5 1.5 - - -  POE (40) Vitamin E - - - 5 - -  Phosphatidylcholine - - - - 5 -  Polysorbate 60 - - - - - 3.5  Sorbitan sesquioleate - - - - - 1.5  C: water-soluble phase  Propylene glycol 1.5 1.5 0.9 1.5 1.5 1.5  Purified water to 100

The instrument used to measure the particle size of nanoemulsions is a laser called Mastersizer 2000 (Malvern Instrument, UK) which measures the particle size of a solution by kinetic light scattering. The particle size of the nano-emulsion was measured under the following conditions by diluting with purified water such that the turbidity of the nano-emulsion was 10-20%. Measurement time: 2 minutes, number of measurements per second: 5 × 10 ³ , temperature: 20 ° C., viscosity: 0.89 centipoise, particle refractive index: 1.4, dispersion refractive index: 1.33

The particle size of the nanoemulsion was measured twice after 1 day storage at room temperature and 6 months storage at 40 ° C. after the preparation. Thermodynamic stability was evaluated.

The particle size of the oil-in-water base nanoemulsion base cosmetic compositions of Table 1 and the comparative composition is measured 1 day after the preparation and after 6 months storage at 40 ℃ is shown in Table 2.

Table 2. Emulsion particle size measurement results and visual observation stability% for the compositions of Examples 1-3 and Comparative Examples 1-3 of Table 1

Prescription No. Particle size, nm Grain size increase% Visual observation oil painting stability% After manufacture, store at room temperature for 1 day 6 months after storage at 40 ℃ Example 1 206 220 6.8 98 Example 2 215 239 11.1 96 Example 3 306 352 15.0 92 Comparative Example 1 1,670 2,345 40.4 35 Comparative Example 2 1,485 2,585 74.0 42 Comparative Example 3 2,585 3,947 52.7 37

As can be seen from Table 2, the size of the emulsion particles obtained in the emulsification method by simple stirring at normal pressure using the propeller stirrer of Examples 1-3 of the present invention was nanoemulsion both after one day of preparation and after six months storage at 40 ° C. It also corresponds to the particle size defined in, and the increase in emulsified particle size after 6 months storage at 40 ℃ also showed a relatively small increase in particle size within 15%. On the other hand, the emulsion particle size of the composition obtained in Comparative Example 1-3 is far beyond the particle size defined in the nanoemulsion, and it can be seen that the emulsion particle size after 6 months storage at 40 ° C. was increased to about 40.4-74.0%. Therefore, it can be seen that the oil-in-water type nanoemulsion base compositions for skin protectants and skin treatments of Examples 1-3 are nanoemulsions and have excellent stability of their particles. On the other hand, the compositions of Comparative Examples 1-3 are normal emulsions (macroemulsion) in terms of the particle size of their emulsions, and it can be seen that the particles after 6 months of storage at 40 ° C. are significantly larger. Particularly, the composition using the phosphatidylcholine emulsifier of Comparative Example 2, which is known to make nanoemulsions when emulsified with a high-pressure homogenizer, also does not produce nanoemulsions and the stability of the particles is not good. Therefore, it can be seen that the POP-POE vitamin used in the present invention is an excellent nanoemulsion emulsifier.

Test Example 2 Emulsification Stability by Visual Observation

The emulsification stability of the oil-based base nanoemulsion compositions for skin protectants and skin treatments obtained in Examples 1-3 can be measured by particle size, but can also be evaluated by observing macroscopic changes with the naked eye. . The compositions of the prepared examples were nutrientd and the emulsion state after 6 months storage at room temperature and 40 ° C. was compared with the state immediately after preparation. Unstable conditions are observed visually with sedimentation, separation, drainage, creaming, and coalescing. Emulsification stability evaluates the unstable part of the whole as a percentage of the limiting stable part.

Emulsification stability% = (total-instability) / total × 100%

Table 2 shows the emulsion stability by visual observation after storage for 6 months at 40 ° C. of the oil-based base nanoemulsion compositions for skin protectants and skin treatments obtained in Examples 1-3. As can be seen from Table 2, the composition of Examples 1-3 can be seen that the emulsification state is quite stable. On the other hand, the emulsification state of the compositions of Comparative Examples 1-3 was unstable, especially severe separation occurred at the base.

Test Example 3 Evaluation of Emulsification Stability by Microscopic Observation

The emulsion stability of the oil-based base nanoemulsion compositions for skin protectants and skin treatments obtained in Examples 1-3 can be confirmed by particle size measurement, visual observation, etc., but microscopically, the emulsion stability can be evaluated in more detail. have. The microscope used in this test (Olympus BH2, Japan) is a microscope with a digital camera that can be observed by polarized light. As a result of observing the emulsions of Examples 1-3 and Comparative Examples 1-3, the emulsions of the Compositions of Examples 1-3 had little change in phase even after 6 months storage at 40 ° C. The emulsion has had many phase changes. This is in good agreement with the results of Table 2 obtained by particle size measurement. Representatively, microscopic observation photographs are shown in FIG. 1 (particle size 206 nm) and FIG. 2 (particle size 220 nm) after 1 day of preparation and 6 months of storage at 40 ° C for nanoemulsion of the composition of Example 1 of the present invention. It was. It can be seen that the state of the emulsion particles in Figures 1 and 2 is almost unchanged. It is also observed that the layers of the emulsifier adsorbed at the interface of the emulsified particles are clearly seen and they are not completely separated from each other but are connected. This is considered to be the reason for stabilizing the nanoemulsion of this example dramatically. (Based on the 22nd IFSCC Edenburgh Congress Proceedings, Novel nanoemulsions of POP-POE tocopheryl ether, Kim Young Dae and 3 others)

Test Example 4 Viscosity Measurement

Viscosity of the emulsified phase of the oil-in-water type nanoemulsion base compositions for skin protectants and skin treatments obtained in Examples 1-3 was measured to determine the relationship between stability and viscosity. Viscosity was measured at 30 ° C using a Brookfield Viscometer LV and the measurement results are shown in Table 3.

Table 3. Viscosity measurement results for the compositions of Examples 1-3 and Comparative Examples 1-3 of Table 1.

Composition Viscosity, centi poise Viscosity decrease% Spindle No./RPM 1 day after room temperature after manufacture 6 months after 40 ℃ Example 1 2,670 2,530 6.7 3/12 Example 2 2,335 2,240 4.2 3/12 Example 3 95 87 8.8 2/60 Comparative Example 1 150 - - 2/60 Comparative Example 2 250 - - 2/60 Comparative Example 3 180 - - 2/60

As can be seen in Table 3, the oil-in-water base nanoemulsion compositions for skin protectants and skin treatments obtained in Examples 1-2 showed a very high viscosity and the composition of Example 3 had a very low viscosity but was not separated. There was no significant decrease in viscosity even after 6 months at 40 ° C. On the other hand, the compositions of Comparative Examples 1-3 showed very low viscosity, and after 6 months of storage at 40 ° C., all of them were separated, and thus the viscosity was not measured. In view of the above results, the POP (20) -POE (50) vitamin E used in Examples 1-3 of the present invention was adsorbed well at the interface of the emulsified particles, and the emulsified particles were closely packed by decreasing the particle size. As the networks are formed with each other, it is judged that the viscosity is high. Also, as shown in FIGS. 1 and 2, a significant bonding force acts between the adsorbed adsorbents, which causes the viscosity to increase, and also prevents particles from approaching and coalescing each other. It is thought that emulation became more stable. However, the smaller the internal phase of the emulsion, the greater the distance between the particles, and this effect is reduced, and it is considered that the viscosity was low in Example 3.

Test Example 5. Human Patch Test

In order to confirm the safety of the nano-emulsion was carried out a human patch test for the compositions of Examples 1-3 and Comparative Examples 1-3 of Table 1. Conventional nanoemulsions up to now have to be careful because the particles are small and relatively many emulsifiers (about 5% or more) are used for this, which is likely to cause safety problems. Phospholipids, in particular, are safe, but nanoemulsions that are made using about 5% are often known to cause skin stability problems. Finn Chamber patch test was performed on 50 women aged 18-50 years with respect to the oil-based base nanoemulsion compositions for skin protectors and skin treatments obtained in Examples 1 to 3 of the present invention. Is shown.

As can be seen from Table 4, the oil-in-water base nanoemulsion compositions for skin protectors and skin treatments obtained in Examples 1-3 of the present invention show superior safety than the compositions of the comparative examples despite the 5% emulsifier. .

Table 4. Human patch test results for the compositions of Examples 1-3 and Comparative Examples 1-3 of the present invention in Table 1

Composition Irritation rate (n = 50) 4 hours later 48 hours later Average Example 1 0 0 0 Example 2 0 0 0 Example 3 0.1 0 0.05 Comparative Example 1 0.3 0.2 0.25 Comparative Example 2 0.24 0.14 0.19 Comparative Example 3 0.4 0.2 0.30

Example 4-5 and Comparative Example 4-5: Oil-in-water nanoemulsion cream composition for skin protection

According to the composition of Table 5, oil-based raw material No. Raw material No. 1-9 and emulsifier 10-14 is injected into the tank and heated to 70 ° C. Next, raw material No. Aqueous ingredient No. 23 except 23. 18-22 as raw material No. About 70% of the 24 is injected into the tank injected, heated to 70 ° C., then injected into the tank in which the oil phase component is dissolved, and slowly stirred to form a high viscosity two-phase complex in which the oil phase and the water phase are combined. The composite was stirred with a propeller stirrer at a rate of about 1000-2500 RPM at normal pressure to form a homogeneous emulsion, cooled to 50 ° C. and then the oil phase component No. 15-17 was added and stirred uniformly again, and the remaining raw material No. heated to 50 ° C. 50% purified water in which 23 was dissolved was added thereto, stirred again at high speed, and cooled to 35 ° C to prepare an oil-in-water type nanoemulsion for skin protection. The composition of Comparative Example 4-5 was also prepared in the same manner as in Example 4-5.

Test Example 1: Evaluation of nanoemulsion stability by measuring particle size of particle and changing particle size

To determine if the skin protector oil-in-water type nanoemulsion compositions obtained in Examples 4-5 had particles of actual nanoemulsion units and to change the size of the particles upon long-term storage of these nanoemulsions at high temperature (40 ° C.). The particle size of the composition of Example 4-5 and the compositions of Comparative Example 4-5 was measured in the same manner as in Test Example 1 of Examples 1-3 to evaluate the stability by the change in particle size.

Table 5. Example 4-5 and Comparative Example 4-5: Skin protectant oil-in-water nanoemulsion cream composition

          Ingredient Example 4 Example 5 Comparative Example 4 Comparative Example 5 One Beeswax 3.0 3.0 3.0 3.0 2 Paraffin wax 2.0 2.0 2.0 2.0 3 Cetostearyl alcohol 3.0 3.0 3.0 3.0 4 Glyceryl Monostearate 2.0 2.0 2.0 2.0 5 Paraffin oil 25.0 25.0 25.0 25.0 6 Squalane 25.0 25.0 25.0 25.0 7 Moon Dog Colostrum 2.0 2.0 2.0 2.0 8 Methylparaben 0.2 0.2 0.2 0.2 9 Butylhydroxytoluene 0.1 0.1 0.1 0.1 10 POP (25) -POE (55) Vitamin E 4.5 4.5 - - 11 POP (5) -POE (2) vitamin E 0.5 0.5 0.5 0.5 12 POE (40) vitamin E - - 4.5 - 13 Polysorbate 60 - - - 3.8 14 Sorbitan sesquioleate - - - 0.7 15 Vitamin A 0.5 - 0.5 - 16 Vitamin E 0.5 0.5 0.5 0.5 17 Spices Quantity Quantity Quantity Quantity 18 glycerin 8.5 8.5 8.5 8.5 19 Propylene glycol 5.0 5.0 5.0 5.0 20 Hyaluronic acid 1.0 1.0 1.0 1.0 21 EDTA-2Na 0,1 0.1 0.1 0.1 22 Bilberry Extract 1.0 1.0 1.0 1.0 23 Ascorbic acid - 2.0 - 2.0 24 Purified water to 100

Table 6.Emulsion particle size measurement results and visual observation stability% of the compositions of Example 4-5 and Comparative Example 4-5 of Table 5

Prescription No. Particle size, nm Grain size increase% Visual observation oil painting stability% After manufacture, store at room temperature for 1 day 6 months after storage at 40 ℃ Example 4 235 242 3.0 99 Example 5 189 197 4.2 96 Comparative Example 4 2.670 4,345 62.7 65 Comparative Example 5 3.485 8,585 146.3 62

Table 6 shows the results of measuring the particle size of the skin protector oil-in-water type nano-emulsion cream compositions of Table 5 and the comparative example compositions after 1 day of preparation and 6 months storage at 40 ℃.

As can be seen from Table 6, the size of the emulsion particles obtained in the emulsification method by simple stirring using the high speed stirrer of Example 4-5 of the present invention is defined in nanoemulsion both after one day of preparation and after 6 months storage at 40 ° C. The increase in emulsified particle size after 6 months storage at 40 ° C. was relatively small, within 4.2%. On the other hand, the emulsion particle size of the composition obtained in Comparative Example 4-5 is far beyond the particle size defined in nanoemulsion, and it can be seen that the emulsion particle size after 6 months storage at 40 ° C. was increased to about 62.7-146.3%. Therefore, it can be seen that the skin-protective oil-in-water type nanoemulsion base composition of this Example 4-5 is clearly nanoemulsion and has excellent stability of their particles. On the other hand, the composition of Comparative Example 4-5 is a general emulsification (macroemulsion) in terms of the particle size of their emulsification, it can be seen that the particles after 6 months storage at 40 ℃ significantly increased. In particular, the compositions of Comparative Examples 3 and 4 using emulsifiers known to make general emulsifiers when emulsifying with general homogenizers did not produce nanoemulsions but produced general emulsification and the stability of the particles was not good. have.

Test Example 2 Emulsification Stability by Visual Observation

The emulsification stability of the skin-protective oil-in-water type nano-emulsion compositions obtained in Example 4-5 can be measured by particle size, but can also be evaluated by observing macroscopic changes with the naked eye. same.

Table 6 shows the results of emulsification stability measurement by visual observation after storage for 6 months at 40 ° C. of the oil-in-water type nanoemulsion compositions obtained in Example 4-5. As can be seen in Table 6, the nanoemulsion composition of this Example 4-5 can be seen that the emulsion state is quite stable. On the other hand, the emulsification state of the general emulsified composition of Comparative Example 4-5 was unstable, especially drainage and oil separation phenomenon in the base and upper portion.

Test Example 3 Evaluation of Emulsification Stability by Microscopic Observation

The emulsification stability of the skin-protective oil-in-water type nano-emulsion compositions obtained in Example 4-5 can be confirmed by particle size measurement, visual observation, etc., but microscopically, the emulsion stability can be evaluated in more detail. As in Test Example 3 of 1. As a result of observing the emulsion of Example 4-5 and Comparative Example 4-5, the emulsion of the composition of Example 4-5 had almost no change in phase even after 6 months storage at 40 ° C. The emulsion has had many phase changes. This is in good agreement with the results in Table 6 obtained by particle size measurement.

Test Example 4: Test Effect

     In order to measure the effect of the skin protector oil-in-water type nano-emulsion compositions obtained in Example 4-5, 80 women in their 20s to 50s were divided into four groups, and the use of the product was evaluated for three months. Example 4 and Comparative Example 4 focused on the wrinkle improvement effect, Example 5 and Comparative Example 5 focused on the whitening effect and other items such as stickiness, spreading on the skin, moisture, skin shine, etc. The evaluation was carried out by dividing into very good, good, normal, and poor, and the results are shown in Table 7. As can be seen from Table 7, Example 4 of the present invention showed a better wrinkle improvement effect than Comparative Example 4 and other items also showed very good results, Comparative Example 4 showed a good result and Example 5 was Comparative Example 5 It showed a better whitening effect. These results can be seen that the compositions of Examples 4 and 5 were easy to penetrate the skin as nano-emulsion of small particles, Comparative Examples 4 and 5 was not easy to penetrate the skin as a general emulsification, and the surface was rough.

Table 7 Example 4-5 and Comparative Example 4-5: Effect of Experimental Use of Oil-in-water Type Nano Emulsion Cream Composition for Skin Protection

Item / Product Example 4 Comparative Example 4 Example 5 Comparative Example 5   wrinkle improvement ○○ △ ○ △   Whitening effect  ○ △ ○○ △ Spreadability ○○ ○ ○○ ○ Smoothness ○○ ○ ○○ ○ Moist ○○ ○ ○○ ○ Skin shine ○○ × ○○ ×               ○○: Very good, ○: Good, △: Normal, ×: Poor

Example 6-7 and Comparative Example 6-7: Skin protectant oil-in-water type nanoemulsion lotion composition

According to the composition of Table 8, the raw material No. which is an oily component. Raw material No. 1-9 and emulsifier 10-14 is injected into the tank and heated to 70 ° C. Next, raw material No. No. which is water component except 23 18-22 as raw material No. About 30% of the 24 is injected into the tank

The mixture is heated to 70 ° C., and then injected into a tank in which an oil phase component is dissolved, and then slowly stirred to form a complex of a high viscosity oil phase and an aqueous phase. The composite was stirred at atmospheric pressure with a propeller stirrer at a rate of about 1000-2000 RPM to form a homogeneous emulsion, cooled to 50 ° C. and then the oil phase component No. 15-17 was added and stirred uniformly again, and the remaining raw material No. heated to 50 ° C. After dissolving 23, 70% purified water was added thereto, and the mixture was stirred at a high speed again and cooled to 35 ° C to prepare an oil-in-water nanoemulsion lotion for skin protection. The composition of Comparative Example 6-7 was also prepared in the same manner as in Example 6-7.

Table 8. Example 6-7 and Comparative Example 6-7: Oil-in-water type nanoemulsion lotion composition for skin protection

Ingredient Example 4 Example 5 Comparative Example 4 Comparative Example 5 One Cetostearyl alcohol 1.0 - 1.0 - 2 Vaseline 0.5 0.5 0.5 0.5 3 Shea Butter 1.0 1.0 1.0 1.0 4 Glyceryl Monostearate 1.0 1.0 1.0 1.0 5 Paraffin oil 25.0 20.0 25,0 20.0 6 Squalene 28.0 280 28.0 28.0 7 Sancho Milk 1.0 1.0 1.0 1.0 8 Phenoxyethanol 0.2 0.2 0.2 0.2 9 Butylhydroxyanisole 0.1 0.1 0.1 0.1 10 POP (30) -POE (70) vitamin E 4.0 4.0 - - 11 POP (5) -POE (0) Vitamin E 0.5 0.5 0.5 0.5 12 POE (18) Vitamin E - - 4 - 13 Polysorbate 80 - - - 3.2 14 Sorbitan monostearate - - - 0.8 15 Vitamin E 0.5 0.5 0.5 0.5 16 Spices 0.5 0.5 0.5 0.5 17 Panthenol 0.2 0.2 0.2 0.2 18 glycerin 8.5 8.5 8.5 8.5 19 Butylene glycol 5.0 5.0 5.0 5.0 20 Beta Glucan 1.0 1.0 1.0 1.0 21 EDTA-2Na 0,1 0.1 0.1 0.1 22 Allantoin 0.2 0.2 0.2 0.2 23 Bilberry Extract 2.0 2.0 2.0 2.0 24 Purified water to 100

Experimental Example 1 Nano-Emulsion by Measuring Particle Size and Particle Size

Stability evaluation

In order to confirm that the skin protector oil-in-water type nanoemulsion compositions obtained in Examples 6-7 had particles in actual nanoemulsion units and these nanoemulsions were changed in particle size upon prolonged storage at high temperature (40 ° C.) The particle size of the composition of Example 6-7 and the compositions of Comparative Example 6-7 was measured in the same manner as in Test Example 1 of Examples 1-3 to evaluate the stability by the change in particle size. Table 9 shows the particle size of the skin-protective oil-in-water type nanoemulsion lotion compositions of Examples 6-7 of the present invention of Table 8 and Comparative Example 6-7 compositions after 1 day of preparation and 6 months after storage at 40 ° C. The measurement result is shown.

Table 9. Emulsion particle size measurement results and visual observation stability% for the compositions of Example 6-7 and Comparative Example 6-7 of Table 8

Prescription No. Particle size, nm Grain size increase% Visual observation oil painting stability% After manufacture, store at room temperature for 1 day 6 months after storage at 40 ℃ Example 6 274 285 4.0 97 Example 7 289 317 9.7 94 Comparative Example 6 1,970 6,345 222.0 55 Comparative Example 7 2,485 7,585 205.0 46

As can be seen from Table 9, the size of the emulsion particles obtained in the emulsification method by simple stirring using the high speed stirrer of Example 6-7 of the present invention is defined in the nanoemulsion both after one day of preparation and after 6 months storage at 40 ℃. In addition, the increase in emulsified particle size after 6 months storage at 40 ° C. also showed a relatively small increase in particle size. On the other hand, the emulsion particle size of the composition obtained in Comparative Example 6-7 is far beyond the particle size defined in nanoemulsion, and it can be seen that the emulsion particle size after 6 months storage at 40 ° C. was increased to about 205.0-222.0%. Therefore, it can be seen that the skin-protective oil-in-water type nanoemulsion base composition of this Example 6-7 is clearly nanoemulsion and has excellent stability of their particles. On the other hand, the composition of Comparative Example 6-7 is a general emulsification from the particle size of their emulsions, and it can be seen that the particles after storage for 6 months at 40 ° C. are significantly larger. In particular, it can be seen that the compositions of Comparative Examples 3 and 4 using emulsifiers known to make general emulsifiers when emulsifying with general homogenizers do not produce nanoemulsions as well as the particle stability thereof.

Test Example 2 Emulsification Stability by Visual Observation

The emulsification stability of the skin-protective oil-in-water type nano-emulsion compositions obtained in Example 6-7 can be measured by particle size, but can also be evaluated by observing macroscopic changes with the naked eye. same.

Table 9 shows the emulsion stability of the skin-protective oil-in-water type nano-emulsion compositions obtained in Example 6-7 by visual observation after 6 months storage at 40 ° C. As can be seen in Table 10, the nanoemulsion composition of this Example 6-7 can be seen that the emulsion state is quite stable. On the other hand, the emulsification state of the general emulsified composition of Comparative Example 6-7 was unstable, especially severe drainage and oil separation phenomenon in the base and upper portion.

Test Example 3 Viscosity Measurement

Viscosity of the emulsified phase of the oil-in-water type nanoemulsion base compositions for skin protectants and skin treatments obtained in Examples 1-3 was measured to determine the relationship between stability and viscosity. Viscosity was measured at 30 ° C using a Brookfield Viscometer LV and the measurement results are shown in Table 10.

Table 10. Viscosity measurement results for the compositions of Examples 6-7 and Comparative Examples 6-7 of Table 8.

Composition Viscosity, centi poise Viscosity decrease% Spindle No./RPM 1 day after room temperature after manufacture 6 months after 40 ℃ Example 6 4,370 4,250 2.7 3/12 Example 7 4,150 3,950 4.8 3/12 Comparative Example 6 3,550 - - 3/12 Comparative Example 7 2,510 - - 3/12

As can be seen in Table 10, the skin protection nanoemulsion lotion compositions obtained in Example 6-7 exhibited relatively high viscosity, and the viscosity decrease was small and stable even after 6 months storage at 40 ° C., but the compositions of Comparative Examples 6-7 were Since the viscosity was relatively low and severely separated when stored at 40 ° C. for 6 months, no viscosity was measured at this time. In view of the above results, the POP (30) -POE (70) vitamin E used in Example 6-7 of the present invention was adsorbed well at the interface of the emulsified particles, and the emulsified particles were closely packed by reducing the particle size. As shown in Figures 1 and 2, it is thought that the nanoemulsion is more stable because a significant bonding force acts between the adsorbed emulsifiers and prevents particles from approaching each other and coalescing.

Example 8-9 and Comparative Example 8-9: Oil-in-water nanoemulsion skin bleaching cream composition for skin treatment

According to the composition of Table 11, raw material No. which is an oily component. Raw material No. 1-9 and emulsifier 10-14 is injected into the tank and heated to 70 ° C. Next, raw material No. No. of water component except 20 18-20 as raw material No. About 50% of 22 is injected into a tank, heated to 70 ° C., and then injected into a tank in which an oil phase component is dissolved, and slowly stirred to form a complex of a high viscosity oil phase and an aqueous phase. Example 8 and Comparative Example 8 were prepared as a homogeneous emulsion with a homogenizer at room pressure, cooled to 50 ° C., and then the aqueous phase No. 15-17 was added and stirred uniformly again, and then heated to 50 ° C. 50% of the remaining 50% of purified water was added thereto, pH was adjusted to 4.0-6.0 as a raw material 21, and then emulsified with a homogenizer and cooled to 35 ° C. to prepare an oil-in-water type nanoemulsion cream for skin protection. Example 9 and Comparative Example 9 were prepared in the same process as in Example 8 and Comparative Example 8, except that a high speed propeller stirrer (1000-2500 RPM) was used instead of the homogenizer in the foregoing process.

Table 11.Example 8-9, Comparative Example 8-9: Oil-in-water nanoemulsion skin bleaching cream composition for skin treatment

Ingredient Example 8 Example 9 Comparative Example 8 Comparative Example 9 One Beeswax 1.0 1.0 1.0 1.0 2 Paraffin wax 2.0 2.0 2.0 2.0 3 Cetostearyl alcohol 3.0 3.0 3.0 3.0 4 Glyceryl Monostearate 3.0 3.0 3.0 3.0 5 Paraffin oil 20.0 20.0 20.0 20.0 6 Squalane 25.0 25.0 25.0 25.0 7 Dimethylpolysiloxane 0.5 0.5 0.5 0.5 8 Propylparaben 0.15 0.15 0.15 0.15 9 Methylparaben 0.1 0.1 0.1 0.1 10 POP (15) -POE (50) Vitamin E 4,5 4.5 - - 11 POP (5) -POE (2) vitamin E 0.5 0.5 0.5 0.5 12 POE (40) stearate - - 3.8 3.8 13 POE (25) propylene glycol stearate - - 0.7 0.7 14 Sodium Metasulfite 0.2 0.2 0.2 0.2 15 Sorbic acid 0.2 0.2 0.2 0.2 16 glycerin 10.0 10.0 10.0 10.0 17 Propylene glycol 5.0 5.0 5.0 5.0 18 Sodium Lauryl Sulfate 0.2 0.2 0.2 0.2 19 EDTA-2Na 0,1 0.1 0.1 0.1 20 Hydroquinone 2.0 2.0 2.0 2.0 21 Citric acid Quantity Quantity Quantity Quantity 22 Purified water to 100     Manufacturing Method: Equipment for Emulsification  Homogenizer  Propeller stirrer  Homogenizer  Propeller stirrer

Experimental Example 1 Nano-Emulsion by Measuring Particle Size and Changing Particle Size

Stability evaluation

In order to confirm that the oil-in-water type nanoemulsion skin bleaching cream compositions obtained in Examples 8-9 have the actual nanoemulsion unit particles and that these nanoemulsions are stored for a long time at high temperature (40 ° C.) The particle size of the compositions of Examples 8-9 and the compositions of Comparative Examples 8-9 was measured as in Test Example 1 of Examples 1-3 to measure the change in size to evaluate the stability by the change in particle size.

Table 12 shows the results of measuring the particle size of the oil-in-water type nano-emulsion skin bleaching cream compositions for skin treatments of Table 11 and the comparative example compositions after 1 day of preparation and after 6 months of storage at 40 ° C.

Table 12. Emulsion particle size measurement results and visual observation stability% for the compositions of Examples 8-9 and Comparative Examples 8-9 of Table 11

Prescription No. Particle size, nm Grain size increase% Visual observation oil painting stability% After manufacture, store at room temperature for 1 day 6 months after storage at 40 ℃ Example 8 306 338 10.5 95 Example 9 226 246 8.8 98 Comparative Example 8 1,750 2,645 51.1 72 Comparative Example 9 3,485 7,885 126.3 54

As can be seen from Table 12, the size of the emulsion particles obtained in the emulsification method using the homogenizer of Example 8 of the present invention and the simple stirring using the high speed stirrer of Example 9 was 6 days after the preparation and at 40 ° C. After months of storage, all of them correspond to the particle size defined in the nanoemulsion, and the increase in emulsified particle size after 6 months of storage at 40 ° C also showed a relatively small increase in particle size within 10.5%. On the other hand, the emulsified particle size of the composition obtained in Comparative Example 8-9 is far beyond the particle size defined in nanoemulsion. Particularly, the emulsified composition using the high speed stirrer of Comparative Example 9 has a particularly large particle and emulsified particles after 6 months storage at 40 ° C. It can be seen that the size is increased to about 126.3%. Therefore, it can be seen that the skin protector oil-in-water type nanoemulsion base composition of this Example 8-9 is clearly nanoemulsion and also excellent in stability of their particles. On the other hand, the composition of Comparative Examples 8-9 is a general emulsification from the particle size of their emulsions, and it can be seen that the particles after storage for 6 months at 40 ° C. have become considerably larger.

Test Example 2 Emulsification Stability by Visual Observation

The emulsification stability of the skin-type nanoemulsion skin bleaching cream compositions for skin treatments obtained in Examples 8-9 can be measured by particle size, but can also be evaluated by observing macroscopic changes with the naked eye. It is the same as Test Example 2. Table 12 shows the emulsion stability of the skin-protective oil-in-water type nanoemulsion compositions obtained in Example 8-9 after visual observation after 6 months storage at 40 ° C. As can be seen from Table 12, the nanoemulsion composition of this Example 8-9 can be seen that the emulsification state is quite stable. On the other hand, the emulsification state of the general emulsion composition of Comparative Example 8-9 was unstable, especially Comparative Example 9 had a severe drainage and oil separation phenomenon in the base and upper portion.

Example 10-11 and Comparative Example 10-11: Oil-in-water type nano-emulsion acne treatment cream composition for skin treatment

According to the composition of Table 13, the raw material No. which is an oily component. Raw material No. 1-9 and emulsifier 10-14 is injected into the tank and heated to 70 ° C. Next, the raw material No. 17-21 as raw material No. About 50% of 22 is injected into a tank, heated to 70 ° C., and then injected into a tank in which an oil phase component is dissolved, and slowly stirred to form a high viscosity composite. This complex combines oil and water to form a complex. The composite was stirred with a propeller stirrer at a speed of about 1000-2500 RPM to form a homogeneous emulsion, cooled to 50 ° C., and then the raw material No. 15-16 was added and stirred uniformly again, and the remaining 50% of purified water heated to 50 ° C. was added thereto, stirred again at high speed, and cooled to 35 ° C. to prepare an oil-in-water type nano-emulsion acne cream for skin treatment. The composition of Comparative Example 10-11 was also prepared in the same manner as in Example 10-11.

Table 13. Example 10-11, Comparative Example 10-11: Oil-in-water type nano-emulsion acne treatment cream composition for skin treatment

Ingredient Example 10 Example 11 Comparative Example 10 Comparative Example 11 One Cetostearyl alcohol 3.0 3.0 3.0 3.0 2 Vaseline 0.2 0.2 0.2 0.2 3 Shea Butter 1.0 1.0 1.0 1.0 4 Glyceryl Monostearate 1.0 1.0 1.0 1.0 5 Paraffin oil 20.0 20.0 20.0 20.0 6 Squalene 15.0 15.0 15.0 15.0 7 Sancho Milk 5.0 5.0 5.0 5.0 8 Phenoxyethanol 0.2 0.2 0.2 0.2 9 Polydimethylsiloxane 0.5 0.5 0.5 0.5 10 POP (25) -POE (60) vitamin E 4.0 4.5 - - 11 POP (3) -POE (0) Vitamin E 0.5 0.5 0.5 0.5 12 POE (18) Vitamin E - - 4.5 - 13 Polysorbate 80 - - - 3.2 14 Sorbitan monostearate - - - 0.8 15 Spices 0.5 0.5 0.5 0.5 16 Sorbic acid 0.3 0.3 0.3 0.3 17 Sedimentation sulfur 1.0 1.0 1.0 1.0 18 1,3 butylene glycol 10.0 10.0 10.0 10.0 19 Zinc oxide 3.0 5.0 5.0 3.0 20 Sodium Metasulfite 0.1 0.1 0.1 0.1 21 Lactic acid 0.5 0.5 0.5 0.5 22 Purified water to 100

Experimental Example 1: Evaluation of nanoemulsion stability by measuring particle size of particle and changing particle size

Oil-in-water type nano-emulsions for skin treatments obtained in Examples 10-11 To check whether the acne treatment cream compositions have particles of actual nano-emulsion units and that these nano-emulsions are stored at high temperatures (40 ° C.) for long periods of time. The particle size of the composition of Example 10-11 and the compositions of Comparative Example 10-11 was measured in the same manner as in Test Example 1 of Examples 1-3 to measure the change in size to evaluate the stability due to the change in particle size. It was.

Table 14 shows the particle size of the oil-in-water type nano-emulsion acne treatment cream compositions for skin treatment of Examples 10-11 of the present invention of Table 12 and Comparative Example 10-11 compositions after 1 day and 6 at 40 ° C. Results measured after months storage are shown.

Table 14.Emulsion particle size measurement results and visual observation stability% of the compositions of Examples 10-11 and Comparative Examples 10-11 of Table 12

Prescription No. Particle size, nm Grain size increase% Visual observation oil painting stability% After manufacture, store at room temperature for 1 day 6 months after storage at 40 ℃ Example 10 415 458 10.4 98 Example 11 455 489 7.5 96 Comparative Example 10 2,570 5,295 106.0 63 Comparative Example 11 3,285 5,885 79.1 56

As can be seen from Table 14, the size of the emulsified particles obtained in the emulsification method by simple stirring using a high speed propeller stirrer at the atmospheric pressure of Example 10-11 of the present invention was measured on the nanoparticles after 1 day of preparation and after 6 months storage at 40 ° C. Corresponding to the particle size defined in Malsion, the increase in emulsified particle size after 6 months storage at 40 ° C also showed a relatively small increase in particle size within 10.4%. On the other hand, the emulsion particle size of the composition obtained in Comparative Example 10-11 is far beyond the particle size defined in nanoemulsion, and it can be seen that the emulsion particle size after 6 months storage at 40 ° C. was increased to about 79.1-106.0%. Therefore, it can be seen that the skin treatment oil-in-water type nano-emulsion acne treatment cream composition of this Example 10-11 is clearly nano-emulsion and the stability of their particles is also excellent. On the other hand, the composition of Comparative Example 10-11 is a general emulsification from the particle size of their emulsions, and it can be seen that the particles after storage at 40 ° C. for 6 months are significantly larger. In particular, the compositions of Comparative Examples 3 and 4 using emulsifiers known to make general emulsifiers when emulsifying with general homogenizers make general emulsification, not nanoemulsion, as well as the stability of the particles. have.

Test Example 2 Emulsification Stability by Visual Observation

The emulsification stability of the skin-protective oil-in-water type nano-emulsion compositions obtained in Example 10-11 can be measured by particle size, but can also be evaluated by observing macroscopic changes with the naked eye. same.

Table 13 shows the emulsification stability by visual observation after storage for 6 months at 40 ° C. of the oil-in-water type nanoemulsion compositions obtained in Example 10-11. As can be seen from Table 14, the nanoemulsion composition of this Example 10-11 can be seen that the emulsion state is quite stable. On the other hand, the emulsification state of the general emulsified composition of Comparative Example 10-11 was unstable, in particular there was a severe oil separation phenomenon in the upper portion.

The oil-in-water type nanoemulsion composition for skin protection and skin treatment of the present invention not only has the characteristics of making stable and safe nanoemulsion by using POP-POE vitamin E as an emulsifier, but also can be prepared simply by stirring at normal pressure. Excellent economical efficiency, excellent flexibility, skin moisturizing and skin elasticity effect in use and excellent spreadability, in particular, the composition for skin treatment has the advantage that the effective long-term effective long-term effective efficacy of the effective drug skin penetration.

Figure 1 shows a microscopic observation photograph (particle size 206 nanometers (nm)) after one day for the nano-emulsion of the composition of Example 1 of the present invention.

Figure 2 shows a microscopic observation picture (particle size 220nm) after storage for 6 months at 40 ℃ for nanoemulsion of the composition of Example 1 of the present invention.

Claims (8)

Oil-in-water type nanoemulsion containing an emulsifier, wherein the emulsifier is a polyoxypropylene-polyoxyethylene vitamin E represented by the following formula (1), characterized in that the nanoemulsion produced by the two-phase complex emulsification method Cosmetic composition: <Formula 1> In the above formula, R ₁ is — (O—CH ₂ CH ₂ ) _m , m is an integer from 0 to 250, R ₂ is H (OCH (CH ₃ ) CH ₂ ) _n −, n is an integer from 1 to 200, A is , B is CH _{3 at} the 5-, 7- or 8- position of vitamin E, and p is 1 or 3. The nanoemulsion cosmetic composition according to claim 1, wherein m is in the range of 20 to 150 and n is in the range of 5 to 120. The nano-emulsion cosmetic composition according to claim 1, wherein the vitamin E portion of the polyoxypropylene-polyoxyethylene vitamin E is natural or synthetic vitamin E. The nano-emulsion cosmetic composition according to claim 1, wherein the polyoxypropylene-polyoxyethylene vitamin E is used in an amount of 0.1 to 60% by weight. The nano-emulsion cosmetic composition according to claim 1, wherein the nano-emulsion cosmetic is in the form of any one of a cream, a lotion, and an essence. In the method for preparing a nano-emulsion cosmetics prepared using polyoxypropylene-polyoxyethylene vitamin E represented by the following formula (1) as an emulsifier, a water-soluble phase is mixed by mixing 30-100% of the water-soluble component and the total purified water. Method of producing a nano-emulsion cosmetic composition, characterized in that to add the oil-soluble phase to make a composite of high viscosity, and then add the remaining ingredients to the composite and emulsify again. <Formula 1> In the above formula, R ₁ is — (O—CH ₂ CH ₂ ) _m , m is an integer from 0 to 250, R ₂ is H (OCH (CH ₃ ) CH ₂ ) _n −, n is an integer from 1 to 200, A is , B is CH _{3 at} the 5-, 7- or 8- position of vitamin E, and p is 1 or 3. The method of claim 6, wherein the emulsifying method uses a high pressure homogenizer, a phase transition temperature principle, or an ultrasonic syringe. 7. The method of claim 6, wherein the emulsifying method further comprises using a high speed stirrer or homogenizer at normal pressure.