KR101151365B1 - Nano-emulsion composition using the high-pressure homogenizer - Google Patents

Abstract

The present invention relates to a nanoemulsifying composition using a high pressure homogenizer, and more particularly, 0.01 to 30% by weight of coenzyme Q10, 1 to 10% by weight of hydrogenated lecithin, which is an emulsifier, and tocopherol as an antioxidant by a high pressure homogenizer. The present invention relates to a nanoemulsion composition using a high pressure homogenizer having a stable, fine and stable particle size by preparing 0.1 to 1.0% by weight and a residual amount of glycerin as a dispersion medium.

Coenzyme Q-10, Hydrogenated Lecithin, High Pressure Homogenizer

Description

Nanoemulsification composition using high pressure homogenizer {NANO-EMULSION COMPOSITION USING THE HIGH-PRESSURE HOMOGENIZER}

The present invention relates to a nanoemulsion composition containing coenzyme Q10, and more particularly to a nanoemulsion composition using a high-pressure homogenizer capable of producing a uniform and fine nano-size highly stable emulsion composition using a high-pressure homogenizer. It is about.

Coenzyme Q is a powerful antioxidant that mediates electron transfer between flavin protein and cytochrome b in the respiratory metabolic electron transport system. It is responsible for the various body damage that can occur from free radicals. Inhibition (Grossi et al., 1992). In particular, coenzyme Q10 is present in the mitochondria, the energy generator, and is essential for the function of mitochondria in each cell. This substance is called ubiquinone (ubiquitous + quinone), which means it is widely distributed in the body (Concise Encyclopedia Biochemistry, Second Edition, Walter de Gruyter Berlin.New York 1988, p619). In addition, Ubidecarenone having an isoprenoid side chain n = 10 bound to the skeleton of benzoquinone is called coenzyme Q10 as a ubiquinone present in humans.

The body's ability to synthesize coenzyme Q-10 begins to decline in its mid-30s, and if that number drops, it can hurt your health. There are many reports that supplementing the deficiency of coenzyme Q-10 can help your organs function and restore your body's overall health. In Europe and the United States, it became a hot topic 10 years ago, and in 1998, Germany's Beiersdorf launched the anti wrinkle cream containing Coenzyme Q-10. Since the Ministry of Health, Labor and Welfare approved the use of coenzyme Q10 as a drug for congestive heart failure in 1974, it has been open to foods such as nutritional supplements in 2001 and recently recognized as a cosmetic ingredient.

Coenzyme Q-10 has the effect of inhibiting collagenase production to prevent photoaging (Coenzyme Q10, a cutaneous antioxdant and energizer. Bilfactors. 9 (1999) p371-378, Paul Gerson Unna Research Center, Beiersdorf AG, Hamburg, Germany). In addition, long-term use of coenzyme Q-10 has been reported to reduce wrinkles around the eyes (Modulation of oxidative stresses in human aging skin, Z Gerontol Geriatr. 32 (1999), p83-88).

However, Coenzyme Q10 is a yellow powder, unstable in air, and very poorly soluble in water. In particular, it is insoluble in cosmetic bases and is difficult to formulate. Thus, there have been efforts to introduce insoluble coenzyme Q10 into cosmetics. Accordingly, there is a growing need for nanotechnology to effectively release the active ingredient inside the formulation through the formulation process in a stable collection of the active ingredient.

For example, Korean Laid-Open Patent Publication No. 10-2005-0054012 discloses a method of manufacturing self-associating polymer nanoparticles. However, this method has a problem of using an organic solvent to dissolve coenzyme Q10.

Korean Patent Publication No. 2002-0080370 discloses a method for preparing a nanocomposite using cyclodextrin. In addition, US Pat. No. 6,107,276 discloses the preparation of coenzyme Q10 particles using TWEEN-80, while US Pat. No. 4,869,900 discloses monoglycerides, diglycerides, triglycerides of lecithin and hydrogenated palm oil. And palmitate-stearate of polyethylene glycol are used together to encapsulate coenzyme Q10. However, these methods have a problem that the percutaneous absorption is not fast due to the large particle size.

In addition, U. S. Patent No. 5,443, 842 discloses a method using PEG-40 hydrogenated castor oil, but the method has a complicated manufacturing process and takes a long time.

On the other hand, in general, lecithin itself is difficult to apply as a cosmetic raw material because the specific odor and seizure stability is not good and the peroxide value (POV, high) is high. Therefore, hydrogenated lecithin is used in which the lecithin is hydrogenated using a catalyst to convert the unsaturated fatty acid of the lecithin into a saturated fatty acid. Unlike the lecithin, the hydrogenated lecithin has been studied to improve stability (odor, POV value, etc.), which is suitable for use in cosmetics and excellent in skin stability (Kutz G., Biehi P., Waldmann-Laue M., Jackwerth B., SOFW-Journal, 123, 145-149 (1997)). In this case, an automatic oxidation measurement method is used as a measure of stability over time to measure peroxide value, which is obtained by monitoring POV and carbonyl value (COV) over time. Here, POV refers to the measurement of peroxide value as a measure of the automatic oxidation of the raw material itself, and COV refers to the measurement of carbonyl value (Japanese Society for Nutrition and Food Science Vol. 39, No. 5, P391 (1986)). ).

However, conventionally emulsified products using hydrogenated lecithin have been mainly used as auxiliary agents due to lowering of interfacial tension or lower emulsification ability than ordinary nonionic surfactants when hydrogenated lecithin is used as an oiling agent. In addition, as interest in nature increases and interest in natural emulsifiers in terms of safety of the skin increases, many emulsion compositions using natural emulsifiers such as lecithin have been developed. However, the emulsification ability of natural emulsifier lecithin has greater interfacial tension than general emulsifiers, and the emulsification capacity is reduced by only about 8 HLB (Hydrophilic Lipophilic Balance), so it is difficult to stabilize the emulsion by a general emulsification method. Only mechanical force was applied to emulsify hydrogenated lecithin to form molecular aggregates and form particles, reducing the particle size.

In addition, Korean Patent No. 0500643 contains 0.05 to 10.0 wt% of ascorbyl tetraisopalmitate, 0.1 to 10.0 wt% of coenzyme Q-10, and 0.01 to 10.0 wt% of tocopherol, based on the total weight of nanoemulsion particles, and an emulsifier. As an anti-oxidant skin external composition comprising nanoemulsified particles prepared by adding 3 to 10 wt% of lecithin as an antimicrobial agent. In addition, Korean Patent Publication No. 2001-0075886 discloses an emulsion composition for cosmetics using a high pressure homogenizer and hydrogenated lecithin. However, in the above methods, since water is used as the dispersion medium, unstable emulsified particles having a particle size of 100 nm or more are formed. That is, in general, when a moisturizing agent or purified water is used as the dispersion medium, the particle size becomes large and stability is low.

In order to solve the problems of the prior art, an object of the present invention is to use nanoemulsification using a high pressure homogenizer that can produce transparent and stable particles with a size of about 100 nm or less by using a simple manufacturing method without using water and organic solvents It is to provide the composition.

In order to achieve the above object, the present invention provides nanoparticles containing 0.01 to 30% by weight of coenzyme Q10, 1 to 10% by weight of hydrogenated lecithin, which is an emulsifier, 0.1 to 1.0% by weight of tocopherol as an antioxidant, and a residual amount of glycerin as a dispersion medium. It provides an emulsion composition.

In addition, the present invention provides a cosmetic prepared by using a nanoemulsified composition having the above-mentioned composition having a viscosity of 50 to 3000 cps and a particle size of 100 nm or less.

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

The present inventors used hydrogenated lecithin as an emulsifier to solve the insolubility problem of coenzyme Q10, glycerin as a dispersion medium of tocopherol as an antioxidant, and using a high pressure homogenizer, the manufacturing process is simple and the particle size is uniform. The present invention was completed by preparing a fine, nano-sized, very stable emulsion composition.

In the emulsion composition of the present invention, the content of coenzyme Q10 can be adjusted according to the purpose and the case. Preferably, when the content of the coenzyme Q10 exceeds 30% by weight, effective collection is not possible, and may be caused to flow out of the particles of the active ingredient, causing aggregation or degeneration in the crystalline form. It is recommended to use in weight percent.

The content of the hydrogenated lecithin as the emulsifier is used in an amount of 0.1 to 20% by weight, preferably 1 to 10% by weight based on the total composition. The hydrogenated lecithin used as an emulsifier in the present invention means a lecithin to which hydrogen has been added to the lecithin, and one prepared by hydrogenation using a catalyst in the lecithin is used.

The tocopherol is used as an oil-soluble antioxidant, the content is used in 0.01 to 5% by weight, preferably 0.1 to 1.0% by weight based on the total composition.

In particular, in the present invention, the particle size can be made small by using glycerin without using water as a dispersion medium as in the prior art, and there is a feature of improving the stability of the emulsified particles. The content of glycerin is included in the remaining amount relative to the total emulsion composition.

In addition, in the present invention, by using a high pressure homogenizer in the preparation of the emulsion composition, by increasing the emulsification capacity than the prior art to stabilize the particles in the composition having a uniform and fine nano-size.

In the method for preparing an emulsion composition of the present invention, the emulsion composition including the above components is firstly emulsified in a homomixer, and then passed through the high-pressure homogenizer one or more times to be secondly emulsified to provide a very stable emulsion having a uniform and fine nano size. A composition can be provided. The pressure of the high pressure homogenizer is a high pressure of 50 to 2500 atmospheres, preferably 200 to 1000 atmospheres.

The high pressure homogenizer is called high pressure emulsification, and refers to the second emulsification by passing an emulsion emulsified primarily by a general stirrer or a homomixer through a high pressure homogenizer. At this time, the process of atomizing the oil particles is to make the emulsified particles small by the pressure fluctuation, cavitation, impact force generated when the emulsion passes from the high pressure to atmospheric pressure 1 atm. When the emulsion is prepared, the homogenizer's emulsifying capacity is converted into energy, which is about 10,000 times larger than a general homomixer (Encyclopedia of Emulsion Technology, Vol 1, page 97 (19830)).

The particle size of the emulsion composition of the present invention prepared by this method is 100 nm or less, preferably 20 to 80 nm, the viscosity is 50 to 3000 cps.

The emulsion composition of the present invention can be applied to various cosmetic formulations such as skins, lotions and creams because the particle size is not only fine and uniform, but also transparent and low in viscosity.

Hereinafter, the present invention will be described in more detail with reference to Examples, but these Examples are only for illustrating the present invention, and the scope of the present invention is not limited by the following Examples.

Example  1 to 4 and Comparative example  1 to 6

The emulsion compositions of Examples 1 to 4 and Comparative Examples 1 to 6 were prepared according to the compositions and contents of Table 1 below. In the method of preparing the emulsion composition, hydrogenated lecithin, coenzyme Q10, tocopherol, and glycerin are mixed, heated to 70 ° C., uniformly stirred to make the first emulsion, and then the primary emulsion is passed through a high pressure homogenizer to undergo secondary emulsion. To prepare an emulsion composition. The working pressure of the high pressure homogenizer was 50 to 25000 atm, but it was cooled by passing once at 200 to 1000 atm.

[Table 1]

Category (% by weight) Example 1 Example 2 Example 3 Example 4 Example 5 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 glycerin To 100 To 100 To 100 To 100 To 100 To 100 To 100 To 100 To 100 To 100 Hydrogen Lecithin 1.0 3.0 5.0 5.0 5.0 5.0 - - 5.0 5.0 Coenzyme Q10 1.0 1.0 1.0 2.0 3.0 - 2.0 - 2.0 - Tocopherol 0.2 0.2 0.2 0.2 0.2 - - 0.2 - 0.2

Experimental Example

Temperature stability and average particle size and coenzyme Q10 long-term storage stability of the coenzyme Q10-containing nanoemulsion composition prepared in Examples and Comparative Examples were measured by the following method.

1) Temperature Stability Evaluation of Coenzyme Q10-Containing Nanoemulsified Compositions

The emulsion compositions of each of Examples and Comparative Examples prepared above were stored for 1 month under the conditions of 50 ° C., 0 ° C., and cycle (-10 ° C. 1 day → 45 1 day → -10 ° C. 1 day cycle), followed by separation and appearance. Changes, changes in particle size, and the like were observed to evaluate the stability as very good (◎), good (○), slightly separated (△), and completely separated (×), and the results are shown in Table 2.

TABLE 2

division Example 1 Example 2 Example 3 Example 4 Example 5 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 50 ℃ ○ ◎ ◎ ○ ○ ◎ × × ○ ◎ 25 ℃ ◎ ◎ ◎ ◎ ◎ ◎ × × ◎ ◎ 0 ℃ ◎ ◎ ◎ ◎ ○ ◎ × × ◎ ◎ cycle ○ ◎ ◎ ○ ○ ◎ × × ○ ◎

2) Measurement of particle average size of coenzyme Q 10 containing nanoemulsified composition

The particle average size of each of the prepared emulsion and comparative examples was measured immediately after preparation using a commonly used particle size analyzer (Particle Sizer), and the results are shown in Table 3.

[Table 3]

division Average diameter (nm) Example 1 240.4 Example 2 38.1 Example 3 35.2 Example 4 60.8 Example 5 118.5 Comparative Example 1 34.5 Comparative Example 2 Not measurable Comparative Example 3 Not measurable Comparative Example 4 60.6 Comparative Example 5 38.6

3) Evaluation of long-term storage stability of coenzyme Q10 in nanoemulsifying composition

The long-term storage stability of the coenzyme Q10-containing nanoemulsion composition of each of the above-prepared examples and comparative examples was confirmed. Coenzyme Q10 content was measured using HPLC (HP-1100, HEWLETT PACKARD Co.) and the results are shown in Table 4.

(How to measure)

About 3mg of Coenzyme Q10 was precisely weighed and dissolved in ethanol to make 100ml. After sonication, a 0.45㎛ filtration membrane was used as the sample solution. Separately, 3 mg of coenzyme Q10 standard was precisely weighed, dissolved in ethanol, and used as a standard solution. Using the test solution and 30 µl each, the peak area of coenzyme Q10 was determined by testing according to the liquid chromatograph method under the following conditions.

[Table 4]

division Condition 7 days 15th 30 days 45 days Example 4 25 ℃ 100% 100% 98% 97% 45 ° C 100% 100% 98% 95% Comparative Example 4 25 ℃ 100% 98% 95% 86% 45 ° C 100% 96% 89% 80%

The nanoemulsifying composition of the present invention includes hydrogenated lecithin, tocopherol as an antioxidant and glycerin as a dispersion medium, and emulsified using a high pressure homogenizer, thereby providing a uniform and fine nano-sized, very stable emulsion composition. Therefore, since the composition of the present invention is transparent and low in viscosity, it is applicable to various cosmetic formulations such as skins, lotions and creams.

Claims (5)

A nanoemulsion composition comprising 0.01 to 30% by weight of coenzyme Q10, 1 to 10% by weight of hydrogenated lecithin, which is an emulsifier, 0.1 to 1.0% by weight of tocopherol as an antioxidant, and a balance of glycerin as a dispersion medium. delete First emulsifying the composition according to claim 1 with a homomixer; And 2nd emulsification by passing it through the high pressure homogenizer at least once Method for producing a nano-emulsion composition comprising a. The method of claim 3, wherein the pressure of the high pressure homogenizer is 50 to 2500 atmospheres. delete