KR102309639B1 - Oil-in-water nano emulsion cosmetic composition containing high content oil - Google Patents

Abstract

The present invention includes a polymer surfactant, an ionic surfactant and a phospholipid, and the mixed weight ratio of the polymer surfactant and the ionic surfactant is 50:1 to 0.5:1, by providing an oil-in-water cosmetic composition and a method for preparing the same , It has excellent long-term stability and temperature stability, and is a translucent liquid formulation unique to nanoemulsion, and has a high viscosity formulation.

Description

Stable oil-in-water nano emulsion cosmetic composition containing high content oil

It relates to a stable oil-in-water nanoemulsion cosmetic composition containing a high oil content.

Cosmetics are mainly prepared in the form of an emulsion because various substances that do not dissolve with each other, such as water-soluble ingredients, oil-soluble ingredients, and active ingredients, must be mixed in order to moisturize and protect the skin and maintain skin health. In the emulsion-related technology, various emulsification methods have been studied so that not only formulation preparation and stabilization, but also efficacy and feeling of use can be improved according to the purpose of each product.

When the droplet size of the emulsion is reduced to nano level, the physical stability of the emulsion is greatly improved. In addition, a low-viscosity emulsion with high transparency can be manufactured to make cosmetics with various feeling of use, and the surface area is large and the particle size is small, which has the advantage of effectively delivering active ingredients to the skin.

In order to prepare a nanoemulsion, an in-bed temperature emulsification method or a high pressure emulsification method has been used. However, nanoemulsions prepared in the prior art generally contain about 5% oil, and it is difficult to secure long-term stability and high temperature stability when trying to stabilize a high content of oil in a translucent emulsion. In addition, since a large amount of surfactant is used together to stabilize the oil, it is sticky, stuffy, and has a poor feeling of use, and also has a problem of causing skin irritation.

Under this technical background, research on a technology for stably dispersing a high content oil in a nanoemulsion is being actively conducted (patent application KR 10-2013-0062912), but it is still insufficient.

One aspect is to provide an oil-in-water cosmetic composition comprising a polymer surfactant, an ionic surfactant, and a phospholipid, and the mixed weight ratio of the polymer surfactant and the ionic surfactant is 50:1 to 0.5:1.

One aspect is i) dissolving a polymer surfactant in a solvent to prepare a polymer surfactant solution; ii) preparing an aqueous solution by dispersing the polymer surfactant solution in an aqueous phase component; iii) preparing an oily solution by dissolving an oil phase containing oil and phospholipids; and iv) high-pressure emulsification after mixing the aqueous phase solution and the oil phase solution, wherein the high-pressure emulsification is performed 2 to 5 times at a pressure of 200 to 1500 bar, and the oil has a high content of 30 to 60% by weight It is to provide a method for preparing the oil-in-water cosmetic composition of claim 1 comprising a.

One aspect provides an oil-in-water cosmetic composition comprising a polymer surfactant, an ionic surfactant, and a phospholipid, and a mixing weight ratio of the polymer surfactant and the ionic surfactant is 50:1 to 0.5:1.

The polymer surfactant is a polymer compound having a plurality of hydrophilic moieties and hydrophobic moieties in a molecule, and may refer to a compound exhibiting surface activity. It may refer to a copolymer including two or more from polymers and derivatives thereof, and may be 0.1 to 10, 0.5 to 10, 2 to 10, 2 to 8% by weight based on the total weight.

The ionic surfactant includes both anionic surfactants, cationic surfactants, and amphoteric surfactants, and includes glycinates, sarcosinates, glutamates, alaninates, and tau. Taurates, sulfosuccinates, carboxylates, alkyl phosphates, alkyl sulfates, alkyl ether sulfates, amphoacetates, alkyl Amidopropyl betaines (alkyl amidopropyl betaines), sulfo betaines (sulfo betaines), alkyl betaines (alkyl betaines), quaternary ammonium (quaternary ammonium), etc. may include, sodium sulfactin It may contain a water-soluble metal salt derived from a surfactant of the same polypeptide family and a simple fatty acid and glyceride. It may be included in 0.01 to 9, 0.3 to 5, 0.3 to 1% by weight relative to the total weight, and when included in less than the range, the effect on the stability and viscosity of the nanoemulsion may be insignificant. there may be

The phospholipids include phosphatidylcholine (PC), phosphatidylserine (PS), phosphatidylethanolamine (PE), phosphatidylinositol (PI), phosphatidylglycerol (phosphatidylserine, PS), phosphatidylglycerol (PG), ) containing at least one of egg yolk lecithin, soybean lecithin, milk lipid, etc. and natural phospholipids and hydrogenated products of natural phospholipids, dimyristoyl phosphatidyl choline (DMPC), dilauryl phosphatidyl ethanolamine (dilauryl Synthetic lipids such as phosphatidyl ethanolamine, DLPE) and distearoyl phosphatidyl serine (DSPS) may include at least one of the above natural phospholipids and derivatives of synthetic lipids. 0.5 to 3, 0.5 to 1.5, 1 to 1.5% by weight relative to the total weight may be included.

The mixing weight ratio of the polymer surfactant and the ionic surfactant may be 50:1 to 0.5:1, preferably, 30:1 to 0.5:1, 20:1 to 0.5:1, 10:1 to 0.5: can be 1.

In one embodiment, the mixing weight ratio of the ionic surfactant and the phospholipid is 1:1 to 1:30 to provide an oil-in-water cosmetic composition.

The mixing weight ratio of the ionic surfactant and the phospholipid may be preferably 1:1 to 1:20, 1:1 to 1:10, 1:1 to 1:5, 1:1 to 1:3.

One aspect is i) dissolving a polymer surfactant in a solvent to prepare a polymer surfactant solution; ii) preparing an aqueous solution by dispersing the polymer surfactant solution in an aqueous phase component; iii) preparing an oily solution by dissolving an oil phase containing oil and phospholipids; and iv) mixing the aqueous phase solution and the oil phase solution and then high-pressure emulsification, wherein the high-pressure emulsification is 2 to 5 times, 2 to 4 times, 3 to 5 times, or 2 and It is made three times, and the oil provides a method for preparing the oil-in-water cosmetic composition comprising a high content of 30 to 60% by weight.

In the high-pressure emulsification, when less than 150 bar, a small amount of energy can be applied compared to the energy required to implement the nano-emulsion particles, and when it exceeds 2000 bar, there is a possibility of phase separation at an oil content of 30% or more, and the high-pressure emulsifier may be difficult. . The pressure range of the high pressure emulsification may be 200 to 1500, preferably 200 to 1000, 200 to 800, 300 to 700 bar.

The solvent has a dissolving power for polymers at a typical emulsification temperature of 60 to 80 ° C. Alcohols such as ethanol and isopropyl alcohol used in cosmetic compositions, propylene glycol, butylene glycol, dipropylene glycol , and diols including methylpropanediol and polyols such as glycerin, diglycerin, polyglycerin, and sorbitol, but are not limited thereto, and may be used in one or a mixture of two or more. The solvent is included in an amount of 1 to 15% by weight based on the total weight, and when it contains 20% or more, there is a problem of exhibiting instability during long-term observation at high temperature or room temperature.

The oil may be emulsified in an amount equal to or greater than that of the surfactant, and may contain up to 60% of the total content, and there is a possibility of phase separation by a strong external force applied during high pressure emulsification at a content higher than this. The oils include octyldodecyl myristate, cetylethyl hexanoate, caprylic/capric triglyceride, isopropyl palmitate, neopentyl glycol caprate, triethylhexanoin, ethylhexyl stearate, penta Ester oil containing erythrityl tetraethyl hexanoate, dicaprylyl carbonate, hydrocarbon oil containing paraffin type, olefin type, squalane, hydrogenated polydecene, macadamia seed oil, meadow foam seed oil, Vegetable oils such as olive oil and waxes with a low melting point such as shea butter and hydrogenated vegetable oil may be used, and silicone oils including dimethicone, cyclomethicone, alkylsiloxane and cycloalkylsiloxane may be partially included.

The oil may be included in 0.5 to 60% by weight relative to the total weight of the cosmetic composition, preferably 30 to 60, 30 to 55, 30 to 50, 40 to 60, 40 to 50% by weight of a high content. In this case, "content of oil" means the total amount of oil phase components that do not include the emulsion stabilizer, and when it is added in approximately 30% by weight or more, it may mean that a high content of oil is added.

The oil-in-water cosmetic composition may have a high viscosity formulation. The viscosity may be 10000 to 40000, 15000 to 40000, 20000 to 40000, 25000 to 40000 cps.

The blending amount of the additional ingredients such as the preservative can be easily selected by those skilled in the art within the range that does not impair the purpose and effect of the present invention, and the blending amount may be 0.001 to 40% by weight based on the total weight of the composition.

There is no particular limitation on the cosmetic containing the oil-in-water cosmetic composition according to the present invention, but it can be used on the skin, mucous membrane, scalp or hair, for example, the basis of softening lotion, nutrient lotion, cream, pack, gel, patch, etc. It can be used in cosmetics, color cosmetics such as lipstick, makeup base and foundation, shampoo, conditioner, body cleanser, toothpaste, mouthwash, etc. have.

A person skilled in the art can select any additional ingredients and/or amounts thereof such that the advantageous properties of the composition according to the present disclosure are not adversely or substantially not adversely affected by the expected addition.

Numerical values set forth herein are intended to include the meaning of “about” even if not specified. For example, the numerical values set forth above may vary by 10%, 5%, 2%, or 1%. In some embodiments, the value may vary by 5%, 2%, or 1%. For example, a value of 5 is meant to include any value between 4.5 and 5.5, between 4.75 and 5.25, or between 4.9 and 5.1, or between 4.95 and 5.05 having a range of approximately 5.

In view of the skill level of those of ordinary skill in the art, the cosmetic composition can be prepared by a conventional manufacturing method including the heating, mixing and cooling.

All technical terms used above have the same meaning as commonly understood by those skilled in the art, unless otherwise defined.

The oil-in-water nanoemulsion cosmetic composition comprising a high content oil according to the present invention has excellent long-term stability and temperature stability, and is a translucent liquid formulation unique to the nanoemulsion, and may have a high viscosity formulation.

1 is a view comparing the transparency of Example 3 and Comparative Examples 1 to 3;
2 is a particle size analysis result for Example 3.

Hereinafter, the present invention will be described in more detail through examples. However, the Examples and Test Examples according to the present invention may be modified in various other forms, and the scope of the present invention should not be construed as being limited to the Examples and Test Examples described below. Examples and test examples of the present invention are provided to more completely explain the present invention to those of ordinary skill in the art. In addition, although preferred methods and samples are described herein, similar or equivalent ones are also included in the scope of the present specification.

1. Preparation of oil-in-water nanoemulsion cosmetic composition

Examples 1 to 3 of oil-in-water nanoemulsion cosmetic compositions were prepared in the following manner with the components and composition ratios shown in Table 1 below.

After measuring the alcohol solvent and the surfactant polymer among the aqueous phase components of A, the mixture was uniformly dissolved at 80°C, and then evenly stirred with purified water heated to 80°C and the rest of the components. The oily component of B was weighed and completely dissolved by heating at 80° C., mixed with A, stirred at 7000 rpm for 15 minutes with a homo-mixer, added C, and further stirred for 3 minutes. After cooling to a temperature of 40°C or less, using M-110F Microfluidizer®, high-pressure emulsification was performed three times at 400 bar, followed by cooling at 30°C.

Comparative Examples 1 to 3 were also prepared in the same manner.

ingredient Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 A: Award menstruum Butylene Glycol 10.00 10.00 10.00 10.00 10.00 10.00 polymer surfactant PEG-PCL-PEG 5.00 5.00 5.00 5.00 5.00 - menstruum Purified water To 100 To 100 To 100 To 100 To 100 To 100 Ionic surfactant Sodium Cocoyl Glutamate 0.30 0.50 0.50 - 0.50 0.50 B: paid ester oil Neopentyl glycol dicaprate 20.00 20.00 20.00 20.00 20.00 20.00 vegetable oil Macadamia Seed Oil 20.00 20.00 20.00 20.00 20.00 20.00 Hydrocarbon oil Hydrogenated Poly (C6-14 Olefin) 10.00 10.00 10.00 10.00 10.00 10.00 Phospholipids lecithin 1.00 1.00 1.50 1.50 - 1.50 C: other antiseptic 1,2-Hexanediol 2.00 2.00 2.00 2.00 2.00 2.00 Spices Spices 0.20 0.20 0.20 0.20 0.20 0.20

Experimental Example 1: Change in viscosity of oil-in-water nanoemulsion cosmetic composition

An experiment was conducted to confirm the difference in viscosity by composition ratio of oil-in-water nanoemulsion cosmetic composition. The method is as follows.

Viscosity was measured with a Brookfield DV2TLV and was measured for 1 minute by applying an LV spindle and rpm suitable for the viscosity of each Example and Comparative Example sample.

As shown in Table 2 below, the difference in viscosity between Examples 1 to 3 and Comparative Examples 1 to 3 is only when the surfactant, ionic surfactant, and phospholipid are in an appropriate ratio, even without a thickener, high-viscosity creamy fine particles. It indicates that emulsions can be prepared. As can be seen from the component ratio and viscosity of Examples 1 to 3, the viscosity range can be adjusted by adjusting the ionic surfactant and phospholipid content, and it can be confirmed that Example 3 is the highest viscosity oil-in-water nanoemulsion cosmetic composition. there was. In addition, as shown in the viscosities of Comparative Examples 1 to 3, it was confirmed that the viscosity dropped sharply even if only one component of the ionic surfactant, phospholipid, and polymer surfactant was not included.

Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Viscosity (cps) 16100 22300 38900 3800 1500 6700

Experimental Example 2: Confirmation of appearance and transparency of oil-in-water nanoemulsion cosmetic composition

In order to confirm the appearance and transparency of the oil-in-water nanoemulsion cosmetic composition, the same amount of the sample was placed in a transparent bottle and the Examples and Comparative Examples were compared.

1 is a result of visually comparing the appearance and transparency of Examples 1 to 3 and Comparative Examples 1 to 3; Nanoparticle emulsions typically appear translucent and bluish in appearance at particle sizes of 200 nm or less. Examples 1 to 3 and Comparative Examples 1 to 3 have the same high internal damage ratio as 50% oil content, but Comparative Example 1 in which the ionic surfactant is excluded, Comparative Example 2 in which the phospholipid component is excluded, and the polymer surfactant It was confirmed that Comparative Example 3, in which is excluded, had an opaque appearance of milky white without blue light, unlike in Examples.

Experimental Example 3: Confirmation of particle size of oil-in-water nanoemulsion cosmetic composition

The following experiment was conducted to confirm the particle size of the oil-in-water nanoemulsion cosmetic composition.

The size and polydispersity index (PDI) of the emulsion drops were analyzed through dynamic light scattering. It was measured using ELS-Z of Otsuka Electronics, and the experiment was repeated 3 times by diluting 15 times with tertiary distilled water.

As a result of the analysis for Example 3, it can be seen that the average size of the nanoemulsion was 177.4 nm and the PDI was 0.130, so it was confirmed that very uniform and stable particles were maintained. 2 is a particle size analysis result for Example 3.

As shown in Table 3 below, the particle size of Comparative Examples 1 to 3, which does not include one of the three components, respectively, compared to Example 3, in which the polymer surfactant, the ionic surfactant, and the phospholipid were included in an appropriate ratio, were relatively You can check the big one. The results of Table 3 can be said to be consistent with the results of Experimental Example 2, which predicted the particle size by comparing the apparent transparency.

Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Particle size (nm) 177.4 229.1 331.6 319.1 PDI 0.130 0.112 0.175 0.214

Experimental Example 4: Stability evaluation of oil-in-water nanoemulsion cosmetic composition

In order to evaluate the stability of the oil-in-water nanoemulsion cosmetic composition, the following experiment was performed.

The experimental method is as follows. The stability evaluation was conducted by observing the visual change over time in a cycle test and at low and high temperatures. The cycle test was conducted for 3 months under the condition that 24 hours was a cycle and changed to 3 different temperatures (45°C, 25°C, 4°C) every 8 hours. Stability evaluation at low temperature (-18 ℃) is the stability at room temperature at three low-temperature stability evaluation times (3 days, 1 week, 2 weeks after storage) after storing each Example and Comparative Example sample at -18 ℃ evaluated. Stability evaluation at high temperature (50 ° C) was evaluated for stability at room temperature at three high temperature stability evaluation periods (1 week, 2 weeks, 1 month after storage) after storing each Example and Comparative Example sample at 50 ° C. .

As shown in Table 4 below, Examples 1 to 3 showed excellent stability, but Comparative Example 1 in which the ionic surfactant was excluded, Comparative Example 2 in which the phospholipid component was excluded, and Comparative Example 3 in which the polymer surfactant was excluded It was found to be unstable over time at low and high temperatures, and was particularly vulnerable to low temperatures.

condition observation period Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Cycle(4℃↔45℃) 1 month ◎ ◎ ◎ ◎ ◎ ◎ 2 months ◎ ◎ ◎ ◎ ◎ ◎ 3 months ◎ ◎ ◎ ◎ △ ◎ Low temperature (-18℃) 3 days ◎ ◎ ◎ △ △ △ 1 week ◎ ◎ ◎ △ X △ 2 weeks △ ◎ ◎ X X △ high temperature (50℃) 1 week ◎ ◎ ◎ ◎ △ ◎ 2 weeks ◎ ◎ ◎ △ △ △ 1 month ◎ ◎ ◎ △ △ △

◎: very stable / △: unstable / X: phase separation

Claims (4)

It contains a polymer surfactant, an ionic surfactant, and a phospholipid, and the mixing weight ratio of the polymer surfactant and the ionic surfactant is 50:1 to 0.5:1,
The polymer surfactant is a polyethylene glycol-polycaprolactone-polyethylene glycol (PEG-PCL-PEG) copolymer,
The ionic surfactant is not a phospholipid, oil-in-water cosmetic composition. The oil-in-water cosmetic composition according to claim 1, wherein the mixing weight ratio of the ionic surfactant and the phospholipid is 1:1 to 1:30. The method according to claim 1, The oil-in-water cosmetic composition having a viscosity of 10000 to 40000 cps. i) dissolving a polymer surfactant in a solvent to prepare a polymer surfactant solution;
ii) preparing an aqueous solution by dispersing the polymer surfactant solution in an aqueous phase component;
iii) preparing an oily solution by dissolving an oil phase containing oil and phospholipids; and
iv) to perform the step of high-pressure emulsification after mixing the aqueous phase solution and the oil phase solution,
The high-pressure emulsification is made 2 to 5 times at a pressure of 200 to 1500 bar, and the oil contains a high content of 30 to 60% by weight,
The polymer surfactant is a polyethylene glycol-polycaprolactone-polyethylene glycol (PEG-PCL-PEG) copolymer,
The method for producing the oil-in-water cosmetic composition of claim 1, wherein the aqueous component includes an ionic surfactant.

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