KR102100820B1 - Rosa centifolia flower petal fermented by aureobasidium pullulans - Google Patents

Abstract

The present invention relates to a cosmetic composition containing Provence rose petal-Aureobasidium pullulans fermentation broth which is obtained by fermenting Provence rose petals with Aureobasidium pullulans. Particularly, the present invention relates to a cosmetic composition containing Provence rose petal-Aureobasidium pullulans fermentation broth obtained with high yield of anthocyanin among active ingredients. The present invention is excellent in the antioxidant effect, moisturizing effect and skin barrier improvement effect.

Description

Cosmetic composition containing Provence rose petal black yeast fermentation liquid {ROSA CENTIFOLIA FLOWER PETAL FERMENTED BY AUREOBASIDIUM PULLULANS}

The present invention relates to a cosmetic composition containing a provence rose petal fermentation broth fermented with Provence rose petals fermented with black yeast mycelium, and more particularly, to a cosmetic composition excellent in antioxidant, moisturizing, and skin barrier improvement effects.

The goal of cosmetics is to maintain beautiful and healthy skin, and to delay the aging of naturally occurring skin with age. In general, aging is due to oxidative damage of biomaterials by free radicals. In other words, highly reactive free radicals such as free radicals, such as hydrogen peroxide, hydroxy radicals, and superoxide radicals, peroxidize the lipids that make up the cell membrane, destroying the cell membrane, oxidizing proteins, and attacking nucleic acids to cause oxidative damage to biomaterials Destroy the cells and eventually kill the cells. The most significant skin characteristics due to aging include wrinkles, decreased elasticity, and dull skin. In addition, in addition to wrinkles and reduced elasticity, after the 40s, the face color is often unclear and gray and dark.

In particular, in the case of young women, while experiencing childbirth, blood clots occur, and blood circulation disorders occur, resulting in a decrease in metabolic ability and skin roughening and dullness. When the metabolic ability decreases and the skin becomes rough, the amount of moisture is also easily reduced. In general, the amount of moisture in the skin is about 70% in the dermal layer, but decreases toward the epidermal layer, resulting in about 10 to 30% in the keratinocyte layer. It is known that in the keratinocyte layer, a substance having a hydrophilic water retention ability called natural moisturizing factor (NMF) exists and plays an important role in moisturizing the skin. In the normal keratinocyte layer, when moisture is maintained at about 10 to 30%, the skin is smooth and soft, and the body protects normally.

Therefore, it is very important to properly maintain the moisture content of the keratinocyte layer of the skin to prevent skin aging, but other natural moisturizing factors such as sodium pyrrolidone carboxylate (PCA-Na), sodium lactate, and urea are electrolytic. This strong, there is a problem that impairs the emulsion stability of the cosmetic. Amino acids, collagen, and elastin also have moisturizing abilities, but have limited moisturizing abilities. The ability to retain moisture in the stratum corneum can be controlled by natural moisturizing factors (NMF) composed of sebum components, amino acids, lactic acid, urea, and inorganic salts. It is safe and excellent in use as a natural moisturizing factor in external preparations for skin. In addition, the development of substances with high moisturizing effects is one of the important research tasks in cosmetics. In addition, substances known to have antioxidant activity include ascorbic acid, dl-α-tocopherol, beta-carotene, dibutylhydroxytoluene (BHT), etc. Since these materials are used as synthetic products, there is an urgent need for the development of new antioxidant cosmetics that can be applied to the skin more safely and usefully because they can cause skin safety problems when used for a long time or when used in large quantities.

Therefore, research on improving skin aging and moisturization is expected to continue, and cosmetics using natural products are being developed to solve these skin problems and reduce skin irritation caused by various chemicals. Natural ingredients have fewer side effects on skin, and recently, as consumers' response to cosmetics using natural materials has increased, the development value of cosmetics has increased.

To this end, studies are being actively conducted to search for the skin physiological activity of various natural plant components and to develop substances having excellent safety and excellent skin beauty effects.

Korean Patent Publication No. 2018-0037728 discloses a cosmetic composition containing a mixed extract of pomegranate, western rose flower, safflower and glycosylation. The cosmetic composition has an MMP-1 production inhibitory effect, collagen biosynthesis effect, antioxidant effect, and the like.

An object of the present invention is to reduce the risk of problems with existing cosmetic cosmetics, and increase the content of useful active ingredients present in trace amounts in natural materials to provide a cosmetic composition having various physiological activity effects such as moisturizing and antioxidant on the skin. Is to do.

The above object is achieved by a cosmetic composition comprising a Provencal rose petal fermentation broth fermented with black yeast mycelium.

Preferably, the cosmetic composition may be for antioxidant, skin moisturizing or skin barrier improvement.

In addition, preferably, the Provence rose petal black yeast fermentation liquid can be obtained by fermenting the solvent extract of the Provence rose petals with the black yeast for 1 to 7 days while maintaining a pH of 5 to 7 under a temperature condition of 20 to 40 ° C. .

Also preferably, the solvent extract of the Provence rose petals contains Provence rose petals in purified water, methanol, ethanol, glycerin, ethyl acetate, butylene glycol, propylene glycol, dichloromethane, chloroform, ethyl ether, butylene glycol, hexane, and the like. It can be extracted using one or more solvents selected from the group consisting of mixtures.

In addition, preferably, the Provence rose petal black yeast fermentation liquid may be contained in an amount of 0.0001 to 30.0 wt% based on the total weight of the cosmetic composition.

Also preferably, the cosmetic composition is a group consisting of solution, suspension, emulsion, paste, gel, cream, lotion, powder, soap, surfactant-containing cleansing, oil, powder foundation, emulsion foundation, wax foundation and spray It may have any one formulation selected from.

The cosmetic composition according to the present invention uses a natural extract, is harmless to the human body and has excellent safety, and has an antioxidant, moisturizing, and skin barrier improvement effect by containing an extract of Provence rose petal with increased anthocyanin content as an active ingredient.

All technical terms used in the present invention, unless defined otherwise, have the following definitions and conform to the meaning as commonly understood by those skilled in the art in the relevant field of the present invention. In addition, although a preferred method or sample is described herein, similar or equivalent ones are included in the scope of the present invention.

   The term “about” means 30, 25, 20, 15, 10, 9, 8, 7, 6, 5, for reference amount, level, value, number, frequency, percent, dimension, size, amount, weight or length It means a quantity, level, value, number, frequency, percentage, dimension, size, quantity, weight or length that varies by 4, 3, 2 or 1%.

   Throughout this specification, the terms "comprises" and "comprising", unless otherwise required by context, include the steps or components presented, or groups of steps or components, but any other steps or components, or It should be understood that it implies that the group of steps or components is not excluded.

A deciduous shrub belonging to the family Rosaceae used as an active ingredient in the cosmetic composition of the present invention, Rosa Centifolia, is a kind of western rose, about 1 to 3 m tall, with thick thorny shrubs, leaves misaligned and feathery The lobules are egg-shaped, and serrates are developed on the leaf edges.

Provence rose petal extract of the present invention means an extract obtained from the petals of Provence rose.

In addition, the Provence rose petal extract of the present invention can be prepared according to conventional methods known in the art. For example, extraction is performed using (a) a solvent extraction method, (b) a supercritical extraction method with reduced pressure and high temperature with carbon dioxide, or (c) an ultrasonic extraction method.

In the present invention, a solvent extraction method using an extraction solvent is preferably used. Provence rose petal extract in the present invention is water, anhydrous or hydrous lower alcohol having 1 to 4 carbon atoms, acetone, ethyl acetate, butyl acetate and 1,3-butylene glycol, propylene glycol, dichloromethane, chloroform, ethyl ether, butylene After extraction using a solvent selected from the group consisting of glycol, hexane, and mixtures thereof, or extracting Provencal rose petals using the solvent, it can be prepared by mixing, but preferably, the solvent is good alcohol, more preferably It is better to use 70% ethanol. And the suitable amount of the extraction solvent is 1 to 15 times the dry weight of Provence rose petals, more preferably 5 to 10 times, and most preferably 7 times.

On the other hand, it is apparent to those skilled in the art that the extract of Provence rose petals of the present invention can obtain an extract exhibiting substantially the same effect using other extraction solvents as well as the above-described extraction solvent.

In addition, the Provence rose petal extract of the present invention includes not only extracts by the above-described extraction solvent, but also extracts that have undergone conventional purification and fermentation processes. For example, decompression by carbon dioxide, extraction by supercritical extraction by high temperature, extraction by ultrasonic extraction, separation using an ultrafiltration membrane having a constant molecular weight cut-off value, various chromatography (size, charge, hydrophobicity or affinity) Active fractions obtained through various purification and extraction methods additionally performed, such as extracting by fermentation products using natural or various microorganisms or separated by a product prepared for separation according to sex) are also included in the extract of the present invention.

In addition, the present invention provides a cosmetic composition characterized in that the extract is obtained by cooling at room temperature, liquefied by heating, and further concentrated or freeze-dried the solvent under reduced pressure.

Decompression by carbon dioxide and extraction by supercritical extraction by high temperature mean supercritical fluid extraction. Generally, supercritical fluid is a liquid that a gas has when it reaches a critical point under high temperature and high pressure conditions, and It has the properties of a gas, has a chemically polarity similar to a non-polar solvent, and because of these properties, supercritical fluids are used for the extraction of fat-soluble materials (J. Chromatogr. A. 1998; 479: 200-205).

Carbon dioxide becomes a supercritical fluid having both liquid and gaseous properties through the process of pressure and temperature reaching the critical point by the operation of a supercritical fluid device, and as a result, solubility in fat-soluble solute increases. When the supercritical carbon dioxide passes through the extraction container containing a certain amount of sample, the fat-soluble substance contained in the sample is extracted from the supercritical carbon dioxide.

After extracting the fat-soluble substance, passing the supercritical carbon dioxide containing a small amount of co-solvent again through the sample remaining in the extraction container may extract components that have not been extracted with pure supercritical carbon dioxide alone.

The supercritical fluid used in the supercritical extraction method of the present invention can effectively extract the active ingredient by using supercritical carbon dioxide or a mixed fluid in which a co-solvent is additionally mixed with carbon dioxide. The co-solvent may use one or two or more mixtures selected from the group consisting of chloroform, olive oil, ethanol, methanol, water, ethyl acetate, nucleic acid and diethyl ether. Preferably, one or two or more mixtures selected from the group consisting of olive oil, ethanol, methanol and water can be used. Most of the extracted samples contain carbon dioxide, and since carbon dioxide volatilizes into the air at room temperature, the extract obtained by the above method can be used as a cosmetic composition, and the co-solvent can be removed by a vacuum evaporator.

In addition, the ultrasonic extraction method is an extraction method that uses energy generated by ultrasonic vibration, and ultrasonic waves can destroy insoluble solvents contained in a sample in a water-soluble solvent, and are located around due to the high local temperature generated at this time. Since the kinetic energy of the reactant particles is increased, sufficient energy necessary for the reaction is obtained, and high pressure is induced by the impact of ultrasonic energy, thereby increasing the mixing effect of the substance and the solvent contained in the sample, thereby increasing extraction efficiency. As an extraction solvent that can be used in the ultrasonic extraction method, one or a mixture of two or more selected from the group consisting of chloroform, ethanol, methanol, water, ethyl acetate, nucleic acid and diethyl ether can be used. The extracted sample is vacuum filtered to recover the filtrate, and then removed by a vacuum evaporator, and an extract can be obtained through a conventional extract preparation method of freeze drying.

Provence rose petal extract according to the present invention also includes an extract that has undergone a fermentation process, and a Provence rose petal fermentation extract can be prepared as follows. After the Provencal rose petals are finely crushed to about 100 to 500 mesh, 1-50 g / L of a conventional microbial culture solution is added, and microorganisms such as yeast strains or lactic acid bacteria are added in an amount of 10,000 to 100,000 cfu / L. The culture temperature is cultured under normal microorganism culture conditions of 30 ~ 37 ℃. The pH is 5 to 7 and cultured for about 5 to 10 days under aerobic or normal anaerobic conditions. It can then be obtained through aging and filtration.

Preferably, the Provence rose petal extract according to the present invention may be a Provencal rose petal fermentation broth fermented with black yeast mycelium.

Black yeast ( Aureobasidium pullulans ) is a microorganism used to make beer, wine, etc., but is a group of single-celled organisms that do not have hyphae and have no photosynthesis or mobility, although they are a group of fungi and mushrooms. It is a microorganism that humans have used for food since 5,000 years ago, and the yeast itself is used as a cheap source of fat or protein. It contains a rich group of vitamin B and some contain vitamin D. In addition, black yeast is a microorganism that produces beta-glucan (β-Glucan), and it is said that the black yeast fermentation itself exhibits moisturizing, antioxidant and soothing effects. Black yeast beta-glucan (β-glucan) contains a large amount of ingredients known to have physiological activities, such as anti-cancer and insulin secretion suppression.

And the Provence rose petal black yeast fermentation solution of the present invention maintains the pH 5 to 7 under the temperature condition of 20 to 40 ° C., while maintaining the solvent extract of the Provence rose petal extract, the black yeast ( Aureobasidium pullulans ).

According to the present invention, the Provence rose petal extract contains 0.001 to 30.0% by weight relative to the total weight of the cosmetic composition, preferably, 0.01 to 20% by weight, and more preferably 0.1 to 10% by weight It is characterized by. When the content of the extract is less than 0.001% by weight, the skin moisturizing effect does not appear, and when it exceeds 30.0% by weight, the degree of increase in the skin moisturizing effect on the increase in content is negligible, and there is a problem in the safety and stability of the formulation. Not even enemies

After using the Provencal rose petal extract prepared by a conventional method in a cosmetic formulation to remove unnecessary components through a purification process, it may include a cosmetic composition exhibiting an efficacy effect. The purification process can be any conventional purification process, and a liquid-liquid extraction method using a difference in solubility, a precipitation and a filter, a chromatography method using a size of polarity and molecular weight, and the like can be used. For example, after dissolving Provence rose petal extract in an ethanol aqueous solution (50%, 70% solution, etc.) or other aqueous solution, use a column filled with HP-20 and sephadex columns to determine the difference between the water-soluble substance and After separating the oil-soluble substance, the oil-soluble substance may be concentrated and freeze-dried by TLC to prepare a concentrate.

The components included in the cosmetic composition of the present invention as active ingredients may include ingredients commonly used in cosmetic compositions in addition to the active ingredients, for example, antioxidants, stabilizers, solubilizers, vitamins, pigments and fragrances Adjuvants, and carriers.

The cosmetic composition of the present invention can be prepared in any formulation conventionally prepared in the art, for example, solution, suspension, emulsion, paste, gel, cream, lotion, powder, soap, surfactant-containing cleansing , Oil, powder foundation, emulsion foundation, wax foundation and spray, etc., and more specifically, flexible lotion, nutrition lotion, nutrition cream, massage cream, essence, eye cream, cleansing cream, cleansing foam, It can be prepared in the form of cleansing water, packs, sprays or powders.

When the formulation of the present invention is a paste, cream or gel, animal oil, vegetable oil, wax, paraffin, starch, trakant, cellulose derivative, polyethylene glycol, silicone, bentonite, silica, talc or zinc oxide, etc. may be used as a carrier component. You can.

When the formulation of the present invention is a powder or a spray, lactose, talc, silica, aluminum hydroxide, calcium silicate or polyamide powder can be used as a carrier component, and in the case of a spray, additionally chlorofluorohydrocarbon, propane / Propellant such as butane or dimethyl ether.

When the formulation of the present invention is a solution or emulsion, a solvent, solubilizing agent or emulsifying agent is used as a carrier component, such as water, ethanol, isopropanol, ethyl carbonate, ethyl acetate, benzyl alcohol, benzyl benzoate, propylene glycol, 1 , 3-butyl glycol oil, glycerol aliphatic ester, polyethylene glycol or sorbitan fatty acid ester.

When the formulation of the present invention is a suspension, liquid diluents such as water, ethanol or propylene glycol as carrier components, suspensions such as ethoxylated isostearyl alcohol, polyoxyethylene sorbitol esters and polyoxyethylene sorbitan esters, microcrystals Sex cellulose, aluminum metahydroxide, bentonite, agar or trakant, etc. can be used.

When the formulation of the present invention is a surfactant-containing cleansing, aliphatic alcohol sulfate, aliphatic alcohol ether sulfate, sulfosuccinic acid monoester, isethionate, imidazolinium derivative, methyltaurate, sarcosinate, fatty acid amide as a carrier component Ether sulfates, alkylamidobetaines, aliphatic alcohols, fatty acid glycerides, fatty acid diethanolamides, vegetable oils, lanolin derivatives or ethoxylated glycerol fatty acid esters and the like can be used.

When the cosmetic composition of the present invention is a soap, a surfactant-containing cleansing agent, or a surfactant-free cleansing formulation, it may be wiped, peeled off, or washed with water after being applied to the skin. As a specific example, the soap is liquid soap, powder soap, solid soap and oil soap, and the surfactant-containing cleansing formulation is a cleansing foam, cleansing water, cleansing towel and cleansing pack, and the surfactant-free cleansing formulation is a cleansing cream , Cleansing lotions, cleansing water and cleansing gels, but are not limited thereto.

Hereinafter, the present invention will be described in more detail through manufacturing examples. These manufacturing examples are only for explaining the present invention in more detail, and according to the gist of the present invention, the scope of the present invention is not limited by these manufacturing examples to those skilled in the art to which the present invention pertains. It will be obvious.

<Production Example 1> Preparation of Provence rose petal extract

After slicing, 300 g of shaded Provencal rose petals were refluxed 3 times for 5 hours by adding 70% ethanol, cooled, filtered with Whatman # 3 filter paper, concentrated under reduced pressure at 50 ° C. or freeze-dried. The freeze-dried product was dissolved to 2% (W / V) using 50% glycerin to prepare a Provence rose petal extract (Preparation Example 1).

<Production Example 2> Preparation of Provence rose petal supercritical extract

The finely shaded Provencal rose petals 300g were extracted by a conventional supercritical extraction method (extracted using olive oil as a co-solvent under supercritical conditions at a pressure of about 300 atmospheres (atm) at a temperature of about 60 ° C) and ultrafiltration membrane After removing the salt using and concentrated under reduced pressure and freeze-dried to obtain a dried Provence rose petal extract powder of 31.5g. It was dissolved in 50% glycerin and dissolved to 2% (W / V) to produce a Provence rose petal supercritical extract (Preparation Example 2).

<Production Example 3> Preparation of Provence rose petal ultrasonic extract

The finely brewed Provencal rose petal 300g was extracted using ultrasonic waves (extracted for 2 hours at 30 ° C at an intensity of 25KHz using a supernonic ultrasonic device) and concentrated under reduced pressure and freeze-dried after removing salt using an ultrafiltration membrane. Through, 7.3g was obtained. The dried Provencal rose petal extract powder was dissolved to 2% (W / V) using 50% glycerin to prepare a Provencal rose petal ultrasonic extract (Preparation Example 3).

<Production Example 4> Preparation of Provence rose petal fermentation extract

The petals of Provence rose were produced by fermenting the petals, and the petals were selected as a sample, washed sufficiently, and then pulverized to finely pass through a 300 mesh sieve. The petals of the Provence rose were added to the culture solution of the genus Saccharomyces (Saccharomyces cerevisiae KCTC 7904) to be 20 g / L. Glucose 2% (W / V) was added as a carbon source, and peptone 0.5% (W / V) was additionally added to culture. Cultivation was carried out using a 5L fermenter, and maintained at pH 5-7 at 37 ° C, preferably at pH 6, and cultured for 1 to 7 days, preferably 5 days. After the culture, the culture medium was centrifuged to remove the culture bacteria first.

After the cultured bacteria were first removed, the petal fermentation product was added with ethanol so as to be a final 70% (V / V) ethanol aqueous solution, refluxed 3 times for 5 hours, cooled, and then filtered with Whatman # 2 filter paper. . The filtered extract was transferred to a concentration tank to concentrate the filtered extract under reduced pressure and freeze-dried. This powder was dissolved to 2% (W / V) using 50% glycerin to prepare a Provencal rose petal fermentation extract (Production Example 4).

<Production Example 5> Preparation of Provence rose petal black yeast fermentation broth

Glucose 2% (W / V) was added as a carbon source to 5 g of Provence rose petal decompression concentrate prepared in Preparation Example 1, and peptone 0.5% (W / V) was further added to sterilize. Here, 20g / L of black yeast ( Aureobasidium pullulans ) strain culture was inoculated. The culture was maintained for 7 days at 37 ° C and pH 6 using a 5L fermenter. After the culture, the culture solution was centrifuged to remove the culture bacteria first, and sterilized to prevent further culture (121 ° C, 15 minutes, 1.5 atm).

After fermentation, the petal fermentation product from which the cultured bacteria were first removed is added to ethanol to make a final 70% (V / V) ethanol aqueous solution, refluxed 3 times for 5 hours, cooled, and filtered with whatman # 3 filter paper. Did. When the filtration was completed, the extract obtained in the extraction step was transferred to a concentration tank and concentrated under reduced pressure or freeze-dried at 50 ° C or lower. The freeze-dried product was dissolved to 2% (W / V) using 50% glycerin to prepare a black yeast fermentation solution of Provence rose petals (Preparation Example 5).

<Formulation Example 1>

A formulation example of a cream in a cosmetic composition containing Provence rose petal black yeast fermentation solution (Preparation Example 5) is shown in Table 1 below.

ingredient Content (unit:% by weight) Provence rose petal black yeast fermentation liquid (Production Example 5) 6.0 glycerin 5.0 Sodium hyaluronate 2.0 Polysorbate 60 1.5 Mineral oil 3.0 Squalane 3.0 Dimethicone 2.0 Triethanolamine 1.0 Lipophilic monostearin glycerin 2.0 Cetearyl alcohol 2.0 Stearic Acid 1.0 Sorbitan stearate 0.5 Sodium magnesium silicate 0.1 Betaine 2.0 antiseptic a very small amount incense a very small amount Coloring a very small amount Purified water Balance system 100

<Comparative Formulation Example 1>

Comparative formulation example 1 of the cream containing no fermentation broth of Provence rose petals is shown in Table 2 below.

ingredient Content (unit:% by weight) glycerin 5.0 Sodium hyaluronate 2.0 Polysorbate 60 1.5 Mineral oil 3.0 Squalane 3.0 Dimethicone 2.0 Triethanolamine 1.0 Lipophilic monostearin glycerin 2.0 Cetearyl alcohol 2.0 Stearic Acid 1.0 Sorbitan stearate 0.5 Sodium magnesium silicate 0.1 Betaine 2.0 antiseptic a very small amount incense a very small amount Coloring a very small amount Purified water Balance system 100

<Comparative Formulation Example 2>

Comparative formulation example 2 of the cream in the cosmetic composition containing Provence rose petal fermentation extract (Production Example 4) is shown in Table 3 below.

ingredient Content (unit:% by weight) Provence rose petal fermentation extract (Production Example 4) 6.0 Sodium hyaluronate 5.0 Polysorbate 60 2.0 Mineral oil 1.5 Squalane 3.0 Dimethicone 3.0 Triethanolamine 2.0 Lipophilic monostearin glycerin 1.0 Cetearyl alcohol 2.0 Stearic Acid 2.0 Sorbitan stearate 1.0 Sodium magnesium silicate 0.5 Betaine 0.1 antiseptic 2.0 incense a very small amount Coloring a very small amount Purified water a very small amount system Balance

<Comparative Formulation Example 3>

Comparative formulation example 3 of the cream in the cosmetic composition containing the Provence rose petal ultrasonic extract (Preparation example 3) is shown in Table 4 below.

ingredient Content (unit:% by weight) Provence rose petals ultrasonic extract (Production Example 3) 6.0 Sodium hyaluronate 5.0 Polysorbate 60 2.0 Mineral oil 1.5 Squalane 3.0 Dimethicone 3.0 Triethanolamine 2.0 Lipophilic monostearin glycerin 1.0 Cetearyl alcohol 2.0 Stearic Acid 2.0 Sorbitan stearate 1.0 Sodium magnesium silicate 0.5 Betaine 0.1 antiseptic 2.0 incense a very small amount Coloring a very small amount Purified water a very small amount system Balance

<Comparative Formulation Example 4>

Comparative formulation example 4 of the cream in the cosmetic composition containing Provence rose petal supercritical extract (Preparation Example 2) is shown in Table 5 below.

ingredient Content (unit:% by weight) Provence rose petal supercritical extract (Production Example 2) 6.0 Sodium hyaluronate 5.0 Polysorbate 60 2.0 Mineral oil 1.5 Squalane 3.0 Dimethicone 3.0 Triethanolamine 2.0 Lipophilic monostearin glycerin 1.0 Cetearyl alcohol 2.0 Stearic Acid 2.0 Sorbitan stearate 1.0 Sodium magnesium silicate 0.5 Betaine 0.1 antiseptic 2.0 incense a very small amount Coloring a very small amount Purified water a very small amount system Balance

<Comparative Formulation Example 5>

Comparative formulation example 5 of the cream in the cosmetic composition containing Provence rose petal extract (Preparation example 1) is shown in Table 6 below.

ingredient Content (unit:% by weight) Provence rose petal extract (Production Example 1) 6.0 Sodium hyaluronate 5.0 Polysorbate 60 2.0 Mineral oil 1.5 Squalane 3.0 Dimethicone 3.0 Triethanolamine 2.0 Lipophilic monostearin glycerin 1.0 Cetearyl alcohol 2.0 Stearic Acid 2.0 Sorbitan stearate 1.0 Sodium magnesium silicate 0.5 Betaine 0.1 antiseptic 2.0 incense a very small amount Coloring a very small amount Purified water a very small amount system Balance

< Experimental example  1> Active ingredient of Provence rose petal extract ( anthocyanin ) Content measurement

The contents of each anthocyanin substance in Provence rose petal extracts of Preparation Examples 1 to 5 were analyzed using HPLC as shown in Table 7.

time water Acetonitrile 0 80 20 5 80 20 25 72 28 35 67 33 40 59 41 45 20 80 47 20 80 50 80 20

As for the analysis column, the optipack C18, the column temperature 30 ° C, and the UV detector absorbance wavelength were analyzed at 203 nm, and the results are shown in Table 8 below.

Preparation Example 1 Preparation Example 2 Preparation Example 3 Preparation Example 4 Preparation Example 5 content Anthocyanin 1.05 2.23 2.98 3.37 4.95 %

As a result of measuring the active ingredient content of Provence rose petal extract of Preparation Examples 1 to 5, anthocyanin of Provencal rose petal black yeast fermentation solution (Preparation Example 5) extracted by fermenting the solvent extract of Provence rose petal of the present invention using a black yeast mycelium It was confirmed that the components were significantly increased compared to other extraction conditions (Preparation Examples 1 to 4).

<Experimental Example 2> Measurement of antioxidant effect

The antioxidant activity of the extracts prepared in Preparation Examples 1 to 5 of the present invention was measured by a thiobarbituric acid method (TBA assay) using a lipid peroxidation system by a Fenton reaction. That is, 10 μl of ethyl linoleate, 0.2% sodium dodecyl sulfoxide (SDS), 10 μmol of ferric chloride, and 2 μmol of hydrogen peroxide were prepared in Preparation Examples 1 to 5 in 5 ml of 25 mM Trizma hydrochloride / 0.75 mM potassium chloride buffer. After adding dimethylsulfoxide (DMSO) test solution of one extract and incubating at 55 ° C for 16 hours, 50 µl of 4% dibutylhydroxytoluene (BHT) was added to stop the reaction. 0.3 ml of this solution was placed in a test tube, and 3.0 ml of 0.05 N hydrochloric acid and 0.67% thiobarbituric acid (TBA) solution were added and boiled for 30 minutes. After cooling the reaction solution, 4.0 ml of 85% butanol was added, and after centrifugation, the absorbance of the butanol layer was measured at 535 nm, and the antioxidant effect of each extract was calculated by the following equation (1). Table 9 shows the results.

Test substance Antioxidative effect(%) Experiment concentration (10㎍ / ml) Experimental concentration (50㎍ / ml) Experimental concentration (100㎍ / ml) Preparation Example 1 5 25 37 Preparation Example 2 12 33 43 Preparation Example 3 19 46 58 Preparation Example 4 25 48 60 Preparation Example 5 40 58 86

Most of the antioxidant effects of Provence rose petal extracts of Preparation Examples 1 to 5 showed high activity, and in particular, it can be seen that the antioxidant effects of Preparation Example 5 according to the present invention are very excellent.

In addition, Provencal rose petal extracts of Preparation Examples 1 to 5 and existing antioxidants ascorbic acid, D-alpha-tocopherol, beta-carotene and dibutylhydroxytoluene The antioxidant activity of (BHT) was measured in the same manner as in Experimental Example 2 to compare IC ₅₀ , which is a 50% inhibitory concentration. The results are shown in Table 10 below.

Test substance IC ₅₀ (10 μg / ml) Preparation Example 1 75.1 Preparation Example 2 62.3 Preparation Example 3 52.4 Preparation Example 4 45.3 Preparation Example 5 32.1 Ascorbic acid 21.90 Dl-a-tocopherol 3.36 Beta-carotene (β-carotene) 29.8 Dibutyl hydroxyl toluene (BHT) <1

Provencal rose petal extracts of Preparation Examples 1 to 5 exhibited high activity comparable to other antioxidants, and it can be seen that Preparation Example 5 exhibits high activity. In particular, it can be seen that these Provencal rose petal extracts have significant antioxidant activity despite being natural extracts.

<Experimental Example 3> Evaluation of the effect of improving the skin moisturizing effect of Provence rose petal black yeast fermentation broth

The anti-wrinkle effect of the cream of Provence rose petal black yeast fermentation cream (Formulation Example 1) and Comparative Formulation Examples 1 to 5 was evaluated as follows. 25 people in their 20s to 40s who do not have skin disorders are divided into two groups of 20 people per group, and the nutrition cream of the creams of the above formulation examples 1 and comparative formulations 1 to 3 for each group is faced twice a day for 1 month and It was made to apply to the forearm. Before starting application, skin conductivity was measured using a corneometer (CM820 courage Khazaka electronic GmbH, Germany) at constant temperature and humidity conditions (24 ° C, humidity 40%), and used as a basic value.After 1, 2, and 4 weeks The rate of increase in skin conductivity (%) was measured to evaluate the rate of increase. The results are shown in Table 11 below.

Experimental product 1 week later After two weeks 3 weeks later Formulation Example 1 40 45 50 Comparative Formulation Example 1 6 10 16 Comparative Formulation Example 2 24 28 33 Comparative Formulation Example 3 14 17 22 Comparative Formulation Example 4 17 20 25 Comparative Formulation Example 5 18 25 30

As shown in Table 11, in the case of a cream containing Provencal rose petal fermentation broth (Formulation Example 1), the skin conductivity increase rate was very excellent as compared to Comparative Formulation Examples 1 to 5. In general, since the skin conductivity is proportional to the amount of moisture in the skin, the above results confirmed that the cosmetics containing the Provence rose petal black yeast fermentation liquid maintains the skin moisture content higher than that of the other cosmetic products. Skin irritation was not observed in most of the subjects who applied the cosmetic to the skin.

<Experiment 4> Evaluation of the effect of improving the skin barrier of Provence rose petal black yeast fermentation broth

In order to investigate the effect of improving the skin barrier of a cosmetic composition containing Provence rose petal fermentation broth of the present invention, the following experiment was conducted. This experimental example was evaluated by performing a comparative experiment using Tewameterr (TM300, Courage and Khazaka Electronic Co., Germany) for the transdermal water loss (TEWL) for the cosmetic of formulation example 1 for humans. For 40 women in their 20s and 40s, apply each sample to the right and left faces, and apply the percutaneous moisture loss of 1 hour, 2 hours, 4 hours, and 6 hours before and after applying the area 1 cm below the right side 3 cm from the eye area. Tewameterr (TM300, Courage and Khazaka Electronic Co., Germany) was measured 3 times to evaluate the percutaneous moisture loss using the average value. The results are shown in Table 12 below.

division 1 hours 2 hours 4 hours 6 hours Formulation Example 1 13.3 14.3 12.0 8.7 Comparative Formulation Example 1 25.3 22.4 19.8 17.5 Comparative Formulation Example 2 17.7 16.3 13.2 11.0 Comparative Formulation Example 3 18.8 17.1 15.0 14.4 Comparative Formulation Example 4 18.9 18.0 16.1 15.2 Comparative Formulation Example 5 21.7 18.4 16.9 16.0

As shown in Table 12 above, as a result of measuring the amount of transdermal moisture loss, it was seen that the amount of transdermal moisture loss was reduced in the facial skin of the experimenter who applied the cream containing the fermentation solution of Provence rose petals black yeast. Was found.

Since the specific parts of the present invention have been described in detail above, it is clear that for those skilled in the art, this specific technology is only a preferred embodiment, and the scope of the present invention is not limited thereto. Therefore, the substantial scope of the present invention will be defined by the appended claims and their equivalents.

Claims (6)

Provencal rose petal black yeast fermentation liquid obtained by fermenting with the black yeast for 1 to 7 days while maintaining the solvent extract of Provence rose petal under a temperature condition of 20 to 40 ° C while maintaining a pH of 5 to 0.0001 to Antioxidant cosmetic composition comprising 30.0% by weight. According to claim 1,
The solvent extract of the Provence rose petal is from the group consisting of Provence rose petals, purified water, methanol, ethanol, glycerin, ethyl acetate, butylene glycol, propylene glycol, dichloromethane, chloroform, ethyl ether, butylene glycol, hexane and mixtures thereof. Extracted using at least one selected solvent, an antioxidant cosmetic composition. According to claim 1,
The cosmetic composition is any one selected from the group consisting of solution, suspension, emulsion, paste, gel, cream, lotion, powder, soap, surfactant-containing cleansing, oil, powder foundation, emulsion foundation, wax foundation and spray Cosmetic composition for antioxidant, having a formulation of. delete delete delete