KR20130073707A - Cosmetic composition using chamaecyparis obtusa supercritical extract and manufacturing method thereof - Google Patents

Abstract

PURPOSE: A method for manufacturing a cosmetic composition using a supercritical extract of Chamaecyparis obtuse is provided to enhance extract yield and to minimize loss of aromatic ingredients of Chamaecyparis obtusa. CONSTITUTION: A cosmetic composition contains a supercritical extract of Chamaecyparis obtusa contains which is prepared by supercritical fluid extraction. The extract is prepared by adding supercritical carbon dioxide to Chamaecyparis obtusa and extracting at 35-45 deg. C and at 100-500 bar for 30-240 minutes. A method for manufacturing the cosmetic composition comprises the steps of: drying Chamaecyparis obtusa; extracting the dried Chamaecyparis obtusa by supercritical fluid extraction to obtain a Chamaecyparis obtusa extract; adding 0.01-10 wt% of the extract; and manufacturing in a form of a lotion, a cream, an essence, a pack, a makeup base, a foundation, a cleansing oil, a cleansing foam, a hair oil, a hair shampoo, and a hair rinse.

Description

Cosmetic composition using chamaecyparis obtusa supercritical extract and manufacturing method

The present invention relates to a cosmetic composition and a method for preparing the same, and more particularly, to a cosmetic composition having a moisturizing activity and containing a protein supercritical extract having a skin improvement effect and a method for producing the same.

Skin is the largest organ in the body and is always in direct contact with the external environment and acts as a protective shield to protect the living body from various irritation or dry environments. It is an organ that actively produces and destroys new cells compared to other organs. In addition, it protects the body from physical abrasion, protects the inside of the body from moisture loss, protects it from ultraviolet rays generated from the sun, and plays a very important role in controlling body temperature.

When the skin is subjected to external stimulation due to various physical factors and external environmental factors, aging such as wrinkle formation, loss of elasticity and keratinization occurs. Skin aging is largely divided into natural aging (or endogenous aging) and external aging. Natural aging is difficult to artificially control because it is influenced by genetic factors, whereas external aging is relatively easy to control because external aging is affected by environmental factors. Do.

The development of various functional cosmetics that can improve the skin using natural products at home and abroad is actively underway.

The natural organic cosmetics market in Europe currently accounts for 3% of the European cosmetics market. Germany, Austria and Switzerland have more than 4% market share, Germany is the fastest growing natural cosmetics market, and the market share of natural cosmetics market is expected to increase 10% in 2010.

The area of application of cosmetics is also expanding from face to neck and body. In particular, body care used throughout the body is a basic concept that uses natural ingredients that are beneficial to the skin, and is being developed into products that add preventive and therapeutic effects, which reflects the propensity of consumers who value health and appearance to the market. It means that there is.

In Japan, it has strengths in body cleansing products focusing on body shampoos, and has many research achievements and intellectual property rights in the development of hypoallergenic surfactants and detergents (Kao, Shiseido). In the last decade, Japan's body care market has grown based on global market-leading ideas, and products containing marine materials that enhance the body's self-healing, or specialized anti-obesity-related anti-cellulite that responds to the individual needs of users. Body care products using body functional materials such as anticellulite and firming have high added value by themselves, and high quality and high price products have recently emerged.

In Korea, examples of using cypress in cosmetics (Korean Patent Publication No. 2007-0102911) are known. However, there is no question about how to prove the true effectiveness of products because there are no proper guidelines and standard protocols for the extraction method.

In addition, the conventional techniques are mainly used as a method for extracting the cypress extract, such as steam distillation or a leaching method using an organic solvent, but there is a problem that the extraction yield is low and the loss of fragrance components of the cypress is large.

Therefore, the present invention was created to improve the above problems, extracting the cypress extract using a supercritical fluid extraction method so that the extraction yield is high and the loss of the fragrance components of the cypress is excellent and at the same time excellent moisturizing activity cosmetic composition and its The purpose is to provide a manufacturing method.

The cosmetic composition of the present invention for achieving the above object is characterized in that it contains a cypress supercritical extract extracted from a cypress using a supercritical fluid extraction method.

The supercritical fluid extraction method uses carbon dioxide as a supercritical fluid, and the one-pack supercritical extract is extracted for 30 to 240 minutes by adding supercritical carbon dioxide at a temperature of 35 to 45 ° C. and a pressure of 100 to 500 bar to the protein.

The cosmetic composition is 1.0% by weight of cetearyl alcohol, 1.6% by weight of glyceryl stearate, 0.5% by weight of beeswax, 0.5% by weight of hydrogenated lecithin, 3.0% by weight of neopentyl glycol dicaprate, hydrogenated poly Decene 4.0 wt%, Capric Triglyceride 2.0 wt%, Cyclopentasiloxane 5.0 wt%, Tocopheryl Acetate 0.2 wt%, Dimethicone 0.3 wt%, Propylparaben 0.1 wt%, Trisodium ethiate 0.02 wt%, Methylparaben 0.2 wt%, glycerin 6.5 wt%, dipropylene glycol 4.5 wt%, xanthan gum 0.03 wt%, carbomer 0.16 wt%, potassium hydroxide 0.071 wt%, phenoxyethanol 0.2 wt%, dipotassium glycidase It is a body care composition consisting of 0.1% by weight, triglyceride supercritical extract 3.5% by weight, the remaining amount of purified water, the cosmetic composition is characterized by having a moisturizing activity.

And the manufacturing method of the cosmetic composition of the present invention for achieving the above object comprises a drying step of drying the white; An extracting step of extracting a protein of supercritical extract from the dried protein, using a supercritical fluid extraction method; It is added to contain the cypress supercritical extract 0.01 to 20% by weight based on the total weight of the composition, lotion, lotion, cream, essence, pack, makeup base, foundation, cleansing oil, cleansing foam, hair oil, hair shampoo and Characterized in that it comprises a; formulating step of preparing to any one of the formulation selected from the hair rinse.

The drying step is characterized in that to dry the protein at a low temperature of 35 ℃.

As described above, according to the present invention, it is possible to increase the extraction yield and minimize the loss of fragrance components of the cypress by extracting the cypress extract using a supercritical fluid extraction method.

In addition, the cosmetic composition of the present invention containing a cypress supercritical extract can be used safely without irritation to the skin and is excellent in moisturizing activity.

1 to 4 are graphs showing the results of GC / MS analysis of the protein extract supercritical extract according to one embodiment of the present invention,
5 and 6 are graphs showing the results of HPLC analysis of the components of the Cyclic supercritical extract according to one embodiment of the present invention,
7 is a graph showing changes in skin moisture before and after applying body essence according to an embodiment of the present invention.
8 is a graph showing the sensory evaluation results of the body essence according to an embodiment of the present invention.

Hereinafter, a cosmetic composition using a protein-based supercritical extract according to a preferred embodiment of the present invention and a manufacturing method thereof will be described in detail.

The cosmetic composition of the present invention contains a flaky supercritical extract.

The protein extract can be extracted in a variety of ways, but preferably a chamaecyparis At least one of the leaves, stems and branches of the obtusa ) is extracted by supercritical fluid extraction. In addition, the active fraction obtained through various purification methods carried out is included in the extract.

Supercritical fluid extraction has low viscosity of supercritical fluid, so it penetrates into the sample with high extraction efficiency and high diffusion coefficient, so extraction speed is high and extraction at relatively low temperature causes damage by heat. Since the density difference between the sample and the supercritical fluid is large and the viscosity of the supercritical fluid is low, the extraction residue and the solvent can be easily separated.

Supercritical fluid means that a fluid under special conditions under high-temperature and high-pressure conditions is applied to supercritical substances, that is, substances such as carbon dioxide, water, alcohol, and helium, with a critical pressure and a critical temperature. This supercritical fluid has a value similar to that of a liquid, its viscosity is close to the gas, and its diffusion coefficient is about 100 times larger than that of liquid. By penetrating the supercritical fluid into the extraction target and reacting with the desired content, extraction of high purity content becomes possible.

In the present invention, the supercritical fluid used for supercritical extraction is carbon dioxide, and extraction conditions are preferably performed at a temperature of 35 to 45 ° C., a pressure of 100 to 500 bar, and 30 to 240 minutes. As the pressure increases, the extraction yield increases, but the content of phytoncide is lower. Therefore, a preferable pressure condition for increasing the content of the low molecular weight phytoncide component is 150 to 200 bar.

As a pretreatment process for supercritical extraction, washing the cypress, drying, and grinding may be performed. The drying step of the pretreatment step is preferably low temperature cold air drying or lyophilization in order to prevent the phytoncide component from volatilizing. In particular, it is preferable to add 35 degreeC low temperature cold air, and to dry.

Supercritical extraction may be performed using a mixed fluid in which co-solvent is added to supercritical fluid carbon dioxide. The cosolvent may use one or more of ethanol, methanol, water, ethyl acetate, hexane and diethyl ether, preferably 80% to 100% ethanol, most preferably 95% ethanol.

The cosmetic composition of the present invention may contain from 0.01 to 10% by weight, based on the total weight of the composition of the supernatant extract. Moisture effect is less when the baekyak supercritical extract is less than 0.01% by weight, it is difficult to have an elevated effect compared to the content when it exceeds 10% by weight.

The cosmetic composition of the present invention can be usefully used as a body care product that protects the skin by applying to the whole body as well as facial cosmetics applied to the face.

Cosmetic composition of the present invention by adding a variety of well-known ingredients and the like using methods known in the art, lotion, lotion, cream, essence, pack, makeup base, foundation, cleansing oil, cleansing foam, hair oil, hair shampoo And hair rinses.

Specifically, when the formulation of the cosmetic composition of the present invention is a paste, cream or gel, pack, as known components, animal fibers, plant fibers, waxes, paraffins, starches, tragacanth, cellulose derivatives, polyethylene glycol, silicone, bentonite, Silica, talc or zinc oxide and the like can be used.

When the formulation of the cosmetic composition of the present invention is a powder, lactose, talc, silica, aluminum hydroxide, calcium silicate or polyamide powder may be used.

When the formulation of the cosmetic composition of the present invention is a solution or emulsion, a solvent, solvating agent or emulsifying agent is used, such as water, ethanol, isopropanol, ethyl carbonate, ethyl acetate, benzyl alcohol, benzyl benzoate, propylene glycol, 1, 3-butylglycol oil, glycerol aliphatic ester, polyethyleneglycol or sorbitan non-dispersion ester and the like can be used.

Water, liquid diluents such as ethanol or propylene glycol, suspending agents such as ethoxylated isostearyl alcohol, polyoxyethylene sorbitol ester and polyoxyethylene sorbitan ester when the formulation of the cosmetic composition of the present invention is a suspension, microcrystalline Cellulose, aluminum metahydroxy, bentonite, agar or tragacanth and the like can be used.

Aliphatic alcohol sulfate, aliphatic alcohol ether sulfate, sulfosuccinic acid monoester, isethionate, imidazolinium derivatives, methyltaurate, sarcosinate, fatty acid amide ether sulfate when the formulation of the cosmetic composition of the present invention is a surfactant-containing detergent , Alkylamidobetaines, aliphatic alcohols, fatty acid glycerides, fatty acid diethanolamides, vegetable oils or ethoxylated glycerol fatty acid esters and the like can be used.

In addition to the cosmetic composition of the present invention can be used as a conventional known ingredients such as stabilizers, solubilizers, vitamins, pigments and fragrances, can be prepared in any formulation commonly prepared in the art, Can be appropriately selected accordingly.

As an example of the formulation, the lotion may contain 0.1 wt% of carbomer, 0.1 wt% of hydroxyethyl cellulose, 2.0 wt% of butylene glycol, 1.0 wt% of glycerin, 0.5 wt% of Fiji-1500, 4.0 wt% of ethanol, poly Sorbate 80 0.2% by weight, triethanolamine 0.1% by weight, preservatives (trace), purified water (residual amount), can be composed of 2% by weight of the supernatant extract.

In addition, as an example of the formulation, the nutrition cream is 1.5% by weight of cetearyl alcohol, 1.0% by weight of glyceryl stearate, 1.0% by weight of polysorbate 60, 0.3% by weight of sorbitan sesquioleate, 6.0% by weight of cetyloctanoate. , 8.0% by weight squalene, 4.0% by weight of apricot kernel oil, 2.0% by weight of dimethicone, butylene glycol 4.0% by weight, glycerin 4.0% by weight, magnesium aluminum silicate 0.4% by weight, xanthan gum 0.03% by weight, preservative ), Purified water (remaining amount), can be composed of 2% by weight of a cypress supercritical extract.

In addition, as an example of the formulation, the foundation may be 2.0% by weight of stearic acid, 0.5% by weight of cetearyl alcohol, 1.0% by weight of glyceryl stearate, 0.5% by weight of polysorbate 60, 0.7% by weight of sorbitan sesquioleate, hydro 2.0% by weight of genelade seed oil, 5.0% by weight of sunflower oil, 6.0% by weight of squalane, 4.0% by weight of cetyloctanoate, 2.0% by weight of cyclomethicone, 5.0% by weight of butylene glycol, 3.0% by weight of glycerin Silicate 0.6%, xanthan gum 0.05%, titanium dioxide 10.0%, talc 3.0%, hydrated ferric oxide 1.3%, ferric oxide 0.3%, ferrus-ferric oxide 0.15%, preservative (trace) , Purified water (remaining amount), may be composed of 2% by weight of a cypress supercritical extract.

In addition, as an example of the formulation, the lotion may include 1.0 wt% of carbomer, 2.0 wt% of dimethicone, 5.0 wt% of jojoba oil, 0.5 wt% of provitamin E, 1.0 wt% of olive emulsion wax, 5.0 wt% of arbutin paste, and T-mixture. 1.2 wt%, foam mix 1.0 wt%, batine 1.0 wt%, cetearyl alcohol 1.5 wt%, glycerin 4.0 wt%, flex oil 5.0 wt%, arbutin paste 5.0 wt%, white powder supercritical extract 5.0 wt%, It may be composed of blending essence oil (trace amount), preservative (trace amount), purified water (residual amount).

In addition, as an example of the formulation, the pack is 5.0 wt% butylene glycol, 12.0 wt% polyvinyl alcohol, 2.0 wt% polyvinylpyrrolidone, ethanol 8.0 wt%, polyvinylacetate 1.0 wt%, preservative (trace), purified water (Residual amount), and may be composed of 2% by weight of a cypress supercritical extract.

In addition, an example of a formulation, in particular, body essence, which is a kind of body care, is 1.0% by weight of cetearyl alcohol, 1.6% by weight of glyceryl stearate, 0.5% by weight of beeswax, 0.5% by weight of hydrogenated lecithin, neopentylgly Cold dicaprate 3.0 wt%, hydrogenated polydecene 4.0 wt%, capric triglyceride 2.0 wt%, cyclopentasiloxane 5.0 wt%, tocopheryl acetate 0.2 wt%, dimethicone 0.3 wt%, propylparaben 0.1 wt% 0.03% trisodium editie, 0.2% methylparaben, glycerin 6.5%, dipropylene glycol 4.5%, xanthan gum 0.03%, carbomer 0.16%, potassium hydroxide 0.071%, It may be composed of 0.2% by weight of phenoxyethanol, 0.1% by weight of dipotassium glycylizate, 3.5% by weight of a cypress supercritical extract, and purified water (residual amount).

Hereinafter, the following Experimental Examples are provided to help the understanding of the present invention, but the following Experimental Examples are merely to illustrate the present invention and the scope of the present invention is not limited to the following Experimental Examples.

Extraction Experiment

1. Sample Collection and Pretreatment

The species used in this experiment were grown on the premises of Jangseong area. The cypress leaves collected in October 2010 from Jangseong Cypress Forest Cooperative Farming Corporation were used for the experiment.

The cypress leaves were washed with water to remove foreign substances, sealed in a polyethylene plastic bag, and then stored in a 4 ° C. cold room to be used as a sample. The low temperature cold air drying method was used for drying, and the low temperature freeze air drying was performed at 35 ° C. for about 24 hours using a low temperature cold air dryer (GCT-0615, Green Cooltec). The dried cypress leaves were ground with a blender and immediately extracted with a supercritical fluid extraction equipment.

2. Extraction process conditions

The pre-treated protein samples (leaflets after grinding) were extracted using a supercritical fluid extraction (CO ₂ Supercritical Fluid Extraction (0.5L)) equipment (SCFE-0500, Ilshin Autoclave).

The temperature of the crystallization tank was preheated to 40 ° C. before injecting the protein in the crystallization tank. When the temperature of the crystallization tank is stabilized at 40 ° C., a high-pressure pump is used to inject the protein into the crystallization tank, and a certain amount of anti-solvent (CO ₂ ) is injected through the upper line until the experimental pressure (100 to 500 bar) is reached. . The valve was adjusted so that the pressure of the crystallization tank changed linearly with time during the gas injection. After a certain period of time (30-240 minutes), the valve in the lower part of the crystallization tank was opened and slowly exhausted, while pure CO ₂ gas was injected from the upper part to maintain a constant pressure in the crystallization tank during the exhaust. . Pure CO ₂ gas was injected and then depressurized to obtain an ocular supercritical extract.

3. Extraction yield of cypress supercritical extract

In order to confirm the extraction yield of the Cyclic supercritical extract according to the extraction conditions, the extraction yield with time at each extraction pressure in the extraction temperature (40 ℃) is shown in Table 1 below. Extraction yield (%) was calculated as (extraction amount (g) / injection sample amount (g)) × 100, extraction amount (g) was calculated as the injection sample amount-sample amount after extraction.

division
 Extraction time (min) 30 60 90 120 150 180 210 240

Extraction pressure (bar)

100 65% 74% 87% 97% 99% 99% 100% 100% 150 61% 76% 78% 80% 90% 93% 97% 100% 200 68% 80% 85% 90% 92% 93% 96% 100% 250 64% 75% 81% 85% 92% 95% 98% 100% 300 57% 68% 76% 84% 88% 91% 96% 100% 400 54% 63% 76% 88% 93% 97% 100% 100% 500 55% 68% 74% 81% 88% 95% 98% 100%

Referring to Table 1, the extraction efficiency increased with increasing time at the same pressure. In general, the yield of hot water extraction was less than 5%, whereas the yield of supercritical fluid extraction was very high.

4. Component Analysis of Cyclic Supercritical Extracts

The extracted cypress supercritical extract was sufficiently stirred in hexane to remove suspended matter using a centrifuge, and then filtered by a micro filter (0.45 μm). Component analysis was performed using the GC / MS equipment (240-MS, Varian) under the following conditions. The column is VF-5ms (30mm × 0.25mm × 0.25mm), Heri (1mL / min) as carrier gas, Injection temperature is 250 ℃, Oven temperature is 50 ~ 300 ℃ / 3 ℃, Injection volume is 1µl, The injection mode was analyzed at the split ratio of 10: 1, and the mass range was 28 ~ 550 in the mass selective detector (MDS).

First, the lag time of the components of the extract of supernatant extracted at 40 ° C., 150 bar and 180 minutes as extraction conditions is shown in the GC / MS graph of FIG. 1. In addition, the qualitative analysis results of the Cyclic supercritical extract are shown in Table 2 below in comparison with the delay times of 33 representative standards among phytoncide components.

Material name RT (min) Material name RT (min) Material name RT (min) Camphene 10.881 Isobornyl acetate 18.832 alpha-gurjunene 32.781 Sabinene 11.988 Thujone 20.315 alpha-(-) cedrene 33.136 Pinene (-)-B- 12.204 Terpinene-4-ol 22.504 Caryophyllene
(-)-trans- 33.289 Myrcene 12.913 Terpineol-alpha 23.229 beta-caryophyllene 33.29 Phellandrene 13.716 alpha-fenchyl acetate 24.276 beta-chamigrene 35.855 alpha-terpinene 14.262 Bornyl acetate 27.39 Nerylisobutyrate 36.031 Cymene 4- 14.662 alpha-thujone 27.502 cis-nerolidol 37.859 Limonene 14.851 Longifolene 32.857 Nerolidol trans- 39.065 Terpinene-r 16.385 Longipinene 30.279 cis-hexanyl benzoate 39.508 Terpinolene 17.755 Linalyl acetate 25.79 Cedrol 40.913 Linalool 18.505 Isolongifolene 32.158 Eudesmol. B. 42.661

 Referring to Figure 1 and Table 1, it can be seen that the main components of the cyanoacidic supercritical extract is the same as the phytoncide component. In addition, phytoncide components contained in the Cyclic supercritical extract showed a peak within 40 minutes.

And the higher the pressure during extraction, it was confirmed that many peaks appeared even after 40 minutes, which seems to be the result of extracting even the components of high molecular weight in the cypress leaf as the pressure increases. Therefore, in order to increase the content of phytoncide components having a relatively low molecular weight (100-300) and high volatility, it may be desirable to extract them under relatively low pressure, that is, 200 bar or less.

Next, the difference in the content of the cypress supercritical extract according to the drying method as a pretreatment process was examined. Volatilization of phytoncide component with high volatility is expected in the drying process, and two drying methods (low temperature cold air drying and freeze drying) were used. Cyclone supercritical extract extracted from the above-mentioned low-temperature cold air drying method (40 ° C., 150 bar, 180 minutes) and cypress extract extracted from the free-dry method (40 ° C., 150 bar, 180 minutes). Critical extracts were compared and shown in the GC / MS graph of FIG. 2. And the content of the main component is shown in Table 3. The lyophilization was performed by lyophilizing the cypress leaves at -40 ° C. for 72 hours using a lyophilizer (OPR-FDT-8650, OPERON).

ingredient Freeze-drying content (%) Low temperature and cold air content (%) alpha-pinene 0.633 0.676 camphene 0.092 0.106 sabinene 6.685 8.471 pinene- (b) 0.13 0.116 myrcene 0.957 1.109 limonene 1.451 1.608 terpinene-gamma 0.733 0.758 terpinolene 0.371 0.423 alpha-fenchyl acetate 0.37 0.446 Linalylacetate 0.507 0.679 bornyl acetate 3.038 3.074 terpinyl acetate 6.043 5.114 alpha-(-)-cedrene 0.358 0.323 caryophyllene-trans 0.366 0.423 neryl isobutyrate 1.328 1.552 cis-nerolidol 0.324 0.298 Nerolidol-trans 1.205 0.801 cedrol 1.594 1.457 Sum 26.385 27.434

Referring to Figure 2 and Table 3, the degree of volatilization of each component is different depending on the drying method, the content of the total component was found to be 1% higher than lyophilization during low temperature cold air drying. Therefore, it was confirmed that the difference in phytoncide content according to the drying method was not great, but the low temperature freeze drying method appeared to be somewhat advantageous in terms of content.

Next, in order to find out the volatility of the phytoncide component contained in the supernatant extract and its residual level, a predetermined amount of the supernatant extract extracted from the protein extract (40 ° C., 150 bar, 180 minutes) using a low temperature cold air drying method was taken. Was left in the air and the other was sealed. After 3 days, each sample was dissolved in hexane, and the results of component analysis are shown in the GC / MS graph of FIG. 3. And the content of the main component is shown in Table 4.

ingredient Content after sealing for 3 days (%) % Content after 3 days alpha-pinene 0.62 0.00 camphene 0.10 0.00 sabinene 7.83 0.01 pinene- (b) 0.11 0.00 myrcene 1.02 0.00 limonene 1.49 0.01 terpinene-gamma 0.65 0.02 terpinolene 0.37 0.03 alpha-fenchyl acetate 0.42 0.29 Linalylacetate 0.65 0.54 bornyl acetate 2.98 2.65 terpinyl acetate 5.05 5.16 alpha-(-)-cedrene 0.32 0.30 caryophyllene-trans 0.41 0.41 neryl isobutyrate 1.52 1.62 cis-nerolidol 1.06 1.24 Nerolidol-trans 0.95 1.10 cedrol 1.44 1.68 Sum 26.98 15.06

Referring to FIG. 3 and Table 4, the peaks were not found 20 minutes before the Cyclic supercritical extract was left in air for 3 days. It was found that more than 95% of the components showing peaks were volatilized 20 minutes before. Most of the components appearing within 20 minutes were volatilized within 3 days because they were relatively low molecular weight components, while those appearing after 40 minutes were almost unvolatiled due to their high molecular weight. These results were markedly different in peaks within 20 minutes compared to the sealed and stored for three days.

In addition, there are more components (cis-nerolidol, nerolidol-trans, cedrol, etc.) that are left in the air for 3 days but sealed and stored for 3 days.The low molecular weight component is volatilized and the high molecular weight component is concentrated. It seems to have been.

Through the above experimental results, it was shown that the mass extraction conditions for obtaining a high-protein cyclic supercritical extract having a high content of phytoncide components using a supercritical fluid extraction method are optimal at a temperature of 40 ° C. and a pressure of 150 to 200 bar. And the extraction time is suitable 30 to 240 minutes, considering the yield 180 to 240 minutes is preferred.

On the other hand, the changes of the components according to the number of extraction when the extraction of the protein samples dried by the low temperature cold air drying method of the optimum extraction conditions at 40 ℃, 150 bar, 180 minutes. For this purpose, the results of analysis of the components of the protein extract supercritical extract (once extract) obtained by extracting once and the protein extract supercritical extract (twice extract) obtained by extracting twice consecutively under the same conditions are shown in FIG. Shown in the / MS graph. And the content of the main component is shown in Table 5.

ingredient Content of single extract (%) Content of twice extract (%) alpha-pinene 0.268 0.545 camphene 0.0528 0.115 sabinene 3.6192 6.392 pinene- (b) 0.0415 0.085 myrcene 0.546 1.096 limonene 1.132 2.057 terpinene-gamma 0.265 1.016 terpinolene - 0.469 alpha-fenchyl acetate 0.5217 0.926 Linalylacetate 0.524 1.197 bornyl acetate 3.514 7.632 terpinyl acetate 8.14 15.39 alpha-(-)-cedrene 0.295 0.533 caryophyllene-trans 0.441 1.02 neryl isobutyrate 0.849 2.693 cis-nerolidol 0.876 0.561 Nerolidol-trans 1.0326 2.473 cedrol 1.485 1.25 Sum 23.6028 45.45

Referring to FIG. 4 and Table 5, about 23.6% of phytoncide components were extracted in one extraction, and about 45.5% of phytoncide components in two extractions. Therefore, it was confirmed that a high purity phytoncide component can be obtained during re-extraction.

On the other hand, the Cyclone supercritical extract, which was extracted under conditions of 40 ° C., 150 bar and 180 minutes, was analyzed by Prep-HPLC.

Specifically, the extracted Cyclic supercritical extract was pretreated under the following conditions by reverse phase HPLC conditions. The cypress extract was first dissolved in methanol, and then centrifuged to separate the supernatant under the following conditions using Prep-HPLC. The column is ODS (250mm L × 20mm ID, 5㎛), flow rate is 10mL / min, injection volume is 1ml, column temperature is room temperature, UV-Vis detector (SPD-20A, Shimadzu) is 210nm, mobile phase composition is Fraction was performed under both conditions of ACN (acetonitrile) 70% and methanol 70%. The results are shown in FIG. 5.

Referring to FIG. 5, it was confirmed that different chromatography appears depending on the composition of the mobile phase. When the mobile phase was analyzed under the ACN 70% condition, the peaks were sharp and clear, while the methanol 70% showed a gentler peak shape than the ACN 70%.

And in order to compare the results according to the drying method is shown in Figure 6 by analyzing the protein extract supercritical extract extracted under conditions of 40 ℃, 150 bar, 180 minutes dried by the freeze-drying method. At this time, the mobile phase was MeOH 70% conditions.

Referring to FIG. 6, the same peaks were observed at the same delay time as a result of analyzing the Cyclic supercritical extract extracted after freeze-drying and cold-air drying in a mobile phase MeOH 70% condition. This means that the same components are detected at the same delay time and the concentrations were somewhat different. In particular, peaks appearing within 15 minutes differed by up to three times in concentration, which appeared to be an error in the pretreatment process of the Cyclic supercritical extract, rather than due to differences in drying methods.

Experimental Example 1: Skin Safety Evaluation

Skin safety evaluation experiment was carried out using the Cyclic supercritical extract. Cyclic supercritical extract used in the experiment is the extract obtained in the above-mentioned extraction experiment, that is, the cold-air dried the cypress leaves, pulverized with a blender, and then the supercritical extract supercritical extract extracted under supercritical conditions at 40 ° C., 150 bar and 180 minutes. It was used (the same in Experimental Examples 2 and 3 described later).

80 μl of a supernatant extract was attached to the skin patch (IQ chamber ultra, sweden) and then attached to the back, and then sealed for 48 hours. After removing the sealed patch, it was read for 3 days at an interval of 24 hours to evaluate the hypersensitivity reaction (allergy, erythema, etc.) occurring on the skin. The subjects were 31 adults (8 males, 13 females) with an average age of 24.8 ± 4.3. The ratio of males to females was 1: 2.8, with a large proportion of females. The sex and age distribution of subjects is shown in Table 6 below.

gender Age distribution personnel male 23-30 years old 8 people female 19-30 years old 23 persons 24.8 ± 4.3 (Average age) 31 people in total

The experimental results of completing the patch test are shown in Table 7 below.

gender Skin irritation Skin sensitization male 0 people 0 people female 0 people 0 people Distribution 0/31 people 0/31 people

Referring to Table 7, all 31 subjects showed no irritation or hypersensitivity reaction such as erythema and edema itching on the skin. In view of these results, it appears that the cosmetic composition containing the supernatant extract can be used safely without irritation.

Experimental Example 2: Skin Moisturizing Evaluation

Thirteen women aged 21 to 36 years old were evaluated by measuring the moisture content of the skin before and after applying the body essence containing the supernatant extract.

The body essence used in the experiment was 1.0% by weight of Cetaryl Alcohol, 1.6% by weight of Glyceryl Stearate, 0.5% by weight of Beeswax, 0.5% by weight of Hydrogenated Lecithin. %, Neopentyl Glycol Dicaprate 3.0 wt%, Hydrogenated Polydecene 4.0 wt%, Capric Triglyceride 2.0 wt%, Cyclopentasiloxane 5.0 wt%, Tocopheryl Acetate 0.2 wt%, Dimethicone 0.3 wt%, Propylparaben 0.1 wt%, Trisodium EDTA 0.02 wt%, Methylparaben ) 0.2% by weight, Glycerin 6.5% by weight, Dipropylene Glycol 4.5% by weight, Xanthan Gum 0.03% by weight, Carbomer 0.16% by weight, Potassium Hydroxide ( Potass ium Hydroxide) 0.071% by weight, phenoxyethanol 0.2% by weight, Dipotassium Glycyrrhizate (0.1% by weight), Cyclic supercritical extract 3.5% by weight, purified water (residual amount).

Body essence 1 FTU (Finger Tip Unit) was taken evenly on the back of the left hand, the skin moisture before and after applying the body essence 20 minutes after measuring three times to calculate the average value. Moisture of the skin was measured using Skin diagnostic SD 27 (Courage & khazaka, Germany) and the results are shown in Table 8 below.

No. Before applying After Before applying
medium Average pack One 22 34 31 39 43 51 29.00 44.33 2 25 32 26 34 34 39 27.67 35.67 3 22 22 22 23 26 29 22.00 26.00 4 15 20 22 54 60 60 19.00 58.00 5 31 29 32 45 48 51 30.67 48.00 6 12 0 8 20 26 31 6.67 25.67 7 40 42 45 63 63 67 42.33 64.33 8 40 37 29 56 65 68 35.33 63.00 9 28 36 32 65 70 67 32.00 67.33 10 37 42 50 68 68 71 43.00 69.00 11 36 42 48 68 63 68 42.00 66.33 12 56 67 63 60 68 73 62.00 67.00 13 15 15 17 31 29 34 15.67 31.33 Mean ± SD 31.33 ± 3.31 51.23 ± 3.06

Referring to Table 8 and FIG. 7, after applying skin essence, which was 31.33 before applying body essence, about 63.5% was increased to 51.23. In view of these results, it is expected that the cosmetic composition of the present invention containing cypress supercritical extract exhibits an excellent moisturizing effect.

Experimental Example 3: Sensory Evaluation

For the experimenters who conducted the skin moisturizing evaluation experiment, the sensory evaluation questionnaire was prepared to subjectively determine the feeling of use, fragrance, moisturizing feeling, spreadability, and persistence of the body essence. Sensory evaluation results are shown in Table 9 and FIG. 8.

Feeling incense Moisturizing Brittle Persistence Average 4.07 ± 0.46 3.93 ± 0.59 4.14 ± 0.64 4.29 ± 0.70 4.07 ± 1.10 4.10 ± 0.74

As a result of the sensory test, the subjects showed high satisfaction with an average of 4.10 (maximum 5 points) in all items of feeling, fragrance, moisturization, applicability, and residualness of body essence. The distinctive scents from the supercritical extracts of the cypress have positive reactions such as `` refreshing as if in the forest '', `` feels comfortable '', `` heads cool '', and `` the fragrance becomes accustomed without reluctance over time. '' Indicated.

In the above, the present invention has been described with reference to one embodiment, which is merely exemplary, and it will be understood by those skilled in the art that various modifications and equivalent embodiments are possible. Therefore, the true scope of protection of the present invention should be defined only by the appended claims.

Claims (5)

Cosmetic composition using a supernatant supercritical extract, characterized in that it contains a supernatant supercritical extract extracted from the supernatant using a supercritical fluid extraction method. The method of claim 1, wherein the supercritical fluid extraction method uses carbon dioxide as a supercritical fluid,
The protein supercritical extract is a cosmetic composition using the protein supercritical extract, characterized in that extracted for 30 to 240 minutes by adding supercritical carbon dioxide at a temperature of 35 to 45 ℃, pressure 100 to 500bar to the pyebaek. According to claim 1 or 2, wherein the cosmetic composition is 1.0% by weight of cetearyl alcohol, 1.6% by weight of glyceryl stearate, 0.5% by weight of beeswax, 0.5% by weight of hydrogenated lecithin, neopentyl glycolica Crate 3.0 wt%, Hydrogenated polydecene 4.0 wt%, Capric triglyceride 2.0 wt%, Cyclopentasiloxane 5.0 wt%, Tocopheryl acetate 0.2 wt%, Dimethicone 0.3 wt%, Propylparaben 0.1 wt%, Tri 0.02% sodium editae, 0.2% methylparaben, 6.5% glycerin, 4.5% dipropylene glycol, xanthan gum 0.03%, carbomer 0.16%, potassium hydroxide 0.071%, phenoxy It is a body care composed of 0.2% by weight of ethanol, 0.1% by weight of dipotassium glycylizate, 3.5% by weight of cypress supercritical extract, and the remaining amount of purified water.
The cosmetic composition is a cosmetic composition using a pike supercritical extract, characterized in that it has a moisturizing activity. A drying step of drying the protein;
An extracting step of extracting a protein of supercritical extract from the dried protein, using a supercritical fluid extraction method;
It is added to contain the supernatant extract in an amount of 0.01 to 10% by weight based on the total weight of the composition, lotion, lotion, cream, essence, pack, makeup base, foundation, cleansing oil, cleansing foam, hair oil, hair shampoo and Formulation step of preparing to any one of the formulations selected from the hair rinse; Method of producing a cosmetic composition using a supernatant supernatant extract comprising a. 5. The method of claim 4, wherein the drying step comprises drying the protein at a low temperature of 35 ° C.

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