JP7222483B2 - Method for preparing cycad extract - Google Patents

Description

Application of Article 30, Paragraph 2 of the Patent Law 1. Posting address: https://evt-reg2. jp/reg3/Usr/citejapan2019/Usr_search. php https://evt-reg2. jp/reg3/Usr/citejapan2019/Usr_detail. php? form_id=182&eid=64417&lang=1 Release date: April 5, 20192. Exhibition name: 9th Cosmetic Industry Technology Exhibition (CITE JAPAN 2019) Exhibition date: May 14, 2019-May 17, 2019 3. Posting address: http://www. katakuraco-op. com/http://www. katakuraco-op. com/business/index. html http://www. katakuraco-op. com/business/cosmetic. html Release date: May 30, 2019 4. Posting address: https://evt-reg2. jp/reg3/Usr/citejapan2019/Usr_search. php https://evt-reg2. jp/reg3/Usr/citejapan2019/Usr_detail. php? form_id=182&eid=64417&lang=1 Release date: April 5, 20195. Exhibition name: 9th Cosmetic Industry Technology Exhibition (CITE JAPAN 2019) Exhibition date: May 14, 2019-May 17, 2019 6. Posting address: http://www. katakuraco-op. com/http://www. katakuraco-op. com/business/index. html http://www. katakuraco-op. com/business/cosmetic. html Publication date: May 30, 2019

In the present invention, a solution (also referred to as "nanobubble liquid" in this specification and the like) containing nano-sized fine bubbles (also referred to as "nanobubble" in this specification and the like) is brought into contact with Matteuccia struthioopteris. The present invention relates to a method for preparing a cycad extract by exposing the cycad extract, to the cycad extract extracted by the method, and to compositions and cosmetics containing the cycad extract.

Differences in hair quality also change with age and gender, and are said to differ between Asians and Westerners. Among them, frizzy hair such as curly hair and wavy hair is considered to be caused by various factors such as genetics, growth process, and lifestyle habits. The structure of hair can be roughly divided into three layers, the central part is called the medulla, the middle part is called the cortex, and the outer layer is called the cuticle. , is considered to be an important tissue that determines hair quality such as thickness and suppleness. When the protein fibers inside the cortex are regularly arranged, the hair maintains a straight hair. In addition, it is known that when the protein structure is non-uniform and the hair absorbs moisture, the moisture balance inside the hair is disrupted, causing the hair to swell and tend to twist.

In this way, the imbalance of the protein fiber structure inside the cortex causes frizzy hair such as curly hair and wavy hair. technology is known. Curly hair straightening is performed, for example, as follows. First, the cystine bonds inside the hair are once cut by treating the hair with a strong chemical. Next, heat the hair with a curling iron to straighten it. After that, cystine bonds are re-formed inside the hair, and the hair is forcibly treated so that it can be maintained in a straight hair state. As described above, the general curly hair straightening method often damages the hair due to the strength of the chemicals used and the heat treatment, and often causes itching and inflammation of the scalp.

For example, as an extract for straightening curly hair, an ergothioneine-containing extract derived from animals or plants or a derivative of ergothioneine has been reported (Patent Document 1).

On the other hand, many of the causes of skin aging are said to be caused by oxidative stress. And oxidative stress can be caused by active oxygen. Active oxygen is a general term for substances that have changed from oxygen molecules to highly reactive substances with stronger oxidizing action. Active oxygen is known to be produced in the body when our body is exposed to sunlight (ultraviolet rays). Furthermore, although we take in oxygen through respiration, reactive oxygen species are also produced as a by-product in the process of the respiratory chain reaction. Reactive oxygen has a strong oxidizing effect, so it has a strong bactericidal effect and plays an important role in protecting the body from bacteria. It denatures the proteins that make up certain collagen and elastin. As a result, the tension and elasticity of the skin decrease, causing skin aging such as sagging and wrinkles.

In addition, our body has various substances that function as an excellent defense system against oxidative stress caused by active oxygen. However, it is known that the activity and production of these substances decrease due to aging and lifestyle habits, and that the production of active oxygen itself is excessive due to changes in the living environment. Among active oxygens, superoxide is a precursor of various active oxygens, and the subsequent chain reaction generates hydroxyl radicals, which have the highest reactivity among active oxygens.

In order to combat oxidative stress caused by such active oxygen, powders and/or extracts of plants of the genus Spruce in the Asteraceae family have been reported as plants having antioxidant activity (Patent Document 2). Moreover, as a plant having a superoxide scavenging action, for example, an organic solvent or aqueous extract of Cuphea balsamona Cham., a perennial herb belonging to the Lythraceae family, has been reported (Patent Document 3). Furthermore, ergosterol, which is a kind of sterol contained in fungi such as mushrooms and yeast, has been reported as having an active oxygen production inhibitory action (Patent Document 4).

JP 2011-144136 A JP-A-2004-155961 JP-A-05-301822 JP 2011-148790 A

However, the ergothioneine-containing animal/plant-derived extract or ergothioneine derivative described in Patent Document 1 does not have a sufficient hair-straightening effect. Therefore, from the standpoint of safety for the hair as well as the scalp, there is a demand for a safe, naturally derived extract that can be used as a natural product, is less irritating, and has a high straightening effect on curly hair.

Furthermore, the antioxidative function of the plants having antioxidative action described in Patent Documents 2 to 4 is also insufficient. Therefore, in order to prevent skin aging in particular, superoxide itself, which is naturally derived and can be used in terms of safety for human skin and has an antioxidant effect that protects against oxidative stress by oxidizing itself, is rapidly produced. There is a demand for further plant extracts that have strong anti-oxidative functions against skin aging, such as anti-oxidant functions such as scavenging effects and suppressing the production of active oxygen itself.

Therefore, the present inventors paid their attention to Kusasotetsu (Matteuccia struthiopteris). Kogomi, which is another name for the young buds of Kusa sotetsu, is a spring wild vegetable that has a shape that looks like a spring when the leaves are not open and the tips are wrapped around. It is eaten by cooking methods such as Kogomi is characterized by a slightly slimy texture, no lye, and a light taste, so freshly harvested kogomi can be eaten raw. Cogomi is rich in dietary fiber and is known to have an intestinal regulation effect by activating the function of the intestines.

Accordingly, an object of the present invention is to provide a method for preparing a sagebrush extract from sagebrush, a sagebrush extract extracted by the method, and compositions and cosmetics containing the sagebrush extract.

The present inventors have made intensive studies in order to solve the above problems, and as a result, using a nanobubble liquid containing nano-sized fine bubbles, the extract from the cycad (in this specification, it is referred to as "the lycopodium nanobubble liquid extraction The resulting extract of sage beetle nanobubbles has a new curly hair straightening action, an antioxidant action, a superoxide scavenging action, and an active oxygen production inhibiting action, which could not be obtained with conventional techniques. The present inventors have completed the present invention.

Here, the nanobubble liquid is a solution containing fine bubbles having a nanometer-level diameter called nanobubbles. For example, nanobubble water, which is obtained by injecting nanobubbles into water, has an extremely small particle size, and is characterized by being transparent with no visible bubbles like carbonated water for drinking. Nanobubble water is known to be highly permeable to normal water. In addition, the effect of nanobubble water varies depending on the type of gas to be nanoized, but when ozone is used, it has a bactericidal effect on microorganisms and cells (see, for example, International Publication No. 2016/088731). It is known that As a method of using nanobubbles, bath water containing carbon dioxide nanobubbles is prepared, and the bath water is used to dissolve calcium ions and magnesium ions and to contain medicinal ingredients of herbal medicines, thereby increasing blood flow. A device that produces artificial carbonated hot springs (see, for example, Japanese Unexamined Patent Application Publication No. 2008-212276), a shower head that generates micro-nano bubbles, and a cartridge containing volcanic ash and volcanic lava are combined to create new functions of detergency and refreshing sensation. There is a shower device (see, for example, Japanese Unexamined Patent Application Publication No. 2017-12644) that realizes this.

That is, the present invention includes the following.
(1) A method of preparing a cycad extract by contacting a nanobubble liquid containing nano-sized fine bubbles with a cycad (Matteuccia struthiopteris).
(2) The method according to (1), wherein the nano-sized fine bubbles are carbon dioxide.
(3) The method according to (1) or (2), wherein the nanobubble liquid is nanobubble water.
(4) A cycad extract extracted from cycad (Matteuccia struthioopteris) using a nanobubble liquid containing nano-sized fine bubbles.
(5) The cycad extract according to (4), wherein the nano-sized fine bubbles are carbon dioxide.
(6) The Kusa cycad extract according to (4) or (5), wherein the nanobubble liquid is nanobubble water.
(7) A composition comprising the cycad extract of any one of (4) to (6).
(8) The composition according to (7), further comprising a nanobubble liquid containing fine nanobubbles.
(9) The composition according to (8), wherein the nano-sized fine bubbles are carbon dioxide.
(10) The composition according to (8) or (9), wherein the nanobubble liquid is nanobubble water.
(11) The composition according to any one of (7) to (10), which is a curly hair straightening composition having a curly hair straightening action.
(12) The composition according to any one of (7) to (11), which is an antioxidant composition having an antioxidant function.
(13) A cosmetic containing the cycad extract according to any one of (4) to (6) or the composition according to any one of (7) to (12).

The present invention provides a method for preparing an extract from S. cysticae, a S. cysticum extract extracted by the method, and compositions and cosmetics containing the S. cysticum extract. ADVANTAGE OF THE INVENTION According to this invention, the antioxidant function of the outstanding curly hair straightening effect|action, an antioxidant effect|action, a superoxide elimination effect|action, and an active oxygen production inhibitory effect|action is provided.

Fig. 10 is a photograph showing the state of a hair bundle before the test in the <curly hair straightening action>. Fig. 10 is a photograph showing the state of a hair bundle after a test in <curly hair straightening action>. 1 is a graph showing radical scavenging rates at 250 ppm and 500 ppm in Example 1 and Comparative Examples 1-7. 1 is a graph showing superoxide scavenging rates at 125 ppm, 250 ppm and 500 ppm in Example 1 and Comparative Examples 1-7. 1 is a graph showing the amount of active oxygen produced in hydrogen peroxide (+) and hydrogen peroxide (−) in Control, Example 1 and Comparative Examples 1 to 3. FIG. 2 is a graph showing the amount of reactive oxygen produced in hydrogen peroxide (+) and hydrogen peroxide (−) in Control and Comparative Examples 4 to 7. FIG.

The present invention will be described in detail below. In addition, the present invention is not limited to the following embodiments, and can be implemented in various forms with modifications, improvements, etc. that can be made by those skilled in the art without departing from the scope of the present invention.

The present invention relates to a method for preparing an extract of sagebrush by contacting a nanobubble liquid containing fine nanobubbles (nanobubbles) with sagebrush. The present invention relates to a sagebrush nanobubble liquid extract, and compositions and cosmetics containing the sagebrush nanobubble liquid extract.

The present invention is based on the finding that the sagebrush nanobubble liquid extract has an excellent curly hair-improving action and an antioxidant function. The present invention further relates to an extract using carbon dioxide nanobubble water of cycad (also referred to herein as "extract of carbon dioxide nanobubble of cycad"). The extract of the present invention has an excellent effect of contributing to straightening of curly hair and antioxidant function, and can be used as an ingredient of cosmetics.

The Kusa scotch used in the present invention may be the whole plant of Kusa sorghum (Matteuccia struthiopteris), or a part of Kusa sorghum, such as the aerial parts, leaves (vegetative leaves and sporophylls), rhizomes, and any combination thereof. Although it may be, part or the whole plant of Pleurotus thunbergii including leaves is preferred, and the leaves of Pleurotus thunbergii, preferably young shoots, are particularly preferred.

The method for preparing the extract of the cysticotes by contacting the nanobubble liquid with the cysticotes can be any method known in the art, except that the nanobubble liquid prepared as described below is used as the solvent for the extraction. extraction techniques can be used.

With respect to the nanobubble liquid to be used, any general treatment that can be generally applied can be selected. For example, nanobubbles may be injected using a water nanocyclone type multifunctional mixing device (manufactured by CO2 Systems, Inc.). By simultaneously injecting gas while flowing liquid into the device, this device can create a jet water flow through multiple partitions and slits inside the device, and the liquid and gas are compressed inside the device. mixed with. At this time, the gas dissolved in the liquid becomes finer to the nano level and becomes a highly concentrated nanobubble liquid.

Examples of gas to be nanoized include, but are not limited to, carbon dioxide, nitrogen, oxygen, and ozone. Carbon dioxide and oxygen are preferred, and carbon dioxide is more preferred. The flow rate and temperature of the liquid flowing into the device and the pressure of the gas such as carbon dioxide are usually 1 L / min when using a small model of a water nanocyclone type multifunctional mixing device (manufactured by CO2 Systems Co., Ltd.). ~20 L/min, temperature 1°C ~ 70°C, pressure 0.1Mpa ~ 1.0Mpa, preferably flow rate 1L/min ~ 10L/min, temperature 1°C ~ 60°C, pressure 0.1Mpa ~ 0.7Mpa, Most preferably, the flow rate is 1 L/min to 7 L/min, the temperature is 1° C. to 50° C., and the pressure is 0.1 Mpa to 0.5 Mpa.

For example, the extract of Pleurotus thunbergii nanobubbles can be obtained by immersing young shoots of Pleurotus thunbergii in a nanobubble liquid as an extraction solvent, such as nanobubble water, and eluting plant components into the extraction solvent. Here, the kogomi, which is the young bud of the cycad, may be used for extraction as it is collected, or may be used for extraction after being subjected to processing suitable for extraction processing, such as drying, cutting or crushing into an appropriate size. may In terms of extraction efficiency, it is preferable to subject some of the kogomi, which is the young shoots of Kusa sotetsu, to extraction after drying and pulverization. Liquids used to prepare the nanobubble liquid, which is an extraction solvent, include, but are not limited to, alcohol, water, buffer solutions, dilute acids, dilute alkalis, and any combinations or mixtures thereof. When alcohol is used, alcohol (absolute alcohol) or aqueous alcohol solution (mixed solvent of alcohol and water) can be used. Alcohols may be monohydric alcohols or polyhydric alcohols. Specific examples of monohydric alcohols include methanol, ethanol, propyl alcohol, butyl alcohol, isobutyl alcohol, and benzyl alcohol. Polyhydric alcohols include ethylene glycol, propylene glycol, glycerin, 1,3-butylene glycol and the like. When an alcohol aqueous solution is used, it is desirable that the alcohol concentration is 10% to 90% (weight ratio) of the entire aqueous solution. Specifically, hydrous ethanol with an ethanol concentration of 20% to 70% (weight ratio) relative to the entire aqueous solution, and hydrous ethanol with a 1,3-butylene glycol concentration of 20% to 70% (weight ratio) relative to the entire aqueous solution. Solvents such as 1,3-butylene glycol are preferably used. Nanobubble water is preferable as the nanobubble liquid.

As an extraction method, for example, it is preferably 1 part by weight to 200 parts by weight, more preferably 2 parts by weight to 100 parts by weight, and still more preferably 5 parts by weight, relative to 1 part by weight (dry weight) of Kogomi, which is the young shoots of Kusasotetsu. Parts to 100 parts by weight, for example, 5 parts to 50 parts by weight of nanobubble liquid are added, and the young shoots of the cycad are immersed for a certain period of time to perform extraction, but the method is not limited to this.

A person skilled in the art can appropriately adjust the extraction temperature and extraction time in the extraction method by considering the type and amount of the liquid used to prepare the nanobubble liquid. For example, the extraction temperature (temperature of the nanobubble liquid) is not limited, but is usually above 0°C to the boiling point under pressure, preferably from room temperature (10°C to 30°C) to the boiling point under pressure. More preferably 15°C to 100°C, for example 20°C to 70°C. For example, the extraction time (time of immersion in the nanobubble liquid) varies depending on the type of liquid used for preparing the nanobubble liquid and the extraction temperature, but it is usually 1 hour to 6 weeks, preferably 2 hours to 4 weeks, more preferably. 3 hours to 1 week is desirable. Extraction time can be, for example, from 10 hours to 72 hours.

As a preferred example, when nanobubble water is used as the extraction solvent, the extraction temperature is 20° C. to 50° C., for example, room temperature (10° C. to 30° C.), and the extraction time is, for example, 1 hour to 2 weeks, preferably 10 hours. can be ~72 hours. Also, when using nanobubble liquid of anhydrous ethanol or 20% to 70% ethanol aqueous solution (hydrous ethanol) as the extraction solvent, the extraction temperature is 20 ° C. to 70 ° C., for example, room temperature (10 ° C. to 30 ° C.), and the extraction time is can be from 10 hours to 72 hours. Furthermore, when 1,3-butylene glycol (anhydrous) or a nanobubble solution of 1,3-butylene glycol aqueous solution with a concentration of 20% to 70% is used as the extraction solvent, the extraction temperature is set to 20°C to 70°C, such as room temperature (10 ° C to 30 ° C), and the extraction time can be 10 hours to 72 hours.

In addition, after extracting the kogomi, which is the young shoots of the cycad, with the nanobubble liquid as described above, alcohol, water, buffer solution, dilute acid, dilute alkali, nanobubble liquid thereof, and any combination or mixed liquid thereof, etc. Further extraction may be performed using

The so-prepared (extracted) Kusa-sotetsu nanobubble liquid extract may be used as it is as the Kusa-sotetsu nanobubble liquid extract. It may be subjected to the usual treatments that are generally applicable to objects. For example, the extracted Kusasotetsu nanobubble liquid extract may be purified by a well-known purification method such as centrifugation and filtration of precipitates. Furthermore, wintering treatment may preferably be carried out on the filtered Kusasotetsu nanobubble liquid extract. It is desirable that the temperature is -30° C. to 0° C. and the wintering treatment time is 3 to 30 days. In addition, purification treatment for deodorization and decoloration by activated carbon column filtration or the like may be performed, and the extract containing the components of the extracted Kusasotetsu nanobubble liquid extract is subjected to concentration treatment, dilution treatment, or solvent exchange treatment by a conventional method. may be performed. In the present invention, the Soxo tetsu nanobubble liquid extract is the Soxo tetsu nanobubble liquid extract prepared in this way or its processed products (for example, purified products, concentrates, dilutions, solutions in solvents other than extraction solvents, or those , etc.).

The Pleurotus nanobubble liquid extract according to the present invention may be further combined with an additional solvent, e.g., additional nanobubble liquid, to form a composition comprising the Pleurotus nanobubble liquid extract and the additional solvent, e.g., additional nanobubble liquid. good. The solid content concentration in the composition containing the Kusa sotetsu nanobubble liquid extract is not limited, but is usually 0.01% to 10%, preferably 0.1% to 5%, relative to the total weight of the composition. . For example, the liquid used for the additional solvent may be the same liquid as the extraction solvent in the combined C. thunbergii nanobubble liquid extract, including, but not limited to, alcohols, water, buffers, dilute acids, dilute alkalis, and the like. It may be a nanobubble liquid, or any combination or mixed liquid thereof.

As shown in the following examples, the Pleurotus thunbergii nanobubble liquid extract according to the present invention exhibits curly hair straightening action, antioxidant action, superoxide scavenging action, and active oxygen production inhibitory action.

The curly hair straightening action, antioxidant action, superoxide scavenging action, and active oxygen production inhibiting action of the Kusasotetsu nanobubble liquid extract according to the present invention can be measured and evaluated by conventional methods. Specifically, each activity can be measured and evaluated as described in the following examples.

The curly hair straightening action, antioxidant action, superoxide scavenging action, and active oxygen production inhibitory action according to the present invention may use skin or skin cells (e.g., skin fibroblasts) in vivo as the target of action, or in Skin cells (e.g., skin fibroblasts) may be used as targets in vitro or ex vivo, or cells other than skin cells (e.g., skin fibroblasts) (e.g., tissues or organs other than skin (such as lungs) fibers Blast cells) or non-cellular substances such as enzymes and radicals may be used as the target.

The cosmetic according to the present invention may be used orally or parenterally, and is particularly advantageous as an external preparation.

The Kusasotetsu nanobubble liquid extract, composition or cosmetic according to the present invention can be used by blending with the following cosmetics. That is, the present invention relates to a cosmetic containing the Kusasotetsu nanobubble liquid extract according to the present invention. Such a cosmetic according to the present invention can exert its respective effects by applying it as an external preparation.

The cosmetic according to the present invention may be a composition in any form such as solution, suspension, emulsion, powder, paste, mousse and gel. The cosmetic according to the present invention may be any cosmetic that can be used in contact with the skin. cream, etc.), face wash (cleansing cream, etc.), mask, shaving cream, sun cream, sunscreen cream, sunscreen lotion, suntan lotion, toilet soap, foundation, face powder, powder, lipstick, lip balm, eyeliner, Examples include eye creams, eye shadows, mascara, bath cosmetics, shampoos, hair rinses, hair treatments, hair packs, scalp care agents, body rinses, body gels, antiperspirant deodorants, hair dyes, and hair cosmetics. The compounding amount of the sagebrush nanobubble liquid extract or the composition containing the sagebrush nanobubble liquid extract, for example, the sagebrush carbon dioxide nanobubble water extract or the composition containing the sagebrush carbon dioxide nanobubble water extract is based on the total weight of the cosmetic composition. 0.0001% to 100%, preferably 0.001% to 30%. The Kusa sotetsu nanobubble liquid extract can be blended into the cosmetic according to the present invention in any form, for example, liquid, gel, powder, granules, capsules, etc. It can be blended.

The cosmetic according to the present invention can be blended with any other ingredients that can be blended in the cosmetic, in addition to the Kusasotetsu nanobubble liquid extract. Other ingredients include additives, excipients, and other active ingredients used in cosmetics (e.g., other anti-skin aging agents, moisturizers, whitening agents, sunscreens, astringents, etc.). However, it is not limited to these, and can be arbitrarily selected and used according to the application and form of the cosmetic. The cosmetic according to the present invention can be produced by conventional methods by mixing and stirring raw materials.

For example, any one of the components listed below can be blended into the cosmetic composition according to the present invention together with the Kusasotetsu nanobubble liquid extract. There are no particular limitations on the ingredients that can be used in combination with cosmetics containing the extract of the present invention, provided that they are bases and drugs that are commonly used in cosmetics, quasi-drugs, and bath agents.

For example, the following ingredients are exemplified:
Proteins such as collagen, collagen hydrolysates, gelatin, gelatin hydrolysates, elastin, elastin hydrolysates, lactoferrin, keratin, keratin hydrolysates, casein, albumin, royal jelly-derived protein hydrolysates, honey-derived protein hydrolysates, etc. and protein hydrolysates;

Hyaluronic acid Na and hyaluronic acid derivatives, xanthan gum, carrageenan, guar gum, alginic acid and its salts, pectin, chondroitin sulfate and its salts, water-soluble chitin, chitosan derivatives and its salts, pullulan, deoxyribonucleic acid, gum arabic, natural high-grade tragacanth, etc. molecules and their derivatives;

Aloe, apple, mandarin orange, peach, mandarin orange, melon, strawberry, Shikuarta, figs and other fruit-derived products; peanut, chestnut, longan, millet, barley, rice, Japanese pine, soybean-derived products, Japanese pear, ginkgo biloba, etc. Leaf-derived substances, rhizome-derived substances such as wasabi, plant-derived substances such as tree-derived substances such as cherry blossoms and rowan;

Humic acid and fulvic acid in humic substances, which are final products formed by decomposition of plants and the like by microorganisms;
Crude drugs such as Physalis albicans, Rakanka, Jujube, Dove, Licorice, Eucommia, Ginger, Udo;
Microbial products such as yeast extract;
Fungal-derived products such as fungal bodies, sclerotia, and mushrooms;
Seaweed-derived polysaccharides such as seaweed powder and seaweed extract;
animal-derived products such as placenta extract;
Water such as carbonated water, hot spring water, purified water, distilled water;

Proteins such as collagen, natural polymers such as pullulan, plant-derived substances such as fruits, seeds, leaves, stems and roots, tree-derived substances, corrosive substance-derived substances, crude drug-derived substances, fungal-derived substances such as mushrooms, placenta etc. Fermented products such as animal-derived products;
among acidic polymers such as carboxyvinyl polymer and its salts, polyacrylic acid and its salts, carboxymethylcellulose and its salts, polyvinyl alcohol, hydroxyethyl cellulose, hydroxypropyl cellulose, methyl cellulose, polyethylene glycol, polyvinyl pyrrolidone, nitrocellulose polyvinyl methyl ether, etc. sexual polymer;

Cationic polymers such as cationic cellulose, polyethylenimine, cationic guar gum;
lower alcohols such as ethanol and isopropyl alcohol;
UV absorbers such as para-aminobenzoic acid UV absorbers, salicylic acid UV absorbers, cinnamic acid UV absorbers, anthraniate UV absorbers, and benzophenone UV absorbers;

Vitamin A, vitamin B group, vitamin C, L-ascorbyl magnesium phosphate and its derivatives, vitamin D group, d-α-tocopherol acetate, vitamin E group, folic acids, β-carotene, γ-oryzanol, nicotinic acid, vitamins such as pantothenic acids, biotins and ferulic acid;

anti-inflammatory agents such as glycyrrhizic acid and its salts, guaiazulene and its derivatives, allantoin;
antioxidants such as stearates, nordihydroguaceretenoic acid, dibutylhydroxytoluene, butylhydroxyanisole, parahydroxyanisole, propylgallate, sesamemol, sesamolin, gossypol;
parabenzoic acid esters such as methyl parabenzoate, ethyl parabenzoate, propyl parabenzoate and butyl parabenzoate; preservatives such as sorbic acid, dehydroacetic acid, phenoxyethanol and benzoic acid;

sequestering agents such as edetic acid, edetic acid and its salts such as disodium edetate, phytic acid, hydroxyethanedisulfonic acid;
Polyhydric alcohols such as glycerin, 1,3-butylene glycol, propylene glycol;
Amino acids such as L-aspartic acid, DL-alanine, L-arginine, L-cysteine, L-glutamic acid, glycine and salts thereof;
Sugars such as maltitol, sorbitol, xylobiose, N-acetyl-D-glucosamine, honey;
Organic acids such as citric acid, lactic acid, α-hydroxyacetic acid, pyrrolidonecarboxylic acid and salts thereof;

Bases such as ammonia water, monoethanolamine, triethanolamine, sodium hydroxide, potassium hydroxide;
Hydrocarbons such as liquid paraffin, squalane, petrolatum;
Fats and oils such as olive oil, coconut oil, evening primrose oil, jojoba oil, castor oil, hydrogenated castor oil;
Fatty acids such as lauric acid, myristic acid, palmitic acid, stearic acid and behenic acid;
Higher alcohols such as myristyl alcohol, cetanol, cetostearyl alcohol, stearyl alcohol and behenyl alcohol;
esters such as isopropyl myristate, isopropyl palmitate, cetyl octanoate, glyceryl trioctanoate, octyldodecyl myristate, octyl stearate, stearyl stearate;

Phospholipids such as lecithin and its derivatives;
Animal and plant-derived lipids such as bovine bone marrow lipid and bovine brain lipid;
Alkyl sulfates such as ammonium lauryl sulfate, ethanolamine lauryl sulfate, sodium lauryl sulfate, triethanolamine lauryl sulfate;
Polyoxyethylene (2EO) lauryl ether sulfate triethanolamine (EO is ethylene oxide and the number before EO indicates the number of moles of ethylene oxide added;), polyoxyethylene (3EO) alkyl (C11-15 or a mixture of two or more) polyoxyethylene alkyl sulfates such as sodium ether sulfate;

Alkyl benzene sulfonates such as sodium lauryl benzene sulfonate, triethanolamine lauryl benzene sulfonate;
Polyoxyethylene alkyl ether sulfates such as polyoxyethylene (3EO) tridecyl ether sodium acetate;

sodium cocoate sarcosine, lauroyl sarcosine triethanolamine, sodium lauroylmethyl-L-glutamate, sodium cocoate L-glutamate, triethanolamine cocoate L-glutamate, sodium cocoate methyltaurate, lauroylmethyltaurate N-acyl amino acid salts such as sodium, sodium ether sulfate, sodium hydrogenated coconut oil fatty acid glycerol sulfate, sodium hydrogenated coconut oil fatty acid glycerol sulfate, disodium undecinoylamidoethylsulfosuccinate, sodium octylphenoxydientoxyethylsulfonate , disodium aminosulfosuccinate oleate, dioctyl sodium sulfosuccinate, dioctyl sodium sulfosuccinate, disodium lauryl sulfosuccinate, polyoxyethylene alkyl (carbon chain 12-15) ether phosphate (8EO-10EO), polyoxyethylene oleyl ether anionic surfactants such as sodium phosphate, sodium polyoxyethylene cetyl ether phosphate, disodium lauryl polyoxyethylene sulfosuccinate, sodium polyoxyethylene lauryl ether phosphate, sodium lauryl sulfoacetate, sodium tetradecene sulfonate;

Stearyldimethylammonium chloride, di(polyoxyethylene)oleylmethylammonium chloride, stearyldimethylbenzylammonium chloride, stearyltrimethylammonium chloride, tri(polyoxyethylene)stearylammonium chloride, polyoxypropylenemethyldiethylammonium chloride, myristyldimethylbenzylammonium chloride , cationic surfactants such as lauryltrimethylammonium chloride;

2-alkyl-N-carboxymethyl-N-hydroxyethylimidazolinium betaine, undecylhydroxyethylimidazolinium betaine sodium, undecyl-N-hydroxyethyl-N-carboxymethylimidazolinium betaine, stearyldihydroxyethylbetaine, coconut Oil fatty acid amidopropyl betaine, coconut oil alkyl-N-carboxyethyl-N-hydroxyethylimidazolinium betaine sodium, coconut oil alkyl-N-carboxymethoxyethyl-N-carboxymethylimidazolinium disodium lauryl sulfate, N-coconut Amphoteric surfactants such as fatty acid acyl-L-arginine ethyl-DL-pyrrolidone carboxylate;

Polyoxyethylene alkyl (C12-C14) ether (7EO), polyoxyethylene octylphenyl ether, polyoxyethylene oleyl ether, polyoxyethylene glycerin oleate, polyoxyethylene stearyl ether, polyoxyethylene cetyl ether, polyoxy Ethylene cetyl stearyl diether, polyoxyethylene sorbitol lanolin (40EO), polyoxyethylene nonylphenyl ether, polyoxyethylene polyoxypropylene cetyl ether, polyoxyethylene polyoxypropylene decyltetradecyl ether, polyoxyethylene lanolin, polyoxy nonionic surfactants such as ethylene lanolin alcohol, polyoxypropylene stearyl ether;

isostearic acid diethanolamide, undecylenic acid monoethanolamide, oleic acid diethanolamide, beef tallow fatty acid monoethanolamide, hydrogenated tallow fatty acid diethanolamide, stearic acid diethanolamide, stearic acid diethylaminoethylamide, stearic acid monoethanolamide, myristic acid diethanolamide, Thickeners such as coconut fatty acid diethanolamide, coconut fatty acid ethanolamide, lauric isopropanolamide, lauric ethanolamide, lauric diethanolamide, lanolin fatty acid diethanolamide;

Silicone oils such as linear or cyclic methylpolysiloxane, methylphenylpolysiloxane, dimethylpolysiloxane polyethylene glycol copolymer, dimethylpolysiloxane polypropylene copolymer, amino-modified silicone oil, quaternary ammonium-modified silicone oil;
thioglycolic acid and its salts;
cysteamine and its salts;
Peroxides such as hydrogen peroxide, persulfates, perborates, urea peroxide;
Bromates such as sodium bromate, potassium bromate; and

In addition, pH adjusters, coloring agents, fragrances, stabilizers, cooling agents, blood flow promoters, keratolytic agents, astringents, wound treatment agents, foaming agents, oral agents, deodorants, deodorants, antiallergic agents agent, cell activator, inert carrier (solid or liquid carrier), excipient, surfactant, binder, disintegrant, lubricant, solubilizer, suspending agent, coating agent, preservative, buffer drug etc.
At least these components can be blended together with the cosmetic of the present invention and used in combination.

The Kusasotetsu nanobubble liquid extract, composition, or cosmetic according to the present invention can be administered (applied) to any mammal (subject) including humans, livestock, pet animals, experimental (test) animals, and the like. However, subjects with curly hair and skin aging, subjects at high risk of accelerated skin aging such as those who are highly exposed to ultraviolet rays, subjects with accelerated skin aging, and the need to prevent or improve skin aging particularly useful for administration to subjects such as those with high The present invention provides a method for preventing skin aging through hair straightening action and antioxidant function by administering (preferably applied as an external preparation) the Kusasotetsu nanobubble liquid extract, composition or cosmetic according to the present invention to a subject. Also related. The present invention also provides a hair straightening action, an antioxidant action, a super It also relates to a method for enhancing oxide scavenging action or active oxygen production inhibitory action.

EXAMPLES The present invention will be described in more detail below using examples. However, the technical scope of the present invention is not limited to these examples.

<Preparation of nanobubble water using carbon dioxide>
While demineralized water with a flow rate of 5 L/min and a water temperature of 38 ° C. is passed through a water nanocyclone type multifunctional mixing device (manufactured by CO2 Systems Co., Ltd.), carbon dioxide is injected at a supply pressure of 0.3 Mpa to form carbon dioxide nano bubbles. 10 L of water was prepared.

<Preparation of carbon dioxide nanobubble water extract of each plant>
10 g of each of the pulverized dried matter of Kogomi, which is the young buds of sage, the pulverized matter of dried butterbur sprout, the pulverized matter of dried sprouts of cod, and the pulverized matter of dried fern are immersed in 190 g of carbon dioxide nanobubble water prepared as described above. Then, extraction was carried out at room temperature for 24 hours. The solution after extraction was centrifuged at 10,000 g for 10 minutes, and the precipitate in the solution was removed by filtration to obtain a clear carbon dioxide nanobubble water extract of each plant. After that, the solid content concentration was calculated and diluted with carbon dioxide nanobubble water so as to be 1%. The carbon dioxide nanobubble water extracts of each plant are summarized below.
Example 1: Carbon dioxide nano-bubble water extract of Kusa sotetsu Comparative example 1: Fukinotou carbon dioxide nano-bubble water extract Comparative example 2: Cod sprout carbon dioxide nano-bubble water extract Comparative example 3: Mainspring carbon dioxide nano-bubble water extract

<Preparation of water extract of each plant>
10 g of each of the pulverized dried matter of Kogomi, which is the young bud of the sage, the pulverized matter of the dried butterbur sprout, the pulverized matter of the dried cod sprouts, and the pulverized matter of the dried fern buds were immersed in 190 g of desalted water for 24 hours at room temperature. I did the extraction. The extracted solution was centrifuged at 10,000 g for 10 minutes, and the precipitate in the solution was removed by filtration to obtain a clear water extract of each plant. After that, the solid content concentration was calculated and diluted with desalted water so as to be 1%. Aqueous extracts of each plant are summarized below.
Comparative Example 4: Kusa cycad water extract Comparative Example 5: Butterbur sprout water extract Comparative Example 6: Cod sprout water extract Comparative Example 7: Osmia fern water extract

<Curly hair straightening action>
The hair straightening effect of the carbon dioxide nanobubble water extract of Pleurotus japonicum of Example 1 was evaluated. An Indian hair tress, which is a curly hair model, was washed with desalted water to remove stains, and then naturally dried overnight. This time point was set as before the test, and the state of the hair bundle was photographed. After that, the hair tresses were immersed for 3 minutes in the Kusa cycad carbon dioxide nanobubble water extract of Example 1 or tap water. The hair was lightly towel-dried, straightened, and dried with a drier. After that, it was left for 1 hour. At this time point, the state of the hair bundle was photographed after the test and compared with that before the test.

Fig. 1 a) shows the state of the hair bundle before the test for use in evaluating the hair straightening action of the Kusasotetsu carbon dioxide nanobubble water extract, and b) is used to evaluate the hair straightening action of tap water. 1 shows the state of the hair tress before the test for In FIG. 2, a) shows the state of the hair tress after the test with the carbon dioxide nanobubble water extract of Kusasotetsu, and b) shows the state of the hair tress after the test with tap water. Compared to the hair tress treated with tap water, the hair tress treated with the water extract of Pleurotus thunbergii carbon dioxide nanobubbles of Example 1 clearly reduced waviness. From this, it was shown that the carbon dioxide nanobubble water extract of Kusa cycad has a curly hair straightening action.

<Antioxidant action>
The antioxidant effect of the carbon dioxide nanobubble water extract of each plant and the water extract of each plant was evaluated by the DPPH radical scavenging method. The DPPH radical scavenging method includes DPPH (1,1-diphenyl-2-picryl-hydrazyl), which is a stable radical that absorbs in the visible region and no longer absorbs when it is reduced, and an antioxidant (that is, 1 and Comparative Examples 1 to 7), the amount of DPPH that was not reduced by the antioxidant was determined by absorbance measurement to evaluate the antioxidant capacity of the antioxidant. The test solutions were carbon dioxide nanobubble water extracts of the plants of Example 1 and Comparative Examples 1-3 and water extracts of the plants of Comparative Examples 4-7. The extracts of Example 1 and Comparative Examples 1-3 were diluted with carbon dioxide nanobubble water, and the extracts of Comparative Examples 4-7 were diluted with demineralized water to 1000 ppm (final concentration 250 ppm) and 2000 ppm (final concentration 500 ppm). bottom. Dispense 900 μL of the reaction indicator (800 μM 1,1-diphenyl-2-picryl-hydrazyl 12 mL, 400 mM 2-morpholinoethanesulfonic acid buffer 12 mL, 50% ethanol aqueous solution 24 mL) into a test tube, and add 300 μL of the test solution. , and the absorbance at 520 nm was measured 20 minutes after the addition of the test solution. As a control, carbon dioxide nanobubble water or demineralized water corresponding to the extraction solvent of each test liquid was added instead of each test liquid, and similar reactions and measurements were performed. The radical scavenging rate of each test solution was compared with the measured value of the control and calculated as follows.

Radical scavenging rate (%) = (absorbance of control - absorbance upon addition of test solution) / absorbance of control x 100
^* Control is carbon dioxide nanobubble water or desalted water

The results are shown in FIG. As shown in FIG. 3, the extract of Kusa cycad was found to have an antioxidant effect. Its radical scavenging level was much higher than other plants. Furthermore, the carbon dioxide nanobubble water extract showed higher results than the water extract, and the action increased in a concentration-dependent manner. From this, it was shown that Kusa cycad has an antioxidant effect, and it was shown that extraction with carbon dioxide nanobubble water has a higher antioxidant effect.

<Superoxide scavenging action>
The carbon dioxide nanobubble water extract of each plant and the superoxide scavenging effect of the water extract of each plant were evaluated. The test solutions were carbon dioxide nanobubble water extracts of the plants of Example 1 and Comparative Examples 1-3 and water extracts of the plants of Comparative Examples 4-7. The extracts of Example 1 and Comparative Examples 1 to 3 were diluted with carbon dioxide nanobubble water, and the extracts of Comparative Examples 4 to 7 were diluted to 1000 ppm with desalted water. After that, each extract was serially diluted to prepare test solutions of 125 ppm, 250 ppm and 500 ppm. Nitroblue tetrazolium (NBT) (+) reagent [2.5 mM NBT aqueous solution, 10 mM EDTA-2Na aqueous solution, 5 mM Hypoxanthine aqueous solution, PBS (-) containing], NBT (-) reagent [distilled water, 10 mM EDTA-2Na aqueous solution, 5 mM Hypoxanthine Aqueous solution containing PBS (-)], Xanthine oxidase solution was prepared with 1 mg/mL BSA, and 25 μL of the test solution and 25 μL each of the NBT (+) reagent or NBT (-) reagent was added to each well using a 96-well plate. Mixed. 25 μL of Xanthine oxidase solution was added thereto and mixed, and after standing in an incubator at 37° C. for 30 minutes, absorbance at 560 nm was measured using a microplate reader. As a control, carbon dioxide nanobubble water or demineralized water corresponding to the extraction solvent of each test liquid was added instead of each test liquid, and similar reactions and measurements were performed. The superoxide scavenging rate of each test solution was compared with the measured value of the control corresponding to the extraction solvent of each extract and calculated as follows.

The results are shown in FIG. As shown in FIG. 4, a high superoxide scavenging effect was observed in the extract of Kusa cycad. Its activity was much higher than that of other plants. Furthermore, the carbon dioxide nanobubble water extract showed higher results than the water extract, and the action increased in a concentration-dependent manner. From this, it was shown that Kusa cycad has a superoxide scavenging effect, and it was shown that extraction with carbon dioxide nanobubble water has a higher superoxide scavenging effect.

<Reactive oxygen production inhibitory action>
The carbon dioxide nanobubble water extract from each plant and the water extract from each plant were evaluated for the active oxygen production inhibitory action. Normal human neonatal skin-derived fibroblasts suspended in DMEM medium containing 5% FBS (fetal bovine serum) were cultured in a 96-well cell culture plate (37° C., CO ₂ incubator) until they became semi-confluent. The medium was removed and the cells washed once with phosphate buffer (-) were added with the carbon dioxide nanobubble water extract of each plant of Example 1 or Comparative Examples 1-3, or each plant of Comparative Examples 4-7. A DMEM medium (0.5% FBS) adjusted to 500 ppm of an aqueous extract of S. was added as a test solution and cultured overnight. After culturing, the medium was removed and the cells were washed twice with Hanks buffer (+). 100 μL of 2′,7′-Dichlorofluorescin diacetate (H2DCFDA) diluted to 20 μM with Hanks buffer solution (+) was added and cultured for 30 minutes. After culturing, the medium was removed and the cells were washed twice with Hanks buffer (+). After that, in order to artificially produce active oxygen in the cells, 500 μMH prepared with Hanks buffer solution (+) to create an H ₂ O ₂ treated group with the addition of hydrogen peroxide (H ₂ O ₂ ). ₂ O ₂ was added at 100 μL/ and incubated for 15 minutes. After washing twice with Hanks buffer (+), 100 µL of Hanks buffer (+) was added, and fluorescence intensity (Ex485 nm, Em535 nm) in the wells was measured using a microplate reader. After the measurement, a phosphate buffer (-) containing 0.5% Triton X-100 was added and homogenized to disrupt the cells to obtain a cell lysate. The amount of protein per well was measured using this cell lysate with a DC Protein Assay Kit (BIO-RAD). As a control, a DMEM medium (FBS 0.5%) supplemented with carbon dioxide nanobubble water or demineralized water corresponding to the extraction solvent of each test solution was added, and the same operation was performed. The active oxygen production inhibitory action of each test solution was shown by calculating the amount of active oxygen production as follows.

Reactive oxygen production = fluorescence intensity/protein amount per well

FIG. 5 shows the results of the carbon dioxide nanobubble water extracts of Example 1 and Comparative Examples 1-3, and FIG. 6 shows the results of the water extracts of Comparative Examples 4-7. As shown in FIGS. 5 and 6, the extract of Kusa cycad was found to have a high active oxygen scavenging effect. Its activity was much higher than that of other plants. Furthermore, the carbon dioxide nanobubble water extract showed higher results than the water extract. From this, it was shown that Kusa cycad has an active oxygen scavenging effect, and it was shown that extraction with carbon dioxide nanobubble water has a higher active oxygen scavenging effect.

<Production of Shampoo>

According to the recipes in Table 1, ingredients (1) to (8) were mixed and stirred at 70° C. and cooled to room temperature to prepare shampoos of Example 2 and Comparative Example 8.

When the hair was washed with the obtained shampoo of Example 2, the hair felt smooth and could be moisturized.

The resulting shampoo of Example 2 did not cause creaking and was easy to comb.

In addition, using the obtained shampoos of Example 2 and Comparative Example 8 for 2 weeks, 15 professional panelists were subjected to a usage test. After use, the hair creakiness and combability were evaluated according to the following 5-grade rating scale.

1. 2. There is considerable squeaking and combing is also quite poor. 3. Slightly creaky and slightly difficult to comb. 4. No change. 5. Slightly smooth and easy to comb. Smooth and supple, and easy to comb.

Table 2 shows the average scores of the 15 panelists. As shown in Table 2, Example 2, in which the Kusa cysticum carbon dioxide nanobubble water extract of Example 1 was added, was smoother to the hair than Comparative Example 8, in which the Kusa cythus carbon dioxide nanobubble water extract was not added. It showed an excellent effect of improving combability.

In addition, 15 professional panelists were subjected to a 2-week use test with respect to irritation to the scalp using the obtained shampoos of Example 2 and Comparative Example 8. After use, the irritation to the scalp was evaluated according to the following 4-grade rating scale.

1. feel strongly stimulated
2. 3. Feel stimulating. 4. I feel a little stimulation. no stimulation

Table 3 shows the average scores of the 15 panelists. As shown in Table 3, Example 2, in which the water extract of Kusa cycad carbon dioxide nanobubbles of Example 1 was added, was less irritating to the scalp, and was shown to be very safe and less burdensome on the scalp.

<Production of hair pack>

According to the recipe shown in Table 4, (1) to (2) were mixed and stirred at 80 ° C., and (3) to (13) were separately mixed and stirred at 80 ° C., and mixed and stirred at 80 ° C. (15) and (14) were further added and mixed with stirring to obtain a hair pack agent of Example 3.

When the hair was treated with the obtained hair pack agent of Example 3, the hair felt smooth and moisturized.

<Manufacturing lotion>

According to the formulation in Table 5, the ingredients (1) to (10) were stirred at 80 ° C., cooled to room temperature after dissolution, and the lotion of Example 4 blended with the extract of carbon dioxide nanobubble water of Example 1, The lotion of Comparative Example 9, which did not contain the carbon dioxide nanobubble water extract of Kusa cycad, was obtained. All of the obtained lotions were clear and stable for 3 months without cloudiness under the conditions of 40°C and 75% relative humidity (RH).

The obtained lotion of Example 4 was non-sticky during use and moistened the skin.

In addition, a one-month usage test was conducted on the obtained lotions of Example 4 and Comparative Example 9 with 10 expert panelists as targets. After use, the effect of improving skin tension and elasticity was evaluated according to the following 5-grade rating scale.

1. 2. Worsened. 3. Slightly worsened. 4. No change. Slightly improved 5. improved

Table 6 shows the average scores of 10 panelists. As shown in Table 6, Example 4, in which the Kusa cycad carbon dioxide nanobubble water extract of Example 1 was added, exhibited superior skin tension than Comparative Example 9, in which the Kusa cycad carbon dioxide nanobubble water extract was not added. It showed an effect of improving the feeling and elasticity.

<Production of Cream>

According to the recipe shown in Table 7, (1) to (6) were mixed and stirred at 80 ° C., and (7) to (10) were separately mixed and stirred at 80 ° C., homogenized, and stirred at room temperature. to obtain creams of Example 5 and Comparative Example 10.

The obtained cream of Example 5 was non-sticky during use and moistened the skin.

In addition, a one-month usage test was conducted on the obtained creams of Example 5 and Comparative Example 10 with 10 expert panelists as targets. After use, the wrinkles and sagging improvement action was evaluated according to the following 5-grade rating evaluation.

1. 2. Worsened. 3. Slightly worsened. 4. No change. Slightly improved 5. improved

Table 8 shows the average scores of 10 panelists. As shown in Table 8, Example 5 with the addition of the Pleurotus carbon dioxide nanobubble water extract of Example 1 has better wrinkles and sagging than Comparative Example 10 without the addition of Pleurotus carbon dioxide nanobubble water extract. showed an improvement effect.

<Production of body gel agent>

According to the formulation in Table 9, (1) to (8) were stirred and dissolved to obtain a body gel preparation of Example 6.

The obtained body gel preparation of Example 6 was non-sticky during use and moistened the skin.

<Production of body rinse agent>

According to the formulation shown in Table 10, the body rinse of Example 7 was obtained by a conventional method.

The obtained body rinse of Example 7 was moist to the skin.

Claims (13)

1. A method for preparing a sotet extract by contacting a nanobubble liquid containing nano-sized fine air bubbles with Matteuccia struthiopteris. 2. The method according to claim 1, wherein the nano-sized fine bubbles are carbon dioxide. 3. The method according to claim 1 or 2, wherein the nanobubble liquid is nanobubble water. An extract of Pleurotus thunbergii extracted from Pleurotus (Matteuccia struthiopteris) using a nanobubble liquid containing nano-sized microbubbles. 5. The Kusa cycad extract according to claim 4, wherein the nano-sized fine air bubbles are carbon dioxide. 6. The Kusa cycad extract according to claim 4 or 5, wherein the nanobubble liquid is nanobubble water. A composition comprising the Kusa cycad extract according to any one of claims 4-6. 8. The composition according to claim 7, further comprising a nanobubble liquid containing nano-sized fine bubbles. 9. The composition according to claim 8, wherein the nano-sized fine bubbles are carbon dioxide. The composition according to claim 8 or 9, wherein the nanobubble liquid is nanobubble water. The composition according to any one of claims 7 to 10, which is a composition for straightening curly hair having a curly hair straightening action. The composition according to any one of claims 7 to 11, which is an antioxidant composition having antioxidant function. A cosmetic comprising the Kusa cycad extract according to any one of claims 4 to 6 or the composition according to any one of claims 7 to 12.

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