JP6827691B2 - Cosmetics - Google Patents

Description

The present invention relates to a functional material obtained from a plant belonging to the genus Citrus of the Rutaceae family and having excellent physiological activity and biosafety, and a cosmetic and an oral composition containing the functional material.

The skin has internal factors such as inactivation of cell proliferation and differentiation with aging, decreased hormone secretion, and quantitative decrease of extracellular matrix components, as well as active oxygen induced by sunlight (ultraviolet rays) and air pollutants. And chemical substances such as environmental hormones, allergic substances such as pollen, and external factors such as environmental stress are intricately intertwined, causing aging, rough skin, and changes in color tone.

For example, various enzymes called matrix metaprotease exist in skin cells, and when activated, they decompose the basement membrane components (collagen, laminin, etc.) that make up the skin, elastin, which is a dermis matrix component, and so on. As a result, it causes wrinkles and tarmi on the skin.

In addition, ultraviolet rays, chemical substances, and allergens, which are external factors, damage cells, tissues, and cells of the skin to alter biological components or generate active oxygen, thereby causing antigens in the skin. This causes skin irritation. Furthermore, it induces abnormal deposition of melanin pigment and causes spots, freckles, chloasma and the like.

In order to prevent the above-mentioned aging and unhealthy skin and keep it in a youthful state, the use of various active ingredients has been proposed, and cosmetics and oral compositions containing these active ingredients have been put on the market. Has been done. For example, antioxidants such as vitamin C, vitamin E and catalase; anti-inflammatory agents such as glycyrrhizic acid or salts thereof, allantin; various ultraviolet absorbers; α-hydroxycarboxylic acid, placenta extract, γ-amino-β-hydroxy Cell-activating components such as butyric acid; extracellular matrix components such as collagen, elastin, hyaluronic acid or salts thereof; moisturizers such as urea; protein glycation inhibitors such as aminoguanidine. Further, kojic acid, linoleic acid and the like are known as substances that suppress the occurrence of pigmentation such as skin spots, freckles and chloasma, and are widely used as active ingredients of whitening agents.

As described above, anti-aging agents and whitening agents have been conventionally proposed based on various skin aging phenomena and unhealthy mechanisms, but they are safe for the skin and the like, and are actually applied to the skin or applied to the skin. There is a problem in terms of efficacy when taking. Therefore, there is a demand for a functional material having improved such points.

In view of the problems of the prior art, the present inventors have conducted diligent research to find a new functional material derived from a natural product from the viewpoint of biosafety. As a result, the extract of bergamot (Citrus aurantium L.subsp. Bergamia [Risso & Poit.] Wight & Arn. Hereinafter referred to as "Citrus bergamia") belonging to the genus Citrus of the Rutaceae family has an excellent collagen gel contraction promoting action, collagen. It has a synthesis-promoting activity, a decorin synthesis-promoting action, a melanosomes uptake inhibitory action, an antioxidant action, and a lipid accumulation inhibitory action, and due to these interactions, the skin (including the scalp) excellent by blending the extract. It has been found that it is possible to provide cosmetics and oral cosmetic compositions which have a healthening effect, an anti-aging effect, a whitening effect, a hair quality improving effect and a hair growing effect, and are also excellent in biosafety.

Conventionally, it is known from Patent Documents 1 to 4 that an extract of a plant belonging to the genus Citrus of the Rutaceae family is used as an external preparation for skin such as cosmetics, but bergamot juice or extract can be used as cosmetics. It was not known for use in cosmetic oral compositions.

Japanese Unexamined Patent Publication No. 07-126142 Japanese Patent Application Laid-Open No. 09-315993 Japanese Patent Application Laid-Open No. 2000-096050 JP-A-2002-068954

The present invention is a cosmetic containing a juice or extract of bergamot (Citrus bergamia) belonging to the genus Citrus of the Rutaceae family as an active ingredient.
The present invention is an oral composition containing a squeezed juice or an extract of bergamot (Citrus bergamia) belonging to the genus Citrus of the Rutaceae family as an active ingredient.
In this specification, the term cosmetics is used in a broad sense to include not only so-called cosmetics but also quasi-drugs.

The present invention is a cosmetic or oral composition containing an extract of freckles belonging to the genus Melasma of the family Chloasma as an active ingredient, and the collagen gel contraction action, collagen synthesis promoting action, decorin synthesis promoting action, which the extract exerts. Remarkably excellent rough skin (inflammation, dry skin, acne, etc.); prevention / improvement of aging phenomenon (wrinkles, age spots, reduction of firmness and texture, etc.) due to melanosomes uptake inhibitory action, antioxidant action and lipid accumulation inhibitory action Effect; Preventing / improving dullness, darkening, opening, clogging, tarmi, etc. of pores; and providing cosmetics and oral cosmetic compositions having an effect of preventing / improving pigmentation such as skin stains, freckles, and chloasma. be able to. Further, it is possible to provide a cosmetic or an oral composition having the effect of protecting the hair and sounding the scalp based on the above action.

Hereinafter, preferred embodiments of the present invention will be described in detail.
The cosmetic or oral composition of the present invention contains an extract "juice (fruit juice) or extract" of bergamot (Citrus bergamia) belonging to the genus Citrus of the Rutaceae family as an active ingredient. The bergamot juice can be prepared by squeezing the fruit as it is, or by crushing the fruit and then squeezing the crushed product. To prepare the bergamot extract, the whole plant or fruit is previously washed with water, dried, etc., if necessary, and then brought into contact with the extraction solvent by an appropriate means such as a dipping method or a countercurrent extraction method. Can be done by Further, a supercritical extraction method or a steam distillation method may be used. In preparing the fruit extract, those containing pericarp and / or seeds may be used. In addition, a mixture of any two or more of bergamot juice, extract, and steam distillation or essential oil may be used.

As the extraction solvent, water; lower alcohols such as methanol, ethanol and propanol; polyhydric alcohols such as ethylene glycol, propylene glycol, 1,3-butylene glycol and glycerin; ethyl acetate, butyl acetate, methyl propionate and the like. Esters; ketones such as acetone and methyl ethyl ketone; ethers such as ethyl ether and isopropyl ether; hydrocarbon solvents such as n-hexane, toluene and chloroform, etc., which may be used alone or in admixture of two or more. Is used.

Among these extraction solvents, water and lower grades are used in the present invention from the viewpoint of the effectiveness of the obtained extract, skin irritation, and the fact that it can be widely applied to cosmetics and the like. Hydrophilic solvents such as alcohols or polyhydric alcohols are suitable. Preferred examples of using this hydrophilic solvent include, for example, water, lower alcohols (eg, ethanol), or polyhydric alcohols (eg, 1,3-butylene glycol, propanediol, glycerin) alone, or , The use of a mixed solvent of water and lower alcohols (particularly ethanol), or a mixed solvent of water and polyhydric alcohols (for example, 1,3-butylene glycol, glycerin), etc., among which water alone is used. , Or a mixed solvent of water and 1,3-butylene glycol or propanediol is particularly preferable.

When a mixed solvent is used, for example, in the case of a mixed solvent of water and 1,3-butylene glycol or propanediol, the volume ratio (hereinafter the same applies) is 1: 1 to 20: 1, and water and ethanol are mixed. The range is preferably 1: 1 to 25: 1 for a mixed solvent and 1: 1 to 20: 1 for a mixed solvent of water and glycerin.

The weight ratio of the dried portion of bergamot to the extraction solvent is preferably in the range of 1: 1 to 1:80, more preferably in the range of 1: 5 to 1:50.

When preparing the extract, the pH is not particularly limited, but is generally preferably in the range of 3 to 9. In this sense, if necessary, an alkali adjusting agent such as sodium hydroxide, sodium carbonate, potassium hydroxide or the like, or an acid adjusting agent such as citric acid, hydrochloric acid, phosphoric acid, sulfuric acid, etc. is added to the extraction solvent, which is desired. The pH may be adjusted to the above.

Extraction conditions such as extraction temperature and extraction time differ depending on the type and pH of the solvent used, but for example, when water or 1,3-butylene glycol or a mixed solution of water and 1,3-butylene glycol is used as the solvent. If so, the extraction temperature is generally in the range of 4 ° C. to 85 ° C., and the extraction time is generally in the range of 0.5 hours to 3 days.

The bergamot fruit juice or extract is treated with activated carbon, non-ion exchange resin, etc. for the purpose of improving stability and removing impurities that are not desirable as components of cosmetics and oral compositions. You may perform the adsorption treatment with the synthetic adsorbent of. Further, for the purpose of concentrating the components contained in the squeezed liquid or extract of bergamot fruit, activated carbon treatment or concentration treatment with a synthetic adsorbent such as a non-ion exchange resin may be performed.

Activated carbon includes trees such as pine, bamboo, coconut husks, peach husks, and other vegetable substances, as well as coal and petroleum husks, and high-temperature carbonization that uses gas such as water vapor, carbon dioxide, and air as the raw materials. Either a physical method such as a method or activated carbon obtained by treating with a chemical such as zinc chloride and then heating to make it porous by a chemical method may be used.

The nonionic porous resin adsorbent is composed of a nonionic resin such as a styrene / divinylbenzene copolymer and a methacrylic acid ester polymer, and has a specific surface area generally in the range of 100 to 2000 m ² / g for synthetic adsorption. Agents (aromatic unsubstituted type, etc.) can be mentioned. For example, styrene / divinylbenzene-based Diaion HP10, 20, 21, Sepabeads SP800, SP850, SP700, SP207 (above, Mitsubishi Chemical Corporation), Amberlite XAD4, 16, Duolite S874, 877. (Rohm and Haas), methacrylic acid ester-based benzene HP1MG, 2MG (Mitsubishi Chemical Co., Ltd.), Amberlite XAD7 (Rohm and Haas) and the like. The synthetic adsorbent that can be used in the present invention is not limited to this, and can be appropriately selected according to the purpose of removing impurities and concentrating.

Further, the extraction site may be subjected to a hydrolysis treatment, if necessary, prior to the extraction treatment of the present invention or in parallel with the extraction treatment. Thereby, there is a possibility that the storage stability of the extract can be improved.

When the extract is subjected to enzyme hydrolysis treatment, the enzymes include proteolytic enzymes such as actinase, papaine and pepsin, starch degrading enzymes such as glucoamylase, α-amylase and β-amylase, and cellulase, hemicellase and pectinase. One or more selected from any of the enzyme groups of fibrinolytic enzyme and lipolytic enzyme such as lipase may be used, but one or more selected from those enzyme groups, respectively. It is more preferable to use the above enzymes in combination.

The amount of the enzyme added is preferably in the range of 0.001 to 50% by weight in total with respect to the solid content of the site where the bergamot is used.

The extract prepared as described above may generally have a pH adjusted to 3 to 9 and then used as it is, or may be used as a desired concentration by concentration under reduced pressure or the like. Further, the extract may be a dried product by a conventional method such as a spray-drying method.

In addition, the extract prepared as described above may be refrigerated for a certain period of time and then the supernatant may be used in order to improve storage stability and the like.

Cosmetics (including non-medicinal products) containing the extract according to the present invention include, for example, milky lotion, cream, lotion, essence, pack, lipstick, foundation, liquid foundation, make-up press powder, blusher, white powder, etc. Examples thereof include facial cleansers, body shampoos, shampoos for hair, soaps, etc., and hair growth agents, bathing agents, etc., but of course, are not limited thereto. In addition, as oral cosmetic compositions, beverages such as beauty beverages, energy drinks, sports drinks, near water, vitamin beverages, mineral beverages, alcoholic beverages; various soups (including powdered soups), dairy products, jellies, candy , Tablets, gums and other foods; can be blended in tablets, liquid, granular or jelly-like health foods / beverages, etc., but the present invention is not limited to this, and can be blended in foods and drinks that can be taken orally. can do.

The blending amount of the extract of the present invention in cosmetics is generally 0.002 to 1.0% by weight (solid content weight%, the same applies hereinafter), preferably 0, as the solid content of the extract in the case of basic cosmetics. In the range of .02 to 0.2% by weight, in the case of make-up cosmetics, generally in the range of 0.002 to 1.0% by weight, preferably in the range of 0.02 to 0.2% by weight, and for cleaning cosmetics. In the case, it is generally in the range of 0.002 to 10.0% by weight, preferably 0.02 to 7.0% by weight. In the case of hair cosmetics, the solid content of the extract is generally 0.0001 to 5.0% by weight, preferably 0.001 to 3.0% by weight. The blending amount of the extract of the present invention in the cosmetological oral composition is preferably in the range of 0.1 to 15% by weight as the solid content of the extract.

In cosmetics, in addition to extracts, which are essential ingredients, ingredients usually used in cosmetics and oral compositions, such as oily ingredients, surfactants (synthetic and natural products), moisturizers, thickeners, etc. Preservatives / bactericides, powder components, ultraviolet absorbers, antioxidants, pigments, fragrances and the like can be appropriately blended as needed. Further, as long as the effectiveness and characteristics of the extract are not impaired, other physiologically active ingredients may be combined and blended at all.

Here, examples of the oily component include bergamot oil, olive oil, jojoba oil, paraffin oil, soybean oil, rice oil, rice bran oil, rice germ oil, palm oil, chamomile oil, palm oil, cacao oil, meadowfoam oil, and rose. Plant-derived fats and oils such as hip oil, lanbender oil, sheer butter, tea tree oil, avocado oil, macadamia nut oil, and plant-derived squalane; animal-derived fats and oils such as mink oil and turtle oil; honey wax, carnauba wax, rice wax , Lanorin and other waxes; liquid paraffin, vaseline, paraffin wax, squalane and other hydrocarbons; myristic acid, palmitic acid, stearic acid, oleic acid, isostearic acid, eicosenoic acid and other fatty acids; lauryl alcohol, cetanol, stearyl Higher alcohols such as alcohols; synthetic esters such as isopropyl myristate, isopropyl palmitate, butyl oleate, 2-ethylhexyl glyceride, higher fatty acid octyldodecyl (octyldodecyl stearate, etc.) and synthetic triglycerides can be mentioned.

Examples of the surfactant include polyoxyethylene alkyl ether, polyoxyethylene fatty acid ester, polyoxyethylene sorbitan fatty acid ester, glycerin fatty acid ester, polyglycerin fatty acid ester, polyoxyethylene glycerin fatty acid ester, polyoxyethylene hydrogenated castor oil, and poly. Nonionic surfactants such as oxyethylene sorbitol fatty acid ester; fatty acid salt, alkyl sulfate, alkylbenzene sulfonate, polyoxyethylene alkyl ether sulfate, polyoxyethylene fatty amine sulfate, polyoxyethylene alkyl phenyl ether sulfate, Anionic surfactants such as polyoxyethylene alkyl ether phosphate, α-sulfonated fatty acid alkyl ester salt, polyoxyethylene alkyl phenyl ether phosphate; quaternary ammonium salt, primary to tertiary fatty amine salt, tri Cationic surfactants such as alkylbenzylammonium salt, alkylpyridinium salt, 2-alkyl-1-alkyl-1-hydroxyethylimidazolinium salt, N, N-dialkylmorphonium salt, polyethylene polyamine fatty acid amide salt; N, N-dimethyl-N-alkyl-N-carboxymethylammoniobetaine, N, N, N-trialkyl-N-alkylene ammoniocarboxybetaine, N-acylamide propyl-N', N'-dimethyl-N'- Amphoteric surfactants such as β-hydroxypropylammoniosulfobetaine can be used.

Examples of emulsifiers or emulsifying aids include stevia derivatives such as enzyme-treated stevia, saponin or derivatives thereof, casein or salts thereof (sodium, etc.), sugar-protein complexes, sucrose or esters thereof, lactic acid, and water-soluble soybeans. Polysaccharide, complex of soybean-derived protein and polysaccharide, lanolin or its derivative, cholesterol, stevia derivative (stevia enzyme treated product, etc.), silicate (aluminum, magnesium, etc.), carbonate (calcium, sodium, etc.), saponin and its Derivatives, lecithin and its derivatives (hydrogenated lecithin, etc.), lactic acid bacteria fermented rice, lactic acid bacteria fermented germinated rice, lactic acid bacteria fermented grains (wheat, beans, miscellaneous grains, etc.) and the like can also be blended.

Examples of the moisturizing agent include glycerin, propylene glycol, dipropylene glycol, 1,3-butylene glycol, polyethylene glycol, sorbitol, xylitol, sodium pyrrolidone carboxylate and the like, and saccharides such as trehalose and mucopolysaccharides (for example, hyalurone). Acids and their derivatives, chondroitin and its derivatives, heparin and its derivatives, etc.), elastin and its derivatives, collagen and its derivatives, NMF-related substances, lactic acid, urea, higher fatty acids octyldodecyl, seaweed extract, silane roots (white) Examples include extracts, various amino acids and derivatives thereof.

Examples of the thickener include ingredients derived from brown algae such as alginic acid, agar, carrageenan, and fucoidan, green algae or red algae; silane root (white and) extract; pectin, locust bean gum, aloe polysaccharide, alkaligenes-producing polysaccharide and the like. Polysaccharides; gums such as xanthan gum, tragant gum, guar gum; cellulose derivatives such as carboxymethyl cellulose and hydroxyethyl cellulose; synthetic polymers such as polyvinyl alcohol, polyvinyl pyrrolidone, carboxyvinyl polymer, alginic acid / methacrylic acid copolymer; hyaluronic acid And derivatives thereof; examples thereof include polyglutamic acid and derivatives thereof.

Examples of preservatives and bactericides include urea; paraoxybenzoic acid esters such as methyl paraoxybenzoate, ethyl paraoxybenzoate, propyl paraoxybenzoate, and butyl paraoxybenzoate; phenoxyethanol, dichlorophenol, hexachlorophene, chlorhexidine hydrochloride, and benza chloride. Plant-derived ethanol such as luconium, salicylic acid, ethanol, undecyleneic acid, phenols, jamar (imidazodeinylurea), propanediol, 1,2-pentanediol, various essential oils, bark dry distillate, radish fermented liquid, sugar cane Alternatively, there are 1,3-butylene glycol and the like.

Examples of powder components include cericite, titanium oxide, talc, kaolin, bentonite, zinc oxide, magnesium carbonate, magnesium oxide, zirconium oxide, barium sulfate, silicic anhydride, mica, nylon powder, polyethylene powder, silk powder, and cellulose. There are system powders, grain powders (rice, wheat, corn, talc, etc.), beans (soybeans, talc, etc.) powders, etc.

Examples of the ultraviolet absorber include ethyl paraaminobenzoate, ethylhexyl paradimethylaminobenzoate, amyl salicylate and its derivatives, 2-ethylhexyl paramethoxycinnamate, octyl silicate, oxybenzone, 2,4-dihydroxybenzophenone, 2-hydroxy-4. -Methoxybenzophenone-5-sulfonate, 4-tershally butyl-4-methoxybenzoylmethane, 2- (2-hydroxy-5-methylphenyl) benzotriazole, urocanic acid, ethyl urocanate, aloe extract, etc. ..

Examples of the antioxidant include butylhydroxyanisole, butylhydroxytoluene, propyl gallate, vitamin E and its derivatives (for example, vitamin E nicotinate, vitamin E linoleate, etc.).

Whitening agents include t-cycloamino acid derivatives, kodiic acid and its derivatives, ascorbic acid and its derivatives, hydroquinone or its derivatives, ellagic acid and its derivatives, nicotinic acid and its derivatives, resorcinol derivatives, tranexamic acid and its derivatives, 4 -Polish potassium methoxysalicylate, magnolignan (5,5'-dipropyl-biphenyl-2,2'-diol), hydroxybenzoic acid and its derivatives, vitamin E and its derivatives, α-hydroxyic acid, AMP (adenosine monophosphate) , Adenosine monophosphate), and these may be blended alone or in combination of two or more.

Examples of the ascorbic acid derivative include ascorbic acid esters such as ascorbic acid monobutyrate, ascorbic acid monocaplate, ascorbic acid monopalmitate, and ascorbic acid dibutyrate, ascorbic acid ethers, and ascorbic acid sugar derivatives such as ascorbic acid glucoside. However, examples of the ascorbic acid derivative include L-ascorbic acid-2-phosphate ester sodium, L-ascorbic acid-2-phosphate ester magnesium, L-ascorbic acid-2-sulfate sodium ester, and L-ascorbic acid-2. -Ascorbic acid ester salts such as magnesium sulfate, L-ascorbic acid-2-glucoside, L-ascorbic acid-5-glucoside, ascorbic acidcopheryl maleic acid, ascorbic acidcopheryl phosphate K, myristyl 3-glyceryl ascorbic acid, caprylyl Ascorbic acid sugar derivatives such as 2-glyceryl ascorbic acid, 6-position acylated products of those ascorbic acid sugar derivatives (acyl groups are hexanoyl group, octanoyl group, decanoyle group, etc.), L-ascorbic acid tetraisopalmitic acid ester, L- L-ascorbic acid tetrafatty acid esters such as ascorbic acid tetralauric acid ester, 3-O-ethylascorbic acid, L-ascorbic acid-2-phosphate-6-O-palmitate sodium, glyceryl ascorbic acid or acylation thereof Derivatives, glycerin ascorbic acid derivatives such as bisglyceryl ascorbic acid, aminopropyl L-ascorbic acid phosphate, hyaluronic acid derivatives of L-ascorbic acid, 3-OD lactose-L-ascorbic acid, isostearyl ascorbic acid, etc. However, as the hydroquinone derivative, albutin (hydroquinone-β-D-glucopyranoside), α-arbutin (hydroquinone-α-D-glucopyranoside) and the like are used, and as the tranexamic acid derivative, a tranexamic acid ester (for example, tranexamic acid lauryl ester, etc.) Examples thereof include tranexamic acid hexadecyl ester, tranexamic acid cetyl ester or a salt thereof), an amide form of tranexamic acid (for example, methylamide tranexamic acid), and examples of the resorcinol derivative include 4-n-butylresorcinol and 4-isoamylresorsinol. As the 2,5-dihydroxybenzoic acid derivative, for example, 2,5-diacetoxybenzoic acid, 2-acetoxy-5-hydroxybenzoic acid, 2-hydroxy-5-propionilo, etc. Xybenzoic acid and the like, nicotinic acid derivatives such as nicotinamide and benzyl nicotinate, and α-hydroxy acids include, for example, lactic acid, malic acid, succinic acid, citric acid, α-hydroxyoctanoic acid and the like. ..

Physiologically active ingredients include, for example, placental extract, soybean extract, yukinoshita extract, perilla extract, rice bran extract or its hydrolyzate, white potato extract or its hydrolyzate, white potato fermented product, shakyaku. Extract or its hydrolyzate, lactic acid fungus fermented rice, purple kib extract, lotus seed extract or its hydrolyzate, lotus seed fermented product, ginseng extract or its hydrolyzate, honeybee hydrolyzate, honeybee seed fermented product, Royal jelly fermented product, liquor lees extract or ceramide contained therein, liquor lees fermented product, Pandanus amaryllifolius Roxb. Extract, Arcangelicia flava Merrilli extract, chamomile extract, etc. Be done. In addition, coral grass extract, rice leaf extract or its hydrolyzate, eggplant (bergamot, Naga eggplant, Kamo eggplant, rice eggplant, etc.) extract or its hydrolyzate, apricot fruit extract, catamen giraffe, etc. Seaweed extract, marine flowering plant extract such as amamo, soymilk fermented product, jellyfish water, rice extract or its hydrolyzate, fermented rice extract, sprouted rice extract or its hydrolyzate, sprouted rice fermentation Products, black bean extract or its hydrolyzate, damask rose flower extract, bamboo shoot skin extract, linoleic acid and its derivatives or processed products (eg, liposomal linoleic acid, etc.), animal or fish-derived collagen and Its derivatives, elastin and its derivatives, glycyrrhizic acid and its derivatives (dipotassium salt, etc.), t-cycloamino acid derivatives, vitamin A and its derivatives, allantin, diisopropylamine dichloroacetate, γ-amino-β-hydroxybutyric acid, gentian extract , Lantern extract, Carrot extract, Otane carrot extract or fermented product thereof, Red ginseng extract, Mitsuishikonbu extract, Hechima extract, Anaaosa extract, Peach extract, Peach seed extract, Kiwi extract, Sunflower extract, Zizyphus joazeiro extract, paudalco bark extract, daily extract or fermented product, hibiscus flower extract or fermented product, hagoromogusa extract, cherimoya extract, mango extract, mangostin extract, funori extract Thing, Karyu tea extract, Benifuki extract, Purple orchid extract, Sansho peel or seed coat extract or hydrolyzate, Benibana flower extract, Casablanca extract, Sweet potato extract or its fermented product, Guava leaf extract, Dokudami There are extracts, evening white yuzu extract, aloe extract, fig flower extract, apple extract, white asparagus extract and the like.

Next, the present invention will be described in more detail with reference to Production Examples, Formulation Examples, and Test Examples, but the present invention is not limited thereto. In the following, all parts mean parts by weight, and% means all parts by weight.

Production example 1. Preparation of bergamot extract (juice juice) 3000 g of bergamot fruit was squeezed to obtain 1000 g of fruit juice. The juice was filtered to obtain 900 g of a slightly yellow transparent liquid. 9 g of an aromatic-unsubstituted synthetic adsorbent was added to the fruit juice, and the mixture was stirred for 1 hour and then filtered to obtain 880 g of a slightly yellow transparent juice. When performing the evaluation shown in the test example described later, the juice was adjusted so that its solid content concentration was 1.0%.

Production example 2. Preparation of bergamot extract (squeezed liquid) 880 g of squeezed liquid was obtained by the same operation as in Production Example 1. To this, 8.8 g of a synthetic adsorbent, which is an aromatic-unsubstituted high specific surface area treated product, was added, and after stirring for 2 hours, the synthetic adsorbent was recovered. The recovered synthetic adsorbent was added to an aqueous solution of 1,3-butylene glycol, and the mixture was stirred and filtered to obtain 400 g of a slightly yellow transparent juice (solid content concentration: 0.1%).

Production example 3. Preparation of bergamot extract (extract) After adding 200 g of 1,3-butylene glycol and 150 g of purified water to 40 g of dried bergamot fruit powder, the mixture was extracted at 80 ° C. The obtained crude extract was filtered to obtain 284 g of a brown transparent bergamot fruit extract solution (solid content concentration 2.30%).

Production example 4. Preparation of bergamot extract (extract) After adding a mixed solvent of 200 g of propanediol and 150 g of purified water to 40 g of dried bergamot fruit powder, extraction was performed at 40 ° C. The obtained crude extract was filtered to obtain 278 g of a brown transparent bergamot fruit extract solution (solid content concentration: 2.21%).

Production example 5. Preparation of bergamot extract (extract) After adding 350 g of a 50% ethanol aqueous solution to 40 g of dried bergamot fruit powder, extraction was performed at 20 ° C. The obtained crude extract was filtered to obtain 289 g of a brown transparent bergamot fruit extract solution (solid content concentration: 2.38%).

Production example 6. Preparation of bergamot extract (extract) After adding a mixed solvent of 400 g of 1,3-butylene glycol and 300 g of purified water to 80 g of dried powder of bergamot whole plant (including fruits, peels and seeds), at 40 ° C. Extracted. The obtained crude extract was filtered to obtain 270 g of a brown transparent bergamot extract solution (solid content concentration 2.09%).

Prescription example 1. Toner [A component] Part Olive oil 1.0
Polyoxyethylene (5.5) cetyl alcohol 5.0
Butylparaben 0.1
[B component]
Juice liquid of Production Example 1 5.0
Ethanol 5.0
Glycerin 5.0
1,3-butylene glycol 5.0
Potassium hydroxide Appropriate amount Purified water 100 parts in total [C component]
Appropriate amount of fragrance After heating each of the A component and the B component to 80 ° C. or higher, the B component was added to the A component and stirred, and further homogenized with hiscotron (5000 rpm) for 2 minutes. After cooling this to 50 ° C., component C was added, stirred and mixed, and further cooled to 30 ° C. or lower to obtain a lotion.

Prescription example 2. Toner A lotion was obtained in the same manner as in Formulation 1, except that 5.0 parts of the juice of Production Example 2 was used instead of the juice of Production Example 1 contained in the B component of Formulation Example 1.

Prescription example 3. Toner Toner was obtained in the same manner as in Formulation Example 1 except that 5.0 parts of the extract of Production Example 3 was used instead of the juice squeezed liquid of Production Example 1 contained in the B component of Formulation Example 1.

Prescription example 4. Toner Toner was obtained in the same manner as in Formulation Example 1 except that 5.0 parts of the extract of Production Example 4 was used instead of the juice of Production Example 1 contained in the B component of Formulation Example 1.

Prescription example 5. Toner Toner was obtained in the same manner as in Formulation Example 1 except that 5.0 parts of the extract of Production Example 5 was used instead of the squeezed liquid of Production Example 1 contained in the B component of Formulation Example 1.

Prescription example 6. Toner Toner was obtained in the same manner as in Formulation Example 1 except that 5.0 parts of the extract of Production Example 6 was used in place of the juice of Production Example 1 contained in the B component of Formulation Example 1.

Prescription example 7. Emulsion [Component A] Part Liquid paraffin 6.0
Hexalan 4.0
Jojoba oil 1.0
Bergamot essential oil 0.025
Polyoxyethylene (20) sorbitan monostearate 1.0
Oil-based glyceryl stearate 1.0
Soy lecithin 1.5
[B component]
Juice liquid of Production Example 1 3.0
L-ascorbic acid-2-glucoside 2.0
Potassium hydroxide 0.5
Glycerin 3.0
1,3-butylene glycol 2.0
Carboxymethyl cellulose 0.3
Sodium hyaluronate 0.01
Water-soluble collagen 0.1
Amount of purified water totaling 100 parts [C component]
Appropriate amount of fragrance The above components A and B were heated to 80 ° C. or higher, and then stirred and mixed. After cooling this to 50 ° C., component C was added and further stirred and mixed to obtain a milky lotion.

Prescription example 8. Emulsion Emulsion in the same manner as in Formulation 7, except that 2.0 parts of tranexamic acid is used instead of 2.0 parts of L-ascorbic acid-2-glucoside and 0.5 part of potassium hydroxide in the B component of Formulation Example 7. Got

Prescription example 9. Emulsion Emulsion was prepared in the same manner as in Formulation 7, except that 3.0 parts of arbutin was used instead of 2.0 parts of L-ascorbic acid-2-glucoside and 0.5 part of potassium hydroxide in the B component of Formulation Example 7. Obtained.

Prescription example 10. Emulsion Same as in Formulation 7, except that 3.0 parts of nicotinamide is used instead of 2.0 parts of L-ascorbic acid-2-glucoside and 0.5 parts of potassium hydroxide in the B component of Formulation Example 7. Emulsion was obtained.

Prescription example 11. Emulsion Same as in Formulation Example 7 except that 5.0 parts of Sohakuhi extract is used instead of 2.0 parts of L-ascorbic acid-2-glucoside and 0.5 parts of potassium hydroxide in the B component of Formulation Example 7. Emulsion was obtained.

Prescription example 12. Emulsion [A component] Part Squalene 3.0
Behenyl alcohol 3.0
Hexalan 4.0
Jojoba oil 1.0
Polyoxyethylene (20) sorbitan monostearate 1.0
Glycerin fatty acid ester 1.0
Soy lecithin 1.5
[B component]
Juice liquid of Production Example 1 2.5
Juice liquid of Production Example 2 2.5
L-ascorbic acid-2-glucoside 2.0
Potassium hydroxide 0.5
Dipotassium glycyrrhizinate 0.1
Glycerin 3.0
1,3-butylene glycol 2.0
Water-soluble collagen 0.1
Sodium hyaluronate 0.01
Amount of purified water totaling 100 parts

Prescription example 13. Lotion [Ingredients] Part Production Example 2 Juice Liquid 10.0
Ethanol 10.0
Glycerin 3.0
1,3-butylene glycol 2.0
Methylparaben 0.2
Citric acid 0.1
Sodium citrate 0.3
Carboxyvinyl polymer 0.1
Xanthan gum 0.1
Perfume Appropriate amount Potassium hydroxide Appropriate amount Purified water 100 parts in total The above components were mixed to obtain a lotion.

Prescription example 14. Lotion A lotion was obtained in the same manner as in Formulation 13 except that 10.0 parts of the extract of Production Example 3 was used instead of the juice of Production Example 2 in the components of Formulation Example 13.

Prescription example 15. Essence [Ingredients] Part Ethanol 2.0
Glycerin 5.0
1,3-butylene glycol 5.0
Methylparaben 0.1
Hyaluronic acid 0.1
Hydrolyzed hyaluronic acid solution 0.1
Juice liquid of Production Example 1 5.0
Citric acid 0.3
Sodium citrate 0.6
Amount of purified water totaling 100 parts Hyaluronic acid was dissolved in purified water, and the remaining raw materials were sequentially added and dissolved by stirring to obtain a transparent essence.

Example 16. Liquid foundation [Component A] Part Stearic acid 2.4
Propylene glycol monostearate 2.0
Setostearyl alcohol 0.2
Liquid lanolin 2.0
Liquid paraffin 3.0
Isopropyl myristate 8.5
Propylparaben 0.05
[B component]
Juice liquid of Production Example 1 5.0
Sodium Carboxymethyl Cellulose 0.2
Bentonite 0.5
Propylene glycol 4.0
Triethanolamine 1.1
Methylparaben 0.1
Amount of purified water totaling 100 parts [C component]
Titanium oxide 8.0
Talc 4.0
Appropriate amount of color pigment The above components A and B were heated and then mixed and stirred. This was reheated, the above C component was added and poured into a mold, and the mixture was stirred until it reached room temperature to obtain a liquid foundation.

Prescription example 17. Body shampoo [Ingredient A] Part N-lauroylmethylalanine sodium 25.0
Coconut oil fatty acid potassium solution (40%) 26.0
Coconut oil fatty acid diethanolamide 3.0
Methylparaben 0.1
[B component]
Juice liquid of Production Example 2 5.0
1,3-butylene glycol 2.0
Amount of purified water totaling 100 parts A component and B component are each heated to 80 ° C and uniformly dissolved, then B component is added to A component, and stirring is continued to cool to room temperature to obtain a body shampoo. It was.

Prescription example 18. Hair growth cosmetics [Ingredients] Part Dipotassium glycyrrhizinate 0.1
Mononitroguaiacol Sodium 0.02
Pyridoxine hydrochloride 0.03
l-Menthol 0.8
Menispermaceae root extract 0.3
Brown algae extract 0.3
Panax ginseng extract 0.3
Swertia japonica extract 2.0
Juice liquid of Production Example 1 3.5
Trimethylglycine 0.5
Lactic acid 0.2
1,3-butylene glycol 10.0
Phenoxyethanol 0.2
Polyoxyethylene hardened castor oil 0.4
L-Arginine Appropriate amount Ethanol 20.0
Amount of purified water totaling 100 parts The above components were sufficiently stirred and mixed to obtain a hair restorer.

Prescription example 19. Hair shampoo [Ingredient A] Part N-coconut oil fatty acid methyl taurine sodium 10.0
Polyoxyethylene (3) Alkylation Ether Sodium Sulfate 20.0
Betaine Lauryldimethylaminoacetic Acid 10.0
Coconut oil fatty acid diethanolamide 4.0
Methylparaben 0.1
[B component]
Citric acid 0.1
Juice liquid of Production Example 1 2.0
1,3-butylene glycol 2.0
Amount of purified water that makes up 100 parts A component and B component are each heated to 80 ° C and uniformly dissolved, then B component is added to A component, and stirring is continued to cool to room temperature to obtain a hair shampoo. It was.

Example 20. Hair conditioner [Component A] Part Polyoxyethylene (10) Hardened castor oil 1.0
Distearyldimethylammonium chloride 1.5
Stearyltrimethylammonium chloride 2.0
Glyceryl 2-ethylhexanoate 1.0
Cetanol 3.2
Stearyl alcohol 1.0
Methylparaben 0.1
[B component] Part Production example 2 juice juice 2.0
1,3-butylene glycol 5.0
Amount of purified water totaling 100 parts A component and B component were each heated to 80 ° C. to dissolve them uniformly, then B component was added to A component, and stirring was continued to cool to room temperature to obtain a hair rinse. ..

Test example 1. Evaluation test of collagen gel shrinkage promoting effect First, collagen gel was prepared as follows. That is, a collagen gel solution under ice-cooling (CellmatrixType IA manufactured by Nitta Gelatin Co., Ltd.), a 0.05 N sodium hydroxide solution containing 200 mM HEPES and 2.2% NaHCO ₃ , and an Eagle MEM (Nissui) 10-fold concentrated solution. (NaHCO ₃ -free) was added in a ratio of 8: 1: 1 and sufficiently stirred and neutralized. A suspension of human skin fibroblasts NB1RGB adjusted to 5 × 10 ⁵ cells / mL with Eagle MEM containing 0.5% NCS was added thereto at a ratio of 8: 2, and the mixture was sufficiently stirred, and each was placed on a 24-well plate. 0.5 mL of each hole was injected and immediately gelled at 37 ° C. After 1 hour, 1 mL of a sample-containing medium prepared by adding the extract of Production Example 2 according to the present invention to Eagle's MEM containing 0.5% NCS was added, and the periphery of the gel was further peeled off and cultured for 3 days. .. Here, the sample solution was prepared so that the final concentration as a solution was 0.5% and 1.0% with respect to the total amount of the medium. The gel area was measured as follows. That is, the 24-hole plate being evaluated was placed on the scanner in which the transmitted light unit was set, and scanning was performed to electronically image the images of collagen gel in all wells. The image was taken into a computer, and the area of each collagen gel was quantified using image analysis software (ImageJ). The group to which 30% 1,3-butylene glycol was added instead of the above sample was used as a control, and the relative value of the collagen gel area of each sample-added group was determined with the area of the collagen gel in the obtained control group as 100. In addition, in order to confirm whether the test system is functioning normally, the same test was performed when Eagle MEM containing 10% NCS was added as a positive control instead of the sample.

The results of Test Example 1 are shown in Table 1.
[Table 1]

As shown in Table 1, it was shown that the bergamot extract according to the present invention has a remarkably excellent collagen gel contraction promoting effect.

Test example 2. Evaluation test of collagen synthesis promoting effect Human dermis-derived fibroblast NB1RGB was seeded at 1 × 10 ⁴ cells / hole in a 96-well microplate containing 0.5% NCS-containing eagle minimum essential medium, and seeded at 37 ° C., 5.0. After pre-culturing under the condition of% CO ₂ for 1 day, the extract of Production Example 2 according to the present invention was added to the medium as a sample solution, and the cells were cultured under the same conditions for another 5 days. Here, the sample solution was prepared so that the final concentration of the solution was 0.5% or 1.0% with respect to the total amount of the medium. Next, the medium was removed, cells were fixed with cold methanol and cold ethanol, and then stained with a saturated aqueous picric acid solution containing 0.1% silius red. After washing with purified water, extraction was performed with a 0.1% NaOH: methanol = 1: 1 solution, and the amount of collagen was measured at a wavelength of 540 nm using a microplate reader (Model 680, manufactured by Biorad). In the case of no sample addition (control) in which 30% 1,3-butylene glycol was added instead of the sample solution, the same operation as above was performed, and the amount of collagen at the time of addition of each sample to the amount of collagen obtained here was calculated. The relative value was calculated and used as the fibroblast collagen synthesis rate (%).

[Table 2]

As shown in Table 2, it was shown that the bergamot extract according to the present invention has a remarkably excellent collagen synthesis promoting effect in a concentration-dependent manner.

Test example 3. Evaluation test of decolin synthesis promoting effect In the present invention, the synthesis promoting effect of decolin, which is a kind of proteoglycan synthesized in fibroblasts and plays an important role in the formation of the collagen network structure of the dermis, was evaluated.
Normal human skin-derived fibroblasts (NB1RGB) were prepared at 1 × 10 ⁵ cells / mL with 0.5% by volume NCS-containing Eagle MEM (manufactured by Nissui Pharmaceutical Co., Ltd.), and 100 μL was seeded on a 96-well microplate. The cells were cultured at 37 ° C. under 5% carbon dioxide and saturated steam. After 24 hours, the culture solution containing the extract of Production Example 2 according to the present invention was added and further cultured so that the final concentration as a solution was 2% with respect to the total amount of the culture solution. In addition, as a control, a test group was set in which a culture solution containing 50% 1,3-butylene glycol was additionally added so that the final concentration was 2%. After 48 hours, the culture supernatant was collected, and the amount of decorin secreted in the culture supernatant was measured by the ELISA method using an anti-decolin antibody using a decorin measurement kit (manufactured by BOSTER).

[Table 3]

As shown in Table 3, the bergamot extract according to the present invention was shown to have a remarkably excellent effect of promoting decorin synthesis.

Test example 4. Evaluation test of melanosome uptake inhibitory effect Human epidermal cell NHEK was seeded in 1 × 10 ⁴ cells / hole in a 96-well microplate containing HuMedia KG2 medium (manufactured by Kurabo) under the conditions of 37 ° C. and 5.0% CO ₂ . After pre-culturing for 1 day underneath, the supernatant is removed, and HuMedia KB2 medium (manufactured by Kurabo) containing the extracts of Production Examples 1 and 3 to 5 according to the present invention as a sample solution is added, and further 2 under the same conditions. Incubated for days. Here, the sample solution was prepared so that the final concentration as a solution was 1.0% and 2.0% with respect to the total amount of the medium. Then, 7.2 × 10 ⁸ cells / mL fluorescent beads (FluoSpheres (registered trademark) Fluorescent Microspheres (Invitrogen)) were added and kept at 37 ° C. for 1 hour. Then, the supernatant was removed, washed twice with PBS (−), 100 μL / hole of hoechst33342 reagent diluted 100-fold with PBS (−) was added, and the mixture was incubated at 37 ° C. for 15 minutes to fluorescently stain the DNA. Then, the fluorescence intensity (excitation: 542 nm, radiation: 590 nm, and excitation: 355 nm, radiation: 460 nm / fluorescent microplate reader (Fluoroscan Ascent, manufactured by Thermo Fisher Scientific)) was measured, and the amount of fluorescent beads taken up per DNA. Asked. In the case of no sample addition (Control) in which 30% 1,3-butylene glucol was added instead of the sample solution, the same operation as above was performed, and the relative value of each sample was added to the value obtained here. The value was determined and used as the fluorescent bead uptake rate (%) per DNA of epidermal cells.

[Table 4]

As shown in Table 4, it was shown that the bergamot extract according to the present invention has a remarkably excellent effect of suppressing melanosomes uptake in a concentration-dependent manner.

Test example 5. Evaluation test of DPPH radical scavenging effect 2.4 parts of DPPH was dissolved in 20 parts of ethanol, and 20 parts of purified water was added thereto to prepare a DPPH solution. To 24 parts of this DPPH solution, 19.2 parts of an 18v / v% ethanol solution and 4.8 parts of a 2M sodium acetate-sodium acetate buffer (pH 5.5) were added to prepare a DPPH-added solution. In addition, in order to subtract the influence of the color tone of the extract itself on the test, a 50v / v% ethanol solution was used instead of the DPPH solution, and a mixture of an 18v / v% ethanol solution and a 2M sodium acetate-sodium acetate buffer solution was used. It was used as a control solution. Next, the extract (squeezed liquid or extract) of Production Examples 1 to 5 according to the present invention was diluted with purified water to prepare a sample solution. Here, as the sample solution, two kinds of concentrations prepared so that the final concentrations of the solution as a solution with respect to the total amount were 1.0% and 2.0%, respectively, were used. This sample solution is mixed with the DPPH-added solution or the control solution at a ratio of 1: 3, and after allowing to stand at room temperature for 10 minutes, the absorbance at 550 nm when each test solution is mixed with the DPPH-added solution and each test solution are also obtained. The difference from the absorbance at 550 nm when mixed with the control solution was measured, and the residual amount of DPPH radical was confirmed. At the same time, the same operation as above was performed using a 30% 1,3-butylene glycol aqueous solution instead of the juices of Production Examples 1 and 2 according to the present invention as a control, and the DPPH radical residual ratio obtained here was obtained. The relative value of the DPPH radical residual rate at the time of adding each sample was determined. Further, in order to confirm whether the test system is functioning normally, the same test was conducted when water-soluble vitamin E (final concentration 25 μM) was added as a positive control instead of the sample solution.

The results of Test Example 5 are shown in Table 5.
[Table 5]

As shown in Table 5, it was shown that the bergamot extract according to the present invention has a remarkably excellent DPPH radical scavenging effect in a concentration-dependent manner.

Test example 6. Evaluation test of SOD-like activity [Test method]
0.2 M Tris-hydrochloric acid buffer 50 μL, 1 mM ethylenediamine tetraacetic acid (EDTA) disodium solution 20 μL, 0.75 mM nitroblue tetrazolium chloride (NBT) solution 10 μL, 1 mM xanthin solution 20 μL, 0.06 U / mL xanthin oxidase solution 50 μL, A sample solution was prepared by mixing 50 μL of the extracts of Production Examples 1 to 5 according to the present invention (adjusted so that their final concentrations were 1.0% and 2.0%). The sample solution was incubated at 37 ° C. for 5 minutes to generate superoxide. Then, the absorbance at 560 nm was measured for the amount of formazan produced by reducing NBT with superoxide. Further, as a control, a 30% 1,3-butylene glycol solution was used instead of the juices of Production Examples 1 and 2 and the same operation as above was performed, and the absorbance at the time of addition of each sample was relative to the absorbance obtained here. The value was calculated and used as the residual rate of superoxide (%). A similar test was also performed when superoxide dismutase (SOD) 8.75 units / mL was added as a positive control instead of the sample solution to confirm that the test system was functioning normally. ..

The results of Test Example 6 are shown in Table 6.
[Table 6]

As shown in Table 6, the bergamot extract according to the present invention was shown to have remarkably excellent SOD-like activity in a concentration-dependent manner.

Test example 7. Evaluation test of lipid accumulation inhibitory effect Normal hamster sebaceous gland cells (Ha-SE) were seeded at 8 × 10 ³ cells / hole on a 96-well microplate containing HuMedia-BG (manufactured by Kurabo) at 37 ° C., 5.0. The cells were cultured for 7 days under the condition of% CO ₂ . After culturing, the medium was replaced with a differentiation-inducing medium containing the extracts of Production Examples 1, 3 to 5 according to the present invention as a sample solution (HuMedia-BD (manufactured by Kurabou) containing 2 μM testosterone instead of insulin), and further under the same conditions. Incubated for 14 days. Here, the sample solution was prepared so that the final concentration of the solution was 0.5% or 1.0% with respect to the total amount of the medium. After culturing, the medium was removed, the cells were washed with PBS (-), and the cells were fixed by adding a 10% formalin solution. The cells were then washed with PBS (-), 60% isopropanol was added, and the mixture was allowed to stand for 1 minute. Then, 0.18% oil red stain solution was added, and the mixture was allowed to stand at room temperature for 30 minutes. Next, after washing with 60% isopropanol, isopropanol was added, and then the amount of accumulated lipid at a wavelength of 540 nm was measured using a microplate reader (Model 680, manufactured by Bio-Rad). A similar test was also performed when 13-cisretinoic acid (2 μM) was added as a positive control instead of the sample solution in order to confirm whether the test system was functioning normally.

[Table 7]

As shown in Table 7, it was shown that the bergamot extract according to the present invention has a significantly excellent lipid accumulation inhibitory effect in a concentration-dependent manner.

Claims (5)

Citrus bergamia, which belongs to the genus Citrus of the Rutaceae family, is a collagen gel shrinkage accelerator containing an aromatic-unsubstituted synthetic adsorbent-treated product of a fruit juice or extract as an active ingredient. Bergamot (Citrus bergamia) belonging to the genus Citrus of the Rutaceae family. A collagen synthesis promoter containing an aromatic-unsubstituted synthetic adsorbent-treated product as an active ingredient. Citrus bergamia, which belongs to the genus Citrus of the Rutaceae family. A decorin synthesis accelerator containing an aromatic-unsubstituted synthetic adsorbent-treated product of a juice or extract of a fruit. Citrus bergamia belonging to the genus Citrus of the Rutaceae family A lipid accumulation inhibitor containing an aromatic-unsubstituted synthetic adsorbent-treated product of a fruit juice or extract as an active ingredient. Bergamot (Citrus bergamia) belonging to the genus Citrus of the Rutaceae family . A whitening agent containing an aromatic-unsubstituted synthetic adsorbent-treated product as an active ingredient .