KR101108783B1 - Hairdye - Google Patents

Abstract

The present invention provides a hair dye containing rhubarb, sewage water, seolja mixed extract.

The hair dye of the present invention has excellent initial hair dye, cumulative hair dye, and has fewer side effects such as hair droop and skin irritation.

Hair dye, rhubarb, sewage, missing

Description

Hair Dye {Hairdye}

The present invention relates to a hair dye containing a natural extract and a preparation method thereof.

Hair dyes are classified into temporary, semi-permanent, and permanent hair dyes depending on the color's persistent condition.

Permanent hair dyes have the mechanism of artificially swelling the hair to decolorize the hair, and the dye penetrated into the decolored hair to form a polymer so that the protein of the hair is dyed. Permanent hair dyes can be divided into oxidation, metal and vegetable hair dyes depending on the dye, and the most frequently used hair dyes are oxidative hair dyes using oxidizing dyes such as aromatic amino compounds.

Oxidative hair dyes are excellent in hair dyeing, but have a disadvantage of slow hair dyeing and discoloration due to sunlight, washing, etc., and strong alkalis and monoethanolamines that swell the hair to facilitate the penetration of dyes and make polymers inside the hair. Since the use of an alkaline agent such as, etc., there is a disadvantage in the case of causing gloss of hair, hair damage, skin irritation and skin troubles. In addition, a large amount of dyes used to increase the dyeing power may reduce the stability of the hair dye and cause hair damage and strong skin irritation. In particular, the skin problems and irritation caused by hair dyes in severe cases, such as redness of the skin, erythema of the skin or erythema may occur in the whole body, so there are more limitations in use for sensitive people.

Therefore, in order to improve the disadvantages and discomforts of these hair dyes, the development of natural hair dye materials containing a large amount of natural hair ingredients, excellent effects such as scalp protection, hair protection, anti-allergy and low cost, and the use of the materials Development of an easy hair dye is essential.

Accordingly, research on hair dyes containing herbal ingredients is underway. For example, U.S. Patent No. 6,656,229 discloses a hair dye that contains indican and beta-glucosidase enzymes derived from indigo plants, and ginseng (Panax ginseng), a saponin-containing plant, as a hair dye conditioner. U.S. Patent No. 5,078,750 discloses hair dyes containing iridoid glycosides and aglycones thereof. In addition, Korean Patent Registration No. 10-0608711 discloses a hair dye to which the herbal medicine red ginseng, sugar, cheongung, licorice extract is added for hair dyeing, color fastness, hair conditioning, hair protection. However, known hair dyes are mainly focused on the development of natural extracts to assist the hair dye and reduce the irritation of the scalp rather than the development of natural hair dye itself.

On the other hand, rhubarb is a polygonaceae plant, also called janggun grass. It is native to China's West and Qinghai areas, and it grows in high altitudes of more than 1,000m above sea level in Korea. ought. Rhubarb root and root stem (root) is used as a constipation treatment to help peristalsis, root extract is used as an antibacterial agent for dysentery, typhoid, Escherichia coli, dry stomach, diarrhea. (The Composition and Use of Herbs, Encyclopedia of Science, January Written, 1994)

Shouo (Polygonum multiflorum Thunberg) is a tuber of Polygonaceae, and is used as a tonic, tonicity, and emollient in oriental medicine. (Industrial Science Research Institute, Korea Institute of Oriental Medicine, p370, Hong Namdu, Kim Nam-jae, Quality of Chinese Medicine Management, Shinil Corporation, p485

The fault is the seeds of Cassia obtusifolia Linne and Cassia tora Linne. In oriental medicine, hepatic (肝火) is used to treat redness, swelling, soreness, and tears, and to treat night blindness. Also used for. In addition, it is known that the deficiency has functions such as lowering blood pressure, diuresis, constipation, uterine contraction and skin fungus suppression, and lowering cholesterol. (Pharmaceutical Plant Research Society, New Drug Botany Science, Hakchangsa, p285, Hong Nam-du, Kim Nam-jae, Quality Management, Shinil Corporation, p282)

Therefore, it is necessary to develop a hair dye of a natural material that is good for the scalp health while minimizing irritation to the skin or causing trouble to the scalp and having excellent hair dyeing power.

SUMMARY OF THE INVENTION An object of the present invention is to provide a natural hair dye which is excellent in dyeing and dyeing fastness when hair is dyed, and is good for hair protection, scalp irritation and scalp health.

The present invention provides hair dyes containing rhubarb, sewage, and deficiency mixed extract.

In the present invention, rhubarb, sewage, the defect may be cultivated directly or taken directly from the mountains and fields, and may be purchased from places such as Gyeongdong market.

In the present invention, the mixed extract is preferably extracted with water, anhydrous or hydrous alcohol of 1 to 4 carbon atoms, butylene glycol, propylene glycol, or a hydrous glycol thereof, it is extracted with 50% (v / v) hydrous ethanol Even more preferred, but the extraction solvent of the present invention is not limited to these examples.

In the present invention, rhubarb, sewage, crystallized mixed extract can be obtained by conventional extraction methods known to those skilled in the art. For example, it can be prepared by a simple extraction method, thermal extraction method or ultrasonic extraction method.

Here, in the simple extraction method, the sample (mixture) is chopped or pulverized, and then an extractant of 1 to 20 times the volume of the dry weight is added, followed by immersion at room temperature for a certain period of time, taking the supernatant, filtration and using a vacuum concentrator. Means to obtain an extract by concentration. In the heat extraction method, the sample is chopped or pulverized, and then, an extractant having a volume of 1 to 20 times the dry weight is added, heated in an extractor equipped with a cooling condenser for a predetermined time, filtered with a filter paper, and left to stand at room temperature for a predetermined time. It means taking a filtration and concentrated using a vacuum concentrator to obtain an extract.

Ultrasonic extraction method is chopped or pulverized, and then the extraction solvent of 1 to 20 times the dry weight is added and immersed at room temperature for a certain time, and then a specific watt (watt) at room temperature or heated in a bath extractor equipped with an ultrasonic oscillator. ) To extract for a certain time to obtain an active ingredient.

The extract thus obtained may be a liquid concentrated with a concentrator or a powder lyophilized with a lyophilizer.

The extract of the present invention is preferably extracted by the ultrasonic extraction method, and rhubarb, sewage and crystallized in the extraction solvent for 4 to 30 days at 1 to 10 days after the ultrasonic wave oscillator attached to the bath extractor ultrasonic wave at 20 to 40 ℃ Even more preferably extracted for 1 to 10 hours.

Referring to the method for producing a mixed extract of the present invention in detail as follows. The dried product of rhubarb and sewage is chopped and mixed by grinding, followed by pulverization, and then an extraction solvent selected from 1 to 10 times the volume of water, anhydrous or hydrous alcohol having 1 to 4 carbon atoms is added thereto, and then at 4 to 30 ° C. After 1-10 days, using a bath extractor equipped with a 40.5kH ultrasonic oscillator, extract the active ingredient for 1-10 hours at a temperature of 20 ~ 60 ℃ and 200 ~ 500watt ultrasonic waves, and then concentrated the extraction solvent in a reduced pressure concentrator The concentrate is obtained by using the lyophilizer as a solid extract of the present invention.

In addition, the dried product of rhubarb, sewage, clarifiers, pulverized and mixed, one selected from the group consisting of water of 1 to 15 times the volume of the dry weight, anhydrous or hydrous alcohol of 1 to 4 carbon atoms, propylene glycol, butylene glycol In order to prevent the solvent from evaporating, the above solvent is used, followed by extracting by heat extraction at 30 to 100 ° C. for 3 to 48 hours or by depositing at 5 to 30 ° C. for 1 to 10 days in order to prevent the solvent from evaporating. The extract is concentrated in a vacuum condenser and dried in a lyophilizer or spray dryer to obtain the mixed extract of the present invention as a solid.

In the present invention, the mixing ratio of rhubarb: sewage: glyph may vary, but it is preferable in the yield of the extract that the mixed dry weight ratio of rhubarb: sewage: glyph is 1: 1: 1.

In the present invention, rhubarb, sewage, clarifier mixed extract may be added as a liquid weight of about 10% to 50% by weight relative to the total liquid weight of the hair dye, 0.1 to 20% by weight dry weight relative to the total dry weight of the hair dye. It may be added, preferably in an amount of 0.01 to 5% by weight, more preferably 0.1 to 3% by weight.

The dye included in the hair dye of the present invention uses an oxidized dye. The oxidation dye is not particularly limited in its kind, but, for example, p-phenylenediamine, o-phenylenediamine, resorcinol, 2-methylresorcinol, m-phenylenediamine, and m-aminophenol , o-aminophenol, p-aminophenol, toluenediamines, aminonitrophenols, diphenylamines, N-phenyldiamines, diaminopyridines, and mixtures thereof. Oxidation dyes contain 0.001 to 3.000 wt% based on the total weight of the hair dye.

Propylene glycol, cetearyl alcohol, oleic acid, cetes, stearamide die, oleic acid, oleyl alcohol, dimethicone, behenyl alcohol, glyceryl stearate SE And mixtures thereof, which contain from 5.00 to 30.00 wt%, preferably from 17.00 to 25.00 wt%, based on the total weight of the hair dye.

The hair dye of the present invention may contain a component that can be blended into a general external preparation for hair, as necessary. For example, it may contain a known hair protector, alkali agent, chelating agent, surfactant, pH adjuster, moisturizer, thickener, preservative, antioxidant, fungicide, anti-inflammatory, antimicrobial agent, solvent, flavoring agent, pigment and the like. .

In the present invention, the hair protector helps to fix the dye on the hair surface, and forms a water-repellent thin film on the hair to slow the discoloration of the dye due to water washing and sunlight, thereby providing excellent conditioning effect on the surface of the hair to prevent hair damage. It also helps stabilize the emulsion. Hair protectants include sodium methyl cocoyl taurate, hydrolyzed keratin, tocopheryl acetate, cetrimonium chloride, glyceryl stearate SE, Fiji-11 methyl ether dimethicone, cyclomethicone, ammonium glycylizate, It may be selected from glyceryl linoleate, linoleic acid, ceramide, mineral oil, petrolatum, polyquaternium-10, polyquaternium-7 and mixtures thereof, based on the total weight of the hair dye, 5.00 to 20.00wt%, preferably 7.00 To 15.00 wt%.

Alkaline aids the dissolution of the dye, swells the hair to facilitate the penetration of dye molecules into the hair, and activates the hydrogen peroxide of the second agent, such as monoethanolamine, strong ammonia water, and the like. 0.01 to 2.0 wt%, preferably 0.1 to 1.0 wt%.

The chelating agent acts as a metal blocker, and there are disodium editiide, tetrasodium idieti, etidronic acid, etc., and if necessary, 0.001 to 2.0 wt%, preferably 0.01 based on the total weight of the hair dye. To 1.0 wt%.

The pH adjusting agent may be any of organic acids such as citric acid, ascorbic acid, succinic acid, tartaric acid, lactic acid, malic acid, glycolic acid, and inorganic acids such as hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, and the like. , Potassium salts or ammonium salts may be used in combination, sodium hydroxide, potassium hydroxide may be used, and may contain 0.001 to 1.0 wt%, preferably 0.01 to 0.5 wt% based on the total weight of the hair dye. .

Dissolution aids can be used, for example, isopropyl myristate, polyethylene glycol, medium chain fatty acid triglycerides, hydrocarbons, glycols, and the like, and 1.0 to 25.0 wt%, preferably 2.0 to 15.0, based on the total weight of the hair dye. It may contain wt%.

The surfactant is, for example, ammonium lauryl sulfosuccinate, ammonium lauryl sulfate, sodium cocoyl isionate, sodium lauryl isionate, sodium lauryl sulfate, triethanolamine lauryl sulfate, sodium lauryl ether Anionic surfactants such as sulfates (EO 1 to 3); Cationic surfactants such as tertiary aliphatic amine salts, quaternary ammonium chlorides having at least one C12-22 alkyl group, alkyltrimethylammonium chloride, dialkyldimethylammonium chloride, alkyltrimethylammonium bromide and the like; And amphoteric surfactants such as betaine, amidebetaine, and sulfobetaine type, may be used alone or in combination. The hair dye of the present invention may contain 0.1 to 10.0 wt% of the surfactant based on the total weight of the hair dye with respect to the weight of the hair dye.

Moisturizing agents may be used, for example, glycerin, propylene glycol, butylene glycol, dipropylene glycol, sorbitol, and the like, and 0.1 to 5.0 wt%, preferably 0.5 to 3.0 wt%, based on the total weight of the hair dye. It may contain.

The thickener is, for example, methyl cellulose, hydroxymethyl cellulose, hydroxyethyl cellulose, carrageenan, carboxymethyl cellulose, carboxymethylhydroxyguanine, cetearyl alcohol, stearic acid, polyquaternium-7, polyquaternium-10 It may be a high molecular compound, and the like can be used in various ways.

Preservatives can be, for example, benzoic acid, paraoxybenzoic acid esters, mixtures of methylchloroisothiazolinones, phenoxyethanol, DMDM hydantoin, and the like, if necessary, based on the total weight of the hair dye, preferably 0.01 to 2.0 wt%. Preferably 0.1 to 1.0 wt%.

Antioxidants can be, for example, ammoniumthioglycolate, dibutylhydroxytoluene, ascorbic acid, sodium sulfate, etc., and if necessary, 0.001 to 0.1 wt%, preferably 0.01 to 0.05, based on the total weight of the hair dye. It may contain wt%.

Fungicides can be, for example, chlorhexidine gluconate, quaternary ammonium salts, pyrotonolamine, zinc pyrithione suspensions, uridopyropicbutylcarbamate, salicylic acid, and the like, if necessary, from 0.001 to 1.0 wt. %, Preferably 0.01 to 0.5 wt%.

The anti-inflammatory component may be, for example, ammonium glycylizate, potassium glycylizate, stearyl glycyretinate, chamomile, alphabisabolol, allantoin and mixtures thereof, and if desired, 0.01 to 10.0 wt%, preferably 0.1 to 5.0 wt%, based on weight.

Antimicrobial components include, for example, phenoxyethanol, chlorhexidine, chlorhexidine gluconate, pyroxtonolamine, ketoconazole, arnica extract, iodopyrrofinylbutylcarbamate, benzalkonium chloride, benzenetonium chloride, benzoic acid and salts thereof, benzyl alcohol, Lavender, rosemary, salicylic acid, triclocarban, zinc pyrithione suspensions and mixtures thereof and the like, and may contain 0.01 to 10.0 wt%, preferably 0.1 to 5.0 wt%, based on the total weight of the hair dye, if necessary. have.

The solvent may be, for example, ethanol, purified water, cyclomethicone, mineral oil, dimethicone, and the like, and may contain 0.1 to 10.0 wt%, preferably 1.0 to 5.0 wt%, based on the total weight of the hair dye. .

Flavoring agents and pigments may use ingredients used in general scalp and hair preparations. The amount used is the amount used in general hair dyes.

The hair dye of the present invention is preferably a cream type or a liquid type, and the oxidizing agent used in combination with the hair dye composition of the present invention may also be a cream type or a liquid type. In addition, it can be prepared in the form of powder, shampoo, jelly, aerosol and the like.

When the hair dye of the present invention is used for hair dyeing, it is preferable to use it as a transdermal administration method such as directly applying or spraying on the hair.

The amount of the hair dye of the present invention can be appropriately adjusted according to the condition of the hair, the age of the user, the length of the hair, and the like, and the application time can also be appropriately adjusted according to the individual. It is preferable to apply about once at about 50-200 mL of content, and about 10 to 60 minutes of treatment time.

Immediately before use, the hair dye of the present invention is used in admixture with an oxidizing agent which is a second agent. At this time, the mixed oxidizing agent such as hydrogen peroxide, propylene glycol, dimethicone, cetes, decyl oleate, cetearyl alcohol, glyceryl stearate SE and other formulation stabilizers, hair such as hydrolyzed keratin PH adjusters, flavoring agents, solvents, etc., such as a protective agent and phosphoric acid, are included.

The present invention therefore also provides a hair dye kit comprising the hair dye of the present invention as the first agent and the oxidant as the second agent. It is preferable that the kit of the present invention contain the first agent and the second agent in the same amount, respectively.

The hair dye of the present invention has excellent dyeing property, color fastness, hair conditioning, and hair protection effect when dyeing hair.

Hereinafter, preferred preparation examples and examples are provided to aid in understanding the present invention. However, the following examples are provided only for the purpose of easier understanding of the present invention, and the present invention is not limited by the examples.

Preparation Example 1 Preparation of Extract of the Present Invention by Ultrasonic Extraction Method

To the sample mixed with 100g of rhubarb, 100g of sewage and 100g of deficiency (dry weight 1: 1: 1 ratio) purchased from medicinal herb (Myeongcheon Pharmaceutical Co., Ltd., Gyeongdong Market), add 3Kg of distilled water and deposit it for 4 days at 4 ~ 30 ℃, and then 40.5kH After extracting by using a water bath extractor equipped with an ultrasonic oscillator (product of Enitech Korea, Incheon City) for 10 hours with a temperature of 40 ° C. and 400 watts of ultrasonic waves, the extract was filtered using a 1um filter cloth and filtered with a 293mm Edbentech No. 5 filter paper. It was filtered twice with only Glass filter paper. And concentrated using a large rotary decompression concentrator (20L manufactured by BUCHI Co., Ltd.) and freeze-dried using a freeze-dryer (Isinshin Lab) to obtain a dry weight of 55.0g.

Preparation Example 2 to 7 Preparation of Water Extract of the Present Invention with Different Mixing Ratios of Rhubarb, Sewage and Cassiae

The extract of Preparation Examples 2 to 7 was obtained by extracting in the same manner as in Preparation Example 1, except that the sample mixing ratio (Rhubarb: Sewage: Clarifier) of Table 1 was used, and the results are shown in Table 1 below.

Table 1

Preparation Examples 8 to 15 Preparation of Extracts of the Present Invention with Different Extraction Solvents

Except that the solvent of Table 2 was used to extract in the same manner as in Preparation Example 1 to obtain an extract of Preparation Examples 8 to 15, the results are shown in Table 2.

TABLE 2

< Manufacturing example  16> By heat extraction  Preparation of the Mixture of the Invention

100 g of rhubarb, 100 g of sewage and 100 g of clarifier (dry weight 1: 1: 1 ratio) were added to 3 kg of 50% (v / v) hydrous ethanol, and extracted by boiling at 80 ° C. for 8 hours in an extractor equipped with a cooling condenser. The resultant was filtered with 300 mesh filter paper, left at room temperature for 1 week, and the supernatant was collected and filtered twice with Edventech No. 5 filter paper and Whatman GFC 47 mm filter paper. After concentrating at 50 ° C. using a vacuum concentrator, the resultant was dried using a spray dryer (manufactured by BUCHI Co., Ltd.) to obtain a dry weight of 78.3 g.

<Comparison Manufacturing example  1 to 3> Preparation of single component extract by ultrasonic extraction

300 g of the medicinal herbs described in Table 3 below were placed in 3 kg of 50% (v / v) hydrous ethanol and deposited at 4 to 30 ° C. for 7 days, followed by a water bath extractor (Enitech Korea, Incheon City) equipped with a 40.5 kH ultrasonic oscillator. After extraction for 10 hours using a 40 watt temperature and 400 watts of ultrasonic waves, the extract was filtered using a 1um filter cloth and filtered twice with 293mm Edbentech No. 5 filter paper and Whatman Glass filter paper. Then, the resultant was concentrated using a large rotary decompression concentrator (20L, manufactured by BUCHI Co., Ltd.), and the concentrate was lyophilized using a lyophilizer (Ilsin Lab) to obtain the title extract. The results are shown in Table 3.

[Table 3]

<Comparison Manufacturing example  4 to 6> Preparation of single component extract by thermal extraction method

300 g of the medicinal herbs shown in Table 4 were added to 3 kg of 50% (v / v) hydrous ethanol, extracted by boiling at 80 ° C. for 8 hours in an extractor equipped with a cooling condenser, filtered through 300 mesh filter paper, and allowed to stand at room temperature for 1 week. The filtrate was filtered twice with Edbentech 5 filter paper and Whatman GFC 47 mm filter paper. After concentrating at 50 ° C. using a vacuum concentrator, the resultant was dried using a spray dryer (manufactured by BUCHI Co., Ltd.) to prepare an extract of the title. The results are shown in Table 4 below.

[Table 4]

Preparation of Hair Dye Using Rhubarb, Sewage, and Cultivator Mixed Extracts

The following ingredients and contents shown in Table 5, according to the method described below, Examples 1 and 2, Comparative Examples 1 to 6, instead of extracts containing powders of Preparation Example 9, Preparation Example 16, Comparative Preparation Examples 1-6 A hair dye (first agent) corresponding to the control example containing purified water was prepared.

TABLE 5

-Production method of hair dye (1 agent)

Polyquaternium-10 (manufacturer: Toho, product name: Cartinal HC200), tetrasodium ithidium (manufacturer: BASF, product name: EDETA B Powder), sodium methyl cocoyl taurate (Manufacturer: Croda chemical, product name: Adinol CT), potassium hydroxide (manufacturer: Duksan Chemical, product name: Potassium Hydroxide), resorcinol (manufacturer: Lowenstein, product name: Rodol Brown DB), m-aminophenol (manufacturer: Lowenstein, product name: Rodol Black) p-aminophenol (manufacturer: Lowenstein, product name: Rodol 2G Y4), p-phenylenediamine (manufacturer: Lowenstein, product name: Rodol Light Brown) and purified water at 80-85 ℃ After heating and feeding into the manufacturing unit, the emulsifier was operated. Here, Example 1 is a component 9, Example 2 is a component 10, Comparative Example 1 is a component 11, Comparative Example 2 is a component 12, Comparative Example 3 is a component 13, In Comparative Example 4, Component 14 was added, Comparative Example 5 was added Component 15, and in Comparative Example 6, Component 16 was added. After that, warm the mineral oil (manufacturer: Rita, product name: Mineral oil), oles (manufacturer: Henkel, product name: Emulgin O), isopropyl myristate (manufacturer: Cognis, product name: Isopropylmyristate) to 80 ℃ The dissolved solution was added to the production unit to emulsify. After emulsification, setrimonium chloride (manufacturer: Lonza, product name: Barquat CT) was added at 55 ° C while stirring and cooling, and monoethanolamine (manufacturer: Lowenstein, product name: Lowenol T) was added at 45 ° C, followed by room temperature. The hair dye according to Table 5 was prepared by cooling. This composition was commercialized by quality inspection, filling and packaging.

-Production method of oxidizing agent (second agent)

0.05 g of etidronic acid (manufacturer: Sabo, product name: Sequestrante HEDP) and 1.00 g of propylene glycol (manufacturer: Rita, product name: Propylene glycol) were added to 69.00 g of purified water and heated to between 80 and 85 ° C with stirring. The emulsifier was operated after being put into the manufacturing unit. 0.90 mg of dimethicone (manufactured by GE Toshiba silicones, product name: Silsoft ME82), 1 g of cethes (manufacturer: Rita, product name: Propylene glycol), and 3.00 g of cetearyl alcohol (manufacturer: Cognis, product name: Lanette O) was warmed to 80 ° C. and then added to the preparation to emulsify the solution. After emulsification, the solution was slowly stirred and cooled, and a solution containing 0.1 mg of phosphoric acid and 0.20 g of sodium phosphate (manufacturer: Duksan Chemical, product name: Sodium Phospate) was added to 7.65 mg of purified water separately at 55 ° C. Thereafter, 17.00 g of hydrogen peroxide (35%) (manufacturer: Dongyang Steel Chemical, product name: Hydrogen peroxide) was added at 40 ° C., followed by cooling to room temperature to prepare an oxidizing agent. This composition was commercialized by quality inspection, filling and packaging.

Experimental Example 1 Confirmation of Cytotoxicity and Cell Proliferation Effect of the Extract of the Present Invention

Using the dry powder of the extract prepared in Preparation Example 9, Comparative Preparation Examples 1, 2, 3 as a sample, the cell proliferation effect using the cell culture was measured.

1) Experimental method

Cytotoxicity and proliferation experiments were carried out in the following manner. Cultured cells (Fibroblast, 3T3, Korea Cell Line Bank) were dispensed in 96-well microplates with 5,000 cells / well and incubated in a thermostat for 30 minutes, and each sample was 0.01, 0.05, 0.1, 0.5, Incubated for 72 hours by administering at 1.0 (% wt / v). Then, thiazolyl blue (sigma) was administered and further incubated for 4 hours. Discard all of the culture medium, 100uL of reaction DMSO (dimethyl sulfoxide, manufacturer; sigma) was added to each well of the microplate and stirred for 5 minutes, and then absorbance was measured at 570 nm. The control group was co-cultured with 10% Fetal Bovine Serum (FBS) medium as the sample injection amount, and the cell proliferation rate of the control group was 100% and the cell proliferation rate was calculated.

2) Experiment result

Cell proliferation was calculated by Equation 1 below, and the results are shown in Table 6 below.

[Equation 1]

TABLE 6

As shown in Table 6, when the cell proliferation at 100% cell growth conditions was 100%, the extracts of the present invention, each of the single extracts of rhubarb, sewage, and gland, and the mixed extracts thereof, were all non-toxic and excellent cell proliferation. It was confirmed to be effective.

Experimental Example 2 of the Extract of the Present Invention Anthraquinones  Content check

Using the extract of the present invention and the extract of each single component as a sample, the content of anthraquinone, which is a higher dye component, was analyzed by the following method.

1) Analysis method

○ Preparation of Standard Solution: Each 10mg of chrysophanic acid, Aloe emodin, and emodin standards were precisely weighed and placed in a 25mL volumetric flask, marked with methanol, and 10mL was taken and placed in a 50mL volumetric flask.

○ Preparation of test solution: 200 ~ 250mg of sample was weighed and placed in a 50mL volumetric flask, which was labeled with methanol and used as a test solution.

○ Sample: The sample was used as 1 wt / v% solution of extract concentrate produced by each extraction process.

○ HPLC conditions

 System Younglin Equipments Autocro 3000 Column Capcell pak C18 250mm × 4.6mm (Shiseido) Column Temp. 30 ℃ Flow rate 1 mL / min Injection Vol. 20 μL Detection UV 254nm Mobile phase 85:15 = Methanol: 0.5% acetic acid (v / v)

2) Analysis result

TABLE 7 Extract prepared by ultrasonic extraction

[Table 8]

As shown in Table 7 and Table 8, the extract of the present invention contains significantly more anthraquinones, aloe emodin, emodin, and Chrysophanic acid, which are components of higher dyes, than the same amount of single component extracts. In particular, the extract by ultrasonic extraction contained more anthraquinone than the extract by thermal extraction.

Specifically, when comparing the anthraquinone content of the extract prepared according to the ultrasonic extraction method described in Table 7, the extract of the present invention (Preparation Example 9) is about 2 to 9 times more anthraquinone than the extract of a single component It was confirmed that it contains.

In addition, it was confirmed that the extract prepared according to the heat extraction method described in Table 8 also contained about 4 to 37 times more anthraquinone than the extract of a single component prepared by the same method of the same amount.

Therefore, the extract of the present invention is confirmed to have an excellent hair dye effect compared to the extract of each single component.

< Experiment 3> Of the hair dye of the present invention Hair dye effect check

Example 1, Comparative Examples 1 to 3, the hair dye effect of the control was measured by the following experimental method.

Experimental method

After dyeing, white hair (purchased by Yang) was bundled in advance to confirm the drainage by the shampoo. Each bundle was 11 cm in length and weighed 1.2 g. The hair dyes of Examples 1, Comparative Examples 1 to 3 and the control examples were mixed with a common oxidizing agent (second agent), respectively. The mixture was applied to each of three hairs and left at 25 ° C. for 20 minutes.

< Dynamism  Evaluation>

The dyeing property of hairs treated according to the above dyeing method was measured by using a spectrophotometer (model name Minolta CM-3700d, JAPAN) between the dyed hair and the untreated hair. This is excellent.

The results are as shown in Table 9 below and No. 1 in FIG.

TABLE 9

<Hair Drowning ( Fastness Evaluate>

After hair dyeing as described above, washed with SLS (Sodium lauryl sulfate) 5% aqueous solution for 25 seconds and rinsed with running water at 45 ℃ until clear water comes out. Thereafter, after washing for 25 seconds with an aqueous solution of SLS 5%, the process of rinsing 20 times with clear water with flowing water at 45 ° C. was repeated 20 times, and then water was confirmed by comparing with the initial color. The result of dripping is the same as No. 2 in FIG. 1, and the results are shown in Table 10 by scoring the results based on the five-point scale method as follows through visual observation of 10 sensory evaluation specialists. (The values shown in Table 10 represent the average of the values evaluated by ten people.)

TABLE 10

{Based on 5-point scale: 1 = near dyeing, 2 = nearly dyed, 3 = nearly dyed, 4 = nearly dyed, 5 = no dye at all}

<Accumulation of hair Dynamism  Evaluation>

After dyeing hair as described above, wash with SLS 5% aqueous solution for 25 seconds, rinse with clear water with running water at 45 ℃, and dry with a hair dryer, that is, repeat the process from dyeing to drying 5 times After that, the cumulative hair dye effect of the hair was confirmed. Cumulative hair dye result is the same as the number 3 of Figure 1, the results are shown in Table 11 by scoring the results based on the five-point scale method through the visual observation of 10 sensory evaluation specialists. (The values shown in Table 11 represent the average of the values evaluated by ten people.)

Table 11

{5-point scale: 1 = no effect, 2 = inferior, 3 = normal, 4 = excellent, 5 = very good}

As shown in Tables 9 to 11 and FIG. 1, the hair dye of the present invention was superior to the hair dye containing the extract of each single component and the control group, and the hair dye was excellent in the initial hair dye effect and cumulative hair effect. .

< Experimental Example  4> present invention Hair dye  Skin irritation effect

Stimulation alleviation effect using SLS (sodium lauryl sulfate, 1.0%) human patch test with respect to 1.0 wt% by dissolving the dry powder extract prepared in Preparation Example 9, Comparative Preparation Examples 1, 2, 3 in purified water Was measured in the following manner. The control is treated with purified water.

SLS (1.0%) human patch test is a rectangular chamber of patch (Haye's test chambers, USA) sold for patch test with 1.0% SLS solution (w / v in distilled water) inside the upper arm of the subject. (1Cm in length, 1Cm in length) was moistened with 20ul and attached for 24 hours to artificially irritate dermatitis and remove the patch. The patch was removed by attaching 20ul of the sample to the square chamber of the patch at the same position where the patch was removed, and after 24 hours, the patch was removed and the skin reaction of the test site was evaluated after 30 minutes. (Korean Journal of Cosmetic Products, Vol. 30, No. 1, 2004, 63 ~ 71)

The criteria for evaluating skin irritant effects were based on the criteria of the International Contact Dermatitis Research Group (ICDRG) (Wooding et al, 1967; Rietschell, 1982; Fischer & Maibach, 1984; Aberer et al, 1993). ), As follows.

(Criteria)

0 = no redness

1 = erythema

2 = redness and papules

3 = redness, papules and vesicles

4 = severe edema and vesicles

The results are shown in Table 12 and Fig. 2 below. (In Fig. 2, the left photograph is a photograph on which a patch is attached, and the right photograph is a photograph after peeling a patch. Comparative Manufacturing Example 3 was processed, 3 was the processing unit of Comparative Manufacturing Example 1, 4 was the processing unit of Comparative Manufacturing Example 2, and 5 represents the processing unit of Manufacturing Example 9.

TABLE 12

As shown in Table 12 and Figure 2, when the SLS (1.0%) stimulation effect test using the human patch test, Control is a skin irritation and blisters on the surface of the skin as a stimulus to the skin It was very strong. In Comparative Examples 1 and 2, which were rhubarb and sewage extracts, there was a weaker but weaker skin redness than Control, and in Comparative Comparative Example 1, which was a deficiency extract, there was no stimulus. In addition, rhubarb, sewage, the extract of Example 1 was confirmed that no irritation at all. Therefore, it was confirmed that the extract of the present invention has a skin irritation-releasing effect as compared to the extract of each single component.

1 is a photograph showing the results of the initial hair dye evaluation, hair dripping evaluation and cumulative hair dye evaluation experiment of Example 1 and Comparative Examples 1 to 3 containing the extract of the present invention and each single component extract .

Figure 2 is a photograph showing the results of the skin irritation relaxation test of Preparation Example 9 and Comparative Preparation Examples 1 to 3 containing the extract of the present invention and each single component extract.

Claims (8)

Hair dyes containing rhubarb, sewage, and bladder extracts. The hair dye according to claim 1, wherein the mixed extract is extracted by ultrasonic extraction. The mixed extract according to claim 2, wherein the extract is mixed with rhubarb, sewage and smelters at 4 to 30 ° C. in an extraction solvent selected from water, anhydrous or hydrous alcohols having 1 to 4 carbon atoms, butylene glycol, propylene glycol or hydrous glycols thereof. After dipped for 10 days, the hair dye prepared by extracting for 1 to 10 hours by ultrasonic at 20 to 40 ℃ with a bath extractor attached to the ultrasonic oscillator. The hair dye according to claim 1 or 2, wherein the mixed extract is extracted with water, anhydrous or hydrous alcohol having 1 to 4 carbon atoms, butylene glycol, propylene glycol or hydrous glycol thereof. The hair dye according to claim 4, wherein the mixed extract is extracted with 50% (v / v) hydrous ethanol. 5. The hair dye according to claim 4, wherein the mixed dry weight ratio of rhubarb: sewage: gland is 1: 1. The hair dye according to claim 4, wherein the mixed extract contains 0.1 to 20% by weight based on the total dry weight of the hair dye. A hair dye kit according to any one of claims 1 to 3, wherein the hair dye is a first agent and an oxidant is a second agent.

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