WO2023120763A1 - Emulsion-type skin elasticity improving cosmetic material using skin elasticity component material of naturally-derived plant fingerroot, preparation method therefor, and emulsion-type skin elasticity improving cosmetics - Google Patents

Emulsion-type skin elasticity improving cosmetic material using skin elasticity component material of naturally-derived plant fingerroot, preparation method therefor, and emulsion-type skin elasticity improving cosmetics Download PDF

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WO2023120763A1
WO2023120763A1 PCT/KR2021/019521 KR2021019521W WO2023120763A1 WO 2023120763 A1 WO2023120763 A1 WO 2023120763A1 KR 2021019521 W KR2021019521 W KR 2021019521W WO 2023120763 A1 WO2023120763 A1 WO 2023120763A1
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extract
weight
parts
liquid
skin elasticity
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Korean (ko)
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이호규
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이호규
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9794Liliopsida [monocotyledons]
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    • A61K8/34Alcohols
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    • AHUMAN NECESSITIES
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    • A61K8/37Esters of carboxylic acids
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    • A61K8/44Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
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    • A61K8/494Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with more than one nitrogen as the only hetero atom
    • A61K8/4946Imidazoles or their condensed derivatives, e.g. benzimidazoles
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    • A61K8/4993Derivatives containing from 2 to 10 oxyalkylene groups
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    • A61K8/64Proteins; Peptides; Derivatives or degradation products thereof
    • A61K8/65Collagen; Gelatin; Keratin; Derivatives or degradation products thereof
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    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89Polysiloxanes
    • A61K8/891Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
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    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
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    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
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    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/98Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
    • AHUMAN NECESSITIES
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    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/98Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
    • A61K8/987Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of species other than mammals or birds
    • AHUMAN NECESSITIES
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    • A61K8/99Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from microorganisms other than algae or fungi, e.g. protozoa or bacteria
    • AHUMAN NECESSITIES
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    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
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    • A61Q19/08Anti-ageing preparations
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    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18
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    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/85Products or compounds obtained by fermentation, e.g. yoghurt, beer, wine

Definitions

  • the present invention relates to an emulsion-type skin elasticity cosmetic with excellent skin whitening and skin wrinkle improvement effects using a finger root rhizome extract from which toxicity has been removed and various natural plant-derived extracts, a method for preparing the same, and an emulsion formulation cosmetic using the same.
  • multi-functional cosmetics having two or more functionalities in one product have a much higher production value and market growth rate than single-functional cosmetics.
  • most of the currently marketed cosmetics do not sufficiently satisfy these demands.
  • Fingerroot (scientific name: Boesenbergia pandurata) is a plant of the ginger family native to Southeast Asia. It is used not only in Asian traditional dishes such as pickles, curry, and drinks, but also as a tonic for childbirth, stomach pain, diarrhea, flatulence, indigestion, ulcer treatment, It has been used for various purposes such as leukocyte prophylaxis and cost supplements.
  • Fingerroot contains flavonoids that inhibit the infection of Helicobacter pylori bacteria, including indigestion and gastritis, and pinostrobin, which has a cytoprotective effect, increases gastric mucus and reduces the area of gastric ulcer formation. It is also effective in treating peptic ulcer.
  • it contains components such as flavonoid derivatives, pinocembrin, pinostrobin, ilpinetin, tadamonin, pandurata, and panduratin A that can inhibit the growth of cancer cells. It is known that the component inhibits the growth of cancer cells, and the panduratin A component has a preventive effect on prostate cancer and colon cancer.
  • panduratin a functional raw material extracted from the root of ginger and plants, especially finger root, is a light yellowish brown powder extracted from the root of finger root. and received a grade 2 physiological activity.
  • Panduratin is a light yellowish brown powder extracted from the root of a plant called finger root. It is known to contribute to reducing body fat by activating 'AMPK (AMP-activated protein kinase)', a sensor protein for maintenance and energy homeostasis in the body.
  • 'AMPK AMP-activated protein kinase
  • panduratin one of the finger root extract components, has strong toxicity, so caution is required in use, and there is a limit to its application as a functional cosmetic using it.
  • the present inventors have developed a method for removing the toxicity of panduratin, a finger root extract that is effective in maintaining skin homeostasis, although it has a slight toxicity disadvantage, as the market demand for multi-functional cosmetics using natural ingredients increases. , By applying the beneficial ingredients of the finger root rhizome extract as a cosmetic using the finger root rhizome extract from which toxicity has been removed as described above, and by applying the mixture with other natural plant-derived extracts, excellent skin whitening, wrinkles, moisturizing, etc. It is an object of the present invention to provide a highly functional cosmetic that can improve skin resistance and skin condition, a manufacturing method thereof, and cosmetics using the same.
  • the emulsion-type cosmetic composition for improving skin elasticity of the present invention includes a first liquid, a second liquid, a third liquid and a fourth liquid, wherein the first liquid contains a viscosity modifier and purified water, ,
  • the second liquid is a conditioning agent containing at least one selected from glycereth-26, allantoin, hydrolyzed collagen, and adenosine skin; moisturizers including glycerin and butylene glycol; preservatives including 1,2-hexanediol; and a cross-linking agent containing sodium hyaluronate;
  • the third solution is a skin conditioning agent containing at least one selected from sunflower seed oil, dimethicone, cetylethylhexanoate, and glyceryl stearate; surfactants including PEG-100 stearate; humectants including Caprylic/Capric Triglyceride;
  • the present invention relates to a method for preparing the emulsion-type cosmetic for improving skin elasticity, comprising the steps of preparing a first liquid by adding purified water and a viscosity modifier to a reactor and stirring; a second step of injecting the second liquid into the reactor in which the first liquid was prepared and performing stirring; Step 3 of stirring after adding the third liquid to the reactor in which Step 2 was performed; 4th step of adding a pH adjusting agent to the reactor in which step 3 was performed and then stirring; Step 5 of performing agitation after injecting the fourth liquid into the reactor in which Step 4 was performed; Step 6 of filtering and defoaming the mixed solution after step 5; It can be prepared by performing a process including; and step 7 of aging the mixed solution after step 6.
  • the present invention relates to a cosmetic for improving skin elasticity using the cosmetic prepared by the method described above, and can provide a cosmetic in an emulsion formulation.
  • the cosmetic composition of the present invention has excellent skin whitening and skin wrinkle improvement effects while having no skin trouble and excellent moisturizing properties, and thus, it is possible to provide a cosmetic product derived from a highly functional natural material.
  • Figure 2 is the cell protection measurement results of the finger root rhizome extract for each solvent conducted in Experimental Example 2.
  • Figure 3 is the result of measuring the cell protection effect of the finger root rhizome extract for each solvent conducted in Experimental Example 2.
  • Figure 4 is a result of measuring the cytotoxicity of each fraction of the finger root rhizome ethanol extract conducted in Experimental Example 3.
  • Figure 5 is a result of measuring the cell protection effect for each fraction of the finger root rhizome ethanol extract conducted in Experimental Example 4.
  • 6 and 7 are the results of measuring the cytotoxicity and cell protection effect of the water fraction of the finger root rhizome ethanol extract performed in Experimental Example 4.
  • Skin improvement used in the detailed description of the present invention means any action or effect that inhibits or delays skin damage, disease symptoms, improves disease symptoms, or improves the health condition of the skin.
  • extract means an active ingredient isolated from a natural product, that is, a substance showing a desired activity.
  • the extract may be obtained by an extraction process using water, an organic solvent, or a mixed solvent thereof, and includes all forms formulated using the extract or its dry powder.
  • the extract includes fractionated extracts subjected to the extraction process.
  • the cosmetic composition of the present invention includes 18 to 22 parts by weight of the second solution, 8 to 12 parts by weight of the third solution, and 10 to 15 parts by weight of the fourth solution, based on 100 parts by weight of the first solution, preferably 100 parts by weight of the first solution.
  • parts by weight 18.5 to 21.0 parts by weight of the second solution, 9.0 to 11.5 parts by weight of the third solution and 10.5 to 14.0 parts by weight of the fourth solution, more preferably preferably 100 parts by weight of the first solution, 18.5 to 20.0 parts by weight of the second solution, 10.0 to 11.5 parts by weight of the third solution, and 11.0 to 13.5 parts by weight of the fourth solution.
  • the first liquid serves as a solvent for cosmetics, and may include 0.20 to 0.40% by weight of a viscosity modifier and the remaining amount of purified water, preferably 0.22 to 0.35% by weight of the viscosity modifier and the remaining amount of purified water.
  • a viscosity modifier exceeds 0.40% by weight, the initial viscosity is too high, so that the components of the second to fourth liquids are not properly dissolved in the first liquid, and miscibility of the composition may be poor.
  • viscosity modifier a general viscosity modifier used in the cosmetics industry may be used, and a preferred example is acrylate/(C 10-30 alkyl)acrylate cross polymer (acrylate/(/(C 10-30 alklyl)acrylate cross polymer) can be used.
  • the second liquid contains 18.5 to 21.0% by weight of skin conditioning agent, 10 to 12.0% by weight of crosslinking agent, 13.0 to 16.0% by weight of whitening agent, 10 to 15.0% by weight of preservative, and the remainder of the total weight of the second liquid.
  • moisturizers preferably 18.8 to 20.5% by weight of skin conditioning agent, 10.2 to 11.7% by weight of crosslinking agent, 13.0 to 15.5% by weight of whitening agent, 12.0 to 15.0% by weight of preservative, and the remainder of the total weight of the second solution of the moisturizer, more preferably 18.8 to 20.0% by weight of the skin conditioning agent, 10.5 to 11.5% by weight of the crosslinking agent, 13.0 to 15.0% by weight of the whitening agent, 13.0 to 15.0% by weight of the preservative and the remaining remaining amount of the moisturizer among the total weight of the second solution can include
  • the skin conditioning agent may include at least one selected from Glycereth-26, Allantoin, Hydrolyzed Collagen, and Adenosine, Preferably, glycereth-26, allantoin, hydrolyzed collagen and adenosine are mixed in a weight ratio of 1:0.1 to 0.4:0.7 to 1.0:0.2 to 0.5, more preferably 1:0.2 to 0.3:0.7 to 0.9:0.2 to 0.4 weight ratio.
  • the crosslinking agent may include sodium hyaluronate, and it is preferable to use a material that does not cause skin trouble as the preservative.
  • a material that does not cause skin trouble for example, 1,2-hexane Diol (1,2-hexane diol) may be included.
  • niacinamide may be used as the whitening agent among the components of the second liquid
  • the moisturizer may include at least one selected from glycerine and butylene glycol.
  • the third liquid contains 15.0 to 20.0% by weight of an emulsifier, 5.0 to 8.0% by weight of an emulsion stabilizer, 10.0 to 12.0% by weight of a surfactant, 5.0 to 8.0% by weight of a humectant, and the remaining balance of the total weight of the third liquid.
  • It may include a skin conditioning agent, preferably 16.5 to 20.0% by weight of an emulsifier, 5.5 to 7.5% by weight of an emulsion stabilizer, 10.5 to 12.0% by weight of a surfactant, 5.2 to 7.5% by weight of a humectant, and the remainder of the total weight of the third solution. of skin conditioning agents.
  • the emulsifier serves to increase the miscibility between cosmetic compositions and the emulsification of the composition, and includes polysorbate 60, stearic acid, and sorbitan sesquioleate (Sorbitan sesquioleate), preferably polysorbate 60, stearic acid and sorbitan sesquioleate in a weight ratio of 1: 0.5 to 1.0: 0.5 to 1.0, more preferably polysorbate 60, stearic acid and sorbitan sesquioleate are mixed and used in a weight ratio of 1: 0.8 to 1.0: 0.5 to 0.9.
  • polysorbate 60, stearic acid, and sorbitan sesquioleate Sorbitan sesquioleate
  • emulsion stabilizers used in the art may be used as the emulsion stabilizer, and preferably, cetearyl alcohol is used.
  • PEG-(40-100) stearate preferably PEG-100 stearate, as the surfactant among the components of the third liquid.
  • the humectant among the components of the third liquid is caprylic acid, caprylic acid, and caprylic / capric triglyceride, which is a mixed triester of capric acid and glycerin. Triglycerides) are recommended.
  • the skin conditioning agent among the components of the third liquid may include at least two selected from sunflower seed oil, dimethicone, cetyl ethyl hexanoate, and glyceryl stearate.
  • sunflower seed oil, dimethicone, cetylethylhexanoate, and glyceryl stearate may be included in a weight ratio of 1:0.8 to 1.0:0.5 to 0.8:0.4 to 0.8.
  • the fourth liquid contains 5.0 to 8.0% by weight of the lactobacillus fermentation lysate, 1.0 to 2.5% by weight of the collagen synthesis promoter, 0.1 to 0.8% by weight of the fragrance, and the remaining balance of the functional extract of the total weight of the fourth liquid. 5.5 to 7.0% by weight of the lactobacillus fermented lysate, 1.2 to 2.3% by weight of the collagen synthesis promoter, 0.1 to 0.8% by weight of the fragrance, and the remaining functional extract of the total weight of the fourth solution. there is.
  • the lactobacillus fermented lysate among the components of the fourth liquid serves to promote the aging of the functional extract, and if the content thereof is less than 5.0% by weight, the functional extract may not mature well and cause skin trouble. Excessive use is uneconomical.
  • the collagen synthesis accelerator is absorbed into the skin and serves to promote collagen synthesis in the skin, and RH-Oligopeptide-1 may be used.
  • the content of the collagen synthesis promoter is less than 1.0% by weight, the amount used is too small and the effect of promoting collagen synthesis in the skin is insufficient, so the effect of improving skin wrinkles may be insufficient. It is recommended to use it within the above range because it may interfere with the
  • fragrance used in the art may be used as long as they do not cause skin trouble or impair the function of the cosmetic of the present invention.
  • the functional extract includes a pearl extract and a natural plant complex extract, the pearl extract and the natural plant complex extract in a weight ratio of 1: 3.5 to 5.0, preferably the pearl extract and the natural plant complex extract in a weight ratio of 1: 3.8 to 4.8 can be included with
  • the pearl of the pearl extract refers to a bead-shaped secretion mass formed in the body of shellfish. After pulverizing 100 g of pearls, 2 to 4 L of 60 to 80 vol% ethanol aqueous solution is used as a solvent for 10 to 16 hours. 1st step of reflux extraction with moderate heating; A second step of cooling the reflux extract and then filtering with a filter paper to obtain a filtrate; It can be prepared by carrying out a process including three steps of concentrating the obtained filtrate by vacuum concentration and vacuum drying to obtain pearl dry powder.
  • the natural plant complex extract is finger root rhizome extract (Boesenbergia Pandurata Rhizome Extract), centella extract, vitamin tree extract (Hippophae Rhamnoides Extract), green tea extract (Camellia Sinensis Leaf Extract), Matricaria extract (Chamomilla Recutita Extract) , Opuntia Humifusa Extract, Morus Alba Leaf Extract, Crataegus Pinnatifida Fruit Extract, Mentha Piperita (Peppermint) Extract, Hibiscus Sabdariffa Flower Extract ), rosemary extract (Rosmarinus Officinalis (Rosemary) Extract), quince extract (Chaenomeles Sinensis Fruit Extract) and red chokeberry extract (Aronia Arbutifolia Extract), preferably with respect to 100 parts by weight of finger root rhizome extract, Centella asiatica Extract 15 ⁇ 30 parts by weight, vitamin tree extract 0.2 ⁇ 2.0 parts by weight, green tea extract 0.2 ⁇ 2.0 parts by weight, Matricaria
  • the finger root rhizome extract is an extract from which toxicity has been removed, and it is recommended to use a finger root rhizome ethanol extract or a water fraction of the finger root rhizome ethanol extract, preferably a finger root rhizome ethanol extract from which toxicity has been removed. It is preferable to use the water fraction, which can be prepared through the following method.
  • the water fraction of the finger root rhizome ethanol extract is obtained by mixing the finger root rhizome powder with an aqueous ethanol solution, stirring, and performing an extraction process at 15 to 30 ° C for 18 to 24 hours to obtain an ethanol extract.
  • DMSO dimethyl sulfoxide
  • ethyl acetate Ether Acetate
  • the cosmetic composition of the present invention includes a first step of preparing a first liquid by adding purified water and a viscosity modifier to a reactor and stirring; a second step of injecting the second liquid into the reactor in which the first liquid was prepared and performing stirring; Step 3 of stirring after adding the third liquid to the reactor in which Step 2 was performed; 4th step of adding a pH adjusting agent to the reactor in which step 3 was performed and then stirring; Step 5 of performing agitation after injecting the fourth liquid into the reactor in which Step 4 was performed; Step 6 of filtering and defoaming the mixed solution after step 5; It can be prepared by performing a process including; and step 7 of aging the mixed solution after step 6.
  • the stirring in the first step is performed at 60 to 80 ° C and a stirring speed of 2500 to 3500 rpm, preferably for 40 to 80 minutes, preferably for 50 to 70 minutes, under the conditions of 65 to 75 ° C and a stirring speed of 2800 to 3200 rpm. good to do
  • the temperature during stirring is less than 60 ° C or the stirring speed is less than 2500 rpm, the viscosity modifier may not be completely dissolved in the purified water, so there may be a problem of lengthening the stirring time, and it is uneconomical when the temperature exceeds 80 ° C during stirring.
  • the stirring speed exceeds 3500 rpm, bubbles may be generated, so it is good to perform stirring under the above conditions.
  • the stirring in the second step is performed at 60 to 80 ° C and a stirring speed of 2000 to 3000 rpm, preferably for 40 to 80 minutes, preferably for 50 to 70 minutes, under the conditions of 65 to 75 ° C and a stirring speed of 2200 to 2700 rpm. good to do
  • the stirring in the third step is performed at 70 to 80 ° C and a stirring speed of 2000 to 3000 rpm, preferably at 65 to 75 ° C and a stirring speed of 2200 to 2700 rpm for 30 to 60 minutes, preferably 30 to 60 ° C. It is better to do it for minutes.
  • step 4 is a process of performing pH adjustment before mixing the fourth liquid in step 5, and after lowering the temperature in the reactor in which step 3 was performed, a pH adjuster is introduced and stirring is performed. At this time, stirring is carried out for 10 to 30 minutes, preferably for 20 to 30 minutes under the conditions of 35 ⁇ 45 °C and stirring speed 2000 ⁇ 3000 rpm, preferably under the conditions of 35 ⁇ 40 °C and stirring speed 2200 ⁇ 2700 rpm It is good.
  • arginine may be used as a preferred example of the pH adjusting agent, and it is appropriate to add 0.10 to 0.50 parts by weight, preferably 0.20 to 0.40 parts by weight, based on 100 parts by weight of the first solution.
  • the stirring in step 5 is performed at 35 to 45 ° C and a stirring speed of 2000 to 3000 rpm, preferably at 35 to 40 ° C and a stirring speed of 2200 to 2700 rpm, for 10 to 30 minutes, preferably for 20 to 30 minutes. It is good to do it while
  • the cosmetic composition for improving skin elasticity of the present invention prepared by the composition and method described above can be prepared as a cosmetic of any formulation conventionally manufactured in the art, and is commonly used in the field of dermatology by containing a dermatologically acceptable medium or base. It can be prepared in the form of an adjuvant that can be applied topically or systemically.
  • the emulsion-type cosmetic may have a viscosity of 45,000 to 51,000 cP and a pH of 6.0 to 7.0.
  • Finger root rhizome extracts were aliquoted at the same concentration and prepared as HLPC samples.
  • panduratin A content in the extract was analyzed by comparing the HPLC chromatogram of the index component panduratin A of the finger root extract and the extract for each solvent.
  • the chemical structure of panduratin A is shown in Formula 1 below.
  • panduratin A was dissolved in methanol and diluted in stages to prepare samples for quantitative writing.
  • the HPLC measurement conditions are shown in Table 1 below, and the validation of the analysis method is shown in Table 2 below.
  • the concentration of the standard solution for which linearity is proven is 1 mg/kg, 5 mg/kg, and 10 mg/kg in consideration of the accuracy test concentration and precision test concentration. , and the concentration range was set at 50 mg/kg. accuracy (recovery rate) After adding a certain amount by concentration using Panduratin A standard stock solution (1,000 mg/kg) to MeOH without Panduratin A, MeOH was added and dispersed by ultrasonic wave for 15 minutes. After filtering (0.20 ⁇ l syringe filter), it was used as the test solution. After repeating the measurement three times independently for each concentration, the recovery rate was confirmed and evaluated.
  • panduratin A was detected at 29.3 minutes in all extraction solvents, and ethyl acetate (4.042), ethanol (4.030), and methanol (3.663) contained high concentrations of panduratin A in that order. I was able to confirm that Experimental Example 1: Toxicity test of finger root rhizome extract
  • a toxicity test was performed on each of the nucleic acid extract (H), dichloroform extract (Ch), ethyl acetate extract (EA), ethanol extract (Et), methanol extract (Me), and water extract prepared in Preparation Example 1, The results are shown in A to C of FIG. 1 .
  • AsA used in the test is labeled with ascorbic acid (Vit.C) as a positive control.
  • a and B of Figure 3 are graphs showing the results of experiments with concentrations of 0.5 and 1 ⁇ g / ml in order to prepare for the cell protection effect of each solvent finger root rhizome extract against UVB stimulation.
  • the effect was the best in the ethanol extract, and the protective effect was significantly increased at 0.5 ⁇ g / ml than at 1 ⁇ g / ml, and the finger root root The cell protection effect of the stem ethanol extract against UVB was the highest.
  • Collagenase production (Pro-collagen synthesis) inhibitory efficacy test was performed at 0.5 ⁇ g / ml, 1.0 ⁇ g / ml, and 2.5 ⁇ g / ml of finger root rhizome ethanol extract, and the results are shown in Table 4 below.
  • the positive control group was TFG-beta1 100ng/ml, and the control group was an ethane water extract untreated group.
  • finger root rhizome powder 100 g was added to 1 L of ethanol and extracted at 25° C. for 24 hours using a shaker. Finger root rhizome ethanol extract was obtained by filtering using a filter (Whatman No.2 filter paper). 100 ml of 1 L of finger root rhizome ethanol extract was taken and 200 ml of distilled water was added.
  • a mixture of finger root rhizome ethanol extract and distilled water was concentrated in vacuo to remove all ethanol, and then transferred to a separatory funnel. A total of 2 L of dichloroform was added thereto, sufficiently shaken, and then separated, and the lower layer was collected and concentrated.
  • Cytotoxicity was performed on the ethanol-extracted fraction obtained in Preparation Example 2, and cell culture and cytotoxicity experiments were as follows.
  • Hs68 cells a human skin fibroblast cell line used in the cytotoxicity test, were purchased from ATCC (American Type Culture Collection, Manassas, VA, USA).
  • DMEM Dulbecco's Modified Eagle's Medium
  • FBS penicillin
  • streptomycin 50 ⁇ g/ml
  • 37°C 5% carbon dioxide
  • CO2 carbon dioxide
  • 95% humid air humid air
  • Hs68 cells were dispensed in a 96-well plate at a concentration of 1.0 ⁇ 10 4 cells/well, and after culture for 24 hours, the medium was replaced with a medium containing the sample and not containing FBS. After 24 hours of sample treatment, 20uL of MTT (1 mg/ml) solution was added to each well and incubated for 2 hours. Finally, the supernatant was removed, and blue formazan crystals generated from viable cells were solubilized with DMSO, and absorbance at 550 nm was measured using a Microplate reader (BioTek, Inc., Winooski, VT, USA). During sample processing, the sample was diluted with medium so that the final concentration of DMSO was less than 0.1% (v/v).
  • hs68 cells were treated with 0.1, 0.5, 1, or 5 ⁇ g/ml.
  • concentration as shown in A and B of FIG. 4, all of the fractions except the water fraction showed cytotoxicity at 5 ⁇ g/ml.
  • Hs68 cells were dispensed in a 96-well plate at a concentration of 1.0 ⁇ 10 4 cells/well and cultured for 24 hours, and then the samples were diluted with FBS-free medium in each well, treated, and cultured for 24 hours.
  • UVB (30mJ/cm 2 ) was irradiated using a UVB lamp (Sankyo Denki Lamps, GL20SE, Marine, Japan), and ultraviolet intensity was monitored using a UV LIGHT METER (LT Lutron, UV-340A, Taiwan). . All UVB irradiation was performed after thinly applying PBS to the cells attached to the 96-well plate. After irradiation, the samples were diluted in FBS-free medium and treated with cells for 24 hours. The control group was run under the same conditions without UVB irradiation.
  • the water fraction of the finger root rhizome ethanol extract was selected and the cytotoxicity and cell protection effect against UVB at each concentration (1, 5, 25, 50 ⁇ g/ml) were measured, and the results are shown in FIG. 6 .
  • cytotoxicity test results of FIG. 6A in the case of cytotoxicity, cytotoxicity was not shown up to 25 ⁇ g / ml, but at 50 ⁇ g / ml, the cell viability was reduced to 86%, which was determined to indicate toxicity.
  • the cell protection effect as shown in B of FIG. 6, which is the result of the cell protection experiment, the cell protection effect was shown at 5 ⁇ g/ml and 25 ⁇ g/ml.
  • the cell viability tended to decrease slightly at 25 ⁇ g/ml of the water fraction of the finger root rhizome ethanol extract. Therefore, the highest concentration was set at 20 ⁇ g/ml in order to obtain an ideal result that increases in a concentration-dependent manner during sample treatment did
  • UVB irradiation reduces cell collagen production. Therefore, the effect of the water fraction of the fingerroot extract on the amount of intracellular collagen was measured.
  • the experimental method is as follows.
  • UVB decreased the amount of intracellular collagen, and the collagen level increased in a concentration-dependent manner as the concentration increased when the water fraction was treated from 1 ⁇ g/ml to 20 ⁇ g/ml.
  • UVB irradiation promotes the decomposition of collagen by increasing the production of MMP-1 (Matrix MetalloProtease), an enzyme that decomposes type 1 collagen, which is the most abundant protein in the skin. Therefore, the effect of the water fraction of the fingerroot extract on the production of MMP-1 was evaluated by the method described above, and the results are shown in FIG. 8B.
  • MMP-1 Microx MetalloProtease
  • the production of MMP-1 increased upon UVB irradiation, and the production of MMP-1 decreased as the concentration increased from 1 ⁇ g/ml to 20 ⁇ g/ml when the water fraction was treated.
  • MMP-3 promotes collagen degradation by activating MMP-1
  • the amount of MMP-3 produced was measured in the same manner as in MMP-1, and the experimental results are shown in FIG. 8C.
  • the production of MMP-3 increased upon UVB irradiation, and the production of MMP-3 decreased as the concentration increased from 1 ⁇ g/ml to 20 ⁇ g/ml when the water fraction was treated.
  • UVB irradiation promotes the generation of intracellular reactive oxygen species (ROS).
  • ROS reactive oxygen species
  • the increase in these abnormal reactive oxygen species induces oxidative stress and induces MMPs in dermal fibroblasts to promote skin aging. Therefore, the effect of the water fraction of the finger root rhizome extract on ROS production was evaluated.
  • the experimental method is as follows.
  • ROS reactive oxygen species
  • ROS 9 shows a graph of fluorescence intensity measurement for measuring ROS generation of reactive oxygen species (ROS) according to concentrations of 1 to 20 ⁇ g/ml of the water fraction of the finger root ethanol extract.
  • UVB irradiation increased intracellular ROS generation, and decreased ROS generation in a concentration-dependent manner when the water fraction was treated.
  • Example 1 Preparation of skin elasticity improving cosmetics (cosmetics) of emulsion formulation
  • Purified water and acrylate/C 10-30 alkyl acrylate crosspolymer (Carbopol ETD-2020) 0.28% by weight and 99.72% by weight of purified water were added, and then stirred at 3,000 rpm for 60 minutes at 70 ° C to prepare a first solution.
  • a second liquid containing a skin conditioning agent, a moisturizer, a preservative, and a crosslinking agent 19.0 parts by weight of the second liquid based on 100 parts by weight of the first liquid was introduced into the reactor where the first liquid was prepared, and then 2,500 rpm at 70 ° C. Stirring was performed for 60 minutes at speed. At this time, the composition of the second liquid is shown in Table 5 below.
  • Butylene Glycol 14.7 whitening agent Niacinamide 14.7 preservative 1,2-Hexanediol 14.7 cross-linking agent sodium hyaluronate
  • skin conditioning agent glycereth-26 9.5 allantoin 2.2 hydrolyzed collagen 7.2 adenosine 0.3 total 100
  • the pearl extract was pulverized with 100 g of pearls, extracted under reflux by heating for 12 hours using 3 L of 70% ethanol aqueous solution as a solvent, cooled, and filtered with a filter paper having a 1.2 ⁇ m permeation size to obtain a filtrate, The obtained filtrate was concentrated under reduced pressure and dried under reduced pressure, and then dried and pulverized to be used.
  • the finger root rhizome extract is the water fraction of the ethanol extract, and is prepared by the following process. The water fraction of the stem ethanol extract was used.
  • finger root rhizome powder 100 g was added to 1 L of ethanol and extracted at 25° C. for 24 hours using a shaker.
  • the finger root rhizome ethanol extract was obtained by filtering using a filter (Whatman No.2 filter paper). 100 ml of 1 L of finger root rhizome ethanol extract was taken and 200 ml of distilled water was added.
  • the mixture of the finger root rhizome ethanol extract and distilled water was concentrated in a vacuum to remove all ethanol, and then transferred to a separatory funnel. A total of 2 L of dichloroform was added thereto, sufficiently shaken, and then separated, and the lower layer was collected and concentrated.
  • composition ratio of the natural plant composite extract is shown in Table 8 below, and other plant extracts other than the finger root rhizome extract were purchased commercially.
  • the prepared cosmetic was an emulsion formulation, and had a viscosity of 47,000 to 49,000 cP and a pH of about 6.4 to 6.6 at 25°C. Comparative Example 1: Preparation of skin elasticity cosmetics
  • Korean Patent No. 10-2288066 discloses a first mixture (emulsion agent, emulsifier, flavoring agent), a second mixture (purified water, adenosine, niacinamide) and a third mixture (natural plant-derived extract, natural plant-derived fermented filtrate, Conditioning agent, stabilizer, preservative, sequestering agent) were prepared, respectively, and skin elasticity cosmetics were prepared through the following process.
  • a first mixture emulsion agent, emulsifier, flavoring agent
  • a second mixture purified water, adenosine, niacinamide
  • a third mixture natural plant-derived extract, natural plant-derived fermented filtrate, Conditioning agent, stabilizer, preservative, sequestering agent
  • the conditioning agents of the third mixture include Acetyl Hexapeptide-8, Copper Tripeptide-1, sh-Oligopeptide-10, Butylene Gly It was prepared by mixing Butylene Glycol, Propylene Glycol, Hyaluronic Acid, and Methyl Perfluoroisobutyl Ether in equal weight ratios. .
  • the second mixture was dispersed, dissolved, and mixed (step 21).
  • the third mixture was dispersed, dissolved, and mixed.
  • the first mixture mixed in step 11, the second mixture mixed in step 21, and the third mixture mixed in step 31 were each transferred to an emulsifier and mixed and stirred in an emulsifier or the like in step 32.
  • the mixed and stirred mixture in step 32 was filtered (step 33), vacuum degassed (step 34), and then transferred to a storage tank to perform storage and aging (step 35) to prepare skin elasticity cosmetics.
  • the prepared cosmetic was put into a container and stored.
  • the variable R3z (Base roughness depth) is expressed as the arithmetic average of five single roughness depths from R3z1 to R3z5.
  • the single roughness depth means the vertical distance between the third highest cross section peak and the third deepest curve at a single evaluation distance (Ir) of the roughness cross section.
  • Ir single evaluation distance
  • Equation 1 A is a measured value after using the product, and B is a measured value before using the product.
  • the skin elasticity improvement effect was measured before and after using the cosmetics of Example 1 and Comparative Example 1, and the test site was measured three times using a Cutometer (Courage and Khazaka Electronic, Germany), and the average value was obtained using the three values.
  • the measurement site was measured at a point 3 cm away from the outer corner of the eye. Cutometer applies negative pressure to the skin surface and measures the degree to which the skin is sucked into the probe using an optical system that can pass through the skin.
  • the light used at this time is infrared, and the degree of elasticity is measured by the ratio of the intensity of light that is reduced while passing through the skin and the intensity of light that does not pass through the skin.
  • R2 (A.U.) was selected as a cutometer measurement variable for elasticity.
  • Variable R2 represents the ratio of the total contraction length of the skin at the maximum value at which the skin can be stretched, and represents the overall elasticity, which is the re-deformation force of the skin. The closer the value of this variable is to 1, the more elastic it is.
  • the skin elasticity improvement rate was calculated according to Equation 1 below. Measurements were taken before use (0 weeks), after 2 weeks and after 4 weeks of use.
  • Equation 2 A is the R2 measured value after product use, and B is the R2 measured value before product use.
  • the whitening activity effect of the cosmetic of Example 1 was evaluated through the ability to inhibit tyrosinase enzyme activity.
  • 1mL of 0.1M sodium phosphate buffer (pH 6.9), various concentrations of the cosmetic sample of Example 1, and 30 ⁇ l of mushroom tyrosinase (1 KU/mL) were mixed and reacted at 37°C for 10 minutes, followed by 1.5mM L-tyrosine 30 as a substrate.
  • ul was mixed and reacted at 25 ° C. for 2 minutes, and DOPA chrome generated in the reaction solution was measured at 475 nm, and the results are shown in Table 12.
  • the absorbance of the control group was referred to as Ab control
  • the absorbance of the sample was referred to as Ab sample , and was calculated according to Equation 3 below.
  • Tyrosinase enzyme activity inhibition rate (%) (1-Ab sample ) / Ab control *100%
  • the cosmetic of the present invention has various effects such as skin whitening and skin wrinkle improvement, and it was confirmed that the cosmetic of the present invention can provide cosmetics for various skin cosmetics. .

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Abstract

The present invention relates to a cosmetic material using a natural material-derived extract, and more specifically to: a cosmetic material using a natural plant extract such as a fingerroot root and stem extract, and having excellent skin whitening and skin wrinkle reducing effects; a preparation method therefor; and cosmetics using same.

Description

자연유래 식물 핑거루트의 피부탄력 성분 소재를 활용한 에멀젼 제형의 피부탄력 개선 화장료, 이의 제조방법 및 에멀젼 제형 피부탄력 개선 화장품Emulsion-formulated skin elasticity-improving cosmetic using natural plant finger root's skin-elasticity ingredient, manufacturing method thereof, and emulsion-formulated skin elasticity-improving cosmetics
본 발명은 독성이 제거된 핑거루트뿌리줄기 추출물과 다양한 천연식물 유래추출물을 이용한 피부 미백 및 피부 주름 개선 효과가 우수한 에멀젼 재형의 피부탄력 화장료, 이를 제조하는 방법 및 이를 이용한 에멀젼 제형 화장품에 관한 것이다.The present invention relates to an emulsion-type skin elasticity cosmetic with excellent skin whitening and skin wrinkle improvement effects using a finger root rhizome extract from which toxicity has been removed and various natural plant-derived extracts, a method for preparing the same, and an emulsion formulation cosmetic using the same.
최근, 피부과학을 통한 생리적 메커니즘에 대한 연구 및 효능이 한 계 높은 새로운 소재로서 천연물로부터 유효성분을 추출 정제하는 연구로부터, 단순히 피부보호 차원에서 머물던 화장품이 그 효능에 있어서 피부개선의 범주까지 확대된 기능성 화장품에 대한 수요가 급증하고 있다.Recently, from research on physiological mechanisms through dermatology and research on extracting and refining active ingredients from natural products as new materials with high efficacy, cosmetics that have simply stayed in terms of skin protection have expanded to the category of skin improvement in terms of their efficacy. Demand for functional cosmetics is rapidly increasing.
특히, 기능성 화장품 중에서 한 제품에 두 가지 이상의 기능성을 갖는 복합기능성 화장품(예로서, 주름개선기능과 미백기능을 동시에 포함)에 대한 생산액 및 시장 성장률이 단일기능성 화장품에 비해 월등히 높게 나타나고 있다. 그러나 이러한 요구를 현재 시판되고 있는 대부분의 화장품들이 충분히 만족시키지 못하고 있는 실정이다.In particular, among functional cosmetics, multi-functional cosmetics having two or more functionalities in one product (eg, wrinkle-improving function and whitening function at the same time) have a much higher production value and market growth rate than single-functional cosmetics. However, most of the currently marketed cosmetics do not sufficiently satisfy these demands.
핑거루트(fingerroot, 학명: Boesenbergia pandurata)는 동남아시아에서 자생하는 생강과의 식물로 피클, 카레, 음료 등 아시아 전통요리뿐만 아니라, 출산을 위한 강장제, 위통, 설사, 헛배부름, 소화불량, 궤양치료제, 백혈구예방제, 비용보조제 등 다양한 용도로 사용되어 왔다.Fingerroot (scientific name: Boesenbergia pandurata) is a plant of the ginger family native to Southeast Asia. It is used not only in Asian traditional dishes such as pickles, curry, and drinks, but also as a tonic for childbirth, stomach pain, diarrhea, flatulence, indigestion, ulcer treatment, It has been used for various purposes such as leukocyte prophylaxis and cost supplements.
핑거루트는 소화불량, 위염을 비롯한 헬리코박터 파일로리 박테리아의 감염을 억제하는 플로보노이드 성분을 함유하고 있으며, 세포보호효과가 있는 피노스트로빈 성분이 함유되어 있어 위 점액을 증가시켜 위궤양 형성면적을 감소시킴으로써 소화성궤양 치료에도 효과적이다. 그 외에도 암세포의 성장을 억제할 수 있는 플라보노이드 유도체, 피노셈브린, 피노스트로빈, 일피네틴, 타다모닌, 판두라타, 판두라틴A 등의 성분이 함유되어 있으며, 특히 판두라타(pandurata) 성분은 암세포 성장을 억제하고, 판두라틴A(panduratin A) 성분은 전립선암 및 대장암에 대한 예방효과가 있는 것으로 알려져 있다.Fingerroot contains flavonoids that inhibit the infection of Helicobacter pylori bacteria, including indigestion and gastritis, and pinostrobin, which has a cytoprotective effect, increases gastric mucus and reduces the area of gastric ulcer formation. It is also effective in treating peptic ulcer. In addition, it contains components such as flavonoid derivatives, pinocembrin, pinostrobin, ilpinetin, tadamonin, pandurata, and panduratin A that can inhibit the growth of cancer cells. It is known that the component inhibits the growth of cancer cells, and the panduratin A component has a preventive effect on prostate cancer and colon cancer.
최근 문헌에 의하면, 생강과 식물, 특히 핑거루트의 뿌리에서 추출한 기능성 원료인 판두라틴(Panduratin)은 핑거루트의 뿌리에서 추출한 밝은 황갈색의 분말로서, 식품의약품안전처에서 2013년 건강기능식품의 기능성 원료로 인정되었으며 생리활성기능 2등급을 받은 바 있다.According to recent literature, panduratin, a functional raw material extracted from the root of ginger and plants, especially finger root, is a light yellowish brown powder extracted from the root of finger root. and received a grade 2 physiological activity.
판두라틴은 핑거루트라는 식물의 뿌리에서 추출한 밝은 황갈색의 분말로서, 식품의약품안전처에서 2013년 건강기능식품의 기능성 원료로 인정(생리활성기능 2등급)되었으며, 자외선에 의한 피부 손상으로부터 피부 건강을 유지하고 체내 에너지 항상성 유지를 위한 센서 단백질인 ‘AMPK(AMP-activated protein kinase)’를 활성화시켜 체지방을 감소하는데 기여하는 것으로 알려져 있다.Panduratin is a light yellowish brown powder extracted from the root of a plant called finger root. It is known to contribute to reducing body fat by activating 'AMPK (AMP-activated protein kinase)', a sensor protein for maintenance and energy homeostasis in the body.
그러나 핑거루트뿌리 추출물 성분 중 하나인 판두라틴은 강한 독성이 있어 사용에 주의를 요하며, 이를 이용한 기능성 화장료로 적용하는데 한계가 있는 실정이다.However, panduratin, one of the finger root extract components, has strong toxicity, so caution is required in use, and there is a limit to its application as a functional cosmetic using it.
본 발명자들은 천연재료를 이용한 복합기능성 화장품에 대한 시장의 요구가 높아짐에 따라, 약간의 독성이 있는 단점이 있지만 피부 항상성 유지에 효과가 있는 핑거루트 추출물인 판두라틴의 독성을 제거하는 방법을 개발하였고, 이와 같이 독성이 제거된 핑거루트뿌리줄기 추출물을 이용하여 핑거루트뿌리줄기 추출물의 유익 성분을 화장료로 적용하면서 이 외 다른 천연 식물 유래 추출물과의 혼합 적용함으로써, 피부 미백, 주름, 보습 등의 우수한 효과에 의해 피부 항성성, 피부 상태를 개선할 수 있는 고기능성 화장료, 이의 제조방법 및 이를 이용한 화장품을 제공하고자 한다.The present inventors have developed a method for removing the toxicity of panduratin, a finger root extract that is effective in maintaining skin homeostasis, although it has a slight toxicity disadvantage, as the market demand for multi-functional cosmetics using natural ingredients increases. , By applying the beneficial ingredients of the finger root rhizome extract as a cosmetic using the finger root rhizome extract from which toxicity has been removed as described above, and by applying the mixture with other natural plant-derived extracts, excellent skin whitening, wrinkles, moisturizing, etc. It is an object of the present invention to provide a highly functional cosmetic that can improve skin resistance and skin condition, a manufacturing method thereof, and cosmetics using the same.
상술한 과제를 해결하기 위한, 본 발명의 에멀젼 타입의 피부탄력 개선 화장료는 제1액, 제2액, 제3액 및 제4액을 포함하며, 상기 제1액은 점도조절제 및 정제수를 포함하고, 상기 제2액은 글리세레스-26, 알란토인, 하이드롤라이즈드콜라겐, 아데노신피부중에서 선택된 1종 이상을 포함하는 컨디셔닝제; 글리세린 및 부틸렌글라이콜을 포함하는 보습제; 1,2-헥산다이올을 포함하는 보존제; 및 소듐하이알루로네이트를 포함하는 가교제;를 포함하며, 상기 제3액은 해바라기씨 오일, 다이메티콘, 세틸에틸헥사노에이트 및 글리세릴스테아레이트 중에서 선택된 1종 이상을 포함하는 피부컨디셔닝제; 피이지-100 스테아레이트를 포함하는 계면활성제; 카프릴릭/카프릭트라이글리세라이드(Caprylic/Capric Triglyceride)을 포함하는 보습제; 폴리솔베이트60, 스테아릭애씨드 및 솔비탄세스퀴올리에이트 중에서 선택된 1종 이상을 포함하는 유화제; 및 세테아릴알코올을 포함하는 유화안정제;를 포함하고, 상기 제4액은 진주 추출물 및 천연식물 복합 추출물을 포함하는 기능성 추출물; 락토바실러스발효 용해물; 콜라겐 합성 촉진제; 및 향료;를 포함한다.In order to solve the above problems, the emulsion-type cosmetic composition for improving skin elasticity of the present invention includes a first liquid, a second liquid, a third liquid and a fourth liquid, wherein the first liquid contains a viscosity modifier and purified water, , The second liquid is a conditioning agent containing at least one selected from glycereth-26, allantoin, hydrolyzed collagen, and adenosine skin; moisturizers including glycerin and butylene glycol; preservatives including 1,2-hexanediol; and a cross-linking agent containing sodium hyaluronate; wherein the third solution is a skin conditioning agent containing at least one selected from sunflower seed oil, dimethicone, cetylethylhexanoate, and glyceryl stearate; surfactants including PEG-100 stearate; humectants including Caprylic/Capric Triglyceride; An emulsifier containing at least one selected from polysorbate 60, stearic acid and sorbitan sesquioleate; and an emulsification stabilizer containing cetearyl alcohol, wherein the fourth liquid is a functional extract containing a pearl extract and a natural plant composite extract; Lactobacillus fermentation lysate; collagen synthesis promoter; And fragrance; contains.
또한, 본 발명은 상기 에멀젼 타입의 피부탄력 개선 화장료를 제조하는 방법에 관한 것으로서, 반응기에 정제수 및 점도조절제를 투입한 후, 교반을 수행하여 제1액을 제조하는 1단계; 제1액이 제조된 반응기에 제2액을 투입한 후, 교반을 수행하는 2단계; 2단계를 수행한 반응기에 제3액을 투입한 후, 교반을 수행하는 3단계; 3단계를 수행한 반응기에 pH 조절제를 투입한 후, 교반을 수행하는 4단계; 4단계를 수행한 반응기에 제4액을 투입한 후, 교반을 수행하는 5단계; 5단계를 수행한 혼합액을 여과 및 탈포하는 6단계; 및 6단계를 수행한 혼합액을 숙성시키는 7단계;를 포함하는 공정을 수행하여 제조할 수 있다.In addition, the present invention relates to a method for preparing the emulsion-type cosmetic for improving skin elasticity, comprising the steps of preparing a first liquid by adding purified water and a viscosity modifier to a reactor and stirring; a second step of injecting the second liquid into the reactor in which the first liquid was prepared and performing stirring; Step 3 of stirring after adding the third liquid to the reactor in which Step 2 was performed; 4th step of adding a pH adjusting agent to the reactor in which step 3 was performed and then stirring; Step 5 of performing agitation after injecting the fourth liquid into the reactor in which Step 4 was performed; Step 6 of filtering and defoaming the mixed solution after step 5; It can be prepared by performing a process including; and step 7 of aging the mixed solution after step 6.
또한, 본 발명은 앞서 설명한 방법으로 제조한 화장료를 이용한 피부탄력 개선 화장품에 관한 것으로서, 에멀젼 제형의 화장품을 제공할 수 있다.In addition, the present invention relates to a cosmetic for improving skin elasticity using the cosmetic prepared by the method described above, and can provide a cosmetic in an emulsion formulation.
본 발명의 화장료는 피부 트러블이 없으면서 보습성이 우수하면서 피부 미백 개선, 피부 주름 개선 효과가 우수한 바, 이를 이용하여 고기능성 천연소재 유래의 화장품을 제공할 수 있다.The cosmetic composition of the present invention has excellent skin whitening and skin wrinkle improvement effects while having no skin trouble and excellent moisturizing properties, and thus, it is possible to provide a cosmetic product derived from a highly functional natural material.
도 1은 실험예 1에서 실시한 용매별 핑거루트뿌리줄기 추출물의 세포 독성 측정결과이다.1 is a result of measuring the cytotoxicity of the finger root rhizome extract for each solvent conducted in Experimental Example 1.
도 2는 실험예 2에서 실시한 용매별 핑거루트뿌리줄기 추출물의 세포 보호 측정 결과이다.Figure 2 is the cell protection measurement results of the finger root rhizome extract for each solvent conducted in Experimental Example 2.
도 3은 실험예 2에서 실시한 용매별 핑거루트뿌리줄기 추출물의 세포 보호 효과 측정 결과이다.Figure 3 is the result of measuring the cell protection effect of the finger root rhizome extract for each solvent conducted in Experimental Example 2.
도 4는 실험예 3에서 실시한 핑거루트뿌리줄기 에탄올 추출물의 각 분획물에 대한 세포독성 측정 결과이다.Figure 4 is a result of measuring the cytotoxicity of each fraction of the finger root rhizome ethanol extract conducted in Experimental Example 3.
도 5는 실험예 4에서 실시한 핑거루트뿌리줄기 에탄올 추출물의 각 분획물에 대한 세포 보호 효과 측정 결과이다.Figure 5 is a result of measuring the cell protection effect for each fraction of the finger root rhizome ethanol extract conducted in Experimental Example 4.
도 6 및 도 7은 실험예 4에서 실시한 핑거루트뿌리줄기 에탄올 추출물의 물 분획물의 세포독성 및 세포 보호 효과 측정 결과이다.6 and 7 are the results of measuring the cytotoxicity and cell protection effect of the water fraction of the finger root rhizome ethanol extract performed in Experimental Example 4.
도 8은 실험예 5에서 실시한 핑거루트뿌리줄기 에탄올 추출물의 물 분획물에 대한 세포 내 콜라겐 영향 평가 결과이다.8 is an evaluation result of intracellular collagen effect on the water fraction of the finger root rhizome ethanol extract conducted in Experimental Example 5.
도 9는 실험예 6에서 실시한 핑거루트뿌리줄기 에탄올 추출물의 물 분획물에 대한 세포 내 항산화 영향 평가 결과이다.9 is an evaluation result of the intracellular antioxidant effect on the water fraction of the finger root rhizome ethanol extract conducted in Experimental Example 6.
본 발명의 상세한 설명에서 사용되는 "피부 개선"이란 피부의 손상, 질환 증세를 억제 또는 지연시키거나, 질환증세를 호전시키거나, 피부의 건강 상태를 향상시키는 모든 행위 또는 효과를 의미한다."Skin improvement" used in the detailed description of the present invention means any action or effect that inhibits or delays skin damage, disease symptoms, improves disease symptoms, or improves the health condition of the skin.
본 발명의 상세한 설명에서 사용되는 "추출물(extract)"이란 천연물로부터 분리된 활성성분 즉, 목적하는 활성을 보이는 물질을 의미한다. 상기추출물은 물, 유기용매 또는 이들의 혼합용매를 이용하는 추출 과정으로 획득할 수 있으며, 추출물 이의 건조분말 또는 이를 이용하여 제형화된 모든 형태를 포함한다. 또한, 상기 추출물에는 상기 추출 과정을 거친 추출물을 분획한 것도 포함된다.As used in the detailed description of the present invention, "extract" means an active ingredient isolated from a natural product, that is, a substance showing a desired activity. The extract may be obtained by an extraction process using water, an organic solvent, or a mixed solvent thereof, and includes all forms formulated using the extract or its dry powder. In addition, the extract includes fractionated extracts subjected to the extraction process.
본 발명의 상세한 설명에서 다르게 정의되지 않는 한, 기술적이거나 과학적인 용어를 포함해서 여기서 사용되는 모든 용어들은 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 자에 의해 일반적으로 이해되는 것과 동일한 의미를 가지고 있다. 일반적으로 사용되는 사전에 정의되어 있는 것과 같은 용어들은 관련 기술의 문맥상 가지는 의미와 일치하는 의미를 가진 것으로 해석되어야 하며, 본 출원에서 명백하게 정의하지 않는 한, 이상적이거나 과도하게 형식적인 의미로 해석되지 않는다.Unless otherwise defined in the detailed description of the present invention, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention belongs. there is. Terms such as those defined in commonly used dictionaries should be interpreted as having a meaning consistent with the meaning in the context of the related art, and unless explicitly defined in the present application, they should not be interpreted in an ideal or excessively formal meaning. don't
이하에서 본 발명의 에멀젼 타입의 피부탄력 개선 화장료 및 이를 제조하는 방법을 통해서 본 발명을 더욱 자세하게 설명한다.Hereinafter, the present invention will be described in more detail through the emulsion-type skin elasticity improving cosmetic of the present invention and a method for preparing the same.
본 발명의 화장료는 제1액 100 중량부에 대하여, 제2액 18 ~ 22 중량부, 제3액 8 ~ 12 중량부 및 제4액 10 ~ 15 중량부를 포함하며, 바람직하게는 제1액 100 중량부에 대하여, 제2액 18.5 ~ 21.0 중량부, 제3액 9.0 ~ 11.5 중량부 및 제4액 10.5 ~ 14.0 중량부를 포함하고, 더욱 바람직하게는 바람직하게는 제1액 100 중량부에 대하여, 제2액 18.5 ~ 20.0 중량부, 제3액 10.0 ~ 11.5 중량부 및 제4액 11.0 ~ 13.5 중량부를 포함할 수 있다.The cosmetic composition of the present invention includes 18 to 22 parts by weight of the second solution, 8 to 12 parts by weight of the third solution, and 10 to 15 parts by weight of the fourth solution, based on 100 parts by weight of the first solution, preferably 100 parts by weight of the first solution. With respect to parts by weight, 18.5 to 21.0 parts by weight of the second solution, 9.0 to 11.5 parts by weight of the third solution and 10.5 to 14.0 parts by weight of the fourth solution, more preferably preferably 100 parts by weight of the first solution, 18.5 to 20.0 parts by weight of the second solution, 10.0 to 11.5 parts by weight of the third solution, and 11.0 to 13.5 parts by weight of the fourth solution.
상기 제1액은 화장료의 용매 역할을 하는 것으로서, 점도조절제 0.20 ~ 0.40 중량% 및 잔량의 정제수를 포함하고, 바람직하게는 점도조절제 0.22 ~ 0.35 중량% 및 잔량의 정제수를 포함할 수 있다. 이때, 점도조절제 함량이 0.40 중량%를 초과하면 초기 점도가 너무 높아져서 제2액 내지 제4액 성분이 제1액에 적절하게 용해되지 않고, 조성물의 혼화성이 떨어질 수 있다. 그리고 상기 점도조절제로는 화장품 업계에서 사용하는 일반적인 점도조절제를 사용할 수 있으며, 바람직한 일례로는 아크릴레이트/(C10~30알킬)아크릴레이트 크로스 폴리머(acrylate/(/(C10~30 alklyl)acrylate cross polymer)를 사용할 수 있다.The first liquid serves as a solvent for cosmetics, and may include 0.20 to 0.40% by weight of a viscosity modifier and the remaining amount of purified water, preferably 0.22 to 0.35% by weight of the viscosity modifier and the remaining amount of purified water. At this time, when the content of the viscosity modifier exceeds 0.40% by weight, the initial viscosity is too high, so that the components of the second to fourth liquids are not properly dissolved in the first liquid, and miscibility of the composition may be poor. In addition, as the viscosity modifier, a general viscosity modifier used in the cosmetics industry may be used, and a preferred example is acrylate/(C 10-30 alkyl)acrylate cross polymer (acrylate/(/(C 10-30 alklyl)acrylate cross polymer) can be used.
다음으로, 화장료 성분 중 상기 제2액은 피부컨디셔닝제 18.5 ~ 21.0 중량%, 가교제 10 ~ 12.0 중량%, 미백제 13.0 ~ 16.0 중량%, 보존제 10 ~ 15.0 중량% 및 제2액 전체 중량% 중 나머지 잔량의 보습제를 포함할 수 있으며, 바람직하게는 피부컨디셔닝제 18.8 ~ 20.5 중량%, 가교제 10.2 ~ 11.7 중량%, 미백제 13.0 ~ 15.5 중량%, 보존제 12.0 ~ 15.0 중량% 및 제2액 전체 중량% 중 나머지 잔량의 보습제를, 더욱 바람직하게는 피부컨디셔닝제 18.8 ~ 20.0 중량%, 가교제 10.5 ~ 11.5 중량%, 미백제 13.0 ~ 15.0 중량%, 보존제 13.0 ~ 15.0 중량% 및 제2액 전체 중량% 중 나머지 잔량의 보습제를 포함할 수 있다.Next, among the cosmetic components, the second liquid contains 18.5 to 21.0% by weight of skin conditioning agent, 10 to 12.0% by weight of crosslinking agent, 13.0 to 16.0% by weight of whitening agent, 10 to 15.0% by weight of preservative, and the remainder of the total weight of the second liquid. of moisturizers, preferably 18.8 to 20.5% by weight of skin conditioning agent, 10.2 to 11.7% by weight of crosslinking agent, 13.0 to 15.5% by weight of whitening agent, 12.0 to 15.0% by weight of preservative, and the remainder of the total weight of the second solution of the moisturizer, more preferably 18.8 to 20.0% by weight of the skin conditioning agent, 10.5 to 11.5% by weight of the crosslinking agent, 13.0 to 15.0% by weight of the whitening agent, 13.0 to 15.0% by weight of the preservative and the remaining remaining amount of the moisturizer among the total weight of the second solution can include
제2액 성분 중 상기 피부컨디셔닝제는 글리세레스-26(Glycereth-26), 알란토인(Allantoin), 하이드롤라이즈드 콜라겐(Hydrolyzed Collagen) 및 아데노신(Adenosine) 중에서 선택된 1종 이상을 포함할 수 있으며, 바람직하게는 글리세레스-26, 알란토인, 하이드롤라이즈드 콜라겐 및 아데노신을 1 : 0.1 ~ 0.4 : 0.7 ~ 1.0 : 0.2 ~ 0.5 중량비로, 더욱 바람직하게는 1 : 0.2 ~ 0.3 : 0.7 ~ 0.9 : 0.2 ~ 0.4 중량비로 포함할 수 있다.Among the components of the second liquid, the skin conditioning agent may include at least one selected from Glycereth-26, Allantoin, Hydrolyzed Collagen, and Adenosine, Preferably, glycereth-26, allantoin, hydrolyzed collagen and adenosine are mixed in a weight ratio of 1:0.1 to 0.4:0.7 to 1.0:0.2 to 0.5, more preferably 1:0.2 to 0.3:0.7 to 0.9:0.2 to 0.4 weight ratio.
제2액 성분 중 상기 가교제는 소듐하이알루로네이트(Sodium hyaluronate)를 포함할 수 있으며, 상기 보존제는 피부에 트러블을 유발하지 않는 소재를 사용하는 것이 좋으며, 바람직한 일례를 들면, 1,2-헥산 다이올(1,2-hexane diol)을 포함할 수 있다.Among the components of the second liquid, the crosslinking agent may include sodium hyaluronate, and it is preferable to use a material that does not cause skin trouble as the preservative. For example, 1,2-hexane Diol (1,2-hexane diol) may be included.
그리고, 제2액 성분 중 상기 미백제로서 나이아신아마이드(Niacinamide)를 사용할 수 있고, 상기 보습제는 글리세린(Glycerine) 및 부틸렌글라이콜(butylene glycol) 중에서 선택된 1종 이상을 포함할 수 있다.In addition, niacinamide may be used as the whitening agent among the components of the second liquid, and the moisturizer may include at least one selected from glycerine and butylene glycol.
다음으로, 화장료 성분 중 상기 제3액은 유화제 15.0 ~ 20.0 중량%, 유화안정제 5.0 ~ 8.0 중량%, 계면활성제 10.0 ~ 12.0 중량%, 보습제 5.0 ~ 8.0 중량% 및 제3액 전체 중량 중 나머지 잔량의 피부컨디셔닝제를 포함할 수 있으며, 바람직하게는 유화제 16.5 ~ 20.0 중량%, 유화안정제 5.5 ~ 7.5 중량%, 계면활성제 10.5 ~ 12.0 중량%, 보습제 5.2 ~ 7.5 중량% 및 제3액 전체 중량 중 나머지 잔량의 피부컨디셔닝제를 포함할 수 있다.Next, among the cosmetic ingredients, the third liquid contains 15.0 to 20.0% by weight of an emulsifier, 5.0 to 8.0% by weight of an emulsion stabilizer, 10.0 to 12.0% by weight of a surfactant, 5.0 to 8.0% by weight of a humectant, and the remaining balance of the total weight of the third liquid. It may include a skin conditioning agent, preferably 16.5 to 20.0% by weight of an emulsifier, 5.5 to 7.5% by weight of an emulsion stabilizer, 10.5 to 12.0% by weight of a surfactant, 5.2 to 7.5% by weight of a humectant, and the remainder of the total weight of the third solution. of skin conditioning agents.
제3액 성분 중 상기 유화제는 화장료 조성 간 혼화성 및 조성의 유화성 증대 역할을 하는 것으로서, 폴리솔베이트 60(polysorbate 60),, 스테아릭애씨드(stearic acid) 및 솔비탄세스퀴올리에이트(Sorbitan sesquioleate) 중에서 선택된 1종 이상을 포함할 수 있고, 바람직하게는 폴리솔베이트 60, 스테아릭애씨드 및 솔비탄세스퀴올리에이트을 1 : 0.5 ~ 1.0 : 0.5 ~ 1.0 중량비로, 더욱 바람직하게는 폴리솔베이트 60, 스테아릭애씨드및 솔비탄세스퀴올리에이트을 1 : 0.8 ~ 1.0 : 0.5 ~ 0.9 중량비로 혼합하여 사용하는 것이 화장료 혼화성 증대 측면에서 효과적이다.Among the components of the third liquid, the emulsifier serves to increase the miscibility between cosmetic compositions and the emulsification of the composition, and includes polysorbate 60, stearic acid, and sorbitan sesquioleate (Sorbitan sesquioleate), preferably polysorbate 60, stearic acid and sorbitan sesquioleate in a weight ratio of 1: 0.5 to 1.0: 0.5 to 1.0, more preferably polysorbate 60, stearic acid and sorbitan sesquioleate are mixed and used in a weight ratio of 1: 0.8 to 1.0: 0.5 to 0.9.
제3액 성분 중 상기 유화안정제로는 당업계에서 사용하는 일반적인 유화안정제를 사용할 수 있으며, 바람직하게는 세테아릴알코올(Cetearyl alcohol)을 사용하는 것이 좋다.Among the components of the third liquid, general emulsion stabilizers used in the art may be used as the emulsion stabilizer, and preferably, cetearyl alcohol is used.
또한, 제3액 성분 중 상기 계면활성제는 피이지-(40~100) 스테아레이트(PEG -(40~100) stearate)를, 바람직하게는 피이지-100 스테아레이트를 사용하는 것이 좋다.In addition, it is preferable to use PEG-(40-100) stearate, preferably PEG-100 stearate, as the surfactant among the components of the third liquid.
또한, 제3액 성분 중 상기 보습제로는 카프릴릭애씨드(Caprylic acid)와 카프릭애씨드(Capric acid) 및 글리세린의 혼합 트라이에스테르(trimester)인 카프릴릭/카프릭트라이글리세라이드(Caprylic/Capric Triglyceride)를 사용하는 것이 좋다.In addition, the humectant among the components of the third liquid is caprylic acid, caprylic acid, and caprylic / capric triglyceride, which is a mixed triester of capric acid and glycerin. Triglycerides) are recommended.
또한, 제3액 성분 중 상기 피부컨디셔닝제는 해바라기씨 오일, 다이메티콘(Dimethicone), 세틸에틸헥사노에이트(Cetyl ethyl hexanoate) 및 글리세릴스테아레이트(Glyceryl stearate) 중에서 선택된 2종 이상을 포함할 수 있으며, 바람직하게는 해바라기씨 오일, 다이메티콘, 세틸에틸헥사노에이트 및 글리세릴스테아레이트를 1 : 0.8 ~ 1.0 : 0.5 ~ 0.8 : 0.4 ~ 0.8 중량비로 포함할 수 있다.In addition, the skin conditioning agent among the components of the third liquid may include at least two selected from sunflower seed oil, dimethicone, cetyl ethyl hexanoate, and glyceryl stearate. Preferably, sunflower seed oil, dimethicone, cetylethylhexanoate, and glyceryl stearate may be included in a weight ratio of 1:0.8 to 1.0:0.5 to 0.8:0.4 to 0.8.
다음으로, 화장료 성분 중 상기 제4액은 락토바실러스발효 용해물 5.0 ~ 8.0 중량%, 콜라겐 합성 촉진제 1.0 ~ 2.5 중량%, 향료 0.1 ~ 0.8 중량% 및 제4액 전체 중량 중 나머지 잔량의 기능성 추출물을 포함할 수 있고, 바람직하게는 락토바실러스발효 용해물 5.5 ~ 7.0 중량%, 콜라겐 합성 촉진제 1.2 ~ 2.3 중량%, 향료 0.1 ~ 0.8 중량% 및 제4액 전체 중량 중 나머지 잔량의 기능성 추출물을 포함할 수 있다. 이때, 제4액 성분 중 락토바실러스발효 용해물은 기능성 추출물이 숙성을 증진시키는 역할을 하는 것으로서 함량이 5.0 중량% 미만이면 기능성 추출물 숙성이 잘 되지 않아서 피부 트러블을 유발시킬 수 있으며, 8.0 중량%를 초과하여 사용하는 것은 비경제적이다.Next, among the cosmetic ingredients, the fourth liquid contains 5.0 to 8.0% by weight of the lactobacillus fermentation lysate, 1.0 to 2.5% by weight of the collagen synthesis promoter, 0.1 to 0.8% by weight of the fragrance, and the remaining balance of the functional extract of the total weight of the fourth liquid. 5.5 to 7.0% by weight of the lactobacillus fermented lysate, 1.2 to 2.3% by weight of the collagen synthesis promoter, 0.1 to 0.8% by weight of the fragrance, and the remaining functional extract of the total weight of the fourth solution. there is. At this time, the lactobacillus fermented lysate among the components of the fourth liquid serves to promote the aging of the functional extract, and if the content thereof is less than 5.0% by weight, the functional extract may not mature well and cause skin trouble. Excessive use is uneconomical.
그리고, 콜라겐 합성 촉진제는 피부에 흡수되어 피부의 콜라겐 합성을 촉진하는 역할을 하는 것으로서, 알에이치-올리고펩타이드-1를 사용할 수 있다. 그리고, 콜라겐 합성 촉진제 함량이 1.0 중량% 미만이면 그 사용량이 너무 적어서 피부의 콜라겐 합성 촉진 효과가 미비하여 피부 주름 개선 증대 효과가 미비할 수 있고, 2.5 중량%를 초과하여 사용하면 다른 조성들의 혼화성을 방해할 수 있으므로 상기 범위 내로 사용하는 것이 좋다.In addition, the collagen synthesis accelerator is absorbed into the skin and serves to promote collagen synthesis in the skin, and RH-Oligopeptide-1 may be used. In addition, if the content of the collagen synthesis promoter is less than 1.0% by weight, the amount used is too small and the effect of promoting collagen synthesis in the skin is insufficient, so the effect of improving skin wrinkles may be insufficient. It is recommended to use it within the above range because it may interfere with the
그리고, 향료의 종류는 피부 트러블을 유발하거나, 본 발명 화장료의 기능을 저해하지 않는다면 당업계에서 사용하는 일반적인 향료를 사용할 수 있다.In addition, as for the type of fragrance, general fragrances used in the art may be used as long as they do not cause skin trouble or impair the function of the cosmetic of the present invention.
또한, 상기 기능성 추출물은 진주 추출물 및 천연 식물 복합 추출물을 포함하며, 진주 추출물 및 천연식물 복합 추출물을 1 : 3.5 ~ 5.0 중량비로, 바람직하게는 진주 추출물 및 천연식물 복합 추출물을 1 : 3.8 ~ 4.8 중량비로 포함할 수 있다.In addition, the functional extract includes a pearl extract and a natural plant complex extract, the pearl extract and the natural plant complex extract in a weight ratio of 1: 3.5 to 5.0, preferably the pearl extract and the natural plant complex extract in a weight ratio of 1: 3.8 to 4.8 can be included with
상기 진주(pearl) 추출물의 진주는 조개류의 체내에서 형성되는 구슬 모양의 분비물 덩어리를 의미하며, 진주 100g을 분쇄한 후 2 ~ 4L의 60 ~ 80부피% 에탄올 수용액을 용매로 사용하여 10 ~ 16시간 정도 가온 환류추출하는 1단계; 환류추출액을 냉침시킨 후, 여과지로 여과하여 여과액을 수득하는 2단계; 수득된 여과액을 감압농축 및 감압 건조로 농축하여 진주 건조 분말을 수득하는 3단계;를 포함하는 공정을 수행하여 제조할 수 있다.The pearl of the pearl extract refers to a bead-shaped secretion mass formed in the body of shellfish. After pulverizing 100 g of pearls, 2 to 4 L of 60 to 80 vol% ethanol aqueous solution is used as a solvent for 10 to 16 hours. 1st step of reflux extraction with moderate heating; A second step of cooling the reflux extract and then filtering with a filter paper to obtain a filtrate; It can be prepared by carrying out a process including three steps of concentrating the obtained filtrate by vacuum concentration and vacuum drying to obtain pearl dry powder.
그리고, 상기 천연 식물 복합 추출물은 핑거루트뿌리줄기 추출물(Boesenbergia Pandurata Rhizome Extract), 병풀 추출물, 비타민나무 추출물(Hippophae Rhamnoides Extract), 녹차 추출물(Camellia Sinensis Leaf Extract), 마트리카리아 추출물(Chamomilla Recutita Extract), 저단선 추출물(Opuntia Humifusa Extract), 뽕나무잎 추출물(Morus Alba Leaf Extract), 산사나무열매 추출물(Crataegus Pinnatifida Fruit Extract), 페퍼민트 추출물(Mentha Piperita(Peppermint) Extract), 히비스커스꽃 추출물(Hibiscus Sabdariffa Flower Extract), 로즈마리 추출물(Rosmarinus Officinalis(Rosemary) Extract), 모과 추출물(Chaenomeles Sinensis Fruit Extract) 및 레드초크베리 추출물(Aronia Arbutifolia Extract)을 포함하며, 바람직하게는 핑거루트뿌리줄기 추출물 100 중량부에 대하여, 병풀 추출물 15 ~ 30 중량부, 비타민나무 추출물 0.2 ~ 2.0 중량부, 녹차 추출물 0.2 ~ 2.0 중량부, 마트리카리아 0.2 ~ 2.0 중량부, 저단선 추출물 0.1 ~ 1.0 중량부, 뽕나무잎 추출물 0.1 ~ 1.0 중량부, 산사나무열매 추출물 0.1 ~ 1.0 중량부, 페퍼민트 추출물 0.1 ~ 1.0 중량부, 히비스커스꽃 추출물 0.1 ~ 1.0 중량부, 로즈마리 추출물 0.1 ~ 1.0 중량부, 모과 추출물 0.1 ~ 1.0 중량부 및 레드초크베리 추출물 0.1 ~ 1.0 중량부로 포함할 수 있으며, 더욱 바람직하게는 핑거루트뿌리줄기 추출물 100 중량부에 대하여, 병풀 추출물 15 ~ 25 중량부, 비타민나무 추출물 0.3 ~ 1.5 중량부, 녹차 추출물 0.3 ~ 1.5 중량부, 마트리카리아 추출물 0.3 ~ 1.5 중량부, 저단선 추출물 0.1 ~ 0.8 중량부, 뽕나무잎 추출물 0.1 ~ 0.8 중량부, 산사나무열매 추출물 0.1 ~ 0.8 중량부, 페퍼민트 추출물 0.1 ~ 0.8 중량부, 히비스커스꽃 추출물 0.1 ~ 0.8 중량부, 로즈마리 추출물 0.1 ~ 0.8 중량부, 모과 추출물 0.1 ~ 0.8 중량부 및 레드초크베리 추출물 0.1 ~ 0.8 중량부를 포함하는 것이 좋다.In addition, the natural plant complex extract is finger root rhizome extract (Boesenbergia Pandurata Rhizome Extract), centella extract, vitamin tree extract (Hippophae Rhamnoides Extract), green tea extract (Camellia Sinensis Leaf Extract), Matricaria extract (Chamomilla Recutita Extract) , Opuntia Humifusa Extract, Morus Alba Leaf Extract, Crataegus Pinnatifida Fruit Extract, Mentha Piperita (Peppermint) Extract, Hibiscus Sabdariffa Flower Extract ), rosemary extract (Rosmarinus Officinalis (Rosemary) Extract), quince extract (Chaenomeles Sinensis Fruit Extract) and red chokeberry extract (Aronia Arbutifolia Extract), preferably with respect to 100 parts by weight of finger root rhizome extract, Centella asiatica Extract 15 ~ 30 parts by weight, vitamin tree extract 0.2 ~ 2.0 parts by weight, green tea extract 0.2 ~ 2.0 parts by weight, Matricaria 0.2 ~ 2.0 parts by weight, low tanseon extract 0.1 ~ 1.0 parts by weight, mulberry leaf extract 0.1 ~ 1.0 parts by weight , hawthorn fruit extract 0.1 ~ 1.0 parts by weight, peppermint extract 0.1 ~ 1.0 parts by weight, hibiscus flower extract 0.1 ~ 1.0 parts by weight, rosemary extract 0.1 ~ 1.0 parts by weight, quince extract 0.1 ~ 1.0 parts by weight and red chokeberry extract 0.1 ~ 1.0 parts by weight 1.0 parts by weight, more preferably 100 parts by weight of finger root rhizome extract, 15 to 25 parts by weight of centella asiatica extract, 0.3 to 1.5 parts by weight of vitamin tree extract, 0.3 to 1.5 parts by weight of green tea extract, Matrica Rhea extract 0.3 ~ 1.5 parts by weight, low tanning extract 0.1 ~ 0.8 parts by weight, mulberry leaf extract 0.1 ~ 0.8 parts by weight, hawthorn fruit extract 0.1 ~ 0.8 parts by weight, peppermint extract 0.1 ~ 0.8 parts by weight, hibiscus flower extract 0.1 ~ 0.8 parts by weight It is preferable to include 0.1 to 0.8 parts by weight of rosemary extract, 0.1 to 0.8 parts by weight of quince extract and 0.1 to 0.8 parts by weight of red chokeberry extract.
상기 핑거루트뿌리줄기 추출물은 독성이 제거된 추출물로서, 핑거루트뿌리줄기 에탄올 추출물 또는 핑거루트뿌리줄기 에탄올 추출물의 물 분획물을 사용하는 것이 좋으며, 바람직하게는 독성이 제거된 핑거루트뿌리줄기 에탄올 추출물의 물 분획물을 사용하는 것이 좋으며 이는 하기와 같은 방법을 통해 제조할 수 있다.The finger root rhizome extract is an extract from which toxicity has been removed, and it is recommended to use a finger root rhizome ethanol extract or a water fraction of the finger root rhizome ethanol extract, preferably a finger root rhizome ethanol extract from which toxicity has been removed. It is preferable to use the water fraction, which can be prepared through the following method.
핑거루트뿌리줄기 에탄올 추출물의 물 분획물은, 핑거루트뿌리줄기 파우더(Powder)을 에탄올(Ethanol) 수용액과 혼합한 후, 교반하여 18 ~ 24 시간 동안 15 ~ 30℃ 조건에서 추출공정을 수행하여 에탄올 추출물을 수득하는 1단계; 상기 에탄올 추출물을 필터링한 후, 증류수(Water)를 첨가한 후 진공 상태에서 농축하여 에탄올을 제거된 농축액을 수득하는 2단계; 및 상기 농축액을 DMSO(Dimethyl sulfoxide)로 재용해한 후, 멸균필터로 여과한 다음 동결 건조하는 3단계;를 포함하는 공정을 수행하여 제조할 수 있다.The water fraction of the finger root rhizome ethanol extract is obtained by mixing the finger root rhizome powder with an aqueous ethanol solution, stirring, and performing an extraction process at 15 to 30 ° C for 18 to 24 hours to obtain an ethanol extract. Step 1 to obtain; A second step of filtering the ethanol extract, adding distilled water, and then concentrating in a vacuum to obtain a concentrated solution from which ethanol is removed; And after re-dissolving the concentrate in DMSO (dimethyl sulfoxide), it can be prepared by performing a process comprising: 3 steps of filtering with a sterile filter and then freeze-drying.
그리고, 물 분획물 제조 공정에서 상기 3단계는 상기 농축액에 디클로로포름(Dichloroform)을 넣고 교반하여 방치한 뒤 하층액을 제거하는 3-1단계; 및 상기 하층액 제거 후, 에틸아세테이트(Ethyl Acetate)를 넣고 교반하여 방치한 뒤 하층액을 수득한 후, 수득물을 동결건조하여 분말화시키는 3-2단계;를 수행할 수도 있다.And, in the water fraction manufacturing process, the 3-step step 3-1 of removing the lower layer solution after adding dichloroform to the concentrated solution, stirring and leaving it to stand; And after removing the lower layer liquid, ethyl acetate (Ethyl Acetate) is added and left to stir to obtain a lower layer liquid, and then 3-2 steps of lyophilizing and powdering the obtained product.
이하에서는 앞서 설명한 제1액 내지 제4액을 포함하는 화장료를 제조하는 방법에 대해 설명한다.Hereinafter, a method for preparing a cosmetic composition containing the first to fourth liquids described above will be described.
본 발명의 화장료는 반응기에 정제수 및 점도조절제를 투입한 후, 교반을 수행하여 제1액을 제조하는 1단계; 제1액이 제조된 반응기에 제2액을 투입한 후, 교반을 수행하는 2단계; 2단계를 수행한 반응기에 제3액을 투입한 후, 교반을 수행하는 3단계; 3단계를 수행한 반응기에 pH 조절제를 투입한 후, 교반을 수행하는 4단계; 4단계를 수행한 반응기에 제4액을 투입한 후, 교반을 수행하는 5단계; 5단계를 수행한 혼합액을 여과 및 탈포하는 6단계; 및 6단계를 수행한 혼합액을 숙성시키는 7단계;를 포함하는 공정을 수행하여 제조할 수 있다.The cosmetic composition of the present invention includes a first step of preparing a first liquid by adding purified water and a viscosity modifier to a reactor and stirring; a second step of injecting the second liquid into the reactor in which the first liquid was prepared and performing stirring; Step 3 of stirring after adding the third liquid to the reactor in which Step 2 was performed; 4th step of adding a pH adjusting agent to the reactor in which step 3 was performed and then stirring; Step 5 of performing agitation after injecting the fourth liquid into the reactor in which Step 4 was performed; Step 6 of filtering and defoaming the mixed solution after step 5; It can be prepared by performing a process including; and step 7 of aging the mixed solution after step 6.
상기 1단계의 교반은 60 ~ 80℃ 및 교반속도 2500 ~ 3500rpm의 조건으로, 바람직하게는 65 ~ 75℃ 및 교반속도 2800 ~ 3200rpm 조건 하에서, 40 ~ 80분 동안, 바람직하게는 50 ~ 70분 동안 수행하는 것이 좋다. 이때, 교반시 온도가 60℃ 미만이거나, 교반속도가 2500rpm 미만이면 점도조절제가 정제수에 완전히 용해되지 않아서 교반시간이 길어지는 문제가 있을 수 있고, 교반시 온도가 80℃를 초과하는 것은 비경제적이며, 교반속도가 3500rpm을 초과하면 거품이 발생할 수 있으므로 상기 조건 하에서 교반을 수행하는 것이 좋다.The stirring in the first step is performed at 60 to 80 ° C and a stirring speed of 2500 to 3500 rpm, preferably for 40 to 80 minutes, preferably for 50 to 70 minutes, under the conditions of 65 to 75 ° C and a stirring speed of 2800 to 3200 rpm. good to do At this time, if the temperature during stirring is less than 60 ° C or the stirring speed is less than 2500 rpm, the viscosity modifier may not be completely dissolved in the purified water, so there may be a problem of lengthening the stirring time, and it is uneconomical when the temperature exceeds 80 ° C during stirring. , If the stirring speed exceeds 3500 rpm, bubbles may be generated, so it is good to perform stirring under the above conditions.
상기 2단계의 교반은 60 ~ 80℃ 및 교반속도 2000 ~ 3000rpm의 조건으로, 바람직하게는 65 ~ 75℃ 및 교반속도 2200 ~ 2700rpm 조건 하에서, 40 ~ 80분 동안, 바람직하게는 50 ~ 70분 동안 수행하는 것이 좋다.The stirring in the second step is performed at 60 to 80 ° C and a stirring speed of 2000 to 3000 rpm, preferably for 40 to 80 minutes, preferably for 50 to 70 minutes, under the conditions of 65 to 75 ° C and a stirring speed of 2200 to 2700 rpm. good to do
또한, 상기 3단계의 교반은 70 ~ 80℃ 및 교반속도 2000 ~ 3000rpm의 조건으로, 바람직하게는 65 ~ 75℃ 및 교반속도 2200 ~ 2700rpm 조건 하에서, 30 ~ 60분 동안, 바람직하게는 30 ~ 60분 동안 수행하는 것이 좋다.In addition, the stirring in the third step is performed at 70 to 80 ° C and a stirring speed of 2000 to 3000 rpm, preferably at 65 to 75 ° C and a stirring speed of 2200 to 2700 rpm for 30 to 60 minutes, preferably 30 to 60 ° C. It is better to do it for minutes.
그리고, 4단계는 5단계의 제4액 혼합 전 pH 조절을 수행하는 공정으로서, 3단계를 수행한 반응기 내 온도를 낮춘 후, pH 조절제를 투입 및 교반을 수행한다. 이때, 교반은 35 ~ 45℃ 및 교반속도 2000 ~ 3000rpm의 조건으로, 바람직하게는 35 ~ 40℃ 및 교반속도 2200 ~ 2700rpm 조건 하에서, 10 ~ 30분 동안, 바람직하게는 20 ~ 30분 동안 수행하는 것이 좋다. 그리고, 상기 pH 조절제의 바람직한 일례로는 알지닌(arginine)을 사용할 수 있으며, 제1액 100 중량부에 대하여, 0.10 ~ 0.50 중량부, 바람직하게는 0.20 ~ 0.40 중량부 정도로 투입하는 것이 적절하다.And, step 4 is a process of performing pH adjustment before mixing the fourth liquid in step 5, and after lowering the temperature in the reactor in which step 3 was performed, a pH adjuster is introduced and stirring is performed. At this time, stirring is carried out for 10 to 30 minutes, preferably for 20 to 30 minutes under the conditions of 35 ~ 45 ℃ and stirring speed 2000 ~ 3000 rpm, preferably under the conditions of 35 ~ 40 ℃ and stirring speed 2200 ~ 2700 rpm It is good. In addition, arginine may be used as a preferred example of the pH adjusting agent, and it is appropriate to add 0.10 to 0.50 parts by weight, preferably 0.20 to 0.40 parts by weight, based on 100 parts by weight of the first solution.
그리고, 5단계의 교반은 35 ~ 45℃ 및 교반속도 2000 ~ 3000rpm의 조건으로, 바람직하게는 35 ~ 40℃ 및 교반속도 2200 ~ 2700rpm 조건 하에서, 10 ~ 30분 동안, 바람직하게는 20 ~ 30분 동안 수행하는 것이 좋다.And, the stirring in step 5 is performed at 35 to 45 ° C and a stirring speed of 2000 to 3000 rpm, preferably at 35 to 40 ° C and a stirring speed of 2200 to 2700 rpm, for 10 to 30 minutes, preferably for 20 to 30 minutes. It is good to do it while
앞서 설명한 조성 및 방법으로 제조한 본 발명의 피부탄력 개선 화장료는 당업계에서 통상적으로 제조되는 어떠한 제형의 화장품으로 제조될 수 있으며, 피부과학적으로 허용 가능한 매질 또는 기제를 함유함으로써 피부과학 분야에서 통상적으로 사용되는 국소적용 또는 전신 적용할 수 있는 보조제 형태로 제조될 수 있다.The cosmetic composition for improving skin elasticity of the present invention prepared by the composition and method described above can be prepared as a cosmetic of any formulation conventionally manufactured in the art, and is commonly used in the field of dermatology by containing a dermatologically acceptable medium or base. It can be prepared in the form of an adjuvant that can be applied topically or systemically.
또한, 바람직하게는 에멀젼 제형의 화장품으로 제조할 수 있으며, 상기 에멀젼 제형 화장품은 점도 45,000 ~ 51,000cP 및 pH 6.0 ~ 7.0일 수 있다.In addition, preferably, it can be prepared as an emulsion-type cosmetic, and the emulsion-type cosmetic may have a viscosity of 45,000 to 51,000 cP and a pH of 6.0 to 7.0.
이상에서 본 발명에 대하여 구현예를 중심으로 설명하였으나 이는 단지 예시일 뿐 본 발명의 구현예를 한정하는 것이 아니며, 본 발명의 실시예가 속하는 분야의 통상의 지식을 가진 자라면 본 발명의 본질적인 특성을 벗어나지 않는 범위에서 이상에 예시되지 않은 여러 가지의 변형과 응용이 가능함을 알 수 있을 것이다. 예를 들어, 본 발명의 구현예에 구체적으로 나타난 각 구성 요소는 변형하여 실시할 수 있는 것이다. 그리고 이러한 변형과 응용에 관계된 차이점들은 첨부된 청구 범위에서 규정하는 본 발명의 범위에 포함되는 것으로 해석되어야 할 것이다.In the above, the present invention has been described with a focus on embodiments, but this is only an example and does not limit the embodiments of the present invention, and those skilled in the art to which the embodiments of the present invention belong will appreciate the essential characteristics of the present invention. It will be appreciated that various modifications and applications not exemplified above are possible within a range that does not deviate. For example, each component specifically shown in the embodiment of the present invention can be modified and implemented. And differences related to these modifications and applications should be construed as being included in the scope of the present invention as defined in the appended claims.
[실시예][Example]
준비예 1 : 핑거루트뿌리줄기 추출물의 제조Preparation Example 1: Preparation of finger root rhizome extract
(1) 핑거루트뿌리줄기 분말 5g을 취한 후, 용매별로 핵산(hexane), 디클로로포름(Dichloroform), 에틸아세테이트(ethyl acetate), 에탄올(ethanol), 메탄올(methanol) 및 물(water) 100ml을 각각 넣고 셰이커(shaker)를 이용하여 24시간 동안 25℃에서 추출하여 추출액을 각각 수득하였다. 다음으로, 수득한 추출액을 필터(Whatman No.2 filter paper)를 이용하여 필터링한 후 용매별 추출물을 진공 상태에서 농축하였다. 농축액을 DMSO(dimethyl sulfoxide, 다이메틸 설폭사이드)로 재용해한 후 0.22um 멸균필터로 여과한 후, -20℃에서 냉동 보관하였다. 그리고, 물 추출물은 필터링한 후 동결건조하여 파우더를 50 부피% DMSO에 재용해한 후 멸균필터로 여과하여 사용하였다.(1) After taking 5 g of finger root rhizome powder, 100 ml of hexane, dichloroform, ethyl acetate, ethanol, methanol and water for each solvent Then, extracts were obtained by extraction at 25° C. for 24 hours using a shaker. Next, the obtained extract was filtered using a filter (Whatman No.2 filter paper), and then the extract for each solvent was concentrated in a vacuum. The concentrate was re-dissolved in DMSO (dimethyl sulfoxide, dimethyl sulfoxide), filtered through a 0.22um sterile filter, and stored frozen at -20°C. Then, the water extract was filtered and lyophilized, and the powder was re-dissolved in 50 vol% DMSO and filtered through a sterile filter before use.
디클로로포름, 에틸아세테이트, 에탄올 및 메탄올 용매 추출물은 연한 노란색을 띄었고, 헥산 추출물은 무색을 띄었다.Dichloroform, ethyl acetate, ethanol, and methanol solvent extracts showed a light yellow color, and hexane extracts showed colorless.
(2) 지표 성분 분석(2) Indicator component analysis
핑거루트뿌리줄기 추출물을 같은 농도로 분취하여 HLPC 시료로 준비하였다.Finger root rhizome extracts were aliquoted at the same concentration and prepared as HLPC samples.
핑거루트 추출물의 지표성분 판투라틴(Panduratin) A와 용매별 추출물의 HPLC 크래마토그램(chromatogram)을 비교하여 추출물 내 판두라틴 A 함량을 분석하였다. 판두라틴 A의 화학구조는 하기 화학식 1과 같다.The panduratin A content in the extract was analyzed by comparing the HPLC chromatogram of the index component panduratin A of the finger root extract and the extract for each solvent. The chemical structure of panduratin A is shown in Formula 1 below.
[화학식 1][Formula 1]
Figure PCTKR2021019521-appb-I000001
Figure PCTKR2021019521-appb-I000001
분석 방법은 정량성 작성을 위해 판두라틴 A는 메탄올에 녹여 단계적으로 희석하여 시료 조제하였으며, HPLC측정 조건은 하기 표 1과 같으며, 분석방법의 유효화(validation)은 하기 표 2와 같다.As for the analysis method, panduratin A was dissolved in methanol and diluted in stages to prepare samples for quantitative writing. The HPLC measurement conditions are shown in Table 1 below, and the validation of the analysis method is shown in Table 2 below.
항목item 분석조건analysis conditions
검출기(Detector)Detector UV 280 nmUV 280 nm
컬럼(Column)Column C18(4.6mm I.D. × 250mm, 5μm)C 18 (4.6mm ID × 250mm, 5μm)
이동상
(Mobile phase)
mobile phase
(Mobile phase)
시간(분)time (minutes) A[DW](%)A[DW] (%) B[메탄올](%)B [methanol] (%)
55 4040 6060
1010 00 100100
1515 00 100100
2525 4040 6060
3030 4040 6060
컬럼온도column temperature 55℃55℃
주입부피injection volume 20μL20μL
유량flux 1mL/min1mL/min
특이성specificity Panduratin A 약 100 mg을 정밀하게 달아 희석액을 넣어 녹여 100mL로 정용하여 표준용액(약 1 000 mg/kg)으로 한 후 이 표준용액을 희석액으로 희석하여 Panduratin A 표준용액과 Panduratin A 미함유 희석액을 분석하여 표준용액의 분석결과와 비교하였다.Weigh accurately about 100 mg of Panduratin A and dissolve it in dilution solution to make it standard solution (about 1 000 mg/kg) in 100 mL. Then, this standard solution is diluted with dilution solution to analyze Panduratin A standard solution and dilution solution without Panduratin A. and compared with the analysis results of the standard solution.
직선성linearity anduratin A 표준품을 4개 농도로 분석하였으며, 직선성의 결정계수(r2)로 평가하였다. 조제된 표준용액(약 1,000 mg/kg)을 MeOH 으로 희석하여 표준용액을 제조하였다.Anduratin A standards were analyzed at 4 concentrations, and the coefficient of determination (r2) of linearity was evaluated. A standard solution was prepared by diluting the prepared standard solution (about 1,000 mg/kg) with MeOH.
범위range 유효화(validation)을 시행한 시험방법에서 Panduratin A 검량선을 작성할 때 직선성이 입증되는 표준용액의 농도는 정확성 시험농도와 정밀성 시험농도를 고려하여 1 mg/kg, 5 mg/kg, 10 mg/kg, 50 mg/kg 으로 농도 범위를 설정하였다.When preparing a calibration curve for Panduratin A in the validation test method, the concentration of the standard solution for which linearity is proven is 1 mg/kg, 5 mg/kg, and 10 mg/kg in consideration of the accuracy test concentration and precision test concentration. , and the concentration range was set at 50 mg/kg.
정확성
(회수율)
accuracy
(recovery rate)
Panduratin A 미 함유 MeOH 에 Panduratin A 표준원액(1,000 mg/kg)을 이용하여 농도별로 일정한 양을 첨가한 후 MeOH 을 넣고 초음파로 15분 동안 분산시켰고 여과(0.20㎕ syringe filter) 후 검액으로 하였다. 각 농도별로 독립적으로 3회씩 반복 측정한 후 회수율을 확인하여 평가하였다.After adding a certain amount by concentration using Panduratin A standard stock solution (1,000 mg/kg) to MeOH without Panduratin A, MeOH was added and dispersed by ultrasonic wave for 15 minutes. After filtering (0.20 μl syringe filter), it was used as the test solution. After repeating the measurement three times independently for each concentration, the recovery rate was confirmed and evaluated.
정밀성
(재현성)
precision
(reproducibility)
Panduratin A 미 함유 MeOH에 Panduratin A 표준원액(1 000 mg/kg)을 이용하여 0.5mL를 첨가한 후 10% MeOH 5mL를 넣고 초음파로 15분 동안 분산시킨 다음 10mL로 정용하고, 여과(0.20㎕ syringe filter) 후 검액으로 하였다. Panduratin A 50 mg/kg 의 농도) 7회 반복 측정한 후 결과 값의 상대표준편차로 시스템 적합성을 확인하였다.After adding 0.5 mL of Panduratin A standard stock solution (1 000 mg/kg) to MeOH without Panduratin A, add 5 mL of 10% MeOH, disperse by ultrasonic wave for 15 minutes, apply 10 mL, and filter (0.20 μl syringe). After filter), it was used as a test solution. The concentration of Panduratin A 50 mg/kg) was measured 7 times, and the system suitability was confirmed by the relative standard deviation of the resultant value.
검출한계와 정량한계Limits of detection and quantification Panduratin A 표준품 약 100 mg을 정밀하게 달아 이동상에 녹여 100mL로 정용하여 표준원액(약 1,000 mg/kg)으로 한 후 이 표준원액을 희석액에 희석하여 최소 표준용액 농도를 10회 반복 측정하여 검출한계와 정량한계를 계산하였다.Approximately 100 mg of the Panduratin A standard was precisely weighed and dissolved in the mobile phase, and the standard stock solution (approximately 1,000 mg/kg) was used as a standard stock solution (approximately 1,000 mg/kg) in 100 mL. Limits of quantification were calculated.
그리고, 용매별 추출물 내 판두라틴 A 함량 측정 결과는 하기 표 3에 나타내었다.In addition, the results of measuring the content of panduratin A in the extract for each solvent are shown in Table 3 below.
추출 용매extraction solvent Retention timeRetention time AreaArea 농도(Concentration, ppm)Concentration (ppm)
Panduratin A 1 ppmPanduratin A 1 ppm 29.37729.377 61336133 1.3481.348
Panduratin A 5 ppm Panduratin A 5 ppm 29.37929.379 4077440774 4.6604.660
Panduratin A 10 ppm Panduratin A 10 ppm 29.38029.380 9617996179 9.9569.956
Panduratin A 50 ppm Panduratin A 50 ppm 29.36529.365 515463515463 50.03650.036
헥산hexane 29.19729.197 33643364 1.0881.088
에틸아세테이트ethyl acetate 29.34629.346 3438234382 4.0424.042
디클로로포름dichloroform 29.33629.336 71347134 1.4371.437
메탄올methanol 29.36429.364 3028130281 3.6633.663
에탄올ethanol 29.36229.362 3423734237 4.0304.030
상기 표 3의 측정 결과를 살펴보면, 모든 추출 용매에서 29.3분에 지표물질 판두라틴 A가 검출이 되었고 에틸아세테이트(4.042), 에탄올(4.030), 메탄올(3.663) 순으로 높은 농도의 판두라틴 A를 함유한 것을 확인할 수 있었다.실험예 1 : 핑거루트뿌리줄기 추출물의 독성 실험 Looking at the measurement results in Table 3, the indicator substance panduratin A was detected at 29.3 minutes in all extraction solvents, and ethyl acetate (4.042), ethanol (4.030), and methanol (3.663) contained high concentrations of panduratin A in that order. I was able to confirm that Experimental Example 1: Toxicity test of finger root rhizome extract
준비예 1에서 제조한 핵산 추출물(H), 디클로로포름 추출물(Ch), 에틸아세테이트 추출물(EA), 에탄올 추출물(Et), 메탄올 추출물(Me) 및 물 추출물 각각에 대한 독성 실험을 수행하였고, 그 결과를 도 1의 A ~ C에 나타내었다. 시험에 사용한 AsA는 양성대조군(positive control)으로 아스코르브산(ascorbic acid, Vit.C)을 표기한 것이다.A toxicity test was performed on each of the nucleic acid extract (H), dichloroform extract (Ch), ethyl acetate extract (EA), ethanol extract (Et), methanol extract (Me), and water extract prepared in Preparation Example 1, The results are shown in A to C of FIG. 1 . AsA used in the test is labeled with ascorbic acid (Vit.C) as a positive control.
핵산(hexane, H), 디클로로포름(dichloroform, Ch), 에틸아세테이트(ethyl acetate, EA), 에탄올(ethanol, Et), 메탄올(methanol, Me) 및 물(water, W)을 각각 용매로 한 추출물을 0.1, 0.5, 1, 5μg/ml 농도로 피부세포 Hs68를 처리한 결과로서, 물 추출물을 제외한 나머지 추출물들 5μg/ml에서 모두 높은 독성이 나타났다.Extracts using nucleic acid (hexane, H), dichloroform (Ch), ethyl acetate (EA), ethanol (ethanol, Et), methanol (Me), and water (water, W) as solvents, respectively As a result of treating skin cell Hs68 at concentrations of 0.1, 0.5, 1, and 5 μg/ml, high toxicity was observed in all extracts except for the water extract at 5 μg/ml.
실험예 2 : 핑거루트뿌리줄기 추출물의 UVB 자극에 대한 세포 보호 효과 및 콜라게나아제 생성 저해 실험Experimental Example 2: Cell protection effect of finger root rhizome extract against UVB stimulation and inhibition of collagenase production
(1) 세포 보호 효과(1) Cell protective effect
UVB 자극에 대한 세포 보호효과를 측정하기 위해 세포독성을 측정할 때와 같은 농도로 처리하여 용매별 핑거루트뿌리줄기 추출물의 UVB 자극에 대한 세포 보호효과를 측정한 실험 결과를 도 2의 A ~ C에 나타내었다. 도 2에 나타난 바와 같이, 에탄올과 메탄올을 제외한 나머지 시료에선 세포 보호효과가 뚜렷하게 나타나지 않았다.In order to measure the cytoprotective effect on UVB stimulation, the experimental results of measuring the cytoprotective effect on UVB stimulation of each solvent were measured at the same concentration as when measuring cytotoxicity, A to C in FIG. shown in As shown in FIG. 2, the cell protection effect was not evident in the samples other than ethanol and methanol.
또한, 도 3의 A 및 B는 용매별 핑거루트뿌리줄기 추출물의 UVB 자극에 대한 세포 보호효과를 대비하기 위하여 0.5 및 1μg/ml의 농도에 대하여 실험한 결과를 함께 나타낸 그래프이다. 도 3에 도시된 바와 같이, UVB자극에 대한 세포 보호효과 실험결과, 에탄올 추출물에서 효과가 가장 좋게 나타났으며, 1μg/ml보다 0.5μg/ml에서 보호효과가 유의적으로 증가하였으며, 핑거루트뿌리줄기 에탄올 추출물의 UVB에 대한 세포 보호효과가 가장 높게 나타났다.In addition, A and B of Figure 3 are graphs showing the results of experiments with concentrations of 0.5 and 1 μg / ml in order to prepare for the cell protection effect of each solvent finger root rhizome extract against UVB stimulation. As shown in Figure 3, as a result of the cell protection effect test for UVB stimulation, the effect was the best in the ethanol extract, and the protective effect was significantly increased at 0.5 μg / ml than at 1 μg / ml, and the finger root root The cell protection effect of the stem ethanol extract against UVB was the highest.
(2) 콜라게나아제 생성 저해 실험(2) Collagenase production inhibition experiment
핑거루트뿌리줄기 에탄올 추출물의 0.5μg/ml, 1.0μg/ml, 2.5μg/ml에서의 콜라게나아제 생성((Pro-collagen synthesis) 저해 효능 시험을 수행하였고, 결과를 하기 표 4에 나타내었다. 양성대조군은 TFG-베타1 100ng/ml이며, 대조군은 에탄물 추출물 미처리군이다.Collagenase production (Pro-collagen synthesis) inhibitory efficacy test was performed at 0.5 μg / ml, 1.0 μg / ml, and 2.5 μg / ml of finger root rhizome ethanol extract, and the results are shown in Table 4 below. The positive control group was TFG-beta1 100ng/ml, and the control group was an ethane water extract untreated group.
구분division MMP-1 생성량(대조군 대비 %)MMP-1 production (% compared to control)
대조군 control group 100%100%
양성대조군positive control 63.5%63.5%
에탄올 추출물 0.5μg/mlEthanol extract 0.5μg/ml 75.6%75.6%
에탄올 추출물 1.0μg/mlEthanol extract 1.0μg/ml 70.8%70.8%
에탄올 추출물 2.5μg/mlEthanol extract 2.5μg/ml 63.3%63.3%
상기 표 4의 콜라게나아제 생성 저해 실험을 통해, 핑거루트뿌리줄기 에탄올 추출물이 콜라게나아제 활성 억제 효과가 있고, 이를 통해 피부 주름 개선 활성 효과가 있음을 확인할 수 있었다.Through the collagenase production inhibition experiment in Table 4, it was confirmed that the ethanol extract of the finger root rhizome has an inhibitory effect on collagenase activity, and through this, there is an active effect on improving skin wrinkles.
준비예 2 : 핑거루트뿌리줄기 추출물의 분획물 제조Preparation Example 2: Preparation of fractions of finger root rhizome extract
핑거루트뿌리줄기 분말 100g을 취하여 에탄올 1L를 넣고 셰이커를 이용하여 24시간 동안 25℃에서 추출하였다. 필터(Whatman No.2 filter paper)를 이용하여 필터링하여 핑거루트뿌리줄기 에탄올 추출물을 수득하였다. 핑거루트뿌리줄기 에탄올 추출물 1L 중 100ml를 취하여 증류수를 200ml 첨가하였다.100 g of finger root rhizome powder was added to 1 L of ethanol and extracted at 25° C. for 24 hours using a shaker. Finger root rhizome ethanol extract was obtained by filtering using a filter (Whatman No.2 filter paper). 100 ml of 1 L of finger root rhizome ethanol extract was taken and 200 ml of distilled water was added.
핑거루트뿌리줄기 에탄올 추출물과 증류수의 혼합물을 진공 상태에서 농축하여 에탄올을 모두 날린 후 분액 깔대기에 옮겼다. 여기에 디클로로포름 총 2L를 넣고 충분히 셰이킹(shaking)하여 방치한 뒤 분리시켰고 하층액을 수집하여 농축하였다.A mixture of finger root rhizome ethanol extract and distilled water was concentrated in vacuo to remove all ethanol, and then transferred to a separatory funnel. A total of 2 L of dichloroform was added thereto, sufficiently shaken, and then separated, and the lower layer was collected and concentrated.
디클로로포름 분획 후에는 에틸아세테이트 총 1L를 넣고 충분히 셰이킹하여 방치한 뒤 분리하여 상층액을 수집하여 농축하였다. 에틸아세테이트를 제거하고 남은 물층은 동결건조하여 파우더 형태로 만들었다. 농축액과 파우더는 모두 DMSO로 재용해한 후 이어서 0.22um 멸균필터로 여과하고, 분석 전까지 -20℃에서 보관하여, 핑거루트뿌리줄기 에탄올 추출물에 대한 에탄올 분획물, 디클로로포름 분획물, 에틸아세테이트 분획 및 물 분획물을 각각 수득하였다.After the dichloroform fractionation, a total of 1 L of ethyl acetate was added, sufficiently shaken, separated, and the supernatant was collected and concentrated. Ethyl acetate was removed and the remaining water layer was lyophilized to form a powder. Both concentrate and powder were re-dissolved in DMSO, then filtered through a 0.22um sterile filter, and stored at -20 ° C until analysis, ethanol fraction, dichloroform fraction, ethyl acetate fraction and water fraction for finger root rhizome ethanol extract were respectively obtained.
실험예 3 : 핑거루트뿌리줄기 에탄올 추출 분획물의 세포 독성 실험Experimental Example 3: Cytotoxicity test of ethanol-extracted fractions of finger root rhizome
준비예 2에서 수득한 에탄올 추출 분획물에 대한 세포독성을 실시하였으며, 세포배양 및 세포독성 실험은 다음과 같다.Cytotoxicity was performed on the ethanol-extracted fraction obtained in Preparation Example 2, and cell culture and cytotoxicity experiments were as follows.
세포독성 실험에 사용된 인체 피부 섬유아세포주인 Hs68세포는 ATCC(American Type Culture Collection, Manassas, VA, USA)에서 구입하였다. 10% FBS와 페니실린(penicillin, 100unit/ml), 스트렙토마이신(streptomycin, 50μg/ml)이 함유된 DMEM(Dulbecco’s Modified Eagle’s Medium)배지를 사용하여 37℃, 5% 이산화탄소(CO2) 및 95% 습공기(humid air)로 조절된 배양기(Thermo Scientific, Tewksbury, MA, USA)에서 배양하였다. Hs68세포를 96-well plate에 1.0×104cells/well의 농도로 분주하여 24시간 배양 후 배지를 샘플이 함유되고, FBS가 함유되지 않은 배지로 교체하였다. 24시간 시료 처리 후 MTT(1 mg/ml)용액 20uL를 각 well에 첨가하고, 2시간 동안 배양하였다. 마지막으로 상층액을 제거하고, 생존세포에서 생성된 청색 포르마잔(formazan)결정을 DMSO로 가용화 시켜 Microplate reader(BioTek, Inc., Winooski, VT,USA)를 사용하여 550nm에서의 흡광도를 측정하였다. 시료처리 시에는 DMSO의 최종 농도가 0.1%(v/v) 미만이 되도록 샘플을 배지로 희석하여 사용하였다.Hs68 cells, a human skin fibroblast cell line used in the cytotoxicity test, were purchased from ATCC (American Type Culture Collection, Manassas, VA, USA). DMEM (Dulbecco's Modified Eagle's Medium) medium containing 10% FBS, penicillin (100 units/ml), and streptomycin (50 μg/ml) was used at 37°C, 5% carbon dioxide (CO2) and 95% humid air ( humid air) and cultured in an incubator (Thermo Scientific, Tewksbury, MA, USA). Hs68 cells were dispensed in a 96-well plate at a concentration of 1.0×10 4 cells/well, and after culture for 24 hours, the medium was replaced with a medium containing the sample and not containing FBS. After 24 hours of sample treatment, 20uL of MTT (1 mg/ml) solution was added to each well and incubated for 2 hours. Finally, the supernatant was removed, and blue formazan crystals generated from viable cells were solubilized with DMSO, and absorbance at 550 nm was measured using a Microplate reader (BioTek, Inc., Winooski, VT, USA). During sample processing, the sample was diluted with medium so that the final concentration of DMSO was less than 0.1% (v/v).
각 분획물의 농도에 따른 세포독성을 평가하기 위해 hs68세포에 0.1, 0.5, 1, 5μg/ml 를 처리하였다. 농도 별로 처리한 결과, 도 4의 A 및 B에 나타낸 바와 같이, 물 분획물을 제외한 나머지 분획물의 5μg/ml에서 모두 세포독성을 나타냈다.To evaluate the cytotoxicity according to the concentration of each fraction, hs68 cells were treated with 0.1, 0.5, 1, or 5 μg/ml. As a result of treatment by concentration, as shown in A and B of FIG. 4, all of the fractions except the water fraction showed cytotoxicity at 5 μg/ml.
실험예 4 : 핑거루트뿌리줄기 에탄올 추출 분획물의 UVB 자극에 대한 세포 보호 효과 실험Experimental Example 4: Cell protection effect test for UVB stimulation of ethanol-extracted fractions of finger root rhizome
Hs68세포를 96-well plate에 1.0×104 cells/well의 농도로 분주하여 24시간 동안 배양한 후, 각 well에 FBS가 없는 배지로 샘플을 희석한 후 처리하여 24시간 동안 배양하였다.Hs68 cells were dispensed in a 96-well plate at a concentration of 1.0 × 10 4 cells/well and cultured for 24 hours, and then the samples were diluted with FBS-free medium in each well, treated, and cultured for 24 hours.
그 후 UVB 램프(Sankyo Denki Lamps, GL20SE, Marine, Japan)를 이용하여 UVB(30mJ/cm2)를 조사하였고, UV LIGHT METER(LT Lutron, UV-340A, Taiwan)를 사용하여 자외선 강도를 모니터링 하였다. 모든 UVB 조사는 96-well plate에 부착된 세포에 PBS를 얇게 도포한 후 수행하였다. 조사 후 FBS가 없는 배지에서 샘플을 희석하여 24시간 동안 세포에 처리하였다. 대조군은 UVB 조사 없이 동일한 조건으로 진행되었다.Then, UVB (30mJ/cm 2 ) was irradiated using a UVB lamp (Sankyo Denki Lamps, GL20SE, Marine, Japan), and ultraviolet intensity was monitored using a UV LIGHT METER (LT Lutron, UV-340A, Taiwan). . All UVB irradiation was performed after thinly applying PBS to the cells attached to the 96-well plate. After irradiation, the samples were diluted in FBS-free medium and treated with cells for 24 hours. The control group was run under the same conditions without UVB irradiation.
에탄올 추출 분획물 각각에 대한 UVB조사에 대한 세포 보호효과를 평가하기 위하여 세포에 UVB조사 전 후에 각 용매별 추출물을 0.1, 0.5, 1, 5μg/ml 농도로 처리하였다. 그 결과, 도 5의 A 및 B에 나타낸 바와 같이 물 분획물만이 5μg/ml까지 독성 없이 보호효과 활성이 유지되었다.In order to evaluate the cell protection effect on UVB irradiation for each of the ethanol-extracted fractions, the extracts for each solvent were treated at concentrations of 0.1, 0.5, 1, and 5 μg/ml before and after UVB irradiation on the cells. As a result, as shown in A and B of FIG. 5, only the water fraction maintained the protective effect activity without toxicity up to 5 μg/ml.
핑거루트뿌리줄기 에탄올 추출물의 물 분획물을 선택하여 농도별(1, 5, 25, 50μg/ml) 세포독성과 UVB에 대한 세포 보호효과를 측정하였고, 그 결과를 도 6에 나타내었다. 세포독성 실험결과인 도 6의 A를 살펴보면, 세포독성의 경우 25μg/ml까지 세포독성을 나타내지 않았으나, 50μg/ml에서 세포 생존율이 86%로 감소하여 독성을 나타내는 것으로 판단하였다. 한편, 세포 보호효과의 경우, 세포보호 실험결과인 도 6의 B에 나타난 바와 같이 5μg/ml, 25μg/ml에서 세포 보호효과를 나타내었다.The water fraction of the finger root rhizome ethanol extract was selected and the cytotoxicity and cell protection effect against UVB at each concentration (1, 5, 25, 50 μg/ml) were measured, and the results are shown in FIG. 6 . Looking at the cytotoxicity test results of FIG. 6A, in the case of cytotoxicity, cytotoxicity was not shown up to 25 μg / ml, but at 50 μg / ml, the cell viability was reduced to 86%, which was determined to indicate toxicity. On the other hand, in the case of the cell protection effect, as shown in B of FIG. 6, which is the result of the cell protection experiment, the cell protection effect was shown at 5 μg/ml and 25 μg/ml.
위 시험결과, 핑거루트뿌리줄기 에탄올 추출물의 물 분획물 25μg/ml에서 세포생존율이 약간 감소하는 경향을 보였으므로, 샘플 처리시 농도의존적으로 증가하는 이상적인 결과를 도출하기 위하여 최고농도를 20μg/ml으로 설정하였다.As a result of the above test, the cell viability tended to decrease slightly at 25μg/ml of the water fraction of the finger root rhizome ethanol extract. Therefore, the highest concentration was set at 20μg/ml in order to obtain an ideal result that increases in a concentration-dependent manner during sample treatment did
핑거루트뿌리줄기 에탄올 추출물의 물 분획물 1 ~ 20μg/ml 의 세포독성 및 UVB에 대한 세포 보호효과를 측정한 결과, 20μg/ml까지 독성을 나타내지 않았고(도 7의 A 참조), UVB에 의해 감소된 세포생존율을 농도의존적으로 증가시켰다(도 7의 B 참조).As a result of measuring the cytotoxicity and cell protection effect against UVB of 1 to 20 μg/ml of the water fraction of the finger root rhizome ethanol extract, no toxicity was shown up to 20 μg/ml (see A in FIG. 7), and the UVB-induced Cell viability was increased in a concentration dependent manner (see B in FIG. 7 ).
실험예 5 : 핑거루트뿌리줄기 에탄올 추출물의 물 분획물에 대한 세포 내 콜라겐 영향 평가Experimental Example 5: Evaluation of Intracellular Collagen Effect on Water Fraction of Finger Root Rhizome Ethanol Extract
UVB 조사는 세포의 콜라겐 생성을 감소시킨다. 따라서 핑거루트 추출물의 물 분획물이 세포 내 콜라겐 양에 미치는 영향을 측정하였다. 실험방법은 하기와 같다.UVB irradiation reduces cell collagen production. Therefore, the effect of the water fraction of the fingerroot extract on the amount of intracellular collagen was measured. The experimental method is as follows.
(1) MMP-1, MMP-3 및 수용성 콜라겐 생성량 측정(1) Measurement of MMP-1, MMP-3 and water-soluble collagen production
UVB 조사에 의해 합성이 증가되는 MMP-1과 MMP-3의 측정은 human MMP-1, MMP-3 ELISA kit(Merck & Co. Inc., Whitehouse Station, NJ, USA)를 이용하여 enzyme-linked immunosorbent assay 방법으로 배지 중의 pro-MMP-1과 MMP-3의 생성량을 측정하였다. UVB 조사 후 수용성 콜라겐 생성량은 SircolTM soluble collagen assay kit를 사용하여 측정하였다. 세포를 배양한 배지를 수집하여 Sirco dye reagent와 혼합, 반응하여 원심분리 후 차가운 산-염 세척액(acid-salt washing reagent)을 침전물에 첨가하여 혼합하였다. 혼합물을 원심분리한 후 침전물을 알칼리 시약(alkali reagent)를 사용하여 용해시키고, 555 nm에서 흡광도를 측정하였고 실험결과를 도 8 의 A에 나타내었다.Measurement of MMP-1 and MMP-3, whose synthesis is increased by UVB irradiation, was performed using enzyme-linked immunosorbents using the human MMP-1 and MMP-3 ELISA kit (Merck & Co. Inc., Whitehouse Station, NJ, USA). The production amount of pro-MMP-1 and MMP-3 in the medium was measured by the assay method. After UVB irradiation, the amount of soluble collagen produced was measured using SircolTM soluble collagen assay kit. The medium in which the cells were cultured was collected, mixed with and reacted with Sirco dye reagent, centrifuged, and then cold acid-salt washing reagent was added to the precipitate and mixed. After centrifuging the mixture, the precipitate was dissolved using an alkali reagent, and the absorbance was measured at 555 nm, and the experimental results are shown in FIG. 8A.
도 8의 A를 살펴보면, UVB는 세포 내 콜라겐 양을 감소시켰고, 1μg/ml부터 20μg/ml까지 물 분획물 처리시 그 농도가 증가함에 따라 콜라겐 수준이 농도의존적으로 증가하였다.Looking at A of FIG. 8, UVB decreased the amount of intracellular collagen, and the collagen level increased in a concentration-dependent manner as the concentration increased when the water fraction was treated from 1 μg/ml to 20 μg/ml.
이때, UVB 조사는 피부에 가장 많이 존재하는 단백질인 Type 1 콜라겐을 분해하는 효소인 MMP-1(Matrix MetalloProtease)의 생성을 증가시켜 콜라겐의 분해를 촉진한다. 따라서 MMP-1 생성에 미치는 핑거루트 추출물의 물 분획물의 영향을 전술한 방법으로 평가하였고 그 결과를 도 8의 B에 나타내었다. UVB조사시 MMP-1 생성이 증가하였고, 물 분획물 처리시 1μg/ml부터 20μg/ml까지 농도가 증가함에 따라 MMP-1생성이 감소하였다.At this time, UVB irradiation promotes the decomposition of collagen by increasing the production of MMP-1 (Matrix MetalloProtease), an enzyme that decomposes type 1 collagen, which is the most abundant protein in the skin. Therefore, the effect of the water fraction of the fingerroot extract on the production of MMP-1 was evaluated by the method described above, and the results are shown in FIG. 8B. The production of MMP-1 increased upon UVB irradiation, and the production of MMP-1 decreased as the concentration increased from 1 μg/ml to 20 μg/ml when the water fraction was treated.
또한, MMP-3는 MMP-1을 활성화시켜 콜라겐의 분해를 촉진하므로, MMP-1과 동일한 방법으로 MMP-3 생성량을 측정하였으며, 실험결과를 도 8의 C에 나타내었다. UVB조사시 MMP-3 생성이 증가하였고, 물 분획물 처리시 1μg/ml부터 20μg/ml까지 농도가 증가함에 따라 MMP-3생성이 감소하였다.In addition, since MMP-3 promotes collagen degradation by activating MMP-1, the amount of MMP-3 produced was measured in the same manner as in MMP-1, and the experimental results are shown in FIG. 8C. The production of MMP-3 increased upon UVB irradiation, and the production of MMP-3 decreased as the concentration increased from 1 μg/ml to 20 μg/ml when the water fraction was treated.
실험예 6 : 핑거루트뿌리줄기 에탄올 추출물의 물 분획물에 대한 세포 내 항산화 영향 평가Experimental Example 6: Evaluation of intracellular antioxidant effect on the water fraction of finger root rhizome ethanol extract
UVB 조사는 세포 내 Reactive oxygen species(ROS, 활성산소종)의 생성을 촉진시킨다. 이러한 비정상적인 활성산소종의 증가는 산화적 스트레스를 유발하고 진피 섬유아세포(fibroblast)에서 MMPs을 유도하여 피부노화를 촉진한다. 따라서 핑거루트뿌리줄기 추출물의 물 분획물의 ROS 생성에 미치는 영향을 평가하였다. 실험방법은 하기와 같다.UVB irradiation promotes the generation of intracellular reactive oxygen species (ROS). The increase in these abnormal reactive oxygen species induces oxidative stress and induces MMPs in dermal fibroblasts to promote skin aging. Therefore, the effect of the water fraction of the finger root rhizome extract on ROS production was evaluated. The experimental method is as follows.
(1) ROS 생성 측정(1) Measurement of ROS generation
활성산소(Reactive Oxygen Species, ROS) 생성을 측정하기 위해 Hs68 세포에 샘플을 24시간 동안 전처리하고, PBS로 세척한 후 세포를 UVB(30mJ/cm2)로 조사하였다. UVB 조사 후 세포에 샘플을 30분간 처리한 후 25uM의 DCFH-DA로 염색하였다. 세포 내 ROS 생성에 해당하는 형광 강도는 485nm의 여기 파장 및 530nm의 방출 파장에서 2시간 동안 fluorescent spectrophotometer(Perkin-Elmer, Norwalk, CT, USA)로 측정하였다.To measure the production of reactive oxygen species (ROS), Hs68 cells were pretreated with samples for 24 hours, washed with PBS, and then irradiated with UVB (30 mJ/cm2). After UVB irradiation, the cells were treated with samples for 30 minutes, and then stained with 25uM DCFH-DA. Fluorescence intensity corresponding to intracellular ROS generation was measured with a fluorescent spectrophotometer (Perkin-Elmer, Norwalk, CT, USA) for 2 hours at an excitation wavelength of 485 nm and an emission wavelength of 530 nm.
핑거루트 에탄올 추출물의 물 분획물 1 ~ 20μg/ml 의 농도에 따른 ROS 활성산소(Reactive Oxygen Species, ROS) 생성을 측정하기 위한 형광 강도 측정 그래프를 도 9에 나타내었다.9 shows a graph of fluorescence intensity measurement for measuring ROS generation of reactive oxygen species (ROS) according to concentrations of 1 to 20 μg/ml of the water fraction of the finger root ethanol extract.
도 9를 살펴보면, UVB조사는 세포 내 ROS의 생성을 증가시켰으며, 물 분획물 처리시 농도의존적으로 ROS 생성을 감소시킴을 확인할 수 있었다.Referring to FIG. 9 , it was confirmed that UVB irradiation increased intracellular ROS generation, and decreased ROS generation in a concentration-dependent manner when the water fraction was treated.
실시예 1 : 에멀젼 제형의 피부탄력 개선 화장료(화장품)의 제조Example 1: Preparation of skin elasticity improving cosmetics (cosmetics) of emulsion formulation
반응기에 정제수 및 아크릴레이트/C10-30알킬아크릴레이트크로스폴리머(Carbopol  ETD-2020) 0.28 중량% 및 정제수 99.72 중량%를 투입한 후, 70℃ 하에서 3,000rpm 속도로 60분간 교반하여 제1액을 제조하였다.Purified water and acrylate/C 10-30 alkyl acrylate crosspolymer (Carbopol  ETD-2020) 0.28% by weight and 99.72% by weight of purified water were added, and then stirred at 3,000 rpm for 60 minutes at 70 ° C to prepare a first solution.
피부 컨디셔닝제, 보습제, 보존제 및 가교제를 포함하는 제2액을 준비한 후, 제1액 100 중량부에 대하여 제2액 19.0 중량부로 제1액이 제조된 반응기에 투입한 후, 70℃ 하에서 2,500rpm 속도로 60분간 교반을 수행하였다. 이때, 제2액의 조성은 하기 표 5과 같다.After preparing a second liquid containing a skin conditioning agent, a moisturizer, a preservative, and a crosslinking agent, 19.0 parts by weight of the second liquid based on 100 parts by weight of the first liquid was introduced into the reactor where the first liquid was prepared, and then 2,500 rpm at 70 ° C. Stirring was performed for 60 minutes at speed. At this time, the composition of the second liquid is shown in Table 5 below.
제2액2nd liquid 성분ingredient 중량%weight%
보습제moisturizer 글리세린glycerin 25.725.7
부틸렌글라이콜Butylene Glycol 14.714.7
미백제whitening agent 나이아신아마이드Niacinamide 14.714.7
보존제preservative 1,2-헥산다이올1,2-Hexanediol 14.714.7
가교제cross-linking agent 소듐하이알루로네이트sodium hyaluronate 1111
피부컨디셔닝제skin conditioning agent 글리세레스-26glycereth-26 9.59.5
알란토인allantoin 2.22.2
하이드롤라이즈드콜라겐hydrolyzed collagen 7.27.2
아데노신adenosine 0.30.3
총합 total 100100
다음으로, 피부 컨디셔닝제, 계면활성제, 보습제, 유화제 및 유화안정제를 포함하는 제3액을 제조한 후, 제1액 100 중량부에 대하여 제3액 10.8 중량부로 제2액이 혼합된 반응기에 투입한 후, 75℃ 하에서 2,500rpm 속도로 50분간 교반을 수행하였다. 이때, 제3액의 조성은 하기 표 6와 같다.Next, after preparing a third liquid containing a skin conditioning agent, surfactant, moisturizer, emulsifier, and emulsion stabilizer, 10.8 parts by weight of the third liquid based on 100 parts by weight of the first liquid is introduced into the reactor in which the second liquid is mixed. After that, stirring was performed at 2,500 rpm for 50 minutes at 75 °C. At this time, the composition of the third liquid is shown in Table 6 below.
제3액3rd liquid 성분ingredient 중량%weight%
피부컨디셔닝제skin conditioning agent 해바라기씨오일sunflower seed oil 16.816.8
다이메티콘dimethicone 15.515.5
세틸에틸헥사노에이트Cetylethylhexanoate 12.9 12.9
글리세릴스테아레이트Glyceryl Stearate 12.312.3
계면활성제Surfactants 피이지-100스테아레이트PEG-100 Stearate 11.5 11.5
보습제moisturizer 카프릴릭/카프릭트라이글리세라이드Caprylic/Capric Triglyceride 6.56.5
유화안정제emulsion stabilizer 세테아릴알코올Cetearyl Alcohol 6.56.5
유화제 emulsifier 폴리솔베이트60Polysorbate 60 6.56.5
스테아릭애씨드Stearic Acid 6.56.5
솔비탄세스퀴올리에이트 Sorbitan Sesquioleate 55
총합 total 100100
다음으로, 제3액이 혼합된 반응기의 온도를 40℃로 낮춘 후, pH 조절제인 알지닌을 제1액 100 중량부에 대하여 0.28 중량부의 양으로 투입한 후, 40℃ 하에서 2,000rpm 속도로 30분간 교반을 수행하였다.다음으로, 알지닌이 혼합된 반응기에 진주 추출물 및 천연식물 복합 추출물을 포함하는 기능성 추출물, 락토바실러스발효 용해물, 콜라겐 합성 촉진제 및 향료를 포함하는 제4액을 제조한 후, 제1액 100 중량부에 대하여 제4액을 11.6 중량부로 pH조절제가 혼합된 반응기에 투입한 후, 40℃ 하에서 2,000rpm 속도로 30분간 교반을 수행하였다. 이때, 제4액의 조성은 하기 표 7과 같다.Next, after lowering the temperature of the reactor in which the third liquid was mixed to 40 ° C, 0.28 parts by weight of arginine as a pH adjuster was added to 100 parts by weight of the first liquid, and then 30 at 2,000 rpm at 40 ° C. Next, a fourth liquid containing functional extracts including pearl extract and natural plant complex extract, Lactobacillus fermentation lysate, collagen synthesis promoter and flavoring was prepared in a reactor in which arginine was mixed. , 11.6 parts by weight of the fourth liquid based on 100 parts by weight of the first liquid was introduced into the reactor in which the pH adjusting agent was mixed, and stirring was performed at 40 ° C. at a speed of 2,000 rpm for 30 minutes. At this time, the composition of the fourth liquid is shown in Table 7 below.
제4액4th liquid 성분ingredient 중량%weight%
기능성 추출물functional extract 진주추출물pearl extract 1818
천연식물 복합 추출물Natural Plant Complex Extract 73.873.8
락토바실러스발효 용해물Lactobacillus fermentation lysate 66
콜라겐합성 촉진제collagen synthesis promoter 알에이치-올리고펩타이드-1RH-Oligopeptide-1 1.81.8
향료Spices 0.40.4
총합 total 100100
이때, 진주 추출물은 진주 100g을 분쇄한 후 3L의 70 부피% 에탄올 수용액을 용매로 사용하여 12시간 가온 환류추출한 후, 냉침시키고, 1.2㎛ 투과 사이즈를 갖는 여과지로 여과하여 여과액을 수득한 다음, 수득된 여과액을 감압농축 및 감압 건조로 농축한 후, 건조 및 분쇄하여 제조한 것을 사용하였다.그리고, 핑거루트뿌리줄기 추출물은 에탄올 추출물의 물 분획물로서, 다음과 같은 공정으로 제조한 핑거루트뿌리줄기 에탄올 추출물의 물 분획물을 사용하였다.At this time, the pearl extract was pulverized with 100 g of pearls, extracted under reflux by heating for 12 hours using 3 L of 70% ethanol aqueous solution as a solvent, cooled, and filtered with a filter paper having a 1.2 μm permeation size to obtain a filtrate, The obtained filtrate was concentrated under reduced pressure and dried under reduced pressure, and then dried and pulverized to be used. In addition, the finger root rhizome extract is the water fraction of the ethanol extract, and is prepared by the following process. The water fraction of the stem ethanol extract was used.
핑거루트뿌리줄기 분말 100g을 취하여 에탄올 1L를 넣고 셰이커를 이용하여 24시간 동안 25℃에서 추출하였다. 다음으로, 필터(Whatman No.2 filter paper)를 이용하여 필터링하여 핑거루트뿌리줄기 에탄올 추출물을 수득하였다. 핑거루트뿌리줄기 에탄올 추출물 1L 중 100ml를 취하여 증류수를 200ml 첨가하였다. 다음으로, 핑거루트뿌리줄기 에탄올 추출물과 증류수의 혼합물을 진공 상태에서 농축하여 에탄올을 모두 날린 후 분액 깔대기에 옮겼다. 여기에 디클로로포름 총 2L를 넣고 충분히 셰이킹(shaking)하여 방치한 뒤 분리시켰고 하층액을 수집하여 농축하였다. 다음으로, 디클로로포름 분획 후에는 에틸아세테이트 총 1L를 넣고 충분히 셰이킹하여 방치한 뒤 상층액을 분리한 다음 하층액을 동결건조하여 물 분획물을 수득한 후, 이를 동결 건조하여 핑거루트뿌리줄기 에탄올 추출물의 물 분획물 건조 분말을 수득하였다.100 g of finger root rhizome powder was added to 1 L of ethanol and extracted at 25° C. for 24 hours using a shaker. Next, the finger root rhizome ethanol extract was obtained by filtering using a filter (Whatman No.2 filter paper). 100 ml of 1 L of finger root rhizome ethanol extract was taken and 200 ml of distilled water was added. Next, the mixture of the finger root rhizome ethanol extract and distilled water was concentrated in a vacuum to remove all ethanol, and then transferred to a separatory funnel. A total of 2 L of dichloroform was added thereto, sufficiently shaken, and then separated, and the lower layer was collected and concentrated. Next, after the dichloroform fractionation, a total of 1 L of ethyl acetate was added, shaken sufficiently, and the supernatant was separated, and the lower layer was lyophilized to obtain a water fraction, which was then freeze-dried to obtain an ethanol extract of finger root rhizome A dry powder of the water fraction was obtained.
그리고, 천연식물 복합 추출물의 조성비는 하기 표 8과 같으며, 핑거루트뿌리줄기 추출물 외에 다른 식물 추출물은 상업적으로 구매하였다.In addition, the composition ratio of the natural plant composite extract is shown in Table 8 below, and other plant extracts other than the finger root rhizome extract were purchased commercially.
쳔연식물 복합 추출물Natural plant complex extract 중량부parts by weight
핑거루트뿌리줄기추출물Finger root rhizome extract 100100
병풀추출물centella asiatica extract 2020
비타민나무추출물Vitamin Tree Extract 0.40.4
녹차추출물green tea extract 0.40.4
마트리카리아추출물Matricaria Extract 0.40.4
저단선추출물low sweetness extract 0.20.2
뽕나무잎추출물Mulberry Leaf Extract 0.20.2
산사나무열매추출물Hawthorn Fruit Extract 0.20.2
페퍼민트추출물Peppermint Extract 0.20.2
히비스커스꽃추출물hibiscus flower extract 0.20.2
로즈마리추출물rosemary extract 0.20.2
모과추출물Chinese quince extract 0.20.2
레드초크베리추출물Red Chokeberry Extract 0.20.2
다음으로, 제4액을 혼합 교반하여 제조한 용액을 여과 및 탈포한 후, 숙성시켜서 최종적으로 화장료를 제조하였다. 제조된 화장료는 에멀젼 제형이었으며, 25℃에서 점도 47,000 ~ 49,000cP 및 pH 6.4 ~ 6.6 정도였다.비교예 1 : 피부탄력 화장료의 제조 Next, the solution prepared by mixing and stirring the fourth liquid was filtered and degassed, and then aged to finally prepare cosmetics. The prepared cosmetic was an emulsion formulation, and had a viscosity of 47,000 to 49,000 cP and a pH of about 6.4 to 6.6 at 25°C. Comparative Example 1: Preparation of skin elasticity cosmetics
한국 등록특허 10-2288066호에 개시된 제1혼합제(유언제, 유화제, 착향제), 제2혼합제(정제수, 아데노신, 나이아신아마이드) 및 제3혼합제(천연식물유래 추출물, 천연식물유래 발효여과물, 컨디셔닝제, 안정제, 보전제, 금속이온봉쇄제)를 각각 제조한 후, 다음과 같은 공정을 통해, 피부탄력 화장료를 제조하였다.Korean Patent No. 10-2288066 discloses a first mixture (emulsion agent, emulsifier, flavoring agent), a second mixture (purified water, adenosine, niacinamide) and a third mixture (natural plant-derived extract, natural plant-derived fermented filtrate, Conditioning agent, stabilizer, preservative, sequestering agent) were prepared, respectively, and skin elasticity cosmetics were prepared through the following process.
하기 표 9에서 제3혼합제의 컨디셔닝제는 아세틸헥사펩타이드-8(Acetyl Hexapeptide-8), 카퍼트라이펩타이드-1(Copper Tripeptide-1), 에스에이치올리고펩타이드-10(sh-Oligopeptide-10), 부틸렌글라이콜(Butylene Glycol), 프로필렌글라이콜(Propylene Glycol), 하이알루로닉애씨드(Hyaluronic Acid), 메틸퍼플루오로이소부틸에터(Methyl Perfluoroisobutyl Ether)를 동일 중량비로 혼합하여 제조한 것을 사용하였다.In Table 9, the conditioning agents of the third mixture include Acetyl Hexapeptide-8, Copper Tripeptide-1, sh-Oligopeptide-10, Butylene Gly It was prepared by mixing Butylene Glycol, Propylene Glycol, Hyaluronic Acid, and Methyl Perfluoroisobutyl Ether in equal weight ratios. .
제1혼합제를 제1용기에 투입에 투입, 분산, 용해 및 혼합한 후(11단계), 제2혼합제를 분산, 용해 및 혼합하였다(21단계), 다음으로, 제3혼합제를 분산, 용해 및 혼합하였다(31단계). 상기 11단계에서 혼합된 제1혼합제와, 제21단계에서 혼합된 제2혼합제 및 제31단계에서 혼합된 제3혼합제는 각각 유화기로 이송되어 32단계에서 유화기 등에서 혼합 교반되었다. 그리고, 상기 32단계에서 혼합교반된 혼합물은 여과(제33단계) 후, 진공탈포(34단계)를 거쳐 저장탱크로 이송되어 저장 및 숙성(35단계)과정을 수행하여 피부탄력 화장료를 제조하였다. 제조한 화장료는 용기에 투입하여 보관하였다.After putting, dispersing, dissolving, and mixing the first mixture into the first container (step 11), the second mixture was dispersed, dissolved, and mixed (step 21). Next, the third mixture was dispersed, dissolved, and mixed. Mixed (step 31). The first mixture mixed in step 11, the second mixture mixed in step 21, and the third mixture mixed in step 31 were each transferred to an emulsifier and mixed and stirred in an emulsifier or the like in step 32. In addition, the mixed and stirred mixture in step 32 was filtered (step 33), vacuum degassed (step 34), and then transferred to a storage tank to perform storage and aging (step 35) to prepare skin elasticity cosmetics. The prepared cosmetic was put into a container and stored.
구분division 성분ingredient 함량(중량%)Content (% by weight)
제1혼합제
(10)
1st mixture
(10)
유화제 emulsifier 폴리소르베이트80polysorbate 80 4.04.0
유연제softener 사이클로펜타실록세인Cyclopentasiloxane 7.57.5
착향제flavoring agent 조합향료Mixed Spices 0.250.25
제2혼합제
(20)
2nd mixture
(20)
정제수Purified water 12.512.5
아데노신adenosine 0.080.08
나이아신아마이드Niacinamide 2.52.5
제3혼합제
(30)
3rd mixture
(30)
핑거루트뿌리 줄기 추출물Fingerroot Root Stem Extract 4.04.0
병풀 추출물centella extract 2.52.5
쇠비름 추출물purslane extract 2.52.5
녹두 추출물mung bean extract 1.01.0
유칼립투스잎 추출물Eucalyptus Leaf Extract 1.01.0
서양산사자 추출물Western Lion Extract 1.01.0
진흙버섯 추출물mud mushroom extract 0.50.5
마트리카리아 추출물Matricaria Extract 0.50.5
버니니아풍년화 추출물Virginia Plum Blossom Extract 2.52.5
콜라겐 추출물collagen extract 2.52.5
연꽃캘러스 배양 추출물Lotus Callus Culture Extract 1.21.2
뽕나무껍질 추출물Mulberry Bark Extract 1.21.2
밤부사불가리스 추출물BAMBUSA VULGARIS EXTRACT 0.50.5
비피다발효 여과물bifida fermentation filtrate 7.57.5
갈락토미세스 발효 여과물Galactomyces fermentation filtrate 2.52.5
효모/동충하초 발효 여과물Yeast/cordyceps ferment filtrate 2.52.5
컨디셔닝제conditioning agent 36.5736.57
안정제stabilizator 하이드록시에틸셀룰로오스Hydroxyethyl Cellulose 0.70.7
보존제 preservative 1,2-헥산다이올1,2-Hexanediol 2.02.0
금속이온봉쇄제sequestering agent 다이소듐이디티에이Disodium EDT 0.50.5
총 중량% Total weight % 100100
실험예 7 : 눈가 주름 개선 효과 측정Experimental Example 7: Measuring the wrinkle improvement effect around the eyes
실시예 1 및 비교예 1의 화장료의 사용 전후 눈가 주름 개선 효과를 측정하였으며, PRIMOS(Phaseshift rapid in-vivo measurement of skin)를 이용한 눈가 주름 측정을 수행하였고, 평가 결과를 하기 표 10에 나타내었다. PRIMOS 분석 변수로는 Ra와 R3z를 선정하였으며, 변수 Ra(Arithmetic roughness average)는 PRIMOS로 측정된 주름의 거칠기 단면 피크(peak)에 대한 산술 평균값으로 Ra값이 작아질수록 피부 주름의 깊이가 낮아져 주름이 개선됨을 의미하며, 단위는 ㎛이다.The effect of improving wrinkles around the eyes before and after using the cosmetics of Example 1 and Comparative Example 1 was measured, and wrinkles around the eyes were measured using PRIMOS (Phaseshift rapid in-vivo measurement of skin), and the evaluation results are shown in Table 10 below. Ra and R3z were selected as PRIMOS analysis variables, and the variable Ra (arithmetic roughness average) is the arithmetic average value of the peak of the roughness section of wrinkles measured by PRIMOS. means improved, and the unit is μm.
변수 R3z(Base roughness depth)는 R3z1부터 R3z5까지 5가지의 단일 거칠기 깊이에 대한 산술 평균으로 나타낸다. 단일 거칠기 깊이는 거칠기 단면의 단일 평가 거리(Ir)에서 세번째로 높은 단면 peak과 세번째로 깊은 곡선 사이의 수직거리를 의미한다. R3z의 값이 작아질수록 피부의 주름 깊이가 낮아짐을 의미하며 주름 개선이 되었음을 의미한다. 단위는 ㎛이다. 일시적 눈가 주름 개선율은 하기 수학식 1에 따라 계산하였다.The variable R3z (Base roughness depth) is expressed as the arithmetic average of five single roughness depths from R3z1 to R3z5. The single roughness depth means the vertical distance between the third highest cross section peak and the third deepest curve at a single evaluation distance (Ir) of the roughness cross section. As the value of R3z decreases, it means that the depth of wrinkles in the skin decreases, which means that wrinkles are improved. Unit is μm. The temporary wrinkle improvement rate was calculated according to Equation 1 below.
[수학식 1][Equation 1]
눈가주름 개선율(%) = 100% - {(A-B)/B}×100%Periorbital wrinkle improvement rate (%) = 100% - {(A-B)/B}×100%
수학식 1에서, A는 제품 사용 후 측정값이고, B는 제품 사용 전 측정값이다.In Equation 1, A is a measured value after using the product, and B is a measured value before using the product.
구분division RaRa R3zR3z
Ra 측정값Ra measurements 눈가주름 개선율(Ra)Periorbital wrinkle improvement rate (Ra) R3z 측정값R3z measurements 눈가주름 개선율(R3z)Periorbital wrinkle improvement rate (R3z)
사용 전before use 15.86915.869 100%100% 42.23742.237 100%100%
비교예 1Comparative Example 1 15.01515.015 105.38%105.38% 40.25040.250 104.70%104.70%
실시예 1Example 1 14.99014.990 105.54%105.54% 40.12240.122 105.00%105.00%
눈가 주름을 분석한 결과, 비교예 1 및 실시예 1의 화장료 모두 사용 전과 비교하여 사용 후에서 변수 Ra와 R3z 모두 통계적으로 유의차 있게 일시적 눈가 주름 개선 효과를 나타냈으며(p<0.05), 비교예 1 보다 실시예 1이 상대적으로 좀 더 우수한 눈가 주름 개선율을 보였다.As a result of analyzing the wrinkles around the eyes, both the variables Ra and R3z showed a statistically significant temporary improvement in wrinkles around the eyes (p<0.05) after use compared to before and after use of the cosmetics of Comparative Example 1 and Example 1 (p<0.05), Comparative Example Example 1 showed a relatively better improvement rate of wrinkles around the eyes than Example 1.
실험예 8 : 피부 탄력 개선 효과 측정Experimental Example 8: Measurement of skin elasticity improvement effect
실시예 1 및 비교예 1의 화장료의 사용 전후 피부 탄력 개선 효과를 측정하였으며, Cutometer(Courage and Khazaka Electronic, Germany)를 이용하여 시험 부위를3회 측정하였으며, 3개의 값을 이용해 평균값을 구하였다. 측정 부위는 눈꼬리에서 3cm 떨어진 지점으로 측정하였다. Cutometer는 피부 표면에 음압을 가하여 피부가 탐침기 안으로 흡입되는 정도를 피부를 통과할 수 있는 광학시스템을 이용하여 측정한다. 이때 사용되는 빛은 적외선으로 피부를 통과하면서 감소되는 빛의 세기와 피부를 통과하지 않는 빛의 세기의 비율로 탄력의 정도를 측정한다. 탄력에 대한 Cutometer 측정 변수로는 R2(A.U.)를 선정하였다.The skin elasticity improvement effect was measured before and after using the cosmetics of Example 1 and Comparative Example 1, and the test site was measured three times using a Cutometer (Courage and Khazaka Electronic, Germany), and the average value was obtained using the three values. The measurement site was measured at a point 3 cm away from the outer corner of the eye. Cutometer applies negative pressure to the skin surface and measures the degree to which the skin is sucked into the probe using an optical system that can pass through the skin. The light used at this time is infrared, and the degree of elasticity is measured by the ratio of the intensity of light that is reduced while passing through the skin and the intensity of light that does not pass through the skin. R2 (A.U.) was selected as a cutometer measurement variable for elasticity.
변수 R2은 피부가 늘어날 수 있는 최대치에서 피부가 총 수축되는 길이와의 비를 나타내며, 피부의 재변형력인 총체적인 탄성을 나타낸다. 이 변수의 값은 1에 가까울수록 더욱 탄성적임을 의미한다. 피부 탄력 개선율은 하기 수학식 1에 따라 계산하였다. 측정은 사용 전(0주), 사용 2주 후 및 사용 4주 후 측정하였다.Variable R2 represents the ratio of the total contraction length of the skin at the maximum value at which the skin can be stretched, and represents the overall elasticity, which is the re-deformation force of the skin. The closer the value of this variable is to 1, the more elastic it is. The skin elasticity improvement rate was calculated according to Equation 1 below. Measurements were taken before use (0 weeks), after 2 weeks and after 4 weeks of use.
평가 기간 동안 시험 제품에 의한 피부 유해사례는 발생하지 않았으며, 피부 탄력 측정 결과는 하기 표 11과 같다.During the evaluation period, adverse skin events caused by the test product did not occur, and the skin elasticity measurement results are shown in Table 11 below.
[수학식 2][Equation 2]
피부 탄력 개선율(%) = {(B-A)/B}×100%Skin elasticity improvement rate (%) = {(B-A)/B}×100%
수학식 2에서, A는 제품 사용 후 R2 측정값이고, B는 제품 사용 전 R2 측정값이다.In Equation 2, A is the R2 measured value after product use, and B is the R2 measured value before product use.
구분 division 0주
R2 측정값
0 weeks
R2 measured value
2주 후
R2 측정값
2 weeks later
R2 measured value
4주 후
R2 측정값
4 weeks later
R2 measured value
4주 후
피부탄력 개선율(%)
4 weeks later
Skin elasticity improvement rate (%)
비교예 1Comparative Example 1 0.77030.7703 0.77670.7767 0.77850.7785 101.06101.06
실시예 1Example 1 0.77120.7712 0.77820.7782 0.78130.7813 101.23101.23
눈가 주름을 분석한 결과, 비교예 1 및 실시예 1의 화장료 모두 사용 전과 비교하여 사용 후에서 피부 탄력 개선 효과를 나타냈으며(p<0.05), 비교예 1 보다 실시예 1이 상대적으로 좀 더 우수한 눈가 주름 개선율을 보였다.As a result of analyzing the wrinkles around the eyes, both the cosmetics of Comparative Example 1 and Example 1 showed an effect of improving skin elasticity after use compared to before use (p<0.05), and Example 1 was relatively better than Comparative Example 1. There was an improvement in wrinkles around the eyes.
실험예 9 : 티로시나제 효소 활성 저해능 평가Experimental Example 9: Evaluation of tyrosinase enzyme activity inhibition
실시예 1의 화장료에 대한 미백 활성 효과는 티로시나제 효소 활성 저해능을 통해 평가하였다. 0.1M sodium phosphate buffer(pH 6.9) 1mL, 다양한 농도의 실시예 1의 화장료 시료, mushroom tyrosinase(1 KU/mL) 30㎕를 혼합하고 37℃에서 10분간 반응시킨 후 기질로서 1.5mM L-tyrosine 30㎕를 혼합하여 25℃에서 2분간 반응시켜 반응액 중에 생성된 DOPA chrome을 475nm에서 측정하였고 그 결과를 표 12에 나타내었다. 대조군의 흡광도를 Abcontrol 이라 하고 시료의 흡광도를 Absample 로 하여 하기 수학식 3에 따라 계산하였다.The whitening activity effect of the cosmetic of Example 1 was evaluated through the ability to inhibit tyrosinase enzyme activity. 1mL of 0.1M sodium phosphate buffer (pH 6.9), various concentrations of the cosmetic sample of Example 1, and 30μl of mushroom tyrosinase (1 KU/mL) were mixed and reacted at 37°C for 10 minutes, followed by 1.5mM L-tyrosine 30 as a substrate. ul was mixed and reacted at 25 ° C. for 2 minutes, and DOPA chrome generated in the reaction solution was measured at 475 nm, and the results are shown in Table 12. The absorbance of the control group was referred to as Ab control , and the absorbance of the sample was referred to as Ab sample , and was calculated according to Equation 3 below.
[수학식 3][Equation 3]
티로시나제 효소 활성 저해율(%) = (1-Absample)/Abcontrol*100%Tyrosinase enzyme activity inhibition rate (%) = (1-Ab sample ) / Ab control *100%
구분(화장료 시료 농도, sample)Classification (cosmetic sample concentration, sample) 티로시나제 효소 활성 저해율(%)Tyrosinase enzyme activity inhibition rate (%)
0.1 mg/ml0.1 mg/ml 9.7%9.7%
0.3 mg/ml0.3 mg/ml 20.1%20.1%
0.5 mg/ml0.5 mg/ml 22.3%22.3%
0.7 mg/ml0.7 mg/ml 30.5%30.5%
1.0 mg/ml1.0 mg/ml 37.4%37.4%
1.5 mg/ml1.5 mg/ml 38.2%38.2%
상기 표 12의 티로시나제 효소 활성 저해율 평가를 통해, 본 발명의 화장료가 티로시나제 효소의 활성 저해를 통한 피부 미백 효과가 있음을 확인할 수 있었다.Through the evaluation of the tyrosinase enzyme activity inhibition rate in Table 12, it was confirmed that the cosmetic of the present invention has a skin whitening effect through inhibition of the tyrosinase enzyme activity.
상기 실시예 및 실험예를 통하여, 본 발명의 화장료가 피부 미백 및 피부 주름 개선 등 다양한 효과가 있는 것을 확인할 수 있었으며, 이러한 본 발명의 화장료는 다양한 피부용 화장품의 화장료를 제공할 수 있음을 확인할 수 있었다.Through the above examples and experimental examples, it was confirmed that the cosmetic of the present invention has various effects such as skin whitening and skin wrinkle improvement, and it was confirmed that the cosmetic of the present invention can provide cosmetics for various skin cosmetics. .
본 발명의 단순한 변형이나 변경은 이 분야의 통상의 지식을 가진 자에 의해서 용이하게 실시될 수 있으며, 이러한 변형이나 변경은 모두 본 발명의 영역에 포함되는 것으로 볼 수 있다.Simple modifications or changes of the present invention can be easily performed by those skilled in the art, and all such modifications or changes can be considered to be included in the scope of the present invention.

Claims (9)

  1. 반응기에 정제수 및 점도조절제를 투입한 후, 2500 ~ 3500rpm 하에서 40 ~ 80분 동안 교반을 수행하여 제1액을 제조하는 1단계;A first step of preparing a first liquid by adding purified water and a viscosity modifier to the reactor and stirring for 40 to 80 minutes at 2500 to 3500 rpm;
    제1액이 제조된 반응기에 제2액을 투입한 후, 2000 ~ 3000rpm 하에서 40 ~ 80분 동안 교반을 수행하는 2단계;A second step of adding the second liquid to the reactor in which the first liquid was prepared and performing stirring at 2000 to 3000 rpm for 40 to 80 minutes;
    2단계를 수행한 반응기에 제3액을 투입한 후, 2000 ~ 3000rpm 하에서 40 ~ 60분 동안 교반을 수행하는 3단계;Step 3 of stirring for 40 to 60 minutes at 2000 to 3000 rpm after adding the third liquid to the reactor in which Step 2 was performed;
    3단계를 수행한 반응기에 pH 조절제를 투입한 후, 1800 ~ 2800rpm 하에서 20 ~ 40분 동안 교반을 수행하는 4단계; 및Step 4 of performing stirring for 20 to 40 minutes at 1800 to 2800 rpm after adding a pH adjuster to the reactor in which Step 3 was performed; and
    4단계를 수행한 반응기에 제4액을 투입한 후, 1800 ~ 2800rpm 하에서 20 ~ 40분 동안 교반을 수행하는 5단계;Step 5 of adding the fourth liquid to the reactor in which step 4 was performed and stirring for 20 to 40 minutes at 1800 to 2800 rpm;
    5단계를 수행한 혼합액을 여과 및 탈포하는 6단계; 및Step 6 of filtering and defoaming the mixed solution after step 5; and
    6단계를 수행한 혼합액을 숙성시키는 7단계;를 포함하는 공정을 수행하며,A process including step 7 of aging the mixed solution after step 6 is performed,
    상기 제1액은 점도조절제 및 정제수를 포함하고,The first liquid contains a viscosity modifier and purified water,
    상기 제2액은 글리세레스-26, 알란토인, 하이드롤라이즈드콜라겐, 아데노신피부중에서 선택된 1종 이상을 포함하는 컨디셔닝제; 글리세린 및 부틸렌글라이콜을 포함하는 보습제; 보존제; 및 가교제;를 포함하며,The second liquid is a conditioning agent containing at least one selected from glycereth-26, allantoin, hydrolyzed collagen, and adenosine skin; moisturizers including glycerin and butylene glycol; preservatives; and a crosslinking agent;
    상기 제3액은 해바라기씨 오일, 다이메티콘, 세틸에틸헥사노에이트 및 글리세릴스테아레이트 중에서 선택된 1종 이상을 포함하는 피부컨디셔닝제; 피이지-100 스테아레이트를 포함하는 계면활성제; 카프릴릭/카프릭트라이글리세라이드(Caprylic/Capric Triglyceride)을 포함하는 보습제; 폴리솔베이트60, 스테아릭애씨드 및 솔비탄세스퀴올리에이트 중에서 선택된 1종 이상을 포함하는 유화제; 및 유화안정제;를 포함하고,The third liquid is a skin conditioning agent containing at least one selected from sunflower seed oil, dimethicone, cetylethylhexanoate and glycerylstearate; surfactants including PEG-100 stearate; humectants including Caprylic/Capric Triglyceride; An emulsifier containing at least one selected from polysorbate 60, stearic acid and sorbitan sesquioleate; And an emulsion stabilizer; including,
    상기 pH 조절제는 알지닌을 포함하며,The pH adjusting agent includes arginine,
    상기 제4액은 진주 추출물 및 천연식물 복합 추출물을 포함하는 기능성 추출물; 락토바실러스발효 용해물; 콜라겐 합성 촉진제; 및 향료;를 포함하는 것을 특징으로 하는 자연유래 식물 핑거루트의 피부탄력 성분 소재를 활용한 에멀젼 제형의 피부탄력 개선 화장료의 제조방법.The fourth liquid is a functional extract containing a pearl extract and a natural plant complex extract; Lactobacillus fermentation lysate; collagen synthesis promoter; And fragrance; manufacturing method of skin elasticity improving cosmetics of the emulsion formulation utilizing the skin elasticity component material of the plant finger root of natural origin, characterized in that it comprises a.
  2. 제1항에 있어서, 2단계는 제1액 100 중량부에 대하여, 제2액을 18 ~ 22 중량부로 투입하며,The method of claim 1, wherein in the second step, 18 to 22 parts by weight of the second liquid is added to 100 parts by weight of the first liquid,
    3단계는 제1액 100 중량부에 대하여, 제3액을 8 ~ 12 중량부로 투입하고,In step 3, 8 to 12 parts by weight of the third solution is added to 100 parts by weight of the first solution,
    5단게는 제1액 100 중량부에 대하여, 제4액을 10 ~ 15 중량부로 투입하는 것을 특징으로 하는 자연유래 식물 핑거루트의 피부탄력 성분 소재를 활용한 에멀젼 제형의 피부탄력 개선 화장료의 제조방법.In step 5, 10 to 15 parts by weight of the 4th liquid is added to 100 parts by weight of the 1st liquid, Method for producing emulsion-type skin elasticity improving cosmetics using natural plant finger root skin elasticity component material .
  3. 제1액 100 중량부에 대하여, 제2액 18 ~ 22 중량부, 제3액 8 ~ 12 중량부 및 제4액 10 ~ 15 중량부를 포함하며,Based on 100 parts by weight of the first solution, 18 to 22 parts by weight of the second solution, 8 to 12 parts by weight of the third solution, and 10 to 15 parts by weight of the fourth solution,
    상기 제1액은 점도조절제 및 정제수를 포함하고,The first liquid contains a viscosity modifier and purified water,
    상기 제2액은 글리세레스-26, 알란토인, 하이드롤라이즈드콜라겐, 아데노신피부중에서 선택된 1종 이상을 포함하는 컨디셔닝제; 글리세린 및 부틸렌글라이콜을 포함하는 보습제; 1,2-헥산다이올을 포함하는 보존제; 및 소듐하이알루로네이트를 포함하는 가교제;를 포함하며,The second liquid is a conditioning agent containing at least one selected from glycereth-26, allantoin, hydrolyzed collagen, and adenosine skin; moisturizers including glycerin and butylene glycol; preservatives including 1,2-hexanediol; And a crosslinking agent including sodium hyaluronate;
    상기 제3액은 해바라기씨 오일, 다이메티콘, 세틸에틸헥사노에이트 및 글리세릴스테아레이트 중에서 선택된 1종 이상을 포함하는 피부컨디셔닝제; 피이지-100 스테아레이트를 포함하는 계면활성제; 카프릴릭/카프릭트라이글리세라이드(Caprylic/Capric Triglyceride)을 포함하는 보습제; 폴리솔베이트60, 스테아릭애씨드 및 솔비탄세스퀴올리에이트 중에서 선택된 1종 이상을 포함하는 유화제; 및 세테아릴알코올을 포함하는 유화안정제;를 포함하고,The third liquid is a skin conditioning agent containing at least one selected from sunflower seed oil, dimethicone, cetylethylhexanoate and glycerylstearate; surfactants including PEG-100 stearate; humectants including Caprylic/Capric Triglyceride; An emulsifier containing at least one selected from polysorbate 60, stearic acid and sorbitan sesquioleate; And an emulsion stabilizer containing cetearyl alcohol;
    상기 제4액은 진주 추출물 및 천연식물 복합 추출물을 포함하는 기능성 추출물; 락토바실러스발효 용해물; 콜라겐 합성 촉진제; 및 향료;를 포함하는 것을 특징으로 하는 자연유래 식물 핑거루트의 피부탄력 성분 소재를 활용한 에멀젼 제형의 피부탄력 개선 화장료.The fourth liquid is a functional extract containing a pearl extract and a natural plant complex extract; Lactobacillus fermentation lysate; collagen synthesis promoter; And fragrance; skin elasticity improvement cosmetic of the emulsion formulation utilizing the skin elasticity component material of the plant finger root of natural origin, characterized in that it comprises a.
  4. 제3항에 있어서, 상기 제1액은 점도조절제 0.20 ~ 0.40 중량% 및 잔량의 정제수를 포함하고,The method of claim 3, wherein the first liquid contains 0.20 to 0.40% by weight of a viscosity modifier and the remaining amount of purified water,
    상기 제2액은 상기 피부컨디셔닝제 18.5 ~ 21.0 중량%, 상기 가교제 10 ~ 12.0 중량%, 상기 미백제 13.0 ~ 16.0 중량%, 상기 보존제 10 ~ 15.0 중량% 및 나머지 잔량의 상기 보습제를 포함하는 것을 특징으로 하는 자연유래 식물 핑거루트의 피부탄력 성분 소재를 활용한 에멀젼 제형의 피부탄력 개선 화장료.The second liquid comprises 18.5 to 21.0% by weight of the skin conditioning agent, 10 to 12.0% by weight of the crosslinking agent, 13.0 to 16.0% by weight of the whitening agent, 10 to 15.0% by weight of the preservative and the remaining amount of the moisturizing agent. Emulsion-type skin elasticity improvement cosmetic using the skin elasticity component of the natural plant finger root.
  5. 제3항에 있어서, 상기 제3액은 상기 유화제 15.0 ~ 20.0 중량%, 상기 유화안정제 5.0 ~ 8.0 중량%, 상기 계면활성제 10.0 ~ 12.0 중량%, 상기 보습제 5.0 ~ 8.0 중량% 및 나머지 잔량의 상기 피부컨디셔닝제를 포함하며,The method of claim 3, wherein the third liquid comprises 15.0 to 20.0% by weight of the emulsifier, 5.0 to 8.0% by weight of the emulsion stabilizer, 10.0 to 12.0% by weight of the surfactant, 5.0 to 8.0% by weight of the humectant, and the remaining amount of the skin. Contains a conditioning agent,
    제4액은 락토바실러스발효 용해물 5.0 ~ 8.0 중량%, 콜라겐 합성 촉진제 1.0 ~ 2.5 중량%, 향료 0.1 ~ 0.8 중량% 및 나머지 잔량의 기능성 추출물을 포함하고,The fourth liquid contains 5.0 to 8.0% by weight of lactobacillus fermented lysate, 1.0 to 2.5% by weight of collagen synthesis promoter, 0.1 to 0.8% by weight of fragrance, and the remaining amount of functional extract,
    상기 기능성 추출물은 진주 추출물 및 천연식물 복합 추출물을 1 : 3.5 ~ 5.0 중량비로 포함하는 것을 특징으로 하는 자연유래 식물 핑거루트의 피부탄력 성분 소재를 활용한 에멀젼 제형의 피부탄력 개선 화장료.The functional extract is a cosmetic for improving skin elasticity of an emulsion formulation using a skin elasticity component material of a natural plant finger root, characterized in that it comprises a pearl extract and a natural plant complex extract in a weight ratio of 1: 3.5 to 5.0.
  6. 제5항에 있어서, 상기 천연식물 복합 추출물은 핑거루트뿌리줄기 추출물, 병풀 추출물, 비타민나무 추출물, 녹차 추출물, 마트리카리아 추출물, 저단선 추출물, 뽕나무잎 추출물, 산사나무열매 추출물, 페퍼민트 추출물, 히비스커스꽃 추출물, 로즈마리 추출물, 모과 추출물 및 레드초크베리 추출물을 포함하는 것을 특징으로 하는 자연유래 식물 핑거루트의 피부탄력 성분 소재를 활용한 에멀젼 제형의 피부탄력 개선 화장료.The method of claim 5, wherein the natural plant complex extract is finger root rhizome extract, centella asiatica extract, vitamin tree extract, green tea extract, matricaria extract, low-danseon extract, mulberry leaf extract, hawthorn fruit extract, peppermint extract, hibiscus A cosmetic composition for improving skin elasticity in an emulsion formulation using a skin elasticity component material of a natural plant finger root, comprising a flower extract, a rosemary extract, a quince extract and a red chokeberry extract.
  7. 제6항에 있어서,According to claim 6,
    상기 천연식물 복합 추출물은 핑거루트뿌리줄기 추출물 100 중량부에 대하여, 병풀 추출물 15 ~ 30 중량부, 비타민나무 추출물 0.2 ~ 2.0 중량부, 녹차 추출물 0.2 ~ 2.0 중량부, 마트리카리아 0.2 ~ 2.0 중량부, 저단선 추출물 0.1 ~ 1.0 중량부, 뽕나무잎 추출물 0.1 ~ 1.0 중량부, 산사나무열매 추출물 0.1 ~ 1.0 중량부, 페퍼민트 추출물 0.1 ~ 1.0 중량부, 히비스커스꽃 추출물 0.1 ~ 1.0 중량부, 로즈마리 추출물 0.1 ~ 1.0 중량부, 모과 추출물 0.1 ~ 1.0 중량부 및 레드초크베리 추출물 0.1 ~ 1.0 중량부를 포함하는 것을 특징으로 자연유래 식물 핑거루트의 피부탄력 성분 소재를 활용한 에멀젼 제형의 피부탄력 개선 화장료.The natural plant complex extract is based on 100 parts by weight of finger root rhizome extract, 15 to 30 parts by weight of Centella asiatica extract, 0.2 to 2.0 parts by weight of vitamin tree extract, 0.2 to 2.0 parts by weight of green tea extract, 0.2 to 2.0 parts by weight of Matricaria , 0.1 ~ 1.0 parts by weight of low tanning extract, 0.1 ~ 1.0 parts by weight of mulberry leaf extract, 0.1 ~ 1.0 parts by weight of hawthorn fruit extract, 0.1 ~ 1.0 parts by weight of peppermint extract, 0.1 ~ 1.0 parts by weight of hibiscus flower extract, 0.1 ~ 1.0 parts by weight of rosemary extract 1.0 parts by weight, 0.1 to 1.0 parts by weight of quince extract, and 0.1 to 1.0 parts by weight of red chokeberry extract, characterized by including 0.1 to 1.0 parts by weight of natural plant finger root skin elasticity improvement cosmetic of emulsion formulation using skin elasticity component material.
  8. 제6항에 있어서, 상기 핑거루트뿌리줄기 추출물은 핑거루트뿌리줄기 에탄올 추출물 또는 핑거루트뿌리줄기 에탄올 추출물의 물 분획물인 것을 특징으로 자연유래 식물 핑거루트의 피부탄력 성분 소재를 활용한 에멀젼 제형의 피부탄력 개선 화장료.The method of claim 6, wherein the finger root rhizome extract is a finger root rhizome ethanol extract or a water fraction of the finger root rhizome ethanol extract. Elasticity improvement cosmetic.
  9. 제3항 내지 제8항 중에서 선택된 어느 한 항의 화장료를 포함하는 것을 특징으로 하는 에멀젼 제형 피부탄력 개선 화장품.Claims 3 to 8, characterized in that the cosmetic composition of any one item selected from the emulsion formulation improving skin elasticity cosmetic.
PCT/KR2021/019521 2021-12-21 2021-12-21 Emulsion-type skin elasticity improving cosmetic material using skin elasticity component material of naturally-derived plant fingerroot, preparation method therefor, and emulsion-type skin elasticity improving cosmetics WO2023120763A1 (en)

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KR101776001B1 (en) * 2016-03-04 2017-09-07 (주)뉴트리 Composition for treating, preventing or improving born loss containing panduratin or fingerroot(boesenbergia pandurata) extract
KR20180050798A (en) * 2016-11-07 2018-05-16 이호규 Cosmetic compositions containing Zingiberaceae extracts for skin homeostasis and nontoxicity and manufacturing method thereof
KR20180086674A (en) * 2017-01-23 2018-08-01 민연홍 Skin care cosmetic composition comprising fingerroot and manufacturing method thereof
KR20190000816A (en) * 2017-06-23 2019-01-03 주식회사 글로원 Mask pack with improved elasticity manufactured by using biodegradable polymer and loess, and the method for manufacturing the mask pack
KR102050351B1 (en) * 2018-05-17 2019-12-02 이호규 Method for detoxing fingerroot extracts and skin homeostasis and nontoxicity cosmetic compositions containing detoxed fingerroot extracts
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101776001B1 (en) * 2016-03-04 2017-09-07 (주)뉴트리 Composition for treating, preventing or improving born loss containing panduratin or fingerroot(boesenbergia pandurata) extract
KR20180050798A (en) * 2016-11-07 2018-05-16 이호규 Cosmetic compositions containing Zingiberaceae extracts for skin homeostasis and nontoxicity and manufacturing method thereof
KR20180086674A (en) * 2017-01-23 2018-08-01 민연홍 Skin care cosmetic composition comprising fingerroot and manufacturing method thereof
KR20190000816A (en) * 2017-06-23 2019-01-03 주식회사 글로원 Mask pack with improved elasticity manufactured by using biodegradable polymer and loess, and the method for manufacturing the mask pack
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