KR102572519B1 - A cosmetic composition for skin whitening containing loess extract - Google Patents

Abstract

The present invention relates to a cosmetic composition for skin whitening, which is non-toxic and effective in improving skin whitening by containing ocher extract as an active ingredient.

Description

A cosmetic composition for skin whitening containing loess extract containing loess extract as an active ingredient {A cosmetic composition for skin whitening containing loess extract}

The present invention relates to a cosmetic composition containing ocher extract as an active ingredient.

As modern people become more interested in health, various studies on natural and eco-friendly cosmetics are being actively conducted. In functional cosmetics, interest in cosmetics using materials derived from natural products is increasing, rather than in the case of chemical ingredient-based whitening, antioxidants, UV protection, preservatives, and antibacterial agents in the past.

Among various natural materials, animal-derived materials are actively developing functional cosmetics using plant-based ingredients as consumers' resistance to animal-derived materials increases due to animal welfare, mad cow disease, swine cholera, and bird flu. Consumer demand for complex functional cosmetics such as wrinkle improvement and sun protection is increasing.

Functional cosmetics refers to cosmetics at various stages of use, such as essence, serum, cream, powder, and base, to which specific functions such as whitening, wrinkle improvement, and UV protection are added. Cosmetics with one function have also been developed to increase the ease of use, and specialized products for various purposes such as pore care, nutrition supply, elasticity enhancement, acne treatment, whitening and UV protection are also being released.

As it is difficult to import new single substances into the country and large cosmetic companies are focusing on developing complex functional products for whitening and UV protection, whitening materials are rapidly emerging.

As known whitening ingredients, arbutin, kojic acid, azelaic acid, aloesin, 4-butylesorcinol, resveratrol, ceramide, sphingosin-1-phosphate, sphingosyl that inhibit tyrosinase enzyme activity There are substances such as phosphorylcholine, hydroquinone, and the like. However, when some whitening ingredients are applied to the skin, there are limitations in usage due to safety issues such as irritation and redness, or there is a problem in that practical effects cannot be expected because the effect is insignificant. In particular, in the case of hydroquinone, its use was banned due to unwanted side effects such as irreversible bleaching, and it was replaced with arbutin, which is a structural analogue of hydroquinone. As such, in the field of whitening, it is particularly important to secure stability as well as to exhibit a tyrosinase activity inhibitory effect and to have a whitening effect, so there is still a need for the development of a substance that satisfies all of the above requirements.

The inventors of the present invention have made diligent efforts to develop a substance that can actually help the skin whitening effect while securing safety when applied to the skin by utilizing natural ingredients as a material for cosmetics with a skin whitening function. The present invention was completed by discovering for the first time that it contains inorganic substances at a high concentration and has excellent whitening efficacy due to its high tyrosinase activity inhibitory ability, and confirming that it can be used for skin whitening purposes.

Republic of Korea Patent Publication No. 10-2019-0176556

An object of the present invention is to provide a cosmetic composition for improving skin whitening containing ocher extract as an active ingredient.

In addition, another object of the present invention relates to a method capable of producing a large amount of ocher extract.

In addition, another object of the present invention is to provide a health functional food composition or quasi-drug composition for improving skin whitening containing ocher extract as an active ingredient.

In order to achieve the above object, the present invention can provide a cosmetic composition for skin whitening, characterized in that it contains the ocher extract as an active ingredient.

The ocher extract may be a concentrate prepared by mixing ocher with water, lower alcohol having 1 to 4 carbon atoms, or a mixed solvent thereof, leaving it to stand for 1 to 500 days, recovering the supernatant, and distilling it under reduced pressure.

During the vacuum distillation, the distillation temperature may be 30 to 50 °C and the pressure may be 50 to 100 torr.

The loess may be obtained from a habitat in which cypress trees grow naturally.

When the ocher extract was analyzed by ICP analysis, it contained 190.16 mg/l of sodium, 30.64 mg/l of magnesium, 8.08 mg/l of aluminum (Al), 3.62 mg/l of iron, 65.3 mg/l of calcium, and 82.04 mg/l of silica. it may be

The ocher extract may inhibit tyrosinase.

In addition, the manufacturing method of the cosmetic composition for skin whitening of the present invention in order to achieve the above other object may include the following steps.

(a) mixing loess with a solvent; and

(b) distilling the mixed solution obtained in step (a) under reduced pressure under pressurized conditions of 30 to 50 ° C and 50 to 100 torr to obtain a loess extract.

The solvent may be water, a lower alcohol having 1 to 4 carbon atoms, or a mixture thereof.

Before step (b), (a1) filtering the mixed solution obtained from step (a); may be further included.

In step (a), the mixing weight ratio of loess and the solvent may be 1:1 to 100.

Step (a) may be performed for 1 to 10 hours under a temperature condition of 10 to 40 °C.

In addition, in order to achieve the above another object, the health functional food composition for skin whitening of the present invention may contain the ocher extract as an active ingredient.

In addition, in order to achieve the above another object, the quasi-drug composition for skin whitening of the present invention may contain the ocher extract as an active ingredient.

The cosmetic composition containing the ocher extract of the present invention as an active ingredient has a high inorganic content, an excellent silica / alumina ratio, and excellent skin penetration, so it is suitable for use in various formulations.

In addition, the cosmetic composition containing the ocher extract of the present invention as an active ingredient can effectively suppress the production of melanin pigment by inhibiting the synthesis of tyrosinase involved in melanin formation. Accordingly, the skin whitening cosmetic composition has an excellent skin whitening effect.

1 is a photograph of a solution obtained by mixing loess extract 1 of Example 1 with distilled water.
2 is a photograph of the solution after filtering loess extract 1 of Example 1.
Figure 3 is a photograph taken of ocher extract 2 prepared from Example 2.
Figure 4 is a graph showing the XRD analysis results for the ocher powder solution obtained from Comparative Example 1.
5 is a graph showing the XRD analysis results for loess extract 1 prepared in Example 1.
6 is an image of the ocher powder solution obtained from Comparative Example 1 observed by SEM-EDS.
7 is an image observed by SEM-EDS of loess extract 1 prepared in Example 1.
8 is a result of confirming the DOPA-oxidase inhibitory efficacy by concentration for loess extract 1 prepared from Example 1.
9 is a result of confirming the DOPA-oxidase inhibitory efficacy by concentration for loess extract 2 prepared from Example 2.
10 is a result of confirming the DOPA-oxidase inhibitory efficacy by concentration for the kojic acid solution prepared from Comparative Example 2.

The present invention relates to a cosmetic composition, a health functional food composition, and a quasi-drug composition containing ocher extract as an active ingredient.

Hereinafter, the present invention will be described in detail.

Ocher is natural soil made up of diatomaceous earth and soil containing hydrous iron oxide and anhydrous iron oxide, and can be easily obtained throughout Korea. In particular, loess in Jeollanam-do contains a lot of iron oxide, so it has a strong red color. The yellow color is strong.

The ocher extract, called loess Jijangsu, is a yellow soil water, also called rootless water. When a pit is dug more than 60 cm deep into the loess ground of a sunny field or a deep ridge, soil like a blue belt comes out, and the bottom of this soil is dug out. It refers to a pale yellow water that is created by mixing water filtered with charcoal and ocher in an appropriate ratio and stirring it several times. Ocher Jijangsu is water containing good ingredients of ocher, purifies the blood, normalizes hormone secretion of the body’s endocrine glands, and has the effect of separating and excreting harmful substances to the human body. It is known to be effective. However, few studies have been conducted on its whitening effect.

The cosmetic composition of the present invention contains ocher extract as an active ingredient, and the ocher extract is an extract obtained by mixing ocher with water, lower alcohol having 1 to 4 carbon atoms, or a mixed solvent thereof, and then set aside for 1 to 500 days, Alternatively, it may be a fraction obtained by fractionating the extract, or a concentrate prepared by distilling the extract under reduced pressure. The meaning of the extract also includes solid extracts obtained by methods such as freeze drying, vacuum drying, hot air drying, and spray drying.

The present invention measured the inhibitory activity of tyrosinase, which causes pigmentation due to an imbalance in the melanin formation process, in order to evaluate the skin whitening effect of ocher extract, and as a result, ocher extract has excellent tyrosinase ( tyrosinase) inhibitory effect, it was confirmed that the skin whitening effect was excellent. In addition, among the ocher extracts, it was confirmed that the concentrate prepared by distilling the extract under reduced pressure was more than 2 to 6 times more effective in inhibiting tyrosinase than Jijangsu obtained by simple extraction of ocher. In addition, as a result of measuring cytotoxicity, it was confirmed that there was no cytotoxicity unlike kojic acid.

The loess extract of the present invention is an extract obtained by mixing loess with water, a lower alcohol having 1 to 4 carbon atoms, or a mixed solvent thereof, and then standing or leaching for 1 to 500 days, or a fraction obtained by fractionating the extract, or It may be a concentrate prepared by distilling the extract under reduced pressure. Preferably, loess is mixed with a solvent, left to stand for 1 to 500 days, and a concentrate obtained by distilling the obtained supernatant under reduced pressure, more preferably, loess is mixed with a solvent. It is a concentrate obtained by leaving it for 1 to 500 days to recover only the supernatant except for the precipitated solid, and distilling it under reduced pressure. Specifically, loess and solvent are 1: 1 to 100, preferably 1: 5 to 20, more preferably Preferably, it is mixed in a weight ratio of 1: 10 at a distillation temperature of 30 to 50 ° C, preferably 40 to 50 ° C, and a distillation pressure of 50 to 100 torr, preferably 60 to 90 torr, more preferably 70 to 85 torr. It may be a concentrate prepared by distillation under reduced pressure.

Filtering the mixture of the loess and the solvent or the supernatant obtained therefrom before distillation under reduced pressure; may further include, through which ocher microparticles and impurities can be removed. In the filtration process, sand filtration, a filtration method using a micro filter, and a filtration method using an ultra filter may be used. The mixture is sent to a vacuum distillation apparatus.

If the extract is not obtained from loess, a small amount of active ingredient is extracted and the skin whitening effect cannot be achieved, and when the vacuum distillation step is omitted, the skin whitening effect is low.

When the weight ratio of the ocher and the solvent is out of the above range, a small amount of the active ingredient of ocher may be present in the extract.

In addition, when the temperature and pressure conditions of the vacuum distillation are less than the lower limit, the active ingredient may be extracted from loess in a small amount, and when the upper limit is exceeded, the active ingredient may also be distilled and the effect may be reduced or an unwanted effect may be added.

In addition, before the vacuum distillation step, the step of mixing the loess and the solvent is 10 to 40 ° C., preferably 20 to 30 ° C., for 1 to 500 days, preferably 150 to 450 days, more preferably It can be carried out for 410 to 420 days. If it is less than the lower limit, the active ingredient of loess can be extracted in a small amount, and if it exceeds the upper limit, it is transformed by heat or components other than the active ingredient are extracted. there is.

The solvent may be water, lower alcohol having 1 to 4 carbon atoms, ethylene glycol, ethyl ether, or a mixture thereof. As the lower alcohol, 20 to 99% by volume of methanol, ethanol, butanol or propanol aqueous solution may be used, and water may be preferably used for excellent whitening effect and non-toxicity.

The loess used in the present invention may be obtained from a habitat where cypress trees grow naturally, and preferably, it is preferable to use that obtained from a forest of galmobong cypress trees located in Idang-ri, Goseong-eup, Goseong-gun. When using ocher obtained from general soil, active ingredients of ocher may be extracted in small amounts, and functionality may be reduced due to impurities.

When the ocher extract was analyzed by ICP analysis, it contained 190.16 mg/l of sodium, 30.64 mg/l of magnesium, 8.08 mg/l of aluminum (Al), 3.62 mg/l of iron, 65.3 mg/l of calcium, and 82.04 mg/l of silica. As a result, it contains various mineral components in high concentration and has the effect of significantly improving the whitening activity.

Even though the ocher extract did not contain flavonoids or polyphenols, it had a high tyrosinase activity inhibitory effect, and the tyrosinase activity inhibitory effect increased in a concentration-dependent manner, confirming that there was a whitening effect.

The ocher extract of the present invention can be used in health functional foods and quasi-drug compositions in addition to cosmetic compositions.

The present invention comprises the steps of (a) mixing ocher with a solvent; And (b) distilling the mixed solution obtained from step (a) under reduced pressure under pressurized conditions of 30 to 50 ° C. and 50 to 100 torr to obtain an ocher extract.

It may be obtained from a habitat where the ocher cypress used in the present invention grows naturally, and preferably, it is preferable to use one obtained from a galmobong cypress forest located in Idang-ri, Goseong-eup, Goseong-gun. When using ocher obtained from general soil, active ingredients of ocher may be extracted in small amounts, and functionality may be reduced due to impurities.

The loess used in the present invention is preferably used by securing 1 m of loess removed from the surface layer in consideration of soil contamination. It can be subjected to high heat treatment at 1000 ° C or higher.

The solvent may be water, lower alcohol having 1 to 4 carbon atoms, ethylene glycol, ethyl ether, or a mixture thereof. As the lower alcohol, 20 to 99% by volume of methanol, ethanol, butanol or propanol aqueous solution may be used, and water may be preferably used for excellent whitening effect and non-toxicity.

In the above production method, in step (a), loess and the solvent may be mixed in a weight ratio of 1: 1 to 100, preferably 1: 5 to 20, and more preferably 1: 10. When the mixed weight ratio of the ocher and the solvent is out of the above range, a small amount of the active ingredient of ocher may be extracted in the extract.

The step (a) may be carried out for 1 to 500 days, preferably 150 to 450 days, more preferably 410 to 420 days under a temperature condition of 10 to 40 ° C, preferably 20 to 30 ° C, If it is less than the lower limit, the active ingredient of loess may be extracted in a small amount, and if it exceeds the upper limit, the functionality may be reduced due to deformation by heat or extraction of components other than the active ingredient.

Before step (b), (a1) filtering the mixed solution obtained from step (a) may be further included, through which ocher microparticles and impurities present in the mixed solution may be removed.

In the filtration process, sand filtration, a filtration method using a micro filter, and a filtration method using an ultra filter may be used. The mixture is sent to a vacuum distillation apparatus.

The step (b) is concentrated by distillation under reduced pressure at a distillation temperature of 30 to 50 °C, preferably 40 to 50 °C, and a distillation pressure of 50 to 100 torr, preferably 60 to 90 torr, more preferably 70 to 85 torr. may have been

In the case of distillation under reduced pressure without going through the leaching process for extracting active ingredients from loess, a sufficient skin whitening effect cannot be expected because a small amount of active ingredients are extracted. In addition, when only the leaching process using ocher is performed and the vacuum distillation step is omitted, the skin whitening effect can be obtained, but since the effect is less than half of the conventional whitening material, steps (a) and (b) are It is most preferred that both be performed.

In addition, when the temperature and pressure conditions of the vacuum distillation are less than the lower limit, a small amount of the active ingredient may remain from the loess, and when it exceeds the upper limit, a large amount of other substances other than the active ingredient are distilled and removed, so the effect is reduced or undesirable. Unexpected effects may be added.

The term 'extract' used herein while referring to ocher includes not only a crude extract obtained by treating an extraction solvent, but also a processed product such as a concentrate obtained by distilling ocher extract under reduced pressure. For example, ocher extract may be prepared in a powder state by an additional process such as freeze drying or spray drying. Preferably, the ocher extract may be a concentrate obtained by distilling a solution obtained by treating an extraction solvent under reduced pressure.

In the cosmetic composition according to the present invention, the cosmetic composition for skin whitening may contain 0.0001 to 90 parts by weight of loess extract based on the total weight, but is not limited thereto as long as it contains an effective amount capable of providing a desired whitening improvement effect. .

In the present invention, the term 'skin whitening or whitening' refers to inhibiting, inhibiting, or alleviating hyperpigmentation of the skin. Hyperpigmentation of the skin includes freckles, melasma, hyperpigmentation after sun exposure, hyperpigmentation after inflammation, senile lentigines, brown spots or age spots.

On the other hand, in the present specification, the term 'contained as an active ingredient' means to include an effective amount sufficient to achieve the efficacy or activity of the ocher extract. For example, the loess extract is used at a concentration of 10 to 1500 μg/ml, preferably 100 to 1000 μg/ml. Ocher extract is a natural product, so there is no side effect on the human body even when used in excess, so the quantitative upper limit of the ocher extract included in the composition of the present invention can be selected and implemented by those skilled in the art within an appropriate range.

In the cosmetic composition of the present invention, in addition to the above cosmetic composition, if necessary, other ingredients commonly used in cosmetics may be mixed. Examples of these ingredients include oils and fats, humectants, emollients, surfactants, organic and inorganic pigments, Organic powders, UV absorbers, preservatives, bactericides, antioxidants, pH adjusters, alcohols, pigments, fragrances, blood circulation promoters, cooling agents, antiperspirants, purified water, water-soluble vitamins, fat-soluble vitamins, high-molecular peptides, polysaccharides, sphingolipids, and seaweed An extract etc. are mentioned.

The cosmetic composition of the present invention may be prepared in the form of an emulsified formulation and a solubilized formulation commonly used in the art.

In addition, the ingredients included in the cosmetic composition of the present invention may include ingredients commonly used in cosmetic compositions in addition to the above ingredients as active ingredients, for example, conventional adjuvants such as stabilizers, pigments and natural flavors, and A carrier may be further included.

Products to which the composition of the present invention can be added include, for example, mist, skin lotion, skin softener, skin toner, astringent, lotion, milk lotion, moisture lotion, nutrient lotion, massage cream, nutrient cream, and sunscreen cream. , Moisture Cream, Hand Cream, Foundation, Essence, Nutritional Essence, Mask Pack, Press Powder, Loose Powder, Eye Shadow, etc. Cosmetics and Soap, Cleansing Foam, Cleansing Lotion, Cleansing Cream, Body Lotion and Body Cleanser.

When the formulation of the present invention is a paste, cream or gel, animal fiber, vegetable fiber, wax, paraffin, starch, tracanth, cellulose derivative, polyethylene glycol, silicone, bentonite, silica, talc or zinc oxide may be used as a carrier component. can

When the formulation of the present invention is a powder or spray, lactose, talc, silica, aluminum hydroxide, calcium silicate or polyamide powder may be used as a carrier component, and in particular, in the case of a spray, additional chlorofluorohydrocarbon, propane , butane or a propellant such as dimethyl ether.

When the formulation of the present invention is a solution or emulsion, a solvent, solvating agent or emulsifying agent is used as a carrier component, such as water, ethanol, isopropanol, ethyl carbonate, ethyl acetate, benzyl alcohol, benzyl benzoate, propylene glycol, 1 ,3-butyl glycol oil, fatty acid esters of glycerol, polyethylene glycol or sorbitan.

When the formulation of the present invention is a suspension, as a carrier component, a liquid diluent such as water, ethanol or propylene glycol, an ethoxylated isostearyl alcohol, a suspending agent such as polyoxyethylene sorbitol ester and polyoxyethylene sorbitan ester, microcrystalline Cellulose, aluminum metahydroxide, bentonite, agar or tracanth and the like may be used.

In addition, the present invention provides a health functional food composition containing ocher extract as an active ingredient.

Health functional food is a food made by adding loess extract to food materials such as beverages, teas, spices, chewing gum, confectionery, etc., or by encapsulation, powdering, suspension, etc. However, unlike general drugs, it has the advantage of not having side effects that may occur when taking drugs for a long time by using food as a raw material. The health functional food of the present invention obtained in this way is very useful because it can be consumed on a daily basis. The addition amount of ocher extract in such a health functional food cannot be uniformly defined depending on the type of target health functional food, but it can be added within a range that does not impair the original taste of the food, and is usually 0.01 for the target food. to 50% by weight, preferably 0.1 to 20% by weight. In addition, in the case of health functional foods in the form of pills, granules, tablets or capsules, it is usually added in the range of 0.1 to 100% by weight, preferably 0.5 to 80% by weight. In one embodiment, the health functional food of the present invention may be in the form of pills, tablets, capsules or beverages.

In addition, the present invention provides a quasi-drug composition containing ocher extract as an active ingredient.

In the present invention, the term 'quasi-drug' refers to items that have a milder action than pharmaceuticals among items used for the purpose of diagnosing, treating, improving, mitigating, treating or preventing human or animal diseases. For example, according to the Pharmaceutical Affairs Act of the Republic of Korea Quasi-drugs are products excluding items used for medicinal purposes, and include products used for the treatment or prevention of human or animal diseases, products with minor or no direct action on the human body, etc.

The quasi-drug composition may be used by adding the ocher extract as it is or in combination with other quasi-drugs or quasi-drug ingredients, and may be appropriately used according to a conventional method. The mixing amount of the active ingredient may be appropriately determined depending on the purpose of use.

The quasi-drug composition of the present invention is not limited thereto, but is preferably a body cleanser, disinfectant cleanser, detergent, kitchen detergent, cleaning detergent, toothpaste, gargling agent, wet tissue, detergent, soap, hand wash, hair detergent, hair softener, and humidifier filler. , It may be one or more formulations selected from the group consisting of masks, ointments and filter fillers. The quasi-drug composition of the present invention may be applied with the same contents as described for the cosmetic composition, except for differences depending on the dosage form.

The present invention provides a method for improving skin whitening comprising administering the ocher extract to a subject.

As used herein, the term "individual" refers to all animals including mammals including rats, livestock, humans, and the like.

In the skin whitening improvement method of the present invention, the dosage, administration route, administration method, etc. of the ocher distillation composition may be appropriately selected.

Specifically, in the present invention, 'administration' means introducing the composition of the present invention to a subject by any suitable method, and the administration route of the composition is through any general route as long as it can reach the target tissue and exhibit a skin whitening effect. can be administered. The administration may include application to the skin, and may include intraperitoneal administration, intravenous administration, intramuscular administration, subcutaneous administration, intradermal administration, oral administration, topical administration, and intranasal administration, but is not limited thereto. Specifically, due to the nature of the composition of the present invention having a skin whitening effect, the administration route of the composition may be administered by applying it to the skin.

The composition of the present invention may be administered daily or intermittently, and the number of administrations per day may be administered once or divided into 2 or 3 times. In addition, the composition of the present invention can be used alone or in combination with other substances for skin whitening. Considering all of the above factors, it is important to administer an amount that can obtain the maximum effect with the minimum amount without side effects, which can be easily determined by those skilled in the art.

Hereinafter, preferred embodiments are presented to aid understanding of the present invention, but the following examples are merely illustrative of the present invention, and various changes and modifications are possible within the scope and spirit of the present invention. It is obvious to those skilled in the art, It goes without saying that these variations and modifications fall within the scope of the appended claims.

Example 1. Loess Extract 1

Ocher was obtained from a cypress forest located in Goseong-gun, and stored in a refrigerator before use. The ocher derived from the cypress forest and distilled water were mixed at a weight ratio of 2: 20, allowed to stand at room temperature (25 ° C) for 416 days (10000 hours), and then only the supernatant was recovered excluding the solids formed by sedimentation, and filtered to After removing the fine solids, 20 ml of ocher extract was obtained by recovering only the filtrate. Photographs taken before and after filtration are shown in FIGS. 1 and 2 .

Example 2. Loess Extract 2

Ocher was obtained from a cypress forest located in Goseong-gun, and stored in a refrigerator before use. The ocher derived from the cypress forest and distilled water were mixed at a weight ratio of 2: 20, allowed to stand at room temperature (25 ° C) for 416 days (10000 hours), and then only the supernatant was recovered excluding the solids formed by sedimentation, and filtered to After removing the fine solids, only the filtrate was recovered. The filtrate (about 20 ml) was distilled under reduced pressure at 45 ° C. and 79 torr, and at this time, by recovering the remaining liquid after concentration, ocher extract (also referred to as ‘loess concentrate’ or ‘loess extract concentrate’) 1 ml was obtained (FIG. 3).

Comparative Example 1. Loess Powder

2 mg of ocher powder obtained from a cypress forest located in Goseong-gun was prepared. In the experiment, a solution in which 1 mg of ocher powder was mixed with 10 ml of distilled water was used for analysis.

Comparative Example 2. Kojic acid solution

Kojic acid (5-hydroxy-2-(hydroxymethyl)-4H-pyran-4-one) (CAS: 501-30-4) was purchased from Sigma and used. The kojic acid was diluted by concentration (0, 0.025, 0.05, 0.075, 0.1, 1 mg/ml) using distilled water to prepare a kojic acid solution.

<Test Example>

Test Example 1. Component Analysis of Hwangcho Extract

1) pH analysis

Immediately after preparing the loess extract of Examples 1 and 2 and the cypress extract of Comparative Example 3, the pH of each solution was measured using pH paper. As a result, it was confirmed that the ocher extracts of Examples 1 and 2 had a pH of 4.5 to 5.

2) XRD analysis

In order to analyze the components of loess extract 1 of Example 1 and loess powder solution of Comparative Example 1, analysis was performed using an X-ray diffractometer (XRD, D8 Advance, Bruker, Germany).

4 is a graph showing the XRD analysis results for the ocher powder solution obtained from Comparative Example 1, and FIG. 5 is a graph showing the XRD analysis results for the loess extract 1 prepared from Example 1.

As shown in FIGS. 4 and 5, in the case of ocher powder, the main component was silica (SiO ₂ ), but in the loess extract, it was confirmed that a large amount of inorganic materials other than silica was present.

3) SEM-EDS analysis

SEM-EDS (Scanning Electron Microscopy with Energy Dispersive Spectroscopy) (Hitachi, S-4800, Japan) was used to analyze the chemical composition of loess extract 1 of Example 1 and loess powder solution of Comparative Example 1. At this time, in the case of ocher powder, 1 mg of ocher powder was mixed with 10 ml of distilled water and then analyzed.

6 is an image observed by SEM-EDS of the loess powder solution obtained from Comparative Example 1, and FIG. 7 is an image observed by SEM-EDS of ocher extract 1 prepared from Example 1.

As shown in FIGS. 6 and 7, it was confirmed that the ocher powder was mixed with a large amount of components, specifically silica (SiO ₂ ), alumina (Al ₂ O ₃ ), organic matter (carbon, C), inorganic matter (Cl , K, Fe, etc.) were confirmed to exist.

On the other hand, it was confirmed that the ocher extract was more diverse than ocher powder and contained a high concentration of inorganic materials, specifically silica (SiO ₂ ), alumina (Al ₂ O ₃ ), organic materials (carbon, C), and inorganic materials (Cl). , K, Fe, Ca, Na, Mg, etc.) were confirmed to exist. In particular, it can be seen that the ocher extract has a greater increase in the content and types of inorganic substances than ocher powder.

In addition, through the high content of oxygen (O) component of the ocher concentrate, it can be seen that inorganic substances exist in an oxidized form. For example, it may be calcium carbonate, magnesium oxide, alumina, silica, iron oxide (Fe ₂ O ₃ ), and the like.

4) ICP analysis

The components and contents of the ocher extract 2 prepared from Example 2 and the ocher powder solution of Comparative Example 1 were quantitatively analyzed with an inductively coupled plasma spectrophotometer (ICP-OES, Perkin Elmer, Waltham, MA, USA), and Table 1 below shown in

division Composition of ions (mg/L) Na Mg Al Fe Ca Si Example 2 190.16 3.064 8.08 3.62 65.3 82.04 Comparative Example 1 0.076 0.005 0.026 0.006 0.015 0.012

According to the ICP analysis shown in Table 1, the loess extract 2 prepared in Example 2 has a Si/Al element composition ratio of about 10.15. In contrast, the loess powder solution of Comparative Example 1 has a Si/Al element composition ratio of about 0.46. That is, it was confirmed that ocher extract 2 prepared from Example 2 had a higher silica/alumina ratio and also had a high concentration of inorganic substances, even though it was a solution obtained by distilling and concentrating ocher. In the case of silica, it is a representative additive that improves the spreadability and applicability of cosmetics on the skin, and inorganic substances such as K, Mg, and Fe (also referred to as 'minerals') play a very important role in improving bio-metabolism and skin penetration. Ocher extract is a cosmetic, and it can be seen that it is easy to use regardless of the formulation.

Test Example 2. Analysis of whitening activity of loess extract and loess water

1) DOPA oxidation inhibition assay

In order to analyze the whitening activity, the inhibitory activity of tyrosinase was confirmed through the inhibition of DOPA oxidation activity, which was tested by modifying Flurkey's method. DOPA oxidation inhibition assay was performed by measuring DOPA quinone production using L-DOPA. Samples used loess extract 1 prepared from Example 1 and loess extract 2 prepared from Example 2, and the samples were dissolved in distilled water and diluted to five concentrations of 0%, 25%, 50%, 75%, and 100%. and used it. As a positive control, the kojic acid solution of Comparative Example 2 was used, which was also used at five concentrations of 0 mg/ml, 0.025 mg/ml, 0.05 mg/ml, 0.075 mg/ml, 0.1 mg/ml, and 1 mg/ml. diluted and used.

Acontrol: 0.2 mL of 10 mM L-3,4-dohydroxyphenylalanine in 0.6 mL of 100 mM sodium phosphate buffer adjusted to pH 6.8, mushroom tyrosinase (100 U/mL) 0.2 mL was added and reacted at 37 °C for 5 minutes.

Bcontrol: 0.2 mL of 10 mM L-DOPA (L-3,4-dohydroxyphenylalanine) was added to 0.8 mL of 100 mM sodium phosphate buffer adjusted to pH 6.8, followed by reaction at 37 °C for 5 minutes.

Asample: 0.2 mL of 10 mM L-DOPA (L-3,4-dohydroxyphenylalanine) in 0.5 mL of 100 mM sodium phosphate buffer adjusted to pH 6.8, mushroom tyrosinase (100 U/mL) 0.2 mL and 0.1 mL of the sample were added and reacted at 37°C for 5 minutes.

Bsample: 0.2 mL of 10 mM L-DOPA (L-3,4-dohydroxyphenylalanine) and 0.1 mL of the sample were added to 0.7 mL of 100 mM sodium phosphate buffer adjusted to pH 6.8 and reacted at 37 ° C. for 5 minutes.

Then, the absorbance of each of the above solutions was measured at a wavelength of 475 nm using a spectrophotometer, and the DOPA oxidation activity inhibitory ability was calculated using Equation 1 below.

[Equation 1]

DOPA oxidation inhibition efficacy (%) = [1 - (Asample-Bsample/Acontrol-Bcontrol)]ㅧ100

8 is a result of confirming the DOPA-oxidase inhibitory efficacy by concentration for loess extract 1 prepared from Example 1, and FIG. 9 is a dopa by concentration for loess extract 2 prepared from Example 2 10 is a result confirming the DOPA-oxidase inhibitory efficacy by concentration for the kojic acid solution prepared from Comparative Example 2, and three Results from independent experiments are expressed as mean ± standard deviation.

8 to 10, it was confirmed that both the loess extract 1 of Example 2 and the loess extract 2 of Example 1 had tyrosinase inhibition rate. In particular, loess extract 2 prepared from Example 2 of the present invention had a tyrosinase inhibition rate more than twice as high as loess extract 1 of Example 1, and was confirmed to be about six times higher at the highest concentration, 100%. , It can be seen that the loess extract 2 prepared from Example 2 of the present invention has a significantly higher effect of inhibiting the oxidation reaction of dopa compared to general loess water.

Loess extract 1 of Example 1 showed only a maximum of 20% tyrosinase inhibition rate, and at a concentration of 50% or more, it was confirmed that the tyrosinase inhibition rate was rather lowered. 2 increased activity in a concentration-dependent manner. That is, it can be seen that the loess extract 2 prepared from Example 2 of the present invention has a difference in effect from components that simply concentrate the loess water (loess soil extract).

It was confirmed that loess extract 2 prepared from Example 2 exhibited a similar level of activity to the kojic acid solution as a positive control.

Test Example 3. Cell viability measurement by MTT assay

MTT assay was used to evaluate the effect of ocher extract 2 prepared in Example 2 on cytotoxicity. The MTT assay is a standard colorimetric assay as a laboratory test method for measuring cell viability. MTT assay, a technique that can accurately measure cell proliferation and living cells, is one of the essential techniques in the field of life science, especially in tumor biology.

In order to confirm the toxicity of ocher extract 2 prepared from Example 2 of the present invention, an experiment was performed with human dermal fibroblast (HDFa). First, human dermal fibroblast (HDFa) was mixed with Low Serum Growth Supplement in Medium 106, and incubated in a medium containing penicillin (100 IU/ml) and streptomycin (100 μg/ml) at 37°C and 5% CO _{2 .} It was cultured in an incubator containing The cells were dispensed into a 96 well plate and cultured for 18 hours under cell culture conditions. After removing the medium and washing with PBS, fresh medium and samples were added, respectively, and cultured for 18 hours. After 18 hours, cell viability was confirmed by performing MTT ASSAY, which can confirm cell viability by measuring mitochondria activity of living cells in order to measure cell viability, and the results are shown in Table 2 below.

division Loess extract of Example 2, concentration mg/ml 0 0.1 One 10 50 100 Cell viability (%) 100 110.2 102.5 105.4 111.4 113.5

As shown in Table 2, ocher extract 2 prepared from Example 2 of the present invention showed a high cell viability of 100% or more in all samples for fibroblasts.

Hereinafter, formulation examples of the composition containing the powder of the present invention will be described, but the present invention is not intended to limit them, but only to be specifically described.

Preparation Example 1. Preparation of granules

1,000 mg of ocher extract of Example 2

Appropriate amount of vitamin mixture

Vitamin A Acetate 70 μg

Vitamin E 1.0 mg

Vitamin B1 0.13 mg

Vitamin B2 0.15 mg

Vitamin B6 0.5 mg

Vitamin B12 0.2 μg

Vitamin C 10 mg

10 μg of biotin

Nicotinamide 1.7 mg

Folic acid 50 μg

Calcium Pantothenate 0.5 mg

Appropriate amount of mineral mixture

Ferrous sulfate 1.75 mg

Zinc Oxide 0.82 mg

Magnesium Carbonate 25.3 mg

Potassium Phosphate Monobasic 15 mg

Dibasic Calcium Phosphate 55 mg

Potassium citrate 90 mg

Calcium Carbonate 100 mg

Magnesium Chloride 24.8 mg

Although the composition ratio of the above vitamin and mineral mixture was prepared by mixing ingredients suitable for granules in a preferred embodiment, the mixing ratio may be arbitrarily modified, and after mixing the above ingredients according to a conventional granule manufacturing method, It can be prepared and used for preparing a health functional food composition according to a conventional method.

Production Example 2. Production of functional beverages

1,000 mg of ocher extract of Example 2

Citric Acid 1,000 mg

100 g of oligosaccharides

2 g plum concentrate

1 g of taurine

Add purified water to total 900 mL

After mixing the above ingredients according to the normal health drink manufacturing method, stirring and heating at 85 ° C. for about 1 hour, the resulting solution is filtered and collected in a sterilized 2 L container, sealed and sterilized, and then refrigerated. It is used for preparing the functional beverage composition of the present invention.

Although the composition ratio is a mixture of ingredients suitable for a relatively favorite beverage in a preferred embodiment, the mixing ratio may be arbitrarily modified according to regional and ethnic preferences such as the class of demand, the country of demand, and the purpose of use.

Preparation examples of cosmetic compositions suitable for application of the present invention will be presented.

Preparation Example 3: Lotion

Table 3 below shows preparation examples of lotion among cosmetics containing the ocher extract of Example 2.

ingredient Content (% by weight) Yellow clay extract of Example 2 5.0 glycerin 6.0 1,3-butylene glycol 3.0 PEG 1500 1.0 allantoin 0.1 DL-panthenol 0.3 EDTA-2Na 0.02 Benzophenone-9 0.04 sodium hyaluronate 5.0 ethanol 10.0 Polysorbate 20 0.2 preservatives, fragrances, colors a very small amount Distilled water balance Sum 100

Preparation Example 4: Lotion

Examples of preparation of a lotion among cosmetics containing the loess extract of Example 2 are shown in Table 4 below.

ingredient Content (% by weight) Yellow clay extract of Example 2 3.0 propylene glycol 6.0 glycerin 4.0 triethanolamine 1.2 Tocopheryl Acetate 3.0 liquid paraffin 5.0 squalane 3.0 macadamia nut oil 2.0 polysorbate 60 1.5 Sorbitan sesquioleate 1.0 carboxyvinyl polymer 1.0 preservatives, fragrances, colors a very small amount Distilled water balance Sum 100

Preparation Example 5: Nutrition Cream

Examples of preparation of nutritional cream among cosmetics containing the loess extract of Example 2 are shown in Table 5 below.

ingredient Content (% by weight) Yellow clay extract of Example 2 1.0 Pro-type glycerin monostearate 1.5 cetearyl alcohol 1.5 stearic acid 1.0 polysorbate 60 1.5 Sorbitan Stearate 0.6 isostearyl isostearate 5.0 squalane 5.0 mineral oil 35.0 dimethicone 0.5 Hydroxyethyl Cellulose 0.12 glycerin 6.0 triethanolamine 0.7 preservatives, fragrances, colors a very small amount Distilled water balance Sum 100

Preparation Example 6: Essence

Table 6 shows examples of preparation of the essence among cosmetics containing the ocher extract of Example 2.

ingredient Content (% by weight) Yellow clay extract of Example 2 1.5 glycerin 10.0 betaine 5.0 PEG 1500 2.0 allantoin 0.1 DL-panthenol 0.3 EDTA-2Na 0.02 Benzophenone-9 0.04 Hydroxyethyl Cellulose 0.1 sodium hyaluronate 8.0 carboxyvinyl polymer 0.2 triethanolamine 0.18 Octyldodecanol 0.3 Octyldodeces-16 0.4 ethanol 6.0 preservatives, fragrances, colors a very small amount Distilled water balance Sum 100

Preparation Example 7: Emulsion for mask pack

Table 7 shows examples of preparation of emulsion for mask pack among cosmetics containing ocher extract of Example 2.

ingredient Content (% by weight) Yellow clay extract of Example 2 1.0 polyvinyl alcohol 15.0 cellulose gum 0.15 glycerin 3.0 PEG 1500 2.0 cyclodextrin 0.15 DL-panthenol 0.4 allantoin 0.1 Monoammonium glycyrrhizinate 0.3 nicotinamide 0.5 ethanol 6.0 PEG 40 hydrogenated castor oil 0.3 preservatives, fragrances, colors a very small amount Distilled water balance Sum 100

Claims (13)

A cosmetic composition for skin whitening, characterized in that it contains ocher extract as an active ingredient,
The ocher extract was prepared by mixing ocher with water, lower alcohol having 1 to 4 carbon atoms, ethylene glycol, ethyl ether, or a mixed solvent thereof, leaving it to stand for 410 to 420 days, recovering the supernatant, and distilling it under reduced pressure. Characterized in a cosmetic composition for skin whitening. delete According to claim 1,
The distillation temperature during distillation under reduced pressure is 30 to 50 ° C, and the pressure is 50 to 100 torr. According to claim 1,
The ocher is a cosmetic composition for skin whitening, characterized in that obtained from a colony in which cypress trees grow naturally. According to claim 1,
When the ocher extract was analyzed by ICP analysis, it contained 190.16 mg/l of sodium, 30.64 mg/l of magnesium, 8.08 mg/l of aluminum (Al), 3.62 mg/l of iron, 65.3 mg/l of calcium, and 82.04 mg/l of silica. A cosmetic composition for skin whitening, characterized in that the. According to claim 1,
The ocher extract is a cosmetic composition for skin whitening, characterized in that inhibiting tyrosinase (tyrosinase). (a) mixing loess with a solvent, allowing it to stand for 410 to 420 days, and then recovering the supernatant; and
(b) distilling the supernatant obtained from step (a) under reduced pressure under pressurized conditions of 30 to 50 ° C and 50 to 100 torr to obtain a loess extract; characterized in that it comprises a, skin whitening cosmetic composition of manufacturing method. According to claim 7,
The solvent is water, lower alcohol having 1 to 4 carbon atoms, ethylene glycol, ethyl ether, or a mixture of these solvents, characterized in that for producing a cosmetic composition for skin whitening. According to claim 7,
Before step (b), (a1) filtering the supernatant obtained from step (a); method for producing a cosmetic composition for skin whitening, characterized in that it further comprises. According to claim 7,
Method for producing a cosmetic composition for skin whitening, characterized in that the mixed weight ratio of ocher and the solvent in step (a) is 1: 1 to 100. delete A health functional food composition for skin whitening, characterized in that it contains ocher extract as an active ingredient,
The ocher extract was prepared by mixing ocher with water, lower alcohol having 1 to 4 carbon atoms, ethylene glycol, ethyl ether, or a mixed solvent thereof, leaving it to stand for 410 to 420 days, recovering the supernatant, and distilling it under reduced pressure. Health functional food composition for skin whitening. A quasi-drug composition for skin whitening, characterized in that it contains ocher extract as an active ingredient,
The ocher extract was prepared by mixing ocher with water, lower alcohol having 1 to 4 carbon atoms, ethylene glycol, ethyl ether, or a mixed solvent thereof, leaving it to stand for 410 to 420 days, recovering the supernatant, and distilling it under reduced pressure. A quasi-drug composition for skin whitening.