Camellia extract and its manufacturing method

Abstract

To provide an extract from camellia leaves having antioxidant action and a method for producing the same.SOLUTION: Drying camellia leaves under light irradiation provides an extract having high antioxidant action.SELECTED DRAWING: None

Description

[Technical field]

[0001] The present invention relates to a camellia, in particular to an extract of camellia leaves and a method for preparing the same. [Background technology]

[0002] Humans use oxygen as energy. As long as we use oxygen as energy, some of the oxygen becomes active oxygen such as superoxide (O2-), hydroxyl radical (OH-), and peroxynitrite (ONOO-), and it has been proposed that these active oxygen are the cause of various aging and diseases. In order to eliminate the harmful effects of active oxygen, the living body can directly eliminate active oxygen using enzymes such as superoxide dismutase (SOD). However, the ability of SOD and other enzymes decreases with age, resulting in various aging phenomena.

[0003] In addition, since the skin is the outermost layer of the body, it is constantly exposed to both endogenous reactive oxygen species and oxidative stress caused by exogenous reactive oxygen species caused by ultraviolet rays. It is known that collagen and hyaluronic acid in the dermis of the skin are denatured, causing the skin to lose firmness and elasticity, leading to wrinkles and sagging.

[0004] Sebum secreted on the skin helps to protect the skin from exogenous stress, but this sebum is oxidized by ultraviolet rays and becomes lipid peroxide, which is said to be involved in aging by irritating the skin, attacking and damaging cells, and causing various other adverse effects. Therefore, protection from active oxygen is considered to be effective not only in preventing the deterioration of the skin condition, but also in preventing skin aging.

[0005] In this situation, materials that protect the skin from oxidation include vitamin E, carotenoids, and sesamin. In addition, plants contain a lot of polyphenols such as flavonoids, tannins, and anthocyanins, and because they have high antioxidant properties, extracts from many kinds of plants are used.

[0006] In this context, it has been reported that camellia leaves and flowers contain antioxidant ingredients. Camellia leaf extract, which is used as a cosmetic ingredient, has been reported to have antioxidant, female hormone-like, cell activation, and collagen production effects. Camellias are evergreen trees and can be used all year round, making them highly valuable as cosmetic ingredients. [Prior art documents] [Patent documents]

[0007] [Patent Document 1] JP 2012-102049 A [Non-patent literature]

[0008] [Non-Patent Document 1] Ken-ichi Onodera, et al, Biosci.Biotechnol.Biochem.,70(8), 1995~1998(2006) [Non-Patent Document 2] Mei Jing Piao, et al, Int. J. Mol. Sci. 12, 2618-2630(2011) Summary of the Invention [Problem to be solved by the invention]

[0009] Usually, to obtain an extract from a plant, it is extracted with water or a mixture of water and an organic solvent. A thick layer of cutin is deposited on the cell walls on the surface of the upper epidermis of camellia leaves, and a cuticle layer permeated with wax has developed, providing protection against strong light and ultraviolet rays and preventing water loss from areas other than the stomata. 、 At room temperature Camellia leaves It is difficult to dry the leaves sufficiently, so the leaves are generally chopped and Direct hot air drying Drying using methods such as has been carried out In addition, camellia, especially its leaves, have antioxidant properties. Contains substances It was known that. However, there is a problem that it is difficult to maintain the antioxidant properties when direct hot air drying is performed. This antioxidant is efficient and highly active maintainedThere has been a demand for a way to obtain this in a stable state. [Means for solving the problem]

[0010] The present inventors have discovered that in the process of drying camellia, particularly camellia leaves, rather than directly drying them with hot air, it is possible to obtain an extract with more active antioxidant activity than conventional methods by drying camellia leaves for a certain period of time under light irradiation and then extracting them with a solvent, thereby achieving the object of the present invention. That is, the present invention is capable of detecting the presence of a substance under irradiation with light having an illuminance of 2,000 Lux to 1,000,000 Lux. 32 The extract is obtained by extracting leaves of a plant of the genus Camellia of the family Theaceae, which have been dried for at least 10 hours and not more than 100 hours, with water, a hydrophilic solvent, or a mixture thereof. Here, the plant of the genus Camellia of the family Theaceae is preferably Camellia japonica or a subspecies thereof. In addition, the illuminance is preferably 10,000 Lux to 100,000 Lux.

[0011] The drying under light irradiation is preferably sun drying, and the dried camellia leaves are preferably additionally dried. The additional drying is preferably hot air drying. The hydrophilic solvent is preferably ethanol or 1,3-butylene glycol, and the mixed solution is preferably a heated 50 (v / v)% ethanol solution. The extract of the present invention preferably has at least DPPH radical scavenging activity or superoxide dismutase-like activity, and more preferably has DPPH radical scavenging activity and superoxide dismutase-like activity.

[0012] The present invention also relates to an antioxidant containing the above-mentioned extract of the leaves of a plant of the genus Camellia of the family Theaceae. The present invention further relates to a method for treating the oxidative stress caused by irradiating the leaves of a plant of the genus Camellia of the family Theaceae under light with an illumination intensity of 2,000 Lux to 1,000,000 Lux. 32 a drying step of drying the additional dried leaves of the plant for a period of not less than 100 hours and not more than 100 hours to obtain dried leaves of the plant, and an extraction step of extracting the additional dried leaves of the plant obtained in the additional drying step with water alone or a mixture of water and a hydrophilic solvent. Preferably, the method further includes an additional drying step of further drying the dried leaves of the plant obtained in the drying step. Effect of the Invention

[0013] The camellia extract of the present invention is produced by a process of drying the extract under light irradiation for a certain period of time, which is different from the conventional manufacturing process. The extract obtained inMore than the Antioxidant Effects of Increase to make It is possible. Therefore, by using the same amount of extract in cosmetics as before, expensive Antioxidant effect Have In addition, it is possible to manufacture cosmetics that Because it produces extracts with high antioxidant properties, As a result, a smaller amount of extract has the same antioxidant effect as conventional extracts. Manufacture cosmetics This allows for the formulation of final products such as cosmetics to be more easily designed. Expand your horizons It is also possible. [Brief description of the drawings]

[0014] [Figure 1] FIG. 1 is a graph showing the results of a diphenylpicrylhydrazyl (hereinafter also referred to as "DPPH") radical test. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0015] The present invention will be specifically described below. The genus Camellia of the family Theaceae used in the present invention specifically includes Camellia japonica, Camellia japonica, Camellia japonica, Camellia sasanqua, Camellia yukari, Camellia japonica ...

[0016] Camellia japonica is an evergreen tall tree and a representative species of evergreen broad-leaved forest in Japan. It is distributed in the hilly areas of Honshu (south of Aomori Prefecture), Shikoku, and Kyushu. Camellia oil is an oil pressed from the seeds (fruit) of camellias, and has been used since ancient times. Its wide range of uses can be said to be comparable to that of Japanese olive oil. It is used as a high-quality cooking oil and hair styling product, and in the past it was often used as fuel oil for lighting. A decoction of camellia leaves is said to be effective against gastrointestinal bleeding, and has been drunk in Okinawa since ancient times, and in Nagasaki it is mixed with green tea and drunk as Goto camellia tea, which suppresses the absorption of neutral fats. In addition, camellia leaves are used as a cosmetic ingredient, and it has been reported that they have antioxidant effects, female hormone-like effects, cell activation effects, and collagen production effects. In addition, because camellias are evergreen, they are highly valuable as a cosmetic ingredient that can be used all year round.

[0017] The tissues of camellia used in the present invention are not particularly limited, but specific examples include leaves, stems, flowers, and fruits. Leaves are preferred. Multiple tissues can be used as long as they do not produce the effects of the present invention.

[0018] The illuminance of light when drying camellia leaves is not particularly limited as long as the effect of the invention is achieved. Specifically, the lower limit of the illuminance is 1,000 lux, preferably 2,000 lux, and more preferably 5,000 lux. The upper limit is 1,000,000 lux or less, preferably 500,000 lux, and more preferably 100,000 lux.

[0019] The light source used to dry camellia leaves is not particularly limited as long as it achieves the effects of the invention. There are natural light sources and artificial light sources. In the case of natural light sources, the sun can be used as the light source. In the case of artificial light sources, incandescent light bulbs, fluorescent lights, LEDs, etc. are included. The most preferred light source is the sun, i.e. drying in the sun.

[0020] The time for drying camellia leaves under light irradiation is not particularly limited as long as the effects of the invention are achieved. Specifically, the lower limit is 3 hours or more, preferably 8 hours or more, more preferably 20 hours or more, and more preferably 30 hours or more. The upper limit is 100 hours or less, preferably 80 hours or less, more preferably 60 hours or less, and more preferably 45 hours or less.

[0021] It is not necessary to continuously irradiate light when drying camellia leaves. In other words, there is no problem if there are periods of light irradiation and periods without light. In that case, the time spent drying while irradiating light is the time during which light is irradiated, and the time without light is not calculated. When drying in the sun, if light is irradiated for 8 hours a day and light is not irradiated for 16 hours a day, the lower limit is 0.5 days or more, preferably 1 day or more, and more preferably 3 days or more, and the upper limit is 10 days or less, preferably 7 days or less, and more preferably 6 days or less.

[0022] The temperature at which camellia leaves are dried is not particularly limited as long as the effects of the invention are achieved. Specifically, the lower limit is 0° C., preferably 10° C., and more preferably 15° C. Specifically, the upper limit is 50° C., preferably 40° C., and more preferably 35° C.

[0023] Regarding the above drying conditions, the humidity is not particularly limited as long as it achieves the effects of the invention. Specifically, it is 95% RH or less, preferably 85% RH or less, and more preferably 60% RH or less. Furthermore, when drying camellia leaves, there is no particular limit to the location. In the case of sunlight, it may be indoors or outdoors.

[0024] In this way, the camellia leaves dried under light can be further dried (hereinafter, this may be referred to as "additional drying"). Further drying reduces the moisture inside the camellia leaves, making it easier to control the next extraction step, and reduces the volume of the camellia leaves, making it easier to carry out the subsequent extraction step. The conditions for the additional drying are not particularly limited as long as the effects of the invention are achieved. Specific examples include hot air drying, freeze drying, and reduced pressure drying. A better drying method is hot air drying. The drying conditions are not particularly limited, but in the case of hot air drying, the lower limit of the temperature condition is 40°C, preferably 45°C, and more preferably 50°C. The upper limit is 90°C, preferably 80°C, and more preferably 70°C. The drying time for the drying is not particularly limited as long as the effects of the invention are achieved. Specifically, it is 12 hours or more, preferably 24 hours or more, and more preferably 48 hours or more.

[0025] In order to efficiently obtain camellia leaf extract in the extraction step, the dried camellia leaves obtained may be cut. By cutting, the contact area with the extraction solvent can be increased, improving the extraction efficiency. The cutting method is not particularly limited. The cut pieces are not particularly limited as long as they can be efficiently extracted in the extraction step, but a sieve of 16 mesh or less, preferably 32 mesh or less, more preferably 42 mesh or less, and even more preferably 100 mesh or less according to the JIS standard can be used. In addition, in this cutting step, cutting may be performed at any stage as long as the effects of the present invention are achieved.

[0026] A general method can be used to obtain an extract from the dried camellia leaves. The solvent used during extraction is not particularly limited as long as it achieves the effects of the present invention. Specifically, water and / or an organic solvent can be used. Preferably, water and / or a hydrophilic solvent can be used. The organic solvent can be an alcohol, a polyhydric alcohol, or the like. Ethanol or 1,3-butylene glycol is preferred.

[0027] The highly antioxidant camellia leaf extract of the present invention can be incorporated into preparations such as medicines, cosmetics, and other skin care products, as well as food and beverage products.

[0028] When preparing a skin external preparation containing camellia leaf extract, the ingredients can be selected according to the mode of use, and for example, purified water, lower alcohols, polyhydric alcohols, higher alcohols, oils and fats, waxes, silicones, powders, surfactants, water-soluble polymers, plant extracts, UV absorbers, thickeners, dyes, preservatives, fragrances, antioxidants, etc. can be used. Similarly, when preparing food and beverage products, diluents or excipients that are commonly used, such as fillers, extenders, binders, disintegrants, surfactants, and lubricants, can be used. In this way, the product can be produced by combining ingredients and additives used in preparations of quasi-drugs, cosmetics, food and beverage products, etc., within the range that does not impair the effects of the present invention, and the content in the preparation is not particularly specified.

[0029] The camellia leaf extract of the present invention, and further the skin external preparation or food and drink may be in any form, and may be used by blending it with quasi-drugs, cosmetics, or food and drink such as ampoules, capsules, powders, granules, pills, tablets, solids, liquids, gels, foams, emulsions, creams, ointments, and sheets. Specifically, for example, skin external preparations include basic cosmetics such as lotions, emulsions, creams, ointments, lotions, oils, and packs, face washes and skin cleansers, and makeup cosmetics such as foundations, face powders, face powders, lipsticks, blushers, eye shadows, eyeliners, mascaras, eyebrow inks, and eyelashes. General food and drink products may also be used in supplements, drinks, cereals, powdered drinks, jellies, biscuits, candies, gums, and the like. EXAMPLES

[0030] The present invention will be described below with reference to examples, but the present invention is not limited to these examples.

[0031] Examples 1 to 5 Camellia leaves were collected and dried outdoors (sun-dried) for 8 hours a day (10:00-18:00, stored in a dark place except for this time) under a clear sky with an average temperature of 25°C. The drying period was the 3rd day (light irradiation time: 24 hours, Example 1), the 4th day (light irradiation time: 32 hours, Example 2), the 5th day (light irradiation time: 40 hours, Example 3), the 6th day (light irradiation time: 48 hours, Example 4), and the 7th day (light irradiation time: 56 hours, Example 5). 20 g of each of the camellia leaves dried in this way was collected. Next, hot air drying was performed for 24 hours under conditions of 50°C and 0% humidity to obtain dried camellia leaves. The dried camellia leaves were crushed in a crusher. The crushed dried camellia leaf powder was passed through a 16-mesh sieve. 18 g of 50 (v / v)% ethanol solution was added to 2 g of the dried camellia leaf powder prepared in this way, and extraction was performed at 50°C for 3 hours. After cooling, the mixture was filtered to obtain an extract.

[0032] Comparative Example 1 An extract was obtained under the same conditions as in Example 1, except that the drying time was set to 0 hours under a clear sky at an average temperature of 25°C.

[0033] Experimental Example 1 DPPH (diphenylpicrylhydrazyl) radical test The extracts obtained in Examples 1 to 5 and Comparative Example 1 were diluted to a final concentration of 0.5 mg / mL. 3 mL of 0.2 mM DPPH absolute ethanol solution was added to 1 mL of the diluted sample to prepare a reaction solution. The reaction was then allowed to proceed at 25°C for 30 minutes, and the absorbance at a wavelength of 517 nm was measured using purified water as the control. In addition, the absorbance of the reaction solution to which purified water was added instead of the sample as a blank was taken as a DPPH radical scavenging rate of 0%, and the DPPH radical scavenging rate was calculated from the absorbance of each sample. The results calculated in this manner were Figure 1 As shown in.

[0034] figure The results of 1 show that drying camellia leaves under light irradiation resulted in a higher DPPH radical scavenging rate than drying without light irradiation.

[0035] Example 6 10 kg of camellia leaves were collected and dried outdoors (sun drying) for 5 days (total light exposure time: 40 hours) at an average temperature of 25°C and sunny weather, 8 hours a day (10:00-18:00, stored in a dark place except for these hours). The dried camellia leaves thus obtained were further dried at 50°C for 48 hours to obtain 3.8 kg of dried camellia leaves. The dried camellia leaves thus obtained were further crushed in a crusher and passed through a 16-mesh sieve to obtain powder. 8,000 g of 50 (v / v)% ethanol solution was added to 400 g of this powder and extracted at 50°C for 5 hours. After cooling, filtration was performed to obtain 7,125 g of extract. The solvent was removed from this extract using an evaporator to obtain 63.4 g of camellia leaf extract.

[0036] Comparative Example 2 1 kg of camellia leaves were dried at 50°C for 48 hours to obtain 375 g of dried camellia leaves. The dried camellia leaves were crushed in a grinder and passed through a 16 mesh sieve to obtain powder. 8,000 g of 50 (v / v)% ethanol solution was added to 400 g of this powder and extracted at 50°C for 5 hours. After cooling, filtration was performed to obtain 7,300 g of extract. The solvent was removed using an evaporator to obtain 70.8 g of camellia leaf extract.

[0037] Experimental Example 2 DPPH radical test The camellia extracts obtained in Example 6 and Comparative Example 2 were adjusted with 0.1 M acetate buffer (pH 5.5) to a final concentration of 0.1 to 1.0 mg / mL (ascorbic acid was 0.01 mg / mL), and 2 mL of absolute ethanol and 1 mL of 0.5 mM DPPH absolute ethanol solution were added to 2 mL of the solution to prepare a reaction solution. After that, the reaction was allowed to proceed at 37°C for 30 minutes, and the absorbance at a wavelength of 517 nm was measured using water as the target. In addition, the absorbance was measured using a reaction solution to which purified water was added instead of the sample as a blank. The concentration of the sample (IC50) at which the absorbance decreased by 50% was calculated in comparison with the blank.

[0038] Experimental Example 3 Superoxide dismutase (SOD)-like activity The camellia extracts obtained in Example 6 and Comparative Example 2 were adjusted to a final concentration of 0.1 to 1.0 mg / mL with 0.1 M acetate buffer (pH 5.5) to 0.1 mL, 0.10 mL of 1 mM sodium xanthine, 0.10 mL of 6 mM nitroblue tetrazolium, 1.70 mL of 0.1 M phosphate buffer (pH 8.0), and 0.10 mL of xanthine oxidase (derived from buttermilk) (1.2 U / mL) were added, reacted at 37°C for 20 minutes, and the absorbance at 560 nm was measured after the reaction was stopped. The concentration of the sample (IC50) at which the absorbance decreased by 50% was calculated compared to the blank. The results of Experimental Examples 2 and 3 are shown below.

[0039] [Table 1]

[0040] The camellia leaf extract subjected to the drying process under light irradiation in Example 6 exhibited approximately twice the DPPH radical scavenging ability and approximately three times the SOD-like activity compared to the camellia leaf extract not subjected to the drying process under light irradiation in Comparative Example 2.

[0041] Experimental Example 4 Quantitative determination of ellagitannins The camellia leaf extracts obtained in Example 6 and Comparative Example 2 were subjected to analysis of ellagitannins using liquid chromatography under the following conditions.

[0042] HPLC analysis conditions Column: Nacarai Tesque COSMOSIL 5C18-ARII (4.6x250) Detection wavelength: 210nm, 280nm, 350nm Flow rate: 0.8mL / min Column temperature: 35℃ Injection volume: 10μL Mobile phase: table 2 As shown in.

[0043] [Table 2]

[0044] As a result of Experimental Example 4, it was confirmed that the extract of Example 6 contained 0.063 mg / mL of ellagitannin, and the extract of Comparative Example 2 contained 0.008 mg / mL of ellagitannin.

[0045] The camellia leaf extract of the present invention has a high antioxidant effect. Therefore, cosmetics and the like containing the extract of the present invention can have a high antioxidant effect. [Industrial Applicability]

[0046] INDUSTRIAL APPLICABILITY The present invention is useful in the technical field of producing cosmetics having enhanced antioxidant properties.

Claims

1. An extract of leaves of a plant of the genus Camellia of the family Theaceae, which has been dried for a total period of 32 to 100 hours under light irradiation with an illumination intensity of 2,000 to 1,000,000 Lux, is extracted with water, a hydrophilic solvent, or a mixture of these.

2. 2. The extract of leaves of a plant of the genus Camellia of the family Theaceae according to claim 1, characterized in that the plant of the genus Camellia of the family Theaceae is Camellia japonica or a subspecies thereof.

3. 3. The extract of leaves of a plant of the genus Camellia of the family Theaceae according to claim 1 or 2, characterized in that the illuminance is from 10,000 Lux to 100,000 Lux.

4. 4. The extract of leaves of a plant of the genus Camellia in the family Theaceae according to any one of claims 1 to 3, characterized in that the drying under light irradiation is drying in the sun.

5. The extract of leaves of a plant of the genus Camellia of the family Theaceae according to claim 4, characterized in that the dried camellia leaves are further dried.

6. 6. The extract of leaves of a plant of the genus Camellia in the family Theaceae according to any one of claims 1 to 5, characterized in that the hydrophilic solvent is ethanol or 1,3-butylene glycol.

7. 7. An extract of leaves of a plant of the genus Camellia in the family Theaceae according to claim 1, having at least one of the effects of DPPH radical scavenging ability or superoxide dismutase-like activity.

8. An antioxidant comprising an extract of the leaves of a plant of the genus Camellia of the family Theaceae according to any one of claims 1 to 7.

9. a drying step of drying leaves of a plant of the genus Camellia in the family Theaceae under light with an illuminance of 2,000 Lux to 1,000,000 Lux for a total period of 32 hours to 100 hours to obtain dried leaves of said plant; an extraction step of extracting the dried leaves obtained in the drying step with water, a hydrophilic solvent, or a mixture thereof; A method for producing an extract of leaves of a plant of the genus Camellia in the family Theaceae, comprising:

10. 10. The method for producing an extract of leaves of a plant of the genus Camellia in the family Theaceae according to claim 9, further comprising an additional drying step of further drying the dried leaves of the plant obtained in the drying step.

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