JP2008255043A - Skincare preparation for external use - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a skincare preparation for external use characterized by containing extract of Cyclocarya paliurus. <P>SOLUTION: It has been found that the extract of Cyclocarya paliurus (Juglandaceae family, another name: Zenigata, Kikurokaya) has excellent DPPH (diphenylpycrylhydrazyl) radical-scavenging effect, collagenase activity-inhibitory effect and melanogenesis-inhibitory effect and is stable. The skincare preparation for external use characterized by containing the extract of Cyclocarya paliurus is highly safe and exhibits excellent anti-skin-aging effect and skin-lightening effect. The extract is usable in cosmetics, pharmaceuticals, quasi-drugs, etc., being preferably such as to be prepared from Cyclocarya paliurus's leaves, and its compounding level in the final preparation is preferably 0.001-10 wt.%. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to a skin external preparation excellent in anti-aging and whitening action by containing an extract of green willow.

  In recent years, free radicals and active oxygen have been taken up as factors that oxidize biological components, and their adverse effects have become a problem. It is said that free radicals and active oxygen are generated in the living body, decompose or cross-link biological tissues such as collagen, and oxidize lipids to form lipid peroxides that damage cells. Such disorders are thought to cause aging such as wrinkles and firmness of the skin, and one method of preventing aging is to incorporate an antioxidant that removes free radicals and active oxygen. Are known. Conventionally, ascorbic acid, tocopherol, 3,5-tert-butyl-4-hydroxytoluene (BHT), superoxide dismutase (SOD) and the like have been used as free radical scavengers used for the purpose of preventing aging.

  The skin is composed of epidermis, dermis, and subcutaneous tissue. Among them, the dermis is extremely important for maintaining the structure of the skin, and the elasticity of the skin is maintained by the dermal connective tissue formed from hyaluronic acid, collagen, and the like. It is believed that this connective tissue loses its contractile force and loses its elasticity, resulting in skin wrinkles and sagging.

  It is also known that matrix metalloproteases such as collagenase are activated when the skin is exposed to ultraviolet rays. These enzymes are said to promote wrinkles and tarmi by reducing collagen, which is a major component of the dermis.

  In recent years, many cosmetics for preventing wrinkles, tarmi and the like of this skin are known, and retinoic acid, α-hydroxy acid, retinol and the like have been reported as active ingredients. However, these active ingredients have problems with skin irritation and stability. In addition, it is known to add a collagenase activity inhibitor as one of the methods for preventing wrinkles and tarmi.

In general, pigmentation of the skin seen in spots, buckwheat, sunburn, etc. is caused by excessive melanin pigment formation by melanin-producing cells present in the skin due to hormonal abnormalities or stimulation of ultraviolet rays, which deposits in the skin. Is considered to be the cause. As one method for preventing such pigmentation, a method for suppressing excessive production of melanin is known. Conventionally, treatments for external application of hydroquinone, ascorbic acid or the like have been performed for the treatment of pigmentation.
However, the plant raw material Seiyanagi has not been studied for the radical scavenging action, collagenase activity inhibitory action, and melanin production inhibitory action, which are the indicators of anti-aging and whitening actions described above.

SOD used for the purpose of preventing skin aging or anti-oxidation is unstable, difficult to formulate, and tocopherol is not effective enough. Moreover, since BHT etc. which are synthetic compounds have a problem in safety | security and there exists a restriction | limiting in compounding quantity, it is not a chemical synthetic product but the natural raw material which is stable and has few side effects is desired. Similarly, it is preferable for preventing aging that it has a safe and stable collagenase activity inhibitory action. In addition, since ascorbic acid used as a whitening agent has drawbacks such as being easily decomposed over time, a skin external preparation derived from natural products having high stability and excellent effect is also desired.
From the above, a skin external preparation that is safe and excellent in stability, excellent in anti-aging and whitening action is desired.

  Under these circumstances, as a result of intensive studies, the present inventors have found that the extract of Seijyanagi has excellent DPPH radical scavenging action, collagenase activity inhibitory action and melanin production inhibitory action, and is also excellent in stability. I found. Furthermore, it discovered that the skin external preparation containing the extract was safe and stable, and was excellent in anti-aging and whitening effect, and came to complete this invention.

  Seianyanagi used in the present invention (Walmiaceae, also known as Zenigata, Kikurokaya) is scientifically named Cyclocarya pariurus and is native to China. It contains cyclocaryoside, which is 200 times sweeter than sugar, and is drunk as a sweet tea. It is said to be good for diabetes and high blood pressure. The plant has not been reported for use as a cosmetic.

  The extract of the green willow used in the present invention is extracted from a part of the plant body such as leaves, stems, bark, flowers, fruits and roots of the plant body or the whole plant. Preferably, those obtained by extraction from the leaves of the plant body are good. The extraction method is not particularly limited, and for example, it may be a heat extraction or a room temperature extraction.

  Examples of the solvent to be extracted include water, lower alcohols (methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, etc.), liquid polyhydric alcohols (1,3-butylene glycol, propylene glycol). , Glycerin, etc.), ketones (acetone, methyl ethyl ketone, etc.), acetonitrile, esters (ethyl acetate, butyl acetate, etc.), hydrocarbons (hexane, heptane, liquid paraffin, etc.), ethers (ethyl ether, tetrahydrofuran, propyl ether) Etc.). Preferred are polar solvents such as water, lower alcohols and liquid polyhydric alcohols, and particularly preferred are water, ethanol, 1,3-butylene glycol and propylene glycol. These solvents may be used alone or in combination of two or more.

  The extract may be used as it is, or may be used after concentration, dilution and filtration treatment, decolorization with activated carbon, deodorization treatment, or the like, if necessary. Further, the extracted solution may be subjected to a treatment such as concentration to dryness, spray drying, freeze drying, etc., and used as a dried product.

  In the external preparation for skin of the present invention, the above extract may be used as it is, and within the range not impairing the effect of the extract, oils and fats, waxes, hydrocarbons, fatty acids which are components used in the external preparation , Alcohols, esters, surfactants, metal soaps, pH adjusters, preservatives, fragrances, moisturizers, powders, UV absorbers, thickeners, pigments, antioxidants, whitening agents, chelating agents, etc. These components can be blended.

  The external preparation for skin of the present invention can be used for any of cosmetics, quasi drugs, and pharmaceuticals. Examples of the dosage form include skin lotions, creams, emulsions, gels, aerosols, essences, Examples include packs, cleaning agents, bath preparations, foundations, dusting powders, lipsticks, ointments, and poultices applied to the skin.

  The amount of the extract used in the present invention is 0.0001% by weight or more, preferably 0.001 to 10% by weight in terms of solid matter, based on the total amount of the external preparation for skin of the present invention. If it is less than 0.0001% by weight, a sufficient effect is hardly expected. When the blending amount exceeds 10% by weight, the effect is hardly recognized and it is uneconomical. In addition, the addition method may be added in advance or during the production, and may be appropriately selected in consideration of workability.

  The Seiyanagi extract of the present invention had excellent DPPH radical scavenging action, collagenase activity inhibition and melanin production inhibition action, and was also excellent in stability. Furthermore, the external preparation for skin containing these extracts showed safe and excellent anti-aging and whitening action.

  Next, in order to describe the present invention in detail, examples of producing the extract used in the present invention, formulation examples and experimental examples of the present invention will be given as examples, but the present invention is not limited thereto. In the examples, the part of the amount is part by weight, and% is% by weight.

Manufacture example 1 Hot water extract of green sen willow 900 mL of purified water is added to 30 g of dried sen willow leaves, extracted at 95-100 ° C. for 2 hours, filtered, and the filtrate is concentrated and lyophilized. 3.3 g of hot water extract of green senyanagi was obtained.

Manufacture example 2 Ethnic extract of green willow leaves 1 g of ethanol is added to 100 g of dried leaves of green willow leaves, extracted at room temperature for 7 days, filtered, and the filtrate is concentrated to dryness. 9.5 g of extract was obtained.

Manufacture example 3 50% 1,3-butylene glycol extract of green sen willow After adding 200 g of purified water and 200 g of 1,3-butylene glycol to 20 g of dry leaves of green sen willow and bark, and extracting at room temperature for 7 days And filtered to obtain 360 g of 50% 1,3-butylene glycol extract of Seishenyanagi.

Formulation Example 1 Lotion Formulation Amount Seianyanagi hot water extract (Production Example 1) 0.1 part 2.1,3-butylene glycol 8.0
3. Glycerin 2.0
4). Xanthan gum 0.02
5. Citric acid 0.01
6). Sodium citrate 0.1
7). Ethanol 5.0
8). Methyl paraoxybenzoate 0.1
9. Polyoxyethylene hydrogenated castor oil (40E.O.) 0.1
10. Perfume
11. [Manufacturing method] Components 1 to 6 and 11 and components 7 to 10 are uniformly dissolved in purified water, and both are mixed and filtered to obtain a product.

Comparative Example 1 Conventional Lotion A conventional lotion was obtained by replacing the hot water extract of Seijyanagi with purified water in Formulation Example 1.

Formulation Example 2 Cream Formulation Amount Seienyanagi ethanol extract (Production Example 2) 0.05 part Squalane 5.5
3. Olive oil 3.0
4). Stearic acid 2.0
5. Beeswax 2.0
6). Octyldodecyl myristate 3.5
7). Polyoxyethylene cetyl ether (20E.O.) 3.0
8). Behenyl alcohol 1.5
9. Glycerol monostearate2.5
10. Fragrance 0.1
11. Methyl paraoxybenzoate 0.2
12 Ethyl paraoxybenzoate 0.05
13.1,3-Butylene glycol 8.5
14 [Manufacturing method] Components 2 to 9 are heated and dissolved and mixed with purified water to a total amount of 100, and kept at 70 ° C to obtain an oil phase. Ingredients 1 and 11 to 14 are dissolved by heating and mixed, and kept at 75 ° C. to form an aqueous phase. The aqueous phase is added to the oil phase to emulsify, and the mixture is cooled while stirring. The component 10 is added at 45 ° C., and further cooled to 30 ° C. to obtain a product.

Comparative Example 2 Conventional Cream In Formulation Example 2, a product obtained by substituting the ethanol extract of Seishiyanagi with purified water was used as a conventional cream.

Formulation Example 3 Emulsion Formulation Formulation 1. 1. Hot spring extract of blue sen willow (Production Example 1) 0.001 part Squalane 5.0
3. Olive oil 5.0
4). Jojoba oil 5.0
5. Cetanol 1.5
6). Glycerol monostearate 2.0
7). Polyoxyethylene cetyl ether (20E.O.) 3.0
8). Polyoxyethylene sorbitan monooleate (20E.O.) 2.0
9. Fragrance 0.1
10. Propylene glycol 1.0
11. Glycerin 2.0
12 Methyl paraoxybenzoate 0.2
13. Make the total volume 100 with purified water
[Manufacturing method] Components 2 to 8 are dissolved by heating and mixed, and kept at 70 ° C to obtain an oil phase. Ingredients 1 and 10-13 are dissolved by heating and mixed, and kept at 75 ° C. to form an aqueous phase. The aqueous phase is added to the oil phase to emulsify, and the mixture is cooled while stirring. The component 9 is added at 45 ° C., and further cooled to 30 ° C. to obtain a product.

Formulation Example 4 Gel formulation Formulation amount 1. 1. 50 parts 1,3-butylene glycol extract of Seishiyanagi (Production Example 3) 1.0 part Ethanol 5.0
3. Methyl paraoxybenzoate 0.1
4). Polyoxyethylene hydrogenated castor oil (60 EO) 0.1
5. Perfume
6.1,3-Butylene glycol 5.0
7). Glycerin 5.0
8). Xanthan gum 0.1
9. Carboxyvinyl polymer 0.2
10. Potassium hydroxide 0.2
11. [Production method] Ingredients 2 to 5 and ingredients 1 and 6 to 11 are uniformly dissolved in purified water, and the two are mixed to obtain a product.

Formulation Example 5 Pack Formulation Formulation 1. 1. Hot water extract of blue sen willow (Production Example 1) 0.1 part Seianyanagi ethanol extract (Production Example 2) 0.1
3. Polyvinyl alcohol 12.0
4). Ethanol 5.0
5.1,3-Butylene glycol 8.0
6). Methyl paraoxybenzoate 0.2
7). Polyoxyethylene hydrogenated castor oil (20 EO) 0.5
8). Citric acid 0.1
9. Sodium citrate 0.3
10. Perfume proper amount11. [Production Method] Components 1 to 11 are uniformly dissolved in purified water to make a total amount of 100 to obtain a product.

Formulation Example 6 Foundation Formulation Amount Ao-shiyanagi ethanol extract (Production Example 2) 1.0 part Stearic acid 2.4
3. Polyoxyethylene sorbitan monostearate (20EO) 1.0
4). Polyoxyethylene cetyl ether (20E.O.) 2.0
5. Cetanol 1.0
6). Liquid lanolin 2.0
7). Liquid paraffin 3.0
8). Isopropyl myristate 6.5
9. Sodium carboxymethylcellulose 0.1
10. Bentonite 0.5
11. Propylene glycol 4.0
12 Triethanolamine 1.1
13. Methyl paraoxybenzoate 0.2
14 Titanium dioxide 8.0
15. Talc 4.0
16. Bengala 1.0
17. Yellow iron oxide 2.0
18. Perfume proper amount19. [Manufacturing method] Components 2 to 8 are heated and dissolved in purified water to a total amount of 100, and kept at 80 ° C to obtain an oil phase. Swell component 9 well in component 19, then add components 1 and 10-13 and mix uniformly. To this, components 14 to 17 pulverized and mixed with a pulverizer are added, and the mixture is stirred with a homomixer and kept at 75 ° C. to obtain an aqueous phase. The oil phase is added to this aqueous phase with stirring, cooled, component 18 is added at 45 ° C., and cooled to 30 ° C. with stirring to give a product.

Example 7 Bath preparation formulation 1. Hot water extract of blue sen willow (Production Example 1) 5.0 parts Sodium bicarbonate 50.0
3. Yellow No. 202 (1) Appropriate amount 4. Perfume appropriate amount 5. [Manufacturing method] Ingredients 1 to 5 are mixed uniformly with sodium sulfate to make a product.

Formulation Example 8 Ointment Formulation Formulation 1. Hot water extract of blue sen willow (Production Example 1) 0.01 part2. 50% 1,3-butylene glycol extract of blue senyanagi (Production Example 3) 0.5
3. Polyoxyethylene cetyl ether (30E.O.) 2.0
4). Glycerol monostearate 10.0
5. Liquid paraffin 5.0
6). Cetanol 6.0
7). Methyl paraoxybenzoate 0.1
8). Propylene glycol 10.0
9. [Production Method] Components 3 to 6 are heated and dissolved and mixed with purified water to a total amount of 100, and kept at 70 ° C. to obtain an oil phase. Ingredients 1, 2, and 7-9 are dissolved by heating and mixed, and kept at 75 ° C. to form an aqueous phase. The aqueous phase is added to the oil phase to emulsify, and the mixture is cooled to 30 ° C. with stirring to obtain a product.
Next, experimental examples will be given to explain the effects of the present invention in detail.

Experimental Example 1 DPPH Radical Scavenging Action Using Production Examples 1 and 2 as samples, the scavenging action of DPPH radical, a kind of free radical, was measured. Ascorbic acid was used as a positive control. In addition, in order to confirm the stability of the sample, the sample was stored at 40 ° C. for 2 weeks and measured in the same manner.

To 0.3 mL of the sample aqueous solution of each concentration, add 0.1 mL of acetate buffer (pH 5.5), 0.4 mL of ethanol, and 0.2 mL of 0.5 mM DPPH (diphenylcyclic hydrazyl) ethanol solution at 37 ° C. for 30 minutes. After the reaction, the absorbance at a wavelength of 517 nm was measured. The erasure rate of each sample was calculated by the following formula.
Erase rate (%) = (1-sample absorbance / blank absorbance) × 100
The test results are shown in Table 1. Ascorbic acid significantly reduced the DPPH radical scavenging action after storage at 40 ° C. for 2 weeks, but the extract of Seijyanagi did not change the scavenging action. From the above, the extract of Seijyanagi showed a stable and excellent DPPH radical scavenging action.

Experimental Example 2 Collagenase activity inhibitory action Using Production Examples 1 and 2 as samples, the collagenase activity inhibitory action was measured. Using a microplate, 50 μL of 0.1 mg / mL collagenase Type IV (Sigma) aqueous solution was added as an enzyme solution to 50 μL of the sample solution. Add and mix 0.39 mg / mL Pz-peptide (Pz-Pro-Leu-Gly-Pro-D-Arg-OH, Sigma) / 20 mM calcium chloride-containing Tris-HCl buffer (pH 7.1) as a substrate solution. Then, after reacting at 37 ° C. for 30 minutes, 1 mL of 25 mM citric acid was added to stop the reaction. Extraction was performed by adding 5 mL of ethyl acetate, and the absorbance of the ethyl acetate layer was measured at 320 nm. Moreover, the inhibitory action of each sample was calculated by the inhibition rate calculated | required from the following formula. For the control, purified water was used instead of the sample, and 20 mM calcium chloride-containing Tris-HCl buffer (pH 7.1) was used instead of collagenase as a blank.
Inhibition rate (%) = [1- (C−D) / (A−B)] × 100
A: Absorbance at 320 nm of control (OD 320)
B: O. D. 320
C: Sample O.D. D. 320
D: Sample blank O.D. D. 320

The results of these experiments are shown in Table 2. As a result, Seiyanagi extract showed an excellent collagenase activity inhibitory action.

Experimental Example 3 Melanin Production Inhibition Test Using B16 Mouse Melanoma Using Production Examples 1 and 2 as samples, the melanin production inhibitory action was measured.

B16 cells, a mouse melanoma-derived cell line, were seeded at 3 × 10 ⁴ cells in a 6 cm dish, and cultured for 5 days in MEM with NEAA containing 10% FBS under 5% CO ₂ and 37 ° C. conditions. At that time, each sample was added after adjusting the final concentration. Next, after the cells were washed twice with PBS (−), 1 mL of PBS (−) was added and collected with a rubber policeman. PBS (-) 0.5mL was added to the pellet obtained by centrifugation, and the pellet was dissolved by ultrasonic crushing operation. Protein quantification was performed using the Lowry method {Lowry, O. H. et al. , J .; Biol. Chem. , 193, 265-275 (1951)}. When measuring the amount of melanin per mg protein, 0.5 mL of 4N sodium hydroxide was added to the remaining cell disruption solution taken for protein quantification and reacted at 60 ° C. for 2 hours. D. 475 was measured, and melanin was determined from the calibration curve. The data was calculated as the amount of melanin per mg protein, the amount of melanin not added to the sample was taken as a control, and the value of the amount of melanin inhibition when the sample was added relative to the control was taken as the melanin inhibition rate.

The results of these experiments are shown in Table 3. Seiyanagi extract showed an excellent inhibitory effect on melanin production at low concentrations.

Experimental example 4 Use test 1
One month use for 20 women (21 to 46 years old) using the lotion of Formulation Example 1, the cream of Formulation Example 2, the conventional lotion of Comparative Example 1 and the conventional cream of Comparative Example 2. A test was conducted. After use, the effect of improving skin wrinkles and tarmi was determined by a questionnaire.

  The test results are shown in Table 4. The topical skin preparation containing the extract of blue senyanagi showed excellent wrinkle and tarmi improving effects. During the test period, there was no skin problem and there was no problem with safety. There was also no problem with the deterioration of the prescription ingredients.

Experiment 5 Use test 2
Using the lotion of Formulation Example 1, the cream of Formulation Example 2, the conventional lotion of Comparative Example 1 and the conventional cream of Comparative Example 2, targeting 20 women (21 to 46 years old) who suffer from spots and freckles A one month use test was conducted. After use, the effect of improving spots and freckles was judged by a questionnaire.

  The test results are shown in Table 5. The topical skin preparation containing the extract of blue sen willows showed an excellent effect of improving spots and freckles. During the test period, there was no skin problem and there was no problem with safety. There was also no problem with the deterioration of the prescription ingredients.

When the usage test was similarly conducted on Examples 3 to 8, excellent wrinkle, tarmi, stain, buckwheat and other improving effects were shown.

Claims (2)

A skin external preparation characterized by containing an extract of blue senyanagi. The skin external preparation according to claim 1, wherein the content of the extract using the leaves of green sen willow is 0.001 to 10%.