JP4489923B2 - Topical skin preparation - Google Patents

Description

【００３１】
実験例２ 活性酸素消去作用（抗酸化作用）
製造例１〜３を試料として用い、活性酸素の一種であるスーパーオキシドの消去作用を測定した。陽性対照として、スーパーオキシドジスムターゼ（ＳＯＤ）を用いた。また、試料の安定性を確認するために、試料の水溶液を９５℃で１時間加熱した液を使用して同様に測定を行った。
【００３２】
活性酸素消去作用の測定方法
各濃度の試料水溶液０．１ｍＬに０．４５ｍＬの発色試薬（０．２４ｍＭニトロブルーテトラゾリウム、０．４ｍＭキサンチンを含む０．１Ｍリン酸緩衝液；ｐＨ８．０）と０．４５ｍＬの酵素液（０．１Ｕ／ｍＬキサンチンオキシダーゼ）を加え、３７℃で２０分間反応させジホルマザンを生じさせた。この溶液に反応停止液（６９ｍＭドデシル硫酸ナトリウム水溶液）１．０ｍＬを加えた後、波長５６０ｎｍにおける吸光度（Ａｔ）を測定した。同様に酵素液の代わりにブランク液（０．１Ｍリン酸緩衝液；ｐＨ８．０）を加えて反応させ、吸光度（Ａｓ）を測定した。一方、コントロールとして試料溶液の代わりに精製水を用いて同様に操作し、吸光度（Ｂｔ）及び（Ｂｓ）を測定した。各試料の活性酸素消去率は次式より算出した。
活性酸素消去率（％）＝｛１−（Ａｓ−Ａｔ）÷（Ｂｓ−Ｂｔ）｝×１００
【００３３】
これらの試験結果を表２に示した。また、ＳＯＤは９５℃で１時間の加熱により、活性酸素消去作用が大きく減少したが、アマメシバの抽出物は消去作用に変化はなかった。以上のことから、アマメシバの抽出物は、９５℃の加熱にも安定で優れた活性酸素消去作用を示した。
【００３４】
【表２】
表２ 活性酸素消去作用

＊括弧内の数字は９５℃で１時間加熱後の消去率を示す。
【００３５】
実験例３ 使用試験
実施例１のクリーム及び比較例１の従来のクリームを用いて、各々女性３０人（３０〜４５才）を対象に１ヶ月間の使用試験を行った。使用後、肌のうるおい、ハリ、しわ及びくすみの改善を総合的に判断するアンケート調査を行った。
【００３６】
その結果、当該皮膚外用剤は、肌のうるおい、ハリ、しわ及びくすみの改善に関して優れた作用を示した（表３）。なお、試験期間中、皮膚トラブルは一人もなく、安全性においても問題なかった。また、処方成分の劣化についても問題なかった。
【００３７】
【表３】
表３ 使用試験

【００３８】
実施例２の化粧水、実施例３の乳液、実施例４の軟膏、実施例５の浴用剤についても使用試験を行ったところ、安全であり、肌のうるおい、ハリ、しわ及びくすみの改善作用に優れていた。
【００３９】
【発明の効果】
以上のことから、本発明のアマメシバの抽出物は、抗酸化作用、安定性に優れていた。さらに、これらの抽出物を含有する皮膚外用剤は、安全であり、肌のうるおい、ハリ、しわ及びくすみの改善作用に優れていた。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to an external preparation for skin which is excellent in action for improving moisture, firmness, wrinkles and dullness of skin by blending an extract of a specific plant.
[0002]
[Prior art]
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 crosslink biological tissues such as collagen, and oxidize fats and oils to form lipid peroxides that damage cells. Such disorders are thought to cause skin aging and aging such as wrinkles. One of the methods to prevent aging is to incorporate an antioxidant that removes free radicals and active oxygen. It has been. Conventional antioxidants used to prevent aging include ascorbic acid (vitamin C), tocopherol (vitamin E), 3,5-tert-butyl-4-hydroxytoluene (BHT), superoxide dismutase (SOD), etc. Has been used.
[0003]
[Problems to be solved by the invention]
Vitamin C and superoxide dismutase used for the purpose of preventing skin aging or antioxidant are unstable, difficult to formulate, and vitamin E cannot be said to be sufficiently effective. 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.
[0004]
In view of the above, there is a demand for an external preparation for skin that is safe and not only excellent in wrinkle and firmness-improving action, but also effective in improving skin moisture and dullness.
[Means for Solving the Problems]
[0005]
Under such circumstances, as a result of intensive studies, the present inventors have found that the extract of Amameshiba is excellent in the unsaturated fatty acid oxidation-preventing action and the active oxygen scavenging action and also in stability. Furthermore, the skin external preparation containing the extract of flaxseed was found to be safe and excellent in improving the moisture, firmness, wrinkles and dullness of the skin, and the present invention was completed.
[0006]
That is, this invention is an external preparation for skin characterized by containing the extract of flaxseed.
[0007]
The flax beetle (scientific name: Sauropus androgynous) used in the present invention is a plant of the Euphorbiaceae family.
[0008]
The extract used in the present invention is extracted from a part of the plant body such as leaves, stems, bark, flowers, fruits, roots or the whole plant, but is not particularly limited, depending on the purpose. May be selected as appropriate. The extraction method is not particularly limited, and for example, it may be a heat extraction or a room temperature extraction.
[0009]
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.
[0010]
The said extract may be used with the extracted solution as it is, and may be used after processing, such as concentration, dilution, and filtration, as needed. 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.
[0011]
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 and hydrocarbons which are components used in normal external preparations , Fatty acids, alcohols, esters, surfactants, metal soaps, pH adjusters, preservatives, fragrances, moisturizers, powders, UV absorbers, thickeners, dyes, antioxidants, whitening agents, chelates Components such as an agent can also be blended.
[0012]
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 lotion, cream, emulsion, gel, aerosol, ointment, and poultice. , Essence, pack, cleaning agent, bath preparation, foundation, dusting powder, lipstick, and the like.
[0013]
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 it exceeds 10% by weight, the effect is hardly increased, which 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.
[0014]
【Example】
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. The part of the amount shown in the examples indicates part by weight, and% indicates% by weight.
[0015]
Production Example 1 Hot water extract of Amameshiba 400 ml of purified water was added to 20 g of dried product of Amamishiba leaves, extracted at 95-100 ° C. for 2 hours, filtered, the filtrate was concentrated, freeze-dried and heat of Amameshiba 5.0 g of water extract was obtained.
[0016]
Production Example 2 50% Ethanol Extract of Amameshiba 1 L of purified water and 1 L of ethanol were added to 100 g of dried Amamishiba, extracted at room temperature for 7 days, filtered, and the filtrate was concentrated to dryness. 18 g of 50% ethanol extract was obtained.
[0017]
Production Example 3 1,3-Butylene Glycol Extract of Amameshiba 1.0 kg of 1,3-butyleneglycol was added to 100 g of dried dwarf root, extracted at room temperature for 7 days, filtered, and 1,3-butyleneglycol of Amamishiba 0.91 kg of butylene glycol extract was obtained.
[0018]
Reference extract 1 Andrographis hot water extract 20 g of dried Andrographis leaves were extracted in the same manner as in Production Example 1 to obtain 3.0 g of Andrographis hot water extract.
[0019]
Reference Extract 2 Andrographis 50% Ethanol Extract 100 g of dried andrographies whole plant was extracted in the same manner as in Production Example 2 to obtain 12 g of Andrographes 50% ethanol extract.
[0020]
Reference Extract 3 50% Ethanol Extract of Yaeyama Aoki 100 g of a dried plant of Yaeyama Aoki was extracted in the same manner as in Production Example 2 to obtain 23 g of a 50% ethanol extract of Yaeyama Aoki.
[0021]
Example 1 Cream 1
Formulation Formulation 1. Hot water extract of flaxseed (Production Example 1) 1.0 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. 1,3-butylene glycol 8.5
12 Ethyl paraoxybenzoate 0.05
13. Methyl paraoxybenzoate 0.2
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 obtain an aqueous phase. The aqueous phase is added to the oil phase to emulsify, and the mixture is cooled while stirring.
[0022]
Comparative Example 1 Conventional cream Example 1 was prepared by replacing the hot water extract of Amameshiba with purified water.
[0023]
Example 2 skin lotion formulation 1. 50 parts ethanol extract of flaxseed (Production Example 2) 0.1 part Andrography 50% ethanol extract ( reference extract 2 ) 0.1
3. 50% ethanol extract of Yaeyama Aoki ( reference extract 3 ) 0.1
4). 1,3-butylene glycol 8.0
5). Glycerin 2.0
6). Xanthan gum 0.02
7). Citric acid 0.01
8). Sodium citrate 0.1
9. Ethanol 5.0
10. Methyl paraoxybenzoate 0.1
11. Polyoxyethylene hydrogenated castor oil (40E.O.) 0.1
12 Perfume appropriate amount13. [Manufacturing method] Components 1 to 8 and 13 and components 9 to 12 are uniformly dissolved in purified water, and the two are mixed and filtered to obtain a product.
[0024]
Example 3 Emulsion Formulation Blending amount 1,3-butylene glycol extract of flaxseed (Production Example 3) 0.5 part Olive oil 5.0
3. Jojoba oil 5.0
4). Cetanol 1.5
5). Glycerol monostearate 2.0
6). Polyoxyethylene cetyl ether (20E.O.) 3.0
7). Polyoxyethylene sorbitan monooleate (20E.O.) 2.0
8). Fragrance 0.1
9. Propylene glycol 1.0
10. Glycerin 2.0
11. Methyl paraoxybenzoate 0.2
12 [Manufacturing method] Components 2 to 7 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 9 to 12 are dissolved by heating and mixed, and kept at 75 ° C. to obtain an aqueous phase. The aqueous phase is added to the oil phase to emulsify, and the mixture is cooled while stirring. The component 8 is added at 45 ° C., and further cooled to 30 ° C. to obtain a product.
[0025]
Example 4 Ointment Formulation Amount 1.0 parts of hot water extract of Amameshiba (Production Example 1) Andrography hot water extract ( reference extract 1 ) 1.0
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. [Manufacturing method] Components 3 to 6 are heated and dissolved and mixed with purified water to 100, and the mixture is 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.
[0026]
Example 5 Bath preparation formulation 50 parts ethanol extract of flaxseed (Production Example 2) 5.0 parts Sodium bicarbonate 50.0
3. Yellow No. 202 (1) Appropriate amount 4. Perfume appropriate amount 5. [Production method] Ingredients 1-5 are uniformly mixed with anhydrous sodium sulfate to make a total amount of 100 to obtain a product.
[0027]
Next, experimental examples will be given to explain the effects of the present invention in detail.
[0028]
Experimental Example 1 Measurement method for antioxidant action of unsaturated fatty acids (antioxidant action)
Make 0.5 mL of sample (per solid content), 2 mL of 0.02 mg / mL linoleic acid / ethanol solution, 1 mL of ethanol and 1 mL of 0.2M phosphate buffer (pH 7.0) to a total volume of 5 mL with purified water. It was made to react at 50 degreeC for 8 days, it was set as the test liquid, and the light absorbency was measured by the rhodan iron method. Specifically, 4.7 mL of 75% (v / v) ethanol, 0.1 mL of 30% ammonium thiocyanate aqueous solution and 0.1 mL of 0.02M ferrous chloride hydrochloric acid solution were added to 0.1 mL of each test solution, and the mixture was left for 3 minutes. The absorbance (A) at a wavelength of 500 nm was measured. On the other hand, the same operation was performed using a test solution to which no sample was added as a blank, and the absorbance (B) was measured. Vitamin E was used as a comparative product. The unsaturated fatty acid antioxidant action of each sample was calculated from the following formula.
Unsaturated fatty acid antioxidant rate (%) = (1−A ÷ B) × 100
[0029]
The test results are shown in Table 1. As a result, the extract of Amameshiba showed an excellent antioxidant effect on unsaturated fatty acids.
[0030]
[Table 1]
Table 1 Antioxidation of unsaturated fatty acids

[0031]
Experimental Example 2 Active oxygen scavenging action (antioxidant action)
Using Production Examples 1 to 3 as samples, the scavenging action of superoxide, which is a kind of active oxygen, was measured. Superoxide dismutase (SOD) was used as a positive control. Further, in order to confirm the stability of the sample, the same measurement was performed using a solution obtained by heating an aqueous solution of the sample at 95 ° C. for 1 hour.
[0032]
Method for measuring reactive oxygen scavenging action 0.45 mL of a coloring reagent (0.1M phosphate buffer containing 0.24 mM nitroblue tetrazolium and 0.4 mM xanthine; pH 8.0) and 0.1 mL of a sample aqueous solution of each concentration and 0 .45 mL of enzyme solution (0.1 U / mL xanthine oxidase) was added and reacted at 37 ° C. for 20 minutes to produce diformazan. After adding 1.0 mL of a reaction stop solution (69 mM sodium dodecyl sulfate aqueous solution) to this solution, the absorbance (At) at a wavelength of 560 nm was measured. Similarly, a blank solution (0.1 M phosphate buffer; pH 8.0) was added in place of the enzyme solution for reaction, and absorbance (As) was measured. On the other hand, the absorbance (Bt) and (Bs) were measured in the same manner using purified water instead of the sample solution as a control. The active oxygen elimination rate of each sample was calculated from the following equation.
Active oxygen elimination rate (%) = {1− (As−At) ÷ (Bs−Bt)} × 100
[0033]
The test results are shown in Table 2. Further, SOD significantly reduced the active oxygen scavenging action by heating at 95 ° C. for 1 hour, but the extract of Amameshiba did not change the scavenging action. From the above, the extract of flaxseed showed stable and excellent active oxygen scavenging action even when heated at 95 ° C.
[0034]
[Table 2]
Table 2 Active oxygen scavenging action

* Numbers in parentheses indicate erasure rate after heating at 95 ° C. for 1 hour.
[0035]
Experiment 3 Use test
Using the cream of Example 1 and the conventional cream of Comparative Example 1, a use test for one month was conducted for 30 women (30 to 45 years old). After use, a questionnaire survey was conducted to comprehensively judge the improvement of moisture, firmness, wrinkles and dullness of the skin.
[0036]
As a result, the external preparation for skin showed an excellent effect on improvement of moisture, firmness, wrinkles and dullness of the skin (Table 3). 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.
[0037]
[Table 3]
Table 3 Usage test

[0038]
The skin lotion of Example 2, the emulsion of Example 3, the ointment of Example 4 and the bath preparation of Example 5 were also tested for use, and were safe and improved on moisture, firmness, wrinkles and dullness of the skin. It was excellent.
[0039]
【The invention's effect】
From the above, the extract of flaxseed of the present invention was excellent in antioxidant action and stability. Furthermore, the external preparation for skin containing these extracts was safe and excellent in improving the moisture, firmness, wrinkles and dullness of the skin.

Claims (3)

A skin external preparation characterized by containing an extract of flaxseed . The skin external preparation according to claim 1, wherein the extract of flaxseed is an extract with a solvent selected from one, two or more of water, lower alcohol, and liquid polyhydric alcohol. An anti-aging agent comprising an extract of flaxseed .