JPH06128141A - External agent for skin - Google Patents

Abstract

PURPOSE:To provide an external agent for skin, having excellent active oxygen elimination effect and exhibiting superoxidation preventing effect on lipid, skin aging preventing effect, chapped skin ameliorating effect, etc. CONSTITUTION:The objective agent contains (A) an asparagus extract produced by extracting the stalk, rhizome, leaf, flower, etc., of asparagus with a proper solvent at room temperature or under heating and (B) a superoxide dismutase produced e.g. by extracting the tissue of an animal such as human, cattle or dog or extracting a substance produced by microorganism. The amount of the component A is 0.0001-10wt.%, preferably 0.01-5wt.% (in terms of dried solid component) and that of the component B is 0.00001-5wt.%, preferably 0.001-3wt.%. The external agent for skin may be compounded with conventional external skin agent components such as aqueous component, powder, surfactant, oiliness agent, humectant, alcohol, pH-modifier, antiseptic agent, pigment, antioxidant, ultraviolet absorber, thickener and perfume.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an external preparation for skin, more specifically, a cosmetic having an excellent active oxygen removing action, a lipid peroxidation preventing effect, a skin aging preventing effect, a skin roughening improving effect, and the like. The present invention relates to an external preparation for skin such as pharmaceuticals.

[0002]

2. Description of the Related Art It is becoming clear that the generation of active oxygen in the skin is greatly involved in the aging of the skin. Therefore, in recent years, active oxygen production inhibitors, active oxygen scavengers, antioxidants, and the like have been increasingly applied to external skin preparations for the purpose of preventing skin aging.

On the other hand, allantoin, aloe extract, ginseng extract, placenta extract, bovine blood deproteinate, fermented metabolite and the like are known as medicinal components for improving rough skin and preventing skin aging.

[0004]

However, the external preparation for skin containing these medicinal components cannot exert a sufficient effect for improving rough skin and preventing skin aging, and has a superior cell activating effect for external use on the skin. The development of agents was desired.

[0005]

Under such circumstances, the present inventors have conducted diligent research, and as a result, by using an asparagus extract in combination with superoxide dismutase, skin roughening improving action and skin aging preventing action. The present invention has been completed by discovering that the effects on the above are exerted synergistically.

[0006] That is, the present invention provides an external preparation for skin characterized by containing (A) an asparagus extract and (B) a superoxide dismutase.

The asparagus extract used in the external preparation for skin of the present invention means asparagus of Asparagus of
ficinalis L .; (3) is obtained by extraction from the stem, rhizome, leaf, flower, etc., and its preparation method is not particularly limited. For example, it is extracted at room temperature to under heating using various suitable solvents. Examples of the extraction solvent include water; lower monohydric alcohols such as methyl alcohol and ethyl alcohol; liquid polyhydric alcohols such as glycerin, propylene glycol and 1,3-butylene glycol; lower alkyl esters such as ethyl acetate; benzene, hexane and the like. The above hydrocarbons; one or more ethers such as diethyl ether can be used. In particular, water, ethyl alcohol, glycerin, and a mixed solvent of one or more kinds of 1,3-butylene glycol are preferable. As the extraction conditions, a solvent is used in a volume ratio of 1 to 1000 times, particularly 5 to 100 times, that of asparagus, at 4 ° C. or higher, particularly 15 to
It is preferable to carry out the treatment at a temperature of 30 ° C. for 1 hour or longer, particularly 1 to 3 days.

The extract obtained under the above-mentioned conditions may be used as it is as an extracted solution, but if necessary, it may be subjected to treatments such as concentration and filtration, and used properly.

The amount of the asparagus extract in the external preparation for skin of the present invention is preferably 0.0 as a dry solid content.
001 to 10% by weight (hereinafter simply referred to as "%"),
It is preferably 0.01 to 5%.

The content of asparagus extract is 0.000
If it is less than 1%, the effect is not sufficiently exhibited, and if it exceeds 10.0%, the effect is not further increased.

On the other hand, the other essential component of the present invention (B)
Superoxide dismutase (hereinafter referred to as "S
"OD") is a superoxide scavenging enzyme widely distributed in living bodies such as animals, plants and microorganisms, and its origin and acquisition method are not particularly limited.

As a method for producing this SOD, humans,
Even if extracted from animal tissues such as cows and dogs, cabbage,
It may be one extracted from plants such as cucumber and lettuce, one extracted from a microorganism, or one produced by genetic engineering. Furthermore, if it has SOD as a main component, it does not necessarily have to be purified.

The content of these SODs in the external preparation for skin of the present invention is generally 0.00001 to 5%, preferably 0.
001 to 3%. SOD content is 0.00001
If it is less than 5%, a sufficient effect may not be obtained, and even if it exceeds 5%, the effect may not be further increased, and adversely affect the formulation.

Further, the external preparation for skin of the present invention contains, in the range not impairing the effects of the present invention, the above-mentioned essential components, an aqueous component, a powder, a surfactant, which is used in a general external preparation for skin.
Oil agents, moisturizers, alcohols, pH adjusters, preservatives, pigments, antioxidants, ultraviolet absorbers, thickeners, fragrances, cosmetic ingredients and the like can be appropriately added as necessary.

The external preparation for skin of the present invention comprises the essential component (A)
And component (B) may be blended to produce the composition according to a conventional method. And emulsion, cream, lotion, beauty essence, cleansing, pack, cleaning agent, foundation, etc.,
In addition, it can be applied as a skin external medicine for dispersion, granule, ointment or the like, for external use for quasi-drugs or for cosmetics.

[0016]

EXAMPLES Next, the present invention will be described in more detail with reference to test examples and examples, but the present invention is not limited thereto.

Production Example 1 (Asparagus Extract) As a raw material, the raw white asparagus root portion was 2365.
0 g (as fresh weight) was weighed, then adjusted to an alcohol concentration of 60% and ethanol was added.
These were ground using a food mixer (National MX-M3) to obtain a mixture. Then, a mixture consisting of these raw materials and a solvent was placed in a poly bucket, and allowed to stand at room temperature for one day to perform extraction, and then the extract was collected by suction filtration into a suction filtration bottle. To the extraction residue, 25 l of 60% ethanol was added again, and after repeating the above operation, about 66 l of the extract was concentrated by a rotary evaporator and the solvent was distilled off to obtain 1000 g of a brown concentrated extract (dry solid content: 4%). (First step).

Then, until the concentrated extract is completely dissolved, n
-Add a mixed solvent of butanol and water (1: 1), shake well, and then centrifuge for about 30 minutes with a centrifuge for about 30 minutes to extract and separate saponin components and the like into an n-butanol layer. (Second step). Then, the n-butanol layer was concentrated by a rotary evaporator and the solvent was distilled off to obtain about 110 g of an extract (third step).

Next, water and benzene were added to the extract in an equivalent amount and suspended to obtain a milky white solution. This solution was centrifuged at 10,000 rpm for 30 minutes using a centrifuge, and the separated benzene layer was discarded by tilting the centrifuge tube to discard the benzene in the upper layer, or by sucking off only the upper layer with a pipette tube. Removes lipid components from the extract,
The same amount of new benzene was added to the remaining aqueous layer, and the same operation was performed. The degreasing step may be performed by adding only benzene, but it has been confirmed that efficient degreasing can be performed by using another solvent such as chloroform or ether (fourth step).

Next, water is concentrated from the obtained water layer portion by a rotary evaporator and dried to dryness, and then n-
About 1 liter of a mixed solvent of butanol and water (1: 1) was added to dissolve the extract, and the saponin component was extracted into the butanol layer by allowing the mixture to stand in a separating funnel for one day. Then, the butanol layer was concentrated by a rotary evaporator and dried to obtain about 18 g of extract (brown extract) (fifth step).

Then, 300 ml of methanol was added to the brown extract to dissolve it, and 75 ml of each was slowly dropped into a separately prepared ethyl ether (2 l) using an injection needle to form a white precipitate, which was allowed to stand for a while. After leaving it for a long time, most of the ether was removed by the gradient method, the precipitate was collected by suction filtration, and the precipitate was washed with fresh ether several times to wash away the dissolved ether of contaminants. The almost white precipitate obtained by such an operation was dried in a vacuum desiccator and then pulverized in a mortar to obtain about 11 g of asparagus savonin powder (sixth step).

Test Example 1 Superoxide removal activity measurement test: No. 1 of Production Example 1
Using the asparagus extract obtained in the step as a sample, the superoxide removing activity was measured by the following measuring method. The activity was also measured for commercially available SOD and a combination thereof with an asparagus extract. The results are shown in Table 1.

(Measurement method) A substrate solution in 2.4 ml of 0.05 M sodium carbonate buffer (pH 10.2) [3.0 mM xanthine (dissolved in 0.05 M sodium carbonate buffer)]
0.1 ml, 3.0 mM EDTA 0.1 ml, 0.15% (W
/ V) bovine serum albumin, 0.75 mM nitroblu-tetrazolium 0.1 ml and 0.1 ml of each sample are mixed, and 2
After standing at 5 ° C for 10 minutes, 0.1 ml of an enzyme solution [xanthine oxidase solution (diluted with purified water about 0.04 units / ml)] is added to start the reaction. 20 at 25 ° C
After incubating for 6 minutes, 6mM CaCl ₂ 0.1m
Stop the reaction by adding l. Then, the absorbance (A) at 560 nm is measured.

As a control, the absorbance (B) of the sample to which purified water was added instead of the sample, and as a blank for each sample, 6 mM was used.
Absorbance of a sample to which 0.1 ml of xanthine oxidase was added after stopping the reaction by adding 0.1 ml of CaCl ₂ (C)
Was measured and the superoxide removal rate was calculated from the following formula.

[0025]

[Equation 1]

A: Absorbance of sample by enzyme reaction B: Absorbance of control enzyme reaction C: Absorbance of sample without enzyme reaction

[0027]

[Table 1]

* 1: Asparagus extract obtained in the first step of Production Example 1. * 2: Sigma; obtained from bovine red blood cells, 3.57
0 units / mg

As is clear from the results of Table 1, the asparagus extract alone had an SOD-like action, but SO
It was shown that the combined use with D exerts a synergistic effect and is extremely effective in removing active oxygen.

This means that asparagus extract and SOD
The external preparation for skin of the present invention in combination with is the production of lipid peroxide due to the production of active oxygen in the skin by ultraviolet rays, inflammation,
It shows that it has an extremely high preventive effect against blackening and aging.

Example 1 Emulsion: An emulsion was prepared according to the composition shown in Table 2 and the following production method, and its skin beautifying effect and skin aging preventing effect were examined. The results are shown in Table 5.

[0032]

[Table 2]

(Production Method) A. Ingredients (6), (7), (9) and (13) are heat mixed and maintained at 70 ° C. B. Heat-mix components (1) to (5) and (10),
Keep at 0 ° C. C. B is added to A and mixed, component (12) is added and the mixture is uniformly emulsified, cooled to 30 ° C., and components (8) and (1
1) is added and mixed uniformly to obtain an emulsion.

(Test method) Fifteen women aged 28 to 58 were used as a panel, and an appropriate amount of the test emulsion was applied to the face after washing the face twice daily in the morning and at night for 12 weeks. The beautiful skin and anti-aging effect of the application were evaluated according to the following criteria.

[0035]

[Table 3] Skin beautifying effect: [Evaluation] [Contents] Effectiveness Dullness of the skin became inconspicuous. Somewhat effective The dullness of the skin became less noticeable. Ineffective No change from before use.

[0036]

[Table 4] Anti-aging effect on skin: [Evaluation] [Contents] Effectiveness The scalp and gloss of the skin were improved. Slightly effective Skin tone and gloss were slightly improved. Ineffective No change from before use. (result)

[0037]

[Table 5]

Example 2 Cream: A cream was prepared by the composition shown in Table 6 and by the following production method, and its skin beautifying effect and skin aging preventing effect were examined. The results are shown in Table 7.

[0039]

[Table 6]

* 3: 10 kg of bovine placenta is finely chopped and doubled to 5
V / V% ethyl alcohol aqueous solution was added, extracted at 37 ° C for 6 hours, and then purified by gel filtration, dialysis and the like. (Yield about 2 kg) Protein amount about 1.0-1.5% * 4: 1 kg of cabbage is cut into small pieces, and the same amount of purified water is added to homogenize. Ammonium sulfate fractionation after filtration and dialysis treatment. (Yield about 10g) Protein amount about 2.0-4.0%

(Production Method) A. Components (1)-(7), (11) and (12) are mixed and heated to maintain 70 ° C. B. Mix components (8) and (13) and heat to 70 ° C.
Keep on. C. After adding B to A, mixing and cooling, (9) and (10) were added and mixed uniformly to obtain a cream. (Test method) Same as Example 1 (Evaluation criteria) Same as Example 1 (Result)

[0042]

[Table 7]

As is clear from the results of Table 7, the product 2 of the present invention
Creams # 3 and # 3 lose the skin's “shine” and “swelling”,
It was effective in preventing and improving skin aging phenomena such as "dullness".

[0044]

Table 3 Example 3 Lotion: (Prescription) (%) (1) Glycerin 5.0 (2) 1,3-Butylene glycol 6.5 (3) Polyoxyethylene sorbitan 1.2 Monolaurate (20E) O.) (4) Ethyl alcohol 8.0 (5) Asparagus extract ^{* 1} 1.0 (6) SOD ^{* 5} 0.5 (7) Preservative proper amount (8) Perfume proper amount (9) Purified water residue Amount * 5: manufactured by Sigma; obtained from human red blood cells, 5.230
units / mg

(Production Method) A. Components (3), (4), (7) and (8) are mixed and dissolved. B. Components (1), (2), (5), (6) and (9) are mixed and dissolved. C. A and B were mixed and made uniform to obtain a lotion.

[0046]

Table 4 Example 4 Pack: (Formulation) (%) (1) Polyvinyl alcohol 20.0 (2) Ethyl alcohol 20.0 (3) Glycerin 5.0 (4) Kaolin 6.0 (5) Asparagus Extract ^{* 1} 0.05 (6) Placenta extract containing SOD ^{* 6} 0.01 (7) Preservative 0.2 (8) Perfume 0.1 (9) Purified water Remainder * 6: Lyophilized

(Production Method) A. Mixing components (1), (3)-(5) and (9),
Heat to 70 ° C. and stir. B. Mix components (2), (7) and (8). C. B was added to A, mixed, and then cooled to uniformly disperse (6) to obtain a pack.

[0048]

Table 5 Example 5 Cleaning agent: (Formulation) (%) (1) Stearic acid 10.0 (2) Palmitic acid 8.0 (3) Myristic acid 12.0 (4) Lauric acid 4.0 (5) ) Oleyl alcohol 1.5 (6) Purified lanolin 1.0 (7) Perfume 0.1 (8) Preservative 0.2 (9) Glycerin 18.0 (10) Potassium hydroxide 6.0 (11) Asparagus Extract ^{* 1} 0.5 (12) SOD ^{* 7} 0.05 (13) Purified water Remainder * 7: Sigma Co .; obtained from Horseradish,
2.150 units / mg

(Production Method) A. Mixing components (9), (10) and (13), 70
Heat to ℃. B. The components (1) to (6) and (8) are mixed and heated to 70 ° C. C. The above B was added to the above A, kept at 70 ° C. for a while, cooled to 50 ° C. after completion of the saponification reaction, and the component (7),
(11) and (12) were added and cooled to obtain a cleaning agent.

[0050]

Table 11 Example 6 Gel ointment: (formulation) (%) (1) carboxyvinyl polymer 1.0 (2) triethanolamine 1.0 (3) 1,3-butylene glycol 10.0 (4) asparagus Gas extract ^{* 1} 0.01 (5) SOD ^{* 7} 0.02 (6) Purified water Remaining amount

(Production Method) A. Components (1) and (3) to (6) are mixed and dissolved. B. Ingredient (2) was added to A, mixed and homogenized to obtain a gel ointment.

[0052]

EFFECT OF THE INVENTION Since the external preparation for skin of the present invention has an excellent action of removing active oxygen, it has a stable and excellent effect for improving rough skin and preventing skin aging. Therefore, the external preparation for skin of the present invention, for the production of lipid peroxide due to the generation of active oxygen in the skin by ultraviolet rays, inflammation, blackening, aging, etc.,
It has an extremely high preventive effect and is extremely useful in beauty and medicine.

Claims (1)

[Claims] 1. An external preparation for skin comprising (A) an asparagus extract and (B) a superoxide dismutase.