JPH06128143A - External agent for skin - Google Patents

Abstract

PURPOSE:To provide an external agent for skin having excellent skin-beautifying effect, effective in preventing and ameliorating spots, freckles and the darkening of skin caused by sunburn, etc., and safely usable because of its stability and safety. CONSTITUTION:The external agent for skin contains (A) an asparagus extract and (B) (B1) N,N'-diacetylcystine dimethyl or (B2) one or more kinds of the extracts of plants selected from Coix laryma-jobi, Polygonum bistorta, Sophora angustifolia, hawthorn, hop, wild rose and Easter lily.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a novel external preparation for skin which is excellent in whitening effect and has high stability and safety.

[0002]

2. Description of the Related Art Conventionally, the problems to be solved by the invention
Whitening cosmetics are widely used for the purpose of obtaining beauty effects such as preventing dark skin, stains, freckles, etc., and as such whitening agents, ascorbic acid, glutathione, colloidal sulfur, etc. are mainly used as whitening agents. It is compounded. However, since ascorbic acid is susceptible to oxidation, it is difficult to expect a certain effect to be exhibited, and glutathione and colloidal sulfur have a drawback that they have a peculiar offensive odor and precipitation.

Therefore, recently, whitening agents have been widely searched from the natural world, for example, screening of plant extracts, and some extracts having the effect have been confirmed.

However, this extract was not sufficiently satisfactory for actual use, since the stability of the product was lowered when it was blended in a high concentration in an external preparation in the expectation of a higher whitening effect. Therefore, there has been a demand for an external preparation for the skin which has excellent whitening effect, stability and safety.

[0005]

Under the circumstances, the present inventor has completed the present invention as a result of earnest research.

That is, the present invention provides the following components (A) and (B), (A) asparagus extract, (B) (A) N,
N'-diacetylcystine dimethyl, or (b) one or two or more kinds of plant extracts selected from Yokuinin, Ibukitoranoo, Clara, hawthorn, hop, Neubara and white lily, for external skin use The agent is provided.

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 and hexane. Hydrocarbons: One kind or two or more kinds of 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 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 compounding amount of the asparagus extract in the external preparation for skin of the present invention is 0.0001 in terms of dry solid content.
-10.0% by weight (hereinafter simply referred to as "%") is preferable, and a range of 0.01-5.0% is particularly preferable. If the content is less than 0.0001%, the effect is not sufficiently exhibited, and if it exceeds 10.0%, no further increase in the effect is observed.

The N, N'- of the component (B) of the component (B) of the present invention.
Diacetylcystine dimethyl has the following structural formula

[0011]

[Chemical 1]

It is known that it is easily absorbed by the skin, converted into cystine and cysteine, and exhibits a skin activating action and a whitening action (Clinical Dermatology 9 (6) p. 444). ). In the present invention, this N,
N'-diacetylcystine dimethyl is preferably contained in the total composition in an amount of 0.0001 to 5%, particularly 0.01 to 3.0%. If it is less than 0.0001%, a sufficient whitening effect cannot be obtained, and if it exceeds 5%, the stability of the product decreases, which is not preferable.

Among the plant extracts of (B) of the component (B) of the present invention, the Yokuinin extract is an adlay (Co) of the Poaceae family.
ix lacryma-jobi L. var. ma-
yuen (ROMAM) STAPF) obtained by extracting from seeds and the like excluding the seed coat. Further, the extract of Ibukitoranoo, Clara, hawthorn, hops, Neubara, white lily, the use part of the plant is not particularly limited, and these leaves, branches, stems, flowers, fruits, roots and the like can be extracted. However, among others, rhizomes for Ibukitoranoo, roots for Clara, hawthorn, fruits of hawthorn, fruits for hops, flowers for white lily, and bulbs for white lily are preferable.

The extraction method is not particularly limited, but it can be extracted, for example, at room temperature or 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 propylene glycol and 1,3-butylene glycol; lower alkyl esters such as ethyl acetate; carbonization such as benzene and hexane. Hydrogen; one or more ethers such as diethyl ether may be used. Among these, water or a water-soluble solvent, particularly water, ethyl alcohol, glycerin, 1,3-butylene glycol, or a mixed solvent of two or more thereof is preferable.

The plant 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 treatment such as concentration and filtration, and may be appropriately used.

These plant extracts of the component (B) can be used alone or in combination of two or more kinds, and 0.0001 to 10.0%, particularly 0.001 as solid content in the whole composition.
It is preferable to mix it up to 5.0%. If it is less than 0.0001%, a sufficient whitening effect cannot be obtained, and if it exceeds 10.0%, the effect does not increase, and depending on the extract, problems such as coloring of the product may occur. Absent.

Further, the external preparation for skin of the present invention contains, in addition to the above-mentioned essential components, aqueous components, powders, surfactants and oils used in ordinary external preparations for skin, as long as the effects of the present invention are not impaired. , Moisturizers, alcohols, pH adjusters, preservatives,
Dyes, 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 can be manufactured by a conventional method by mixing the above-mentioned components (A) and (B), which are essential components, and can be manufactured by a conventional method. It can be applied as a cleansing, pack, detergent, foundation, and other external medicines for dispersion, granules, ointments, etc. for medicine, quasi-drugs or cosmetics.

[0019]

The present invention will be described in more detail with reference to Test Examples and Examples, but the present invention is not limited to these.

Test Example 1 Tyrosinase activity inhibition test: <Sample> Asparagus extract: Raw white asparagus root portion was weighed at 23650 g (as fresh weight) as a raw material,
Next, ethanol was added after adjusting the alcohol concentration to 60%. 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 for extraction, and then the extract was collected by suction filtration into a suction filtration bottle. To the extraction residue, 25 liters of 60% ethanol was added again, the above operation was repeated, and about 66 liters of the extract was concentrated by a rotary evaporator and the solvent was distilled off to obtain a brown concentrated extract.
00 g (dry solid content 4%) was obtained (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 equivalent amounts to suspend the extract, 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 tilted by centrifuging the centrifuge tube to discard the benzene in the upper layer, or by sucking off only the upper layer with a pipette tube. The lipid component in the extract was removed, and 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 aqueous 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 several times with fresh ether to wash away the dissolved ether of the contaminants. The almost white precipitate obtained by such an operation was dried in a vacuum desiccator and then ground in a mortar to obtain about 11 g of asparagus saponin powder (sixth step).

In this test example, the asparagus extract obtained in the first step was used.

Yokuinin extract: Yokuinin extract (manufactured by Maruzen Pharmaceutical Co., Ltd.) Ibuquitranoo extract: Ibukitranoo extract (A.
M. Company I) Clara extract: Kujin extract (Maruzen Pharmaceutical Co., Ltd.) Hawthorn extract: Hawthorn extract (Maruzen Pharmaceutical Co., Ltd.) Hop extract: Hop extract (Maruzen Pharmaceutical Co., Ltd.) Neubara extract: Harbex Novara Extract (Koei Kogyo Co., Ltd.) Shirayuri extract: Shirayuri extract GR-327 (Maruzen Pharmaceutical Co., Ltd.)

<Measuring method> An enzyme solution [manufactured by Sigma, 28,000 units of tyrosinase (10 mg)]
Dissolved in 20 ml of phosphate buffer (pH 6.8)]
Add 1 ml and add 0.1M phosphate buffer (pH 6.8)
Was added to make 4 ml, and this was incubated at 25 ° C. for 10 minutes. A substrate solution [L-DOPA (Tokyo Kasei) 198.0 mg, which had been kept at 25 ° C. in advance, was added to this.
1.0 ml of a solution dissolved in 100 ml of 1 M phosphate buffer (pH 6.8) was added and reacted for 10 minutes. Then 4
Absorbance (OD _s ) at 75 nm was measured. Further, the absorbance (OD _HE ) of the same reaction using the enzyme deactivated by heating and the absorbance (OD _B ) when no sample was added were measured, and the activity inhibition rate of tyrosinase activity was calculated from the following formula.

[0028]

[Equation 1]

The results are shown in Tables 1 and 2.

[0030]

[Table 1]

[0031]

[Table 2]

As is clear from Tables 1 and 2, when the components (A) and (B) were combined, the tyrosinase activity inhibitory action was higher than when they were used alone, and a synergistic whitening effect was exhibited. .

Example 1 Emulsion: An emulsion having the composition shown in Table 3 was prepared and evaluated for its whitening effect. The results are shown in Table 4.

[0034]

[Table 3]

<Production Method> A. (6) to (11), (15) and (16) are mixed by heating and kept at 70 ° C. B. (1) to (5), (12) and (13) are mixed by heating and kept at 70 ° C. C. B is added to A and mixed, and (14) is further added to emulsify uniformly and cooled to 30 ° C. to obtain an emulsion.

<Whitening effect test> Women aged 23 to 44 years 15
Name the panel, and sample 1 after washing the face twice daily, morning and night
The use test was performed by applying an appropriate amount of each of the 6 to 23 milky lotions to each face for 12 weeks, and evaluated according to the following criteria.

Evaluation Criteria: Effective: Spots and freckles became inconspicuous. Slightly effective: Spots and freckles are less noticeable. Ineffective: No change.

[0038]

[Table 4]

As is apparent from Table 4, the emulsion of the present invention (Samples 21 to 2) prepared by combining the components (A) and (B) in combination.
3) is excellent in the effect of making spots and freckles inconspicuous not only when compared with Sample 16 which does not contain any of these, but also when compared with Samples 17 to 20 in which the component (A) or (B) is blended alone. , Showed a remarkable whitening effect.

[0040]

Table 2 Example 2 Cosmetics: <Prescription> (%) (1) Glycerin 5.0 (2) 1,3-butylene glycol 6.5 (3) Polyoxyethylene sorbitan monolaurate ester (20E.O. ) 1.2 (4) Ethyl alcohol 8.0 (5) Yellowtail extract (as dry solids) 0.01 (6) Asparagus extract ^{* 1} 2.0 (7) Yokuinin extract ^{* 2} (Dry solids) As a minute) 0.05 (8) Preservative Suitable amount (9) Perfume Suitable amount (10) Purified water Remaining amount

<Production Method> A. (3), (4), (8) and (9) are mixed and dissolved. B. (1), (2), (5) to (7) and (10) are mixed and dissolved. C. A and B were mixed and made uniform to obtain a lotion.

[0042]

Table 6 Example 3 Cream: <Prescription> (%) (1) Beeswax 6.0 (2) Cetanol 5.0 (3) Reduced lanolin 5.0 (4) Squalane 30.0 (5) Glycerin monostea Rate 4.0 (6) Lipophilic glyceryl monostearate 2.0 (7) Polyoxyethylene sorbitan monolaurate ester (20 EO) 2.0 (8) Asparagus extract ^{* 1} 1.0 (9) Yokuinin extract ^{* 2} (as dry solids) 0.2 (10) Preservative 0.3 (11) Perfume 0.05 (12) Purified water Remaining amount

<Production Method> A. (1) to (7), (10) and (11) are mixed,
Heat and keep at 70 ° C. B. Mix (8), (9) and (12) and heat to 7
Keep at 0 ° C. C. B was added to A, mixed, and then cooled to obtain a cream.

[0044]

Table 4 Example 4 Pack: <Formulation> (%) (1) Polyvinyl alcohol 20.0 (2) Ethanol 20.0 (3) Glycerin 5.0 (4) Kaolin 6.0 (5) Asparagus extraction ^{* 1} 0.1 (6) Yokuinin extract ^{* 2} 2.0 (7) Preservative 0.3 (8) Perfume 0.1 (9) Purified water Remaining amount

<Production Method> A. (1), (3) to (6) and (9) are mixed to obtain 70
Heat to ℃ and stir. B. Mix (2), (7) and (8). C. B was added to A, mixed, and then cooled to obtain a pack.

[0046]

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} 0.2 (12) Yokuinin extract ^{* 2} (as dry solids) 0.01 (13) Purified water Remaining amount

<Production Method> A. Mix (9), (10) and (13) and heat to 70 ° C. B. Mix (1) to (6) and (8) and heat to 70 ° C. C. B was added to A and maintained at 70 ° C. for a while, and after the saponification reaction was completed, it was cooled to 50 ° C., (7), (11) and (12) were added and cooled to obtain a cleaning agent.

Example 6 An emulsion having the composition shown in Table 9 was produced and evaluated for its whitening effect. The results are shown in Tables 10 and 11.

[0049]

[Table 9]

<Production Method> A. (6) to (9) and (14) are heated and mixed, and the temperature is 70 ° C.
Keep on. B. (1) to (5), (10) and (11) are mixed by heating and kept at 70 ° C. C. B is added to A and mixed, and then (12) is added and uniformly mixed, then (13) is added and uniformly emulsified, and cooled to 30 ° C. to obtain an emulsion.

Test Example 2 The whitening effect of a test substance was examined by utilizing the fact that the back of a colored guinea pig was shaved and the pigmentation was caused by irradiation with ultraviolet rays under anesthesia. UV irradiation is FL2 made by Toshiba Corporation
Three 0S / BLB lamps and three FL20S / E30 lamps are irradiated at the same time, and the amount of ultraviolet rays is 4.8 × 10 ⁶ erg / cm ²
And 24 hours before UV irradiation, immediately after irradiation, and irradiation 2
After 4 hours, in 4 places (2 x 2 cm) on the back of the guinea pig,
Samples 24-27 were rubbed well in 0.2 ml increments. However,
Prior to irradiation, the application site was thoroughly washed with warm water. Seven days after the irradiation, the degree of pigmentation at each site was observed and judged according to the following criteria. The results are shown in Table 10.

<Evaluation criteria> Pigmentation evaluation score: 0: No pigmentation is observed. 1: Very slight pigmentation is observed. 2: Pigmentation is observed, but the boundary with the non-irradiated site is unclear. 3: Pigmentation was observed, and the boundary with the non-irradiated site was clear. Whitening effect; Pigmentation score of 1 or less out of 10 guinea pigs: 8 or more: excellent effect 6 or more: effective 4 or more: moderately effective 3 or less: ineffective

[0053]

[Table 10]

As is apparent from Table 10, the emulsion of the present invention containing the components (A) and (B) in combination (Sample 27).
Shows a remarkable pigmentation-preventing effect not only when compared to Sample 24 which does not contain any of these, but also when compared to Samples 25 and 26 in which each of them is blended alone.

Test Example 3 Use-effect test 15 women aged 23 to 44 years were used as a panel, and each day, twice a day in the morning and at night, and after washing the face, the emulsions of Samples 24 to 27 were applied to the face in appropriate amounts for 12 weeks. According to the above, a usage test was conducted and evaluated according to the following criteria. Evaluation criteria; Effective: Spots and freckles are not noticeable. Slightly effective: Spot freckles are less noticeable. Ineffective: No change.

[0056]

[Table 11]

As is clear from Table 11, the emulsion of the present invention (Sample 27) was not only compared with Sample 24 containing no such emulsion, but also Sample 2 in which each of them was blended alone.
Compared with Nos. 5 and 26, the effect of making spots and freckles inconspicuous was excellent and a remarkable whitening effect was exhibited.

[0058]

Table 7 Example 7 Lotion: <Prescription> (%) (1) Glycerin 5.0 (2) 1,3-Butylene glycol 6.5 (3) Polyoxyethylene sorbitan monolaurate ester (20E.O. ) 1.2 (4) Ethyl alcohol 8.0 (5) Assembly extract (as dry solids) 0.01 (6) Asparagus extract ^{* 1} 2.0 (7) N, N'-diacetylcystine dimethyl 0.2 (8) Preservative Suitable amount (9) Perfume Suitable amount (10) Purified water Remaining amount

<Production Method> A. (3), (4), (8) and (9) are mixed and dissolved. B. (1), (2), (5) to (7) and (10) are mixed and dissolved. C. A and B were mixed and made uniform to obtain a lotion.

[0060]

Table 8 Example 8 Cream: <Formulation> (%) (1) Beeswax 6.0 (2) Cetanol 5.0 (3) Reduced lanolin 5.0 (4) Squalane 30.0 (5) Glycerin monostea Rate 4.0 (6) Lipophilic glyceryl monostearate 2.0 (7) Polyoxyethylene sorbitan monolaurate ester (20 EO) 2.0 (8) Asparagus extract ^{* 1} 1.0 (9 ) N, N'-Diacetylcystine dimethyl 1.0 (10) Inositol 0.1 (11) Preservative 0.3 (12) Perfume 0.05 (13) Purified water Remaining amount

<Production Method> A. (1) to (7), (11) and (12) are mixed,
Heat and keep at 70 ° C. B. Mix (8) to (10) and (13), heat and keep at 70 ° C. C. B was added to A, mixed, and then cooled to obtain a cream.

[0062]

Table 14 Example 9 Pack: <Formulation> (%) (1) Polyvinyl alcohol 20.0 (2) Ethanol 20.0 (3) Glycerin 5.0 (4) Kaolin 6.0 (5) Rosemary extraction Liquid (Maruzen Pharmaceutical Co., Ltd.) (as dry solids) 0.02 (6) Asparagus extract ^{* 1} 0.1 (7) N, N'-diacetylcystine dimethyl 0.2 (8) Preservative 0.3 (9) Perfume 0.1 (10) Purified water Remaining amount

<Production Method> A. Mixing (1), (3) to (7) and (10),
Heat to 0 ° C. and stir. B. Mix (2), (8) and (9). C. B was added to A, mixed, and then cooled to obtain a pack.

[0064]

Table 10 Example 10 Cleaning agent: <Prescription> (%) (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} 0.2 (12) N, N'-diacetylcystine dimethyl 0.1 (13) Purified water Remaining amount

<Production Method> A. (9) to (10) and (13) are mixed and heated to 70 ° C. B. Mix (1) to (6) and (8) and heat to 70 ° C. C. B was added to A and maintained at 70 ° C. for a while, and after the saponification reaction was completed, it was cooled to 50 ° C., (7), (11) and (12) were added and cooled to obtain a cleaning agent.

[0066]

As described above in detail, since the external preparation for skin of the present invention has an excellent whitening effect, it is effective for blackening the skin due to sunburn and preventing / improving spots / freckles. Furthermore, since the external preparation for skin of the present invention is stable and safe, it can be used with confidence.

─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. ⁵ Identification code Internal reference number FI technical display area A61K 35/78 C 7167-4C

Claims (1)

[Claims] 1. The following components (A) and (B), (A) asparagus extract, (B) (a) N, N'-diacetylcystine dimethyl, or (b) yokuinin, ibukitranoo, clara, An external preparation for skin, which comprises one or more kinds of plant extracts selected from hawthorn, hops, white roses and white lilies.