JPH08301745A - Skin cosmetic - Google Patents

Abstract

PURPOSE: To obtain a skin cosmetic containing an extract of Citrus reticulata, preventing chapped skin, spots and freckles caused by ultraviolet light, excellent in inhibitory effect on aging of skin resulting from peroxidation of lipid. CONSTITUTION: This skin cosmetic contains 0.001-20wt.% calculated as a dried substance of an extract from pericarp of Citrus reticulata based on the total of the cosmetic. The extract of Citrus reticulata is excellent in ultraviolet light preventing effect in an UV-A range, further has eliminating action on free radicals and anti-oxidizing action, high water solubility and safety. The extract is obtained by drying pericarp of Citrus reticulata, immersing it in ethanol, etc., at a room temperature for 1 week to extract it, washing the extracted solution by passing it through a column of a synthetic adsorbent, eliminating the extract with an aqueous solution of ethanol and distilling away the solvent. The skin cosmetic is properly mixed with conventional components excepts the extract of Citrus reticulata and prepared into a cream, milky lotion, oil, lotion, pack, ointment, etc.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a skin cosmetic composition which is excellent in the effects of preventing rough skin, stains and freckles caused by ultraviolet rays and of suppressing skin aging due to lipid peroxidation.

[0002]

2. Description of the Related Art Generally, as a means for preventing spots and freckles, which are considered to be caused by ultraviolet rays, it is necessary to add UV absorbers and scattering agents to cosmetics or cosmetics so that ultraviolet rays reach the skin. Ways to interfere are being taken. In addition, as a method of reducing inflammation caused by already caused spots, freckles and ultraviolet rays, a method of adding a melanin production inhibitor, a whitening agent to a cosmetic or an external preparation, a method of adding an anti-inflammatory agent, and further ultraviolet rays In order to prevent the peroxidation of lipids caused by the above, methods such as blending an antioxidant are taken.

However, in the method of blending ultraviolet scattering, absorbing and shielding substances, when a powder of titanium oxide, zinc oxide or the like is blended in cosmetics or cosmetics, it is necessary to blend in a large amount to improve the usability and application. Since it causes a problem in color and the like, it is difficult to mix it in a sufficient amount. In the method of blending UV absorbers such as paramethoxycinnamate, it is difficult to blend an effective amount due to safety issues, and most of them are oil-soluble substances, which often impose restrictions on formulation. There was a problem. Also,
In this way, the method of incorporating a drug aiming at repair of the damage caused by the ultraviolet rays penetrating into the skin is SO
D, β-carotene, vitamin C and the like are known. However, all of these drugs have poor stability, and even if incorporated into cosmetics, they deteriorate or decompose and it is difficult to achieve the intended purpose sufficiently.

[0004]

SUMMARY OF THE INVENTION The present invention has been made in view of the above circumstances, and its purpose is to prevent skin roughness, spots and freckles caused by ultraviolet rays, and to suppress skin aging due to lipid peroxidation. An object is to provide a skin cosmetic having the effect of

[0005]

In view of the present situation, as a result of intensive studies, the present inventors have found that the ponkan extract has an excellent effect of preventing ultraviolet rays in the UV-A region.
Further, it has free radical scavenging action and anti-oxidant action as well as high water solubility and excellent safety, and it was found that there are almost no restrictions on the formulation, and the present invention has been completed.

That is, the present invention is a skin cosmetic containing an extract of poncan.

The cosmetic material of the present invention will be described in detail below.

The poncan extract applied to the present invention is preferably extracted from the skin of poncan with an aqueous solvent.

A production example of the ponkan extract applied to the present invention is shown below.

Manufacturing Example 1. After drying the skin of ponkan in a drier at 40 ° C for 2 days, 200 g of it is about 10 mm x 5 m.
Shred to about m, 1000 ml of 60% aqueous ethanol solution
Extraction was carried out by immersing it in room temperature at room temperature for 1 week. The extract was passed through a column of synthetic adsorbent (Diaion HP-20), washed with water, desorbed with a 50% aqueous ethanol solution, and the solvent was distilled off to obtain 4.2 g of an extract. Production example 2. After drying the skin of ponkan for 2 weeks at room temperature, 200 g was immersed in 1000 ml of 30% ethanol aqueous solution for 1 week at room temperature for extraction. The extract was passed through a column of synthetic adsorbent (Diaion HP-20), washed with water, desorbed with an aqueous 30% ethanol solution, and the solvent was distilled off to obtain 2.5 g of an extract. Production example 3. After drying the skin of ponkan for 2 weeks at room temperature, 200 g was immersed in 1000 ml of 30% ethanol aqueous solution for 1 week at room temperature for extraction. The extract was adsorbed on a column of cation exchange resin (Dowex 50W), desorbed with a 30% aqueous ethanol solution, and the solvent was distilled off to obtain 5.8 g of an extract.

The ponkan extract thus obtained is extremely stable, and when it is used as a preparation, it causes discoloration, odor,
Since it does not change over time such as decomposition and inactivation, it can be blended stably and easily in various dosage forms. Also, it has good water solubility, so it is easy to use in various dosage forms such as creams, emulsions and lotions Is applicable to.

The dosage form as a cosmetic is not particularly specified, but specific examples include creams, emulsions, oils, lotions, packs, ointments and the like. From the viewpoint of transdermal absorbability, creams, emulsions, It can be said that oil and the like are particularly preferable.

Here, the following experiment was conducted to evaluate the ultraviolet protection effect of the ponkan extract applied to the present invention.

Experiment 1. UV absorption spectrum The UV absorption spectrum of the ponkan extract was measured. The results are shown in Fig. 1. This extract has an absorption maximum near 329 nm, and is UV-comparable with 2-hydroxy-4-methoxybenzophenone which is widely used as an ultraviolet absorber.
Shows the same level of UV absorption at the same concentration in the A region,
It was proved to be effective as an ultraviolet absorber.

[0015]

[Figure 1]

Experiment 2. Free radical scavenging test 2,2'-diphenyl-1 which is a neutral free radical
The free radical scavenging ability of ponkan extract was measured using an ethanol solution of picrylhydrazyl (DPPH). As a control, the free radical scavenging ability of vitamin E was similarly measured.

<Experimental Method> 1 ml of 0.5 mM DDPH ethanol solution and 2 ml of acetate buffer (0.1 M, pH 5.5) were added to 5 ml of ethanol solution of vitamin E (α-tocopherol) or poncan extract, and the mixture was kept at room temperature for 60 minutes. After standing, the absorbance at 517 nm was measured with a spectrophotometer. Varying the concentration of vitamin E or ponkan extract, a graph of X-axis: sample amount Y-axis: DDPH radical scavenging amount was drawn, and a sample amount for halving DDPH radical was determined as an EC50 value. As a result, the EC50 value of the ponkan extract was 67.6 μg / 5 ml and that of vitamin E was 43.0 μg / 5 ml. As a result, although Ponkan extract is slightly inferior to Vitamin E, DPP
It became clear that H radicals are effectively eliminated. FIG. 2 shows a measurement graph of the erasing ability of DPPH.

[0018]

FIG. 2

Experiment 3. Squalene Oxidation Inhibition Test Squalene was peroxidized by UV irradiation, and the amount of lipid peroxide produced was measured when the ponkan extract was added, when vitamin E was added, and when it was not added.

<Sample> 1. Blank: 10 ml of 99.5% ethanol added to 1 ml of squalene. 2. Control: Vitamin E or E in 1 ml of squalene
Mix D 4.3 mg (1 mM) was added, 99.5%
10 ml with ethanol added. 3. Sample: 4.3 mg of sample in 1 ml of squalene
Was added, and 99.5% ethanol was added to make 10 ml. <Test method> 1. Put the above sample in a test tube, mix thoroughly with a touch mixer, and stir until dissolved. 2. Transfer the sample liquid that has been mixed and dissolved into a glass dish having a diameter of 4.5 cm and wrap it. 3. Irradiate with ultraviolet rays from an ultraviolet lamp for 6 hours. (Total amount of ultraviolet rays: 19 vwh / cm ² ) 4. The sample after irradiation is measured by the TBA method. <Preparation of TBA solution> 1.7.5 g of trichloroacetic acid is weighed in a beaker and dissolved in a small amount of distilled water. 2.1 Add 12.5 ml of N-HCl. 3. Add 0.1875 g of TBA and dissolve by sonication. Add 20 mg of BHT to a 4.50 ml volumetric flask, and
Add 1 ml of 9.5% ethanol to dissolve. Add 3 to 5.4, make up to 50 ml with distilled water,
Mix well. <Measurement procedure> 1. Put 2 ml of test solution and 4 ml of TBA solution into a test tube,
Stir well with a touch mixer. At this time, 4 ml of TBA solution was added to 2 ml of 99.5% ethanol as a standard for measurement.
Also prepare the one with. 2. Boil for 30 minutes. 3. Cool rapidly with ice. 4. After centrifuging for 10 minutes, spectrophotometer 535n
The absorbance at m is measured. <Calculation of measurement result> The TBA value of the sample was calculated by the formula (1) with the blank value being 100 and the vitamin E value being 50.

[0021]

## EQU1 ## TBA value = 100- (50 (B-X) / B-E) (1) where B = blank absorbance, X = sample absorbance,
E = absorbance of vitamin E

Table 1 shows the obtained calculation results.

[0023]

[Table 1]

As is apparent from Table 1, the poncan extract applied to the present invention was superior to vitamin E in the lipid peroxide production-inhibiting action.

Examples of the present invention will be shown below, but the present invention is not limited to these examples. The mixing ratio is parts by weight.

Example 1. Lotion (A) Ethanol 15 1,3-butylene glycol 2 Polyoxyethylene (50) Hydrogenated castor oil 1 (B) Ethylparaben 0.05 Perfume 0.05 Ponkan extract 0.5 Citric acid 0.1 Sodium citrate 0.15 Purified water 81.15 (Production method) The components of (A) are combined and dissolved at room temperature. On the other hand, each component (B) is also dissolved at room temperature, and this is added to the component (A) to solubilize it.

Example 2. Emulsion (A) Polyoxyethylene (20) hydrogenated castor oil 1.5 Coconut oil fatty acid monoglyceride 1 Oleic acid triglyceride 7.5 (B) Glycerin 2.5 Ponkan extract 0.05 Purified water 87.25 (C) Perfume 0 .2 (Manufacturing method) Combine with each component of (A), mix by heating, and 70 ° C
And The respective components of (B) are combined and mixed by heating at 70 ° C., the component (A) is added to this and emulsified, and (C) is added while cooling.

Example 3. Cream (A) Vaseline 18 Cetanol 8 Polyoxyethylene (20) oleyl ether 1.4 Sorbitan monostearate 0.8 (B) Ethylparaben 0.3 Ponkan extract 0.1 Purified water 71.2 (C) Perfume 0 .2 (Manufacturing method) Combine with each component of (A), mix by heating, and 70 ° C
And The components of (B) are combined and mixed by heating at 70 ° C, the component (B) is added to the component (A) to emulsify, the mixture is cooled to 35 ° C, and the component (C) is added.

Example 4. Cream (A) POE (30) Cetyl ether 2 Glycerin monostearate 10 Liquid paraffin 10 Vaseline 4 Cetanol 5 γ Tocopherol 0.05 2-Hydroxy-4-methoxybenzophenone 0.5 Butylparaben 0.2 (B) Purified water 63.25 Ponkan Extract 5 (Production Method) The components of (A) are combined and heated to 80 ° C.
The component (B) is heated to 80 ° C. The component (B) is added to the component (A), the mixture is stirred and emulsified, and then cooled to 35 ° C.

Example 5. Emulsion (A) Synthetic Geyrow 2.5 Cetanol 1 Squalane 4 Stearic acid 1 Polyethylene glycol monostearate (25EO) 2.2 Glycerin monostearate 0.5 Butylparaben 0.1 γ-tocopherol 0.05 BHT 0.01 4 -(1,1-Dimethylethyl) -4'-methoxy-dibenzoylmethane 0.5 (B) 1,3-butylene glycol 3 propylene glycol 7 xanthan gum 0.1 carboxyvinyl polymer 0.2 potassium hydroxide 0.2 poncan extract 1 Purified water 76.64 (Production method) Components (A) and (B) are dissolved with stirring at 70 ° C. The component (A) is added to the component (B), preliminarily emulsified, uniformly emulsified with a homomixer, and after emulsification, cooled to 30 ° C. with stirring.

Example 6. Lotion (A) POE (20) sorbitan monolaurate 1.5 POE (20) lauryl ether 0.5 ethanol 10 γ-tocopherol 0.02 (B) glycerin 5 sodium isoferurate 0.5 citric acid 0.15 citric acid Sodium acid 0.1 Ponkan extract 3 Purified water 79.23 (Manufacturing method) The components of (A) are combined and dissolved at room temperature. On the other hand, each component of (B) is also dissolved at room temperature and added to the component (A) to be solubilized.

Experimental Example 1 Light (UV) Aging Reaction Inhibition Test (Sample) (a) 1% by weight aqueous solution of poncan extract of Production Example 1 (b) 1% by weight aqueous solution of poncan extract of Production Example 2 ( C) 1% by weight aqueous solution of ponkan extract of Production Example 3 (d) Control (purified water only) (Method) Four groups of hairless mice (9 to 10 weeks old, female) were prepared as experimental animals, one group consisting of five groups. The dorsal skin was irradiated with UV-A 5 times a week for 6 months, once a day. A Toshiba BLB lamp was used as a light source, and a plate glass having a thickness of 7 mm was attached between the animal and the lamp in order to cut UV-B. The amount of irradiation energy was 14 to 28 mJ / cm ² / day, but the amount of energy was gradually increased every month. U
One hour before irradiation with VA, samples (a) to (d) were applied to each group of hairless mice, and 200 μm was applied to the entire back of the animal.
1 was evenly applied. After 6 months, the photoaging reaction generated on the skin was visually evaluated according to the following criteria. (Judgment Criteria) 0: Light-skinned pink color and tajiwa are observed. 1: The skin color turned pale and Tajiwa disappeared. 2: The skin color was moderately pale, and Tajiwawa disappeared,
Weak nodules and large wrinkles and tarmi are observed. 3: The skin color was intensely pale, the white wrinkles disappeared, strong nodules, and strong wrinkles and tarmi were observed.

The average value of the scores of 5 animals was obtained, and the inhibition rate was calculated using the following formula. Table 2 shows the results.

[0034]

[Equation 2] Inhibition rate = 100 × (average value of control group−average value of sample administration group) / average value of control group

[0035]

[Table 2]

From these results, it was found that the poncan extract applied to the cosmetic of the present invention has an effect of suppressing the UV-A photoaging reaction of hairless mice.

<Experimental Example 2> UV erythema suppression test (Sample) (a) 1% by weight aqueous solution of poncan extract of Production Example 1 (b) 1% by weight aqueous solution of poncan extract of Production Example 2 (c) Production Example 1 wt% aqueous solution of poncan extract of 3 (d) Control (only purified water) (Method) Prepare 4 groups of 5 Hartley guinea pigs (body weight 700 to 900 g, male) as experimental animals
The back was removed and shaved beforehand. To prevent the ultraviolet rays from hitting other than the irradiated area, a wide bandage with 6 small holes of 1.5 × 1.5 cm (3 in parallel on the left and right) was placed on the hair removal area, and ultraviolet rays were irradiated from above. did. Toshiba FL3 as the light source
0-SE was used. Irradiation energy amount is 768 mJ / c
It was set to m ² . After 24 hours, a uniform erythema reaction was observed at the above 6 sites. The sample was administered once before and three times after the ultraviolet irradiation. The single dose was 50 μl / site. The erythema reaction 24 hours after UV irradiation was evaluated according to the following criteria. (Judgment Criteria) 0: No skin reaction is observed. 1: Weak or erythema with unclear boundaries is observed. 2: Moderate erythema with unclear boundaries is observed. 3: Severe unclear erythema (sometimes accompanied by edema) is observed.

The average of the scores of 5 animals was determined, and the inhibition rate of erythema of ultraviolet rays by each sample was determined in the same manner as in Experimental Example 1 above. The results are shown in Table 3.

[0039]

[Table 3]

As is clear from the above results, the poncan extract applied to the cosmetics of the present invention showed a remarkable inhibitory effect on the UV erythema of Hartley guinea pigs.

<Evaluation of Skin Cosmetics of the Present Invention> Healthy Japanese adult women 40 having dry rough skin, wrinkles, and tarmi on the face 40
Named as panelists and asked to divide into 10 groups of 4 groups (A group, B group, C group, D group). For group A, the lotion obtained in Example 1 on the face and for group B were implemented. The lotion of Comparative Example 1 in which the poncan extract of the lotion of Example 1 was replaced with purified water, the cream obtained in Example 3 for the C group, and the poncan extract of the cream of Example 3 for the D group were purified. The cream of Comparative Example 2 which had been replaced with water was used each day by a usual use method and continuously used for 3 months.

Comparative Example 1. Lotion (A) Ethanol 15 1,3-butylene glycol 3 Dipropylene glycol 2.0 Polyoxyethylene (30) Hydrogenated castor oil 1 PEG-1500 0.5 (B) Methylparaben 0.1 Perfume 0.08 Citric acid 0 .1 Sodium citrate 0.15 Sodium hyaluronate 0.01 Methyl cellulose 0.01 Purified water 78.05 (Manufacturing method) The respective components of (A) are combined and dissolved at room temperature. On the other hand, each component (B) is also dissolved at room temperature, and this is added to the component (A) to solubilize it.

Comparative Example 2. Cream (A) Squalane 15 Microcrystalline wax 1.6 Synthetic whale wax 0.5 Orange Raffy oil 2.5 Macadamia nut oil 7 Dimethyl silicone oil 5 Stearic acid 2.5 Stearyl alcohol 2 Stearate monoglyceride 2.5 Cholesteryl hydroxystearate 1 .5 P0E (20) sorbitan monostearate 2 butylparaben 0.1 (B) glycerin 5 dipropylene glycol 5.5 maltitol 0.5 potassium hydroxide 0.2 ethylparaben 0.2 purified water 46.2 (C ) Fragrance 0.2 (Manufacturing method) Combine with each component of (A), mix by heating, and 70 ° C.
And The components of (B) are combined and mixed by heating at 70 ° C, the component (B) is added to the component (A) to emulsify, the mixture is cooled to 35 ° C, and the component (C) is added.

Three months after the start of use of each cosmetic, self-evaluation was carried out on the evaluation condition of each of the evaluation items such as makeup paste, rough skin, wrinkles, and tarmi, or the state of natural deterioration, based on the following evaluation criteria. Table 4 shows the number of people with each grade and the average of the grades for each group and each evaluation item.

(Evaluation Criteria) 3: There was a marked improvement. 2: It improved considerably. 1: Somewhat improved. 0: No change. -1: Natural deterioration.

[0046]

[Table 4]

From these results, the cosmetics of the examples of the present invention were compared with the cosmetics of the comparative examples containing no ponkan extract.
It is clear that it improves well on makeup paste, rough skin, wrinkles and tarmi.

[0048]

INDUSTRIAL APPLICABILITY According to the present invention, it is highly safe and can be used also as a water-soluble ultraviolet absorber, and has a free radical scavenging action and a lipid peroxide inhibiting action which are superior to those of vitamin E. A cosmetic having the effects of improving rough skin, wrinkles and tarmi, preventing spots and freckles and suppressing skin aging is obtained.

[Brief description of drawings]

FIG. 1 is a diagram showing an ultraviolet absorption spectrum of a ponkan extract obtained in Production Example 1.

FIG. 2 is a diagram showing the free radical scavenging ability of the ponkan extract obtained in Production Example 2.

Claims (3)

[Claims] 1. A skin cosmetic containing a ponkan extract. 2. The skin cosmetic according to claim 1, wherein the poncan extract is extracted from the skin of poncan with an aqueous solvent. 3. The skin cosmetic according to claim 1, wherein the content of the ponkan extract is 0.001% by weight to 20% by weight in terms of dry matter.