JP2000128765A - Skin cosmetic - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a skin cosmetic, in which an ingredient obtained in good yield from a readily available plant body is compounded, having excellent active oxygen seed-eliminating action and useful for preventing and improving blackening and aging of skin by including an extract obtained from branch and leaf part of olive by using water, etc., as an extraction solvent. SOLUTION: This skin cosmetic comprises an extract obtained from branch and leaf part of olive at a ratio of preferably 0.05-2 wt.% by extraction using water, a hydrophilic organic solvent (preferably methanol or ethanol) or a mixture thereof as extracting solvent. The extract is obtained by immersing the branch and leaf part of olive into the above extraction solvent, preferably at 5-15 weight ratio of the extraction solvent to the branch and leaf part of olive, eluting a soluble ingredient while gently stirring under heating at ordinary temperature to about 100 deg.C, filtering or centrifuging the eluate, distilling the solvent away from the resultant extract, as necessary carrying out treatment such as drying or purification. The cosmetic has forms of ointment, cream, milky lotion, etc.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a skin having a skin-protecting action mainly for preventing or improving roughening, wrinkles, dullness, dullness, and abnormal pigmentation due to external stimuli such as sunburn. It concerns cosmetics.

[0002]

2. Description of the Related Art Since skin is an organ that easily receives active factors such as ultraviolet rays and easily generates active oxygen, it often causes damage due to an increase in active oxygen concentration.
In other words, a large amount of superoxide (O ₂ ⁻ ) is generated in inflamed or ultraviolet-irradiated skin, which is converted into hydrogen peroxide (H ₂ O ₂ ) by the action of SOD (superoxide dismutase) or the like. further hydroxy radical (HO ·), sequentially changes the singlet oxygen ⁽¹ O ₂₎ or the like. When these reactive oxygen species are in large amounts, they act on melanocytes, which are pigment cells, to promote abnormal production of melanin, and to promote pigmentation. In addition, by causing cross-linking and fragmentation of elastin and collagen, which play an important role in the maintenance of skin tissue, the elasticity of the skin is reduced, causing wrinkles and lumps. Excessive reactive oxygen species also reduce the activity of cells by oxidizing squalane, a skin lipid, and cell membrane lipids, and exacerbate wrinkles, tarmi, rough skin, and the like.

[0003] Oxidative damage caused by these reactive oxygen species is usually avoided by maintaining a low concentration of reactive oxygen species by the action of reactive oxygen-scavenging enzymes such as SOD, catalase, glutathione and peroxidase. When a large amount of oxygen is generated and a part thereof remains without being completely erased, the above-described trouble occurs.

[0004] In order to prevent and improve skin aging caused by active oxygen, a search for a substance having a reactive oxygen species-eliminating effect has been conducted, and glutathione, vitamin C, vitamin E, vitamin B ₆ , butylhydroxytoluene, butyl Hydroxyaniline and the like were confirmed to be effective, but all of them had difficulty in stability and safety when incorporated into skin cosmetics.

In recent years, attempts have been made widely to obtain substances having an active oxygen scavenging action from natural products that are advantageous in terms of safety, and as a result, there is a possibility that elegans such as Prunusol A of Eucalyptus cherry and Eucalyptus may be used. Acids, barley, black rice, flavonoids of cereals such as black beans, catechin of tea, sesame of sesame, sage, carnosol and rosmanol contained in herbs such as rosemary were found, but generally less effective, Some are relatively effective,
The yield from raw material plants is extremely small and practically difficult; it has the property of irritating the skin; its solubility and stability when formulated in cosmetics are poor; .

[0006]

SUMMARY OF THE INVENTION Accordingly, an object of the present invention is to provide an excellent reactive oxygen species-eliminating action, obtain a plant from an easily available plant at a high yield, and furthermore, have an suitability as a skin cosmetic component. An object of the present invention is to provide a skin cosmetic which has an effect of preventing and improving blackening and aging of the skin by finding a substance provided and blending the substance.

Another object of the present invention is to add a substance which is suitable as a skin cosmetic component, has a function of eliminating reactive oxygen species, and is also effective in suppressing skin inflammation and allergic symptoms. An object of the present invention is to provide a multifunctional skin cosmetic.

[0008]

Means for Solving the Problems The skin cosmetic of the present invention, which has succeeded in achieving the above object, comprises a hydrophilic organic solvent such as methanol, ethanol, 1,3-butylene glycol and propylene glycol, water, The extract contains an extract obtained from olive branch by extraction using a mixture of the above as an extraction solvent.

[0009] The term "olives" refers to the branches and / or leaves of evergreen olives (Olea europaea L.) belonging to the Oleaceae family.

[0010] The olive branch extract has not only a reactive oxygen species eliminating effect but also a platelet aggregation inhibiting effect, thereby preventing skin inflammation and allergic symptoms caused by platelet aggregation. is there.

[0011]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Olives are trees native to the Mediterranean region, but are also cultivated in Japan for the purpose of utilizing fruits. The leaves have been used for nutrients, palliatives, laxatives, trauma treatments, etc. for a long time, but they are folk remedies, and the details of the active ingredients and their pharmacological actions have not been elucidated. Of course, it has not been known that the olive branch contains a substance having an active oxygen species eliminating action.

Although there is an example in which the antioxidant property of a phenolic compound extracted from olive leaves has been confirmed, since the extraction solvent is a non-polar solvent, the active oxygen species-scavenging component of the present invention which is extracted with an aqueous solvent is not used. Are considered different.

A substance obtained from olive branches and having a reactive oxygen species-eliminating action is water-soluble, is stable even when incorporated in many cosmetics, and is well absorbed percutaneously into the human body. Of the nature. Moreover, even when applied to the skin, it does not irritate the skin or cause irritation. Therefore, it has very advantageous properties for being incorporated into skin cosmetics and utilizing its useful effects.

In order to extract the active oxygen species-eliminating substance from the olive branch, various hydrophilic organic solvents, water, or a mixture thereof can be used. Particularly preferred extraction solvents are methanol, ethanol, , 3-butylene glycol, propylene glycol, water, or a mixture thereof.

The olive branches and leaves to be subjected to the extraction treatment may be either raw or dried. If lipids are extracted from a raw material for extraction using a non-polar solvent such as hexane in advance, active oxygen species-scavenging components can be efficiently extracted.

The extraction conditions and the apparatus used for the extraction are not particularly limited. Preferably, the olives are immersed in an extraction solvent in a weight ratio of 5 to 15 times, and gently heated at room temperature to about 100 ° C. Elute soluble components with stirring. When the solvent is distilled off from the extract obtained by filtration or centrifugation, a paste-like concentrate is obtained, and when further dried, a solid extract is obtained. The partial extract need not be a solid extract, but may be in the form of the above-mentioned extract or its concentrate. These can be used as it is as the skin cosmetic component of the present invention. However, as long as the active oxygen species elimination action is not impaired, activated carbon treatment, adsorption resin treatment, ion exchange resin treatment, liquid-liquid countercurrent distribution, etc. It may be used after purification by a method.

The preferred blending ratio of the olive branch extract to the skin cosmetics varies depending on the type of skin cosmetics.
About 0.001 to 10% by weight (particularly preferably 0.01 to 10% by weight)
5 to 2% by weight).

Representative forms of the skin cosmetics according to the present invention include ointments, creams, emulsions, lotions, packs,
Examples include, but are not limited to, bath additives.

The selection of other skin cosmetic constituents is not restricted by blending the olive branch and leaf extract, for example, avocado oil, rice bran oil, rice germ oil,
Oily components such as lanolin and squalane; glycerin, 1,3-
Butylene glycol, collagen, hyaluronic acid and its salts, chondroitin sulfate and its salts, chitosan,
Moisturizing agents such as chitin; complex lipids such as glycerophospholipid, sphingolipid, glyceroglycolipid, glycosphingolipid;
SOD, catalase, β-carotene, ginkgo biloba extract, vitamin C and its derivatives, vitamin E and its derivatives, gongo extract, kujin extract and other active oxygen-scavenging substances; guaiazulene, kamaazulene and its derivatives; glycyrrhizic acid, Glycyrrhetinic acid and its salts, glycyrrhetinic acid derivatives, anti-inflammatory agents such as zinc oxide; other plant extracts, thickeners, preservatives, ultraviolet absorbers, fragrances, antioxidants, water, alcohol, etc. Can be arbitrarily compounded.

[0020]

Example 1 Extraction of olive branch and leaf part 1 1 kg of a dried crushed olive leaf was put into 10 liters of water and extracted for 5 hours under reflux and heating. Thereafter, the extract obtained by filtration was concentrated under reduced pressure to obtain a paste, which was freeze-dried to obtain 136 g of a powder extract.

Example 2 Extraction of olive branch and leaf part 1 kg of dried crushed olive leaf was put into 10 liters of 50% by volume aqueous ethanol and extracted under reflux for 5 hours. Thereafter, the extract obtained by filtration was concentrated under reduced pressure to obtain a paste, which was freeze-dried to obtain 142 g of a powder extract.

Example 3 Extraction of olive branch and leaf portion 1 kg of the dried crude olive leaf was subjected to n-hexane extraction to extract and remove lipids. The residue was dried under reduced pressure, and then poured into 10 liters of ethanol. For 10 hours. The obtained extract was concentrated under reduced pressure to obtain a paste, which was freeze-dried to obtain 42 g of a powder extract.

Example 4 Extraction of olive branch and leaf part 1 kg of dried crushed olive leaf was put into 7 liters of 1,3-butylene glycol and extracted at 95 ° C. for 5 hours.
After cooling, the filtrate obtained by filtration was allowed to stand at 5 ° C. for 5 days,
The resulting deposits and precipitates were filtered using diatomaceous earth to obtain 4.5 liters of a clear extract (solid concentration 0.87% by weight).

Olive branch and leaf part extraction example 5
It poured into 0 liter and extracted under reflux heating for 5 hours. The obtained extract was concentrated under reduced pressure to obtain a paste, which was freeze-dried to obtain 28 g of a powder extract.

Olive branch and leaf extraction example 6 1 kg of dried crude olive branch was put into 7 liters of propylene glycol and extracted at 95 ° C for 5 hours. After cooling, the filtrate obtained by filtration was allowed to stand at 5 ° C. for 5 days, and the formed deposits and precipitates were filtered using diatomaceous earth to give a clear extract (solid content: 0.67% by weight). 9 liters were obtained.

Test Example 1 The olive branch and leaf extract obtained in each of the above examples was tested for superoxide elimination action, hydrogen peroxide elimination action, and radical elimination action for DPPH (diphenylpicrylhydroradical). The test method is as follows.

Superoxide elimination action (NBT
Method): 3 mM xanthine, 0.05 M Na ₂ CO ₃ buffer (pH
10.2) 3 mM EDTA, BSA solution and 0.75 mM N
0.1 ml of BT is placed in a test tube, 0.1 ml of the sample solution is added thereto, and the mixture is left at 25 ° C. for 10 minutes. Then, add a xanthine oxidase solution and stir quickly,
Let stand for minutes. Thereafter, the reaction is stopped by adding 6 mM copper chloride, and the absorbance at 560 nm is measured. The same operation and absorbance measurement are performed without adding an enzyme solution. further,
The same measurement is performed for the case where distilled water is added without adding the sample solution, and the superoxide elimination ratio is determined by the following equation.

Erasure rate (%) = [1- (St-So) / (B
t-Bo)] × 100 where St: absorbance when sample solution is added and enzyme solution is added. So: absorbance when sample solution is added and enzyme solution is not added. Bt: absorbance when sample solution is not added and enzyme solution is added. Bo: sample solution. Absorbance without additive and enzyme solution

The above-mentioned inhibition rate was measured by changing the sample concentration of the sample solution stepwise, and the inhibition rate of active oxygen production was found to be 50%.
The concentration IC ₅₀ (ppm) of the sample solution is calculated by interpolation.

Hydrogen peroxide scavenging action: 10 μl of a sample solution was added to 10 μl of a standard solution (concentration: 1.5 mM) of hydrogen peroxide.
After incubating at 37 ° C for 20 minutes, the coloring reagent [D
To a 0.1 M PIPES buffer (pH 7.0) containing 10 mM of A-64 (Wako Pure Chemical) and 0.5% of Triton X-100, 1 ml of a peroxidase solution (100 unit / ml, Wako Pure Chemical) was added.
The total amount was adjusted to 100 ml] 2.98 ml was added,
Incubate at 37 ° C. for 5 minutes, then measure the absorbance at 727 nm. Similar operation and absorbance measurement
Perform without the addition of a standard solution of hydrogen peroxide. Further, the same measurement is performed when distilled water is added without adding the sample solution, and the elimination rate of hydrogen peroxide is determined by the following equation.

Erasure rate (%) = [1- (CD) / (A-
B)] × 100 where A: Absorbance when hydrogen peroxide standard solution was added and sample solution was not added B: Absorbance when hydrogen peroxide standard solution was not added and sample solution was not added C: Hydrogen peroxide standard solution was added and sample solution Absorbance at the time of addition D: Absorbance at the time of adding no hydrogen peroxide standard solution and adding a sample solution

The erasing rate is measured by changing the sample concentration of the sample solution stepwise, and the concentration (ppm) of the sample solution at which the erasing rate of hydrogen peroxide becomes 50% is determined by an interpolation method.

Radical scavenging action on DPPH: 1.
3 ml of the sample solution is added to 3 ml of a 5 × 10 ⁻⁴ M methanol solution of DPPH, and the container is immediately sealed, shaken, and allowed to stand for 30 minutes. Thereafter, the absorbance at 520 nm is measured. As a control test, the same operation is performed using the solvent instead of the sample solution, and the absorbance at 520 nm is measured. As a blank test, immediately after adding 3 ml of the sample solution to methanol, the absorbance at 520 nm is measured, and the radical scavenging rate is calculated by the following equation.

Elimination rate (%) = [1- (BC) / A] × 100 where A: absorbance of control test B: absorbance when sample solution is added C: absorbance of blank test

The erasure rate was measured by changing the sample concentration of the sample solution in a stepwise manner.
The concentration (ppm) of the sample solution that becomes 0% is determined by interpolation.

Table 1 shows the test results. In addition, about the extract liquid by the extraction example 4 and the extraction example 6, it tested using the test sample prepared by concentrating and drying a part.

[0037]

Table 1 50% Elimination Concentration (ppm) Extract Elimination of Superoxide Elimination of Hydrogen Peroxide Elimination of Radical Extraction Example 1 28.2 8.0 37.2 Extraction Example 2 16.1 6.5 35.0 Extraction Example 3 15.3 6.6 34.5 Extraction example 4 17.4 9.4 31.3 Extraction example 5 18.3 7.2 33.3 Extraction example 6 16.1 9.6 25.5

Test Example 2 The olive leaf extract obtained in each of Extraction Example 1, Extraction Example 2 and Extraction Example 5 was tested for its platelet aggregation inhibitory activity by the following method.

Test method: 77 mM in blood of Japanese white rabbits
One-tenth volume of EDTA is added, and centrifuged at 1000 rpm for 10 minutes to remove a precipitate. Supernatant at 10 rpm at 2100 rpm
Centrifuge for minutes and collect the precipitated platelets. The obtained platelets are suspended in a platelet washing solution, and 10
Centrifuge for minutes. The precipitated platelets are collected and suspended in a platelet suspension so that the platelet count becomes 300,000 / μl. Washed platelet suspension 223 prepared as described above
To 1 μl, add 1 μl of a calcium chloride solution and keep at 37 ° C. for 1 minute. 1 μl of the sample solution is added thereto, and the mixture is kept at the same temperature for 2 minutes, and then stirred for 1 minute. Next, 25 μl of a collagen solution is added, and the mixture is kept at 37 ° C. for 10 minutes, and then the visible light transmittance A is measured to be used as an index of the platelet aggregation state. Separately, the procedure is the same as above except that the sample solution is not added, the visible light transmittance B is measured, and the platelet aggregation inhibition rate is determined by the following equation.

Platelet aggregation inhibition rate (%) = [(BA) / B] × 100 The platelet aggregation inhibition rate is measured by changing the concentration of the sample solution stepwise, and the concentration at which the inhibition rate becomes 50% IC ₅₀ (ppm)
Is determined by interpolation. Table 2 shows the test results.

[0041]

TABLE 2 extract IC ₅₀ Extract Example 1 201.5 Extract Example 2 296.1 Extract Example 5 212.6

Example 1 An emulsion of the following composition containing the olive leaf extract obtained in Example 2 of olive branch and leaf extraction was produced according to a conventional method of emulsion production.

Olive leaf extract 1 g Cetyl alcohol 0.5 g Beeswax 2 g POE (10) sorbitan monooleate 1 g Glycerin monostearate 1 g Sodium hyaluronate 0.1 g Propylene glycol 5 g Ethanol 3 g Ethyl paraben 0.3 g Flavor 0.03 g Remaining purified water (total amount is 100ml)

The following coating test was carried out on a milky lotion and a milky lotion of a comparative example similarly prepared from the same raw materials except that the olive leaf extract was not blended.

Subjects: From among many women aged 18 to 40, 20 persons who were judged as having rough skin corresponding to the evaluation 1 or 2 according to the evaluation criteria of the following judgment 1 were selected and used as subjects.

Application test: To each subject, the emulsion of Example 1 was applied to the left half of the face, the comparative emulsion was applied to the right half, and once each in the morning and evening.
It was applied for 30 days.

[Judgment 1: Rough Skin Improving Effect] After the completion of the coating test, a replica of the facial skin was taken using a replica method by Sylflo (manufactured by FLEXICL DEVELOPMENTS LTD), and the state of the skin pattern and exfoliation were observed with a 50-fold microscope. The condition was observed, and the condition of the skin was determined according to the following evaluation criteria.

[0048] is very large separation of the score evaluation one corner layer. Skin grooves and skin hills have disappeared. (Rough skin condition) 2 Extensive peeling of the stratum corneum. Skin crevices / skins are not clear. (Rough skin condition) 3 The stratum corneum is slightly peeled off. Skin grooves and ridges are recognized but flat. (Normal skin) 4 Peeling of the stratum corneum is slightly observed. Skin grooves and skin hills are clear. (Relatively beautiful skin) 5 Almost no peeling of the stratum corneum. The crevices and ridges are clear and well-organized. (Beautiful skin)

The results are shown in Table 3. The portion to which the emulsion of the example was applied was significantly improved in roughness compared to the portion to which the emulsion of the comparative example was applied.

[0050]

[Table 3] Example before the start of the evaluation test Comparative example of the emulsion application section Example of the emulsion application section 1 11 0 7 7 2 9 0 7 7 30 7 4 4 0 11 2 5 0 2 First name 0

[Judgment 2. Effect of improving dullness] The amount of melanin and the amount of erythema, which are indicators of dullness, were measured with a megsamer (manufactured by Eurotech Japan Co., Ltd.) on the skin before and after the application of the emulsion and applied for 30 days. The effect of reducing dullness was determined by the following evaluation criteria from the rate of decrease in the amount of melanin and the amount of erythema.

[0052] Score melanin amount and Erisuma amount of reduction rate Remarks 1 10% or more dull improvement dull less than remarkable 25% or more less than 10% dullness improving effect is 3 1% to 5% less dullness improvement weak 4 1% No improvement effect

Table 4 shows the results. The skin to which the emulsion of the Example was applied was clearly improved in terms of dullness as compared with the skin to which the emulsion of the Comparative Example was applied.

[0054]

[Table 4] Evaluation Example Emulsion application part Comparative example Emulsion application part 14 0 0 2 7 2 3 3 8 11 4 1 7

[Judgment 3: Sensory evaluation] With respect to the feeling of use and the effect on the skin, all the subjects were asked about the superiority and inferiority when comparing the example product and the comparative example product. The total result of the answers is as shown in Table 5, and the sensory evaluation confirmed that the effect matched the evaluation result by the device and the excellent feeling of use.

[0056]

[Table 5] Evaluation items Example product is good Comparative example product is good or bad No skin familiarity 13 5 2 Moist 18 18 1 1 Skin stretch 15 3 2 Wrinkle improvement 14 1 person 5 people

Example 2 A cream having the following composition containing the olive leaf extract according to Example 2 of olive branch and leaf extraction was produced by a conventional method for producing cream. Olive leaf extract 2 g setosteryl alcohol 3.5 g squalane 40 g beeswax 3 g reduced lanolin 5 g ethyl paraben 0.3 g POE (20) sorbitan monostearate 2 g glycerin monostearate 2 g 1,3-butylene glycol 5 g flavor 0.03 g glycerin 5g purified water remainder (total amount 100ml)

Example 3 A lotion having the following composition containing the olive leaf extract according to Olive branch and leaf part extraction example 3 was produced by a conventional method of producing a lotion. Olive leaf extract 0.5 g Glycerin 4 g 1,3-butylene glycol 4 g Ethanol 7 g POE (20) sorbitan monooleate 0.5 g Methyl paraben 0.05 g Citric acid 0.01 g Sodium citrate 0.1 g Flavor 0.05 g Purified water The rest (total amount is 100ml)

Example 4 A pack having the following composition containing the olive leaf extract obtained in Example 4 for extracting olive branch and leaves was produced by a conventional method. Olive leaf extract 6 g (0.052 g as solid content) Polyvinyl alcohol 15 g Polyethylene glycol 3 g Propylene glycol 7 g Ethanol 10 g Methyl paraben 0.05 g Perfume 0.05 g Purified water The remainder (total 100 ml)

Example 5 An olive leaf extract prepared according to Example 5 of the olive branch and leaf extract was blended with a bath preparation having the following composition by a conventional method. Olive leaf extract 5 g Sorbitan monolaurate 1 g POE (20) sorbitan monooleate 1.5 g Carboxyvinyl polymer 0.05 g Methyl paraben 0.1 g 1,3-butylene glycol 10 g Denatured alcohol 10 g Perfume Small amount Purified water The remainder (total 100 ml) Do)

Example 6 An emulsion having the following composition was prepared by mixing the olive branch extract according to Example 6 for olive branch extraction. Olive branch extract 10 g (0.067 g as solid content) Cetyl alcohol 0.5 g Beeswax 2 g POE (20) sorbitan monooleate 1 g Glycerin monostearate 1 g Sodium hyaluronate 0.1 g Propylene glycol 5 g Ethanol 3 g Ethyl paraben 0 0.3g Perfume 0.03g Purified water Remainder (total amount is 100ml)

──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. ⁷ Identification symbol FI Theme coat ゛ (Reference) // A61K 35/78 A61K 35/78 C (72) Inventor Shinobu Inohara 14703-10 Mukohigashicho, Onomichi City, Hiroshima Prefecture Within Maruzen Pharmaceutical Co., Ltd. CC04 CC05 CC07 CC25 EE16 EE17 4C088 AB64 AC05 BA09 BA10 BA37 CA02 CA05 CA06 CA11 CA17 ZA89

Claims (2)

[Claims] 1. A skin cosmetic comprising an extract obtained from an olive branch by extraction using water, a hydrophilic organic solvent or a mixture thereof as an extraction solvent. 2. A skin containing an extract obtained from olive branch by extraction using water, methanol, ethanol, 1,3-butylene glycol, propylene glycol or a mixture thereof as an extraction solvent. Cosmetics.