JP2001240527A - Skin-astringent formulation and cosmetics - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a skin-astringent formulation and cosmetic having excellent skin-astringent effect. SOLUTION: The formulation comprises compression filtered materials and/or extracts of cranberry fruits which comprise mainly anthocyanine polymer having molecular weight of 30,000 or more and have anthocyanidine content less than 0.5% by mass without containing caffeic acid glycoside and cosmetics contain compression filtered materials and/or extracts of cranberry fruits which comprise mainly anthocyanine polymer having molecular weight of 30,000 or more and have anthocyanidine content of 0.5% by mass without containing caffeic acid glycoside.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a skin tightening agent and a cosmetic which have an excellent skin tightening effect. More specifically, a skin tightening agent consisting of a pressed and filtered extract and / or extract of cranberry fruit, which is a natural component and has an excellent skin tightening effect, and a cosmetic composition containing the pressed and filtered extract and / or extract About.

[0002]

2. Description of the Related Art Cranberries (Vaccinium m.)
(acrocarpon) is a red-fruited plant that is commonly produced in the United States and is a member of the Japanese name "Tsuruko-kemo". The extract of cranberry has an effect as a therapeutic agent for urinary tract infection, and its application as a whitening agent containing caffeic acid glycoside derived from cranberry or the like as disclosed in JP-A-5-201846. The utility in various fields such as a method for obtaining proanthocyanidins from cranberries as disclosed in JP-A-222484 is known. However, it has not been found that cranberry has a skin tightening effect and that it is effective for cosmetics.

[0003]

On the other hand, components such as green tea and oyster tannin have been used as having a skin tightening effect. However, although these components can provide a feeling of skin, they often have a problem in stability in a formulation, and there is a problem that it is difficult to use. In addition, depending on the type of plant, there were cases where there was concern about the supply side.

[0004]

Means for Solving the Problems The inventors of the present invention have searched for squeezed filtrates and extracts of various plants that can realize the effect of tightening the skin. as a result,
Coincidentally, it has been found that the cranberry squeezed filtrate and extract have a skin tightening effect, and that the squeezed liquid and extract have excellent stability. Furthermore, when purifying and separating the cranberry pressed filtrate or extract, it was found that a stronger feeling of tightening of the skin was obtained. In addition, cranberries are widely used as a food material, and have the advantage that there is no concern about the supply amount.

[0005] That is, a first aspect of the present invention is a skin tightening agent comprising a press-filtered product and / or an extract of cranberry fruit mainly comprising an anthocyanin polymer.

[0006] A second aspect of the present invention is a cosmetic composition comprising a press-filtered and / or an extract of cranberry fruit mainly composed of an anthocyanin polymer.

[0007] A third aspect of the present invention is the above-mentioned skin tightening agent, which comprises a pressed product and / or an extract of cranberry fruit, which is further purified by a gel filtration method or an ultrafiltration method.

[0008] A fourth aspect of the present invention is the above-mentioned cosmetic composition, which further comprises a purified filtered product and / or an extract of cranberry fruit, which is further purified by a gel filtration method or an ultrafiltration method.

A fifth aspect of the present invention is the above-mentioned skin tightening agent, wherein the molecular weight of the anthocyanin polymer is 30,000 or more.

A sixth aspect of the present invention is the above-mentioned cosmetic wherein the molecular weight of the anthocyanin polymer is 30,000 or more.

[0011]

BEST MODE FOR CARRYING OUT THE INVENTION Cranberry (V) used in the present invention
(accinium macrocarpon) is a member of the Japanese name "tsurukokemo" of the azalea family. In the present invention, a cranberry fruit press filtered product is used.The pressed filter product is a juice obtained by crushing and pressing cranberry fruit, or a concentrate thereof. In order to reduce the viscosity of pectin, it is preferable to perform a pectin inactivation treatment. In addition, as an extract of cranberry fruit, cranberry fruit can be obtained by using water, 1,3-butylene glycol, propylene glycol, glycerin,
Polyhydric alcohols such as diglycerin, ethanol, isopropyl alcohol, lower alcohols such as propyl alcohol, solvents such as acetone, their mixed solvents, preferably water, polyhydric alcohols, lower alcohols, their mixed solvents, more preferably, It is an extract obtained by extraction with water such as warm water or hot water, and a concentrate thereof. Examples of the form of the extract include an extract containing a solvent, a solvent-removed product, and the like. In the present invention, it is preferable to use a press-filtrate because the production of the raw material is easy and economical.

The pressed filtered cranberry fruit extract or extract used in the present invention may cause a problem of fading due to light depending on the production conditions. Further, it is preferably purified by a gel filtration method or an ultrafiltration method. As the degree of purification, the content of anthocyanidins in the purified product is reduced to less than 0.5% by mass, preferably less than 0.1% by mass, based on the mass of the purified product having properties to be incorporated into the cosmetic. Preferably. The purified cranberry contains mainly an anthocyanin polymer, and the molecular weight of the polymer is preferably 30,000 or more. It is considered that these components have a skin tightening effect.

As a method of measuring the anthocyanidin content, the following methods can be used. 2g sample
Is taken accurately, 60 mL of 2% methanolic hydrochloric acid is added, and the mixture is heated under reflux on a water bath for 30 minutes, and then cooled. This is 2
% Hydrochloric acid methanol is added to make exactly 100 mL, and the mixture is filtered with filter paper to obtain a test solution. The absorbance at the maximum absorption portion at a wavelength of about 530 nm to 550 nm is measured using 2% hydrochloric acid methanol as a control, and is determined by the following equation. Anthocyanidin content (% by mass) = {absorbance x dilution ratio (100) / sampled amount (g)} x {1/76000}
× 100

Hereinafter, a method for purifying a cranberry fruit press-filtered product or extract used in the present invention will be described. A method for purifying cranberry fruit squeezed filtrate, or extract, is as follows:
Preferably, an ultrafiltration method and a gel filtration method are used. As the membrane used in the ultrafiltration method, a membrane having a cut-off molecular weight of 5,000 to 500,000 is useful, but a membrane having a cut-off molecular weight of 10,000 to 100,000 can obtain good results. Examples of the material of the film include polyethersulfone and regenerated cellulose, and polyethersulfone is preferable. As a filtration method, there are a pressure filtration method using a pump or a centrifuge, a suction filtration method, and the like, but any method may be used.

Gels used in the gel filtration method include Sephadex, Sepharose (above, manufactured by Amersham Pharmacia), Toyopearl (manufactured by Tosoh Corporation), and Biogel (manufactured by Biorat). In addition, various buffers, aqueous organic solvents (methanol, ethanol,
Acetone, acetonitrile, etc.) can be used.

The cosmetics of the present invention include basic cosmetics such as lotions, creams, packs, massages, makeup bases, makeup cosmetics such as foundations, cheek colors, blushers, hair restorations, shampoos, tonics and the like. Examples thereof include hair cosmetics, facial cleansers, body cosmetics, bath additives, and the like. Among them, when applied to cosmetics for tightening the skin, such as makeup bases, it is preferable since makeup collapse can be prevented. In the cosmetic of the present invention, the blended amount (converted to pure content excluding the solvent) of the pressed and filtered cranberry fruit extract is 0.001 to 99.9% by mass based on the cosmetic. And more preferably 0.005 to 15.
% By mass.

In the cosmetic of the present invention, it is preferable to use a combination of the following various extracts in addition to the above-mentioned compressed and / or extracted extract of cranberry fruit. These ingredients have anti-inflammatory action, anti-aging action, tightening action, antioxidant action, hair growth action, hair growth action, moisturizing action, blood circulation promotion action, antibacterial action, bactericidal action, cooling action, warming action,
Effects such as a wound healing accelerating effect, a stimulating alleviating effect, an analgesic effect, a cell activating effect and the like are known, and it is possible to bring out a variety of effects of the preparation. Examples of these components include, for example, Ashitaba extract, Avocado extract, Amacha extract, Altea extract, Arnica extract, Aloe extract, Apricot extract, Apricot kernel extract, Ginkgo extract,
Fennel extract, turmeric extract, oolong tea extract,
Agetsu extract, Gardenia leaf extract, Japanese gourd extract,
Oak extract, spinach extract, barley extract, hypericum perforatum extract, hydrangea extract, dutch mustard extract, orange extract, seawater dried product, seaweed extract,
Hydrolyzed elastin, hydrolyzed wheat powder, hydrolyzed silk, chamomile extract, carrot extract, sagebrush extract, licorice extract, calcade extract, syllium extract,
Kiwi extract, kina extract, cucumber extract, guanosine, gardenia extract, kumazasa extract, clara extract, walnut extract, grapefruit extract, clematis extract, chlorella extract, mulberry extract, gentian extract, tea extract, yeast extract, burdock extract, rice bran fermented extract, rice Germ oil, Comfrey extract, Collagen, Psychic extract, Psychoextract, Saitai extract, Salvia extract, Sabonso extract, Sasa extract, Hawthorn extract, Sansho extract, Shiitake mushroom extract, Jio extract, Shikon extract, Perilla extract, Shinanoki extract, Shimotsusou extract, Peony extract, shobu root extract, birch extract, horsetail extract, vegetative extract, hawthorn extract, elderberry extract, cedar extract Achillea millefolium extract, Common mint extract, Sage extract, Zeniaoi extract, Senkyu extract, Assembly extract, Soybean extract, Tissou extract, Thyme extract, Tea extract, Clove extract, Chigaya extract, Chimpi extract, Touki extract, Tonenkin extract, Spruce extract, Spruce extract, Dokudami extract, tomato extract, natto extract, carrot extract, garlic extract, nobara extract, hibiscus extract, bacmondou extract, parsley extract, honey, hamamelis extract, parietararia extract, chickpea extract, bisabolol, loquat extract, coltsfoot extract,
Fukinotou extract, boukuro extract, butcher bloom extract, grape extract, propolis, loofah extract, safflower extract, peppermint extract, bodaige extract, button extract, hop extract, pine extract, marronnier extract, lycopodium extract, mukuroji extract,
Melissa extract, peach extract, cornflower extract, eucalyptus extract, saxifrage extract, yuzu extract, yokuinin extract, mugwort extract, lavender extract, apple extract, lettuce extract, lemon extract, astragalus extract, rose extract, rosemary extract, roman chamomile extract, royal jelly extract And the like.

The amount of these various extracts and the like in cosmetics (in terms of pure content excluding the extraction solvent) is preferably 0.001 to 30% by mass relative to the cosmetics, and more preferably. 0.005 to 15% by mass.

[0019]

The present invention will be described below in more detail with reference to Examples and Comparative Examples.

Production Example 1 (Production of Purified Cranberry Extract), Example 1 (Lotion) An undiluted juice obtained by pressing and filtering cranberry fruit (manufacturer: MILNE FRUIT PRODUCT, USA)
(Company S, trade name: cranberry concentrate) is purified by ultrafiltration. That is, 10 kg of undiluted cranberry juice was added to Sartorius Sartcon Slice P
Fractionation was carried out using SU-30K (fraction molecular weight 30,000) by pressurization with a pump. 400 g of concentrate is 10
A low-molecular-weight component was removed by washing by adding 400 g of a 5% ethanol solution five times. 1600 g of 10% ethanol was added to the obtained purified cranberry concentrate to obtain a purified cranberry extract. When the anthocyanidin content of this purified cranberry extract was tested by the method described above, 0.0
1% by mass, and the polyphenol content is 0.2%.
% By mass, and the dry residue amount was 2.1% by mass. Further, as a result of analysis under the following conditions by high performance liquid chromatography, no peak of caffeic acid glycoside was detected.

[Method for Analyzing Caffeic Acid Glycoside] Conditions for High-Performance Liquid Chromatography Apparatus: Waters Co., Ltd. Column: Puresil C18 4.6 × 150 mm (Waters Co., Ltd.) Mobile phase: A (0.5%) Phosphoric acid aqueous solution) B (5 parts of phosphoric acid + 295 parts of water + 700 parts of acetonitrile) B10% → 100% (30 minutes) gradient Flow rate: 0.7 mL / min Detector: 996 photodiode array, detection wavelength 200 nm to 600 nm

Further, in order to clarify the difference between the above purified cranberry extract and the known proanthocyanidins disclosed in Japanese Patent No. 2528087 and the like, the following confirmation experiments were conducted.

A UV-Vis spectrum (FIG. 1) of a diluted solution of the purified cranberry extract in citrate buffer (pH 3.0) confirmed that the solution had a maximum absorption at 510 to 520 nm. The property of having an absorption maximum around 520 nm in an acidic solution is a characteristic property of anthocyanins. Confirmation test of anthocyanin Citrate buffer of purified cranberry extract (pH 3.
0) The solution (1 + 100) exhibited a red to dark blue color. When the solution was made alkaline by adding a sodium hydroxide solution (1 + 25) to the solution, it was confirmed that the solution was anthocyanin. From the HPLC chart (FIG. 2), it was confirmed that most of the constituent components were polymers. [HPLC Analysis Conditions] Apparatus: Waters Co. Column: SymmetrySild RP18 5 μm, 4.6 × 150 mm (Waters Co.) Mobile phase: A Phosphoric acid 5 Acetonitrile 100 Water 895 B Phosphoric acid 5 Water 295 Acetonitrile 700 A 100% → B 100% (30 minutes) linear gradient Flow rate: 0.7 mL / min Detector: 996 photodiode array, detection wavelength 200 nm to 600 nm

According to Japanese Patent No. 2528087, proanthocyanidin is a flavan-3-one represented by the following formula 1.
It contains at least one member selected from the group consisting of dimers and octamers combined with all or flavan-3,4-diol as a constituent unit, such as conker shells, cranberry (cranberry) and barley. Of various plant bodies as a raw material using a solvent, and the extract is fractionated and purified by liquid chromatography or the like, or is treated with a selective adsorbent of procyanidin to concentrate the proanthocyanidin fraction. Is stipulated.

[0025]

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Considering the chemical structure of flavan-3,4-diol, the molecular weight of flavan-3,4-diol is 306, and proanthocyanidin is a 2- to 10-mer of flavan-3,4-diol. As a result, the molecular weight was found to be 5000 or less. From these points, it is considered that purified cranberry extract is a compound mainly composed of an anthocyanin polymer having a molecular weight of 30,000 or more, while proanthocyanidin is a compound having a molecular weight of 5,000 or less flavan-3,4-diol or flavan-3-ol. Since it is known that the extract is a condensed tannin as a structural unit, it was found that the extract of the present invention was an anthocyanin polymer, not a known proanthocyanidin, and did not contain proanthocyanidin.

Using the above purified cranberry extract,
According to the formulation of Table 1, the lotion of Example 1 was obtained. The unit of the compounding amount is mass% (the same applies hereinafter).

(Table 1) Ingredients Compounding amount --------------------------------------- --------- Purified cranberry extract 85 1.3 3-butylene glycol 10 Preservatives Appropriate amount Purified water balance

Production Example 2 (Production of Purified Cranberry Extract), Example 2 (Lotion) A hot water extract of cranberries was concentrated under reduced pressure with a rotary evaporator to obtain a 5-fold conch product. To 50 g of this cranberry concentrate, the same amount of 60% ethanol was added and dissolved. This solution was applied to a column (bed volume φ5 × 21 cm) packed with Sephadex LH-20. Using 60% ethanol as the eluate, flow rate 10
Chromatography treatment was performed at 0 mL / hr, and 200 mL fractions were collected. Fr1 to Fr2 fractions were obtained, and Fr9 to Fraction 12 fractions eluted last were concentrated to 40 fractions.
0 g. The resulting purified cranberry extract has an anthocyanidin content of 0.004% by mass, a polyphenol content of 0.06% by mass, and a dry residue of 0.1% by mass.
It was 7% by mass. Further, as a result of analysis by high performance liquid chromatography, no peak of caffeic acid glycoside was detected. Using this purified cranberry extract, a lotion of Example 2 was obtained in the same manner as in Example 1.

Example 3 (Lotion) Instead of the purified cranberry extract of Example 1, the same purified cranberry extract (80% by mass) and a hibiscus extract containing a large amount of organic acids (1,3-butylene glycol extract of flowers, sensitization) A lotion was obtained in the same manner as in Example 1 except that 5% by mass of a source removal type and a dry residue amount of 6% by mass was used.

Comparative Example 1 (Lotion) A lotion was obtained in the same manner as in Example 1 except that the same amount of purified water was used instead of the purified cranberry extract of Example 1.

Comparative Example 2 (Lotion) Instead of the purified cranberry extract of Example 1, a green tea extract (30 parts of green tea) known as a skin tightening component was used.
% Ethanol-water extract, dry residue amount 0.8% by mass) except that the same amount was used to obtain a lotion in the same manner as in Example 1.

The sensory characteristics when the cosmetics of the above Examples and Comparative Examples were applied directly to the skin were evaluated by the following evaluation methods. The evaluation results are shown in Table 3, and the samples were further applied to the half face. The half-face was coated with purified water, and the results of evaluation of the difficulty of makeup collapse when a commercially available foundation was used on the half-face by the following evaluation method are shown in Table 4. Table 5 shows the results of visually evaluating the stability (presence or absence of discoloration) when the samples of Examples and Comparative Examples were stored at room temperature by the window for one month.

The evaluation methods for various properties of the cosmetics of the examples and comparative examples are shown below.

[Skin usefulness evaluation method] Ten specialized panelists were prepared for each evaluation item (however, panelists may be duplicated depending on the item), and evaluation was performed according to the evaluation criteria shown in Table 2, and all panelists were evaluated. The evaluation result was determined based on the total score of the above. Therefore, the higher the score, the higher the usefulness for the evaluation item is shown (full score: 50 points).

[0036]

[0037]

[0038]

[0039]

The results shown in Table 3 were obtained by evaluating the feeling of real skin. It can be seen that each of the examples is more excellent in tightening the skin than the comparative examples. The results in Table 4 show whether the sample tightens the skin and suppresses the secretion of sebum as a result of which the makeup collapse hardly occurs. Each example is superior to each comparative example. Showed the effect. Also,
The results in Table 5 were obtained by evaluating the stability of the preparation. The results of Tables 3 and 4 show that the preparation of Comparative Example 2 which showed relatively excellent performance was also inferior in stability. Understand. Further, in Example 3, a beautiful skin effect of making the skin smooth after continuous use was recognized.

[0041]

From the above, it can be seen that the present invention provides a pressed product of cranberry fruit, which is a natural ingredient, that the extract has an excellent skin tightening effect, and a cosmetic that contains the pressed product, extract. It is clear that the skin tightening effect is excellent and the preparation stability is also excellent.

[Brief description of the drawings]

FIG. 1: Citrate buffer of purified cranberry extract (p
H3.0) is a UV-Vis spectrum diagram of a diluted solution.

FIG. 2 is an HPLC chart of a purified cranberry extract.

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[Procedure amendment]

[Submission date] October 18, 2000 (2000.10.
18)

[Procedure amendment 1]

[Document name to be amended] Statement

[Correction target item name] Claims

[Correction method] Change

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[Claims]

[Procedure amendment 2]

[Document name to be amended] Statement

[Correction target item name] 0005

[Correction method] Change

[Correction contents]

That is, the first present invention relates to an anthocyanin
Gin content of less than 0.5% by mass and containing caffeic acid glycosides
No, mainly anthocyani with a molecular weight of 30,000 or more
Press filtration of fruit cranberries consisting emissions polymers and /
Or a skin tightening agent comprising an extract.

[Procedure amendment 3]

[Document name to be amended] Statement

[Correction target item name] 0006

[Correction method] Change

[Correction contents]

[0006] A second aspect of the present invention relates to anthocyanidin content.
Is less than 0.5% by mass and contains no caffeic acid glycoside,
The present invention relates to a cosmetic composition containing a press-filtered product and / or an extract of cranberry fruits comprising an anthocyanin polymer having a molecular weight of 30,000 or more .

[Procedure amendment 4]

[Document name to be amended] Statement

[Correction target item name] 0007

[Correction method] Change

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According to a third aspect of the present invention, there is provided the skin tightening agent according to claim 1, wherein the press-filtered product and / or the extract of cranberry is a purified product obtained by a gel filtration method or an ultrafiltration method. is there.

[Procedure amendment 5]

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[0008] A fourth invention, pressing filtrate and / or extract of fruit of cranberry is in cosmetic of claim 2 wherein the purified product was purified by gel filtration or ultrafiltration, .

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[Procedure amendment 8]

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[Correction contents]

The pressed filtered cranberry fruit extract or extract used in the present invention may cause a problem of fading due to light depending on the production conditions. Further, it is necessary that the product be purified by gel filtration or ultrafiltration.
You . As the degree of purification, the content of anthocyanidins in the purified product is reduced to less than 0.5% by mass, preferably less than 0.1% by mass, based on the mass of the purified product having properties to be incorporated into the cosmetic. Preferably. Purification of the cranberry is intended primarily containing anthocyanin polymer, the molecular weight of the polymer state, and are more than 30,000, considered that these components result in a tightening effect of skin.

[Procedure amendment 9]

[Document name to be amended] Statement

[Correction target item name] 0014

[Correction method] Change

[Correction contents]

Hereinafter, a method for purifying a cranberry fruit press-filtered product or extract used in the present invention will be described. A method for purifying cranberry fruit squeezed filtrate, or extract, is as follows:
Preferably, an ultrafiltration method and a gel filtration method are used. Fractional molecular weight as membrane used in ultrafiltration 1000
Good results are obtained with films from 0 to 100000.
Examples of the material of the film include polyethersulfone and regenerated cellulose, and polyethersulfone is preferable. Pressure method using a pump or centrifuge as a filtration method,
There is a suction filtration method and the like, but any method may be used.

Continued on the front page (72) Inventor Mika Izawa 335 Karijuku, Hasegawa-Karyo, Nakahara-ku, Kawasaki-shi, Kanagawa Prefecture F-term (reference) 4C083 AA111 AA112 AC122 AD391 BB21 CC02 CC04 DD23 EE12 FF01

Claims (6)

[Claims] 1. A skin tightening agent comprising a press-filtered and / or an extract of cranberry fruit mainly comprising an anthocyanin polymer. 2. A cosmetic composition comprising a press-filtered product and / or an extract of cranberry fruit mainly comprising an anthocyanin polymer. 3. The skin tightening agent according to claim 1, wherein the cranberry berry pressed filtrate and / or extract is further purified by a gel filtration method or an ultrafiltration method. 4. The cosmetic composition according to claim 2, further comprising a purified filtered product and / or extract of cranberry fruit, which is further purified by a gel filtration method or an ultrafiltration method. 5. The molecular weight of the anthocyanin polymer is 300.
4. The skin tightening agent according to claim 3, which is at least 00. 6. The molecular weight of the anthocyanin polymer is 300.
The cosmetic according to claim 4, wherein the cosmetic content is not less than 00.