JP2007261951A - Cosmetic - Google Patents

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JP2007261951A
JP2007261951A JP2006085233A JP2006085233A JP2007261951A JP 2007261951 A JP2007261951 A JP 2007261951A JP 2006085233 A JP2006085233 A JP 2006085233A JP 2006085233 A JP2006085233 A JP 2006085233A JP 2007261951 A JP2007261951 A JP 2007261951A
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hydrophobic mixture
cosmetic
adsorbent
effect
hydrophobic
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JP2007261951A5 (en
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Keiko Watanabe
景子 渡邉
Masatomo Nakano
真知 中野
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Gekkeikan Sake Co Ltd
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Gekkeikan Sake Co Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To solve the problem that especially when a sake is added as a cosmetic, a significant amount of this must be added so as to exhibit various cosmetic functions, and to improve it from both an aspect of cost and an aspect of compositional constitution. <P>SOLUTION: Hydrophobic compositions in the sake are efficiently concentrated in order to obtain the cosmetic with high effects of improving skin/antioxidant effectiveness/whitening effectiveness and a manufacturing method thereof. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

本発明は米発酵液に吸着剤を添加・回収し、該吸着剤から疎水性混合物を抽出する方法に関し、特に該疎水性混合物を原料とした化粧料およびその製造方法に関するものである。 The present invention relates to a method for adding and recovering an adsorbent to a rice fermentation broth and extracting a hydrophobic mixture from the adsorbent, and more particularly to a cosmetic using the hydrophobic mixture as a raw material and a method for producing the same.

清酒、ワインなどの醸造酒には原料由来の様々な有効成分が含まれるのみならず、酵母・麹菌・乳酸菌などの代謝物が大量に含まれており、皮膚に塗布することにより肌の保湿・つや・張りなどを向上させる効果があることは古くから知られている。特に清酒に関してはその特徴を生かした化粧品が種々存在する。 Brewed sake such as sake and wine contains not only various active ingredients derived from raw materials, but also contains a large amount of metabolites such as yeast, koji molds, and lactic acid bacteria. It has been known for a long time that it has the effect of improving gloss and tension. Especially for sake, there are various cosmetics that take advantage of its characteristics.

特開平6−199679には米発酵物、特に清酒生産副産物である酒粕から得られる有機溶媒可溶物に、チロシナーゼ活性阻害効果があることが開示されている。また、特開2001−106610には発酵酒に含まれるアルデヒド類、ケトン類、有機酸類等を活性炭により吸着除去した活性炭処理発酵酒を含有することを特徴とする発酵酒からなる化粧料の製造方法が開示されている。一方、特開2004−248592には、蒸留酒である黒糖焼酎の蒸留残渣を吸着剤に接触させてチロシナーゼ活性阻害剤を回収する方法について開示されている。   Japanese Patent Laid-Open No. Hei 6-199679 discloses that an organic solvent soluble material obtained from fermented rice, particularly sake lees, which is a by-product of sake production, has an inhibitory effect on tyrosinase activity. Japanese Patent Application Laid-Open No. 2001-106610 includes a method for producing a cosmetic comprising fermented liquor, comprising activated charcoal-treated fermented liquor obtained by adsorbing and removing aldehydes, ketones, organic acids and the like contained in fermented liquor by activated carbon. Is disclosed. On the other hand, Japanese Patent Application Laid-Open No. 2004-245852 discloses a method for recovering a tyrosinase activity inhibitor by bringing a distillation residue of brown sugar shochu, which is distilled liquor, into contact with an adsorbent.

特開平6−199679号公報Japanese Patent Laid-Open No. 6-199679 特開2001−106610号公報JP 2001-106610 A 特開2004−248592号公報JP 2004-2458592 A

しかしながら特許文献1に開示の方法は清酒副産物である酒粕をエタノールで懸濁することにより、原料由来あるいは発酵中に不溶化した成分を回収するものであり、従来知られている酒粕の美容効果物質を濃縮したものであると考えられる。
また、特許文献2に開示の方法は清酒中に含まれる成分をやしがら活性炭により吸着させたものであるが、これら吸着成分はアルデヒド類、ケトン類、有機酸類等の刺激物質であるとしており、化粧料として有効な部分はこれら吸着成分を取り除いた活性炭処理清酒であることが示されている。
さらに特許文献3に開示の方法は蒸留酒である黒糖焼酎の蒸留粕から特許文献1に類似の方法で活性炭に有効成分を吸着させる方法であるが、清酒とは異なり蒸留粕は長時間の加熱によって本来もろみ中に存在しなかった化合物が形成されている可能性が高い。
このように発酵酒である清酒に美容効果があることは知られていたが、その有効成分は清酒粕あるいは清酒中の活性炭非吸着画分に存在すると考えられてきており、成分本体についてはいまだ明確になっていない。
すなわち、特に清酒を化粧料として添加する際、各種美容機能を発揮させるには相当程度添加しなければならず、コストの面からも組成構成上の面からも改善が求められてきた。
本発明はかかる問題点に鑑みてなされたものであり、清酒中に含まれる疎水性組成物を効率よく濃縮し、皮膚改善効果・抗酸化効果・美白効果の高い化粧料およびその製造方法を提供しようとするものである。
However, the method disclosed in Patent Document 1 recovers components derived from raw materials or insolubilized during fermentation by suspending sake lees, which are by-products of sake, with ethanol. It is thought to be concentrated.
In addition, the method disclosed in Patent Document 2 is a method in which components contained in sake are adsorbed by activated carbon, but these adsorbed components are stimulating substances such as aldehydes, ketones and organic acids. It has been shown that the part effective as a cosmetic is activated charcoal-treated sake from which these adsorbing components have been removed.
Further, the method disclosed in Patent Document 3 is a method in which an active ingredient is adsorbed on activated carbon by a method similar to Patent Document 1 from a distilled spirit of brown sugar shochu, which is a distilled liquor. Unlike sake, a distilled spirit is heated for a long time. Therefore, it is highly possible that a compound originally not present in the mash is formed.
It was known that sake, a fermented liquor, has a cosmetic effect, but its active ingredients are thought to exist in the sake lees or the non-adsorbed fraction of activated carbon in sake. It is not clear.
That is, particularly when sake is added as a cosmetic, it must be added to a considerable extent in order to exhibit various beauty functions, and improvements have been demanded from the standpoint of cost and composition.
The present invention has been made in view of such problems, and efficiently concentrates a hydrophobic composition contained in sake to provide a cosmetic having a high skin improvement effect, antioxidant effect, and whitening effect, and a method for producing the same. It is something to try.

上記課題を解決するため本発明者は研究を重ねた結果、米発酵液に吸着剤を添加し、回収した吸着剤に極性溶媒又は非極性溶媒(例えば、クロロホルム、メタノール、又はその混合物、ヘキサン、アセトンなど)を吸着剤量の2〜10倍量添加して撹拌した後に濾過などにより吸着剤を除去して得られる疎水性混合物には、以下のような効果があるという知見が得られた。
(1)保水性試験の結果、1.6%疎水性混合物は市販セラミドよりも優れた水分保持率を示した。このことから疎水性混合物は化粧品の保湿成分として優れた効果が見られ、十分な肌の保湿効果が期待できる。
(2)閉塞性試験を行うために、疎水性混合物、市販乳液、水のいずれかを塗布したフィルターを装着したバイアル瓶に水5mlを入れ、1時間後の水分蒸散量を測定したところ、疎水性混合物は市販乳液と同程度に水分蒸散を抑制した。このことからも疎水性混合物は化粧品の保湿成分として優れた効果が見られ、十分な肌の保湿効果が期待できる。
(3)抗酸化試験の結果、疎水性混合物の抗酸化力は米発酵液の180倍であり、抗酸化物質として知られるフェルラ酸と比較した場合、1%フェルラ酸と同程度であった。このことから、疎水性混合物は酸化防止やフリーラジカル発生防止などの効果も期待できる。
(4)チロシナーゼ阻害活性を測定したところ、疎水性混合物のチロシナーゼ阻害活性は米発酵液の約900倍であった。さらにアルブチンと比較したところ、疎水性混合物の阻害活性は0.3%アルブチンに相当した。このことから疎水性混合物は美白成分としての効果も期待できる。
本発明は上記知見に基づき完成されたものであり、以下の疎水性混合物、および化粧料などを提供する。
項1. 米発酵液に添加した吸着剤を回収し、該吸着剤から溶媒で抽出した物からなる疎水性混合物。
項2. 吸着剤が木粉および/または素灰を原料とする活性炭である項1に記載の疎水性混合物。
項3. 吸着剤が樹脂である項1に記載の疎水性混合物。
項4. 溶媒が極性溶媒である項1に記載の疎水性混合物。
項5. 溶媒が非極性溶媒である項1に記載の疎水性混合物。
項6. 項1から5に記載の疎水性混合物を含んでなる化粧料。
項7. 皮膚改善効果、抗酸化効果、美白効果のうち少なくとも一つの機能を有する項6に記載の化粧料。
項8. 皮膚改善効果が保水性の向上および/または閉塞性の向上である項7に記載の化粧料。
項9. 抗酸化効果が酸化防止および/またはフリーラジカル発生予防である項7に記載の化粧料。
項10. 美白効果がチロシナーゼ阻害活性および/またはメラニン分解活性によるものである項7に記載の化粧料。
In order to solve the above-mentioned problems, the present inventor has repeatedly studied to add an adsorbent to the rice fermentation broth, and to the recovered adsorbent, a polar solvent or a nonpolar solvent (for example, chloroform, methanol, or a mixture thereof, hexane, It was found that a hydrophobic mixture obtained by adding 2 to 10 times the amount of adsorbent and stirring the mixture after removing the adsorbent by filtration or the like has the following effects.
(1) As a result of the water retention test, the 1.6% hydrophobic mixture showed a moisture retention rate superior to that of the commercially available ceramide. From this, the hydrophobic mixture has an excellent effect as a moisturizing component of cosmetics, and a sufficient skin moisturizing effect can be expected.
(2) In order to conduct an occlusive test, 5 ml of water was put into a vial equipped with a filter coated with a hydrophobic mixture, a commercial emulsion, or water, and the amount of water transpiration after 1 hour was measured. The sex mixture suppressed water transpiration to the same extent as commercial emulsions. Also from this fact, the hydrophobic mixture shows an excellent effect as a moisturizing component for cosmetics, and a sufficient skin moisturizing effect can be expected.
(3) As a result of the antioxidant test, the antioxidant power of the hydrophobic mixture was 180 times that of the rice fermentation broth, and was comparable to 1% ferulic acid when compared with ferulic acid known as an antioxidant. From this, the hydrophobic mixture can be expected to have effects such as prevention of oxidation and generation of free radicals.
(4) When tyrosinase inhibitory activity was measured, the tyrosinase inhibitory activity of the hydrophobic mixture was about 900 times that of the rice fermentation broth. Furthermore, when compared with arbutin, the inhibitory activity of the hydrophobic mixture was equivalent to 0.3% arbutin. From this, the hydrophobic mixture can also be expected to have an effect as a whitening component.
The present invention has been completed based on the above findings, and provides the following hydrophobic mixture, cosmetics and the like.
Item 1. The hydrophobic mixture which consists of the thing which collect | recovered the adsorbent added to the rice fermentation liquor, and extracted with the solvent from this adsorbent.
Item 2. Item 2. The hydrophobic mixture according to Item 1, wherein the adsorbent is activated carbon made from wood flour and / or raw ash.
Item 3. Item 2. The hydrophobic mixture according to Item 1, wherein the adsorbent is a resin.
Item 4. Item 2. The hydrophobic mixture according to Item 1, wherein the solvent is a polar solvent.
Item 5. Item 2. The hydrophobic mixture according to Item 1, wherein the solvent is a nonpolar solvent.
Item 6. Item 6. A cosmetic comprising the hydrophobic mixture according to Item 1 to 5.
Item 7. Item 7. The cosmetic according to Item 6, which has at least one of a skin improvement effect, an antioxidant effect, and a whitening effect.
Item 8. Item 8. The cosmetic according to Item 7, wherein the skin improvement effect is an improvement in water retention and / or an improvement in occlusion.
Item 9. Item 8. The cosmetic according to Item 7, wherein the antioxidant effect is prevention of oxidation and / or prevention of free radical generation.
Item 10. Item 8. The cosmetic according to Item 7, wherein the whitening effect is due to tyrosinase inhibitory activity and / or melanolytic activity.

米発酵液に活性炭、シリカゲルなどの吸着剤を加えて攪拌し、吸着剤に吸着した成分を有機溶媒で抽出した米発酵液由来疎水性混合物は、保湿性、閉塞性、抗酸化性、チロシナーゼ阻害作用といった多様な機能をもち、従来の米発酵液とは異なる新しい化粧料として利用できる。
また当該原料は化粧料に求められる多種類の機能性(保湿性、閉塞性、抗酸化性、チロシナーゼ阻害作用)を併せ持つことから、天然素材由来の優れた化粧料として利用することができる。
Rice fermentation broth-derived hydrophobic mixture obtained by adding adsorbents such as activated carbon and silica gel to rice fermentation broth and stirring and extracting the components adsorbed on the adsorbent with organic solvent is moisturizing, occlusive, antioxidant, tyrosinase inhibition It has various functions such as action and can be used as a new cosmetic different from conventional rice fermentation broth.
In addition, since the raw materials have various functions (humidity retention, occlusiveness, antioxidant properties, tyrosinase inhibitory action) required for cosmetics, they can be used as excellent cosmetics derived from natural materials.

以下、本発明を詳細に説明する。
(1)米発酵液
本発明における米発酵液は蒸米に水・米麹・酵母を添加して発酵させた発酵もろみを圧搾濾過などの方法により固液分離して得られる清澄な液体をいう。蒸米の原料となる米は特に限定されるものではなく、日本産米はもとよりタイ米を始めとする海外産米でもよい。また、米は玄米、精白米のいずれでもよく、赤糠あるいは白糠を原料としてもよい。米麹はもろみの発酵に必要な量を添加すればよく、場合によってはグルコアミラーゼなどの酵素剤によって代替してもよい。酵母は清酒酵母を使用するのが好ましいが、場合によっては実験室酵母・組換え酵母など特定の機能を付与した酵母を使用してもよい。
固液分離方法は一般的な圧搾式濾過を使用してもよく、連続遠心分離を使用してもよい。
(2)吸着剤
本発明で使用する吸着剤は活性炭、シリカゲル、スチレン系吸着剤、のほか陰イオン交換樹脂、陽イオン交換樹脂のほか珪藻土、ゼオライト、合成ポリマーなどの多孔性の物質であればよいが、清酒製造の工程を鑑みると活性炭であることが好ましい。
活性炭の種類は特に限定されるものではないが、醸造用資材として認定されている木粉あるいは素灰を原料とするものが好ましい。活性炭の賦活方法としては塩化亜鉛または水蒸気による賦活された塩化亜鉛炭または水蒸気炭が好ましい。形状は特に限定されないが、効率的な抽出を行う観点からは微粉末であることが好ましく、作業上の取り扱い性の観点からは粒状であることが好ましい。
(3)吸着剤からの疎水性混合物抽出方法
吸着剤に吸着された清酒に含有される疎水性混合物の抽出には極性溶媒または非極性溶媒、およびその混合物を用いればよいが、例としてはメタノール、エタノール、プロパノール、ブタノール、プロピレングリコール、ブチレングリコール、グリセリン等のアルコール類や、アセトン、アセトニトリル、ヘキサン、クロロホルム等が挙げられる。
(4)疎水性混合物の形状
疎水性混合物は液状そのままで使用してもよいが、必要に応じて凍結乾燥、噴霧乾燥、濃縮乾固などの方法により粉末化・濃縮を行ってもよい。
(5)製造方法
本発明の化粧料は本発明により得られる疎水性混合物を既存の化粧料組成物に添加することで製造できる。化粧料組成物の剤型は任意であり、カプセル状、粉末状、顆粒状、固形状、液状、ゲル状、気泡状、乳液状、クリーム状、軟膏状、シート状、ムース状、粉末分散状、多層状、エアゾール状等の剤型を成す。具体的には、化粧水、美容液、美白化粧水、乳液、美白乳液、クリーム、美白クリーム、軟膏、美白軟膏、ローション、美白ローション、オイル、パック等の基礎化粧料、石鹸、クレンジングクリーム、クレンジングローション、クレンジングミルク、洗顔料等の皮膚洗浄料、ファンデーション、白粉、おしろい、口紅、頬紅、アイシャドウ、アイライナー等のメークアップ化粧料、浴用剤等が挙げられる。また化粧料組成物中に含有される疎水性混合物の含有量としては、組成物全量中、0.0001質量%以上の濃度範囲で使用されるのが一般的であり、好ましくは0.01〜50.0質量%の、特に好ましくは0.1〜20質量%が化粧品組成物を構成する上で期待される美容効果の発現の点から有効である。
本発明の美白剤を用いて構成される化粧料組成物には、必須成分である前記化合物に加え、更に下記に例示する色素沈着抑制剤、チロシナーゼ活性阻害剤、メラノサイトメラニン生成抑制剤、保湿剤、細胞賦活剤/代謝活性化剤、抗酸化剤、活性酸素消去剤/ラジカル生成抑制剤、脂肪代謝促進剤、紫外線防御剤/紫外線吸収促進剤、収斂剤、抗炎症剤/インターロイキン産生抑制剤/消炎剤、抗脂漏剤、抗菌剤/抗ウイルス剤、血流促進剤/血管刺激剤、抗アンドロゲン剤、構造タンパク質分解酵素(エラスターゼ、コラゲナーゼ、ケラチンプロテアーゼ、セリンプロテアーゼ、インテグリン分解酵素、インボルクリン分解酵素、フィラグリン分解酵素、ラミニン分解酵素、フィブロネクチン分解酵素、プロテオグリカン分解酵素等)活性阻害剤、構造タンパク質合成促進剤、ムコ多糖類(ヒアルロン酸、コンドロイチン硫酸等)分解酵素阻害剤、ムコ多糖類合成促進剤、細胞間脂質生成促進剤/細胞間脂質状態改善剤、角質溶解剤/角層剥離促進剤、プラスミノーゲンアクチベーター拮抗阻害剤、メイラード反応阻害剤、テストステロン5αレダクターゼ活性阻害剤/毛乳頭活性化剤/発毛促進剤、毛母細胞増殖抑制剤/発毛抑制剤、毛髪膨潤剤/毛髪保護剤、有臭物質消去剤等の有効成分や、その他に化粧料組成物の形態を形成する上で使用が好まれる植物系原料、動物系原料、微生物系原料、その他天然物原料等を由来とするエキスや代謝物等成分、又は種々の化合物を添加剤として任意に選択並びに併用することにより、更に多種の機能性を有する優れた化粧料組成物を提供できる。製剤中における含有量は、特に規定しないが、通常、0.0001〜50質量%の濃度範囲が一般的である。
Hereinafter, the present invention will be described in detail.
(1) Rice fermented liquid The rice fermented liquid in the present invention refers to a clear liquid obtained by solid-liquid separation of fermented mash that has been fermented by adding water, rice bran, or yeast to steamed rice. The rice used as the raw material for the steamed rice is not particularly limited, and may be Japanese rice as well as overseas rice such as Thai rice. The rice may be brown rice or polished rice, and red rice bran or white rice bran may be used as a raw material. Rice bran may be added in an amount necessary for fermentation of moromi, and may be replaced by an enzyme agent such as glucoamylase in some cases. As the yeast, sake yeast is preferably used, but in some cases, yeast having a specific function such as laboratory yeast or recombinant yeast may be used.
The solid-liquid separation method may use general squeeze filtration or continuous centrifugation.
(2) Adsorbent If the adsorbent used in the present invention is a porous substance such as activated carbon, silica gel, styrene-based adsorbent, anion exchange resin, cation exchange resin, diatomaceous earth, zeolite, or synthetic polymer. Although it is good, it is preferably activated carbon in view of the sake production process.
The type of the activated carbon is not particularly limited, but is preferably made of wood flour or raw ash that is certified as a brewing material. The activated carbon activation method is preferably zinc chloride charcoal or steam charcoal activated with zinc chloride or water vapor. The shape is not particularly limited, but is preferably a fine powder from the viewpoint of efficient extraction, and is preferably granular from the viewpoint of workability during work.
(3) Hydrophobic mixture extraction method from adsorbent A polar solvent or nonpolar solvent and a mixture thereof may be used for extraction of the hydrophobic mixture contained in sake adsorbed on the adsorbent. , Ethanol, propanol, butanol, propylene glycol, butylene glycol, glycerin and other alcohols, acetone, acetonitrile, hexane, chloroform and the like.
(4) Shape of the hydrophobic mixture The hydrophobic mixture may be used as it is, but may be pulverized and concentrated by freeze drying, spray drying, concentration to dryness, or the like, if necessary.
(5) Manufacturing method The cosmetics of this invention can be manufactured by adding the hydrophobic mixture obtained by this invention to the existing cosmetics composition. The dosage form of the cosmetic composition is arbitrary, and it is a capsule, powder, granule, solid, liquid, gel, foam, emulsion, cream, ointment, sheet, mousse, powder dispersion It forms dosage forms such as multilayers and aerosols. Specifically, skin lotion, essence, whitening lotion, milk, whitening milk, cream, whitening cream, ointment, whitening ointment, lotion, whitening lotion, oil, pack and other basic cosmetics, soap, cleansing cream, cleansing Examples include skin cleansing agents such as lotions, cleansing milks, and facial cleansers, foundations, white powders, white powders, makeup cosmetics such as lipsticks, blushers, eye shadows, and eyeliners, and bath preparations. The content of the hydrophobic mixture contained in the cosmetic composition is generally used in a concentration range of 0.0001% by mass or more, preferably 0.01 to 50.0% by mass in the total amount of the composition. Particularly preferably, 0.1 to 20% by mass is effective from the viewpoint of expression of a cosmetic effect expected in constituting a cosmetic composition.
In addition to the above-mentioned compounds that are essential components, the cosmetic composition constituted using the whitening agent of the present invention further includes a pigmentation inhibitor, a tyrosinase activity inhibitor, a melanocyte melanin production inhibitor, and a humectant exemplified below. , Cell activator / metabolic activator, antioxidant, active oxygen scavenger / radical production inhibitor, fat metabolism promoter, UV protection agent / UV absorption promoter, astringent, anti-inflammatory agent / interleukin production inhibitor / Antiinflammatory agent, Antiseborrheic agent, Antibacterial agent / Antiviral agent, Blood flow promoter / Vessel stimulant, Antiandrogen agent, Structural proteolytic enzyme (elastase, collagenase, keratin protease, serine protease, integrin degrading enzyme, involucrin degradation Enzyme, filaggrin degrading enzyme, laminin degrading enzyme, fibronectin degrading enzyme, proteoglycan degrading enzyme, etc.) Harmful agents, structural protein synthesis promoters, mucopolysaccharide (hyaluronic acid, chondroitin sulfate, etc.) degrading enzyme inhibitors, mucopolysaccharide synthesis promoters, intercellular adipogenesis promoters / intercellular lipid state improvers, keratolytic agents / Stratum corneum peeling promoter, plasminogen activator antagonist inhibitor, Maillard reaction inhibitor, testosterone 5α reductase activity inhibitor / hair papilla activator / hair growth promoter, hair matrix cell growth inhibitor / hair growth inhibitor, Active ingredients such as hair swelling agents / hair protecting agents, odorous substance erasing agents, and other plant-based materials, animal-based materials, microbial-based materials, and other natural materials that are preferred for use in forming cosmetic composition forms It is possible to provide an excellent cosmetic composition having various functions by arbitrarily selecting and using ingredients such as extracts and metabolites derived from raw materials, etc., or various compounds as additives. Can be provided. The content in the preparation is not particularly defined, but usually a concentration range of 0.0001 to 50% by mass is common.

以下、実施例を示して本発明をより詳細に説明するが、本発明はこれらの実施例に限定されるものではない。   EXAMPLES Hereinafter, although an Example is shown and this invention is demonstrated in detail, this invention is not limited to these Examples.

疎水性混合物の製造方法
清酒500lに活性炭(武田キリン食品株式会社製、吟撰白鷺50W)500gを添加後、攪拌して疎水性成分を吸着させ、撹拌しながら移送ポンプにより加圧濾過機へ注入し、約2000ml/分の濾過速度により循環濾過した。これにより清酒に含まれる疎水性混合物が活性炭に吸着濃縮される。循環される清酒が無色になった時点で濾過を終了し、活性炭を回収した。この活性炭に極性溶媒(クロロホルム:メタノール=2:1)を3l添加して攪拌した後ろ過し、活性炭を除去して、溶媒抽出物を含む極性溶媒を得た。これをロータリーエバポレーターにて溶媒を除去し、疎水性混合物約20gを得た。疎水性混合物は常温では固体と液体の混合物であるが、各種試験に使用する際は50℃に加熱し、均一な液体として使用した。
Method for producing hydrophobic mixture After adding 500 g of activated carbon (Takeda Kirin Foods Co., Ltd., Ginjo Hakuho 50 W) to 500 liters of sake, the mixture is stirred to adsorb hydrophobic components and injected into a pressure filter with a transfer pump while stirring. And circulatingly filtered at a filtration rate of about 2000 ml / min. As a result, the hydrophobic mixture contained in the sake is adsorbed and concentrated on the activated carbon. When the circulated sake became colorless, the filtration was terminated and the activated carbon was recovered. 3 l of a polar solvent (chloroform: methanol = 2: 1) was added to the activated carbon and stirred, followed by filtration to remove the activated carbon to obtain a polar solvent containing a solvent extract. The solvent was removed using a rotary evaporator to obtain about 20 g of a hydrophobic mixture. The hydrophobic mixture is a mixture of a solid and a liquid at normal temperature, but when used in various tests, it was heated to 50 ° C. and used as a uniform liquid.

保水性試験
疎水性混合物の保水性を検討した。比較の対照として、米由来のセラミドを使用した。疎水性混合物およびセラミドは水への溶解性が低いため、それぞれの乳化液を作成した。乳化液の組成は表1の通りである。
Water retention test The water retention of the hydrophobic mixture was examined. As a control for comparison, ceramide derived from rice was used. Since the hydrophobic mixture and ceramide have low solubility in water, respective emulsions were prepared. The composition of the emulsion is as shown in Table 1.

Figure 2007261951
Figure 2007261951

これを恒温恒湿器中で40℃、湿度40%の水分条件下で放置し、24時間後の重量を計測することにより水分保持率を測定した結果を図1に示す。
対照(疎水性混合物、セラミドともに不含)の水分保持率を1として比較すると、1.6%の疎水性混合物を使用した場合、水分保持率は1.1を上回っていた。すなわち1.6%の疎水性混合物添加により1割以上の水分保持率向上効果が認められた。また、比較のために用いた市販セラミドの場合よりも高い値を示した。
FIG. 1 shows the result of measuring the moisture retention rate by leaving this in a constant temperature and humidity chamber under a moisture condition of 40 ° C. and a humidity of 40% and measuring the weight after 24 hours.
When the moisture retention of the control (containing neither hydrophobic mixture nor ceramide) was compared with 1, the moisture retention was higher than 1.1 when 1.6% hydrophobic mixture was used. That is, the moisture retention improvement effect of 10% or more was recognized by adding 1.6% of the hydrophobic mixture. Moreover, the value higher than the case of the commercially available ceramide used for the comparison was shown.

閉塞性試験
疎水性混合物との比較には水および乳液を用いた。乳液は市販の乳液(月桂冠株式会社製;主成分:水、スクワラン、エタノール、グリセリン)を用いた。
バイアル瓶(10ml容)に水5mlを入れ、穴を開けたキャップの内側にサンプルまたは水50μlを塗布したフィルター(ミリポア製、ポアサイズ0.45μm)を装着し、室温24℃、湿度27%の状態で放置し、1〜3時間後の水分蒸散量をTewameter TM300(Integral社製)で測定した結果を図2に示す。
実験開始後1〜3時間において、水を塗布したフィルターを使用した場合の水分蒸散量が約16.7〜18.6g/hmであったのに対し、疎水性混合物を用いた場合の水分蒸散量は9.35〜9.70g/hmであった。
一方、市販の乳液を使用した場合の水分蒸散量は11.3〜13.0であり、試験期間を通じて疎水性混合物は乳液を上回る閉塞性を示した。
この結果から、疎水性混合物の皮膚からの水分の蒸発を抑える水分保持能力が期待できる。
Occlusion test Water and emulsion were used for comparison with the hydrophobic mixture. As the emulsion, a commercially available emulsion (manufactured by Laurel Wreath Co., Ltd .; main components: water, squalane, ethanol, glycerin) was used.
Place 5 ml of water in a vial (10 ml), and install a filter (Millipore, pore size 0.45 μm) coated with 50 μl of sample or water inside the holed cap, at room temperature of 24 ° C. and humidity of 27% FIG. 2 shows the results of measuring the amount of water transpiration after 1 to 3 hours using a Tewmeter TM300 (manufactured by Integral).
In the first to third hours after the start of the experiment, the moisture transpiration when using a filter coated with water was about 16.7 to 18.6 g / hm 2 , whereas the moisture when using a hydrophobic mixture transpiration rate was 9.35~9.70g / hm 2.
On the other hand, the amount of water transpiration when using a commercially available emulsion was 11.3 to 13.0, and the hydrophobic mixture showed an occlusive property exceeding that of the emulsion throughout the test period.
From this result, it is possible to expect a moisture retention ability that suppresses evaporation of moisture from the skin of the hydrophobic mixture.

抗酸化性試験
抗酸化力の測定はDPPH(1、1−Diphenyl−2−picrylhydrazyl)法を用い、疎水性混合物の抗酸化力を米発酵液(月桂冠株式会社製、純米酒)、フェルラ酸(和光純薬製)と比較した。フェルラ酸は米糠に含まれている生理活性成分で、抗酸化効果があり、フリーラジカルの発生を防ぐため、化粧品に配合されている成分の一つである。
DPPH法による抗酸化性試験は次のようにして行った。50%アルコール2mlに、疎水性混合物または米発酵液、フェルラ酸のいずれかと水を合わせて0.5mlにし、これに2M酢酸バッファー(pH5.0)を0.2ml、1mM DPPHを0.3ml加えたものを30分間暗所に置き、OD520を測定した。
疎水性混合物、米発酵液、フェルラ酸の濃度を変えて測定し、その値からそれぞれのIC50を求めた結果を表2に示す。
Antioxidant Test Antioxidant power was measured using DPPH (1,1-Diphenyl-2-picrylhydrazyl) method, and the antioxidant power of the hydrophobic mixture was measured using rice fermented liquid (manufactured by Gekkeikan Co., Ltd., pure rice sake), ferulic acid ( Wako Pure Chemical). Ferulic acid is a physiologically active ingredient contained in rice bran and has an antioxidant effect and is one of the ingredients blended in cosmetics to prevent the generation of free radicals.
The antioxidant test by the DPPH method was performed as follows. Add 2 ml of 50% alcohol to 0.5 ml of either hydrophobic mixture or rice fermentation liquid, ferulic acid and water, and add 0.2 ml of 2M acetate buffer (pH 5.0) and 0.3 ml of 1 mM DPPH. Was placed in the dark for 30 minutes, and OD 520 was measured.
Table 2 shows the results obtained by measuring each of the hydrophobic mixture, the rice fermentation broth, and ferulic acid at different concentrations, and calculating the respective IC 50 values from the measured values.

Figure 2007261951
Figure 2007261951

その結果、疎水性混合物は抗酸化性を有し、抗酸化力は1%フェルラ酸とほぼ同等の抗酸化性を示した。また、米発酵液の抗酸化性は疎水性混合物の約1/180であった。このことから疎水性混合物は、米発酵液中の抗酸化成分が本発明の処理により効果的に抽出・濃縮されたことが示された。   As a result, the hydrophobic mixture had antioxidant properties, and the antioxidant power was almost the same as 1% ferulic acid. Moreover, the antioxidant property of the rice fermentation broth was about 1/180 of the hydrophobic mixture. From this, it was shown that the hydrophobic mixture effectively extracted and concentrated the antioxidant component in the rice fermentation broth by the treatment of the present invention.

チロシナーゼ活性阻害試験
疎水性混合物または米発酵液、α−アルブチン(江崎グリコ株式会社製)のチロシナーゼ活性阻害効果を比較した。α−アルブチンは、美白効果物質としてよく知られているβ−アルブチンを上回るチロシナーゼ活性阻害効果を示すことが知られている。
Tyrosinase activity inhibition test The tyrosinase activity inhibitory effect of a hydrophobic mixture or rice fermentation broth, α-arbutin (manufactured by Ezaki Glico Co., Ltd.) was compared. α-Arbutin is known to exhibit a tyrosinase activity inhibitory effect that exceeds β-arbutin, which is well known as a whitening effect substance.

チロシナーゼ活性阻害試験は次のようにして測定した。1Mリン酸バッファー(pH6.0)150μlに1mMチロシン(0.01N HCl)150μlとチロシナーゼ(150u/ml;麹菌由来)10μlを加え、これに水と試験溶液(疎水性混合物または米発酵液、アルブチン)を合わせた2.7mlを加え、直ちにOD475を経時的に測定し、チロシナーゼ活性阻害率が50%となるサンプル濃度をIC50とした。その結果を表3に示す。 The tyrosinase activity inhibition test was measured as follows. Add 150 μl of 1 mM tyrosine (0.01N HCl) and 10 μl of tyrosinase (150 u / ml; derived from Aspergillus) to 150 μl of 1M phosphate buffer (pH 6.0), and add water and test solution (hydrophobic mixture or rice fermentation broth, arbutin) ) the 2.7ml of the combined added, immediately measured over time OD 475, was sample concentration tyrosinase activity inhibition rate is 50% and the IC 50. The results are shown in Table 3.

Figure 2007261951
Figure 2007261951

疎水性混合物は、米発酵液と比較して著しく高いチロシナーゼ活性阻害効果を示した(900倍以上)。この阻害活性は、0.3%アルブチンの阻害活性に相当した。このことから疎水性混合物は、米発酵液中のチロシナーゼ活性阻害成分が本発明の処理により効果的に抽出・濃縮されたことが示された。   The hydrophobic mixture showed an extremely high tyrosinase activity inhibitory effect (900 times or more) compared to the rice fermentation broth. This inhibitory activity corresponded to the inhibitory activity of 0.3% arbutin. From this, it was shown that the hydrophobic mixture effectively extracted and concentrated the tyrosinase activity inhibitory component in the rice fermentation broth by the treatment of the present invention.

米発酵液由来疎水性混合物とセラミドの保湿性を比較した図である。It is the figure which compared the moisture retention of the hydrophobic mixture derived from a rice fermentation liquid, and ceramide. 水と米発酵液由来疎水性混合物と市販乳液の閉塞性を比較した図である。It is the figure which compared the obstruction | occlusion property of the hydrophobic mixture derived from water and a rice fermentation liquid, and a commercially available emulsion.

Claims (10)

米発酵液に添加した吸着剤を回収し、該吸着剤から溶媒で抽出した物からなる疎水性混合物。 The hydrophobic mixture which consists of the thing which collect | recovered the adsorbent added to the rice fermentation liquid, and extracted with the solvent from this adsorbent. 吸着剤が木粉および/または素灰を原料とする活性炭である請求項1に記載の疎水性混合物。 The hydrophobic mixture according to claim 1, wherein the adsorbent is activated carbon made from wood flour and / or raw ash. 吸着剤が樹脂である請求項1に記載の疎水性混合物。 The hydrophobic mixture according to claim 1, wherein the adsorbent is a resin. 溶媒が極性溶媒である請求項1に記載の疎水性混合物。 The hydrophobic mixture according to claim 1, wherein the solvent is a polar solvent. 溶媒が非極性溶媒である請求項1に記載の疎水性混合物。 The hydrophobic mixture according to claim 1, wherein the solvent is a nonpolar solvent. 請求項1から5に記載の疎水性混合物を含んでなる化粧料。 Cosmetics comprising the hydrophobic mixture according to claim 1. 皮膚改善効果、抗酸化効果、美白効果のうち少なくとも一つ、又は二つ以上の機能を有する請求項6に記載の化粧料。 The cosmetic according to claim 6, which has at least one function or two or more functions among a skin improvement effect, an antioxidant effect, and a whitening effect. 皮膚改善効果が保水性の向上および/または閉塞性の向上である請求項7に記載の化粧料。 The cosmetic according to claim 7, wherein the skin improvement effect is an improvement in water retention and / or an improvement in occlusion. 抗酸化効果が酸化防止および/またはフリーラジカル発生予防である請求項7に記載の化粧料。 The cosmetic according to claim 7, wherein the antioxidant effect is prevention of oxidation and / or prevention of free radical generation. 美白効果がチロシナーゼ阻害活性および/またはメラニン分解活性によるものである請求項7に記載の化粧料。
The cosmetic according to claim 7, wherein the whitening effect is due to tyrosinase inhibitory activity and / or melanolytic activity.
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JPS62149629A (en) * 1985-09-05 1987-07-03 Kazumi Ogata Humectant skin agent
JPH05301823A (en) * 1992-04-23 1993-11-16 Soken Kk Eliminator for active oxygen from rice
JPH07188656A (en) * 1993-12-27 1995-07-25 Soken Kk Antioxidant and freshness-reserving agent from rice
JPH08133960A (en) * 1994-01-28 1996-05-28 Kirindou:Kk Bathing agent
JPH11196849A (en) * 1998-01-09 1999-07-27 Ogita Bio Science Kenkyusho:Kk Extraction of antimelanin substance-containing material and fractionation and purification of antimelanin substance
JP2000080025A (en) * 1998-06-24 2000-03-21 Aioi Hakko:Kk Production of rice-fermented extract for bathing agent or cosmetic
JP2003009841A (en) * 2001-06-27 2003-01-14 Gekkeikan Sake Co Ltd Method for adsorbing and recovering ferrichrome compounds or their deferri compounds
JP2004248592A (en) * 2003-02-20 2004-09-09 Sanpo Kk Tyrosinase inhibitor and method for producing the same
JP2005015456A (en) * 2003-06-05 2005-01-20 Chugoku Jozo Kk Prophylactic and therapeutic agent for eczema/dermatitis group
JP2005132850A (en) * 2001-01-31 2005-05-26 Tekunooburu:Kk Compounding agent for cosmetic and cosmetic compounded with the same

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62149629A (en) * 1985-09-05 1987-07-03 Kazumi Ogata Humectant skin agent
JPH05301823A (en) * 1992-04-23 1993-11-16 Soken Kk Eliminator for active oxygen from rice
JPH07188656A (en) * 1993-12-27 1995-07-25 Soken Kk Antioxidant and freshness-reserving agent from rice
JPH08133960A (en) * 1994-01-28 1996-05-28 Kirindou:Kk Bathing agent
JPH11196849A (en) * 1998-01-09 1999-07-27 Ogita Bio Science Kenkyusho:Kk Extraction of antimelanin substance-containing material and fractionation and purification of antimelanin substance
JP2000080025A (en) * 1998-06-24 2000-03-21 Aioi Hakko:Kk Production of rice-fermented extract for bathing agent or cosmetic
JP2005132850A (en) * 2001-01-31 2005-05-26 Tekunooburu:Kk Compounding agent for cosmetic and cosmetic compounded with the same
JP2003009841A (en) * 2001-06-27 2003-01-14 Gekkeikan Sake Co Ltd Method for adsorbing and recovering ferrichrome compounds or their deferri compounds
JP2004248592A (en) * 2003-02-20 2004-09-09 Sanpo Kk Tyrosinase inhibitor and method for producing the same
JP2005015456A (en) * 2003-06-05 2005-01-20 Chugoku Jozo Kk Prophylactic and therapeutic agent for eczema/dermatitis group

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