JP6266857B2 - Cosmetics - Google Patents
Cosmetics Download PDFInfo
- Publication number
- JP6266857B2 JP6266857B2 JP2011165015A JP2011165015A JP6266857B2 JP 6266857 B2 JP6266857 B2 JP 6266857B2 JP 2011165015 A JP2011165015 A JP 2011165015A JP 2011165015 A JP2011165015 A JP 2011165015A JP 6266857 B2 JP6266857 B2 JP 6266857B2
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- Prior art keywords
- extract
- acid
- solution
- component
- flower part
- Prior art date
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Landscapes
- Cosmetics (AREA)
Description
本発明は、すぐれた美肌化、美白作用を有し、安全性の高い化粧料に関するものである。 The present invention relates to cosmetics having excellent skin beautification and whitening effects and high safety.
皮膚の老化は、加齢に伴う細胞増殖・分化の不活化、ホルモン分泌の低下、細胞外マトリックス成分の量的低下などの内的要因と、太陽光(紫外線)に誘発される活性酸素による細胞・組織の損傷、又は炎症などの外的要因とが複雑に絡み合って生ずる現象である。 Skin aging is caused by internal factors such as inactivation of cell growth / differentiation associated with aging, decreased hormone secretion, quantitative decrease of extracellular matrix components, and cells caused by active oxygen induced by sunlight (ultraviolet rays). -Phenomenon caused by complex intertwining with external factors such as tissue damage or inflammation.
皮膚老化の外的要因である活性酸素は皮膚細胞に直接傷害を及ぼすばかりでなく、細胞外マトリックス成分のコラーゲンを変性又は架橋させてシワの形成や皮膚の弾力性の低下をもたらし、さらにはメラニン色素の異常沈着を誘発してシミ、ソバカスを生じさせるなど、肌に様々なダメージを与える。 Reactive oxygen, an external factor of skin aging, not only directly damages skin cells, but also denatures or crosslinks the collagen of the extracellular matrix component, resulting in wrinkle formation and reduced skin elasticity. It causes various damages to the skin, such as causing abnormal pigmentation and causing spots and freckles.
この皮膚の老化を防ぎ、皮膚を健全、かつ、若々しい状態に保持するため、従来、種々の活性成分の使用が提案され、それら美肌化及び美白成分を配合した化粧品が上市されている。例えば、ビタミンC、ビタミンE、スーパーオキシドジスムターゼ(Superoxide dismutase;以下SODと略記)、カタラーゼなどの抗酸化剤;グリチルリチン酸などの抗炎症剤;各種紫外線吸収剤;α−ヒドロキシカルボン酸、胎盤抽出液、γ−アミノ−β−ヒドロキシ酪酸などの細胞賦活成分;コラーゲン、エラスチン、ヒアルロン酸などの細胞外マトリックス成分;尿素などの保湿剤がそれである。また、皮膚のシミ、ソバカス等の色素沈着の発生を抑制する物質としては、アルブチン、コウジ酸などが知られており、美白剤の有効成分として広く使用されている。 In order to prevent this skin aging and keep the skin healthy and youthful, the use of various active ingredients has been proposed in the past, and cosmetics containing these skin-beautifying and whitening ingredients have been put on the market. For example, vitamin C, vitamin E, superoxide dismutase (hereinafter abbreviated as SOD), an antioxidant such as catalase; an anti-inflammatory agent such as glycyrrhizic acid; various ultraviolet absorbers; α-hydroxycarboxylic acid, placenta extract Cell activation components such as γ-amino-β-hydroxybutyric acid; extracellular matrix components such as collagen, elastin and hyaluronic acid; and humectants such as urea. Further, arbutin, kojic acid, and the like are known as substances that suppress the occurrence of pigmentation such as skin spots and buckwheat, and are widely used as active ingredients of whitening agents.
しかし、それら従来の美肌化剤及び美白剤には、皮膚などに対する安全性、また、実際に皮膚に適用した際の有効性の観点で問題が存在する。また、種々の天然成分由来の美肌化剤及び美白剤も提案されているが、それらの剤の美肌化及び美白効果は、化粧料配合原料として見た場合に、皮膚などに対する安全性、また、実際に皮膚に適用した際の有効性の観点で問題が存在する。従って、かかる点が改善された化粧料配合成分を含む化粧料が求められている。 However, these conventional skin-beautifying agents and whitening agents have problems in terms of safety to the skin and the like and effectiveness when actually applied to the skin. In addition, skin-beautifying agents and whitening agents derived from various natural ingredients have been proposed, but the skin-beautifying and whitening effects of these agents are safe for the skin when viewed as cosmetic ingredients, There are problems in terms of effectiveness when actually applied to the skin. Accordingly, there is a need for cosmetics containing cosmetic ingredients with improved such points.
本発明者らは、かかる従来技術の問題点に鑑みて、皮膚安全性の観点から天然物由来の新たな美肌化及び美白成分を見出すべく鋭意研究を行った。その結果、ボタン科ボタン属に属する植物の花部の抽出物が、チロシナーゼ活性抑制作用、抗酸化作用、エラスターゼ活性阻害作用、コラゲナーゼ活性阻害作用、及びゼラチナーゼ活性阻害作用を有し、これにより、当該花部の抽出物を配合することですぐれた美肌化及び美白効果を奏し、かつ、皮膚安全性にすぐれた化粧料の提供が可能になることを見出し、本発明を完成するに至った。 In view of the problems of the prior art, the present inventors have intensively studied to find new skin-beautifying and whitening ingredients derived from natural products from the viewpoint of skin safety. As a result, the flower extract of the plant belonging to the genus Buttonaceae has a tyrosinase activity inhibitory action, an antioxidant action, an elastase activity inhibitory action, a collagenase activity inhibitory action, and a gelatinase activity inhibitory action. It has been found that blending the flower part extract makes it possible to provide cosmetics with excellent skin beautification and whitening effects and excellent skin safety, and the present invention has been completed.
従来、ボタン科ボタン属の植物であるシャクヤクの根(生薬の芍薬)やボタンの根(生薬のボタンピ)が肌荒れ、シミ、ソバカスの改善、活性酸素消去効果を有することを見出して、当該効果を利用した化粧料が提案されている(特許文献1、2)。また、ボタン科ボタン属の植物の花弁が活性酸素消去作用や抗炎症作用を有することを見出し、当該作用効果を利用した化粧料も提案されている(特許文献3,4)。
しかし、ボタン科ボタン属に属する植物の花部の抽出物がすぐれた美白作用及び抗老化作用の両作用を併せ持つことについては何ら報告されていなかった。
以上のことに鑑みて、本発明者が鋭意研究を行った結果、ボタン科ボタン属の植物の花部(花弁、萼等を含む)の抽出物が、すぐれたチロシナーゼ活性抑制作用、並びに抗酸化作用、及びMMP(エラスターゼ、コラゲナーゼ、及びゼラチナーゼ)活性阻害作用等の抗老化作用を併せ持つことを新たに見出し、本発明を完成するに至った。
Traditionally, we found that peonies roots (herbal medicine glazes) and button roots (herbal medicine buttonpis), which belong to the genus Button family, have the effects of rough skin, spots and freckles, and active oxygen scavenging effects. Utilized cosmetics have been proposed (Patent Documents 1 and 2). In addition, it has been found that petals belonging to the genus Buttonaceae have an active oxygen scavenging action and an anti-inflammatory action, and cosmetics using the action effects have also been proposed (Patent Documents 3 and 4).
However, it has not been reported at all that an extract of a flower part of a plant belonging to the genus Buttonaceae has both an excellent whitening action and an anti-aging action.
In view of the above, as a result of intensive studies by the present inventor, the extract of the flower part (including petals, buds, etc.) of the genus Buttonaceae has excellent tyrosinase activity inhibitory activity and antioxidant properties. It has been newly found out that it has both an action and an anti-aging action such as MMP (elastase, collagenase, and gelatinase) activity inhibition action, and has completed the present invention.
本発明はボタン科(Paeoniaceae)ボタン属(Paeonia)に属する植物の花部の抽出物を配合したことを特徴とする化粧料である。
また、上記ボタン科ボタン属に属する植物としては、シャクヤク(Paeonia lactiflora)が好ましい。
また、上記ボタン科ボタン属に属する植物としては、ボタン(Paeonia suffruticosa)が好ましい。
なお、ここで、化粧料なる文言は、所謂化粧料のほかに医薬部外品をも含む広義で用いる。
The present invention is a cosmetic comprising an extract of a flower part of a plant belonging to the genus Paeoniaceae and Paeonia.
The plant belonging to the genus Button is preferably peony (Paeonia lactiflora).
As the plant belonging to the genus Button family, a button (Paeonia suffruticosa) is preferable.
Here, the term cosmetics is used in a broad sense including so-called cosmetics and quasi-drugs.
ボタン科ボタン属に属する植物の花部の抽出物を配合してなる本発明の化粧料は、有効成分として含む花部の抽出物が示す強いチロシナーゼ活性抑制作用、抗酸化作用、並びにMMP活性阻害作用を併せ持ち、これにより、シミ、ソバカス等の色素沈着を予防・改善、さらにシワ、タルミを改善することができる。加えて、当該抽出物は天然物由来のものであるため、皮膚に対する刺激が少なく安全性にすぐれている。 The cosmetic composition of the present invention comprising a flower part extract of a plant belonging to the genus Buttonaceae has a strong tyrosinase activity inhibitory action, antioxidant action, and MMP activity inhibitory effect exhibited by the flower part extract contained as an active ingredient. It also has an action, thereby preventing and improving pigmentation such as spots and buckwheat, and further improving wrinkles and tarmi. In addition, since the extract is derived from a natural product, there is little irritation to the skin and it is excellent in safety.
以下、本発明について詳細に説明する。
本発明で用いるボタン科(Paeoniaceae)ボタン属(Paeonia)の植物の種は、特に限定されるものではなく、例えば、シャクヤク(Paeonia lactiflora)、ヤマシャクヤク(Paeonia japonica)、ベニバナヤマシャクヤク(Paeonia obovata)、ボタン(Paeonia suffruticosa)等が挙げられる。
Hereinafter, the present invention will be described in detail.
The species of Paeoniaceae plant used in the present invention is not particularly limited, and for example, peony (Paeonia lactiflora), peony (Peonia japonica), safflower (Paeonia obovata) , Buttons (Paeonia suffruticosa) and the like.
ボタン科ボタン属に属する植物の花部の開花時期及び大きさ等は特に限定されるものではなく、いずれのものを使用しても良い。又本発明における花部としては、花弁、萼等のいずれかまたはそれらの全部を含むものを指す。 The flowering time, size, etc. of the flower part belonging to the genus Button family are not particularly limited, and any one may be used. In addition, the flower part in the present invention refers to a flower including any one of petals, buds or the like.
抽出物の調製は、まず、ボタン科ボタン属の植物の花部を、必要ならば予め水洗して異物を除いた後、そのまま又は乾燥した上、必要に応じて細切又は粉砕し、抽出溶媒と接触させて抽出を行う。抽出は、浸漬法等の常法に従って抽出溶媒と接触させることで行うことが可能であるが、超臨界抽出法を用いることも可能である。 For the preparation of the extract, first, if necessary, the flower part of the plant belonging to the genus Buttonaceae is washed with water in advance to remove foreign substances, and then, as it is or dried, and then chopped or crushed as necessary, and the extraction solvent Extract with contact. The extraction can be performed by contacting with an extraction solvent according to a conventional method such as an immersion method, but a supercritical extraction method can also be used.
抽出溶媒としては、水;メタノール、エタノール、プロパノールなどの低級アルコール類;エチレングリコール、プロピレングリコール、1,3−ブチレングリコール、グリセリンなどの多価アルコール類;酢酸エチル、酢酸ブチル、プロピオン酸メチルなどのエステル類;アセトン、メチルエチルケトンなどのケトン類;エチルエーテル、イソプロピルエーテルなどのエーテル類;n−ヘキサン、トルエン、クロロホルムなどの炭化水素系溶媒などが挙げられ、それらは単独で又は二種以上混合して用いられる。 As an extraction solvent, water; lower alcohols such as methanol, ethanol, propanol; polyhydric alcohols such as ethylene glycol, propylene glycol, 1,3-butylene glycol, glycerin; ethyl acetate, butyl acetate, methyl propionate, etc. Esters; Ketones such as acetone and methyl ethyl ketone; Ethers such as ethyl ether and isopropyl ether; Hydrocarbon solvents such as n-hexane, toluene and chloroform, and the like. These may be used alone or in combination of two or more. Used.
それら抽出溶媒のうちでも、得られる抽出物のチロシナーゼ活性抑制作用、及び抗酸化作用、さらには、皮膚刺激性の観点から、又化粧料への幅広い適用が可能であるという点からも、本発明においては水、低級アルコール類又は多価アルコール類などの親水性溶媒が好適である。この親水性溶媒を用いる場合の好ましい例としては、例えば、水、低級アルコール類(特にエタノール)、又は多価アルコール(特に、1,3−ブチレングリコール)の単独使用、或いは、水と低級アルコール類(特にエタノール)との混合溶媒、又は水と多価アルコール類(特に1,3−ブチレングリコール)との混合溶媒の使用等が挙げられるが、なかでも水と1,3−ブチレングリコールの混合溶媒が最も好ましい。 Among these extraction solvents, the extract obtained has a tyrosinase activity inhibitory action and an antioxidant action, and also from the viewpoint of skin irritation and from the viewpoint that it can be widely applied to cosmetics. In water, hydrophilic solvents such as water, lower alcohols and polyhydric alcohols are suitable. Preferable examples of using this hydrophilic solvent include, for example, water, lower alcohols (especially ethanol), or polyhydric alcohols (especially 1,3-butylene glycol) alone, or water and lower alcohols. (Especially use of a mixed solvent of ethanol) or a mixed solvent of water and a polyhydric alcohol (especially 1,3-butylene glycol), among others, a mixed solvent of water and 1,3-butylene glycol Is most preferred.
混合溶媒を用いる場合の混合比は、例えば水とエタノールとの混合溶媒であれば、容量比(以下同じ)で1:1〜25:1、水とグリセリンとの混合溶媒であれば1:1〜20:1、水と1,3−ブチレングリコールとの混合溶媒であれば、1:1〜20:1の範囲とすることが好ましい。 The mixing ratio in the case of using a mixed solvent is, for example, 1: 1 to 25: 1 in a volume ratio (hereinafter the same) if the mixed solvent is water and ethanol, and 1: 1 if the mixed solvent is water and glycerin. If it is -20: 1 and it is a mixed solvent of water and 1,3-butylene glycol, it is preferable to set it as the range of 1: 1 to 20: 1.
また、ボタン科ボタン属に属する植物の花部(乾燥したもの)と抽出溶媒との重量比は好ましくは1:1〜1:50の範囲であり、より好ましくは、1:10〜1:30の範囲である。 In addition, the weight ratio between the flower part (dried) of the plant belonging to the genus Buttonaceae and the extraction solvent is preferably in the range of 1: 1 to 1:50, more preferably 1:10 to 1:30. Range.
抽出物の調製に際して、そのpHに特に限定はないが、一般には4〜9の範囲とすることが好ましい。かかる意味で、必要であれば、前記抽出溶媒に、水酸化ナトリウム、炭酸ナトリウム、水酸化カリウムなどのアルカリ性調整剤、又はクエン酸、塩酸、リン酸、硫酸などの酸性調整剤を配合し、所望のpHとなるように調整してもよい。 In preparing the extract, the pH is not particularly limited, but it is generally preferably in the range of 4-9. In this sense, if necessary, the extraction solvent is blended with an alkaline adjusting agent such as sodium hydroxide, sodium carbonate or potassium hydroxide, or an acidic adjusting agent such as citric acid, hydrochloric acid, phosphoric acid or sulfuric acid. You may adjust so that it may become pH of.
抽出温度、抽出時間等の抽出条件は、用いる溶媒の種類やpHによっても異なるが、例えば、水、1,3−ブチレングリコール、又は水と1,3−ブチレングリコールとの混液を溶媒とする場合であれば、抽出温度は好ましくは40℃〜95℃の範囲であり、より好ましく60℃〜90℃の範囲であり、又抽出時間は好ましくは30分〜6時間であり、より好ましくは1〜4時間の範囲である。 Extraction conditions such as extraction temperature and extraction time vary depending on the type and pH of the solvent used. For example, water, 1,3-butylene glycol, or a mixture of water and 1,3-butylene glycol is used as the solvent. The extraction temperature is preferably in the range of 40 ° C to 95 ° C, more preferably in the range of 60 ° C to 90 ° C, and the extraction time is preferably 30 minutes to 6 hours, more preferably 1 to 1. The range is 4 hours.
なお、本発明の抽出処理の前段階としての抽出液作成に際して、又は抽出と並行して、必要に応じて加水分解処理を行ってもよい。これによって、ボタン科ボタン属に属する植物の花部の抽出物の保存安定性等を改善して、化粧料配合剤としての抽出物をより有効に利用できる可能性がある。 In addition, you may perform a hydrolysis process as needed at the time of the extraction liquid preparation as a pre-stage of the extraction process of this invention, or in parallel with extraction. As a result, the storage stability of the flower part extract of plants belonging to the genus Buttonaceae may be improved and the extract as a cosmetic preparation may be used more effectively.
抽出物に酵素加水分解処理を施す場合、酵素としては、アクチナーゼ、パパイン、ペプシンなどの蛋白分解酵素、グルコアミラーゼ、α−アミラーゼ、β−アミラーゼなどの澱粉分解酵素、セルラーゼ、ヘミセルラーゼ、ペクチナーゼなどの繊維素分解酵素、及びリパーゼなどの脂肪分解酵素から選ばれた1種、又はそれらの酵素群からそれぞれ選ばれた1種又は2種以上の酵素を組み合わせて用いることが好ましい。 In the case of subjecting the extract to an enzymatic hydrolysis treatment, examples of the enzyme include proteolytic enzymes such as actinase, papain and pepsin, starch degrading enzymes such as glucoamylase, α-amylase and β-amylase, cellulase, hemicellulase and pectinase. It is preferable to use one kind selected from a fibrinolytic enzyme and a lipolytic enzyme such as lipase, or a combination of one kind or two or more kinds of enzymes selected from these enzyme groups.
酵素の添加量は、ボタン科ボタン属に属する植物の花部の固形分に対して、合計で0.01〜10重量%の範囲とすることが好ましく、より好ましくは0.1〜2.0重量%の範囲である。 The amount of the enzyme added is preferably in the range of 0.01 to 10% by weight, more preferably 0.1 to 2.0%, based on the solid content of the flower part of the plant belonging to the genus Buttonaceae. It is in the range of wt%.
上述のように調製した抽出物は、一般にはpHを4〜8に調製した上で、これをそのままの状態で化粧料配合剤として使用しても良く、又減圧濃縮等により所望の濃度として使用しても良い。また、抽出物はスプレードライ法等の常法により乾燥物としても良い。 In general, the extract prepared as described above may be adjusted to a pH of 4 to 8 and used as it is as a cosmetic compounding agent as it is or as a desired concentration by vacuum concentration or the like. You may do it. In addition, the extract may be dried by a conventional method such as spray drying.
また、上述のように調製した抽出物は、保存安定性等を高めるために、一定時間冷蔵保存した上で、化粧料配合剤として使用しても良い。 Further, the extract prepared as described above may be used as a cosmetic compounding agent after being refrigerated for a certain period of time in order to enhance storage stability and the like.
以上のように調製される本発明の抽出物は、後述の試験例に示す通り、顕著なチロシナーゼ活性抑制作用、抗酸化作用及びMMP活性抑制作用を有すると共に、皮膚に対する刺激性が少なく生体安全性にもすぐれているので、当該抽出物を配合した化粧料は、シワ、たるみ、シミ、ソバカスの発生を予防し又はそれらの症状を改善して、肌を若々しく健全な状態に維持することができる。 The extract of the present invention prepared as described above has remarkable tyrosinase activity inhibitory action, antioxidant action and MMP activity inhibitory action as shown in the test examples described later, and is less irritating to the skin and biologically safe. Therefore, cosmetics containing the extract should maintain the skin in a youthful and healthy state by preventing the generation of wrinkles, sagging, spots and freckles or improving their symptoms. Can do.
本発明のボタン科ボタン属に属する植物の花部の抽出物を含む化粧料としては、例えば乳液、クリーム、ローション、エッセンス、パックなどの基礎化粧料、口紅、ファンデーション、リクイドファンデーション、メイクアッププレスパウダー、ほほ紅、白粉などのメイクアップ化粧料、洗顔料、ボディシャンプー、石けんなどの清浄用化粧料、さらには浴剤等が挙げられるが、勿論これらに限定されるものではない。 Cosmetics containing the flower part extract of plants belonging to the genus Button family of the present invention include, for example, basic cosmetics such as emulsions, creams, lotions, essences, packs, lipsticks, foundations, liquid foundations, makeup press powders Examples include makeup cosmetics such as cheeks and white powder, cleansing cosmetics such as facial cleansers, body shampoos, and soaps, and bath agents, but are not limited thereto.
本発明の化粧料におけるボタン科ボタン属に属する植物の花部の抽出物の配合量は、抽出物の固形分として、基礎化粧料の場合は、一般に0.002〜1.0重量%、好ましくは0.02〜0.2重量%の範囲、メイクアップ化粧料の場合は、一般に0.002〜1.0重量%、好ましくは0.02〜0.2重量%の範囲、又清浄用化粧料の場合は、一般に0.002〜10.0重量%、好ましくは0.02〜7.0重量%の範囲である。 The blending amount of the flower part extract of the plant belonging to the genus Buttonaceae in the cosmetics of the present invention is generally 0.002 to 1.0% by weight, preferably in the case of basic cosmetics, as the solid content of the extract. Is in the range of 0.02 to 0.2% by weight, in the case of makeup cosmetics, generally in the range of 0.002 to 1.0% by weight, preferably in the range of 0.02 to 0.2% by weight. In the case of a material, it is generally in the range of 0.002 to 10.0% by weight, preferably 0.02 to 7.0% by weight.
本発明の化粧料には、必須成分のボタン科ボタン属に属する植物の花部の抽出物のほかに、通常化粧料に用いられる成分、例えば油性成分、界面活性剤(合成系、天然物系)、保湿剤、増粘剤、防腐・殺菌剤、粉体成分、紫外線吸収剤、抗酸化剤、色素、香料等を必要に応じて適宜配合することができる。また、本発明のボタン科ボタン属に属する植物の花部の抽出物の有効性、特長を損なわない限り、他の生理活性成分と組み合わせて化粧料に配合することも何ら差し支えない。 The cosmetics of the present invention include, in addition to extracts of flower parts of plants belonging to the genus Buttonaceae as an essential component, components commonly used in cosmetics, such as oily components, surfactants (synthetic systems, natural products systems) ), A moisturizer, a thickener, an antiseptic / bactericidal agent, a powder component, an ultraviolet absorber, an antioxidant, a pigment, a fragrance and the like can be appropriately blended as necessary. Moreover, as long as the effectiveness and characteristics of the flower part extract of the plant belonging to the genus Buttonaceae of the present invention are not impaired, it may be combined with other physiologically active ingredients in cosmetics.
ここで、油性成分としては、例えばオリーブ油、ホホバ油、ヒマシ油、大豆油、米油、米胚芽油、ヤシ油、パーム油、カカオ油、メドウフォーム油、シアーバター、ティーツリー油、アボガド油、マカデミアナッツ油、植物由来スクワランなどの植物由来の油脂類;ミンク油、タートル油などの動物由来の油脂類;ミツロウ、カルナウバロウ、ライスワックス、ラノリンなどのロウ類;流動パラフィン、ワセリン、パラフィンワックス、スクワランなどの炭化水素類;ミリスチン酸、パルミチン酸、ステアリン酸、オレイン酸、イソステアリン酸、cis−11−エイコセン酸などの脂肪酸類;ラウリルアルコール、セタノール、ステアリルアルコールなどの高級アルコール類;ミリスチン酸イソプロピル、パルミチン酸イソプロピル、オレイン酸ブチル、2−エチルヘキシルグリセライド、高級脂肪酸オクチルドデシル(ステアリン酸オクチルドデシル等)などの合成エステル類及び合成トリグリセライド類等が挙げられる。 Here, as the oil component, for example, olive oil, jojoba oil, castor oil, soybean oil, rice oil, rice germ oil, palm oil, palm oil, cacao oil, meadow foam oil, sheer butter, tea tree oil, avocado oil, Oils derived from plants such as macadamia nut oil and plant-derived squalane; Fats derived from animals such as mink oil and turtle oil; waxes such as beeswax, carnauba wax, rice wax, lanolin; liquid paraffin, petrolatum, paraffin wax, squalane, etc. Hydrocarbons; fatty acids such as myristic acid, palmitic acid, stearic acid, oleic acid, isostearic acid, cis-11-eicosenoic acid; higher alcohols such as lauryl alcohol, cetanol, stearyl alcohol; isopropyl myristate, palmitic acid Isopropyl, me Butyl phosphate, 2-ethylhexyl glycerides, higher fatty acid octyldodecyl (octyl stearate dodecyl and the like), and the synthetic esters and synthetic triglycerides such like.
界面活性剤としては、例えばポリオキシエチレンアルキルエーテル、ポリオキシエチレン脂肪酸エステル、ポリオキシエチレンソルビタン脂肪酸エステル、グリセリン脂肪酸エステル、ポリグリセリン脂肪酸エステル、ポリオキシエチレングリセリン脂肪酸エステル、ポリオキシエチレン硬化ヒマシ油、ポリオキシエチレンソルビトール脂肪酸エステルなどの非イオン界面活性剤;脂肪酸塩、アルキル硫酸塩、アルキルベンゼンスルホン酸塩、ポリオキシエチレンアルキルエーテル硫酸塩、ポリオキシエチレン脂肪アミン硫酸塩、ポリオキシエチレンアルキルフェニルエーテル硫酸塩、ポリオキシエチレンアルキルエーテル燐酸塩、α−スルホン化脂肪酸アルキルエステル塩、ポリオキシエチレンアルキルフェニルエーテル燐酸塩などのアニオン界面活性剤;第四級アンモニウム塩、第一級〜第三級脂肪アミン塩、トリアルキルベンジルアンモニウム塩、アルキルピリジニウム塩、2−アルキル−1−アルキル−1−ヒドロキシエチルイミダゾリニウム塩、N,N−ジアルキルモルフォルニウム塩、ポリエチレンポリアミン脂肪酸アミド塩などのカチオン界面活性剤;N,N−ジメチル−N−アルキル−N−カルボキシメチルアンモニオベタイン、N,N,N−トリアルキル−N−アルキレンアンモニオカルボキシベタイン、N−アシルアミドプロピル−N′,N′−ジメチル−N′−β−ヒドロキシプロピルアンモニオスルホベタインなどの両性界面活性剤等を使用することができる。
また、乳化剤乃至乳化助剤として、酵素処理ステビアなどのステビア誘導体、レシチン及びその誘導体、乳酸菌醗酵米、乳酸菌醗酵発芽米、乳酸菌醗酵穀類(麦類、豆類、雑穀など)、ジュアゼイロ(Rhamnaceae zizyphus joazeiro)抽出物等を配合することもできる。
Examples of the surfactant include polyoxyethylene alkyl ether, polyoxyethylene fatty acid ester, polyoxyethylene sorbitan fatty acid ester, glycerin fatty acid ester, polyglycerin fatty acid ester, polyoxyethylene glycerin fatty acid ester, polyoxyethylene hydrogenated castor oil, polyoxyethylene Nonionic surfactants such as oxyethylene sorbitol fatty acid esters; fatty acid salts, alkyl sulfates, alkylbenzene sulfonates, polyoxyethylene alkyl ether sulfates, polyoxyethylene fatty amine sulfates, polyoxyethylene alkyl phenyl ether sulfates, Polyoxyethylene alkyl ether phosphates, α-sulfonated fatty acid alkyl ester salts, polyoxyethylene alkyl phenyl ether phosphates, Quaternary ammonium salt, primary to tertiary fatty amine salt, trialkylbenzylammonium salt, alkylpyridinium salt, 2-alkyl-1-alkyl-1-hydroxyethylimidazolinium salt, N N, N-dimethyl-N-alkyl-N-carboxymethylammoniobetaine, N, N, N-trialkyl-N-, N, N-dimethyl-N-alkyl-N-carboxymethylammoniobetaine Amphoteric surfactants such as alkylene ammoniocarboxybetaine and N-acylamidopropyl-N ′, N′-dimethyl-N′-β-hydroxypropylammoniosulfobetaine can be used.
In addition, as emulsifiers or emulsifiers, stevia derivatives such as enzyme-treated stevia, lecithin and its derivatives, lactic acid bacteria fermented rice, lactic acid bacteria fermented rice, lactic acid bacteria fermented cereals (wheat, legumes, cereals, etc.), juzairo (Rhamnaceae zizyphus joazeiro) An extract or the like can also be blended.
保湿剤としては、例えばグリセリン、プロピレングリコール、ジプロピレングリコール、1,3−ブチレングリコール、ポリエチレングリコール、ソルビトール、キシリトール、ピロリドンカルボン酸ナトリウム等があり、さらにトレハロース等の糖類、乳酸菌醗酵米、ムコ多糖類(例えば、ヒアルロン酸及びその誘導体、コンドロイチン及びその誘導体、ヘパリン及びその誘導体など)、エラスチン及びその誘導体、コラーゲン及びその誘導体、NMF関連物質、乳酸、尿素、高級脂肪酸オクチルドデシル、海藻抽出物、ビャッキュウ抽出物、魚介類由来コラーゲン及びその誘導体、各種アミノ酸及びそれらの誘導体が挙げられる。 Examples of humectants include glycerin, propylene glycol, dipropylene glycol, 1,3-butylene glycol, polyethylene glycol, sorbitol, xylitol, sodium pyrrolidonecarboxylate, and sugars such as trehalose, lactic acid bacteria fermented rice, and mucopolysaccharides. (For example, hyaluronic acid and its derivatives, chondroitin and its derivatives, heparin and its derivatives, etc.), elastin and its derivatives, collagen and its derivatives, NMF related substances, lactic acid, urea, higher fatty acid octyldodecyl, seaweed extract, beech extract Products, seafood-derived collagen and derivatives thereof, various amino acids and derivatives thereof.
増粘剤としては、例えばアルギン酸、寒天、カラギーナン、フコイダン等の褐藻、緑藻又は紅藻由来成分;ビャッキュウ抽出物;ペクチン、ローカストビーンガム、アロエ多糖体等の多糖類;キサンタンガム、トラガントガム、グアーガム等のガム類;カルボキシメチルセルロース、ヒドロキシエチルセルロース等のセルロース誘導体;ポリビニルアルコール、ポリビニルピロリドン、カルボキシビニルポリマー、アクリル酸・メタクリル酸共重合体等の合成高分子類;ヒアルロン酸及びその誘導体;ポリグルタミン酸及びその誘導体等が挙げられる。 Examples of the thickener include brown algae, green algae or red algae-derived components such as alginic acid, agar, carrageenan and fucoidan; beech extract; polysaccharides such as pectin, locust bean gum and aloe polysaccharide; xanthan gum, tragacanth gum, guar gum and the like Gums; Cellulose derivatives such as carboxymethylcellulose and hydroxyethylcellulose; Synthetic polymers such as polyvinyl alcohol, polyvinylpyrrolidone, carboxyvinyl polymer and acrylic acid / methacrylic acid copolymer; Hyaluronic acid and its derivatives; Polyglutamic acid and its derivatives Is mentioned.
防腐・殺菌剤としては、例えば尿素;パラオキシ安息香酸メチル、パラオキシ安息香酸エチル、パラオキシ安息香酸プロピル、パラオキシ安息香酸ブチルなどのパラオキシ安息香酸エステル類;フェノキシエタノール、ジクロロフェン、ヘキサクロロフェン、塩酸クロルヘキシジン、塩化ベンザルコニウム、サリチル酸、エタノール、ウンデシレン酸、フェノール類、ジャマール(イミダゾデイニールウレア)、1,2−ペンタンジオール、各種精油類、樹皮乾留物等がある。 Examples of the antiseptic / bactericidal agent include urea; paraoxybenzoates such as methyl paraoxybenzoate, ethyl paraoxybenzoate, propyl paraoxybenzoate, and butyl paraoxybenzoate; phenoxyethanol, dichlorophene, hexachlorophene, chlorhexidine hydrochloride, benzaza chloride Luconium, salicylic acid, ethanol, undecylenic acid, phenols, jamal (imidazodenyl urea), 1,2-pentanediol, various essential oils, bark dry matter, and the like.
粉体成分としては、例えばセリサイト、酸化チタン、タルク、カオリン、ベントナイト、酸化亜鉛、炭酸マグネシウム、酸化マグネシウム、酸化ジルコニウム、硫酸バリウム、無水ケイ酸、雲母、ナイロンパウダー、ポリエチレンパウダー、シルクパウダー、セルロース系パウダー、穀類(米、麦、トウモロコシ、キビなど)のパウダー、豆類(大豆、小豆など)のパウダー等がある。 Examples of powder components include sericite, titanium oxide, talc, kaolin, bentonite, zinc oxide, magnesium carbonate, magnesium oxide, zirconium oxide, barium sulfate, silicic anhydride, mica, nylon powder, polyethylene powder, silk powder, and cellulose. System powders, powders of cereals (rice, wheat, corn, millet, etc.), powders of beans (soybeans, red beans, etc.).
紫外線吸収剤としては、例えばパラアミノ安息香酸エチル、パラジメチルアミノ安息香酸エチルヘキシル、サリチル酸アミル及びその誘導体、パラメトキシ桂皮酸2−エチルヘキシル、桂皮酸オクチル、オキシベンゾン、2,4−ジヒドロキシベンゾフェノン、2−ヒドロキシ−4−メトキシベンゾフェノン−5−スルホン酸塩、4−ターシャリーブチル−4−メトキシベンゾイルメタン、2−(2−ヒドロキシ−5−メチルフェニル)ベンゾトリアゾール、ウロカニン酸、ウロカニン酸エチル、アロエ抽出物等がある。 Examples of the ultraviolet absorber include ethyl paraaminobenzoate, ethylhexyl paradimethylaminobenzoate, amyl salicylate and derivatives thereof, 2-ethylhexyl paramethoxycinnamate, octyl cinnamate, oxybenzone, 2,4-dihydroxybenzophenone, 2-hydroxy-4 -Methoxybenzophenone-5-sulfonate, 4-tertiarybutyl-4-methoxybenzoylmethane, 2- (2-hydroxy-5-methylphenyl) benzotriazole, urocanic acid, ethyl urocanate, aloe extract, etc. .
抗酸化剤としては、例えばブチルヒドロキシアニソール、ブチルヒドロキシトルエン、没食子酸プロピル、ビタミンE及びその誘導体、ビャッキュウ抽出物、イネ抽出物等がある。 Antioxidants include, for example, butylhydroxyanisole, butylhydroxytoluene, propyl gallate, vitamin E and its derivatives, beech extract, rice extract and the like.
生理活性成分としては、例えば美白成分として、t−シクロアミノ酸誘導体、コウジ酸及びその誘導体、アスコルビン酸及びその誘導体、ハイドロキノン誘導体、エラグ酸及びその誘導体、レゾルシノール誘導体、トラネキサム酸及びその誘導体、4−メトキシサリチル酸カリウム塩、マグノリグナン(5,5'−ジプロピル−ビフェニル−2,2’−ジオール)、4−HPB(ロドデノール、4−(4−ヒドロキシフェニル)−4−ブタノール))、AMP(アデノシンモノホスフェイト、アデノシン1リン酸)、胎盤抽出液、ニコチン酸及びその誘導体、ソウハクヒ抽出物、ユキノシタ抽出物、米糠抽出物、米糠抽出物加水分解物、乳酸菌醗酵米、乳酸菌醗酵発芽米、乳酸菌醗酵穀類(麦類、豆類、雑穀類)、白芥子抽出物、白芥子加水分解抽出物、ムラサキシキブ抽出物、ハス種子発酵物、党参抽出物、ハトムギ発酵物、ローヤルゼリー発酵物、酒粕発酵物、パンダヌス・アマリリフォリウス(Pandanus amaryllifolius Roxb.)抽出物、アルカンジェリシア・フラバ(Arcangelicia flava Merrilli)抽出物、カミツレ抽出物(商品名:カモミラET)、コンブ等の海藻の抽出物、アマモ等の海草の抽出物、リノール酸及びその誘導体もしくは加工物(例えばリポソーム化リノール酸など)、2,5−ジヒドロキシ安息香酸誘導体等が、又皮膚老化防止・美肌化成分として、動物又は魚由来のコラーゲン及びその誘導体、エラスチン及びその誘導体、ニコチン酸及びその誘導体、グリチルリチン酸及びその誘導体(ジカリウム塩等)、t−シクロアミノ酸誘導体、ビタミンA及びその誘導体、ビタミンE及びその誘導体、アラントイン、α−ヒドロキシ酸類、ジイソプロピルアミンジクロロアセテート、γ−アミノ−β−ヒドロキシ酪酸、ゲンチアナエキス、甘草エキス、ハトムギエキス、カミツレエキス、ニンジンエキス、アロエエキスなどの生薬抽出エキス、米抽出物加水分解物、米糠抽出物加水分解物、米醗酵エキス、ミツイシコンブ抽出物、アナアオサ抽出物、アマモ等の海草の抽出物、ソウハクヒエキス、ジョアゼイロ(Zizyphus joazeiro)抽出物等がある。 Examples of physiologically active ingredients include whitening ingredients such as t-cycloamino acid derivatives, kojic acid and derivatives thereof, ascorbic acid and derivatives thereof, hydroquinone derivatives, ellagic acid and derivatives thereof, resorcinol derivatives, tranexamic acid and derivatives thereof, 4-methoxy Salicylic acid potassium salt, magnolignan (5,5′-dipropyl-biphenyl-2,2′-diol), 4-HPB (rhodenol, 4- (4-hydroxyphenyl) -4-butanol)), AMP (adenosine monophos) Fate, adenosine monophosphate), placenta extract, nicotinic acid and its derivatives, Sakuhakuhi extract, yukinoshita extract, rice bran extract, rice bran extract hydrolyzate, lactic acid bacteria fermented rice, lactic acid bacteria fermented rice, lactic acid bacteria fermented cereals ( Wheat, beans, cereals), white coconut extract, white coconut hydrolyzed extract Murasakixikib extract, lotus seed fermented product, ginseng extract, pearl barley fermented product, royal jelly fermented product, sake lees fermented product, Pandanus amaryllifolius Roxb. Extract, Arcangelicia flava Merrilli extract , Chamomile extract (trade name: Chamomira ET), seaweed extract such as kombu, seaweed extract such as sea cucumber, linoleic acid and its derivatives or processed products (eg liposomal linoleic acid), 2,5- Dihydroxybenzoic acid derivatives, etc. are also used as skin aging preventing / beautifying components such as collagen derived from animals or fish and derivatives thereof, elastin and derivatives thereof, nicotinic acid and derivatives thereof, glycyrrhizic acid and derivatives thereof (dipotassium salt, etc.), t -Cycloamino acid derivatives, vitamin A and its derivatives, vitamin E and its derivatives Body, allantoin, α-hydroxy acids, diisopropylamine dichloroacetate, γ-amino-β-hydroxybutyric acid, gentian extract, licorice extract, pearl barley extract, chamomile extract, carrot extract, aloe extract, etc., rice extract water Examples include hydrolysates, rice bran extract hydrolysates, rice fermentation extracts, honey comb extracts, anaaaosa extracts, seaweed extracts such as sea cucumbers, Sohakuhihi extract, and Zizyphus joazeiro extract.
上記のコウジ酸誘導体としては、例えばコウジ酸モノブチレート、コウジ酸モノカプレート、コウジ酸モノパルミテート、コウジ酸ジブチレートなどのコウジ酸エステル類、コウジ酸エーテル類、コウジ酸グルコシドなどのコウジ酸糖誘導体等が、アスコルビン酸誘導体としては、例えばL−アスコルビン酸−2−リン酸エステルナトリウム、L−アスコルビン酸−2−リン酸エステルマグネシウム、L−アスコルビン酸−2−硫酸エステルナトリウム、L−アスコルビン酸−2−硫酸エステルマグネシウムなどのアスコルビン酸エステル塩類、L−アスコルビン酸−2−グルコシド(2−O−α−D−グルコピラノシル−L−アスコルビン酸)、L−アスコルビン酸−5−グルコシド(5−O−α−D−グルコピラノシル−L−アスコルビン酸)などのアスコルビン酸糖誘導体、それらアスコルビン酸糖誘導体の6位アシル化物(アシル基は、ヘキサノイル基、オクタノイル基、デカノイル基など)、L−アスコルビン酸テトライソパルミチン酸エステル、L−アスコルビン酸テトララウリン酸エステルなどのL−アスコルビン酸テトラ脂肪酸エステル類、3−O−エチルアスコルビン酸、L−アスコルビン酸−2−リン酸−6−O−パルミテートナトリウム等が、ハイドロキノン誘導体としては、アルブチン(ハイドロキノン−β−D−グルコピラノシド)、α−アルブチン(ハイドロキノン−α−D−グルコピラノシド)等が、レゾルシノール誘導体としては、例えば4−n−ブチルレゾルシノール、4−イソアミルレゾルシノール等が、2,5−ジヒドロキシ安息香酸誘導体としては、例えば2,5−ジアセトキシ安息香酸、2−アセトキシ−5−ヒドロキシ安息香酸、2−ヒドロキシ−5−プロピオニルオキシ安息香酸等が、ニコチン酸誘導体としては、例えばニコチン酸アミド、ニコチン酸ベンジル等が、ビタミンE誘導体としては、例えばビタミンEニコチネート、ビタミンEリノレート等が、α−ヒドロキシ酸としては、例えば乳酸、リンゴ酸、コハク酸、クエン酸、α−ヒドロキシオクタン酸等がある。 Examples of the kojic acid derivatives include kojic acid esters such as kojic acid monobutyrate, kojic acid monocaprate, kojic acid monopalmitate, kojic acid dibutyrate, kojic acid ethers, kojic acid sugar derivatives such as kojic acid glucoside, etc. However, as the ascorbic acid derivatives, for example, L-ascorbic acid-2-phosphate sodium, L-ascorbic acid-2-phosphate magnesium, L-ascorbic acid-2-sulfate sodium, L-ascorbic acid-2 -Ascorbic acid ester salts such as magnesium sulfate, L-ascorbic acid-2-glucoside (2-O-α-D-glucopyranosyl-L-ascorbic acid), L-ascorbic acid-5-glucoside (5-O-α) -D-glucopyranosyl-L-ascorbine Acid) ascorbic acid sugar derivatives, acylated 6-positions of these ascorbic acid sugar derivatives (acyl groups are hexanoyl, octanoyl, decanoyl, etc.), L-ascorbic acid tetraisopalmitate, L-ascorbic acid tetra L-ascorbic acid tetrafatty acid esters such as lauric acid ester, 3-O-ethylascorbic acid, L-ascorbic acid-2-phosphate-6-O-palmitate sodium and the like are hydroquinone derivatives such as arbutin (hydroquinone). -Β-D-glucopyranoside), α-arbutin (hydroquinone-α-D-glucopyranoside) and the like, and as resorcinol derivatives, for example, 4-n-butylresorcinol, 4-isoamylresorcinol and the like are 2,5-dihydroxybenzoic acid. Derivatives and For example, 2,5-diacetoxybenzoic acid, 2-acetoxy-5-hydroxybenzoic acid, 2-hydroxy-5-propionyloxybenzoic acid, etc., and nicotinic acid derivatives include, for example, nicotinic acid amide, nicotinic acid benzyl, etc. However, examples of the vitamin E derivative include vitamin E nicotinate and vitamin E linoleate, and examples of the α-hydroxy acid include lactic acid, malic acid, succinic acid, citric acid, and α-hydroxyoctanoic acid.
次に、製造例、実施例(処方例)及び試験例によって本発明をさらに具体的に説明するが、本発明はそれらに限定されるものではない。なお、以下において、部はすべて重量部を、また%はすべて重量%を意味する。 Next, the present invention will be described more specifically with reference to production examples, examples (formulation examples), and test examples, but the present invention is not limited thereto. In the following, all parts are parts by weight, and all percentages are% by weight.
製造例1.シャクヤクの花部の抽出液の調製(1)
ボタン科ボタン属に属する植物のシャクヤク(Paeonia lactiflora)の花を乾燥、粉砕して得られる粉砕物30gを、30%1,3−ブチレングリコール溶液(精製水/1,3ブチレングリコール=70/30)300gに接触させ、80℃で2時間抽出を行った。次に、得られた抽出液を濾過して淡黄色〜褐色透明の花部の抽出液260gを得た(固形分濃度2.59%)。
Production Example 1 Preparation of peony flower part extract (1)
30g 1,3-butylene glycol solution (purified water / 1,3 butylene glycol = 70/30) was obtained by drying and pulverizing the flowers of the peony (Paeonia lactiflora) plant belonging to the genus Buttonaceae. ) It was brought into contact with 300 g and extracted at 80 ° C. for 2 hours. Next, the obtained extract was filtered to obtain 260 g of a light yellow to brown transparent flower part extract (solid content concentration 2.59%).
製造例2.シャクヤクの花部の抽出液の調製(2)
抽出溶媒として、30%1,3−ブチレングリコール溶液に代えて、1,3−ブチレングリコールを使用すること以外は製造例1と同様の方法により、淡黄色〜褐色透明の花部の抽出液280gを得た(固形分濃度0.9%)。
Production Example 2 Preparation of peony flower part extract (2)
As an extraction solvent, 280 g of a light yellow to brown transparent flower part extract is obtained in the same manner as in Production Example 1, except that 1,3-butylene glycol is used instead of 30% 1,3-butylene glycol solution. (Solid content concentration 0.9%) was obtained.
製造例3.シャクヤクの花部の抽出液の調製(3)
抽出溶媒として、30%1,3−ブチレングリコールに代えて、精製水を使用すること以外は製造例1と同様の方法により、褐色透明の花部の抽出液260gを得た(固形分濃度1.37%)。
Production Example 3 Preparation of peony flower part extract (3)
As an extraction solvent, instead of 30% 1,3-butylene glycol, 260 g of a brown transparent flower part extract was obtained by the same method as in Production Example 1 (solid content concentration 1). 37%).
製造例4.ヤマシャクヤクの花部の抽出液の調製(1)
ボタン科ボタン属に属する植物として、シャクヤクに代えて、ヤマシャクヤク(Paeonia japonica)を使用すること以外は製造例1と同様の方法により、淡黄色〜褐色透明の花部の抽出液275gを得た(固形分濃度2.56%)。
Production Example 4 Preparation of flower extract of peony flower (1)
As a plant belonging to the genus Button family, 275 g of a light yellow to brown transparent flower part extract was obtained in the same manner as in Production Example 1 except that instead of peonies, peony (Paeonia japonica) was used. (Solid concentration 2.56%).
製造例5.ベニヤマシャクヤクの花部の抽出液の調製(1)
ボタン科ボタン属に属する植物として、シャクヤクに代えて、ベニバナヤマシャクヤク(Paeonia obovata)を使用すること以外は製造例1と同様の方法により、淡黄色〜褐色透明の花部の抽出液278gを得た(固形分濃度2.51%)。
Production Example 5 Preparation of extract of flower part of peonies (1)
As a plant belonging to the genus Button family, 278 g of a light yellow to brown transparent flower part extract is obtained by the same method as in Production Example 1 except that sae peony is used instead of peony. (Solid content concentration 2.51%).
製造例6.ボタンの花部の抽出液の調製(1)
ボタン科ボタン属に属する植物として、シャクヤクに代えて、ボタン(Paeonia suffruticosa)の花部を使用すること以外は製造例1と同様の方法により、淡黄色〜褐色透明の花部の抽出液278gを得た(固形分濃度1.2%)。
Production Example 6 Preparation of button flower extract (1)
As a plant belonging to the genus Button family, 278 g of a light yellow-brown transparent flower part extract is obtained in the same manner as in Production Example 1 except that the flower part of a button (Paeonia suffruticosa) is used instead of peonies. Obtained (solid content concentration 1.2%).
製造例7.シャクヤクの花部の酵素分解液(1)
ボタン科ボタン属に属する植物のシャクヤク(Paeonia lactiflora)の花部を乾燥、粉砕して得られる粉砕物30gを、精製水300gに接触させ、かつ、この溶液に0.3gのペクチナーゼを添加し、40℃で1時間、酵素分解処理を行った後、80℃で1時間抽出を行った。得られた抽出液を濾過して淡黄色〜褐色透明の花部の抽出液260gを得た(固形分濃度1.8%)。
Production Example 7 Enzymatic decomposition solution of peony flower (1)
30 g of a pulverized product obtained by drying and pulverizing the flower part of a peony (Paeonia lactiflora) belonging to the genus Buttonaceae is brought into contact with 300 g of purified water, and 0.3 g of pectinase is added to this solution, After carrying out the enzymatic decomposition treatment at 40 ° C. for 1 hour, extraction was carried out at 80 ° C. for 1 hour. The obtained extract was filtered to obtain 260 g of a light yellow to brown transparent flower part extract (solid content concentration 1.8%).
実施例1.クリーム
[A成分] 部
流動パラフィン 5.0
ヘキサラン (注1) 4.0
パラフィン 5.0
グリセリルモノステアレート 2.0
ポリオキシエチレン(20)ソルビタンモノステアレート 6.0
ブチルパラベン 0.1
(注1)株式会社テクノーブル製 トリオクタン酸グリセリル
[B成分]
製造例1の抽出液 5.0
グリセリン 5.0
カルボキシメチルモノステアレート 0.1
モイストン・C (注2) 1.0
精製水 全量が100部となる量
(注2)株式会社テクノーブル製 NMF成分
[C成分]
香料 適量
上記のA成分とB成分をそれぞれ80℃以上に加熱した後、攪拌混合した。これを50℃まで冷却した後、C成分を加えてさらに攪拌混合してクリームを得た。
Example 1. Cream [Component A] Liquid paraffin 5.0
Hexalan (Note 1) 4.0
Paraffin 5.0
Glyceryl monostearate 2.0
Polyoxyethylene (20) sorbitan monostearate 6.0
Butylparaben 0.1
(Note 1) Technoble Co., Ltd. glyceryl trioctanoate
[B component]
Extraction liquid of Production Example 1 5.0
Glycerin 5.0
Carboxymethyl monostearate 0.1
Moiston C (Note 2) 1.0
Amount of purified water 100 parts (Note 2) NMF component manufactured by Technoble Co., Ltd.
[C component]
Perfume
The components A and B were each heated to 80 ° C. or higher and then mixed by stirring. After this was cooled to 50 ° C., component C was added and further stirred and mixed to obtain a cream.
実施例2.乳液
[A成分] 部
流動パラフィン 6.0
ヘキサラン 4.0
ホホバ油 1.0
ポリオキシエチレン(20)ソルビタンモノステアレート 2.0
大豆レシチン 1.5
メチルパラベン 0.15
エチルパラベン 0.03
[B成分]
製造例1の抽出液 5.0
グリセリン 3.0
1,3−ブチレングリコール 2.0
カルボキシメチルセルロース 0.3
ヒアルロン酸ナトリウム 0.01
精製水 全量が100部となる量
[C成分]
香料 適量
上記のA成分とB成分をそれぞれ80℃以上に加熱した後、攪拌混合した。これを50℃まで冷却した後、C成分を加えてさらに攪拌混合して乳液を得た。
Example 2 Emulsion [Component A] Part Liquid paraffin 6.0
Hexalan 4.0
Jojoba oil 1.0
Polyoxyethylene (20) sorbitan monostearate 2.0
Soy lecithin 1.5
Methylparaben 0.15
Ethylparaben 0.03
[B component]
Extraction liquid of Production Example 1 5.0
Glycerin 3.0
1,3-butylene glycol 2.0
Carboxymethylcellulose 0.3
Sodium hyaluronate 0.01
Amount of purified water totaling 100 parts
[C component]
Perfume
The components A and B were each heated to 80 ° C. or higher and then mixed by stirring. After cooling this to 50 ° C., component C was added and further stirred and mixed to obtain an emulsion.
実施例3.乳液
実施例2のB成分中、製造例1の抽出液に代えて製造例6の抽出液5.0部を用いるほかは実施例2と同様にして乳液を得た。
Example 3 FIG. Emulsion An emulsion was obtained in the same manner as in Example 2 except that 5.0 parts of the extract of Production Example 6 was used instead of the extract of Production Example 1 in the component B of Example 2.
実施例4.ローション
[A成分] 部
製造例1の抽出液 5.0
エタノール 10.0
グリセリン 3.0
1,3−ブチレングリコール 2.0
メチルパラベン 0.2
クエン酸 0.1
クエン酸ナトリウム 0.3
カルボキシビニルポリマー 0.1
香料 適量
水酸化カリウム 適量
精製水 全量が100部となる量
上記の成分を混合してローションを得た。
Example 4 Lotion [component A] part Extraction liquid of Production Example 1 5.0
Ethanol 10.0
Glycerin 3.0
1,3-butylene glycol 2.0
Methylparaben 0.2
Citric acid 0.1
Sodium citrate 0.3
Carboxyvinyl polymer 0.1
Perfume
Potassium hydroxide appropriate amount Purified water Amount that makes 100 parts in total
The above ingredients were mixed to obtain a lotion.
実施例5.化粧水
[A成分] 部
オリーブ油 1.0
ポリオキシエチレン(5.5)セチルアルコール 5.0
ブチルパラベン 0.1
[B成分]
製造例1の抽出液 5.0
エタノール 5.0
グリセリン 5.0
1,3−ブチレングリコール 5.0
メチルパラベン 0.1
水酸化カリウム 適量
精製水 全量が100部となる量
[C成分]
香料 適量
A成分及びB成分をそれぞれ80℃以上に加温後、A成分にB成分を加えて攪拌し、さらにヒスコトロン(5000rpm)で2分間ホモジナイズを行った。これを50℃まで冷却した後、C成分を加えて攪拌混合し、さらに30℃以下まで冷却して化粧水を得た。
Example 5 FIG. Lotion [A component] part olive oil 1.0
Polyoxyethylene (5.5) cetyl alcohol 5.0
Butylparaben 0.1
[B component]
Extraction liquid of Production Example 1 5.0
Ethanol 5.0
Glycerin 5.0
1,3-butylene glycol 5.0
Methylparaben 0.1
Potassium hydroxide appropriate amount Purified water Amount that makes 100 parts in total
[C component]
Perfume
After each component A and component B was heated to 80 ° C. or higher, the component B was added to the component A and stirred, and further homogenized with Hiscotron (5000 rpm) for 2 minutes. After cooling this to 50 degreeC, C component was added and stirred and mixed, and also it cooled to 30 degrees C or less, and the lotion was obtained.
実施例6.化粧水
実施例5のB成分中、製造例1の抽出液に代えて製造例6の抽出液5.0部を用いるほかは実施例5と同様にして乳液を得た。
Example 6 Lotion lotion A milky lotion was obtained in the same manner as in Example 5 except that 5.0 parts of the extract of Production Example 6 was used instead of the extract of Production Example 1 in the component B of Example 5.
実施例7.乳液
[A成分] 部
流動パラフィン 6.0
ヘキサラン 4.0
ホホバ油 1.0
ポリオキシエチレン(20)ソルビタンモノステアレート 2.0
大豆レシチン 1.5
メチルパラベン 0.15
エチルパラベン 0.03
[B成分]
製造例1の抽出液 5.0
L−アスコルビン酸−2−グルコシド 2.0
水酸化カリウム 0.5
グリセリン 3.0
1,3−ブチレングリコール 2.0
カルボキシメチルセルロース 0.3
ヒアルロン酸ナトリウム 0.01
精製水 全量が100部となる量
[C成分]
香料
適量
上記のA成分とB成分をそれぞれ80℃以上に加熱した後、攪拌混合した。これを50℃まで冷却した後、C成分を加えてさらに攪拌混合して乳液を得た。
Example 7 Emulsion [Component A] Part Liquid paraffin 6.0
Hexalan 4.0
Jojoba oil 1.0
Polyoxyethylene (20) sorbitan monostearate 2.0
Soy lecithin 1.5
Methylparaben 0.15
Ethylparaben 0.03
[B component]
Extraction liquid of Production Example 1 5.0
L-ascorbic acid-2-glucoside 2.0
Potassium hydroxide 0.5
Glycerin 3.0
1,3-butylene glycol 2.0
Carboxymethylcellulose 0.3
Sodium hyaluronate 0.01
Amount of purified water totaling 100 parts
[C component]
Fragrance
Appropriate amount
The components A and B were each heated to 80 ° C. or higher and then mixed by stirring. After cooling this to 50 ° C., component C was added and further stirred and mixed to obtain an emulsion.
実施例8.乳液
実施例5のB成分中、L−アスコルビン酸−2−グルコシド2.0部及び水酸化カリウム0.5部に代えてL−アスコルビン酸−2−リン酸エステルマグネシウム2.0部を用いるほかは実施例と同様にして乳液を得た。
Example 8 FIG. Emulsion Other than using 2.0 parts of L-ascorbic acid-2-phosphate magnesium in place of 2.0 parts of L-ascorbic acid-2-glucoside and 0.5 parts of potassium hydroxide in the component B of Example 5. Obtained an emulsion in the same manner as in Example.
実施例9.乳液
実施例5のB成分中、L−アスコルビン酸−2−グルコシド2.0部及び水酸化カリウム0.5部に代えてL−アスコルビン酸−2−リン酸エステルナトリウム2.0部を用いるほかは実施例5と同様にして乳液を得た。
Example 9 Emulsion In addition to using 2.0 parts of L-ascorbic acid-2-phosphate and 2.0 parts of L-ascorbic acid-2-phosphate in place of 2.0 parts of L-ascorbic acid-2-glucoside and 0.5 parts of potassium hydroxide in the component B of Example 5 Obtained an emulsion in the same manner as in Example 5.
実施例10.乳液
実施例5のB成分中、L−アスコルビン酸−2−グルコシド2.0部及び水酸化カリウム0.5部に代えてアルブチン2.0部を用いるほかは実施例5と同様にして乳液を得た。
Example 10 Emulsion In the component B of Example 5, the emulsion was prepared in the same manner as in Example 5 except that 2.0 parts of arbutin was used instead of 2.0 parts of L-ascorbic acid-2-glucoside and 0.5 parts of potassium hydroxide. Obtained.
実施例11.乳液
実施例5のB成分中、L−アスコルビン酸−2−グルコシド2.0部及び水酸化カリウム0.5部に代えて米糠抽出物加水分解物(株式会社テクノーブル製、商品名「グレイスノウ*雪*HP」、固形分濃度3.5%)5.0部を用いるほかは実施例5と同様にして乳液を得た。
Example 11 Latex In the component B of Example 5, in place of 2.0 parts of L-ascorbic acid-2-glucoside and 0.5 parts of potassium hydroxide, a rice bran extract hydrolyzate (trade name “Grace Snow” manufactured by Technoble Co., Ltd.) An emulsion was obtained in the same manner as in Example 5 except that 5.0 parts of * Snow * HP ", solid concentration 3.5%) were used.
実施例12.乳液
実施例5のB成分中、L−アスコルビン酸−2−グルコシド2.0部及び水酸化カリウム0.5部に代えて白芥子抽出物(株式会社テクノーブル製、商品名「シナブランカ−WH」、固形分濃度1.0%)5.0部を用いるほかは実施例5と同様にして乳液を得た。
Example 12 Emulsion White coconut extract (trade name “Sinablanca-WH” manufactured by Technoble Co., Ltd.) instead of 2.0 parts of L-ascorbic acid-2-glucoside and 0.5 part of potassium hydroxide in the B component of Example 5 A solid emulsion was obtained in the same manner as in Example 5 except that 5.0 parts of a solid content concentration of 1.0% was used.
実施例13.乳液
実施例5のB成分中、L−アスコルビン酸−2−グルコシド2.0部及び水酸化カリウム0.5部に代えてγ−アミノ−β−ヒドロキシ酪酸1.0部を用いるほかは実施例5と同様にして乳液を得た。
Example 13 Emulsion Example 5 in the component B of Example 5, except that 2.0 parts of L-ascorbic acid-2-glucoside and 0.5 part of potassium hydroxide were used instead of 1.0 part of γ-amino-β-hydroxybutyric acid In the same manner as in No. 5, an emulsion was obtained.
実施例14.リクイドファンデーション
[A成分] 部
ステアリン酸 2.4
モノステアリン酸プロピレングリコール 2.0
セトステアリルアルコール 0.2
液状ラノリン 2.0
流動パラフィン 3.0
ミリスチン酸イソプロピル 8.5
プロピルパラベン 0.05
[B成分]
製造例1の抽出液 5.0
カルボキシメチルセルロースナトリウム 0.2
ベントナイト 0.5
プロピレングリコール 4.0
トリエタノールアミン 1.1
メチルパラベン 0.1
精製水 全量が100部となる量
[C成分]
酸化チタン 8.0
タルク 4.0
着色顔料 適量
上記のA成分とB成分をそれぞれ加温した後混合攪拌した。これを再加温し、上記のC成分を添加して型に流し込み、室温になるまで攪拌してリクイドファンデーションを得た。
Example 14 Liquid foundation [component A] part Stearic acid 2.4
Propylene glycol monostearate 2.0
Cetostearyl alcohol 0.2
Liquid lanolin 2.0
Liquid paraffin 3.0
Isopropyl myristate 8.5
Propylparaben 0.05
[B component]
Extraction liquid of Production Example 1 5.0
Sodium carboxymethylcellulose 0.2
Bentonite 0.5
Propylene glycol 4.0
Triethanolamine 1.1
Methylparaben 0.1
Purified water Amount of total 100 parts [C component]
Titanium oxide 8.0
Talc 4.0
Coloring pigment appropriate amount The components A and B were heated and mixed and stirred. This was reheated, the above C component was added, poured into a mold, and stirred until it reached room temperature to obtain a liquid foundation.
実施例15.クリームファンデーション
[A成分] 部
ステアリン酸 5.0
セタノール 2.0
モノステアリン酸グリセリル 3.0
流動パラフィン 5.0
スクワラン 3.0
ミリスチン酸イソプロピル 8.0
ポリオキシエチレン(20)モノステアリン酸グリセリル 2.0
プロピルパラベン 0.1
[B成分]
製造例1の抽出液 5.0
ソルビトール 3.0
1,3−ブチレングリコール 5.0
トリエタノールアミン 1.5
メチルパラベン 0.1
精製水 全量が100部となる量
[C成分]
酸化チタン 8.0
タルク 2.0
カオリン 5.0
ベントナイト 1.0
着色顔料 適 量
[D成分]
香料 0.3
C成分を混合し、粉砕機で粉砕した。B成分を混合し、これに粉砕したC成分を加え、コロイドミルで均一分散させた。A成分及び均一分散させたB、C成分をそれぞれ80℃に加温後、B、C成分にA成分を攪拌しながら加え、さらにヒスコトロン(5000rpm)で2分間ホモジナイズを行った。これを50℃まで冷却した後、D成分を加えて攪拌混合し、さらに攪拌しながら30℃以下まで冷却してクリームファンデーションを得た。
Example 15. Cream foundation [component A] part Stearic acid 5.0
Cetanol 2.0
Glyceryl monostearate 3.0
Liquid paraffin 5.0
Squalane 3.0
Isopropyl myristate 8.0
Polyoxyethylene (20) glyceryl monostearate 2.0
Propylparaben 0.1
[B component]
Extraction liquid of Production Example 1 5.0
Sorbitol 3.0
1,3-butylene glycol 5.0
Triethanolamine 1.5
Methylparaben 0.1
Purified water Amount of total 100 parts [C component]
Titanium oxide 8.0
Talc 2.0
Kaolin 5.0
Bentonite 1.0
Coloring pigment appropriate amount [Component D]
Fragrance 0.3
Component C was mixed and pulverized with a pulverizer. The component B was mixed, and the pulverized component C was added thereto and uniformly dispersed in a colloid mill. The components A and B and C dispersed uniformly were each heated to 80 ° C., and then the components A were added to the components B and C while stirring, and further homogenized with Hiscotron (5000 rpm) for 2 minutes. After cooling this to 50 degreeC, D component was added and stirred and mixed, and also it cooled to 30 degrees C or less, stirring, and obtained the cream foundation.
実施例16.ボディシャンプー
[A成分] 部
N−ラウロイルメチルアラニンナトリウム 25.0
ヤシ油脂肪酸カリウム液(40%) 26.0
ヤシ油脂肪酸ジエタノールアミド 3.0
メチルパラベン 0.1
[B成分]
製造例1の抽出液 5.0
1,3−ブチレングリコール 2.0
精製水 全量が100部となる量
A成分及びB成分をそれぞれ80℃に加温して均一に溶解した後、A成分にB成分を加え、攪拌を続けて室温まで冷却してボディシャンプーを得た。
Example 16 Body shampoo [component A] part N-lauroylmethylalanine sodium 25.0
Palm oil fatty acid potassium liquid (40%) 26.0
Palm oil fatty acid diethanolamide 3.0
Methylparaben 0.1
[B component]
Extraction liquid of Production Example 1 5.0
1,3-butylene glycol 2.0
Purified water Amount to be 100 parts A component and B component are each heated to 80 ° C and dissolved uniformly, then B component is added to A component and stirring is continued to cool to room temperature to obtain a body shampoo It was.
試験例1.チロシナーゼ活性抑制作用(チロシン−チロシナーゼ反応法)
まず、マックイルベイン緩衝液(pH6.8)を用いて125U/mLのチロシナーゼ酵素液を調製した。次に、精製水を用いて製造例1のシャクヤクの花部の抽出液をその終濃度が0.5%及び1.0%になるように調製した後、当該液を96ウェルマイクロプレートに100μL/ウェルずつ添加した。これに、0.03%L−チロシン溶液を同じく100μL/ウェルずつ添加し、十分に混合した。これに前記チロシナーゼ酵素液を100μL/ウェルずつ添加して十分に混合し、この溶液の波長490nmにおける吸光度を直ちに測定した後に、室温で反応させ、10分経過後、再び波長490nmにおける吸光度を測定し、下式からチロシナーゼ活性指数を求めた。また、処理物の代わりに30%1,3−ブチレングリコール溶液(精製水/1,3−ブチレングリコール=70/30)を用いて同様に操作したものをブランクとした。
チロシナーゼ活性指数=[(T10−T0)/(B10−B0)]×100(%)
(式中、T10は試験開始から10分間経過後の試料が添加された溶液の吸光度、B10は試験開始から10分間経過後の試料の代わりに30%1,3−ブチレングルコール溶液が添加された溶液の吸光度、T0は試験開始直後の試料が添加された溶液の吸光度、B0は試験開始直後の試料のかわりに30%1,3−ブチレングルコール溶液が添加された溶液の吸光度を示す)。
Test Example 1 Tyrosinase activity inhibitory action (tyrosine-tyrosinase reaction method)
First, a 125 U / mL tyrosinase enzyme solution was prepared using McIlvain buffer (pH 6.8). Next, after preparing the peony flower part extract of Production Example 1 so as to have final concentrations of 0.5% and 1.0% using purified water, 100 μL of the solution was added to a 96-well microplate. Per well. To this, 0.03% L-tyrosine solution was similarly added at 100 μL / well and mixed well. 100 μL / well of the tyrosinase enzyme solution was added thereto and mixed well. The absorbance of the solution was measured immediately at a wavelength of 490 nm, reacted at room temperature, and after 10 minutes, the absorbance at a wavelength of 490 nm was measured again. The tyrosinase activity index was determined from the following equation. Moreover, what was operated similarly using a 30% 1,3- butylene glycol solution (purified water / 1,3-butylene glycol = 70/30) instead of the treated product was used as a blank.
Tyrosinase activity index = [(T 10 −T 0 ) / (B 10 −B 0 )] × 100 (%)
(In the formula, T 10 is the absorbance of a solution to which a sample after 10 minutes has passed since the start of the test, and B 10 is a 30% 1,3-butylene glycol solution instead of the sample after 10 minutes from the start of the test. The absorbance of the added solution, T 0 is the absorbance of the solution to which the sample immediately after the start of the test was added, and B 0 is the solution to which 30% 1,3-butylene glycol solution was added instead of the sample immediately after the start of the test. Absorbance is shown).
試験例1の結果を表1に示す。
[表1]
The results of Test Example 1 are shown in Table 1.
[Table 1]
表1に示すように、製造例1のシャクヤクの花部の抽出液は、濃度依存的に格段にすぐれたチロシナーゼ活性抑制作用を有することが明らかとなった。なお、陽性対照のアルブチンも同様にチロシナーゼ活性抑制作用が認められたことから、本実験系が正常であることも確認された。 As shown in Table 1, it was revealed that the peony flower part extract of Production Example 1 has a remarkably excellent tyrosinase activity inhibitory effect in a concentration-dependent manner. In addition, since the positive control arbutin also showed a tyrosinase activity inhibitory action, it was also confirmed that this experimental system was normal.
試験例2.細胞内チロシナーゼ活性抑制作用
[試験方法]
培養B16−F10マウスメラノーマ細胞を、96穴マイクロプレートに8×103個/穴播種し、10%仔牛血清(FBS)含有RPMI培地中、37℃、5%CO2の条件下に1日間プレ培養した後、10%FBS含有RPMI培地で製造例1のシャクヤクの花部の抽出液をその終濃度が0.1%及び0.5%となるように希釈した液に置換し、同条件で2日間培養した。次に培養液を除去し、0.3mg/mLのMTT溶液を添加するか、又は、界面活性剤(Triton X-100)と5mMのLドーパ溶液を添加して37℃で反応を行った後、マイクロプレートリーダー(Model 450、バイオラッド社製)を用い、波長570−630nmでMTT値を、波長490nmでドーパ値をそれぞれ測定した。
なお、比較のため、PBS(−)の添加の場合及びコウジ酸の添加の場合(陽性対照)についても同様の試験を行った。
Test Example 2 Inhibition of intracellular tyrosinase activity [Test method]
Cultured B16-F10 mouse melanoma cells are seeded at 8 × 10 3 cells / well in a 96-well microplate and pre-treated for 1 day under conditions of 37 ° C. and 5% CO 2 in RPMI medium containing 10% calf serum (FBS). After culturing, the extract of the peony flower part of Production Example 1 was replaced with a solution diluted to a final concentration of 0.1% and 0.5% in an RPMI medium containing 10% FBS. Cultured for 2 days. Next, after removing the culture solution and adding 0.3 mg / mL MTT solution or adding a surfactant (Triton X-100) and 5 mM L-dopa solution and reacting at 37 ° C. The MTT value was measured at a wavelength of 570-630 nm and the dopa value was measured at a wavelength of 490 nm using a microplate reader (Model 450, manufactured by Bio-Rad).
For comparison, the same test was performed with PBS (-) and with kojic acid (positive control).
結果を表2に示す。
[表2]
The results are shown in Table 2.
[Table 2]
表2に示すように、製造例1のシャクヤクの花部の抽出液は、細胞にダメージを与えることなく、濃度依存的に格段にすぐれたチロシナーゼ活性抑制作用を有することが明らかとなった。なお、陽性対照のコウジ酸も同様にチロシナーゼ活性抑制作用が認められたことから、本実験系が正常であることも確認された。 As shown in Table 2, it was revealed that the peony flower part extract of Production Example 1 has a remarkable tyrosinase activity inhibitory effect in a concentration-dependent manner without damaging cells. The positive control kojic acid was also found to have a normal tyrosinase activity-inhibiting action, confirming that this experimental system was normal.
試験例3.DPPHラジカル消去試験
まず、DPPH 2.4部をエタノール20部に溶解後、精製水20部を加えてDPPH溶液を調製した。このDPPH溶液24部に対して、18v/v%エタノール溶液を19.2部、2M酢酸−酢酸ナトリウム緩衝液(pH5.5)を4.8部加えて、DPPH添加溶液として調製した。また、抽出液そのものの色調が試験に及ぼす影響を差し引くため、DPPH溶液の代わりに50v/v%エタノール溶液を用いて、18v/v%エタノール溶液と2M酢酸−酢酸ナトリウム緩衝液を混合した液を対照液とした。
製造例1のシャクヤクの花部の抽出液を精製水で希釈してその終濃度が0.1%、1.0%及び10.0%になるように調製した液を試験溶液とし、この試験溶液とDPPH添加溶液又は対照液とを1:3の割合で混合し、室温で10分静置後、各試験溶液をDPPH添加溶液と混合した場合の550nmにおける吸光度と、同じく各試験溶液を対照液と混合した場合の550nmにおける吸光度との差を測定し、DPPHラジカルの残存量を確認した。
また、同時にコントロールとして製造例1のシャクヤクの花部の抽出液の代わりに、30%1,3−ブチレングリコール溶液を用いて上記と同様の操作を行い、ここに得られるDPPHラジカル残存率に対する各試料添加時のDPPHラジカル残存率の相対値を求め、DPPHラジカル残存率とした。また、試験系が正常に機能しているかを確認するために、試料溶液の代わりに陽性対照としてビタミンE(終濃度5μM)を添加した場合についても、同様の試験を行った。
Test Example 3 DPPH radical scavenging test First, 2.4 parts of DPPH was dissolved in 20 parts of ethanol, and then 20 parts of purified water was added to prepare a DPPH solution. To 24 parts of this DPPH solution, 19.2 parts of 18 v / v% ethanol solution and 4.8 parts of 2M acetic acid-sodium acetate buffer (pH 5.5) were added to prepare a DPPH addition solution. In addition, in order to subtract the effect of the color of the extract itself on the test, a 50 v / v% ethanol solution was used instead of the DPPH solution, and a solution obtained by mixing an 18 v / v% ethanol solution and a 2M acetic acid-sodium acetate buffer solution was used. A control solution was used.
A test solution was prepared by diluting the peony flower extract of Production Example 1 with purified water to a final concentration of 0.1%, 1.0%, and 10.0%. The solution and DPPH-added solution or control solution were mixed at a ratio of 1: 3, allowed to stand at room temperature for 10 minutes, and the absorbance at 550 nm when each test solution was mixed with DPPH-added solution and each test solution were also controlled. The difference in absorbance at 550 nm when mixed with the liquid was measured to confirm the remaining amount of DPPH radicals.
In addition, as a control, instead of the peony flower part extract of Production Example 1, a 30% 1,3-butylene glycol solution was used in the same manner as described above, and each DPPH radical residual rate obtained here was measured. The relative value of the DPPH radical residual rate at the time of sample addition was determined and used as the DPPH radical residual rate. Moreover, in order to confirm whether the test system is functioning normally, the same test was also performed when vitamin E (final concentration 5 μM) was added as a positive control instead of the sample solution.
結果を表3に示す。
[表3]
The results are shown in Table 3.
[Table 3]
表3に示すように、製造例1のシャクヤクの花部の抽出液は、濃度依存的に、格段にすぐれたDPPHラジカル消去作用を有することが明らかとなった。なお、陽性対照のビタミンEも同様にDPPHラジカル消去作用を示したことから、本実験系が正常であることも確認された。 As shown in Table 3, it was revealed that the peony flower part extract of Production Example 1 has a significantly superior DPPH radical scavenging action in a concentration-dependent manner. In addition, since the positive control vitamin E similarly showed DPPH radical scavenging action, it was confirmed that this experimental system was normal.
試験例4.活性酸素消去能(SOD様活性)
[試験方法]
0.2Mトリス塩酸緩衝液50μL、1mMエチレンジアミン四酢酸(EDTA)二ナトリウム溶液20μL、0.75mMニトロブルーテトラゾリウムクロリド(NBT)溶液10μL、1mMキサンチン溶液20μL、0.06U/mLキサンチンオキシターゼ溶液50μL、製造例1のシャクヤクの花部の抽出液50μL(その終濃度が1.0%及び2.0%になるように調製した抽出液)を混合して試料溶液を調製した。この試料溶液を37℃、5分間インキュベートし、スーパーオキシドを発生させた。そして、NBTがスーパーオキシドによって還元されて生成するホルマザン量を560nmにおける吸光度を測定した。
また、コントロールとして製造例1のシャクヤクの花部の抽出液の代わりに、30%1,3−ブチレングリコール溶液を用いて上記と同様の操作を行い、ここに得られる吸光度に対する各試料添加時の吸光度の相対値を求め、スーパーオキシド残存率(%)とした。また、試験系が正常に機能しているかを確認するために、試料溶液の代わりに陽性対照として、スーパーオキシドジスムターゼ(SOD)8.75units/mLを添加した場合についても、同様の試験を行った。
Test Example 4 Active oxygen scavenging ability (SOD-like activity)
[Test method]
0.2 μM Tris-HCl buffer solution 50 μL, 1 mM ethylenediaminetetraacetic acid (EDTA) disodium solution 20 μL, 0.75 mM nitroblue tetrazolium chloride (NBT) solution 10 μL, 1 mM xanthine solution 20 μL, 0.06 U / mL xanthine oxidase solution 50 μL, production A sample solution was prepared by mixing 50 μL of the peony flower part extract of Example 1 (extracts prepared to have final concentrations of 1.0% and 2.0%). This sample solution was incubated at 37 ° C. for 5 minutes to generate superoxide. Then, the absorbance at 560 nm was measured for the amount of formazan produced by reducing NBT with superoxide.
Further, as a control, instead of the extract of the peony flower part of Production Example 1, the same operation as described above was performed using a 30% 1,3-butylene glycol solution, and each sample was added to the absorbance obtained here. The relative value of the absorbance was determined and used as the superoxide residual rate (%). In addition, in order to confirm whether the test system is functioning normally, the same test was performed when 8.75 units / mL of superoxide dismutase (SOD) was added as a positive control instead of the sample solution. .
[表4]
[Table 4]
表5に示すように、製造例1のシャクヤクの花部の抽出液は、濃度依存的に格段にすぐれたSOD様作用を有することが明らかとなった。なお、陽性対照のSODも同様の効果を示したことから、本実験系が正常であることも確認された。 As shown in Table 5, it has been clarified that the peony flower part extract of Production Example 1 has an excellent SOD-like action in a concentration-dependent manner. Since the positive control SOD also showed the same effect, it was also confirmed that this experimental system was normal.
試験例5.エラスターゼ活性抑制試験
[試験方法]
<調製溶液>
(1)10容量%NCS含有イーグルMEM
(2)細胞溶解液
(3)基質溶液
<調製方法>
(1)イーグルMEM培地(日水製薬(株)製)9.4gに蒸留水1Lを加え、それぞれ終濃度10容量%NCS(仔牛血清)、1.4重量%炭酸水素ナトリウム、0.03重量%グルタミン酸を添加して調製する。
(2)1mM PMSF、1% TritonX−100を100mM
Tris−HCl(pH 8.0)に溶解した。
(3)スクシニル-L-アラニル-L-アラニル-L-アラニン-p-ニトロアニリド(Suc-Ala-Ala-Ala-pNA)を100mM
Tris−HCl(pH 8.0)に溶解した。
<測定方法>
製造例1のシャクヤクの花部の抽出液を5.0%の濃度(溶液として)となるよう希釈して試料溶液に調製した。なお、試料無添加(コントロール)として、5%PBS(−)溶液を使用した。
正常ヒト皮膚由来線維芽細胞(NB1RGB)を10容量%NCS含有イーグルMEMにて1×105個/mLに調製し、96穴マイクロプレートに100μLずつ播種して、5%炭酸ガス、飽和水蒸気下、37℃で培養した。48時間後、培養液を除去し、PBS(−)で細胞を1回洗浄した後、細胞溶解液を50μL添加し室温で10分間静置することにより細胞を溶解し、これを酵素液として用いた。96穴マイクロプレートに、酵素液50μLに対して製造例1のシャクヤクの花部の抽出液を精製水で希釈してその終濃度が5.0%になるように調製した試料溶液を50μL添加し、さらに、基質溶液を100μLずつ添加後、37℃で、暗所で2時間反応させた。ブランクとしては酵素液の代わりに細胞溶解液を試験に供した。その後、プレートリーダーで、405nmにおける反応後の吸光度を測定した。各吸光度の測定値から以下の式(1)を用いて、エラスターゼ活性率を算出した。なお、陽性対照として、0.037%のEDTAを試料溶液として用いて同様の試験を行った。
式(1):線維芽細胞エラスターゼ活性率(%)= (Es-Esb)/(Ec-Ecb)×100
Ec;コントロール(PBS(-))の試験区の吸光度
Ecb;コントロール(PBS(-))のブランク区の吸光度
Es;試料溶液を添加した試験区の吸光度
Esb;試料溶液を添加したブランク区の吸光度
Test Example 5 Elastase activity inhibition test [Test method]
<Prepared solution>
(1) Eagle MEM containing 10% NCS
(2) Cell lysate (3) Substrate solution <Preparation method>
(1) 1 L of distilled water was added to 9.4 g of Eagle MEM medium (manufactured by Nissui Pharmaceutical Co., Ltd.), and the final concentration was 10% by volume NCS (calf serum), 1.4% by weight sodium bicarbonate, 0.03% by weight, respectively. Prepare by adding% glutamic acid.
(2) 1 mM PMSF, 1% Triton X-100 at 100 mM
Dissolved in Tris-HCl (pH 8.0).
(3) 100 mM succinyl-L-alanyl-L-alanyl-L-alanine-p-nitroanilide (Suc-Ala-Ala-Ala-pNA)
Dissolved in Tris-HCl (pH 8.0).
<Measurement method>
The extract of the peony flower part of Production Example 1 was diluted to a concentration of 5.0% (as a solution) to prepare a sample solution. In addition, 5% PBS (-) solution was used as a sample non-addition (control).
Normal human skin-derived fibroblasts (NB1RGB) were prepared to 1 × 10 5 cells / mL with Eagle's MEM containing 10% by volume of NCS, seeded at 100 μL each in a 96-well microplate, and under 5% carbon dioxide gas and saturated water vapor. And cultured at 37 ° C. After 48 hours, the culture solution was removed, and the cells were washed once with PBS (−). Then, 50 μL of the cell lysate was added and left at room temperature for 10 minutes to lyse the cells, and this was used as an enzyme solution. It was. To a 96-well microplate, add 50 μL of the sample solution prepared by diluting the peony flower extract of Production Example 1 with purified water to a final concentration of 5.0% with respect to 50 μL of the enzyme solution. Further, 100 μL each of the substrate solution was added, followed by reaction at 37 ° C. in the dark for 2 hours. As a blank, a cell lysate was used for the test instead of the enzyme solution. Thereafter, the absorbance after the reaction at 405 nm was measured with a plate reader. The elastase activity rate was calculated from the measured value of each absorbance using the following formula (1). As a positive control, a similar test was performed using 0.037% EDTA as a sample solution.
Formula (1): Fibroblast elastase activity rate (%) = (Es-Esb) / (Ec-Ecb) × 100
Ec: Absorbance of control (PBS (-)) test group Ecb: Absorbance of control (PBS (-)) blank group Es; Absorbance of test group to which sample solution was added Esb; Absorbance of blank group to which sample solution was added
[結果]
試験例5の結果を表5に示す。
[表5]
[result]
The results of Test Example 5 are shown in Table 5.
[Table 5]
表5に示すように、製造例1のシャクヤクの花部の抽出液は、格段にすぐれたエラスターゼ活性阻害作用を有することが明らかとなった。なお、陽性対照であるEDTAも同様の効果を示したことから、本実験系が正常であることも確認された。 As shown in Table 5, it was revealed that the peony flower part extract of Production Example 1 had a remarkable elastase activity inhibitory action. In addition, since EDTA which is a positive control showed the same effect, it was also confirmed that this experimental system is normal.
試験例6.コラゲナーゼ活性抑制効果
0.25ng/mLのIL−1αを用いて、MMP(マトリックスメタロプロテアーゼ)の合成誘導した線維芽細胞(NB1RGB)の培養上清をコラゲナーゼ酵素液として用いた。コラゲナーゼ酵素液に5μg/mLトリプシンを添加し30分間37℃で反応させ活性化処理を行い、50μg/mLトリプシンインヒビターで反応を停止後の液をコラゲナーゼ活性化酵素液とした。コラゲナーゼ活性の測定は、I型コラゲナーゼアッセイキット(株式会社プライマリーセル製品)を応用して測定を行った。マイクロチューブに上記コラゲナーゼ活性化酵素液を50μL、FITCラベルされたI型コラーゲン基質液50μL、その終濃度が5.0%になるように調製した製造例1のシャクヤクの花部の抽出液50μLを添加した。37℃で30分間反応度、反応停止液300μLを添加し、遠心分離により未反応のコラーゲン基質を沈殿させ、上清の蛍光強度(Ex=485,Em=520)を測定した。
上記シャクヤクの花部の抽出液の代わりに精製水を添加した区(対照)についても同様の操作を行い、この対照に対する蛍光強度の相対値をコラゲナーゼ活性率(%)とした。また、試験系が正常に機能しているかを確認するために、上記試料溶液の代わりに陽性対照として1mMのEDTAを添加した場合についても、同様の試験を行った。
Test Example 6. Collagenase activity inhibitory effect
The culture supernatant of fibroblasts (NB1RGB) in which MMP (matrix metalloproteinase) synthesis was induced using 0.25 ng / mL of IL-1α was used as a collagenase enzyme solution. 5 μg / mL trypsin was added to the collagenase enzyme solution and reacted at 37 ° C. for 30 minutes for activation treatment. The solution after stopping the reaction with 50 μg / mL trypsin inhibitor was used as a collagenase activating enzyme solution. The collagenase activity was measured by applying a type I collagenase assay kit (Primary Cell product, Inc.). In a microtube, 50 μL of the collagenase activating enzyme solution, 50 μL of a FITC-labeled type I collagen substrate solution, and 50 μL of the peony flower part extract of Production Example 1 prepared so that its final concentration is 5.0%. Added. The reactivity was 30 minutes at 37 ° C., 300 μL of a reaction stop solution was added, unreacted collagen substrate was precipitated by centrifugation, and the fluorescence intensity (Ex = 485, Em = 520) of the supernatant was measured.
The same operation was performed for the group (control) to which purified water was added instead of the extract of the peony flower part, and the relative value of the fluorescence intensity relative to this control was defined as the collagenase activity rate (%). Moreover, in order to confirm whether the test system is functioning normally, the same test was performed when 1 mM EDTA was added as a positive control instead of the sample solution.
[表6]
[Table 6]
表6に示すように、製造例1のシャクヤクの花部の抽出液は、格段にすぐれたコラゲナーゼ活性抑制作用を有することが明らかとなった。なお、陽性対照であるEDTAも同様の効果を示したことから、本実験系が正常であることも確認された。 As shown in Table 6, it was revealed that the peony flower part extract of Production Example 1 has a markedly excellent collagenase activity inhibitory action. In addition, since EDTA which is a positive control showed the same effect, it was also confirmed that this experimental system is normal.
試験例7.ゼラチナーゼ活性阻害効果
0.25ng/mLIL−1αを用いて、MMP(マトリックスメタロプロテアーゼ)の合成誘導した線維芽細胞(NB1RGB)の培養上清をゼラチナーゼ酵素液として用いた。ゼラチナーゼ酵素液に5μg/mLトリプシンを添加し30分間37℃で反応させ活性化処理を行い、50μg/mLトリプシンインヒビターで反応を停止後の液をゼラチナーゼ活性化酵素液とした。96ウェルマイクロプレートにゼラチナーゼ活性化酵素液120μL、製造例1のシャクヤクの花部の抽出液をその終濃度が5.0%になるように調製した溶液10μL添加した後、1μg/mL
基質溶液(MOCAc-pro-leu-gly-leu-a2pr(DNP) -ala-arg-NH2,ペプチド研究所)を20μL添加し、初期の蛍光強度 (Ex=355nm、Em=460nm) を測定してから30分間室温で反応させた。30分後の蛍光強度から初期値を引いた増加量を求めた。上記シャクヤクの花部の抽出液の代わりに精製水を添加した区(対照)についても同様の操作を行い、この対照に対する蛍光強度の増加量の相対値をゼラチナーゼ活性率(%)とした。また、試験系が正常に機能しているかを確認するために、試料溶液の代わりに陽性対照として1mMのEDTAを添加した場合についても、同様の試験を行った。
Test Example 7 The culture supernatant of fibroblasts (NB1RGB) in which MMP (matrix metalloprotease) synthesis was induced using 0.25 ng / mL IL-1α with gelatinase activity inhibitory effect was used as the gelatinase enzyme solution. 5 μg / mL trypsin was added to the gelatinase enzyme solution, and the mixture was reacted at 37 ° C. for 30 minutes for activation treatment. The solution after stopping the reaction with 50 μg / mL trypsin inhibitor was used as a gelatinase-activating enzyme solution. After adding 120 μL of gelatinase activating enzyme solution and 96 μL of the peony flower part extract of Production Example 1 to a 96-well microplate, the final concentration is 5.0%, and then 1 μg / mL.
Add 20 μL of substrate solution (MOCAc-pro-leu-gly-leu-a2pr (DNP) -ala-arg-NH 2 , Peptide Institute) and measure the initial fluorescence intensity (Ex = 355 nm, Em = 460 nm). The reaction was allowed to proceed for 30 minutes at room temperature. The increase amount obtained by subtracting the initial value from the fluorescence intensity after 30 minutes was determined. The same operation was performed for the group (control) to which purified water was added instead of the peonies flower part extract, and the relative value of the increase in fluorescence intensity relative to this control was defined as the gelatinase activity rate (%). Moreover, in order to confirm whether the test system is functioning normally, the same test was performed when 1 mM EDTA was added as a positive control instead of the sample solution.
[表7]
[Table 7]
表7に示すように、製造例1のシャクヤクの花部の抽出液は、格段にすぐれたゼラチナーゼ活性抑制作用を有することが明らかとなった。なお、陽性対照であるEDTAも同様の効果を示したことから、本実験系が正常であることも確認された。 As shown in Table 7, it was revealed that the peony flower part extract of Production Example 1 has a remarkable gelatinase activity inhibitory action. In addition, since EDTA which is a positive control showed the same effect, it was also confirmed that this experimental system is normal.
また、製造例6のボタンの花部の抽出液についても、試験例1〜7の評価試験を行ったところ、製造例1のシャクヤクの花部の抽出液と同様にすぐれたチロシナーゼ活性抑制効果、抗酸化効果、及びMMP(エラスターゼ、コラゲナーゼ及びゼラチナーゼ)活性抑制効果が認められた。 Moreover, also about the extract of the flower part of the button of Production Example 6, when the evaluation test of Test Examples 1 to 7 was performed, the tyrosinase activity inhibitory effect excellent as in the extract of the flower part of Peony of Production Example 1, Antioxidant effects and MMP (elastase, collagenase and gelatinase) activity inhibitory effects were observed.
Claims (3)
A method for producing a cosmetic comprising a step of extracting from a peony or a flower part of a button belonging to the genus Paeoniaceae with a solvent obtained from a mixed solvent of water and 1,3-butylene glycol. A method for producing a cosmetic, characterized in that the ratio of solvent water to 1,3-butylene glycol is 1: 1 to 20: 1.
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