JP5983908B2 - Anti-inflammatory agents and skin preparations - Google Patents
Anti-inflammatory agents and skin preparations Download PDFInfo
- Publication number
- JP5983908B2 JP5983908B2 JP2007341983A JP2007341983A JP5983908B2 JP 5983908 B2 JP5983908 B2 JP 5983908B2 JP 2007341983 A JP2007341983 A JP 2007341983A JP 2007341983 A JP2007341983 A JP 2007341983A JP 5983908 B2 JP5983908 B2 JP 5983908B2
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- Prior art keywords
- skin
- acid
- camellia
- inflammation
- defatted
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Landscapes
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Description
本発明は、ツバキ科ツバキ属に属するツバキ(Camellia japonica)の種子の脱脂粕の水性成分を有効成分として配合することを特徴とする抗炎症剤及びこれを用いる皮膚外用品の製造方法に関する。本発明の抗炎症剤は紫外線照射により引き起こされる皮膚の炎症を抑制するためのTGF−β1増強剤を意味する。TECHNICAL FIELD The present invention relates to an anti-inflammatory agent characterized by containing an aqueous component of defatted cocoons of camellia (Camellia japonica) seeds belonging to the camellia family as an active ingredient, and a method for producing an external skin product using the same. The anti-inflammatory agent of the present invention means a TGF-β1 enhancer for suppressing skin inflammation caused by ultraviolet irradiation.
近年の地球環境の変化(温暖化、オゾン層の破壊等)にともない、地球上の生物が受ける紫外線量は、現在は概ね許容範囲内にあるとされながらも増加傾向にあり、人においては、従来の皮膚美容のみならず健康に対する影響に関心が高まっている。すなわち、紫外線は肌に対してシミ、そばかす、黒皮等の色素沈着、シワ、たるみ等の皮膚組織の老化を誘発及び促進し、又、とりわけ欧米地域では皮膚癌の多発が懸念されている。With recent changes in the global environment (warming, destruction of the ozone layer, etc.), the amount of ultraviolet rays received by organisms on the earth is currently increasing, although it is generally within an acceptable range. There is growing interest in health effects as well as conventional skin beauty. That is, ultraviolet rays induce and promote aging of skin tissues such as stains, freckles, and black skin pigmentation, wrinkles, sagging, and the like, and there is a concern that skin cancer frequently occurs particularly in the western region.
紫外線が皮膚に及ぼす影響について次のようなことが知られている。太陽光に含まれる紫外線のうち、長波長の紫外線(400nm〜320nm、UV−A)は、細胞の物質代謝に関与して細胞機能を活性化させ、皮膚の日焼け(褐色化)を生じさせる。又、真皮層に作用して蛋白質を変性させ、コラーゲンやエラスチンを変性させて皮膚の弾力性を失わせてシワやたるみの原因をつくり、皮膚の老化を促進する。光毒性あるいは光アレルギー反応を誘発する場合もあり、UV−Bによって生成されるメラニン色素を酸化して褐色に変化させる。中波長の紫外線(320nm〜280nm、UV−B)は、表皮層に作用するが、色素細胞がメラニンを生成して生体組織を防御する。肌を赤く日焼け(サンバーン)させ、炎症、紅斑、水泡を生じさせ、シミ、ソバカス等の形成の一因であると考えられている。又、大量に浴びると免疫低下、皮膚癌、白内障等を誘発するといわれている。短波長の紫外線(280nm未満、UV−C)は強い殺菌作用を有し、生体に対する破壊性が最も強いが、290nm以下の紫外線は大気圏のオゾン、大気中の酸素や窒素によって吸収されるため地上には到達しない。The following is known about the effect of ultraviolet rays on the skin. Among ultraviolet rays contained in sunlight, long-wavelength ultraviolet rays (400 nm to 320 nm, UV-A) are involved in cellular metabolism of the cells to activate cell functions and cause skin tanning (browning). In addition, it acts on the dermis layer to denature proteins and collagen and elastin to denature the skin, thereby causing skin wrinkles and sagging to promote skin aging. In some cases, phototoxicity or photoallergic reaction is induced, and the melanin pigment produced by UV-B is oxidized to turn brown. Medium wavelength ultraviolet light (320 nm to 280 nm, UV-B) acts on the epidermis layer, but pigment cells generate melanin to protect living tissues. It is considered that the skin is tanned (sunburn) red, causing inflammation, erythema and blisters, and contributing to the formation of spots, freckles and the like. In addition, it is said that a large amount of exposure induces immune decline, skin cancer, and cataract. Short wavelength ultraviolet rays (less than 280 nm, UV-C) have a strong bactericidal action and are most destructive to living organisms, but ultraviolet rays below 290 nm are absorbed by atmospheric ozone, oxygen and nitrogen in the atmosphere, so Will not reach.
かかる紫外線とりわけUV−AやUV−Bによる皮膚障害を予防、改善又は治療するために、従来の皮膚外用剤には桂皮酸系化合物、アミノ安息香酸誘導体、ベンゾフェノン誘導体、サリチル酸系化合物、ウロカニン酸誘導体等の紫外線吸収剤、酸化亜鉛、酸化チタン等の紫外線遮蔽剤が利用されてきた。しかしながら、例えば、桂皮酸系誘導体には光毒性を示すものがあり、アミノ安息香酸類は変色や樹脂状物質に変性することがある等安全性や安定性、使用性、コスト等の問題から、必ずしも十分な効果が得られていたわけではなかった。又、皮膚の炎症を抑制するために吉草酸ベタメタゾン、トリアムシノロンアセトニド等のステロイド系薬剤やイブプロフェンピコノール、ベンダザック等の非ステロイド系薬剤が従来から利用されてきたが、免疫力の低下、発疹、発赤等の副作用を示すものがあり、医師の指導のもとで適切に使用する必要がある等の制限条件が多く、十分満足できるものではなかった。In order to prevent, ameliorate, or treat skin damage caused by ultraviolet rays, particularly UV-A and UV-B, conventional skin external preparations include cinnamic acid compounds, aminobenzoic acid derivatives, benzophenone derivatives, salicylic acid compounds, urocanic acid derivatives. UV absorbers such as zinc oxide and titanium oxide have been used. However, for example, some cinnamic acid derivatives exhibit phototoxicity, and aminobenzoic acids may be discolored or denatured into a resinous substance, for example, because of safety, stability, usability, cost, etc. A sufficient effect was not obtained. In addition, steroidal drugs such as betamethasone valerate and triamcinolone acetonide and nonsteroidal drugs such as ibuprofen piconol and bendazac have been used for the purpose of suppressing skin inflammation. However, some of them show side effects such as redness, and there are many restrictive conditions such as the need to use them appropriately under the guidance of a doctor, and they are not satisfactory.
一方、ツバキについては次のようなことが知られている。すなわち、ツバキは古来より観賞用園芸植物として利用されてきた歴史があり、種子から採取した油脂は燃料油、整髪料、高級食用油等に、木部は灰化して日本酒の醸造に、又、種子の脱脂粕は農作物の肥料等に利用されてきた。ツバキ種子から採取した油は、その構成脂肪酸としてオレイン酸を豊富に含み、小児アトピーのようなアレルギー症状を軽減するという報告がある(非特許文献1)。又、脱脂粕にはサポニンやタンニンが含まれ、これを加工して殺虫防虫剤(特許文献1)、農園芸用線虫防除剤(特許文献2)、乳化剤(特許文献3)等となす提案もある。しかしながら、種子の脱脂粕に含まれる成分を生体組織の炎症の抑制のために用いる例は見当たらない。On the other hand, the following is known about camellia. That is, camellia has a history of being used as an ornamental horticultural plant since ancient times, and fats and oils collected from seeds are used as fuel oil, hair styling, high-grade edible oil, etc., and xylem is ashed to brew sake. Seed defatted lees have been used as fertilizers for agricultural crops. There is a report that oil collected from camellia seeds is rich in oleic acid as a constituent fatty acid and reduces allergic symptoms such as childhood atopy (Non-patent Document 1). In addition, defatted cocoons contain saponins and tannins, which are processed to become insecticides (Patent Document 1), agricultural and horticultural nematode control agents (Patent Document 2), emulsifiers (Patent Document 3), etc. There is also. However, there is no example in which the components contained in the defatted cocoons of seeds are used for suppressing inflammation of living tissues.
かかる現状に鑑み、本発明者らは、紫外線、活性酸素、加齢等を起因とする皮膚組織の炎症を軽減及び/又は回復させ、皮膚の前記トラブルを予防及び/又は改善するための、安全かつ安定な素材を開発し、これを利用した皮膚外用品を提供することを課題とした。In view of the current situation, the present inventors have proposed a safety for reducing and / or recovering skin tissue inflammation caused by ultraviolet rays, active oxygen, aging, etc., and preventing and / or improving the skin troubles. In addition, we developed a stable material and provided an external skin product using this material.
前記課題を解決するために、本発明者らは、紫外線照射による皮膚組織の炎症を軽減させる素材について鋭意検討を重ねた結果、前記皮膚トラブルを改善するためにはツバキが極めて有効であり、ツバキには紫外線照射による炎症を軽減し、皮膚の老化症状を顕著に改善し得る成分が含まれていること、又、これを化粧料等の皮膚外用品に有効利用できることを見出し、本発明を完成するに至った。In order to solve the above problems, the present inventors have made extensive studies on materials that reduce skin tissue inflammation caused by ultraviolet irradiation, and as a result, camellia is extremely effective in improving the skin trouble. Has found that it contains ingredients that can reduce inflammation caused by UV irradiation and can significantly improve skin aging symptoms, and that it can be effectively used in cosmetics and other external skin products. It came to do.
すなわち、本発明によれば、ツバキ科ツバキ属に属するツバキ(Camellia japonica)の種子の脱脂粕の水性成分を有効成分として含有してなる抗炎症剤が提供される。That is, according to the present invention, there is provided an anti-inflammatory agent comprising, as an active ingredient, an aqueous component of defatted camellia seeds of Camellia japonica belonging to the genus Camellia.
この抗炎症剤においては、有効成分がツバキ科ツバキ属に属するツバキ(Camellia japonica)の種子の脱脂粕を水及び/又は低級アルコールで抽出処理した抽出物であることが望ましく、さらには前記水性成分の加水分解生成物が少なくともケンフェロールを含有するものであることがより一層望ましい。又、抗炎症が血液中のIL−1β濃度を低減させる作用に基づくものであるか、及び/又は、血液中又は皮膚組織中のTGF−β1濃度を増大させる作用に基づくものであることが望ましく、本発明ではこの両作用を満足するものが最も望ましい。炎症は紫外線照射により引き起こされるものを対象にすることがより好適である。In this anti-inflammatory agent, the active ingredient is preferably an extract obtained by extracting defatted cocoons of camellia (Camellia japonica) seeds with water and / or a lower alcohol, and further, the aqueous component. It is even more desirable that the hydrolysis product of at least contain kaempferol. It is also desirable that anti-inflammation is based on the action of reducing the IL-1β concentration in the blood and / or is based on the action of increasing the TGF-β1 concentration in the blood or skin tissue. In the present invention, it is most desirable to satisfy both of these actions. It is more preferable to target inflammation caused by ultraviolet irradiation.
本発明によれば、又、前記抗炎症剤を含有してなることを特徴とする、皮膚の炎症を抑制するための皮膚外用品が提供される。ここで、皮膚の炎症は紫外線照射によって引き起こされるものであることが望ましい。According to the present invention, there is also provided an external skin product for suppressing skin inflammation, comprising the anti-inflammatory agent. Here, it is desirable that the skin inflammation is caused by ultraviolet irradiation.
本発明によれば、更に、ツバキ科ツバキ属に属するツバキ(Camellia japonica)の種子の脱脂粕の水性成分を皮膚に塗布及び/又は接触することを特徴とする、紫外線暴露によって生じる皮膚の炎症を軽減するための方法が提供される。ここで、前記水性成分は、ツバキ科ツバキ属に属するツバキ(Camellia japonica)の種子の脱脂粕を水及び/又は低級アルコールで抽出処理した抽出物であることが望ましく、さらにはその加水分解処理物が少なくともケンフェロールを含むものがより望ましい。又、炎症の軽減は血液中のIL−1β濃度を低減させる作用に基づくものであるか、及び/又は、血液中又は皮膚組織中のTGF−β1濃度を増大させる作用に基づくものであることが望ましく、この両作用を満たすものが最も望ましい。According to the present invention, skin inflammation caused by exposure to ultraviolet rays, further characterized by applying and / or contacting the skin with an aqueous component of camellia japonica seed defatted camellia belonging to the genus Camellia japonica A method for mitigating is provided. Here, the aqueous component is preferably an extract obtained by extracting defatted cocoons of Camellia japonica seeds with water and / or a lower alcohol, and further hydrolyzed product thereof. It is more desirable that at least contains kaempferol. In addition, the reduction of inflammation may be based on the action of decreasing the IL-1β concentration in the blood and / or the effect of increasing the TGF-β1 concentration in the blood or skin tissue. Desirably, those satisfying both of these effects are most desirable.
本発明に係るツバキ(Camellia japonica)の種子の脱脂粕から抽出された水性成分は、品質安定性に優れ、これを皮膚に塗布することにより、血中IL−1β濃度を低減させる作用を呈し、及び/又は,血中又は皮膚組織中のTGF−β1濃度を増加させる作用を呈することによって、紫外線照射による皮膚の炎症を顕著に抑制する効果を奏する。そして、本発明に係る前記水性成分を配合してなる、皮膚の炎症、とりわけ紫外線照射によって引き起こされる炎症を軽減するための皮膚外用品が提供される。The aqueous component extracted from the camellia (Camellia japonica) seed defatted lees according to the present invention is excellent in quality stability and exhibits an action of reducing blood IL-1β concentration by applying it to the skin. And / or by exhibiting the effect | action which increases the TGF- (beta) 1 density | concentration in blood or skin tissue, there exists an effect which suppresses the inflammation of the skin by ultraviolet irradiation notably. And the external skin goods for reducing the inflammation of the skin formed by mix | blending the said aqueous component which concerns on this invention, especially the inflammation caused by ultraviolet irradiation are provided.
以下に本発明を詳細に説明する。まず、本発明の抗炎症剤は、紫外線暴露によって生じる皮膚の炎症を軽減させる機能を有するものであり、ツバキ科(Theaceae)のツバキ属(Camellia)に属するツバキ(Camellia japonica)の種子の脱脂粕の水性成分を有効成分として含有してなることを特徴とする。The present invention is described in detail below. First, the anti-inflammatory agent of the present invention has a function of reducing skin inflammation caused by exposure to ultraviolet rays, and the defatted pods of camellia (Camellia japonica) seeds belonging to the genus Camellia of Theaceae The aqueous component is contained as an active ingredient.
ツバキ属に属する植物として、一般に、ツバキ節に属するツバキ(Camellia japonica)等、チャ節に属するチャ(C.sinensis)等、サザンカ節に属するサザンカ(C.sasanqua)等、カワリバツバキ節に属するグランサムツバキ(C.granthamiana)等、ヤナギバサザンカ節に属するヤナギバサザンカ(C.salicifolia)等、ヒメサザンカ節に属するヒメサザンカ(C.lutchuensis)等が知られているが、本発明ではツバキ節に属するものを用いる。この例としてヤブツバキ(C.japonica var.japonica)、ユキツバキ(C.japonica subsp.rusticana)、リンゴツバキ(C.japonica var.macrocarpa)、ホウザンツバキ(C.japonica subsp.hozanensis)、ホンコンツバキ(C.hongkongenesis)、トウツバキ(C.reticulata)、サルウィンツバキ(C.saluenensis)、ピタールツバキのピタルディー種(C.pitardii var.pitardii)及びユンナン種(C.pitardii var.yunnanica)、金花茶(C.nitidissima)、ヤマツバキ(ヤブツバキと同種)、山茶花(ヤブツバキと同種)、ヤクシマツバキ(リンゴツバキと同種)等を挙げることができる。これらのツバキは日本列島、朝鮮半島、中国山東半島等で自生し又は栽培されているものを適宜に利用すればよい。As the plant belonging to the camellia genus, generally, the camellia camellia camellia (Camelia japonica), the tea belonging to the tea section (C. sinensis), the sasanqua (C. sasanqua), etc. (C. granthamiana), etc., areowed sasanqua (C. salicifolia), and so on, and in the present invention, those that belong to camellia are known. Use. Examples of this are C. japonica var. Japonica, C. japonica subsp. Rusticana, C. japonica var. Macrocarpa, C. japonich. Hong Konggenesis, C. reticulata, C. salenensis, Pitaldi var. pitaldi, and C. partidi var. yunnica C, p. Yamabe camellia (same kind as Ayaba camellia), mountain tea flower (same kind as Ayers camellia), Kushimatsubaki can be mentioned (apple camellia and the like) and the like. What is necessary is just to utilize suitably these camellia which are growing naturally in the Japanese archipelago, the Korean peninsula, the Shandong peninsula of China, etc.
本発明では、前記のツバキの種子を圧搾処理、ヘキサンやヘプタン等の疎水性有機溶媒又は液化二酸化炭素、液化プロパン等の液化ガスを用いた抽出処理に供して、常法により油分を抽出した残渣である脱脂粕を必須の原料とする。ここで、ツバキの種子は早熟実及び成熟実のいずれに由来するものでもよいが、脱脂粕及び有効成分の収量の点から成熟実からのものを用いることが望ましく、種子あるいは種子及び果皮を含む実全体を用いることができる。本発明では、成熟実全体あるいは種子を1〜2週間程度、天日等で乾燥させたものを用いるのがよい。In the present invention, the above-mentioned camellia seeds are subjected to a compression treatment, an extraction treatment using a hydrophobic organic solvent such as hexane or heptane, or a liquefied gas such as liquefied carbon dioxide or liquefied propane, and a residue obtained by extracting oil by a conventional method. This is the essential raw material. Here, the camellia seeds may be derived from either early-ripening seeds or matured seeds, but it is preferable to use seeds from mature seeds from the viewpoint of defatted straw and the yield of active ingredients, including seeds or seeds and peels. The whole can be used. In the present invention, it is preferable to use matured whole seeds or seeds dried for about 1-2 weeks in the sun.
前記脱脂粕の水性成分は任意の方法で製造することができるが、水及び/又は低級アルコールを用いて抽出処理するのが好ましい。低級アルコールは、その炭素数が大きくなると脱脂粕中の油性物質が抽出される傾向が大きくなるため、炭素数が小さいものが望ましく、メタノール、エタノール、ノルマルプロパノール、イソプロパノール、ノルマルブタノール、イソブタノール等を例示できる。炭素数が大きい低級アルコールを使用する場合は、脱脂粕中の油性成分の抽出を抑制するために含水率を高めるのがよい。例えば、プロパノールの場合の含水率は約20重量%〜約50重量%とし、ブタノールの場合の含水率は約40重量%〜約70重量%とする。望ましい抽出溶媒は水、メタノール及びエタノール、及びこれらの含水アルコール(含水率:0〜100重量%)である。The aqueous component of the defatted lees can be produced by any method, but it is preferable to extract it with water and / or lower alcohol. The lower alcohol has a tendency to extract the oily substance in the defatted soot as the carbon number increases, so that a lower carbon number is desirable, such as methanol, ethanol, normal propanol, isopropanol, normal butanol, isobutanol, etc. It can be illustrated. When using a lower alcohol having a large carbon number, it is preferable to increase the water content in order to suppress the extraction of oily components in the defatted soot. For example, the water content in the case of propanol is about 20 wt% to about 50 wt%, and the water content in the case of butanol is about 40 wt% to about 70 wt%. Desirable extraction solvents are water, methanol and ethanol, and water-containing alcohols thereof (water content: 0 to 100% by weight).
脱脂粕を抽出するには、脱脂粕1重量部に対して前記抽出溶媒を約1重量倍〜約30重量倍加え、常圧下又は1〜5気圧の加圧下、常温ないしは約120℃で、約10分〜約3時間、必要に応じて撹拌して混合後、常温に冷却して濾過し、濾液を減圧乾燥、噴霧乾燥、凍結乾燥等の適当な手段により濃縮、乾燥する。尚、乾燥物は適宜に粉砕処理してもよい。このようにして本発明に係る脱脂粕の水性成分である淡黄色ないし黄色の固体を得ることができる。前記抽出方法は、一旦抽出処理した抽出残渣を繰り返し抽出処理したり、1〜3気圧の加圧下、約100℃〜約130℃で行うことが望ましい。これにより本発明に係る水性成分の収量が増える。この水性成分はサポニン、タンニン、ケンフェロール、その配糖体等を含む。すなわち、本発明に係る水性成分は、これを加水分解すると少なくともケンフェロールを含む生成物が得られる。In order to extract the defatted lees, the extraction solvent is added in an amount of about 1 to 30 times by weight with respect to 1 part by weight of the defatted lees, at about normal temperature or 1 to 5 atm. After stirring and mixing for 10 minutes to about 3 hours as necessary, the mixture is cooled to room temperature and filtered, and the filtrate is concentrated and dried by an appropriate means such as drying under reduced pressure, spray drying or freeze drying. The dried product may be appropriately pulverized. In this way, a light yellow to yellow solid which is an aqueous component of the defatted soot according to the present invention can be obtained. The extraction method is preferably performed by repeatedly extracting the extraction residue once extracted, or under a pressure of 1 to 3 atmospheres at about 100 ° C. to about 130 ° C. This increases the yield of the aqueous component according to the present invention. This aqueous component includes saponins, tannins, kaempferol, glycosides thereof and the like. That is, when the aqueous component according to the present invention is hydrolyzed, a product containing at least kaempferol is obtained.
本発明の抗炎症剤は、前記水性成分を有効成分として、これに必要に応じて公知の賦形剤、結合剤、崩壊剤、潤沢剤、希釈剤等、例えば、後述のような糖類、糖アルコール類、澱粉類、セルロース類、精製水等を適量混合して、固体状、ペースト状又は液体状の形態に加工することができる。本発明の抗炎症剤における前記有効成分の含量は約0.1重量%〜100重量%であり、より好ましくは約10重量%〜約80重量%である。約0.1重量%を下回ると本発明の抗炎症剤を利用する皮膚外用品において所望の効果を発現しなくなることがある。The anti-inflammatory agent of the present invention contains the aqueous component as an active ingredient, and, as necessary, known excipients, binders, disintegrants, lubricants, diluents, etc. Alcohols, starches, celluloses, purified water and the like can be mixed and processed into a solid, paste or liquid form. The content of the active ingredient in the anti-inflammatory agent of the present invention is about 0.1 wt% to 100 wt%, more preferably about 10 wt% to about 80 wt%. If it is less than about 0.1% by weight, the desired effect may not be exhibited in an external skin product using the anti-inflammatory agent of the present invention.
本発明の皮膚外用品は、前記抗炎症剤をそのまま皮膚外用品としてもよいが、必要に応じて通常の皮膚外用剤に利用される公知の添加物を併用して、常法により含有せしめて組成物として調製することが望ましい。ここで、公知の添加物としては、医薬品、化粧品、トイレタリー製品等に利用されるものであって且つ本発明の趣旨に反しないものであればよく、例えば、賦形剤、結合剤、崩壊剤、滑沢剤、湿潤剤、流動化剤、保存剤、界面活性剤、安定剤、希釈剤、溶解剤、殺菌剤、防腐剤、着色剤、香料等の各種添加物質を使用することができる。In the external skin preparation of the present invention, the anti-inflammatory agent may be used as it is as an external skin preparation, but if necessary, a known additive used for an ordinary external skin preparation may be used in combination with a conventional method. It is desirable to prepare it as a composition. Here, the known additive may be any one that is used in pharmaceuticals, cosmetics, toiletry products, etc. and does not violate the gist of the present invention. For example, excipients, binders, disintegrants Various additives such as lubricants, wetting agents, fluidizing agents, preservatives, surfactants, stabilizers, diluents, solubilizers, bactericides, preservatives, colorants, and fragrances can be used.
前記の公知添加物のうち、賦形剤の例としてセルロース及びその誘導体、澱粉、化工澱粉、デキストリン、難消化性デキストリン、乳糖、マンニトール、ソルビトール等の糖アルコール類、第二リン酸カルシウム、マイカ、タルク等が挙げられる。Among the above-mentioned known additives, examples of excipients include cellulose and derivatives thereof, starch, modified starch, dextrin, resistant digestive dextrin, sugar alcohols such as lactose, mannitol, sorbitol, dicalcium phosphate, mica, talc, etc. Is mentioned.
結合剤や崩壊剤としては結晶セルロース、メチルセルロース、エチルセルロース、ヒドロキシプロピルセルロース、カルボキシメチルセルロース、ヒドロキシプロピルメチルセルロースアセテートサクシネート、カルメロースナトリウム等のセルロース系誘導体、小麦、米、トウモロコシ、馬鈴薯等由来の澱粉、これらのα化澱粉、部分α化澱粉、ヒドロキシプロピルスターチ等の化工澱粉、デキストリン、プルラン、ポリビニルピロリドン、アミノアルキルメタクリレートコポリマー、メタクリル酸コポリマー、ポリビニルアセタールジエチルアミノアセテート、ポリビニルアルコール、アラビアゴム、寒天、ゼラチン、白色セラック、トラガント、マクロゴール等を例示できる。Binders and disintegrators include cellulose derivatives such as crystalline cellulose, methylcellulose, ethylcellulose, hydroxypropylcellulose, carboxymethylcellulose, hydroxypropylmethylcellulose acetate succinate, carmellose sodium, starch derived from wheat, rice, corn, potato, etc. Pregelatinized starch, partially pregelatinized starch, modified starch such as hydroxypropyl starch, dextrin, pullulan, polyvinylpyrrolidone, aminoalkyl methacrylate copolymer, methacrylic acid copolymer, polyvinyl acetal diethylaminoacetate, polyvinyl alcohol, gum arabic, agar, gelatin, white Examples include shellac, tragacanth, and macro goal.
滑沢剤として、例えば、小麦、米、トウモロコシ、馬鈴薯等由来の澱粉、ステアリン酸、ステアリン酸カルシウム、ステアリン酸マグネシウム、含水二酸化ケイ素、軽質無水ケイ酸、合成ケイ酸アルミニウム、乾燥水酸化アルミニウムゲル、タルク、メタケイ酸アルミン酸マグネシウム、リン酸水素カルシウム、無水リン酸水素カルシウム、ショ糖脂肪酸エステル、ロウ類、水素添加植物油、ポリエチレングリコール等がある。As a lubricant, for example, starch derived from wheat, rice, corn, potato, stearic acid, calcium stearate, magnesium stearate, hydrous silicon dioxide, light anhydrous silicic acid, synthetic aluminum silicate, dried aluminum hydroxide gel, talc , Magnesium aluminate metasilicate, calcium hydrogen phosphate, anhydrous calcium hydrogen phosphate, sucrose fatty acid ester, waxes, hydrogenated vegetable oil, polyethylene glycol and the like.
湿潤剤、保湿剤、エモリエント剤としては、スクワラン、スクワレン、レシチン、リゾレシチン、コレステロール、スフィンゴ脂質、セリン、グルタミン、ソルビトール、マンニトール、グリセリン、ピロリドンカルボン酸、1,3−ブチレングリコール、プロピレングリコール、ジプロピレングリコール、乳酸及びその塩、ヒアルロン酸、ヒアルロン酸ナトリウム、コラーゲン、水溶性コラーゲン、加水分解エラスチン、アルギン酸及びその塩、ムコ多糖類、ポリエチレングリコール、ポリアスパラギン酸塩、水溶性キチン、水溶性キトサン、グルコサミン類及びその誘導体、N−アセチル−D−グルコサミン、長鎖アシルグルタミン酸コレステリル、ヒドロキシステアリン酸コレステリル、硬化ヒマシ油、12−ヒドロキシステアリン酸、リシノール酸、ステアリン酸、ロジン酸、ラノリン、ラノリン脂肪酸コレステリルエステル、ミリスチン酸イソプロピル、パルミチン酸セチル、イソノナン酸イソノニル、シリコン油(メチコン、ジメチコン、シクロメチコン等)、乳ホエー等を例示することができる。Wetting agents, moisturizing agents, and emollients include squalane, squalene, lecithin, lysolecithin, cholesterol, sphingolipid, serine, glutamine, sorbitol, mannitol, glycerin, pyrrolidone carboxylic acid, 1,3-butylene glycol, propylene glycol, dipropylene Glycol, lactic acid and its salt, hyaluronic acid, sodium hyaluronate, collagen, water-soluble collagen, hydrolyzed elastin, alginic acid and its salt, mucopolysaccharide, polyethylene glycol, polyaspartate, water-soluble chitin, water-soluble chitosan, glucosamine And its derivatives, N-acetyl-D-glucosamine, cholesteryl long-chain acyl glutamate, cholesteryl hydroxystearate, hydrogenated castor oil, 12-hydroxystearic acid Ricinoleic acid, stearic acid, rosin acids, lanolin, lanolin fatty acid cholesteryl ester, isopropyl myristate, cetyl palmitate, isononyl isononanoate, silicone oils (cyclomethicone, dimethicone, cyclomethicone, etc.), can be exemplified milk whey, or the like.
流動化剤の例として、微粒二酸化ケイ素、含水二酸化ケイ素、軽質無水ケイ酸、乾燥水酸化アルミニウムゲル、合成ケイ酸アルミニウム、ケイ酸マグネシウム等が挙げられる。Examples of the fluidizing agent include fine silicon dioxide, hydrous silicon dioxide, light anhydrous silicic acid, dry aluminum hydroxide gel, synthetic aluminum silicate, magnesium silicate and the like.
酸化防止剤としては、アスコルビン酸、トコトリエノール、dl−α−トコフェロール、α−トコフェロール、γ−トコフェロール、δ−トコフェロール、酢酸トコフェロール等のトコフェロール類、クエン酸イソプロピル、エチレンジアミン四酢酸カルシウム二ナトリウム、ジブチルヒドロキシトルエン、フィチン酸、カフェ酸、カテキン、没食子酸、没食子酸プロピル、エリソルビン酸及びそのナトリウム塩、チオジプロピオン酸ジラウリル、L−システイン塩酸塩等を例示できる。Antioxidants include ascorbic acid, tocotrienol, dl-α-tocopherol, α-tocopherol, γ-tocopherol, δ-tocopherol, tocopherols such as tocopherol acetate, isopropyl citrate, ethylenediaminetetraacetate calcium disodium, dibutylhydroxytoluene Phytic acid, caffeic acid, catechin, gallic acid, propyl gallate, erythorbic acid and its sodium salt, dilauryl thiodipropionate, L-cysteine hydrochloride and the like.
保存剤や防腐剤の例として安息香酸、ソルビン酸、パラオキシ安息香酸、パラオキシ安息香酸メチル、パラオキシ安息香酸プロピル、パラオキシ安息香酸イソプロピル、プロピオン酸、亜硫酸ナトリウム、クロロブタノール等がある。Examples of preservatives and preservatives include benzoic acid, sorbic acid, paraoxybenzoic acid, methyl paraoxybenzoate, propyl paraoxybenzoate, isopropyl paraoxybenzoate, propionic acid, sodium sulfite, chlorobutanol and the like.
界面活性剤の例としては、大豆レシチン、卵黄レシチン、リゾレシチン、ホスファチジルコリン、ホスファチジルエタノールアミン、ホスファチジルイノシトール、ホスファチジルセリン等のグリセロリン脂質、ショ糖脂肪酸エステル、グリセリン脂肪酸エステル、ジグリセリン脂肪酸エステル等のポリグリセリン脂肪酸エステル、モノステアリン酸ソルビタン、セスキオレイン酸ソルビタン等のソルビタン脂肪酸エステル、ポリオキシエチレン高級アルコールエーテル、ポリオキシプロピレン高級アルコールエーテル、ポリオキシエチレン脂肪酸エステル、ポリオキシプロピレン脂肪酸エステル、ポリソルベート80、ポリオキシエチレンソルビタン脂肪酸エステル、ポリオキシエチレン硬化ヒマシ油等の非イオン界面活性剤、塩化ベンザルコニウム、塩化ステアリルトリメチルアンモニウム、塩化ジセチルジメチルアンモニウム、塩化ベヘニルトリメチルアンモニウム等のカチオン界面活性剤、2−ココイル−N−カルボキシメチル−N−ヒドロキシエチルイミダゾリニウムベタイン、アミド酢酸ベタイン等の両性界面活性剤、高級アルコール硫酸塩、高級アルコールエーテル硫酸塩、長鎖脂肪酸アルカリ金属塩、長鎖脂肪酸アルカリ土類金属塩、長鎖脂肪酸塩基性アミノ酸塩、N−長鎖アシルアミノ酸、N−長鎖アシルアミノ酸塩等のアニオン界面活性剤がある。Examples of surfactants include glycerophospholipids such as soybean lecithin, egg yolk lecithin, lysolecithin, phosphatidylcholine, phosphatidylethanolamine, phosphatidylinositol, phosphatidylserine, polyglycerin fatty acids such as sucrose fatty acid ester, glycerin fatty acid ester, diglycerin fatty acid ester Sorbitan fatty acid esters such as esters, sorbitan monostearate, sorbitan sesquioleate, polyoxyethylene higher alcohol ethers, polyoxypropylene higher alcohol ethers, polyoxyethylene fatty acid esters, polyoxypropylene fatty acid esters, polysorbate 80, polyoxyethylene sorbitan Nonionic surfactants such as fatty acid esters, polyoxyethylene hydrogenated castor oil, benzil chloride Cationic surfactants such as conium, stearyltrimethylammonium chloride, dicetyldimethylammonium chloride, and behenyltrimethylammonium chloride; amphoteric surface activities such as 2-cocoyl-N-carboxymethyl-N-hydroxyethylimidazolinium betaine and betaine amidoacetate Agent, higher alcohol sulfate, higher alcohol ether sulfate, long chain fatty acid alkali metal salt, long chain fatty acid alkaline earth metal salt, long chain fatty acid basic amino acid salt, N-long chain acyl amino acid, N-long chain acyl amino acid There are anionic surfactants such as salts.
安定剤としては、例えば、メチルパラベン、プロピルパラベン等のパラオキシ安息香酸エステル類、クロロブタノール、ベンジルアルコール、フェニルエチルアルコール等のアルコール類、塩化ベンザルコニウム、無水酢酸、ソルビン酸等が挙げられる。Examples of the stabilizer include paraoxybenzoates such as methylparaben and propylparaben, alcohols such as chlorobutanol, benzyl alcohol, and phenylethyl alcohol, benzalkonium chloride, acetic anhydride, sorbic acid, and the like.
希釈剤、溶解剤、可溶化剤として精製水、エタノール、ラウリル硫酸トリエタノールアミン、エチレングリコール、ジエチレングリコール、プロピレングリコール、ジプロピレングリコール、グリセリン、オリーブ油、ヒマシ油、シリコンオイル、流動パラフィン、シクロデキストリン等がある。Diluent, solubilizer, solubilizer, purified water, ethanol, lauryl sulfate triethanolamine, ethylene glycol, diethylene glycol, propylene glycol, dipropylene glycol, glycerin, olive oil, castor oil, silicone oil, liquid paraffin, cyclodextrin, etc. is there.
等張化剤の例として塩化ナトリウム、塩化カリウム、グリセリン、ホウ酸等がある。Examples of isotonic agents include sodium chloride, potassium chloride, glycerin, boric acid and the like.
pH調整剤としては、乳酸、コハク酸、フマル酸、クエン酸、リンゴ酸、酒石酸、グルコン酸、及びこれらのナトリウム塩又はカリウム塩、グルコノデルタラクトン、アジピン酸、酢酸ナトリウム、アルギニン、トリエタノールアミン、水酸化ナトリウム、水酸化カリウム、リン酸、リン酸二水素ナトリウム、リン酸水素三カリウム等が含まれる。Examples of pH adjusters include lactic acid, succinic acid, fumaric acid, citric acid, malic acid, tartaric acid, gluconic acid, and sodium or potassium salts thereof, glucono delta lactone, adipic acid, sodium acetate, arginine, triethanolamine. Sodium hydroxide, potassium hydroxide, phosphoric acid, sodium dihydrogen phosphate, tripotassium hydrogen phosphate and the like.
紫外線吸収剤は、例えば、パラアミノ安息香酸、パラジメチルアミノ安息香酸オクチル等のパラアミノ安息香酸誘導体、2−ヒドロキシ−4−メトキシベンゾフェノン、ジヒドロキシジメトキシベンゾフェノン等のベンゾフェノン誘導体、パラメトキシ桂皮酸エチル、パラメトキシ桂皮酸オクチル等のメトキシ桂皮酸誘導体、サリチル酸オクチル、サリチル酸ホモメンチル等のサリチル酸誘導体、N−ベンゾイル−O−メチル−α−デヒドロチロシン−2−エチルヘキシルエステル等のα−デヒドロアミノ酸誘導体、4−(3,4−ジメトキシフェニル)メチレン−2,5−ジオキソ−1−イミダゾリジンプロピオン酸2−エチルヘキシルエステル等のベンザールヒダントイン誘導体、ウロカニン酸、ウロカニン酸エチル、4−ter−ブチル−4’−メトキシジベンゾイルメタン、2−(2’−ヒドロキシ−5’−メチルフェニル)ベンゾトリアゾール等を挙げることができる。Examples of the ultraviolet absorber include paraaminobenzoic acid derivatives such as paraaminobenzoic acid and octylparadimethylaminobenzoate, benzophenone derivatives such as 2-hydroxy-4-methoxybenzophenone and dihydroxydimethoxybenzophenone, ethyl paramethoxycinnamate, and octyl paramethoxycinnamate. Methoxycinnamic acid derivatives such as octyl salicylate, salicylic acid derivatives such as homomenthyl salicylate, α-dehydroamino acid derivatives such as N-benzoyl-O-methyl-α-dehydrotyrosine-2-ethylhexyl ester, 4- (3,4-dimethoxy) Benzalhydantoin derivatives such as phenyl) methylene-2,5-dioxo-1-imidazolidinepropionic acid 2-ethylhexyl ester, urocanic acid, ethyl urocanate, 4-ter-butyl -4'-methoxydibenzoylmethane, 2- (2'-hydroxy-5'-methylphenyl) benzotriazole, and the like.
殺菌剤として、例えば、ヒノキチオール、トリクロサン、クロルヘキシジングルコン酸塩、フェノキシエタノール、レゾルシン、イソプロピルメチルフェノール、アズレン、サリチル酸、ジンクピリチオン等がある。Examples of the disinfectant include hinokitiol, triclosan, chlorhexidine gluconate, phenoxyethanol, resorcin, isopropylmethylphenol, azulene, salicylic acid, zinc pyrithione and the like.
着色剤の例として、酸化亜鉛、酸化チタン、酸化鉄、シリカ、タルク、マイカ、銅クロロフィル、水溶性アナトー、β−カロテン、リボフラビン及びその酪酸エステル、クチナシ黄、青色1号、赤色202号、食用赤色2号、同105号、食用黄色4号、食用緑色3号、食用青色2号等を挙げることができる。Examples of colorants include zinc oxide, titanium oxide, iron oxide, silica, talc, mica, copper chlorophyll, water-soluble anato, β-carotene, riboflavin and its butyrate, gardenia yellow, blue No. 1, red No. 202, edible Examples include Red No. 2, No. 105, Edible Yellow No. 4, Edible Green No. 3, Edible Blue No. 2, and the like.
その他、各種香料や植物エッセンスも必要に応じて利用でき、又、油脂類としてアボガド油、オリーブ油、ホホバ油等の植物油、オレイン酸、イソステアリン酸等の脂肪酸、ワセリン、ラノリン、セレシン、マイクロクリスタリンワックス、カルナバロウ、キャンデリラロウ、椰子油脂肪酸、ラウリン酸、硬化牛脂脂肪酸等の脂肪酸、2−エチルヘキサン酸セチル、ミリスチン酸イソプロピル、ミリスチン酸−2−オクチルドデシル、ジ−2−エチルヘキサン酸ネオペンチルグリコール、トリ−2−エチルヘキサン酸グリセロール、オレイン酸−2−オクチルドデシル、トリイソステアリン酸グリセロール、2−エチルヘキサン酸ジグリセリド等のエステル油、長鎖アシルグルタミン酸オクチルドデシルエステル等のエステル油、ジメチルポリシロキサン、メチルハイドロジェンポリシロキサン、メチルフェニルポリシロキサン、オクタメチルシクロテトラシロキサン等のシリコン油、流動パラフィン、スクワレン、スクワラン等の液状炭化水素油等も適宜に使用できる。尚、本発明はこれらの各例示によって何ら限定されるものではない。In addition, various fragrances and plant essences can be used as necessary, and as fats and oils, vegetable oils such as avocado oil, olive oil and jojoba oil, fatty acids such as oleic acid and isostearic acid, petrolatum, lanolin, ceresin, microcrystalline wax, Carnauba wax, candelilla wax, coconut oil fatty acid, lauric acid, hardened beef tallow fatty acid and other fatty acids, cetyl 2-ethylhexanoate, isopropyl myristate, 2-octyldodecyl myristate, neopentyl glycol di-2-ethylhexanoate, Ester oil such as glycerol tri-2-ethylhexanoate, oleic acid-2-octyldodecyl, glycerol triisostearate, 2-ethylhexanoic acid diglyceride, ester oil such as long chain acyl glutamic acid octyldodecyl ester, Siloxane, methyl hydrogen polysiloxane, methylphenyl polysiloxane, silicone oils such as octamethylcyclotetrasiloxane, liquid paraffin, can be used squalene, etc. in appropriate liquid hydrocarbon oils squalane. In addition, this invention is not limited at all by these each illustration.
本発明の皮膚外用品の形態は、特に限定されるものではなく、皮膚や毛髪・頭皮に適用されるもの全般を対象にして、ローション剤,乳剤,ゲル剤,クリーム剤,軟膏等の剤型で提供することができ、例えば、化粧水、乳液、クリーム、ファンデーション、パック、エッセンス、口紅、洗顔料、シャンプー、リンス、ヘアトニック、ヘアトリートメント等を挙げることができる。又、軟膏、パップ剤、浴用剤、洗浄剤、エアゾル剤等の医薬部外品を含めてもよい。The form of the external skin product of the present invention is not particularly limited, and is generally applied to the skin, hair and scalp, and is a dosage form such as a lotion, emulsion, gel, cream, ointment, etc. For example, lotion, emulsion, cream, foundation, pack, essence, lipstick, face wash, shampoo, rinse, hair tonic, hair treatment and the like can be mentioned. In addition, quasi-drugs such as ointments, poultices, bath preparations, cleaning agents and aerosols may be included.
本発明の皮膚外用品を製造するには、前記の公知添加物を適宜選択し、これに本発明に係る前記水性成分を所定量加え、通常の製造法により加工処理すればよい。ここで、本発明に係る前記水性成分の配合量は約0,01重量%〜約90重量%、より望ましくは約0.1重量%〜約70重量%である。約0.01重量%を下回ると本発明の皮膚外用品が所望効果を発現しない場合があり、約90重量%を超えると皮膚外用品としての通常の剤型を加工し難くなることがある。本発明の皮膚外用品は、その用途目的から、肌の炎症、とりわけ紫外線を多量に及び/又は長時間にわたり受ける際に生じる皮膚の炎症を予防及び/又は改善するために,皮膚や毛髪・頭皮に塗布したり接触させる方法で適宜使用することができる。In order to produce the skin external product of the present invention, the above-mentioned known additives are appropriately selected, and a predetermined amount of the above-mentioned aqueous component according to the present invention is added thereto, followed by processing by an ordinary production method. Here, the blended amount of the aqueous component according to the present invention is about 0.01 wt% to about 90 wt%, more desirably about 0.1 wt% to about 70 wt%. If the amount is less than about 0.01% by weight, the external skin product of the present invention may not exhibit the desired effect, and if it exceeds about 90% by weight, it may be difficult to process a normal dosage form as an external skin product. In order to prevent and / or ameliorate skin irritation, particularly skin irritation caused by exposure to a large amount of ultraviolet rays and / or over a long period of time, the external skin product of the present invention is used for its intended purpose. It can use suitably by the method of apply | coating to or contacting.
次に、実施例を挙げて本発明を詳細に説明するが、本発明はこれによって何ら限定されるものではない。各例において、%、部及び比率はいずれも重量基準である。Next, although an Example is given and this invention is demonstrated in detail, this invention is not limited at all by this. In each example, all the percentages, parts and ratios are based on weight.
製造例1
長崎県五島産ヤブツバキ(C.japonica var.japonica)の乾燥種子を粗粉砕して蒸煮後、圧搾して圧搾油を分離した圧搾粕を得、次いで圧搾粕にノルマルヘキサンを加えて常法により抽出処理し、抽出液を分離して抽出粕を採取した。この抽出粕をノルマルヘキサンで洗浄して油分を取り除き脱脂粕を採取した。この脱脂粕100gに水400mLを加え、常圧下、85℃に加熱して1時間適宜に撹拌した後、室温まで冷却し、濾過して濾液を分離した。この濾過残渣に再度水200mLを加えて同様に加熱し、冷却後、濾過して濾液を採取した。両濾液を合わせて減圧下に濃縮し、凍結乾燥及び粉砕して、本発明に係る水性成分を含む粉末(試料1とする)15.8gを得た。この粉末は、これを加水分解してHPLC分析したところ、サポニンのアグリコンであるサポゲニンを15.2%、フラボノールの一種であるケンフェロールを2.8%含むものであった。Production Example 1
After coarsely crushing dried seeds of C. japonica var. Japonica from Goto, Nagasaki Prefecture, steaming and then pressing to obtain a press knead separated from the compressed oil, followed by adding normal hexane to the press koji and extracting by a conventional method After processing, the extract was separated and the extract was collected. The extracted soot was washed with normal hexane to remove oil, and defatted soot was collected. 400 mL of water was added to 100 g of this defatted soot, heated to 85 ° C. under normal pressure and stirred for 1 hour as appropriate, then cooled to room temperature and filtered to separate the filtrate. 200 mL of water was again added to the filtration residue and heated in the same manner. After cooling, the filtrate was collected by filtration. Both filtrates were combined, concentrated under reduced pressure, lyophilized and pulverized to obtain 15.8 g of a powder (referred to as sample 1) containing an aqueous component according to the present invention. When this powder was hydrolyzed and analyzed by HPLC, it contained 15.2% sapogenin, which is an aglycon of saponin, and 2.8% kaempferol, which is a kind of flavonol.
製造例2
屋久島産リンゴツバキ(C.japonica var.macrocarpa)の乾燥種子を製造例1に記載の方法で脱脂して脱脂粕を採取した。この脱脂粕100gに水400mLを加え、2気圧の加圧下、120℃で25分間加熱した後、室温まで冷却し、濾過して濾液を分離した。この濾過残渣に再度水200mLを加えて同様に加熱し、冷却後、濾過して濾液を採取した。両濾液を合わせて減圧下に濃縮し、凍結乾燥及び粉砕して、本発明に係る水性成分を含む粉末(試料2とする)16.4gを得た。該粉末を製造例1と同様に加水分解してHPLC分析した結果、サポゲニン含量は13.7%であり、ケンフェロール含量は2.2%であった。Production Example 2
The dried seeds of Yakushima apple camellia (C. japonica var. Macrocarpa) were defatted by the method described in Production Example 1 and defatted cocoons were collected. 400 mL of water was added to 100 g of the defatted soot, and the mixture was heated at 120 ° C. for 25 minutes under a pressure of 2 atm, then cooled to room temperature and filtered to separate the filtrate. 200 mL of water was again added to the filtration residue and heated in the same manner. After cooling, the filtrate was collected by filtration. Both filtrates were combined, concentrated under reduced pressure, lyophilized and pulverized to obtain 16.4 g of a powder containing the aqueous component according to the present invention (referred to as sample 2). The powder was hydrolyzed in the same manner as in Production Example 1 and analyzed by HPLC. As a result, the sapogenin content was 13.7% and the kaempferol content was 2.2%.
製造例3
製造例1に記載の方法で得た脱脂粕100gに含水エタノール(含水率35%)300mLを加え、80℃で1時間加熱還流した後、室温まで冷却し、濾過して濾液を分離した。この濾過残渣に再度含水エタノール(含水率35%)200mLを加えて同様に加熱し、冷却後、濾過して濾液を採取した。両濾液を合わせて減圧下に濃縮し、凍結乾燥及び粉砕して、本発明に係る水性成分を含む粉末(試料3とする)11.3gを得た。該粉末を製造例1と同様に加水分解してHPLC分析した結果、サポゲニン含量は11.3%であり、ケンフェロール含量は2.7%』であった。Production Example 3
300 g of water-containing ethanol (water content 35%) was added to 100 g of the defatted lees obtained by the method described in Production Example 1, and the mixture was heated to reflux at 80 ° C. for 1 hour, cooled to room temperature, and filtered to separate the filtrate. To this filtration residue, 200 mL of water-containing ethanol (water content 35%) was added again and heated in the same manner. After cooling, the filtrate was collected by filtration. Both filtrates were combined, concentrated under reduced pressure, freeze-dried and pulverized to obtain 11.3 g of powder (referred to as sample 3) containing an aqueous component according to the present invention. The powder was hydrolyzed in the same manner as in Production Example 1 and analyzed by HPLC. As a result, the sapogenin content was 11.3% and the kaempferol content was 2.7%.
製造例4
製造例2に記載の方法で得た脱脂粕100gにエタノール(純度99.5%)300mLを加え、80℃で1時間加熱還流した後、室温まで冷却し、濾過して濾液を分離した。この濾過残渣に再度エタノール(純度99.5%)200mLを加えて同様に加熱し、冷却後、濾過して濾液を採取した。両濾液を合わせて減圧下に濃縮し、凍結乾燥及び粉砕して、本発明に係る水性成分を含む粉末(試料4とする)4.5gを得た。該粉末を製造例1と同様に加水分解してHPLC分析した結果、サポゲニン含量は13.0%であり、ケンフェロール含量は2.7%であった。Production Example 4
Ethanol (purity 99.5%) 300 mL was added to 100 g of the defatted lees obtained by the method described in Production Example 2, and the mixture was heated to reflux at 80 ° C. for 1 hour, cooled to room temperature, and filtered to separate the filtrate. 200 mL of ethanol (purity 99.5%) was again added to the filtration residue and heated in the same manner. After cooling, the filtrate was collected by filtration. Both filtrates were combined, concentrated under reduced pressure, freeze-dried and pulverized to obtain 4.5 g of a powder (referred to as sample 4) containing an aqueous component according to the present invention. The powder was hydrolyzed in the same manner as in Production Example 1 and analyzed by HPLC. As a result, the sapogenin content was 13.0% and the kaempferol content was 2.7%.
試験例1
本発明に係る水性成分を含む粉末(試料1〜試料4)が、紫外線暴露によって生じる皮膚の炎症の軽減に及ぼす影響を以下の方法で調べた。すなわち、ヘアレスマウス(HR−1/Hos、雄性、7週齢、36匹(1群6匹))を用い、その背部の一定面積部位に紫外線照射(UV−B、強度:30mJ/cm2、ATTO社製UVランプ使用)を1日1回、1回につき1分間の割合で7日間行った。この間毎日、紫外線照射直後に0.1%の濃度で精製水に溶かした被験物質(試料1〜試料4)水溶液又は精製水の各0.5mlを5×4cmの滅菌ガーゼに染み込ませ背部に塗布した。Test example 1
The effect of the powder (Sample 1 to Sample 4) containing the aqueous component according to the present invention on the reduction of skin inflammation caused by ultraviolet exposure was examined by the following method. That is, using hairless mice (HR-1 / Hos, male, 7 weeks old, 36 (6 mice per group)), ultraviolet irradiation (UV-B, intensity: 30 mJ / cm 2 ) on a certain area of the back part, ATTO UV lamp was used) once a day at a rate of 1 minute per time for 7 days. During this time, 0.5 ml each of test substance (sample 1 to sample 4) aqueous solution or purified water dissolved in purified water at a concentration of 0.1% immediately after UV irradiation is soaked in 5 x 4 cm sterile gauze and applied to the back. did.
紫外線照射部位の炎症度合いは肉眼観察によって判定した。さらに炎症性サイトカインのIL−1βと抗炎症性サイトカインのTGF−β1を測定した。血液中のIL−1β濃度及びTGF−β1濃度は、EDTAを添加した遠心管にマウス血液を採取し、遠心分離処理(4℃、3000回転、20分)により血漿を採取し、それぞれELISAキット(IL−1β(BIO SORCE社製)、TGF−β1(PROMEGA社製))を用いて測定した。皮膚組織中のTGF−β1濃度は、マウスを屠殺した後、背部の皮膚組織を採取し、ELISAキット中の緩衝液に懸濁し、冷却下にてホモジネートした後、遠心分離処理(室温、2000回転、15分)して上清を回収し、この上清中のTGF−β1濃度をELISAキット(PROMEGA社製)を用いて測定した。The degree of inflammation at the ultraviolet irradiation site was determined by visual observation. In addition, IL-1β as an inflammatory cytokine and TGF-β1 as an anti-inflammatory cytokine were measured. IL-1β concentration and TGF-β1 concentration in blood were collected by collecting mouse blood in a centrifuge tube to which EDTA was added, and collecting plasma by centrifugation (4 ° C., 3000 rpm, 20 minutes). IL-1β (manufactured by BIO SOURCE), TGF-β1 (manufactured by PROMEGA)). The TGF-β1 concentration in the skin tissue was determined by collecting the skin tissue on the back after slaughtering the mouse, suspending it in a buffer solution in an ELISA kit, homogenizing under cooling, and then centrifuging (room temperature, 2000 rpm). 15 minutes), the supernatant was recovered, and the TGF-β1 concentration in the supernatant was measured using an ELISA kit (manufactured by PROMEGA).
この結果を表1に示す。同表において、数値は同時に実施した紫外線非照射試験(紫外線を照射しない場合)の値を100としたときの相対値で示した。又、紫外線照射部位の炎症の度合いは、炎症なし:−、やや赤斑:+、赤斑と肌荒れ:++、肌荒れ・しわ形成:+++で表した。The results are shown in Table 1. In the table, the numerical value is shown as a relative value when the value of the ultraviolet ray non-irradiation test (when no ultraviolet ray is irradiated) carried out at the same time is taken as 100. In addition, the degree of inflammation at the site irradiated with ultraviolet rays was expressed as follows: no inflammation:-, slightly red spots: +, red spots and rough skin: ++, rough skin / wrinkle formation: ++.
この結果、紫外線を照射しなかった対照群では炎症の発生がなくシワ形成や肌荒れも認められなかったが、紫外線を照射した陽性対照群では明確な赤斑、シワ形成及び肌荒れが発生していた。一方、紫外線を照射しながら各試料をそれぞれ塗布した群の場合はいずれも、紫外線照射による赤斑、シワ形成及び肌荒れがほぼ半減していた。このことから、本発明に係る前記水性成分は紫外線照射による皮膚トラブルを軽減し得る皮膚老化防止効果を有することが確認された。又、炎症性サイトカインであるIL−1βは紫外線照射によって増加していたが、各試料をそれぞれ塗布した群ではいずれもIL−1βの増加が軽減しており、炎症が軽減されていた。一方で、抗炎症性サイトカインであるTGF−β1は紫外線照射によって増加していたが、各試料をそれぞれ塗布した群ではいずれもTGF−β1の増加がより一層増しており、炎症による組織の修復機能がより高まっていることが示唆された。As a result, in the control group not irradiated with ultraviolet rays, there was no inflammation and no wrinkle formation or rough skin was observed, but in the positive control group irradiated with ultraviolet rays, clear red spots, wrinkle formation and rough skin were generated. . On the other hand, in each of the groups where each sample was applied while being irradiated with ultraviolet rays, red spots, wrinkle formation and rough skin caused by ultraviolet irradiation were almost halved. From this, it was confirmed that the said aqueous component which concerns on this invention has the skin aging prevention effect which can reduce the skin trouble by ultraviolet irradiation. In addition, IL-1β, which is an inflammatory cytokine, was increased by ultraviolet irradiation, but in each group to which each sample was applied, the increase in IL-1β was reduced, and inflammation was reduced. On the other hand, TGF-β1, which is an anti-inflammatory cytokine, was increased by ultraviolet irradiation, but in each group to which each sample was applied, the increase in TGF-β1 was further increased, and the tissue repair function due to inflammation was increased. It has been suggested that is increasing.
試験例2
スクワラン:10部、ステアリン酸:5部、セタノール:3部及びステアリン酸モノグリセリド:3部からなる油相成分を80℃にて加熱溶解し、一方、グリセリン:15部、パラオキシ安息香酸メチル:0.1部、カルボキシビニルポリマー(1%水溶液):10部、ポリグリセリン(平均重合度4)モノオレアート:3部、アルギニン(20%水溶液):15部、試料2:1部及び精製水:34.9部からなる水相成分を80℃にて加熱溶解した。この水相成分に前記油相成分を撹拌しながら加え、ホモジナイザーにより均一に乳化して試験用クリームを調製した。又、このクリームにおいて、試料2を配合しない比較用クリーム(精製水で調整)を調製した。ボランティアの健康な成人女性10名(22歳〜54歳、平均年齢:31.0歳)の左手に試験用クリームを、右手に比較用クリームをそれぞれ1日2回塗布して2ヵ月間(7月〜8月)日常生活をしてもらい、皮膚への影響をアンケート調査(3段階評価)した。Test example 2
An oil phase component consisting of squalane: 10 parts, stearic acid: 5 parts, cetanol: 3 parts and stearic acid monoglyceride: 3 parts was heated and dissolved at 80 ° C., while glycerin: 15 parts, methyl paraoxybenzoate: 0. 1 part, carboxyvinyl polymer (1% aqueous solution): 10 parts, polyglycerol (average polymerization degree 4) monooleate: 3 parts, arginine (20% aqueous solution): 15 parts, sample 2: 1 part and purified water: 34 The aqueous phase component consisting of 9 parts was dissolved by heating at 80 ° C. The oil phase component was added to the aqueous phase component with stirring, and the mixture was uniformly emulsified with a homogenizer to prepare a test cream. Further, in this cream, a comparative cream (adjusted with purified water) not containing Sample 2 was prepared. 10 volunteer healthy adult women (22-54 years old, average age: 31.0 years old) apply the test cream to the left hand and the comparative cream to the right hand twice a day for 2 months (7 (Month-August) We had daily life and conducted a questionnaire survey (three-level evaluation) on the effects on the skin.
この結果、(1)皮膚の紅斑、発赤の発生について、比較用クレームでは無し:5名、わずかな紅斑ないし発赤があった:4名、明らかな発赤があった:1名であり、試験用クリームでは無し:8名、わずかな紅斑があった:2名であった。(2)肌のかさつき、肌荒れについて、比較用クリームでは強い:3名、普通:5名、弱い:2名であり、試験用クリームでは強い:0名、普通:4名、弱い:6名であった。このことから、本発明に係る前記水性成分を配合したクリームを継続的に皮膚に塗布することにより、夏期において肌の紅斑や発赤の発生を軽減し、かさつきや肌荒れの防止にも有効であることを確認した。As a result, (1) Regarding the occurrence of erythema and redness on the skin, there were no comparison claims: 5 people, slight erythema or redness: 4 people, obvious redness: 1 people, for testing No cream: 8 people, slight erythema: 2 people. (2) About the roughness and roughness of the skin, the comparison cream is strong: 3 people, normal: 5 people, weak: 2 people, and the test cream is strong: 0 people, normal: 4 people, weak: 6 people there were. From this, by continuously applying the cream containing the aqueous component according to the present invention to the skin, the occurrence of erythema and redness of the skin is reduced in summer, and it is also effective in preventing roughness and rough skin. It was confirmed.
試作例1〜7
以下に示す処方(数値は全て重量%)を用いて各種皮膚外用品を試作した。
(1)ローション
(a)ソルビット 2
(b)1,3−ブチレングリコール 4
(c)ポリエチレングリコール1000 2
(d)エタノール 10
(e)試料1 1
(f)防腐剤(メチルパラベン) 適量
(g)精製水 残量
(a)〜(f)を80℃に加熱した(g)に加え、撹拌して溶解した後、室温まで冷却して容器に充填した。Prototype examples 1-7
Various types of external skin products were made using the following formulation (all values are% by weight).
(1) Lotion (a) Sorbit 2
(B) 1,3-butylene glycol 4
(C) Polyethylene glycol 1000 2
(D) Ethanol 10
(E) Sample 1 1
(F) Preservative (Methylparaben) Appropriate amount (g) Purified water The remaining amount (a) to (f) is added to (g) heated to 80 ° C., stirred and dissolved, then cooled to room temperature and filled into a container did.
(2)乳液
(a)スクワラン 4
(b)ワセリン 1
(c)ステアリルアルコール 0.5
(d)ソルビタンモノステアラート 1.5
(e)ポリオキシエチレン(20)ソルビタンモノオレアート 3
(f)1,3−ブチレングリコール 5
(g)試料2 0.1
(h)茶カテキン 0.1
(i)精製水 残量
(a)〜(d)を80℃で加熱溶解して油相成分とし、(e)〜(i)を80℃で加熱溶解して水相成分とした。同温度にて、水相成分に油相成分を撹拌しながら加え、ホモジナイザーにより均一に乳化した後、室温まで冷却、脱気して容器に充填した。この乳液は肌の炎症を抑制するために利用できる。(2) Latex (a) Squalane 4
(B) Vaseline 1
(C) Stearyl alcohol 0.5
(D) Sorbitan monostearate 1.5
(E) Polyoxyethylene (20) sorbitan monooleate 3
(F) 1,3-butylene glycol 5
(G) Sample 2 0.1
(H) Tea catechin 0.1
(I) Purified water The remaining amounts (a) to (d) were heated and dissolved at 80 ° C. to obtain an oil phase component, and (e) to (i) were heated and dissolved at 80 ° C. to obtain an aqueous phase component. At the same temperature, the oil phase component was added to the aqueous phase component with stirring, and the mixture was uniformly emulsified with a homogenizer, cooled to room temperature, degassed, and filled into a container. This emulsion can be used to suppress skin inflammation.
(3)クリーム
(a)スクワラン 20
(b)ミツロウ 5
(c)ホホバ油 5
(d)ソルビタンモノステアラート 1
(e)グリセリンモノオレアレート 3
(f)ポリオキシエチレン(20)ソルビタンモノステアラート 3
(g)グリセリン 5
(h)試料3 5
(i)N−アセチルグルコサミン 2
(j)精製水 残量
(a)〜(e)を80℃で加熱溶解して油相成分とし、(f)〜(j)を80℃で加熱溶解して水相成分とした。同温度にて、水相成分に油相成分を撹拌しながら加え、ホモジナイザーにより均一に乳化した後、室温まで冷却、脱気して容器に充填した。このクリームは抗炎症用の皮膚外用品として利用できる。(3) Cream (a) Squalane 20
(B) Beeswax 5
(C) Jojoba oil 5
(D) Sorbitan monostearate 1
(E) Glycerol monooleate 3
(F) Polyoxyethylene (20) sorbitan monostearate 3
(G) Glycerin 5
(H) Sample 3 5
(I) N-acetylglucosamine 2
(J) Purified water The remaining amounts (a) to (e) were heated and dissolved at 80 ° C. to obtain an oil phase component, and (f) to (j) were heated and dissolved at 80 ° C. to obtain an aqueous phase component. At the same temperature, the oil phase component was added to the aqueous phase component with stirring, and the mixture was uniformly emulsified with a homogenizer, cooled to room temperature, degassed, and filled into a container. This cream can be used as an external skin preparation for anti-inflammation.
(4)ボディーソープ
(a)ラウリン酸カリウム 13
(b)ミリスチン酸カリウム 5
(c)プロピレングリコール 7
(d)試料4 10
(e)ハイビスカス花抽出物 3
(f)pH調整剤(クエン酸) 適量
(g)防腐剤(メチルパラベン) 適量
(h)精製水 残量
(a)及び(b)を予め80℃で加熱溶解した(c)〜(h)の溶液に撹拌しながら加え、ホモジナイザーにより均一に混合した後、室温まで冷却、脱気して容器に充填した。このボディーソープは皮膚の炎症軽減や肌荒れ防止用の皮膚外用品として利用できる。(4) Body soap (a) Potassium laurate 13
(B) Potassium myristate 5
(C) Propylene glycol 7
(D) Sample 4 10
(E) Hibiscus flower extract 3
(F) pH adjuster (citric acid) appropriate amount (g) preservative (methyl paraben) appropriate amount (h) purified water The remaining amount (a) and (b) were dissolved in advance by heating at 80 ° C. (c) to (h) The mixture was added to the solution with stirring and mixed uniformly with a homogenizer, then cooled to room temperature, degassed and filled into a container. This body soap can be used as an external skin product for reducing skin inflammation and preventing rough skin.
(5)シャンプー
(a)ラウリン酸ジエタノールアミド 2
(b)ラウリル硫酸トリエタノールアミン 5
(c)ポリオキシエチレンラウリルエーテル硫酸ソーダ 12
(d)1,3−ブチレングリコール 4
(e)エデト酸二ナトリウム 0.1
(f)試料2 0.05
(g)防腐剤及び香料 各適量
(h)精製水 残量
(b)〜(h)を加熱溶解して70℃とし、(a)を添加してホモミキサーにより乳化後、冷却、脱気して容器に充填した。(5) Shampoo (a) Lauric acid diethanolamide 2
(B) Lauryl sulfate triethanolamine 5
(C) Polyoxyethylene lauryl ether sodium sulfate 12
(D) 1,3-butylene glycol 4
(E) Edetate disodium 0.1
(F) Sample 2 0.05
(G) Preservative and perfume appropriate amount (h) Purified water The remaining amount (b) to (h) is heated and dissolved to 70 ° C., (a) is added, emulsified with a homomixer, cooled and deaerated. Filled into a container.
(6)ヘアトニック
(a)オレイン酸エチル 1
(b)エタノール 45
(c)ポリオキシエチレン(40)硬化ヒマシ油 2
(d)試料1 15
(e)精製水 残量
(c)〜(e)を加熱溶解して60℃とし、同温度に加熱した(a)及び(b)の混合物を添加してホモミキサーにより可溶化後、冷却、脱気して容器に充填した。(6) Hair tonic (a) Ethyl oleate 1
(B) Ethanol 45
(C) Polyoxyethylene (40) hydrogenated castor oil 2
(D) Sample 1 15
(E) Purified water The remaining amount (c) to (e) are dissolved by heating to 60 ° C., the mixture of (a) and (b) heated to the same temperature is added, solubilized by a homomixer, cooled, Degassed and filled into containers.
(7)粉末浴用剤
(a)炭酸水素ナトリウム 50
(b)無水硫酸ナトリウム 35
(c)ホウ砂 3
(d)試料3 7
(e)カミツレ抽出末 4
(f)着色料及び香料 各適量
(a)〜(f)を粉体混合機で混合して容器に充填した。この粉末浴用剤は入浴時に使用して肌の紅斑やほてり感を鎮めるために利用できる。(7) Powder bath agent (a) Sodium bicarbonate 50
(B) Anhydrous sodium sulfate 35
(C) Borax 3
(D) Sample 3 7
(E) Chamomile extraction powder 4
(F) Colorant and fragrance Each appropriate amount (a) to (f) was mixed with a powder mixer and filled into a container. This powder bath preparation can be used for bathing and soothing erythema and hot flashes on the skin.
ツバキ種子の脱脂物から得られる水性成分は、紫外線暴露によって生じる皮膚の炎症を軽減し、肌荒れやかさつきを抑制する等の効果を有するため、これを皮膚に塗布又は接触させることにより、皮膚の本来の生理機能を回復させ、皮膚トラブルの改善や皮膚損傷の早期回復に役立つ皮膚外用品として利用できる。Aqueous components obtained from camellia seed defatted have the effect of reducing skin irritation caused by exposure to ultraviolet rays and suppressing rough skin and roughness. It can be used as an external skin product that restores the physiological function of the skin, helps improve skin troubles, and recovers early skin damage.
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JP5736737B2 (en) * | 2010-11-10 | 2015-06-17 | 日油株式会社 | Epidermal keratinocyte activator |
JP2012116898A (en) * | 2010-11-29 | 2012-06-21 | Kracie Home Products Ltd | Detergent composition |
JP6326611B2 (en) * | 2012-10-24 | 2018-05-23 | ビーエイチエヌ株式会社 | CMA production inhibitor |
KR101797072B1 (en) | 2015-12-10 | 2017-11-14 | 전남대학교산학협력단 | Composition for preventing, treating, or improving ocular fatigue, ocular inflammation, or dry eye syndrome comprising Camellia japonica extracts |
JP2018090639A (en) * | 2018-03-16 | 2018-06-14 | ビーエイチエヌ株式会社 | Cma production inhibiting agent |
CN113164604A (en) * | 2018-11-02 | 2021-07-23 | 株式会社资生堂 | Inhibitors of ultraviolet-induced inflammation comprising alternative autophagy inducers |
CN115066251A (en) * | 2020-08-27 | 2022-09-16 | 株式会社资生堂 | Inhibitor of reduction of expression of CD39 gene |
KR102453894B1 (en) * | 2020-09-15 | 2022-10-11 | (주)아모레퍼시픽 | Composition for skin protection comprising kaempferol saccharides compounds |
EP4066847A1 (en) * | 2021-03-29 | 2022-10-05 | Chanel Parfums Beauté | Hydroalcoholic extract of camellia japonica and cosmetic compositions comprising same |
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