JP2013043018A - Polypeptide-containing cyclodextrin aqueous solution - Google Patents
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本発明はシクロデキストリン含有水溶液の消臭性能、抗菌性能の耐久性向上ならびに抗アレルゲン性能付与に係るものである。 The present invention relates to deodorizing performance, antibacterial performance durability improvement and antiallergen performance imparting of a cyclodextrin-containing aqueous solution.
シクロデキストリンは環状構造を持つ糖であり、環の空洞内部に香料や油溶性の成分などの物質を取り込む性質があり、分子レベルのカプセルとしての働きを有することより、水溶性、揮発性、光分解性が不安定な化粧品原料を、安定した状態で配合するためや香料の保香性を高める目的で使われたりするなど、吸着剤、キレート剤、可溶化剤、起泡剤、脱臭剤として、化粧水、乳液、クリーム、美容液、パウダー、シャンプーなど日用品、さらには医療、食品の分野に広く用いられてきている（例えば特許文献１参照）。特に、シクロデキストリン素材の消臭剤としての用途は最近、急速に伸びており、主に水溶液の噴霧形態で製品化されたものの需要の伸びが顕著である。 Cyclodextrins are sugars with a cyclic structure, and have the property of incorporating substances such as fragrances and oil-soluble ingredients inside the ring cavity, and they function as capsules at the molecular level, making them water-soluble, volatile, and light. As an adsorbent, chelating agent, solubilizing agent, foaming agent, deodorant, etc., in order to blend cosmetic ingredients with unstable degradability in a stable state or for the purpose of enhancing the fragrance retention. It has been widely used in the fields of daily necessities such as lotion, milky lotion, cream, cosmetic liquid, powder and shampoo, as well as medical and food (see, for example, Patent Document 1). In particular, the use of a cyclodextrin material as a deodorant has been rapidly increasing recently, and the demand for products manufactured mainly in the form of sprays of aqueous solutions is remarkable.
例えば、消臭を目的としたシクロデキストリン含有噴霧剤（例えば特許文献２参照）や、さらに４級アンモニウム塩等の抗菌成分を包含させて抗菌作用を付与（例えば特許文献３、特許文献４参照）した例がある。またカテキンなど抗アレルゲン性能を有する素材が加えられた製品も開発されている（特許文献５参照）。
しかしシクロデキストリン含有噴霧液製品は、単に雨に濡れるだけでもその大半が洗い流されてしまい、その後の機能発現は望めない等、耐久性に問題があった。
For example, a cyclodextrin-containing spray for the purpose of deodorization (see, for example, Patent Document 2) and an antibacterial component such as a quaternary ammonium salt are included to provide an antibacterial effect (see, for example, Patent Document 3 and Patent Document 4). There are examples. A product to which a material having antiallergen performance such as catechin is added has also been developed (see Patent Document 5).
However, the cyclodextrin-containing spray liquid product has a problem in durability, such as being mostly washed away even when it gets wet in the rain, and subsequent functional expression cannot be expected.
噴霧等単純な操作で、水不溶性のシクロデキストリン含有膜を形成して消臭効果を有しさらにシクロデキストリンの持つ種々の機能の持続的な発揮を可能にする耐久性の良いシクロデキストリン含有水溶液の開発目指した。 By a simple operation such as spraying, a water-insoluble cyclodextrin-containing film is formed, which has a deodorizing effect, and further enables the continuous display of various functions possessed by cyclodextrin. Aimed at development.
本発明は以下の構成を有するものである。 The present invention has the following configuration.
１）． 水不溶性膜形成ポリペプチド含有シクロデキストリン水溶液。 1). A water-insoluble film-forming polypeptide-containing cyclodextrin aqueous solution.
２）． シクロデキストリンがα、β、γ、これらの誘導体及び／またはこれらの混合物である１）記載のポリペプチド含有シクロデキストリン水溶液。 2). The polypeptide-containing cyclodextrin aqueous solution according to 1), wherein the cyclodextrin is α, β, γ, derivatives thereof and / or mixtures thereof.
３）． ポリペプチドがコラーゲン、ゼラチン、ゼラチンペプチド、これらの誘導体及び／またはこれらの混合物である１）または２）記載のポリペプチド含有シクロデキストリン水溶液。 3). The polypeptide-containing cyclodextrin aqueous solution according to 1) or 2), wherein the polypeptide is collagen, gelatin, gelatin peptide, derivatives thereof and / or mixtures thereof.
４）． 抗菌性物質をさらに配合したことを特徴とする１）〜３）いずれかに記載のポリペプチド含有シクロデキストリン水溶液。 4). The polypeptide-containing cyclodextrin aqueous solution according to any one of 1) to 3), further comprising an antibacterial substance.
本発明により、噴霧等の操作を行うだけで、対象物表面にシクロデキストリンとポリペプチドの水不溶性の被膜形成が可能となり、対象物の耐洗濯、水拭き取り耐性など耐水性を保持しつつシクロデキストリンの持つ機能の耐久性向上に繋がるとともに、コラーゲンあるいはゼラチンなどポリペプチドに起因する抗アレルゲン性能の付与、また抗菌性物質を用いた場合は抗菌性の付与ができる。 According to the present invention, it is possible to form a water-insoluble film of cyclodextrin and polypeptide on the surface of an object simply by performing an operation such as spraying, and cyclodextrin while maintaining water resistance such as washing resistance and water wiping resistance of the object. In addition to improving the durability of the functions of the anti-allergen, it is possible to impart anti-allergen performance due to a polypeptide such as collagen or gelatin, and to impart antibacterial properties when an antibacterial substance is used.
本発明のポリペプチド含有シクロデキストリン水溶液のシクロデキストリンとは、非還元性のオリゴ糖でグルコースの分子がリング状につながった環状構造糖であり、リングを構成する分子の数が６個のものをαシクロデキストリン、７個のものをβシクロデキストリン、８個のものをγシクロデキストリンと呼ぶ。 The cyclodextrin of the polypeptide-containing cyclodextrin aqueous solution of the present invention is a cyclic structure sugar in which glucose molecules are connected in a ring shape with a non-reducing oligosaccharide, and the number of molecules constituting the ring is six. α-cyclodextrin, 7 are called β-cyclodextrin, and 8 are called γ-cyclodextrin.
本発明のポリペプチド含有シクロデキストリン水溶液を消臭用途で使用する場合、用いるシクロデキストリンは臭気物質など除去対象物質を包接しやすいように、未包接のシクロデキストリンであることが好ましい。ただし、香料などを包接したシクロデキストリンを少量含んでいてもよい。特に消臭だけでなく芳香を期待する場合はその割合が高くなる。また、シクロデキストリンは主成分がα−、β−、γ−シクロデキストリン及び／またはそれらの混合物であることが好ましいが、メチル化あるいはアセチル化などの化学修飾されたα−、β−、γ−シクロデキストリン及び／またはそれらの混合物を用いることもできる。 When the polypeptide-containing cyclodextrin aqueous solution of the present invention is used for deodorization, it is preferable that the cyclodextrin to be used is non-inclusion cyclodextrin so as to facilitate inclusion of a substance to be removed such as an odor substance. However, it may contain a small amount of cyclodextrin containing a fragrance. In particular, when not only deodorization but also fragrance is expected, the ratio becomes high. The cyclodextrin is preferably α-, β-, γ-cyclodextrin and / or a mixture thereof as a main component, but α-, β-, γ- chemically modified such as methylation or acetylation. Cyclodextrins and / or mixtures thereof can also be used.
本発明のポリペプチドとしては、ゼラチンあるいはコラーゲンを用いることが出来る。ゼラチンとしては、他に、ゼラチンを分解したゼラチンペプチド、ゼラチンおよびゼラチンペプチドの化学処理による修飾物など、水に可溶なものを用いることができる。ここで化学処理による修飾物とは、ゼラチンあるいはゼラチンペプチドなどのポリペプチド中のアミノ酸側鎖に種々分子を反応させたもの、たとえば糖鎖付加、アセチル化、リン酸化、脂質付加したものなどが含まれる。またゼラチン、コラーゲン等のポリペプチドの原料としては魚類、ほ乳類、鳥類由来のものを用いることができるが、本発明においてはポリペプチドの純度さらには得られる水溶液の純度の面から魚類（水に住むほ乳類を含む）から得られるポリペプチドが好ましい。 As the polypeptide of the present invention, gelatin or collagen can be used. Other gelatins that can be used are those soluble in water, such as gelatin peptides obtained by degrading gelatin, gelatin, and modified products obtained by chemical treatment of gelatin peptides. Here, the modified products by chemical treatment include those obtained by reacting various molecules with amino acid side chains in a polypeptide such as gelatin or gelatin peptide, for example, glycosylation, acetylation, phosphorylation, lipid addition, etc. It is. In addition, as a raw material for polypeptides such as gelatin and collagen, those derived from fish, mammals and birds can be used. However, in the present invention, fish (having living in water) is used in view of the purity of the polypeptide and the purity of the aqueous solution obtained. Polypeptides obtained from (including mammals) are preferred.
本発明の水不溶性とは、本発明の水溶液を噴霧乾燥させて形成した不溶物が、通常の水洗操作では実質的にはほとんど溶解されないことである。通常の水洗操作とは、たとえば噴霧乾燥させた不溶物を常温の十分な量の水で２〜３時間洗浄する操作、あるいは常温で通常の洗濯操作、たとえば洗濯機の標準洗浄設定で洗浄したりする操作である。この操作で実質的に減量が認められないことである。 The water insolubility according to the present invention means that the insoluble matter formed by spray drying the aqueous solution of the present invention is substantially hardly dissolved by a normal water washing operation. The normal washing operation is, for example, washing the spray-dried insoluble matter with a sufficient amount of water at room temperature for 2 to 3 hours, or washing at normal temperature in a normal washing operation, for example, standard washing settings of a washing machine. It is an operation to do. In this operation, the weight loss is not substantially recognized.
本発明の水溶液は、噴霧等により対象物に吹き付けるあるいは、対象物を浸漬することによりその表面等に付着させることができる。水溶液であるために通常は自然乾燥により溶媒の水が蒸発し、水溶液中に含まれている成分が対象物に残ることになる。水溶液を乾燥させることにより、ポリペプチドおよびシクロデキストリンが水不溶性となり、対象物に水不溶性物として残留する。 The aqueous solution of the present invention can be applied to the surface or the like by spraying on the object by spraying or by immersing the object. Since it is an aqueous solution, the solvent water is usually evaporated by natural drying, and the components contained in the aqueous solution remain in the object. By drying the aqueous solution, the polypeptide and cyclodextrin become water-insoluble and remain on the object as water-insoluble substances.
本発明の水溶液は噴霧による塗布、はけ等による塗布あるいは浸漬による塗布等により対象物の表面へ付着させることができ、同水溶液の成分は対象物表面に実質的には膜状物として付着することになる。 The aqueous solution of the present invention can be attached to the surface of an object by application by spraying, application by brushing, or application by immersion, and the components of the aqueous solution are substantially attached to the surface of the object as a film. It will be.
塗布対象物としては、繊維、繊維からなる不織布、織布、プラチックシート、用途に合わせて種々の形態に成型加工されたプラスチック製品が対象として用いることができる。 As an object to be coated, fibers, non-woven fabrics made of fibers, woven fabrics, plastic sheets, and plastic products molded and processed into various forms according to applications can be used as targets.
繊維としては例えば天然繊維、化学繊維、鉱物繊維が挙げられる。天然繊維としては具体的に例えば、綿、羊毛、麻、パルプ、絹、などを挙げることができる。 Examples of the fibers include natural fibers, chemical fibers, and mineral fibers. Specific examples of natural fibers include cotton, wool, hemp, pulp, silk, and the like.
化学繊維としては具体的には例えば、レーヨン、ナイロン、ポリエステル、ポリプロピレン、アクリル繊維、ビニロン、アラミド繊維などを挙げることができる。鉱物繊維としては具体的には例えば、ガラス繊維、炭素繊維などを挙げることができる。不織布、織布はこれら繊維を用いて作ることができる。
なかでも取り扱い易さ、価格などの点から、好ましくは天然繊維及びまたは化学繊維が挙げられる、具体的には綿、レーヨン、ポリエステル、ポリプロピレン、パルプが挙げられる。
Specific examples of the chemical fiber include rayon, nylon, polyester, polypropylene, acrylic fiber, vinylon, and aramid fiber. Specific examples of the mineral fiber include glass fiber and carbon fiber. Nonwoven fabrics and woven fabrics can be made using these fibers.
Of these, natural fibers and / or chemical fibers are preferable from the viewpoint of ease of handling, price, and the like. Specifically, cotton, rayon, polyester, polypropylene, and pulp can be used.
またプラスチックシート、プラスチック製品の素材としては、ポリエチレン樹脂、ポリプロピレン樹脂、ホリカーボネート樹脂、ＡＢＳ樹脂、ポリアミド樹脂、塩化ビニル樹脂、ポリウレタン樹脂、ポリエステル樹脂、ポリアクリル樹脂、スチレン樹脂、アクリルシリコン系樹脂、エポキシエステル樹脂、フッ素系樹脂、ポリオレフィン系エラストマー、ポリエステル系エラストマー、スチレン系エラストマーなどの樹脂を対象とすることができる。 Plastic sheets and plastic products are made of polyethylene resin, polypropylene resin, polycarbonate resin, ABS resin, polyamide resin, vinyl chloride resin, polyurethane resin, polyester resin, polyacrylic resin, styrene resin, acrylic silicon resin, epoxy Resins such as ester resins, fluorine resins, polyolefin elastomers, polyester elastomers, and styrene elastomers can be targeted.
本発明の水溶液が形成する膜は、シクロデキストリンとポリペプチドからなる水不溶性の膜形成が基本であるが、シクロデキストリンとポリペプチド以外の種々機能を有する物質を混合し、これによる機能が付与された塗膜を形成させることもできる。 The film formed by the aqueous solution of the present invention is basically formed of a water-insoluble film consisting of cyclodextrin and polypeptide, but a substance having various functions other than cyclodextrin and polypeptide is mixed and the function by this is given. It is also possible to form a coated film.
本発明の抗菌性物質としては、有機系抗菌剤、無機系抗菌剤、光触媒物質が用いることが出来る。有機系抗菌剤としては４級アンモニウム塩、キトサンなど天然系抗菌剤を、無機系抗菌剤としては銀、銅、亜鉛などの金属塩を、光触媒物質としては酸化亜鉛、酸化チタンをそれぞれあげることができる。中でも４級アンモニウム塩が最も好ましい。 As the antibacterial substance of the present invention, organic antibacterial agents, inorganic antibacterial agents, and photocatalytic substances can be used. Organic antibacterial agents include quaternary ammonium salts, natural antibacterial agents such as chitosan, inorganic antibacterial agents include silver, copper, zinc and other metal salts, and photocatalytic substances include zinc oxide and titanium oxide. it can. Of these, quaternary ammonium salts are most preferred.
また抗アレルゲン機能付与の点では、本発明にあるゼラチンなどポリペプチドを用いることにより発現できる。この効果はポリペプチドとアレルゲンとの親和性に基づく吸着除去効果による抗アレルゲン機能付与されると考えられる。ポリペプチドの他に、アレルゲン不活性化機能があるとされるカテキンなどポリフェノール類を含む化合物を用いることもできる。 In terms of imparting anti-allergen function, it can be expressed by using a polypeptide such as gelatin according to the present invention. It is considered that this effect is imparted with an anti-allergen function due to an adsorption removal effect based on the affinity between the polypeptide and the allergen. In addition to the polypeptide, a compound containing polyphenols such as catechin, which has an allergen inactivating function, can also be used.
消臭機能の付与の点では、シクロデキストリンによる、臭気物質の包接効果また香料など芳香剤の徐放効果以外に、ゼラチンなどポリペプチドによる臭気物質の吸着による臭気物質の除去、また光触媒物質を混合することで光触媒による臭気物質の分解による消臭効果も期待することができる。 In addition to the inclusion effect of odorous substances by cyclodextrin and the sustained release effect of fragrances such as fragrances, removal of odorous substances by adsorption of odorous substances by polypeptides such as gelatin, and photocatalytic substances By mixing, the deodorizing effect by decomposition | disassembly of the odorous substance by a photocatalyst can also be anticipated.
さらに抗ウィルス機能付与という点でも、カテキンなどポリフェノール類を含む化合物など抗ウィルス性能を有することが知られている化合物を混合することも可能である。 Furthermore, also in terms of imparting antiviral function, it is possible to mix a compound known to have antiviral performance such as a compound containing polyphenols such as catechin.
その他、本発明が提供する技術は、自動車、家電、住宅内装、衣類、靴など生活日用品から化粧品等コスメ、食品、医療まで地球上で人類が快適に生活する上で必要とする幅広い分野の製品に適用可能な技術であるといえる。 In addition, the technology provided by the present invention is a product in a wide range of fields that are necessary for humans to live comfortably on the earth, from daily necessities such as automobiles, home appliances, house interiors, clothing, and shoes to cosmetics such as cosmetics, food, and medical care. It can be said that this technology can be applied to this.
（実施例１） シクロデキストリンとゼラチン混合後の保存期間と牛アルブミン吸着性能の関係／（牛アルブミン吸着試験−１）
関東化学社製ベータ型シクロデキストリン（以下、βＣＤとする）０．１重量％水溶液に新田ゼラチン社製魚ゼラチン顆粒を終濃度０．２重量％になるように添加し、噴霧液を作成した。
(Example 1) Relationship between storage period after mixing cyclodextrin and gelatin and bovine albumin adsorption performance / (bovine albumin adsorption test-1)
A spray solution was prepared by adding Nitta Gelatin's fish gelatin granules to a final concentration of 0.2% by weight in a 0.1% by weight aqueous solution of Kanto Chemical's beta cyclodextrin (hereinafter referred to as βCD). .
噴霧液の作製直後、１３日経過、１８日経過、４５日経過した噴霧液をそれぞれ２ｃｍ角の合成繊維不織布（目付け３５ｇ/ｍ２）両面に、不織布全体が十分液に浸るように噴霧し、さらに同噴霧不織布を紙タオルの上に置き、余分の液を除去する操作を行った後に、それぞれ室温で乾燥させた。乾燥後、それぞれの不織布を十分な量の水で２〜３時間洗浄した。洗浄後、それぞれの不織布を室温で乾燥させた。なお本実施例のゼラチン／シクロデキストリン混合物の固着量は、本実施例中の１８日経過噴霧液使用の場合で、２ｃｍ角不織布１枚あたり約０．１６ｍｇの固着量である。 Immediately after the preparation of the spray solution, the spray solution that has passed 13 days, 18 days, and 45 days is sprayed on both sides of the 2 cm square synthetic fiber nonwoven fabric (weight per unit 35 g / m 2 ) so that the entire nonwoven fabric is sufficiently immersed in the liquid, Further, the sprayed nonwoven fabric was placed on a paper towel, and after removing the excess liquid, each was dried at room temperature. After drying, each nonwoven fabric was washed with a sufficient amount of water for 2 to 3 hours. After washing, each nonwoven fabric was dried at room temperature. In addition, the fixed amount of the gelatin / cyclodextrin mixture of the present example is about 0.16 mg per 2 cm square nonwoven fabric in the case of using the 18-day elapsed spray liquid in the present example.
洗浄乾燥した不織布に０．２ｍｇ／ｍｌの牛アルブミン（以下ＢＳＡとする）液２５０μｌを添加し、十分液を含浸させた後、３０分間室温に静置した。室温静置後、液を回収し、蛋白定量試薬を用いて回収液中のＢＳＡ濃度を計測した。比較対照として、ゼラチンを添加していない０．１％βＣＤ水溶液およびβＣＤを添加していない０．２％魚ゼラチン水溶液を用いて同様の処理を行った不織布を作製し、ＢＳＡ吸着試験を行った。 250 μl of 0.2 mg / ml bovine albumin (hereinafter referred to as “BSA”) solution was added to the washed and dried nonwoven fabric, sufficiently impregnated with the solution, and then allowed to stand at room temperature for 30 minutes. After standing at room temperature, the liquid was recovered, and the BSA concentration in the recovered liquid was measured using a protein quantification reagent. As a comparative control, a non-woven fabric subjected to the same treatment was prepared using a 0.1% βCD aqueous solution containing no gelatin and a 0.2% fish gelatin aqueous solution containing no βCD, and a BSA adsorption test was performed. .
結果を表１に示した。すなわち、本発明に係る噴霧液を用いた不織布のＢＳＡ吸着除去性能は、比較対照の噴霧液で処理したものより有意に高く、１３日を越えて１８日以降は安定的に９０％を越える吸着除去性能を有した。 The results are shown in Table 1. That is, the BSA adsorption / removal performance of the nonwoven fabric using the spray solution according to the present invention is significantly higher than that of the non-woven fabric treated with the control spray solution, and more than 90% is stably adsorbed after 18 days. Has removal performance.
（実施例２） シクロデキストリンと混合する魚ゼラチン濃度を変えた場合のゼラチン濃度と牛アルブミン吸着性能の関係／（牛アルブミン吸着試験−２）
実施例１において作製後４５日経過した０．２％魚ゼラチン／０．１％βＣＤ噴霧液を０．１％βＣＤ液で１０倍、１００倍、１０００倍、１００００倍希釈し、その各々の液を実施例１で用いたのと同じ２ｃｍ角の合成繊維不織布の両面に不織布全体が十分液に浸るように噴霧し、さらに同噴霧不織布を紙タオルの上に置き、余分の液を除去する操作を行った後に、それぞれ室温で乾燥させた。乾燥後、それぞれの不織布を十分な量の水で２〜３時間洗浄処理を実施した。洗浄後、それぞれの不織布を室温で乾燥させた。
(Example 2) Relationship between gelatin concentration and bovine albumin adsorption performance when the concentration of fish gelatin mixed with cyclodextrin was changed / (bovine albumin adsorption test-2)
In Example 1, the 0.2% fish gelatin / 0.1% βCD spray solution that had passed 45 days after preparation was diluted 10-fold, 100-fold, 1000-fold, and 10000-fold with a 0.1% βCD solution. Was sprayed on both sides of the same 2 cm square synthetic fiber nonwoven fabric used in Example 1 so that the entire nonwoven fabric was sufficiently immersed in the liquid, and the sprayed nonwoven fabric was placed on a paper towel to remove excess liquid. Then, each was dried at room temperature. After drying, each nonwoven fabric was washed with a sufficient amount of water for 2 to 3 hours. After washing, each nonwoven fabric was dried at room temperature.
洗浄乾燥した不織布を用いて実施例１と同様の操作でＢＳＡ吸着除去試験を行った。
結果を表２に示した。すなわち、１０倍希釈の噴霧液では弱い吸着除去性能が認められたが、１０倍を越えて希釈した噴霧液ではほとんど吸着除去性能が認められなかった。
A BSA adsorption removal test was performed in the same manner as in Example 1 using the washed and dried nonwoven fabric.
The results are shown in Table 2. That is, weak adsorption removal performance was observed with the 10-fold diluted spray solution, but almost no adsorption removal performance was observed with the spray solution diluted more than 10-fold.
（実施例３） ゼラチン含有シクロデキストリン水溶液噴霧塗付プラスチックシャーレのアルブミン吸着性能／（牛アルブミン吸着試験−３）
βＣＤ０．１％水溶液に魚ゼラチン顆粒を終濃度０．２％になるように添加した水溶液を作製した。作製後４５日経過した同水溶液を径１０ｃｍのプラスチックシャーレ内面に約１ｍｌの液量を噴霧し、室温で乾燥させた。乾燥後、シャーレに約１０ｍｌの水を入れ振とうしながら２〜３時間洗浄した。洗浄後、シャーレを室温で乾燥させた。
(Example 3) Albumin adsorption performance of plastic petri dish with gelatin-containing cyclodextrin aqueous solution spray coated / (Bovine albumin adsorption test-3)
An aqueous solution in which fish gelatin granules were added to a βCD 0.1% aqueous solution to a final concentration of 0.2% was prepared. About 45 ml of the same aqueous solution, which had passed 45 days after production, was sprayed on the inner surface of a plastic petri dish having a diameter of 10 cm and dried at room temperature. After drying, about 10 ml of water was placed in a petri dish and washed for 2 to 3 hours while shaking. After washing, the petri dish was dried at room temperature.
水で洗浄したシャーレに０．２ｍｇ／ｍｌのＢＳＡ液１００μｌを添加、さらに同液上に２ｃｍ四方の透明ナイロンフィルムを置き液を均一拡散させた状態にして３０分間室温静置した。室温静置後、液を回収し、実施例１と同様にＢＳＡ濃度を計測した。比較対照として、魚ゼラチンを添加していない０．１％βＣＤ水溶液、βＣＤを添加していない０．２％魚ゼラチン水溶液をそれぞれ用いて同様の操作を行い作製したシャーレについてもＢＳＡ吸着試験を行った。結果を表３に示す。 To a petri dish washed with water, 100 μl of 0.2 mg / ml BSA solution was added, and a transparent nylon film of 2 cm square was placed on the solution, and the solution was uniformly diffused and allowed to stand at room temperature for 30 minutes. After standing at room temperature, the liquid was recovered and the BSA concentration was measured in the same manner as in Example 1. As a comparative control, a BSA adsorption test was also performed on petri dishes prepared by performing the same operation using a 0.1% βCD aqueous solution containing no fish gelatin and a 0.2% fish gelatin aqueous solution containing no βCD. It was. The results are shown in Table 3.
０．１％βＣＤのみ、および０．２％魚ゼラチンのみのそれぞれ単独で処理したものは開始濃度０．２ｍｇ／ｍｌに対し、いずれも０．１９８ｍｇ／ｍｌと僅かな濃度低下であるが、両方組み合わせた場合には０．１８７ｍｇ/ｍｌまで低下が観られ、βＣＤと魚ゼラチンを混合したものに有意なアルブミン吸着性能が認められた。 Both 0.1% βCD alone and 0.2% fish gelatin alone treated with a starting concentration of 0.2 mg / ml are both slightly reduced to 0.198 mg / ml, but both When combined, a decrease to 0.187 mg / ml was observed, and a significant albumin adsorption performance was observed in a mixture of βCD and fish gelatin.
（実施例４） ゼラチン含有シクロデキストリン水溶液噴霧不織布の抗菌性能／（抗菌性能試験−１）
βＣＤ０．１％水溶液に終濃度０．２％になるように魚ゼラチンを添加、溶解させ、１８日経過した液１００ｍｌにさらに４級アンモニウム塩として５０％塩化ベンザルコニウム溶液を４００ｍｇを添加した液を作製した。同液を実施例１で用いたのと同じ２ｃｍ角の合成繊維不織布の両面に噴霧塗布処理し、室温で乾燥させた。乾燥後、不織布を十分な量の水で２〜３時間洗浄した。洗浄後、不織布を室温で乾燥させた。
(Example 4) Antibacterial performance of gelatin-containing cyclodextrin aqueous solution spray nonwoven fabric / (Antimicrobial performance test-1)
Fish gelatin was added and dissolved in a βCD 0.1% aqueous solution to a final concentration of 0.2%, and a solution obtained by adding 400 mg of a 50% benzalkonium chloride solution as a quaternary ammonium salt to 100 ml of the solution after 18 days. Was made. The same solution was spray coated on both sides of the same 2 cm square synthetic fiber nonwoven fabric used in Example 1, and dried at room temperature. After drying, the nonwoven fabric was washed with a sufficient amount of water for 2 to 3 hours. After washing, the nonwoven fabric was dried at room temperature.
同乾燥不織布をエッペンチューブに入れ、これに２５０μｌの２０倍希釈したニュートリエント培地（肉エキス５ｇ、ペプチド１０ｇを蒸留水１Ｌに溶解しｐＨ６．８±０．２とし高圧蒸気滅菌したもの）を添加、含浸させ、さらに一晩ニュートリエント培地で培養した大腸菌液を水で１００００倍に希釈した液１０μｌを添加、混合し、３７℃で２４時間静置培養した。 Put the dried non-woven fabric into an Eppendorf tube and add 250 μl of 20-fold diluted nutrient medium (5 g of meat extract, 10 g of peptide dissolved in 1 L of distilled water to pH 6.8 ± 0.2 and autoclaved). Then, 10 μl of an E. coli solution that had been impregnated and further cultured overnight in a nutrient medium was diluted 10,000 times with water, mixed, and incubated at 37 ° C. for 24 hours.
培養後、回収した培養液を水で１００倍希釈した液１００μｌを寒天培地プレートに接種、スプレッダーで一面に塗布した後、３７℃で一晩培養した。同培養後のプレート上の大腸菌成育状況を肉眼で観察した。比較対照として、魚ゼラチンを添加していないβＣＤ０．１％水溶液１００ｍｌに５０％塩化ベンザルコニウム溶液４００ｍｇを添加した液を用いて、同様の操作を行い作製した不織布についても同様に抗菌性評価を行った。 After culturing, 100 μl of the collected culture solution diluted 100-fold with water was inoculated on an agar plate, coated on one surface with a spreader, and then cultured at 37 ° C. overnight. The growth of E. coli on the plate after the same culture was observed with the naked eye. As a comparative control, antibacterial evaluation was similarly performed on a non-woven fabric prepared by performing the same operation using a solution obtained by adding 400 mg of 50% benzalkonium chloride solution to 100 ml of βCD 0.1% aqueous solution to which fish gelatin was not added. went.
結果を図１に示した。すなわち、魚ゼラチンおよび塩化ベンザルコニウム塩の両方を添加したβＣＤ水溶液で処理した大腸菌液を塗布したプレートではまったく菌が認められなかった。
それに対し、魚ゼラチンを添加せず塩化ベンザルコニウム塩だけを添加したβＣＤ水溶液で処理した大腸菌液を塗布したプレートでは一面に大腸菌の生育が観られた。
The results are shown in FIG. That is, no bacteria were observed on the plate coated with the E. coli solution treated with βCD aqueous solution to which both fish gelatin and benzalkonium chloride salt were added.
On the other hand, the growth of E. coli was observed all over the plate coated with the E. coli solution treated with the βCD aqueous solution to which only fish benzalkonium chloride was added without adding fish gelatin.
（実施例５） ゼラチン含有シクロデキストリン水溶液噴霧塗布不織布の消臭性能／（消臭性能試験−１）
１０ｍｌのＬＢ培地（０．５％酵母エキス、１％ポリペプトン、０．５％塩化ナトリウム）に一晩同じＬＢ培地で培養した大腸菌液１０μｌを添加した液を作製した。大腸菌液を添加したＬＢ培地に実施例１で用いたのと同じ２ｃｍ角の合成繊維不織布４枚を浸漬、直ちに取り出し、プラスチックシャーレに入れ、乾燥しないようにシールした状態で３７℃、一晩培養した。培養後、同処理不織布４枚すべてが強い大腸菌臭を有することを確認した。
(Example 5) Deodorizing performance of spray-coated nonwoven fabric containing gelatin-containing cyclodextrin aqueous solution / (deodorizing performance test-1)
A solution was prepared by adding 10 μl of E. coli solution cultured in the same LB medium overnight to 10 ml of LB medium (0.5% yeast extract, 1% polypeptone, 0.5% sodium chloride). The same 4 cm 2 synthetic fiber nonwoven fabric used in Example 1 was immersed in LB medium supplemented with E. coli solution, immediately removed, placed in a plastic petri dish, and sealed at 37 ° C. overnight to prevent drying. did. After culturing, it was confirmed that all four of the treated nonwoven fabrics had a strong E. coli odor.
この大腸菌臭が強い不織布をそれぞれ一枚ずつプラスチックシャーレ（シャーレＡ、Ｂ、Ｃ、Ｄ）に入れた。次に、シャーレＡに実施例１で作製した作製後１８日経過ゼラチン含有シクロデキストリン液を用いて実施例１と同様に噴霧、乾燥、洗浄等を行った２ｃｍ角サイズの不織布を１枚、シャーレＢに同不織布を４枚入れ、シャーレＣには実施例１で比較対照として作製したβＣＤのみの液で処理した不織布４枚、シャーレＤには実施例１で同じく比較対照として作製した魚ゼラチンのみの液で処理した不織布１枚を入れ、各々シールした状態で室温に４時間静置した。静置後、各シャーレについて順に開放操作を行い、その開けた瞬間の臭いを大腸菌臭の強弱を指標に官能評価した。 One piece of each non-woven fabric with strong E. coli odor was placed in a plastic petri dish (petri dish A, B, C, D). Next, one piece of 2 cm square nonwoven fabric, which was sprayed, dried, washed, etc. in the same manner as in Example 1 using the gelatin-containing cyclodextrin solution produced in Example 1 after 18 days from preparation in the Petri dish, Petri dish Four sheets of the same non-woven fabric were put into B, and four pieces of non-woven fabric treated with only the βCD solution prepared as a comparison control in Example 1 were used in Petri dish C, and only fish gelatin prepared as a comparison control in Example 1 was also used in Petri dish D. One non-woven fabric treated with the above solution was put, and each was sealed and allowed to stand at room temperature for 4 hours. After standing, each petri dish was opened in order, and the odor at the opening was sensorially evaluated using the intensity of the Escherichia coli odor as an index.
表４に示した通り、シャーレＣおよびＤで強い大腸菌臭を有していたが、シャーレＡ、Ｂではその臭いに大幅な低下が認められた。特にシャーレＢではその低下は顕著であった。 As shown in Table 4, petri dishes C and D had a strong E. coli odor, but petri dishes A and B showed a significant reduction in odor. In particular, in Petri dish B, the decrease was remarkable.
Claims (4)
The polypeptide-containing cyclodextrin aqueous solution according to any one of claims 1 to 3, further comprising an antibacterial substance.
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