JP5806698B2 - 新規抗微生物性基体およびその使用 - Google Patents
新規抗微生物性基体およびその使用 Download PDFInfo
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- JP5806698B2 JP5806698B2 JP2013077746A JP2013077746A JP5806698B2 JP 5806698 B2 JP5806698 B2 JP 5806698B2 JP 2013077746 A JP2013077746 A JP 2013077746A JP 2013077746 A JP2013077746 A JP 2013077746A JP 5806698 B2 JP5806698 B2 JP 5806698B2
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- metal particles
- metal
- electron donating
- silver
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- 230000000845 anti-microbial effect Effects 0.000 title description 17
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- 239000002923 metal particle Substances 0.000 claims description 61
- 229910052709 silver Inorganic materials 0.000 claims description 57
- 229910052751 metal Inorganic materials 0.000 claims description 56
- 239000002184 metal Substances 0.000 claims description 56
- 239000004332 silver Substances 0.000 claims description 56
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 53
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- 239000010931 gold Substances 0.000 claims description 43
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- 229910052763 palladium Inorganic materials 0.000 claims description 38
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 34
- 238000000151 deposition Methods 0.000 claims description 30
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
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- 239000004676 acrylonitrile butadiene styrene Substances 0.000 claims description 5
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- BBKFSSMUWOMYPI-UHFFFAOYSA-N gold palladium Chemical compound [Pd].[Au] BBKFSSMUWOMYPI-UHFFFAOYSA-N 0.000 claims 2
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- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 7
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- 239000003381 stabilizer Substances 0.000 description 4
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- 229910052782 aluminium Inorganic materials 0.000 description 3
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- 229910001961 silver nitrate Inorganic materials 0.000 description 2
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- 235000011083 sodium citrates Nutrition 0.000 description 2
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- PJVXUVWGSCCGHT-ZPYZYFCMSA-N (2r,3s,4r,5r)-2,3,4,5,6-pentahydroxyhexanal;(3s,4r,5r)-1,3,4,5,6-pentahydroxyhexan-2-one Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O.OC[C@@H](O)[C@@H](O)[C@H](O)C(=O)CO PJVXUVWGSCCGHT-ZPYZYFCMSA-N 0.000 description 1
- FUSNOPLQVRUIIM-UHFFFAOYSA-N 4-amino-2-(4,4-dimethyl-2-oxoimidazolidin-1-yl)-n-[3-(trifluoromethyl)phenyl]pyrimidine-5-carboxamide Chemical compound O=C1NC(C)(C)CN1C(N=C1N)=NC=C1C(=O)NC1=CC=CC(C(F)(F)F)=C1 FUSNOPLQVRUIIM-UHFFFAOYSA-N 0.000 description 1
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- 102000003886 Glycoproteins Human genes 0.000 description 1
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- 241000588748 Klebsiella Species 0.000 description 1
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- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- NEIHULKJZQTQKJ-UHFFFAOYSA-N [Cu].[Ag] Chemical compound [Cu].[Ag] NEIHULKJZQTQKJ-UHFFFAOYSA-N 0.000 description 1
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- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
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- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
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- 150000001879 copper Chemical class 0.000 description 1
- YCKOAAUKSGOOJH-UHFFFAOYSA-N copper silver Chemical compound [Cu].[Ag].[Ag] YCKOAAUKSGOOJH-UHFFFAOYSA-N 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
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- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine hydrate Chemical compound O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 239000012493 hydrazine sulfate Substances 0.000 description 1
- 229910000377 hydrazine sulfate Inorganic materials 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- TVZISJTYELEYPI-UHFFFAOYSA-N hypodiphosphoric acid Chemical compound OP(O)(=O)P(O)(O)=O TVZISJTYELEYPI-UHFFFAOYSA-N 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
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- 210000004185 liver Anatomy 0.000 description 1
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- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
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- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
- AVTYONGGKAJVTE-OLXYHTOASA-L potassium L-tartrate Chemical compound [K+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O AVTYONGGKAJVTE-OLXYHTOASA-L 0.000 description 1
- 229940111695 potassium tartrate Drugs 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 239000001476 sodium potassium tartrate Substances 0.000 description 1
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 1
- 239000001433 sodium tartrate Substances 0.000 description 1
- 229960002167 sodium tartrate Drugs 0.000 description 1
- 235000011004 sodium tartrates Nutrition 0.000 description 1
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 description 1
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- YUOWTJMRMWQJDA-UHFFFAOYSA-J tin(iv) fluoride Chemical compound [F-].[F-].[F-].[F-].[Sn+4] YUOWTJMRMWQJDA-UHFFFAOYSA-J 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/08—Materials for coatings
- A61L31/082—Inorganic materials
- A61L31/088—Other specific inorganic materials not covered by A61L31/084 or A61L31/086
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
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Description
本発明は、反復可能および制御された様式で抗微生物特性に関して表面特性を改変することを可能とするナノ粒子を有する新規な抗微生物性基体に関する。改変されうる表面特性の例としては、これらに限定されないが、疎水性、タンパク質吸着および細菌の付着が挙げられる。本発明の基体の使用の例としてはこれらに限定されないが、細菌の定着の遅延、細菌の感染、特に院内感染の防止である。本発明はさらに、該新規な基体を含む対象にも関する。本発明はさらに該基体の使用に関する。最後に、本発明はかかる基体の製造方法にも関する。
表面特性を有用な特性を達成するように改変することが常に望まれてきた。特に、抗微生物対象に関して重要である表面特性を改変することを可能にすることが望まれている。様々な目的での既知の表面改変の例を以下に記載する。
表面に関する技術水準における問題は、例えば、抗微生物性であって、疎水性、タンパク質吸着、および細菌の付着を反復可能に改変することが出来る、表面の提供方法である。
定義
本発明を詳細に開示および記載する前に、本発明は本明細書に開示された特定の配置、方法の工程および材料に限定されず、かかる配置、方法の工程および材料はいくらか変動しうることを理解されたい。また本明細書において用いる用語は、特定の態様を記載する目的でのみ用いられており、限定の意図はないことを理解されたい。本発明の範囲は添付の請求の範囲およびその均等物にのみ限定されるからである。
本発明によると、基体は所望の特性を示すよう処理される。基体は広範な材料から構成されうる。一つの態様において、基体は電子供与表面を有する材料から構成される。別の態様において、それは電子供与表面を有さない材料から構成される。電子供与表面の場合、金属粒子を電子供与表面に直接適用してもよい。表面が電子供与性でない場合、電子供与表面を作るには電子供与材料の層が適用されなければならない。
1.前処理
2.すすぎ
3.活性化
4.電子供与表面の沈着
5.すすぎ
6.金属粒子の沈着
7.すすぎ
8.乾燥。
1.すすぎ
2. 金属粒子の沈着
3.すすぎ
4.乾燥。
金属粒子の量の関数としての表面の疎水性
銀の均一な層を以下の方法にしたがってガラス基体上に沈着させた。基体をクロム酸洗浄溶液に5 分間58℃で浸漬し、次いで脱塩水ですすいだ。基体表面を塩化第一スズ水溶液中での浸漬により活性化し、次いで脱塩水ですすいだ。基体表面を次いで銀イオンを含む3 沈着溶液中での浸漬により銀の均一な層でめっきした(plate)。これにより約 115オングストロームの厚さに対応する適用量1.2μg/cm2の銀表面が得られた。23% パラジウムおよび77% 金からなる粒子を次いで第一の銀表面上に金/パラジウムの金属粒子を含む希釈懸濁液中への浸漬により沈着させた。金属粒子の懸濁液を金塩およびパラジウム塩を還元剤で還元し、 懸濁液を安定化剤で安定化させることにより作った。基体を次いで脱塩水ですすぎ、乾燥させた。
金属粒子の量の関数としてのタンパク質吸着
銀の均一な層を二酸化ケイ素基体上に沈着させた。基体を20% 硫酸洗浄溶液に10 分間 室温で浸漬し、次いで脱塩水ですすいだ。基体表面を塩化第一スズ水溶液への浸漬により活性化し、脱塩水ですすいだ。基体表面を次いで銀イオンを含む沈着溶液の4 浴に浸漬することにより銀の均一な層でめっきした。これにより約 77 オングストロームの厚さに対応する0.8 μg/cm2の適用量を有する銀表面が得られた。95% パラジウムおよび5% 金からなる粒子を次いでPd/Au-粒子の希釈懸濁液への浸漬により第一の銀表面上に沈着させた。金属粒子の適用量はそれぞれ0.05、0.12、0.48および0.59 μg/cm2であった。基体を脱塩水ですすぎ、乾燥させた。
金属粒子の量の関数としての細菌の増殖
実施例 1に示す方法にしたがってパラジウム/金ナノ粒子を銀基底層上に様々な量にて沈着させた。粒子は95% パラジウムおよび5% 金を含んでいた。基底層における銀の量はすべてのサンプルについて一定に維持した。したがって沈着した Pd/Au 粒子の量は変動した。沈着したナノ粒子 (Pd/Au)の量の関数としての細菌の増殖を以下の方法を用いて研究した:
いくつかの種についての微生物増殖
パラジウム/金ナノ粒子をシリコーンの基体上の銀基底層上に、実施例 1に記載の方法にしたがって様々な量にて沈着させた。粒子は95% パラジウムおよび5% 金を含んでいた。基底層中の銀の量はすべてのサンプルについて一定に維持した。沈着したPd/Au 粒子の量は0.36 μg/cm2であった。様々な細菌株についての抗微生物特性を研究した。
緑膿菌(P. aeruginosa)の一次付着および細胞回復
実施例 1に記載の方法にしたがってパラジウム/金ナノ粒子を様々な量で銀の基層に沈着させた。基層における銀の量はすべてのサンプルについて一定に維持した。粒子中のAuおよび Pdの量を表5に示すように変動させた。
ポリエステル繊維の網をまず5% 水酸化カリウム 溶液で5分間30℃ですすいだ。脱塩水中で繰り返しすすいだ後、基体を1 g/l 塩化第一スズの酸性溶液に室温で10分間浸漬した。脱塩水ですすいだ後、それを2 g/l 硫酸銅、5 g/l 水酸化ナトリウム、50 g/l クエン酸ナトリウムおよび0.005 ml/l ホルムアルデヒドを含むめっき浴に10分間35℃で浸漬した。約 200 オングストロームの銅層が得られ、脱塩水で新たにすすいだ後、基体をそれぞれ0.05 g/lのパラジウム粒子および金粒子を含む粒子懸濁液に浸漬した。金属粒子の適用量は0.4 μg/cm2であった。
PMMA の基体を5% 塩酸で 2 分間清浄にし、次いで脱塩水ですすいだ後、0.02 g/l のスズイオンを含むpH2.5の溶液に浸漬した。すすいだ後、基体を0.005 g/lの銀イオン、0.02 ml/l アンモニア、0.05 g/l 水酸化カリウムおよび 0.0005 ml/l ホルムアルデヒドを含む溶液に5 分間室温で浸漬した。これにより0.12 μg/cm2 の銀を有する表面が得られた。すすいだ後、それを0.005 g/l パラジウム および0.002 g/l 金粒子を含む粒子懸濁液に浸漬した。金属粒子の適用量は0.05 μg/cm2であった。
不織ポリイミド基体をNaOH の12% 溶液に40℃で 10 分間浸漬した。脱塩水で繰り返しすすいだ後、それを0.5 g/l 塩化第一スズを含むアルコール溶液に5 分間室温で浸漬した。すすいだ後、それを実施例 3にしたがって銅浴に浸漬した。2 μg/cm2の銅層が得られた。すすいだ後、それを懸濁液の総重量に対して計算して1% のPdおよび0.2%の金粒子を含む懸濁液に浸漬した。金属粒子の適用量は0.6 μg/cm2であった。
ナイロン繊維を5% NaOHで10 分間40℃で清浄にし脱塩水ですすいだ後、pH 2.2の 0.6 g/l 塩化第一スズ溶液に15 分間室温で浸漬した。この後、表面は0.8 μg/cm2の銀量を含んでいた。新たにすすいだ後、それを実施例 2にしたがって銀浴に浸漬し、 新たにすすいだ後、1% Pdおよび0.05% Au 粒子を含む懸濁液に浸漬した。金属粒子の適用量は0.12 μg/cm2であった。
アルミニウムの基体を10% 硝酸および3% フッ化水素酸の溶液中で60℃で20 分間処理した。すすいだ後、基体を3 g/l 塩化第一スズの酸性溶液に浸漬し、新たに すすいだ後、実施例 2による銀浴に浸漬した。この工程の後、約80 オングストロームの銀量が表面上に得られた。さらにすすいだ後、基体を1% Pdおよび2% Au 粒子を含む懸濁液に浸漬した。金属粒子の適用量は0.7 μg/cm2であった。
PTFEの基体を水酸化ナトリウム水溶液中で5 分間エッチング処理した。すすぎおよび乾燥の後、それを 0.7 g/l 塩化第一スズを含む溶液に20 分間室温で浸漬した。基体をすすいだ後、0.2 g/l 硝酸銀、0.5 ml/l アンモニアおよび水酸化ナトリウムを含む pH 10.5のめっき浴に5 分間浸漬した。この工程の後約 2.2 μg/cmの銀量が表面上に得られた。新たにすすいだ後、それを3% Pd および0.1% Au 粒子を含む懸濁液に5 分間室温で浸漬した。金属粒子の適用量は0.03 μg/cm2であった。
ガラスプレートを10% 硫酸 および1% フッ化水素酸で室温で15 分間すすいだ。すすいだ後、それを1% フッ化スズ 溶液に浸漬し、 新たにすすいだ後、実施例 2による銀浴に浸漬した。この工程の後、約140 オングストロームの銀量が表面上に得られた。新たにすすいだ後それを1% ルテニウムおよび2% パラジウム 粒子を含む懸濁液に浸漬した。金属粒子の適用量は0.25 μg/cm2であった。
ステンレス鋼基体を15% 硝酸および5% HFの溶液に室温で30 分間浸漬し、次いで脱塩水ですすいだ。実施例 11の工程にしたがってプロセスを続けた。金属粒子の適用量は0.9 μg/cm2であった。
チタンの棒を18% 硝酸および2% HFの溶液 で20 分間室温で清浄にした。電子供与表面の適用および金属粒子の適用を実施例 11のように行った。金属粒子の適用量は0.6 μg/cm2であった。
Claims (23)
- 電子供与表面を有する基体であって、
該電子供与表面上に金属粒子が存在することを特徴とし、
該金属粒子が、パラジウムおよび金を含み、
該金属粒子の量が0.001〜8 μg/cm2であって、
該金属粒子は、被覆層を形成せず、該電子供与表面上に均一に分布した粒子またはクラスターであり、
該電子供与表面が、銀、銅および亜鉛からなる群より選択される金属である、基体。 - 該電子供与表面が、0.05〜12 μg/cm2の量にて該基体上に適用された前記電子供与材料の均一な層である請求項 1の基体。
- 該基体がポリマー性基体である請求項 1または2の基体。
- 該ポリマー性基体が、ラテックス、ビニル基を含むポリマー、シリコーン、ポリ塩化ビニル、ポリプロピレン、ポリウレタン、ポリエステル、エチレン酢酸ビニルのコポリメリゼート、ポリスチレン、ポリカーボネート、ポリエチレン、ポリアクリレート、ポリメタクリレート、アクリロニトリルブタジエンスチレン、ポリアミド、およびポリイミド、またはそれらの混合物からなる群から選択される請求項 3の基体。
- 該ポリマー性基体が、天然ポリマー、分解可能ポリマー、食用ポリマー、生分解性ポリマー、および医療グレードポリマーからなる群から選択される請求項 3の基体。
- 該基体が金属である請求項1または2の基体。
- 該金属が、ステンレス鋼、医療グレード鋼、チタン、医療グレードチタン、コバルト、およびクロム またはそれらの混合物からなる群から選択される請求項 6の基体。
- 該基体が、ガラス、無機質、ゼオライト、石およびセラミクスからなる群から選択される請求項1または2の基体。
- 該基体が、紙、木、織り繊維、繊維、セルロース繊維、革、炭素、炭素繊維、グラファイト、ポリテトラフルオロエチレン、およびポリパラフェニレンテレフタルアミドからなる群から選択される請求項1または2の基体。
- 該基体が粒子の形状を有する請求項1-9のいずれかの基体。
- 金属粒子の量が0.01〜4 μg/cm2である請求項1-10のいずれかの基体。
- 該金属粒子におけるパラジウムの金に対する比が0.01:99.99〜99.99:0.01である請求項1-11のいずれかの基体。
- 該金属粒子におけるパラジウムの金に対する比が0.5:99.5〜99.8:0.2である請求項1-11のいずれかの基体。
- 該金属粒子におけるパラジウムの金に対する比が2:98〜95:5である請求項1-11のいずれかの基体。
- 該金属粒子の平均サイズが10-10000 オングストロームである請求項1-14のいずれかの基体。
- 該金属粒子の平均サイズが100-600オングストロームである請求項1-14のいずれかの基体。
- 請求項 1-16のいずれかの基体を含む対象。
- 該対象が医療機器である請求項 17の対象。
- 該対象が使い捨て商品である請求項 17の対象。
- 該対象が歯科用品である請求項 17の対象。
- 請求項1-16のいずれかの基体の、細菌の増殖を阻止するための使用。
- 以下の工程を含む請求項1-16のいずれかの基体の製造方法:
a.銀、銅および亜鉛からなる群より選択される金属からなる電子供与表面を有する基体を準備する工程、
b. パラジウムおよび金を含む金属粒子を懸濁液から該基体の該電子供与表面上に沈着させる工程、
c.該基体をすすぐ工程、
d.該基体を乾燥させる工程。 - 工程a.は、該基体上に電子供与材料を沈着させて均一な層を形成することを含む請求項 22の方法。
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