JP6625051B2 - 広い範囲の微生物の除去のための官能基及び表面に吸着された柑橘類抽出物で改質されたナノ粒子の二酸化チタンナノ材料 - Google Patents
広い範囲の微生物の除去のための官能基及び表面に吸着された柑橘類抽出物で改質されたナノ粒子の二酸化チタンナノ材料 Download PDFInfo
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- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
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Classifications
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
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- A61K47/69—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/16—Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/02—Local antiseptics
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- A—HUMAN NECESSITIES
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- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/10—Antimycotics
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- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/12—Antivirals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
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- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Description
植物は、多くの成分を含有し、そして抗菌特性を有する新規な生物学的に活性な分子の価値ある供給源を構成する。前記の成分は、規格化された抽出物又は純粋な化合物の供給源のいずれかとしてある種の植物から抽出され、その化学的多様性のために、微生物の増殖の制御のために無制限の機会を提供する。多くの植物抽出物は、各種の細菌、酵母及びカビに対する抗菌活性を有するが、しかし生体活性成分の品質及び量の変化は、顕著な欠点である。規格化された抽出物を産出する有効な単離方法の開発、並びに前記抗菌剤の安全性及び毒性評価は、更なる研究を必要とする(45−47)。
米国特許第6,117,814号。この特許は、酸化チタンを含有する支持体を記載し、これは、更にその構造中に結合剤としてシリカ及びアルミナの両方を組込んでいる。前記結合剤の目的は、支持体に改良された機械的特性を与えることである。支持体のサイズの範囲は、約20〜120ミクロンである。前記支持体は、ゾル−ゲル法によって製造された約50%の結合剤を含む。
本明細書は以下の発明の開示を包含する:
[1]a)ナノ粒子の金属酸化物支持体、
b)表面に化学的に吸着された官能基、
c)表面及びポアに物理的に吸着されたハーブ及び果実抽出物
を含む、複合ナノ材料。
[2]前記ナノ粒子の金属酸化物が、約1nm〜約100nmの範囲の平均直径のサイズを有する、[1]に記載のナノ材料。
[3]ヒドロキシル、ホスフェート、サルフェート、クロライド、アミノ、メチル、フォレートであり、そして前記材料に病原性微生物に対する選択性の特性を与える、[1]に記載の官能基。
[4]表面に吸着されたハーブ又は果実抽出物を伴う二酸化チタンナノ材料を調製するための方法であって、
a)ハーブ及び果実抽出物を調製し、
b)前記表面を官能基の化学的吸着によって改質し、
c)ハーブ及び果実抽出物を物理的に吸着すること
を含む、前記方法。
[5][6]に記載の前記抽出物が、柑橘類植物及び果実の各種の部分、例えば、樹皮、幹、根、葉、皮、果肉、及び種からのものであることができる、[4]に記載の方法。
[6]前記表面の改質が、100〜400RPMの範囲の平均速度における一定の撹拌を維持しながら行われる、[4]に記載の方法。
[7]前記表面の改質が、30〜100℃の範囲内の一定の温度を維持しながら行われる、[4]に記載の方法。
[8]前記表面の改質が、[4]に記載の官能基を与える溶液を1.4%の濃度で加え、そして[4]に記載の順序でこれらを加えることによって官能基を化学的に吸着させることによって行われる、[4]に記載の方法。
[9]官能基の吸着による前記表面の改質が、それぞれの官能基を完全に吸着するために、[9]に記載のそれぞれの溶液の添加後、5〜30分の平均静置時間を必要とする、[4]に記載の方法。
[10]前記表面の改質が、30〜100℃の範囲の平均温度での乾燥期間を必要とする、[4]に記載の方法。
[11]前記ハーブ及び果実抽出物の吸着が、50m 2 /gより大きい又はそれに等しい表面積を有する[1]に記載のナノ材料を必要とする、[4]に記載の方法。
[12]前記ハーブ及び果実抽出物の吸着が、少なくとも70%の抽出物を含む、[6]及び[7]によって得られる抽出物を必要とする、[4]に記載の方法。
[13]前記ハーブ及び果実抽出物の吸着が、100〜400RPMの範囲の平均の一定の撹拌を維持することを必要とする、[4]に記載の方法。
[14]前記ハーブ及び果実抽出物の吸着が、30〜50℃の範囲の平均温度を維持することを必要とする、[4]に記載の方法。
[15]前記ハーブ及び果実抽出物の吸着が、24時間の撹拌期間を必要とする、[4]に記載の方法。
[16]a)[1]に記載のナノ材料、
b)各種の比率の選択された原材料
を含む、殺菌剤溶液。
抽出物の製造は、二つの工程を含む。第1に、エタノール工程で、選択された果実、前記果実は、ブドウ、タンジェリン、オレンジ、グレープフルーツ、レモン、グアバである、の種、葉、皮、及び殻が、24〜48時間、30〜50℃の温度で、100〜400RPMの一定の撹拌下で少なくとも70%のエチルアルコール溶液との接触に置かれる。アルコール部分は、抽出物から濾過によって除去される。
支持体を官能化するための方法は、抽出物を含ませるために改良される。
抽出物の組込みを実現するために、使用される酸化物は、50m2/gより大きい又はそれに等しい表面積を有していなければならない。
これらの例示的試験において、酸化チタンを支持体として使用した。
細胞培養
10%のウシ胎児血清(Invitrogen,Mexico D.F.)及び抗生物質(ペニシリン100IU/mL、ストレプトマイシン100mg/mL及びアムホテリシンB10mg/mL)(Sigma−Aldrich,Inc.,St.Louis M.USA)で補充された最小必須培地(MEM)(Gibco/BRL,NY,USA)を伴う25cm2フラスコにおいて、37℃で5%CO2を伴って培養されたMDCK細胞系が使用される。細胞は、80%集密まで増殖させなければならない。
試験管内、又はV字のウェルプレート上で、ウイルス含有試料の二重の希釈物を、赤血球の一定の懸濁液(一般的に10,000,000細胞/mLを使用)と一緒に混合し、そして次いでインキュベートした。結果を評価するために、加えた細胞の量を、分光光度計を使用して定量化し、完全な血液凝集(HA)を示す最終希釈度を、限界稀釈度と考え、そして血液凝集単位(HAU)として表示する。
3〜5日齢のヒヨコからの赤血球を使用する。ヒヨコを血液の抜き取りによって安楽死させ;血液をアルセバー液中に入れる。細胞を、1800×gで5分間の遠心によって数回洗浄し、上清が透明になった時点で、これを取出し、そして細胞をPBS中で10%に調節する。溶液を使用する時に、これをPBS中で0.5%に調節する。
それぞれのウイルスのバッチを滴定しなければならない。1:10〜1:2560の二重の希釈物を、0.05mLの体積のそれぞれの希釈物をV字底の96ウェルプレートのウェルに入れることによって作製した。対照としての赤血球のための一つのウェルを含めなければならない。
試験のために必要なウイルスの量並びに細胞に対する清浄薬の効果が標準化される。その表面上に吸着されたハーブ又は果実抽出物を伴う二酸化チタンナノ材料の溶液が、清浄薬容器からの推奨される希釈度(5リットルの水中に75mLを注ぐことによって調製)で使用される。40μlのウイルスを、異なったHAU(40、20及び4HAU)で希釈物と混合し、そして異なった時間:1、5及び15分の間インキュベートする。それぞれの相互作用時間からの混合物(ウイルス−ナノ材料)にMDCK細胞の集密単層を接種し、そして湿潤雰囲気及び5%CO2下で、37℃で2時間インキュベートする。その後、ウイルスの接種材料を除去し、ウシ胎児血清を含まない新鮮な培養培地を加え、そして単層を24時間インキュベートする。
MDCK細胞を、24ウェルプレート上で集密まで培養する。一定の感染性投与量のウイルスと混合された、異なった体積の清浄溶液が使用される。これらを10〜15分間室温でインキュベートし、そして次いで、マイクロタイタープレート上において単層の集密細胞を2時間接種する。
研究所の分析及び試料維持のために、分析される産物の代表的副次試料を無作為に選択し、そしてロット番号を記録する。
0.25Mのリン酸緩衝溶液
1000mLのメスフラスコで、34gの一塩基性リン酸カリウムを、500mLの水中に溶解し、水酸化ナトリウム溶液でpHを7.1〜7.3に調整し、水で体積を合わせ、混合し、そして100mLの部分に分割する。オートクレーブ中で394K(121℃)で15分間滅菌し、冷却し、そして冷蔵下で保存する。
1.25mLの0.25Mのリン酸緩衝溶液を、1Lのメスフラスコに入れ、そして水で体積を合わせ、混合し、そして試験管及びフラスコ中に、それぞれ9mL及び99mLで分割し、オートクレーブ中で394K(121℃)で15分間滅菌する。
40gのアゾレシチンを、280mLのポリソルベート80mL及び1.25mLのリン酸緩衝溶液と混合し、水で希釈して1Lを得る;水酸化ナトリウム滴定液又は塩酸滴定液でpHを7.2に調整し、次いで100mlの部分に分配する。オートクレーブ中で394K(121℃)で20分間滅菌する。
100mlの濃縮された中和用溶液を、25mlの0.25Mのリン酸緩衝溶液と混合し、1675mlの水を加え、一緒に混合し、そして20mm×150mmのネジ付き試験管に9mlの部分に分配する。オートクレーブ中で394K(121℃)で20分間滅菌する。
製品のラベル上の製造業者の説明により、培養培地を調製し、そして滅菌する。中和溶液を伴う、滅菌前の標準的な方法のための寒天培養培地の場合、1リットルの標準的方法のための寒天培養培地に25mLの中和溶液を加える。
表1に示す成分を一緒に混合し、溶解が起こるまで加熱し、pHを7.2に調整し、オートクレーブに入れ、そして394K(121℃)で15分間滅菌する。
黄色ブドウ球菌(Staphylococcus aureus)(EMB寒天)
大腸菌(Escherichia coli)(EMB寒天)
緑膿菌(Psudomona aeruginosa)
サルモネラ種(Salmonella sp)(EMB寒天)
エンテロバクター種(Enterobacter sp)(E.M.B.寒天)
肺炎桿菌(Klebsiella pneumoniae)(EMB寒天)
カンジダ・アルビカンス(Candida albicans)(EMB寒天)
黒色アスペルギルス(Aspergillus niger)(EMB寒天)
試験微生物の保存
微生物株を、斜面培養培地(7mlの栄養寒天)を伴う16mm×125mmの試験管に毎週再播種することによって保存し、20時間〜24時間、308K〜310K(35℃〜37℃)の温度でインキュベートし、そして冷蔵下で保存した。
試験の前に、それぞれの試験微生物の二つの再播種物を作製し、そして20時間〜24時間、308K〜310K(35℃〜37℃)の温度でインキュベートした。
99mLの滅菌された希釈リン酸緩衝溶液を含有するエルレンマイヤーフラスコに、1mLの試験微生物懸濁液を移し、そしてそれぞれが25〜250個のコロニーを含有するプレートを得るために必要な10倍法による希釈を行った。
1.株の播種及び培養;
2.残存細胞の決定;
3.試料の調製;
必要な場合、容器のラベル上で製造業者によって推奨されている産物の濃度に達するまで水で適当な希釈を行った。
それぞれの試験微生物のために、99mLの産物又はその稀釈物を、正確に、そして二重で測定し、ネジ蓋を持つ250mLの滅菌エルレンマイヤーフラスコに移した。
減少%の決定
初期の生存数及び残存細胞のプレートからの結果の平均値を求め、次いで以下の式を使用して減少%を計算した:
減少%=100−S×100/V.C.
式中:
Sは、残存細胞のCFU/mLであり、そして
V.C.は、初期生存数である。
殺菌剤とラベルされた産物は、初期の生存数が75〜125×108CFU/mLである場合、推奨される濃度における接触の30秒以内で生存数の99.999%の減少を持たなければならない。
有効性の試験を、AOAC966.04の方法論に基づいて行い、ここで、枯草菌に対する60個のレプリカ中、59個が得られた。
Claims (22)
- 消毒剤、防腐剤、治療剤又は洗浄剤組成物の調製のための二酸化チタンの複合ナノ材料であって、前記複合ナノ材料は、有機官能基と、無機ラジカルと、その表面及びポアに吸着させた果実及び/又はハーブの抽出物とで改質され、前記複合ナノ材料は、少なくとも50m2/gの表面積を有し、アナターゼ結晶構造をなし、二酸化チタンナノ粒子の平均サイズは直径1〜100nmであり、前記果実及び/又はハーブの抽出物の粒子サイズは0.3〜10nmであることを特徴とする複合ナノ材料。
- 前記有機官能基がヒドロキシルを含むことを特徴とする請求項1に記載の複合ナノ材料。
- 前記無機ラジカルがホスフェート、サルフェート、クロライド、アミノ、メチル及びフォレートを含むことを特徴とする請求項1に記載の複合ナノ材料。
- 前記果実及び/又はハーブの抽出物が花、蕾、種、葉、樹皮、草、木及び根から選択される植物の部分から得られる少なくとも3種の果実及び/又はハーブの抽出物の混合物を含んでいることを特徴とする請求項1に記載の複合ナノ材料。
- 前記果実の抽出物がタンジェリン、オレンジ、グレープフルーツ、レモンを含む柑橘類及びブドウ、グアバ、柘榴からなるグループから選択される植物の部分から得られることを特徴とする請求項1又は請求項4のいずれかに記載の複合ナノ材料。
- 前記ハーブの抽出物がオレガノ、桂皮又は胡椒から選択されることを特徴とする請求項1又は請求項4のいずれかに記載の複合ナノ材料。
- 消毒剤、防腐剤、治療剤又は洗浄剤の組成物の調製のための二酸化チタンの複合ナノ材料を得るための方法であって、
a)種、葉、皮、及び殻が所定温度で一定の撹拌下で少なくとも70%のエチルアルコール溶液との接触に置かれ、アルコール部分が抽出物から濾過によって除去される第1のエタノール工程で、果実及び/又はハーブの抽出物を製造する工程と、
b)蒸留水を第1のフラスコに入れて加熱する従来の蒸気トラップシステムを用いて、果実及びハーブの活性剤及びオーガニックオイルを抽出し、蒸留水を第1のフラスコに入れて加熱し、発生した蒸気を、前記第1のエタノール工程で得られた残渣が入っている高温に維持された第2のフラスコに管路を通して送り、前記蒸気を、前記第2のフラスコの出口で、循環冷水を有する凝縮器で回収し、得られた液体を、前記第1のエタノール工程で得られたものと混合し、混合物を、室温で12時間静置する工程と、
c)有機官能基及び無機ラジカルの前駆体溶液を、1.4%の濃度で調製する工程と、
d)二酸化チタンの複合ナノ材料支持体を、100〜400rpmの範囲の一定速度で撹拌した状態の水の入ったフラスコに入れて、前記工程c)で調製された有機官能基及び無機ラジカルの前駆体溶液を加えることによって、化学的に改質する工程と、
e)30〜100℃の温度で乾燥し残存する液体を除去する工程と、
f)前記工程b)で得られた70%抽出物の混合物の水溶液を取り出して一定の撹拌下のフラスコに入れ、前記官能基で処理した二酸化チタンの複合ナノ材料支持体をゆっくりと加え、一定の撹拌を維持する工程と
を有する方法。 - 前記果実の抽出物がタンジェリン、オレンジ、グレープフルーツ、レモンを含む柑橘類及びブドウ、グアバ、柘榴からなるグループから選択される植物の部分から得られることを特徴とする請求項7に記載の方法。
- 前記ハーブの抽出物がオレガノ、桂皮又は胡椒から選択されることを特徴とする請求項7に記載の方法。
- 前記抽出物の粒子サイズが0.3〜10nmであることを特徴とする請求項8又は請求項9に記載の方法。
- 前記工程a)において、前記撹拌が、100〜400rpmの速度で、30〜50℃の温度で、24〜48時間の間、維持されることを特徴とする請求項7に記載の方法。
- 前記工程b)において、前記第1のフラスコが100〜130℃の温度まで加熱され、前記第2のフラスコが40〜60℃の温度に維持される一方で、前記凝集器内の水の温度が4〜10℃であることを特徴とする請求項7に記載の方法。
- 前記二酸化チタンの複合ナノ材料支持体が少なくとも50m2/gの表面積を有し、アナターゼ結晶構造をなすものであることを特徴とする請求項7に記載の方法。
- 二酸化チタンナノ粒子の平均直径サイズが1〜100nmであることを特徴とする請求項7又は請求項13のいずれかに記載の方法。
- 二酸化チタン/水の比が1:200であることを特徴とする請求項7に記載の方法。
- 前記有機官能基がヒドロキシルを含むことを特徴とする請求項7に記載の方法。
- 前記無機ラジカルがホスフェート、サルフェート、クロライド、アミノ、メチル及びフォレートを含むことを特徴とする請求項7に記載の方法。
- 前記官能基及び無機ラジカルの前駆体溶液を一滴ずつ添加すること、その際、それぞれの溶液添加の間に待機時間をおいて添加することを特徴とする請求項16又は請求項17のいずれかに記載の方法。
- 前記官能基及び無機ラジカルの前駆体溶液を一回に一滴ずつ滴下により完全に加えることを特徴とする請求項18に記載の方法。
- それぞれの溶液添加の間の前記待機時間を5〜30分として、各有機官能基および無機ラジカルを前記複合ナノ材料支持体の表面およびポアに完全に吸着させることを特徴とする請求項18に記載の方法。
- 前記70%抽出物の混合物の水溶液が少なくとも3種の果実及び/又はハーブの抽出物であることを特徴とする請求項7に記載の方法。
- 有機官能基、無機ラジカル、及び、表面及びポアに吸着させたハーブ及び/又は果実の抽出物で改質された二酸化チタンの複合ナノ材料を最大40%と、許容可能な賦形剤とを含む、消毒剤、防腐剤、治療剤又は洗浄剤組成物。
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FI91713C (fi) | 1992-04-23 | 1994-08-10 | Axidental Oy | Uusia bioaktiivisia pinnotteita ja niiden valmistus ja käyttö |
EP0727427A4 (en) | 1993-11-05 | 1997-10-15 | Meiji Milk Prod Co Ltd | ANTIBACTERIAL, ANTIFUNGAL AND ANTIVIRAL AGENT |
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FR2835246B1 (fr) | 2002-01-29 | 2004-03-19 | Centre Nat Rech Scient | Polymere a base d'oxyde de titane |
CN1634604A (zh) * | 2004-11-18 | 2005-07-06 | 黄琴根 | 复合纳米空气净化材料 |
FR2881133B1 (fr) | 2005-01-27 | 2007-03-02 | Commissariat Energie Atomique | Procede de preparation de solutions sol-gel stable precurseurs de ceramiques oxydes a base de plomb, de titane, de zirconium et de lanthanide(s) et procede de preparation de ladite ceramique |
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KR20080102204A (ko) * | 2006-02-16 | 2008-11-24 | 작스트레벤 케미 게젤샤후트밋트베슈렝크테르하후트웅 | 살생물제 조성물 |
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CA2769627A1 (en) | 2009-06-30 | 2011-01-06 | The Trustees Of Columiba University In The City Of New York | Antimicrobial/preservative compositions comprising botanicals |
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MY160412A (en) | 2009-12-04 | 2017-03-15 | Colgate Palmolive Co | Oral compositions containing extracts of zingiber officinale and related methods |
CA2779708A1 (en) | 2009-12-04 | 2011-06-09 | Colgate-Palmolive Company | Oral compositions containing extracts of zizyphus joazeiro and related methods |
US8372382B2 (en) | 2010-10-01 | 2013-02-12 | Mary Kay, Inc. | Skin moisturizer and age fighting formula |
US8404743B2 (en) | 2010-10-29 | 2013-03-26 | Mary Kay Inc. | Zinc oxide complexes |
CN102077865B (zh) * | 2010-11-19 | 2013-12-04 | 华南农业大学 | 一种二氧化钛纳米颗粒及荔枝纳米保鲜剂 |
CN102772715A (zh) * | 2012-07-05 | 2012-11-14 | 成钢 | 释放微量元素负离子防螨防电磁波纳米富银硒锗蛇油膏 |
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MY184044A (en) | 2021-03-17 |
CU20150182A7 (es) | 2016-10-28 |
AU2014281904A1 (en) | 2016-02-18 |
CN105517956A (zh) | 2016-04-20 |
PH12015502838A1 (en) | 2016-03-21 |
IL243239B (en) | 2020-07-30 |
WO2014204290A1 (es) | 2014-12-24 |
HK1217099A1 (zh) | 2016-12-23 |
SA515370298B1 (ar) | 2017-06-07 |
KR20160034299A (ko) | 2016-03-29 |
EP3012225A1 (en) | 2016-04-27 |
EA201690030A1 (ru) | 2016-10-31 |
EA030364B1 (ru) | 2018-07-31 |
US10342840B2 (en) | 2019-07-09 |
AP2016009043A0 (en) | 2016-02-29 |
AR120069A2 (es) | 2022-02-02 |
CA2916216A1 (en) | 2014-12-24 |
ZA201509284B (en) | 2017-09-27 |
MX2013007201A (es) | 2014-12-22 |
SG11201510528YA (en) | 2016-01-28 |
JP2016530222A (ja) | 2016-09-29 |
AR096661A1 (es) | 2016-01-27 |
BR112015031884A2 (pt) | 2017-07-25 |
CR20160028A (es) | 2016-03-30 |
CN105517956B (zh) | 2017-09-29 |
MA38707A1 (fr) | 2017-09-29 |
US20160143981A1 (en) | 2016-05-26 |
MX339086B (es) | 2016-05-09 |
CL2015003674A1 (es) | 2016-08-19 |
UY35623A (es) | 2015-01-30 |
EP3012225A4 (en) | 2017-02-22 |
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