TWI533890B - 口腔保健抗菌材料以及潔牙劑組成物 - Google Patents
口腔保健抗菌材料以及潔牙劑組成物 Download PDFInfo
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- TWI533890B TWI533890B TW102105991A TW102105991A TWI533890B TW I533890 B TWI533890 B TW I533890B TW 102105991 A TW102105991 A TW 102105991A TW 102105991 A TW102105991 A TW 102105991A TW I533890 B TWI533890 B TW I533890B
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- zinc oxide
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- hollow tube
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- dentifrice composition
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- 239000000203 mixture Substances 0.000 title claims description 45
- 239000000463 material Substances 0.000 title claims description 22
- 239000012459 cleaning agent Substances 0.000 title 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 262
- 239000011787 zinc oxide Substances 0.000 claims description 129
- 239000000551 dentifrice Substances 0.000 claims description 31
- 239000002105 nanoparticle Substances 0.000 claims description 23
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- 238000000034 method Methods 0.000 claims description 7
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- 238000000224 chemical solution deposition Methods 0.000 claims description 3
- 239000013078 crystal Substances 0.000 description 17
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 208000002925 dental caries Diseases 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 238000004140 cleaning Methods 0.000 description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 8
- 239000000606 toothpaste Substances 0.000 description 8
- 229940034610 toothpaste Drugs 0.000 description 8
- 241000894006 Bacteria Species 0.000 description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 229940051866 mouthwash Drugs 0.000 description 7
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- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 4
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 4
- 239000003906 humectant Substances 0.000 description 4
- 231100000252 nontoxic Toxicity 0.000 description 4
- 230000003000 nontoxic effect Effects 0.000 description 4
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- 238000003756 stirring Methods 0.000 description 4
- 239000004246 zinc acetate Substances 0.000 description 4
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
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- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 2
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- -1 alkylene glycol Chemical compound 0.000 description 2
- RJGDLRCDCYRQOQ-UHFFFAOYSA-N anthrone Chemical compound C1=CC=C2C(=O)C3=CC=CC=C3CC2=C1 RJGDLRCDCYRQOQ-UHFFFAOYSA-N 0.000 description 2
- 150000003934 aromatic aldehydes Chemical class 0.000 description 2
- ZJRXSAYFZMGQFP-UHFFFAOYSA-N barium peroxide Chemical compound [Ba+2].[O-][O-] ZJRXSAYFZMGQFP-UHFFFAOYSA-N 0.000 description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 description 2
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical class C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 2
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- 235000010299 hexamethylene tetramine Nutrition 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- QPJVMBTYPHYUOC-UHFFFAOYSA-N methyl benzoate Chemical compound COC(=O)C1=CC=CC=C1 QPJVMBTYPHYUOC-UHFFFAOYSA-N 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- 238000000103 photoluminescence spectrum Methods 0.000 description 2
- 239000004323 potassium nitrate Substances 0.000 description 2
- 235000010333 potassium nitrate Nutrition 0.000 description 2
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- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 2
- XDFGPVSVSMWVQE-UHFFFAOYSA-M sodium;dodecanoic acid;hydrogen sulfate Chemical compound [Na+].OS([O-])(=O)=O.CCCCCCCCCCCC(O)=O XDFGPVSVSMWVQE-UHFFFAOYSA-M 0.000 description 2
- 239000000600 sorbitol Substances 0.000 description 2
- 239000000080 wetting agent Substances 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- 239000004343 Calcium peroxide Substances 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 244000223760 Cinnamomum zeylanicum Species 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 208000018035 Dental disease Diseases 0.000 description 1
- 238000002965 ELISA Methods 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
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- 235000006679 Mentha X verticillata Nutrition 0.000 description 1
- 244000024873 Mentha crispa Species 0.000 description 1
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- 244000227633 Ocotea pretiosa Species 0.000 description 1
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- 208000014151 Stomatognathic disease Diseases 0.000 description 1
- 241000194019 Streptococcus mutans Species 0.000 description 1
- 235000016639 Syzygium aromaticum Nutrition 0.000 description 1
- 244000223014 Syzygium aromaticum Species 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
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- 206010044038 Tooth erosion Diseases 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
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- 206010052428 Wound Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
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- 239000007844 bleaching agent Substances 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- LHJQIRIGXXHNLA-UHFFFAOYSA-N calcium peroxide Chemical compound [Ca+2].[O-][O-] LHJQIRIGXXHNLA-UHFFFAOYSA-N 0.000 description 1
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- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
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- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/884—Preparations for artificial teeth, for filling teeth or for capping teeth comprising natural or synthetic resins
- A61K6/887—Compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- A61K6/889—Polycarboxylate cements; Glass ionomer cements
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- A—HUMAN NECESSITIES
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- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0241—Containing particulates characterized by their shape and/or structure
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- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0241—Containing particulates characterized by their shape and/or structure
- A61K8/0279—Porous; Hollow
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- A—HUMAN NECESSITIES
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- 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
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
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- A—HUMAN NECESSITIES
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Cosmetics (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
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Description
本發明係關於一種口腔保健抗菌材料及/或潔牙劑組成物,尤指一種包含有結晶型氧化鋅奈米顆粒、結晶型氧化鋅奈米柱、奈米氧化鋅中空管、或其混合物之口腔保健抗菌材料及/或潔牙劑組成物。
蛀牙是十分常見的牙科疾病,也是牙科診療最常見的項目,而補牙則為一般蛀牙最常使用的治療方法。由於牙齒本身沒有修復的能力,蛀牙形成後不修補會使蛀洞愈大,惟有藉牙體復形工作,先除去窩洞中的腐敗物,並將適當的材料填補進去,才能阻止蛀牙的擴大,剛開始蛀牙時馬上填補即可治療,否則等到蛀進牙髓,不但疼痛尚且較難治療。
此外,口腔清潔也是口腔保健的重要一環,口腔清潔不僅可預防蛀牙,也是預防牙周病的基本方法。通常口腔清潔係以刷牙的方式進行,並伴隨著如牙膏、潔牙粉及漱口水等產品一同使用使牙齒清潔更提升,而有效去除齒菌斑,預防蛀牙。而若口腔清潔產品如牙膏、潔牙粉及漱口水等內添加有除去牙菌斑的物質(如,氧化鋅顆粒之潔牙劑組成物),則可降低蛀牙形成的機率。
因此,本領域極需一種可添加於牙齒窩洞填補材料或如牙膏、潔牙粉及漱口水等口腔清潔產品中之潔牙劑組成物,使提升預防蛀牙的效果,造福人群。
本發明係提供一種口腔保健抗菌材料,該口腔保健抗菌材料之材質係氧化鋅(ZnO),且該氧化鋅係選自由:結晶型氧化鋅奈米顆粒、結晶型氧化鋅奈米柱、奈米氧化鋅中空管、及其混合物所組成之群組;其中,該結晶型氧化鋅奈米顆粒之直徑係為25nm-200nm,該結晶型氧化鋅奈米柱之截面直徑係為50nm-1000nm,該奈米氧化鋅中空管係具有一中空管狀結構,且該及奈米氧化鋅中空管之截面直徑係為500nm-3μm。
本發明中之氧化鋅具有以下特點:可減少或抑制齲齒的形成;可減少或抑制齒齦炎(gingivitis);可增進口中疼痛或傷口的痊癒;可減少產酸細菌的水準;g.可抑制口腔中微生物生物膜(biofilm)形成;可減少牙菌斑累積;可減少牙齒受到侵蝕;及/或可協助清潔牙齒與口腔。
本發明之口腔保健抗菌材料中,該奈米氧化鋅中空管較佳可由複數個氧化鋅奈米顆粒所組成,而此構成奈米氧化鋅中空管之氧化鋅奈米顆粒大小較佳為20nm-100nm。亦即,奈米氧化鋅中空管較佳可具有多晶型(crystalline)結構。
本發明之口腔保健抗菌材料中,該結晶型氧化鋅奈米顆粒較佳可選自由:單晶型氧化鋅顆粒、多晶型氧化鋅顆粒、及其混合物所組成之群組。
本發明之口腔保健抗菌材料中,該結晶型氧化鋅奈米顆粒之直徑較佳可為50nm-100nm。
本發明之口腔保健抗菌材料中,該結晶型氧化鋅奈米柱之截面直徑較佳可為200nm-500nm。
本發明另提供一種潔牙劑組成物,包括:一口腔可接受賦形劑;以及一氧化鋅(ZnO),其係選自由:結晶型氧化鋅奈米顆粒、結晶型氧化鋅奈米柱、奈米氧化鋅中空管、及其混合物所組成之群組,該氧化鋅於該潔牙劑組成物中之含量係為10-60重量百分比;其中,該結晶型氧化鋅奈米顆粒之直徑係為25nm-200nm,該結晶型氧化鋅奈米柱之截面直徑係為50nm-1000nm,該奈米氧化鋅中空管係具有一中空管狀結構,且該及奈米氧化鋅中空管之截面直徑係為500nm-3μm。
本發明之潔牙劑組成物例如可為牙膏、牙粉、漱口水等清潔牙齒用之組成物。本發明之潔牙劑組成物由於包括有具結晶構造之氧化鋅,因此可更增加殺菌、維持口腔清潔之效果。同時,本發明潔牙組成物中所使用之氧化鋅因具有特殊的光催化活性與奈米尺度效應,故可達到自固性抗菌與深入隙縫清除牙菌的功效,而提升口腔清潔之效果。
各種其他成分可被組合於本發明之潔牙劑組成物中,包括去敏感劑,諸如硝酸鉀;潔白劑,諸如過氧化氫、過
氧化鈣及過氧化鍶;保存劑;矽酮及葉綠素化合物。這些添加劑,當存在時,被組合於本發明潔牙劑組成物中之用量為不會實質影響所期望之性質及特徵者。
本發明之潔牙劑組成物中,該口腔可接受賦形劑較佳可包括水、及濕潤劑。賦形劑通常為一種水、濕潤劑、醇之混合物。醇為無毒性醇,諸如乙醇或異丙醇。濕潤劑,諸如甘油、山梨醇、硫酸月桂酸鈉、礦物油、聚乙二醇或伸烷二醇(例如乙二醇或丙二醇)可存在之用量為約10至30重量%,口腔沖洗劑包含大於約45重量%之水,較佳約50至85重量%之水、約0至20重量%之無毒性醇及約10至40重量%之濕潤劑。
本發明之潔牙劑組成物,較佳可更包括一香味劑。被用於實施本發明之香味劑包括精油以及各種芳香醛類、酯類、醇類及類似物質。精油之實例包括綠薄荷、薄荷、冬青、黃樟、丁香、鼠尾草、尤加利、墨角蘭、肉桂、檸檬、萊姆、葡萄及柳橙之油。
本發明之潔牙劑組成物中,該奈米氧化鋅中空管較佳可由複數個氧化鋅奈米顆粒所組成。
本發明之潔牙劑組成物中,該氧化鋅奈米顆粒之直徑較佳可為20nm-100nm。
本發明之潔牙劑組成物中,該結晶型氧化鋅奈米顆粒較佳可選自由:單晶型氧化鋅顆粒、多晶型氧化鋅顆粒、及其混合物所組成之群組。
本發明之潔牙劑組成物中,該結晶型氧化鋅奈米顆粒之直徑較佳可為50nm-100nm。
本發明之潔牙劑組成物中,該結晶型氧化鋅奈米柱之截面直徑較佳可為200nm-500nm。
本實施例是以化學浴沉積法(chemical bath deposition method)合成氧化鋅奈米柱。其步驟包括:將0.1M硝酸鋅(Zn(NO3)2,購自Aldrich)加至0.1M的六次甲基四胺(Hexamethylenetetramine,HMTA)溶液中並均勻攪拌。而攪拌期間,由於氧化鋅成核現象,會有白色沉澱物產生。接著,迅速將此溶液移至95℃的爐中置放8小時使生長出氧化鋅晶體。晶體成長完成後,以3500rpm的離心速率離心10分鐘將晶體分離。接著,以蒸餾水以及乙醇依序沖洗分離得到的氧化鋅結晶奈米柱,最後乾燥得到本實施例之氧化鋅結晶奈米柱(截面直徑約為200nm-500nm)。
本實施例是以模板輔助法(Template-based method)生成奈米氧化鋅中空管。其步驟包括:以棉纖維(5cmx5cm)作為模板將其浸於3.5%醋酸鋅(購自JTBaker)溶液中,使棉纖維表面附有醋酸鋅。接著,以50℃乾燥2小時移除濕氣以降低孔洞形成。然後,將該表面附有醋酸鋅之棉纖維以600℃之烘箱、於空氣氣氛(air atmosphere)中煅燒
(calcined)2小時,接著緩慢冷卻至室溫。於煅燒期間,該些棉纖維會被燒成二氧化碳、水、以及其他碳氫化合物小分子,並且醋酸鋅煅燒成氧化鋅,而生成得到本實施例中空管狀之奈米氧化鋅中空管。
本實施例中空管狀之奈米氧化鋅中空管具有多晶型(crystalline)結構,亦即,本實施例之奈米氧化鋅中空管是由複數個直徑約20nm-100nm之氧化鋅奈米顆粒構成。
取實施例2之奈米氧化鋅中空管,將其搗碎後可得到複數個粒徑大小範圍為約50-100nm的氧化鋅奈米顆粒(grains)。
本實施例之潔牙劑組成物為牙膏,其製備方法為1.75g羧甲基纖維素鈉(城乙化工)加入7mL水攪拌至呈現外觀為透明膠體;20g聚乙二醇(PEG 400,J.T.BAKER)、8.2g甘油(wako)、0.02g苯甲酸甲脂(城乙化工)、2g硫酸月桂酸鈉(sigma)加入1mL水,攪拌均勻混合後,再加入之前配置的羧甲基纖維素鈉中,充分混合,置於研缽中,一邊攪拌研磨一邊緩慢加入10g結晶型氧化鋅奈米柱與40g碳酸鈣;最後加入1g礦物油(showa)並以水補到總體積為100mL。
本實施例中,結晶型氧化鋅奈米柱亦可選擇性地由實施例2所製得之奈米氧化鋅中空管或是實施例3所製得之氧化鋅奈米顆粒代替。
此外,選擇性地,各種其他成分也可被組合於本發明實施例之潔牙劑組成物中,例如去敏感劑,諸如硝酸鉀;潔白劑,諸如過氧化氫、過氧化鈣及過氧化鍶;保存劑;矽酮及葉綠素化合物。這些添加劑,當存在時,可被組合於本發明實施例之潔牙劑組成物中之用量為不會實質影響所期望之性質及特徵者。
本實施例中,濕潤劑,諸如甘油、山梨醇、聚乙二醇或伸烷二醇(例如乙二醇或丙二醇)可存在之用量為約1至10重量%,例如作為口腔沖洗劑可包含大於約45重量%之水,較佳約50至85重量%之水、約0至20重量%之無毒性醇及約10至40重量%之濕潤劑。
此外,選擇性地,本實施例之潔牙劑組成物亦可更包含香味劑,如精油以及各種芳香醛類、酯類、醇類及類似物質。
此外,當本實施例之潔牙劑組成物製作成漱口水時,潔牙劑組成物可更包括一醇,如乙醇或異丙醇之無毒性醇。
取市售氧化鋅顆粒(購自SHOFU,HY-Bond)、實施例1所製得之氧化鋅結晶奈米柱、及實施例2所製得之奈米氧化鋅中空管以X-光繞射(X-ray Diffraction,以Rigaku D/MAX-2000機型進行)分析其晶體結構。所得到之結果如圖1所示。
由圖1的XRD圖形可看出,此些氧化鋅與六方鎢采結構(hexagonal wurtzite structure)標準品所測得之標準數據
(JCPDS,36-1451)相當接近。此外,由圖1中可看到,本發明所合成得到之氧化鋅(氧化鋅結晶奈米柱、奈米氧化鋅中空管)之圖形中無出現雜質波峰,也代表著由本發明所合成得到之氧化鋅具有相當高的純度。
取市售氧化鋅顆粒(購自SHOFU,HY-Bond)、實施例1所製得之氧化鋅結晶奈米柱、及實施例2所製得之奈米氧化鋅中空管進行場發射掃描式電子顯微鏡(FE-SEM,JEOL JSM-7000F)照相。所得到之結果如圖2A-2C所示。
由圖2A可看到,市售氧化鋅顆粒的大小約為數個微米,且其形狀不規則。
由圖2B可看到,本發明實施例1所製得之氧化鋅結晶奈米柱具有六角柱狀之結構,且其直徑範圍約200-500nm。
由圖2C可看到,本發明實施例2所製得之奈米氧化鋅中空管維持了棉纖維的原有形狀,且其直徑範圍為約1-2μm。
取實施例2所製得之奈米氧化鋅中空管進行穿透式電子顯微分析(transmission electron microscopy,TEM,JEOL 2010),分析其組成顆粒,結果如圖2D所示,
由圖2D可看到,實施例2之奈米氧化鋅中空管係由非常大量的氧化鋅奈米顆粒接合而成,而此些氧化鋅奈米顆粒之粒徑大小範圍為約50-100nm。
取市售氧化鋅顆粒(購自SHOFU,HY-Bond)、實施例1所製得之氧化鋅結晶奈米柱、及實施例2所製得之奈米氧化鋅中空管,以螢光分析儀(型號:Perkin-Elmer LS55),使用氙燈雷射(xenon laser)、以325nm作為激發源,進行室溫光激光譜(photoluminescence spectra)測試,其所得之光致螢光光譜係如圖3A-3C所示,其中圖3A為氧化鋅結晶奈米柱,圖3B為奈米氧化鋅中空管,圖3C為取市售氧化鋅顆粒。
由圖3A-3C可看到,其光譜主要包含紫外光放射(約375nm)及綠光放射(約530nm)。此綠光波峰是電子在光致電洞(photogenerated hole)與帶一個正電的氧空位之間的躍遷所放出的光子。該強度與氧化鋅材料的尺寸相關。詳細地說,當氧化鋅材料的尺寸降至奈米等級時,綠光波峰的強度則會增加,甚至於某些情形會高於UV的吸收峰。此外,氧化鋅結晶奈米柱的測試結果有紅位移的現象,其可能是由於型態與球形不同而造成。
取市售氧化鋅顆粒、實施例1所製得之氧化鋅結晶奈米柱、及實施例2所製得之奈米氧化鋅中空管進行微-最小抑菌濃度試驗(micro-MIC test)。其首先將轉糖鏈球菌(Streptococcus mutans,ATCC 25175)隔夜活化,接著移置96孔微量盤,測得初始細胞OD600nm為0.03。使測試標準菌長至對數生長期中期(mid-log phase)。稱出適當重量的氧化鋅並加入至營養培養基(nutrient broth)中,使氧化鋅的最終濃度範圍至約每1000μl孔中0.05mg/ml與0.1mg/ml。使用不
含氧化鋅的培養基作為控制組。將沒有微生物,但含有相同濃度氧化鋅作為空白組。經過37℃、4小時的培養後,將96孔微量盤以酵素免疫分析測讀儀(ELISA reader,TECAN,sunrise)、600nm的波長分析。以MIC50作為抑制50%菌的最低濃度,與不含氧化鋅之控制組比較。
所測得結果如圖4所示。由圖4可看到,本發明之氧化鋅結晶奈米柱、以及奈米氧化鋅中空管在濃度為0.05mg/ml或以上時,對於細菌的抑制效果很明顯優於市售的氧化鋅顆粒。由此可證實本發明之氧化鋅結晶奈米柱、或奈米氧化鋅中空管應用於口腔保健抗菌材料或潔牙劑組成物時,可更減少或抑制齲齒的形成,更提升預防蛀牙的效果。
綜上所述,本發明之口腔保健抗菌材料及/或潔牙劑組成物由於包含有結晶型氧化鋅奈米顆粒、結晶型氧化鋅奈米柱、奈米氧化鋅中空管、或其混合物,具有特殊的催化活性與奈米尺度效應,故可達到自固性抗菌與深入隙縫清除牙菌,且對於細菌具有更好抑制效果,故更優於傳統含有大粒徑之氧化鋅顆粒的口腔保健抗菌材料及/或潔牙劑組成物。
上述實施例僅係為了方便說明而舉例而已,本發明所主張之權利範圍自應以申請專利範圍所述為準,而非僅限於上述實施例。
圖1係本發明測試例1之X-光繞射圖。
圖2A-2C係本發明測試例2之場發射掃描式電子顯微鏡照相圖。
圖2D係本發明測試例3之穿透式電子顯微鏡照相圖。
圖3A-3C係本發明測試例4之室溫光致螢光光譜。
圖4係本發明測試例5之細菌抑制效果測試圖。
Claims (8)
- 一種口腔保健抗菌材料,該口腔保健抗菌材料之材質係氧化鋅(ZnO),且該氧化鋅包含:結晶型氧化鋅奈米柱、或奈米氧化鋅中空管、或兩者之混合物;其中,該結晶型氧化鋅奈米柱之截面直徑係為200nm-1000nm,該奈米氧化鋅中空管係具有一中空管狀結構,且該奈米氧化鋅中空管之截面直徑係為500nm-3μm;其中,該結晶型氧化鋅奈米柱係以化學浴沉積法合成,而該奈米氧化鋅中空管係以模板輔助法合成。
- 如申請專利範圍第1項所述之口腔保健抗菌材料,其中,該奈米氧化鋅中空管係由複數個氧化鋅奈米顆粒所組成。
- 如申請專利範圍第2項所述之口腔保健抗菌材料,其中,該氧化鋅奈米顆粒之直徑係為20nm-100nm。
- 如申請專利範圍第1項所述之口腔保健抗菌材料,其中,該結晶型氧化鋅奈米柱之截面直徑係為200nm-500nm。
- 一種潔牙劑組成物,包括:一口腔可接受賦形劑;以及氧化鋅(ZnO),其包含:結晶型氧化鋅奈米柱、或奈米氧化鋅中空管、或兩者之混合物,該氧化鋅於該潔牙劑組成物中之含量係為10-60重量百分比; 其中,該結晶型氧化鋅奈米柱之截面直徑係為200nm-1000nm,該奈米氧化鋅中空管係具有一中空管狀結構,且該奈米氧化鋅中空管之截面直徑係為500nm-3μm;其中,該結晶型氧化鋅奈米柱係以化學浴沉積法合成,而該奈米氧化鋅中空管係以模板輔助法合成。
- 如申請專利範圍第5項所述之潔牙劑組成物,其中,該奈米氧化鋅中空管係由複數個氧化鋅奈米顆粒所組成。
- 如申請專利範圍第6項所述之潔牙劑組成物,其中,該氧化鋅奈米顆粒之直徑係為20nm-100nm。
- 如申請專利範圍第5項所述之潔牙劑組成物,其中,該結晶型氧化鋅奈米柱之截面直徑係為200nm-500nm。
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TWI533890B true TWI533890B (zh) | 2016-05-21 |
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TW101137418A TWI449544B (zh) | 2012-02-23 | 2012-10-11 | 硬組織修補複合材料及其製作方法 |
TW102105991A TWI533890B (zh) | 2012-02-23 | 2013-02-21 | 口腔保健抗菌材料以及潔牙劑組成物 |
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TW101137418A TWI449544B (zh) | 2012-02-23 | 2012-10-11 | 硬組織修補複合材料及其製作方法 |
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JP7278957B2 (ja) * | 2017-03-15 | 2023-05-22 | スリーエム イノベイティブ プロパティズ カンパニー | グラスアイオノマー組成物及び無機繊維を含む方法 |
CN111994944B (zh) * | 2020-09-01 | 2021-10-22 | 浙江大学 | 一种以α-半水石膏为模板导向的中空氧化锌微球的制备方法 |
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US4152418A (en) * | 1970-04-01 | 1979-05-01 | Lever Brothers Company | Zinc and enzyme mouthwash and mouthwash concentrate for reducing dental plaque and calculus formation |
WO2003057792A2 (en) * | 2001-12-29 | 2003-07-17 | 3M Innovative Properties Company | Composition containing a polymerizable reducing agent, kit, and method |
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2012
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2013
- 2013-02-21 TW TW102105991A patent/TWI533890B/zh not_active IP Right Cessation
- 2013-02-21 US US13/772,429 patent/US20140056948A1/en not_active Abandoned
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TWI449544B (zh) | 2014-08-21 |
US20140056948A1 (en) | 2014-02-27 |
US20130236519A1 (en) | 2013-09-12 |
TW201334815A (zh) | 2013-09-01 |
TW201334796A (zh) | 2013-09-01 |
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