CN101600442A - 口腔护理产物 - Google Patents
口腔护理产物 Download PDFInfo
- Publication number
- CN101600442A CN101600442A CNA200780050884XA CN200780050884A CN101600442A CN 101600442 A CN101600442 A CN 101600442A CN A200780050884X A CNA200780050884X A CN A200780050884XA CN 200780050884 A CN200780050884 A CN 200780050884A CN 101600442 A CN101600442 A CN 101600442A
- Authority
- CN
- China
- Prior art keywords
- oral care
- care product
- compositions
- calcium
- tooth
- 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.)
- Granted
Links
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910001424 calcium ion Inorganic materials 0.000 claims abstract description 40
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 31
- 229940085991 phosphate ion Drugs 0.000 claims abstract description 28
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- 238000005282 brightening Methods 0.000 claims abstract description 23
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 108
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 239000011575 calcium Substances 0.000 claims description 16
- 239000001506 calcium phosphate Substances 0.000 claims description 15
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 15
- 235000011010 calcium phosphates Nutrition 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 235000012241 calcium silicate Nutrition 0.000 claims description 14
- 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 claims description 14
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 7
- 239000011574 phosphorus Substances 0.000 claims description 7
- 229910052698 phosphorus Inorganic materials 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 150000002500 ions Chemical class 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 239000011148 porous material Substances 0.000 claims description 4
- 208000002925 dental caries Diseases 0.000 claims description 3
- 239000002390 adhesive tape Substances 0.000 claims description 2
- 239000003814 drug Substances 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 claims description 2
- 239000000499 gel Substances 0.000 description 36
- 210000003298 dental enamel Anatomy 0.000 description 23
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 23
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 23
- -1 fluorine chemical compound Chemical class 0.000 description 20
- 210000003296 saliva Anatomy 0.000 description 20
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 17
- 239000010452 phosphate Substances 0.000 description 15
- 229910019142 PO4 Inorganic materials 0.000 description 14
- 238000012545 processing Methods 0.000 description 13
- 239000000463 material Substances 0.000 description 12
- 229940034610 toothpaste Drugs 0.000 description 12
- 239000000606 toothpaste Substances 0.000 description 12
- 239000000126 substance Substances 0.000 description 11
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 10
- 230000002087 whitening effect Effects 0.000 description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 9
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 9
- 229910001573 adamantine Inorganic materials 0.000 description 9
- 235000001465 calcium Nutrition 0.000 description 9
- 229960005069 calcium Drugs 0.000 description 9
- 229910052791 calcium Inorganic materials 0.000 description 9
- 239000008187 granular material Substances 0.000 description 9
- 229920001282 polysaccharide Polymers 0.000 description 9
- 239000005017 polysaccharide Substances 0.000 description 9
- 150000004804 polysaccharides Chemical class 0.000 description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- 239000000017 hydrogel Substances 0.000 description 8
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical group CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 7
- 238000001237 Raman spectrum Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 229920000642 polymer Polymers 0.000 description 7
- 238000001878 scanning electron micrograph Methods 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 230000008901 benefit Effects 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 230000003203 everyday effect Effects 0.000 description 6
- 210000000214 mouth Anatomy 0.000 description 6
- 238000005498 polishing Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 235000010413 sodium alginate Nutrition 0.000 description 6
- 239000000661 sodium alginate Substances 0.000 description 6
- 229940005550 sodium alginate Drugs 0.000 description 6
- 235000010443 alginic acid Nutrition 0.000 description 5
- 229920000615 alginic acid Polymers 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical group [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 4
- 229920002125 Sokalan® Polymers 0.000 description 4
- 229940072056 alginate Drugs 0.000 description 4
- 210000004268 dentin Anatomy 0.000 description 4
- 150000002978 peroxides Chemical class 0.000 description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000004408 titanium dioxide Substances 0.000 description 4
- 229940095688 toothpaste product Drugs 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 229920002472 Starch Polymers 0.000 description 3
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 3
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 3
- 159000000007 calcium salts Chemical class 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 229920000591 gum Polymers 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 235000019698 starch Nutrition 0.000 description 3
- 239000008107 starch Substances 0.000 description 3
- 229940032147 starch Drugs 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Natural products OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 229920002101 Chitin Polymers 0.000 description 2
- 229920001661 Chitosan Polymers 0.000 description 2
- GHXZTYHSJHQHIJ-UHFFFAOYSA-N Chlorhexidine Chemical compound C=1C=C(Cl)C=CC=1NC(N)=NC(N)=NCCCCCCN=C(N)N=C(N)NC1=CC=C(Cl)C=C1 GHXZTYHSJHQHIJ-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- 229920002558 Curdlan Polymers 0.000 description 2
- 239000001879 Curdlan Substances 0.000 description 2
- 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
- SHZGCJCMOBCMKK-UHFFFAOYSA-N D-mannomethylose Natural products CC1OC(O)C(O)C(O)C1O SHZGCJCMOBCMKK-UHFFFAOYSA-N 0.000 description 2
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
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- 229920002148 Gellan gum Polymers 0.000 description 2
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- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 2
- NBGXQZRRLOGAJF-UHFFFAOYSA-N Maltulose Natural products OC1C(O)C(O)C(CO)OC1OC1C(O)C(O)(CO)OCC1O NBGXQZRRLOGAJF-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- INVGWHRKADIJHF-UHFFFAOYSA-N Sanguinarin Chemical compound C1=C2OCOC2=CC2=C3[N+](C)=CC4=C(OCO5)C5=CC=C4C3=CC=C21 INVGWHRKADIJHF-UHFFFAOYSA-N 0.000 description 2
- 229920002305 Schizophyllan Polymers 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
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- 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
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Abstract
一种口腔护理产物,所述口腔护理产物包含钙离子源、磷酸根离子源和用于沉积于牙齿上的不溶性增白剂,其特征在于所述钙离子源和磷酸根离子源在产物使用前物理分离。
Description
本发明涉及适用于保持和/或增强牙质的口腔护理产物。所述产物包含不溶性增白剂和用于增白剂的双组合物输送系统。
牙齿的釉质层本来为不透明白色或略带灰色,然而,此牙釉质层可变得着色或变色。牙齿的釉质层由产生稍微多孔表面的羟基磷灰石矿物晶体组成。相信牙釉质层的这种多孔性质允许着色物质和变色物质透过牙釉质并使牙齿变色。
很多物质能使牙齿着色或降低牙齿的白度,具体为某些食品、烟草制品以及诸如茶和咖啡一类的流体。这些着色和变色物质通常能够透过牙釉质层。此问题经很多年逐渐发生,但却使牙齿釉质明显变色。
目前有多种产品用于牙齿增白。此类产品通常包含过氧化物(单独或与酶组合)。此类产品可以条的形式使用。此类产品一般必须在精确限定的时间后除去,如果保留太长时间,过氧化物就会损伤牙齿和/或牙龈。使用过氧化物(和包含擦洗剂的牙膏)的一个具体问题是能使牙齿表面变粗糙。
已知某些现有技术的处理导致在牙齿表面上产生羟基磷灰石。
US 5,605,675(Enamelon,1997)公开一种通过施加双相组合物使牙釉质重新矿化的方法,其中一相包含水溶性钙化合物,一相包含水溶性无机磷酸盐和水溶性氟化合物。
US 4,083,955(P&G,1978)公开一种通过依次施加两种组合物使牙釉质重新矿化的方法,第一种包含钙离子,第二种包含磷酸根离子,或者反之亦然。
WO 04/017929(Septodont ou Specialites Sepodont S.A.,2004)公开一种特别在牙科领域用于恢复矿化物质的制剂,所述制剂包含含水液体部分、包含至少一种选自硅酸三钙和硅酸二钙的硅酸盐的固体部分、氯化钙和减水剂。
本发明的目的是向牙齿表面输送不溶性增白剂,同时能够在牙齿的表面上产生羟基磷灰石。
本发明包括将钙离子源输送到牙齿表面,并通过同时或依次施加磷酸根离子源最终使钙离子原位转化成羟基磷灰石。钙离子源和磷酸根离子源从独立相输送,因此使它们过早相互作用的能力减到最小。
原位产生羟基磷灰石使牙齿重新矿化,潜在减少龋齿的可能性,并改善牙齿的外观,特别是改善其白度,并通过沉积增白剂产生增白效果。牙齿也可因此显得较为光滑和有光泽。由于很多“增白”处理使牙齿表面粗糙,因此,增白而减小表面粗糙度的能力是本发明的特别益处。
由本发明给予的益处主要是针对牙釉质;然而也可期望有利影响暴露的牙本质。
本发明的第一方面提供一种口腔护理产物,所述口腔护理产物包含钙离子源、磷酸根离子源和用于沉积于牙齿上的不溶性增白剂,其特征在于所述钙离子源和磷酸根离子源在产物使用前物理分离。
本发明的第二方面提供一种将不溶性增白剂输送到牙齿的方法,所述方法包括施加不溶性增白剂与钙离子源和磷酸根离子源的组合,其特征在于所述钙离子源和磷酸根离子源从物理分离的组合物施加。
本发明的第三方面提供用作药物的本发明第一方面的产物。
本发明的第四方面提供
1.钙离子源;
2.物理独立的磷酸根离子源;和
3.用于沉积于牙齿上的不溶性增白剂,
用于制备改善牙齿白度和/或减少龋齿和/或降低敏感性的口腔护理产物的用途。
本发明的产物包含不溶性增白剂和双输送系统,所述双输送系统一般包含含钙离子源的第一组合物和含磷酸根离子源的第二组合物。
不溶性增白剂通过沉积于牙齿上并因此改变其外观而起作用。相信在牙齿上沉积由双输送系统帮助,即,从独立的源施加钙离子和磷酸根离子。可使用以前面方式起作用的任何不溶性增白剂。
适合的不溶性增白剂为粒状固体。它们可包括白色颗粒,或者可包括蓝色颗粒;蓝色颗粒通过降低牙齿的“黄度”(b*)给予牙齿白度增加的外观。已发现不溶性增白剂与双输送系统协同作用,从而提高增白益处。
“不溶性增白颗粒”在口腔通常的温度下不溶于水。不溶性增白颗粒一般具有在25℃小于0.01mol/L的溶解度。
不溶性增白颗粒优选具有200nm至300nm,更优选220nm至280nm,最优选245nm至265nm的平均粒径。这些粒径是优选的,因为它们给予最强的蓝光散射(波长约450nm),因此给予最佳的增白特性。平均粒径为数均粒径,并可从以次级电子图像(SEI)模式拍摄的扫描电子显微镜(SEM)图像的图像分析计算。
不溶性增白颗粒优选以0.01%重量至5%重量,更优选0.03%重量至2.5%重量的量加入它们所属的组合物。
为白色颗粒的不溶性增白颗粒是优选的,特别是二氧化钛和氧化锌。使用时,这些颗粒优选以0.1%重量至5%重量,更优选0.25%重量至3%重量,最优选0.5%重量至2.5%重量的量加入它们所属的组合物。
在本发明环境下,蓝色颗粒具有在CIELAB系统220至320°,优选250至290°的色彩角h。使用时,这些颗粒优选以0.01%重量至0.3%重量,更优选0.02%重量至0.1%重量,最优选0.03%重量至0.08%重量的量加入它们所属的组合物。蓝色颗粒为蓝色颜料,优选为颜料蓝15,更优选为颜料蓝15:1、15:2、15:3、15:4、15:5或15:6,最优选为颜料蓝15:1。
优选的钙离子源为不溶性钙盐。在使用此钙离子源的实施方案中,相信钙在与口腔唾液中磷酸盐的任何过早相互作用之前沉积于牙齿上。在牙釉质和/或牙本质上已沉积后,与唾液中存在的磷酸盐和重要的是利用第二种组合物加入的磷酸盐缓慢反应,导致恰好在需要处产生羟基磷灰石,并帮助沉积不溶性增白剂。
适合的不溶性钙盐可以为能够在施加组合物时输送到牙齿表面的磷酸钙以外的任何盐,磷酸钙不为本发明的钙离子源。因此,诸如羟基磷灰石和氟磷灰石的钙盐不是适合的不溶性钙盐。
优选的不溶性钙盐为硅酸钙(CS),作为复合物质氧化钙-二氧化硅:CaO-SiO2存在。优选使用此不溶性钙盐,因为其在牙齿表面上转化为羟基磷灰石极佳。不受理论限制,相信CS与磷酸根离子反应生成钙硅酸盐-磷酸盐粘固物(calcium silicate-phosphate cement)(CSPC),并且此物质强力结合到牙齿,然后逐渐在牙齿表面上转变成羟基磷灰石。相信CSPC对牙齿表面的高亲合力成为得到优良重新矿化和增白益处的基础。
在利用CS时,钙与硅之比(Ca∶Si)可以为1∶10至3∶1。Ca∶Si之比优选为1∶5至2∶1,更优选1∶3至1∶1,最优选约1∶2。CS可包括硅酸单钙、硅酸二钙或硅酸三钙。钙与硅的较高比率是优选的,因为相信此比率促进对牙齿表面的有效结合及随后转变成羟基磷灰石;然而,为了容易得到所需pH,较低比率也是优选的(参见下文)。
应了解,在整个说明书中钙与硅之比(Ca∶Si)为原子比。
优选不溶性钙盐为“生物物质”,生物物质是指能够结合到人和/或动物组织的物质。生物物质能够结合到牙釉质和/或牙本质尤其优选。
“不溶性钙盐”在口腔通常温度不溶于水。不溶性钙盐一般具有在25℃小于0.01mol/L的溶解度。
适合的不溶性钙盐可以为结晶态或非晶态,优选为非晶态,更优选为中孔态,即,为具有1至50微米直径孔的物质。中孔硅酸钙特别优选,在本说明书中缩写为MCS。
在本发明的一个方面,MCS具有优选0.4至4nm,更优选0.4至3.5nm,最优选0.4至3nm的平均孔径(直径)。
在本发明的另一个方面,MCS具有优选2至4nm,更优选2至3.5nm,最优选2至3nm的平均孔径(直径)。
在本发明的另一个方面,MCS具有优选1至2.7nm,更优选1.35至2.45nm的平均孔径(直径)。
孔径可用任何适合方法或装置测定。例如,孔径可用BET氮吸附或汞孔隙率测定技术(特别是BET氮吸附技术)测定。
钙离子源的含量一般为要施加到牙齿上的产物的所有制剂组分重量的0.05至25%重量,特别是0.5至15%重量,尤其是2.5至10%重量。就它所属的具体组合物而言,钙离子源一般以0.1至50%重量,特别是1至30%重量,尤其是5至20%重量存在。
优选钙离子源存在于基本不含磷酸根离子的组合物中。词语“基本不含”是指磷酸根离子的量相对于钙离子重量小于2.5%重量,特别小于1%重量,更特别小于0.1%重量,尤其小于0.01%重量。通过使用高纯度原料,例如,使用China National Pharmaceutical GroupCorporation(SINOPHARM),Beijing提供的纯度大于99%的氮化钙,可制备含小于0.005%重量磷酸根离子的氧化钙-二氧化硅。
优选钙离子源存在于基本不含氟离子的组合物中。词语“基本不含”是指氟离子的量相对于不溶性钙盐中钙的重量小于2.5%重量,特别小于1%重量,更特别小于0.1%重量,尤其小于0.01%重量。
适用于本发明的硅酸钙可通过同时待审申请PCT/EP2007/057556中所述的方法制备。
钙离子源优选存在于具有7至11,更优选8至10.5,最优选9至10pH的组合物中。这些组合物优选包含酸性缓冲剂,如柠檬酸。这些物质使组合物能够以所需pH配制,并且特别合乎需要地为较高Ca∶Si比率,例如1∶1和更高,尤其2∶1和更高。
所用磷酸根离子源可以为任何能够将磷酸根离子输送到牙齿的源。优选磷酸根离子源为水溶性盐(参见下文)。适合的水溶性盐包括磷酸三钠、磷酸氢二钠和磷酸二氢钠。
为避免疑虑,磷酸根离子源连同钙离子源加到口腔。虽然在口腔中自然存在的唾液提供磷酸根离子源,但不应将此唾液认为是本发明的磷酸根离子源。
磷酸根离子源优选以1mM至100mM,更优选5mM至50mM,最优选10mM至40mM的浓度存在于组合物中。
优选磷酸根离子源存在于基本不含钙离子的组合物中。词语“基本不含”是指钙离子的量相对于磷酸根离子重量小于2.5%重量,特别小于1%重量,更特别小于0.1%重量,尤其小于0.01%重量。
磷酸根离子源优选存在于含氟离子源的组合物中。这种源可以为例如氟化钠或单氟磷酸钠。存在的氟离子含量可以为200ppm至10,000ppm,优选1000ppm至4000ppm,更优选2000ppm至3000ppm。氟离子,特别是优选浓度的氟离子,可有助于不溶性钙盐和从第二组合物加入及存在于唾液中的磷酸根离子之间的反应。
钙离子源和磷酸根离子源一般通过使它们处于独立的组合物相互保持物理分离。将这些独立组合物输送到牙齿可以依次或同时。在某些实施方案中,例如双相牙膏,组合物优选同时输送。
输送装置可包括具有第一隔室和第二独立隔室的双管,第一隔室用于含钙离子源的第一组合物,第二独立隔室用于含磷酸根离子源的第二组合物。此双管一般有一个隔室围绕另一个隔室。此双管一般允许两种组合物共同挤出。
输送装置可包括具有如上所述在相同管内作为独立组合物存在的第一组合物和第二组合物的单管。在此实施方案中,组合物或相从管作为一体挤出,此挤出被称为“接触挤出”。在此实施方案中,一种组合物可作为另一组合物内的条存在。在优选的实施方案中,组合物之一作为围绕芯中另一种组合物的套存在。在特别优选的实施方案中,芯组合物包含钙离子源,而套组合物包含磷酸根离子源。
当两种组合物在相同管内作为独立的组合物存在时,各组合物内水的量优选小于35%重量,更优选小于30%重量,最优选小于25%重量。在此类型的一个尤其优选的实施方案中,第一组合物具有小于20%重量水,第二组合物具有小于25%重量水。已发现,使水的量减至最小可降低钙盐与磷酸根离子源的过早相互作用。
在一个优选的实施方案中,本发明的产物包含凝胶组合物。凝胶组合物优选包含钙离子源,或者可包含钙离子源。在某些实施方案中,有两种独立的凝胶组合物,第一种包含钙离子源,而第二种包含磷酸根离子源。用独立的凝胶组合物处理一般包括在施加时将组合物混合,并使混合的组合物与牙齿接触。在此施加后,一般使混合的组合物保留在牙齿上10分钟至10小时,更一般30分钟至8小时。施加可每日进行。组合物可从双隔室管的独立隔室施加,或者从单一容器(一般为管)内所含产物的独立相施加。
在某些实施方案中,特别是包含凝胶组合物的那些实施方案,输送装置可包括带,特别是粘合带,在带与牙齿接触前在上面施加钙离子源和磷酸根离子源。利用此输送装置,组合物可与牙齿表面保持紧密接触,这有利于高浓度钙盐和/或磷酸根离子源接近牙齿表面。利用此输送装置,可使非常少的组合物损失进入唾液中。
凝胶组合物包括使用凝胶。凝胶一般包含聚合物基质,更一般为水凝胶(参见下文)。不包括任何存在的水,聚合物基质一般以它所属的组合物的1至25%重量存在。
在本发明环境下,“凝胶”为其中互连纳米颗粒的多孔网络跨越液体介质体积的胶体系统。通常,凝胶表面上为固态、胶状物质。从重量和体积两个方面,凝胶在组成上主要为液体,因此显示类似于液体的密度,然而,它们具有固体的结构凝聚性。
聚合物基质物质可以为水凝胶,在本发明环境下,水凝胶为含吸收的含水相的不溶性聚合物网络。聚合物网络一般交联。在含水凝胶的组合物中,其他液体组分的含量一般不大于10%重量。
含水凝胶的组合物中水的含量一般为80至99%。
用于制备水凝胶的单体可选自乙烯醇和丙烯酸盐,具体为丙烯酸钠。也可使用包含许多亲水基团的其他单体。
优选的水凝胶包括多糖、聚丙烯酰胺或聚丙烯酸。
适合的多糖可以为贮存多糖(如淀粉或糖原)或结构多糖(如纤维素或甲壳质)。
适合的多糖可包括选自以下一种或多种的糖单元:异麦芽糖、葡萄糖、果糖、半乳糖、木糖、甘露糖、山梨糖、阿拉伯糖、鼠李糖、岩藻糖、麦芽糖、蔗糖、乳糖、麦芽酮糖(maltulose)、核糖、来苏糖、阿洛糖、阿卓糖、古洛糖、艾杜糖、塔罗糖、海藻糖、黑霉糖、曲二糖和乳果糖。
优选的水凝胶包括一种或多种选自罗望子胶、瓜耳胶、刺槐豆胶、他拉(tara)、葫芦巴、芦荟、芡欧鼠尾草、亚麻子、车前子、榅桲子、黄原胶、结冷胶(gellan)、文莱胶(welan)、鼠李糖胶(rhamsan)、葡聚糖、凝胶多糖(curdlan)、普鲁兰多糖(pullulan)、硬葡聚糖、裂裥多糖、甲壳质、羟基烷基纤维素、阿拉伯聚糖、脱支阿拉伯聚糖、阿拉伯糖基木聚糖、半乳聚糖、果胶半乳聚糖、半乳甘露聚糖、葡甘露聚糖、地衣多糖、甘露聚糖、茯苓聚糖、鼠李半乳糖醛酸聚糖、阿拉伯胶、琼脂、藻酸盐、角叉菜胶、脱乙酰壳多糖、clavan、透明质酸、肝素、菊糖、纤维糊精、纤维素和纤维素衍生物的多糖。
特别优选的水凝胶包括选自藻酸钠、藻酸羟基丙酯、角叉菜胶、gum grabic、瓜耳胶、剌梧桐树胶、脱乙酰壳多糖、果胶和淀粉的多糖。
形成水凝胶的其他优选组分为购自Noveon的Carbopol聚合物。
本发明使用的组合物也可包含本领域常见的其他成分,如:
·抗微生物剂,例如三氯生、氯己定、铜、锌和亚锡盐(如柠檬酸锌、硫酸锌、甘氨酸锌、柠檬酸锌钠和焦磷酸亚锡)、血根碱提取物、甲硝唑、季铵化合物(如氯化鲸蜡基吡啶鎓)、双胍(bis-guanides)(如二葡糖酸氯己定、海克替啶、奥替尼啶、阿来西定和卤化的双酚化合物(如2,2′亚甲基双(4-氯-6-溴苯酚));
·抗炎剂,如布洛芬、氟比洛芬、阿司匹林、吲哚美辛等;
·抗龋剂,如三偏磷酸钠和酪蛋白
·牙斑缓冲剂,如尿素、乳酸钙、甘油磷酸钙和聚丙烯酸锶;
·维生素,如维生素A、C和E;
·植物提取物;
·脱敏剂,例如柠檬酸钾、氯化钾、酒石酸钾、碳酸氢钾、草酸钾和硝酸钾;
·抗牙垢剂,例如碱金属焦磷酸盐、含次磷酸盐的聚合物、有机膦酸盐和磷柠檬酸盐(phosphocitrate)等;
·生物分子,例如细菌素、抗体、酶等;
·香料,例如薄荷油和留兰香油;
·蛋白质物质,如胶原蛋白;
·防腐剂;
·不透明剂;
·着色剂;
·pH调节剂;
·甜味剂;
·药学上可接受的载体,例如淀粉、蔗糖、水或水/醇系统等;
·表面活性剂,如阴离子、非离子、阳离子和两性离子或两性表面活性剂;
·粒状磨料,如二氧化硅、氧化铝、碳酸钙、磷酸二钙、焦磷酸钙、羟基磷灰石、三偏磷酸盐、不溶性六偏磷酸盐等,包括附聚的粒状磨料,通常为口腔护理组合物3至60%重量的量;
·湿润剂,如甘油、山梨糖醇、丙二醇、木糖醇、乳糖醇等;
·粘合剂和增稠剂,如羧甲基纤维素钠、黄原胶、阿拉伯树胶等以及合成聚合物,如聚丙烯酸酯和羧基乙烯基聚合物,如
·也可包含能够增强活性成分输送的聚合化合物,例如,抗微生物剂。此类聚合物的实例为聚乙烯基·甲基醚与马来酸酐的共聚物及其他类似的输送增强聚合物,如DE-A-3,942,643(Colgate)所述的那些聚合物;
·缓冲剂和盐,用于缓冲口腔护理组合物的pH和离子强度;和
·可包含的其他任选成分,例如漂白剂(如过氧化合物,例如过氧二磷酸钾)、泡腾系统(如碳酸氢钠/柠檬酸系统)、变色系统等。
附图说明
图1为用含磷酸盐唾液中的MCS-凝胶以8小时/天循环处理两星期之前(a)和之后(b)人牙釉质表面形态学的扫描电子显微镜法(SEM)图像。
图2为经处理牙齿的横截面SEM图像。在原牙釉质(左区域)上已形成5微米厚薄层(右明亮区域)。
图3为跨越图2的SEM横截面图像上所示暗线扫描的(左至右)Ca和P的能量色散X射线(EDX)元素分析。所示“距离”为微米距离。
图4为含磷酸盐组合物存在下MCS-凝胶处理之前和之后牙齿表面的拉曼光谱。
图5a为用磷酸“浸蚀”之前牙齿表面的SEM图像。
图5b为用磷酸“浸蚀”之后牙齿表面的SEM图像。
图6a为磷酸浸蚀牙齿表面的拉曼光谱。
图6b为用MCS-凝胶组合物和含磷酸盐组合物处理一星期后磷酸浸蚀牙齿表面的拉曼光谱。
图7为实施例14和15中所用二氧化钛原料的SEM图像。
图8为用实施例14处理的HAP盘的SEM图像。
图9为用实施例14处理的HAP盘的能量色散谱(EDS)。
以下实施例用于说明本发明,而本发明不限于这些实施例。除非另外说明,百分比和份数均以重量计。
实施例
步骤I-制备包含MCS的凝胶组合物
利用超声作用,以表1所示约0.5%至5%范围浓度,形成蒸馏水中细粉MCS(Ca∶Si=1∶2)的均匀悬浮体。然后在剧烈搅拌下加入藻酸钠凝胶颗粒。约5至15分钟后,得到均匀的白色凝胶悬浮体。测定凝胶悬浮体的pH,pH也显示于表1中。
表1:MCS组合物
1 | 2 | 3 | 4 | |
MSC粉末(g) | 0.5 | 1.5 | 3 | 5 |
水(g) | 100 | 100 | 100 | 100 |
藻酸钠(g) | 5 | 5 | 5 | 5 |
pH | 9.32 | 9.72 | 9.76 | 10.03 |
如上所述用以1g、1.5g和3g存在的藻酸钠制备另外的组合物。发现所得组合物的粘度为藻酸盐含量的函数,藻酸盐含量越高,粘度越高。
步骤II-施加包含MCS的凝胶组合物
用75%醇清洗已拔出的人类牙齿,并用牙膏刷洗,以除去表面细菌和碎屑。将表1中标为4的组合物以每六颗牙齿1.0g的量均匀涂到牙齿上。然后将牙齿浸入37℃人的唾液中。8小时后,用自来水洗掉凝胶,将牙齿再次浸入37℃唾液经历当日剩余的时间。此处理继续两个星期。
使用的人的唾液从很多受试者收集。其钙浓度为23至60ppm,磷浓度(作为磷酸根离子存在)为124至154ppm。
牙齿的表面形态学用处理之前和之后的SEM研究。图1(a)代表处理之前的外观,图1(b)代表处理之后的外观。可以看到,在处理之前表面是光滑的,在处理之后从原来的光滑表面生长出某些新的晶体结构。在10,000放大倍数,可清楚地看到微小的晶体结构,测量为约100nm。
为了对新生成的羟基磷灰石的量定量,在处理之前和处理之后将牙齿样品切开,并在SEM检查之前抛光。结果显示于图2中。可清楚地看到,在原来的牙釉质顶上形成薄的涂层。层的厚度为2至10微米,但显得与牙齿表面粗糙度具有正关系。因此,显示出该处理针对最需要修复的那些牙齿。
由处理产生的新结晶物质的化学性质由EDX元素分析(见图3)和拉曼光谱(见图4)研究。图3显示新生成羟基磷灰石中钙和磷的含量非常类似于下面原来的牙釉质。图4显示,新生成羟基磷灰石中存在的磷酸根的化学性质基本上与未处理的牙齿相同,因此强烈暗示,只有“自然”的羟基磷灰石加到牙齿上。
利用纳米压痕进行硬度试验
在此试验中研究再生牙釉质层的机械性质。机械坚固性对牙釉质的长期稳定性至关重要,并且对咬食食物期间牙齿的维护很重要。因此需要牙釉质具有高水平的机械硬度。
使用与“步骤II”所述相同的方法(参见上文),首先清洗人的牙齿样品,然后经两个星期每日用组合物5和含磷酸盐的唾液处理。然而在此时引入另外的步骤:在唾液中浸入涂过的牙齿8小时后,用含白垩的牙膏刷牙1分钟。然后如以上所述的“步骤II”方法重新浸入唾液中。
用现代纳米压痕仪器检测牙齿表面上羟基磷灰石的新沉积薄膜的薄膜硬度。检测三个经处理的牙齿样品,在每个样品上产生九个压痕。如表3中所示,重新矿化层的硬度为5.4至5.7GPa。这非常接近原来牙釉质表面的硬度,硬度也显示于表3中。另一个重要的机械参数为杨氏模量,材料弹性的基础值。此值越高,材料越硬。合乎需要的是重新矿化层类似于自然的牙釉质。从表2所示结果清楚地看出,重新矿化的薄膜具有类似于原来牙釉质的机械性质。
表2:处理前后牙齿的机械性质
硬度(GPa) | 杨氏模量(GPa) | |
处理前(文献值) | 5.0-6.0 | 95-120 |
形成新牙釉质层后 | 5.4-5.7 | 111-121 |
受损牙齿的再生
为了模拟很多类型酸性果汁对牙齿的去矿化作用,用37%重量磷酸浸蚀人的牙齿1分钟。由SEM拍摄原牙齿和磷酸浸蚀牙齿的图像。图5a代表浸蚀前的牙齿表面,图5b代表浸蚀后的牙齿表面。通过以上述方式用组合物5(下述)和含磷酸盐的唾液处理,发现可在一星期内治愈磷酸产生的浸蚀。
组合物5:将MCS粉末(0.5g)加到水(10g)中,如上所述分散,然后在剧烈搅拌下加入藻酸钠(0.3g)。在搅拌约10分钟后形成均匀凝胶。
发现经处理的样品生长出显著厚度的新层。新形成的层用拉曼光谱法表征。图6a为处理前牙齿表面的拉曼光谱,图6b为处理后牙齿表面的拉曼光谱。表3指示处理前后主峰的位置。在961.42cm-1有相应于主磷酸根带的峰。处理后的样品得到与样品处理前基本相同的拉曼光谱,包括在961.42cm-1磷酸根带的位置。这意味着增加的物质与原来存在的相同,这一结果有些使人意外。
表3:处理前后人牙釉质的拉曼峰位置
带 | 处理前位置 | 处理后位置 |
V1PO4 3- | 961 | 961 |
V2PO4 3- | 445 | 444 |
V3PO4 3- | 1072 | 1069 |
V4PO4 3- | 579 | 579 |
拉曼带V1、V2、V3和V4为磷灰石晶格的结晶性/完整性的特征。
实施例6:双相凝胶产物
制备一种产物,所述产物包含两种凝胶组合物:凝胶I和凝胶II。明细在表4中给出。将如以上“步骤I”下所述的MSC粉末通过“步骤I”下所述的方法加入凝胶I。通过加藻酸钠到磷酸盐缓冲剂和氟化钠的溶液制备凝胶II。
表4:双相凝胶产物
MCS粉末(%重量) | 藻酸盐粉末(%重量) | 磷酸盐(mM) | 氟化物(mM) | |
凝胶I | 5 | 3 | 0 | 0 |
凝胶II | 0 | 3 | 25 | 25 |
通过混合等重量凝胶I和凝胶II,并用棉签将混合物(总重量2g)涂在六颗牙齿上施加产物。在轻搅下,将经处理的牙齿浸入37℃人唾液(15ml)中1小时。在此时间后,冲洗牙齿,并用棉签弄干净,以除去任何剩余的凝胶。然后将它们放入新鲜的唾液另外两小时。一天两次进行此过程两个星期,总共进行28次处理。
在另一个试验中,将如上所述的实施例6(即1∶1重量凝胶I和凝胶II的混合物)施加到塑料粘合带。然后将带包裹在各牙齿周围,并将包裹的牙齿浸入唾液8小时。施加剂量为每6颗牙齿2g凝胶I和凝胶II的混合物。在此时间后,用水冲洗牙齿,然后放入新鲜的唾液中。重复此过程两个星期,包括每天刷牙一次模拟真实生活使用。
将以上用实施例6处理与“对照”处理的牙齿增白效果一起研究,“对照”处理包括刷牙(一天一次)和只用唾液处理。
用Minolta Chromameter CR-321(3mm孔,45/0)定量检测处理之前和处理之后各牙齿的L*和b*值,量度增白效果。L*表示从试验表面反射的总光强度,b*表示来自黄-蓝的光作用(light contribution)。牙齿增白由反射光强度(L*)增加和“黄度”(b*)减小指示。结果显示于表5中。将处理两星期后的平均颜色变化表示为ΔL*和Δb*。对本发明的两个处理都观察到优良增白效果。
表5:用实施例6处理后的增白效果
实施例7-9:双相牙膏产物
表6:组合物明细
1.精细研磨的天然白垩。
2.羧甲基纤维素钠。
3.月桂基硫酸钠。
4.在各“第一组合物”中,0.25%硝酸钾、0.05%甲醛和0.15%三氯生。
参照表6:
实施例7:1∶1重量第一组合物7和第二组合物的混合物;
实施例8:1∶1重量第一组合物8和第二组合物的混合物;
实施例9:1∶1重量第一组合物9和第二组合物的混合物;
实施例A:1∶1重量第一组合物A和第二组合物的混合物。
用这些实施例处理经抛光的牙釉质块。处理包括用水中双相牙膏的浆料(1份牙膏与2份水)刷牙3分钟,随后在37℃唾液中将块培育2小时。一天两次经四星期进行此过程。用常规的“增白”牙膏和水作为对照。
如上所述用Chromameter监测牙釉质块的颜色。最终结果显示于表7中,ΔL*和ΔW*表示处理前后之间的“亮度”和“白度”变化。“W”为“白度量度”,计算为:
W=100-√{(100-L*)2+a*2+b*2)
表7:使用双相牙膏产物后的增白效果
所用实施例 | ΔL* | ΔW* |
7 | 2.32 | 1.91 |
A | 1.21 | 1.09 |
牙膏对照 | 0.73 | 0.36 |
水对照 | 0.56 | 0.21 |
这些结果表明,实施例7得到与对照相比优良的“增亮”和“增白”。
经发现,使用实施例7的L*值随时间增加。此结果由表8中的数字说明。
表8:处理时间的影响
处理(星期) | 0 | 1 | 2 | 3 | 4 |
L* | 63.52 | 64.82 | 65.37 | 65.85 | 65.84 |
同样研究处理对经抛光牙釉质块硬度的影响。这使用HM-122硬度试验机(购自Mitutoyo,Japan)通过测量努普硬度来进行。每个处理测量10个样品,对每个样品产生5个压痕。表9中所示的结果说明,实施例8和9使牙釉质硬度显著增加(p<0.05)。
表9:使用双相牙膏产物后的硬度效果
同样研究处理对经抛光牙釉质块粗糙度的影响。这用表面轮廓仪(SV2000,购自Mitutoyo,Japan)进行。每个处理检测10个样品。表10中所示的结果说明,实施例8和9使牙釉质粗糙度显著减小,即,平滑度和光亮显著增加。
表10:处理对牙釉质粗糙度的影响
所用实施例 | 粗糙度变化(%) |
8 | -10.9 |
9 | -10.2 |
A | +5.2 |
牙膏对照 | +20 |
水对照 | -2.2 |
在一个独立的研究中,检验处理对全部牙齿(whole teeth)白度的影响。试验方法基本与关于抛光牙釉质块所述(如上所述)相同,唯一区别是使用全部牙齿。表11所示结果例证与常规增白牙膏比较实施例7的优良效力。
表11:对全部牙齿的增白效果
所用实施例 | ΔL* | Δb* | ΔW* |
7 | 1.76 | -0.77 | 1.88 |
牙膏对照 | 0.20 | -0.28 | 0.26 |
实施例10:双相牙膏产物
表12中细列的两种组合物旨在以1∶1重量比使用。这些组合物适合从相同管的相同隔室内作为独立的组合物/相挤出,例如,第一组合物形成芯,第二组合物形成周围的套。此实施例的组合物中水的量特别低。
表12:用于接触挤出的双相牙膏
组成 | 第一组合物 | 第二组合物 |
硅酸钙 | 20 | - |
Na2HPO4 | - | 10 |
山梨糖醇,70%(水) | 48 | 61 |
PEG 1500 | 2 | 2 |
研磨二氧化硅 | 9 | 9 |
增稠二氧化硅 | 8.5 | 7.5 |
SLS | 6.6 | 6.6 |
SCMC | 0.6 | 0.6 |
香料 | 1.3 | 1.3 |
糖精 | 0.2 | 0.2 |
水和少量物质* | 3.8 | 1.8 |
*在“第一组合物”中为2ppm蓝色颜料。
实施例11-13:双相凝胶产物
以下实施例为50∶50重量表13中所示“第一”组合物和表13中细列各“第二”组合物的混合物。因此:
实施例11:第一组合物+第二组合物B;
实施例12:第一组合物+第二组合物C;
实施例13:第一组合物+第二组合物D。
表13
用实施例11、12和13经4星期时间每天处理羟基磷灰石盘(disc)(n=6-8)30分钟。在每天处理30分钟后将盘浸入模拟口腔流体。如上所述,用Chromameter监测羟基磷灰石盘的颜色。最终结果显示于表14的底部。
表14
这些结果说明可用本发明得到的极佳的增白益处。
实施例14-15和比较性实施例H
这些实施例为50∶50重量来自表15的“第一”组合物和“第二”组合物的混合物。因此:
实施例14:第一组合物E+第二组合物14;
实施例15:第一组合物F+第二组合物15;
实施例G:第一组合物E+第二组合物G。
表15
用实施例14、15和比较性实施例G处理已在37℃用红茶和咖啡经2-4星期着色,然后用水刷洗的抛光羟基磷灰石盘。处理包括将组合物混合,然后涂到着色盘的表面上(n=5)。经两星期每天将所述处理保留30分钟。在每天30分钟处理后,将盘用水清洗,然后浸入模拟口腔流体。每天还刷洗盘,以模拟真实生活使用。
所用二氧化钛具有约255nm平均粒径,材料的SEM图像显示于图7中。用实施例14处理的羟基磷灰石盘表面的SEM图像如图8所示。可以看到,二氧化钛已包埋到新形成的羟基磷灰石层中,并且保持其形态学特征。图9为经处理盘的表面的EDS谱,并且显示特有的钛峰(由向下箭头指示),这进一步证明增白剂加入到羟基磷灰石表面。
如前所述,用Chromameter监测羟基磷灰石盘的颜色。最终结果显示于表16的底部。
表16
这些结果进一步说明可用本发明得到的极佳的增白益处。
Claims (17)
1.一种口腔护理产物,所述口腔护理产物包含钙离子源、磷酸根离子源和用于沉积于牙齿上的不溶性增白剂,其特征在于所述钙离子源和磷酸根离子源在产物使用前物理分离。
2.权利要求1的口腔护理产物,所述口腔护理产物包含硅酸钙。
3.权利要求2的口腔护理产物,其中所述硅酸钙具有1∶3至3∶1的Ca∶Si比。
4.权利要求3的口腔护理产物,其中所述硅酸钙为中孔性。
5.权利要求4的口腔护理产物,其中所述中孔硅酸钙具有0.4至4nm的平均孔径(直径)。
6.权利要求2至5中任一项的口腔护理产物,其中所述不溶性钙盐以所施加产物的0.5至15%重量存在。
7.前述权利要求中任一项的口腔护理产物,所述口腔护理产物包括具有8.5至10的pH的组合物。
8.前述权利要求中任一项的口腔护理产物,其中所述磷酸根离子源为水溶性盐。
9.前述权利要求中任一项的口腔护理产物,所述口腔护理产物包含凝胶组合物。
10.前述权利要求中任一项的口腔护理产物,所述口腔护理产物包括输送装置,所述输送装置包括具有第一隔室和第二独立隔室的双管,第一隔室用于含钙离子源的组合物,第二独立隔室用于含磷酸根离子源的组合物。
11.前述权利要求中任一项的口腔护理产物,所述口腔护理产物包括输送装置,所述输送装置包括带,特别为粘合带,在带与牙齿接触前在上面施加钙离子源和磷酸根离子源。
12.权利要求1至9中任一项的口腔护理产物,所述口腔护理产物包括输送装置,所述输送装置包括单管,单管具有含钙离子源的第一组合物和含磷酸根离子源的第二独立组合物,两种组合物均存在于相同的管内。
13.权利要求12的口腔护理产物,其中各组合物内水的量小于30%重量。
14.权利要求13的口腔护理产物,其中第一组合物具有小于20%重量的水,第二组合物具有小于25%重量的水。
15.一种将不溶性增白剂输送到牙齿的方法,所述方法包括施加不溶性增白剂以及钙离子源和磷酸根离子源,其特征在于所述钙离子源和磷酸根离子源从物理分离的组合物施加。
16.权利要求1的产物,所述产物用作药物。
17.1.钙离子源;
2.物理独立的磷酸根离子源;和
3.用于沉积于牙齿上的不溶性增白剂,
用于制备改善牙齿白度和/或减少龋齿和/或降低敏感性的口腔护理产物的用途。
Priority Applications (1)
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CN200780050884.XA CN101600442B (zh) | 2006-12-05 | 2007-12-04 | 口腔护理产物 |
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CN2006003278 | 2006-12-05 | ||
CNPCT/CN2006/003278 | 2006-12-05 | ||
CN200780050884.XA CN101600442B (zh) | 2006-12-05 | 2007-12-04 | 口腔护理产物 |
PCT/EP2007/063252 WO2008068248A1 (en) | 2006-12-05 | 2007-12-04 | Oral care product |
Publications (2)
Publication Number | Publication Date |
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CN101600442A true CN101600442A (zh) | 2009-12-09 |
CN101600442B CN101600442B (zh) | 2015-01-14 |
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CN200780050962.6A Active CN101600443B (zh) | 2006-12-05 | 2007-11-23 | 口腔护理产品 |
CN200780050963.0A Expired - Fee Related CN101600444B (zh) | 2006-12-05 | 2007-12-04 | 口腔护理产品 |
CN200780050884.XA Expired - Fee Related CN101600442B (zh) | 2006-12-05 | 2007-12-04 | 口腔护理产物 |
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CN200780050963.0A Expired - Fee Related CN101600444B (zh) | 2006-12-05 | 2007-12-04 | 口腔护理产品 |
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US (3) | US20100143423A1 (zh) |
EP (3) | EP2089040B1 (zh) |
CN (3) | CN101600443B (zh) |
AT (2) | ATE539759T1 (zh) |
BR (3) | BRPI0720183B1 (zh) |
CL (1) | CL2007003497A1 (zh) |
DE (1) | DE602007012463D1 (zh) |
ES (2) | ES2378282T3 (zh) |
MX (1) | MX2009006027A (zh) |
PL (3) | PL2089040T3 (zh) |
WO (3) | WO2008068149A1 (zh) |
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- 2007-12-04 CN CN200780050884.XA patent/CN101600442B/zh not_active Expired - Fee Related
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Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2011109919A1 (en) * | 2010-03-09 | 2011-09-15 | Unilever Plc | Stable oral care compositions |
US9180318B2 (en) | 2010-03-09 | 2015-11-10 | Conopco, Inc. | Stable oral care compositions |
CN103079526A (zh) * | 2010-09-10 | 2013-05-01 | 荷兰联合利华有限公司 | 有益于牙齿的口腔护理组合物 |
CN104602756A (zh) * | 2012-07-10 | 2015-05-06 | 伦敦国王学院 | 用于矿化生物材料的改进装置以及方法 |
US10076392B2 (en) | 2012-07-10 | 2018-09-18 | Reminova Ltd | Apparatus and method for mineralising biological material |
CN104602756B (zh) * | 2012-07-10 | 2018-10-19 | 黎明诺瓦有限公司 | 用于矿化生物材料的改进装置以及方法 |
CN104703575A (zh) * | 2012-10-12 | 2015-06-10 | 荷兰联合利华有限公司 | 口腔护理组合物 |
CN104703575B (zh) * | 2012-10-12 | 2017-12-12 | 荷兰联合利华有限公司 | 口腔护理组合物 |
CN107624064A (zh) * | 2015-05-13 | 2018-01-23 | 荷兰联合利华有限公司 | 口腔护理组合物 |
CN107624064B (zh) * | 2015-05-13 | 2021-06-15 | 荷兰联合利华有限公司 | 口腔护理组合物 |
CN107743386A (zh) * | 2015-06-05 | 2018-02-27 | 荷兰联合利华有限公司 | 口腔护理装置 |
US10595976B2 (en) | 2015-06-05 | 2020-03-24 | Conopco Inc. | Oral care device |
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