CN107308010A - 复合颗粒活性物及其制造方法 - Google Patents
复合颗粒活性物及其制造方法 Download PDFInfo
- Publication number
- CN107308010A CN107308010A CN201710421176.8A CN201710421176A CN107308010A CN 107308010 A CN107308010 A CN 107308010A CN 201710421176 A CN201710421176 A CN 201710421176A CN 107308010 A CN107308010 A CN 107308010A
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- Prior art keywords
- calcium
- composite particles
- active matter
- particles active
- core
- Prior art date
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- 239000011246 composite particle Substances 0.000 title claims abstract description 91
- 238000004519 manufacturing process Methods 0.000 title claims description 19
- 238000000034 method Methods 0.000 title claims description 17
- 239000000203 mixture Substances 0.000 claims abstract description 110
- 239000011248 coating agent Substances 0.000 claims abstract description 57
- 238000000576 coating method Methods 0.000 claims abstract description 57
- 239000011575 calcium Substances 0.000 claims abstract description 43
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052791 calcium 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 30
- 210000003298 dental enamel Anatomy 0.000 claims abstract description 20
- 210000004268 dentin Anatomy 0.000 claims abstract description 16
- 229940085991 phosphate ion Drugs 0.000 claims abstract description 8
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 5
- 239000011162 core material Substances 0.000 claims description 45
- 229960005069 calcium Drugs 0.000 claims description 39
- 239000002002 slurry Substances 0.000 claims description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 27
- 239000000047 product Substances 0.000 claims description 27
- -1 and optionally Chemical compound 0.000 claims description 18
- 235000012241 calcium silicate Nutrition 0.000 claims description 18
- 239000000377 silicon dioxide Substances 0.000 claims description 15
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 13
- 239000004408 titanium dioxide Substances 0.000 claims description 13
- 239000000606 toothpaste Substances 0.000 claims description 11
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 10
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 10
- 238000011065 in-situ storage Methods 0.000 claims description 10
- 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 claims description 10
- 229940034610 toothpaste Drugs 0.000 claims description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims description 8
- 239000007937 lozenge Substances 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 7
- 229960003563 calcium carbonate Drugs 0.000 claims description 7
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 7
- 230000003993 interaction Effects 0.000 claims description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 6
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 6
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 6
- 239000010445 mica Substances 0.000 claims description 6
- 229910052618 mica group Inorganic materials 0.000 claims description 6
- 239000001506 calcium phosphate Substances 0.000 claims description 5
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 5
- 235000011010 calcium phosphates Nutrition 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 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 5
- 239000011787 zinc oxide Substances 0.000 claims description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- 239000004115 Sodium Silicate Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 4
- 239000000920 calcium hydroxide Substances 0.000 claims description 4
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 4
- MKJXYGKVIBWPFZ-UHFFFAOYSA-L calcium lactate Chemical compound [Ca+2].CC(O)C([O-])=O.CC(O)C([O-])=O MKJXYGKVIBWPFZ-UHFFFAOYSA-L 0.000 claims description 4
- 239000001527 calcium lactate Substances 0.000 claims description 4
- 235000011086 calcium lactate Nutrition 0.000 claims description 4
- 229960002401 calcium lactate Drugs 0.000 claims description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000292 calcium oxide Substances 0.000 claims description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 235000010410 calcium alginate Nutrition 0.000 claims description 3
- 239000000648 calcium alginate Substances 0.000 claims description 3
- 229960002681 calcium alginate Drugs 0.000 claims description 3
- OKHHGHGGPDJQHR-YMOPUZKJSA-L calcium;(2s,3s,4s,5s,6r)-6-[(2r,3s,4r,5s,6r)-2-carboxy-6-[(2r,3s,4r,5s,6r)-2-carboxylato-4,5,6-trihydroxyoxan-3-yl]oxy-4,5-dihydroxyoxan-3-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylate Chemical compound [Ca+2].O[C@@H]1[C@H](O)[C@H](O)O[C@@H](C([O-])=O)[C@H]1O[C@H]1[C@@H](O)[C@@H](O)[C@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@H](O2)C([O-])=O)O)[C@H](C(O)=O)O1 OKHHGHGGPDJQHR-YMOPUZKJSA-L 0.000 claims description 3
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 3
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 3
- 229940112822 chewing gum Drugs 0.000 claims description 3
- 235000015218 chewing gum Nutrition 0.000 claims description 3
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 229910002974 CaO–SiO2 Inorganic materials 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 239000004111 Potassium silicate Substances 0.000 claims description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 2
- JHXCINJSAAFBDH-UHFFFAOYSA-N [Ca].O[Si](O)(O)O Chemical compound [Ca].O[Si](O)(O)O JHXCINJSAAFBDH-UHFFFAOYSA-N 0.000 claims description 2
- 235000013361 beverage Nutrition 0.000 claims description 2
- 239000004227 calcium gluconate Substances 0.000 claims description 2
- 235000013927 calcium gluconate Nutrition 0.000 claims description 2
- 229960004494 calcium gluconate Drugs 0.000 claims description 2
- 239000011635 calcium salts of citric acid Substances 0.000 claims description 2
- 235000019842 calcium salts of citric acid Nutrition 0.000 claims description 2
- 229940095672 calcium sulfate Drugs 0.000 claims description 2
- NEEHYRZPVYRGPP-UHFFFAOYSA-L calcium;2,3,4,5,6-pentahydroxyhexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(O)C([O-])=O.OCC(O)C(O)C(O)C(O)C([O-])=O NEEHYRZPVYRGPP-UHFFFAOYSA-L 0.000 claims description 2
- 239000006071 cream Substances 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 229960002816 potassium chloride Drugs 0.000 claims description 2
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 2
- 239000003826 tablet Substances 0.000 claims description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims 1
- 229940003214 aluminium chloride Drugs 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- NEEHYRZPVYRGPP-IYEMJOQQSA-L calcium gluconate Chemical compound [Ca+2].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O NEEHYRZPVYRGPP-IYEMJOQQSA-L 0.000 claims 1
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- 238000005660 chlorination reaction Methods 0.000 claims 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical class OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims 1
- 239000000470 constituent Substances 0.000 claims 1
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- 239000001301 oxygen Substances 0.000 claims 1
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- 239000011574 phosphorus Substances 0.000 claims 1
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- 229910052882 wollastonite Inorganic materials 0.000 claims 1
- 239000011701 zinc Substances 0.000 claims 1
- 229910052725 zinc Inorganic materials 0.000 claims 1
- 229910019142 PO4 Inorganic materials 0.000 abstract description 22
- 239000010452 phosphate Substances 0.000 abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 28
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Abstract
描述了适用于口腔护理组合物的复合颗粒活性物。该复合颗粒活性物具有核和涂层,借此该涂层与磷酸盐离子相互作用,产生钙和磷酸盐反应产物,其适于附着到牙釉质和/或牙本质上以改善牙齿的特性。
Description
本申请是2011年3月9日提交的名称为“复合颗粒活性物及其制造方法”的201180043399.6号申请的分案申请。
发明领域
本发明涉及复合颗粒活性物和制造该复合颗粒的方法。更具体地,本发明涉及这样的复合颗粒活性物,其适用于口腔以最起码通过与磷酸盐离子相互作用和将钙和磷酸盐源递送到消费者的牙齿而有助于牙齿的再矿化和增白。该颗粒因此适用于口腔中所用的组合物中。这样的颗粒可以例如用于牙膏或凝胶组合物、漱口液以及口香糖组合物中。此外,本发明的复合颗粒活性物包含第一组分芯(其适于即刻改善口腔护理特性)和第二组分涂层(其适于与磷酸盐离子相互作用产生钙和磷酸盐原位反应产物,该反应产物令人惊讶地非常好地附着到牙齿上来提供即刻的和长期的益处。
发明背景
我们消费的许多产品对于我们的牙齿和口腔具有不利的影响。酸性饮品和糖果例如会通过侵蚀包覆和保护牙齿的釉质而导致牙齿腐蚀。在牙釉质上这样的侵蚀往往和不期望地会导致牙齿的过敏症。此外,我们消耗的食物和饮料如番茄酱、浆果、甜菜、苏打水或汽水、咖啡和茶会玷污牙齿,并由此导致微笑不灿烂。番茄基产品和某些药物也会导致牙齿看起来发黄或甚至变成褐色。当然,不健康的牙齿会导致难闻的气味和有害细菌在口腔内的生长。
已经开发了解决牙齿变坏和/或增白的产品。这样的产品经常包含过氧化物、磨料或二者来清洁和增白牙齿。这些类型的产品经常是不期望的,因为它们不会产生牙齿的再矿化,并且过度使用时会导致损害牙齿和齿龈。已经开发了含钙源的产品来尝试增强牙齿的特性。但是这样的产品不会主动粘附到牙齿上,并由此在被用清洗水冲洗出口腔之前,仅仅与牙齿接触短暂的时间。
人们越来越感兴趣的是开发为牙齿提供了即刻和长期益处的产品。此外,越来越感兴趣的是开发复合颗粒活性物,当其从多种形式如牙膏或凝胶组合物、漱口液以及口香糖组合物提供时,能够有益于牙齿。本发明因此涉及复合颗粒活性物,其适于将钙和磷酸盐源递送到牙齿足够长的时间,来确保优异的增白结果。本发明还涉及制造其的方法。本发明的复合颗粒活性物包含第一组分芯(用于即刻改善口腔护理特性)和第二组分涂层(其适于与磷酸盐离子相互作用产生钙和磷酸盐原位反应产物,该反应产物令人惊讶地非常好地附着到牙齿上来同时提供即刻和长期的益处。
附加信息
已经公开了制造口腔护理产物的努力。在WO2008/068149A1和WO2008/068248A1中描述了具有钙和磷酸盐的口腔护理产物。
还公开了制造口腔护理产物的其他努力。在US专利4083955,5605675和6214321B1中,描述了用于再矿化牙釉质的方法和组合物。
还公开了制造口腔护理产物的其他努力。在US专利No.6365132B1和5735942中,描述了用于牙齿上的组合物。
在US专利申请2002/0064504A1和2009/0264291A1中,公开了制造口腔护理组合物另外的努力。前者描述了牙齿抗过敏症组合物,后者描述了用于使用具有生物活性玻璃的牙粉来防止或减少菌斑和/或齿龈炎的组合物和方法。
上述附加信息都没有描述本文所述的包含芯和涂层的复合颗粒活性物。此外,这些附加信息都没有描述本文所述的制造这样的颗粒的方法。
发明内容
在第一方面,本发明涉及一种复合颗粒活性物,其包含:
(a)用于改善口腔护理特性的第一组分芯;和
(b)第二组分涂层,其与磷酸盐离子相互作用产生磷酸钙原位反应产物,该反应产物附着到牙釉质、牙本质或二者上并且是形成羟磷灰石的前体。
在第二方面,本发明涉及制造本发明第一方面的复合颗粒活性物的方法。
本发明的所有其他方面将通过考虑下面的详细说明和实施例而更易于变得显而易见。
作为此处使用的,可溶和不溶指的是物质源(source)(例如钙)在水中的溶解度。可溶表示物质源在室温下溶解在水中来产生浓度至少0.1mol/L的溶液。不溶表示物质源在室温下溶解在水中来产生浓度小于0.001mol/L的溶液。因此微溶定义为表示物质源在室温下溶解在水中来产生浓度大于0.001mol/L和小于0.1mol/L的溶液。口腔护理组合物表示这样的组合物,其适用于口腔中和用于兽医和/或人应用,但是特别适用于人口腔使用。有益于牙齿表示最起码增白、再矿化或脱敏牙齿或减少口腔内的细菌,这里细菌的减少可以是使用抗菌剂的结果,牙齿的脱敏是复合颗粒活性物与口腔和/或口腔护理组合物中的磷酸盐离子相互作用的结果,并且附着到牙齿上来例如在牙本质小管上产生新的羟磷灰石形成。在该复合颗粒活性物不是理想的球形的情况下,直径表示可测量的最长距离。作为此处使用的,再矿化表示在牙齿上原位产生羟磷灰石来降低牙齿变坏的可能性和通过这样的新的羟磷灰石的产生来增白从而改善牙齿外观。这样的再矿化也导致了牙齿的增白,其全都可以是复合颗粒活性物附着到牙齿上和/或在牙齿上形成无定形磷酸钙的结果。单相组合物表示在分配或打开包装和使用之前,其中具有钙和磷酸盐源二者中的一个相的组合物。作为此处使用的,无水表示基本上没有水(例如没有水到小于5重量%的水、优选小于1重量%的水)。双相产物表示在分别的组合物中具有所需的和互补的钙和磷酸盐羟磷灰石前体,并且存储在分别的隔间中。作为此处使用的,组合物包括例如糊料、粉末、凝胶、液体(如漱口液)、喷剂、泡沫、香膏(balm)、负载在含片(mouthstrip)或口腔贴片上的组合物、咀嚼片(或药锭)、锭剂、乳霜、饮料或口香糖条。但是优选该组合物是糊料如牙膏或用于牙齿的凝胶。作为此处使用的,载体表示组合物中不同于复合颗粒活性物和磷酸盐源的组分,据此该载体适于递送其中存在的活性物和任何磷酸盐源。作为此处使用的,第一组分芯表示包括被涂覆的那部分复合颗粒活性物,据此该芯可以包含颗粒或颗粒聚集体如TiO2聚集体。芯还表示包括经由物理机理为牙齿提供即刻(例如在组合物的三(3)次使用内,但是优选在使用的1秒-5分钟内)增白益处的组分。长期益处表示包括将持续至少数周,但是优选至少四(4)个月的益处。通常,芯意味着能够改善牙齿特性的组分。作为此处使用的,第二组分涂层表示在至少一部分的第一组分芯上形成外涂层或包层的涂层。不受限于理论,作为此处使用的,粘附可以包括作为该复合颗粒活性物的涂层中的钙和磷酸盐离子相互作用的结果而产生的有效的沉积和/或结合或“粘贴”到牙齿。涂层还表示包括这样的组分,其通过生物或化学机理如形成羟磷灰石,而随着时间的过去为牙齿提供的益处。复合颗粒活性物因此表示在使用后能够为牙齿提供即刻的和长期的益处二者的颗粒。原位反应产物表示在口腔中产生的包含钙和磷酸盐的产物。
除非另有明确的指示,此处所定义的所有范围都表示包括了包含在其内的所有的范围。作为此处使用的,“包含”表示包括了“基本由…组成”和“由…组成”,并且应该理解为不排除还包括其他的组分。
附图说明
在申请文件的结尾部分具体指出和明确要求保护了被认为是本发明的主题。但是,本发明可以通过参考下面的说明和结合附图而最好地理解,在其中:
图1(A和B)显示了在一次处理之后复合颗粒活性物在牙釉质上的粘附。
图2(A和B)显示了在十四次处理之后复合颗粒活性物在牙釉质上的粘附。
图3显示了在一次处理之后复合颗粒活性物在牙本质上的粘附。
图4显示了在十四次处理之后复合颗粒活性物在牙本质上的粘附。
图(A和B)显示了沉积在牙齿表面上的常规二氧化硅与复合颗粒活性物;
图6(a-d)显示了未涂覆的和涂覆的二氧化钛颗粒的透射电子显微镜图象;和
图7显示了在2周和4周处理之后,与基线相比,消费者牙齿增白研究的结果。
具体实施方式
对于能够用于本发明的复合颗粒活性物的唯一限制是其适用于口腔中。典型地,该复合颗粒活性物的芯包含适于物理地即刻改善牙齿特性,特别是增白牙齿的材料。这样的材料典型地具有1.2-3,优选1.3-2.8,最优选1.5-2.8的折射率,包括其中包含的所有范围。适于物理改善牙齿的这样的芯材料的示例性,但是非限定性的例子包括二氧化硅、二氧化钛、氧化锌、云母(包括包覆的云母如市售的氧化铁包覆的云母)、碳酸钙、硫酸钡或其混合物。该复合颗粒活性物的芯通常构成该复合颗粒活性物的3-98重量%,优选6-65重量%,最优选10-55重量%,基于该复合颗粒活性物的总重量,并且包括其中所包含的所有范围。在一种特别优选的实施方案中,该芯是至少50重量%的二氧化钛或氧化锌,最优选60-100重量%的二氧化钛或氧化锌,基于该第一组分芯的总重量。
适于附着到牙釉质、牙本质或二者上的涂层通常包含金属元素例如钙,和任选地,其他金属,如钾、钠、铝、镁及其混合物。在一种优选的实施方案中,其适于为牙齿提供生物或化学改善,其是长期的和短期的二者(例如导致增白和羟磷灰石形成)。优选采用的涂层包含至少50重量%的元素钙,最优选至少65重量%的元素钙,基于涂层中金属的总重量。在一种特别优选的实施方案中,涂层中的金属元素是80-100重量%的元素钙,基于第二组分涂层中金属的总重量,并且包括其中所包含的所有范围。在另外一种特别优选的实施方案中,芯和涂层在水中是微溶的或不溶的,但是最优选在水中是不溶的。
通常,芯的至少5%的外表面涂覆有涂层,优选至少50%的芯涂覆有涂层。在一种最优选的实施方案中,该第一组分芯的70-100%的外表面积涂覆有该第二组分涂层。
该复合颗粒活性物的直径往往是10nm-小于50微米,优选75nm-小于10微米。在一种特别优选的实施方案中,该复合颗粒活性物的直径是500nm-5微米,包括其中所含的所有范围。在又一种特别优选的实施方案中,该复合颗粒活性物直径的至少40%、优选至少60%、最优选75-99.5%是由芯构成的,包括其中所含的所有范围。
适于负载本发明的复合颗粒活性物的口腔护理组合物通常包含0.25-40%、优选0.5-20%、最优选0.5-15%重量的复合颗粒活性物,基于口腔护理组合物的总重量,并且包括其中所含的所有范围。在一种特别优选的实施方案中,该组合物包含所有金属(例如钙离子)含量小于40%、优选小于30%、最优选1-25%重量的金属元素,基于组合物的总重量,并且包括其中所含的所有范围。
在又一种特别优选的实施方案中,复合颗粒活性物可以与另外的金属源(如钙源)一起加入到组合物中。这样的另外的金属源可以与用于涂覆该复合颗粒活性物的芯的那些相同(例如硅酸钙或氧化钙)。当加入时,该另外的金属源通常构成口腔护理组合物总重量的0.1-35%、优选1-25%、最优选10-20%重量,并且包括其中所含的所有范围。
在一种特别期望的实施方案中,该第二组分涂层可以包含例如磷酸钙,葡糖酸钙,氧化钙,乳酸钙,碳酸钙,氢氧化钙,硫酸钙,羧甲基纤维素钙,藻酸钙,柠檬酸的钙盐,硅酸钙,其混合物等。在另外一种期望的实施方案中,涂层中的钙源将包含硅酸钙。当制造本发明的复合颗粒活性物时,这些化合物还适于作为用于钙源的试剂而包括在内。代替钙的钠、镁、铝和钾的类似盐可以例如用作试剂来在颗粒制造过程中提供该第二组分涂层的阴离子部分。
在又一种优选的实施方案中,该涂层可以包含钙源,其是不溶性硅酸钙,作为复合材料氧化钙-二氧化硅(CaO-SiO2)而存在,如在共同拥有的申请,国际专利申请2008/015117和2008/068248中所述。
当硅酸钙复合材料被用作涂层时,钙与硅之比(Ca:Si)可以是1:10-3:1。该Ca:Si比优选是1:5-2:1、更优选1:3-2:1、最优选大约1:2-2:1。该硅酸钙可以包含硅酸单钙、硅酸二钙或硅三酸钙,由此钙与硅之比(Ca:Si)应当理解为是原子比。
本发明所用的、在复合颗粒活性物上产生第二组分涂层的优选的钙源可以处于结晶态或无定形态。在一种往往优选的实施方案中,用于涂层的钙源处于介孔态,即,该源是孔径为1nm-1微米的材料。介孔硅酸钙(MCS)往往是优选的。
能够用于本发明的第二组分涂层中的MCS可以如下来制造:将钙盐(例如氯化钙、碳酸钙、氢氧化钙)、二氧化硅前体(如硅酸盐,例如硅酸钠、硅酸钾、正硅酸四乙酯或硅酸四乙酯)和结构导向剂相组合,来产生适于煅烧的固体。能够实施来制造适用于本发明的MCS的方法在前述共同拥有的申请公开WO2008/015117中有更详细的说明。
在一种经常期望的实施方案中,涂层可以由CaO-SiO2形成。
在又一种经常优选的实施方案中,包含本发明的复合颗粒活性物的口腔护理组合物进一步包含磷酸盐源。对能够用于本发明的磷酸盐源的限制仅到其可用于适用于口腔的组合物中的程度。适用于本发明,并且与所述的复合颗粒活性物一起加入的磷酸盐源类型的示例性例子包括磷酸单钠,磷酸二氢钠,磷酸氢二钠,焦磷酸钠,焦磷酸四钠,三聚磷酸钠,六偏磷酸钠,磷酸二氢钾,磷酸三钠,磷酸三钾,其混合物等。该磷酸盐源优选是水溶性的。
当使用时,该磷酸盐源通常构成口腔护理组合物的0.5-22%、优选2-18%、最优选4-16%重量,基于该口腔护理组合物的总重量,并且包括其中所含的所有范围。在一种优选的实施方案中,所用的磷酸盐源是能产生pH为5.5-8、优选6-7.5、最优选大约中性的口腔护理组合物(如果是双相产物,则为组合的组合物)的磷酸盐源。在一种最优选的实施方案中,所用的磷酸盐源是磷酸三钠和磷酸二氢单钠,并且磷酸三钠和磷酸二氢单钠的重量比是1:4-4:1,优选1:3-3:1,最优选1:2-2:1,包括其中所含的所有比例。
用于有益于牙齿,并且包含本发明的复合颗粒活性物的口腔护理组合物可以包含本领域常用的任选成分。这些成分包括:
·抗菌剂,例如三氯生,洗必太(chlorhexidine),铜-、锌-和锡盐(例如柠檬酸锌、硫酸锌、甘氨酸锌、柠檬酸锌钠和焦磷酸锡),血根碱提取物,灭滴灵(metronidazole),季铵化合物(例如十六烷基吡啶钠),双胍(例如洗必太二葡糖酸盐、海克替啶(hexetidine)、奥替泥啶(octenidine)、阿来西定(alexidine)),和卤代双酚化合物(例如2,2’亚甲基双-(4-氯-6-溴酚));
·消炎剂,例如布洛芬(ibuprofen)、氟比洛芬(flurbiprofen)、阿司匹林、吲哚美辛(indomethacin)等;
·防龋齿剂,例如三偏磷酸钠和干酪素;
·噬菌区缓冲剂,例如脲、乳酸钙、甘油磷酸钙和聚丙烯酸锶;
·维生素,例如维生素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;
·抗结石剂,例如碱金属焦磷酸盐,包含次磷酸盐的聚合物,有机膦酸盐和膦柠檬酸盐等;
·生物分子,例如细菌素、抗体、酶等;
·香料,例如薄荷油和荷兰薄荷油;
·蛋白质材料,例如胶原质;
·防腐剂;
·遮光剂;
·着色剂,如FD&C蓝色、黄色和/或红色染料/着色剂;
·pH调节剂;
·甜味剂;
·表面活性剂,例如阴离子、非离子、阳离子和两性离子或两性表面活性剂(例如月桂基硫酸钠、十二烷基苯磺酸钠);
·微粒磨料,例如磨料二氧化硅,氧化铝,碳酸钙,硅酸锆,聚甲基丙烯酸甲酯,磷酸二钙,焦磷酸钙,羟磷灰石,三偏磷酸盐,不溶性六偏磷酸盐以及聚集的微粒磨料;
·氟化物源,如氟化钠,氟化锡,单氟磷酸钠,氟化锌铵,氟化锡铵,氟化钙,氟化钴铵或其混合物;
·还可以包括能够增强活性成分如抗菌剂的递送的聚合物。这样的聚合物的例子是聚乙烯基甲醚与马来酸酐的共聚物和其他类似的增强递送的聚合物,例如DE-A03942643中所述的那些;
·用于缓冲口腔护理组合物的pH和离子强度的缓冲剂和盐;和
·可包括的其他任选的成分是,例如漂白剂(如过氧化物化合物,例如过氧化二磷酸钾),泡腾体系(例如碳酸氢钠/柠檬酸体系),变色体系等。
这些成分通常合起来构成包含本发明的复合颗粒活性物的口腔护理组合物的小于20重量%,优选是该口腔护理组合物的0.0-15重量%,最优选0.01-12重量%,包括其中所含的所有范围。
增稠剂也可以用于本发明中,限制仅在于其能够与本发明的复合颗粒活性物一起加入到适用于口腔的组合物中。能够用于本发明的增稠剂类型的示例性的例子包括羧甲基纤维素钠,羟乙基纤维素,甲基纤维素,乙基纤维素,黄蓍胶,阿拉伯树胶,刺梧桐树胶,藻酸钠,角叉菜胶,瓜尔胶,黄原胶,爱尔兰苔藓(Irishmoss),淀粉,改性淀粉,二氧化硅基增稠剂(包括二氧化硅气凝胶),硅酸镁铝(即,Veegum),Carbomers(交联的丙烯酸酯)及其混合物。
典型地,羧甲基纤维素钠和/或Carbomer是优选的。当使用Carbomer时,期望的是分子量为至少700000的那些,并且优选期望的是分子量是至少1200000的那些,最优选分子量为至少大约2500000的那些。在此还可以使用Carbomer的混合物。
在一种特别优选的实施方案中,Carbomer是980。它被描述为一种高分子量和交联的聚丙烯酸,且通过CAS号9063-87-0来识别。其市售自Lubrizol AdvancedMaterial,Inc。
在另外一种特别优选的实施方案中,所用的羧甲基纤维素钠(SCMC)是SCMC9H。它被描述为具有键合到吡喃葡萄糖主链单体的羟基上的羧甲基的纤维素衍生物的钠盐,且通过CAS号9004-32-4来识别。其市售自供应商如Alfa Chem。
增稠剂通常构成口腔护理组合物的0.01-约10%、优选0.1-8%、最优选1.5-6%重量,基于该口腔护理组合物的总重量,包括其中所含的所有范围。
能够用于本发明的合适的载体是例如甘油,山梨糖醇,丙二醇,二丙二醇,双甘油,三醋精,矿物油,聚乙二醇(优选PEG-400),烷烃二醇(如丁二醇和己二醇),乙醇,戊二醇或其混合物。载体在任何情况下应当基本上不含水,并且如果期望的是包含磷酸盐作为添加剂和复合颗粒活性物的单相产品,则优选是无水的。该载体可以例如以固体形式使用,但是在单相产品中甘油往往是优选的载体或润湿剂。
载体用于将单相组合物补足到100%,其含量可以是单相口腔护理组合物的10-90重量%。优选载体构成单相口腔护理组合物的25-80%、最优选45-70%重量,基于单相口腔护理组合物的总重量,并且包括其中所含的所有范围。
在期望的是具有磷酸盐源的含水口腔护理产物的情况下,推荐双相口腔护理组合物,以防磷酸盐和复合颗粒活性物的第二组分涂层之间的相互作用(在使用前)。
当期望的是双相口腔护理组合物时,水可以充当载体(与此处所述的增稠剂和/或另外的载体一起),并且构成双相产物的每个组合物的补足量,其中第一组合物将包含复合颗粒活性物,和第二组合物将包含所加入的磷酸盐源。在双相产物中,该第一和第二组合物应当直到消费者将其分配到他或她的口腔中时才彼此接触。当使用双相口腔护理组合物时,此处所述的重量百分比描述的是第一和第二组合物组合之后的口腔护理组合物的特征。每个组合物(在期望双组合物产物的情况下)可以依次或同时,但是优选同时进行递送。在一种优选的实施方案中,双相口腔护理组合物中的每个组合物包含小于35重量%的水、最优选15-25重量%的水,基于每个组合物的总重量,并且包括其中所含的所有范围。
可将双相口腔护理组合物中的一个或优选两个组合物施用到牙齿上,并且牙齿的处理包括所述组合物的混合。无论单相还是双相,所述组合物优选在使用后留在牙齿上。在这样的施用之后,本发明的口腔护理组合物应当典型地在牙齿上停留5s-10小时和更典型地35s-30分钟。该施用可以每日进行。如果使用双相组合物,则其可以从双隔间管的独立的隔间中施用或从容纳在单个容器(其通常是管)中的产品的独立的相中施用。
在某些实施方案中,特别是包括凝胶组合物的那些中,递送的手段可以任选地涉及带子,特别是胶带条,在使该胶带条与牙齿接触之前,可以将本发明的组合物施用到其上。当使用这样的递送手段时,该组合物可以保持与牙齿表面密切接触,这促进了高浓度的复合颗粒活性物和磷酸盐接近牙齿的表面。
当凝胶是期望的时,其典型地包含聚合物基质,并且更典型地是水凝胶。不包括所存在的任何的水,该聚合物基质通常以包含它的组合物的1-25重量%存在。
用于制备水凝胶的单体可以选自例如乙烯醇和丙烯酸盐,特别是丙烯酸钠。也可以使用包含大量亲水基团的其他单体。
经常优选的水凝胶包括多糖、聚丙烯酰胺、聚丙烯酸或其混合物。
合适的多糖可以是存储型多糖,例如淀粉或肝糖,或结构型多糖,例如纤维素或几丁质。
能够使用的示例性多糖包括具有选自以下的一种或多种的糖单元的那些:异麦芽糖,葡萄糖,果糖,半乳糖,木糖,甘露糖,山梨糖,树胶醛糖,鼠李糖,海藻糖,麦芽糖,蔗糖,乳糖,麦芽糖,芯糖,来苏糖,阿洛糖,阿卓糖,古洛糖,艾杜糖,塔罗糖,海藻糖,黑曲霉糖(nigerose),曲二糖和乳果糖(lactulose)。
经常优选的水凝胶包含选自以下的至少一种多糖:罗望子胶,瓜尔胶,洋槐籽树胶,塔拉胶(Tara),胡芦巴,芦荟,芡欧鼠尾草,亚麻子,洋车前子的籽,温柏籽,黄原胶,结冷胶(gellan),维纶胶(welan),鼠李胶(rhamsan),右旋糖苷,卡德兰(curdlan),支链淀粉,硬葡聚糖(scleroglucan),裂裥菌素(schizophyllan),几丁质,羟烷基纤维素,阿拉伯树胶酸,脱支化阿拉伯树胶酸,阿拉伯糖基木聚糖,半乳糖体,果胶半乳糖体,半乳甘露聚糖,葡甘露聚糖,苔藓,甘露聚糖,茯苓聚糖,鼠李糖半乳糖醛酸聚糖(rhamnogalacturonan),阿拉伯树胶,琼脂,藻酸盐,角叉菜胶,壳聚糖,棒状体(clavan),透明质酸,肝磷脂,菊粉,纤维糊精,纤维素和纤维素衍生物。
特别优选的水凝胶可以包含多糖,如选自以下的那些:藻酸钠,藻酸羟丙酯,角叉菜胶,阿拉伯树胶,瓜尔胶,刺梧桐树胶,壳聚糖和果胶。
包含本发明的复合颗粒活性物的组合物(无论是单相还是双相)是通过制造口腔护理组合物的常规方法来制备的。这样的方法包括在中等剪力和大气压力下混合所述成分。该组合物期望地是用于口腔的,并且优选的是能够用牙刷刷到牙齿上的形式的。出乎意料地,本发明的口腔护理组合物产生了牙齿的优异的再矿化(即,形成新的羟磷灰石)和牙齿增白(其可以是即刻的,并且通过该复合颗粒活性物的芯来提供),这是复合颗粒活性物附着到牙釉质和/或牙本质上的结果。此外,在使用本发明的组合物之后,牙齿出乎意料地变得不太过敏和更有光泽,这同样是复合颗粒活性物附着到牙釉质和/或牙本质上的直接结果。
本发明的复合颗粒活性物可以通过产生包含芯材料和溶剂(例如低分子量酮类,如丙酮,低分子量醇类,如C3-6链烷醇,水或其混合物)的浆料来制备,该浆料包含3-60%、优选5-30%、最优选5-20%重量的芯材料,基于浆料的总重量。水通常是优选的溶剂。应当将该芯材料(如氧化钛或云母)浆料在25-95℃、优选55-95℃、最优选70-90℃加热,包括其所含的所有范围。在加热的同时,则应当将用于涂层阴离子部分的前体(如硅酸钠或二氧化硅)加入到该加热的浆料中,来提供在芯材料上的涂层。该阴离子部分(即,阴离子前体部分)在浆料内的固化应当在碱性pH(优选8.5-pH11、最优选9-pH10.5)下持续0.5小时-3小时、优选0.5小时-1小时。进一步但是优选地,当该芯材料在酸性条件(即,优选3-pH5)下不溶于浆料时,可以在这样的酸性条件下实现浆料的固化,持续额外的0.5-2小时。在涂层的阴离子部分固化之后,应当将适于施用阳离子(如钙离子)的化学金属材料加入到所形成的固化的芯浆料中。所形成的具有阳离子的混合物应当在pH9-13和用于固化芯的温度范围内固化0.5小时-24小时、优选0.5小时-2小时。在一种通常优选的步骤中,为了在浆料中原位产生涂覆材料,可以进一步加入阴离子前体试剂,如藻酸钠和/或硫酸钠。浆料pH可以用常规的成分如NaOH或HCL来调整。成分的混合可以用常规混合设备来实现。但是通常,经常优选的是具有紊流区的管道式反应器。常规的催化剂或结构导向剂可以用于产生复合颗粒。这些试剂在它们使用时通常构成浆料的0.01-3重量%。一种经常优选的试剂是十六基三烷基卤化铵,如十六基三甲基溴化铵等。在一种特别优选的实施方案中,将二氧化硅用于芯材料中和用于制造涂层的溶剂浆料中。所形成的颗粒可以通过常规技术来清洁,其包括过滤和/或离心分离以及随后的干燥。期望的本发明的复合颗粒可以通过干燥这样的所形成的颗粒来回收,这里干燥可以通过加热来加速,并且当加热到65℃-1000℃的温度时,通常需要大约10分钟到两(2)小时。
当本发明的口腔护理组合物是牙膏或凝胶时,其典型的粘度是大约50000-180000厘泊、优选60000-170000厘泊、最优选65000-165000厘泊,在室温用Brookfield粘度计No.4转子来测量。
在牙膏或凝胶形式中,所述组合物可以包装在常规的塑料层合体、金属管或单隔间分配器中。其可以通过任何物理装置例如牙刷、指套施用到牙齿表面上,或通过施涂器直接施用到过敏区域。固体剂型类型包括药锭、锭剂、口香糖、片剂、含片(mouthstrip)、香膏(balm)等。它们可以容纳在适合消费者使用的常规包装中。
提供了以下实施例来帮助理解本发明。这些实施例不是提供来限制权利要求的范围的。
实施例1
通过将下面的成分在中等剪力、大气压力和环境温度条件下混合,制造了一种有益于牙齿并且与本发明一致(即,包含复合颗粒活性物)的双相水基口腔护理组合物是。所制造的组合物适于用牙刷来使用,并且在大致相等地组合时不是砂砾状的,且在施用到牙刷上时产生了优异的条。所组合的组合物具有消费者可接受的味道特性,其产生了本发明的口腔护理组合物。
含钙相:
成分 | 重量百分比 |
山梨糖醇(70%) | 20.0 |
水 | 补足量 |
防腐剂 | 1.0 |
单氟磷酸钠 | 1.1 |
甜味剂(人造) | 0.2 |
硅酸钙* | 20.0 |
磨料二氧化硅 | 6.0 |
增稠性二氧化硅(气相二氧化硅) | 2.5 |
硅酸钙涂覆的二氧化钛** | 4.00 |
香料 | 0.9 |
羧甲基纤维素钠 | 0.6 |
月桂基硫酸钠(30%) | 6.60 |
*由Ineos Silicas,Ltd提供。
**复合颗粒活性物,涂层~10nm;颗粒直径~100-300nm。
含磷酸盐的相:
实施例2
使用碳化硅研磨纸(1200粒)将牙釉质和牙本质块(3cm2)抛光大约5分钟。将牙本质块使用36%的磷酸蚀刻60s,随后水洗。该块购自市售供应商。
将包含20重量%的硅酸钙和4重量%的复合颗粒活性物的浆料(类似于实施例1所述的那种)加入到补足量的水中来制造浆料。磷酸钠浆料是通过将20重量%的磷酸钠加入补足量的水中来制造的。使用常规搅拌设备将所形成的浆料均质化大约10分钟来产生均匀的组合物。
将该均质化的浆料倾倒入皮氏培养皿中。使用足够的浆料来覆盖置于所述培养皿中的块的表面。将所述块用牙刷刷1分钟,并且在浆料中培养1分钟。随后用蒸馏水清洗所述块3次,并且进一步在37℃水浴中,在模拟的口腔流体中培养大约2小时。将每个块重复处理14次。
处理结果–牙釉质块
图1A显示了在1次处理后牙釉质块的扫描电子显微镜图象。在1次处理后复合颗粒活性物(圈出的)令人惊讶地显示附着到牙釉质块的表面上。
图1B显示了相同块的能量分散x射线图(元素分布图(elemental maps),Ti Ka1,20KV)。在1次处理后复合颗粒活性物显示为令人惊讶地充分附着到牙釉质块上的亮点(圈出的)。
图2A显示了在14次处理之后牙釉质块的扫描电子显微镜图象,图2B显示了同一块在经受14次处理后的能量分散x射线图象。结果出乎意料地证实了复合颗粒活性物在牙釉质表面上的优异附着。
处理结果–牙本质块
图3A显示了在1次处理后牙本质块的扫描电子显微镜图象。复合颗粒活性物令人惊讶的显示附着在牙本质表面上。
图3B显示了同一块的能量分散x射线图象(元素分布图,Ti Ka1,20KV)。复合颗粒活性物令人惊讶地显示附着在牙本质上粘附。
图4A显示了在14次处理之后牙本质块的扫描电子显微镜图象,图4B显示了同一块在经受14次处理后的能量分散x射线图象。结果出乎意料地证实了复合颗粒活性物在牙本质表面上的优异附着。
本发明的活性物组合物在牙釉质和牙本质上出乎意料的附着不可避免地将产生牙齿再矿化、脱敏和增亮。
实施例3
为了研究实施例1的示例性双相口腔护理组合物的增白效果,进行了下面的体外测试。
清洁人类牙齿并分成两组(N=8)。在处理的同时,将实施例1的组合物用棉棒施用到牙齿表面(组I)。30分钟后,将处理过的牙齿用市售牙膏和水的浆料(例如含氟牙膏,1%氟化钠:水=1:2)刷一(1)分钟来清洁所处理的表面。将该清洁的牙齿在模拟的口腔流体中培养大约2小时。对该牙齿进行14个上述处理循环。模拟的口腔护理流体是通过组合下面的成分来制造的:
模拟的口腔流体
对组II的牙齿的处理与组I相同,除了仅仅使用市售的牙膏之外。
处理前后的白度变化是使用Konica Minolta–2600D颜色分析仪来获得的。
结果出乎意料的证实了用本发明的组合物处理过的牙齿具有大约4.80的优异的增白指数,而常规的市售产品仅仅具有大约-0.91的增白指数。此外,图5显示了用常规的含有二氧化硅的牙膏(5A)和本发明的硅酸钙涂覆的二氧化硅(复合颗粒活性物)(5B)处理过的牙齿的扫描电子显微镜图象。令人惊讶的是,从该图中可以观察到,当与本发明一致时,明显更多的颗粒(特别是尺寸为直径大约2μm的颗粒/聚集体)沉积在牙齿表面上。
实施例4
通过在大气条件下搅拌来制备10重量%的二氧化钛和水的浆料。将该浆料加热到大约90℃持续30-35分钟。将1M硅酸钠溶液加入到该加热的浆料(S1O2/T1O2,10重量%)中。加入盐酸(0.5M)来将浆料的pH缓冲到9-10.5持续一(1)小时的时间。停止加热,将所形成的浆料冷却到大约70℃。向该冷却的浆料中加入1M的CaCl2溶液(CaCl2/SiO2,1M,1M)。还向所形成的浆料中加入1M氢氧化钠溶液来将pH缓冲到10.5-12的范围持续一(1)小时的时间。将所形成的浆料通过离心分离清洁,并且在90℃干燥大约45分钟。所形成的颗粒是根据本发明的复合颗粒活性物。
图6显示了未涂覆的二氧化钛6a和6b和根据本发明的硅酸钙涂覆的二氧化钛(6c和6d)的透射电子显微图象。该第二组分涂层是均质的,这归因于所有的二氧化钛芯都是涂覆的并且硅酸钙涂层为约10nm厚。
实施例5
类似于实施例4所述制造了复合颗粒活性物,除了使用氧化锌代替二氧化钛之外。透射电子显微图象揭示了当进行本发明的方法时,氧化锌芯上成功的涂覆了硅酸钙涂层。
实施例6
为了研究实施例1的示例性双相口腔护理组合物的增白效果,进行了下面的消费者研究。
将所选择的受测试者(其具有高于3M1的初始牙齿颜色范围,这是通过来自VitaZahnfabrik的牙齿指南3D-Master确定的)分成大约三个相等的组,(N=55)和组A、B和C。所有受测试者被要求每日刷牙两次。给予每组不同的牙膏。给予组B的受测试者实施例1的双相口腔护理组合物,这是根据本发明的组合物;给予组A的受测试者这样的双相组合物,其类似于实施例1所述的组合物,除了使用30重量%的硅酸钙和不使用复合颗粒活性物之外。组C(对照组)的受测试者使用市售的没有与牙齿再矿化相关的活性成分的牙膏组合物刷牙。
使用前述的来自Vita Zahnfabrik的VITA色调牙齿指南3D-Master获得处理前后的白度变化(刷牙2周和4周后)。
图7中所示的结果出乎意料的证实了在4周的处理后,组B的受测试者的牙齿获得了VITA值的明显降低,并且在处理仅仅2周后就获得了可测出的降低。组A的受测试者的牙齿获得了VITA值的降低,但是该降低在4周的处理之前基本上没有测出。对照组C的受测试者的牙齿在4周的处理后没有表现出VITA值的明显变化。
该结果证实了对于使用根据本发明的组合物的受测试者的牙齿来说,VITA值明显降低,由此使用本发明的口腔护理组合物的受测试者的牙齿的增白效应明显优于用没有复合颗粒活性物的组合物处理的牙齿。图7显示了对于所测试的组来说,在2周和4周后VITA值相对于基线的变化。组B表现出当使用本发明的口腔护理组合物时获得了出乎意料的、更好的增白结果。
Claims (20)
1.一种复合颗粒活性物,其包含:
a)用于改善口腔护理特性的第一组分芯;和
b)第二组分涂层,其与磷酸盐离子相互作用产生磷酸钙原位反应产物,该反应产物附着到牙釉质、牙本质或二者上并且是形成羟磷灰石的前体。
2.根据权利要求1的复合颗粒活性物,其中该第一组分芯包含二氧化硅、二氧化钛、氧化锌、云母、碳酸钙、硫酸钡或其混合物,和该第二组分涂层包含元素钙,和任选地,钾、钠、铝、镁或其混合物。
3.根据权利要求1或2的复合颗粒活性物,其中至少5%的该第一组分芯涂覆有该第二组分涂层。
4.根据前述任一项权利要求的复合颗粒活性物,其中该复合颗粒活性物的直径小于50微米。
5.根据前述任一项权利要求的复合颗粒活性物,其中该复合颗粒活性物的芯构成该复合颗粒活性物的3-98重量%。
6.根据权利要求2-5任一项的复合颗粒活性物,其中该第一组分芯包含至少50重量%的二氧化钛,和该第二组分涂层包含至少50重量%的钙元素。
7.根据前述任一项权利要求的复合颗粒活性物,其中该第二组分涂层包含磷酸钙、葡糖酸钙、氧化钙、乳酸钙、碳酸钙、氢氧化钙、硫酸钙、羧甲基纤维素钙、藻酸钙、柠檬酸的钙盐、硅酸钙或其混合物。
8.根据权利要求1的复合颗粒活性物,其中该第二组分涂层包含硅酸钙,其是CaSiO3、CaO-SiO2或其混合物。
9.根据前述任一项权利要求的复合颗粒活性物,其中该第二组分涂层与磷酸盐离子相互作用,并附着到牙釉质、牙本质或二者上。
10.根据前述任一项权利要求的复合颗粒活性物,其中该复合颗粒活性物包含10nm到小于10微米的直径。
11.根据权利要求10的复合颗粒活性物,其中该复合颗粒活性物的至少40%的直径是由芯构成的。
12.根据前述任一项权利要求的复合颗粒活性物,其中至少70-100%的该第一组分芯涂覆有该第二组分涂层。
13.根据权利要求1的复合颗粒活性物,其中该第二组分涂层包含氧化钙-二氧化硅。
14.根据前述任一项权利要求的复合颗粒活性物,其中该第二组分涂层包含钙:二氧化硅为1:10到3:1的硅酸钙。
15.根据前述任一项权利要求的复合颗粒活性物,其中该第二组分涂层包含介孔硅酸钙。
16.根据前述任一项权利要求的复合颗粒活性物,其中该复合颗粒活性物可以负载在牙膏、牙齿凝胶、片剂、口香糖、乳霜、饮料、锭剂、含片或贴片中。
17.一种制造权利要求1的复合颗粒活性物的方法,其包含步骤:
a)将芯材料和溶剂混合来产生芯浆料;
b)将该芯浆料加热到25℃-95℃持续0.5-3小时;
c)加入适于原位产生涂覆材料的试剂来产生芯和涂覆材料浆料;和
d)干燥该芯和涂覆材料浆料来回收复合颗粒活性物,
其中如果该芯材料在酸性条件下是不溶的,则将该芯浆料首先在碱性条件下和接着在酸性条件下加热。
18.根据权利要求17的方法,其中该芯材料包括二氧化硅、二氧化钛、氧化锌、云母、碳酸钙、硫酸钡或其混合物。
19.根据权利要求17或18的方法,其中该适于原位产生涂覆材料的试剂包括二氧化硅、硅酸钠、硅酸钾、藻酸钠、硫酸钠、正硅酸四乙酯或其混合物。
20.根据权利要求17或18的方法,其中该适于原位产生涂覆材料的试剂包括硅酸钙、磷酸钙、葡糖酸钙、氧化钙、氯化钾、乳酸钙、碳酸钙、氢氧化钙、硫酸钙、羧甲基纤维素钙、氯化钙、氯化镁、氯化铝、藻酸钙、柠檬酸的钙盐、其混合物等。
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BR (1) | BR112013004354B8 (zh) |
SA (1) | SA111320297B1 (zh) |
WO (1) | WO2012031785A2 (zh) |
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EA033259B1 (ru) * | 2013-09-10 | 2019-09-30 | Юнилевер Н.В. | Композиция для ухода за полостью рта |
WO2015095606A1 (en) | 2013-12-20 | 2015-06-25 | Colgate-Palmolive Company | Core shell silica particles and uses thereof as an anti-bacterial agent |
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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 |
WO2016180601A1 (en) | 2015-05-13 | 2016-11-17 | Unilever N.V. | Oral care composition |
CN107743387A (zh) * | 2015-06-05 | 2018-02-27 | 荷兰联合利华有限公司 | 口腔护理装置 |
EA035881B1 (ru) * | 2015-06-05 | 2020-08-26 | Юнилевер Н.В. | Способ косметического отбеливания зубов |
EP3302349B1 (en) | 2015-06-05 | 2019-11-20 | Unilever PLC | Oral care device |
DE102015110367A1 (de) * | 2015-06-26 | 2016-12-29 | Karlsruher Institut für Technologie | Online-Phosphor-Nachweis durch Infrarotspektroskopie |
CN108024912A (zh) * | 2015-09-24 | 2018-05-11 | 荷兰联合利华有限公司 | 口腔护理组合物 |
EA036458B1 (ru) | 2015-11-10 | 2020-11-12 | Юнилевер Н.В. | Композиция для ухода за полостью рта |
CN106380769A (zh) * | 2016-10-21 | 2017-02-08 | 浙江九天寰宇生物科技有限公司 | 一种牙齿美白仪牙托用美白凝胶及其制备方法 |
WO2018224331A1 (en) * | 2017-06-07 | 2018-12-13 | Unilever N.V. | Oral care composition |
BR112020000242B1 (pt) * | 2017-07-07 | 2023-01-10 | Unilever Ip Holdings B.V. | Composição de cuidados orais, processo de fabricação de uma composição de cuidados orais e uso de uma composição |
WO2019029917A1 (en) * | 2017-08-10 | 2019-02-14 | Unilever N.V. | COMPOSITION FOR ORAL CARE |
CN108264235B (zh) * | 2017-12-28 | 2021-04-06 | 东莞市鸿元医药科技有限公司 | 一种促进创面愈合的生物活性玻璃粉末的制备方法及应用 |
BR112021002528B1 (pt) | 2018-09-12 | 2023-12-05 | Unilever Ip Holdings B.V | Composição de cuidado pessoal não aquosa e uso de um ph 9,45 ou superior |
WO2020212159A1 (en) | 2019-04-17 | 2020-10-22 | Unilever Plc | Oral care product |
CN110511060A (zh) * | 2019-08-22 | 2019-11-29 | 德化县顺尔美工艺品有限公司 | 一种仿绞胎陶瓷及其制作工艺 |
CN111110576B (zh) * | 2020-02-13 | 2022-04-19 | 西安科技大学 | 一种牙釉质再生组合物的制备方法 |
EP3888621A1 (en) | 2020-04-02 | 2021-10-06 | Unilever Global IP Ltd | Oral care device |
EP3888620A1 (en) | 2020-04-02 | 2021-10-06 | Unilever Global IP Ltd | Oral care system |
EP3888619A1 (en) | 2020-04-02 | 2021-10-06 | Unilever Global IP Ltd | Oral care device |
EP3888622A1 (en) | 2020-04-02 | 2021-10-06 | Unilever Global IP Ltd | Oral care system |
EP3888623A1 (en) | 2020-04-02 | 2021-10-06 | Unilever Global IP Ltd | Oral care system |
CN111481740A (zh) * | 2020-04-17 | 2020-08-04 | 中山职业技术学院 | 一种高分散性无定形磷酸钙纳米粉体及其制备方法和应用 |
CN111494706A (zh) * | 2020-04-17 | 2020-08-07 | 中山职业技术学院 | 一种多孔改性无定形磷酸钙纳米粉体及其制备方法和应用 |
BR112022021230A2 (pt) | 2020-05-21 | 2022-12-27 | Unilever Ip Holdings B V | Composição de cuidados orais, produto de cuidados orais, método de remineralização e/ou redução da hipersensibilidade dos dentes e uso de composição |
CA3220437A1 (en) | 2021-05-20 | 2022-11-24 | Smile Makers, Llc | Oral hygiene compositions and methods of use |
CN113995682B (zh) * | 2021-11-04 | 2022-11-11 | 浙江大学 | 牙齿修复组合物在牙齿修复上的应用 |
CN115887251B (zh) * | 2022-12-15 | 2023-07-04 | 金三江(肇庆)硅材料股份有限公司 | 一种二氧化硅-硫酸钙复合颗粒及其制备方法和应用 |
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- 2011-03-11 WO PCT/EP2011/053740 patent/WO2012031785A2/en active Application Filing
- 2011-03-11 BR BR112013004354A patent/BR112013004354B8/pt active IP Right Grant
- 2011-03-11 EP EP11710153.5A patent/EP2613850B1/en active Active
- 2011-03-11 US US13/820,154 patent/US20130164359A1/en not_active Abandoned
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Also Published As
Publication number | Publication date |
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EP2613850A2 (en) | 2013-07-17 |
CN103079645A (zh) | 2013-05-01 |
EP2613850B1 (en) | 2016-11-23 |
BR112013004354B1 (pt) | 2017-12-05 |
US20130164359A1 (en) | 2013-06-27 |
SA111320297B1 (ar) | 2014-11-12 |
BR112013004354B8 (pt) | 2018-10-23 |
BR112013004354A2 (pt) | 2016-05-10 |
WO2012031785A3 (en) | 2012-10-18 |
WO2012031785A2 (en) | 2012-03-15 |
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