WO2014069595A1 - 歯牙用貼付シート - Google Patents
歯牙用貼付シート Download PDFInfo
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- WO2014069595A1 WO2014069595A1 PCT/JP2013/079614 JP2013079614W WO2014069595A1 WO 2014069595 A1 WO2014069595 A1 WO 2014069595A1 JP 2013079614 W JP2013079614 W JP 2013079614W WO 2014069595 A1 WO2014069595 A1 WO 2014069595A1
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- UNXHWFMMPAWVPI-ZXZARUISSA-N erythritol Chemical compound OC[C@H](O)[C@H](O)CO UNXHWFMMPAWVPI-ZXZARUISSA-N 0.000 description 1
- 229940009714 erythritol Drugs 0.000 description 1
- 235000003599 food sweetener Nutrition 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
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- 238000010191 image analysis Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
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- 239000004615 ingredient Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229920000831 ionic polymer Polymers 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000832 lactitol Substances 0.000 description 1
- 235000010448 lactitol Nutrition 0.000 description 1
- VQHSOMBJVWLPSR-JVCRWLNRSA-N lactitol Chemical compound OC[C@H](O)[C@@H](O)[C@@H]([C@H](O)CO)O[C@@H]1O[C@H](CO)[C@H](O)[C@H](O)[C@H]1O VQHSOMBJVWLPSR-JVCRWLNRSA-N 0.000 description 1
- 229960003451 lactitol Drugs 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 229920001684 low density polyethylene Polymers 0.000 description 1
- 239000004702 low-density polyethylene Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000000845 maltitol Substances 0.000 description 1
- 235000010449 maltitol Nutrition 0.000 description 1
- VQHSOMBJVWLPSR-WUJBLJFYSA-N maltitol Chemical compound OC[C@H](O)[C@@H](O)[C@@H]([C@H](O)CO)O[C@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O VQHSOMBJVWLPSR-WUJBLJFYSA-N 0.000 description 1
- 229940035436 maltitol Drugs 0.000 description 1
- 239000000594 mannitol Substances 0.000 description 1
- 235000010355 mannitol Nutrition 0.000 description 1
- 229960001855 mannitol Drugs 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 235000007686 potassium Nutrition 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229940083542 sodium Drugs 0.000 description 1
- CAVXVRQDZKMZDB-UHFFFAOYSA-M sodium;2-[dodecanoyl(methyl)amino]ethanesulfonate Chemical compound [Na+].CCCCCCCCCCCC(=O)N(C)CCS([O-])(=O)=O CAVXVRQDZKMZDB-UHFFFAOYSA-M 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 229960002920 sorbitol Drugs 0.000 description 1
- 235000010356 sorbitol Nutrition 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000003765 sweetening agent Substances 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000036962 time dependent Effects 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical class [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 1
- 238000003221 volumetric titration Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Images
Classifications
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- A61C19/06—Implements for therapeutic treatment
- A61C19/063—Medicament applicators for teeth or gums, e.g. treatment with fluorides
- A61C19/066—Bleaching devices; Whitening agent applicators for teeth, e.g. trays or strips
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- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/36—Carboxylic acids; Salts or anhydrides thereof
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- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
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- A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- A61K8/8135—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid; Compositions of derivatives of such polymers, e.g. vinyl esters (polyvinylacetate)
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- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/92—Oral administration
Definitions
- the present invention relates to a tooth sticking sheet excellent in tooth whitening effect.
- Human teeth are colored by the addition of tartar and plaque, as well as various colored materials attached to the surface, and the gloss is lowered. These reductions in coloring and gloss are not cosmetically desirable, and various means for whitening teeth have been developed.
- Patent Document 1 discloses a tooth whitening patch having a multilayer structure of a contact pressure-sensitive adhesive layer, an active substance storage layer, and a support layer, and the contact pressure-sensitive adhesive layer exhibits an adhesive force when applied to a tooth.
- the peroxide contained in the active substance storage layer provides a whitening effect on the teeth.
- Patent Document 2 discloses a first film having a first whitening agent and a first water-soluble or water-dispersible polymer system, and a second whitening agent and a second water-soluble or water-dispersible polymer system.
- a multilayer strip is disclosed that includes a second film having a whitening agent such as hydrogen peroxide contained in each film.
- Patent Document 3 discloses a method for producing a laminate including an individual layer, in which at least one layer can contain at least one drug or cosmetic active substance, and the like. It is also described that the coating composition used to form the layer may have a different concentration, viscosity, crosslinkability, solid content, solvent content or pH.
- the present invention relates to a layer (A) having a pH of 6.6 to 10.5 when dissolved in water, phytic acid, hexametaphosphoric acid, an organic acid having a pKa of 4.5 to 7.0 at 25 ° C. And a layer (B) containing one or more components (b) selected from these salts and having a pH of 3.5 or more and 6.5 or less when dissolved in water
- the present invention provides a tooth sticking sheet (hereinafter also referred to as “the sticking sheet of the present invention”).
- Example 6 is a graph showing the change with time of pH after storage based on Measurement Method 1 in the laminated sheets of Examples 46 to 49. It is a graph which shows the time-dependent change of pH after the preservation
- the tooth whitening patches and multilayer strips described in Patent Documents 1 and 2 above use peroxides such as hydrogen peroxide as a whitening component, the tooth surface and the oral mucosa are stimulated more than necessary or perceived. It may cause hypersensitivity, etc., and there is a possibility that a sufficient effect cannot be obtained for discoloration of teeth due to aging or the like. Furthermore, the manufacturing method of the laminated body described in Patent Document 3 does not disclose specific components and pH for applying the whitening effect by sticking the laminated body to the teeth, and has safety. Sufficient studies have not been made to obtain a product that improves the whitening effect of the teeth while increasing the amount.
- peroxides such as hydrogen peroxide
- the present invention relates to a tooth sticking sheet that has a high safety and can obtain an excellent tooth whitening effect by simple means of sticking to a tooth.
- the inventors of the present invention have examined substances that can cause coloring of teeth due to aging, and found that components in a minute solid product having a thickness of less than several ⁇ m attached to the tooth surface are coloring factors. Furthermore, when this minute solid product was analyzed in detail, this minute solid product contains not only inorganic substances such as calcium phosphates but also organic substances, and these inorganic substances and organic substances are uniformly mixed. Rather, it was discovered that there are many locations where each is unevenly distributed to form a solid product. Therefore, the present inventors unexpectedly apply a specific component to a minute solid product on the tooth surface where the organic substance and the inorganic substance are unevenly distributed while giving a temporal change to the pH environment of the tooth surface.
- the pH environment of the tooth surface can be changed over time while sufficiently applying specific components when sticking to the tooth. It exhibits excellent whitening effect and can make teeth white and glossy.
- the fine dirt or solid product adhering to or depositing on the tooth refers to a solid material having a thickness of less than several ⁇ m generated on the surface of the tooth, and the solid material includes an inorganic substance or an organic substance, Or what has the structure of the composite aggregate
- This minute solid product is thought to be gradually formed mainly by the deposition of components such as protein, calcium, and phosphorus in saliva, and the oral environment deteriorates due to aging and decreased salivary secretion. Etc., and is difficult to remove by normal brushing processing.
- the adhesive sheet of the present invention has a layer (A) having a pH of 6.6 to 10.5 when dissolved in water, phytic acid, hexametaphosphoric acid, and a pKa at 25 ° C. of 4.5 to 7.0. It has a layer (B) containing one or more components (b) selected from organic acids and salts thereof and having a pH of 3.5 or more and 6.5 or less when dissolved in water.
- the layer (A) having a pH of 6.6 or more and 10.5 or less when dissolved in water and the component (b) are contained, and the pH is 3.5 or more and 6 when dissolved in water.
- the layer (A) and the layer (B) are sequentially dissolved on the tooth surface when applied to the tooth, and the pH environment on the tooth surface is changed over time.
- the component (b) contained in the layer (B) can be released to the tooth surface.
- the layer (A) of the patch sheet of the present invention has a pH of 6.6 or more and 10.5 or less when dissolved in water.
- the pH environment of the tooth surface is set to 6.6 or more and 10.5 or less, and it is particularly effective for the organic soil in the solid product to make it easy to remove the inorganic soil in the solid product.
- the component (b) is likely to act under the environment, and the low crystalline apatite can be selectively and satisfactorily removed to sufficiently exhibit an immediately effective gloss imparting effect.
- the pH of the layer (A) when dissolved in water is a value at room temperature (25 ° C.), and it is 6.6 or more from the viewpoint of providing a gloss imparting effect and a whitening effect while making it easy to remove organic matter stains.
- 7.1 or more is preferable, 7.5 or more is more preferable, and 8 or more is particularly preferable.
- From the viewpoint of action on the oral mucosa it is 10.5 or less, and further 10 or less. Further, it is preferably 9.5 or less, more preferably 9 or less.
- the layer (A) has a pH of 6.6 to 10.5 when dissolved in water, preferably 7.1 to 10, and preferably 7.5 to 9.5. Most preferably, it is 8-9.
- the measuring method of pH of a layer (A) applies and measures the minimum amount of water which can measure pH on a layer (A). Specifically, at room temperature (25 ° C.), water that can dissolve the layer (A) on the adhesive sheet of the present invention inclined at 45 degrees from the horizontal plane with the layer (A) facing up, for example, 0 After dropping 1 to 0.5 g, the dropped water is promptly collected, and the pH is measured, for example, with a compact pH meter B-712 (Horiba, Ltd.).
- the water in which the layer (A) is dissolved is purified water and includes distilled water or ion exchange water.
- the solid (B) is solidified in a state in which minute solid products are easily removed. You may use 1 type individually or in combination of 2 or more types in the range which can suppress the demineralization of a tooth
- the layer (A) of the adhesive sheet of the present invention preferably further contains a gelling agent.
- a gelling agent include pullulan, sodium carboxymethylcellulose, hydroxyethylcellulose, carboxyvinyl polymer, xanthan gum, carrageenan, sodium alginate, hydroxypropylcellulose, hydroxypropylmethylcellulose, guar gum, and chondroitin sulfate sodium.
- non-ionic polymers such as pullulan, hydroxyethyl cellulose, hydroxypropyl methylcellulose, guar gum, hydroxypropyl cellulose, etc., from the viewpoint that the sheet can be prepared well and the solubility of the layer (A) can be controlled well.
- 1 type (s) or 2 or more types it is preferable to contain 1 type (s) or 2 or more types, and from the viewpoint of an immediate effect of gloss imparting effect and whitening effect, 1 type or 2 types or more selected from pullulan, hydroxyethylcellulose, hydroxypropylmethylcellulose, and hydroxypropylcellulose It is more preferable to contain.
- the layer (A) of the adhesive sheet of the present invention is a component of fluctuation in pH environment and components by releasing the component (b) contained in the layer (B) into the oral cavity while changing the pH environment in the oral cavity.
- this component (a) is effective as a gloss-enhancing action enhancer by the component (b) contained in the layer (B) described later, each of the components (a) and (b) can be applied simultaneously.
- the layer (A) and the layer (B) can be made to act in order when the sheet is stuck to a tooth, and the gloss imparting action of the component (a) is improved by the component (b). It can effectively act as an enhancer, and can enhance the whitening effect and gloss imparting effect of the teeth.
- Examples of the component (a) alkyl sulfuric acid, acylmethyl tauric acid, N-acyl sarcosine acid and salts thereof include lauryl sulfate, lauroylmethyl tauric acid, N-lauroyl sarcosine acid and salts thereof. Salts are preferable, and as these salts, alkali metal salts such as sodium salts and potassium salts are more preferable. Specifically, sodium lauryl sulfate, potassium lauryl sulfate, sodium lauroylmethyl taurine, potassium lauroylmethyl taurine, sodium lauroyl sarcosine And lauroyl sarcosine potassium.
- orthophosphoric acid and condensed phosphoric acid examples include pyrophosphoric acid, tripolyphosphoric acid, tetrapolyphosphoric acid, and metaphosphoric acid.
- alkali metal salts such as sodium salt and potassium salt are preferable.
- examples thereof include sodium pyrophosphate, potassium pyrophosphate, sodium tripolyphosphate, and potassium tripolyphosphate.
- pyrophosphoric acid, tripolyphosphoric acid or a salt thereof is preferable, and sodium pyrophosphate or sodium tripolyphosphate is more preferable from the viewpoint of enhancing the whitening effect and gloss-imparting effect of the tooth by short-term use.
- the content of the component (a) in the layer (A) is from the viewpoint of satisfactorily exhibiting the effect of removing this fine solid product while easily removing it, the effect of enhancing glossiness, and the whitening effect.
- the dry mass is preferably 1% by mass or more, more preferably 2% by mass or more, and further preferably 3% by mass or more.
- the content of the component (a) in the layer (A) is dry mass, preferably 15% by mass or less, more preferably 10% by mass or less, from the viewpoint of use feeling such as taste and squeaky. More preferably, it is 8.5 mass% or less, More preferably, it is 7 mass% or less.
- the content of the component (a) in the layer (A) is preferably 1 to 15% by mass, more preferably 2 to 10% by mass, and further preferably 3 to 8.5% by mass in terms of dry mass. %, More preferably 3 to 7% by mass.
- the thickness of the layer (A) is preferably 100 ⁇ m or less, more preferably 50 ⁇ m or less, and even more preferably 20 ⁇ m or less from the viewpoint of dissolving the layer (A) in an appropriate time and ensuring appropriate flexibility as a sheet. .
- the thickness of the layer (A) is preferably 1 ⁇ m or more, more preferably 5 ⁇ m or more, and even more preferably 7 ⁇ m or more, from the viewpoint of enabling enhancement of the whitening action and gloss imparting action of the teeth.
- the thickness of the layer (A) is preferably 1 to 100 ⁇ m, more preferably 5 to 50 ⁇ m, and further preferably 7 to 20 ⁇ m.
- the layer (A) is preferably formed using the stock solution (A).
- the layer (A) can be formed by forming a layer using the stock solution (A) and then performing a drying process.
- the content of the component (a) in the stock solution (A) is an effect of satisfactorily removing the component while keeping the minute solid product easy to remove. From the viewpoint of sufficiently exhibiting the gloss enhancement effect and the whitening effect, it is preferably 0.025% by mass or more, more preferably 0.125% by mass or more, and further preferably 0.25% by mass or more. is there.
- the content of the component (a) in the undiluted solution (A) is preferably 7.5% by mass or less, more preferably 5% by mass or less, and still more preferably from the viewpoint of feeling of use such as taste and squeakiness. Is 2.5% by mass or less.
- the content of component (a) in the stock solution (A) is preferably 0.025% by mass to 7.5% by mass, more preferably 0.125-5% by mass, and still more preferably 0 .25 to 2.5% by mass.
- the content of component (a) in the stock solution (A) is measured after neutralization with potassium hydroxide or sodium hydroxide, and the total amount is converted to an acid.
- the pH of the stock solution (A) is preferably 6.6 or more, more preferably 7.1 or more, and still more preferably 7.5 or more, particularly preferably 8 or more. From the viewpoint of action on the oral mucosa, it is 10.5 or less, more preferably 10 or less, and further preferably 9.5 or less. In particular, it is preferably 9 or less. From the same viewpoint, the pH of the stock solution (A) is preferably 6.6 to 10.5, more preferably 7.1 to 10, and further preferably 7.5 to 9.5 or less. In particular, 8 to 9 is preferable.
- the layer (A) using the stock solution (A) from the viewpoint of film formability when the stock solution (A) has a high salt concentration, as a gelling agent, a nonionic polymer, that is, pullulan, It is preferable to contain one or more of hydroxyethylcellulose, guar gum, hydroxypropylcellulose, hydroxypropylmethylcellulose and the like.
- the layer (A) or the stock solution (A) may contain about 1 to 20 times the amount of water and / or a solvent such as ethanol.
- the stock solution (A) contains water and It is preferable to form a slurry using a solvent such as ethanol.
- the layer (A) is formed using a slurry-like stock solution (A) formed using a solvent such as water and / or ethanol, and then formed through a drying step, and the water content in the layer (A) is
- the layer (A) has a dry weight of 100 parts by mass, preferably 18 parts by mass or less, more preferably 15 parts by mass or less, and still more preferably 14 parts by mass or less. From the viewpoints of productivity and manufacturability, it is preferably 2 parts by mass or more, more preferably 3 parts by mass or more, and further preferably 5 parts by mass or more.
- the layer (B) in the adhesive sheet of the present invention comprises one or more components selected from phytic acid, hexametaphosphoric acid, an organic acid having a pKa of 4.5 to 7.0 at 25 ° C., and salts thereof ( b). Since this component (b) has an excellent whitening effect and gloss imparting effect on teeth in the acidic to weakly acidic region, the gloss imparting effect can be obtained by causing the layer (A) and the layer (B) to act on the teeth in order. Can be remarkably enhanced, and excellent tooth glossing effect and tooth whitening effect can be obtained even by short-term use.
- Examples of the organic acid having a pKa at 25 ° C. of 4.5 to 7.0 include fumaric acid, malic acid, tartaric acid, citric acid, glutaric acid and the like.
- a component (b) a phytic acid or its salt is preferable from a viewpoint which exhibits the outstanding whitening effect
- pKa in 25 degreeC is the reciprocal value of the logarithm of an acid dissociation constant (for example, "Chemical Handbook basic edition 2nd revised edition", page 993, Maruzen Co., Ltd., September 20, 1986 No.
- the layer (B) has a pH of 3.5 or more and 6.5 or less when dissolved in water.
- the layer (B) has a pH of 3.5 or more and 6.5 or less when dissolved in water.
- the pH when the layer (B) is dissolved in water to pH 3.5 or more and 6.5 or less
- the adhesive sheet of the present invention is applied to a tooth, it is dissolved in saliva or the like.
- the pH environment of the tooth surface is adjusted to pH 3.5 or more and 6.5 or less, and particularly low crystalline apatite is selectively removed from the tooth surface to the enamel trabecular space. It can effectively act on inorganic soils to remove fine solid products, and suppress the decalcification of the tooth surface, so that it can sufficiently exhibit a gloss imparting effect and a whitening effect with immediate effect.
- the pH when the layer (B) is dissolved in water is a value at 25 ° C., and is 3.5 or more from the viewpoint of suppressing decalcification of the tooth surface and exhibiting an immediate gloss imparting effect and whitening effect. Further, it is preferably 3.7 or more, more preferably 4.0 or more, particularly preferably 4.2 or more, and a gloss imparting effect and a whitening effect by removing the solid product. From the viewpoint of sufficiently achieving the above, it is 6.5 or less, preferably 6.0 or less, more preferably 5.5 or less, and particularly preferably 5.0 or less.
- the layer (B) has a pH of 3.5 to 6.5 when dissolved in water, preferably 3.7 to 6.0, and more preferably 4.0 to 5.5.
- the pH measurement method for the layer (B) is the same as the pH measurement method for the layer (A).
- a minimum amount of water capable of measuring pH is applied on the layer (B).
- water for example, 0.1 to 0.5 g, in which the layer (B) is dissolved is dropped onto the adhesive sheet of the present invention inclined at 45 degrees from the horizontal plane with the layer (B) facing up. Thereafter, the dropped water is promptly collected, and the pH is measured, for example, with a compact pH meter B-712 (Horiba, Ltd.).
- the water in which the layer (B) is dissolved is purified water, and includes distilled water or ion exchange water.
- the content of the component (b) in the layer (B) is a dry mass, preferably 5% by mass or more, more preferably, from the viewpoint of sufficiently exerting a fine solid product removing effect and a gloss imparting effect. It is 10 mass% or more, More preferably, it is 12 mass% or more.
- the content of the component (b) in the layer (B) is a dry mass, preferably 30% by mass or less, more preferably 28% by mass, from the viewpoint of suppressing tooth decalcification and from the viewpoint of taste and creaking. From the viewpoint of manufacturability, it is more preferably 20% by mass or less.
- the content of the component (b) in the layer (B) is preferably 5 to 30% by mass, more preferably 10 to 28% by mass, and further preferably 12 to 28% by dry mass. From the viewpoint of manufacturability, it is more preferably 12 to 20% by mass or more.
- what converted the whole quantity into the acid (acid conversion amount) is employ
- a pH adjusting agent As the pH adjusting agent, the gloss imparting effect and the whitening effect by the component (b) are not inhibited, and Insofar as deashing can be suppressed, inorganic acids such as hydrochloric acid and sulfuric acid, hydroxides such as sodium hydroxide, ammonia or aqueous ammonia, lower alkanolamines, basic amino acids such as arginine and lysine, etc. You may use individually by 1 type or in combination of 2 or more types. Of these, hydroxides such as sodium hydroxide are preferable.
- the layer (B) of the patch sheet of the present invention preferably further contains a gelling agent.
- a gelling agent include pullulan, sodium carboxymethylcellulose, hydroxyethylcellulose, carboxyvinyl polymer, xanthan gum, carrageenan, sodium alginate, hydroxypropylcellulose, hydroxypropylmethylcellulose, guar gum, and chondroitin sulfate sodium.
- nonionic polymers such as pullulan, hydroxyethylcellulose, guar gum, hydroxypropylcellulose, hydroxypropylmethylcellulose and the like may be contained.
- the thickness of the layer (B) is preferably 200 ⁇ m or less, more preferably 100 ⁇ m or less, and even more preferably 60 ⁇ m or less from the viewpoint of dissolving in an appropriate time and ensuring appropriate flexibility as a sheet. .
- the thickness of the layer (B) is preferably 5 ⁇ m or more, more preferably 10 ⁇ m or more, and even more preferably 15 ⁇ m or more, from the viewpoint of enabling enhancement of the whitening effect and gloss imparting action of the teeth by short-term use. And more preferably 20 ⁇ m or more.
- the thickness of the layer (B) is preferably 5 to 200 ⁇ m, more preferably 10 to 100 ⁇ m, still more preferably 15 to 60 ⁇ m, and still more preferably 20 to 60 ⁇ m.
- the layer (B) is preferably formed using a stock solution (B) containing the component (b).
- the layer (B) can be formed by forming a layer using the stock solution (B) and then performing a drying process.
- the content of the component (b) in the stock solution (B) is preferably 0.25% by mass or more, more preferably 1 from the viewpoint of sufficiently exhibiting the effect of removing a fine solid product and the effect of imparting gloss. .25% by mass or more, more preferably 2.5% by mass or more.
- the content of the component (b) in the stock solution (B) is preferably 12.5% by mass or less, more preferably 10% by mass or less, from the viewpoint of suppressing tooth decalcification and from the viewpoint of taste and creaking.
- the content of the component (b) in the stock solution (B) is preferably 0.25 mass% or more and 12.5 mass% or less, more preferably 1.25 to 10 mass%, further preferably. Is 2.5 to 7.5% by mass.
- the content of component (b) in the stock solution (B) is measured after neutralization with potassium hydroxide or sodium hydroxide, and the total amount is converted to an acid.
- the pH of the stock solution (B) is preferably 3.5 or more, more preferably 3.7 or more, and further preferably It is 4.0 or more, and more preferably 4.2 or more. From the same viewpoint, the pH of the stock solution (B) is preferably 6.5 or less, more preferably 6.0 or less, still more preferably 5.5 or less, particularly 5.0 or less. It is preferable to do.
- the pH in the stock solution is also a value at 25 ° C.
- the same gelling agent as in the case of forming the layer (A) from the viewpoint of film formability when the stock solution (A) has a high salt concentration. It is preferable to contain one or two or more nonionic polymers such as pullulan, hydroxyethylcellulose, guar gum, hydroxypropylcellulose, hydroxypropylmethylcellulose and the like.
- the layer (B) or the stock solution (B) may contain about 1 to 20 times the amount of a solvent such as water and / or ethanol in the same manner as the layer (A) or the stock solution (A).
- the stock solution (B) preferably forms a slurry using a solvent such as water and / or ethanol.
- the layer (B) is formed using a slurry stock solution (B) formed using a solvent such as water and / or ethanol, and then formed through a drying step, and the water content in the layer (B) is
- the layer (B) has a dry weight of 100 parts by mass, preferably 18 parts by mass or less, more preferably 15 parts by mass or less, and still more preferably 14 parts by mass or less. From the viewpoints of productivity and manufacturability, it is preferably 2 parts by mass or more, more preferably 3 parts by mass or more, and further preferably 5 parts by mass or more.
- the layer (B) is preferably one in which the content of the polyvalent cation is kept low from the viewpoint of preventing the component (b) from becoming insoluble or reducing the effect of removing the solid product.
- the content of the polyvalent cation is measured by an ICP emission analysis method (ICP emission analysis apparatus: Perkin Elmer Optima 5300 DV), and is less than 0.1-fold mol relative to the component (b) as the total polyvalent cation. 0.02 times mol or less is preferable and 0.01 times mol or less is more preferable.
- an agent mainly supplying a polyvalent cation such as a cationic antibacterial agent, a cationic surfactant, aluminum, calcium, magnesium, iron, zinc, tin or the like is not included in the layer (B), and is unavoidable. Except for the case where it is mixed in the layer, the layer (B) preferably does not contain a polyvalent cation.
- the content of the adsorbent in the layer (B) is 0.
- the content is preferably less than 005% by mass, more preferably 0.0005% by mass or less, and it is preferably not contained unless inevitably mixed.
- the layer (A) and the layer (B) may be dissolved first when the tooth sticking sheet of the present invention is stuck on the tooth, that is, the layer constituting the surface to be stuck on the tooth is a layer ( A) may be sufficient and a layer (B) may be sufficient.
- the patch sheet of the present invention is applied to a tooth, the tooth surface is first brought to an environment of pH 6.6 to 10.5, and then component (b) is taken to an environment of pH 3.5 to 6.5.
- the layer constituting the surface to be affixed to the tooth is preferably the layer (A).
- the component (a) is first allowed to sufficiently act in an environment of pH 6.6 to 10.5, and then the component (b) is pH 3.5 to 6.
- the layer constituting the surface to be attached to the tooth is preferably a layer (A).
- the patch sheet of the present invention is affixed to a tooth, first, the component (b) is allowed to act sufficiently in an environment of pH 3.5 to 6.5, and then the component (a) is pH 6.6 to 10.
- the layer constituting the surface to be attached to the tooth is preferably a layer (B).
- the pH of the layer (B) it is preferable to adjust the pH of the layer (B) so that the component (b) acts in an environment of pH 5.5 or more and 6.5 or less in order to prevent enamel decalcification on the tooth surface. That is, the layer (B) preferably has a pH of 5.5 to 6.5 when dissolved in water.
- the thickness ratio (A t : B t ) of the layer (A) and the layer (B) is preferably 1: 1 to 1:10, more preferably 1: 2 to 1: 9, Preferably it is 1: 3 to 1: 8.
- the layer (A) and the layer (B) exhibit a whitening effect on teeth by bringing different pH environments to each other when dissolved in water. It is preferable to maintain performance that can result in different pH environments. Thus, since the layer (A) and the layer (B) are water-soluble, each component contained in one layer is prevented from moving to the other layer, and the flexibility and usability of the sheet are reduced.
- the water content in the tooth sticking sheet of the present invention is preferably 18 parts by weight or less, more preferably 15 parts by weight or less, with respect to 100 parts by weight of the dry weight of the tooth sticking sheet. From the viewpoint of ensuring the flexibility, stickability and manufacturability of the sheet, it is preferably 2 parts by mass or more, more preferably 3 parts by mass or more, and 5 parts by mass. More preferably, it is the above.
- the solubility of the layer (A) and the layer (B) in water is preferably lower in the layer (B) than in the layer (A).
- the adhesion to the teeth is high, The tooth sticking sheet which has moderate rigidity and can be stuck even with wet hands can be obtained.
- the pasting sheet can be peeled off and pasted again.
- the adhesive sheet of the present invention has a layer (C) that does not collapse during dissolution of the layer (A) and / or the layer (B) as a layer other than the layer (A) and the layer (B). Is preferred. Especially, it is preferable to make a layer (C) into the layer which comprises the surface on the opposite side to the surface which affixes on a tooth.
- the layer (C) constitutes a surface opposite to the surface to be applied to the tooth
- the adhesive sheet of the present invention is applied to the tooth, the surface on the side where the layer of the sheet is applied to the tooth by saliva etc. It is possible to effectively prevent dissolution from the surface opposite to the surface, and the layer of the sheet can be preferentially dissolved from the surface to be attached to the tooth.
- the layer (C) that does not disintegrate during the dissolution of the layer (A) and / or the layer (B) is formed, for example, by containing the component (c) that is a hardly water-soluble substance. That is, in the present invention, the poorly water-soluble substance means that the layer (C) does not collapse during the dissolution of the layer (A) and / or the layer (B), and preferably the layer (A) and / Or disintegrates after dissolution of the layer (B). In addition, it does not collapse
- disintegrate means that disintegration advances and a layer (A) and / or a layer (B) will not be exposed.
- the component (c) is selected from cellulose acetate phthalate, polyvinyl acetate, ethyl cellulose, polymethyl methacrylate, methacryloylethyl betaine-methacrylate copolymer, methacrylic acid copolymer and aminoalkyl methacrylate copolymer.
- species or 2 or more types (co) polymer is mentioned.
- ethyl cellulose and cellulose acetate phthalate are preferable from the viewpoints of improving the followability with the layer (A) and the layer (B) in the layer (C), and having an immediate effect of imparting gloss and whitening.
- the content of the component (c) in the layer (C) effectively prevents dissolution of the layer from the surface opposite to the surface to be applied to the tooth, and constitutes the surface to be applied to the tooth.
- the dry mass is preferably 40% by mass or more, more preferably 50% by mass or more, and further preferably 60% by mass or more.
- the content of the component (c) in the layer (C) is dry mass, preferably 100% by mass or less, more preferably 90% by mass or less, and further preferably from the viewpoint of ease of use by the user. Is 80 mass% or less. Further, the content of the component (c) in the layer (C) is preferably 40 to 100% by mass, more preferably 50 to 90% by mass in terms of dry mass.
- the thickness of the layer (C) is a viewpoint that effectively prevents dissolution of the layer from the surface opposite to the surface to be affixed to the tooth, and preferentially dissolves from the layer constituting the surface to be affixed to the tooth Therefore, it is preferably 0.5 ⁇ m or more, more preferably 1 ⁇ m or more.
- the thickness of the layer (C) is preferably 40 ⁇ m or less, more preferably 10 ⁇ m or less, from the viewpoint of ease of use by the user.
- the adhesive sheet of the present invention can further have an intermediate layer (X) in addition to the layer (A), layer (B) and layer (C).
- an intermediate layer (X) can be formed between any of the layers (A), (B), and (C).
- the layers (A) and the layer (B) are separated at the time of production without mixing the layers (A) and (B).
- it becomes easy to improve the pH stability of the layers (A) and (B) and during use, one layer dissolves and contains the components contained in the mouth. After that, it becomes easy to dissolve the other layer and release the contained component into the oral cavity.
- nonionic polymers such as pullulan, hydroxyethyl cellulose, guar gum, hydroxypropyl cellulose, and the like are preferable from the viewpoint of enhancing the followability to other layers, and the layers (A) and ( From the viewpoint of enhancing the separability of B), one or more selected from cellulose acetate phthalate, polyvinyl acetate, ethyl cellulose, polymethyl methacrylate, methacryloylethyl betaine-methacrylate copolymer, methacrylic acid copolymer and aminoalkyl methacrylate copolymer Two or more (co) polymers and shellac are preferred.
- the water content of the intermediate layer (X) is 100 parts by weight of the dry weight of the intermediate layer (X). Is preferably 18 parts by mass, more preferably 15 parts by mass or less, and still more preferably 14 parts by mass or less, from the viewpoints of flexibility, adhesiveness and manufacturability of the adhesive sheet. It is preferably at least 3 parts by mass, more preferably at least 3 parts by mass, and even more preferably at least 5% by mass.
- the thickness of the intermediate layer (X) is, for example, from the viewpoint of separability between the layer (A) and the layer (B) and the improvement in pH stability of the layer (A) and the layer (B).
- it is preferably 1 ⁇ m or more, more preferably 5 ⁇ m or more, and further preferably 10 ⁇ m or more.
- the thickness of the intermediate layer (X) is preferably 100 ⁇ m or less, more preferably 50 ⁇ m or less, and even more preferably 30 ⁇ m or less.
- the thickness of the intermediate layer (X) is preferably 0.1 ⁇ m or more, more preferably 0.5 ⁇ m or more, and even more preferably 1 ⁇ m or more when using ethyl cellulose, shellac or the like.
- the thickness of the intermediate layer (X) is preferably 5 ⁇ m or less, more preferably 3 ⁇ m or less, from the viewpoint of ease of use by the user.
- the intermediate layer (X) preferably has a pH of 6.5 to 7.0.
- the adhesive sheet of the present invention has a total thickness of preferably 10 ⁇ m or more, more preferably from the viewpoint of enhancing the followability to the teeth when applied and from the viewpoint of providing an immediate effect of imparting gloss and whitening. It is 20 ⁇ m or more, more preferably 30 ⁇ m or more, preferably 1000 ⁇ m or less, more preferably 500 ⁇ m or less, and further preferably 100 ⁇ m or less.
- the adhesive sheet of the present invention may further contain, as appropriate, other components such as sweeteners, preservatives, bactericides, medicinal ingredients, pigments, dyes, and fragrances. As long as the effects of the present invention are not impaired, these other components can be contained in the layer (A), the layer (B), and an appropriate layer such as the layer (C) or the intermediate layer (X) as necessary.
- other components such as sweeteners, preservatives, bactericides, medicinal ingredients, pigments, dyes, and fragrances.
- the sticking sheet of the present invention imparts appropriate rigidity and flexibility to these layers.
- a plasticizer examples include sugar alcohols such as sorbitol, erythritol, mannitol, maltitol, and lactitol, polyhydric alcohols such as glycerol, propylene glycol, and polyethylene glycol. These may be used alone or in combination of two or more.
- the content of the plasticizer in each layer is preferably 0.01% by mass or more, more preferably 0.1% by mass or more, and still more preferably 1% by mass or more in terms of dry mass.
- the content of the plasticizer in each layer is preferably 50% by mass or less, more preferably 40% by mass or less, and further preferably 30% by mass or less in terms of dry mass.
- a sheet consisting of a single layer (A) after preparing a stock solution (A) containing component (a), a polyethylene terephthalate (PET) that has been subjected to a mold release treatment and the like while taking into account its thickness ) Apply the stock solution (A) on the film and dry. And the sheet
- seat which will comprise the surface of the side stuck on a tooth
- a PET film is placed in the lowermost layer, a sheet composed of a single layer constituting the surface to be affixed to the teeth thereon, and another sheet composed of a single layer are sequentially laminated, for example, a heated pressure device Crimp using the.
- the adhesive sheet of the present invention can be obtained by peeling off the lowermost PET film.
- a layer (A) comprises the surface of the side affixed on a tooth
- a PET film is made into a base material first, stock solution (A) is applied, and it is made to dry. Layer (A). Next, while forming the intermediate layer (X) on the layer (A) as necessary, the stock solution (B) is applied and dried to form the layer (B).
- the adhesive sheet of this invention can also be obtained by crimping
- the tooth sticking sheet of the present invention is preferably sealed in a moisture barrier packaging bag.
- packaging bags include multi-layered resin sheets whose innermost layer is polyethylene, and packaging bags in which three or four sides of the sheets are heat-sealed.
- packaging bags such as pillow bags and gusset bags A bag form can be used.
- the resin sheet of the multilayer structure which comprises this packaging bag equips an intermediate
- the adhesive sheet of the present invention can bring about an excellent gloss imparting effect and whitening effect on the tooth of the adherend only by being applied to the tooth.
- the time from immediately after applying the adhesive sheet to the tooth until the layer (A) and the layer (B) are completely dissolved in water is the component (a) and component (b) released to the tooth surface. )
- it is preferably 90 minutes or less, more preferably 60 minutes or less, and even more preferably 30 minutes or less.
- the patch sheet of the present invention is stuck on a tooth, it is preferably 1 minute or more, more preferably 5 minutes or more, and even more preferably 10 minutes or more, from the viewpoint of effectively exhibiting the gloss imparting effect and the whitening effect. is there.
- the tooth patch sheet of the present invention has an appropriate interval, specifically preferably 1 to 24 hours, more preferably 2 to 12 hours, preferably 2 times or more, More preferably 4 times or more, more preferably 6 times or more, when applied to the tooth, that is, by repeated use, the effect of the present invention can be further exerted, and damage to the enamel surface of the tooth is caused. It is possible to suppress teeth and to obtain teeth with more natural luster and gloss.
- the time until the layer (A) is completely dissolved in water is preferably 15 minutes from the viewpoint of maintaining the concentration of the component (a) released to the tooth surface and ease of use by the user. Or less, more preferably 10 minutes or less, and even more preferably 5 minutes or less. From the viewpoint of effectively exerting the gloss imparting effect and the whitening effect when the adhesive sheet of the present invention is applied to a tooth, it is preferably 0.1 minutes or more, more preferably 0.3 minutes or more, and still more preferably 0.5 minutes or longer.
- the time until the layer (B) is completely dissolved in water is preferably 75 minutes from the viewpoint of maintaining the concentration of the component (b) released to the tooth surface and ease of use by the user. Or less, more preferably 50 minutes or less, still more preferably 30 minutes or less, still more preferably 25 minutes or less, and even more preferably 15 minutes or less. From the viewpoint of effectively exhibiting the gloss imparting effect and the whitening effect when the patch sheet of the present invention is stuck on a tooth, it is preferably 1 minute or longer, more preferably 3 minutes or longer, and even more preferably 5 minutes or longer. is there.
- the time (dissolution time) until all of the layer (B) is dissolved in water is preferably longer than the time (dissolution time) until all of the layer (A) is dissolved in water, and the layers (A) and ( The ratio (A m : B m ) of the time until B) is completely dissolved in water (A m : B m ) is preferably 1: 1 to 1:15, more preferably 1: 1 to 1:10. More preferably, it is 1: 2 to 1: 9, and still more preferably 1: 3 to 1: 8.
- dissolution time for example, in the case of an adhesive sheet in which the layers (A) and (B) are laminated, 0.1 g on the layer (A) side.
- the time from application of water at a rate of / min to the release of the components contained in the layer (B) is defined as the time until the layer (A) is completely dissolved in water (dissolution time).
- the layer (B) is completely dissolved in water until the amount of the components contained in the layer (B) does not increase in water by applying water. Time (dissolution time).
- the amount of the component (a) contained in the layer (A) is determined by applying water to the layer (A) side.
- the time until it does not increase in water is defined as the time until all the layer (A) is dissolved in water (dissolution time).
- a tooth sticking sheet having: [2]
- the layer (A) contains one or more components (a) selected from alkylsulfuric acid, acylmethyl tauric acid, N-acyl sarcosine acid, orthophosphoric acid, condensed phosphoric acid and salts thereof.
- Component (a) is sodium lauryl sulfate, potassium lauryl sulfate, sodium lauroylmethyl taurate, potassium lauroylmethyl taurine, sodium lauroyl sarcosine, potassium lauroyl sarcosine, pyrophosphoric acid, orthophosphoric acid, tripolyphosphoric acid, tetrapolyphosphoric acid, metaphosphoric acid And one or more selected from these salts, preferably one or more selected from pyrophosphoric acid, tripolyphosphoric acid and their alkali metal salts, more preferably sodium pyrophosphate.
- the pH when the layer (A) is dissolved in water is 7.1 or more, preferably 7.5 or more, more preferably 8 or more, preferably 10 or less, preferably
- the tooth patch sheet according to any one of the above [1] to [3], which is 9.5 or less, more preferably 9 or less.
- the thickness of the layer (A) is 100 ⁇ m or less, preferably 50 ⁇ m or less, more preferably 20 ⁇ m or less, 1 ⁇ m or more, preferably 5 ⁇ m or more, and more preferably 7 ⁇ m or more.
- the tooth sticking sheet according to any one of [1] to [4] above.
- the layer (A) is formed using the stock solution (A), and the pH of the stock solution (A) is 6.6 or more, preferably 7.1 or more, more preferably 7.5. Or more, more preferably 8 or more, 10.5 or less, preferably 10 or less, more preferably 9.5 or less, and further preferably 9 or less. 5] Any one tooth sticking sheet.
- the content of the component (a) in the layer (A) is 1% by mass or more, preferably 2% by mass or more, more preferably 3% by mass or more, in terms of dry mass, 15 Any one of the above [1] to [6], which is not more than 10% by mass, preferably not more than 10% by mass, more preferably not more than 8.5% by mass, and still more preferably not more than 7% by mass. Tooth paste sheet.
- the content of the component (a) in the stock solution (A) is 0.025% by mass or more, preferably 0.125% by mass or more, more preferably 0.125% by mass or more.
- One or two layers (A) are further selected from pullulan, sodium carboxymethylcellulose, hydroxyethylcellulose, carboxyvinyl polymer, xanthan gum, carrageenan, sodium alginate, hydroxypropylcellulose, hydroxypropylmethylcellulose, guar gum, sodium chondroitin sulfate
- Component (b) is one or more selected from phytic acid, fumaric acid, malic acid, tartaric acid, glutaric acid, pyrophosphoric acid and hexametaphosphoric acid and their salts, preferably phytic acid or its
- the pH when the layer (B) is dissolved in water is 3.7 or more, preferably 4.0 or more, more preferably 4.2 or more, and 6.0 or less.
- the thickness of the layer (B) is 200 ⁇ m or less, preferably 100 ⁇ m or less, 5 ⁇ m or more, preferably 10 ⁇ m or more, more preferably 15 ⁇ m or more, and even more preferably 20 ⁇ m or more.
- the layer (B) is formed using the stock solution (B), and the pH of the stock solution (B) is 3.5 or more, preferably 3.7 or more, more preferably 4. 0 or more, more preferably 4.2 or more, 6.5 or less, preferably 6.0 or less, more preferably 5.5 or less, and further preferably 5.0 or less.
- a tooth patch sheet according to any one of [1] to [12] above.
- the content of the component (b) in the layer (B) is 5% by mass or more, preferably 10% by mass or more, more preferably 12% by mass or more, in terms of dry mass, 30
- the content of the component (b) in the stock solution (B) is 0.25% by mass or more, preferably 1.25% by mass or more, more preferably 2.5% by mass or more,
- the tooth patch sheet according to any one of the above [1] to [14] which is 12.5% by mass or less, preferably 10% by mass or less, and more preferably 7.5% by mass or less.
- the content of the polyvalent cation is less than 0.1 times mol, preferably 0.02 times mol or less, more preferably less than the component (b). Is a 0.01 times mole or less, and more preferably, it contains no polyvalent cation, and any one of the above [1] to [15].
- One or two layers (B) are further selected from pullulan, sodium carboxymethylcellulose, hydroxyethylcellulose, carboxyvinyl polymer, xanthan gum, carrageenan, sodium alginate, hydroxypropylcellulose, hydroxypropylmethylcellulose, guar gum, sodium chondroitin sulfate
- the dental patch sheet according to any one of the above [1] to [16], which contains a gelling agent that is a seed or more.
- the thickness ratio (A t : B t ) of the layer (A) and the layer (B) is preferably 1: 1 to 1:15, more preferably 1: 1 to 1:10. More preferably, it is 1: 2 to 1: 9, more preferably 1: 3 to 1: 8, any one of the above [1] to [17].
- the moisture content in the tooth sticking sheet is preferably 18 parts by weight or less, more preferably 15 parts by weight or less, and still more preferably 14 parts by weight or less with respect to 100 parts by weight of the dry weight of the tooth sticking sheet. Yes, preferably 2 parts by mass or more, more preferably 3 parts by mass or more, and still more preferably 5 parts by mass or more, [1] to [18] any one of [1] to [18].
- a layer (C) that does not collapse during dissolution of the layer (A) and / or the layer (B) and constitutes a surface opposite to the surface to be applied to the tooth
- the tooth paste sheet according to any one of the above [1] to [19].
- the tooth patch sheet according to [20] which is a seed or more (co) polymer, and is preferably ethyl cellulose or cellulose acetate phthalate.
- the time until the layer (A) and the layer (B) are completely dissolved in water immediately after being applied to the tooth is 90 minutes or less, preferably 60 minutes or less, more preferably 30 minutes or less.
- the ratio of time until all the layers (A) and (B) are dissolved in water (A m : B m ) is 1: 1 to 1:10, preferably 1: 2 to 1:
- the material of the intermediate layer (X) is selected from cellulose acetate phthalate, polyvinyl acetate, ethyl cellulose, polymethyl methacrylate, methacryloylethyl betaine-methacrylate copolymer, methacrylic acid copolymer and aminoalkyl methacrylate copolymer.
- the tooth paste sheet according to [27] above which is a seed or two or more (co) polymers and shellac.
- [30] Use of the tooth patch sheet according to any one of the above [1] to [29] for producing a tooth patch sheet.
- [32] Use of the tooth sticking sheet according to any one of the above [1] to [29] for whitening teeth.
- ⁇ b * was determined as the difference ⁇ (b * after sticking) ⁇ (b * before sticking) ⁇ between b * before sticking and 10 minutes after sticking.
- ⁇ b * that is, the larger the absolute value of ⁇ b *, the greater the whiteness.
- ⁇ Evaluation of tooth gloss> A method of measuring the intensity of reflected light from the image analysis using polarized light was used.
- the camera is a digital camera D2x (made by Nikon)
- the lens is Ai AF Micro Nikkor 105mm F2.8D
- the flash emission is Wireless Remote Speedlight SB-R200 (all made by Nikon). What was installed in combination was used.
- Photographing was carried out by placing a plastic polarizing plate (manufactured by Edmond) in front of the light emitting part of the speedlight and the lens so that the transmission axes intersected 30 degrees.
- the average brightness of the highlight portion was determined using Adobe Photoshop (manufactured by Adobe Systems).
- Luminance means that the larger the value, the higher the gloss.
- the difference in luminance (luminance after pasting ⁇ luminance before pasting) 10 minutes after pasting (before the above treatment) and after pasting (after the above 14 treatments) was obtained as ⁇ luminance. It was. The larger the value of ⁇ luminance, the higher the gloss.
- Measurement was performed by a volumetric titration method using a Karl Fischer moisture meter (trace moisture measuring device CA-200 type, Mitsubishi Chemical Analytech Co., Ltd.). The moisture content is measured for a sheet before being applied at 25 ° C., and when it is stored until sealed in a bag made of a resin sheet having an aluminum layer in the middle, it is stored for the sheet before being sealed in the bag. It was measured.
- the dissolution time is 25 ° C.
- Each sheet before lamination of each layer (layer (A), layer (B)) of 10 mm ⁇ 10 mm is immersed in water in which the entire sheet is immersed, and the sheet dissolves visually. It was time until it disappeared.
- water was continuously applied to the layer (A) side at a rate of 0.1 g / min, and the time for dissolution in water up to the layer (B) (dissolution time AB) was measured.
- the dissolution time shown was 11.5 minutes, the same as 11.5 minutes.
- Example 1 Each component was mixed to prepare a stock solution (A) while using ethanol or purified water as a solvent as appropriate so that the sheet (A) shown in Table 1 was obtained. Subsequently, after apply
- the obtained sheet (B) and sheet (A) were laminated, pressure-bonded using a pressure roll, and peeled from the PET film to obtain the sheet of Example 1. None of the stock solutions was mixed with a polyvalent cation, and the polyvalent cations such as magnesium, aluminum, and calcium in the stock solution were less than 0.02 moles compared to phytic acid as measured by IPC emission spectrometry.
- the pH of each layer was determined by dropping 0.3 g of water on a sheet inclined at 45 degrees from the horizontal surface with each layer facing upward, and then quickly collecting the dropped water to obtain a compact pH meter B-712 (stock) Measured by using HORIBA, Ltd.
- the extracted tooth is washed with ion-exchanged water, and the sheet (A) side surface of the laminated sheet material is applied so as to be in contact with the tooth. It was immersed in saliva for about 3 hours. This was treated as one time and repeated up to 14 times. Specifically, it is as follows. 1. At room temperature (25 ° C.), the extracted tooth was washed with ion-exchanged water, and the laminated sheet material was stuck so that the surface on which the sheet (A) was exposed was in contact with the tooth. 2.
- the surface to which the sheet material of the extracted tooth was affixed was contacted for 10 minutes to a 20 mm square sponge (manufactured by INOAC, continuous porous sponge MAPS K001) supplied with artificial saliva at a rate of 0.1 g / min. 3. After that, the remaining sheet debris was removed by light brushing and then immersed in artificial saliva for about 3 hours. 4). The above processes 1 to 3 were repeated 14 times.
- Example 2 In the same manner as in Example 1, the stock solution (A) and the stock solution (B) were prepared so that the sheet (A) and the sheet (B) shown in Table 1 were obtained, and these sheets (A) and (B) were prepared. Laminated and crimped. Subsequently, the undiluted
- Example 3 Furthermore, the sheet of Example 3 was obtained in the same manner as in Example 2 except that the stock solution (X) was used and the sheet (X) was laminated on one side of the sheet (A) and then the sheet (B) was further laminated. Using the obtained sheet, the above-described evaluation was performed on teeth (extracted teeth) that had been treated in the same manner as in Example 1. The results are shown in Table 1.
- Example 4 In the same manner as in Example 1, the sheet (B) and the sheet (A) were laminated and pressure-bonded to obtain each sheet shown in Table 1. Using the obtained sheet, the above-described evaluation was performed on teeth (extracted teeth) that had been treated in the same manner as in Example 1. The results are shown in Table 1.
- Examples 7 to 45 According to Examples 1 to 3, each sheet shown in Tables 4, 9, 12, 14, 17, and 19 to 23 was obtained using various stock solutions as appropriate, and then evaluated in the same manner as described above. All the sheets exhibited excellent tooth whitening effect and tooth gloss effect. According to Examples 1 to 3, the various sheets shown in Tables 3, 5 to 8, 10 to 11, 13, 15 to 16, and 18 can be obtained as appropriate using various stock solutions. These sheets can also exhibit excellent tooth whitening effects and tooth gloss effects.
- Example 46 In order to obtain the sheet (A) shown in Table 24, each component was mixed to prepare a stock solution (A) while appropriately using ethanol or purified water as a solvent. Next, the obtained undiluted solution (A) was applied onto a PET film, and then dried to obtain the water content shown in Table 25 to obtain a sheet (A). Similarly, in order to obtain the sheet (B) shown in Table 24, each component was mixed to prepare a stock solution (B) while appropriately using ethanol or purified water as a solvent. Subsequently, after apply
- the obtained sheet (B) and the sheet (A) are laminated, pressure-bonded using a pressure roll, peeled from the PET film, and then the side of the sheet (A) opposite to the surface on which the sheet (B) is laminated.
- the laminated sheet of Example 46 was obtained by applying the undiluted solution (C) shown in Table 24 on one side and drying the whole laminated sheet so that the moisture content in the entire sheet was as shown in Table 25. None of the stock solutions was mixed with a polyvalent cation, and the polyvalent cations such as magnesium, aluminum, and calcium in the stock solution were less than 0.02 moles compared to phytic acid as measured by IPC emission spectrometry.
- the pH of each layer was determined by dropping 0.3 g of water on a sheet inclined at 45 degrees from the horizontal surface with each layer facing upward, and then quickly collecting the dropped water to obtain a compact pH meter B-712 (stock) Measured by using HORIBA, Ltd.
- the innermost layer is a polyethylene-structured resin sheet (polyethylene terephthalate 12 ⁇ m / chlorinated polyethylene resin 15 ⁇ m / aluminum 7 ⁇ m / chlorinated polyethylene resin 20 ⁇ m / low-density polyethylene 60 ⁇ m). ) And sealed at 25 ° C. for 1 week.
- the pH of the sheet after storage was measured by the following method, and the change in pH with time was observed by Measurement Method 1 shown below. The results are shown in FIG.
- the moisture content shown in Table 25 is the moisture content before sealing the pillow bag.
- ⁇ Measurement method 1 of pH change with time The sheet taken out from the pillow bag was peeled off from the PET film, and then measured using a pH meter (AS-212, Horiba, Ltd.). Specifically, at 25 ° C., 0.1 g of ion-exchanged water is dropped on the sensor (electrode part) of the pH measuring device, and the sheet (10 mm ⁇ 10 mm) is positioned so that the layer (A) is positioned on the ion-exchanged water side. The pH value indicated by the pH meter was measured every 5 seconds with the time of placement as the start time.
- a silicone stent that covers the two teeth of the subject's right mandibular incisor and right mandibular canine is covered with a thin film, and the two teeth in a state where the silicone stent is attached to the tooth During this period, the electrode of the pH meter (custom pH antimony electrode SP-Sb-010, Chemical Equipment Co., Ltd.) is fixed so as to come out on the surface side of the silicone stent, and a sheet is attached to the surface of the silicone stent. did. The pH was measured every 100 milliseconds after the application.
- Example 47 to 49 Following the same procedure as in Example 46, stock solutions (A) to (C) shown in Table 24 were prepared, and dried to obtain the moisture content shown in Table 25 to obtain each laminated sheet. In addition, Examples 47 to 49 were produced while being sealed in a pillow bag before absorbing moisture after drying to prevent an increase in water content. Using the obtained laminated sheet, the change in pH was observed by the measuring method 1 in the same manner as in Example 46. The result is shown in FIG. Furthermore, the change in pH of the laminated sheet of Example 48 was observed by Measurement Method 2. The result is shown in FIG.
- Example 46 was superior in sheet flexibility and stickability.
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Abstract
Description
フィチン酸、ヘキサメタリン酸、25℃におけるpKaが4.5~7.0である有機酸及びこれらの塩から選ばれる1種又は2種以上の成分(b)を含有し、かつ水に溶解したときのpHが3.5以上6.5以下となる層(B)
を有する歯牙用貼付シート(以下、「本発明の貼付シート」ともいう)を提供するものである。
なお、本発明において、歯牙に付着又は堆積した微小汚れ又は固形生成物とは、歯の表面に生成される厚み数μm未満の固形物をいい、かかる固形物には、無機物主体又は有機物主体、或いはその両者が偏在した層状又は海島状等を呈する複合集合体の構造を有するものも含まれる。この微小な固形生成物は、主に唾液中のタンパク質やカルシウム、リン等の成分の沈着によって徐々に堆積して形成されていくと考えられ、加齢や唾液分泌の減少による口腔内環境の悪化等によって生成されやすくなり、通常のブラッシング処理では除去することが難しいものである。
なお、層(A)のpHの測定方法は、層(A)上にpH測定可能な最低限量の水を適用して測定する。具体的には、室温(25℃)にて、層(A)を上にして水平面から45度に傾斜させた本発明の貼付シート上に、層(A)が溶解する程度の水、例えば0.1~0.5gを滴下した後、滴下した水を速やかに回収し、例えばコンパクトpHメータB-712(株式会社堀場製作所)等によりpHを測定する。なお、層(A)を溶解させる水とは精製水であって、蒸留水又はイオン交換水をも含む意味である。
上記層(A)又は原液(A)には、上記成分の他、約1~20倍量の水及び/又はエタノール等の溶媒を含有させてもよく、なかでも原液(A)は、水及び/又はエタノール等の溶媒を用いてスラリーを形成することが好ましい。層(A)は、水及び/又はエタノール等の溶媒を用いて形成したスラリー状の原液(A)を用いて層状にした後、乾燥工程を経て形成され、層(A)中の含水量は、層(A)の乾燥重量100質量部に対して、好ましくは18質量部以下であり、より好ましくは15質量部以下であり、さらに好ましくは14質量部以下であり、シートの柔軟性、貼付性及び製造性の観点から2質量部以上であることが好ましく、3質量部以上であることがより好ましく、5質量部以上であることがさらに好ましい。
これらフィチン酸、ヘキサメタリン酸、及び25℃におけるpKaが4.5~7.0である有機酸の塩としては、ナトリウム塩、カリウム塩等のアルカリ金属塩が好ましい。
なお、層(B)のpHの測定方法は、層(A)のpH測定方法と同様に、室温(25℃)にて、層(B)上にpH測定可能な最低限量の水を適用して測定する。具体的には、層(B)を上にして水平面から45度に傾斜させた本発明の貼付シート上に、層(B)が溶解する程度の水、例えば0.1~0.5gを滴下した後、滴下した水を速やかに回収し、例えばコンパクトpHメータB-712(株式会社堀場製作所)等によりpHを測定する。なお、層(B)を溶解させる水とは精製水であって、蒸留水又はイオン交換水をも含む意味である。
上記層(B)又は原液(B)には、上記成分の他、層(A)又は原液(A)と同様、約1~20倍量の水及び/又はエタノール等の溶媒を含有させてもよく、なかでも原液(B)は、水及び/又はエタノール等の溶媒を用いてスラリーを形成することが好ましい。層(B)は、水及び/又はエタノール等の溶媒を用いて形成したスラリー状の原液(B)を用いて層状にした後、乾燥工程を経て形成し、層(B)中の含水量は、層(B)の乾燥重量100質量部に対して、好ましくは18質量部以下であり、より好ましくは15質量部以下であり、さらに好ましくは14質量部以下であり、シートの柔軟性、貼付性及び製造性の観点から2質量部以上であることが好ましく、3質量部以上であることがより好ましく、5質量部以上であることがさらに好ましい。
なお、層(A)と層(B)の厚みの比率(At:Bt)は、好ましくは1:1~1:10であり、より好ましくは1:2~1:9であり、さらに好ましくは1:3~1:8である。
また、例えば成分(a)を含有する層(A)と中間層(X)を積層した場合、層(A)側に水をかけて層(A)に含有される成分(a)の量が水中で増加しなくなるまでの時間を、層(A)が全て水に溶解するまでの時間(溶解時間)とする。
[1]水に溶解したときのpHが6.6以上10.5以下となる層(A)、並びに
フィチン酸、ヘキサメタリン酸、25℃におけるpKaが4.5~7.0である有機酸及びこれらの塩から選ばれる1種又は2種以上の成分(b)を含有し、かつ水に溶解したときのpHが4以上6.5以下になる層(B)
を有する歯牙用貼付シート。
[2]層(A)は、アルキル硫酸、アシルメチルタウリン酸、N‐アシルサルコシン酸、オルトリン酸、縮合リン酸及びこれらの塩から選ばれる1種又は2種以上の成分(a)を含有する上記[1]の歯牙用貼付シート。
[3]成分(a)が、ラウリル硫酸ナトリウム、ラウリル硫酸カリウム、ラウロイルメチルタウリンナトリウム、ラウロイルメチルタウリンカリウム、ラウロイルサルコシンナトリウム、ラウロイルサルコシンカリウム、ピロリン酸、オルトリン酸、トリポリリン酸、テトラポリリン酸、メタリン酸、及びこれらの塩から選ばれる1種又は2種以上であり、好ましくはピロリン酸、トリポリリン酸及びこれらのアルカリ金属塩から選ばれる1種又は2種以上であり、より好ましくはピロリン酸ナトリウムである上記[2]の歯牙用貼付シート。
[5]層(A)の厚みは、100μm以下であり、好ましくは50μm以下であり、より好ましくは20μm以下であり、1μm以上であり、好ましくは5μm以上であり、さらに好ましくは7μm以上である上記[1]~[4]いずれか1の歯牙用貼付シート。
[6]層(A)が原液(A)を用いて形成されてなり、原液(A)のpHが、6.6以上であり、好ましくは7.1以上であり、より好ましくは7.5以上であり、さらに好ましくは8以上であり、10.5以下であって、好ましくは10以下であり、より好ましくは9.5以下であり、さらに好ましくは9以下である上記[1]~[5]いずれか1の歯牙用貼付シート。
[7]層(A)中における成分(a)の含有量は、乾燥質量で、1質量%以上であって、好ましくは2質量%以上であり、より好ましくは3質量%以上であり、15質量%以下であって、好ましくは10質量%以下であり、より好ましくは8.5質量%以下であり、よりさらに好ましくは7質量%以下である上記[1]~[6]いずれか1の歯牙用貼付シート。
[8]原液(A)中における成分(a)の含有量は、0.025質量%以上であり、好ましくは0.125質質量%以上であり、より好ましくは0.125質質量%以上であり、7.5質量%以下であり、好ましくは5質量%以下であり、より好ましくは2.5質量%以下である上記[1]~[7]いずれか1の歯牙用貼付シート。
[9]層(A)が、さらにプルラン、カルボキシメチルセルロースナトリウム、ヒドロキシエチルセルロース、カルボキシビニルポリマー、キサンタンガム、カラギーナン、アルギン酸ナトリウム、ヒドロキシプロピルセルロース、ヒドロキシプロピルメチルセルロース、グアガム、コンドロイチン硫酸ナトリウムから選ばれる1種又は2種以上であるゲル化剤を含有する上記[1]~[8]いずれか1の歯牙用貼付シート。
[11]層(B)が水に溶解したときのpHが、3.7以上であって、好ましくは4.0以上であり、より好ましくは4.2以上であり、6.0以下であって、好ましくは5.5以下であり、より好ましくは5.0以下である上記[1]~[10]いずれか1の歯牙用貼付シート。
[12]層(B)の厚みは、200μm以下であり、好ましくは100μm以下であり、5μm以上であり、好ましくは10μm以上であり、さらに好ましくは15μm以上であり、よりさらに好ましくは20μm以上である上記[1]~[11]いずれか1の歯牙用貼付シート。
[14]層(B)中における成分(b)の含有量は、乾燥質量で、5質量%以上であって、好ましくは10質量%以上であり、より好ましくは12質量%以上であり、30質量%以下であって、好ましくは28質量%以下であり、より好ましくは20質量%以下である上記[1]~[13]いずれか1の歯牙用貼付シート。
[15]原液(B)中における成分(b)の含有量は、0.25質量%以上であり、好ましくは1.25質量%以上であり、より好ましくは2.5質量%以上であり、12.5質量%以下であり、好ましくは10質量%以下であり、より好ましくは7.5質量%以下である上記[1]~[14]いずれか1の歯牙用貼付シート。
[16]層(B)又は原液(B)は、多価カチオンの含有量が成分(b)に対して0.1倍モル未満であり、好ましくは0.02倍モル以下であり、さらに好ましくは0.01倍モル以下であり、よりさらに好ましくは多価カチオンを含有しない上記[1]~[15]いずれか1の歯牙用貼付シート。
[17]層(B)が、さらにプルラン、カルボキシメチルセルロースナトリウム、ヒドロキシエチルセルロース、カルボキシビニルポリマー、キサンタンガム、カラギーナン、アルギン酸ナトリウム、ヒドロキシプロピルセルロース、ヒドロキシプロピルメチルセルロース、グアガム、コンドロイチン硫酸ナトリウムから選ばれる1種又は2種以上であるゲル化剤を含有する上記[1]~[16]いずれか1の歯牙用貼付シート。
[19]歯牙貼付シートにおける水分量が、歯牙貼付シートの乾燥質量100質量部に対し、好ましくは18質量部以下であり、より好ましくは15質量部以下であり、さらに好ましくは14質量部以下であり、好ましくは2質量部以上であり、より好ましくは3質量部以上であり、さらに好ましくは5質量部以上である上記[1]~[18]いずれか1の歯牙用貼付シート。
[20]さらに、前記層(A)及び/又は前記層(B)の溶解中に、崩壊してしまわず、かつ歯牙に貼付する側の面と反対側の面を構成する層(C)を有する上記[1]~[19]いずれか1の歯牙用貼付シート。
[21]成分(c)が、セルロースアセテートフタレート、ポリビニルアセテート、エチルセルロース、ポリメチルメタクリレート、メタクリロイルエチルベタイン-メタクリレート共重合体、メタクリル酸共重合体及びアミノアルキルメタクリレート共重合体から選ばれる1種又は2種以上の(共)重合体であり、好ましくは、エチルセルロース又はセルロースアセテートフタレートである上記[20]の歯牙用貼付シート。
[23]層(A)が、歯牙に貼付する側の面を構成する上記[1]~[22]いずれか1の歯牙用貼付シート。
[24]層(B)が、歯牙に貼付する側の面を構成する上記[1]~[22]いずれか1の歯牙用貼付シート。
[25]歯牙に貼付した直後から、層(A)及び層(B)が全て水に溶解するまでの時間が、90分以下であり、好ましくは60分以下であり、より好ましくは30分以下であり、1分以上であり、好ましくは5分以上であり、より好ましくは10分以上である上記[1]~[24]いずれか1の歯牙用貼付シート。
[26]層(A)と層(B)の全て水に溶解するまでの時間の比率(Am:Bm)が、1:1~1:10であり、好ましくは1:2~1:9であり、より好ましくは1:3~1:8である上記[1]~[25]いずれか1の歯牙用貼付シート。
[27]さらに、中間層(X)を有する上記[1]~[26]いずれか1の歯牙用貼付シート。
[28]中間層(X)の材質が、セルロースアセテートフタレート、ポリビニルアセテート、エチルセルロース、ポリメチルメタクリレート、メタクリロイルエチルベタイン-メタクリレート共重合体、メタクリル酸共重合体及びアミノアルキルメタクリレート共重合体から選ばれる1種又は2種以上の(共)重合体、並びにセラックである上記[27]の歯牙用貼付シート。
[29]包装袋に密封されてなる上記[1]~[27]いずれか1の歯牙用貼付シート。
[30]歯牙用貼付シート製造のための上記[1]~[29]いずれか1の歯牙用貼付シートの使用。
[31]歯に適用し唾液による溶解により層(A)と層(B)を歯に適用するための上記[1]~[29]いずれか1の歯牙用貼付シート。
[32]歯の美白のための上記[1]~[29]いずれか1の歯牙用貼付シートの使用。
[33]歯に光沢を付与するための上記[1]~[29]いずれか1の歯牙用貼付シートの使用。
なお、各測定及び評価については、下記方法及び基準にしたがって行った。
下記の方法にしたがってb*を測定することにより、上記処理前と上記処理後の歯(抜去歯)の白さを評価した。
具体的には、デジタルカメラD1x(ニコン製)とレンズはAi AFマイクロ・ニッコール105mm F2.8D、ストロボ発光はワイヤレス・リモート・スピードライトSB-R200(いずれもニコン製)を組み合せて設置したものを用いた。撮影された画像をAdobe Photoshop(アドビシステムズ製)を用いてL*a*b*表色系で表し、得られたシートを貼付する前のb*の値と貼付後10分経過した後のb*を測定した。次いで、これらシート貼付前と貼付後10分経過後のb*の差{(貼付後のb*)-(貼付前のb*)}としてΔb*を求めた。Δb*が小さいほど、すなわちΔb*の絶対値が大きいほど白さが増したことを意味する。
偏光を利用した画像解析から表面反射光強度を測定する方法を用いた。評価用画像を撮影する装置として、カメラはデジタル一カメラD2x(ニコン製)、レンズはAi AFマイクロ・ニッコール105mm F2.8D、ストロボ発光はワイヤレス・リモート・スピードライトSB-R200(いずれもニコン製)を組み合せて設置したものを用いた。スピードライトの発光部及びレンズの前にプラスチック偏光板(エドモンド製)を透過軸が30度交差するように配置して撮影した。撮影画像はAdobe Photoshop(アドビシステムズ製)を用いてハイライト部分の平均輝度を求めた。輝度は数値が大きいほど光沢が高いことを意味する。得られたシートを貼付する前(上記処理前)と貼付後(上記14回の処理後)10分経過した後の輝度の差(貼付後の輝度-貼付前の輝度)を、Δ輝度として求めた。Δ輝度の数値が大きいほど光沢が増したことを意味する。
カールフィッシャー水分計(微量水分測定装置CA―200型、株式会社三菱化学アナリテック)を用い、容量滴定方式により測定を行った。なお、水分量は、25℃において貼付する前のシートについて測定し、中間にアルミニウム層を有する樹脂シートからなる袋に密封して貼付するまで保存する場合には、袋に密封する前のシートについて測定した。
溶解時間は、25℃において、10mm×10mmの各層(層(A)、層(B))の積層する前の各々のシートについて、シート全体が浸漬する水に浸漬し、目視でシートが溶解してなくなるまでの時間とした。なお、実施例1についてのみ、層(A)側に0.1g/minの速度で水をかけ続け、層(B)まで水に溶解する時間(溶解時間AB)を測定したところ、表1に示す溶解時間11.5分と同じ11.5分であった。
表1に示すシート(A)が得られるよう、適宜エタノールや精製水を溶媒として用いつつ、各成分を混合して原液(A)を調製した。次いで、得られた原液(A)をPETフィルム上に塗布した後、乾燥してシート(A)を得た。同様に、表1に示すシート(B)が得られるよう、適宜エタノールや精製水を溶媒として用いつつ、各成分を混合して原液(B)を調製した。次いで、得られた原液(B)をPETフィルム上に塗布した後、乾燥し、PETフィルムから剥離してシート(B)を得た。
得られたシート(B)とシート(A)を積層し、加圧ロールを用いて圧着し、PETフィルムから剥離することによって実施例1のシートを得た。いずれの原液にも多価カチオンを配合せず、原液中のマグネシウム、アルミニウム、カルシウム等の多価カチオンはIPC発光分析法で測定してフィチン酸に対して0.02倍モル未満であった。
なお、各層のpHは、各層を上にして水平面から45度に傾斜させたシート上に、水0.3gを滴下した後、滴下した水を速やかに回収し、コンパクトpHメータB-712(株式会社堀場製作所)を用いることによって測定した。
具体的には、下記のとおりである。
1.室温(25℃)にて、抜去歯をイオン交換水につけて洗浄し、積層したシート材のシート(A)が露出している側の面を歯に接触するように貼付した。
2.0.1g/minの速度で人工唾液を供給した20mm角のスポンジ(INOAC社製 連通多孔質スポンジ MAPS K001)に当該抜去歯のシート材を貼付した面を10分間接触させた。
3.その後、残ったシートの残骸を軽いブラッシングで除去した後に人工唾液に約3時間浸漬。
4.上記1~3の処理を14回繰り返した。
得られたシートを用い、処理後の歯(抜去歯)について、上記評価を行った。結果を表1に示す。
実施例1と同様にして、表1に示すシート(A)及びシート(B)が得られるよう、原液(A)及び原液(B)を調製し、これらシート(A)及びシート(B)を積層圧着した。次いで、シート(B)の、シート(A)を積層した反対側の片面に原液(C)を塗布して、表1に示すシート(C)を積層した。得られたシートを乾燥して実施例2のシートを得た。
得られたシートを用い、実施例1と同様の処理を行った歯(抜去歯)について、上記評価を行った。結果を表1に示す。
さらに原液(X)を用い、シート(A)の片面にシート(X)を積層した後、さらにシート(B)を積層した以外、実施例2と同様にして実施例3のシートを得た。
得られたシートを用い、実施例1と同様の処理を行った歯(抜去歯)について、上記評価を行った。結果を表1に示す。
実施例1と同様にして、シート(B)及びシート(A)を積層圧着し、表1に示す各シートを得た。
得られたシートを用い、実施例1と同様の処理を行った歯(抜去歯)について、上記評価を行った。結果を表1に示す。
表2にしたがって、各原液を用いてPETフィルム上に塗布した後、乾燥させ、PETフィルムから剥離することによって単層からなる各シートを製造した。
得られた各シートを用い、実施例1と同様の処理を行った歯(抜去歯)について、上記評価を行った。結果を表2に示す。
実施例1~3に準じ、適宜各種原液を用いて表4、9、12、14、17、19~23に示す各シートを得た後、適宜上記と同様にして各評価を行った。いずれのシートも優れた歯の美白効果及び歯の光沢効果を発揮するものであった。
実施例1~3に準じ、適宜各種原液を用いて表3、5~8、10~11、13、15~16、18に示す各シートを得ることができる。これらのシートについても優れた歯の美白効果及び歯の光沢効果を発揮することができる。
表24に示すシート(A)が得られるよう、適宜エタノールや精製水を溶媒として用いつつ、各成分を混合して原液(A)を調製した。次いで、得られた原液(A)をPETフィルム上に塗布した後、表25に示す水分量となるように乾燥してシート(A)を得た。同様に、表24に示すシート(B)が得られるよう、適宜エタノールや精製水を溶媒として用いつつ、各成分を混合して原液(B)を調製した。次いで、得られた原液(B)をPETフィルム上に塗布した後、表25に示す水分量となるように乾燥し、PETフィルムから剥離してシート(B)を得た。
なお、各層のpHは、各層を上にして水平面から45度に傾斜させたシート上に、水0.3gを滴下した後、滴下した水を速やかに回収し、コンパクトpHメータB-712(株式会社堀場製作所)を用いることによって測定した。
得られた積層シートを、PETフィルムにて支持してから、最内層がポリエチレンの多層構造の樹脂シート(ポリエチレンテレフタレート12μm/塩素化ポリエチレン樹脂15μm/アルミニウム7μm/塩素化ポリエチレン樹脂20μm/低密度ポリエチレン60μm)からなるピロー袋に密封し、25℃1週間保存した。
保存後におけるシートのpHを下記方法により測定し、pHの経時変化を次に示す測定方法1により観察した。
結果を図1に示す。なお、表25に示す水分量は、ピロー袋に密封する前の水分量である。
ピロー袋から取り出したシートを、PETフィルムから剥離した後に、pH測定器(AS―212、株式会社堀場製作所)を用いて測定した。具体的には、25℃において、pH測定器のセンサ(電極部)上にイオン交換水0.1gを滴下し、さらにシート10mm×10mmをイオン交換水の側に層(A)が位置するように載置し、載置した時点を開始時刻として、5秒経過するごとにpH測定器に示されるpHの値を測定した。
《pHの経時変化の測定方法2》
ピロー袋から取り出したシートを、PETフィルムから剥離した後に、pH測定器(PH―201Z ポータブルpHメーター、ケミカル機器株式会社)の電極を固定した口腔内の歯牙に貼付してpHを測定した。具体的には、被験者の右側下顎側切歯と右側下顎犬歯の並んだ2本の歯を薄膜で覆うシリコーン製のステントを作成し、シリコーン製のステントを歯に装着した状態における2本の歯の間に、pH測定器の電極(特注pHアンチモン電極 SP―Sb―010、ケミカル機器株式会社)をシリコーン製のステントの表面側に出るように固定し、シリコーン製のステントの表面にシートを貼付した。貼付した直後から100ミリ秒経過するごとにpHを測定した。
実施例46と同様の手順にしたがい、表24に示す原液(A)~(C)を調製し、表25に示す水分量となるように乾燥させて各積層シートを得た。なお、実施例47~49は、乾燥後に吸湿する前にピロー袋に密封して水分量の増加を防止しながら製造した。
得られた積層シートを用い、実施例46と同様にしてpHの変化を測定方法1により観察した。その結果を図1に示す。
さらに、測定方法2により実施例48の積層シートのpHの変化を観察した。その結果を図2に示す。
Claims (15)
- 水に溶解したときのpHが6.6以上10.5以下となる層(A)、並びに
フィチン酸、ヘキサメタリン酸、25℃におけるpKaが4.5~7.0である有機酸及びこれらの塩から選ばれる1種又は2種以上の成分(b)を含有し、かつ水に溶解したときのpHが3.5以上6.5以下になる層(B)
を有する歯牙用貼付シート。 - 層(B)の全て水に溶解する時間が、層(A)の全て水に溶解する時間より長い請求項1に記載の歯牙用貼付シート。
- 層(A)が、アルキル硫酸、アシルメチルタウリン酸、N‐アシルサルコシン酸、オルトリン酸、縮合リン酸及びこれらの塩から選ばれる1種又は2種以上の成分(a)を含有する請求項1又は2に記載の歯牙用貼付シート。
- 層(A)が、歯牙に貼付する側の面を構成する請求項1~3のいずれか1項に記載の歯牙用貼付シート。
- 層(A)及び層(B)の厚みの比率(At:Bt)が、1:1~1:10である請求項1~4のいずれか1項に記載の歯牙用貼付シート。
- さらに、前記層(A)及び/又は前記層(B)の溶解中に、崩壊してしまわず、かつ歯牙に貼付する側の面と反対側の面を構成する層(C)を有する請求項1~5のいずれか1項に記載の歯牙用貼付シート。
- 層(C)が、セルロースアセテートフタレート、ポリビニルアセテート、エチルセルロース、ポリメチルメタクリレート、メタクリロイルエチルベタイン-メタクリレート共重合体、メタクリル酸共重合体及びアミノアルキルメタクリレート共重合体から選ばれる1種又は2種以上の(共)重合体である成分(c)を含有する請求項6に記載の歯牙用貼付シート。
- 総厚みが、10μm以上1000μm以下である請求項1~6のいずれか1項に記載の歯牙用貼付シート。
- 歯牙に貼付した直後から、層(A)及び層(B)が全て水に溶解するまでの時間が、1分以上90分以下である請求項1~7のいずれか1項に記載の歯牙用貼付シート。
- 層(A)と層(B)の全て水に溶解するまでの時間の比率(Am:Bm)が、1:1~1:15である請求項1~8のいずれか1項に記載の歯牙用貼付シート。
- 層(A)と層(B)との間に中間層(X)を有する請求項1~9のいずれか1項に記載の歯牙用貼付シート
- 層(B)が、歯牙に貼付する側の面を構成する請求項1又は請求項3~10のいずれか1項に記載の歯牙用貼付シート。
- 層(A)がpH6.6以上10.5以下の原液(A)を用いて形成されてなり、かつ層(B)がpH3.5以上6.5以下の原液(B)を用いて形成されてなる請求項1~11のいずれか1項に記載の歯牙用貼付シート。
- 層(A)中における成分(a)の含有量が乾燥重量で1質量%以上15質量%以下であり、層(B)中における成分(b)の含有量が乾燥重量で5質量%以上30質量%以下である請求項1~13のいずれか1項に記載の歯牙用貼付シート。
- 歯牙用貼付シートにおける水分量が、歯牙貼付シートの乾燥質量100質量部に対して18質量部以下であり、かつ包装袋に密封されてなる請求項1~14のいずれか1項に記載の歯牙用貼付シート。
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JP7456752B2 (ja) | 2019-11-14 | 2024-03-27 | 花王株式会社 | 唾液溶解性歯牙貼付シート |
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CN105616173A (zh) * | 2016-01-26 | 2016-06-01 | 浙江浙北药业有限公司 | 一种美白牙贴及其制备方法 |
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RU2663585C2 (ru) | 2018-08-07 |
US20150289961A1 (en) | 2015-10-15 |
CN104755070B (zh) | 2017-12-29 |
TW201427698A (zh) | 2014-07-16 |
RU2015120280A (ru) | 2016-12-20 |
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