Aqueous oral care solutions, methods, kits, and tooth surfaces having a coating derived from an oral care solution

By using silver cations and thiocyanate anions in an aqueous oral care solution to form Ag-rich and CaF2-rich layers, the problems of inconvenient operation and uneven fluoride intake in existing tooth fluoride treatment methods are solved, achieving rapid and effective fluoride protection and caries prevention.

CN113038921BActive Publication Date: 2026-03-20SOLVENTUM INTELLECTUAL PROPERTIES CO
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2019-08-27
Publication Date
2026-03-20

AI Technical Summary

Technical Problem

Existing methods for fluoride treatment of teeth suffer from inconvenience, uneven fluoride intake, and poor patient comfort. In particular, fluoride varnishes need to be maintained for a long time and can easily cause unpleasant sensations, while fluoride gels/foams need to be suctioned out and cannot provide effective fluoride protection in a short period of time.

Method used

An aqueous oral care solution is provided, comprising silver cations, thiocyanate anions, and fluoride anions, forming an Ag-rich layer and a CaF2-rich layer, providing fluoride protection through short-time contact, and forming a precipitate in the oral environment to enhance the effect.

Benefits of technology

It achieves a fluoride protection effect similar to a coating in a short time, reducing the incidence of tooth decay and tooth sensitivity, while avoiding unnecessary fluoride intake and operational complexity.

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Abstract

The present disclosure relates to aqueous oral care solutions, kits comprising such solutions, methods of making such solutions, methods of using such solutions (e.g., methods of providing fluoride to a tooth surface of a patient), and tooth surfaces having a coating derived from an aqueous oral care solution, wherein the oral care solution comprises: silver cations; thiocyanate anions provided by a source of thiocyanate, the source of thiocyanate comprising Ca(SCN)2; fluoride anions; and water; wherein the molar ratio of silver ions to thiocyanate ions is at most 0.40:1, and the water is at most 57 wt.%, based on the total weight of the solution.
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Description

BACKGROUND

[0001] Fluoride treatments involve the application of fluoride to the surface of the teeth, while forming fluorapatite and calcium fluoride.

[0002] There are currently two main office fluoride treatment methods in use. One treatment method uses fluoride gel / foam in a dental tray. This method requires several grams of fluoride gel to be stored in a dental tray, which is then placed over the teeth in the patient's mouth. The tray is left in the mouth while the gel / foam is in contact with the teeth for 1 to 4 minutes. The gel / foam formulation is an aqueous system containing 2% sodium fluoride. This material requires the use of suction to draw excess gel from the mouth to avoid ingestion of an unnecessary amount of fluoride.

[0003] Another treatment method is dental fluoride varnish. Most fluoride varnishes on the market are rosin / ethanol based formulations with hydrophobic properties. The varnish is painted on the teeth and left in place for several hours to allow fluoride to be released from the composition. Typically, fluoride varnish is used by dentists for office fluoride treatment. Most dental fluoride varnishes contain 5% sodium fluoride. The dosage of varnish is about 0.5 grams. Compared to fluoride gel / foam, dental varnish places much less amount of fluoride into the patient's mouth. Therefore, there is less fluoride ingestion in the case of fluoride varnish. Additionally, fluoride varnishes are easier to apply because they are simply painted on the patient's teeth; however, fluoride varnish treatment is more labor intensive than gel treatment and fluoride varnish treatment leaves the patient with an unpleasant "dirty teeth" feeling.

[0004] It would be desirable to have a composition that is as simple to apply to the teeth as a varnish and that can function in as short a time period as a gel / foam formulation. BRIEF DESCRIPTION OF DRAWINGS

[0005] Figure 1 SEM for the material of Comparative Example CE-16, which is an untreated control dentin surface.

[0006] Figure 2 SEM for the material of Comparative Example CE-17, which is a dentin surface treated with the solution of Comparative Example CE-10.

[0007] Figure 3 SEM for the material of Example Ex-27, which is a dentin surface treated with the solution of Example Ex-7. SUMMARY

[0008] The present disclosure provides aqueous oral care solutions, methods of making such solutions, methods of treatment using such solutions (e.g., methods of providing fluoride to the surface of a patient's teeth), kits, and treated teeth.

[0009] Such solutions can be used as a clinic oral care solution (e.g., as a fluoride treatment solution). If desired, they can be formulated as a solution that can be painted on the surface of the teeth. They can provide fluoride efficacy similar to that of a varnish in a shorter period of time in a gel / foam formulation.

[0010] In one embodiment, the present disclosure provides an aqueous oral care solution comprising: silver cations; thiocyanate anions provided by a thiocyanate source, the thiocyanate source comprising Ca(SCN)2; fluoride anions; and water in an amount of up to 57 wt.%, based on the total weight of the solution; wherein the molar ratio of silver ions to thiocyanate ions is up to 0.40:1.

[0011] In certain embodiments of such solutions, the aqueous oral care solution comprises: 12.5 wt.% to 20.2 wt.% silver cations; and 1.0 wt.% to 6.0 wt.% (preferably 2.2 wt.% to 3.5 wt.%) fluoride anions; wherein the weight percentages are based on the total weight of the solution; wherein the molar ratio of silver ions to thiocyanate ions is at least 0.10:1 and up to 0.40:1; and wherein the oral care solution forms a precipitate (e.g., an Ag-rich layer and a CaF2-rich layer) upon contact with additional water or saliva.

[0012] In another embodiment, the present disclosure provides a method of providing fluoride to a tooth surface of a patient. The method involves applying to the tooth surface of the patient an aqueous oral care solution as disclosed herein.

[0013] In another embodiment, the present disclosure provides a method of reducing the incidence of dental caries in a patient in need thereof. The method involves applying to the tooth surface of the patient an aqueous oral care solution as disclosed herein.

[0014] In another embodiment, the present disclosure provides a method of reducing dentin sensitivity and / or root sensitivity (e.g., during a caries cavity treatment and / or on an exposed root) in a patient in need thereof. The method includes applying to the tooth surface of the patient an aqueous oral care solution as disclosed herein.

[0015] In another embodiment, the present disclosure provides a kit comprising an aqueous oral care solution as described herein and an applicator device.

[0016] In another embodiment, the present disclosure provides a tooth comprising a tooth surface having dentin tubules and a coating disposed on the tooth surface, wherein the coating comprises silver-rich particles and a CaF2-rich layer that occludes at least a portion of the dentin tubules.

[0017] The terms "comprise" and variations thereof, when appearing in the specification and claims, do not have a limiting meaning. Such terms will be understood to imply the inclusion of the stated steps or elements or groups of steps or elements but not the exclusion of any other steps or elements or groups of steps or elements. By "consisting of" is meant including, and limited to, whatever follows the phrase "consisting of." Thus, the phrase "consisting of" indicates that the listed elements are required or mandatory, and that no other elements can be present. By "consisting essentially of" is meant including any elements listed after the phrase, and limited to other elements that do not materially affect or substantially alter the activity or action of the listed elements. Thus, the phrase "consisting essentially of' indicates that the listed elements are required or mandatory, but that other elements are optional and can or can not be present depending upon whether or not they materially affect or substantially alter the activity or action of the listed elements.

[0018] The words "preferred" and "preferably" refer to embodiments of the disclosure that can provide certain benefits under certain circumstances. However, other embodiments can also be preferred under the same or other circumstances. Additionally, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, and is not intended to exclude those other embodiments from the scope of the disclosure.

[0019] In this application, the terms "a," "an," "the," and "said" are not limited to refer only to singular forms, but include plural forms unless the content clearly dictates otherwise. The terms "a," "an," "the," and "said" are used interchangeably with the phrase "at least one" and "one or more." The phrases "at least one of" and "comprising at least one of" followed by a list of items mean that any of the items can be present, along with zero or more of the other listed items.

[0020] The term "or" is generally employed in its ordinary sense, including the possible

[0021] The term "and / or" means one or all of the listed elements or a combination of any two or more of the listed elements.

[0022] Also herein, all numerical values are assumed to be modified by the term "about" and, where appropriate, preferably by the term "exactly". As used herein, the term "about" with reference to a measured quantity, refers to a deviation of that quantity, which is reasonably carelessly made by one of ordinary skill in the art, commensurate with the exactness of the measurement devices used and the objectives of the measurement. Herein, "up to" a number (e.g., up to 50) includes the number (e.g., 50).

[0023] Also herein, numerical ranges expressed in terms of "from" and "to" include all numbers included within the range limits (e.g., from 1 to 50 includes 1, 1.5, 2, 2.75, 3, 3.80, 4, 5, etc.).

[0024] References throughout this specification to "one implementation", "an implementation", "certain implementations" or "some implementations" and the like, mean that a particular feature, configuration, composition or characteristic described in connection with the implementation is included in at least one implementation of the disclosure. Thus, appearances of such phrases in various places throughout this specification are not necessarily intended to refer to the same implementation of the disclosure. Furthermore, a particular feature, configuration, composition or characteristic can be combined in any suitable manner in one or more implementations.

[0025] The foregoing summary of the disclosure is not intended to describe every disclosed implementation or implementation of the disclosure. The following description more particularly describes illustrative implementations. Throughout this application, guidance is provided by way of example in a number of embodiments. In each instance, the listed list is used only as representative of a group and should not be construed as an exclusive list. DETAILED DESCRIPTION

[0026] The present disclosure provides aqueous oral care solutions. The present disclosure also provides methods of providing fluoride to a tooth surface of a patient in need of fluoride to a tooth surface of a patient, methods of reducing the incidence of caries, and methods of reducing dentin sensitivity and / or root sensitivity (e.g., during caries treatment and / or on exposed roots). Such methods involve applying an aqueous oral care solution (e.g., a fluoride treatment solution) as described herein to a tooth surface of a patient.

[0027] In certain implementations, applying an aqueous oral care solution includes painting the oral care solution on a tooth surface of a patient.

[0028] In certain implementations, applying an aqueous oral care solution includes dispensing the oral care solution into a dental tray and attaching the tray with the oral care solution therein to a tooth surface of a patient. In certain implementations, the dental tray includes an orthodontic aligner treatment tray.

[0029] In certain embodiments, the aqueous oral care solution comprises: silver cations; thiocyanate anions provided by a thiocyanate source comprising Ca(SCN)2; fluoride anions; and water.

[0030] In certain embodiments, silver ions (also referred to herein as silver cations) are present in an amount of at least 12.5 weight percent (wt%), at least 13.0 wt%, at least 14.0 wt%, or at least 15.0 wt%, where the weight percent is based on the total weight of the solution. In certain embodiments, silver cations are present in an amount of at most 20.2 wt%, at most 20.0 wt%, at most 19.0 wt%, or at most 18.0 wt%, where the weight percent is based on the total weight of the solution.

[0031] In certain embodiments, the silver cation source is selected from the group consisting of silver fluoride, silver chloride, silver nitrate, silver ammine fluoride, and combinations thereof.

[0032] In certain embodiments, fluoride ions (also referred to herein as fluoride anions) are present in an amount of at least 1.0 wt%, at least 1.5 wt%, at least 2.0 wt%, or at least 2.2 wt%, where the weight percent is based on the total weight of the solution. In certain embodiments, fluoride anions are present in an amount of at most 6.0 wt%, at most 5.0 wt%, at most 4.5 wt%, at most 4.0 wt%, at most 3.5 wt%, where the weight percent is based on the total weight of the solution.

[0033] In certain embodiments, the fluoride anion source is selected from the group consisting of silver fluoride, silver ammine fluoride, sodium fluoride, ammonium fluoride, potassium fluoride, ammine fluoride, and combinations thereof.

[0034] In certain embodiments, the aqueous oral care solution comprises: 12.5 wt% to 20.2 wt% silver cations; and 2.2 wt% to 3.5 wt% fluoride anions; where the weight percent is based on the total weight of the solution. In certain embodiments, the thiocyanate ions are provided by Ca(SCN)2, which is provided in an amount of 1 wt% to 55 wt%.

[0035] The molar ratio of silver ions to thiocyanate ions is at most 0.40:1, at most 0.39:1, or at most 0.38:1. In certain embodiments, the molar ratio of silver ions to thiocyanate ions is at least 0.10:1, at least 0.15:1, at least 0.20:1, at least 0.25:1, at least 0.27:1, or at least 0.30:1. In certain embodiments, the source of thiocyanate ions (also referred to herein as thiocyanate anions) comprises Ca(SCN)2and optionally a second source of thiocyanate ions selected from the group consisting of ammonium thiocyanate, sodium thiocyanate, potassium thiocyanate, guanidinium thiocyanate, and combinations thereof.

[0036] In certain embodiments, the aqueous oral care solution comprises water in an amount of at least 20 wt.%, at least 25 wt.%, or at least 30 wt.%, based on the total weight of the solution. The amount of water is at most 57 wt.%, at most 55 wt.%, or at most 50 wt.%, based on the total weight of the solution.

[0037] The oral care solution forms a precipitate (i.e., a solid formed from the solution) upon contact with additional water or saliva in an oral environment. The precipitate comprises Ag, AgSCN, and CaF2. It is believed that the resulting silver-containing precipitate provides an antibacterial effect. Without being bound by theory, it is believed that CaF2, AgSCN, fluoride ions, and / or excess thiocyanate ions complex with calcium in the teeth.

[0038] In certain embodiments, the oral care solution comprises: 12.5 wt.% to 20.2 wt.% of silver cations; and 1.0 wt.% to 6.0 wt.% (or 2.2 wt.% to 3.5 wt.%) of fluoride anions; wherein the weight percentages are based on the total weight of the solution; and thiocyanate anions, wherein the molar ratio of silver ions to thiocyanate ions is at least 0.10:1 and at most 0.40:1; wherein the oral care solution forms a precipitate upon contact with additional water or saliva.

[0039] The oral care solutions of the present disclosure are aqueous solutions, but they can comprise a small amount of one or more organic solvents. Examples of organic solvents are selected from the group consisting of ethanol, isopropyl alcohol, dimethyl sulfoxide (DMSO), isoprene sulfone (IS), butadiene sulfone (BS), piperylene sulfone (PS), ethyl acetate, methyl acetate, isopropyl acetate, acetone, methyl ethyl ketone (MEK), methyl isobutyl ketone (MIBK), and combinations thereof.

[0040] Preferably, the aqueous oral care solution does not contain any organic solvent used as a liquid carrier (as opposed to organic solvents used as carriers / solvents for flavoring or sweetening). For example, certain additives may be provided as solutions or dispersions in the form of organic solvents that serve as liquid carriers. If any organic solvent (which serves as a liquid carrier) is present in the aqueous oral care solution of this disclosure, it is present in an amount of less than 5% by weight based on the total weight of the aqueous solution.

[0041] Preferably, the aqueous oral care solution of this disclosure does not stain teeth. This can be achieved by combining the oral care solution with a 1% phosphate solution in a 3:1 ratio and exposing the mixture to light at a wavelength of 430 nm to 480 nm with an output of approximately 1500 mW / cm². 2 Use a blue LED light (-10% / +20%) (such as the 3M ELIPAR DEEPCURE-S LED curing lamp, commercially available from 3M Company, St. Paul, MN) for 20 seconds to check if a black precipitate forms in the mixture. If no black precipitate forms, the solution will not stain teeth.

[0042] The aqueous oral care solutions disclosed herein are generally not shelf-stable because they form layered compositions; however, shaking or stirring the compositions yields a homogeneous composition.

[0043] Additional optional active agents

[0044] The aqueous oral care solution disclosed herein may also contain one or more active agents in addition to a fluoride source. When contained, the one or more additional active agents typically, but not always, contain one or more active agents that are effective in the oral cavity for obstacles, diseases, or conditions of the teeth, gums, cheeks, tongue, palate, etc.

[0045] Examples of adjunct surfactants that may be used include one or more other fluorinated compounds, such as sodium monofluorophosphate, stannous fluoride, calcium fluoride, strontium fluoride, zinc fluoride, potassium zinc fluoride, magnesium potassium fluoride, and combinations thereof.

[0046] Examples of adjuvant surfactants that may be used include one or more whitening agents, anti-tartar agents, remineralizing agents, tin sulfate sources, antimicrobial agents, antioxidants, saliva stimulants, breath fresheners, anti-plaque agents, anti-inflammatory agents, H2 antagonists, desensitizing agents, nutrients, and proteins. Various combinations of such adjuvant surfactants may be used if desired. When used, one or more adjuvant surfactants will typically be applied in amounts sufficient to achieve their intended effect.

[0047] When employed, the whitening agent can be a variety of suitable whitening agents. The whitening agent can include, for example, a peroxide whitening agent, a non-peroxide whitening agent, or both. Peroxide whitening agents include hydrogen peroxide, alkali or alkaline earth metal peroxides such as sodium peroxide, potassium peroxide, lithium peroxide, magnesium peroxide, calcium peroxide, barium peroxide, and the like, glyceryl hydroperoxide, alkyl hydroperoxide, dialkyl peroxide, peroxy acid or peroxy acid salt, benzoyl peroxide, urea peroxide, and the like. Hydrogen peroxide is most common. Non-peroxide whitening agents include chlorine dioxide, chlorite and hypochlorite salts. The chlorite and hypochlorite salts are typically in the form of alkali or alkaline earth metal salts, such as lithium, potassium, sodium, magnesium, calcium, or barium salts. Colorants, titanium dioxide, and hydroxyapatite can also be used.

[0048] When employed, the anti-calculus agent can be a variety of suitable anti-calculus agents. The anti-calculus agent can include, for example, a phosphate ester, a polyphosphate ester such as a pyrophosphate ester, a polyolefin sulfonate, a polyolefin phosphate ester, a bisphosphonate, a phosphonoalkanecarboxylic acid, and salts thereof, typically alkali or ammonium salts.

[0049] When employed, the remineralization agent can be a variety of suitable remineralization agents. The remineralization agent can include, for example, a material that releases calcium ions, phosphorus ions, or both, such as calcium phosphate (e.g., monocalcium phosphate, dicalcium phosphate, and / or tricalcium phosphate), hydroxyapatite, calcium carbonate, and the like.

[0050] An example of a material that releases calcium ions is a water-soluble calcium salt, such as one selected from the group consisting of calcium chloride, calcium nitrate, calcium gluconate, calcium lactogluconate, calcium acetate, hydrates thereof, and combinations thereof. In certain embodiments, the calcium salt is selected from the group consisting of calcium chloride, calcium nitrate, hydrates thereof, and combinations thereof.

[0051] The calcium salt can also be used to modulate the fluoride release profile.

[0052] When employed, the stannous source can be a variety of suitable stannous ion sources. The stannous ion source can include, for example, stannous halides, stannous salts of organic carboxylic acids such as stannous formate, stannous acetate, stannous gluconate, stannous lactate, stannous tartrate, and stannous citrate. When the fluoride source is stannous fluoride, it can also serve as the stannous source.

[0053] When employed, the antimicrobial agent can include a variety of orally acceptable antimicrobial agents. Examples include triclosan, 8-hydroxyquinoline, zinc ions, stannous ions, copper compounds, phthalic acid and salts thereof, quaternary ammonium compounds, sanguinarine, salicylanilide, salicylic acid, thymol, eugenol, neomycin, kanamycin, clindamycin, amoxicillin, tetracycline, doxycycline, minocycline, metronidazole, chlorhexidine, and the like.

[0054] When employed, the antioxidant can be any of a variety of orally acceptable antioxidants. Examples include butylated hydroxyanisole, butylated hydroxytoluene, vitamin A, carotenoids, vitamin E, flavonoids, polyphenols, ascorbic acid or salts thereof, chlorophyll, melatonin, and the like.

[0055] When employed, the saliva stimulant can be any of a variety of orally acceptable saliva stimulants. Examples include citric acid, lactic acid, succinic acid, ascorbic acid, adipic acid, fumaric acid, and tartaric acid.

[0056] When employed, the breath freshener can be any of a variety of orally acceptable breath fresheners. Examples include zinc salts such as zinc gluconate, zinc citrate, zinc chlorite, violet ketone, and the like.

[0057] When employed, the antiplaque agent can be any of a variety of orally acceptable antiplaque agents. Examples include stannous salts, salts of copper, magnesium, or strontium, polydimethylsiloxane copolyols such as cetyl polydimethylsiloxane copolyol, papain, glucoamylase, glucose oxidase, urea, calcium lactate, calcium glycerophosphate, strontium polyacrylate, and the like. Additional examples of antiplaque agents include biofilm inhibitors, especially those described in U.S. Patent 8,968,709 (Yang et al.).

[0058] When employed, the anti-inflammatory agent can be any of a variety of orally acceptable anti-inflammatory agents. Examples include steroids such as flucinolone and hydrocortisone, non-steroidal anti-inflammatory drugs such as ketorolac, flurbiprofen, ibuprofen, naproxen, indomethacin, diclofenac, etodolac, indomethacin, sulindac, tolmetin, ketoprofen, fenoprofen, piroxicam, nabumetone, aspirin, salicylic acid, diflunisal, meclofenamate, mefenamic acid, oxyphenbutazone, phenylbutazone, and the like.

[0059] When employed, the H2 antagonist can be any of a variety of orally acceptable H2 antagonists. Examples include cimetidine, nizatidine, ranitidine, tiotidine, lupitidine, denetidine, famotidine, roxatidine, pifatidine, loretidine, zaltidine, nizatidine, fentanyl, reslotidine, lavotidine, bifen-tidine, sufotidine, ethylnitidine, impromidine, and the like.

[0060] When employed, the desensitizing agent can be any of a variety of orally acceptable desensitizing agents. Examples include potassium citrate, potassium chloride, potassium tartrate, potassium bicarbonate, potassium oxalate, potassium nitrate, strontium salts, arginine, acetylsalicylic acid or salts thereof, salicylic acid or salts thereof, codeine, acetaminophen, and the like.

[0061] When employed, the nutrient can be a variety of orally acceptable nutrients. Examples include vitamins, such as vitamin C, D, thiamine, riboflavin, folic acid, niacinamide, niacin, pyridoxine, bioflavonoids, and the like; supplements, such as amino acids, anti-fatty liver agents, fish oil, polyunsaturated fatty acids, eicosapentaenoic acid, docosahexaenoic acid, coenzyme Q10, ubiquinone; minerals, such as potassium, and the like.

[0062] When employed, the protein can include a variety of orally acceptable proteins. Examples include milk proteins, enzymes producing peroxidase, amylase, papain, glucoamylase, glucose oxidase, and the like.

[0063] Buffering agents

[0064] The aqueous oral care solutions of the present disclosure can include a pharmaceutically acceptable buffer. The type and amount of such buffer is selected to provide an oral care solution having a pH of at least 5.5, at least 6, or at least 6.5. In certain embodiments, the type and amount of such buffer is selected to provide an oral care solution having a pH of at most 9, at most 8.5, at most 7.5, or at most 7. In certain embodiments, the type and amount of such buffer is selected to provide an oral care solution having a pH of 6.5 to 7.5 or a pH of 7.0. A variety of suitable pharmaceutically acceptable buffers can be included. Examples include acetate (e.g., sodium acetate), sodium carbonate, citrate (e.g., sodium citrate), tartrate, dipeptide, histidine, glycine, lysine, arginine, monobasic sodium phosphate, dibasic sodium phosphate, sodium phosphate, tris(hydroxymethyl)-aminomethane, or mixtures thereof.

[0065] Thickening agents

[0066] In certain embodiments, the aqueous oral care solutions of the present disclosure include a thickening agent to provide a solution having a suitable viscosity to allow for the desired method of application. For example, a sufficient amount of a suitable thickening agent can be used to obtain a solution viscosity that is sufficient to hold the solution in an inverted mouth tray applicator for up to four minutes (a typical time for a professional fluoride treatment) and still be sufficiently fluidized to have handling characteristics acceptable to a dental operator (e.g., when dispensed into a dental tray applicator). Alternatively, a sufficient amount of a suitable thickening agent can be used to obtain a solution viscosity that is sufficient for painting on a tooth surface.

[0067] In certain embodiments, the type and amount of thickening agent is selected to provide an oral care solution having a viscosity of at least 0.5 Pascal seconds at a shear rate of 1.0 / second. In certain embodiments, the type and amount of thickening agent is selected to provide an oral care solution having a viscosity of at most 500 Pascal seconds at a shear rate of 1.0 / second.

[0068] In certain embodiments, the thickening agent is present in the oral care solution in an amount of less than 2.5% by weight, based on the total weight of the aqueous solution. In certain embodiments, the thickening agent is present in an amount of at least 0.5% by weight, based on the total weight of the aqueous solution.

[0069] Suitable thickening agents are generally those that are generally safe for human ingestion (approved by the U.S. Food and Drug Administration (FDA) for internal use), do not bind fluoride ions, and do not significantly affect the bioavailability of fluoride ions.

[0070] In certain embodiments, the thickening agent is selected from natural gums, non-acidic cellulose derivatives (e.g., hydroxyethyl cellulose), inorganic fillers (e.g., colloidal silica, fumed silica, aluminum oxide, titanium dioxide, and zinc oxide), alkylene oxide polymers (e.g., polyethylene glycol, polypropylene glycol, and copolymers of polyethylene glycol and polypropylene glycol), non-acid modified starches, and combinations thereof.

[0071] Optional additives

[0072] In certain embodiments, the aqueous oral care solutions of the present disclosure comprise one or more optional additives, including flavorants (i.e., flavoring agents) and sweeteners. Other optional additives include surfactants. Various combinations of such additives can be used, if desired.

[0073] In certain embodiments, the aqueous oral care solutions of the present disclosure comprise a sweetener. A variety of orally acceptable sweeteners can be used. Common sweeteners include xylitol, sorbitol, sucralose, aspartame, saccharin (typically as sodium saccharin), and the like. When present, sweeteners can be used in any suitable amount, most commonly in an amount sufficient to impart a pleasing sweet taste to the solution. Suitable amounts are typically 0.5% to 15% by weight, based on the total weight of the aqueous solution.

[0074] In certain embodiments, the aqueous oral care solutions of the present disclosure comprise a flavorant. A variety of orally acceptable flavorants can be used. Common flavorants include peppermint oil, spearmint oil, cherry flavor, citric acid, orange flavor, vanilla, strawberry flavor, coconut flavor, and bubble gum flavor. When present, flavorants can be used in any suitable amount, most commonly in an amount sufficient to impart a desired flavor to the solution. Suitable amounts are typically 1% to 4% by weight, based on the total weight of the aqueous solution.

[0075] In certain embodiments, the aqueous oral care solutions of the present disclosure comprise a surfactant. Typically, such surfactants are anionic surfactants, examples of which include polysorbates, glycerin, polyglycerin-based surfactants, or combinations thereof. When present, the surfactant can be used in any suitable amount, most commonly in an amount sufficient to impart wetting properties. Suitable amounts are typically 0.1 wt% to 5.0 wt% based on the total weight of the aqueous solution.

[0076] Kit

[0077] In certain embodiments, the aqueous oral care solutions of the present disclosure are included in a kit. Typically, such kits comprise an applicator device (e.g., a toothbrush, a cotton swab) for the oral care solution. Such applicator devices can be integrated into a container having the oral care solution therein.

[0078] In certain embodiments, the oral care solution is provided in a separately sealed unit dose container. In use, the seal of such a separately sealed unit dose container is broken and the solution is picked up with an applicator device and applied to the tooth surface.

[0079] In certain embodiments, the oral care solution is provided in a multi-dose container. In use, a drop of the solution can be dispensed onto a dental tray, a plastic sheet, paper, a dish, a well, a plate, or the like, and picked up with an applicator device and applied to the tooth surface.

[0080] In certain embodiments, the kit can further comprise one or more of a dental restorative, a dental tray, a dish, a well, or a plate. Examples of dental restoratives include, but are not limited to, an adhesive, a primer, a cement, a liner, a sealant, an amalgam, a resin, a resin composite, a glass ionomer, a resin-modified glass ionomer, a glass ceramic, a ceramic, a metal, a plastic, or a combination thereof.

[0081] Method of making and using

[0082] The aqueous oral care solutions of the present disclosure can be prepared using any technique known to one of skill in the art. In certain embodiments, the components are added together to water and dissolved in no particular order. Alternatively, the order of addition can be important in obtaining the solution. For example, in certain embodiments, one or more silver and fluoride sources (e.g., AgF) are first dissolved in water and then a thiocyanate source (including Ca(SCN)2, as well as optionally one or more second thiocyanate sources) is added. Alternatively, each component can be dissolved separately in water and then combined to form the aqueous oral care solution.

[0083] In certain embodiments, the aqueous oral care solution of the present disclosure is used in a method of providing fluoride to a tooth surface of a patient. The method includes applying to the tooth surface of the patient the aqueous oral care solution described herein.

[0084] In certain embodiments, the aqueous oral care solution of the present disclosure is used in a method of reducing the incidence of dental caries (e.g., by preventing or arresting dental caries) in a patient in need of reducing the incidence of dental caries. The method includes applying to the tooth surface of the patient the aqueous oral care solution described herein.

[0085] In certain embodiments, the aqueous oral care solution of the present disclosure is used in a method of reducing dentin sensitivity and / or root sensitivity (e.g., during a caries cavity treatment and / or on an exposed root) in a patient in need of reducing dentin sensitivity and / or root sensitivity. The method includes applying to the tooth surface of the patient the aqueous oral care solution described herein.

[0086] In certain embodiments, the tooth surface of a patient treated with the method as described herein includes enamel, dentin, cementum, a root, or a combination thereof.

[0087] In certain embodiments of the above methods, applying includes painting the oral care solution on the tooth surface of the patient. In certain embodiments of the above methods, applying includes dispensing the oral care solution into a dental tray (e.g., an orthodontic aligner treatment tray) and attaching the tray with the oral care solution therein to the tooth surface of the patient.

[0088] In certain embodiments of the above method, the oral care solution is subsequently dried (e.g., using flowing air) after being applied to the tooth surface. The source of flowing air can be delivered from an air compressor that delivers at a high pressure limit of 115 pounds per square inch (psi). One example of a suitable air compressor is the Osprey compressor from RAMVAC (Model OSP22, OSP13, OSP23, OSP24, OSP25, OSP28), which is commercially available from Dental EZ Integrated Solutions, Malvern, PA or Patterson Dental, St. Paul, MN. Another example of an air compressor is the AirStar Neo air compressor from AIR TECHNIQUES (Model such as AirStar 10 Neo, AirStar 21 Neo), which is commercially available from Patterson Dental, St. Paul, MN. Alternatively, the compressed gas device can be a typical air / water syringe that is present in most dental offices for delivering compressed air. The optimal air pressure for using a typical dental air / water syringe is 40 psi to 80 psi. Such syringes are used to dry teeth or to blow dislodged calculus away from teeth. One example of such a syringe is the Johnson-Promident 3-way air / water syringe, which is commercially available from Patterson Dental Supply Inc., Patterson Part No.: 404-1893. Regardless, the gas is blown from some source of pressurized gas and can be air or some other inert gas or gas mixture. For example, the gas can be nitrogen, helium, argon, carbon dioxide, or nitrous oxide. The source of pressurized gas can be part of a permanently installed "internal" pressurized air / gas system or a hand-held self-contained tank.

[0089] In certain embodiments of the above method, water is subsequently applied to the oral care solution after it has been applied to the tooth surface to form a precipitate thereon (i.e., on the tooth surface). In certain embodiments of the above method, saliva is subsequently allowed to contact the oral care solution on the tooth surface to form a precipitate thereon (i.e., on the tooth surface).

[0090] In some embodiments of the above method, the method further includes placing a dental restorative on a tooth surface to which an oral care solution has been applied (before or after the solution dries or forms a deposit on the tooth surface). Examples of dental restoratives include, but are not limited to, adhesives, primers, cements, linings, sealants, amalgam, resins, resin composites, glass ionomers, resin-modified glass ionomers, glass ceramics, ceramics, metals, plastics, or combinations thereof.

[0091] In some embodiments, a tooth is provided comprising a tooth surface having dentinal tubules and a coating disposed on the tooth surface, wherein the coating comprises silver-rich particles and a CaF2-rich layer that closes at least a portion of the dentinal tubules.

[0092] like Figure 3 The SEM image shows a tooth surface treated with an aqueous oral care solution containing Ca(SCN)₂ tetrahydrate (Example Ex-7 solution). The tooth surface 300 has a tooth surface 310 and a fluoride-rich calcium layer 340. The tooth surface 310 has dentinal tubule openings 320 and silver-rich particles 330 (e.g., in the form of "snowflake" silver crystals). The fluoride-rich calcium layer 340 is dried on the tooth surface, thereby sealing at least a portion of the dentinal tubules. This is consistent with... Figure 1 SEM images (showing a tooth surface 100 with a dentin surface 110 having a plurality of (unclosed) dentinal tubule openings 120) and Figure 2 The SEM (which shows a tooth surface 200 with a dentin surface 210 having (unclosed) dentinal tubule openings 220 and silver-rich particles 230 (e.g., in the form of "snowflake" silver crystals), but without a calcium fluoride-rich layer) forms a contrast.

[0093] Enclosed dentinal tubules help reduce the incidence of tooth decay (e.g., by preventing or stopping tooth decay), reduce dentin and / or root sensitivity (e.g., during caries treatment and / or on exposed roots), and / or replenish minerals and strengthen tooth structure.

[0094] Exemplary embodiments

[0095] Implementation Scheme 1 is an aqueous oral care fluoride solution comprising: silver cations; thiocyanate anions provided by a thiocyanate source, the thiocyanate source including calcium thiocyanate Ca(SCN)2; fluoride anions; and water in an amount of up to 57% by weight (up to 55% by weight or up to 50% by weight) based on the total weight of the solution; wherein the molar ratio of silver ions to thiocyanate ions is up to 0.40:1.

[0096] Embodiment 2 is the oral care solution of Embodiment 1, comprising at least 12.5 wt.%, at least 13.0 wt.%, at least 14.0 wt.%, or at least 15.0 wt.% silver cations, based on the total weight of the solution.

[0097] Embodiment 3 is the oral care solution of Embodiment 1 or Embodiment 2, comprising at most 20.2 wt.%, at most 20.0 wt.%, at most 19.0 wt.%, or at most 18.0 wt.% silver cations, based on the total weight of the solution.

[0098] Embodiment 4 is the oral care solution of any of the preceding embodiments, comprising at least 1.0 wt.%, at least 1.5 wt.%, at least 2.0 wt.%, or at least 2.2 wt.% fluoride anions, based on the total weight of the solution.

[0099] Embodiment 5 is the oral care solution of any of the preceding embodiments, comprising at most 6.0 wt.%, at most 5.0 wt.%, at most 4.5 wt.%, at most 4.0 wt.%, or at most 3.5 wt.% fluoride anions, based on the total weight of the solution.

[0100] Embodiment 6 is the oral care solution of any of the preceding embodiments, wherein the molar ratio of silver ions to thiocyanate ions is at most 0.39:1 or at most 0.38:1.

[0101] Embodiment 7 is the oral care solution of any of the preceding embodiments, wherein the molar ratio of silver ions to thiocyanate ions is at least 0.10:1, at least 0.15:1, at least 0.20:1, at least 0.25:1, at least 0.27:1, or at least 0.30:1.

[0102] Embodiment 8 is the oral care solution of any of the preceding embodiments, wherein calcium thiocyanate (Ca(SCN)2) is provided in an amount of at least 1.0 wt.%, based on the total weight of the solution.

[0103] Embodiment 9 is the oral care solution of any of the preceding embodiments, wherein calcium thiocyanate (Ca(SCN)2) is provided in an amount of at most 55 wt.%, based on the total weight of the solution.

[0104] Embodiment 10 is the oral care solution of any of the preceding embodiments, comprising at least 20 wt.%, at least 25 wt.%, or at least 30 wt.% water, based on the total weight of the solution.

[0105] Embodiment 11 is an oral care solution according to any of the preceding embodiments, comprising: 12.5 wt.% to 20.2 wt.% silver cations; and 1.0 wt.% to 6.0 wt.% fluoride anions; wherein the weight percentages are based on the total weight of the solution; wherein the molar ratio of silver ion to thiocyanate ion is at least 0.10:1 and at most 0.40:1; and wherein the oral care solution forms a precipitate (e.g., Ag and CaF2) upon contact with additional water or saliva.

[0106] Embodiment 12 is an oral care solution according to any of the preceding embodiments, comprising: 12.5 wt.% to 20.2 wt.% silver cations; 1 wt.% to 55 wt.% Ca(SCN)2; and 2.2 wt.% to 3.5 wt.% fluoride anions based on the total weight of the solution.

[0107] Embodiment 13 is an oral care solution according to any of the preceding embodiments, comprising a silver cation source selected from the group consisting of silver fluoride, silver chloride, silver nitrate, silver ammonium fluoride, and combinations thereof.

[0108] Embodiment 14 is an oral care solution according to any of the preceding embodiments, comprising a fluoride anion source selected from the group consisting of silver fluoride, silver ammonium fluoride, sodium fluoride, ammonium fluoride, potassium fluoride, amine fluoride, and combinations thereof.

[0109] Embodiment 15 is an oral care solution according to any of the preceding embodiments, comprising a second thiocyanate anion source selected from the group consisting of ammonium thiocyanate, sodium thiocyanate, potassium thiocyanate, guanidinium thiocyanate, and combinations thereof.

[0110] Embodiment 16 is an oral care solution according to any of the preceding embodiments, further comprising a pharmaceutically acceptable buffer.

[0111] Embodiment 17 is an oral care solution according to any of the preceding embodiments, further comprising a thickening agent.

[0112] Embodiment 18 is an oral care solution according to Embodiment 17, wherein the thickening agent is present in an amount of 0.5 wt.% to 2.5 wt.% based on the total weight of the solution.

[0113] Embodiment 19 is an oral care solution according to any of the preceding embodiments, having a pH of 5.5 to 9.

[0114] Embodiment 20 is the oral care solution according to any of the preceding embodiments, comprising less than 5 wt.% of an organic solvent, based on the total weight of the solution.

[0115] Embodiment 21 is the oral care solution according to Embodiment 20, wherein the organic solvent is selected from the group consisting of ethanol, isopropyl alcohol, dimethyl sulfoxide (DMSO), isoprene sulfone (IS), butadiene sulfone (BS), piperylene sulfone (PS), ethyl acetate, methyl acetate, isopropyl acetate, acetone, methyl ethyl ketone (MEK), methyl isobutyl ketone (MIBK), and combinations thereof.

[0116] Embodiment 22 is the oral care solution according to any of the preceding embodiments, further comprising one or more active agents.

[0117] Embodiment 23 is the oral care solution according to Embodiment 22, wherein the one or more active agents comprise a whitening agent, an anti-calculus agent, a remineralization agent, a stannous source, an antimicrobial agent, an antioxidant, a saliva stimulant, a breath freshening agent, an anti-plaque agent, an anti-inflammatory agent, an H2 antagonist, a desensitizing agent, a nutrient, a protein, or combinations thereof.

[0118] Embodiment 24 is the oral care solution according to any of the preceding embodiments, further comprising a flavoring agent.

[0119] Embodiment 25 is the oral care solution according to any of the preceding embodiments, further comprising a sweetener.

[0120] Embodiment 26 is the oral care solution according to any of the preceding embodiments, further comprising a calcium cation.

[0121] Embodiment 27 is the oral care solution according to Embodiment 26, comprising a second calcium cation source selected from the group consisting of calcium chloride, calcium nitrate, calcium gluconate, calcium lactogluconate, calcium acetate, hydrates thereof, and combinations thereof.

[0122] Embodiment 28 is the oral care solution according to any of the preceding embodiments, further comprising a surfactant.

[0123] Embodiment 29 is the oral care solution according to Embodiment 28, wherein the surfactant is an anionic surfactant.

[0124] Embodiment 30 is the oral care solution of Embodiment 29, wherein the anionic surfactant is selected from the group consisting of polysorbate, glycerin, polyglycerin-based surfactants, and combinations thereof.

[0125] Embodiment 31 is the oral care solution of any of the preceding embodiments, which is non-staining to teeth.

[0126] Embodiment 32 is the oral care solution of Embodiment 31, which does not form a black precipitate when combined with a 1% phosphate solution at a 3:1 ratio, and the mixture is exposed to blue LED light having a wavelength of 430 nm to 480 nm and an output of about 1500 mW / cm 2 for 20 seconds.

[0127] Embodiment 33 is a method of providing fluoride to a tooth surface of a patient, the method comprising applying to the tooth surface of the patient the aqueous oral care solution of any of the preceding embodiments.

[0128] Embodiment 34 is a method of reducing the incidence of dental caries (e.g., by preventing or arresting dental caries) in a patient in need of reducing the incidence of dental caries, the method comprising applying to a tooth surface of the patient the aqueous oral care solution of any of Embodiments 1-32.

[0129] Embodiment 35 is a method of reducing dentin sensitivity and / or root sensitivity (e.g., during a caries cavity treatment and / or on an exposed root) in a patient in need of reducing dentin sensitivity and / or root sensitivity, the method comprising applying to a tooth surface of the patient the aqueous oral care solution of any of Embodiments 1-32.

[0130] Embodiment 36 is the method of any of Embodiments 33-35, wherein the tooth surface of the patient comprises enamel, dentin, cementum, a root, or a combination thereof.

[0131] Embodiment 37 is the method of any of Embodiments 33-36, wherein applying comprises painting the oral care solution on the tooth surface of the patient.

[0132] Embodiment 38 is the method of any of Embodiments 33-36, wherein applying comprises dispensing the oral care solution into a dental tray (e.g., an orthodontic aligner treatment tray) and attaching the tray with the oral care solution therein to the tooth surface of the patient.

[0133] Embodiment 39 is the method according to any one of embodiments 33-38, wherein the oral care solution is subsequently dried (e.g., using flowing air) after being applied to the tooth surface.

[0134] Embodiment 40 is the method according to any one of embodiments 33-38, wherein water is subsequently applied to the oral care composition after the oral care solution is applied to the tooth surface to form a deposit thereon (i.e., on the tooth surface).

[0135] Embodiment 41 is the method according to any one of embodiments 33-38, wherein saliva is subsequently allowed to contact the oral care solution on the tooth surface to form a deposit thereon (i.e., on the tooth surface).

[0136] Embodiment 42 is the method according to any one of embodiments 33-41, further comprising placing a dental restorative on the tooth surface to which the oral care solution was applied (before or after the solution is dried or a deposit is formed on the tooth surface).

[0137] Embodiment 43 is the method according to embodiment 42, wherein the dental restorative comprises an adhesive, a primer, a cement, a liner, a sealant, an amalgam, a resin, a resin composite, a glass ionomer, a resin modified glass ionomer, a glass ceramic, a ceramic, a metal, a plastic, or a combination thereof.

[0138] Embodiment 44 is a kit comprising the aqueous oral care solution according to any one of embodiments 1-32 and an application device (e.g., a toothbrush, a cotton swab).

[0139] Embodiment 45 is the kit according to embodiment 44, wherein the oral care solution is provided in a separately sealed unit dose container.

[0140] Embodiment 46 is the kit according to embodiment 44, wherein the oral care solution is provided in a multi-dose container.

[0141] Embodiment 47 is the kit according to any one of embodiments 44-46, wherein the application device is integrated into the container having the oral care solution therein.

[0142] Embodiment 48 is the kit according to any one of embodiments 44-47, further comprising a dental restorative.

[0143] Embodiment 49 is the kit of Embodiment 48, wherein the dental restorative comprises an adhesive, primer, cement, liner, sealant, amalgam, resin, resin composite, glass ionomer, resin-modified glass ionomer, glass ceramic, ceramic, metal, plastic, or a combination thereof.

[0144] Embodiment 50 is the kit of any one of Embodiments 44-49, further comprising a tray, dish, well, or plate.

[0145] Embodiment 51 is a method of making the aqueous oral care solution of any one of Embodiments 1-32, the method comprising combining and dissolving in water a silver source and a fluoride source (which can be the same, such as AgF); and adding a thiocyanate source comprising Ca(SCN)2and optionally one or more second thiocyanate sources, and dissolving in water to form the aqueous oral care solution.

[0146] Embodiment 52 is a tooth comprising a tooth surface having dentin tubules and a coating disposed on the tooth surface, wherein the coating comprises silver-rich particles and a CaF2-rich layer occluding at least a portion of the dentin tubules.

[0147] Examples

[0148] Objects and advantages of this application are further illustrated by the following examples, but the particular materials and amounts thereof recited in these examples, as well as other conditions and details, should not be construed to unduly limit this application. These examples are merely for illustrative purposes and are not intended to limit the scope of the appended claims. Unless otherwise indicated, all amounts are in weight percent.

[0149] Table 1. Materials

[0150]

[0151] Example preparation and evaluation

[0152] For each example or comparative example, 0.5 grams of silver fluoride was weighed into a plastic tube and 0.8 grams of deionized (DI) water was added and mixed thoroughly to form a solution. To achieve the weight percentages reported in the example tables below, the remaining components of each example or comparative example were weighed out and combined in a weighing boat as a dry mixture. Additional dry components were then added slowly to the silver fluoride solution while mixing. This is an exothermic process as heat is generated during the addition of the thiocyanate. A pasty precipitate formed as an additional dry component was initially added partially. This is reported in the tables below.

[0153] The remaining dry components were added slowly with continued mixing. For the working examples, the precipitate fully dissolved after the appropriate amount of thiocyanate was added. After all of the remaining dry components, including the calcium thiocyanate, were fully added, the example solution, which had become turbid, was mixed on a vortex mixer and remained turbid. The example solution was allowed to stand at room temperature for 1 week. After 1 week, it was observed that the example solution had separated into two phases: a clear solution on top and a turbid bottom layer.

[0154] For the comparative examples, except for comparative example CE-10, the remaining dry components were added without re-dissolving the initial precipitate.

[0155] Table 2. Comparative Examples CE-1 to CE-5 .

[0156] Component CE-1 CE-2 CE-3 CE-4 CE-5 AgF 16.7 16.7 16.7 16.7 16.7 Disodium citrate sesquihydrate 50.0 0.0 0.0 0.0 0.0 Sodium carbonate 0.0 50.0 0.0 0.0 0.0 Potassium dihydrogen phosphate 0.0 0.0 50.0 0.0 0.0 NH4CI 0.0 0.0 0.0 50.0 0.0 Ca(SCN)2 tetrahydrate 0.0 0.0 0.0 0.0 0.0 Potassium sulfate 0.0 0.0 0.0 0.0 50.0 DI water 33.3 33.3 33.3 33.3 33.3 Total (%) 100 100 100 100 100 Ag % 14.2 14.2 14.2 14.2 14.2 F% 2.5 2.5 2.5 2.5 2.5 Ag / SCN molar ratio NA NA NA NA NA Precipitate formed upon initial addition of additional dry components Yes Yes Yes Yes Yes Precipitate dissolved after further addition of dry components No No No No No

[0157] Table 3. Comparative Examples CE-6 to CE-9 .

[0158] Component CE-6 CE-7 CE-8 CE-9 AgF 18.4 18.5 19.2 19.2 Disodium citrate sesquihydrate 0.0 0.0 0.0 0.0 Sodium carbonate 0.0 0.0 0.0 0.0 Potassium dihydrogen phosphate 0.0 0.0 0.0 0.0 NH4Cl 22.1 0.0 0.0 26.9 NH4SCN 0.0 22.2 0.0 0.0 [NH4I] 22.8 22.2 26.9 0.0 Ca(SCN)2 tetrahydrate 0.0 0.0 15.4 15.4 Potassium sulfate 0.0 0.0 0.0 0.0 DI water 36.8 37.0 38.5 38.5 Total (%) 100 100 100 100 Ag % 15.6 15.7 16.3 16.3 F% 2.8 2.8 2.9 2.9 Ag / SCN molar ratio NA NA 1.12 1.12 Precipitate formed upon initial addition of additional dry components Yes Yes Yes Yes Precipitate dissolved after further addition of dry components No No No No

[0159] Table 4. Examples Ex-1 to Ex-5 .

[0160]

[0161] Table 5. Examples Ex-6 to Ex-11 .

[0162]

[0163] Table 6. Examples Ex-12 to Ex-16 and Comparative Example CE-10 .

[0164]

[0165] Table 7. Examples Ex-17 to Ex-18 and Comparative Examples CE-11 to CE-13 .

[0166] It was shown that the molar ratio of silver to thiocyanate must be < 0.40:1 to dissolve the precipitate.

[0167]

[0168] Table 8. Examples: Ex-19 to Ex-23, and Comparative Example CE-14 .

[0169] It was shown that the total water % must be < 57%.

[0170]

[0171] Example Ex-24

[0172] A silver fluoride solution (38%) from Elevate Oral Care was used as the source of silver and fluoride. A 0.122 gram quantity of the silver fluoride solution was mixed with 0.025 grams of NH4SCN and 0.100 grams of Ca(SCN)2tetrahydrate. A precipitate formed initially. After mixing in a weighing boat, the precipitate dissolved and a solution formed.

[0173] Photosensitivity of examples

[0174] The following examples show that solutions of the inventive compositions do not turn black after (1) precipitation by the addition of a buffer solution (to simulate saliva in the oral environment), and (2) exposure to light using a 3M ELIPAR DEEPCURE-S LED curing light.

[0175] Comparative Example CE-15

[0176] A 58 mg quantity of silver fluoride solution (ADVANTAGE ARREST silver fluoride solution (38%)) was mixed with 108 mg of 1% KH2PO4 aqueous solution. The mixture formed a precipitate and released ammonia. The mixture was exposed to blue LED light at a wavelength of about 450 nm and an output of approximately 1500 mW / cm2for 20 seconds using a 3M ELIPAR DEEPCURE-S LED curing light, and the mixture turned black. 2

[0177] Example Ex-25

[0178] A 35 mg quantity of Ex-22 solution was mixed with 90 mg of 1% KH2PO4 aqueous solution. The mixture formed a precipitate. The mixture was exposed to blue LED light at a wavelength of about 450 nm and an output of approximately 1500 mW / cm2for 20 seconds using a 3M ELIPAR DEEPCURE-S LED curing light. The mixture did not turn black. 2

[0179] Example Ex-26

[0180] A 40 mg quantity of Ex-24 solution was mixed with 104 mg of 1% KH2PO4 aqueous solution. The mixture formed a precipitate. The mixture was exposed to blue LED light at a wavelength of about 450 nm and an output of approximately 1500 mW / cm2for 20 seconds using a 3M ELIPAR DEEPCURE-S LED curing light. The mixture did not turn black. 2

[0181] Dentin surface treatment and characterization

[0182] ​​​Bovine teeth were polished with 120 grit sandpaper to expose dentin, then 320 grit sandpaper was used to polish the dentin surface. The dentin was etched using SCOTCHBOND Universal Primer (commercially available from 3M Company, St. Paul, MN) for 10 seconds to clean the dentin surface. The etched bovine teeth were rinsed with water to clean the surface, then the teeth were blown dry with pressurized air. The prepared dentin surfaces (teeth) were swabbed with the different example and comparative example solutions, allowed to sit for one minute, rinsed with water, and then air dried before evaluation using a tabletop scanning electron microscope. The prepared dentin controls and prepared dentin treated with the example and comparative example solutions were examined by Hitachi TM3000 SEM to observe the structure and properties of the coating deposited on the dentin surface.

[0183] Comparative Example CE-16

[0184] Comparative Example CE-16 was a control prepared dentin surface that was not treated with an example or comparative example solution and was evaluated by SEM. The SEM of CE-16 is shown in Figure 1 The acid-etched, washed, and dried tooth surface 100 shows a clean dentin surface 110 and many dentin tubule openings 120.

[0185] Comparative Example CE-17

[0186] Comparative Example CE-17 was a prepared dentin surface that was treated with the comparative example CE-10 solution that did not contain Ca(SCN)2tetrahydrate and was evaluated by SEM. The SEM of CE-17 is shown in Figure 2 The acid-etched, washed, and dried tooth surface 200 shows a clean dentin surface 210 covered with dried CE-1 solution. The SEM shows dried dentin tubule openings 220 and “snowflake-like” silver crystals 230 on the dentin surface.

[0187] Example Ex-27

[0188] Example Ex-27 was a prepared dentin surface that was treated with the example Ex-7 solution that contained Ca(SCN)2tetrahydrate and was evaluated by SEM. The SEM of Ex-27 is shown in Figure 3 The acid-etched, washed, and dried tooth surface 300 shows a clean dentin surface 310 covered with dried Ex-7 solution. The SEM shows dried dentin tubule openings 320, “snowflake-like” silver crystals 330, and a separate calcium fluoride layer 340 on the dentin surface.

[0189] The entire disclosure of all patents, patent documents, and publications cited herein are hereby incorporated by reference in their entirety as if each were individually incorporated. Various modifications and alterations to this disclosure will become apparent to those of ordinary skill in the art without departing from the scope and spirit of this disclosure. It should be understood that this disclosure is not intended to be unduly limited by the illustrative embodiments and examples disclosed herein and that such examples and embodiments are presented by way of example only with the scope of the disclosure intended to be limited only by the claims as set forth herein.

Claims

1. An aqueous oral care solution, said aqueous oral care solution comprising: A silver cation source, wherein the silver cation source is present in an amount providing 12.5% ​​by weight to 20.2% by weight of silver cations; One or more thiocyanate sources, said one or more thiocyanate sources being present in an amount providing a molar ratio of silver cations to thiocyanate ions of up to 0.40:1, wherein at least one thiocyanate source is Ca(SCN)2. A fluorine anion source, said fluorine anion source being present in an amount providing 1% to 6% fluorine anions; and Water present in amounts of 20% to 50% by weight; The weight percentage is based on the total weight of the solution.

2. The aqueous oral care solution of claim 1, wherein the one or more thiocyanate sources are present in an amount providing a molar ratio of silver cations to thiocyanate ions of at least 0.10:

1.

3. The aqueous oral care solution according to claim 1, wherein the fluoride anion source is present in an amount providing 2.2% to 3.5% fluoride anions.

4. The aqueous oral care solution according to claim 1, wherein the aqueous oral care solution contains 1% to 55% by weight of Ca(SCN)2.

5. The aqueous oral care solution according to claim 1, wherein the silver cation source is selected from silver fluoride, silver chloride, silver nitrate, silver ammonium fluoride, and combinations thereof.

6. The aqueous oral care solution according to claim 1, wherein the fluoride anion source is selected from silver fluoride, silver ammonium fluoride, sodium fluoride, ammonium fluoride, potassium fluoride, amine fluoride, and combinations thereof.

7. The aqueous oral care solution according to claim 1, wherein the aqueous oral care solution comprises a second thiocyanate anion source, the second thiocyanate anion source being selected from ammonium thiocyanate, sodium thiocyanate, potassium thiocyanate, guanidine thiocyanate, and combinations thereof.

8. The aqueous oral care solution according to claim 1, wherein the aqueous oral care solution further comprises a thickener.

9. The aqueous oral care solution according to claim 1, wherein the aqueous oral care solution has a pH of 5.5 to 9.

10. The aqueous oral care solution according to claim 1, wherein the aqueous oral care solution contains less than 5% by weight of an organic solvent.

11. The aqueous oral care solution according to claim 1, wherein the aqueous oral care solution contains silver fluoride as a silver cation source and a fluoride anion source.

12. The aqueous oral care solution according to claim 1, wherein the aqueous oral care solution further comprises one or more active agents.

13. The aqueous oral care solution according to claim 1, wherein the aqueous oral care solution contains ammonium thiocyanate as a thiocyanate source.

14. The aqueous oral care solution according to claim 1, wherein the aqueous oral care solution further comprises a surfactant.

15. The aqueous oral care solution according to claim 1, wherein the aqueous oral care solution does not stain teeth.

16. The oral care solution according to any one of claims 1 to 15, wherein the oral care solution is used in the manufacture of a medicament for delivering fluoride to the surface of a patient's teeth.

17. The oral care solution according to any one of claims 1 to 15, wherein the oral care solution is used in the manufacture of a medicament for reducing the incidence of dental caries in patients who require a reduction in the incidence of dental caries.

18. The oral care solution according to any one of claims 1 to 15, wherein the oral care solution is used in the manufacture of a medicament for reducing tooth sensitivity and / or root sensitivity in patients who require it.

19. A kit comprising an aqueous oral care solution according to any one of claims 1 to 15 and an application device.

20. An aqueous oral care solution, said aqueous oral care solution comprising: Silver fluoride present in amounts providing 12.5% ​​to 20.2% silver cations; Calcium thiocyanate or calcium thiocyanate and ammonium thiocyanate; and Water present in amounts of 20% to 50% by weight; Silver fluoride is present in an amount providing a molar ratio of silver cations to thiocyanate ions of 0.30:1 to 0.40:1, and The weight percentage is based on the total weight of the aqueous oral care solution.

Citation Information

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