Glass composition

Abstract

To provide a glass composition for dentin desensitizing compositions.SOLUTION: The present disclosure provides a glass composition that includes: from about 50 mol% to about 95 mol% of B2O3; and from about 5 mol% to about 50 mol% of one or more glass components selected from the group consisting of: Li2O, Rb2O, K2O, Na2O, SrO, CaO, MgO, and ZnO. The glass composition includes less than 30 mol% of Rb2O. The glass composition is a quaternary system. The glass composition is a particulate material that includes particles that are from about 1 to about 50 μm in size. The glass composition loses at least 5 mass% within 24 hours when exposed to a buffered saline solution. The glass composition may be used to desensitize dentin. The present disclosure also provides a dentin desensitizing composition.SELECTED DRAWING: None

Description

[Technical field]

[0001] The present disclosure relates to glass compositions for dentin desensitizing compositions. [Background technology]

[0002] The following paragraphs are not an admission that anything discussed therein is prior art or part of the knowledge of those skilled in the art.

[0003] Dentin sensitivity is tooth pain resulting from exposed dentin surfaces in response to thermal, evaporative, tactile, osmotic, chemical, or electrical stimuli. Dentin sensitivity can be caused by gingival recession with exposure of the root surface (receding gums), loss of the cementum and smear layers, tooth wear, acid erosion, root flattening, or tooth whitening.

[0004] Dentin has thousands of tiny tubular structures radiating outward from the pulp. Alterations in the flow of the plasma-like fluid present in the dentinal tubules trigger mechanoreceptors present in the nerves adjacent to the tooth pulp, thereby causing a pain response. This hydrodynamic flow can be increased by cold air pressure, dryness, sugar, acidity (dehydrating agents), or forces acting on the tooth. Hot or cold foods and drinks, and physical pressure are typical triggers for individuals with dental sensitivity.

[0005] There is no globally accepted gold standard treatment that reliably relieves the pain of dental sensitivity in the long term, however treatments can be divided into in-office (i.e., those intended to be applied by a dentist or dental therapist) or those that can be performed at home, over-the-counter or prescription.

[0006] The mechanism of action of these treatments is thought to be either occlusion of dentinal tubules or desensitization of nerve fibers / blockade of nerve conduction. Summary of the Invention

[0007] introduction The following introduction is intended to orient the reader to the present specification, but does not define any invention. One or more inventions may be present in any combination or subcombination of the apparatus elements or method steps described below, or elsewhere in this specification. The inventors have not waived or relinquished any rights to any inventions disclosed herein, merely by not claiming such other inventions.

[0008] One example of a dentin desensitizing composition known in the art is disclosed in PCT Publication WO2007144662A1. The disclosed toothpaste includes a bioactive glass containing strontium. The disclosed bioactive glass occludes dentin tubules and induces the precipitation and crystallization of carbonated hydroxyapatite. The disclosed bioactive glass is designed to degrade at the same rate as the rate of induced tissue ingrowth.

[0009] One example of a dentin desensitizing composition known in the art is disclosed in U.S. Patent No. 5,735,942. The disclosed toothpaste contains a mineral component consisting of CaO, Na2O, P2O5, and SiO2. The disclosed mineral composition chemically reacts with the dentin surface and intimately bonds with the tooth structure.

[0010] One or more described embodiments attempt to address or ameliorate one or more shortcomings associated with dentin desensitizing compositions that include non-degradable particulate materials that occlude dentinal tubules. In some embodiments, the disclosed particulate materials substantially degrade over a period of 12-24 hours under ambient conditions. In some embodiments, the disclosed particulate materials provide a controlled release of fluoride over the same period.

[0011] In some embodiments, the present disclosure provides a glass composition comprising about 50 mol% to about 5 mol% of a glass component selected from the group consisting of Li2O, Rb2O, KO, Na2O, SrO, CaO, MgO, ZnO, and any combination thereof; 0 mol% of CuO; less than 0.1 mol% of BaO; and less than 0.1 mol% of PO5, wherein the glass composition comprises less than 30 mol% of Rb2O; the glass composition loses at least 5 mol% within 24 hours upon exposure to a buffered saline solution; and the glass composition is a particulate material comprising particles of about 1 to about 50 μm in size. The glass composition does not consist solely of BO3 and Na2O.

[0012] In some examples of glass compositions according to the present disclosure, less than 20 mol%, such as less than 15 mol%, less than 10 mol%, or less than 5 mol% of the glass composition are CaO, MgO, and Na2O.

[0013] The glass composition may further include up to about 30 mol % fluoride, where the fluoride is in the form of CaF2, NaF, Na2PO3F, KF, or SnF2.

[0014] In another embodiment, the present disclosure provides a glass composition for desensitizing dentin, the glass composition comprising about 50 mol% to about 95 mol% of a glass component selected from the group consisting of: B2O3; Li2O, Rb2O, KO, Na2O, SrO, CaO, MgO, ZnO, and any combination thereof, wherein the glass composition comprises less than 30 mol% Rb2O. The glass composition loses at least 5% by weight within 24 hours upon exposure to a buffered saline solution, and the glass composition is a particulate material comprising particles having a size of about 1 to about 50 μm.

[0015] In some examples of the glass composition, less than 20 mol%, such as less than 15 mol%, less than 10 mol%, or less than 5 mol% of the glass composition are CaO, MgO, and Na2O.

[0016] The glass composition may further include up to about 30 mol % fluoride, where the fluoride is in the form of CaF2, NaF, Na2PO3F, KF, or SnF2.

[0017] In another embodiment, the present disclosure provides a glass composition comprising: about 5 mol % to about 10 mol % of fluoride provided as CaF, SnF, NaF, KF, or any combination thereof; and about 90 mol % to about 95 mol % of a combination of B2O3, Na2O, MgO, and CaO, where boron, magnesium, any combination of Na and K, and any combination of Ca and Sn in the glass composition are present in an elemental ratio of about 20: about 4: about 6: about 3, respectively.

[0018] One example of such a specific glass composition according to the present disclosure includes about 50 mol% B2O3, about 15 mol% Na2O, about 20 mol% MgO, about 10 mol% CaOC, and about 5 mol% CaF2.

[0019] The glass compositions according to the present disclosure can be formulated into dentin desensitizing compositions such as toothpastes, prophylactic pastes, dental varnishes, mouthwashes, dental gels, or adhesives. The dentin-desensitizing compositions according to the present disclosure are substantially anhydrous.

[0020] Glass compositions according to the present disclosure can be used to desensitize dentin, for example, in a method comprising applying a toothpaste, prophylactic paste, dental varnish, mouthwash, dental gel, or adhesive according to the present disclosure to an individual's dentin.

[0021] The glass compositions according to the present disclosure can be prepared from the corresponding bulk glasses. The chemical formulation is the same between the bulk glasses and the particulate matter. Another aspect of the present disclosure is a bulk glass having a chemical formulation as disclosed herein.

[0022] Embodiments of the present disclosure will now be described, by way of example only, with reference to the accompanying drawings. [Brief description of the drawings]

[0023] [Figure 1] FIG. 1 shows the average surface profile of a resin composite after 20,000 brushing cycles with Gel 7HT toothpaste ("Gel") formulated with a glass composition of the present disclosure ("Gel + Additives") versus Gel 7HT toothpaste ("Gel"). [Diagram 2] FIG. 2 shows the average surface profile of the resin composite after 20,000 brushing cycles for Gel 7HT ("Gel") toothpaste versus Colgate™ Enamel Health Sensitivity Relief™ toothpaste formulated with a glass composition ("Colgate EN+Additive"). [Diagram 3] FIG. 3 shows the average surface profile of the resin composite after 20,000 brushing cycles with Gel 7HT toothpaste ("Gel") versus Colgate™ Optic White™ toothpaste ("Colgate Optic"). [Figure 4] FIG. 4 shows the average surface profile of a resin composite resin after 20,000 brushing cycles with Gel 7HT ("Gel") toothpaste versus Colgate™ Enamel Health Sensitivity Relief™ toothpaste ("Colgate EN"). [Diagram 5] FIG. 5 shows the average surface profile of the resin composite after 20,000 brushing cycles using Gel 7HT toothpaste ("Gel") and Sensodyne™ Whitening Restorative and Protect™ Toothpaste ("Sensodyne"). [Figure 6] FIG. 6 shows the average surface profile of the enamel surface after 20,000 brushing cycles with Gel 7HT toothpaste ("Sensodyne") formulated with a glass composition ("Gel + Additive") versus Sensodyne™ Whitening Restorative and Protect™ Toothpaste ("Sensodyne"). [Figure 7]FIG. 7 shows the average surface profile of enamel surfaces after 20,000 brushing cycles with Gel 7HT toothpaste formulated with a glass composition ("Gel + additive") versus Colgate™ Enamel Health Sensitivity Relief™ toothpaste formulated with a glass composition ("Colgate EN + additive"). [Figure 8] FIG. 8 shows the average surface profile of the enamel surface after 20,000 brushing cycles for Gel 7HT toothpaste ("Gel") and Gel 7HT toothpaste formulated with a glass composition ("Gel + additive"). [Figure 9] FIG. 9 shows the average surface profile of the enamel surface after 20,000 brushing cycles with Gel 7HT toothpaste formulated with a glass composition ("Gel + Additive") versus Colgate™ Optic White™ toothpaste ("Colgate Optic"). [Figure 10] FIG. 10 shows the average surface profile of enamel surfaces after 20,000 brushing cycles with Gel 7HT toothpaste formulated with a glass composition ("Gel + Additives") versus Colgate™ Enamel Health Sensitivity Relief™ Toothpaste ("Colgate EN"). [Figure 11] FIG. 11 is an image from a scanning electron microscope of an exemplary glass composition of the present disclosure after 30 minutes at 37° C. in simulated body fluid (SBF). [Figure 12] FIG. 12 is an image from a scanning electron microscope of an exemplary glass composition according to the present disclosure after 3 hours in simulated body fluid (SBF) at 37° C. [Figure 13] FIG. 13 is an image from a scanning electron microscope of an exemplary glass composition according to the present disclosure after 12 hours in simulated body fluid (SBF) at 37° C. [Figure 14] FIG. 14 is another photograph from a scanning electron microscope of an exemplary glass composition according to the present disclosure after 12 hours in simulated body fluid (SBF) at 37° C. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0024] The glass composition according to the present disclosure is at least a quaternary system. The glass composition includes about 50 mol% to about 95 mol% B2O3; and about 5 mol% to about 50 mol% of one or more glass components selected from the group consisting of Li2O, Rb2O, K2O, Na2O, SrO, CaO, MgO, and ZnO. The glass composition includes less than 30 mol% Rb2O. The glass composition according to the present disclosure degrades under physiological conditions, losing at least 5% by mass within 24 hours upon exposure to buffered saline.

[0025] The glass composition is a particulate material comprising particles of about 1 to about 50 μm in size. The glass composition comprises at least some particles of a size that occludes dentinal tubules, thereby desensitizing dentin. In the context of the present disclosure, particles of a size that occludes dentinal tubules should be understood to mean that the particles are present in or on the dentinal tubules, reducing dentinal fluid movement.

[0026] In the context of this disclosure, a glass composition that is "at least quaternary" should be understood to refer to a glass having four or more distinct elements. For example, a glass composition consisting only of B2O3, Li2O, and ZnO would be considered quaternary because the glass contains boron, lithium, zinc, and oxygen. Similarly, a glass composition consisting only of B2O3, CaO, and CaF2 would be considered quaternary because the glass contains boron, calcium, fluorine, and oxygen. In contrast, a glass composition consisting only of B2O3 and Na2O would be considered ternary because it contains the elements boron, sodium, and oxygen.

[0027] It should be understood that "about 5 mol% to about 50 mol% of one or more glass components" refers to the total mol% of the glass components, not the mol% of each component. For example, a glass composition according to the present disclosure can include 2.5 mol% Li2O and 2.5 mol% ZnO to provide the recited 5 mol% additional glass components.

[0028] It is to be understood that "about X mol%" refers to a value within ±2% of the reported percentage. For example, "about 10 mol%" refers to values ​​between 8 mol% and 12 mol%, since all of these values ​​are within ±2% of the reported 10%; "about 50 mol%" refers to values ​​between 48 mol% and 52 mol%, since all of these values ​​are within ±2% of the reported 50%.

[0029] It is to be understood that "about X μm" in the context of particle size is determined based on the tolerances accepted according to ASTM for the test sieve of the size in question. For example, the tolerance for a 50 μm test sieve is 3 μm. Thus, "about 50 μm" refers to particles with a size between 47 μm and 53 μm. In another example, the tolerance for a 35 μm test sieve is 2.6 μm. Thus, "about 35 μm" refers to particles with a size between 32.4 μm and 38.6 μm. The ASTM tolerance for a 25 μm sieve is 2.2 μm. For test sieves without standard tolerances (e.g., test sieves smaller than 20 μm), the expression "about X μm" refers to ±15% for sizes between 5 and 15 μm and ±50% for sizes smaller than 5 μm. For example, "about 1 μm" refers to particles with a size between 0.5 and 1.5 μm.

[0030] Glass composition The glass composition according to the present disclosure may include a fluoride source such as CaF2, NaF, Na2PO3F, KF, or SnF2. The inclusion of fluoride in the glass composition releases fluoride as the glass degrades. The released fluoride forms fluoride apatite (Ca5(PO4)3F) in or around the dentinal tubules, forming a protective precipitate and further reducing dentin sensitivity. In glass compositions that include fluoride, the fluoride source may be up to 30 mol% of the glass composition. In some examples, the fluoride source may be about 1 mol% to about 10 mol%, such as about 1 mol% to about 5 mol%, of the glass composition. In certain examples, the fluoride source is about 15 mol% of the composition. Compositions that include CaF2 or SnF2 provide double the amount of fluoride per mole of starting material compared to compositions that use NaF, Na2PO3F, or KF.

[0031] In some examples, the glass composition includes between about 1 mol % and about 10 mol % fluoride.In some examples, the glass composition includes between about 1 mol % and about 5 mol % fluoride.

[0032] In some examples, the glass composition contains sufficient fluoride such that 0.1 g of particulate material releases fluoride in 10 mL of buffered saline at an average rate of about 1 ppm / hr to about 15 ppm / hr over 1, 2, 4, 8, 12, 18, or 24 hours. In the context of this disclosure, ppm is measured as mass / mass. In particular examples, the glass composition contains sufficient fluoride such that about 4 to about 6 ppm of fluoride is released per hour over a 1 hour period.

[0033] In some examples of glass compositions according to the present disclosure, less than 20 mol%, such as less than 15 mol%, less than 10 mol%, or less than 5 mol% of the glass composition are CaO, MgO, and Na2O.

[0034] In one example of a glass composition according to the present disclosure, the glass composition is free of CuO, contains less than 0.1 mol% BaO, and contains less than 0.1 mol% P2O5. In particular, the glass composition is free of CuO, BaO, or P2O5.

[0035] A glass composition according to the present disclosure may include about 5 mol % to about 50 mol % of one or more glass components selected from the group consisting of Li2O, Rb2O, KO, Na2O, SrO, and ZnO, and the glass composition includes less than 0.1 mol % CaO and less than 0.1 mol % MgO.

[0036] A glass composition according to the present disclosure may include about 5 mol % to about 50 mol % of one or more glass components selected from the group consisting of Li2O, Rb2O, KO, SrO, and ZnO, and the glass composition includes less than 0.1 mol % CaO, less than 0.1 mol % MgO, and less than 0.1 mol % Na2O.

[0037] Glass compositions according to the present disclosure can include about 50 mol % to about 80 mol % B2O3, for example about 50 mol % B2O3.

[0038] The glass composition according to the present disclosure may contain about 5 mol % to about 40 mol %, for example about 20 mol % to about 40 mol %, of one or more glass components selected from the group consisting of Li2O, Rb2O, K2O, Na2O, SrO, CaO, MgO, and ZnO.

[0039] Glass compositions according to the present disclosure may include B2O3, Li2O, and ZnO, and optionally Rb2O, Na2O, and / or a fluoride source. Specifically, the glass composition may include about 5 mol% to about 25 mol% Li2O, about 5 mol% to about 25 mol% Rb2O, or about 5 mol% to about 25 mol% Li2O, about 5 mol% to about 15 mol% ZnO, and optionally about 5 mol% to about 15 mol% Na2O, and the glass composition may include about 50 mol% B2O3, or about 70 mol% B2O3.

[0040] Glass compositions according to the present disclosure can include B2O3, and ZnO, and optionally Rb2O and / or a fluoride source. In particular, the glass composition includes about 5 mol% to about 30 mol% ZnO. When present, RbO2 can be included in an amount of about 5 mol% to about 30 mol%. The glass composition can include about 50 mol% B2O3.

[0041] Glass compositions according to the present disclosure may include B2O3, SrO, and optionally ZnO and / or a fluoride source. In particular, the glass composition includes about 5 mol% to about 30 mol% SrO. When present, ZnO may be included in an amount of about 5 mol% to about 30 mol%. The glass composition may include about 50 mol% B2O3.

[0042] As discussed above, the present disclosure also provides a glass composition comprising: about 5 mol % to about 10 mol % of fluoride provided as CaF, SnF, NaF, KF, or any combination thereof; and about 90 mol % to about 95 mol % of a combination of B2O3, Na2O, MgO, and CaO, where boron, magnesium, any combination of Na and K, and any combination of Ca and Sn in the glass composition are present in an elemental ratio of about 20:about 4:about 6:about 3, respectively.

[0043] One specific example of such a glass composition includes about 50 mol% B2O3, about 15 mol% Na2O, about 20 mol% MgO, about 10 mol% CaO, and about 5 mol% CaF2, which may be referred to herein as composition "PBF1."

[0044] Another specific example of such a glass composition includes about 48 mol% B2O3, about 9 mol% Na2O, about 19 mol% MgO, about 14 mol% CaO, and about 10 mol% NaF, which may be referred to herein as the composition "PBF1-Na."

[0045] Particle size distribution The glass composition according to the present disclosure is a particulate material comprising particles having a size of about 1 to about 50 μm. At least some of the particles are sized to sit in or on the dentinal tubules. The dentinal tubules have natural variations in diameter, primarily ranging in size from about 0.5 to about 8 μm, for example, from about 0.5 to about 5 μm. Thus, the glass composition according to the present disclosure can be used for desensitization of dentin, which can temporarily relieve pain associated with sensitive teeth.

[0046] In some embodiments, at least 75% of the particles making up the particulate material are smaller than 50 μm in size. In other embodiments, at least 85% or at least 95% of the particles are smaller than 50 μm in size. In some embodiments, at least 5% of the particles making up the particulate material are less than 7 μm in size.

[0047] In certain embodiments, the particulate material is comprised of a plurality of particles, with at least 5% of the particles smaller than 35 μm, at least 5% of the particles smaller than 15 μm, and at least 5% of the particles smaller than 7 μm.

[0048] In certain embodiments, the particulate material is comprised of a plurality of particles, at least 5% of the particles having a size between about 15 μm and about 35 μm, at least 5% of the particles having a size between about 6 μm and about 15 μm, and at least 5% of the particles having a size between about 3 μm and about 7 μm.

[0049] In some particular examples, the particulate material is comprised of a plurality of particles having a particle size distribution of about 5 μm Dx10, about 15 μm Dx50, and about 30 μm Dx90.

[0050] Decomposition Glass compositions according to the present disclosure degrade under physiological conditions, losing at least 5% by weight within 24 hours upon exposure to a buffered saline solution, hi some examples, the glass compositions can lose at least 20%, at least 40%, at least 60%, or at least 80% by weight within 24 hours upon exposure to a buffered saline solution.

[0051] Dentin desensitizing composition The glass composition according to the present disclosure can be formulated into a dentin desensitizing composition comprising an anhydrous, orally compatible carrier. The dentin desensitizing composition according to the present disclosure does not contain water since the glass composition deteriorates when exposed to water.

[0052] In the context of this disclosure, "anhydrous" should be understood to mean that the dentin desensitizing composition contains so little water that the glass composition remains capable of reducing dentin sensitivity over the expected life of the product, which refers to the longest expected time from when the dentin desensitizing composition is produced to when the dentin desensitizing composition is completely used up or discarded.

[0053] The orally compatible carrier used in the dentin desensitizing composition may be an orally compatible viscous carrier such as a mouthwash, a carrier formulated for mixing with additional ingredients to form a mouthwash, or a toothpaste, a dental gel, a prophylactic paste, a dental varnish, an adhesive, or a carrier formulated for mixing with additional ingredients to form a toothpaste. The orally compatible viscous carrier may have a viscosity of about 100 cP at 30° C. to about 150,000 cp at 30° C.

[0054] The dentin desensitizing composition may comprise a glass composition according to the present disclosure, as described above, wherein the glass composition comprises fluoride present in an amount sufficient for the desensitizing composition to comprise from about 100 ppm to about 5,000 ppm fluoride.

[0055] One example of a dentin desensitizing composition according to the present disclosure is a toothpaste that includes an abrasive, a detergent such as sodium lauryl sulfate, a fluoride source, an antimicrobial agent, a flavoring, a remineralizing agent, a sugar alcohol such as glycerol, sorbitol, or xylitol, another dentin desensitizing agent, a hydrophilic polymer such as polyethylene glycol, or any combination thereof. The glass composition may be about 0.5 to about 15% by weight of the toothpaste.

[0056] A specific example of a dentin desensitizing composition according to the present disclosure is a toothpaste comprising a glass composition according to the present disclosure, glycerin, silica, polyethylene glycol (such as PEG400), titanium dioxide, carbomer, and a sweetener (such as acesulfame potassium or sodium saccharin).

[0057] Another specific example of a dentin desensitizing composition according to the present disclosure is a toothpaste comprising a glass composition according to the present disclosure and α-carbomer, DL-limonene, glycerin, mint flavor, polyethylene glycol (e.g., PEG-8), silica, titanium dioxide, sodium lauryl sulfate, and a sweetener (e.g., acesulfame potassium or sodium saccharin).

[0058] Another example of a dentin desensitizing composition according to the present disclosure is a carrier comprising a glass composition according to the present disclosure, where the carrier is formulated to be mixed with additional ingredients to form a toothpaste.

[0059] Yet another example of a dentin desensitizing composition according to the present disclosure is a carrier formulated to be mixed with additional components to form a mouthwash. Particular examples of carriers include a glass composition according to the present disclosure, and: absolute alcohol, cetylpyridinium chloride, chlorhexidine, essential oils, benzoic acid, poloxamer, sodium benzoate, flavoring agents, coloring agents, or any combination thereof. Additional components that are mixed / mixed with the carrier to form a mouthwash include water, peroxide, cetylpyridinium chloride, chlorhexidine, essential oils, alcohol, benzoic acid, poloxamer, sodium benzoate, flavoring agents, coloring agents, or any combination thereof. The carrier and additional components may be held in separate compartments and mixed together before the mixture is used as a mouthwash. The separate compartments may be in the form of a multi-chambered bottle, such as a branched bottle.

[0060] Another example of a dentin desensitizing composition according to the present disclosure is a prophylactic paste (also called a "prophy paste") comprising a glass composition according to the present disclosure. Specific examples of contemplated saprophytic pastes include a glass composition according to the present disclosure, and: pumice, glycerin, diatomaceous earth (preferably fine grain), sodium silicate, methyl salicylate, monosodium phosphate, sodium carboxymethylcellulose, a sweetener (e.g., acesulfame potassium or sodium saccharin), a flavoring agent, a coloring agent, or any combination thereof.

[0061] method Glass compositions according to the present disclosure can be synthesized by mixing appropriate molar amounts of starting reagents; loading the precursor blend into a platinum crucible (Johnson Matthey, Noble Metals, PA); placing the loaded crucible in a furnace (Carbolite, RHF1600) at room temperature; heating the furnace (e.g., at a rate of 25°C / min) to an initial dwell temperature of 600°C; holding the temperature for 60 minutes; increasing the temperature to a dwell temperature of 1,100°C; holding the temperature for 60 minutes; and quenching the glass melt between two stainless steel plates.

[0062] It should be understood that the specific ramp rates, times, and temperatures above can be modified so long as the glass melts. A ramp rate of 10-20 degrees / minute and a hold at dwell temperature can remove at least some of the bubbles from the glass.

[0063] The resulting quenched glasses can be separately ground / milled in a planetary micromill (Pulverisette 7, Fritsch, Germany) and sieved through ASTM E-11 compliant sieves (Cole Palmer, USA) to obtain particles of <25 μm. The glasses can be stored under vacuum in glass scintillation vials.

[0064] The resulting glass composition includes oxides, while the starting reagents can include oxides, carbonates, or both. For example, the starting reagents can include boron oxide, rubidium carbonate, lithium carbonate, and calcium fluoride. Rubidium carbonate and lithium carbonate decompose in the furnace to release CO2 and generate the corresponding oxides.

[0065] Particle size is measured using a Malvern Mastersizer (MS) 3000 laser diffraction particle size analyzer. The glass powders are suspended separately in deionized water to a suspension opacity of 5-8%. The suspensions are measured using both a blue laser (λ = 470 nm) and a red laser (λ = 632.8 nm) and are measured five times (n = 5).

[0066] Fluoride release is measured by placing 0.1 g of the glass composition in 10 ml of TRIS buffered saline (BioUltra, Sigma Aldrich, Canada) in a 15 ml Falcon tube. The solution is stirred at 120 rpm and maintained at a temperature of 37° C. for the desired release period, e.g., 1, 3, 6, 12 or 24 hours. Upon completion, the liquid portion is decanted and filtered using a 0.22 μm filter (Sarstedt Syringe Filter, Canada) into a new clean 15 ml Falcon tube, which is capped and stored at 4° C. until the amount of fluoride is quantified. The concentration of released fluoride is quantified using an Accumet® AB250 pH / Ion Selective Electrode Meter (Accumet®) equipped with a fluoride electrode combination. Standard solutions are prepared using fluoride analytical standards dedicated to the ion selective electrode (NaF, 0.1 MF, Sigma Aldrich, Canada) and calibration cures are collected prior to analysis. Liquid extracts derived from the extraction of each composition were prepared for ion analysis according to the electrode manufacturer's instructions. Ion concentrations are reported as the mean of n=3±SD.

[0067] In the context of this disclosure, the mass loss of the glass composition is in relation to a solid glass cylinder of 6 mm length and 4 mm diameter. The glass cylinder is prepared by producing molten glass as described above, placing the molten glass into a stainless steel mold (6 mm length, 4 mm diameter) and quenching it by placing it between two stainless steel plates. The excess glass on the cylinder is carefully etched away by a speedy sharpening tool, and the remaining excess glass is removed using a grinding / polishing wheel with 240 grit sandpaper and pressure applied to the mold / glass on the wheel. The glass cylinder with uneven edges, bubbles, and chips is removed.

[0068] Mass loss for a given glass composition is measured using three cylinders. The length and diameter of each cylinder are measured and recorded three times (changing the measurement position) and recorded as the mean ± SD. The mass of each cylinder is measured separately (Sartorius Cubis, model MSU-224S 100DI, Cole Palmer). The three cylinders are placed in separate 50 mL Falcon tubes with 20 mL of TRIS-buffered saline (BioUltra, Sigma Aldrich, Canada) in each tube. The tubes are then placed in a shaking incubator (Thermos Scientific, MaxQ 4000) at 37 °C and agitated at 120 rpm for 24 h. After 24 h, the cylinders are filtered from the solution, washed with cold distilled H2O, and dried overnight in an oven at 37 °C. After drying, the length, diameter, and mass are measured.

[0069] The abrasivity of the compositions is determined by measuring the gloss and surface roughness of the resin composite or enamel surface after brushing with the composition. ESPE Filtek Supreme Ultra Universal Restorative, shade A2B (3M, St. Paul, Minnesota, USA) is cured in a metal split mold with a diameter of 12.7 mm and a thickness of 2 mm. Mylar sheets are placed above and below the mold, and glass plates are used to press the flats of the composite and squeeze out excess material. A broadband multiwave LED light curing unit (Valo Grand, Ultradent Products, South Jordan, Utah, USA) is placed directly on the specimen and cured for 20 seconds at standard settings. Excess material is removed by hand before mounting the specimen to be brushed.

[0070] The specimens are stored at 37°C in the dark for a minimum of 24 hours before use. The surfaces of the enamel specimens are prepared by polishing with different levels of grit to generate a flat and smooth surface. Low-grit sandpaper is used to create an initial flat surface (P800C, Klingspor, Haiger, Germany), which is then polished using larger amounts of grit. The final polishing step is performed on a cloth pad with 3 μm and then 0.3 μm alumina oxide powder slurry (Buehler Ltd., Lake Bluff, IL, USA). Each polishing step is performed for approximately 1 minute under hand pressure.

[0071] A custom-made brushing machine (Ultradent, South Jordan, USA) simulates tooth brushing of 10 specimens simultaneously. The toothbrushes (GμM brand 459PC, Sunstar, Guelph, Ontario, Canada) are equipped with a toothbrush that is loaded with a constant load of 176 g during brushing. The toothbrushes are replaced after 10,000 brush cycles. The specimens are covered with a minimum of 3 mm of toothpaste slurry in a 5:8 weight ratio with distilled water during brushing. The specimens are rotated to a different position every 2,500 brush cycles (ensuring that the specimens are brushed with the same toothpaste each time they are moved). 20,000 brush cycles represent approximately 2 years of brushing. The toothpaste repetitions and positions within the machine are randomized with a random number generator (for each substrate material), while the rotation of the toothbrushes is manually ensured that there are a minimum of two repetitions of the same toothpaste during one run.

[0072] The gloss of the composite and enamel surfaces is measured using a glossmeter (Novo-Curve G, Rhopoint Instruments, Hastings, UK). Gloss is measured at three random points and an average value is created for the surface. Glossmeter calibration is verified daily using traceable calibration tiles of high and low reflectance. Gloss is measured at 0, 5,000, 10,000, 15,000 and 20,000 brush cycles and new toothpaste slurry is used after the gloss is measured.

[0073] The average roughness of the surface was also measured before brushing and after 20,000 brushing cycles. An atomic force microscope (nGauge, ICSPI Corporation, Rev. 1.0, Waterroo, Ontario, Canada) was used to measure the average roughness at three different locations to form the average of the surface. An area of ​​25 × 25 μm was scanned at a speed of 1200 μs / pixel. Analysis was performed using Gwyddion (http: / / gwyddion.net) software. EXAMPLES

[0074] All glass compositions shown in Table 1 were synthesized by weighing out quantitative amounts of analytical grade reagents (boron oxide, rubidium carbonate, lithium carbonate, and calcium fluoride) (Sigma Aldrich, Canada). To ensure homogeneity, each formulation was mixed for 60 minutes. Each precursor blend was placed and packed into a 50 mL platinum crucible (Johnson Matthery, Noble Metals, Pennsylvania). The packed crucible was then placed into a furnace (Carbolite, RHF 1600) at room temperature. The furnace was heated (25°C / min) to an initial dwell temperature of 600°C and held for 60 minutes. The temperature was then increased (20°C / min) to a final dwell temperature of 1,100°C and held for 60 minutes. Upon removal, each glass melt was quenched between two stainless steel plates. The resulting quenched glasses were separately ground / milled in a planetary micromill (Pulverisette 7, Fritsch, Germany) and sieved through ASTM E-11 compliant sieves (Cole Palmer, USA) to obtain particles of <25 μm.

[0075] [Table 1]

[0076] The particle size distribution of the exemplary glasses in Table 1 is shown in Table 2.

[0077] [Table 2]

[0078] Here, it is to be understood that "Dx(#)" refers to the #% of particles that are smaller in size than the noted value. For example, BCF100 has a Dx(10) of 5.16 microns, which means that 10% of the particles are less than 5.16 microns in size.

[0079] The exemplary glass particles of Table 1 were evaluated for fluoride release in buffered saline solution over 12 and 24 hours using the method described above. The ppm values ​​of fluoride released are shown in Table 3.

[0080] [Table 3]

[0081] BCF201 was formulated into two toothpastes to test the abrasive effect of the glass particles and compare it to the abrasive effect of Sensodyne™ Whitening Restorative and Protect™ Toothpaste ("Sensodyne") and Colgate™ Optic White™ Toothpaste ("Colgate Optic"). The exemplary glass was formulated in (a) Colgate™ Enamel Health Sensitivity Relief™ (Colgate-Palmolive, Toronto, ON, Canada) ("Colgate EN") or (b) Gel 7HT (Germiphene, Brantford, ON, Canada) ("Gel"), a neutral pH fluoride gel toothpaste that does not contain any abrasive materials.

[0082] The results of the polishing tests are shown in the following tables and Figures 1-10. Table 4 shows the gloss of the resin composite surface after different numbers of brushing cycles with different toothpastes. Table 5 shows the gloss of the resin composite after different numbers of brushing cycles with different toothpastes. Table 6 shows the roughness of the resin composite surface after 20,000 brushing cycles with different toothpastes. Table 7 shows the roughness of the enamel surface after 20,000 brushing cycles with different toothpastes.

[0083] [Table 4]

[0084] [Table 5]

[0085] [Table 6]

[0086] [Table 7]

[0087] Further exemplary glass compositions according to the present disclosure are shown in Table 8 along with glass compositions that are not examples of the present disclosure showing the mol percentages of the different components.

[0088] [Table 8-1]

[0089] [Table 8-2]

[0090] The exemplary glass compositions and additional compositions shown in Table 8 were selected based on the design of the mixture (Design Expert 8.0.4, Stat-Ease Inc.) to evaluate the effect of various ranges of ingredients on the glass composition.

[0091] The glass compositions were synthesized as described above. Briefly, sufficient analytical grade reagents (Sigma Aldrich, Canada) were weighed out to form each of the above compositions. To ensure homogeneity, each formulation was mixed for 60 minutes. Each precursor blend was placed and packed into a 50 mL platinum crucible (Johnson Matthery, Noble Metals, Pennsylvania). The packed crucible was then placed into a furnace (Carbolite, RHF 1600) at room temperature. The furnace was heated (25°C / min) to an initial residence temperature of 600°C and held for 60 minutes. The temperature was then increased (20°C / min) to a final residence temperature of 1,100°C and held for 60 minutes. Upon removal, each glass melt was quenched between two stainless steel plates.

[0092] The following compositions are specific examples of compositions that formed glasses under the quench conditions described above, and such conditions represent one option for standard quench conditions suitable for manufacturing scale processes.

[0093] [Table 9]

[0094] The resulting quenched glasses for the exemplary compositions listed in Table 9 had the following bulk properties:

[0095] [Table 10]

[0096] The resulting quenched glasses for the exemplary compositions listed in Table 9 were separately ground / milled in a planetary micromill (Pulverisette 7, Fritsch, Germany) and sieved through an ASTM E-11 compliant sieve (Cole Palmer, USA) to obtain particles of <25 μm.

[0097] The particle size distributions of the exemplary glasses listed in Table 9 are shown in Table 11. BCF315, BCF326 decomposed too quickly in deionized water to obtain accurate particle size measurements.

[0098] [Table 11]

[0099] Exemplary glass particles listed in Table 9 were evaluated for mass loss and fluoride release in buffered saline solution at 1, 4, and 24 hours. Samples were prepared in 15 mL Erlenmeyer tubes (n=3), weighed, and recorded. 0.1 grams of each glass powder (<25 microns) was weighed separately into 10 mL TRIS buffered saline (BioUltra, Sigma Aldrich, Canada) in a weighed 15 mL Falcon tube. The tubes were sealed with parafilm and then placed in a shaking incubator at 37° C. and agitated at 120 rpm for four separate time points: 5 minutes, 30 minutes, 1 hour, 3 hours, 24 hours, and 48 hours. After the designated times, the tubes were removed from the incubator and the solutions were immediately centrifuged (Eppendorf, Centrifuge 5702) at 3.0 RCF / 4.4 RPM for 15 minutes. The supernatant was decanted into a fresh 15 mL Falcon tube. Additionally, samples of the 48-h incubated powder were resuspended in 10 mL of fresh TRIS-buffered saline by vortex mixing and incubated for an additional 8 h (for a total incubation of 56 h). The reincubated powder was treated in the same manner as the other samples. The pellets were dried in their respective Falcon tubes in a 50° C. oven.

[0100] Fluoride ion release was measured using an Accμmet AB250 pH / ion-selective meter equipped with a fluoride electrode (Fisher Scientific). To calibrate the probe, six standard solutions were prepared using fluoride analytical standards for ion-selective electrodes (NaF, 0.1F, Sigma Aldrich, Canada). Standards with fluoride concentrations of 1000 ppm, 100 ppm, 10 ppm, 1 ppm, 0.1 ppm, and 0.01 ppm, respectively, were synthesized using TRIS-buffered saline (BioUltra, Sigma Aldrich, Canada) as the solvent. TISAB concentrate (4.5 mL) was added to each standard prior to calibration (following the manufacturer's instructions). Once the probe was calibrated, the slope of the standards was checked to ensure it was within the range from the instructions. TISAB concentrate (1.0 mL) was added to the decanted supernatant and then measured for its fluoride concentration using the calibrated probe. Ion concentrations are reported as mean ± SD.

[0101] The mass loss and ppm values ​​of released fluoride are shown in Table 12. BCF314 was completely degraded in the buffered saline solution before the 1 hour time point and no fluoride source was included.

[0102] [Table 12]

[0103] The compositions listed in Table 8 reflect the design space. The results of the compositions tested provided the following equations that may allow for relative comparison of different compositions and / or may be useful in identifying trends associated with different components of the composition. Although experimental and modeling errors prevent absolute prediction of glass properties, the equations can be used to guide and refine glass composition design. Used together, these models will help suggest which factors may be traded off in tailoring multi-component compositions within the composition space tested. In the following equations, the values ​​of the listed components are given as percentages (rather than decimals). For example, 50 mol% B2O3 is "50" (rather than "0.5").

[0104] Glass is generally expected to form under the quench conditions tested if the following formula is less than or equal to 1.60: (2.01×e y +0.99) / (1+e y ) Here, y=-0.086622×[B2O3]+0.14169×[Li2O]-0.565849×[ZnO]+0.192175×[Na2O]-0.461537×[CaF2]+0.036 636×[KF]+0.00365×[NaF]+0.191201×[SnF2]+0.192612×[RbO2]+0.199999×[SrO]+0.01393×[B2O3]×[ZnO] +0.012239×[B2O3]×[CaF2]-0.012412×[Li2O]×[CaF2]-0.013904×[Li2O]×[RbO2]-0.010857×[ZnO]×[CaF2 ]-0.013296×[ZnO]×[RbO2]-0.010699×[ZnO]×[SrO]+0.010128×[CaF2]×[KF]-0.012103×[CaF2]×[SrO].

[0105] The density of glass can generally be predicted using the following formula: ρ=0.018783×[B2O3]+0.026444×[Li2O]+0.046191×[ZnO]+0.033814×[Na2O]+0.0 39196×[CaF2]+0.026997×[KF]+0.029458×[NaF]+0.049441×[SnF2]+0.047057×[R b O2] + 0.054984 × [SrO] Approximately 1.3g / cm 3 to about 2.2 g / cm 3 Glass densities up to 1.3 and 2.2 g / cm3 can be particularly beneficial in non-aqueous oral care formulations. Glycerol and silica are the main liquid and solid components of non-aqueous toothpastes, with densities of 1.3 and 2.2 g / cm3, respectively. 3 has a density of

[0106] Glass transition temperature (T g ) can generally be predicted using the following formula: T g =3.49398×[B2O3]+3.66342×[Li2O]+6.38755×[ZnO]+6.23689×[Na2O]+6.43079×[CaF2 ]+3.31695×[KF]+5.04074×[NaF]+9.88761×[SnF2]+3.29777×[RbO2]+10.51264×[SrO] It should be understood that phase separated glasses can exhibit multiple glass transitions, the magnitude of which does not necessarily represent the volume distribution of the phases. Although the above formula predicts the onset of the glass transition, if phase separation occurs, the predicted onset may not be the main glass transition of the composition. Thus, the predicted glass transition temperature may differ significantly from the measured main glass transition temperature.

[0107] The formula for the percent mass loss after 1 hour under the test conditions is: (100×e y ) / (1+e y ) Here, y = 0.088098 × [B2O3] + 0.062481 × [Li2O] - 0.262486 × [ZnO] + 0.05542 × [Na2O] - 0.165517 × [CaF2] + 0.089171 × [KF] + 0.075875 × [NaF] + 0.10439 × [SnF2] + 0.109897 × [RbO2] - 0.089987 × [SrO] The above equation is very predictive in identifying glass compositions that show complete dissolution within one hour under the conditions tested, and may be useful in identifying other glasses that degrade under this time frame. Furthermore, although the equation does not provide accurate mass loss estimates for slower decomposing compositions, the equation may be useful in predicting the relative change in decomposition that is expected to occur with a change in composition. Such relative changes may be used as a guide for glass composition design.

[0108] The formula for fluoride release (ppm) after 1 hour under test conditions is: (2750×e y ) / (1+e y ) Here, y = -0.05785 x [B2O3] -0.15837 x [Li2O] -0.170872 x [ZnO] -0.184773 x [Na2O] +0.05638 x [CaF2] +0.101381 x [KF] +0.053886 x [NaF] -0.307462 x [SnF2] -0.183034 x [RbO2] -0.184126 x [SrO] While the above equation does not provide an accurate estimate of the amount of fluoride released for all glass compositions, the model is still useful for predicting the relative changes in fluoride release that can be expected to occur with changes in composition.

[0109] PBF1 was synthesized by weighting 11.60 g B2O3, 5.30 g Na2CO3, 2.69 g MgO, 3.33 g CaCO3, and 0.7 g CaF2 (Sigma Aldrich, Canada). The starting materials were mixed for 60 min to ensure homogeneity. The blend was placed and packed into a 50 mL platinum crucible (Johnson Matthey, Noble Metals, PA). The packed crucible was then placed into a furnace (Carbolite, RHF 1600) at room temperature. The furnace was heated (25 °C / min) to an initial occupancy temperature of 600 °C and held for 60 min. The temperature was then increased (20 °C / min) to a final occupancy temperature of 1,200 °C and held for 60 min. Upon removal, the glass melt was quenched between two stainless steel plates. The resulting quenched glasses were separately ground / milled in a planetary micromill (Pulverisette 7, Fritsch, Germany) and sieved through ASTM E-11 compliant sieves (Cole Palmer, USA) to obtain particles of <25 μm.

[0110] Comparative glass compositions (designated Comparative Examples (CE) 1 and 2) were similarly synthesized using 5.80 g B2O3, 23.66 g P2O5, 5.30 g Na2CO3, 1.34 g MgO, 6.67 g CaCo3, and 0.70 g CaF2, with CE1 being about 25 mol% B2O3, about 25 mol% P2O5, about 15 mol% Na2O, about 10 mol% MgO, about 20 mol% CaO, and about 0.70 mol% CaF2. and 5.80 g B2O3, 23.66 g P2O5, 7.07 Na2CO3, 1.34 g MgO, 5.00 g CaCO3, and 0.70 g CaF2, and CE2 had about 25 mol% B2O3, about 25 mol% P2O5, about 20 mol% Na2O, about 10 mol% MgO, about 15 mol% CaO, and about 5 mol% CaF2.

[0111] The density of glass powder is 1cm 3 The measurements were made using an AccuPyc 1340 helium pycnometer (Micromerix, USA) equipped with an insert. Prior to use, the volume was measured at 0.718512 cm3 The pycnometer was calibrated using a standard of 1000 ppm. For glass analysis, the insert was filled with approximately 0.5-0.7 grams of glass powder. Three samples of each glass were measured, and each measurement is the average of 10 readings.

[0112] The density of PBF1 is 2.5951±0.0072g / cm 3 The density of CE1 was measured as 2.7079 ± 0.0021 g / cm 3 The CE2 density was measured as 2.6749 ± 0.0013 g / cm 3 was measured.

[0113] Fluoride release and mass loss were measured for PBF1, CE1 and CE2. Samples were prepared in 15mL Erlenmeyer tubes (n=3), weighed and recorded. 0.1 grams of each glass powder (<25 microns) was weighed separately into 10mL TRIS buffered saline (BioUltra, Sigma Aldrich, Canada) in a weighed 15mL Falcon tube. The tubes were sealed with parafilm and then placed in a shaking incubator at 37°C and agitated at 120 rpm for four separate time points: 5 minutes, 30 minutes, 1 hour, 3 hours, 24 hours and 48 hours. After the designated times, the tubes were removed from the incubator and the solutions were immediately centrifuged (Eppendorf, Centrifuge 5702) at 3.0RCF / 4.4 RPM for 15 minutes. The supernatant was decanted into a fresh 15mL Falcon tube. Additionally, samples of the 48-h incubated powder were resuspended in 10 mL of fresh TRIS-buffered saline by vortex mixing and incubated for an additional 8 h (for a total incubation of 56 h). The reincubated powder was treated in the same manner as the other samples. The pellets were dried in their respective Falcon tubes in a 50° C. oven.

[0114] Fluoride ion release was measured using an Accμmet AB250 pH / ion-selective meter equipped with a fluoride electrode (Fisher Scientific). To calibrate the probe, six standard solutions were prepared using fluoride analytical standards for ion-selective electrodes (NaF, 0.1F, Sigma Aldrich, Canada). The sodium fluoride concentrations of the standards were synthesized as follows: 1000 ppm, 100 ppm, 10 ppm, 1 ppm, 0.01 ppm, and 0.001, respectively, using TRIS-buffered saline (BioUltra, Sigma Aldrich, Canada) as the solvent. TISAB concentrate (4.5 mL) was added to each standard prior to calibration (according to the manufacturer's instructions). Once the probe was calibrated, the slope of the standards was checked to ensure it was within the range from the instructions. TISAB concentrate (1.0 mL) was added to the decanted supernatant and then measured for its fluoride concentration using the calibrated probe. Ion concentrations are reported as mean ± SD.

[0115] The amount of fluoride ion released by PBF1 was measured to be 89±2 ppm at 5 min, 94±3 ppm at 30 min, 105±5 ppm at 1 hr, and 94±7 ppm at 3 hr. No measurable fluoride ion was released by CE1 or CE2.

[0116] Mass loss was calculated by comparing the mass of the dried sample after exposure to TRIS-buffered saline with the initial mass of the sample. The mass loss of PBF1 was 42.0 ± 2.1% after 5 min, 47.3 ± 2.7% after 30 min, 51.5 ± 4.3% after 1 h, 41.7 ± 5.7% after 3 h, 70.1 ± 6.8% after 24 h, and 100% after 48 h.

[0117] The particle size of seven different samples of PBF1 was measured using a Malvern Mastersizer 3000 model laser diffraction particle size analyzer. Glass particles were separately suspended in distilled water to obtain 2-5% opacity. Prior to analysis, the glass powder was stored in a vacuum desiccator and removed for analysis, 3 x 5 times, lasting approximately 20 s / time. The suspensions were measured using both blue (λ = 470 nm) and red (λ = 632.8 nm) lasers (n = 5).

[0118] [Table 13]

[0119] Apatite formation in simulated body fluids was observed in PBF1, but was not evident in CE1 or CE2. The simulated body fluids were synthesized according to the methods and instructions published by Kokubo and Takadama (Kokubo, T. and Takadama, H. Biomaterials (2006) 27:15, pp 2907-2915).

[0120] A 1 L batch of SBF was prepared in a 1000 mL Nalgene bottle (FEP bottle). The prepared SBF was stored at room temperature for 24 h immediately after synthesis to ensure stability before experimental use. SBF was stored in a tightly capped Nalgene bottle and kept at 6 °C if not immediately needed (maximum of 30 days for experimental use).

[0121] According to the TCO4 method (published in Mason, ALB, Kim, TB, Valliant, EM et al. J Mater Sci: Mater Med (2015) 26:115), 0.75 g of glass powder of each glass composition (n=3) as synthesized above was immersed in 50 mL of SBF in a polyethylene container. The container was then placed in an incubator orbital shaker at 37°C and agitated at 120 rpm for three time points: 30 min, 3 h, and 12 h. After the elapsed time, each sample was vacuum filtered through Whatman 42 or 5 grade filter paper (particle retention 2.5 μm) to recover the solid material from the solution. The solid was immediately washed with distilled water and acetone to stop further reaction.

[0122] The filtered samples were dried in a vacuum desiccator for further analysis. Imaging of each sample was performed using a Hitachi S-4700 FEG (Hitachi, Chula Vista, Ca) scanning electron microscope operated at 3 KV and 15 mA at magnifications of 1000× and 10000×. Samples were mounted on stubs using double-sided carbon tape and sputter coated with gold-palladium for 70 s (Leica EM ACE200, Wetzlar, Germany). Scanning electron microscope images of PBF1 at 30 min, 3 h, and 12 h are shown in Figures 11-14.

[0123] PBF1 also developed an application protocol and evaluated dentin tubule occlusion by statistical analysis of SEM images graded by two assessors according to a categorical occlusion scale. Sections of human dentin (approximately 1-1.5 mm thick) were prepared from caries-free, unreserved molar crowns perpendicular to the long axis of the root using a diamond disc saw. Each section was etched with 10% citric acid for 2 min, followed by rinsing with water for 60 s, sonication for 2 min, and rinsing with water for another 60 s. Each section was placed in a 25 mm diameter mold and covered with 3 mm deep acrylic resin. Once the resin had hardened, the dentin surface was polished sequentially with 800 and 2500 grit paper for a mirror finish. After rinsing with deionized water, the surface was etched, sonicated, and rinsed again. The integrity, tubule density, and patency of the specimens were again examined under a light microscope and then with a SEM.

[0124] One dentin specimen was assigned to each treatment group. The dentin specimen was treated with (i) the unformed mixture of exemplary glass particles, (ii) the test toothpaste containing the exemplary mixture of glass particles, or (iii) the control toothpaste without additional glass particles. The unformed mixture was applied for 10 seconds using a non-powdered nitrile gloved finger. The test and control toothpastes were applied to the specimen with an electric toothbrush for 10 seconds. The toothpaste was left on for 30 seconds and then rinsed until all visible paste was removed. This was repeated for a total of four applications of toothpaste.

[0125] Dentin specimens were dried in an oven at 37°C for 1 hour, coated with gold, and visualized using a Phenom ProX scanning electron microscope. Five images at 3000x magnification were taken of different sections of each specimen, where the tubules were perpendicular to the surface. Each 3000x photomicrograph was examined by two single-blind assessors for the extent of dentinal tubule obliteration based on a 5-point categorical scale. Grading was defined as follows: 1. Occlusion (100% occlusion) 2. Nearly blocked (75% blocked) 3. Equal (50% occlusion) 4. Nearly non-obstructed (25% obstruction) 5. Non-occlusion (0% occlusion)

[0126] The mean score for each image was calculated from the scores of the two assessors, and standard deviations were calculated, but formal statistical comparisons were not performed because only one dentin specimen was used per treatment group.

[0127] Seven different treatment arms were tested, as outlined in Table 14.

[0128] [Table 14]

[0129] Each sample treatment group was tested on dentin specimens as described above and five SEM photomicrographs of each specimen were taken at ×3000. Each photomicrograph was categorically scored by two assessors. The average scores for each photomicrograph and the five photomicrographs per specimen were combined to determine the group mean scores and standard deviations (see Table 15).

[0130] [Table 15]

[0131] The baseline mean score of 4.90 for treatment group 1 indicates that virtually all dentinal tubules were unobstructed. The mean score of 1.50 for the shapeless PBF1 rubbed directly into the dentin specimen indicates nearly complete tubule obliteration.

[0132] Treatment groups 5, 6 and 7 (control groups lacking PBF1 or other glass compositions according to the present disclosure) had mean obstruction scores ranging from 3.2 to 3.6. Treatment groups 3 and 4 (commercial toothpastes containing 5% or 15% PBF1 w / w) had lower mean obstruction scores, indicating a higher degree of tubular obstruction. The degree of obstruction for the commercial toothpaste Sensodyne™ Complete Protection increased from approximately 30% obstruction (score 3.6) to approximately 50% obstruction (score 2.5) with the addition of 15% w / w of PBF1.

[0133] PBF1 was further evaluated for dentin tubule occlusion using 5% w / w PBF1 sodium lauryl sulfate (SLS) paste. In this evaluation, PBF1 and control toothpastes were applied to three different dentin samples from each treatment group. Each sample was brushed once with the treated toothpaste for 2 minutes. Specifically, each dentin sample was brushed with 0.25 g of treated toothpaste for 120 seconds, followed by rinsing with DI water for 30 seconds. The 5% PBF1-SLS paste resulted in a mean occlusion score of 2.7 ± 0.84. The SLS paste without PBF1 resulted in a mean occlusion score of 3.80 ± 1.03. A control test using Sensodyne™ Repair & Protect resulted in a mean occlusion score of 3.90 ± 0.66.

[0134] PBF1-Na was prepared according to the protocol described above. Briefly, the glass was synthesized by weighting 11.05 g B2O3, 3.36 g Na2CO3, 2.56 g MgO, 4.77 g CaCO3, and 1.33 g NaF (Sigma Aldrich, Canada). The starting materials were mixed for 60 minutes to ensure homogeneity. The blend was placed and packed into a 50 mL platinum crucible (Johnson Matthey, Noble Metals, Pennsylvania). The packed crucible was then placed into a furnace (Carbolite, RHF 1400) at room temperature. The furnace was heated (25 °C / min) to an initial dwell temperature of 600 °C and held for 60 minutes. The temperature was then increased (20 °C / min) to a final dwell temperature of 1,200 °C and held for 60 minutes. Upon removal, the glass melt was quenched between two stainless steel plates. The resulting quenched glasses were separately ground / milled in a planetary micromill (Pulverisette 6, Fritsch, Germany) and sieved through ASTM E-11 compliant sieves (Cole Palmer, USA) to obtain particles of <25 μm.

[0135] The particle size of ten different samples of PBF1-Na was measured as described above.

[0136] [Table 16]

[0137] The density, % crystallinity, and glass transition temperature of the ten samples were also measured as described above.

[0138] [Table 17]

[0139] Mass loss and fluoride release after 24 hours for 10 different samples were also measured as above.

[0140] [Table 18]

[0141] In the foregoing description, for purposes of explanation, numerous details are set forth in order to provide a thorough understanding of the embodiments. However, it will be apparent to one skilled in the art that these specific details are not required. Thus, what has been described is merely illustrative of applications of the described embodiments, and numerous modifications and variations are possible in light of the above teachings.

[0142] Because the above description provides examples, it will be understood that modifications and variations may be made to the specific examples by those skilled in the art. Accordingly, the claims should not be limited by the specific examples described herein, but should be construed in a manner consistent with the specification as a whole.

Claims

1. About 50 mol% to about 95 mol% of B ２ O ３ ; About 5 mol% to about 50 mol% of CaO, MgO, and K ２ O and Na ２ O, one or both of them, and optionally ZnO and / or SrO; 0 mol% of CuO; less than 0.1 mol% of BaO; and Less than 0.1 mol% of P ２ O ５ a glass composition comprising The glass composition contains less than 30 mol% of Rb ２ O and the glass composition is at least a four-component system, the above glass composition.

2. About 50 mol% to about 80 mol% of B ２ O ３ The glass composition according to claim 1, comprising

3. The glass composition according to claim 1, wherein the glass composition contains about 5 mol% to about 30 mol% of ZnO.

4. The glass composition according to claim 1, wherein the glass composition contains about 5 mol% to about 30 mol% of SrO.

5. The glass composition according to claim 1, wherein the glass composition contains about 5 mol% to about 30 mol% of ZnO and about 5 mol% to about 30 mol% of SrO.

6. The glass composition contains 0 mol% of CuO, 0 mol% of BaO, and 0 mol% of P ２ O ５ The glass composition according to claim 1, which contains

7. The glass composition according to any one of claims 1 to 6, wherein the glass composition is a particulate material containing particles having a size of about 1 to about 50 μm, and at least 75% of the particles have a size smaller than 50 μm.

8. The glass composition according to any one of claims 1 to 6, wherein the glass composition is a particulate material containing particles having a size of about 1 to about 50 μm, and at least 85% of the particles have a size smaller than 50 μm.

9. The glass composition according to any one of claims 1 to 6, wherein the glass composition is a particulate material containing particles having a size of about 1 to about 50 μm, and at least 95% of the particles have a size smaller than 50 μm.

10. The glass composition is a particulate material containing particles having a size of about 1 to about 50 μm, at least 5% of the particles have a size smaller than 35 μm, at least 5% of the particles have a size smaller than 15 μm, and at least 5% of the particles have a size smaller than 7 μm, the glass composition according to any one of claims 1 to 6.

11. The glass composition is a particulate material containing particles having a size of about 1 to about 50 μm, at least 5% of the particles have a size of about 15 μm to about 35 μm, at least 5% of the particles have a size of about 6 μm to about 15 μm, and at least 5% of the particles have a size of about 3 μm to about 7 μm, the glass composition according to any one of claims 1 to 6.

12. The glass composition is a particulate material containing particles having a size of about 1 to about 50 μm, about 10% of the particles have a size smaller than 5 μm, about 50% of the particles have a size smaller than 15 μm, and about 90% of the particles have a size smaller than 30 μm, the glass composition according to any one of claims 1 to 6.

13. (i)The glass composition according to any one of claims 7 to 12; and (ii)An anhydrous orally acceptable carrier A dentin desensitizing composition comprising the same.

14. The dentin desensitizing composition according to claim 13, wherein the orally acceptable carrier is mouse wash.

15. The dentin desensitizing composition according to claim 13, wherein the orally acceptable carrier is formulated to be mixed with mouse wash.

16. The dentin desensitizing composition according to claim 13, wherein the orally acceptable carrier is an orally acceptable viscous carrier.

17. The dentin desensitizing composition according to claim 16, wherein the orally acceptable viscous carrier has a viscosity of about 100 cP at 30°C to about 150,000 cp at 30°C.

18. The dentin desensitizing composition according to claim 16, wherein the orally acceptable viscous carrier is toothpaste, dental gel, prophylactic paste, dental varnish, or adhesive.

19. About 5 mol% to about 10 mol% of CaF ２ , SnF ２ , NaF, KF, or a fluoride provided as any combination thereof; About 90 mol% to about 95 mol% of B ２ O ３ , Na ２ O, MgO, and CaO, and combinations of boron, magnesium, Na and any K, and Ca and any Sn in the glass composition are present in an elemental ratio of about 20:about 4:about 6:about 3, respectively A glass comprising the same.

20. Approximately 50 mol% of B ２ O ３ , Approximately 15 mol% of Na ２ O, About 20 mol% of MgO, About 10 mol% of CaO, and About 5 mol% of NaF, KF, CaF ２ , SnF ２ , or any combination thereof The glass according to claim 19, comprising the same.

21. About 5 mol% of CaF ２ The glass according to claim 20, comprising

22. The glass according to claim 19, comprising about 10 mol% of NaF.

Images