Glass composition

Abstract

A glass composition that can be formulated for a dentin desensitizing composition is provided. [Solution] The present disclosure provides a glass composition comprising about 20 mol% to 45 mol% B2O3 and about 10 mol% to about 80 mol% of one or more glass components selected from the group consisting of CaO and MgO. The glass composition also comprises less than 0.1 mol% CdO. The glass composition can include one or more of Na2O, K2O, and a phosphate source, wherein the sum of B2O3 and the phosphate source is about 60 mol% or less. The glass composition can include a fluoride source. The glass composition can be used to desensitize dentin. The present disclosure also provides dentin desensitizing compositions, as well as methods and uses of the disclosed glass compositions.

Description

[Technical Field]

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS This patent application claims the benefit of priority from U.S. Application No. 62 / 987,192, filed March 9, 2020, the entire contents of which are incorporated herein by reference.

[0002] Field The present disclosure relates to glass compositions that can be formulated for dentin desensitizing compositions. [Background technology]

[0003] background The following paragraphs are not an admission that what is discussed therein is prior art or part of the knowledge of those skilled in the art.

[0004] Dentin hypersensitivity is tooth pain arising from exposed dentin surfaces in response to stimuli such as heat, vapor, touch, osmotic pressure, chemical, or electrical stimuli. Dentin hypersensitivity can be caused by gingival recession (recession of the gums) with exposed root surfaces, loss of cementum and smear layers, tooth wear, acid erosion, periodontal root planing, or tooth bleaching.

[0005] Dentin contains thousands of microtubular structures radiating outward from the dental pulp. Alterations in the flow of plasma-like biological fluid present in the dentinal tubules can trigger mechanoreceptors present in nerves located at the dental pulp surface, thereby inducing a pain response. This hydrodynamic flow can be increased by cold, air pressure, dryness, sugar, acidity (dehydrating chemicals), or forces acting on the tooth. Hot or cold foods or drinks and physical pressure are typical triggers for individuals with sensitive teeth.

[0006] There is no universally accepted gold standard treatment that reliably provides long-term relief from dental sensitivity pain, however, treatments can be divided into in-office treatments (i.e., those intended to be applied by a dentist or dental therapist) or treatments that are available over the counter or can be performed at home by prescription.

[0007] The mechanism of action of these treatments is either occlusion of dentinal tubules or desensitization of nerve fibers / blocking of nerve conduction.

[0008] Introduction The following introduction is intended to introduce the reader to this specification, but is not intended to define the invention. One or more inventions may reside in combinations or subcombinations of apparatus elements or method steps described below or elsewhere in this document. The inventors of the present invention do not waive or abstain from any rights to one or more inventions disclosed herein merely because they do not recite such other invention(s) in the claims.

[0009] E.I. Kamitsos, in J. Phys. Chem. 1989, 93, 1604-1611, discloses alkali metal borate glasses of the formula xMO*(1-x)BO, where M is Li, Na, K, Rb, or Cs, and x is 0 to 0.4. That is, Kamitsos teaches alkali metal borate glasses containing at least 60 mole percent BO.

[0010] YD Yiannopolous and EI Kamitsos, in Phys. Chem. Glasses, 2001, 42(3), 164-72, studied alkaline earth borate glasses of the formula xMO*(1-x)B2O3, where M is Mg, Ca, Sr, or Ba, and x is between 0.15 and 0.55. Yiannopolous and Kamitsos state in Table 1 that the glass-forming region when M is Mg is when x is between 0.45 and 0.55, and when M is Ca, the glass-forming region is when x is between 0.33 and 0.50.

[0011] One or more of the described embodiments seek to address or ameliorate one or more drawbacks associated with dentin desensitizing compositions comprising particulate materials that occlude dentinal tubules. In some embodiments, the disclosed particulate materials substantially degrade under ambient conditions in 12 to 24 hours. In some embodiments, the disclosed particulate materials provide a controlled release of fluoride over the same period. In some embodiments, the disclosed particulate materials provide a controlled release of potassium over the same period. Summary of the Invention

[0012] Glass compositions according to the present disclosure include about 20 mol% to 45 mol% B2O3 and about 10 mol% to about 80 mol% CaO and one or more glass components selected from the group consisting of MgO. Glass compositions according to the present disclosure also include less than 0.1 mol% CdO. The glass compositions may further include less than 0.1 mol% CuO, less than 0.1 mol% Li2O, less than 0.1 mol% Rb2O, less than 0.1 mol% BaO, less than 0.1 mol% SrO, less than 0.1 mol% SiO2, or any combination thereof.

[0013] Glass compositions according to the present disclosure can include one or more glass components selected from the group consisting of Na2O, K2O, and a phosphate source. When the composition includes a phosphate source, the total moles of B2O3 and the phosphate source is about 60 mol% or less. The phosphate source can be P2O5, NaH2PO4, Na2HPO4, Na3PO4, KH2PO4, K2HPO4, K3PO4, or any combination thereof.

[0014] Glass compositions according to the present disclosure may additionally or alternatively include up to about 45 mol% CaF2, SnF2, NaF, KF, Na2PO3F, or combinations thereof.

[0015] One exemplary composition according to the present disclosure includes about 43 mol% B2O3, about 21 mol% MgO, about 21 mol% CaO, and about 15 mol% Na2O, such as 43.0 mol% B2O3, 20.7 mol% MgO, 20.7 mol% CaO, and 15.6 mol% Na2O.

[0016] Glass compositions according to the present disclosure can be in the form of bulk glass or granular materials prepared from bulk glass. The chemical composition is the same between the bulk glass and the granular material formed therefrom. The granular material can include particles ranging in size from about 1 to about 50 μm. At least 75% of the particles can be less than 50 μm in size, at least 5% of the particles can be less than 7 μm in size, or both.

[0017] Some exemplary glass compositions formulated as particulate materials may lose at least 5% by weight within 24 hours when exposed to a buffered saline solution. Some exemplary compositions may lose at least 20, at least 40, at least 60, or at least 80% by weight within 24 hours when exposed to a buffered saline solution. Other exemplary glass compositions formulated as particulate materials may lose less than 5% by weight after 24 hours of exposure to a buffered saline solution.

[0018] The glass compositions according to the present disclosure may be formulated into dentin desensitizing compositions such as toothpastes, prophylactic pastes, dental varnishes, mouthwashes, dental gels or binders. The dentin desensitizing compositions according to the present disclosure are substantially free of water.

[0019] Glass compositions according to the present disclosure can be used to desensitize dentin, such as in methods comprising applying a toothpaste, prophylactic paste, dental varnish, mouthwash, dental gel or bonding agent according to the present disclosure to the dentin of an individual. DETAILED DESCRIPTION OF THE INVENTION

[0020] Detailed Description The glass composition according to the present disclosure includes about 20 mol% to 45 mol% B2O3 and about 10 mol% to about 80 mol% of one or more glass components selected from the group consisting of CaO and MgO. The glass composition according to the present disclosure also includes less than 0.1 mol% CdO.

[0021] Glass compositions according to the present disclosure can include one or more glass components selected from the group consisting of NaO, KO, and a phosphate source. When the composition includes a phosphate source, the total molar amount of B2O3 and the phosphate source is about 60 mol% or less. For example, exemplary compositions can include any combination of B2O3 and a phosphate source, with the total molar amount being about 25 mol% to about 30 mol%, about 30 mol% to about 35 mol%, about 35 mol% to about 40 mol%, about 40 mol% to about 45 mol%, about 45 mol% to about 50 mol%, about 50 mol% to about 55 mol%, or about 55 mol% to about 60 mol%. Furthermore, the phosphate source can be, for example, less than 40 mol%, less than 35 mol%, less than 30 mol%, less than 25 mol%, less than 20 mol%, less than 15 mol%, less than 10 mol%, or less than 5 mol%. The phosphate source can be P2O5, NaH2PO4, Na2HPO4, Na3PO4, KH2PO4, K2HPO4, K3PO4, or any combination thereof.

[0022] Glass compositions according to the present disclosure may include up to about 45 mol% CaF2, SnF2, NaF, KF, Na2PO3F, or combinations thereof.

[0023] The glass composition can be formulated as a granular material containing particles having a size of about 1 to about 50 μm. The glass composition can include at least some particles sized to luminally occlude dentinal tubules, thereby desensitizing dentin. In the context of the present disclosure, particles sized to luminally occlude dentinal tubules should be understood to mean that the particles are lodged in or on the dentinal tubules, reducing the movement of dentinal fluid. The glass composition can include at least some particles sized to provide surface occlusion of dentinal tubules, thereby desensitizing dentin.

[0024] It should be understood that the phrase "about X mol % to about Y mol % of one or more glass components" refers to the total mol % of the glass components, and not the mol % percentage of the individual components. For example, a glass composition according to the present disclosure may include 5 mol % each of CaO and MgO to provide the indicated 10 mol % of one or more glass components selected from the group consisting of CaO and MgO.

[0025] It should be understood that the disclosure of a range of possible values ​​also includes the disclosure of any value or subrange within the stated range, including the endpoints. For example, the possible range of "1 to 100" also includes, for example, 1, 10, 25 to 57, 32 to 84, 25 to 84, and 32 to 75.

[0026] It is understood that "about X mole %" refers to any value within ±2% of the reported percentage. For example, "about 10 mole %" refers to values ​​between 8 mole % and 12 mole %, since all of these values ​​fall within ±2% of the reported 10%. Also, "about 50 mole %" refers to values ​​between 48 mole % and 52 mole %, since all of these values ​​fall within ±2% of the reported 50%.

[0027] It should be understood that a range of possible values ​​is also a disclosure of any value or subrange within the stated range, including the endpoints. For example, a possible range of "1 to 100" is also a disclosure of, for example, 1, 10, 25 to 57, 32 to 84, 25 to 84, and 32 to 75.

[0028] It should be understood that "about X μm" in the context of particle size is determined based on the tolerances set forth by ASTM E-11 for the test sieve of the indicated size. For example, a 50 μm test sieve has a tolerance of 3 μm. Therefore, "about 50 μm" refers to particles between 47 μm and 53 μm in size. In another example, a 35 μm test sieve has a tolerance of 2.6 μm. Therefore, "about 35 μm" refers to particles between 32.4 μm and 38.6 μm in size. The ASTM tolerance for a 25 μm sieve is 2.2 μm. For test sieves without standard tolerances (such as test sieves smaller than 20 μm), the phrase "about X μm" refers to ±15% for sizes between 5 and 15 μm and ±50% for sizes below 5 μm. For example, "about 1 μm" refers to particles between 0.5 and 1.5 μm in size.

[0029] A "glass" according to the present disclosure is understood to be a ceramic material that exhibits a glass transition temperature above room temperature, the primary phase of which is predominantly amorphous, e.g., at least 50% amorphous, at least 75% amorphous, at least 90% amorphous, at least 95% amorphous, or at least 97% amorphous. In some instances, glasses according to the present disclosure are substantially free or completely free of discernible crystalline species.

[0030] In the context of the present disclosure, an "optional" component of a glass composition is a component that may be present in some exemplary compositions and may be absent in other exemplary compositions. Reference to more than one "optional" component should be understood to mean that a composition according to the present disclosure can include zero optional components, one optional component, or any combination of optional components. For example, a glass composition according to the present disclosure (a) optionally includes one or more glass components selected from the group consisting of NaO, KO, and a phosphate source, and (b) optionally includes a fluoride source. Accordingly, the present disclosure contemplates exemplary glass compositions that (i) lack all optional ingredients, (ii) include one or more glass components selected from the group consisting of NaO, KO, and a phosphate source, but lack a fluoride source, (iii) include a fluoride source, but lack NaO, KO, and a phosphate source, and (iv) include one or more glass components selected from the group consisting of NaO, KO, and a phosphate source, and a fluoride source.

[0031] Glass compositions containing CaO, MgO, a phosphate source, or a combination thereof can aid in the formation of apatite precipitation and / or mineralization, such as hydroxyapatite, the primary component of tooth enamel. Precipitation within or around dentinal tubules or mineralization of apatite can form protective deposits and further reduce dentin sensitivity.

[0032] Glass compositions containing potassium (e.g., KO, KHPO, KHPO, KPO, or KF) release potassium as the glass decomposes. Without wishing to be bound by theory, it is believed that the released potassium blocks or reduces action potentials generated in the intradental nerve, thereby reducing dentin sensitivity.

[0033] Glass compositions according to the present disclosure may contain, for example, from about 10 mol % to about 80 mol % of the following: (a) CaO, (b) MgO, (c) a combination of CaO and MgO, (d) (i) CaO and (ii) (e) a combination of (i) MgO and (ii) NaO and / or KO, (f) a combination of (i) CaO and (ii) MgO and (iii) NaO and / or KO, (g) a combination of (i) CaO or MgO and (ii) a phosphate source, (h) a combination of (i) CaO and (ii) MgO and (iii) a phosphate source, (i) a combination of (i) CaO or MgO and (ii) a phosphate source and (iii) NaO and / or KO, or (j) a combination of (i) CaO and (ii) MgO and (iii) a phosphate source and (iv) NaO and / or KO. Any of these exemplary compositions can further include a fluoride source.

[0034] In the context of the present disclosure, it should be understood that a glass composition containing NaO, KO, a phosphate source, or a combination thereof must further contain at least 10 mol% CaO, MgO, or a combination thereof, and when the composition includes a phosphate source, the total number of moles of B2O3 and the phosphate source must still be about 60 mol% or less. For example, a reference to a composition containing "about 10 mol% to about 80 mol% of a combination of (i) CaO, (ii) MgO, and (iii) a phosphate source" should be understood to refer to any combination of CaO, MgO, and a phosphate source, where at least 10 mol% of the composition is a combination of CaO and MgO, the combination of CaO, MgO, and the phosphate source is 10 mol% to 80 mol%, and the combination of B2O3 and the phosphate source is about 60 mol% or less. Similarly, a reference to a composition comprising "about 10 mol% to about 80 mol% of a combination of (i) CaO or MgO, (ii) a phosphate source, and (iii) NaO and / or KO" should be understood to refer to any combination of (i) CaO or MgO + (ii) a phosphate source + (iii) NaO, KO, or a combination of NaO and KO, where at least 10 mol% of the composition is CaO or MgO, the combination of CaO or MgO, the phosphate source, and NaO and KO is between 10 mol% and 80 mol%, and the combination of BO and the phosphate source is about 60 mol% or less.

[0035] Some exemplary glass compositions according to the present disclosure include a fluoride source, such as up to about 45 mol% CaF, SnF, NaF, KF, NaPOF, or a combination thereof. The inclusion of fluoride in the glass composition results in the release of fluoride as the glass decomposes. The released fluoride can form fluorapatite, such as fluoroapatite (Ca(PO)F), within or around dentinal tubules, which can form protective precipitates and further reduce dentin sensitivity.

[0036] Compositions containing CaF or SnF provide twice the amount of fluoride per mole of starting material compared to compositions using NaF, NaPOF, or KF. In some instances, the glass contains less than 30 mole percent CaF, SnF, or a combination thereof.

[0037] In some examples, the glass composition can include about 2 mol% to about 15 mol% of CaF, SnF, NaF, KF, NaPOF, or a combination thereof. In some examples, the glass composition according to the present disclosure can include one or more of NaF, KF, and CaF in an amount of about 5 mol% to about 15 mol%.

[0038] In some examples, glass compositions according to the present disclosure contain sufficient fluoride such that 0.1 g of particulate material releases fluoride in 10 mL of buffered saline solution at an average rate of about 0.5 ppm / hour to about 2000 ppm / hour over a 1, 2, 4, 8, 12, 18, or 24 hour period. In the context of the present disclosure, when determining fluoride release rate, ppm is measured as mass / volume. In particular examples, the glass composition contains sufficient fluoride to release about 4 to about 6 ppm of fluoride per hour over a 1 hour period.

[0039] The glass composition according to the present disclosure may contain Na2O, CaO, and MgO in a molar ratio of 1.0:0.5-2.5:0.5-2.5 (Na2O:CaO:MgO). In some examples, the glass composition includes: a) about 16 mol% to about 22 mol% NaO, about 11 mol% to about 17 mol% CaO, and about 16 mol% to about 22 mol% MgO; b) about 14 mol% to about 20 mol% NaO, about 14 mol% to about 20 mol% CaO, and about 16 mol% to about 22 mol% MgO; c) about 11 mol% to about 17 mol% NaO, about 16 mol% to about 22 mol% CaO, and about 16 mol% to about 22 mol% MgO; or d) about 13 mol% to about 19 mol% NaO, about 18 mol% to about 24 mol% CaO, and about 18 mol% to about 24 mol% MgO.

[0040] Glass compositions according to the present disclosure may include B2O3, MgO, CaO, Na2O, and K2O in a molar ratio of (B2O3+MgO):(CaO+Na2O+K2O) greater than 1.0, such as greater than 1.15 or greater than 1.30.

[0041] In some exemplary glass compositions according to the present disclosure, the composition includes (a) at least 54 mol%, e.g., at least 57 mol%, of a combination of B2O3 and MgO; (b) at least 33 mol%, e.g., at least 40 mol% or at least 50 mol% of a combination of CaO and MgO; (c) at least 7 mol%, e.g., at least 15 mol% or at least 30 mol% of a combination of N2O and K2O; (d) or any combination thereof. Exemplary glass compositions may include less than 0.1 mol% phosphate. Exemplary glass compositions may consist essentially of B2O3, one or both of Na2O and K2O, and one or both of CaO and MgO.

[0042] Exemplary glass compositions according to the present disclosure include B2O3, one or both of Na2O and K2O, and one or both of CaO and MgO in amounts according to any of the compositions listed in Tables 1A and 1B.

[0043] In some exemplary glass compositions according to the present disclosure, the composition includes about 25 mol% to about 43 mol% B2O3, about 14 mol% to about 21 mol% CaO, about 19 mol% to about 29 mol% MgO, about 9 mol% to about 15 mol% Na2O, about 9 mol% to about 15 mol% NaF, KF, CaF2, or any combination thereof.

[0044] In one particular example of a glass composition according to the present disclosure, the composition includes about 43 mol% B2O3, about 21 mol% MgO, about 21 mol% CaO, and about 15 mol% Na2O, such as 43.0 mol% B2O3, 20.7 mol% MgO, 20.7 mol% CaO, and 15.6 mol% Na2O.

[0045] In some exemplary glass compositions according to the present disclosure, the composition includes about 25 mol% to about 45 mol%, e.g., about 41 mol% to about 45 mol% BO, about 10 mol% to about 23 mol%, e.g., about 13 mol% to about 23 mol% CaO, about 10 mol% to about 30 mol%, e.g., about 18 mol% to about 23 mol% MgO, and about 8 mol% to about 22 mol%, e.g., about 13 mol% to about 22 mol% NaO. The composition optionally includes about 8 mol% to about 15 mol% NaF, KF, CaF, or any combination thereof.

[0046] In some exemplary glass compositions according to the present disclosure, the composition includes about 29 mol% to about 45 mol% B2O3, about 5 mol% to about 22 mol% CaO, about 1 mol% to about 22 mol% MgO, 0 mol% to about 15 mol% K2O, and about 5 mol% to about 18 mol% Na2O.

[0047] Glass compositions according to the present disclosure can include less than 0.1 mol% ZnO, such as being substantially free of ZnO, less than 0.1 mol% CuO, less than 0.1 mol% LiO, less than 0.1 mol% RbO, less than 0.1 mol% BaO, less than 0.1 mol% SrO, less than 0.1 mol% SiO, or any combination thereof.

[0048] Particle Size Distribution The glass composition according to the present disclosure can be formulated as a granular material containing particles having a size of about 1 to about 50 μm. Such a glass composition may be referred to as a "granular glass composition." In some instances, at least a portion of the particles are sized to lodge within or on dentinal tubules. The diameter of dentinal tubules naturally varies, primarily ranging from about 0.5 to about 8 μm, e.g., from about 0.5 to about 5 μm. Thus, the glass composition according to the present disclosure formulated as a granular material can be used to desensitize dentin, which can temporarily relieve pain associated with sensitive teeth.

[0049] In some instances, at least 75% of the particles comprising the granular material are less than 50 μm in size. In other instances, at least 85% or at least 95% of the particles are less than 50 μm in size. In some instances, at least 5% of the particles comprising the granular material are less than 7 μm in size.

[0050] In certain instances, the particulate material is comprised of a plurality of particles, wherein at least 5% of the particles are less than 35 μm in size, at least 5% of the particles are less than 15 μm in size, and at least 5% of the particles are less than 7 μm in size.

[0051] In certain examples, the granular material is composed of a plurality of particles, at least 5% of the particles being between about 15 μm and about 35 μm in size, at least 5% of the particles being between about 6 μm and about 15 μm in size, and at least 5% of the particles being between about 3 μm and about 7 μm in size.

[0052] In some particular examples, the particulate material is comprised of a plurality of particles having a particle size distribution of Dx10 of about 5 μm, Dx50 of about 15 μm, and Dx90 of about 30 μm.

[0053] Decomposition Some particulate glass compositions according to the present disclosure can degrade under physiological conditions, for example, a particulate glass composition according to the present disclosure can lose at least 5% by weight within 24 hours when exposed to a buffered saline solution. In some examples, the glass composition can lose at least 20%, at least 40%, at least 60%, or at least 80% by weight within 24 hours when exposed to a buffered saline solution.

[0054] Other particulate glass compositions according to the present disclosure can resist degradation under physiological conditions, for example losing less than 5% by weight after exposure to a buffered saline solution for 24 hours.

[0055] Surface microhardness and remineralization Glass compositions according to the present disclosure, such as particulate glass compositions according to the present disclosure, can increase surface enamel microhardness. In some instances, toothpastes, varnishes, or prophylactic pastes according to the present disclosure can be used to increase surface enamel microhardness. In the context of this disclosure, the increase in microhardness is compared to the surface enamel microhardness before application of the composition of the present disclosure. In some instances, the surface enamel microhardness can increase by a greater amount than the increase associated with an otherwise identical toothpaste, varnish, or prophylactic paste lacking the glass composition of the present disclosure.

[0056] Glass compositions according to the present disclosure, such as particulate glass compositions according to the present disclosure, may remineralize surface enamel. Without wishing to be bound by theory, the authors of the present disclosure believe that this remineralization may be at least partially responsible for the increase in surface enamel microhardness.

[0057] In some instances, a toothpaste, varnish, or prophylactic paste according to the present disclosure can be used to at least partially remineralize surface enamel. In the context of this disclosure, surface enamel remineralization is compared to the surface enamel mineralization prior to application of the composition of the present disclosure. In some instances, the surface enamel can be remineralized to a greater extent than the remineralization associated with an otherwise identical toothpaste, varnish, or prophylactic paste lacking the glass composition of the present disclosure.

[0058] Toothpastes according to the present disclosure can be applied to an individual's enamel, for example, for 30 seconds to 2 minutes, once or twice daily. In some individuals, surface enamel microhardness may increase after about 2, 3, or 4 days. In other individuals, surface enamel microhardness may increase after 5 days or more. In some individuals, surface enamel may be at least partially remineralized after about 2, 3, or 4 days. In other individuals, surface enamel may be at least partially remineralized after 5 days or more.

[0059] Dentin desensitizing composition The particulate glass compositions according to the present disclosure can be formulated into dentin desensitizing compositions comprising a water-free, oral compatible carrier. Such dentin desensitizing compositions according to the present disclosure are water-free because the glass compositions degrade when exposed to water.

[0060] In the context of the present disclosure, "anhydrous" or "water-free" should be understood to mean that the dentin desensitizing composition has such low water content 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 manufactured until the dentin desensitizing composition is completely used up or discarded.

[0061] The orally compatible carrier used in the dentin desensitizing composition can be a mouthwash, a carrier formulated to be mixed with additional ingredients to form a mouthwash, or an orally compatible viscous carrier, such as a toothpaste, dental gel, prophylactic paste, dental varnish, binder, or a carrier formulated to be mixed with additional ingredients to form a toothpaste. The orally compatible viscous carrier can have a viscosity of from about 100 cP at 30° C. to about 150,000 cP at 30° C.

[0062] A dentin desensitizing composition can include a particulate glass composition according to the present disclosure in an amount sufficient to provide the desensitizing composition with about 100 ppm to about 5,000 ppm of fluoride. In some compositions according to the present disclosure, the glass composition lacks fluoride, and another fluoride source, such as sodium fluoride (NaF), can be added to the dentin desensitizing composition. In the context of the present disclosure, when determining the concentration of fluoride in the desensitizing composition, ppm is measured on a mass / mass basis.

[0063] Without wishing to be bound by theory, the authors of the present disclosure believe that some glass compositions according to the present disclosure containing potassium, such as in the form of KO, KF, or both, may have beneficial dentin desensitization properties. Potassium in such glass compositions can increase the extracellular potassium ion concentration around nerves found in dentinal tubules. High levels of extracellular potassium ions can reduce the ability to depolarize and / or repolarize nerve fiber membranes, which improves pain in patients. In dentin desensitizing compositions containing an occluding agent and a separate potassium salt, the occluding agent may inhibit the potassium salt's access to nerves, thereby reducing the ability of the separate potassium salt to improve pain in patients. In contrast, some potassium-containing glass compositions according to the present disclosure may decompose while occluding dentinal tubules, releasing enough potassium ions into the dentinal tubules so that the potassium concentration is high enough to relieve pain in patients.

[0064] One example of a dentin desensitizing composition according to the present disclosure is a toothpaste comprising a particulate glass composition according to the present disclosure and an abrasive, a detergent such as sodium lauryl sulfate, a fluoride source, an antibacterial agent, a flavoring agent, 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 particulate glass composition can be about 0.5 to about 15% by weight of the toothpaste, for example, about 2.5 to about 7.5% by weight of the toothpaste.

[0065] One particular example of a dentin desensitizing composition according to the present disclosure is a toothpaste comprising a particulate glass composition according to the present disclosure, glycerin, silica, polyethylene glycol (e.g., PEG 400), titanium dioxide, carbomer, and a sweetener (e.g., acesulfame potassium or saccharin sodium).

[0066] Another specific example of a dentin desensitizing composition according to the present disclosure is a toothpaste comprising a particulate 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 saccharin sodium).

[0067] Another specific example of a dentin desensitizing composition according to the present disclosure is a toothpaste comprising a particulate glass composition according to the present disclosure, glycerin, sodium lauryl sulfate, silica (also known as silicon dioxide), Carbopol 940 (a cross-linked polyacrylic acid polymer, also known as Carbomer 940), and a flavoring agent (e.g., spearmint oil). The glycerin can be pure glycerol.

[0068] In a specific example, a toothpaste can include about 85 wt% glycerol, about 1.2 wt% sodium lauryl sulfate, about 7.5 wt% silica, about 0.5 wt% Carbopol 940, about 1.0 wt% flavoring, and about 5.0 wt% of a particulate glass composition according to the present disclosure. The toothpaste can optionally include sufficient sodium fluoride to provide about 1000 ppm to about 1500 ppm fluoride, such as about 0.23 wt% NaF. The particulate glass composition can be glass composition #10 in Table 1A below, sieved to obtain particles ≦25 μm.

[0069] Another example of a dentin desensitizing composition according to the present disclosure is a carrier comprising a particulate glass composition according to the present disclosure, which carrier is formulated to be mixed with additional ingredients to form a toothpaste.

[0070] Yet another example of a dentin desensitizing composition according to the present disclosure is a carrier formulated to be mixed with additional ingredients to form a mouthwash. A specific example of a carrier includes a particulate glass composition according to the present disclosure and anhydrous alcohol, cetylpyridinium chloride, chlorhexidine, essential oils, benzoic acid, poloxamer, sodium benzoate, flavorings, colorings, or any combination thereof. Additional ingredients mixed with the carrier to form the mouthwash may include water, peroxide, cetylpyridinium chloride, chlorhexidine, essential oils, alcohol, benzoic acid, poloxamer, sodium benzoate, flavorings, colorings, or any combination thereof. The carrier and additional ingredients 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.

[0071] Another example of a dentin desensitizing composition according to the present disclosure is a prophylactic paste (also called a "prophy paste") comprising a particulate glass composition according to the present disclosure. A specific example of a contemplated prophy paste comprises a glass composition according to the present disclosure and pumice, glycerin, diatomaceous earth (preferably fine granules), sodium silicate, methyl salicylate, monosodium phosphate, sodium carboxymethylcellulose, a sweetener (e.g., acesulfame potassium or saccharin sodium), a flavoring agent, a coloring agent, or any combination thereof.

[0072] 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-rhodium crucible (XRF Scientific, Perth Australia), placing the loaded crucible into a furnace (Carbolite, RHF 14 / 3) at an initial dwell temperature of 600-750°C, holding the temperature for 60 minutes, ramping the temperature (e.g., at a rate of 20°C / min) to a dwell temperature of 1,200°C, holding the temperature for 60 minutes, and quenching the glass melt between two stainless steel plates.

[0073] It should be understood that the specific ramp rates, times, and temperatures disclosed above can be varied so long as the glass melts. A ramp rate of 10-20°C per minute and a dwell temperature hold can remove at least some of the bubbles from the glass.

[0074] While the resulting glass composition includes an oxide, the starting reagents can include an oxide, a carbonate, a phosphate, or any combination thereof. For example, the starting reagents can include boron oxide, calcium carbonate, sodium carbonate, and NaH2PO4. Calcium carbonate and sodium carbonate decompose in the furnace to release CO2 and produce the corresponding oxide. Sodium phosphate decomposes in the furnace to provide sodium and phosphorus ions within the glass oxide network. In the context of this disclosure, it should be understood that a glass composition including a "phosphate source" refers to a composition including decomposition products from the phosphate source, and that the mole percent of the phosphate source refers to the mole percent of the phosphate source starting material.

[0075] The resulting quenched glasses were individually crushed / ground in a planetary micromill (Pulverisette 6, Fritsch, Germany) and sieved through an ASTM E-11 compliant sieve (Cole Palmer, USA) to obtain particles ≤25 μm. The glasses could be stored under dry conditions in sealed storage vials.

[0076] In the context of the present disclosure, mass loss of a granular glass composition was measured by placing approximately 0.1 grams of sample into a pre-weighed 15 ml Falcon tube. Then, 10 ml of TRIS-buffered saline (BioUltra, Sigma-Aldrich, Canada) was pipetted into the tube. The tube was agitated at 120 rpm in an incubator and maintained at 37°C for the desired release time, such as 30 minutes, 1, 3, 6, 12, or 24 hours. After the designated time point, the tube was removed from the incubator and centrifuged at 1500 RCF for 15 minutes. The supernatant was decanted into a new 15 ml Falcon tube. For granular glass compositions containing a fluoride source, the tube containing the supernatant was sealed and stored at 4°C until the amount of fluoride was quantified. The original 15 ml Falcon tube was placed at 70°C to dry until a constant weight was reached, allowing the residual mass of the granular glass composition to be assessed and the mass loss to be calculated.

[0077] For particulate glass compositions containing a fluoride source, the concentration of released fluoride was quantified using an Accumet® AB250 pH / ion-selective electrode meter (Fisher Scientific, Massachusetts, USA) equipped with an Accumet® electrode-fluoride combination. Standard solutions were prepared using a fluoride analytical standard (NaF, 0.1 M F, Sigma-Aldrich, Canada) specifically for the ion-selective electrode, and a calibration curve was obtained prior to analysis. At the time of analysis, 1 ml of TISAB III (Fisher Scientific, Massachusetts, USA) was added to the 15 mL Falcon tube containing the supernatant at room temperature. Ion concentrations are reported as the mean ± SD of n=3.

[0078] Scanning electron micrograph analysis was performed using a Phenon PRoX scanning electron microscope (Thermofisher Scientific, Waltham, MA).

[0079] Thermal analysis of the glass samples was completed in a high-temperature differential scanning calorimeter, DSC 404 F3A-0230, equipped with a silicon carbide furnace, in a Pt / Rh crucible (NETZSCH Instruments North America, Burlington, MA, USA). Approximately 0.025 grams of sample was weighed and loaded into the Pt / Rh crucible. The sample was heated at a rate of 10 K / min from 20 to 900 °C at a rate of 10 K / min under nitrogen (Praxair, Danbury, Connecticut, USA) protective gas with a flow rate of 50 mL / min, at a rate of 100 pts / min. The onset temperature (To), inflection temperature (Ti), final temperature (Tf), and crystallization onset temperature (Tp1) were determined using Netzsch Proteus Thermal Analysis Software (Version 6.1.0). The glass transition temperatures reported in Table 3 are obtained from the onset temperature (To) of the sample.

[0080] 11 B Magic Angle Spinning (MAS) NMR spectra were obtained on a 16.4T Bruker Avance NMR spectrometer ( 11 The measurements were performed using a 2.5 mm HX probe head operating in single resonance mode (B Larmor frequency = 224.67 MHz). 11 The B parameter was calibrated and also used as an external chemical shift reference standard (-42.1 ppm relative to BF3Et2O). All samples were spun at a MAS frequency of 20 kHz to determine the center band and identify spinning sidebands. For all compositions and experiments, 11 B NMR was acquired using a 0.53 μs pulse, corresponding to a 15° pulse angle, in a nearly cubic NaBH4 environment. To eliminate background noise, an empty rotor spectrum was acquired at each spinning speed and subtracted from the experimental spectrum.

[0081] The in vitro remineralization model was designed to serve as a surrogate test for the ability of glass powders to promote the precipitation of mineral phases (e.g., apatite and fluorapatite) in the oral environment. While ISO standards exist for the in vitro assessment of bioactivity, the ISO method was developed for the evaluation of macroscopic samples, and incubation conditions are standardized to a surface-to-volume ratio, which was not deemed appropriate for the analysis of powders (ISO 23317:2014, "Surgical implants - In vitro assessment of the apatite-forming ability of implant materials"). Because the glass powders examined here were fine (d90 < 30 μm), this study was based on a protocol developed by Technical Committee 4 of the International Committee on Glass (TCO4) to assess the bioactivity of powdered bioactive glasses, normalized to powder weight (Macon, A.K., "Uniform in vitro assessment of the apatite-forming ability of bioactive glasses and their variants," Journal of Materials Science: Materials in Medicine, (2015) 26(2) p. 115). Crushed glass powder was incubated in simulated body fluid at 37°C. The simulated body fluid was synthesized according to the method and instructions published by Kokubo and Takadama (Kokubo, T. and Takadama, H. Biomaterials (2006) 27:15, pp. 2907-2915). Because significant particle size reduction was expected due to the rapid degradation of the studied glass, the glass sample size was doubled from the recommended 75 mg to 125 mg, and the volume of SBF was increased accordingly from 50 mL to 100 mL. Incubated samples were removed after 30 minutes, then filtered and dried, and imaging was performed to visualize the formation of mineral phases. Due to the intended rapid degradation of glass powder in an aqueous environment, the TCO4 method was modified to incubate glass powder in simulated body fluid for 30 minutes, 3 hours, and 24 hours, compared to the 8 hours, 24 hours, 72 hours, 1 week, and 2 weeks used in the TCO4 method. Elemental analysis was performed using an Oxford Instruments EDX unit equipped with an 80 mm SDD with 5 min elemental mapping. [Example]

[0082] example All glass compositions shown in Tables 1A and 1B were synthesized by weighing out the required amounts of analytical-grade reagents (boron oxide, calcium carbonate, sodium carbonate, magnesium oxide, and sodium fluoride) (Sigma-Aldrich, Canada). To ensure homogeneity, each formulation was mixed for at least 60 minutes in a dry powder blender. Each precursor blend was loaded into a 100 mL platinum-rhodium crucible (XRF Scientific, Perth, Australia). The loaded crucible was then placed in a furnace (Carbolite, RHF 14 / 3) with an initial dwell temperature of 600–750 °C and held for 60 minutes. The temperature was then increased (20 °C / min) to a final hold temperature of 1,200 °C and held for 60 minutes. Upon removal, each glass melt was quenched between two stainless steel plates. The resulting quenched glasses were individually crushed / ground in a planetary micromill (Pulverisette 6, Fritsch, Germany) and sieved through an ASTM E-11 compliant sieve (Cole Palmer, USA) to obtain particles ≤25 μm. [Table 1] [Table 2]

[0083] Some of the exemplary glass particles in Table 1A were evaluated for mass loss using the method described above. The % mass loss after 1 hour and 24 hours is shown in Table 2. [Table 3]

[0084] Some of the exemplary glass particles in Table 1B were evaluated for mass loss using the method described above, and the % mass loss after 30 minutes is shown in Table 3. [Table 4]

[0085] The density of glass powder is 1cm 3 Measurements were performed using an AccuPyc 1340 helium hydrometer (Micromeritics, USA) equipped with an insert. Prior to use, the hydrometer was calibrated using a traceable volume standard. For glass powder analysis, the insert was loaded with approximately 1 g of glass powder. Each measurement was calculated from the average of 10 readings.

[0086] The percentage of amorphous phase in samples was evaluated using a D2 Phaser X-ray diffractometer equipped with a Cu source and a Lynxeye linear array detector (Bruker AXS Inc, Maddison, Wisconsin, USA). Diffraction spectra of finely crushed samples were collected at 2-theta angles from 10 to 60° with a step size of 0.02 degrees and a dwell time of 2 seconds. The relative volume of amorphous material was calculated by fitting the background curve to the amorphous halo and calculating the relative intensity of the background-corrected reduced area to the uncorrected global area. The % amorphous phase is related to the % crystallinity by the formula (% crystallinity) + (% amorphous phase) = 100.

[0087] The exemplary glass particles of Table 1A had the following bulk properties: [Table 5]

[0088] Table 1B includes the composition of the design space defined by the following table, in mole %: [Table 6]

[0089] The results of tested compositions within the design space provide the following equations, which allow for relative comparison of different compositions and / or can be useful in identifying trends associated with different components of the composition. While experimental and modeling errors prevent absolute prediction of glass properties, the equations can be used to guide and refine the design of glass compositions. Used together, these models can help suggest which factors may be traded off when adjusting multi-component compositions within the tested composition space. In the equations below, the component values ​​listed are percentages (not fractions or decimals). For example, 50 mole % B2O3 would be listed as "50" (not "0.5").

[0090] The crystallinity of the melt can generally be predicted under the quench conditions tested using the following equation: Crystallinity=-7.21994*[B2O3]+10.5814*[K2O]+13.6798*[CaO]+16.9661*[MgO]+4.75849*[NaO]-35.849*[ B2O3][K2O]-45.4598*[B2O3][CaO]-66.4434*[K2O][MgO]-66.849*[CaO][MgO]-72.7346*[MgO][NaO]

[0091] The density of glass can generally be predicted using the following formula: ρ=2.14644*[B2O3]+2.24491*[K2O]+2.92911*[CaO]+2.43832*[MgO]+2.42776*[NaO]

[0092] Approximately 1.3g / cm 3 ~Approx. 2.2g / cm 3 A glass density of 1.3 g / cm3 can be particularly useful in non-aqueous oral care formulations. The densities of glycerol and silica, the primary liquid and solid components of non-aqueous toothpaste, are 1.3 and 2.2 g / cm3, respectively. 3 is.

[0093] NMR B3 chemical shifts (ppm) can generally be predicted using the following formula: ppm=6.74673*[B2O3]+3.33975*[K2O]+7.20888*[CaO]+10.1749*[MgO]+4.01478*[NaO]-11.8899*[B2O3][K2O]-25.2187*[B 2O3][CaO]-25.023*[B2O3][MgO]-12.4656*[B2O3][NaO]-12.5781*[K2O][MgO]-18.8676*[CaO][MgO]-19.0726*[MgO][NaO]

[0094] NMR shows that 11 This provides a tool for probing the local environment of B atoms. The proportion of networks organized as B3 (trihedral) versus B4 (tetrahedral) coordinates can be determined using NMR. Surprisingly, the authors of this disclosure determined that the influence of alkali and alkaline earth elements (from coefficients) affects network organization similarly. The ratios provided by this data support a mechanistic basis for degradation in addition to compositional chemistry.

[0095] The formula relating percent mass loss after 30 minutes under test conditions is: 1189.44*[B2O3]-87.7623*[K2O]-62.9762*[CaO]+375.296*[MgO]-80.86*[ NaO]-982.106*[B2O3][K2O]-1169.24*[B2O3][CaO]-2192.55*[B2O3][MgO]- 1040.75*[B2O3][NaO]+485.18*[K2O][CaO]-139.18*[K2O][MgO]+283.37*[ K2O][NaO]-460.87*[CaO][MgO]+475.861*[CaO][NaO]-304.428*[MgO][NaO]

[0096] Six exemplary glass compositions were tested for their ability to remineralize surface enamel. The compositions tested were composition 10, as identified in Table 1A, and compositions 3.01, 3.04, 3.06, 3.20, and 3.24, as identified in Table 1B.

[0097] The remineralization results are shown in Tables 6, 7 and 8 below. [Table 7] [Table 8] [Table 9]

[0098] Additionally, the remineralization results of Compound 10 were measured at 3 hours, and the atomic percentages as the mean (±SD) of three replicates were as follows: B: not detected, O: 75.7±2.3, Na: 0.1±0.006, Mg: 1.9±0.09, K: not detected, Ca: 12.1±1.3, C: not detected, and P: 10.3±0.9.

[0099] Calcium (Ca) and phosphorus (P) are the building blocks of amorphous calcium phosphate and apatite and act to remineralize teeth. Identifying these elements on the surface of glass incubated in SBF indicates the glass's mineralization potential. According to the literature, mineralization typically occurs over several hours (typically 24 hours), days, or weeks. Test formulations lacking P exhibit Ca- and P-containing precipitates after only 30 minutes. The results in Tables 6, 7, and 8 show that at time = 0, no phosphorus was detected on the surface of the glass particles. The detected carbon ("C") reflects surface contamination that occurred during sample preparation. At time = 24 hours, phosphorus was detected in calcium ratios ranging from 1.13:1 to 1.31:1 (Ca:P), which approximates the calcium to phosphorus ratio of approximately 1.6 present in apatite.

[0100] Glass composition No. 10 (i.e., a glass composition consisting of 43.0 mol% BO, 20.7 mol% MgO, 20.7 mol% CaO, and 15.6 mol% NaO) was used to prepare an exemplary toothpaste ("5% SIP-FF+NaF") according to the following table. [Table 10]

[0101] The glass particles were sieved to collect particles ≤25 microns. Particle size analysis confirmed that the powder particles were the appropriate size to occlude dentinal tubules, which are typically 1-5 μm in diameter. The mean particle size distribution of the glass was D10 = 6.46 μm, D50 = 16.6 μm, and D90 = 33.0 μm. Here, Dx is the diameter, and X% of the distribution has a diameter less than Dx.

[0102] An exemplary toothpaste, 5% SIP-FF+NaF, was tested in single and multi-timepoint dentin occlusion studies, as well as in a single-timepoint hydraulic conductivity study.

[0103] Single-time point dentin occlusion study The 5% SIP-FF+Na toothpaste was compared to commercially available toothpaste products: (Control Article #1) Sensodyne® Repair and Protect with NOVAMIN® (5% Novamin and 1040 ppm fluoride as sodium fluoride), and (Control Article #2) Colgate® Sensitive ProRelief™ (8% arginine, 35% calcium carbonate, 1320 ppm fluoride as sodium monofluorophosphate) in a single time point dentin occlusion study.

[0104] The degree of dentin tubule blockage caused by the target toothpaste is measured one day after treatment by analyzing dentin samples treated with both simulated brushing for two minutes twice a day and by applying a pea-sized amount directly to the sensitive area using a clean finger. The degree of dentin tubule blockage is generally understood in the art to be an indirect measure of the ability to reduce dentin hypersensitivity. That is, as the level of blockage increases, the flow of dentin fluid decreases, resulting in a decrease in pain sensation. The decrease in dentin fluid flow reduces sensitivity, and the precipitation of fluorinated apatite provides a barrier for rapid relief. Fluorinated apatite, which is useful in preventing caries or tooth decay, can be formed in the presence of fluoride ions in solution, which are incorporated into the mineral.

[0105] Human dentin samples (approximately 1.0 to 1.5 mm thick) were prepared from the crowns of caries-free, unrestored molars perpendicular to the long axis of the root using a diamond disc saw. Each section was etched in 10% citric acid for 2 minutes, followed by a 60-second rinse in water, sonication in deionized water for 2 minutes, and a further 60-second rinse in water. Each section was placed in a mold and covered with acrylic resin. Once cured, the dentin surface was polished to a mirror finish. After rinsing with deionized water, the surface was etched, sonicated, and rinsed again. The integrity, tubule density, and patency of the samples were examined by scanning electron microscopy (SEM) using a Phenom PRoX scanning electron microscope (Thermo Fisher Scientific, Waltham, MA).

[0106] Artificial saliva (30 mM potassium chloride, 13 mM sodium chloride, 10 mM potassium dihydrogen orthophosphate, 3 mM calcium chloride dehydrate, 0.22% w / w type II porcine gastric mucin, and 0.02% w / w sodium azide) was prepared. The dentin samples were soaked in the artificial saliva for at least 60 minutes at 37°C before being treated with toothpaste.

[0107] For brushing applications, 0.67g of toothpaste was applied to the dentin samples for 10 seconds using a vibrating Oral-B Precision toothbrush. For direct application, 0.25g of toothpaste was pressed onto the dentin sample with light pressure and applied in a circular motion with a gloved finger for 10 seconds. Dentin sample treatments and application conditions are summarized in Table 10 below. [Table 11]

[0108] For both application methods, samples were rinsed with deionized water for 30 seconds after application to remove visible traces of toothpaste, then stored in artificial saliva for at least 1 hour before the application cycle was repeated to simulate twice-daily use. After the second application, samples were treated with simulated saliva for 60 seconds, then dried and prepared for SEM imaging.

[0109] Dentin samples treated with gold sputter coating were imaged using a Phenon ProX scanning electron microscope, with three images collected for each sample at a magnification of x3000. Each SEM image was assessed by two double-blind assessors for the degree of tooth occlusion based on a five-point categorical scale using the following grading classification: 1. Blockage 2. Almost blocked 3. Equals 4. Almost no obstruction 5. Not blocked

[0110] Data analysis was performed using Minitab 18 software. All treatment groups were evaluated, and descriptive statistics were provided for group means, standard deviations, minimums, maximums, and number of replicates. All datasets were then tested for normality. For datasets that met the normality assumption, pairwise comparisons between datasets were performed using a two-sample t-test. For pairings in which one or more datasets did not meet the normality assumption, pairwise statistical comparisons were performed using the Mann-Whitney test. All statistical tests were performed at a significance level of 0.05.

[0111] Initial performance data supports the effectiveness of the 5% SIP-FF+Na toothpaste and its ability to partially occlude dentinal tubules. Mean occlusion scores are as follows: [Table 12]

[0112] SEM images of dentinal tubules treated with 5% SIP-FF+Na toothpaste show tubule obstruction due to both large undegraded particles retained within the tubules or on the dentin surface and the occurrence of small mineral deposits within the dentinal tubules.

[0113] In addition to intracanalicular occlusion, the formation of a layer on exposed dentin surfaces can block the tubules. As the glass composition decomposes, the rate is affected by particle size, and beneficial ions are released to promote the formation of apatite, including fluoride-containing apatite.

[0114] Sensodyne® Repair and Protect with NOVAMIN® was the worst-performing toothpaste at occluding dentin tubules, both through brushing and direct application. Marketing materials claim that Sensodyne® Repair and Protect with NOVAMIN® is "effective from the first week," confirming that it may have a more cumulative effect over several days rather than the immediate benefits shown by Sensi-IP®. An independent in vivo study conducted by Technical Committee 4 of the International Commission on Glass (TCO4) on the initial bioactive glass composition 45S5, the basis of Novamin Technology, found that it took 24 hours for the effects of in vitro surface reactions to become visible (J Mater Sci: Mater Med 2015).

[0115] Multi-time point dentin occlusion study The 5% SIP-FF+Na toothpaste was also compared to commercially available toothpaste products (Control Article #1) Sensodyne® Repair and Protect™ with NOVAMIN® (5% Novamin and 1040 ppm fluoride as sodium fluoride) and (Control Article #2) Colgate® Sensitive ProRelief™ (8% arginine, 35% calcium carbonate, 1320 ppm fluoride as sodium monofluorophosphate) in a multiple time point dentin occlusion study over a 5 day sham treatment.

[0116] Analysis of dentin samples treated with two minutes of simulated brushing twice daily for 1-5 days provides a measure of the degree of dentin tubule occlusion by the target toothpaste over several days. The degree of dentin tubule occlusion is generally understood in the art to be an indirect measure of the ability to reduce dentin hypersensitivity. That is, increased levels of occlusion decrease dentin fluid flow, resulting in decreased pain sensation.

[0117] Human dentin samples were prepared in the same manner as in the single-time point dentin occlusion study described above.

[0118] An artificial saliva solution (30 mM potassium chloride, 13 mM sodium chloride, 10 mM potassium dihydrogen orthophosphate, 3 mM calcium chloride dehydrate, 0.22% w / w type II porcine gastric mucin, and 0.02% w / w sodium azide) was prepared. The dentin samples were immersed in the artificial saliva solution at 37°C for at least 60 minutes before the first treatment with toothpaste.

[0119] Samples were treated with toothpaste (Table 12) twice daily by brushing with 0.67 g of toothpaste for 10 seconds using a vibrating toothbrush. [Table 13]

[0120] Samples were treated for 1-5 days as outlined in Table 13. Samples were rinsed with deionized water for 30 seconds after application to remove visible traces of toothpaste and then stored in artificial saliva for at least 1 hour, after which the application cycle was repeated to simulate twice-daily use. After twice-daily applications, samples were soaked in simulated saliva for 3 hours before being transferred to moist tissue until the next treatment time point. [Table 14]

[0121] Treated dentin samples, including the gold sputter coating, were imaged using a Phenon ProX scanning electron microscope, with three images collected for each sample at a magnification of x3000. Each SEM image was assessed by two double-blind assessors for the degree of tooth occlusion based on a five-point categorical scale using the following grading classification: 1. Blockage 2. Almost blocked 3. Equals 4. Almost no obstruction 5. Not blocked

[0122] Data analysis was performed using Minitab 18 software. All treatment groups were evaluated and descriptive statistics of group means, standard deviations, minimums, maximums, and number of replicates were provided. All datasets were then tested for normality. For datasets that met the normality assumption, pairwise comparisons between datasets were performed using a two-sample t-test. For pairings in which one or more datasets did not meet the normality assumption, pairwise statistical comparisons were performed using a Mann-Whitney test. All statistical tests were performed at a significance level of 0.05.

[0123] Initial performance data supports the effectiveness of the 5% SIP-FF+Na toothpaste and its ability to partially occlude dentinal tubules. Mean occlusion scores are as follows: [Table 15]

[0124] Complete occlusion (represented by an occlusion score of 1) was achieved in some dentin samples treated with Sensi-IP® toothpaste after 3 days of application of 5% SIP-FF+Na toothpaste. No other toothpaste achieved an occlusion score of 1 for any of the treated samples over the treatment period.

[0125] Sensodyne® Repair and Protect with NOVAMIN® and Colgate® Sensitive ProRelief™ performed equally at all time points and were inferior to 5% SIP-FF+Na toothpaste in providing visual occlusion.

[0126] Surface Microhardness Approximately 4x4mm enamel blocks were sliced ​​from bovine labial incisors, lapped, and polished to a 0.04µm grit. One corner was removed to allow for sample orientation. Samples were stored, refrigerated, and moistened with 0.1% thymol until use.

[0127] Baseline surface microhardness measurements were assessed using a Wilson Tukon 1202 microhardness tester. A series of eight indentations were made at 100 μm intervals using a 50 g load and a 10-second dwell time. Indentation size measurements were performed using a 50X objective. Samples were accepted for the study with an SMH of ≥ 250 HK and a standard deviation of ≤ 20 HK. Following baseline assessment, an initial decalcification challenge was applied by immersing the samples in 8 ml of decalcification solution per block for 60 minutes at 37°C, followed by a rinse with deionized water. Surface microhardness measurements were performed on each enamel block both after the initial decalcification treatment and after the pH cycling procedure, prior to decalcification as a quality check for inclusion in the study. [Table 16]

[0128] A negative control paste consisting of the equivalent toothpaste chassis without SIP-FF was used for comparison, along with a positive control consisting of the equivalent chassis without SIP-FF and spiked with 1040 ppm F as NaF.

[0129] Surface microhardness (SMH) was analyzed using a series of eight indentations made at 100 μm intervals using a 50 g load and a 10 second dwell time. Indentation measurements were taken using a 50X objective and hardness was expressed as Knoop hardness.

[0130] The surface microhardness recovery rate (SMHR) was calculated using the following formula:

number

[0131] All statistical analyses were performed using Minitab 18 software. Summary statistics (n, mean, standard deviation) were generated for each experiment and for each treatment group and time point. All data sets were tested for normality using the Anderson-Darling test. Pairwise comparisons were performed between treatment groups for each experiment and time point. For the enamel surface microhardness experiment, all data sets met the assumed criteria, and experimental results were compared using one-way analysis of variance. For the visual occlusion and fluoride uptake experiments, pairwise comparisons were performed between occlusion scores using a two-sample T-test if the normality assumption was met, and a Mann-Whitney test if one or more pairs did not meet the normality assumption. All statistical tests were performed at a significance level of 0.05. [Table 17]

[0132] In the above description, for purposes of explanation, numerous details are set forth in order to provide a thorough understanding of the examples. 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 examples, and many modifications and variations are possible in light of the above teachings.

[0133] It should be understood that the above description provides examples, and that those skilled in the art may make modifications and variations to the particular examples. Accordingly, the claims should not be limited by the specific examples set forth herein, but should instead be construed consistent with the specification as a whole.

Claims

1. 20 mol% to 45 mol% of B2O3, One or more glass components selected from the group consisting of 10 mol% to 80 mol% CaO and MgO, Depending on the case, one or more glass components selected from the group consisting of Na₂O, K₂O, and a phosphate source, Depending on the circumstances, CaF₂, SnF₂, NaF, KF, Na₂PO₃F, or combinations thereof in amounts of 45 mol% or less. A glass composition comprising, wherein the total amount of B2O3 and phosphate source is 60 mol% or less, and The composition is a glass composition comprising less than 0.1 mol% of CdO and less than 0.1 mol% of SiO2.

2. The glass composition according to Claim 1, (a) The phosphate source is further less than 35 mol%, less than 30 mol%, less than 25 mol%, less than 20 mol%, less than 15 mol%, less than 10 mol%, or less than 5 mol% of the glass composition; (b) The phosphate source is P₂O₅, NaH₂PO₄, Na₂HPO₄, Na₃PO₄, KH₂PO₄, K₂HPO₄, K₃PO₄, or any combination thereof; (c) The glass composition contains Na₂O, CaO, and MgO in a molar ratio of 1.0:0.5 to 2.5:0.5 to 2.5 (Na₂O:CaO:MgO); or (d) Any combination of (a) to (c), Glass composition.

3. The glass composition is a) 10 mol% to 80 mol% CaO, b) 10 mol% to 80 mol% MgO, c) A combination of CaO and MgO in amounts of 10 mol% to 80 mol%, d) 10 mol% to 80 mol% of (i) CaO and (ii) Na₂O or K₂O or both, e) 10 mol% to 80 mol% of (i) MgO and (ii) Na₂O or K₂O or both, f) 10 mol% to 80 mol% of (i) CaO, (ii) MgO and (iii) Na₂O or K₂O or both, g) A combination of (i) CaO or MgO and (ii) a phosphate source in an amount of 10 mol% to 80 mol%, h) A combination of (i) CaO, (ii) MgO and (iii) phosphate sources in an amount of 10 mol% to 80 mol%, i) 10 mol% to 80 mol% of (i) CaO or MgO, (ii) a phosphate source and (iii) Na₂O or K₂O or a combination of both, j) 10 mol% to 80 mol% of (i) CaO, (ii) MgO, (iii) phosphate source and (iv) Na₂O or K₂O or both, A glass composition according to claim 1 or 2, comprising:

4. The glass composition contains Na₂O, CaO, and MgO in a molar ratio of 1.0:0.5 to 2.5:0.5 to 2.5 (Na₂O:CaO:MgO), and The glass composition is a) 16 mol% to 22 mol% Na₂O, 11 mol% to 17 mol% CaO, and 16 mol% to 22 mol% MgO, b) 14 mol% to 20 mol% Na₂O, 14 mol% to 20 mol% CaO, and 16 mol% to 22 mol% MgO, c) 11 mol% to 17 mol% Na₂O, 16 mol% to 22 mol% CaO and 16 mol% to 22 mol% MgO, or d) 13 mol% to 19 mol% Na₂O, 18 mol% to 24 mol% CaO, and 18 mol% to 24 mol% MgO, A glass composition according to any one of claims 1 to 3, comprising:

5. The molar ratio of (B₂O₃ + MgO):(CaO + Na₂O + K₂O) is greater than 1.0; The glass composition contains at least 54 mol% of a combination of B2O3 and MgO; The glass composition contains at least 33 mol% of a combination of CaO and MgO; The glass composition contains at least 7 mol% of a combination of Na₂O and K₂O; or any combination thereof The glass composition according to any one of claims 1 to 3.

6. The glass composition according to claim 5, wherein the glass composition contains less than 0.1 mol% of phosphate.

7. The glass composition according to claim 5 or 6, wherein the glass composition essentially consists of one or both of B₂O₃, Na₂O and K₂O, and one or both of CaO and MgO.

8. The glass composition according to claim 1, comprising B₂O₃, Na₂O and K₂O, and CaO and MgO, in an amount corresponding to one of the compositions listed in the following table: Table 1

9. The glass composition comprises less than 30 mol% of CaF₂ or SnF₂, and comprises less than 30 mol% of a combination of CaF₂ and SnF₂; or, The glass composition contains 2 mol% to 15 mol% of CaF₂, SnF₂, NaF, KF, Na₂PO₃F, or a combination thereof. The glass composition according to any one of claims 1 to 6.

10. 25 mol% to 45 mol% of B2O3, 10 mol% to 23 mol% CaO, 10 mol% to 30 mol% MgO, and 8 mol% to 22 mol% Na₂O, In addition, as appropriate, 8 mol% to 15 mol% of NaF, KF, CaF2, or any combination thereof. A glass composition according to any one of claims 1 to 7, comprising:

11. 25 mol% to 43 mol% of B2O3, 14 mol% to 21 mol% CaO, 19 mol% to 29 mol% MgO, 9 mol% to 15 mol% Na₂O, and, 9 mol% to 15 mol% of NaF, KF, CaF2, or any combination thereof, The glass composition according to claim 1, comprising:

12. 29 mol% to 45 mol% of B2O3, 5 mol% to 22 mol% CaO, 1 mol% to 22 mol% MgO, 0 mol% to 15 mol% K₂O, and, 5 mol% to 18 mol% Na₂O, A glass composition according to any one of claims 1 to 3 and 5 to 7, comprising:

13. The glass composition according to any one of claims 1 to 12, wherein the glass composition comprises less than 0.1 mol% of ZnO, less than 0.1 mol% of CuO, less than 0.1 mol% of Li₂O, less than 0.1 mol% of Rb₂O, less than 0.1 mol% of BaO, less than 0.1 mol% of SrO, or any combination thereof.

14. The glass composition according to any one of claims 1 to 13, wherein the glass composition is a granular material containing particles having a size of 1 to 50 μm.

15. The glass composition according to claim 14, wherein at least 75%, at least 85%, or at least 95% of the particles are less than 50 μm in size.

16. The glass composition according to claim 14 or 15, wherein at least 5% of the particles are less than 7 μm in size.

17. At least 5% of the particles are less than 35 μm in size, At least 5% of the aforementioned particles are less than 15 μm in size, At least 5% of the aforementioned particles are less than 7 μm in size. The glass composition according to claim 14 or 15.

18. At least 5% of the particles are 15 μm to 35 μm in size, At least 5% of the aforementioned particles are 6 μm to 15 μm in size, At least 5% of the aforementioned particles are 3 μm to 7 μm in size. The glass composition according to any one of claims 14 to 16.

19. 10% of the particles are less than 5 μm in size, 50% of the aforementioned particles are less than 15 μm in size, and 90% of the aforementioned particles are less than 30 μm in size. The glass composition according to claim 14.

20. The glass composition according to any one of claims 14 to 19, wherein when exposed to a buffered saline solution, the glass composition loses at least 5% by mass, at least 20% by mass, at least 40% by mass, at least 60% by mass, or at least 80% by mass within 24 hours.

21. Toothpaste, preventive paste, or dental varnish comprising the glass composition according to any one of claims 14 to 19.

22. Toothpaste comprising the glass composition according to any one of claims 14 to 19, as dependent on claim 9, 10 or 11, wherein the toothpaste comprises an amount of the glass composition sufficient to yield 500 ppm to 1,500 ppm of fluoride; A preventive paste comprising the glass composition according to any one of claims 14 to 19, as dependent on claim 9, 10 or 11, wherein the preventive paste comprises an amount of the glass composition sufficient to yield 1,000 ppm to 1,500 ppm of fluoride; or, A dental varnish comprising the glass composition according to any one of claims 14 to 19, as dependent on claim 9, 10, or 11, wherein the dental varnish comprises an amount of the glass composition sufficient to yield 1,000 ppm to 5,000 ppm of fluoride.

23. Toothpaste comprising a glass composition according to any one of claims 14 to 19, as dependent on any one of claims 1 to 8, 10, 12 and 13, wherein the glass composition is fluoride-free, and the toothpaste contains a fluoride source in an amount sufficient to yield 1,000 ppm to 1,500 ppm of fluoride; A preventive paste comprising a glass composition according to any one of claims 14 to 19, relating to any one of claims 1 to 8, 10, 12 and 13, wherein the glass composition is fluoride-free, and the preventive paste comprises a fluoride source in an amount sufficient to yield 1,000 ppm to 1,500 ppm of fluoride; or, A dental varnish comprising a glass composition according to any one of claims 14 to 19, which is dependent on any one of claims 1 to 8, 10, 12 and 13, wherein the glass composition is fluoride-free, and the dental varnish comprises a fluoride source in an amount sufficient to yield 1,000 ppm to 5,000 ppm of fluoride.

24. The toothpaste according to any one of claims 21 to 23, wherein the glass composition is 2.5 wt% to 7.5 wt% of the toothpaste.

25. The toothpaste, preventive paste, or dental varnish according to any one of claims 21 to 24, wherein the toothpaste, preventive paste, or dental varnish is substantially water-free.

26. (i) The glass composition according to any one of claims 14 to 19, (ii) Anhydrous oral-fit carrier, A dentin desensitizing composition containing the following:

27. ​​The dentin desensitizing composition according to claim 26, wherein the oral compatibility carrier is a mouthwash, formulated to be mixed with a mouthwash, or an oral compatibility viscous carrier, and the viscous carrier is a toothpaste, dental gel, preventive paste, dental varnish, or binder.

28. The glass composition according to any one of claims 1 to 14, wherein the glass is bulk glass for preparing the granular glass composition according to any one of claims 14 to 19.

29. A glass composition according to any one of claims 14 to 19, for at least partially remineralizing surface enamel or for at least partially occluding one or more dentin tubules.

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