Oral treatment compositions to promote gum health.

Description

1 / 42 “ORAL HYGIENE COMPOSITIONS TO PROMOTE GUM HEALTH” FIELD OF THE INVENTION

[0001] The present invention relates to oral hygiene compositions comprising a source of stannous ions and a taurate-based surfactant to promote the oral health of a user's gums. In particular, such oral hygiene compositions are useful for controlling plaque bacteria and / or protecting against bacterial / toxin invasion. BACKGROUND OF THE INVENTION

[0002] Dental plaque (also known as dental biofilm) is a sticky, colorless deposit of bacteria that constantly forms on the tooth surface. Dental plaque is generally composed of bacteria and extracellular polymeric substances (EPS). Extracellular polymeric substances (EPS) are biopolymers of microbial origin in which biofilm microorganisms are embedded. J. Bacteriol. 2007, 189 (22): 7945. Saliva, food, and fluids combine to produce these deposits, which accumulate where teeth and gums meet. Plaque buildup is a major factor in poor oral health, which can lead to caries and periodontal disease (in the gums), including gingivitis.One of the ways in which toothpaste compositions help prevent and control plaque is through the advantageous use of antibacterial agents; however, the disadvantage and challenge of the formulation is the unintentional reactivity of antibacterial agents with formulation ingredients. This can include oxidative degradation. Petition 870260030969, dated 02 / 04 / 2026, page 5 / 57 2 / 42 hydrolysis, adsorption or precipitation of oxyhydroxide species, any of which may affect the bioavailability of the antibacterial agent.

[0003] Soluble zinc salt is one of the antibacterial agents that have been used in toothpaste compositions, but it has several challenges, including unintentional reaction with fluoride ions to produce insoluble zinc fluoride, as well as an unpleasant astringent mouthfeel, etc. Furthermore, zinc ions will react with anionic surfactants, such as sodium lauryl sulfate, thus interfering with foaming and cleaning. Therefore, there is a need to optimize the use of zinc in the formulation.

[0004] Sodium lauryl sulfate (SLS) is widely used in toothpaste formulations, offering numerous benefits with broad compatibility with other ingredients, a neutral taste, and good foaming properties. However, there is ongoing consumer interest in the development of oral hygiene products that do not contain sodium lauryl sulfate. One concern has been that SLS may be a potential source of irritation, scaling, and epithelial barrier dysfunction in the gingiva. Having a strong barrier function in the gingival epithelium is a physical barrier that separates biofilm from gingival tissue, providing the first line of defense against bacterial invasion in gingivitis or periodontal disease. Stannous fluoride has a bactericidal and bacteriostatic effect on plaque bacteria.It has also been shown to reduce the virulence of bacterial endotoxin biofilms, such as lipopolysaccharide (LPS) and lipoteichoic acid (LTA). Petition 870260030969, dated 02 / 04 / 2026, p. 6 / 57 3 / 42 are associated with the initiation of inflammatory processes involved in periodontal disease and the disruption of epithelial barrier function. Brushing with stannous fluoride toothpaste leads to a reduction in gingivitis and, as a result, to the restoration of barrier function, making the gum tissue more resistant to bacterial attacks.

[0005] Thus, there is a continuing need to provide enhanced stannous and fluoride-containing products to help control plaque bacteria on teeth and / or protect against bacterial / toxin invasion, which do not contain sodium lauryl sulfate, but nevertheless have adequate stability and aesthetics and do not irritate or compromise the gingival epithelium. SUMMARY OF THE INVENTION

[0006] The present invention relates to a composition for oral hygiene comprising: (a) from 0.01% to 5%, by weight of the composition, of a source of stannous ions; (b) from 0.1% to 5%, by weight of the composition, of a taurate-based surfactant represented by formula (I): R2 II I Rj--C—N—CH2—CH2—SO3-M+, (I) where Ri is a saturated or unsaturated alkyl chain, linear or branched with 6 to 18 C atoms; R2 is H or methyl, and M is H, sodium or potassium; and wherein the oral hygiene composition is substantially free of a zinc ion source. Petition 870260030969, dated 02 / 04 / 2026, p. 7 / 57 4 / 42

[0007] Significant disruption and destabilization of dental biofilm can be achieved by an aqueous oral hygiene composition comprising a stannous ion source and a taurate-based surfactant in the absence of a zinc ion source. An advantage of the present invention is the optimized deep penetration into the biofilm and / or extermination of bacteria. To this end, surprisingly, it has also been found that the penetration depth and / or penetration rate of stannous ion / zinc ion into biofilms can be increased when used in combination with taurate. In summary, the synergistic combination of taurate as a stannous ion source in the oral hygiene composition can be such that an improvement in gum health benefits is obtained.

[0008] It is an advantage of the present invention to provide effective antibacterial properties by combining a taurate-based surfactant with a stannous element in a zinc-free oral hygiene composition. It is a further advantage of the present invention to provide oral hygiene compositions with improved deposition / penetration of Sn / Zn ions into the biofilm, as well as to provide impact toxin neutralization of the healing recovery of human gingival epithelial cells (HGE).

[0009] It is also an added advantage that the oral hygiene composition be a toothpaste and preferably provide pleasant sensory experiences, such as taste, foam and mouthfeel.

[0010] It is also an added advantage that the oral hygiene composition exhibits good stability over a wide pH range. It is also an added advantage that the Petition 870260030969, dated 02 / 04 / 2026, page 8 / 57 5 / 42 Oral hygiene compositions have physical and chemical stability over a range of manufacturing, handling, and storage conditions. It is a further advantage that the oral hygiene compositions have stable product quality (e.g., consistent visual appearance and no discoloration, etc.) even after three months of storage at 40°C. It is also a further advantage that the oral hygiene compositions of the present invention minimize the use of antibacterial agents.

[0011] It is a further advantage that the oral hygiene compositions of the present invention use taurate to reduce and / or eliminate the instability and / or discoloration problems of conventional toothpastes containing tin, as described above. It is also a further advantage that the oral hygiene composition of the present invention surprisingly provides an improved sensory profile and / or reduces potential astringency during and after brushing.

[0012] The present invention further encompasses a method for treating dental biofilm comprising the step of brushing teeth with an oral hygiene composition of the present invention.

[0013] The invention further provides a method for preventing or mitigating plaque formation on dental enamel comprising the step of brushing teeth with an oral hygiene composition of the present invention. DETAILED DESCRIPTION OF THE INVENTION Definitions

[0014] For use in the present invention, the indefinite articles a and an, when used in a Petition 870260030969, dated 02 / 04 / 2026, page 9 / 57 6 / 42 claim, are understood to mean one or more of the items claimed or described.

[0015] The terms relieve and relieving are used interchangeably and mean to minimize, prevent, delay and / or treat at least one symptom of gum disease to produce a positive change (i.e., a benefit) for the user.

[0016] The term biofilms for use in the present invention means a bacterial population embedded in a matrix that adheres to each other and / or to surfaces or interfaces in the oral cavity.

[0017] The term comprising, as used herein, means that steps and ingredients beyond those specifically mentioned may be added. This term encompasses the terms consisting of and consisting essentially of. The compositions of the present invention may comprise, consist of, and consist essentially of the essential elements and limitations of the invention described herein, as well as any of the additional or optional ingredients, components, steps, or limitations described herein.

[0018] The term oral hygiene composition or oral hygiene compositions for use in the present invention refers to a product that, in its normal use, is retained in the oral cavity for a sufficient time to come into contact with some or all of the dental surfaces and / or oral tissues for purposes of oral activity. In one example, the composition provides a gum care benefit when used in the oral cavity. The oral hygiene composition of the present invention may be of various types. Petition 870260030969, dated 02 / 04 / 2026, page 10 / 57 7 / 42 forms, including toothpaste, toothbrush, dental gel, dental powders, tablets, mouthwash, mouth rinse, subgingival gel, foam, mousse, chewing gum, lipstick, sponge, dental floss, prophylactic paste, petrolatum gel, denture adhesive or denture product. In one example, the oral composition exists in the form of a paste or gel. In another example, the oral composition exists in the form of a toothpaste. The oral composition may also be incorporated into strips or films for direct application or fixation to oral surfaces or incorporated into dental floss.

[0019] As used in the present invention, the term dentifrice means paste, gel, powder, tablets or liquid formulations, except where otherwise specified, that are used to clean the surfaces of the oral cavity. Preferably, the dentifrice compositions of the present invention are single-phase compositions, although the compositions may be two-phase or multi-phase compositions. An example of a dentifrice composition is toothpaste (for brushing teeth). The term teeth, as used in the present invention, refers to natural teeth as well as artificial teeth or dental prostheses.

[0020] The term partially soluble or partially soluble in water, as used herein, means that a compound has a solubility of 1 g / 1000 mL or more in water at 25 °C. The term insoluble, as used herein, means that a compound has a solubility of less than 0.1 g / 1000 mL at 25 °C.

[0021] The term effective amount, as used in the present invention, refers to an amount of a compound or composition sufficient to induce a benefit. Petition 870260030969, dated 02 / 04 / 2026, page 11 / 57 8 / 42 positive, or an oral health benefit, and / or in a quantity low enough to avoid serious side effects, that is, to provide an adequate benefit-risk ratio, within the good judgment of one skilled in the art. In one example, effective quantity means at least 0.01% of the material, by weight of the composition, and alternatively, at least 0.1%.

[0022] As used herein, the words preferred, preferably, and their variants refer to embodiments of the invention that provide certain benefits under certain circumstances. However, other embodiments may also be preferred under the same circumstances or under different circumstances. Furthermore, mention of one or more preferred embodiments does not imply that other embodiments are not useful and is not intended to exclude other embodiments from the scope of the invention.

[0023] The term substantially free, as used herein, refers to an unintentional amount of that material that is added to the composition or an amount of a material that is less than 0.05%, 0.01%, or 0.001% of the composition. The term essentially free, as used herein, means that the indicated material is not deliberately added to the composition or, preferably, is not present in analytically detectable amounts. This includes compositions in which the indicated material is present only as an impurity of one of the other deliberately added materials. The term free, for use in the present invention, refers to the fact that no reasonably detectable amount of that material is present in the composition. Petition 870260030969, dated 02 / 04 / 2026, page 12 / 57 9 / 42

[0024] The term total water content, as used herein, means both free water and water that is bound by other components in the oral hygiene composition.

[0025] All percentages, parts, and ratios are based on the total weight of the compositions of the present invention, except where otherwise specified. All weights mentioned that refer to ingredients mentioned herein are based on the active content and therefore do not include solvents or by-products that may be included in commercially available materials, except where otherwise indicated. The term percentage by weight may be denoted as % by weight in this document. All molecular weights, as used in this document, are weight-average molecular weights expressed in grams / mol, except where otherwise specified.

[0026] All measurements mentioned in the present invention are made at 25 °C (i.e., room temperature) unless otherwise specified. Oral hygiene products

[0027] Surprisingly, it has been found that the combination of stannous ions (i.e., an antibacterial agent) and an amino acid-based taurate surfactant, in the absence of a zinc ion source, in an oral hygiene composition is particularly useful for controlling plaque bacteria and maintaining the integrity and barrier function of the gums, i.e., promoting gum health benefits for users. In particular, the surprising finding relates to the fact that the penetration of stannous ions into biofilms is markedly improved when combined with taurate. Without adhering to theory, the surfactant Petition 870260030969, dated 02 / 04 / 2026, p. 13 / 57 10 / 42 taurate-based compounds are derived from an amino acid containing both carboxylic and amine groups. Stannous ions are believed to bind strongly to these chemical moieties of the amino acid, positively influencing stannous ion penetration into biofilms.

[0028] It was also surprisingly discovered that the penetration depth and / or penetration rate of stannous ions into biofilms can be increased, or markedly increased, when formulated with a taurate-based surfactant, compared to other anionic surfactants such as SLS. In summary, the presence of taurate in combination with the stannous ion source in a zinc-free composition aids in the effectiveness of the composition in mediating the harmful effects of bacteria in biofilms on the gingiva.

[0029] In one aspect, the present invention is directed to an oral hygiene composition comprising: (a) from 0.01% to 5%, by weight of the composition, of a source of stannous ions; (b) from 0.1% to 5%, by weight of the composition, of a taurate-based surfactant represented by formula (I) o r2 II I R] CN—CH2—CH2—SOfM1, (I) where Ri is a saturated or unsaturated, linear or branched alkyl chain with 6 to 18 carbon atoms; R2 is H or methyl, and M is H, sodium or potassium; and Petition 870260030969, dated 02 / 04 / 2026, p. 14 / 57 11 / 42, with the oral hygiene formula being substantially free of a zinc ion source. Source of stannous ions

[0030] The present invention relates to the oral hygiene compositions mentioned above comprising, in a preferred example, the stannous ion source present in an amount of 0.01% to 5%, or 0.05% to 5%, preferably 0.05% to 4%, or, more preferably, 0.1% to 2%, by weight of the composition, to provide antibacterial efficacy. The stannous ion source used in the present invention may include any safe and effective stannous salt.Suitable examples of stannous ion sources are selected from soluble stannous salts, and preferably from the group consisting of stannous chloride, stannous fluoride, stannous acetate, stannous gluconate, stannous oxalate, stannous sulfate, stannous lactate, stannous tartrate, stannous iodide, stannous chlorofluoride, stannous hexafluorozirconate, stannous citrate, stannous malate, stannous glycinate, stannous carbonate, stannous phosphate, stannous pyrophosphate, stannous metaphosphate, and combinations thereof; preferably, the stannous ion source is selected from stannous chloride, stannous fluoride, or a combination thereof.

[0031] In a preferred example, the stannous ion source comprises stannous chloride. In another preferred example, the stannous ion source comprises stannous fluoride. In a particular preferred example, the stannous ion source comprises a combination of stannous fluoride and stannous chloride. Petition 870260030969, dated 02 / 04 / 2026, p. 15 / 57 12 / 42

[0032] In some examples, the oral hygiene composition of the present invention is substantially free of stannous oxide from the source of insoluble stannous ions, preferably and essentially free of stannous oxide, more preferably free of stannous oxide. Taurate-based surfactant

[0033] The oral hygiene composition of the present invention contains a taurate-based surfactant as the main surfactant. Taurate is represented by formula (I): R2 II I Rj C—N—CH2—CH2—SO3-M+, (I) where Ri is a saturated or unsaturated alkyl chain, linear or branched with 6 to 18 C atoms; R2 is H or methyl, and M is H, sodium or potassium.

[0034] Preferably, Ri is a saturated or unsaturated, linear or branched alkyl chain with 8 to 18 C atoms. Optionally, but preferably, the taurate-based surfactant of the present invention comprises one or more selected from the group consisting of potassium cocoyl taurate, potassium methyl cocoyl taurate, sodium caproyl methyl taurate, sodium cocoyl taurate, sodium lauroyl taurate, sodium methyl cocoyl taurate, sodium methyl lauroyl taurate, sodium methyl myristoyl taurate, sodium methyl oleoyl taurate, and combinations thereof. Petition 870260030969, dated 02 / 04 / 2026, page 16 / 57 13 / 42 Free from zinc ion sources

[0035] Preferably, oral hygiene compositions are substantially free of a zinc ion source. For example, the zinc ion source may be selected from soluble zinc ion sources such as zinc citrate, zinc chloride, zinc sulfate, zinc gluconate, zinc lactate, or from insoluble ion sources such as zinc phosphate, zinc oxide, zinc carbonate, and combinations thereof. In some examples, the zinc ion source is present in an amount of 0% to less than 0.005%, or preferably from 0% to 0.001%, by weight of the composition. Preferably, the oral hygiene composition is free of a zinc ion source. Source of fluoride ions

[0036] The compositions may optionally, but preferably, include an effective amount of an anticaries agent as a source of fluoride ions. The fluoride ion may be present in a sufficient amount to result in a fluoride ion concentration in the composition at 25 °C and / or, in one embodiment, may be used in amounts of about 0.0025% to about 5% by weight of the composition; preferably from about 0.005% to about 2.0%; preferably from 0.5% to about 1.5% by weight of the composition, to provide anticaries efficacy. Representative sources of fluoride ions include stannous fluoride, sodium fluoride, potassium fluoride, sodium monofluorophosphate, or mixtures thereof. In one aspect, the oral hygiene compositions of the present invention may have a dual fluoride ion source, specifically sodium monofluorophosphate and an alkali metal fluoride. Alternatively, the compositions Petition 870260030969, dated 02 / 04 / 2026, page 17 / 57 14 / 42 for oral hygiene of the present invention may contain a dual fluoride ion source that is a combination of stannous fluoride and sodium fluoride. Without delving into theory, such an approach may provide an improvement in average fluoride absorption.

[0037] In some preferred examples, the fluoride ion source is selected from stannous fluoride, sodium monofluorophosphate, sodium fluoride, or combinations thereof.

[0038] In one aspect, the oral hygiene composition of the present invention does not contain amine fluoride (also called olaflur). Secondary surfactant

[0039] The oral hygiene compositions of the present invention may include a secondary surfactant, other than the taurate-based surfactant. The composition may include a secondary surfactant in a content of about 0.01% to about 10%, about 0.025% to about 9%, about 0.05% to about 5%, about 0.1% to about 2.5%, about 0.5% to about 2%, or about 0.1% to about 1%, by weight, of the composition.

[0040] Preferably, the secondary surfactant may be an amphoteric surfactant, for example, selected from the group consisting of betaine surfactants. Non-limiting examples of amphoteric surfactants may be composed of a betaine or a sultaine selected from the group consisting of: almondamidopropyl betaine, apricotamidopropyl betaine, avocadomidopropyl betaine, babassuamidopropyl betaine, behamidopropyl betaine, canolamidopropyl betaine, capryl / capramidopropyl betaine, cocoamidopropyl betaine, Petition 870260030969, dated 02 / 04 / 2026, p. 18 / 57 15 / 42 coco / oleamidopropyl betaine, coco / sunflower starch propyl betaine, cupuaçu starch propyl betaine, isostearamidopropyl betaine, lauramidopropyl betaine, meadowfoamidopropyl betaine, milk starch propyl betaine, vinoamidopropyl betaine, myristamidopropyl betaine, oat starch propyl betaine, oleamidopropyl betaine, olivamidopropyl betaine, palmamidopropyl betaine, palmitamidopropyl betaine, palm oil starch propyl betaine, ricinoleamidopropyl betaine, sesamidopropyl betaine, shea butter starch propyl betaine, soybean starch propyl betaine, stearamidopropyl betaine, tallow starch propyl betaine, undecylene starch propyl betaine, wheat germ starch propyl betaine, cocamidopropyl hydroxysultaine (CAPHS), Lauramidopropyl hydroxysultaine (LAPHS), oleamidopropyl hydroxysultaine (OAPHS), tallowamidopropyl hydroxysultaine (TAPHS), and combinations thereof;Preferably selected from the group consisting of cocoamidopropyl betaine, lauramidopropyl betaine, oleamidopropyl betaine, seboamidopropyl betaine, cocamidopropyl hydroxysultain and combinations thereof; and, more preferably, selected from cocoamidopropyl betaine, lauramidopropyl betaine or a combination thereof.

[0041] In addition, the secondary surfactant may also be a nonionic surfactant or another anionic surfactant other than SLS taurate or sulfate. In some embodiments, the secondary surfactant in the oral hygiene compositions of the present invention may be nonionic surfactants that are, for example, compounds produced by the condensation of alkylene oxide groups (of a hydrophilic nature) with a hydrophobic organic compound, which may be of an aliphatic nature. Petition 870260030969, dated 02 / 04 / 2026, page 19 / 57 16 / 42 or alkylaromatic. Examples of suitable nonionic surfactants may include Pluronics® which are poloxamers, alkyl phenol polyethylene oxide condensates, products derived from the condensation of ethylene oxide with the reaction product of propylene oxide and ethylenediamine, aliphatic alcohol ethylene oxide condensates, long-chain tertiary amine oxides, long-chain tertiary phosphine oxides, long-chain dialkyl sulfoxides and combinations of such materials. Suitable anionic surfactants as the secondary surfactant of the composition of the present invention may include sarcosinates, isethionates, alkyl phosphates, etc.

[0042] In one aspect, the composition of the present invention is substantially free of sodium lauryl sulfate (SLS). Preferably, the composition of the present invention is essentially free of, more preferably, sodium lauryl sulfate (SLS). Without delving into theory, such an approach may provide an improvement in the consumer's sensory experience by reducing oral tissue irritation. Abrasive containing calcium

[0043] The compositions of the present invention may optionally, and in some respects preferably, comprise from about 5% to about 50%, preferably from about 10% to about 50%, by weight of the composition, of a calcium-containing abrasive, wherein the calcium-containing abrasive is preferably selected from the group consisting of calcium carbonate, calcium glycerophosphate, dicalcium phosphate, tricalcium phosphate, calcium orthophosphate, calcium metaphosphate, calcium polyphosphate, calcium oxyapatite, sodium carbonate and mixtures thereof; wherein, Petition 870260030969, dated 02 / 04 / 2026, page 20 / 57 17 / 42 more preferably, the calcium-containing abrasive is calcium carbonate. Preferably, the composition comprises from about 15% to about 50%; preferably from about 15% to about 40%; preferably from about 15% to about 25%, by weight, of the composition, of a calcium-containing abrasive.

[0044] Preferably, the abrasive containing calcium is calcium carbonate. More preferably, the abrasive containing calcium is selected from the group consisting of finely ground natural chalk, ground calcium carbonate, precipitated calcium carbonate, and combinations thereof. Some non-limiting examples of the percentages by weight of the abrasive containing calcium include: about 15%, about 20%, about 25%, or about 30% by weight of the composition, preferably the abrasive containing calcium being calcium carbonate. Silica-based abrasive

[0045] Dental abrasives based on silica, of various types, are preferred due to their unique benefits of exceptional tooth cleaning and polishing performance without undue abrasion of enamel or dentin. The silica-based abrasive polishing materials of the present invention, as well as other abrasives, generally have an average particle size in the range of about 0.1 to about 30 microns, preferably about 5 to about 15 microns. For example, the silica-based abrasives used in the present invention are precipitated silica (e.g., sodium silicate solution by destabilization with acid to produce very fine particles), such as those of the ZEODENT® series from Huber Engineered Materials (e.g., ZEODENT® 103, 124, 113, 115, 163, 165, Petition 870260030969, dated 02 / 04 / 2026, page 21 / 57 18 / 42 167). It is recognized that some of these silicas (e.g., synthetic amorphous silica) can perform both thickening and abrasive functions, but are included in the present invention under the term abrasive for the purposes of the present invention. Preferably, the oral hygiene composition comprises from 1% to 35%, more preferably from 5% to 25%, by weight of the composition, of abrasive. Water

[0046] The oral hygiene compositions of the present invention may include from 10% to 60%, by weight of the composition, of the total water content. In some examples, the oral hygiene composition may include from 10% to 50% or, preferably, from 10% to 40%, by weight of the composition, of the total water content. The term total water content, as used herein, means the total amount of water present in the composition, added separately or present as a solvent or carrier for other raw materials, but excluding that which may be present as water of crystallization in certain inorganic salts. Preferably, the water is USP water.

[0047] Water is commonly used as a carrier material in oral hygiene compositions due to its many benefits. For example, water is useful as a processing aid, is benign to the oral cavity, and helps in the rapid foaming of toothpastes. Water can be added as a standalone ingredient or can be present as a carrier for other common raw materials, for example, sorbitol. Petition 870260030969, dated 02 / 04 / 2026, page 22 / 57 19 / 42 pH

[0048] The pH of the oral hygiene composition may be in the range of about 4.0 to about 9.0; preferably, from about 4.3 to about 8.0; more preferably, from about 4.6 to about 7.5. In some examples, the composition has a pH that is in the range of 4.0 to 4.9. In alternative examples, the composition may have a pH in the range of 5.0 to 6.0. In other examples, the composition has a pH in the range of 6.1 to 7.3. In some other examples, the composition may have a pH in the range of 7.5 to 9.0. A method for evaluating the pH of oral hygiene is described below. For clarification purposes, although the analytical method describes testing the oral hygiene composition when freshly prepared, for the purposes of the present invention claim, the pH can be taken at any time during the reasonable life cycle of the product (including, but not limited to, the time when the product is purchased from a store and taken to the user's home). pH modifying agent

[0049] The oral hygiene compositions of the present invention may include an effective amount of a pH modifying agent, preferably a pH buffering agent. pH modifying agents, as used herein, refer to agents that can be used to adjust the pH of the oral hygiene compositions to the pH range identified above. The compositions may comprise from about 0.001% to about 5%, by weight of the composition, of pH modifying agent. pH modifying agents may include alkali metal hydroxides, ammonium hydroxide, organic ammonium compounds, carbonates, sesquicarbonates, borates, silicates, phosphates, Petition 870260030969, dated 02 / 04 / 2026, page 23 / 57 20 / 42 imidazole and mixtures thereof. Specific pH agents include monosodium phosphate (monobasic sodium phosphate or MSP), trisodium phosphate (tribasic sodium phosphate dodecahydrate or TSP), sodium benzoate, benzoic acid, sodium hydroxide, potassium hydroxide, alkali metal carbonate salts, sodium carbonate, imidazole, pyrophosphate salts, tripolyphosphate salts, sodium gluconate, lactic acid, sodium lactate, citric acid, sodium citrate, and phosphoric acid. Without adhering to theory, phosphate may also have calcium ion chelating activity and therefore provide some stabilization of monofluorophosphate (in those formulations containing monofluorophosphate).

[0050] A method for evaluating oral hygiene pH is described. The pH is measured by a pH meter with an automatic temperature compensating (ATC) probe. The pH meter is capable of reading down to 0.001 pH units. The pH electrode can be selected from one of the following elements: (i) Orion Ross Sure-Flow combinations: glass body - VWR No. 34104-834 / Orion No. 8172BN or VWR No. 10010-772 / Orion No. 8172BNWP; epoxy body - VWR No. 34104-830 / Orion No. 8165BN or VWR No. 10010-770 / Orion No. 8165BNWP; (i) epoxy body, semimicro - VWR No. 34104837 / Orion No. 8175BN or VWR No. 10010-774 / Orion No. 3175BNWP; or (ii) combination of Orion Perfect: glass body, semimicro VWR No. 34104-843 / Orion No. 8203BN; or (iii) suitable equivalent. The probe with automatic temperature compensation is a Fisher Scientific, cat. No. 13-620-16.

[0051] A 25% by weight fluid oral hygiene paste is prepared with deionized water and then centrifuged for 10 minutes at 15,000 revolutions per minute. Petition 870260030969, dated 02 / 04 / 2026, page 24 / 57 21 / 42 using a SORVALL RC 28S centrifuge and an SS34 rotor (or equivalent gravitational force, at 24149 g of force). The pH is assessed in the supernatant after one minute or when the reading stabilizes. After each pH assessment, the electrode is washed with deionized water. Any excess water is wiped off with a laboratory-grade tissue. When not in question, the electrode is kept immersed in a pH 7 buffer solution or an appropriate electrode storage solution. Humectants

[0052] The oral hygiene compositions of the present invention may include humectants present in amounts of 0% to 70% or 15% to 55% by weight of the compositions. Humectants prevent the oral hygiene compositions from hardening after exposure to air, and certain humectants may also impart a desirable sweetness of taste to the oral hygiene compositions. Suitable examples of humectants may include glycerin, sorbitol, polyethylene glycol, propylene glycol, xylitol, trimethyl glycine, and mixtures thereof. Other examples may include other edible polyhydric alcohols. In some examples, the humectant is selected from sorbitol, glycerin, and combinations thereof. In a preferred example, the humectant is sorbitol. In another preferred example, the humectant is glycerin. In one example, the composition comprises 10% to 66%, or alternatively, 20% to 55%, by weight of the composition, of humectant. Thickening system

[0053] The oral hygiene compositions of the present invention may comprise a thickening system. Of Petition 870260030969, dated 02 / 04 / 2026, page 25 / 57 22 / 42 Preferably, the oral hygiene composition comprises from about 0.5% to about 10%; preferably from about 0.8% to about 5%; more preferably from about 1% to about 5%, by weight of the composition, of a thickening system. More preferably, the thickening system comprises a thickening polymer, a thickening silica, or a mixture thereof. Even more preferably, when the thickening system comprises a thickening polymer, the thickening polymer is selected from carboxymethylcellulose, a linear sulfated polysaccharide, a natural gum, or mixtures thereof.Even more preferably, when the thickening system comprises a thickening polymer, the thickening polymer is selected from the group consisting of: (a) from about 0.01% to about 3% of a carboxymethylcellulose (CMC), by weight, of the composition; preferably from about 0.1% to about 2.5%; more preferably from about 0.5% to about 1.7%, by weight, of CMC; (b) from about 0.01% to about 2.5%; preferably from about 0.05% to about 2%; more preferably from about 0.1% to about 1.5%, by weight, of a linear sulfated polysaccharide, wherein, preferably, the linear sulfated polysaccharide is a carrageenan; (c) from about 0.01% to about 3%; preferably from about 0.1% to about 2%; more preferably from about 0.2% to about 1.8%, by weight, of the composition of a natural gum; or (d) mixtures thereof.

[0054] The thickening polymer may also include non-colloidal microcrystalline cellulose, colloidal microcrystalline cellulose, or a mixture thereof. Non-colloidal microcrystalline cellulose, typically called cellulose Petition 870260030969, dated 02 / 04 / 2026, page 26 / 57 23 / 42 microcrystalline cellulose, or MCC, is a purified, partially depolymerized cellulose, for example, AVICEL® PH 102 or PH 105. Colloidal microcrystalline cellulose is obtained by reducing the particle size of microcrystalline cellulose and stabilizing the particles to prevent the formation of hard aggregates, for example, AVICEL® CL 611 or RC 591.

[0055] Preferably, when the thickening system comprises a thickening silica, the thickening silica is from about 0.01% to about 8%; preferably from about 0.1% to about 5%; preferably from about 1% to about 3%, by weight of the composition.

[0056] Preferably, the linear sulfated polysaccharide is a carrageenan (also known as carrageenan). Examples of carrageenan include kappa-carrageenan, iotacarrageenan, lambda-carrageenan, or mixtures thereof.

[0057] In one aspect, thickening silica is obtained from a sodium silicate solution by destabilizing it with acid to produce very fine particles. A commercially available example is the ZEODENT® brand silicas, available from Huber Engineered Materials (e.g., ZEODENT® 103, 124, 113, 115, 163, 165 and 167).

[0058] In one aspect, CMC is prepared from cellulose by treatment with alkali and monochloroacetic acid or its sodium salt. Different varieties are commercially distinguished by viscosity. A commercially available example is Aqualon™ brand CMC from Ashland Special Ingredients (e.g., Aqualon™ 7H3SF; Aqualon™ 9M3SF Aqualon™ TM9A; Aqualon™ TM12A). Petition 870260030969, dated 02 / 04 / 2026, page 27 / 57 24 / 42

[0059] Preferably, a natural gum is selected from the group consisting of karaya gum, gum arabic (also known as acacia gum), tragacanth gum, xanthan gum, and mixtures thereof. Preferably, the natural gum is xanthan gum. Xanthan gum is a polysaccharide secreted by the bacterium Xanthomonas camestris. In general, xanthan gum is composed of repeating pentasaccharide units comprising glucose, mannose, and glucuronic acid in a molar ratio of 2:2:1, respectively. The chemical formula (of the monomer) is C35H49O29. In one aspect, xanthan gum is available from CP Kelco Inc. (Okmulgee, USA).

[0060] In one aspect, the thickening polymer is selected from the group consisting of a carboxymethylcellulose, a linear sulfated polysaccharide, a natural gum and mixtures thereof. Viscosity

[0061] Preferably, the oral hygiene compositions of the present invention have a viscosity range of about 200,000 centipoises to about 850,000 centipoises (cP). A method for evaluating viscosity is described. The viscometer is a Brookfield® viscometer, model DV-I Prime, with a Brookfield Helipath holder. The viscometer is placed in the Helipath holder and leveled using a bubble level. Spindle E is fixed, and the viscometer is set to 2.5 RPM. Separate the spindle, zero the viscometer, and install spindle E. Then, lower the spindle until the crosshead is partially submerged in the paste before starting the measurement. Simultaneously turn on the power switch on the viscometer and the helipath to start the spindle's downward rotation. Adjust Petition 870260030969, dated 02 / 04 / 2026, p. 28 / 57 Set a timer for 48 seconds at 25 / 42 and turn the timer on at the same time as the motor and the helipath. Take a reading after 48 seconds. The reading is in cP. Dye

[0062] The compositions of the present invention may include a colorant. Titanium dioxide is an example of a colorant. Titanium dioxide is a white powder that imparts opacity to the compositions. The colorant, for example, titanium dioxide, may generally comprise from about 0.25% to about 5% by weight of the composition. Flavoring agent

[0063] The toothpaste composition of the present invention may include from 0.01% to 5%, preferably from 0.1% to 2%, by weight of the composition, of a flavoring agent. Examples of suitable flavoring agents that may be used in the toothpaste composition include those described in U.S. Patent No. 8,691,190; Haught, JC, from column 7, line 61, to column 8, line 21. In some examples, the flavoring agent may be selected from methyl salicylate, menthol, eugenol, and cineole. In some examples, the toothpaste composition may comprise a flavor and aroma mixture that is free or substantially free of methyl salicylate, menthol, eugenol, and cineole. Sweetener

[0064] The toothpaste compositions of the present invention may include a sweetening agent. The sweetening agent is generally present in the toothpaste compositions in proportions of 0.005% to 5% by weight of the composition. Suitable examples of sweeteners include saccharin, dextrose, sucrose, lactose, xylitol, maltose, levulose, aspartame, cyclamate. Petition 870260030969, dated 02 / 04 / 2026, page 29 / 57 26 / 42 sodium, D-tryptophan, dihydrochalcones, acesulfame, sucralose, neotame, and mixtures thereof. Other examples of suitable sweeteners are described in U.S. Patent No. 8,691,190; Haught, JC, from Column 9, line 18 to Column 10, line 18. Other ingredients

[0065] The present oral hygiene composition may comprise the usual and conventional auxiliary components known to those skilled in the art. Optional ingredients include, for example, but are not limited to, anti-plaque agent, anti-sensitivity agent, whitening and oxidizing agent, anti-inflammatory agent, anti-calculus agent, chelating agent, tooth-adhering agent, analgesic and anesthetic agent. It will be understood that the components selected for the oral hygiene compositions need to be chemically and physically compatible with each other.

[0066] Preferably, the oral hygiene composition of the present invention is essentially free of glycyrrhetinic acid and its salt. Method of use

[0067] In one aspect, the present invention relates to a method for treating dental biofilm. The method comprises the step of brushing / cleaning the teeth with an oral hygiene composition according to the present invention. The method comprises placing an individual's teeth in contact with the oral hygiene compositions according to the present invention.

[0068] In another aspect, the present invention also relates to a method for controlling plaque bacteria in an individual comprising administering to the individual's oral cavity an oral hygiene composition in accordance with Petition 870260030969, dated 02 / 04 / 2026, p. 30 / 57 27 / 42 present invention, and preferably, administration occurs at least once a day, more preferably at least twice a day. TESTING METHODS Test method 1: Assay for measuring the enhanced endotoxin neutralization of the antibacterial agent in biofilms

[0069] To determine the enhanced endotoxin neutralization of the antibacterial agent in biofilms, the subsequent assay is used to evaluate the LPS binding efficiency of stannous ions via measurement of a fluorescent dye that is bound to LPS lipid A in plaque biofilms in situ for oral hygiene compositions of the present invention and controls. Details of the invention are described below. (a) Substrate for biofilm growth

[0070] Hydroxyapatite (HA) discs are used for in situ biofilm growth. HA discs are designed with three parallel grooves (i.e., 200 µm wide; 200 µm deep for the two-sided grooves; while 500 µm wide and 500 µm deep for the intermediate groove) on each disc. When fixing the discs in an individual's mouth, keeping these grooves vertical mimics the interproximal space between teeth, the hard-to-clean area where plaque tends to accumulate. This design allows for the collection of undisturbed plaque from the grooves. HA discs are manufactured by Shanghai Beierkang Biomedicine Limited. Petition 870260030969, dated 02 / 04 / 2026, page 31 / 57 28 / 42 (b) Using the splint

[0071] Human subjects use the splint. Each patient uses up to 12 HA discs in the splint to ensure that at least 9 HA discs are available after 48 hours. In a specific example, and with reference to Figure 2, the HA disc has three parallel grooves (the grooves on the two sides are 300 μm wide and 300 μm deep; while the intermediate groove (between the two lateral grooves) is 500 μm wide and 500 μm deep). The intermediate groove is designed wider and deeper than the two lateral grooves so that the HA disc can be more easily separated into two identical half-discs for head-to-head comparison purposes. Further details of the HA discs are described in US2017 / 0056531 (e.g., paragraphs

[0019] to

[0020] ).

[0072] The discs can be positioned so that the indentation is in the interdental space between the teeth (since this area is prone to plaque formation (given the difficulty of cleaning, etc.)). Individuals remove the splint only during meals (the splint is stored in an opaque container under humid conditions) and to perform oral hygiene procedures. Immediately afterwards, the splint is used again. Individuals are asked to use a straw when drinking. (c) In situ release of biofilms from the HA disc

[0073] All HA discs are removed from the splint after 48 hours using forceps. The forceps are used to hold the edge of the HA chips and transfer the HA disc to a 2 mL centrifuge tube containing phosphate-buffered saline (PBS). The Petition 870260030969, dated 02 / 04 / 2026, p. 32 / 57 29 / 42 forceps are thoroughly washed (water; 75% alcohol; and then deionized water) before each disc transfer. (d) Preparation of toothpaste supernatants

[0074] 15 grams of deionized water are added to 5 grams of toothpaste from test samples. After vigorous shaking, the mixture is centrifuged at 12000 rpm for 20 minutes. The supernatant is prepared one day before use and stored at 4 °C. (e) Confocal laser scanning microscopy

[0075] After the HA discs are removed from the splint. The HA discs are used for ex vivo treatment by the different compositions of the invention and control. After being treated with the supernatant in question and labeled with the microbial fluorescent probe and the stannous fluorescent probe, the biofilms in the grooves are measured by confocal laser scanning microscopy (CLSM) (as described below). Preferably, the neutralized LPS fluorescent probe is BODIPY-TR-cadaverine (BC) (available from Thermo Fisher). Preferably, the microbial fluorescent probe is the Molecular Probes™ LIVE / DEAD® BacLight™ system (available from Thermo Fisher). (f) Disc preparation

[0076] The HA discs are rinsed in PBS solution, and each HA disc is divided into two halves using forceps. After that, each disc half is placed in 500 to 1000 μL of PBS solution statically for 1 minute. Each disc is treated for two minutes with PBS solution or toothpaste supernatant. Each disc is washed, each being held by forceps, shaken ten times forward. Petition 870260030969, dated 02 / 04 / 2026, page 33 / 57 30 / 42 and back in 1 mL of PBS solution, and then this washing cycle is repeated. Then, each disc is immersed in 500 to 1000 μL of PBS solution, statically, for 5 minutes. (g) Staining and fluorescence microscopy

[0077] The neutralizing effect of LPS is evaluated using BODIPY-TR-cadaverine (BC), a fluorescent dye that is bound to lipid A, thus suppressing its fluorescence. BC is displaced by agents with an affinity for this lipid. When LPS is bound by other ions, for example, tin, BC is released from LPS and its fluorescence is proportional to the amount of free (unbound) BC present. Therefore, the fluorescence level indicates the amount of neutralized (bound) LPS versus free (unbound) LPS, and the effectiveness of an antibacterial agent in reducing biofilm toxicity. The greater the amount of bound LPS, the lower its toxicity.

[0078] After treatment and immersion, each disc is stained with the BODIPY-TR-cadaverine (BC) probe together with the Syto-9 probe (containing 5 μM BC probe and 5 μM Sn probe) for 30 minutes in the dark. After staining, each disc is immersed in 500 to 1000 μL of PBS solution statically for 2 minutes. The discs are washed again, holding each disc with tweezers, agitated five times back and forth in 1 mL of PBS solution, and then the cycle is repeated. For samples stained with SYTO-9 / BC dye, the following parameters are used: λex = 488 nm / 543 nm, λem = 500 / 580 nm, 20X objective lens and scanning from the bottom of the bacteria to the surface to 60 μm with a step size = 3 μm. Petition 870260030969, dated 02 / 04 / 2026, page 34 / 57 31 / 42 (h) Confocal Laser Scanning Microscopy

[0079] The Leica™ TCS SP8 AOBS spectral confocal microscope is used. The confocal system consists of a Leica™ DM6000B upright microscope and a Leica™ DMIRE2 inverted microscope. An upright stand is used for applications involving slide-mounted samples, while the inverted stand, which has a 37 °C incubation chamber and CO2 enrichment accessories, provides live cell applications. The microscopes share an interchangeable laser scanning head and, in addition to their own electromotor-driven stages, a high-precision galvanometer-driven Z-stage, which facilitates rapid focal plane (Z) imaging. In addition to epifluorescence, the microscopes support various transmitted light contrast methods, including bright field, polarizing light, and differential interference contrast, and are equipped with Leica™ 5x, 20x, 40x, 63x (oil and dry), and 100x (oil) objective lenses.

[0080] The laser detection and scanning system is described. The TCS SP8 AOBS confocal system is equipped with four lasers (one diode laser, one argon laser, and two helium lasers), thus allowing the excitation of a wide range of fluorochromes within the UV, visible, and ultraviolet ranges of the electromagnetic spectrum. The design of the laser scanning head, which incorporates acousto-optical tunable filters (AOTFs), an acousto-optical beam splitter (AOBS), and four prism spectrophotometer detectors, enables the simultaneous excitation and detection of three fluorochromes. The upright microscope also Petition 870260030969, dated 02 / 04 / 2026, p. 35 / 57 32 / 42 has a light transmission detector that makes it possible to superimpose a transmitted light image onto a fluorescence recording.

[0081] Leica™ Confocal software is used. Confocal microscopy is controlled via a standard Pentium PC equipped with two monitors and running Leica™ Confocal software. Leica Confocal software provides an interface for capturing, processing, and analyzing multidimensional image series, including 3D reconstruction and measurement, physiological recording and analysis, time-lapse, fluorochrome colocalization, photobleaching techniques such as fluorescence recovery after photobleaching (FRAP) and fluorescence resonance energy transfer (FRET), spectral mixing, and multicolor restoration. Regarding image analysis, samples stained with SYTO-9 / BC probe are selected to quantify the fluorescence intensity of red and green pixels. Efficacy of neutralizing LPS endotoxin

[0082] Using the software, the fluorescence intensity ratio (FIR) bound LPS / bacterial cell is calculated. This fluorescence intensity ratio indicates the relative amount of bound (neutralized) LPS per unit of bacteria, and the effectiveness of an agent in reducing biofilm toxicity. The higher the fluorescence intensity ratio, the greater the effectiveness in neutralizing LPS endotoxin. Petition 870260030969, dated 02 / 04 / 2026, page 36 / 57 33 / 42 Rate of penetration of the active ingredient into the biofilm.

[0083] Using the software, the pixel overlap of the green bacterial probes and the red stannous probes is identified, and then this value is divided by all non-black pixels (which includes non-overlapping stannous probes) to provide a percentage of stannous colocalization in the bacteria. Generally, the higher this stannous colocalization percentage, the greater the effectiveness of the oral hygiene product in releasing stannous to the bacteria. (See Xiang J, Li H, Pan B, Chang J, He Y, He T, Strand R, Shi Y, Dong W. (2018) Penetration and Bactericidal Efficacy of Two Oral Care Products in an Oral Biofilm Model. Am J Dent, Vol. 31, Issue 1: 53-60). Test Method 2: EC50 Test (Irritation) --- 2D cell-based method for evaluating oral irritation.

[0084] Half the maximum effective concentration (EC50) is a toxic unit that measures the concentration of a formula or toxicant that induces an intermediate response between the baseline and the maximum after a specified exposure time. (1) Cell line culture and test preparation:

[0085] Human gingival epithelial cells (HGE) were maintained in an incubator at 37 °C with 5% CO2 and 95% humidity. Dulbecco's modified Eagle's medium (DMEM), Gibco, containing 10% fetal calf serum and 1% penicillin-streptomycin, is used as the complete culture medium, which is changed every 2 to 3 days. Petition 870260030969, dated 02 / 04 / 2026, page 37 / 57 34 / 42

[0086] One day before the test, 20,000 cells / well are seeded in a 96-well plate and incubated at 37 °C with 5% CO2 and 95% humidity for 24 h. (2) Toothpaste preparation:

[0087] 6 + / -0.001 g of toothpaste is added to 18 mL of DMEM in a sterilized 100 mL beaker. The sample is stirred at 500 rpm for 20 min using a magnetic stir bar. The paste is then transferred to a sterilized 50 mL tube and centrifuged at 15000 rpm for 15 min. The supernatant is diluted with DMEM to provide a 25 mg / mL core stock solution. The core stock solution is further diluted with DMEM to the assay solutions according to Table 1 below. Table (1) ID Final Concentration (mg / mL) Stock (mg / mL) Stock Volume (μL) Average Volume (pL) Final Volume (pL) 1 14.063 25 450 350 800 2 12.500 25 400 400 800 3 10.938 25 350 450 800 4 9.375 25 300 500 800 5 7.813 25 250 550 800 6 6.250 25 200 600 800 7 4.688 25 150 650 800 8 3.125 25 100 700 800 9 1.563 25 50 750 800 10 0.781 25 25 775 800 Petition 870260030969, dated 02 / 04 / 2026, page 38 / 57 35 / 42 (3) Dosage of plaque solutions:

[0088] The medium is removed from the 96-well plate. 150 μL of selected dosing solutions are added to the 96-well plate. There is a duplicate for each dosing solution concentration. The cell is incubated with serial concentrations of toothpaste dosing solutions for 30 min at 37 °C with 5% CO2 and 95% humidity. (4) CCK8 test for evaluating HGE cell viability:

[0089] The working solution of the cell counting kit 8 (CCK8, from DOJINDO) is prepared by diluting the CCK8 reagent with DMEM (CCK8: DMEM=1:10). The toothpaste dosage solution is then carefully removed from the 96-well plate. 100 μL of CCK8 working solution is added to each well and the cell is continuously incubated for 1.5 ha at 37 °C, 5% CO2, 95% humidity. Then, the 96-well plate is read by SpectraMax i3 (Molecular Devices) for absorbance at 450 nm at room temperature. (5) Data processing:

[0090] The initial OD value is deducted from the blank control OD (the wells without cells), which is then followed by normalization with the average positive control OD (the wells with cells only). The data are then processed by GraphPad to generate a 30-minute EC50 for each toothpaste. EXAMPLES

[0091] The following examples and descriptions clarify in more detail the embodiments within the scope of the present invention. These examples are provided for illustrative purposes only and should not be considered a limitation of the present invention, since many Petition 870260030969, dated 02 / 04 / 2026, p. 39 / 57 36 / 42 variations of the same are possible, without deviating from its character and scope. Example A: Preparing examples 1 to 4

[0092] Formulation examples 1 to 4 are toothpaste compositions shown below with component quantities in weight percent. Examples 1 and 3 are comparative formulations, while example 4 is an inventive formulation according to the present invention. Example 4 is made with a stannous ion source, a soluble zinc ion source, and a taurate-based surfactant (SMCT). In parallel, comparative formulation examples 1 & 2 are made without a stannous ion source and use SLS and SMCT surfactants, respectively. Example 3 is a formulation containing a stannous ion source and sodium lauryl sulfate (SLS) surfactant, but without a taurate-based surfactant. All examples 1 to 4 are zinc-free formulations. All compositions are prepared by mixing the components described in Table 2, in the indicated proportions.A commercial comparative formulation containing a source of zinc ions and stannous ions is prepared, namely, comparative example 5. Table 2: Examples 1 to 4 Name Ex. Comparative 1 Ex. Comparative 2 Ex. Comparative 3 Ex. 4 of the present invention Water qsp qsp qsp qsp Glycerin 27,000 27,000 Sorbitol (70%) 65,200 65,200 35,000 35,000 Petition 870260030969, dated 02 / 04 / 2026, pp. 40 / 57 37 / 42 Stannous fluoride 0.454 0.454 Stannous chloride (in 10% silica) 0.562 0.562 Sodium fluoride 0.321 0.321 Sodium gluconate 1.150 1.150 Sodium hydroxide (50%) 0.740 0.740 Monosodium phosphate 0.400 0.400 Trisodium phosphate 0.930 0.930 Sodium saccharin 0.300 0.300 0.500 0.500 Xanthan gum 0.613 0.613 Carrageenan 1.050 1.050 Carbomer 0.220 0.220 Sodium carboxymethyl cellulose CMC 0.700 0.700 Sodium citrate 1,550 1,550 Zinc citrate Titanium dioxide Hydrated silica 16,000 16,000 15,000 15,000 Sodium lauryl sulfate (29%) 5,000 5,000 Petition 870260030969, dated 02 / 04 / 2026, page 41 / 57 38 / 42 Methyl cocoyl taurate sodium (29%) 5.000 5.000 Flavor 1.000 1.000 1.000 1.000 Total 100.000 100.000 100.00 100.00 Example B: Improving endotoxin neutralization and stannous (Sn) penetration in biofilm

[0093] Test method 2 is conducted to measure bacterial endotoxin neutralization in biofilm from examples of the present invention and comparators, as well as to measure the rate of penetration of active Sn into biofilm that neutralizes endotoxin. The results are provided in Table 3 and Table 4. Table 3 - Neutralization of bacterial endotoxins in biofilm Treatment Fluorescence intensity ratio (FIR) LPS bound / bacterial cell Cluster* Negative control (phosphate buffer solution) 0.1033 D Comparative example 1 0.1267 D Comparative example 2 0.1300 D Comparative example 3 1.0600 B Example of the invention 4 1.3767 A Petition 870260030969, dated 02 / 04 / 2026, pp. 42 / 57 39 / 42 Comparative example 5 0.8500 C * Means for groups in homogeneous subsets, those that do not share a letter are significantly different (alpha = 0.05) and average sample size = 6. Student-Newman-Keuls Method1Comparative example 5 is a commercially available toothpaste from Colgate® Total™SF (LOT 1249US56C1) which has the following ingredients: water, sorbitol, hydrated silica, glycerin, PEG-12, tetrasodium pyrophosphate, flavor, sodium lauryl sulfate, zinc phosphate, cellulose gum, sodium citrate, stannous fluoride; microcrystalline cellulose, sodium saccharin, cocamidopropyl betaine, xanthan gum, citric acid, sucralose and titanium dioxide. Table 4 - Rate of penetration of active Sn into biofilm Treatment % of Sn penetration Grouping* Negative control (phosphate buffer solution) 0.1067 D Comparative example 1 1.5333 D Comparative example 2 1.6667 D Comparative example 3 75.907 B Example of the invention 4 90.913 A Comparative example 5 64.0010 C Same as above.

[0094] The results in Table 3 demonstrate the significantly higher fluorescence intensity ratio (FIR) of bound LPS / bacterial cell with the biofilms treated with Petition 870260030969, dated 02 / 04 / 2026, pp. 43 / 57 40 / 42 examples 4 (i.e., compositions containing Sn + taurate), both in relation to comparative example 3 (i.e., Sn + SLS compositions) and in relation to example 5 (which contains Sn, SLS and cocamidopropyl betaine cosurfactant). Furthermore, comparative examples 1 and 2 (i.e., which do not contain a source of Sn) have no effect on endotoxin neutralization, regardless of the type of surfactant taurate or SLS.

[0095] The results in Table 4 demonstrate a significantly greater penetration of Sn ion into the biofilm for invention examples 4 containing stannous element and taurate vs. comparative examples 3 and 5 containing stannous element and SLS.

[0096] The use of taurate without a source of stannous ions, comparative example 2, has a very low FIR of bound LPS / bacterial cell, indicating that the taurate-based surfactant does not neutralize bacterial endotoxins (LPS).

[0097] The surprising combination of stannous element and taurate has a significant improvement in the neutralization of bacterial endotoxin due to the increased penetration of stannous ions into the biofilm. Example 3: EC50 irritation test

[0098] Test method 3 is conducted to measure half the maximum effective concentration (EC50) of the invention's examples and comparators. EC50 measures the concentration of a formula or toxicant that induces a midpoint response between baseline and maximum after a specified exposure time. The higher the numerical score, the better, showing that the cells are more tolerant / less irritated and not harmed. Petition 870260030969, dated 02 / 04 / 2026, pp. 44 / 57 41 / 42 Table 5 - EC50 irritation test Treatment EC50 (mg / mL) Grouping* Comparative example 1 5.807 B Comparative example 2 8.002 A Comparative example 3 5.240 B Example of the invention 4 8.335 A Comparative example 5 5.683 B Same as above.

[0099] The results in Table 5 demonstrate the significantly greater tolerance to irritation of human gingival epithelial cells for invention examples 4 and for comparative example 2 (compositions containing taurate-based surfactant).

[0100] The surprising combination of stannous element and taurate has a significant improvement in the neutralization of bacterial endotoxin from the penetration of stannous ions into the biofilm and reduces irritation of the gingival epithelium that can be compromised to allow bacterial toxins to infiltrate and cause gingival inflammation.

[0101] The dimensions and values ​​disclosed herein should not be understood as strictly limited to the exact numerical values ​​mentioned. Instead, except where otherwise specified, each of these dimensions is intended to mean both the value mentioned and a range of functionally equivalent values ​​around that value. For example, a dimension disclosed as 40 mm is intended to mean approximately 40 mm.

[0102] Each document cited in the present invention, including any patent or patent application referenced herein. Petition 870260030969, dated 02 / 04 / 2026, pp. 45 / 57 42 / 42 reference or related, and any patent application or patent in which the present application claims priority or benefit thereof, is hereby incorporated in its entirety into the present invention by reference, except where expressly excluded or otherwise limited. Mention of any document is not an admission that it constitutes prior art in relation to any invention disclosed or claimed herein, nor that it, by itself or in any combination with any other reference or references, teaches, suggests or discloses such invention. Furthermore, if there is a conflict between any meaning or definition of a term in this document and any meaning or definition of the same term in a document incorporated by reference, the meaning or definition ascribed to that term in this document shall prevail.

[0103] Although specific embodiments of the present invention have been illustrated and described, it will be evident to those skilled in the art that various other alterations and modifications can be made without departing from the spirit and scope of the invention. Therefore, it is intended to cover in the appended claims all such alterations and modifications that are within the scope of the present invention. Petition 870260030969, dated 02 / 04 / 2026, pp. 46 / 57

Claims

1 / 4 CLAIMS 1. Oral hygiene composition characterized by comprising: (a) from 0.01% to 5%, by weight of the composition, of a source of stannous ions; (b) from 0.1% to 5%, by weight of the composition, of a taurate-based surfactant represented by the formula r2 II I Rj--C—N—CH2—CH2—SO3'M+, where Ri is a saturated or unsaturated alkyl chain, linear or branched, with 6 to 18 C atoms; R2 is H or methyl, and M is H, sodium or potassium; and wherein the oral hygiene composition is substantially free of a source of zinc ions.

2. Oral hygiene composition, according to claim 1, characterized in that Ri is a saturated or unsaturated alkyl chain, linear or branched, with 8 to 18 C atoms, wherein, optionally, the taurate-based surfactant comprises one or more of the following: potassium cocoyl taurate, potassium methyl cocoyl taurate, sodium caproyl methyl taurate, sodium cocoyl taurate, sodium lauroyl taurate, sodium methyl cocoyl taurate, sodium methyl lauroyl taurate, sodium methyl myristoyl taurate, sodium methyl oleoyl taurate.

3. Oral hygiene composition, according to any of the preceding claims, characterized in that the source of stannous ions is selected from soluble stannous salts and, preferably, is selected from the group consisting of stannous chloride, stannous fluoride, stannous acetate, stannous gluconate, stannous oxalate, stannous sulfate, stannous lactate, stannous tartrate, stannous iodide, stannous chlorofluoride, stannous hexafluorozirconate, stannous citrate, stannous malate, stannous glycinate, stannous carbonate, stannous phosphate, stannous pyrophosphate, stannous metaphosphate and combinations thereof; Preferably, the source of stannous ions is selected from stannous chloride, stannous fluoride, or a combination thereof.

4. Oral hygiene composition, according to any of the preceding claims, characterized by additionally comprising from 0.01% to 10% by weight of a secondary surfactant, wherein the secondary surfactant is an amphoteric surfactant selected from the group consisting of cocamidopropyl betaine, lauramidopropyl betaine, oleamidopropyl betaine, seboamidopropyl betaine, cocamidopropyl hydroxysultaine and combinations thereof; and, more preferably, selected from cocamidopropyl betaine, lauramidopropyl betaine or a combination thereof.

5. Oral hygiene composition, according to any of the preceding claims, characterized by being substantially free of sodium lauryl sulfate (SLS).

6. Oral hygiene composition, according to any of the preceding claims, characterized by additionally comprising 0.5% to 5%, preferably 0.5% to 1.5%, by weight of the composition, of a source of fluoride ions; preferably, the source of fluoride ions is selected from the group consisting of stannous fluoride, Petition 870260030969, dated 02 / 04 / 2026, page 48 / 57 3 / 4, sodium fluoride, potassium fluoride, sodium monofluorophosphate or mixtures thereof.

7. Oral hygiene composition, according to any of the preceding claims, characterized by comprising from 10% to 60%, preferably from 10% to 40%, by weight of the composition, of total water content.

8. Oral hygiene composition, according to any of the preceding claims, characterized by additionally comprising from 0.01% to 5%, by weight of the composition, of a thickening system, wherein the thickening system is selected from a thickening polymer, a thickening silica or a combination thereof.

9. Oral hygiene composition, according to any of the preceding claims, characterized by further comprising from 1% to 35%, more preferably from 5% to 25%, by weight of the composition, of an abrasive, wherein the abrasive is selected from an abrasive containing calcium, a silica-based abrasive or a combination thereof; and wherein, more preferably, the abrasive is a silica-based abrasive.

10. Oral hygiene composition, according to any of the preceding claims, characterized by being free of glycyrrhetinic acid and its salt.

11. Oral hygiene composition, according to any of the preceding claims, characterized by having a pH in the range of 4.0 to 9.0, preferably 4.3 to 8.0, and more preferably 4.6 to 7.

5.

12. Oral hygiene composition, according to any of the preceding claims, characterized by being a monophasic toothpaste. Petition 870260030969, dated 02 / 04 / 2026, pp. 49 / 57 4 / 4 13. Use of a composition for oral hygiene, as defined in any one of claims 1 to 12, characterized in that in the manufacture of a composition for treating dental biofilm, the step of brushing the teeth is included.

14. Use of a composition for oral hygiene, as defined in any of claims 1 to 12, characterized by being in the manufacture of a composition to prevent or mitigate plaque formation on dental enamel. Petition 870260030969, dated 02 / 04 / 2026, pp. 50 / 57