Non-aqueous non-oily tooth powder containing bioactive glass and preparation method therefor

Abstract

A non-aqueous non-oily tooth powder containing bioactive glass, comprising, in weight percentage, the following raw materials: abrasive agent: 40%-95%; bioactive glass: 0.3%-50%; foaming agent: 1%-10%; fragrance: 0%-10%; and pigment: 0%-5%. The tooth powder contains neither water nor an oily carrier, and thus not only maintains a high concentration of the abrasive agent to provide strong cleaning and decontamination capabilities, but also does not affect the performance of the bioactive glass, enabling the tooth powder to have good efficacy in occluding dentinal tubules and repairing tooth enamel. The method for preparing the tooth powder is simple and convenient, requiring only the mixing of the various raw materials in dry powder form.

Description

A non-aqueous, non-oil-based tooth powder containing bioactive glass and its preparation method Technical Field

[0001] This invention belongs to the field of oral care technology, and particularly relates to tooth powder containing bioactive glass, which is a water-free and oil-free tooth powder, specifically relating to a non-aqueous and non-oil-free tooth powder containing bioactive glass and its preparation method. Background Technology

[0002] Tooth powder, as a traditional teeth cleaning agent, has evolved from its main ingredient, salt, to various modern formulas. However, most commercially available tooth powders only provide basic cleaning and have limited effectiveness in treating dental diseases. Bioactive glass, as a novel material, shows great potential in oral care. Initially developed by the University of Florida in 1969, it can integrate with surrounding bone tissue, demonstrating good clinical results in bone defect repair. In dentistry, the application of bioactive glass is increasing. Adding it to toothpaste can treat dentin hypersensitivity; after brushing, the bioactive glass in the toothpaste adheres to the dentin surface, forming a hydroxyapatite layer. The addition of bioactive glass allows toothpaste or tooth powder to not only clean but also effectively combat dentin hypersensitivity and promote tooth remineralization. Furthermore, the structural and performance characteristics of bioactive glass make it widely used in biomedical fields, especially in oral care products such as toothpaste, mouthwash, and tooth powder.

[0003] Currently, many toothpastes on the market contain bioactive glass, but their effectiveness is limited because the oily wetting agent coats the bioactive glass. Some tooth powders without bioactive glass have also begun to appear on the market. While they offer good cleaning results, there is still significant room for improvement in their ability to seal dentinal tubules and repair enamel. Summary of the Invention

[0004] The technical problem to be solved by this invention is to provide a non-aqueous and non-oil-based tooth powder containing bioactive glass and its preparation method, thereby solving the problem of poor efficacy in sealing dentinal tubules and repairing tooth enamel.

[0005] To solve the above-mentioned technical problems, the specific technical solution adopted by the present invention is as follows:

[0006] In a first aspect of the present invention, a non-aqueous, non-oil-based dental powder containing bioactive glass is provided, comprising, by weight percentage, the following raw materials:

[0007] Friction agent: 40%–95%;

[0008] Bioactive glass: 0.3%–50%;

[0009] Foaming agent: 1-10%;

[0010] Flavorings: 0-10%;

[0011] Pigment: 0-5%.

[0012] Non-aqueous and non-oily tooth powder refers to tooth powder that contains neither water nor oily components. Non-aqueous and non-oily tooth powder does not suffer from the problem of water weakening the bioactive properties of glass, nor is it inhibited from acting on teeth by oily carriers such as glycerin.

[0013] Bioactive glass refers to inorganic glass materials with silicon oxide as their main component that can bond with growing tissues when reacting with physiological solutions.

[0014] Furthermore, the bioactive glass may be, but is not limited to, 45S5, 45S5.4F, S63.5P6, S53P4, S45P7, 52S4.6, 55S4.3, 60S3.8, 42SF, 46SF, 49SF, 52SF, 55SF, 60SF, 58S, 68S, 77S, 86S, or bioacceptable (or biologically active) glass. Bioactive glass refers to inorganic glass materials having silicon oxide as their main component and capable of bonding with growing tissues when reacting with physiological solutions, such as glass compositions forming a hydroxyapatite layer.

[0015] Preferably, the bioactive glass 45S5 has the following mass fractions (wt%): SiO2: 45%; CaO: 24.5%; NaO: 24.5%; P2O5: 6%.

[0016] In some specific implementations, the bioactive glass is obtained in-house.

[0017] In some specific embodiments, the abrasive is selected from one or more of hydrated silica, dicalcium phosphate, calcium pyrophosphate, aluminum hydroxide, montmorillonite, natural walnut shell powder, and silica sand.

[0018] Abrasives in tooth powder help remove dirt and plaque from teeth and keep the mouth clean.

[0019] Preferably, the friction agent is selected from one or more of dicalcium phosphate and hydrated silica.

[0020] In some specific embodiments, the foaming agent is selected from one or more of sodium lauryl sulfate, sodium lauroyl sarcosinate, polysorbate derivatives, cocamidopropyl betaine, and sodium laureth sulfate.

[0021] Anionic foaming agents commonly used in the oral care industry can slow down the healing of oral ulcers due to their high irritation. However, anionic surface foaming agents used in some specific implementation schemes do not have the above-mentioned disadvantages.

[0022] The main function of foaming agents in tooth powder is to emulsify and break down oily residues in the mouth, helping to clean teeth and the oral cavity, while providing a visible brushing effect.

[0023] Preferably, the foaming agent is sodium lauryl sulfate.

[0024] In some specific embodiments, the fragrance is selected from one or more of menthol, citral, fennel oil, wintergreen oil, borneol, and herbal fragrance.

[0025] The role of flavoring in tooth powder is to enhance the user experience and increase freshness and fragrance.

[0026] Preferably, the flavoring is menthol.

[0027] In some specific embodiments, the pigment is selected from one or more of natural antibacterial polyphenols, chlorophyll, pearl powder, white tea extract, and CI42090.

[0028] In some specific implementations, tooth powder also includes sweeteners and preservatives.

[0029] In some specific embodiments, the content of bioactive glass is 3% to 50% by weight, preferably 8% to 15%.

[0030] In some specific implementation schemes, the following raw materials are included: dicalcium phosphate, bioactive glass, hydrated silica, sodium lauryl sulfate, sodium monofluorophosphate, flavoring, menthol, sodium bicarbonate, sodium benzoate, sodium saccharin, dipotassium glycyrrhizate, and CI42090.

[0031] In some specific embodiments, by weight percentage, the content of dicalcium phosphate is 40%–66%, the content of bioactive glass is 3%–30%, the content of hydrated silica is 7%–12%, the content of sodium lauryl sulfate is 2.5%–3%, the content of sodium monofluorophosphate is 1%, the content of fragrance is 0.999%–1%, the content of menthol is 2%, the content of sodium bicarbonate is 15%, the content of sodium benzoate is 0.2%, the content of sodium saccharin is 0.1%, the content of dipotassium glycyrrhizate is 0.2%, and the content of CI42090 is 0.001%.

[0032] When using tooth powder to brush your teeth, dip your toothbrush in a small amount of water, then dip it in the tooth powder and brush for 30 seconds to 5 minutes. After spitting out the foam, holding the toothbrush in your mouth for a few more minutes (e.g., 0 to 30 minutes) will allow the bioactive glass to perform better and play a better role in repairing tooth enamel and sealing dentinal tubules.

[0033] In a second aspect of the present invention, a method for preparing a non-aqueous, non-oil-based dental powder containing bioactive glass is provided: the raw materials are put into a mixer and mixed evenly.

[0034] In some specific implementations, the raw materials include abrasives, bioactive glass, foaming agents, fragrances, and pigments.

[0035] The raw materials are all in dry powder form and can be directly mixed to make tooth powder.

[0036] CI42090 in this invention refers to a specific synthetic organic colorant, commonly known as Acid Blue 9, and its sodium salt form is Brilliant Blue FCF. This colorant is widely used in food, pharmaceuticals, and daily chemical products (including tooth powder) to provide stable blue to blue-green hues.

[0037] Compared with the prior art, the present invention has the following beneficial effects:

[0038] The tooth powder of this invention contains no water or oily carrier, maintaining a high concentration of abrasives for strong cleaning and stain removal capabilities without affecting the performance of bioactive glass, thus providing excellent sealing of dentinal tubules and enamel repair. The enamel repair composition of this invention is a dry powder texture, which, compared to paste or gel-based oral care compositions, has extremely low water content. Based on this characteristic, the composition can maintain stable physicochemical properties and microbiological stability over a long period without relying on conventional or high-dose chemical preservatives during storage. Therefore, the formulation of this invention can significantly reduce or eliminate the need for preservatives, thereby reducing the potential irritation risk introduced by preservatives and improving product safety. The method for preparing the tooth powder of this invention is simple, requiring only the mixing of various dry powder raw materials.

[0039] The following will further explain the concept and technical effects of the present invention in conjunction with the accompanying drawings, so as to fully understand the purpose, features and effects of the present invention. Attached Figure Description

[0040] Figure 1 shows a scanning electron microscope (SEM) image of the negative control group in Example 3. Figure 1(a) is an SEM image of the untreated area; Figure 1(b) is an SEM image of the treated area.

[0041] Figure 2 shows scanning electron microscope (SEM) images of the sample group in Example 3. Figure 2(a) is an SEM image of the untreated area; Figure 2(b) is an SEM image of the treated area of ​​the sample group. Detailed Implementation

[0042] To make the technical means, inventive features, objectives, and effects of the invention readily understandable, the invention is further illustrated below with reference to specific figures. However, the invention is not limited to the embodiments described below.

[0043] It should be noted that the accompanying drawings are only used to complement the content disclosed in this specification, so as to enable those skilled in the art to understand and read them, and are not intended to limit the conditions under which the present invention can be implemented. Therefore, they have no substantial technical significance. Any non-creative adjustments, without affecting the effects and objectives that the present invention can produce, should still fall within the scope of the technical content disclosed in the present invention.

[0044] All raw materials involved in the examples are commercially available products and can be commercially produced.

[0045] A method for preparing bioactive glass: using SiO2, CaO, Na2O, and P2O5 as raw materials, and proportioning them by weight according to the principle of SiO2: 45%, P2O5: 6%, CaO: 24.5%, and Na2O: 24.5%; grinding the raw materials into micron-sized particles using a ball mill, pressing and calcining them at 900℃~1100℃ for 1~3h, pulverizing them into micron-sized particles, and then sintering them at 1150℃~1350℃ for 1~3h, controlling the furnace cooling process at 10℃~15℃ / min, and then pulverizing them into micron and submicron-sized particles to obtain bioactive glass.

[0046] Example 1

[0047] The raw material composition table of the tooth powder in this embodiment is shown in Table 1:

[0048] Table 1. Tooth powder raw material composition table for Example 1

[0049] The method for preparing tooth powder is as follows:

[0050] 1. First, mix sodium hydrogen phosphate, hydrated silica, and sodium bicarbonate.

[0051] 2. Mix the bioactive glass, sodium lauryl sulfate, sodium monofluorophosphate, sodium benzoate, sodium saccharin, dipotassium glycyrrhizate, and CI42090, and then add them to the mixture from step 1 and mix again.

[0052] 3. Dissolve the flavoring and menthol in 75% alcohol, spray it in with a spray bottle while mixing.

[0053] 4. After the mixed materials pass the inspection, they are bottled and sealed on the production line.

[0054] Preparation method of bioactive glass: SiO2, CaO, Na2O and P2O5 are used as raw materials, and the proportions are made according to the principle of SiO2: 45%, P2O5: 6%, CaO: 24.5% and Na2O: 24.5% by weight. The raw materials are ground into micron-sized particles using a ball mill, pressed and calcined at 1000℃ for 2 hours, pulverized into micron-sized particles, sintered at 1200℃ for 2 hours, and the furnace cooling process is controlled at 10℃ / min. The particles are then pulverized into micron and submicron-sized particles to obtain bioactive glass.

[0055] Comparative Example 1

[0056] The tooth powder used in this comparative example is a commercially available tooth powder, and its ingredient list is shown in Table 2:

[0057] Table 2 Comparative Example 1 Tooth Powder Raw Material Composition Table

[0058] For the preparation method of tooth powder, please refer to Example 1.

[0059] Example 3

[0060] The evaluation item in this embodiment is the evaluation of the effect of sealing dentinal tubules, based on GQT / ZY-HJ-A-17 "Detailed Rules for Evaluation of the Effect of Toothpaste on Sealing Dental Tubules".

[0061] 1. Experimental Grouping

[0062] Sample group: Example 1 Tooth powder

[0063] Negative control group: Comparative example 1 tooth powder

[0064] 2. Test Methods

[0065] 1) Preparation of artificial saliva: Dissolve 0.380 g / L sodium chloride, 0.213 g / L calcium chloride dihydrate, 0.738 g / L potassium dihydrogen phosphate, 1.114 g / L potassium chloride, and 2.200 g / L gastric mucoprotein in deionized water. Adjust the pH of the solution to 7.0 with 1 mol / L sodium hydroxide, add water to make up the volume, and store in a refrigerator at 4°C for later use.

[0066] 2) Dentin Sample Preparation: Twelve dentin blocks (5mm × 5mm × 2mm) were cut from the root of a bovine incisor and embedded in resin to prepare dentin samples. The dentin surfaces were then polished using P180 and P600 grinding wheels, followed by polishing with a polishing cloth and 6μm polishing solution. The samples were then soaked in 40% orthophosphoric acid solution and agitated for 20 minutes, rinsed, and then soaked in 5% sodium hypochlorite solution and agitated for 5 minutes. Finally, they were ultrasonically cleaned with deionized water for 20 minutes. Observation was performed under a polarized light microscope to ensure full exposure of the dentinal tubules.

[0067] 3) Zonal treatment: One half of the dentin area (approximately 5mm × 2.5mm) was taped to serve as the untreated area, while the other half (approximately 5mm × 2.5mm) was left uncovered as the experimental treatment area. Dentin samples were randomly divided into a negative control group and a sample group, with 6 samples in each group. The negative control group and the sample group were treated with the corresponding test substance.

[0068] 4) Preparation of test tooth powder: Weigh a certain amount of tooth powder and artificial saliva according to the ratio of 1:1.6 (tooth powder: artificial saliva), stir with a glass rod to disperse the tooth powder, and then stir with an electric stirrer to form a homogenate for later use.

[0069] 5) Dentin cyclic treatment: Brush teeth for 3 minutes, then rinse the surface of the dentin sample with water to remove any remaining sample. Immerse the sample in artificial saliva at 37°C for 55 minutes. Repeat brushing for 3 minutes, rinsing the surface of the dentin sample with water, and immersing in artificial saliva at 37°C overnight. Repeat this step for 2 days. After cyclic treatment, place the dentin sample in a 25°C incubator to dry for 24 hours.

[0070] 6) Scanning electron microscopy observation: The surface of the dried dentin sample was sputtered with gold and then observed under a scanning electron microscope. Three fields of view (2000x magnification) were taken from the treated area and the untreated area respectively. The exposed dentinal tubules were counted and recorded as C.

[0071] 7) Calculate the dentinal tubule occlusion rate R (%) for each group:

[0072] Where Ri(%) is the occlusion rate of each tooth block; Ci is the number of exposed dentinal tubules in each image; R(%) is the average occlusion rate of each group; and n is the sample size.

[0073] 3. Evaluation Methods

[0074] Independent samples t-tests were used to compare the dentinal tubule occlusion rates R (%) between the sample group and the negative control group, with a significance level of α = 0.05. The difference in occlusion rates R (%) between the sample group and the negative control group was statistically significant (P < 0.05), indicating that the sample group was more effective at occluding dentinal tubules than the negative control group and demonstrated the effectiveness of dentinal tubule occlusion.

[0075] 4. Test data and statistical results

[0076] Table 3 Dentin tubule occlusion rate R (%)

[0077] The relevant scanning electron microscope images are shown in Appendix 1.

[0078] 5. Conclusion

[0079] Compared with the control group, the bioactive glass dental cleaning powder had a higher rate of dentinal tubule sealing than the negative control group, and the difference between the groups was statistically significant (P<0.05), indicating that the sample had a significant sealing effect on dentinal tubules.

[0080] Example 4

[0081] The evaluation item in this embodiment is the in vitro evaluation of the effect of enamel repair (remineralization), based on GQT / ZY-HG-41 "In vitro evaluation method for the effect of enamel repair (remineralization)".

[0082] 1. Experimental Grouping

[0083] Sample group: Example 1 Tooth powder

[0084] Control group: Deionized water

[0085] 2. Test Methods

[0086] 1) Preparation of enamel specimens: Select a certain number of bovine teeth, cut them into pieces approximately 5mm × 5mm in size, and embed them in denture resin. Under water cooling conditions, use a P180 grinding wheel on a polishing machine to grind the enamel surface of the tooth block until it is completely exposed and the surface of the tooth block is horizontal. Then, polish it with a P600-6μm-1μm-0.5μm grinding wheel. The prepared tooth blocks are stored in deionized water for later use.

[0087] 2) Preparation of artificial saliva: Weigh 0.246g calcium nitrate, 0.122g potassium dihydrogen phosphate, 8.394g potassium chloride, and 20.920g bis(2-hydroxyethyl)aminotris(hydroxymethyl)methane into a 1L beaker. Add 800mL of deionized water and stir thoroughly to dissolve. Then add 5μL of 1% sodium fluoride solution and adjust the pH to 7.0±0.05 with 1mol / L HCl. Transfer this solution to a 1L volumetric flask and dilute to the mark with deionized water.

[0088] 3) Preparation of demineralization solution: Weigh 5g of citric acid into a 500mL volumetric flask, add deionized water to make up to 500mL, and shake well before use.

[0089] 4) Screening of enamel specimens: The hardness of enamel specimens was measured using a Vickers hardness tester (pressure 300g, loading time 5s). Four points were measured for each specimen and the average value was taken. The hardness value was recorded as H0. Specimens with a hardness of 300-330 were selected and randomly grouped according to their surface hardness values, with 8 specimens in each group.

[0090] 5) Preparation of test sample slurry: Weigh a certain weight of the tooth powder to be tested and deionized water according to a 1:3 ratio (tooth powder: water), stir and mix well, avoiding foaming. Each enamel specimen requires at least 5 mL of sample slurry.

[0091] 6) Demineralization treatment: Immerse the enamel specimen in 1% citric acid for 30 minutes at a temperature of 37℃±2℃, and stir with a propeller at a low speed (60r / min), keeping the propeller 5cm above the enamel specimen. Then rinse the specimen thoroughly with deionized water and dry it.

[0092] 7) Test Cycle: Immerse the tooth block in sample slurry for 3 minutes, then rinse thoroughly with deionized water. Immerse the tooth block in artificial saliva for 3 hours, then immerse it in sample slurry for another 3 minutes, and rinse thoroughly with deionized water. Finally, soak the tooth block in artificial saliva overnight. Repeat the above operation for a total of 8 days. Except for the rinsing step, all immersion treatments were carried out in a water bath at 37℃±2℃.

[0093] 8) Hardness test: The hardness of the treated enamel specimen was measured using a Vickers hardness tester (pressure 300g, loading time 5s), and recorded as H2; the hardness of the acid-treated enamel specimen was recorded as H1.

[0094] 9) Calculate the hardness recovery rate R for each tooth block: R = (H2 - H1) / (H0 - H1) × 100%.

[0095] 3. Evaluation Methods

[0096] SPSS 27.0 statistical software was used, and an independent samples t-test was performed with a significance level of α = 0.05. If the hardness recovery rate R of the tooth blocks in the sample group after cyclic treatment was greater than that in the control group, and the difference between the groups was statistically significant (P < 0.05), the test samples could be considered to have an enamel repair (remineralization) effect.

[0097] 4. Test data and statistical results

[0098] Table 4 Surface Hardness Test Results

[0099] 5. Conclusion

[0100] Compared with the control group, the hardness recovery rate R of the sample group was greater than that of the control group, and the difference in hardness recovery rate between the groups was statistically significant (P<0.05). Bioactive glass dental powder has a good effect on enamel repair (remineralization).

[0101] Example 5

[0102] The raw material composition of the tooth powder in this embodiment is shown in Table 5:

[0103] Table 5. Tooth powder raw material composition table for Example 5

[0104] The tooth powder preparation method is the same as in Example 1.

[0105] Example 6

[0106] The raw material composition of the tooth powder in this embodiment is shown in Table 6:

[0107] Table 6. Tooth powder raw material composition table for Example 6

[0108] The tooth powder preparation method is the same as in Example 1.

[0109] The tooth powders in Examples 5 and 6 showed excellent performance in both in vitro evaluations of their effectiveness in sealing dentinal tubules and in enamel repair (remineralization).

[0110] Example 7

[0111] To further demonstrate the technical effectiveness of this solution, the evaluation item in this embodiment is the in vitro evaluation of the enamel repair (remineralization) effect, based on GQT / ZY-HG-41 "In vitro evaluation method for the effect of enamel repair (remineralization)".

[0112] 1. Experimental Grouping

[0113] The samples were divided into experimental and control groups; experimental group: 1, 2; control group: 1, 2, 3, 4, 5; sample size n = 8 for each group.

[0114] The raw material composition table for experimental group 1 is shown in Table 7:

[0115] Table 7. Composition of Tooth Powder Raw Materials in Experimental Group 1

[0116] The raw material composition of Experimental Group 2 is shown in Table 8:

[0117] Table 8. Composition of Tooth Powder Raw Materials in Experimental Group 2

[0118] The raw material composition of control group 1 is shown in Table 9:

[0119] Table 9. Raw material composition of tooth powder in control group 1

[0120] The raw material composition of control group 2 is shown in Table 10:

[0121] Table 10. Raw material composition of tooth powder in control group 2

[0122] The raw material composition of control group 3 is shown in Table 11:

[0123] Table 11. Raw material composition of tooth powder in control group 3

[0124] Control group 4 was a toothpaste containing bioactive glass, with the following raw materials: glycerin, polyethylene glycol-8, hydrated silica, sodium calcium phosphosilicate, perlite, cocamidopropyl betaine, sodium methyl cocoyl taurate, fragrance, CI77891, carbomer, silica, sodium saccharin, and sodium fluoride.

[0125] Control group 5 consisted of deionized water.

[0126] 2. Test Methods

[0127] 1) Preparation of enamel specimens: Select a certain number of bovine teeth, cut them into pieces approximately 5mm × 5mm in size, embed them in denture resin, and polish them on a grinding and polishing machine under water-cooling conditions.

[0128] The enamel surface of the dental abrasive block was polished until it was fully exposed and level using a P180 grinding wheel, followed by polishing with a P600-6μm-1μm-0.5μm grinding wheel. The prepared dental abrasive block was then stored in deionized water for later use.

[0129] 2) Preparation of artificial saliva: Weigh 0.246g calcium nitrate, 0.122g potassium dihydrogen phosphate, 8.394g potassium chloride, and 20.920g bis(2-hydroxyethyl)aminotris(hydroxymethyl)methane into a 1L beaker. Add 800mL of deionized water and stir thoroughly to dissolve. Then add 5μL of 1% sodium fluoride solution and adjust the pH to 7.0±0.05 with 1mol / L HCl. Transfer this solution to a 1L volumetric flask and dilute to the mark with deionized water.

[0130] 3) Preparation of demineralization solution: Weigh 5g of citric acid into a 500mL volumetric flask, add deionized water to make up to 500mL, and shake well before use.

[0131] 4) Screening of enamel specimens: The hardness of enamel specimens was measured using a Vickers hardness tester (pressure 300g, loading time 5s). Four points were measured for each specimen and the average value was taken. The hardness value was recorded as H0. Specimens with a hardness of 300-330 were selected and randomly grouped according to their surface hardness values, with 8 specimens in each group.

[0132] 5) Preparation of test sample slurry: Weigh a certain weight of the tooth powder / toothpaste to be tested and deionized water according to a 1:3 ratio (tooth powder:water / toothpaste:water), stir well and avoid foaming. Each enamel specimen requires at least 5 mL of sample slurry.

[0133] 6) Demineralization treatment: Immerse the enamel specimen in 1% citric acid for 30 minutes at a temperature of 37℃±2℃, and stir with a propeller at a low speed (60 r / min), keeping the propeller 5 cm above the enamel specimen. Then rinse the specimen thoroughly with deionized water and dry it.

[0134] 7) Test Cycle: Immerse the tooth block in sample slurry for 3 minutes, then rinse thoroughly with deionized water. Immerse the tooth block in artificial saliva for 3 hours, then immerse it in sample slurry for another 3 minutes, and rinse thoroughly with deionized water. Finally, soak the tooth block in artificial saliva overnight. Repeat the above operation for a total of 8 days. Except for the rinsing step, all immersion treatments were carried out in a water bath at 37℃±2℃.

[0135] 8) Hardness test: The hardness of the treated tooth enamel specimen was measured using a Vickers hardness tester (pressure 300g, loading time 5s), and recorded as H2.

[0136] 9) Calculate the hardness recovery rate R for each tooth block: R = (H2 - H1) / (H0 - H1) × 100%.

[0137] 3. Evaluation Methods

[0138] SPSS 27.0 statistical software was used, and an independent samples t-test was performed with a significance level of α = 0.05. If the hardness recovery rate R of the tooth blocks in the experimental group was greater than that in the control group after cyclic treatment, and the difference between the groups was statistically significant (P < 0.05), the test samples could be considered to have excellent enamel repair (remineralization) effects.

[0139] 4. The test data and statistical results are shown in Table 12.

[0140] Table 12 Surface hardness test results (p=0.05)

[0141] 5. Conclusion

[0142] The difference in hardness recovery rate between groups was statistically significant (P≤0.05), and this invention has excellent enamel repair (remineralization) effects, as detailed below:

[0143] (1) Overall effect analysis: The tooth powder of this invention exhibits the best enamel repair efficacy.

[0144] The average R values ​​of the two embodiments of the present invention (experimental groups 1 and 2) ranked among the top two in all tested samples, with experimental group 2 (15% content) showing the most outstanding effect (39.18%).

[0145] The effect of experimental group 1 (8% content) (30.73%) was also significantly better than all control groups except experimental group 2.

[0146] Therefore, the bioactive glass tooth powder formulation provided by this invention exhibits excellent enamel hardness recovery ability at two representative contents of 8% and 15%.

[0147] (2) Specificity analysis: Verification of the key role of bioactive glass in the formulation of this invention

[0148] By comparing groups with the same matrix formulation but different bioactive glass content, the dose-dependent effect can be clearly observed:

[0149] Experimental group 1 (8%) > Control group 2 (0.2%) > Control group 3 (0%): recovery rates were 30.73%, 21.54%, and 12.50%, respectively. This indicates that in the specific formulation system of this invention, the addition of bioactive glass significantly improves the repair effect, and the effect increases with increasing content.

[0150] Although control group 2 (0.2%) was effective, it was significantly weaker than experimental group 1 (8%). This directly supports the necessity and rationality of setting the lower limit of bioactive glass content to 0.3% in this invention. While a content of 0.2% provides some basic effect, it does not reach the optimal synergistic repair level that this invention can achieve through optimized formulation.

[0151] Therefore, bioactive glass is the core functional component that produces excellent repair effects in this invention. When its content is within the scope of the claims of this invention, it has a synergistic effect with the specific matrix formula, achieving a leap in technical effect.

[0152] (3) Formula Advantage Analysis: The specific formula combination of this invention has significant inventiveness.

[0153] 1) Experimental Group 1 (8%) vs. Control Group 1 (8%): ​​Both groups had the same bioactive glass content, but completely different formulations. The average R value of Experimental Group 1 (30.73%) was significantly higher than that of Control Group 1 (24.86%). This strongly demonstrates that simply adding 8% bioactive glass is not sufficient to achieve the effects of this invention; rather, the specific combination of components in this invention produces a unique synergistic effect with the bioactive glass.

[0154] 2) Experimental group 1 (8%) vs. control group 4 (commercially available toothpaste): The effect of experimental group 1 was also better than that of commercially available toothpaste (30.73% vs. 27.61%), indicating that the formula of this invention is superior to existing market products in achieving efficient repair.

[0155] Therefore, the beneficial effects of the present invention come from the organic combination of "bioactive glass with a specific content range" and "tooth powder matrix with a specific composition". This combination is not a simple superposition of technologies in the field, and the resulting technical effects are unexpected, demonstrating the inventiveness of the invention.

[0156] (4) Scope of protection verification: Supporting the reasonableness of the claims

[0157] Control group 2 (0.2%), serving as a comparative sample adjacent to the lower limit of the protection scope of this invention (0.3%), showed a significantly lower effect (21.54%) than Example 1 of this invention (8%, 30.73%). This data provides sufficient experimental evidence and data support for setting the lower limit of the protection scope at 0.3% rather than lower (such as covering 0.2%), demonstrating the technical rationality of this threshold division.

[0158] In summary, the specific tooth powder formulation containing 0.3%-50% bioactive glass provided by this invention exhibits significantly superior hardness recovery compared to the control group in an in vitro enamel repair model. The effect is better than products using the same amount of bioactive glass but with different formulations (control group 1), demonstrating the irreplaceable synergistic effect of the overall formulation design of this invention. The effect is significantly better than formulations using only 0.2% bioactive glass with the same matrix (control group 2), and better than existing commercially available toothpaste products of the same type (control group 4).

[0159] This invention provides an oral care composition with superior enamel repair (remineralization) effect by optimizing the ratio of bioactive glass content to a specific matrix. The effectiveness of this technology has been confirmed through standardized in vitro experiments and statistical analysis.

[0160] Example 8

[0161] To further demonstrate the technical effectiveness of this solution, the evaluation item in this embodiment is the evaluation of the sealing effect on dentinal tubules, based on GQT / ZY-HJ-A-17 "Detailed Rules for Evaluation of the Sealing Effect of Toothpaste on Dental Tubules".

[0162] 1. Experimental Grouping

[0163] The samples were divided into experimental groups and control groups; experimental groups: 1, 2; control groups: 1, 2, 3, 4; the sample size of each group was n = 6. The specific components of experimental groups 1 and 2 and control groups 1, 2, 3, 4 in this embodiment are the same as the specific components of the corresponding groups in Example 7, and will not be repeated here.

[0164] 2. Test Methods

[0165] 1) Preparation of artificial saliva: Dissolve 0.380 g / L sodium chloride, 0.213 g / L calcium chloride dihydrate, 0.738 g / L potassium dihydrogen phosphate, 1.114 g / L potassium chloride, and 2.200 g / L gastric mucoprotein in deionized water. Adjust the pH of the solution to 7.0 with 1 mol / L sodium hydroxide, add water to make up the volume, and store in a refrigerator at 4°C for later use.

[0166] 2) Dentin Sample Preparation: Twelve dentin blocks (5mm × 5mm × 2mm) were cut from the root of a bovine incisor and embedded in resin to prepare dentin samples. The dentin surfaces were then polished using P180 and P600 grinding wheels, followed by polishing with a polishing cloth and 6μm polishing solution. The samples were then soaked in 40% orthophosphoric acid solution and agitated for 20 minutes, rinsed, and then soaked in 5% sodium hypochlorite solution and agitated for 5 minutes. Finally, they were ultrasonically cleaned with deionized water for 20 minutes. Observation was performed under a polarized light microscope to ensure full exposure of the dentinal tubules.

[0167] 3) Zonal treatment: One half of the dentin area (approximately 5mm × 2.5mm) was taped to serve as the untreated area, while the other half (approximately 5mm × 2.5mm) was left uncovered as the experimental treatment area. Dentin samples were randomly divided into a negative control group and a sample group, with 6 samples in each group. The negative control group and the sample group were treated with the corresponding test substance.

[0168] 4) Preparation of tooth powder / toothpaste: Weigh a certain amount of tooth powder / toothpaste and artificial saliva according to the ratio of 1:1.6 (tooth powder: artificial saliva / toothpaste: artificial saliva). After dispersing the tooth powder / toothpaste with a glass rod, stir it into a homogenate with an electric mixer for later use.

[0169] 5) Dentin cyclic treatment: Brush teeth for 3 minutes, then rinse the surface of the dentin sample with water to remove any remaining sample. Immerse the sample in artificial saliva at 37°C for 55 minutes. Repeat brushing for 3 minutes, rinsing the surface of the dentin sample with water, and immersing in artificial saliva at 37°C overnight. Repeat this step for 2 days. After cyclic treatment, place the dentin sample in a 25°C incubator to dry for 24 hours.

[0170] 6) Scanning electron microscopy observation: The surface of the dried dentin sample was sputtered with gold and then observed under a scanning electron microscope. Three fields of view (2000x magnification) were taken from the treated area and the untreated area respectively. The exposed dentinal tubules were counted and recorded as C.

[0171] 7) Calculate the dentinal tubule occlusion rate R (%) for each group:

[0172] Where Ri(%) is the occlusion rate of each tooth block; Ci is the number of exposed dentinal tubules in each image; R(%) is the average occlusion rate of each group; and n is the sample size.

[0173] 3. Evaluation Methods

[0174] Independent samples t-test was used to compare the dentinal tubule occlusion rate R (%) between the sample group and the negative control group, with a significance level of α = 0.05. The difference in occlusion rate R (%) between the sample group and the negative control group was statistically significant (P ≤ 0.05), indicating that the experimental group had a better effect on dentinal tubule occlusion than the control group and had the effect of occluding dentinal tubules.

[0175] 4. The test data and statistical results are shown in Table 13.

[0176] Table 13 Dentin tubule occlusion rate R (%) (p = 0.05)

[0177] 5. Conclusion

[0178] The difference in dentinal tubule occlusion rate R (%) was statistically significant (P≤0.05), and this invention has the effect of occluding dentinal tubules. Specific analysis is as follows:

[0179] (1) Comparison of formulation advantages: Demonstrating the synergistic effect of the specific formulation of this invention.

[0180] Comparison: Experimental group 1 (8%) vs. Control group 1 (8%)

[0181] Data Comparison: Blocking Rate 77.31% vs 65.08%

[0182] Therefore, although both contain the same amount of bioactive glass, the blocking effect of experimental group 1 is significantly better (approximately 12 percentage points higher) due to the difference in the overall formulation system. This strongly demonstrates that the superior effect of this invention does not stem solely from the conventional operation of "adding 8% bioactive glass," but rather from the unexpected synergistic blocking effect produced between the specific component combination protected by the claims and the bioactive glass. This comparison is the most direct evidence proving the non-obviousness and inventiveness of the technical solution of this invention.

[0183] (2) Content gradient comparison

[0184] Comparison items: Experimental group 1 (8%) vs. Control group 2 (0.2%) vs. Control group 3 (0%)

[0185] Data comparison: Blocking rate 77.31% > 62.92% > 25.49%

[0186] Therefore, under the same matrix, the sealing effect increases significantly with the increase of bioactive glass content, proving that this component is the key functional component for effective sealing of dentinal tubules.

[0187] (3) Market competitiveness comparison: demonstrating the advanced nature of the technical effects of this invention.

[0188] Comparison: Experimental group 1 & 2 vs. control group 4 (commercially available toothpaste)

[0189] Data comparison: The occlusion rates of experimental group 1 (77.31%) and experimental group 2 (84.18%) were both higher than those of similar products on the market (72.73%).

[0190] Therefore, the dentinal tubule sealing effect provided by the formulation of this invention is superior to that of existing commercially available products, demonstrating its advanced technical effect and market application potential.

[0191] In summary, the specific dental powder formulations provided by this invention, containing 0.3%-50% (particularly 8% and 15%) bioactive glass, exhibit exceptionally superior sealing capabilities in in vitro dentinal tubule occlusion models, with an average sealing rate reaching up to 84.18%. At the same bioactive glass content (8%), the sealing effect of this invention is significantly superior to products with different formulations, demonstrating that its technical effect stems from a unique overall formulation design and is non-obvious. The effect shows a clear content-dependent relationship and is significantly better than the low-content (0.2%) control group, supporting the content range specified in the claims.

[0192] This invention successfully combines a specific amount of bioactive glass with an optimized tooth powder matrix, providing not only excellent enamel repair (remineralization) effects (see Example 7) but also effectively sealing dentinal tubules, achieving a dual and synergistic protective effect on the hard tissues of the tooth. The beneficial effects of this combination have been fully verified through standardized in vitro experiments.

[0193] The preferred embodiments of the present invention have been described in detail above. It should be understood that those skilled in the art can make numerous modifications and variations based on the concept of the present invention without creative effort. Therefore, all technical solutions that can be obtained by those skilled in the art based on the concept of the present invention through logical analysis, reasoning, or limited experimentation on the basis of existing technology should be within the scope of protection defined by the claims.

Claims

1. A non-aqueous, non-oil-based tooth powder containing bioactive glass, characterized in that, By weight percentage, it includes the following raw materials: Friction agent: 40%–95%; Bioactive glass: 0.3%–50%; Foaming agent: 1-10%; Flavorings: 0-10%; Pigment: 0-5%.

2. The non-aqueous, non-oil-based tooth powder containing bioactive glass according to claim 1, characterized in that, The abrasive is selected from one or more of the following: hydrated silica, dicalcium phosphate, calcium pyrophosphate, aluminum hydroxide, montmorillonite, natural walnut shell powder, and silica sand.

3. The non-aqueous, non-oil-based tooth powder containing bioactive glass according to claim 2, characterized in that, The friction agent is selected from one or more of dicalcium phosphate and hydrated silica.

4. The non-aqueous, non-oil-based tooth powder containing bioactive glass according to claim 1, characterized in that, The foaming agent is selected from one or more of sodium lauryl sulfate, sodium lauroyl sarcosinate, polysorbate derivatives, cocamidopropyl betaine, and sodium laureth sulfate.

5. The non-aqueous, non-oil-based tooth powder containing bioactive glass according to claim 1, characterized in that, The fragrance is selected from one or more of the following: menthol, citral, fennel oil, wintergreen oil, borneol, and herbal fragrance.

6. The non-aqueous, non-oil-based tooth powder containing bioactive glass according to claim 1, characterized in that, The pigment is selected from one or more of the following: natural antibacterial polyphenols, chlorophyll, pearl powder, white tea extract, and CI42090.

7. The non-aqueous, non-oil-based tooth powder containing bioactive glass according to claim 1, characterized in that, It also includes sweeteners and preservatives.

8. The non-aqueous, non-oil-based tooth powder containing bioactive glass according to claim 1, characterized in that, The bioactive glass content is 3% to 50% by weight, preferably 8% to 15%.

9. The non-aqueous, non-oil-based tooth powder containing bioactive glass according to claim 1, characterized in that, Specifically, it includes the following raw materials: dicalcium phosphate, bioactive glass, hydrated silica, sodium lauryl sulfate, sodium monofluorophosphate, flavoring, menthol, sodium bicarbonate, sodium benzoate, sodium saccharin, dipotassium glycyrrhizate, and CI42090.

10. The non-aqueous, non-oil-based tooth powder containing bioactive glass according to claim 9, characterized in that, By weight percentage, the content of the dicalcium phosphate is 40%–66%, the content of the bioactive glass is 3%–30%, the content of the hydrated silica is 7%–12%, the content of the sodium lauryl sulfate is 2.5%–3%, the content of the sodium monofluorophosphate is 1%, the content of the fragrance is 0.999%–1%, the content of the menthol is 2%, the content of the sodium bicarbonate is 15%, the content of the sodium benzoate is 0.2%, the content of the sodium saccharin is 0.1%, the content of the dipotassium glycyrrhizate is 0.2%, and the content of CI42090 is 0.001%.

11. A method for preparing non-aqueous, non-oil-based tooth powder containing bioactive glass, characterized in that, Add the raw materials into the mixer and mix them evenly.

12. The preparation method according to claim 11, characterized in that, The raw materials include abrasives, bioactive glass, foaming agents, fragrances, and pigments, all in dry powder form.

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