A toothpaste for repairing tooth enamel and its preparation method

Abstract

This invention discloses a toothpaste for repairing tooth enamel and its preparation method. The toothpaste comprises calcium phosphosilicate, sodium calcium phosphosilicate, porous silica, polyethylene glycol, sodium fluoride, olaflumethoxam, hydrated silica, and a toothpaste base component. This invention regulates the release rate of calcium and phosphorus ions by optimizing the ratio between calcium phosphosilicate and sodium calcium phosphosilicate. Simultaneously, fluoride and polyethylene glycol are loaded into porous silica. The hydrogen bonding between fluoride and polyethylene glycol further slows down the release rate of fluoride in the oral cavity. The small amount of fluoride ions released in the early stages of brushing promotes remineralization, while the large amount of fluoride ions released in the later stages of brushing converts newly formed hydroxyapatite into fluorapatite, which has higher hardness.

Description

Technical Field

[0001] This invention relates to the field of oral care product technology, and in particular to a toothpaste for repairing tooth enamel and its preparation method. Background Technology

[0002] Dental caries has a high incidence and wide distribution, making it a major oral disease and one of the most common diseases in humans. The World Health Organization has listed it as one of the three major diseases requiring prevention and control. Tooth decay has five stages. The first stage is demineralization—the initial stage of tooth decay manifests as white or brown spots on the tooth surface. This occurs when the enamel becomes brittle and at risk of peeling off. Using toothpaste containing materials that promote enamel remineralization can reverse this stage of tooth decay. Therefore, a significant amount of research has been devoted to enamel remineralization.

[0003] Remineralization is a natural tooth repair process. Calcium and phosphates in saliva form mineral deposits on the enamel surface. Studies have found that calcium phosphosilicate and bioactive glass (sodium calcium phosphosilicate) can effectively release calcium and phosphate ions, thereby promoting tooth repair. Research indicates that fluoride can promote remineralization and increase the microhardness of teeth while reducing surface roughness. However, calcium fluoride is extremely insoluble, and its rapid formation reduces the concentration of calcium ions in the oral cavity. Therefore, a slow-release strategy is best for fluoride ions to promote remineralization. Currently, commercially available toothpastes do not consider how to control the release of fluoride ions to achieve remineralization while avoiding the impact of rapid formation of insoluble calcium fluoride on calcium ion concentration. Furthermore, commercially available toothpastes do not control the release of fluoride ions to convert the remineralized hydroxyapatite into fluorapatite, which is harder and has better anti-caries properties. Summary of the Invention

[0004] To address the shortcomings of existing technologies, this invention provides a toothpaste for repairing tooth enamel and its preparation method. This invention regulates the release rate of calcium and phosphorus ions by optimizing the ratio between calcium phosphosilicate and sodium calcium phosphosilicate. Simultaneously, fluoride and polyethylene glycol are loaded into porous silica. The hydrogen bonding between fluoride and polyethylene glycol further slows down the release rate of fluoride ions in the oral cavity. The small amount of fluoride released in the early stages of brushing promotes remineralization, while the large amount of fluoride ions released in the later stages of brushing converts newly formed hydroxyapatite into harder fluorapatite.

[0005] The technical solution of the present invention is as follows:

[0006] The first aspect of the present invention provides a toothpaste for repairing tooth enamel, comprising calcium phosphosilicate, sodium calcium phosphosilicate, porous silica, polyethylene glycol, sodium fluoride, orafil, hydrated silica, and toothpaste base components.

[0007] In some embodiments, the toothpaste comprises, by weight percentage, the following raw material components: 0-15% calcium phosphosilicate, 0-10% sodium calcium phosphosilicate, 2-8% porous silica, 2-20% polyethylene glycol, 0.05-0.3% sodium fluoride, 0.05-1.6% olaflumethrin, 20-30% hydrated silica, and 31-50% toothpaste base components; and the total proportion m of calcium phosphosilicate and sodium calcium phosphosilicate in the toothpaste satisfies: 3% ≤ m ≤ 15%; the total fluoride content in the toothpaste is not greater than 0.15%.

[0008] In some embodiments, the toothpaste comprises, by weight percentage, the following raw material components: 0-15% calcium phosphosilicate, 0-10% sodium calcium phosphosilicate, 2-8% porous silica, 2-20% polyethylene glycol, 0.05-0.3% sodium fluoride, 0.05-1.6% olaflumethrin, 20-30% hydrated silica, and 31-43% toothpaste base components; and the total percentage m of calcium phosphosilicate and sodium calcium phosphosilicate in the toothpaste satisfies: 3% ≤ m ≤ 15%; the total fluoride content in the toothpaste is not greater than 0.15%.

[0009] In some embodiments, the calcium phosphosilicate has a particle size of 1-10 μm, preferably 1-5 μm; the sodium calcium phosphosilicate has a particle size of 1-10 μm, preferably 1-5 μm.

[0010] In some embodiments, the specific surface area of ​​the porous silica is 100-400 m². 2 / g, with a particle size of 1-100μm and a pore size of 2-100 nm.

[0011] In some embodiments, the polyethylene glycol has a molecular weight of 282-810 Daltons; and the hydrated silica has a particle size of 1-100 μm.

[0012] In some embodiments, the total mass ratio of the calcium phosphosilicate and sodium calcium phosphosilicate to the mass ratio of olaflu is 1:0.01-1.

[0013] Preferably, the total mass ratio of calcium phosphosilicate and sodium calcium phosphosilicate to olaflu is 1:0.03-0.2.

[0014] In some embodiments, the toothpaste base components include glycerin, sodium lauroyl sarcosinate, and carbomer.

[0015] In some embodiments, the toothpaste, by mass fraction, comprises the following raw material components: 0-15% calcium phosphosilicate, 0-10% sodium calcium phosphosilicate, 2-8% porous silica, 2-20% polyethylene glycol, 0.05-0.3% sodium fluoride, 0.05-1.6% olafur, 20-30% hydrated silica, 30-42% glycerin, 0.5-1.5% sodium lauroyl sarcosinate, and 0.5-1.5% carbomer; and the total proportion m of calcium phosphosilicate and sodium calcium phosphosilicate in the toothpaste satisfies: 3% ≤ m ≤ 15%; the total fluoride content in the toothpaste is not greater than 0.15%.

[0016] Another aspect of the present invention provides a method for preparing the toothpaste described in the first aspect, comprising the following steps, by weight percentage:

[0017] (1) Dissolve polyethylene glycol, 0.05-1.6% olaflumethrin and 0.05-0.3% sodium fluoride in water, heat to 50°C to aid dissolution, then add 2-8% porous silica, and dry to obtain fluoride-loaded porous silica;

[0018] (2) Mix 2-8% hydrated silica, 0-15% calcium phosphosilicate and 0-10% sodium calcium phosphosilicate and disperse them evenly to obtain a mixture;

[0019] (3) Stir 0.5-1.5% carbomer, the remaining polyethylene glycol and 30-42% glycerin evenly and then pour into a container;

[0020] (4) Then add the mixture prepared in step (2) into the container, stir, and then add 0.5-1.5% sodium lauroyl sarcosinate and stir.

[0021] (5) Then add the porous silica loaded with fluoride prepared in step (1), stir under vacuum until smooth and free of particles, degas for 20 minutes, vacuum degree -0.097±0.001MPa, and obtain the toothpaste product.

[0022] The stirring speed is 1000~3000 r / min and the stirring time is 20~40 min.

[0023] In step (1), the total amount of olaflu and sodium fluoride is in a mass ratio of 1:0.5~2 to polyethylene glycol; the total mass of olaflu and sodium fluoride is in a mass ratio of 1:5~10 to water.

[0024] The beneficial technical effects of this invention are as follows:

[0025] This invention optimizes the release rate of calcium and phosphorus ions by combining calcium phosphosilicate and sodium calcium phosphosilicate. Through the synergistic effect of calcium phosphosilicate and sodium calcium phosphosilicate, remineralization can be promoted more efficiently. Porous silica can load fluoride, preventing fluoride from reacting with calcium phosphosilicate and sodium calcium phosphosilicate to form calcium fluoride with lower solubility. At the same time, the combination of porous silica and polyethylene glycol can further slow down the release of fluoride ions in the oral cavity. This allows the small amount of fluoride ions released in the early stage of brushing to promote remineralization, while the large amount of fluoride ions released in the later stage of brushing will transform the hydroxyapatite generated in the remineralization process into fluorapatite with higher hardness.

[0026] Furthermore, in this invention, the toothpaste prepared by mixing calcium phosphosilicate, sodium calcium phosphosilicate, and olaflue in a specific ratio exhibits the optimal synergistic effect, manifested in the formation of the densest and most uniform remineralized layer with the highest hardness. This may be because an appropriate amount of olaflue can promote in-situ remineralization, while an excessive amount of olaflue leads to excessive fluoride ion release and accelerates the formation of insoluble calcium fluoride, thereby severely reducing the anti-caries effect. Attached Figure Description

[0027] Figure 1 The image shows a SEM image of bovine teeth treated with the toothpaste prepared in Example 1.

[0028] Figure 2 SEM image of bovine teeth treated with toothpaste prepared in Comparative Example 3.

[0029] Figure 3 SEM image of bovine teeth treated with toothpaste prepared in Comparative Example 4.

[0030] Figure 4 SEM image of bovine teeth treated with toothpaste prepared in Comparative Example 5. Detailed Implementation

[0031] The present invention will now be described in detail with reference to the accompanying drawings and embodiments.

[0032] This invention provides a toothpaste that releases a small amount of fluoride ions in the early stages of brushing to promote the remineralization process, while fluoride ions released in the later stages of brushing can react with the newly formed remineralized layer to form fluorapatite, which has higher hardness and better protects teeth.

[0033] The first aspect of the present invention provides a toothpaste for repairing tooth enamel, comprising calcium phosphosilicate, sodium calcium phosphosilicate, porous silica, polyethylene glycol, sodium fluoride, orafil, hydrated silica, and toothpaste base components.

[0034] In this invention, the release rate of calcium phosphosilicate and sodium calcium phosphosilicate can be controlled by optimizing the ratio, thereby optimizing the remineralization effect of tooth enamel. Hydrated silica can clean the tooth surface, providing better conditions for the deposition of the remineralized layer on the enamel surface. Porous silica can load fluoride, realizing the slow release of fluoride and preventing the release of fluoride ions too quickly to produce calcium fluoride, which would affect the total amount of free fluoride ions. At the same time, it can be combined with calcium phosphosilicate and sodium calcium phosphosilicate to achieve controlled release of fluoride ions first to promote the remineralization process and then form a new mineralized layer, thereby obtaining fluorapatite with higher hardness and improving the repair effect on tooth enamel.

[0035] In some embodiments, the toothpaste comprises, by weight percentage, the following raw material components: 0-15% calcium phosphosilicate, 0-10% sodium calcium phosphosilicate, 2-8% porous silica, 2-20% polyethylene glycol, 0.05-0.3% sodium fluoride, 0.05-1.6% olaflumethrin, 20-30% hydrated silica, and 31-43% toothpaste base components; the total fluoride content in the toothpaste is not greater than 0.15%.

[0036] In some embodiments, the calcium phosphosilicate has a particle size of 1-10 μm, including but not limited to 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, and 10 μm; preferably 1-5 μm; the sodium calcium phosphosilicate has a particle size of 1-10 μm, including but not limited to 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, and 10 μm; preferably 1-5 μm.

[0037] In some embodiments, the specific surface area of ​​the porous silica is 100-400 m². 2 / g, with a particle size of 1-100μm, including but not limited to 1μm, 10μm, 20μm, 30μm, 40μm, 50μm, 60μm, 70μm, 80μm, 90μm, and 100μm; and a pore size of 2-100 nm, including but not limited to 2nm, 10nm, 20nm, 30nm, 40nm, 50nm, 60nm, 70nm, 80nm, 90nm, and 100nm.

[0038] In some embodiments, the polyethylene glycol has a molecular weight of 282-810 Daltons; for example, the polyethylene glycol includes, but is not limited to, PEG-8, PEG-10, and PEG-12.

[0039] In some embodiments, the hydrated silica has a particle size of 1-100 μm, including but not limited to 1 μm, 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, and 100 μm.

[0040] In some embodiments, the total mass ratio of calcium phosphosilicate and sodium calcium phosphosilicate to olaflu is 1:0.01-1, including but not limited to 1:0.01, 1:0.02, 1:0.05, 1:0.1, 1:0.2, 1:0.3, 1:0.4, 1:0.5, 1:0.6, 1:0.7, 1:0.8, 1:0.9, and 1:1; preferably, the total mass ratio of calcium phosphosilicate and sodium calcium phosphosilicate to olaflu is 1:0.03-0.2.

[0041] In some embodiments, the toothpaste base components include glycerin, sodium lauroyl sarcosinate, carbomer, etc.

[0042] In some embodiments, the toothpaste, by mass fraction, comprises the following raw material components: 0-15% calcium phosphosilicate, 0-10% sodium calcium phosphosilicate, 2-8% porous silica, 2-20% polyethylene glycol, 0.05-0.3% sodium fluoride, 0.05-1.6% olafon, 20-30% hydrated silica, 30-42% glycerin, 0.5-1.5% sodium lauroyl sarcosinate, and 0.5-1.5% carbomer; and the total proportion m of calcium phosphosilicate and sodium calcium phosphosilicate in the toothpaste satisfies: 3% ≤ m ≤ 15%; the total fluoride content in the toothpaste is not greater than 0.15%.

[0043] It is understood that in this invention, the toothpaste base component also includes conventional additives such as sweeteners and flavorings, as well as any component that can be used as a toothpaste base and does not affect the effectiveness of this application. For example, the toothpaste base component also includes peach extract, strawberry extract, honeydew melon extract, blueberry extract, flavorings, xylitol, aspartame, sucrose, etc.

[0044] Another aspect of the present invention provides a method for preparing the toothpaste described in the first aspect, comprising the following steps, by weight percentage:

[0045] (1) Dissolve polyethylene glycol, 0.05-1.6% olaflumethrin and 0.05-0.3% sodium fluoride in water, heat to 50°C to aid dissolution, then add 2-8% porous silica, and dry to obtain fluoride-loaded porous silica;

[0046] (2) Mix 2-8% hydrated silica, 0-15% calcium phosphosilicate and 0-10% sodium calcium phosphosilicate and disperse them evenly to obtain a mixture;

[0047] (3) Stir 0.5-1.5% carbomer, the remaining polyethylene glycol and 30-42% glycerin evenly and then pour into a container;

[0048] (4) Then add the mixture prepared in step (2) into the container and stir until smooth and free of particles; then add 0.5-1.5% sodium lauroyl sarcosinate and stir until smooth and free of particles;

[0049] (5) Then add the porous silica loaded with fluoride prepared in step (1), stir under vacuum until smooth and free of particles; degas for 20 minutes, vacuum degree -0.097±0.001MPa, to obtain the toothpaste product;

[0050] In some embodiments, the stirring speed is 1000~3000 r / min and the stirring time is 20~40 min.

[0051] In some embodiments, in step (1), the total mass ratio of olafron and sodium fluoride to polyethylene glycol is 1:0.5~2; including but not limited to 1:0.5, 1:0.8, 1:1, 1:1.2, 1:1.4, 1:1.6, 1:1.8, and 1:2. The total mass ratio of olafron and sodium fluoride to water is 5~10:1, including but not limited to 5:1, 6:1, 7:1, 8:1, 9:1, and 10:11.

[0052] The present invention will be further illustrated below through examples and comparative examples.

[0053] Example 1

[0054] A toothpaste for repairing tooth enamel includes toothpaste base components, hydrated silica, porous silica, calcium phosphosilicate, and sodium calcium phosphosilicate, etc. Specific components and their contents are shown in Table 1.

[0055] Table 1: Toothpaste Raw Material Components and Proportions

[0056]

[0057] A method for preparing the above-mentioned toothpaste includes the following steps: (by weight percentage):

[0058] (1) Dissolve 0.461 kg of polyethylene glycol, 0.251 kg of olaflumethrin and 0.21 kg of sodium fluoride in 0.5 kg of deionized water, heat to 50°C to aid dissolution, then add 6 kg of porous silica to fully absorb the solution, and dry to obtain fluoride-loaded porous silica.

[0059] (2) Mix and disperse 25 kg of hydrated silica, 4.2 kg of calcium phosphosilicate and 2.8 kg of sodium calcium phosphosilicate evenly to obtain a mixture.

[0060] (3) Mix 1 kg of carbomer, 17.539 kg of polyethylene glycol and 41.539 kg of glycerin evenly and then pour the mixture into the main pot;

[0061] (4) Add the mixture prepared in step (2) to the main pot and stir until smooth and free of particles.

[0062] (5) Add 1 kg of sodium lauroyl sarcosinate to the main pot and stir until smooth and free of particles;

[0063] (6) Add the fluoride-loaded porous silica prepared in step (1) to the main pot and stir under vacuum until smooth and free of particles;

[0064] (8) Defoam the product for 20 minutes and apply a vacuum of -0.097±0.001MPa to obtain toothpaste for repairing tooth enamel.

[0065] The stirring speed was 2000 r / min and the stirring time was 30 min.

[0066] Example 2

[0067] A toothpaste for repairing tooth enamel, the composition and content of which are shown in Table 2.

[0068] Table 2 Toothpaste Raw Material Components and Proportions

[0069]

[0070] The toothpaste preparation method is the same as in Example 1.

[0071] Example 3

[0072] A toothpaste for repairing tooth enamel, the components and their contents are shown in Table 3.

[0073] Table 3: Toothpaste Raw Material Components and Proportions

[0074]

[0075] The toothpaste preparation method is the same as in Example 1.

[0076] Example 4

[0077] A toothpaste for repairing tooth enamel includes toothpaste base components, hydrated silica, porous silica, calcium phosphosilicate, and sodium calcium phosphosilicate. Specific components and their contents are shown in Table 4.

[0078] Table 4: Toothpaste Raw Material Components and Proportions

[0079]

[0080] The toothpaste preparation method is the same as in Example 1.

[0081] Example 5

[0082] A toothpaste for repairing tooth enamel has the following components and contents as shown in Table 4.

[0083] Table 4: Toothpaste Raw Material Components and Proportions

[0084]

[0085] The toothpaste preparation method is the same as in Example 1.

[0086] Example 6

[0087] A toothpaste for repairing tooth enamel has the following components and contents as shown in Table 5.

[0088] Table 5: Toothpaste Raw Material Components and Proportions

[0089]

[0090] The toothpaste preparation method is the same as in Example 1.

[0091] Comparative Example 1

[0092] Same as Example 5, except that the amount of calcium phosphosilicate used is 2 kg and the amount of glycerol used is 46.539 kg.

[0093] Comparative Example 2

[0094] Similar to Example 6, except that the amount of sodium calcium phosphosilicate added is 2 kg and the amount of glycerol used is 46.539 kg.

[0095] Comparative Example 3

[0096] A toothpaste for repairing tooth enamel, the components and their contents are shown in Table 6.

[0097] Table 6: Toothpaste Raw Material Components and Proportions

[0098]

[0099] The toothpaste preparation method is the same as in Example 1.

[0100] Comparative Example 4

[0101] A toothpaste for repairing tooth enamel, the components and their contents are shown in Table 7.

[0102] Table 7: Toothpaste Raw Material Components and Proportions

[0103]

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

[0105] Comparative Example 5

[0106] A toothpaste for repairing tooth enamel, the components and their contents are shown in Table 8.

[0107] Table 8: Toothpaste Raw Material Components and Proportions

[0108]

[0109] The toothpaste formulation of Comparative Example 5 is shown in the table above. The target product can be obtained through the following preparation process:

[0110] (1) Dissolve 0.251 kg of olaflur and 0.21 kg of sodium fluoride in 0.5 kg of deionized water, then add 6 kg of porous silica to fully absorb the solution, and dry to obtain porous silica loaded with fluoride.

[0111] (2) Mix and disperse 25 kg of hydrated silica, 4.2 kg of calcium phosphosilicate and 2.8 kg of sodium calcium phosphosilicate evenly to obtain a mixture;

[0112] (3) Mix 1 kg of carbomer, 18 kg of polyethylene glycol and 41.539 kg of glycerin evenly and then pour the mixture into the main pot.

[0113] (4) Add the mixture prepared in step (2) to the main pot and stir until smooth and free of particles.

[0114] (5) Add 1 kg of sodium lauroyl sarcosinate to the main pot and stir until smooth and free of particles.

[0115] (7) Add the fluoride-loaded porous silica prepared in step (1) to the main pot and stir under vacuum until smooth and free of particles.

[0116] (8) Degas the product for 20 minutes and apply a vacuum of -0.097±0.001MPa to obtain toothpaste.

[0117] The stirring speed was 2000 r / min and the stirring time was 30 min.

[0118] Comparative Example 6

[0119] A toothpaste for repairing tooth enamel, the components and their contents are shown in Table 9.

[0120] Table 9: Toothpaste Raw Material Components and Proportions

[0121]

[0122] The toothpaste formulation of Comparative Example 6 is shown in the table above. The target product can be obtained through the following preparation process:

[0123] (1) Mix 25kg of hydrated silica, 6kg of porous silica, 4.2kg of calcium phosphosilicate and 2.8kg of sodium calcium phosphosilicate evenly to obtain a mixture.

[0124] (2) Add 1 kg of carbomer, 0.1 kg of magnolia bark extract, 18 kg of polyethylene glycol-8 and 41.539 kg of glycerin into the main pot and stir until well mixed.

[0125] (3) Add the mixture prepared in step (1) to the main pot and stir until smooth and free of particles.

[0126] (4) Add 1 kg of sodium lauroyl sarcosinate to the main pot and stir until smooth and free of particles. Finally, add 0.21 kg of sodium fluoride and 0.251 kg of olaflumethine to the main pot and stir under vacuum until smooth and free of particles.

[0127] (5) Defoam the product for 20 minutes, and apply a vacuum of -0.097±0.001 to obtain toothpaste.

[0128] The stirring speed was 2000 r / min and the stirring time was 30 min.

[0129] Comparative Example 7

[0130] Similar to Example 1, except that the amount of calcium phosphosilicate added is 10 kg, sodium calcium phosphosilicate is 7 kg, and the amount of glycerol is 31.539 kg. The other components remain unchanged, and the preparation method is the same as in Example 1.

[0131] Test example:

[0132] (1) Characterization of sample surface after using toothpaste

[0133] The toothpaste samples from Example 1 and Comparative Examples 3-5 were characterized after use using a ZISS Sima 300 scanning electron microscope. The specific method was as follows:

[0134] The toothpastes prepared in Example 1 and Comparative Examples 3-5 were applied to toothbrushes, and the teeth were brushed for 2 minutes twice daily on pretreated isolated bovine tooth slices using a toothbrush abrasive device for 4 weeks, with intermittent placement in artificial saliva at 37°C. The morphology of the samples was photographed using a ZISS Sima300 scanning electron microscope. Specific details are as follows... Figure 1-4 As shown.

[0135] Depend on Figure 1-4 It can be seen that the remineralized layer on the surface of bovine teeth treated with the toothpaste prepared in Example 1 is dense and uniform. Figure 1 This demonstrates the synergistic effect between calcium phosphosilicate, sodium calcium phosphosilicate, and olaflu; compared to Example 1, Comparative Example 3 shows a much less dense remineralized layer with a different morphology. Figure 2 This demonstrates that olaflume is essential; compared to comparative example 3, comparative example 4 showed limited remineralization (…). Figure 3This indicates that a specific ratio of calcium phosphosilicate and sodium calcium phosphosilicate is required to synergistically promote remineralization. Compared with Example 1, Comparative Example 5 showed a significant decrease in the density of the remineralized layer, highlighting the importance of the combined use of polyethylene glycol and porous silica for the slow release of fluoride ions.

[0136] (2) Microhardness test

[0137] The enamel restoration effect was evaluated using a hardness test. To assess the impact of the test samples (prepared toothpaste) on tooth surface hardness in the examples and comparative examples, the surface hardness of extracted bovine tooth sections was measured using a Vickers hardness tester (VH1102, Buehler). The specific method is as follows:

[0138] 1) Preparation of artificial saliva:

[0139] Weigh out 0.1g sodium chloride, 0.1g potassium chloride, 0.17g calcium chloride, 0.25g urea, 0.0026g sodium sulfide nonahydrate, and 0.17g sodium dihydrogen phosphate. Dissolve them in deionized water and bring the volume to 250mL. Adjust the pH to 6.80 with 1mol / L sodium hydroxide solution to obtain artificial saliva.

[0140] 2) Processing of extracted bovine tooth fragments:

[0141] A. Pretreatment of bovine teeth: Select freshly extracted or recently extracted third molars, remove plaque and attached soft tissue, soak in 75% ethanol for at least 15 minutes, and cut a 1 mm thick slice at an angle perpendicular to the long axis of the tooth. Place the slice in a 35% phosphoric acid solution for 30 seconds, remove it, rinse immediately with deionized water, and clean with an ultrasonic cleaner (KQ-300E, Kunshan Shumei) for 10 minutes. Dry and set aside.

[0142] B. Acid etching model of bovine teeth:

[0143] Extracted bovine tooth fragments were treated with 1% lactic acid solution twice daily for 2 minutes each time, for a total of 2 weeks, with intermittent treatment in artificial saliva at 37°C.

[0144] 3) Experimental sample processing:

[0145] Control group: Pretreated isolated bovine tooth fragments were placed in artificial saliva at 37°C for 28 days;

[0146] Sample group: Take the toothpaste prepared in Examples 1-6 or Comparative Examples 3-7, apply it to the toothbrush, and use a brushing device to brush the teeth on the pretreated isolated bovine tooth slices for 2 minutes, twice a day, for a total of 4 weeks. During the intermittent period, place it in artificial saliva at 37°C.

[0147] 4) Hardness test:

[0148] Using a Vickers hardness tester, hardness tests were conducted on dental radiographs in the blank group, negative control group, and sample group under fixed load and loading time of 100g and 10s, respectively. A straight line was drawn along the middle of each sample, and seven points were marked at fixed intervals. The average value was used to calculate the surface hardness of the radiograph. The results are shown in the table below.

[0149] Table 10: Microhardness values ​​of toothpastes prepared in the examples and comparative examples

[0150]

[0151] *The toothpaste used for testing was stored for less than one month; other toothpastes used for testing were stored for more than one year.

[0152] Table 10 shows that the surface hardness of the tooth films in the sample treatment group was higher than that in the blank group, indicating that the samples were beneficial in promoting an increase in tooth surface hardness. Meanwhile, the toothpastes prepared in Examples 1-3 all exhibited superior hardness values. In Comparative Example 3, sodium fluoride was used to replace olaflurium in Comparative Example 3, resulting in a significantly lower microhardness value compared to Example 1. In Comparative Example 4, sodium fluoride was used to replace olaflurium in Comparative Example 4, and the mass ratio of calcium phosphosilicate to sodium calcium phosphosilicate was changed; compared to Comparative Example 3, its microhardness value was lower. The enamel repair effect of the toothpaste prepared in Comparative Example 5, compared to Example 1, demonstrates the importance of combining polyethylene glycol with porous silica to enhance the sustained-release effect. Comparative Example 6, without porous silica loading, showed a significantly lower enamel repair effect compared to Example 1.

[0153] This application optimizes the toothpaste to improve the repair and remineralization effect on tooth enamel. It successfully provides a toothpaste that releases a small amount of fluoride ions in the early stage of brushing to promote the remineralization process, while releasing a large amount of fluoride ions in the later stage of brushing to react with the newly formed mineralized layer to form fluorapatite with higher hardness, thus better protecting teeth.

[0154] The above description is merely a preferred embodiment of the present invention, and the present invention is not limited to the above embodiments. It is understood that other improvements and variations that are directly derived or conceived by those skilled in the art without departing from the spirit and concept of the present invention should be considered to be included within the protection scope of the present invention.

Claims

1. A toothpaste for repairing tooth enamel, characterized in that, The toothpaste, by weight percentage, comprises the following raw material components: 0-15% calcium phosphosilicate, 0-10% sodium calcium phosphosilicate, 2-8% porous silica, 2-20% polyethylene glycol, 0.05-0.3% sodium fluoride, 0.05-1.6% olaflumethrin, 20-30% hydrated silica, and 31-43% toothpaste base components; and the total proportion m of calcium phosphosilicate and sodium calcium phosphosilicate in the toothpaste satisfies: 3% ≤ m ≤ 15%; the total fluoride content in the toothpaste is not greater than 0.15%. The calcium phosphosilicate has a particle size of 1-10 μm; the sodium calcium phosphosilicate has a particle size of 1-10 μm. The molecular weight of the polyethylene glycol is 282-810 Daltons; In the preparation of the toothpaste, a portion of polyethylene glycol, 0.05-1.6% olaflumethrin and 0.05-0.3% sodium fluoride are dissolved in water, and then 2-8% porous silica is added. After drying, porous silica loaded with fluoride is obtained. The total mass ratio of the olafon and sodium fluoride to the partial polyethylene glycol is 1:0.5~2; the total mass ratio of the olafon and sodium fluoride to water is 1:5~10.

2. The toothpaste according to claim 1, characterized in that, The calcium phosphosilicate has a particle size of 1-5 μm; the sodium calcium phosphosilicate has a particle size of 1-5 μm.

3. The toothpaste according to claim 1, characterized in that, The porous silica has a specific surface area of ​​100-400 m². 2 / g, with a particle size of 1-100μm and a pore size of 2-100 nm.

4. The toothpaste according to claim 1, characterized in that, The hydrated silica has a particle size of 1-100 μm.

5. The toothpaste according to claim 1, characterized in that, The total mass ratio of calcium phosphosilicate and sodium calcium phosphosilicate to olaflu is 1:0.01-1.

6. The toothpaste according to claim 1, characterized in that, The total mass ratio of calcium phosphosilicate and sodium calcium phosphosilicate to olaflu is 1:0.03-0.

2.

7. The toothpaste according to claim 1, characterized in that, The toothpaste base components include glycerin, sodium lauroyl sarcosinate, and carbomer.

8. The toothpaste according to claim 7, characterized in that, By mass percentage, the toothpaste comprises the following raw material components: 0-15% calcium phosphosilicate, 0-10% sodium calcium phosphosilicate, 2-8% porous silica, 2-20% polyethylene glycol, 0.05-0.3% sodium fluoride, 0.05-1.6% olafur, 20-30% hydrated silica, 30-42% glycerin, 0.5-1.5% sodium lauroyl sarcosinate, and 0.5-1.5% carbomer; and the total proportion m of calcium phosphosilicate and sodium calcium phosphosilicate in the toothpaste satisfies: 3% ≤ m ≤ 15%; the total fluoride content in the toothpaste is not greater than 0.15%.

9. A method for preparing the toothpaste according to claim 8, characterized in that, Includes the following steps, by weight percentage: (1) Dissolve some polyethylene glycol, 0.05-1.6% olaflumethrin and 0.05-0.3% sodium fluoride in water, then add 2-8% porous silica, and dry to obtain fluoride-loaded porous silica; (2) Mix 20-30% hydrated silica, 0-15% calcium phosphosilicate and 0-10% sodium calcium phosphosilicate and disperse them evenly to obtain a mixture; (3) After mixing 0.5-1.5% carbomer, the remaining polyethylene glycol and 30-42% glycerin evenly, pour the mixture into a container; (4) Then add the mixture prepared in step (2) into the container, stir, and then add 0.5-1.5% sodium lauroyl sarcosinate and stir. (5) Then add the porous silica loaded with fluoride prepared in step (1), stir under vacuum, degas, and obtain the toothpaste product; In step (1), the total mass ratio of the olaflu and sodium fluoride to the partial polyethylene glycol is 1:0.5~2; the total mass ratio of the olaflu and sodium fluoride to water is 1:5~10. The stirring speed was 1000~3000 r / min and the stirring time was 20~40 min.

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