Toothpaste for repairing tooth enamel and preparation method therefor

Abstract

Disclosed in the present invention are a toothpaste for repairing tooth enamel and a preparation method therefor. The toothpaste of the present invention comprises calcium phosphosilicate, calcium sodium phosphosilicate, porous silica, polyethylene glycol, sodium fluoride, olaflur, hydrated silica, and a toothpaste matrix component. According to the present invention, the release speed of calcium and phosphate ions is regulated and controlled by optimizing the ratio of the calcium phosphosilicate to the calcium sodium phosphosilicate, and in addition, the fluoride and the polyethylene glycol are loaded in the porous silica, such that the hydrogen bond effect between the fluoride and the polyethylene glycol can further reduce the release speed of the fluoride in the oral cavity, a small number of fluorine ions released in the early stage of tooth brushing can promote remineralization, and a large number of fluorine ions released in the later stage of tooth brushing can convert newly generated hydroxyapatite into fluorapatite with higher hardness.

Description

Toothpaste for repairing tooth enamel and preparation method thereof Technical Field

[0001] The present invention relates to the technical field of oral care products, and in particular to a toothpaste for repairing tooth enamel and a preparation method thereof. Background Art

[0002] Dental caries, with its high prevalence and widespread distribution, is 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 to be prevented and controlled. Tooth decay has five stages. The first is demineralization—the initial stage of tooth decay manifests as white or brown spots on the tooth surface. This occurs when tooth enamel becomes fragile and in danger of dissolution. Using toothpaste containing agents that promote enamel remineralization can reverse this stage of tooth decay. Consequently, considerable research is being devoted to enamel remineralization.

[0003] Remineralization is a natural tooth repair process. Calcium and phosphate in saliva form minerals that are deposited on the surface of tooth enamel. Studies have found that calcium phosphosilicate and bioactive glass (sodium calcium phosphosilicate) can effectively release calcium and phosphate ions, thereby promoting tooth repair. Studies have shown that fluoride can promote the remineralization process and can increase the microhardness of teeth and reduce tooth surface roughness. However, calcium fluoride is an extremely insoluble substance, and the rapid formation of calcium fluoride will reduce the calcium ion concentration in the mouth. Therefore, to promote the remineralization process, it is best to adopt a slow-release strategy for fluoride ions. Currently, toothpastes circulating on the market have not considered how to control the release of fluoride ions to achieve remineralization while avoiding the impact of the rapid formation of insoluble calcium fluoride on calcium ion concentration. In addition, toothpastes circulating on the market do not control the release of fluoride ions to convert the hydroxyapatite formed by remineralization into fluorapatite with higher hardness and better caries prevention effect.

[0004] Summary of the Invention

[0005] To address the shortcomings of existing technologies, the present invention provides a toothpaste for repairing tooth enamel and a preparation method thereof. This invention optimizes the ratio between calcium phosphosilicate and sodium calcium phosphosilicate to regulate the release rate of calcium and phosphate ions. Fluoride and polyethylene glycol are simultaneously loaded into porous silica. The hydrogen bonding between fluoride and polyethylene glycol further slows the release rate of fluoride ions in the oral cavity. The small amount of fluoride released during the initial brushing phase promotes remineralization, while the larger amount of fluoride released during the later stages of brushing converts newly formed hydroxyapatite into harder fluorapatite.

[0006] The technical solutions of the present invention are as follows:

[0007] A 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, olafluor, hydrated silica and a toothpaste base component.

[0008] In some embodiments, the toothpaste comprises the following raw material components, calculated by mass percentage: 0-15% calcium phosphosilicate, 0-10% sodium calcium phosphosilicate, 2-8% porous silica, 2-20% polyethylene glycol, 0.05-0.36% sodium fluoride, 0.05-1.6% olafluan, 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%.

[0009] In some embodiments, the toothpaste comprises the following raw material components, calculated by mass percentage: 0-15% calcium phosphosilicate, 0-10% sodium calcium phosphosilicate, 2-8% porous silica, 2-20% polyethylene glycol, 0.05-0.36% sodium fluoride, 0.05-1.6% olafluan, 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%.

[0010] In some embodiments, the particle size of the calcium silicophosphate is 1-10 μm, preferably 1-5 μm; the particle size of the calcium sodium phosphosilicate is 1-10 μm, preferably 1-5 μm.

[0011] In some embodiments, the specific surface area of ​​the porous silica is 100-400 m 2 / g, particle size is 1-100μm, and pore size is 2-100nm.

[0012] In some embodiments, the molecular weight of the polyethylene glycol is 282-810 Daltons; and the particle size of the hydrated silica is 1-100 μm.

[0013] In some embodiments, the mass ratio of the total mass of the calcium phosphosilicate and sodium calcium phosphosilicate to the mass of olafluanid is 1:0.01-1.

[0014] Preferably, the mass ratio of the total mass of the calcium phosphosilicate and sodium calcium phosphosilicate to the mass of olafluanid is 1:0.03-0.2.

[0015] In some embodiments, the toothpaste base components include glycerin, sodium lauroyl sarcosinate, and carbomer.

[0016] In some embodiments, the toothpaste comprises the following raw material components by mass: 0-15% calcium phosphosilicate, 0-10% sodium calcium phosphosilicate, 2-8% porous silica, 2-20% polyethylene glycol, 0.05-0.36% sodium fluoride, 0.05-1.6% olafluan, 20-30% hydrated silica, 30-42% glycerol, 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%.

[0017] Another aspect of the present invention provides a method for preparing the toothpaste according to the first aspect, comprising the following steps, in percentage by mass:

[0018] (1) dissolving polyethylene glycol, 0.05-1.6% olafluanid and 0.05-0.36% sodium fluoride in water, heating to 50° C. to promote dissolution, then adding 2-8% porous silica, and drying to obtain fluoride-loaded porous silica;

[0019] (2) mixing 2-8% hydrated silica, 0-15% calcium phosphosilicate, and 0-10% sodium calcium phosphosilicate, and uniformly dispersing the mixture to obtain a mixed material;

[0020] (3) Mix 0.5-1.5% carbomer, the remaining polyethylene glycol, and 30-42% glycerol and pour into the container;

[0021] (4) adding the mixture prepared in step (2) into a container, stirring, and then adding 0.5-1.5% sodium lauroyl sarcosinate and stirring;

[0022] (5) Then, the fluoride-loaded porous silica prepared in step (1) was added, and the mixture was stirred under vacuum until smooth and free of particles, and then degassed for 20 minutes at a vacuum degree of -0.097±0.001 MPa to obtain the toothpaste product;

[0023] The stirring speed is 1000-3000 r / min, and the stirring time is 20-40 min;

[0024] In step (1), the mass ratio of the total amount of olafluanid and sodium fluoride to polyethylene glycol is 1:0.5-2; the mass ratio of the total mass of olafluanid and sodium fluoride to water is 1:5-10.

[0025] The beneficial technical effects of the present invention are:

[0026] The present invention optimizes the release rate of calcium and phosphate ions by compounding calcium phosphosilicate and sodium calcium phosphosilicate. Through the synergistic effect of calcium phosphosilicate and sodium calcium phosphosilicate, remineralization can be promoted more efficiently. The porous silica can achieve the loading of fluoride and prevent the reaction of fluoride with calcium phosphosilicate and sodium calcium phosphosilicate to generate calcium fluoride with lower solubility. At the same time, the combination of porous silica and polyethylene glycol can further slow the release of fluoride ions in the oral cavity, so that the small amount of fluoride ions released in the early stage of brushing can promote remineralization, and the large amount of fluoride ions released in the later stage of brushing can convert hydroxyapatite generated in the remineralization process into fluorapatite with higher hardness.

[0027] Furthermore, in the present invention, the toothpaste prepared by mixing calcium phosphosilicate, sodium calcium phosphosilicate and olafluor in a specific ratio has the best synergistic effect, which is manifested in that the remineralized layer formed is the most dense and uniform and has the highest hardness. The possible reason is that an appropriate amount of olafluor can promote the occurrence of in situ remineralization, while an excessive amount of olafluor leads to excessive fluoride ion release and accelerates the formation of insoluble calcium fluoride, thereby seriously reducing the anti-caries effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] FIG1 is a SEM image of bovine teeth treated with the toothpaste prepared in Example 1.

[0029] Figure 2 is a SEM image of bovine teeth treated with the toothpaste prepared in Comparative Example 3.

[0030] FIG3 is a SEM image of bovine teeth treated with the toothpaste prepared in Comparative Example 4.

[0031] FIG4 is a SEM image of bovine teeth treated with the toothpaste prepared in Comparative Example 5. DETAILED DESCRIPTION

[0032] The present invention will be described in detail below with reference to the accompanying drawings and embodiments.

[0033] The present invention provides a toothpaste that releases a small amount of fluoride ions in the early stage of brushing to promote the remineralization process. At the same time, the fluoride ions released in the later stage of brushing can react with the newly formed remineralized layer to form fluorapatite with higher hardness, thereby better protecting teeth.

[0034] A 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, olafluor, hydrated silica and a toothpaste base component.

[0035] In the present invention, the release rate of calcium and phosphorus ions can be controlled by optimizing the ratio of calcium phosphosilicate and sodium calcium phosphosilicate, thereby optimizing the remineralization effect of tooth enamel; hydrated silica can clean the tooth surface, providing more optimal conditions for the deposition of a remineralization layer on the tooth enamel surface; porous silica can load fluoride, thereby achieving a slow release of fluoride, preventing the fluoride ions from being released too quickly to produce calcium fluoride, which affects the total amount of free fluoride ions; and at the same time, it can be combined with calcium phosphosilicate and sodium calcium phosphosilicate to achieve controlled release of fluoride ions, which are first used to promote the remineralization process and then form a new mineralization layer, thereby obtaining fluorapatite with higher hardness and improving the repair effect on tooth enamel.

[0036] In some embodiments, the toothpaste comprises the following raw material components, calculated by mass percentage: 0-15% calcium phosphosilicate, 0-10% sodium calcium phosphosilicate, 2-8% porous silica, 2-20% polyethylene glycol, 0.05-0.36% sodium fluoride, 0.05-1.6% olafluanid, 20-30% hydrated silica, and 31-43% toothpaste base components.

[0037] In some embodiments, the particle size of the calcium silicophosphate is 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, 10 μm; preferably 1-5 μm; the particle size of the sodium calcium phosphosilicate is 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, 10 μm; preferably 1-5 μm.

[0038] In some embodiments, the specific surface area of ​​the porous silica is 100-400 m 2 / g, the particle size is 1-100μm, including but not limited to 1μm, 10μm, 20μm, 30μm, 40μm, 50μm, 60μm, 70μm, 80μm, 90μm, 100μm; the pore size is 2-100nm, including but not limited to 2nm, 10nm, 20nm, 30nm, 40nm, 50nm, 60nm, 70nm, 80nm, 90nm, 100nm.

[0039] In some embodiments, the molecular weight of the polyethylene glycol is 282-810 Daltons; illustratively, the polyethylene glycol includes but is not limited to PEG-8, PEG-10, and PEG-12.

[0040] In some embodiments, the particle size of the hydrated silica is 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.

[0041] In some embodiments, the mass ratio of the total mass of the calcium phosphosilicate and the sodium calcium phosphosilicate to the olafluan 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 mass ratio of the total mass of the calcium phosphosilicate and the sodium calcium phosphosilicate to the olafluan is 1:0.03-0.2.

[0042] In some embodiments, the toothpaste base components include glycerin, sodium lauroyl sarcosinate, carbomer, and the like.

[0043] In some embodiments, the toothpaste comprises the following raw material components by mass: 0-15% calcium phosphosilicate, 0-10% sodium calcium phosphosilicate, 2-8% porous silica, 2-20% polyethylene glycol, 0.05-0.36% sodium fluoride, 0.05-1.6% olafluan, 20-30% hydrated silica, 30-42% glycerol, 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%.

[0044] It is understood that, in the present invention, the toothpaste base components also include conventional additives such as sweeteners and flavoring ingredients, as well as any component that can be used as a toothpaste base and does not affect the effects of the present application. Exemplary components include peach extract, strawberry extract, honeydew melon extract, blueberry extract, flavoring, xylitol, aspartame, sucrose, etc.

[0045] Another aspect of the present invention provides a method for preparing the toothpaste according to the first aspect, comprising the following steps, in percentage by mass:

[0046] (1) dissolving polyethylene glycol, 0.05-1.6% olafluanid and 0.05-0.36% sodium fluoride in water, heating to 50° C. to promote dissolution, then adding 2-8% porous silica, and drying to obtain fluoride-loaded porous silica;

[0047] (2) mixing 2-8% hydrated silica, 0-15% calcium phosphosilicate, and 0-10% sodium calcium phosphosilicate, and uniformly dispersing the mixture to obtain a mixed material;

[0048] (3) Mix 0.5-1.5% carbomer, the remaining polyethylene glycol, and 30-42% glycerol and pour into the container;

[0049] (4) The mixture prepared in step (2) is then added to a container and stirred until smooth and free of particles; 0.5-1.5% sodium lauroyl sarcosinate is then added and stirred until smooth and free of particles;

[0050] (5) Then, the fluoride-loaded porous silica prepared in step (1) was added, and the mixture was stirred under vacuum until smooth and free of particles; degassing was performed for 20 minutes, and the vacuum degree was -0.097±0.001 MPa to obtain the toothpaste product;

[0051] In some embodiments, the stirring speed is 1000-3000 r / min, and the stirring time is 20-40 min.

[0052] In some embodiments, in step (1), the mass ratio of the total mass of olafluanid 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 mass ratio of the total mass of olafluanid 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.

[0053] The present invention will be further described below by way of examples and comparative examples.

[0054] Example 1

[0055] A toothpaste for repairing tooth enamel, comprising a toothpaste base component, hydrated silica, porous silicon dioxide, calcium phosphosilicate, and sodium calcium phosphosilicate. Specific components and contents are shown in Table 1.

[0056] Table 1: Toothpaste raw material components and ratios

[0057] A method for preparing the above toothpaste comprises the following steps: by mass percentage:

[0058] (1) 0.461 kg of polyethylene glycol, 0.251 kg of olafluanid, and 0.21 kg of sodium fluoride were dissolved in 0.5 kg of deionized water, heated to 50°C for dissolution, and then 6 kg of porous silica was added to fully absorb the solution. After drying, porous silica loaded with fluoride was obtained.

[0059] (2) 25 kg of hydrated silica, 4.2 kg of calcium phosphosilicate and 2.8 kg of sodium calcium phosphosilicate were mixed and dispersed uniformly to obtain a mixed material.

[0060] (3) Stir 1 kg of carbomer, 17.539 kg of polyethylene glycol, and 41.539 kg of glycerol until evenly combined and pour 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 mixing bowl 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 vacuum stir until smooth and free of particles;

[0064] (8) Degas the product for 20 minutes at a vacuum degree of -0.097±0.001 MPa to obtain a 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 components and contents of which are shown in Table 2.

[0068] Table 2 Toothpaste raw material components and ratios

[0069] The toothpaste preparation method is the same as that in Example 1.

[0070] Example 3

[0071] A toothpaste for repairing tooth enamel, the components and contents of which are shown in Table 3.

[0072] Table 3: Toothpaste raw material components and ratios

[0073] The toothpaste preparation method is the same as that in Example 1.

[0074] Example 4

[0075] A toothpaste for repairing tooth enamel, comprising a toothpaste base component, hydrated silica, porous silicon dioxide, calcium phosphosilicate, sodium calcium phosphosilicate, etc. Specific components and contents are shown in Table 4.

[0076] Table 4: Toothpaste raw material components and ratios

[0077] The toothpaste preparation method is the same as that in Example 1.

[0078] Example 5

[0079] A toothpaste for repairing tooth enamel, the components and contents of which are shown in Table 4.

[0080] Table 4: Toothpaste raw material components and ratios

[0081] The toothpaste preparation method is the same as that in Example 1.

[0082] Example 6

[0083] A toothpaste for repairing tooth enamel, the components and contents of which are shown in Table 5.

[0084] Table 5: Toothpaste raw material components and ratios

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

[0086] Comparative Example 1

[0087] The 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.

[0088] Comparative Example 2

[0089] The same as Example 6, except that the addition amount of sodium calcium phosphosilicate is 2 kg and the amount of glycerol used is 46.539 kg.

[0090] Comparative Example 3

[0091] A toothpaste for repairing tooth enamel, the components and contents of which are shown in Table 6.

[0092] Table 6: Toothpaste raw material components and ratios

[0093] The toothpaste preparation method is the same as that in Example 1.

[0094] Comparative Example 4

[0095] A toothpaste for repairing tooth enamel, the components and contents of which are shown in Table 7.

[0096] Table 7: Toothpaste raw material components and ratios

[0097] The toothpaste preparation method is the same as that in Example 1.

[0098] Comparative Example 5

[0099] A toothpaste for repairing tooth enamel, the components and contents of which are shown in Table 8.

[0100] Table 8: Toothpaste raw material components and ratios

[0101] The toothpaste formula of Comparative Example 5 is shown in the table above, and the target product can be obtained through the following preparation process:

[0102] (1) 0.251 kg of olafluanid and 0.21 kg of sodium fluoride were dissolved in 0.5 kg of deionized water, and then 6 kg of porous silica was added to fully absorb the solution. After drying, porous silica loaded with fluoride was obtained.

[0103] (2) 25 kg of hydrated silica, 4.2 kg of calcium phosphosilicate and 2.8 kg of sodium calcium phosphosilicate were mixed and dispersed uniformly to obtain a mixed material;

[0104] (3) Mix 1 kg of carbomer, 18 kg of polyethylene glycol and 41.539 kg of glycerol and pour them into the main pot.

[0105] (4) Add the mixture prepared in step (2) to the main pot and stir until smooth and free of particles.

[0106] (5) Add 1 kg of sodium lauroyl sarcosinate to the mixing bowl and stir until smooth and free of particles.

[0107] (7) Add the fluoride-loaded porous silica prepared in step (1) into the main pot and vacuum stir until it is smooth and free of particles.

[0108] (8) Degas the product for 20 minutes at a vacuum degree of -0.097±0.001 MPa to obtain toothpaste.

[0109] The stirring speed was 2000 r / min and the stirring time was 30 min.

[0110] Comparative Example 6

[0111] A toothpaste for repairing tooth enamel, the components and contents of which are shown in Table 9.

[0112] Table 9: Toothpaste raw material components and ratios

[0113] The toothpaste formula of Comparative Example 6 is shown in the table above, and the target product can be obtained through the following preparation process:

[0114] (1) 25 kg of hydrated silica, 6 kg of porous silicon dioxide, 4.2 kg of calcium phosphosilicate and 2.8 kg of sodium calcium phosphosilicate were mixed and dispersed uniformly to obtain a mixed material.

[0115] (2) Pour 1 kg of carbomer, 0.1 kg of Magnolia officinalis bark extract, 18 kg of polyethylene glycol-8 and 41.539 kg of glycerol into the main pot and mix well.

[0116] (3) Add the mixture prepared in step (1) into the main pot and stir until smooth and free of particles.

[0117] (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 olafluanid to the main pot and stir under vacuum until smooth and free of particles.

[0118] (5) Degas the product for 20 minutes at a vacuum degree of -0.097±0.001 to obtain toothpaste.

[0119] The stirring speed was 2000 r / min and the stirring time was 30 min.

[0120] Comparative Example 7

[0121] The same as Example 1, except that the added amount of calcium phosphosilicate is 10 kg, the amount of sodium calcium phosphosilicate is 7 kg, the amount of glycerol used is 31.539 kg, and the other components remain unchanged. The preparation method is the same as Example 1.

[0122] Example 7

[0123] A toothpaste for repairing tooth enamel, the components and contents of which are shown in Table 10.

[0124] Table 10: Toothpaste raw material components and ratios

[0125] The toothpaste preparation method is the same as that in Example 1.

[0126] Example 8

[0127] A toothpaste for repairing tooth enamel, the components and contents of which are shown in Table 11.

[0128] Table 11: Toothpaste raw material components and ratios

[0129] Test example:

[0130] (1) Sample surface characterization after using toothpaste

[0131] The toothpaste samples of Example 1 and Comparative Examples 3-5 were characterized by a ZISS Sima 300 scanning electron microscope after use. The specific method is as follows:

[0132] The toothpastes prepared in Example 1 and Comparative Examples 3-5 were applied to toothbrushes and applied to pretreated ex vivo bovine tooth slides using a toothbrush abrader for 2 minutes twice daily for 4 weeks, with the slides exposed to artificial saliva at 37°C. The sample morphologies were photographed using a ZISS Sima 300 scanning electron microscope. Details are shown in Figures 1-4.

[0133] As can be seen from Figures 1-4, the remineralized layer on the surface of bovine teeth treated with the toothpaste prepared in Example 1 is dense and uniform (Figure 1), reflecting the synergistic effect between calcium phosphosilicate, sodium calcium phosphosilicate and olafluanid; compared with Example 1, the remineralized layer of Comparative Example 3 is very non-dense and has a different morphology (Figure 2), proving that olafluanid is indispensable; compared with Comparative Example 3, the remineralization effect of Comparative Example 4 is limited (Figure 3), indicating that a specific ratio of calcium phosphosilicate and sodium calcium phosphosilicate can synergistically promote remineralization; compared with Example 1, the density of the remineralized layer of Comparative Example 5 has obviously deteriorated, indicating the importance of using polyethylene glycol and porous silica in combination to release fluoride ions.

[0134] (2) Microhardness test

[0135] The enamel repair effect was evaluated by hardness measurement test. In order to evaluate the effect of the test samples (prepared toothpastes) in the examples and comparative examples on the surface hardness of teeth, the surface hardness of isolated bovine tooth slices was measured using a Vickers hardness tester (VH1102, Buehler). The specific method is as follows:

[0136] 1) Preparation of artificial saliva:

[0137] Weigh 0.1 g of sodium chloride, 0.1 g of potassium chloride, 0.17 g of calcium chloride, 0.25 g of urea, 0.0026 g of sodium sulfide nonahydrate, and 0.17 g of sodium dihydrogen phosphate, add deionized water to dissolve, and dilute to 250 mL. Adjust the pH to 6.80 with 1 mol / L sodium hydroxide solution to obtain artificial saliva.

[0138] 2) Treatment of in vitro bovine tooth slices:

[0139] A. Bovine Tooth Pretreatment: Select freshly or recently extracted third molars, remove tartar and attached soft tissue, and soak them in 75% ethanol for at least 15 minutes. Cut a 1mm thick slice perpendicular to the long axis of the tooth. Place the slice in 35% phosphoric acid solution for 30 seconds, then remove it. Immediately rinse it with deionized water and clean it with an ultrasonic cleaner (KQ-300E, Kunshan Shumei) for 10 minutes. Dry it and set aside.

[0140] B. Bovine tooth acid etching modeling:

[0141] Treat the isolated bovine tooth slices with 1% lactic acid solution twice a day for 2 minutes each time for a total of 2 weeks. During the interval, place them in artificial saliva at 37°C.

[0142] 3) Experimental sample processing:

[0143] Blank group: The pretreated isolated bovine tooth slices were placed in artificial saliva at 37°C for 28 days;

[0144] Sample group: toothpaste prepared in Examples 1-6 or Comparative Examples 3-7 was applied on a toothbrush, and brushed on pretreated in vitro bovine tooth slices using a toothbrush abrader for 2 minutes, twice a day, for a total of 4 weeks, with an interval of placing in 37°C artificial saliva.

[0145] 4) Hardness test:

[0146] Using a Vickers hardness tester, the hardness of tooth slices from the blank group, negative control group, and sample group was tested under a fixed load of 100g and a loading time of 10s. Seven points were punched along a straight line at regular intervals along the middle of each sample, and the average value was used to calculate the surface hardness of the tooth slice. The results are shown in the table below.

[0147] Table 12: Microhardness values ​​of toothpastes prepared in Examples and Comparative Examples *The toothpastes used in the tests were stored for less than one month; the toothpastes used in other tests were stored for more than one year.

[0148] As can be seen from Table 12, the surface hardness of the tooth pieces in the sample treatment group is higher than that in the blank group, indicating that the sample is beneficial to promoting the increase in the surface hardness of the teeth. At the same time, the hardness values ​​of the toothpastes prepared in Examples 1-3 are all relatively good. In Comparative Example 3, olafluanid is replaced by sodium fluoride. Compared with Example 1, the microhardness value is significantly reduced. In Comparative Example 4, olafluanid is replaced by sodium fluoride, and the mass ratio of calcium phosphosilicate and sodium calcium phosphosilicate is changed. Compared with Comparative Example 3, its microhardness value is reduced. The enamel repair effect of the toothpaste prepared in Comparative Example 5 is compared with that in Example 1, reflecting the importance of combining polyethylene glycol with porous silica to improve the sustained release effect. Comparative Example 6 is not loaded with porous silica, and the enamel repair effect is significantly reduced compared with Example 1.

[0149] Through optimization, the toothpaste prepared in this application improves the repair and remineralization effects on tooth enamel, and successfully provides a toothpaste that releases a small amount of fluoride ions in the early stage of brushing to promote the remineralization process. At the same time, the large amount of fluoride ions released in the later stage of brushing can react with the newly formed mineral layer to form fluoroapatite with higher hardness, thereby better protecting teeth.

[0150] The above description is merely a preferred embodiment of the present invention, and the present invention is not limited to the above embodiment. It is understood that other improvements and variations directly derived or imagined by those skilled in the art without departing from the spirit and concept of the present invention should be considered to be included in the scope of protection of the present invention.

Claims

1. A toothpaste for repairing tooth enamel, characterized in that, It includes calcium phosphosilicate, calcium sodium phosphosilicate, porous silica, polyethylene glycol, sodium fluoride, oranoft, hydrated silica and toothpaste matrix components.

2. The toothpaste according to claim 1, wherein By mass percentage, the toothpaste includes the following raw material components: 0-15% calcium phosphosilicate, 0-10% calcium sodium phosphosilicate, 2-8% porous silica, 2-20% polyethylene glycol, 0.05-0.3% sodium fluoride, 0.05-1.6% oranoft, 20-30% hydrated silica, 31-43% toothpaste matrix components; and the total proportion m of calcium phosphosilicate and calcium sodium phosphosilicate in the toothpaste satisfies: 3% ≤ m ≤ 15%.

3. The toothpaste according to claim 2, wherein, The particle size of the calcium phosphosilicate is 1-10 μm, preferably 1-5 μm; the particle size of the calcium sodium phosphosilicate is 1-10 μm, preferably 1-5 μm.

4. The toothpaste according to claim 2, wherein The specific surface area of the porous silica is 100 - 400 m 2 / g, the particle size is 1 - 100 μm, and the pore diameter is 2 - 100 nm.

5. The toothpaste according to claim 2, characterized in that, The molecular weight of the polyethylene glycol is 282-810 daltons; the particle size of the hydrated silica is 1-100 μm.

6. The toothpaste according to claim 2, characterized in that, The mass ratio of the total mass of the calcium phosphosilicate and the calcium sodium phosphosilicate to the mass of the oranoft is 1:0.01-1.

7. The toothpaste according to claim 2, characterized in that, The mass ratio of the total mass of the calcium phosphosilicate and the calcium sodium phosphosilicate to the mass of the oranoft is 1:0.03-0.

2.

8. The toothpaste according to claim 2, characterized in that, The toothpaste matrix components include glycerol, sodium lauroyl sarcosinate, carbomer.

9. The toothpaste according to claim 8, characterized in that, By mass fraction, it includes the following raw material components: 0-15% calcium phosphosilicate, 0-10% calcium sodium phosphosilicate, 2-8% porous silica, 2-20% polyethylene glycol, 0.05-0.36% sodium fluoride, 0.05-1.6% oranoft, 20-30% hydrated silica, 30-42% glycerol, 0.5-1.5% sodium lauroyl sarcosinate, 0.5-1.5% carbomer; and the total proportion m of calcium phosphosilicate and calcium sodium phosphosilicate in the toothpaste satisfies: 3% ≤ m ≤ 15%.

10. A method for preparing the toothpaste according to claim 1, characterized in that, It includes the following steps, by mass percentage: (1) Dissolve polyethylene glycol, 0.05-1.6% oranoft and 0.05-0.36% sodium fluoride in water, then add 2-8% porous silica, and obtain fluoride-loaded porous silica after drying. (2) Mix 20-30% hydrated silica, 0-15% calcium phosphosilicate and 0-10% calcium sodium phosphosilicate, and disperse evenly to obtain a mixed material. (3) Stir 0.5-1.5% carbomer, the remaining polyethylene glycol and 30-42% glycerol evenly, and inject them into a container. (4) Then add the mixed material prepared in step (2) into the container, stir, and then add sodium lauroyl sarcosinate and stir. (5) Then add the fluoride-loaded porous silica prepared in step (1), stir under vacuum, and defoam to obtain the toothpaste product. The stirring speed is 1000-3000 r / min, and the time is 20-40 min. In step (1), the mass ratio of the total mass of the oranoft and the sodium fluoride to the mass of the polyethylene glycol is 1:0.5-2; the mass ratio of the total mass of the oranoft and the sodium fluoride to the mass of the water is 1:5-10.

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