Nano calcium polyphosphate-containing toothpaste with repairing effect and preparation method thereof

Abstract

The invention discloses nano calcium polyphosphate-containing toothpaste with a repairing effect and a preparation method of the nano calcium polyphosphate-containing toothpaste. The toothpaste is prepared from the following components in percentage by mass: 5 to 15 percent of water, 55 to 75 percent of a polyol humectant, 0.2 to 1 percent of sodium carboxymethyl cellulose, 2 to 8 percent of sodium lauryl sulfate, 15 to 20 percent of silicon dioxide, 0.01 to 0.4 percent of menthol, 0.01 to 0.07 percent of a preservative and 0.01 to 0.1 percent of nano calcium polyphosphate. The nano calcium polyphosphate is introduced into a toothpaste system, and the nano calcium polyphosphate can be effectively attached to and actively repair microscopic defects on the enamel surface by utilizing the high specific surface activity and biomimetic mineralization characteristics of the nano calcium polyphosphate. The toothpaste not only has a conventional cleaning function, but also can remarkably reduce tooth surface roughness, recover microhardness and relieve dentin sensitivity, daily active repair of tooth hard tissue is achieved, and the defect of existing toothpaste in the aspect of direct structural repair is overcome.

Description

Technical Field

[0001] This invention relates to the field of oral care products technology, and in particular to a toothpaste containing nano-polyphosphate calcium with repairing effects and its preparation method. Background Technology

[0002] As a non-regenerative hard tissue organ, the health and long-term maintenance of teeth are the core goals of oral medicine and daily care. Once permanent teeth erupt, they accompany a person throughout their life, facing various irreversible risks of damage, including chewing wear, acid erosion, and the effects of bacterial metabolic products. Therefore, in addition to therapeutic interventions, daily prevention and restorative care are particularly important.

[0003] Toothpaste, as the most widely used and frequently used oral care medium, has evolved from its early function of simple cleaning to a comprehensive care platform with multiple effects such as anti-caries, anti-sensitivity, antibacterial, anti-inflammatory, and whitening. This evolution mainly relies on the introduction of specific functional ingredients: for example, the widespread use of fluoride (such as sodium fluoride and sodium monofluorophosphate) significantly reduces the incidence of tooth decay by promoting enamel remineralization; potassium nitrate and strontium chloride relieve tooth sensitivity by blocking dentinal tubules or inhibiting nerve signals; triclosan and zinc citrate act as antibacterial agents to help control plaque and gingival inflammation; in addition, the combination of various abrasives (such as silica and calcium carbonate) and surfactants (such as sodium lauryl sulfate) ensures basic cleaning efficacy. Although current toothpaste technology has achieved significant results in the above areas, its ability to actively repair and strengthen the microscopic defects in tooth hard tissue (mainly composed of hydroxyapatite) caused by physical wear or acid etching still has significant shortcomings. Summary of the Invention

[0004] To address the aforementioned problems, this invention proposes a toothpaste containing nano-polyphosphate calcium with repairing effects and its preparation method. This invention solves the problem that existing toothpastes lack the function of repairing microscopic defects in teeth.

[0005] This invention can be achieved through the following technical solutions: A toothpaste with repairing effects containing nano-polyphosphate comprises the following percentages by weight: water 5-15%, polyol humectant 55-75%, sodium carboxymethyl cellulose 0.2-1%, sodium lauryl sulfate 2-8%, silica 15-20%, peppermint flavor 0.01-0.4%, preservative 0.01-0.07%, and nano-polyphosphate 0.01-0.1%.

[0006] Preferably, the polyol moisturizer is one or more of sorbitol, glycerin, and xylitol.

[0007] Preferably, the preservative is one or more of 1,2-hexanediol, 1,2-pentanediol, p-hydroxyacetophenone, phenoxyethanol, and ethylhexylglycerin.

[0008] A method for preparing a toothpaste with repairing effects containing nano-sized calcium polyphosphate includes the following steps: Step 1: Add water, polyol humectant, and sodium carboxymethyl cellulose to an emulsifying pot and stir until homogeneous. Heat the mixture to 50-55℃. Step 2: Turn on the vacuum, add silica under homogenization, keep warm and stir at 50-55℃, then add sodium lauryl sulfate, cool down to 40℃, add peppermint flavor, preservative, and nano-polyphosphate, stir evenly, and cool to room temperature to obtain toothpaste with repairing effects containing nano-polyphosphate.

[0009] Preferably, the stirring speed in step 1 is 1000-3000 rpm and the time is 10-30 min.

[0010] Preferably, the time for heat preservation and stirring in step 2 is 20-40 minutes.

[0011] Preferably, the cooling rate in step 2 is 1-3℃ / min.

[0012] Preferably, the cooling in step 2 is achieved through a circulating water cooling system.

[0013] Preferably, the stirring speed is 500-1500 rpm.

[0014] Preferably, step 2 is carried out entirely under a vacuum of -0.05 to -0.09 MPa.

[0015] The beneficial effects of this invention are: This invention introduces nano-sized calcium polyphosphate as the core active ingredient into a traditional toothpaste matrix, resulting in a novel toothpaste capable of actively repairing microscopic defects in tooth hard tissues. Utilizing the high specific surface area and strong surface activity of nanoparticles, this toothpaste can tightly adhere to the enamel surface and the interior of micro-defects, effectively inducing a biomimetic mineralization process. This achieves structural repair at the microscopic level of the tooth, from "internal filling" to "surface reconstruction." Performance tests simulating clinical use have verified that after 28 days of use, this toothpaste significantly reduces the surface roughness of early demineralized areas (reduction rate exceeding 85%), restores microhardness by over 80%, and effectively reduces dentinal tubule permeability (reduction rate approximately 75%), thereby simultaneously achieving tooth surface smoothing, structural strengthening, and improved sensitivity. Compared to control toothpastes that do not contain this ingredient, comparative products that use similar micron-sized materials, or products that contain only conventional fluoride, this invention demonstrates significant advantages in repair efficiency, depth of action, and comprehensive functionality. It effectively addresses the shortcomings of existing toothpastes in directly repairing tooth wear and provides an innovative solution for daily oral care that combines cleaning and active repair capabilities. Attached Figure Description

[0016] The accompanying drawings are provided to further illustrate the invention and form part of the specification. They are used in conjunction with embodiments of the invention to explain the invention and do not constitute a limitation thereof. In the drawings: Figure 1 These are the performance test results for the toothpaste. Detailed Implementation

[0017] The following provides a detailed description of the embodiments of the present invention: These embodiments are implemented based on the technical solution of the present invention, and provide detailed implementation methods and processes. However, the scope of protection of the present invention is not limited to the following embodiments. Experimental methods in the following embodiments that do not specify specific conditions are generally performed under conventional conditions.

[0018] Example 1 A toothpaste with repairing properties containing nano-polyphosphate comprises the following percentages by weight: 12.3% water, 65% sorbitol, 0.4% sodium carboxymethyl cellulose, 4% sodium lauryl sulfate, 18% silica, 0.15% peppermint flavor, 0.05% 1,2-pentanediol, and 0.1% nano-polyphosphate.

[0019] This embodiment describes a method for preparing a toothpaste with repairing effects containing nano-sized calcium polyphosphate, comprising the following steps: Step 1: Add water, sorbitol, and sodium carboxymethyl cellulose to an emulsifying pot, stir and homogenize at 3000 rpm for 20 minutes, and heat to 55°C. Step 2: Maintain a vacuum of -0.09 MPa, add silica under homogenization, keep warm at 50°C and stir for 30 minutes, then add sodium lauryl sulfate, and cool to 40°C at a rate of 1°C / min using a circulating water cooling system. Add peppermint flavor, 1,2-pentanediol, and nano-polyphosphate, and stir evenly at 1500 rpm. Cool to room temperature to obtain a toothpaste with repairing effects containing nano-polyphosphate.

[0020] Example 2 A toothpaste with repairing properties containing nano-polyphosphate comprises the following percentages by weight: 5% water, 55% glycerin, 0.2% sodium carboxymethyl cellulose, 2% sodium lauryl sulfate, 15% silica, 0.01% peppermint flavor, 0.01% 1,2-hexanediol, and 0.01% nano-polyphosphate.

[0021] This embodiment describes a method for preparing a toothpaste with repairing effects containing nano-sized calcium polyphosphate, comprising the following steps: Step 1: Add water, glycerin, and sodium carboxymethyl cellulose to an emulsifying pot, stir at 1000 rpm for 10 minutes to homogenize, and heat to 50°C. Step 2: Maintain a vacuum of -0.05 MPa, add silica under homogenization, keep warm at 50°C and stir for 40 min, then add sodium lauryl sulfate, and cool to 40°C at a cooling rate of 1-3°C / min using a circulating water cooling system. Add peppermint flavor, 1,2-hexanediol, and nano-polyphosphate, and stir evenly at 500 rpm. Cool to room temperature to obtain a toothpaste with repairing effects containing nano-polyphosphate.

[0022] Example 3 A toothpaste with repairing properties containing nano-polyphosphate comprises the following percentages by weight: 10% water, 65% xylitol, 0.6% sodium carboxymethyl cellulose, 5% sodium lauryl sulfate, 17.5% silica, 0.2% peppermint flavor, 0.04% p-hydroxyacetophenone, and 0.05% nano-polyphosphate.

[0023] This embodiment describes a method for preparing a toothpaste with repairing effects containing nano-sized calcium polyphosphate, comprising the following steps: Step 1: Add water, xylitol, and sodium carboxymethyl cellulose to an emulsifying pot, stir and homogenize at 2000 rpm for 20 minutes, and heat to 50°C. Step 2: Maintain a vacuum of -0.05 MPa, add silica under homogenization, keep warm at 50°C and stir for 30 minutes, then add sodium lauryl sulfate, and cool to 40°C at a rate of 2°C / min using a circulating water cooling system. Add peppermint flavor, p-hydroxyacetophenone, and nano-polyphosphate, and stir evenly at 1000 rpm. Cool to room temperature to obtain a toothpaste with repairing effects containing nano-polyphosphate.

[0024] Example 4 A toothpaste with repairing properties containing nano-polyphosphate comprises the following percentages by weight: 15% water, 75% sorbitol, 1% sodium carboxymethyl cellulose, 8% sodium lauryl sulfate, 20% silica, 0.4% peppermint flavor, 0.07% phenoxyethanol, and 0.1% nano-polyphosphate.

[0025] This embodiment describes a method for preparing a toothpaste with repairing effects containing nano-sized calcium polyphosphate, comprising the following steps: Step 1: Add water, sorbitol, and sodium carboxymethyl cellulose to an emulsifying pot, stir and homogenize at 3000 rpm for 30 minutes, and heat to 55°C. Step 2: Maintain a vacuum of -0.09 MPa, add silica under homogenization, keep warm at 55°C and stir for 20 minutes, then add sodium lauryl sulfate, and cool to 40°C at a rate of 3°C / min using a circulating water cooling system. Add peppermint flavor, phenoxyethanol, and nano-polyphosphate, and stir evenly at 1500 rpm. Cool to room temperature to obtain a toothpaste with repairing effects containing nano-polyphosphate.

[0026] Comparative Example 1: The difference between this comparative example and Example 1 is that no nano-polyphosphate calcium is added.

[0027] A toothpaste with repairing properties comprises the following percentages by weight: 12.3% water, 65% sorbitol, 0.4% sodium carboxymethyl cellulose, 4% sodium lauryl sulfate, 18% silica, 0.15% peppermint flavor, and 0.05% 1,2-pentanediol.

[0028] The preparation method of a toothpaste with repairing effects in this comparative example includes the following steps: Step 1: Add water, sorbitol, and sodium carboxymethyl cellulose to an emulsifying pot, stir and homogenize at 3000 rpm for 20 minutes, and heat to 55°C. Step 2: Maintain a vacuum of -0.09 MPa, add silica under homogenization, keep warm at 50°C and stir for 30 minutes, then add sodium lauryl sulfate, cool to 40°C at a rate of 1°C / min using a circulating water cooling system, add peppermint flavor and 1,2-pentanediol, stir evenly at 1500 rpm, and cool to room temperature to obtain toothpaste with repairing effects.

[0029] Comparative Example 2: The difference between this comparative example and Example 1 is that micron-sized calcium polyphosphate is used instead of nano-sized calcium polyphosphate.

[0030] A toothpaste with repairing properties comprises the following percentages by weight: 12.3% water, 65% sorbitol, 0.4% sodium carboxymethyl cellulose, 4% sodium lauryl sulfate, 18% silica, 0.15% peppermint flavor, 0.05% 1,2-pentanediol, and 0.1% micron-sized calcium polyphosphate.

[0031] The preparation method of a toothpaste with repairing effects in this comparative example includes the following steps: Step 1: Add water, sorbitol, and sodium carboxymethyl cellulose to an emulsifying pot, stir and homogenize at 3000 rpm for 20 minutes, and heat to 55°C. Step 2: Maintain a vacuum of -0.09 MPa, add silica under homogenization, keep warm at 50°C and stir for 30 minutes, then add sodium lauryl sulfate, and cool to 40°C at a rate of 1°C / min using a circulating water cooling system. Add peppermint flavor, 1,2-pentanediol, and micron-sized calcium polyphosphate, and stir evenly at 1500 rpm. Cool to room temperature to obtain toothpaste with repairing effects.

[0032] Comparative Example 3: The difference between this comparative example and Example 1 is that sodium fluoride is used instead of nano-polyphosphate calcium.

[0033] A toothpaste with repairing properties comprises the following percentages by weight: 12.3% water, 65% sorbitol, 0.4% sodium carboxymethyl cellulose, 4% sodium lauryl sulfate, 18% silica, 0.15% peppermint flavor, 0.05% 1,2-pentanediol, and 0.1% sodium fluoride.

[0034] The preparation method of a toothpaste with repairing effects in this comparative example includes the following steps: Step 1: Add water, sorbitol, and sodium carboxymethyl cellulose to an emulsifying pot, stir and homogenize at 3000 rpm for 20 minutes, and heat to 55°C. Step 2: Maintain a vacuum of -0.09 MPa, add silica under homogenization, keep warm at 50°C and stir for 30 minutes, then add sodium lauryl sulfate, and cool to 40°C at a rate of 1°C / min using a circulating water cooling system. Add peppermint flavor, 1,2-pentanediol and sodium fluoride, stir evenly at 1500 rpm, and cool to room temperature to obtain toothpaste with repairing effects.

[0035] Performance testing Test sample preparation: Purchase legally sourced human tooth samples from a biosample company, including caries-free and crack-free human premolars or third molars. Remove soft tissue and store in a 0.1% thymol solution for later use. Create a standardized early demineralization / micro-defect area in the buccal enamel region of each tooth by etching with 37% phosphoric acid for 30 seconds, simulating the initial stage of daily wear or acid etching.

[0036] Simulated brushing treatment: The toothpaste prepared according to this invention was mixed with artificial saliva at a weight ratio of 1:3 to form a slurry. Using an automated brushing simulator, the samples were treated twice a day for 2 minutes each time at standard pressure (200g) and frequency, simulating usage cycles of 14 and 28 days. Between treatments, the samples were soaked in fresh artificial saliva.

[0037] 1 Surface micromorphology repair rate After creating the artificial defect and before any treatment, a three-dimensional scan of the defect area was performed using a laser confocal microscope to obtain the initial surface morphology and calculate the initial arithmetic mean surface roughness Sa0. After the simulated brushing cycle ended on day 14 and day 28, the sample was thoroughly cleaned, and the same defect area was scanned three-dimensionally again to calculate the post-treatment surface roughness Sa14 and Sa28. The roughness reduction rate (%) = [(Sa0-Sa14) / Sa0] × 100%. The larger this value, the smoother and flatter the surface, and the better the repair effect.

[0038] 2 Surface microhardness recovery rate Initial microhardness (HV0 healthy, HV0 defective) was measured in the healthy enamel area adjacent to the defective area and at the center of the defect, respectively. On days 14 and 28, post-treatment microhardness (HV14, HV28) was measured near the same location in the defective area. The hardness recovery rate (%) was calculated as: [(HV14 - HV0 defective) / (HV0 healthy - HV0 defective)] × 100%.

[0039] 3. Dentin hypersensitivity simulation relief Selected teeth were subjected to partial enamel abrasion to expose dentin. Acid etching was used to open the dentinal tubules, establishing a sensitivity model. The samples were placed in a hydrodynamic apparatus under a fixed pressure (20 cm H2O), and the fluid flow rate (F0) through the dentin sheet was measured. Higher flow rates indicate greater tubular opening and increased sensitivity. The samples underwent the same 14-day / 28-day simulated brushing treatment. After treatment, the fluid flow rate was measured again under the same pressure (F14, F28). The permeability reduction rate (%) was calculated as [(F0-F14) / F0]×100%. A higher value indicates a better effect of the toothpaste in sealing the dentinal tubules and a stronger anti-sensitivity potential.

[0040] Table 1 Performance Test Data

[0041] Note: The testing period is 28 days.

[0042] Table 1 shows that after 28 days of use, the toothpastes prepared in Examples 1-4 resulted in smoother tooth surfaces (surface roughness reduction rate between 70.2% and 87.3%), enhanced structure (hardness recovery rate as high as 84.7%), and physical sealing (permeability reduction rate ≥ 65.4%). This is mainly because all examples contain nano-sized calcium polyphosphate. The nanoparticles, with their high specific surface area and surface activity, can adhere tightly to the tooth surface and, as the core of biomimetic mineralization, directly guide the deposition of hydroxyapatite at the defect site, achieving active repair from "internal filling" to "surface reconstruction." In contrast, Comparative Example 1 lacks core repair components and has no active repair capability. The micron-sized particles used in Comparative Example 2 cannot fully utilize the penetration and efficient mineralization advantages of nanomaterials, resulting in a significant reduction in repair efficiency. Comparative Example 3, using sodium fluoride, lacks the ability to directly repair structural defects and rapidly seal, failing to meet the need for "repairing" existing wear.

[0043] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A toothpaste containing nano-sized calcium polyphosphate with repairing effects, characterized in that, It includes the following percentages by weight: water 5-15%, polyol humectant 55-75%, sodium carboxymethyl cellulose 0.2-1%, sodium lauryl sulfate 2-8%, silica 15-20%, peppermint flavor 0.01-0.4%, preservative 0.01-0.07%, and nano-polyphosphate calcium 0.01-0.1%.

2. The toothpaste with repairing effects containing nano-sized calcium polyphosphate according to claim 1, characterized in that, The polyol moisturizer is one or more of sorbitol, glycerin, and xylitol.

3. The toothpaste with repairing effects containing nano-sized calcium polyphosphate according to claim 1, characterized in that, The preservative is one or more of 1,2-hexanediol, 1,2-pentanediol, p-hydroxyacetophenone, phenoxyethanol, and ethylhexylglycerin.

4. The toothpaste with repairing effects containing nano-sized calcium polyphosphate according to claim 1, characterized in that, The method for preparing the toothpaste with repairing effects containing nano-sized calcium polyphosphate includes the following steps: Step 1: Add water, polyol humectant, and sodium carboxymethyl cellulose to an emulsifying pot and stir until homogeneous. Heat the mixture to 50-55℃. Step 2: Turn on the vacuum, add silica under homogenization, keep warm and stir at 50-55℃, then add sodium lauryl sulfate, cool down to 40℃, add peppermint flavor, preservative, and nano-polyphosphate, stir evenly, and cool to room temperature to obtain toothpaste with repairing effects containing nano-polyphosphate.

5. The method for preparing toothpaste with repairing effects containing nano-sized calcium polyphosphate according to claim 4, characterized in that, In step 1, the stirring speed for homogenization is 1000-3000 rpm, and the time is 10-30 min.

6. The method for preparing toothpaste with repairing effects containing nano-sized calcium polyphosphate according to claim 4, characterized in that, The time for heat preservation and stirring in step 2 is 20-40 minutes.

7. The method for preparing toothpaste with repairing effects containing nano-sized calcium polyphosphate according to claim 4, characterized in that, The cooling rate in step 2 is 1-3℃ / min.

8. The method for preparing toothpaste with repairing effects containing nano-sized calcium polyphosphate according to claim 4, characterized in that, In step 2, the cooling is achieved through a circulating water cooling system.

9. The method for preparing toothpaste with repairing effects containing nano-sized calcium polyphosphate according to claim 4, characterized in that, The stirring speed is 500-1500 rpm.

10. The method for preparing toothpaste with repairing effects containing nano-sized calcium polyphosphate according to claim 4, characterized in that, Step 2 is carried out entirely under a vacuum of -0.05 to -0.09 MPa.

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