Enamel repairing toothpaste and preparation method thereof

Abstract

The invention provides tooth enamel repairing toothpaste and a preparation method thereof, and the tooth enamel repairing toothpaste comprises the following components in percentage by mass: 15-30% of glycerol, 15-30% of glycerol, 5-10% of sodium dodecyl sulfate, 5-10% of sodium dodecyl sulfate, 5-10% of sodium dodecyl sulfate and the balance of deionized water. 10%-25% of hydrated silica; 3%-10% of polyethylene glycol-8; 3%-7% of calcium phosphosilicate; 1%-5% of a surfactant; 0.5%-3% of a binder; 0.05%-0.5% of an antibacterial agent; 0.1%-1.5% of a compound enzyme; the compound enzyme comprises lysozyme, papain and bromelain; the mass ratio of the lysozyme to the papain to the bromelain is 1: (0.4-0.6): (0.4-0.6); and the balance of water. The toothpaste can be used for remarkably improving the repairing effect of enamel and the oral health maintenance capability.

Description

Technical Field

[0001] The present application relates to the technical field of daily necessities, and in particular to an enamel repairing toothpaste and a preparation method thereof. Background Art

[0002] Tooth enamel, the hardest tissue in the human body, covers the surface of tooth crowns and is primarily composed of hydroxyapatite crystals. It plays an important role in protecting dentin and resisting chemical and mechanical erosion. However, due to long-term exposure to factors such as acidic substances, plaque, and mechanical wear in the oral environment, tooth enamel is prone to demineralization, surface roughness, and even microcracks, leading to tooth sensitivity, reduced aesthetics, and an increased risk of caries.

[0003] To address the issue of enamel damage, some toothpaste products have introduced remineralizing materials (such as calcium phosphate and bioactive glass) to promote the redeposition of hydroxyapatite, thereby achieving initial repair of enamel. However, existing repair toothpaste technologies generally have the following shortcomings: Limited remineralization capacity: Traditional calcium phosphate ingredients have poor stability in the weak acid environment of the oral cavity, making it difficult to continuously release effective calcium and phosphorus ions, and the crystal deposition efficiency is low, resulting in a loose structure of the repair layer and the inability to form a dense, continuous protective barrier.

[0004] Insufficient antibacterial and acid-resistant capabilities: Although some products have certain repair capabilities, they do not have effective antibacterial or buffering functions at the same time, making it difficult to inhibit the reproduction of caries-causing bacteria and sugar and acid attacks. The repaired area is easily damaged again, affecting the long-term use effect.

[0005] Insufficient consideration of dentin sensitivity: Enamel damage is often accompanied by dentin exposure. If there is a lack of sealing and protection of the dentinal tubules, it is easy to cause discomfort caused by sensitivity to cold and heat. Most repair toothpastes fail to effectively seal the tubules or form a stable sealing layer, resulting in insignificant anti-sensitivity effect.

[0006] Poor synergy of functional ingredients: Existing products mostly use single or two types of functional components, lack of synergistic design between ingredients, and it is difficult to achieve a balance between repair, antibacterial, whitening and comfortable experience, resulting in unsatisfactory comprehensive oral care effects.

[0007] Oral compatibility and safety issues: Some highly effective ingredients may cause oral irritation or lead to adverse experiences such as residual odor and dry mouth during long-term use. There is a lack of systematic optimization for oral mucosa friendliness and sensory acceptance.

[0008] In summary, existing enamel repair toothpastes still have obvious shortcomings in structural repair efficiency, plaque control and sensitivity protection. There is an urgent need for a technical solution that can synergistically improve the effectiveness of oral health protection in multiple dimensions. Summary of the Invention

[0009] This application provides an enamel repair toothpaste and its preparation method, aiming to solve the problems existing in existing repair toothpastes, such as low remineralization efficiency, poor acid resistance, insufficient dentinal tubule sealing, and difficulty in balancing antibacterial and sensory effects. By optimizing the formula system and the combination of functional ingredients, the toothpaste provided in this application not only enhances the enamel remineralization effect, but also has good dentin sealing ability, sugar and acid resistance, and oral adaptability, thereby achieving multi-dimensional protection and comfortable care for teeth, and is suitable for daily oral health maintenance and long-term use by people with sensitive teeth.

[0010] In the first aspect, the present application provides an enamel repair toothpaste, which includes the following components, calculated by mass percentage: glycerin: 15%~30%; hydrated silica: 10%~25%; polyethylene glycol-8: 3%~10%; calcium phosphosilicate: 3%~7%; surfactant: 1%~5%; binder: 0.5%~3%; antibacterial agent: 0.05%~0.5%; complex enzyme: 0.1%~1.5%; the complex enzyme includes lysozyme, papain and bromelain; the mass ratio of lysozyme, papain and bromelain is 1:(0.4~0.6):(0.4~0.6); the balance is water.

[0011] According to this application, through the scientific combination and synergistic compatibility of the above-mentioned functional components, toothpaste can achieve efficient enamel remineralization, plaque biofilm degradation, continuous tooth surface cleaning and protein pollution inhibition, thereby significantly improving the enamel repair effect and oral health maintenance ability.

[0012] Specifically, calcium phosphosilicate as the core inorganic repair component can continuously release Ca in the weak acid or neutral environment of the oral cavity. 2+ With PO4 3- ions, and release Si-OH groups during the hydrolysis process, silanol condensation forms a negatively charged SiO2-rich porous colloidal layer, Ca in body fluids 2+ With PO4 3- Migrate and accumulate on the surface of the silica gel layer to form an amorphous CaO-P205 layer, which reacts with OH in the body fluid. - and CO3 2- Calcium ions combine to form carbonated hydroxyapatite crystals, which are deposited on the enamel surface and promote remineralization of demineralized enamel. Calcium ions also promote thrombin production, accelerating wound healing and hemostasis, and increase fibroblast proliferation and collagen fiber network contraction. Phosphate ions can upregulate pro-angiogenic genes, such as vascular endothelial growth factor α, and promote the expression of basic fibroblast growth factor. Silicate ions can stimulate type I collagen formation by downregulating transforming growth factor-β, inhibiting fibroblast differentiation into myofibroblasts and excessive collagen deposition, thereby inhibiting scar formation.

[0013] The complex enzyme system uses a combination of lysozyme, papain, and bromelain, and is optimized with a mass ratio of 1:(0.4-0.6):(0.4-0.6) to achieve the best spatial distribution of each enzyme function in the target area and the synergistic degradation ability: Lysozyme, as the main enzyme, accounts for the largest proportion in this ratio. Its ability to specifically lyse the cell walls of Gram-positive bacteria enables it to quickly weaken the stability of the plaque structure and create a permeable environment for the action of proteases.

[0014] The introduction of papain and bromelain is used to synergistically hydrolyze adhesion proteins, glycoproteins and membrane proteins in the plaque matrix. The former tends to act on non-polar hydrophobic regions, while the latter has a stronger degradation ability for polar hydrophilic structures. The two work together to achieve more comprehensive extracellular polymer degradation and plaque peeling.

[0015] The above-mentioned ratio design can prevent the problem of incomplete clearance caused by insufficient degradation efficiency of a single protease or biased hydrolysis, while reducing irritation to the oral mucosa and improving the biological adaptability of the system.

[0016] There is a clear structural synergistic effect between the complex enzyme system and calcium phosphosilicate: the complex enzyme degrades the tooth surface biofilm, destroys the bacterial aggregation structure and removes protein pollutants, which significantly enhances the adsorption capacity of calcium phosphosilicate particles on the exposed area of ​​the tooth surface, which is conducive to the enrichment of inorganic ions and the directional deposition of crystal nuclei, and improves the starting rate of the remineralization reaction and the uniformity of the crystals. At the same time, the residual small molecular peptide chains and polypeptide ions released after the complex enzyme degradation can further react with Ca 2+ Form a weak coordination structure, enhancing Ca 2+ The local retention time on the tooth surface creates a "soft template" effect, thereby assisting in the orderly and dense deposition of calcium phosphate. Furthermore, lysozyme can reduce the acidic metabolic burden of Streptococcus mutans, indirectly reducing the surface dissolution rate of calcium phosphosilicate, prolonging its mineral release period, and enhancing the sustainability of the repair.

[0017] Glycerin and polyethylene glycol-8 together form a moisturizing and dispersing system. Glycerin maintains the paste's water activity, preventing premature deposition and ineffectiveness of the mineral components. Polyethylene glycol-8, with its excellent water solubility and low interfacial tension, effectively disperses and stabilizes the calcium phosphosilicate particles, enhancing their accessibility and effective area on the tooth surface. Simultaneously, these two factors regulate the paste's fluidity and adhesion, ensuring even distribution and coverage of the tooth surface microstructure during use, facilitating the full mineralization reaction.

[0018] Surfactants are used to assist in removing organic film, food debris, and initial plaque from the tooth surface, exposing a clean enamel surface and enhancing the adsorption and deposition efficiency of calcium and phosphate ions. Their moderate foaming ability also aids in the diffusion and retention of complex enzymes within the oral cavity, allowing proteolytic enzymes to more fully contact and decompose the structural proteins and extracellular polymeric matrix in dental plaque.

[0019] Binders enhance the adhesion of the active ingredients in the paste (including calcium phosphosilicate and enzyme complex) to the tooth surface, slowing their scouring and dilution by saliva, thereby prolonging the effective duration of mineral release and enzyme reaction. Furthermore, binders form a three-dimensional gel network with glycerin and surfactants, maintaining a stable distribution of the paste.

[0020] Antibacterial agents are used to quickly inhibit the cariogenic bacteria in the oral cavity, mainly Streptococcus mutans, block their acid production metabolism process, and slow down the acid erosion process of the enamel surface.

[0021] In summary, the toothpaste provided in this application establishes a five-in-one functional system of cleaning-nucleation-deposition-curing-antibacterial through the organic integration of a complex enzyme system, an inorganic remineralization system and auxiliary functional components, thereby effectively repairing damaged enamel in daily oral environment, improving tooth surface tolerance and structural stability, and having significant oral protection and clinical promotion value.

[0022] In some embodiments, the surfactant includes sodium lauroyl sarcosinate and sodium methyl lauroyl taurate, and the mass ratio of sodium lauroyl sarcosinate to sodium methyl lauroyl taurate is 1:1-2.

[0023] In some of the aforementioned embodiments, sodium lauroyl sarcosinate is a highly hydrophilic amphoteric surfactant with excellent foaming and mildness, effectively reducing oral interfacial tension and promoting the uniform spreading of the enzyme complex and calcium phosphosilicate on the tooth surface. Sodium methyl lauroyl taurate, on the other hand, exhibits high lipophilicity and adhesion, facilitating the adsorption and retention of active ingredients on the tooth surface and exposed dentin. Combining these two in a 1:1-2 ratio creates a complementary hydrophilic-lipophilic structure, enhancing the toothpaste system's interfacial control capabilities and oral residual efficiency without compromising overall mildness.

[0024] Therefore, the above surfactant combination can improve the bioavailability and repair efficiency of the composite active substance, so that the enamel repair toothpaste has a better repair effect on the enamel.

[0025] In some embodiments, the binder comprises polyvinyl pyrrolidone, and the weight average molecular weight of the polyvinyl pyrrolidone is 40,000-60,000.

[0026] In some of the above embodiments, polyvinylpyrrolidone (PVP), as a hydrophilic nonionic polymer, can play multiple roles in the toothpaste system. On the one hand, its good film-forming property and molecular embedding ability can enhance the dispersion stability and sustained release of active ingredients such as complex enzymes and calcium phosphosilicate in the paste, inhibiting the loss of enzyme activity or the aggregation of mineral particles; on the other hand, the highly polar amide structure in its molecular chain can react with Ca 2+ , protein fragments, amino acids, etc. to form weak bonds, helping the active ingredients to form a lasting action interface on the tooth surface, thereby increasing their local residence time and bioavailability.

[0027] When the weight-average molecular weight of PVP is controlled within the range of 40,000-60,000, it can provide sufficient molecular chain entanglement and sustained release while avoiding the problems of increased viscosity, sticky mouthfeel, or decreased compatibility stability caused by excessive molecular weight. Compared to low-molecular-weight PVP (e.g., molecular weight <30,000), which is easily soluble but has poor film-forming ability and weak water washability, the preferred molecular weight range in this application can enhance the retention of active ingredients while maintaining good paste rheology and user comfort.

[0028] Therefore, through the use of PVP with appropriate molecular weight, not only can the stability of the paste and the synergistic release of key functional substances be improved, but the adhesion bridging ability in the complex enzyme-calcium phosphosilicate action chain can also be further strengthened, thereby enhancing the sustainability and effectiveness of the enamel repair effect.

[0029] In some embodiments, the antimicrobial agent comprises cetylpyridinium chloride.

[0030] In some of the aforementioned embodiments, cetylpyridinium chloride is a broad-spectrum cationic quaternary ammonium salt antibacterial agent that rapidly kills Gram-positive and some Gram-negative bacteria by disrupting bacterial cell membrane structure, altering membrane potential and permeability, and exhibiting a potent inhibitory effect against common oral cariogenic and inflammatory strains such as Streptococcus mutans and Porphyromonas gingivalis. Its cationic nature allows it to bind to negatively charged dental plaque and oral mucosal surfaces, prolonging their retention time in the oral cavity and thereby enhancing their bactericidal efficiency and persistence.

[0031] More importantly, cetylpyridinium chloride, as a low-irritation antibacterial agent, does not inhibit the activity of proteases and lysozymes when it exists in synergy with the complex enzyme system, and does not cause obvious burning or bitterness in the mouth. It is superior to certain metal ion or alcohol antibacterial ingredients. It can ensure the efficiency of enamel repair while reducing oral discomfort and improving compliance with use.

[0032] Therefore, by introducing cetylpyridinium chloride as the antibacterial component of the toothpaste of this application, it can not only effectively control oral pathogenic bacteria and prevent secondary caries or gingivitis, but also synergize with the complex enzyme-mineral repair pathway to enhance the stability of the oral microecology and create a cleaner, low-inflammatory environment for the repair and protection of tooth enamel.

[0033] In some embodiments, the present invention further comprises: 0.01% to 0.0.5% sweetener, wherein the sweetener comprises galactose.

[0034] In some of the aforementioned embodiments, galactose is a high-intensity, non-nutritive sweetener with a sweetness approximately 400 to 800 times that of sucrose. Even at very low addition levels, it can impart a pleasant sweetness experience to toothpaste. Compared to traditional sweeteners (such as sodium saccharin and aspartame), which can be bitter, irritating, or thermally unstable, galactose exhibits excellent stability and broad pH adaptability in aqueous systems, making it particularly suitable for use in enzyme systems and weakly acidic environments.

[0035] Its high sweetness and low dosage properties can avoid interfering with the rheological and foaming properties of the paste, while also providing a metabolizable carbon source for oral microorganisms, which helps maintain an antibacterial environment. Its combination with active ingredients such as the complex enzyme and calcium phosphosilicate in this application can not only mask the potential medicinal or astringent taste of the active ingredients, enhancing the user experience of the product, but also strengthen consumer acceptance and compliance.

[0036] Therefore, trichlorogalactose is the preferred sweetener. While improving the overall taste and usage experience of toothpaste, it does not interfere with the stability and biological functions of the active ingredients and can promote the effectiveness of enamel repair toothpaste.

[0037] In some embodiments, the present invention further comprises: 0.1% to 0.3% of a cooling agent, wherein the cooling agent comprises menthane carboxamide.

[0038] In some of the aforementioned embodiments, menthane carboxamide, as a mild, long-lasting cooling agent, possesses excellent lipophilicity and biocompatibility. Its molecular structure activates cooling receptors in the mouth, producing a refreshing, long-lasting, and non-irritating cooling sensation. Compared to traditional cooling agents such as L-menthol and menthol, menthane carboxamide is less irritating and provides a longer cooling effect, making it particularly suitable for complex enzyme and sensitivity-repair toothpaste systems.

[0039] In the toothpaste provided herein, menthane carboxamide not only alleviates the slight bitterness and astringency that may be caused by functional ingredients such as complex enzymes and mineral salts, but also enhances oral freshness and user comfort. Furthermore, it does not participate in protein denaturation reactions, interfere with protease activity, or weaken the biological function of complex enzymes, thus exhibiting excellent biocompatibility with the overall repair system.

[0040] Therefore, by selecting menthane carboxyethylamide as a cooling agent, not only can the sensory pleasure of the product be enhanced, but also a mild and long-lasting cooling effect can be achieved, which helps to improve the adaptability and daily use frequency of the product in sensitive people, and further promotes the maintenance and enhancement of the enamel repair effect.

[0041] In some embodiments, the present invention further comprises: 0.3% to 1% of a foaming aid, wherein the foaming aid comprises sodium laurate.

[0042] In some of the aforementioned embodiments, sodium laurate is a widely available, stable anionic surfactant with excellent detergency and foam control capabilities. In toothpaste systems, sodium laurate acts as a foaming aid, synergizing with the primary surfactants (sodium lauroyl sarcosinate and sodium methyl lauroyl taurate) to enhance the richness, stability, and diffusivity of the foam, effectively improving the cleaning experience and enhancing the sensory effects. Furthermore, sodium laurate has a relatively simple molecular structure and low irritation potential, making it less likely to overly irritate the oral mucosa, making it particularly suitable for use in toothpaste products designed to treat sensitive skin.

[0043] In the toothpaste provided in this application, the introduction of an appropriate amount of sodium laurate helps to improve the foam's extensibility while maintaining low irritation, and cooperates with the complex enzyme system to strengthen the cleaning of the enamel surface, reduce plaque adhesion, and provide a cleaner base for the mineral repair process.

[0044] Therefore, sodium laurate, as an auxiliary foaming ingredient, improves the foam structure while ensuring a mild formula, enhances the user's smoothness and cleanliness during the brushing process, and can improve the sensory effect of consumers.

[0045] In some embodiments, the present invention further comprises: 0.2% to 0.8% electrolyte salt, wherein the electrolyte salt comprises sodium chloride.

[0046] In some of the above embodiments, sodium chloride, as a common oral electrolyte salt component, can moderately adjust the ionic strength and osmotic pressure of the toothpaste system, help enhance the physiological adaptability of the paste, make it more compatible with the osmotic balance of the oral environment, and reduce irritation to the gums and mucous membranes. It is particularly suitable for sensitive toothpastes containing complex enzymes and active minerals.

[0047] More importantly, an appropriate amount of sodium chloride can optimize the catalytic environment of the complex enzyme. The activity of lysozyme, papain, and bromelain is often dependent on electrolyte concentration. An appropriate salt concentration can stabilize the enzyme's conformation, prolong its activity in the paste, and improve its efficiency in decomposing dental plaque and protein impurities, thereby further supporting the remineralization process of calcium phosphosilicate. Furthermore, sodium chloride can affect the paste's thixotropy and dispersibility, helping to stabilize particle uniformity in aqueous systems and inhibiting paste stratification or water precipitation, thereby ensuring product stability and consistency during storage.

[0048] Therefore, by introducing an appropriate amount of sodium chloride, it is possible to take into account electrolytic regulation, enzyme environment stabilization and system physical stability, and to improve the long-term activity of the enamel repair system.

[0049] In some embodiments, the composition further comprises: 0.5% to 1% of flavor.

[0050] In some of the above embodiments, the flavor can be selected from natural plant extracts, synthetic flavors or a combination of the two, so as to be formulated into a fresh or fruity compound flavor, which is used to improve the odor characteristics of toothpaste and the taste experience when brushing teeth, thereby enhancing consumers' pleasure and long-term acceptance when using it.

[0051] It should be noted that this application does not further limit the type of flavor and may be selected based on actual needs. For example, a refreshing mint flavor whose main ingredients include menthol, peppermint oil, and spearmint oil may be used; a light fruity flavor whose main ingredients include lemon oil, orange oil, geraniol, and ethyl acetate may be used; or an herbal refreshing flavor whose main ingredients include eucalyptus oil, rosemary essential oil, thyme oil, and sage extract may be used. Similarly, the above three flavors may be combined to produce composite flavors with different aromas.

[0052] In a second aspect, the present application provides a method for preparing an enamel repair toothpaste, comprising: Providing components of the enamel repairing toothpaste according to any embodiment of the first aspect; The components are mixed and homogenized, and then degassed to obtain the tooth enamel repairing toothpaste.

[0053] According to the present application, the preparation method comprises sequentially or simultaneously adding glycerin, hydrated silica, polyethylene glycol-8, calcium phosphosilicate, a surfactant, a binder, an antibacterial agent, a complex enzyme, and water, homogenously mixing the mixture under controlled temperature and stirring rate conditions, and subjecting the mixture to vacuum degassing to obtain a finished toothpaste having moderate fluidity, good stability, and a uniform structure. The method is simple, easily scalable, and exhibits good dispersibility and synergy among the components. It can maintain the functionality of the active ingredients while ensuring consistent product appearance and performance, making it suitable for the industrial production of enamel-repairing toothpaste.

[0054] In some embodiments, the method specifically comprises: Put glycerin and part of deionized water into a mixing tank, start stirring at a low speed, add the binder and continue stirring until it is completely dissolved to form a uniform basic colloid system; Under continuous stirring, slowly add hydrated silica and continue stirring to disperse it evenly; then add polyethylene glycol-8 to adjust the viscosity and moisturizing properties of the system; Add calcium phosphosilicate and surfactant in sequence, control the stirring speed to avoid the introduction of bubbles, and fully disperse and homogenize; Add antimicrobial agent, complex enzyme, sweetener, cooling agent, foaming agent, electrolyte salt and flavor at a temperature below 40°C, and add the remaining water.

[0055] The obtained mixed slurry is subjected to vacuum degassing treatment to remove bubbles introduced during the mixing process to obtain a uniform and bubble-free toothpaste paste, which is then transferred to a filling device for quantitative packaging to obtain the finished product.

[0056] Compared with the prior art, the present invention has the following advantages: 1. By synergistically introducing calcium phosphosilicate and complex enzymes (including lysozyme, papain and bromelain) into the toothpaste system, it not only achieves effective repair and remineralization of tooth enamel, but also achieves biodegradation of dental plaque and protein film, significantly improving the overall repair efficiency and oral cleaning effect of toothpaste.

[0057] 2. The components of the complex enzyme are optimized in a mass ratio of 1:(0.4~0.6):(0.4~0.6), taking into account the triple functions of protein dissolution, antibacterial and tooth stain removal, and improving the adaptability and effectiveness of toothpaste on sensitive enamel areas based on a mild formula.

[0058] 3. It is formulated with low-irritation, amino acid and taurine surfactants and their ratio is optimized to effectively improve the fineness and cleaning power of the foam while avoiding potential damage to the mucous membrane and tooth enamel. It is suitable for long-term use by sensitive people.

[0059] 4. The various components in the full formula system work together to create a compound toothpaste product that has both repairing functions and a refreshing and comfortable taste. It has good paste stability, user experience and compatibility with active ingredients, and is suitable for industrial production. DETAILED DESCRIPTION

[0060] The various embodiments or implementation schemes in this specification are described in a progressive manner, and each embodiment focuses on the differences from other embodiments.

[0061] Throughout this specification, reference to terms such as "one embodiment," "some embodiments," "illustrative embodiments," "examples," "specific examples," or "some examples" means that a specific feature, structure, material, or characteristic described in conjunction with an embodiment or example is included in at least one embodiment or example of the present application. In this specification, illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

[0062] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of the technical features being referred to. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of such features. Throughout the description of this application, "plurality" means at least two, for example, two, three, etc., unless otherwise specifically defined.

[0063] In the description of this specification, unless otherwise specified, "parts" refer to "parts by mass".

[0064] Below, the embodiment of the present application is described. The embodiment described below is exemplary and is only used to explain the present application, and is not to be construed as limiting the present application. Where specific techniques or conditions are not specified in the embodiments, the techniques or conditions described in the literature in this area or the product specifications are used. Reagents or instruments used that do not specify the manufacturer are conventional products that can be obtained commercially.

[0065] Calcium phosphosilicate, Regesi®.

[0066] Example 1

[0067] Preparation of enamel repair toothpaste: Prepared according to the following components by weight percentage: glycerin: 20%; hydrated silica: 18%; polyethylene glycol-8: 6%; calcium phosphosilicate: 5%; sodium lauroyl sarcosinate: 1%; sodium methyl lauroyl taurate: 1.5%; polyvinylpyrrolidone (weight-average molecular weight approximately 50,000): 1%; cetylpyridinium chloride: 0.2%; lysozyme: 0.5%; papain: 0.25%; bromelain: 0.25%; trichlorogalactose: 0.1%; menthanecarboxamide: 0.2%; sodium laurate: 0.6%; sodium chloride: 0.4%; flavor: 0.8%; deionized water: balance (to 100%); The preparation steps are as follows: Add glycerol and part of deionized water into a high-speed stirring device, slowly add polyvinyl pyrrolidone, and stir until it is completely dissolved to form a basic solution.

[0068] Add hydrated silica and polyethylene glycol-8 in sequence, mix evenly under stirring, and form a dispersed system with a certain viscosity.

[0069] Add calcium phosphosilicate and continue stirring for 30 minutes to ensure that it is evenly dispersed in the system.

[0070] Sodium lauroyl sarcosinate and sodium methyl lauroyl taurate are added, and then sodium laurate is added as a foaming agent.

[0071] Cool down to no more than 40℃, add cetylpyridinium chloride, lysozyme, papain, bromelain, trichlorogalactose, menthanecarboxamide, sodium chloride and essence in sequence, and stir slowly and evenly.

[0072] After vacuum degassing for 30 minutes, a stable paste is obtained, which is then filled and sealed to produce an enamel repairing toothpaste product.

[0073] Test section Enamel Repair Efficacy Test: Tests were conducted according to Q / CTI LD-SHPHCD-1044, "Toothpaste Efficacy Test Instructions," under these experimental conditions. Acid-etched enamel specimens were subjected to a 28-day cyclical treatment using toothpaste samples and a control group for comparison. The results showed that the hardness difference ΔHV before and after treatment in the sample group was greater than that in the control group, with a significant difference between the two groups (P<0.05). The experimental toothpaste sample repaired damaged enamel. After 28 days of simulated cycling, enamel hardness was repaired by 28%, resulting in a 72% improvement in enamel hardness repair, demonstrating a certain remineralization effect on teeth.

[0074] Tooth anti-sensitivity (dentinal tubule blocking rate) test: The test was conducted according to YY / T 1829-2022 "In vitro evaluation method for dentinal tubule blocking effect in dentistry". Under the experimental conditions, compared with the blank control group, the average dentinal tubule blocking rate of the experimental group toothpaste samples after 2 days of treatment was 64.75%±2.84%, indicating that the experimental group toothpaste samples have a certain blocking effect on the dentinal tubules.

[0075] Glycolic Acid Resistance Test: The test was conducted according to Q / CTI LD-SHPHCD-1049 "Toothpaste Efficacy Test Instructions for Maintaining Oral pH Balance (Glycolic Acid Resistance)". After the oral pH balance maintenance test, under conventional culture medium, the pH value of the control group culture medium gradually decreased to below 4.3 within 24 hours, while the pH value of the sample group culture medium continued to maintain a neutral level of 6.4 for 48 hours. This shows that the tested toothpaste samples can inhibit the growth of cariogenic bacteria in the mouth, effectively resist sugar acid, and maintain oral pH balance.

[0076] Oral repair (gum protection) effect test: The test was conducted in accordance with WI-GZB-726 "Cosmetic In Vitro Efficacy Test-Cell Proliferation Experiment Operating Procedure". Under the experimental conditions, compared with the blank control group, the sample at concentrations of 0.01% and 0.001% had a significant promoting effect on the cell proliferation of gingival fibroblasts.

[0077] Breath freshening efficacy test: According to Q / CTI LD-SHPHCD-1227 "Breath Freshening Efficacy Verification Operation Instructions", the value of methyl mercaptan in the sample group was lower than that in the control group, and the difference was statistically significant (P < 0.05). This shows that after 12 hours of co-incubation with saliva, the sample can reduce the production of methyl mercaptan and has the effect of freshening breath for 12 hours.

[0078] Thermal effect test: According to Q / CTI LD-SHPHCD-1050 "Toothpaste Thermal Sensitivity Test Operating Instructions", in an environment simulating the human oral temperature of 36.3°C to 37.2°C, after the toothpaste is mixed with artificial saliva, the temperature rises to above 39°C within half a minute and remains above 39°C for about 2 minutes.

[0079] Whitening effect test: According to Q / CTI LD-SHPHCD-1441 "Tooth Whitening (Colorimetric Card Method) Operating Instructions", the test was conducted using the sample toothpaste and the control sample under the experimental conditions. The results were compared using a colorimetric plate and the whitening degree was scored. The results showed that the difference in brushing scores before and after the simulated toothbrushing of the sample group was T 样品组 Greater than the difference in scores before and after simulated toothbrushing in the control group T 对照组 Compared with the control group, the score change of the sample group was significantly different (P < 0.05). After 5 days of simulated brushing with the sample toothpaste, the score was 2.0 points, and the whitening degree increased by 2.6. The sample toothpaste has a whitening effect.

[0080] Oral mucosa irritation test: The sample was tested in accordance with YY / T0127.13-2018 "Biological Evaluation of Oral Medical Devices Part 13: Oral Mucosa Irritation Test". The irritation index of the sample in the oral mucosa irritation test on golden hamsters was 0. According to the oral mucosa irritation intensity classification of YY / T0127.13-2018 "Biological Evaluation of Oral Medical Devices Part 13: Oral Mucosa Irritation Test", it is non-irritating (according to the toothpaste usage method, the test is carried out with two contacts, each with an interval of 6 hours and each contact for 5 minutes).

[0081] Bad breath suppression effect test: The test was conducted in accordance with WS / T 650-2019 "Antibacterial and Antibacterial Effect Evaluation Method". According to the test results, the antibacterial rate was >99.96%, which was judged to have a strong inhibitory effect on Streptococcus mutans and can reduce the generation of bad breath to a certain extent.

[0082] Anticorrosion test: The test was conducted according to the United States Pharmacopoeia USP 51. The results are shown in Table 1.

[0083] Table 1

[0084] The microbiological standard requirements for Category 2 products are shown in Table 2.

[0085] Table 2

[0086] Note: "Cannot increase" in Table 2 means that compared with the previous value, log 10 The growth value cannot be greater than 0.5.

[0087] According to Table 1 and Table 2, the toothpaste provided in this application meets the relevant anti-corrosion requirements.

[0088] In summary, the enamel-repairing toothpaste prepared in Example 1 demonstrated significant comprehensive efficacy across multiple in vitro experiments. This toothpaste, through the combined action of a complex enzyme and calcium phosphosilicate, effectively enhanced enamel hardness, achieving a 72% hardness recovery rate after 28 days of simulated cyclic use, demonstrating a clear remineralization capacity. Furthermore, it achieved a 64.75% occlusion rate for dentinal tubules, demonstrating excellent anti-allergic effects. It also inhibited sugar-acid corrosion and maintained oral pH balance, demonstrating excellent anti-caries potential.

[0089] Furthermore, this toothpaste significantly promotes the proliferation of gingival fibroblasts, demonstrating potential for oral repair (gum protection). Its formula also effectively inhibits the production and release of methyl mercaptan, providing a 12-hour breath freshening effect. Under simulated conditions, it exhibits a warming sensation and a 2.6-point whitening effect. Microbial challenge testing demonstrates that its preservative system complies with USP51 standards, demonstrating effective inhibition against common pathogens and molds.

[0090] The toothpaste formula provided in this application has clear synergistic effects and comprehensive efficacy, taking into account multiple needs such as repair, anti-sensitivity, whitening, fresh breath and biosafety.

[0091] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit them. Although the present application has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some or all of the technical features therein. These modifications or replacements do not deviate the essence of the corresponding technical solutions from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A toothpaste for repairing tooth enamel, characterized in that: Calculated by mass percentage, it includes the following components: Glycerol: 15%~30%; Hydrated silica: 10%~25%; Polyethylene glycol-8: 3%~10%; Calcium phosphosilicate: 3%~7%; Surfactant: 1%~5%; Binder: 0.5%~3%; Antimicrobial agent: 0.05%~0.5%; Complex enzyme: 0.1%~1.5%; the complex enzyme includes lysozyme, papain and bromelain; the mass ratio of the lysozyme, papain and bromelain is 1:(0.4~0.6):(0.4~0.6); The balance is water.

2. The toothpaste for repairing tooth enamel according to claim 1, characterized in that: The surfactant includes sodium lauroyl sarcosinate and sodium methyl lauroyl taurate, and the mass ratio of sodium lauroyl sarcosinate to sodium methyl lauroyl taurate is 1:1-2.

3. The enamel repairing toothpaste according to claim 1, characterized in that The binder includes polyvinyl pyrrolidone, and the weight average molecular weight of the polyvinyl pyrrolidone is 40,000-60,000.

4. The enamel repairing toothpaste according to claim 1, characterized in that The antibacterial agent includes cetylpyridinium chloride.

5. The toothpaste for repairing tooth enamel according to claim 1, characterized in that: Also includes: 0.01% to 0.0.5% sweetener, wherein the sweetener includes trichlorogalactose.

6. The toothpaste for repairing tooth enamel according to claim 1, characterized in that: Also includes: 0.1% to 0.3% cooling agent, wherein the cooling agent includes menthane carboxamide.

7. The toothpaste for repairing tooth enamel according to claim 1, characterized in that: Also includes: 0.3% to 1% of a foaming aid, wherein the foaming aid includes sodium laurate.

8. The toothpaste for repairing tooth enamel according to claim 1, characterized in that: Also includes: 0.2% to 0.8% electrolyte salt, wherein the electrolyte salt includes sodium chloride.

9. The toothpaste for repairing tooth enamel according to claim 1, characterized in that: Also includes: 0.5%~1% flavor.

10. A method for preparing toothpaste for tooth enamel repair, characterized in that: include: Providing components of the enamel repair toothpaste according to any one of claims 1 to 9; The components are mixed and homogenized, and then degassed to obtain the tooth enamel repairing toothpaste.

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