Preparation and application of color-changing toothpaste composition for children

Abstract

The invention discloses a color-changing toothpaste composition for children as well as a preparation method and application thereof, and belongs to the technical field of oral care. The composition comprises a decayed tooth prevention functional component, an anti-inflammatory composition, a color-changing microcapsule and toothpaste acceptable auxiliary materials, the decayed tooth prevention functional component is formed by compounding ten components including sodium fluoride, casein phosphopeptides and the like, and the anti-inflammatory composition is prepared from a notopterygium root extract, a mangnolia officinalis extract, a bunge cherry seed extract and a kale leaf extract according to a specific proportion. The preparation method is completed through the steps of water phase preparation, liquid phase blending, powder mixing, paste making machine stirring, vacuum degassing and the like, and the process is stable and controllable. The toothpaste has the effects of preventing decayed teeth and resisting inflammation, the color-changing microcapsules can generate color change during tooth brushing, the tooth brushing interestingness of children is improved, cleaning is prompted to be in place, the toothpaste is suitable for preparing special oral care products for children, the components are safe and mild, and the toothpaste is adaptive to the oral physiological environment of children.

Description

Technical Field

[0001] This invention relates to the field of oral care technology, and more specifically, to the preparation and application of a color-changing toothpaste composition for children. Background Technology

[0002] Oral health is crucial for children's growth and development, with dental caries and periodontal inflammation being common oral problems in childhood. Data shows that the global incidence of dental caries in children aged 5-12 is over 60%, primarily due to the fragile oral microecology in children, which allows cariogenic bacteria (such as Streptococcus mutans and Lactobacillus) to thrive. Furthermore, children's lack of initiative in brushing and incomplete cleaning lead to food residue buildup, causing enamel demineralization and cavities. Simultaneously, children's delicate gum mucosa is easily irritated by oral bacteria, causing inflammation, manifesting as red, swollen, and bleeding gums. Long-term neglect of this can affect the development of periodontal tissues.

[0003] Existing children's toothpastes have several shortcomings: First, their effects are limited, with most focusing only on preventing cavities or cleaning, lacking a combined effect of both cavity prevention and anti-inflammation, making it difficult to comprehensively address children's oral health issues. Second, their design lacks engagement; while some products add pigments, they lack color-changing indicators, failing to effectively guide children in proper brushing. Third, many anti-inflammatory ingredients are chemically synthesized, which are highly irritating and unsuitable for children's sensitive oral environments, while anti-inflammatory systems formulated with natural plant extracts are rarely used and lack a clear synergistic mechanism. Fourth, some cavity-preventing ingredients are poorly combined, resulting in low bioavailability and difficulty in achieving sustained remineralization effects. Furthermore, children's toothpaste requires extremely high safety and stability of its ingredients; some existing products suffer from issues such as easily ruptured microcapsules and poor paste stability, affecting their effectiveness.

[0004] Therefore, developing a children's toothpaste composition that is comprehensive in efficacy, gentle and safe, and fun has become an urgent need in the current oral care field. Summary of the Invention

[0005] In view of the shortcomings of existing children's toothpastes, such as limited efficacy, strong irritation from anti-inflammatory ingredients, lack of fun, and poor stability, the purpose of this invention is to provide a children's toothpaste composition that has the dual core functions of preventing tooth decay and anti-inflammation. By scientifically compounding natural extracts and bioactive ingredients, it achieves comprehensive protection for children's oral health.

[0006] To achieve the above objectives, the present invention discloses the following technical solutions: In a first aspect, the present invention provides a children's color-changing toothpaste composition, the composition containing an active ingredient for preventing tooth decay, an anti-inflammatory composition, color-changing microcapsules, and toothpaste-acceptable excipients; The active ingredient for preventing tooth decay consists of sodium fluoride, casein phosphopeptide, Lactobacillus paracasei, Lactobacillus salivarius, glucanase, papain, lysozyme, PVM / MA copolymer, calcium lactate, and hydroxyapatite. The anti-inflammatory composition consists of Notopterygium root extract, Magnolia officinalis root extract, Prunus japonica seed extract, and Kale leaf extract.

[0007] Preferably, by mass fraction, the proportions of each component in the toothpaste composition of the caries-preventing active ingredient are as follows: sodium fluoride 0.1-0.4%, casein phosphopeptide 0.01-5%, *Lactobacillus paracasei* 0.01-5%, *Lactobacillus salivarius* 0.01-5%, dextranase 0.01-5%, papain 0.01-5%, lysozyme 0.01-5%, PVM / MA copolymer 0.01-5%, calcium lactate 0.01-2%, and hydroxyapatite 0.01-20%; The anti-inflammatory composition is present in the toothpaste composition at a concentration of 0.1-1%. The color-changing microcapsules constitute 0.1-5% of the toothpaste composition.

[0008] More preferably, the mass ratio of the Notopterygium root extract, Magnolia officinalis root extract, Prunus japonica seed extract and Kale leaf extract is (1-5):(10-12):(3-6):(8-10).

[0009] Preferably, the excipients are at least one selected from humectants, abrasives, thickeners, surfactants, fragrances, cooling agents, stabilizers, preservatives, conditioning agents, sweeteners, colorants, and solvents.

[0010] More preferably, the moisturizer is at least one selected from sorbitol, glycerin, polyethylene glycol, caprylyl glycol, and ethylhexylglycerin; The friction agent is at least one of hydrated silica and dicalcium phosphate; The thickener is at least one of sodium carboxymethyl cellulose and xanthan gum; The surfactant is at least one of sodium lauroyl sarcosinate and cocamidopropyl betaine; The stabilizer is at least one of sodium pyrophosphate and sodium fluoride; The conditioning agent is persimmon fruit extract and zinc citrate; The sweetener is at least one of trichlorogalactose and xylitol; The solvent is distilled water.

[0011] Secondly, the present invention provides a method for preparing the aforementioned toothpaste composition, the method comprising the following steps: Step 1: Add the anti-inflammatory composition, stabilizer, sweetener, sodium fluoride, Lactobacillus paracasei, Lactobacillus salivarius, conditioning agent, glucanase, papain, lysozyme, PVM / MA copolymer, and colorant to water and stir until homogeneous to form an aqueous phase; Step 2: Add the humectant to the aqueous phase and stir for 5 to 10 minutes to obtain a homogeneous liquid phase; Step 3: Mix the abrasive, thickener, and casein phosphopeptide evenly into a powder and set aside. Step 4: Add the liquid phase and powder to the ointment making machine, control the vacuum degree above -0.92Mpa, and stir rapidly for 20 to 30 minutes under the condition of controlling the water bath temperature at 42℃. Step 5: Add surfactant, calcium lactate, cooling agent, and fragrance. Control the vacuum degree above -0.94 MPa and stir rapidly for 15-20 minutes. Open the lid and add color-changing microcapsules. Under vacuum, control the scraper speed at 10-50 r / min and the double stirring speed at 10-400 r / min, stir for 1-5 minutes, and control the vacuum degree to be no less than -0.094 MPa. Continue to evacuate and degas to obtain the children's color-changing toothpaste.

[0012] Thirdly, the present invention provides the application of the toothpaste composition described in the first aspect in the preparation of oral care products with anti-caries and anti-inflammatory effects.

[0013] In this invention: The Lactobacillus paracasei and Lactobacillus salivarius provided by this invention can reduce the number of cariogenic bacteria such as Streptococcus mutans and Lactobacillus in saliva and plaque biofilm, alleviate oral microecological imbalance, help improve the oral microecological environment, and are beneficial for the prevention of oral diseases and dental caries.

[0014] Sodium fluoride primarily works by inhibiting demineralization of tooth hard tissues and promoting enamel remineralization. It typically combines with calcium and phosphate ions in the enamel to form calcium fluoride and calcium fluorophosphate, thereby increasing the hardness and toughness of the enamel. This allows teeth to effectively resist acidic environments, reducing acid erosion and inhibiting demineralization of hard tissues. It can also combine with minerals in the oral cavity to form a protective fluoride deposit, promoting tooth remineralization and repair.

[0015] Casein phosphopeptides are bioactive peptides containing phosphoserine clusters, obtained from bovine casein through enzymatic hydrolysis and purification. They promote the absorption and utilization of mineral salts such as calcium, iron, and zinc by the intestinal mucosa and are a group of bioactive peptides involved in multiple functions, often referred to as "mineral carriers." They can chelate calcium and phosphate ions to a certain extent, stabilizing them in an amorphous, non-crystalline state, thus promoting mineral deposition on tooth surfaces.

[0016] Hydroxyapatite possesses excellent biocompatibility and osteoconductive properties, and is a major inorganic component of human and animal bones. It can chemically bond with body tissues at the interface, has a certain solubility in vivo, releases harmless ions, participates in metabolism, stimulates or induces bone hyperplasia, and promotes the repair of damaged tissues. Adding hydroxyapatite to toothpaste can stimulate and activate tissues, and has special therapeutic effects on tooth remineralization, treatment, and antibacterial properties.

[0017] Papain can effectively hydrolyze biological membranes and help remove extrinsic stains from teeth; lysozyme, derived from egg white, can enzymatically break down the β-1,4 glycosidic bonds between N-acetylmuramic acid and N-acetylglucosamine in the cell wall, causing the insoluble polysaccharides in the cell wall to decompose into soluble glycopeptides, leading to the release of bacterial contents and bacterial death, thus exhibiting a good antibacterial effect and helping to reduce oral bacteria and inhibit the formation of dental plaque; dextranase can decompose dextran, the main component of dental plaque matrix, reducing the adhesion and accumulation of this mucopolysaccharide, effectively removing stains and tartar from the tooth surface, and maintaining oral health.

[0018] PVM / MA copolymer, a copolymer of vinyl methyl ether and maleic acid, is an effective inhibitor of alkali metal phosphatase. It can effectively chelate pyrophosphatase and alkali metal phosphatase, thereby inhibiting the formation of dental calculus. It can improve the retention of active substances on the tooth surface, solubilize poorly soluble components, improve the bioavailability of active substances, and prolong the release of active substances when used in combination with active ingredients.

[0019] Color-changing microcapsules are pigmented microcapsule materials prepared through a special process. Under the premise of correct brushing force and brushing time, the color of the foam changes during brushing, creating a visually pleasing effect, enhancing the fun of brushing for children, and increasing the enjoyment of brushing. At the same time, it can remind children to brush their teeth thoroughly and clean them properly, which helps to develop good cleaning habits, better clean the oral cavity, and reduce bacterial residue.

[0020] This anti-inflammatory composition is a blend of Notopterygium root extract, Magnolia officinalis root extract, Prunus japonica seed extract, and Kale leaf extract in a specific mass ratio. The components work synergistically to exert a highly effective and gentle anti-inflammatory effect: Notopterygium root extract contains volatile oils and coumarin-like active ingredients, which can inhibit the activity of key enzymes in the inflammatory pathway, reduce the release of inflammatory mediators, and relieve periodontal tissue redness and swelling; Magnolia officinalis root extract's main components, honokiol and magnolol, have significant antibacterial and anti-inflammatory effects, inhibiting the growth of periodontal pathogens such as Porphyromonas gingivalis, while downregulating the expression of inflammatory factors; Prunus japonica seed extract is rich in flavonoids, which can soothe the oral mucosa, reduce discomfort caused by inflammatory stimulation, and enhance the mucosal barrier function; Kale leaf extract contains abundant vitamins and polyphenols, possessing antioxidant and anti-inflammatory activities, clearing free radicals in the oral cavity, reducing oxidative stress damage to periodontal cells, and when combined with the other three extracts, it can significantly reduce the levels of inflammatory factors such as IL-1β and TNF-α through multi-target synergistic effects, protect the vitality of human periodontal ligament fibroblasts, and effectively relieve oral inflammation in children.

[0021] The beneficial effects of this invention are: 1. The anti-caries active ingredients provided by this invention have multiple targets and synergistic effects. Sodium fluoride, combined with hydroxyapatite and calcium lactate, can both inhibit enamel demineralization and promote remineralization. Probiotics (Lactobacillus paracasei and Lactobacillus salivarius) regulate the oral microecology and reduce the number of cariogenic bacteria. Glucanase, papain, and other enzymes can remove dental plaque matrix and extrinsic staining. PVM / MA copolymer prolongs the residence time of active ingredients and significantly improves the anti-caries effect.

[0022] 2. This invention uses an anti-inflammatory composition formulated with natural plant extracts. It is free from the irritation of chemical anti-inflammatory ingredients, is suitable for children's sensitive mouths, and can effectively inhibit periodontal inflammation, protect periodontal ligament cells, and reduce the incidence of problems such as gingival redness and bleeding.

[0023] 3. The color-changing microcapsules provided by this invention change color with the force and time during brushing, which not only enhances children's interest in brushing, but also provides a visual indication of whether the cleaning is in place, helping to develop proper brushing habits and solving the pain points of children's lack of enthusiasm for brushing and incomplete cleaning. Detailed Implementation

[0024] To better illustrate the objectives, technical solutions, and advantages of this invention, the invention will be further described below with reference to specific embodiments. Those skilled in the art should understand that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

[0025] Unless otherwise specified, the test methods used in the examples and comparative examples are conventional methods; the materials and reagents used are commercially available unless otherwise specified; and the percentages mentioned in the examples and comparative examples are mass percentages unless otherwise specified.

[0026] I. In this invention Casein phosphopeptide: a structural fragment obtained by enzymatic hydrolysis of bovine casein. Its basic structure is -SerP-SerP-SerP-Glu-Glu-, with a molecular weight of 1000-5000 Da. It is commercially available. Lactobacillus paracasei: viable count 1.0 × 10⁻⁶ 9 -9.0×10 10 CFU / g, commercially available; Lactobacillus salivarius: viable count 1.0 × 10⁻⁶ 9 -9.0×10 10 CFU / g, commercially available; Dextranase: Enzyme activity not less than 1.0 × 10⁻⁶ 11 U / g, purchased from Zhongnuo Biotechnology Development Jiangsu Co., Ltd.; Papain: Enzyme activity not less than 300 U / g, commercially available; Lysozyme: Enzyme activity not less than 5 × 10 5 U / g, commercially available; Notopterygium root extract: purchased from Wanyuan Biotechnology Co., Ltd.; Magnolia officinalis extract: purchased from Wanyuan Biotechnology Co., Ltd.; Prunus japonica seed extract: purchased from Wanyuan Biotechnology Co., Ltd.; Kale leaf extract: purchased from Wanyuan Biotechnology Co., Ltd.; All other raw materials used in the examples are commercially available.

[0027] II. Color-changing microcapsules The specific steps for preparing color-changing microcapsules are as follows: Step 1, Colorant pre-dispersion treatment: Mix the water-soluble colorant with 3 times its mass of deionized water and dissolve it evenly to form a uniform dispersion for later use; Step 2, Preparation of aqueous solution: Weigh sorbitol, propylene glycol, sodium carboxymethyl cellulose (30-40% of the total amount), mannitol and sodium pyrophosphate, add deionized water, place in a 50℃ constant temperature water bath, keep warm and disperse at 200 rpm for 45 min until all components are completely dissolved to form a transparent and homogeneous aqueous solution, cool to room temperature for later use; Step 3, Microcapsule Core Preparation: Slowly add the pre-dispersed pigment solution from Step 1 to the aqueous solution from Step 2, maintain room temperature, stir at 1000 rpm, mix for 30 min to ensure uniform pigment dispersion, transfer to a spray dryer, set the inlet air temperature to 110℃ and the outlet air temperature to 65℃, collect the solid particles after drying to obtain the microcapsule core. Step 4, Mixing the kernel and interstitial material: Mix the kernel particles from Step 3 with corn starch and dextrin, add them to a high-speed mixer, and mix at room temperature for 20 minutes at a dispersion disc speed of 600 rpm to form pretreated particles; Step 5, Preparation of wall material solution: Weigh the remaining sodium carboxymethyl cellulose, add the remaining deionized water, stir at 700 rpm at room temperature for 25 min until completely dissolved to form a wall material solution; Step 6, Microcapsule Forming and Post-processing: Mix the pretreated particles from Step 4 with the wall material solution from Step 5, stir at 700 rpm, disperse at room temperature for 25 minutes to ensure uniform adsorption of the wall material by the particles, and transfer to a spray dryer again. Set the inlet air temperature to 105℃ and the outlet air temperature to 65℃. After spray drying, sieve through a 60-mesh standard sieve and collect the sieve-underfill material to obtain color-changing microcapsules.

[0028] The specific dosage of the color-changing microcapsule raw materials is detailed in Table 1.

[0029] Table 1 Raw material name Amount Water-soluble colorant 0.8% Sorbitol 10% Propylene glycol 3% Sodium carboxymethyl cellulose 4.0% Mannitol 3.0% Corn starch 12% Malt dextrin 6% Deionized water Balance Sodium pyrophosphate 0.3% III. Anti-inflammatory Composition 1. Composition 1-3 The composition is prepared by compounding the raw material components in Table 2 according to a specific mass ratio, as follows: Table 2 Raw material name Composition 1 Composition 2 Composition 3 Notopterygium extract 1 3 5 Magnolia officinalis extract 10 11 12 Prunus domestica extract 3 4.5 6 Kale leaf extract 8 9 10 2. Anti-inflammatory performance test 2.1 Test Sample Compositions 1-3 and control compositions 1-5, wherein control compositions 1-5 are based on the formulation of composition 2 with adjustments, as shown in Table 3.

[0030] Table 3 Raw material name Control composition 1 Control composition 2 Control composition 3 Control composition 4 Control composition 5 Notopterygium extract / 3 3 3 1 Magnolia officinalis extract 11 / 11 11 1 Prunus domestica extract 4.5 4.5 / 4.5 1 Kale leaf extract 9 9 9 / 1 Note: " / " in the table indicates no addition.

[0031] 2.2 Experimental Subjects Human periodontal ligament fibroblasts (hPDLCs) of 5th to 8th generation with good growth status were selected for the experiment to ensure uniform cell morphology and stable proliferation.

[0032] 2.3 Reagents Lipopolysaccharide (LPS), DMEM high-glucose medium (containing 10% fetal bovine serum, 100 U / mL penicillin, and 100 mg / L streptomycin), CCK-8 cell viability kit, IL-1β ELISA kit, and TNF-α ELISA kit; 2.4 Experimental Methods 2.4.1 Cell Culture and Preliminary Experiments Cell culture: hPDLCs were seeded in T25 culture flasks containing complete culture medium and placed in a 37°C, 5% CO2 incubator. When the cell confluence reached 80%-90%, the cells were digested with 0.25% trypsin (containing EDTA) and passaged every 2-3 days for later use. Preliminary experiment: hPDLCs were co-cultured with culture medium containing concentration gradients of 0.01%, 0.02%, 0.05%, 0.1%, 0.5%, and 1% (compositions 1-3 and control compositions 1-5) for 48 h. Cell viability was then detected by CCK-8 assay to confirm that all composition concentration ranges had no significant inhibitory effect on the viability of normal hPDLCs (viability ≥90%, P>0.05), thus eliminating the interference of cytotoxicity on the experimental results.

[0033] When the concentration was ≤0.1%, the cell viability was ≥90%, and 0.1% was finally confirmed as the working concentration.

[0034] 2.4.2 Experimental Grouping and Treatment Table 4

[0035] 2.4.3 Detection of inflammatory factors hPDLCs at 1×10 5 Cells were seeded per well in a 6-well plate. After 72 hours of treatment according to the groups, the supernatant of each group was collected, centrifuged at 1000 r / min for 10 min, and the supernatant was used for later use. The concentrations of IL-1β and TNF-α in the supernatant were detected according to the ELISA kit instructions.

[0036] 2.5 Test Results Table 5 Effects on inflammatory factors in hPDLCs Group IL-1β (pg / mL) TNF-α (pg / mL) Blank control group 112.33±1.62** 102.26±2.08** Model group 231.65±19.26 183.74±16.35 Composition 1 group 135.62±8.95** 124.38±7.63** Composition 2 group 121.57±6.32** 115.24±5.81** Composition 3 group 130.45±7.88** 120.17±6.45** Control composition 1 group 189.73±12.46* 162.85±10.32* Control composition 2 group 195.36±13.12* 168.42±11.05* Control composition 3 group 182.49±11.78* 156.73±9.87* Control composition 4 group 191.64±12.83* 164.39±10.58* Control composition 5 group 203.58±14.21* 172.65±11.63* Dexamethasone group 118.74±5.96** 110.35±4.92** Note: * indicates a significant difference compared to the model group, P < 0.05, **P < 0.01.

[0037] 2.6 Results Analysis Comparison between the model group and the blank control group: After LPS induction, the concentrations of IL-1β and TNF-α in the model group were as high as 231.65 pg / mL and 183.74 pg / mL, respectively, which were significantly higher than those in the blank control group (P < 0.01), indicating that LPS successfully induced inflammatory responses in human periodontal ligament fibroblasts and the experimental model was effectively constructed.

[0038] The concentrations of IL-1β and TNF-α in groups 1-3 were significantly lower than those in the model group (P<0.01) and close to those in the blank control group and the positive control group. Among them, the inflammatory factor levels in group 2 were the lowest, with IL-1β at 121.57 pg / mL and TNF-α at 115.24 pg / mL, indicating that the anti-inflammatory effect was optimal under this ratio. The four extracts can synergistically inhibit the release of inflammatory factors after being combined.

[0039] Control compositions 1-4 each lacked one extract, while control composition 5 was a mixture of four extracts in equal proportions. Its IL-1β and TNF-α concentrations were significantly higher than those of composition 2 (P<0.05) and much higher than those of the blank control group, indicating that all four extracts are indispensable and that a specific ratio of the mixture can produce a synergistic anti-inflammatory effect. The absence of any component or an imbalance in the ratio will lead to a decrease in anti-inflammatory efficacy, thus verifying the scientific nature of the anti-inflammatory composition ratio of the present invention.

[0040] IV. Children's Color-Changing Toothpaste Composition The specific steps for preparing the color-changing toothpaste composition for children are as follows: Step 1: Add the anti-inflammatory composition, sodium salt, xylitol, trichlorogalactose, sodium fluoride, Lactobacillus paracasei, Lactobacillus salivarius, persimmon fruit extract, zinc citrate, glucanase, papain, lysozyme, PVM / MA copolymer, and pigment to water and stir until homogeneous to form an aqueous phase. Step 2: Add sorbitol, glycerol, polyethylene glycol-8, caprylyl glycol, and ethylhexylglycerol to the aqueous phase and stir for 5 to 10 minutes to obtain a homogeneous liquid phase; Step 3: Mix hydrated silica, sodium carboxymethyl cellulose, xanthan gum, casein phosphopeptide, hydroxyapatite, and dicalcium phosphate evenly into a powder and set aside. Step 4: Add the liquid phase and powder to the ointment making machine, control the vacuum degree above -0.92Mpa, and stir rapidly for 20 to 30 minutes under the condition of controlling the water bath temperature at 42℃. Step 5: Add sodium lauroyl sarcosinate, cocamidopropyl betaine, calcium lactate, menthol, and flavoring. Maintain a vacuum of -0.94 MPa or higher and stir rapidly for 15–20 minutes. Open the lid and add the color-changing microcapsules. Under vacuum, control the scraper speed at 10–50 rpm and the double stirring speed at 10–400 rpm for 1–5 minutes. Maintain a vacuum of no less than -0.094 MPa and continue vacuuming to degas, obtaining the children's color-changing toothpaste.

[0041] For details of the toothpaste ingredients in Examples 1-4, please refer to Table 6. Table 6. Percentage of Toothpaste Raw Materials by Mass (Unit: %) Component Example 1 Example 2 Example 3 Example 4 Discolored microcapsule 0.1 2 3 5 Sorbitol 30 40 50 70 Hydrated silica 10 20 20 30 Glycerin 1 5 7 10 Polyethylene glycol-8 1 10 15 20 Fragrance 0.1 1 1.5 2 Sodium lauroyl glutamate 0.5 2 2 5 Cocamidopropyl betaine 0.5 2 2 5 Sodium salt (crystalline sodium pyrophosphate) 0.1 1 0.5 2 Sodium carboxymethyl cellulose 0.1 2 0.5 5 Xanthan gum 0.1 2 0.5 5 Octisalate 0.1 0.5 0.5 1 Sodium fluoride 0.1 0.2 0.3 0.4 Ethylhexylglycerin 0.1 0.2 0.3 1 Casein phosphopeptide 0.01 1 2 5 Paracasei lactis 0.01 1 2 5 Salivarius lactis 0.01 0.05 0.08 3 Calcium hydrogen phosphate 0.01 1 3 5 Persimmon fruit extract 0.0001 0.003 0.01 1 Zinc citrate 0.01 0.05 0.1 2 Dextranase 0.01 0.05 0.1 2 Papain 0.01 0.05 0.05 2 Lysozyme 0.01 0.01 0.05 2 PVM / MA copolymer 0.01 0.1 1 3 Calcium lactate 0.01 1 1.5 2 Anti-inflammatory composition 0.1 0.4 0.6 1 Hydroxyapatite 0.01 1 5 20 Xylitol 0.1 1 1 2 Trichlorogalactose 0.01 1 1 2 Menthol 0.01 0.5 0.5 1 Colorant 0.001 0.01 0.005 0.05 Deionized water Added to 100 Added to 100 Added to 100 Added to 100 The specific steps for preparing the comparative toothpaste composition are as follows: Step 1: Add sodium salt, xylitol, trichlorogalactose, and pigment to water and stir until a homogeneous aqueous phase is formed; Step 2: Add sorbitol, glycerol, polyethylene glycol-8, caprylyl glycol, and ethylhexylglycerol to the aqueous phase and stir for 5 to 10 minutes to obtain a homogeneous liquid phase; Step 3: Mix hydrated silica, sodium carboxymethyl cellulose, and xanthan gum evenly into a powder and set aside. Step 4: Add the liquid phase and powder to the ointment making machine, control the vacuum degree above -0.92Mpa, and stir rapidly for 20min to 30min under the condition of controlling the water bath temperature at 42℃. Step 5: Add sodium lauroyl sarcosinate, cocamidopropyl betaine, menthol, and flavoring. Control the vacuum degree to above -0.94 MPa, stir rapidly for 15 to 20 minutes, and control the vacuum degree to not be lower than -0.094 MPa. Continue to degas under vacuum to obtain the comparative toothpaste composition.

[0042] For the comparative toothpaste ingredients, please refer to Table 7; Table 7. Percentage of Toothpaste Raw Materials by Mass (Unit: %) Component Comparative example 1 Sorbitol 30 Hydrated silica 10 Glycerin 1 Polyethylene glycol-8 1 Fragrance 0.1 Sodium lauroyl glutamate 0.5 Cocamidopropyl betaine 0.5 Sodium salt 0.1 Sodium carboxymethyl cellulose 0.1 Xanthan gum 0.1 Octisalate 0.1 Ethylhexylglycerin 0.1 Xylitol 0.1 Trichlorogalactose 0.01 Menthol 0.01 Colorant 0.001 Deionized water Added to 100 V. Example and Comparative Test Results 1. Stability Test The results of the stability test of the product in Example 1 are as follows: Table 8 Product stability in Example 1

[0043] After a 3-month stability study of the ointment in Example 1, the overall stability of the ointment was normal, and the microcapsules contained therein remained intact without any abnormal phenomena such as breakage or swelling, indicating normal stability.

[0044] The results of the stability test for the product in Example 2 are as follows: Table 9 Product stability in Example 2

[0045] After a 3-month stability study of the ointment in Example 2, the overall stability of the ointment was normal, and the microcapsules contained therein remained intact without any abnormal phenomena such as breakage or swelling, indicating normal stability.

[0046] The results of the stability test for Example 3 are as follows: Table 10 Product stability in Example 3

[0047] After a 3-month stability study of the ointment in Example 3, the overall stability of the ointment was normal, and the microcapsules contained therein remained intact without any abnormal phenomena such as breakage or swelling, indicating normal stability.

[0048] The results of the stability test for Example 4 are as follows: Table 11 Product stability in Example 4

[0049] After a 3-month stability test of the ointment in Example 4, the overall stability of the ointment was normal, and the microcapsules contained therein remained intact without any abnormal phenomena such as breakage or swelling, indicating normal stability.

[0050] 2. Antibacterial test Oral health is particularly important for children during their growth, and dental caries is one of the major problems affecting children's oral health. In a healthy state, the oral cavity contains a variety of microorganisms, primarily bacteria such as Proteus, Streptococcus, and Lactobacillus. Beneficial microorganisms inhibit the growth of harmful bacteria by producing antibacterial substances or competing for nutrients, maintaining a dynamic balance and preserving the oral microecology. However, due to various factors such as lifestyle, diet, and hygiene habits, the oral microecology can be disrupted, breaking the balance. Pathogenic microorganisms can then overgrow. Overactive acid-producing bacteria such as Streptococcus and Lactobacillus can convert sugars in food debris into acid, leading to enamel demineralization and dental caries. The proliferation of anaerobic bacteria such as Porphyromonas gingivalis can also cause oral inflammation and damage oral health. Therefore, reducing the growth of harmful bacteria, maintaining oral microbial diversity, and balancing the oral microecology helps prevent dental caries in its early stages and reduces the risk of oral diseases.

[0051] The toothpastes prepared in Example 1 and Comparative Example 1 were tested according to the following steps, and the results are shown in Table 12.

[0052] 1) Preparation of bacterial strains: Prepare culture media, inoculate Porphyromonas gingivalis, Fusobacterium nucleatum, and Streptococcus mutans into the corresponding culture media, and culture anaerobicly for 18-48 hours.

[0053] 2) Collection and culture of human saliva.

[0054] 3) Preparation of test sample slurry: Weigh a certain amount of the toothpaste to be tested and deionized water, stir with a glass rod to disperse the toothpaste, and then stir into a homogenate for later use.

[0055] 4) Sample slurry treatment: Take a certain amount of bacterial suspension and incubate it together with the test sample slurry. After 48-72 hours of incubation, count the colonies and calculate the reduction rate = (average colony count of control group - average colony count of experimental group) / average colony count of control group × 100%.

[0056] Table 12 Results of the sterilization experiment in Example 1

[0057] 3. Evaluation of in vitro anti-caries efficacy Dental caries is a chronic, progressive, and destructive disease affecting the hard tissues of teeth. It is primarily caused by bacteria, but also involves multiple factors working together. When the overall function of the dental microbiome is disrupted, harmful microbial metabolism increases, cariogenic bacteria easily accumulate on the tooth surface, increasing plaque pathogenicity. Rapid decomposition of food debris leads to increased acid production by cariogenic bacteria, resulting in a decrease in oral pH, all of which contribute to tooth demineralization. Therefore, effectively inhibiting the decomposition of sugars by harmful bacteria, reducing acid production, and simultaneously enhancing enamel remineralization and increasing enamel hardness play a crucial role in protecting teeth and reducing the incidence of dental caries.

[0058] The compositions of Example 1 and Comparative Example 1 were tested according to the following steps, and the results are shown in Table 13.

[0059] 1) Fabrication of enamel blocks: Select a number of smooth, caries-free bovine permanent incisors, cut them into approximately 5mm x 5mm pieces, embed them in polymethyl methacrylate resin, and after drying, polish them with silicon carbide sandpaper of various grits until the tooth surface is smooth and uniform, without any visible cracks or imperfections. Rinse the prepared enamel block samples with deionized water, keep them moist, and refrigerate them for later use.

[0060] 2) Preparation of experimental reagents: a) Preparation of growth medium: Dissolve tryptic soy peptone and sucrose in deionized water, sterilize at 121°C for 20 min and cool; b) Preparation of inhibition medium: Dissolve tryptic soy peptone in deionized water, sterilize at 121°C for 20 min and then cool; c) Human saliva collection: Select 3-5 volunteers without serious oral diseases. Do not use toothpaste containing antibacterial substances to brush your teeth or rinse your mouth with mouthwash within two hours before collecting saliva. Mix the saliva after collection and set aside.

[0061] d) Preparation of test sample slurry: Weigh a certain amount of the toothpaste to be tested and deionized water, stir with a glass rod to disperse the toothpaste, and then stir into a homogenate for later use.

[0062] 3) Hardness test of tooth grinding blocks: The surface hardness of tooth enamel is measured using a Vickers microhardness tester with a load of 50-100g for 5-10s. The distance between the measurement point and the edge of the tooth block is not less than 0.5mm. Three points are measured for each tooth enamel sample. The sample hardness is the average value of the three measurements. After measurement, the tooth grinding blocks are placed in an autoclave at 121℃ for 15min.

[0063] 4) Oral microbial culture: Take the growth medium into a sterile centrifuge tube, place the sterile enamel block into the test tube with sterile forceps, add human saliva to the sample group and negative control group, and immerse in 37°C.

[0064] 5) Sample processing: Add sample slurry to each test tube of the sample group and add sterile physiological saline to the negative control group. Vortex the tubes and incubate them. After vortexing, wash the tubes with sterile physiological saline and transfer them to centrifuge tubes containing inhibitory medium. Incubate at 37°C.

[0065] 6) Use a Vickers hardness tester to measure the hardness of the tooth grinding block after treatment and perform data statistics.

[0066] Table 13 Hardness test results

[0067] 4. Evaluation of efficacy in removing extrinsic pigmentation Intrinsic and extrinsic stains are the main factors causing unsightly teeth. The tooth surface typically absorbs proteins from saliva, forming an acquired membrane. After food intake, due to factors such as inadequate or improper cleaning, easily staining substances like cola, orange juice, and tea can adhere to the tooth surface, forming extrinsic stains within the acquired membrane, thus affecting the appearance of the teeth.

[0068] The compositions of Example 1 and Comparative Example 1 were tested according to the following steps, and the results are shown in Table 14.

[0069] 1) Making tooth grinding blocks: Take a cow incisor tooth, cut it into enamel blocks, embed them, and polish them smooth.

[0070] 2) Acid etching: Immerse the dental grinding block in the acid etching solution, stir, and then rinse it with clean water.

[0071] 3) Preparation of staining solution: Weigh out gastric mucoprotein, cola, orange juice, soy sauce, coffee, black tea, etc., and stir well.

[0072] 4) Staining of tooth abrasive blocks: After acid etching, the tooth abrasive blocks are placed in a staining machine for staining. The stained tooth abrasive blocks are numbered and marked. The color of the tooth enamel is measured with a colorimeter and randomly assigned to the sample group and the control group for brushing treatment.

[0073] 5) Preparation of test sample slurry: Weigh a certain amount of the toothpaste to be tested and deionized water, stir with a glass rod to disperse the toothpaste, and then stir into a homogenate for later use.

[0074] 6) Simulated brushing: Place the tooth grinding block into the automatic mechanical toothbrush and brush your teeth according to the program. After brushing, remove the tooth grinding block from the toothbrush, rinse it with water, absorb the water with a paper towel, let it dry, and use a colorimeter to measure the color of the tooth enamel.

[0075] Table 14 Results of experiments on the removal of exogenous pigmentation spots

[0076] 5. Analysis of the above test results Stability: The toothpaste products of Examples 1-4 remained stable in appearance, aroma, consistency and pH value after being stored at 25°C and 45°C for 3 months. The color-changing microcapsules did not break or swell, indicating that the products have good storage stability and meet the needs of market circulation.

[0077] Antibacterial effect: The reduction rate of Porphyromonas gingivalis, Fusobacterium nucleatum, and Streptococcus mutans in Example 1 was >99.99%, which was significantly higher than that in Comparative Example 1. This indicates that the anti-caries active ingredient and the anti-inflammatory composition work synergistically to effectively inhibit harmful bacteria in the oral cavity and maintain the balance of the oral microecology.

[0078] Anti-caries efficacy: The hardness difference of the tooth grinding block after treatment in Example 1 was 76.3, which was significantly lower than that in Comparative Example 1 (P<0.05), indicating that the composition can effectively resist acid erosion, inhibit enamel demineralization, increase enamel hardness, and exert a good anti-caries effect.

[0079] Stain removal efficacy: The color difference of the tooth grinding block after treatment in Example 1 was significantly higher than that in Comparative Example 1 (P<0.05), indicating that the papain, glucanase and other components can effectively remove extrinsic stains on teeth and improve the aesthetics of teeth.

[0080] In summary, the children's color-changing toothpaste composition of the present invention achieves multiple effects such as preventing tooth decay, anti-inflammation, and fun cleaning through scientific ingredient compounding and process optimization. The ingredients are safe, gentle, and have good stability, and can comprehensively solve the core problems in children's oral care.

[0081] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A color-changing toothpaste composition for children, characterized in that, The composition contains an active ingredient for preventing tooth decay, an anti-inflammatory composition, color-changing microcapsules, and toothpaste-acceptable excipients. The active ingredient for preventing tooth decay consists of sodium fluoride, casein phosphopeptide, Lactobacillus paracasei, Lactobacillus salivarius, glucanase, papain, lysozyme, PVM / MA copolymer, calcium lactate, and hydroxyapatite. The anti-inflammatory composition consists of Notopterygium root extract, Magnolia officinalis root extract, Prunus japonica seed extract, and Kale leaf extract.

2. The toothpaste composition according to claim 1, characterized in that, By mass fraction, the proportions of each component in the toothpaste composition of the caries-preventing active ingredient are as follows: sodium fluoride 0.1-0.4%, casein phosphopeptide 0.01-5%, Lactobacillus paracasei 0.01-5%, Lactobacillus salivae 0.01-5%, dextranase 0.01-5%, papain 0.01-5%, lysozyme 0.01-5%, PVM / MA copolymer 0.01-5%, calcium lactate 0.01-2%, and hydroxyapatite 0.01-20%; The anti-inflammatory composition is present in the toothpaste composition at a concentration of 0.1-1%. The color-changing microcapsules constitute 0.1-5% of the toothpaste composition.

3. The toothpaste composition according to claim 2, characterized in that, The mass ratio of the notopterygium root extract, magnolia bark extract, apricot kernel extract and kale leaf extract is (1-5):(10-12):(3-6):(8-10).

4. The toothpaste composition according to claim 1, characterized in that, The excipients are at least one of the following: humectant, abrasive, thickener, surfactant, fragrance, cooling agent, stabilizer, preservative, conditioning agent, sweetener, colorant, and solvent.

5. The toothpaste composition according to claim 4, characterized in that, The moisturizer is at least one of sorbitol, glycerin, polyethylene glycol, caprylyl glycol, and ethylhexylglycerin; The friction agent is at least one of hydrated silica and dicalcium phosphate; The thickener is at least one of sodium carboxymethyl cellulose and xanthan gum; The surfactant is at least one of sodium lauroyl sarcosinate and cocamidopropyl betaine; The stabilizer is at least one of sodium pyrophosphate and sodium fluoride; The conditioning agent is at least one of persimmon fruit extract and zinc citrate; The sweetener is at least one of trichlorogalactose and xylitol; The solvent is distilled water.

6. A method for preparing the toothpaste composition according to claim 5, characterized in that, The preparation method includes the following steps: Step 1: Add the anti-inflammatory composition, stabilizer, sweetener, sodium fluoride, Lactobacillus paracasei, Lactobacillus salivarius, conditioning agent, glucanase, papain, lysozyme, PVM / MA copolymer, and colorant to water and stir until homogeneous to form an aqueous phase; Step 2: Add the humectant to the aqueous phase and stir for 5 to 10 minutes to obtain a homogeneous liquid phase; Step 3: Mix the abrasive, thickener, and casein phosphopeptide evenly into a powder and set aside. Step 4: Add the liquid phase and powder to the ointment making machine, control the vacuum degree above -0.92Mpa, and stir rapidly for 20 to 30 minutes under the condition of controlling the water bath temperature at 42℃. Step 5: Add surfactant, calcium lactate, cooling agent, and fragrance. Control the vacuum degree above -0.94 MPa and stir rapidly for 15-20 minutes. Open the lid and add color-changing microcapsules. Under vacuum, control the scraper speed at 10-50 r / min and the double stirring speed at 10-400 r / min, stir for 1-5 minutes, and control the vacuum degree to be no less than -0.094 MPa. Continue to evacuate and degas to obtain the children's color-changing toothpaste.

7. The use of the toothpaste composition according to any one of claims 1-5 in the preparation of an oral care product having the functions of preventing tooth decay and anti-inflammation.

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