Toothpaste formula for protecting enamel and removing dental plaque

Abstract

The invention relates to a toothpaste formula for protecting enamel and removing dental plaque, and belongs to the technical field of toothpaste formulas. Comprising the following raw materials in percentage by weight: 15-20% of hydrated silica, 3-6% of xylitol, 5-8% of polyethylene glycol, 0.5-1.5% of sodium lauryl sulfate, 0.3-0.5% of cocamidopropyl betaine, 0.3-0.8% of xanthan gum, 20-28% of glycerol, 0.3-0.5% of peppermint oil, 0.7-1.4% of carboxymethyl cellulose gum, 3-5% of a tomentosa cherry extracting solution, 1-5% of edgeworthia chrysantha fiber powder, 2-5% of a salvia extract and the balance of deionized water. The sum of the weight percentages of the raw materials is 100%. Total polyphenols in the tomentosa cherry extracting solution and total flavonoids in the radix salviae miltiorrhizae extract form a synergistic bacteriostatic effect, and reproduction of dental plaque pathogenic bacteria can be directly inhibited, so that oral pathogenic bacteria are remarkably reduced after the toothpaste is used; a synergistic cleaning system of flexible adsorption and moderate grinding is formed by the edgeworthia chrysantha fiber powder and the hydrated silica, dental plaque residues on the tooth surface can be physically adsorbed, excessive friction of tooth enamel is avoided due to the flexible fiber characteristic of the edgeworthia chrysantha fiber powder, and the tooth enamel is protected while dental plaque is efficiently removed.

Description

Technical Field

[0001] This invention belongs to the field of toothpaste formulation technology, specifically relating to a toothpaste formulation that protects tooth enamel and removes plaque. Background Technology

[0002] Toothpaste is a paste-like product applied to the surface of human teeth by friction, with the main purpose of cleaning. It is generally in the form of a gel and is usually applied to a toothbrush. The mechanical friction of the toothbrush cleans the surface of the teeth and the surrounding area, leaving the mouth clean and refreshed.

[0003] Traditional toothpastes have significant shortcomings in their design for cleaning and removing plaque. They often rely on a high proportion of hard abrasives as the core cleaning ingredient, completely lacking the combination and synergy of gentle cleaning components. Their cleaning method is simplistic and harsh, relying solely on strong physical abrasion to remove plaque. This cleaning method can easily cause mechanical wear on tooth enamel. Long-term continuous use will directly lead to the gradual thinning of the enamel layer, a decrease in hardness, and the loss of an effective protective barrier for the teeth, resulting in tooth sensitivity problems. When exposed to stimuli such as hot, cold, sour, or sweet, toothpastes are prone to causing pain. They fail to achieve both cleaning effectiveness and enamel protection, and also damage the basic health of teeth. Summary of the Invention

[0004] The purpose of this invention is to provide a toothpaste formula that protects tooth enamel and removes plaque in order to solve the above-mentioned problems.

[0005] The present invention achieves the above objectives through the following technical solutions: This invention provides a toothpaste formula for protecting tooth enamel and removing plaque, comprising the following ingredients by weight percentage: 15-20% hydrated silica, 3-6% xylitol, 5-8% polyethylene glycol, 0.5-1.5% sodium lauryl sulfate, 0.3-0.5% cocamidopropyl betaine, 0.3-0.8% xanthan gum, 20-28% glycerin, 0.3-0.5% peppermint oil, 0.7-1.4% carboxymethyl cellulose gum, 3-5% cherry blossom extract, 1-5% Daphne odora fiber powder, and 2-5% Senna extract, with the remainder being deionized water; the sum of the weight percentages of all ingredients is 100%.

[0006] As a further optimization of the present invention, the preparation process of the cherry extract is as follows: (a) Select green hairy cherry fruits, remove the stems, wash them clean, and dry them. Mix the dried green hairy cherry fruits with deionized water, crush them into a fine pulp, add vitamin C and citric acid, and mix them in the dark to obtain green fruit pulp. (ii) Add the green plum pulp to a 50% ethanol aqueous solution at a material-to-liquid ratio of 1:10 (g / mL), reflux at 60℃ for 1.5-2 hours, repeat 1-3 times, and combine the extracts; (III) The extract was filtered through four layers of gauze to remove the fruit residue and obtain green fruit liquid. The green fruit liquid was then filtered through a 0.45μm microporous membrane. The filtered green fruit liquid was placed in a rotary evaporator and the vacuum degree was controlled at 0.08-0.09MPa and the water bath temperature at 55-65℃. The liquid was concentrated under reduced pressure to 1 / 5 of the original volume and cooled to room temperature to obtain the hairy cherry extract.

[0007] As a further optimization of the present invention, the preparation process of the euphorbia humifusa fiber powder is as follows: (a) Select 2-3 year old Daphne odora branches, cut the branches, remove leaves, tender shoots and impurities, put the branches into a steamer, steam at normal pressure for 2-8 hours, peel off the bark, scrape off the outer brown cork, and obtain Daphne odora bast fiber. (ii) Place the bast fiber of Daphne odora in a container, add 5% sodium hydroxide aqueous solution, boil at 100℃ for 60-120 minutes, cool naturally to 70-80℃, add 3-5% hydrogen peroxide and keep warm for 30-60 minutes, add acetic acid and soak for 5-10 minutes, wash with water until pH 6.5-7.5 to obtain Daphne odora fiber material; (iii) Use an air jet mill to grind the resinous material to 300-500 mesh to obtain resinous fiber powder.

[0008] As a further optimization of the present invention, the preparation process of the snowdrop extract is as follows: (a) Take the whole plant of Snowdrop during the flowering period, remove mud, sand, withered leaves and impurities, dry it at a low temperature of 40-50℃, and then pulverize it through a 40-60 mesh sieve to obtain Snowdrop plant powder. (ii) Add the powdered *Symplocos edulis* plant to a 60-80% ethanol aqueous solution at a material-to-liquid ratio of 1:10 (g / mL), reflux at 80℃ for 1.5-2 hours, repeat 1-2 times, combine the extracts, place the extracts in a rotary evaporator, control the vacuum degree at 0.08-0.09MPa and the water bath temperature at 50-65℃, concentrate under reduced pressure to 1 / 5 of the original volume, cool to room temperature, and then pulverize through a 200-300 mesh sieve to obtain *Symplocos edulis* extract.

[0009] As a further optimization of the present invention, the mass ratio of green hairy cherry fruit, deionized water, vitamin C and citric acid is 1:1:0.08:0.06.

[0010] As a further optimization of the present invention, the mass ratio of Daphne odora bast fiber, 5% sodium hydroxide aqueous solution and hydrogen peroxide is 1:15:5.

[0011] The method for preparing toothpaste includes the following steps: S1, according to the formula ratio, first mix xylitol, sodium lauryl sulfate, cocamidopropyl betaine, cherry extract, and snow jasmine extract with 2 / 3 of the formula amount of deionized water, and after mixing, obtain an aqueous solution. S2, mix xanthan gum, carboxymethyl cellulose gum and 1 / 3 of the formula amount of glycerin, and stir to make a uniform paste; S3. Pour the aqueous solution into a high-shear mixing vessel and start stirring at 300-500 r / min. Heat to 45-55℃, add the gel, and continue stirring for 30-45 min. Add the remaining glycerin and continue stirring for 10-15 min. Maintain the temperature at 45-55℃ and adjust the stirring speed to 400-600 r / min. Add hydrated silica and eucalyptus fiber powder and continue stirring for 30-40 min until the paste is smooth and free of lumps. S4, stop heating, reduce the temperature inside the reactor to 35-40℃, add liquid polyethylene glycol, stir for 10 minutes, add peppermint oil dropwise, start stirring at 600-800 r / min, stir for 15-20 minutes, add the remaining deionized water, stir for 20-30 minutes to obtain the paste; S5. Place the mixed paste in a vacuum degassing machine, control the vacuum degree to 0.07-0.08MPa, degas for 10-15 minutes, fill and seal to obtain the finished toothpaste.

[0012] The beneficial effects of this invention are as follows: In this formula, the total polyphenols in the cherry extract and the total flavonoids in the snow jasmine extract form a synergistic antibacterial effect, which can directly inhibit the reproduction of dental plaque pathogens, resulting in a significant reduction of oral pathogens after toothpaste use; through the synergistic cleaning system of "flexible adsorption + moderate grinding" formed by the euphorbia fiber powder and hydrated silica, it can physically adsorb plaque residue on the tooth surface, and its flexible fiber properties avoid excessive friction on the enamel, so as to protect the enamel while effectively removing dental plaque, achieving the triple effect of "antibacterial plaque removal + physical plaque removal + enamel protection", which greatly improves the comprehensive performance of toothpaste in cleaning and protecting teeth. Detailed Implementation

[0013] The present application will now be described in further detail. It should be noted that the following specific embodiments are only used to further illustrate the present application and should not be construed as limiting the scope of protection of the present application. Those skilled in the art can make some non-essential improvements and adjustments to the present application based on the above application content.

[0014] Unless otherwise specified, all methods used in this invention are conventional methods known to those skilled in the art, and all reagents and materials used are commercially available products. Example 1

[0015] The toothpaste formula contains the following ingredients by weight percentage: hydrated silica 15%, xylitol 3%, polyethylene glycol 5%, sodium lauryl sulfate 0.5%, cocamidopropyl betaine 0.3%, xanthan gum 0.3%, glycerin 20%, peppermint oil 0.3%, carboxymethyl cellulose gum 0.7%, wild cherry extract 3%, Daphne odora fiber powder 1%, and Senna alexandrina extract 2%, with the remainder being deionized water; the sum of the weight percentages of all ingredients is 100%. The preparation process of the cherry extract is as follows: (a) Select green hairy cherry fruits, remove the stems, wash them clean, and dry them. Mix the dried green hairy cherry fruits with deionized water, crush them into a fine pulp, add vitamin C and citric acid, and mix them in the dark to obtain green fruit pulp (the mass ratio of green hairy cherry fruits, deionized water, vitamin C and citric acid is 1:1:0.08:0.06). (ii) Add the green plum pulp to a 50% ethanol aqueous solution at a material-to-liquid ratio of 1:10 (g / mL), reflux at 60℃ for 1.5 h, repeat once, and combine the extracts; (III) The extract was filtered through four layers of gauze to remove the fruit residue and obtain green fruit liquid. The green fruit liquid was filtered through a 0.45μm microporous membrane. The filtered green fruit liquid was placed in a rotary evaporator, and the vacuum degree was controlled at 0.08MPa and the water bath temperature at 55℃. The liquid was concentrated under reduced pressure to 1 / 5 of the original volume. After cooling to room temperature, the hairy cherry extract was obtained. The preparation process of Daphne odora fiber powder is as follows: (a) Select two-year-old Daphne odora branches, cut the branches, remove leaves, tender shoots and impurities, put the branches into a steamer, steam at normal pressure for 2 hours, peel off the bark, scrape off the outer brown cork, and obtain Daphne odora bast fiber. (ii) Place the bast fiber of *Dendrobium nobile* in a container, add 5% sodium hydroxide aqueous solution, boil at 100℃ for 60 minutes, cool naturally to 70℃, add 3% hydrogen peroxide and keep warm for 30 minutes, add acetic acid and soak for 5 minutes, wash with water until pH 6.5, and obtain *Dendrobium nobile* fiber material (mass ratio of *Dendrobium nobile* bast fiber, 5% sodium hydroxide aqueous solution and hydrogen peroxide is 1:15:5). (iii) The resin fiber material is pulverized to 300 mesh using an air jet mill to obtain resin fiber powder; The preparation process of snowdrop extract is as follows: (a) Take the whole plant of Snowdrop during the flowering period, remove mud, sand, withered leaves and impurities, dry it at a low temperature of 40℃, and then pulverize it through a 40-mesh sieve to obtain Snowdrop plant powder. (ii) Add the powder of *Symplocos edulis* plant to a 60% ethanol aqueous solution at a material-to-liquid ratio of 1:10 (g / mL), reflux at 80℃ for 1.5 h, repeat once, combine the extracts, place the extract in a rotary evaporator, control the vacuum degree at 0.08 MPa and the water bath temperature at 50℃, concentrate under reduced pressure to 1 / 5 of the original volume, cool to room temperature, and then pulverize through a 200-mesh sieve to obtain *Symplocos edulis* extract; The toothpaste preparation process is as follows: S1, according to the formula ratio, first mix xylitol, sodium lauryl sulfate, cocamidopropyl betaine, cherry extract, and snow jasmine extract with 2 / 3 of the formula amount of deionized water, and after mixing, obtain an aqueous solution. S2, mix xanthan gum, carboxymethyl cellulose gum and 1 / 3 of the formula amount of glycerin, and stir to make a uniform paste; S3. Add the aqueous solution to the high-shear mixing vessel, start stirring at 300 r / min, heat to 45℃, add the gel, continue stirring for 30 min, add the remaining glycerin, continue stirring for 10 min, keep the temperature at 45℃, adjust the stirring speed to 400 r / min, add hydrated silica and eugenol fiber powder, continue stirring for 30 min until the paste is smooth and free of lumps. S4, stop heating, reduce the temperature inside the vessel to 35°C, add liquid polyethylene glycol, stir for 10 minutes, add peppermint oil dropwise, start stirring at 600 r / min, stir for 15 minutes, add the remaining deionized water, stir for 20 minutes to obtain the paste; S5. Place the mixed paste in a vacuum degassing machine, control the vacuum degree to 0.07MPa, degas for 10 minutes, fill and seal to obtain the finished toothpaste. Example 2

[0016] The toothpaste formula contains the following ingredients by weight percentage: hydrated silica 18%, xylitol 5%, polyethylene glycol 6%, sodium lauryl sulfate 1%, cocamidopropyl betaine 0.4%, xanthan gum 0.5%, glycerin 24%, peppermint oil 0.4%, carboxymethyl cellulose gum 1%, wild cherry extract 4%, Daphne odora fiber powder 3%, and Senna alexandrina extract 4%, with the remainder being deionized water; the sum of the weight percentages of all ingredients is 100%. The preparation process of the cherry extract is as follows: (a) Select green hairy cherry fruits, remove the stems, wash them clean, and dry them. Mix the dried green hairy cherry fruits with deionized water, crush them into a fine pulp, add vitamin C and citric acid, and mix them in the dark to obtain green fruit pulp (the mass ratio of green hairy cherry fruits, deionized water, vitamin C and citric acid is 1:1:0.08:0.06). (ii) Add the green plum pulp to a 50% ethanol aqueous solution at a material-to-liquid ratio of 1:10 (g / mL), reflux at 60℃ for 1.7 h, repeat twice, and combine the extracts; (III) The extract was filtered through four layers of gauze to remove the fruit residue and obtain green fruit liquid. The green fruit liquid was filtered through a 0.45μm microporous membrane. The filtered green fruit liquid was placed in a rotary evaporator, and the vacuum degree was controlled at 0.08MPa and the water bath temperature at 60℃. The liquid was concentrated under reduced pressure to 1 / 5 of the original volume. After cooling to room temperature, the hairy cherry extract was obtained. The preparation process of Daphne odora fiber powder is as follows: (a) Select 3-year-old Daphne odora branches, cut the branches, remove leaves, tender shoots and impurities, put the branches into a steamer, steam at normal pressure for 5 hours, peel off the bark, scrape off the outer brown cork, and obtain Daphne odora bast fiber. (ii) Place the bast fiber of *Dendrobium nobile* in a container, add 5% sodium hydroxide aqueous solution, boil at 100℃ for 85 minutes, cool naturally to 75℃, add 4% hydrogen peroxide and keep warm for 45 minutes, add acetic acid and soak for 8 minutes, wash with water until pH 7.0 to obtain *Dendrobium nobile* fiber material (mass ratio of *Dendrobium nobile* bast fiber, 5% sodium hydroxide aqueous solution and hydrogen peroxide is 1:15:5). (iii) The resin fiber material is pulverized to 400 mesh using an air jet mill to obtain resin fiber powder; The preparation process of snowdrop extract is as follows: (a) Take the whole plant of Snowdrop during the flowering period, remove mud, sand, withered leaves and impurities, dry it at a low temperature of 45℃, and then pulverize it through a 50-mesh sieve to obtain Snowdrop plant powder. (ii) Add the powder of *Symplocos edulis* plant to a 70% ethanol aqueous solution at a material-to-liquid ratio of 1:10 (g / mL), reflux at 80℃ for 1.8 h, repeat twice, combine the extracts, place the extract in a rotary evaporator, control the vacuum degree at 0.09 MPa and the water bath temperature at 55℃, concentrate under reduced pressure to 1 / 5 of the original volume, cool to room temperature, and then pulverize through a 250-mesh sieve to obtain *Symplocos edulis* extract; The toothpaste preparation process is as follows: S1, according to the formula ratio, first mix xylitol, sodium lauryl sulfate, cocamidopropyl betaine, cherry extract, and snow jasmine extract with 2 / 3 of the formula amount of deionized water, and after mixing, obtain an aqueous solution. S2, mix xanthan gum, carboxymethyl cellulose gum and 1 / 3 of the formula amount of glycerin, and stir to make a uniform paste; S3. Add the aqueous solution to the high-shear mixing vessel, start stirring at 400 r / min, heat to 50℃, add the gel, continue stirring for 40 min, add the remaining glycerin, continue stirring for 12 min, keep the temperature at 50℃, adjust the stirring speed to 500 r / min, add hydrated silica and eucalyptus fiber powder, continue stirring for 35 min until the paste is smooth and free of lumps. S4, stop heating, reduce the temperature inside the vessel to 37°C, add liquid polyethylene glycol, stir for 10 minutes, add peppermint oil dropwise, start stirring at 700 r / min, stir for 18 minutes, add the remaining deionized water, stir for 25 minutes to obtain the paste; S5. Place the mixed paste in a vacuum degassing machine, control the vacuum degree to 0.08MPa, degas for 12 minutes, fill and seal to obtain the finished toothpaste. Example 3

[0017] The toothpaste formula contains the following ingredients by weight percentage: hydrated silica 20%, xylitol 6%, polyethylene glycol 8%, sodium lauryl sulfate 1.5%, cocamidopropyl betaine 0.5%, xanthan gum 0.8%, glycerin 28%, peppermint oil 0.5%, carboxymethyl cellulose gum 1.4%, wild cherry extract 5%, Daphne odora fiber powder 5%, and Senna alexandrina extract 5%, with the remainder being deionized water; the sum of the weight percentages of all ingredients is 100%. The preparation process of the cherry extract is as follows: (a) Select green hairy cherry fruits, remove the stems, wash them clean, and dry them. Mix the dried green hairy cherry fruits with deionized water, crush them into a fine pulp, add vitamin C and citric acid, and mix them in the dark to obtain green fruit pulp (the mass ratio of green hairy cherry fruits, deionized water, vitamin C and citric acid is 1:1:0.08:0.06). (ii) Add the green plum pulp to a 50% ethanol aqueous solution at a material-to-liquid ratio of 1:10 (g / mL), reflux at 60℃ for 2 hours, repeat 3 times, and combine the extracts; (III) The extract was filtered through four layers of gauze to remove the fruit residue and obtain green fruit liquid. The green fruit liquid was filtered through a 0.45μm microporous membrane. The filtered green fruit liquid was placed in a rotary evaporator, and the vacuum degree was controlled at 0.09MPa and the water bath temperature at 65℃. The liquid was concentrated under reduced pressure to 1 / 5 of the original volume. After cooling to room temperature, the hairy cherry extract was obtained. The preparation process of Daphne odora fiber powder is as follows: (a) Select 3-year-old Daphne odora branches, cut the branches, remove leaves, tender shoots and impurities, put the branches into a steamer, steam at normal pressure for 8 hours, peel off the bark, scrape off the outer brown cork, and obtain Daphne odora bast fiber. (ii) Place the bast fiber of *Dendrobium nobile* in a container, add 5% sodium hydroxide aqueous solution, boil at 100℃ for 120 minutes, cool naturally to 80℃, add 5% hydrogen peroxide and keep warm for 60 minutes, add acetic acid and soak for 10 minutes, wash with water until pH 7.5, and obtain *Dendrobium nobile* fiber material (mass ratio of *Dendrobium nobile* bast fiber, 5% sodium hydroxide aqueous solution and hydrogen peroxide is 1:15:5). (iii) The resinous material is pulverized to 500 mesh using an air jet mill to obtain resinous fiber powder; The preparation process of snowdrop extract is as follows: (a) Take the whole plant of Snowdrop during the flowering period, remove mud, sand, withered leaves and impurities, dry it at a low temperature of 50℃, and then pulverize it through a 60-mesh sieve to obtain Snowdrop plant powder. (ii) Add the powder of *Symplocos edulis* plant to an 80% ethanol aqueous solution at a material-to-liquid ratio of 1:10 (g / mL), reflux at 80℃ for 2 hours, repeat twice, combine the extracts, place the extract in a rotary evaporator, control the vacuum degree at 0.09MPa and the water bath temperature at 65℃, concentrate under reduced pressure to 1 / 5 of the original volume, cool to room temperature, and then pulverize through a 300-mesh sieve to obtain *Symplocos edulis* extract; The toothpaste preparation process is as follows: S1, according to the formula ratio, first mix xylitol, sodium lauryl sulfate, cocamidopropyl betaine, cherry extract, and snow jasmine extract with 2 / 3 of the formula amount of deionized water, and after mixing, obtain an aqueous solution. S2, mix xanthan gum, carboxymethyl cellulose gum and 1 / 3 of the formula amount of glycerin, and stir to make a uniform paste; S3. Add the aqueous solution to the high-shear mixing vessel, start stirring at 500 r / min, heat to 55℃, add the gel, continue stirring for 45 min, add the remaining glycerin, continue stirring for 15 min, keep the temperature at 55℃, adjust the stirring speed to 600 r / min, add hydrated silica and eugenol fiber powder, continue stirring for 40 min until the paste is smooth and free of lumps. S4, stop heating, reduce the temperature inside the vessel to 40℃, add liquid polyethylene glycol, stir for 10 minutes, add peppermint oil dropwise, start stirring at 800 r / min, stir for 20 minutes, add the remaining deionized water, stir for 30 minutes to obtain the paste; S5. Place the mixed paste in a vacuum degassing machine, control the vacuum degree to 0.08MPa, degas for 15 minutes, fill and seal to obtain the finished toothpaste.

[0018] Comparative Example 1 The toothpaste formula contains the following ingredients by weight percentage: hydrated silica 21%, xylitol 5%, polyethylene glycol 6%, sodium lauryl sulfate 1%, cocamidopropyl betaine 0.4%, xanthan gum 0.5%, glycerin 24%, peppermint oil 0.4%, carboxymethyl cellulose gum 1%, wild cherry extract 4%, and snowdrop extract 4%, with the remainder being deionized water; the sum of the weight percentages of all ingredients is 100%. The preparation process of the cherry extract is as follows: (a) Select green hairy cherry fruits, remove the stems, wash them clean, and dry them. Mix the dried green hairy cherry fruits with deionized water, crush them into a fine pulp, add vitamin C and citric acid, and mix them in the dark to obtain green fruit pulp (the mass ratio of green hairy cherry fruits, deionized water, vitamin C and citric acid is 1:1:0.08:0.06). (ii) Add the green plum pulp to a 50% ethanol aqueous solution at a material-to-liquid ratio of 1:10 (g / mL), reflux at 60℃ for 1.7 h, repeat twice, and combine the extracts; (III) The extract was filtered through four layers of gauze to remove the fruit residue and obtain green fruit liquid. The green fruit liquid was filtered through a 0.45μm microporous membrane. The filtered green fruit liquid was placed in a rotary evaporator, and the vacuum degree was controlled at 0.08MPa and the water bath temperature at 60℃. The liquid was concentrated under reduced pressure to 1 / 5 of the original volume. After cooling to room temperature, the hairy cherry extract was obtained. The preparation process of snowdrop extract is as follows: (a) Take the whole plant of Snowdrop during the flowering period, remove mud, sand, withered leaves and impurities, dry it at a low temperature of 45℃, and then pulverize it through a 50-mesh sieve to obtain Snowdrop plant powder. (ii) Add the powder of *Symplocos edulis* plant to a 70% ethanol aqueous solution at a material-to-liquid ratio of 1:10 (g / mL), reflux at 80℃ for 1.8 h, repeat twice, combine the extracts, place the extract in a rotary evaporator, control the vacuum degree at 0.09 MPa and the water bath temperature at 55℃, concentrate under reduced pressure to 1 / 5 of the original volume, cool to room temperature, and then pulverize through a 250-mesh sieve to obtain *Symplocos edulis* extract; The toothpaste preparation process is as follows: S1, according to the formula ratio, first mix xylitol, sodium lauryl sulfate, cocamidopropyl betaine, cherry extract, and snow jasmine extract with 2 / 3 of the formula amount of deionized water, and after mixing, obtain an aqueous solution. S2, mix xanthan gum, carboxymethyl cellulose gum and 1 / 3 of the formula amount of glycerin, and stir to make a uniform paste; S3. Add the aqueous solution to the high-shear mixing vessel, start stirring at 400 r / min, heat to 50℃, add the gel, continue stirring for 40 min, add the remaining glycerin, continue stirring for 12 min, keep the temperature at 50℃, adjust the stirring speed to 500 r / min, add hydrated silica, continue stirring for 35 min, until the paste is smooth and free of lumps. S4, stop heating, reduce the temperature inside the vessel to 37°C, add liquid polyethylene glycol, stir for 10 minutes, add peppermint oil dropwise, start stirring at 700 r / min, stir for 18 minutes, add the remaining deionized water, stir for 25 minutes to obtain the paste; S5. Place the mixed paste in a vacuum degassing machine, control the vacuum degree to 0.08MPa, degas for 12 minutes, fill and seal to obtain the finished toothpaste.

[0019] Comparative Example 2 The toothpaste formula contains the following ingredients by weight percentage: xylitol 5%, polyethylene glycol 6%, sodium lauryl sulfate 1%, cocamidopropyl betaine 0.4%, xanthan gum 0.5%, glycerin 24%, peppermint oil 0.4%, carboxymethyl cellulose gum 1%, wild cherry extract 4%, Daphne odora fiber powder 21%, and Senna alexandrina extract 4%, with the remainder being deionized water; the sum of the weight percentages of all ingredients is 100%. The preparation process of the cherry extract is as follows: (a) Select green hairy cherry fruits, remove the stems, wash them clean, and dry them. Mix the dried green hairy cherry fruits with deionized water, crush them into a fine pulp, add vitamin C and citric acid, and mix them in the dark to obtain green fruit pulp (the mass ratio of green hairy cherry fruits, deionized water, vitamin C and citric acid is 1:1:0.08:0.06). (ii) Add the green plum pulp to a 50% ethanol aqueous solution at a material-to-liquid ratio of 1:10 (g / mL), reflux at 60℃ for 1.7 h, repeat twice, and combine the extracts; (III) The extract was filtered through four layers of gauze to remove the fruit residue and obtain green fruit liquid. The green fruit liquid was filtered through a 0.45μm microporous membrane. The filtered green fruit liquid was placed in a rotary evaporator, and the vacuum degree was controlled at 0.08MPa and the water bath temperature at 60℃. The liquid was concentrated under reduced pressure to 1 / 5 of the original volume. After cooling to room temperature, the hairy cherry extract was obtained. The preparation process of Daphne odora fiber powder is as follows: (a) Select 3-year-old Daphne odora branches, cut the branches, remove leaves, tender shoots and impurities, put the branches into a steamer, steam at normal pressure for 5 hours, peel off the bark, scrape off the outer brown cork, and obtain Daphne odora bast fiber. (ii) Place the bast fiber of *Dendrobium nobile* in a container, add 5% sodium hydroxide aqueous solution, boil at 100℃ for 85 minutes, cool naturally to 75℃, add 4% hydrogen peroxide and keep warm for 45 minutes, add acetic acid and soak for 8 minutes, wash with water until pH 7.0 to obtain *Dendrobium nobile* fiber material (mass ratio of *Dendrobium nobile* bast fiber, 5% sodium hydroxide aqueous solution and hydrogen peroxide is 1:15:5). (iii) The resin fiber material is pulverized to 400 mesh using an air jet mill to obtain resin fiber powder; The preparation process of snowdrop extract is as follows: (a) Take the whole plant of Snowdrop during the flowering period, remove mud, sand, withered leaves and impurities, dry it at a low temperature of 45℃, and then pulverize it through a 50-mesh sieve to obtain Snowdrop plant powder. (ii) Add the powder of *Symplocos edulis* plant to a 70% ethanol aqueous solution at a material-to-liquid ratio of 1:10 (g / mL), reflux at 80℃ for 1.8 h, repeat twice, combine the extracts, place the extract in a rotary evaporator, control the vacuum degree at 0.09 MPa and the water bath temperature at 55℃, concentrate under reduced pressure to 1 / 5 of the original volume, cool to room temperature, and then pulverize through a 250-mesh sieve to obtain *Symplocos edulis* extract; The toothpaste preparation process is as follows: S1, according to the formula ratio, first mix xylitol, sodium lauryl sulfate, cocamidopropyl betaine, cherry extract, and snow jasmine extract with 2 / 3 of the formula amount of deionized water, and after mixing, obtain an aqueous solution. S2, mix xanthan gum, carboxymethyl cellulose gum and 1 / 3 of the formula amount of glycerin, and stir to make a uniform paste; S3. Add the aqueous solution to the high-shear mixing vessel, start stirring at 400 r / min, heat to 50℃, add the gel, continue stirring for 40 min, add the remaining glycerin, continue stirring for 12 min, keep the temperature at 50℃, adjust the stirring speed to 500 r / min, add the euphorbia fiber powder, continue stirring for 35 min, until the paste is smooth and free of lumps. S4, stop heating, reduce the temperature inside the vessel to 37°C, add liquid polyethylene glycol, stir for 10 minutes, add peppermint oil dropwise, start stirring at 700 r / min, stir for 18 minutes, add the remaining deionized water, stir for 25 minutes to obtain the paste; S5. Place the mixed paste in a vacuum degassing machine, control the vacuum degree to 0.08MPa, degas for 12 minutes, fill and seal to obtain the finished toothpaste.

[0020] Comparative Example 3 The toothpaste formula contains the following ingredients by weight percentage: hydrated silica 18%, xylitol 5%, polyethylene glycol 6%, sodium lauryl sulfate 1%, cocamidopropyl betaine 0.4%, xanthan gum 0.5%, glycerin 24%, peppermint oil 0.4%, carboxymethyl cellulose gum 1%, wild cherry extract 8%, and euphorbia citric acid fiber powder 3%, with the remainder being deionized water; the sum of the weight percentages of all ingredients is 100%. The preparation process of the cherry extract is as follows: (a) Select green hairy cherry fruits, remove the stems, wash them clean, and dry them. Mix the dried green hairy cherry fruits with deionized water, crush them into a fine pulp, add vitamin C and citric acid, and mix them in the dark to obtain green fruit pulp (the mass ratio of green hairy cherry fruits, deionized water, vitamin C and citric acid is 1:1:0.08:0.06). (ii) Add the green plum pulp to a 50% ethanol aqueous solution at a material-to-liquid ratio of 1:10 (g / mL), reflux at 60℃ for 1.7 h, repeat twice, and combine the extracts; (III) The extract was filtered through four layers of gauze to remove the fruit residue and obtain green fruit liquid. The green fruit liquid was filtered through a 0.45μm microporous membrane. The filtered green fruit liquid was placed in a rotary evaporator, and the vacuum degree was controlled at 0.08MPa and the water bath temperature at 60℃. The liquid was concentrated under reduced pressure to 1 / 5 of the original volume. After cooling to room temperature, the hairy cherry extract was obtained. The preparation process of Daphne odora fiber powder is as follows: (a) Select 3-year-old Daphne odora branches, cut the branches, remove leaves, tender shoots and impurities, put the branches into a steamer, steam at normal pressure for 5 hours, peel off the bark, scrape off the outer brown cork, and obtain Daphne odora bast fiber. (ii) Place the bast fiber of *Dendrobium nobile* in a container, add 5% sodium hydroxide aqueous solution, boil at 100℃ for 85 minutes, cool naturally to 75℃, add 4% hydrogen peroxide and keep warm for 45 minutes, add acetic acid and soak for 8 minutes, wash with water until pH 7.0 to obtain *Dendrobium nobile* fiber material (mass ratio of *Dendrobium nobile* bast fiber, 5% sodium hydroxide aqueous solution and hydrogen peroxide is 1:15:5). (iii) The resin fiber material is pulverized to 400 mesh using an air jet mill to obtain resin fiber powder; The toothpaste preparation process is as follows: S1. According to the formula ratio, xylitol, sodium lauryl sulfate, cocamidopropyl betaine, and cherry extract are mixed with 2 / 3 of the formula amount of deionized water and mixed well to obtain an aqueous solution. S2, mix xanthan gum, carboxymethyl cellulose gum and 1 / 3 of the formula amount of glycerin, and stir to make a uniform paste; S3. Add the aqueous solution to the high-shear mixing vessel, start stirring at 400 r / min, heat to 50℃, add the gel, continue stirring for 40 min, add the remaining glycerin, continue stirring for 12 min, keep the temperature at 50℃, adjust the stirring speed to 500 r / min, add hydrated silica and eucalyptus fiber powder, continue stirring for 35 min until the paste is smooth and free of lumps. S4, stop heating, reduce the temperature inside the vessel to 37°C, add liquid polyethylene glycol, stir for 10 minutes, add peppermint oil dropwise, start stirring at 700 r / min, stir for 18 minutes, add the remaining deionized water, stir for 25 minutes to obtain the paste; S5. Place the mixed paste in a vacuum degassing machine, control the vacuum degree to 0.08MPa, degas for 12 minutes, fill and seal to obtain the finished toothpaste.

[0021] Comparative Example 4 The toothpaste formula contains the following ingredients by weight percentage: hydrated silica 18%, xylitol 5%, polyethylene glycol 6%, sodium lauryl sulfate 1%, cocamidopropyl betaine 0.4%, xanthan gum 0.5%, glycerin 24%, peppermint oil 0.4%, carboxymethyl cellulose gum 1%, euphorbia citrifolia fiber powder 3%, and snowdrop extract 8%, with the remainder being deionized water; the sum of the weight percentages of all ingredients is 100%. The preparation process of the cherry extract is as follows: (a) Select green hairy cherry fruits, remove the stems, wash them clean, and dry them. Mix the dried green hairy cherry fruits with deionized water, crush them into a fine pulp, add vitamin C and citric acid, and mix them in the dark to obtain green fruit pulp (the mass ratio of green hairy cherry fruits, deionized water, vitamin C and citric acid is 1:1:0.08:0.06). (ii) Add the green plum pulp to a 50% ethanol aqueous solution at a material-to-liquid ratio of 1:10 (g / mL), reflux at 60℃ for 1.7 h, repeat twice, and combine the extracts; (III) The extract was filtered through four layers of gauze to remove the fruit residue and obtain green fruit liquid. The green fruit liquid was filtered through a 0.45μm microporous membrane. The filtered green fruit liquid was placed in a rotary evaporator, and the vacuum degree was controlled at 0.08MPa and the water bath temperature at 60℃. The liquid was concentrated under reduced pressure to 1 / 5 of the original volume. After cooling to room temperature, the hairy cherry extract was obtained. The preparation process of Daphne odora fiber powder is as follows: (a) Select 3-year-old Daphne odora branches, cut the branches, remove leaves, tender shoots and impurities, put the branches into a steamer, steam at normal pressure for 5 hours, peel off the bark, scrape off the outer brown cork, and obtain Daphne odora bast fiber. (ii) Place the bast fiber of *Dendrobium nobile* in a container, add 5% sodium hydroxide aqueous solution, boil at 100℃ for 85 minutes, cool naturally to 75℃, add 4% hydrogen peroxide and keep warm for 45 minutes, add acetic acid and soak for 8 minutes, wash with water until pH 7.0 to obtain *Dendrobium nobile* fiber material (mass ratio of *Dendrobium nobile* bast fiber, 5% sodium hydroxide aqueous solution and hydrogen peroxide is 1:15:5). (iii) The resin fiber material is pulverized to 400 mesh using an air jet mill to obtain resin fiber powder; The preparation process of snowdrop extract is as follows: (a) Take the whole plant of Snowdrop during the flowering period, remove mud, sand, withered leaves and impurities, dry it at a low temperature of 45℃, and then pulverize it through a 50-mesh sieve to obtain Snowdrop plant powder. (ii) Add the powder of *Symplocos edulis* plant to a 70% ethanol aqueous solution at a material-to-liquid ratio of 1:10 (g / mL), reflux at 80℃ for 1.8 h, repeat twice, combine the extracts, place the extract in a rotary evaporator, control the vacuum degree at 0.09 MPa and the water bath temperature at 55℃, concentrate under reduced pressure to 1 / 5 of the original volume, cool to room temperature, and then pulverize through a 250-mesh sieve to obtain *Symplocos edulis* extract; The toothpaste preparation process is as follows: S1. According to the formula ratio, xylitol, sodium lauryl sulfate, cocamidopropyl betaine, and snowdrop extract are mixed with 2 / 3 of the formula amount of deionized water and mixed well to obtain an aqueous solution. S2, mix xanthan gum, carboxymethyl cellulose gum and 1 / 3 of the formula amount of glycerin, and stir to make a uniform paste; S3. Add the aqueous solution to the high-shear mixing vessel, start stirring at 400 r / min, heat to 50℃, add the gel, continue stirring for 40 min, add the remaining glycerin, continue stirring for 12 min, keep the temperature at 50℃, adjust the stirring speed to 500 r / min, add hydrated silica and eucalyptus fiber powder, continue stirring for 35 min until the paste is smooth and free of lumps. S4, stop heating, reduce the temperature inside the vessel to 37°C, add liquid polyethylene glycol, stir for 10 minutes, add peppermint oil dropwise, start stirring at 700 r / min, stir for 18 minutes, add the remaining deionized water, stir for 25 minutes to obtain the paste; S5. Place the mixed paste in a vacuum degassing machine, control the vacuum degree to 0.08MPa, degas for 12 minutes, fill and seal to obtain the finished toothpaste.

[0022] Performance testing (a) The toothpastes in Examples 1-3 and Comparative Examples 1-4 were tested according to the methods in GB / T8372-2017 "Toothpaste". The test results are shown in Table 1.

[0023]

[0024] As shown in Table 1, the total bacterial count in the examples was only 80-85 CFU / g, far lower than the 94-98 CFU / g in the comparative examples, and the value was more stable. Meanwhile, the viscosity of the examples (11300-12000 mPa·s) was significantly higher than that of the comparative examples, and the lead and arsenic contents were also significantly lower, with a pH value closer to neutral. In summary, the examples showed superior antibacterial effects. Combined with better viscosity and heavy metal indicators, this fully demonstrates that the formulation and process significantly improved the product's hygiene, safety, and quality stability.

[0025] (ii) The toothpastes in Example 2 and Comparative Examples 1-4 were tested according to the method in GB / T35832-2025 "Test Method for Friction Value of Toothpaste". The test standards are shown in Table 2.

[0026]

[0027] As can be seen from Table 2, the RDA value of Example 2 is 210, which is the lowest among all samples; the RDA values ​​of Comparative Examples 1-4 are 215-235, which are all higher than that of Example 2. This result confirms that the synergistic system of "flexible euphorbia fiber powder + moderately ground hydrated silica" in the optimized formula effectively reduces the mechanical abrasion of tooth enamel by toothpaste, and significantly improves the enamel protection ability while ensuring the anti-plaque cleaning power.

[0028] The embodiments described above are merely examples of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention.

Claims

1. A toothpaste formulation for protecting the enamel and removing plaque, characterized in that it comprises: Raw materials including the following by weight percentage: hydrated silica 15-20%, xylitol 3-6%, polyethylene glycol 5-8%, sodium lauryl sulfate 0.5-1.5%, cocamidopropyl betaine 0.3-0.5%, xanthan gum 0.3-0.8%, glycerol 20-28%, peppermint oil 0.3-0.5%, carboxymethyl cellulose gum 0.7-1.4%, Prunus tomentosa extract 3-5%, Gossampinus malabarica fiber powder 1-5%, and Yushania niitakayamensis extract 2-5%, the rest being deionized water; the sum of the weight percentages of each raw material is 100%.

2. A toothpaste formulation for protecting enamel and removing plaque according to claim 1, wherein The preparation process of the Prunus tomentosa extract is as follows: (1) Green Prunus tomentosa fruits are selected, the fruit stems are removed, cleaned, and dried, and the dried green Prunus tomentosa fruits are mixed with deionized water, crushed into fine pulp, and mixed with vitamin C and citric acid in the dark to obtain green fruit pulp; (2) The green fruit pulp is added to 50% ethanol aqueous solution, the solid-liquid ratio is 1:10 (g / mL), and the mixture is extracted at 60°C for 1.5-2 h, repeated 1-3 times, and the extraction solutions are combined; (3) The extraction solution is filtered with four layers of gauze to remove the fruit residue, and the green fruit liquid is obtained, which is filtered with a 0.45 μm microporous filter membrane, and the filtered green fruit liquid is placed in a rotary evaporator, the vacuum degree is controlled at 0.08-0.09 MPa, the water bath temperature is controlled at 55-65°C, and the extraction solution is concentrated under reduced pressure to 1 / 5 of the original volume, and then cooled to room temperature to obtain the Prunus tomentosa extract.

3. A toothpaste formulation for protecting enamel and removing plaque according to claim 1, wherein The preparation process of the Gossampinus malabarica fiber powder is as follows: (1) 2-3 year old Gossampinus malabarica branches are selected, the branches are cut, the leaves, tender shoots, and impurities are removed, the branches are placed in a steamer, steamed at normal pressure for 2-8 h, the bark is peeled off, and the outer layer of brown bark is scraped off to obtain Gossampinus malabarica bast fiber; (2) The Gossampinus malabarica bast fiber is placed in a container and added with 5% sodium hydroxide aqueous solution, boiled at 100°C for 60-120 min, naturally cooled to 70-80°C, added with 3-5% hydrogen peroxide, and soaked for 30-60 min, added with acetic acid and soaked for 5-10 min, washed with water until the pH is 6.5-7.5 to obtain Gossampinus malabarica fiber material; (3) The Gossampinus malabarica fiber material is crushed to 300-500 mesh with an air flow crusher to obtain Gossampinus malabarica fiber powder.

4. The toothpaste formulation for protecting enamel and removing plaque according to claim 1, wherein The preparation process of the Yushania niitakayamensis extract is as follows: (1) Flowers of Yushania niitakayamensis are selected, and the mud, dry leaves, and impurities are removed, and the flowers are dried at a low temperature of 40-50°C, crushed to pass through a 40-60 mesh sieve to obtain Yushania niitakayamensis plant powder; (2) The Yushania niitakayamensis plant powder is added to 60-80% ethanol aqueous solution, the solid-liquid ratio is 1:10 (g / mL), and the mixture is extracted at 80°C for 1.5-2 h, repeated 1-2 times, and the extraction solutions are combined, and then placed in a rotary evaporator, the vacuum degree is controlled at 0.08-0.09 MPa, the water bath temperature is controlled at 50-65°C, and the extraction solution is concentrated under reduced pressure to 1 / 5 of the original volume, and then cooled to room temperature, crushed to pass through a 200-300 mesh sieve to obtain Yushania niitakayamensis extract.

5. A toothpaste formulation for protecting enamel and removing plaque according to claim 2, wherein The mass ratio of the green Prunus tomentosa fruits, deionized water, vitamin C, and citric acid is 1:1:0.08:0.

06.

6. A toothpaste formulation for protecting enamel and removing plaque according to claim 3, wherein The mass ratio of the Gossampinus malabarica bast fiber, 5% sodium hydroxide aqueous solution, and hydrogen peroxide is 1:15:

5.

7. A process for the preparation of a toothpaste according to any one of claims 1 to 6, characterised in that, The method comprises the following steps: S1, according to the formula proportion, first xylitol, sodium lauryl sulfate, cocamide propyl betaine, cherry extract, snow extract and 2 / 3 of the formula amount of deionized water were mixed, and a water phase solution was obtained after mixing uniformly; S2, xanthan gum, carboxymethyl cellulose gum and 1 / 3 of the formula amount of glycerol were mixed and stirred to form a uniform glue slurry; S3, the water phase solution was put into a high shear mixing kettle, the stirring was started at a speed of 300-500 r / min, the temperature was raised to 45-55℃, the glue slurry was added, the stirring was continued for 30-45 min, the remaining glycerol was added, the stirring was continued for 10-15 min, the temperature was kept at 45-55℃, the stirring speed was adjusted to 400-600 r / min, hydrated silica and konjac fiber powder were added, the stirring was continued for 30-40 min, until the paste was fine and free of lumps; S4, stop heating, reduce the temperature in the kettle to 35-40℃, add liquid polyethylene glycol, stir for 10 min, add peppermint oil dropwise, start stirring at a speed of 600-800 r / min, stir for 15-20 min, add the remaining deionized water, stir for 20-30 min, to obtain a paste; S5, the mixed paste was placed in a vacuum defoaming machine, the vacuum degree was controlled at 0.07-0.08 MPa, defoaming was carried out for 10-15 min, filling, sealing, to obtain the finished toothpaste.

Images