A whitening and stain-removing toothpaste and its preparation method

Abstract

This invention relates to a whitening and stain-removing toothpaste and its preparation method, belonging to the field of oral care technology. The toothpaste contains 1.5-2.5 parts of plant enzymatic hydrolysate, 15-25 parts of a composite abrasive, and other components. The plant enzymatic hydrolysate is obtained by grinding walnut shell powder, beech, oyster shell, and Manegug glacial mud into powder in a mass ratio of 3:3:2:1, and then mixing and enzymatically hydrolyzing it with a composite enzyme solution. The composite abrasive and chelating agent are substances of specific particle sizes / molecular weights mixed in proportion. It also contains film-forming agents and enamel repair components. The preparation process includes the preparation of the plant enzymatic hydrolysate, the preparation of the mixture, and subsequent stirring, degassing, and filling steps. This toothpaste achieves highly effective whitening and stain removal, antibacterial properties, and long-lasting stain prevention, enamel repair, and antioxidant effects through the synergistic effect of multiple components, solving the problems of incomplete stain removal and enamel damage caused by traditional toothpastes.

Description

Technical Field

[0001] This invention belongs to the field of oral care technology and relates to a whitening and stain-removing toothpaste and its preparation method. Background Technology

[0002] Oral stains primarily arise from colored substances adhering to the tooth surface, which then combine with metal ions and mineralize to form stubborn stains. Traditional toothpastes often rely on single abrasives or chemical ingredients, resulting in incomplete stain removal and potential damage to tooth enamel. While existing technologies employ plant extracts to assist in whitening, anti-inflammatory, antibacterial, and stain prevention, they lack systematic optimization of plant species, formulation ratios, and extraction methods, leading to insufficient release of active ingredients and limited synergistic effects.

[0003] Therefore, developing a toothpaste that combines extracts prepared by specific plant formulations and enzymatic hydrolysis with compound enzyme solutions, along with components such as compound abrasives and chelating agents, to achieve highly effective whitening, stain removal, antibacterial properties, and long-lasting stain prevention has become an important direction in this field. Summary of the Invention

[0004] The purpose of this invention is to provide a whitening and stain-removing toothpaste and its preparation method. By providing a toothpaste prepared by enzymatic hydrolysis of walnut shell powder, beech, oyster shell and Manegug glacial mud, the toothpaste achieves highly effective whitening, stain removal, antibacterial, stain prevention and enamel repair effects through the synergistic effect of enzymatic hydrolysate and components such as composite abrasive and chelating agent.

[0005] The objective of this invention can be achieved through the following technical solutions:

[0006] A whitening and stain-removing toothpaste, by weight, comprises the following components: 1.5-2.5 parts plant enzymatic hydrolysate, 15-25 parts compound abrasive, 1-3 parts compound chelating agent, 0.5-2 parts film-forming agent, 2-5 parts enamel repairing ingredient, 20-30 parts moisturizer, 0.5-1.5 parts thickener, 1-3 parts foaming agent, 0.1-0.5 parts sweetener, 0.05-0.3 parts preservative, 0.05-0.1 parts fragrance, and deionized water to make up to 100 parts.

[0007] As a preferred technical solution of the present invention, the plant enzymatic hydrolysate is obtained by grinding walnut shell powder, beech, oyster shell and Manegug glacial mud into 100-mesh powder in a mass ratio of 3:3:2:1, mixing it with a compound enzyme solution in a mass-volume ratio of 1:8, and enzymatically hydrolyzing it at 37°C for 10 minutes.

[0008] The complex enzyme solution was obtained by mixing glucanase and glucose oxidase at a volume ratio of 1:1 and then diluting the mixture with 0.1 mol / L pH 6.0 phosphate buffer to an enzyme concentration of 100 U / mL.

[0009] As a preferred embodiment of the present invention, the composite friction agent is a mixture of dicalcium phosphate with a particle size >10μm and silicon dioxide with a particle size of 1-10μm, wherein the mass fraction of dicalcium phosphate is 5-8.5 parts and the mass fraction of silicon dioxide is 10-16.5 parts.

[0010] As a preferred embodiment of the present invention, the composite chelating agent is a mixture of tetrasodium pyrophosphate with a molecular weight <1000 and polyvinylpyrrolidone with a molecular weight >1000, wherein the mass fraction of tetrasodium pyrophosphate is 0.75-2.25 parts and the mass fraction of polyvinylpyrrolidone is 0.25-0.75 parts.

[0011] As a preferred embodiment of the present invention, the film-forming agent is a PVM / MA copolymer, with a mass fraction of 0.5-2 parts.

[0012] As a preferred embodiment of the present invention, the enamel repair component is hydroxyapatite with a particle size of 100nm-5μm and a mass fraction of 2-10 parts.

[0013] As a preferred embodiment of the present invention, the moisturizer is a mixture of glycerin and sorbitol in a mass ratio of 3:2, wherein the mass fraction of glycerin is 12-18 parts and the mass fraction of sorbitol is 8-12 parts.

[0014] As a preferred embodiment of the present invention, the thickener is sodium carboxymethyl cellulose, with a mass fraction of 0.5-1.5 parts;

[0015] The foaming agent is sodium lauryl sulfate, in parts by weight of 1-3 parts.

[0016] As a preferred embodiment of the present invention, the sweetener is sodium saccharin, with a mass fraction of 0.1-0.5 parts;

[0017] The preservative is potassium sorbate, with a mass fraction of 0.05-0.3 parts;

[0018] The flavoring is peppermint flavoring, with a weight of 0.05-0.1 parts.

[0019] A method for preparing the above-mentioned toothpaste includes the following steps:

[0020] W1. Walnut shell powder, beech, oyster shell, and Manegug glacial mud were mixed in a mass ratio of 3:3:2:1 and ground to 100 mesh to obtain plant powder. Dextranase and glucose oxidase were mixed in a volume ratio of 1:1 and diluted with 0.1 mol / L pH 6.0 phosphate buffer to an enzyme concentration of 100 U / mL to obtain a compound enzyme solution. The plant powder and compound enzyme solution were mixed in a mass-volume ratio of 1:8, and enzymatically hydrolyzed in a 37°C constant temperature water bath with magnetic stirring at 150 r / min for 10 minutes. The mixture was then filtered through a 100-mesh filter cloth to obtain the plant enzymatic hydrolysate.

[0021] W2. Add the humectant, compound abrasive, compound chelating agent, enamel repair ingredients, and thickener to deionized water, and stir at 50°C and 300 rpm for 30 minutes to obtain mixture A; after mixture A cools to 30°C, add the plant enzymatic hydrolysate, film-forming agent, foaming agent, sweetener, preservative, and fragrance, stir at 200 rpm for 20 minutes, degas under vacuum ≥0.09 MPa for 15 minutes, and then fill and seal.

[0022] The beneficial effects of this invention are:

[0023] (1) After the plant powder and compound enzyme solution are hydrolyzed in a specific ratio, active ingredients such as flavonoids are produced, which can decompose pigments and enhance permeability; the compound abrasive removes surface and groove stains respectively, and the compound chelating agent softens and binds metal ions in a synergistic manner. The three work together to make the ΔE value reach more than 6.8, which is significantly better than the single component.

[0024] (2) The film-forming agent forms a protective film on the tooth surface, which, combined with the enamel repair components, fills the grooves and gives it long-lasting stain resistance. Detailed Implementation

[0025] To further illustrate the technical means and effects of the present invention in achieving its intended purpose, the following detailed description of the specific implementation methods, structures, features, and effects of the present invention, in conjunction with embodiments, is provided below.

[0026] Example 1

[0027] Preparation of plant enzymatic hydrolysates:

[0028] Weigh out 30g of walnut shell powder, 30g of beech, 20g of oyster shell, and 10g of Manegugen glacial mud, mix and grind to 100 mesh; mix with glucanase-glucose oxidase complex enzyme solution at a ratio of 1:8 (g / mL), enzymatically hydrolyze at 37℃ for 10 minutes, and filter to obtain the enzymatic hydrolysate.

[0029] Toothpaste preparation:

[0030] Mixture A: 20g glycerol, 13.3g sorbitol, 5g dicalcium phosphate, 10g silica, 2.25g tetrasodium pyrophosphate, 0.75g polyvinylpyrrolidone (Aslan, model pvp29 / 32), 2g hydroxyapatite, 0.8g sodium carboxymethyl cellulose (Changzhou Guoyu Environmental Protection Technology Co., Ltd.), add 41.05g deionized water, stir at 50℃ for 30 minutes;

[0031] Add 1.5g of plant enzymatic hydrolysate, 1g of PVM / MA copolymer (Gantaz S97), 2g of sodium lauryl sulfate, 0.2g of sodium saccharin, 0.1g of potassium sorbate, and 0.05g of peppermint flavor. Stir at 30°C for 20 minutes, degas under vacuum, and then fill to obtain toothpaste.

[0032] Example 2

[0033] Plant enzymatic hydrolysates:

[0034] 27g of walnut shell powder, 27g of beech, 18g of oyster shell, 9g of Manegugen glacial mud, and the rest are the same as in Example 1.

[0035] Toothpaste preparation:

[0036] Mixture A: 18g glycerol, 12g sorbitol, 4.5g dicalcium phosphate, 9g silica, 2.0g tetrasodium pyrophosphate, 0.65g polyvinylpyrrolidone, 5g hydroxyapatite, 0.7g sodium carboxymethyl cellulose, plus 43g deionized water;

[0037] Add 2.0g of plant enzymatic hydrolysate, 0.8g of PVM / MA copolymer, and the remaining additives in proportion, and the process is the same as in Example 1.

[0038] Example 3

[0039] Plant enzymatic hydrolysates:

[0040] 33g of walnut shell powder, 33g of beech, 22g of oyster shell, 11g of Manegugen glacial mud, and the rest are the same as in Example 1.

[0041] Toothpaste preparation:

[0042] Mixture A: 22g glycerol, 14.7g sorbitol, 5.5g dicalcium phosphate, 11g silica, 2.5g tetrasodium pyrophosphate, 0.85g polyvinylpyrrolidone, 10g hydroxyapatite, 0.9g sodium carboxymethyl cellulose, plus 26.5g deionized water;

[0043] Add 2.5g of plant enzymatic hydrolysate, 1.2g of PVM / MA copolymer, and the remaining additives in proportion, and the process is the same as in Example 1.

[0044] Comparative Example 1

[0045] The walnut shell powder was missing. The plant powder consisted of 30g of beech, 20g of oyster shell, and 10g of Manegugen glacial mud. The rest was the same as in Example 1.

[0046] Comparative Example 2

[0047] The beech tree was missing. The plant powder consisted of 30g of walnut shell powder, 20g of oyster shell powder, and 10g of Manegugen glacial mud. The rest was the same as in Example 1.

[0048] Comparative Example 3

[0049] Oyster shells were not used; the plant powder consisted of 30g of walnut shell powder, 30g of beech, and 10g of Manegugen glacial mud, with the rest being the same as in Example 1.

[0050] Comparative Example 4

[0051] Lacking glacial mud, the plant powder consisted of 30g of walnut shell powder, 30g of beech powder, and 20g of oyster shell powder, with the rest being the same as in Example 1.

[0052] Comparative Example 5

[0053] Walnut shell powder: beech: oyster shell: glacial mud = 2:2:3:3, the rest is the same as in Example 1.

[0054] Comparative Example 6

[0055] Only glucanase was used, without glucose oxidase, otherwise the same as in Example 1.

[0056] Comparative Example 7

[0057] The ratio of glucanase to glucose oxidase was 2:1, and the rest was the same as in Example 1.

[0058] Comparative Example 8

[0059] The plant powder was extracted using a water extraction and alcohol precipitation method to obtain an extract that replaced the enzymatic extraction method; the rest was the same as in Example 1.

[0060] Performance testing

[0061] 1. Detection Method

[0062] (1) Whitening and stain removal effect test

[0063] Carrier preparation: Select healthy extracted bovine teeth (aged 2-3 years, without cavities or cracks), remove the tooth root and cementum, cut into 10mm×10mm×2mm pieces, polish them with 400#, 800# and 1200# sandpaper in sequence, ultrasonically clean for 10 minutes (deionized water, power 300W), and dry for later use.

[0064] Artificial staining: The dental slides were immersed in a 5% coffee solution (commercially available instant coffee, prepared with distilled water) and stained in a 37°C constant temperature incubator for 24 hours. After removal, they were rinsed three times with deionized water. The initial color value was measured using a colorimeter (model: CR-400, Konica Minolta). , , );

[0065] Simulated brushing: Use an automatic toothbrush with a load of 150g, a speed of 300r / min, a toothpaste dosage of 0.5g / brush, and a deionized water dosage of 1mL / brush. Brush for 2 minutes each time, twice a day, for 2 weeks.

[0066] Evaluation of results: After brushing, the final color value of the dental X-ray was measured. , , ), calculate color difference value The larger the ΔE, the better the whitening and stain removal effect (ΔE≥5.5 is excellent, 4.0≤ΔE<5.5 is good, and ΔE<4.0 is poor).

[0067] (2) Antibacterial effect test

[0068] Strain preparation: Streptococcus mutans was inoculated into MH liquid medium and incubated at 37°C for 18 hours. The bacterial concentration was then adjusted to... CFU / mL;

[0069] Agar diffusion method: Take 100 μL of bacterial solution and spread it evenly on the surface of MH agar medium. After the bacterial solution is absorbed, place a sterile filter paper (6 mm in diameter) and add 20 μL of toothpaste sample solution (20% mass concentration, diluted with deionized water). Incubate at 37℃ for 24 hours.

[0070] Effect evaluation: The diameter of the inhibition zone (including the diameter of the filter paper) was measured with a vernier caliper (accuracy 0.02mm). The larger the diameter, the stronger the antibacterial effect (≥20mm is excellent, 15mm≤diameter<20mm is good, and diameter<15mm is poor).

[0071] (3) Stain-resistant effect test

[0072] Sample preparation: The dental films obtained after "simulating brushing teeth for 2 weeks" were soaked again in 5% coffee solution and incubated at 37°C for 24 hours.

[0073] Evaluation of results: Measurement of color values ​​of dental radiographs after secondary staining ( , , ), calculate secondary staining The smaller the ΔE, the better the stain-resistant effect (≤1.5 is excellent, 1.5<ΔE≤2.5 is good, and ΔE>2.5 is poor).

[0074] (4) Testing of enamel restoration effect

[0075] Dentin slice preparation: Healthy extracted bovine teeth were selected and cut into dentin slices of 10mm×10mm×2mm. After polishing, the slices were immersed in 0.1mol / L lactic acid solution (pH=4.5) and demineralized at 37℃ for 48 hours to prepare an artificial sensitive dentin model.

[0076] Sample preparation: The demineralized dentin slices were immersed in toothpaste dilution (10% by mass, diluted with deionized water) and incubated at 37°C for 24 hours.

[0077] Evaluation of Results: The morphology of dentinal tubules was observed using a scanning electron microscope (model: SU8010, Hitachi). Five fields of view were randomly selected (magnification × 2000). The number of closed dentinal tubules and the total number of tubules were counted. The closure rate was calculated as (number of closed tubules / total number of tubules) × 100% (≥70% is excellent, 60%≤closure rate<70% is good, and closure rate<60% is poor).

[0078] (5) Antioxidant effect test

[0079] Sample preparation: Dilute the toothpaste sample with deionized water to a mass concentration of 5%, centrifuge (5000 r / min, 10 minutes), and collect the supernatant for later use;

[0080] DPPH method: Mix 2 mL of supernatant with 2 mL of 0.1 mmol / L DPPH ethanol solution, react in the dark for 30 minutes, and measure the absorbance at 517 nm using a UV-Vis spectrophotometer (model: UV-2600, Shimadzu) (sample A); the blank group is 2 mL of deionized water + 2 mL of DPPH solution (blank A).

[0081] Effect evaluation: Calculate DPPH free radical scavenging rate = [(A blank - A sample) / A blank] × 100%. The higher the scavenging rate, the stronger the antioxidant effect (≥80% is excellent, 70%≤scavenging rate<80% is good, and scavenging rate<70% is poor).

[0082] 2. The test results are as follows:

[0083] Table 1. Results of Whitening and Stain Removal Effect Tests

[0084] sample ΔE value Effect evaluation Difference from Example 1 (ΔE Example 1 - ΔE Sample) Example 1 6.9 Excellent - Example 2 6.6 Excellent 0.3 Example 3 6.8 Excellent 0.1

[0085] Table 2 Results of antibacterial effect test

[0086] sample Diameter of the inhibition zone (mm) Effect evaluation Difference from Example 1 (mm) Example 1 22.5 Excellent - Example 2 22.0 Excellent 0.5 Example 3 22.3 Excellent 0.2 Comparative Example 1 15.0 good 7.5 Comparative Example 2 15.8 good 6.7 Comparative Example 3 16.5 good 6.0 Comparative Example 4 18.3 good 4.2 Comparative Example 5 19.2 good 3.3 Comparative Example 6 19.0 good 3.5 Comparative Example 7 19.8 good 2.7 Comparative Example 8 12.5 Poor 10.0

[0087] Table 3. Results of Stain-Repellent Effect Test

[0088] sample Secondary staining ΔE value Effect evaluation Difference from Example 1 (ΔEsample - ΔEExample 1) Example 1 1.1 Excellent - Example 2 1.2 Excellent 0.1 Example 3 1.1 Excellent 0.0 Comparative Example 1 2.1 good 1.0 Comparative Example 2 2.2 good 1.1 Comparative Example 3 1.9 good 0.8 Comparative Example 4 2.3 good 1.2 Comparative Example 5 2.1 good 1.0 Comparative Example 6 2.2 good 1.1 Comparative Example 7 1.7 good 0.6 Comparative Example 8 3.6 Poor 2.5

[0089] Table 4 Results of Enamel Restoration Effect Test

[0090] sample Closure rate (%) Effect evaluation Difference from Example 1 (%) Example 1 73.0 Excellent - Example 2 72.0 Excellent 1.0 Example 3 72.5 Excellent 0.5 Comparative Example 1 50.0 Poor 23.0 Comparative Example 2 51.5 Poor 21.5 Comparative Example 3 53.2 Poor 19.8 Comparative Example 4 60.5 good 12.5 Comparative Example 5 62.3 good 10.7 Comparative Example 6 61.8 good 11.2 Comparative Example 7 66.0 good 7.0 Comparative Example 8 45.5 Poor 27.5

[0091] Table 5 Results of Antioxidant Effect Test

[0092] sample Clearance rate (%) Effect evaluation Difference from Example 1 (%) Example 1 83.0 Excellent - Example 2 82.0 Excellent 1.0 Example 3 82.5 Excellent 0.5 Comparative Example 1 55.0 Poor 28.0 Comparative Example 2 57.5 Poor 25.5 Comparative Example 3 59.2 Poor 23.8 Comparative Example 4 65.8 good 17.2 Comparative Example 5 68.7 good 14.3 Comparative Example 6 67.9 good 15.1 Comparative Example 7 72.5 good 10.5 Comparative Example 8 43.0 Poor 40.0

[0093] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A whitening and stain-removing toothpaste, characterized by, By mass parts, including the following components: plant enzymatic 1.5-2.5 parts, complex friction agent 15-25 parts, complex chelating agent 1-3 parts, film forming agent 0.5-2 parts, enamel repair ingredients 2-5 parts, humectant 20-30 parts, thickening agent 0.5-1.5 parts, foaming agent 1-3 parts, sweetener 0.1-0.5 parts, preservative 0.05-0.3 parts, essence 0.05-0.1 parts, deionized water to 100 parts; The plant enzymatic is obtained by grinding walnut shell powder, beech, oyster shell, manikin Greenland river mud into 100 mesh powder according to mass ratio 3:3:2:1, mixing with complex enzyme liquid according to mass volume ratio 1:8, and enzymolysis at 37℃ for 10 minutes; The complex enzyme liquid is obtained by mixing dextranase and glucose oxidase according to volume ratio 1:1, and then diluting with 0.1mol / L pH=6.0 phosphate buffer to enzyme concentration 100U / mL; The complex friction agent is obtained by mixing calcium hydrogen phosphate with particle size greater than 10μm and silicon dioxide with particle size 1-10μm, wherein the mass parts of calcium hydrogen phosphate is 5-8.5 parts, and the mass parts of silicon dioxide is 10-16.5 parts; The complex chelating agent is obtained by mixing tetrasodium pyrophosphate with molecular weight less than 1000 and polyvinylpyrrolidone with molecular weight greater than 1000, wherein the mass parts of tetrasodium pyrophosphate is 0.75-2.25 parts, and the mass parts of polyvinylpyrrolidone is 0.25-0.75 parts; The enamel repair ingredients is hydroxyapatite with particle size 100nm-5μm, and mass parts is 2-5 parts.

2. The toothpaste according to claim 1, characterized in that, The film forming agent is PVM / MA copolymer, and mass parts is 0.5-2 parts.

3. The toothpaste according to claim 1, wherein The humectant is obtained by mixing glycerol and sorbitol according to mass ratio 3:2, wherein the mass parts of glycerol is 12-18 parts, and the mass parts of sorbitol is 8-12 parts.

4. The toothpaste according to claim 1, wherein The thickening agent is sodium carboxymethyl cellulose, and mass parts is 0.5-1.5 parts; The foaming agent is sodium lauryl sulfate, and mass parts is 1-3 parts.

5. The toothpaste according to claim 1, wherein The sweetener is sodium saccharin, and mass parts is 0.1-0.5 parts; The preservative is potassium sorbate, and mass parts is 0.05-0.3 parts; The essence is peppermint essence, and mass parts is 0.05-0.1 parts.

6. A process for the preparation of a toothpaste according to any one of claims 1 to 5, characterized in that, Including the following steps: W1. Mix walnut shell powder, beech, oyster shell, manikin Greenland river mud according to mass ratio 3:3:2:1, and grind to 100 mesh to obtain plant powder; mix dextranase and glucose oxidase according to volume ratio 1:1, dilute with 0.1mol / L pH=6.0 phosphate buffer to enzyme concentration 100U / mL to obtain complex enzyme liquid; mix plant powder and complex enzyme liquid according to mass volume ratio 1:8, 37℃ constant temperature water bath, 150r / min magnetic stirring enzymolysis for 10 minutes, filter through 100 mesh filter cloth to obtain plant enzymatic; W2. Moisturizing agent, composite friction agent, composite chelating agent, enamel repair ingredients, thickening agent into deionized water, 50 ℃, 300 r / min stirring 30 minutes to get mixed liquid A; mixed liquid A cooling to 30 ℃, add plant enzymatic hydrolysate, film forming agent, foaming agent, sweetener, preservative, essence, 200 r / min stirring 20 minutes, under the vacuum degree ≥0.09MPa degassing 15 minutes, filling and sealing.