Toothpaste with antibacterial and bacteriostatic efficacy and preparation method thereof

Abstract

The application relates to the technical field of toothpaste, and discloses toothpaste with antibacterial and bacteriostatic effects and a preparation method thereof. The toothpaste is prepared from bacteriostatic paste base, silicon dioxide, titanium dioxide, sodium lauryl sulfate, sodium saccharin and peppermint essence. The bacteriostatic paste base is prepared from deionized water, sorbitol aqueous solution, sodium carboxymethyl cellulose, alpha-lipoic acid powder, sodium hydroxide aqueous solution and zinc sulfate aqueous solution. The toothpaste has good bacteriostatic performance.

Description

Technical Field

[0001] This invention relates to the field of toothpaste technology, specifically to a toothpaste with antibacterial and bacteriostatic effects and its preparation method. Background Technology

[0002] The oral cavity is an important habitat for microorganisms in the human body, containing a large number of bacteria. When the number of bacteria in the oral cavity is unbalanced and harmful bacteria proliferate excessively, it can easily lead to various oral diseases such as tooth decay, gingivitis, and periodontitis. It can also cause problems such as bad breath, seriously affecting human oral health and quality of life.

[0003] Patent CN105232378A discloses a whitening toothpaste that removes stains and whitens without adding oxidants or bleaching agents, using food-grade raw materials sodium phytate and zinc citrate combined with traditional Chinese medicine extracts, as well as the preparation method of toothpaste containing these components. The stain-removing and whitening raw materials and components are: sodium phytate 0.5-1.5%, zinc citrate 0.5-1%, angelica dahurica extract 0.5-1%, atractylodes macrocephala extract 0.2-0.6%, bletilla striata extract 0.3-0.8%, ampelopsis japonica extract 0.7-1.0%, and poria cocos extract 0.1-0.3%. The above raw materials are mixed and stirred evenly before use. Toothpaste is made by adding the above-mentioned stain-removing and whitening ingredients to the following raw materials: sorbitol 40-45%, highly abrasive hydrated silica 15-25%, propylene glycol 10-15%, cellulose gum 1-1.5%, xylitol 5-15%, titanium dioxide 0.2-0.6%, sodium lauryl sulfate 1.5-2.5%, sodium saccharin 0.2-0.3%, carrageenan 0.2-0.5%, and flavoring agent 0.8-1.5%, with water added to 100%. However, the existing toothpaste has insufficient antibacterial and bacteriostatic effects and cannot meet the needs of users. Summary of the Invention

[0004] The purpose of this invention is to provide a toothpaste with antibacterial and bacteriostatic effects and its preparation method, so as to solve the problems existing in the prior art.

[0005] To solve the above-mentioned technical problems, the present invention provides the following technical solution: A toothpaste with antibacterial and bacteriostatic effects, wherein the toothpaste is made from an antibacterial paste base, silica, titanium dioxide, sodium lauryl sulfate, sodium saccharin and peppermint flavor; the antibacterial paste base is made from deionized water, sorbitol aqueous solution, sodium carboxymethyl cellulose, α-lipoic acid powder, sodium hydroxide aqueous solution and zinc sulfate aqueous solution.

[0006] Furthermore, the mass ratio of deionized water, sorbitol aqueous solution, sodium carboxymethyl cellulose, α-lipoic acid powder, and zinc sulfate aqueous solution is 15-20:40-60:0.8-1.5:1-3:5.5-11.5.

[0007] Furthermore, the mass ratio of the antibacterial paste base, silica, titanium dioxide, sodium lauryl sulfate, sodium saccharin, and peppermint flavor is 60-100:15-25:0.5-1.0:1.5-2.5:0.1-0.3:0.8-1.5.

[0008] Furthermore, the zinc sulfate aqueous solution has a mass fraction of 10-15%.

[0009] A method for preparing toothpaste with antibacterial and bacteriostatic effects includes the following steps: (1) Under nitrogen protection, deionized water and sorbitol aqueous solution are added to the reaction vessel. Sodium carboxymethyl cellulose is added within 5-8 minutes while stirring at 40-60 rpm. After the addition is complete, the temperature is heated to 70-80℃ and stirred for 30-40 minutes. Then the temperature is lowered to 45-55℃, α-lipoic acid powder is added and stirred for 15-20 minutes. The pH value is adjusted to 8.0-8.5 with sodium hydroxide aqueous solution and stirred for 10-15 minutes. Then zinc sulfate aqueous solution is added dropwise. After the addition is complete, the stirring is continued for 20-30 minutes to obtain antibacterial paste base. (2) Under stirring conditions of 45-50℃ and 60-80rpm, add silica and titanium dioxide to the antibacterial paste base obtained in step (1) within 10-15 minutes. After the addition is completed, turn on the vacuum degassing and control the vacuum degree to -0.06MPa to -0.08MPa. Stir at 80-100rpm for 15-20 minutes, then add sodium lauryl sulfate, sodium saccharin and peppermint flavor, and continue stirring for 20-30 minutes to obtain toothpaste.

[0010] Furthermore, the mass fraction of the sorbitol aqueous solution in step (1) is 60-70%.

[0011] Furthermore, in step (1), the zinc sulfate aqueous solution is added over a period of 10-15 minutes.

[0012] Furthermore, the mass fraction of the sodium hydroxide aqueous solution in step (1) is 9-11%.

[0013] Furthermore, in step (2), the particle size of silica is 10-20 μm.

[0014] Furthermore, in step (2), the particle size of titanium dioxide is 0.5-1.0 μm.

[0015] Compared with the prior art, the beneficial effects achieved by the present invention are: 1. In this invention, because the complexation constant of the thiol group generated after α-lipoic acid ring-opening under alkaline conditions with zinc ions is very high, much greater than that of the precipitation reaction of zinc ions with hydroxide ions, zinc ions preferentially combine with lipoic acid molecules during the slow addition of zinc sulfate to form a stable soluble complex, thereby effectively avoiding the formation of zinc hydroxide precipitate and ensuring the homogeneity of the reaction system; under weakly alkaline conditions, α-lipoic acid can partially open its ring, and the addition of zinc ions forms a stable complex with the ring-opening product, breaking the reaction equilibrium and driving the ring-opening reaction of α-lipoic acid to proceed to the end in the forward direction. Therefore, in this invention, alkaline conditions induce a ring-opening reaction of the disulfide five-membered ring in the α-lipoic acid molecule, generating a linearized lipoic acid molecule containing two free thiol groups and one sodium carboxylate group. Both the sulfur atom in the thiol group and the oxygen atom in the carboxyl group contain lone pairs of electrons, which can serve as active sites for coordination reactions. The thiol and carboxyl groups on the activated lipoic acid molecule coordinate with zinc ions, forming a coordination polymer with a cross-linked network structure through the interconnection of zinc ions with the coordination groups on multiple lipoic acid molecules. The zinc ions in the coordination polymer can bind to the thiol groups of cysteine ​​residues in bacterial cell membrane proteins, leading to conformational changes and loss of function, disrupting cell membrane integrity, and causing intracellular leakage. The free zinc ions released by the coordination polymer can enter the bacterial interior and bind to deoxyribonucleic acid and enzyme proteins, interfering with bacterial genetic material replication and energy metabolism. The free lipoic acid molecules released by the coordination polymer act as antioxidants, disrupting the redox balance within bacteria and producing oxidative stress, thus giving the toothpaste excellent antibacterial properties. Detailed Implementation

[0016] The following embodiments are provided to better understand the present invention and are not limited to the preferred embodiments described. They do not constitute a limitation on the content and scope of protection of the present invention. Any product that is the same as or similar to the present invention, derived by any person under the guidance of the present invention or by combining the features of the present invention with other prior art, falls within the protection scope of the present invention.

[0017] A toothpaste with antibacterial and bacteriostatic effects, wherein the toothpaste is made from an antibacterial paste base, silica, titanium dioxide, sodium lauryl sulfate, sodium saccharin and peppermint flavor; the antibacterial paste base is made from deionized water, sorbitol aqueous solution, sodium carboxymethyl cellulose, α-lipoic acid powder, sodium hydroxide aqueous solution and zinc sulfate aqueous solution.

[0018] For experiments not specifically described in the examples, the procedures or conditions should be followed according to the conventional experimental procedures described in the literature in this field. Reagents or instruments whose manufacturers are not specified are all commercially available conventional reagent products.

[0019] Example 1

[0020] (1) Under nitrogen protection, deionized water and 60% sorbitol aqueous solution were added to the reactor. Sodium carboxymethyl cellulose was added within 5 minutes while stirring at 40 rpm. After the addition was completed, the temperature was raised to 70°C and stirred for 30 minutes. Then the temperature was lowered to 45°C and α-lipoic acid powder was added and stirred for 15 minutes. The pH value was adjusted to 8.0 with 9% sodium hydroxide aqueous solution and stirred for 10 minutes. Then 10% zinc sulfate aqueous solution was added dropwise over 10 minutes. After the addition was completed, the mixture was stirred for 20 minutes to obtain the antibacterial paste base. The mass ratio of deionized water, sorbitol aqueous solution, sodium carboxymethyl cellulose, α-lipoic acid powder and zinc sulfate aqueous solution was 15:40:0.8:1:5.5.

[0021] (2) Under stirring conditions of 45℃ and 60rpm, silica with a particle size of 10μm and titanium dioxide with a particle size of 0.5μm are added to the antibacterial paste base obtained in step (1) within 10 minutes. After the addition is completed, vacuum degassing is turned on and the vacuum degree is controlled at -0.06MPa. Stir at 80rpm for 15 minutes, then sodium lauryl sulfate, sodium saccharin and peppermint flavor are added, and stirring is continued for 20 minutes to obtain toothpaste. The mass ratio of antibacterial paste base, silica, titanium dioxide, sodium lauryl sulfate, sodium saccharin and peppermint flavor is 60:15:0.5:1.5:0.1:0.8.

[0022] Example 2

[0023] (1) Under nitrogen protection, deionized water and 65% sorbitol aqueous solution were added to the reactor. Sodium carboxymethyl cellulose was added over 6.5 minutes while stirring at 50 rpm. After the addition was completed, the mixture was heated to 75°C and stirred for 35 minutes. Then the mixture was cooled to 50°C and α-lipoic acid powder was added and stirred for 17.5 minutes. The pH was adjusted to 8.3 with 10% sodium hydroxide aqueous solution and stirred for 12.5 minutes. Then 12.5% ​​zinc sulfate aqueous solution was added dropwise over 12.5 minutes. After the addition was completed, the mixture was stirred for 25 minutes to obtain the antibacterial paste base. The mass ratio of deionized water, sorbitol aqueous solution, sodium carboxymethyl cellulose, α-lipoic acid powder and zinc sulfate aqueous solution was 17.5:50:1.15:2:8.5.

[0024] (2) Under stirring conditions of 47.5℃ and 70rpm, silica with a particle size of 15μm and titanium dioxide with a particle size of 0.7μm were added to the antibacterial paste base obtained in step (1) within 12.5 minutes. After the addition was completed, vacuum degassing was turned on and the vacuum degree was controlled at -0.07MPa. Stirring was carried out at 90rpm for 17.5 minutes. Then sodium lauryl sulfate, sodium saccharin and peppermint flavor were added and stirring was continued for 25 minutes to obtain toothpaste. The mass ratio of antibacterial paste base, silica, titanium dioxide, sodium lauryl sulfate, sodium saccharin and peppermint flavor was 80:20:0.75:2.0:0.2:1.15.

[0025] Example 3

[0026] (1) Under nitrogen protection, deionized water and 70% sorbitol aqueous solution were added to the reactor. Sodium carboxymethyl cellulose was added within 8 minutes while stirring at 60 rpm. After the addition was completed, the temperature was raised to 80°C and stirred for 40 minutes. Then the temperature was lowered to 55°C and α-lipoic acid powder was added and stirred for 20 minutes. The pH value was adjusted to 8.5 with 11% sodium hydroxide aqueous solution and stirred for 15 minutes. Then zinc sulfate aqueous solution with 15% sorbitol was added dropwise over 15 minutes. After the addition was completed, the mixture was stirred for 30 minutes to obtain the antibacterial paste base. The mass ratio of deionized water, sorbitol aqueous solution, sodium carboxymethyl cellulose, α-lipoic acid powder and zinc sulfate aqueous solution was 20:60:1.5:3:11.5.

[0027] (2) Under stirring conditions of 50℃ and 80rpm, silica with a particle size of 20μm and titanium dioxide with a particle size of 1.0μm are added to the antibacterial paste base obtained in step (1) within 15 minutes. After the addition is completed, vacuum degassing is turned on and the vacuum degree is controlled at -0.08MPa. Stir at 100rpm for 20 minutes, then sodium lauryl sulfate, sodium saccharin and peppermint flavor are added, and stirring is continued for 30 minutes to obtain toothpaste. The mass ratio of antibacterial paste base, silica, titanium dioxide, sodium lauryl sulfate, sodium saccharin and peppermint flavor is 100:25:1.0:2.5:0.3:1.5.

[0028] Comparative Example 1 The only difference between Comparative Example 1 and Example 1 is that α-lipoic acid powder is not added.

[0029] Comparative Example 2 The only difference between Comparative Example 2 and Example 1 is that zinc sulfate aqueous solution is not added.

[0030] Comparative Example 3 The only difference between Comparative Example 3 and Example 1 is that the pH adjustment with sodium hydroxide aqueous solution is omitted.

[0031] Antibacterial properties: The test was conducted according to the quantitative suspension bactericidal test method specified in QB / T2738-2023 "Evaluation Method for Antibacterial and Bacteriostatic Effects of Daily Chemical Products". *Porphyromonas gingivalis* (ATCC33277) and *Streptococcus mutans* (ATCC25175) were selected as test strains, with an action time of 5 minutes, and the inhibition rate was calculated.

[0032] Table 1 below shows the performance analysis results of the embodiments and comparative examples of the present invention.

[0033] Table 1

[0034] Experimental data from the examples and comparative examples show that the present invention opens the five-membered disulfide ring of α-lipoic acid using sodium hydroxide, generating a linearized lipoic acid molecule containing two free thiol groups and one sodium carboxylate group. The thiol and carboxyl groups on the activated lipoic acid molecule serve as coordination active sites, coordinating with zinc ions provided by zinc sulfate. The zinc ions, as the central ion, crosslink with multiple lipoic acid molecules to form a coordination polymer. The zinc ions of the coordination polymer can bind to the thiol groups in cell membrane proteins, causing membrane protein denaturation, disrupting cell membrane integrity, and causing leakage of intracellular substances. In the aqueous environment of the oral cavity, the coordination polymer slowly dissociates and releases free zinc ions and lipoic acid. The free zinc ions enter the bacteria and bind to deoxyribonucleic acid and enzyme proteins, interfering with genetic material replication and energy metabolism. The free lipoic acid disrupts the redox balance inside the bacteria, producing an oxidative stress effect. Through multiple synergistic effects, the toothpaste has good antibacterial properties.

[0035] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No markings in the claims should be construed as limiting the scope of the claims.

Claims

1. A toothpaste with antibacterial and bacteriostatic effects, characterized in that, The toothpaste is made from an antibacterial paste base, silica, titanium dioxide, sodium lauryl sulfate, sodium saccharin, and peppermint flavoring; the antibacterial paste base is made from deionized water, sorbitol aqueous solution, sodium carboxymethyl cellulose, α-lipoic acid powder, sodium hydroxide aqueous solution, and zinc sulfate aqueous solution.

2. The toothpaste with antibacterial and bacteriostatic effects according to claim 1, characterized in that: The mass ratio of deionized water, sorbitol aqueous solution, sodium carboxymethyl cellulose, α-lipoic acid powder, and zinc sulfate aqueous solution is 15-20:40-60:0.8-1.5:1-3:5.5-11.

5.

3. The toothpaste with antibacterial and bacteriostatic effects according to claim 1, characterized in that: The mass ratio of antibacterial paste base, silicon dioxide, titanium dioxide, sodium lauryl sulfate, sodium saccharin and peppermint flavor is 60-100:15-25:0.5-1.0:1.5-2.5:0.1-0.3:0.8-1.

5.

4. The toothpaste with antibacterial and bacteriostatic effects according to claim 1, characterized in that: The mass fraction of zinc sulfate aqueous solution is 10-15%.

5. A method for preparing a toothpaste with antibacterial and bacteriostatic effects, applicable to the toothpaste with antibacterial and bacteriostatic effects as described in any one of claims 1-4, characterized in that, Includes the following steps: (1) Under nitrogen protection, deionized water and sorbitol aqueous solution are added to the reaction vessel. Sodium carboxymethyl cellulose is added within 5-8 minutes while stirring at 40-60 rpm. After the addition is complete, the temperature is heated to 70-80℃ and stirred for 30-40 minutes. Then the temperature is lowered to 45-55℃, α-lipoic acid powder is added and stirred for 15-20 minutes. The pH value is adjusted to 8.0-8.5 with sodium hydroxide aqueous solution and stirred for 10-15 minutes. Then zinc sulfate aqueous solution is added dropwise. After the addition is complete, the stirring is continued for 20-30 minutes to obtain antibacterial paste base. (2) Under stirring conditions of 45-50℃ and 60-80rpm, add silica and titanium dioxide to the antibacterial paste base obtained in step (1) within 10-15 minutes. After the addition is completed, turn on the vacuum degassing and control the vacuum degree to -0.06MPa to -0.08MPa. Stir at 80-100rpm for 15-20 minutes, then add sodium lauryl sulfate, sodium saccharin and peppermint flavor, and continue stirring for 20-30 minutes to obtain toothpaste.

6. The method for preparing a toothpaste with antibacterial and bacteriostatic effects according to claim 5, characterized in that: In step (1), the mass fraction of the sorbitol aqueous solution is 60-70%.

7. The method for preparing a toothpaste with antibacterial and bacteriostatic effects according to claim 5, characterized in that: The zinc sulfate aqueous solution is added dropwise over 10-15 minutes in step (1).

8. The method for preparing a toothpaste with antibacterial and bacteriostatic effects according to claim 5, characterized in that: The mass fraction of the sodium hydroxide aqueous solution in step (1) is 9-11%.

9. A method for preparing a toothpaste with antibacterial and bacteriostatic effects according to claim 5, characterized in that: In step (2), the particle size of silica is 10-20 μm.

10. A method for preparing a toothpaste with antibacterial and bacteriostatic effects according to claim 5, characterized in that: In step (2), the particle size of titanium dioxide is 0.5-1.0 μm.

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