Novel anti-caries toothpaste containing chlorine dioxide and preparation method thereof

By forming a complex compound with chlorine dioxide and polyvinylpyrrolene, and combining sodium dodecyl sulfate, the stability and long-term bactericidal ability of chlorine dioxide in toothpaste is solved, and an efficient and safe toothpaste product is achieved.

CN119970529APending Publication Date: 2025-05-13BEIJING TINGLE LAIKELI MEDICAL APPLIANCES CO LTD
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Patent Information

Application Number
CN202510205016.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-02-24
Publication Date
2025-05-13

AI Technical Summary

Technical Problem

How to effectively integrate chlorine dioxide into toothpaste to maintain its stability and long-term sterilization ability, and solve the problem that it is easily soluble in water and has active chemical properties at room temperature.

Method used

By dissolving chlorine dioxide gas in polyvinylpyrrolidone (PVP) solution, a complex compound is formed to form a stable organic chlorine dioxide solution, and combined with sodium dodecyl sulfate to reduce the surface tension of water and promote the uniform distribution of chlorine dioxide.

Benefits of technology

The stability and long-term bactericidal ability of chlorine dioxide are achieved, the cleaning and antibacterial properties of toothpaste are improved, the risk of tooth fluorosis is avoided, and the use process is simplified.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

The invention relates to the field of oral care, and particularly discloses novel anti-caries toothpaste containing chlorine dioxide and a preparation method of the novel anti-caries toothpaste. A novel anti-caries toothpaste containing chlorine dioxide comprises an active component and a paste-based material, and the active component is an organic chlorine dioxide solution obtained by complexing a solution containing chlorine dioxide gas and a polyvinylpyrrolidone solution; the preparation method comprises the following steps: introducing a solution containing chlorine dioxide gas into a polyvinylpyrrolidone solution, uniformly mixing and stirring, adding lauryl sodium sulfate, fully stirring to obtain an organic chlorine dioxide solution, adding sodium polyacrylate into the organic chlorine dioxide solution, and stirring at a high speed until sodium polyacrylate is completely dissolved, thereby obtaining the product. And soaking and homogenizing the polymer thick paste for a long time, filling, sealing and packaging to obtain a finished product. The toothpaste can be used for preventing decayed teeth and has the advantages of being good in antibacterial durability and high in stability.
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Description

Technical Field

[0001] The present application relates to the field of oral care and daily cosmetics, and more specifically, to a novel anti-caries toothpaste containing chlorine dioxide and a preparation method thereof. Background Art

[0002] As a key product for daily oral care, toothpaste is widely used for personal teeth cleaning, breath freshening and prevention of various oral diseases. It removes food debris and plaque on the surface of teeth through mechanical friction, and provides additional protection with the help of active ingredients, such as antibacterial and anti-caries. As the public's attention to oral health continues to increase, the market demand for efficient and safe oral care products is also growing. In the field of oral care, fluoride has long been used as the main anti-caries ingredient because it can enhance the acid resistance of tooth enamel and inhibit the growth of caries-causing bacteria. However, long-term use of fluoride toothpaste may cause problems such as fluorosis, affecting the appearance of teeth. At the same time, consumers' preference for natural ingredients and fluoride-free products has gradually increased, promoting the development of a new generation of toothpaste that does not contain fluoride but can still effectively prevent tooth decay.

[0003] As a broad-spectrum bactericide, chlorine dioxide is widely used in drinking water disinfection, food processing and other fields. Studies have shown that chlorine dioxide can not only quickly kill a variety of oral pathogenic microorganisms, but also has a significant inhibitory effect on Streptococcus mutans and Porphyromonas gingivalis, the main bacteria that cause dental caries. In addition, oral care products containing chlorine dioxide have been proven to be safe and effective in controlling dental plaque and treating gingivitis.

[0004] Chlorine dioxide has excellent bactericidal properties. It is easily soluble in water at room temperature, but its chemical properties are very active and its stability is greatly affected by temperature, which makes it difficult to maintain its activity for a long time. Therefore, how to effectively integrate it into toothpaste and maintain its stability and long-term bactericidal ability is a technical problem that has yet to be solved. Summary of the invention

[0005] In order to improve the bactericidal longevity and stability of chlorine dioxide toothpaste, the present application provides a novel anti-caries toothpaste containing chlorine dioxide and a preparation method thereof.

[0006] In the first aspect, the present application provides a novel anti-caries toothpaste containing chlorine dioxide, which adopts the following technical scheme: a novel anti-caries toothpaste containing chlorine dioxide, comprising an active ingredient and a paste-based material, wherein the active ingredient is an organic chlorine dioxide solution obtained by complexing a solution containing chlorine dioxide gas with a polyvinylpyrrolidone solution.

[0007] By adopting the above technical solution and utilizing the strong broad-spectrum antibacterial properties of chlorine dioxide, a variety of pathogenic microorganisms including Streptococcus mutans can be quickly killed, effectively inhibiting the formation of dental plaque, thereby achieving a better anti-caries effect. The added sodium dodecyl sulfate reduces the surface tension of water, produces rich foam, and helps clean food residues and plaque on the surface of teeth and in between teeth. The combination of the two significantly improves the cleaning and antibacterial properties of toothpaste.

[0008] Polyvinyl pyrrolidone (PVP) is a polymer compound with good solubility and stability. Chlorine dioxide gas is dissolved in the PVP solution to form a complex compound, forming a stable organic chlorine dioxide solution. This complexation not only improves the stability of chlorine dioxide and prevents it from decomposing or losing activity during storage and use, but also makes it unnecessary to add acid to activate the toothpaste when using it, simplifying the use process. When this solution is added to the toothpaste base, due to the viscosity of PVP, the chlorine dioxide molecules can more easily adhere to the toothpaste particles and achieve uniform distribution.

[0009] On the basis of this application, taking into account the different taste requirements of users and the requirements for the appearance of the finished product, appropriate amounts of flavoring agents and pigments, such as peppermint oil to increase the sense of freshness, or edible pigments to improve the color of the product, can be added. At the same time, in order to ensure the safety and stability of the product, the amount of each added component is strictly controlled, and safety assessments and stability tests are carried out. The flavoring agents and pigments must comply with the relevant provisions of the "Regulations on the Supervision and Administration of Cosmetics" and have no adverse effects on the physical and chemical indicators (such as pH value, viscosity, etc.) and antibacterial properties of the toothpaste. The final formula of the product must pass the sensory test of consumers on the premise of meeting the safety and efficacy requirements to achieve a high market acceptance effect.

[0010] Optionally, the toothpaste comprises 95-98 parts of organic chlorine dioxide solution and 2-5 parts of paste-based materials.

[0011] Optionally, the preparation of the organic chlorine dioxide solution comprises the following steps: (1) using sodium chlorite and citric acid monohydrate to react to prepare chlorine dioxide gas, washing with water twice to remove impurities and cool down, and then passing into purified water until the concentration of chlorine dioxide in the purified water reaches 600-700 ppm, thereby obtaining a solution containing chlorine dioxide gas; (2) A polyvinyl pyrrolidone solution with a mass concentration of 10% is heated to 45-55° C., the prepared solution containing chlorine dioxide gas is added and stirred evenly, then the temperature is lowered to below 37° C., sodium dodecyl sulfate is added and stirred sufficiently to obtain a stable organic chlorine dioxide solution.

[0012] By adopting the above technical solution, chlorine dioxide has extremely strong volatility and instability, so an on-site production method is adopted. After the gas is obtained, it is mixed with a polyvinyl pyrrolidone solution to form a stable organic chlorine dioxide solution. Polyvinyl pyrrolidone, as a polymer with good biocompatibility, can not only effectively adsorb and stabilize chlorine dioxide molecules, but also prevent them from premature decomposition or escape, ensuring the long-term effectiveness and reliability of the bactericidal active ingredients during storage. At the same time, sodium dodecyl sulfate, as a surfactant, can reduce the interfacial tension between the chlorine dioxide solution and the toothpaste base, further promoting the uniform distribution of chlorine dioxide.

[0013] Optionally, a temperature-sensitive material and polyvinyl alcohol may be added to the organic chlorine dioxide solution to prepare microcapsules which are added to toothpaste, specifically comprising the following steps: after adding sodium dodecyl sulfate and stirring evenly, adding the temperature-sensitive material and polyvinyl alcohol and stirring evenly to obtain a chlorine dioxide gel solution, and freezing and drying the chlorine dioxide gel solution to obtain microencapsulated organic chlorine dioxide.

[0014] By adopting the above technical solution, the hydrogel remains stable at room temperature through the addition of thermosensitive materials, thus avoiding the premature release of chlorine dioxide. During the brushing process, the heat generated by friction causes a slight increase in local temperature. When the thermosensitive material senses this temperature change, a phase change occurs, prompting the release of the chlorine dioxide encapsulated therein. The release of chlorine dioxide is synchronized with the brushing behavior, thereby enhancing its immediate effect, reducing unnecessary long-term exposure, and improving safety of use.

[0015] Polyvinyl alcohol as the shell material of the microcapsule can form a three-dimensional network structure with the paste-based material sodium polyacrylate. This structure has excellent water absorption capacity and biocompatibility, can better wrap chlorine dioxide to prevent unnecessary reactions during storage, and enhance the stability and use effect of the toothpaste.

[0016] Optionally, the paste-based material may be sodium polyacrylate, xanthan gum, sodium carboxymethyl cellulose, carrageenan, and the like.

[0017] Preferably, the paste-based material is sodium polyacrylate.

[0018] By adopting the above technical solution, sodium polyacrylate is selected as the paste-based material to stably carry the chlorine dioxide solution and evenly disperse it in the paste, and release chlorine dioxide molecules when brushing teeth to play an anti-caries effect. At the same time, the good stability of sodium polyacrylate also ensures the lasting effectiveness of chlorine dioxide in toothpaste. Even during long-term storage and use, chlorine dioxide can maintain its bactericidal activity, thereby continuously playing an anti-caries and whitening effect. In addition, sodium polyacrylate has good compatibility with polyvinyl alcohol, which is conducive to the uniform distribution of organic chlorine dioxide microcapsules in toothpaste and improves the use effect of toothpaste.

[0019] Optionally, the weight ratio of the polyvinyl pyrrolidone solution to the temperature-sensitive material and polyvinyl alcohol in the organic chlorine dioxide solution is 1:0.5-0.8:1.2.

[0020] Optionally, the temperature-sensitive material is poly(N-isopropylacrylamide).

[0021] By adopting the above technical solution, poly(N-isopropylacrylamide) has good temperature responsiveness, can trigger the controlled release of chlorine dioxide at the oral temperature, and provide a continuous and mild antibacterial effect. When brushing teeth, the temperature change causes the response of poly(N-isopropylacrylamide), and gradually releases the chlorine dioxide wrapped inside it, which not only ensures the effective utilization of active ingredients, but also avoids the problem of irritation caused by direct contact of high-concentration chlorine dioxide released at one time. At the same time, it has good biocompatibility and is easy to mix with other ingredients without affecting its own sensitivity, ensuring the integrity of the microcapsule structure.

[0022] In a second aspect, the present application provides a method for preparing a novel chlorine dioxide-containing anti-caries toothpaste, using the following technical solution: A method for preparing a novel chlorine dioxide-containing anti-caries toothpaste comprises the following steps: (1) adding an appropriate amount of sodium polyacrylate to an organic chlorine dioxide solution and stirring at high speed to obtain a polymer viscous paste, and then soaking for 12-15 hours and homogenizing to obtain a toothpaste mixture; (2) filling, sealing and packaging the prepared toothpaste mixture to obtain a finished anti-caries toothpaste containing chlorine dioxide.

[0023] In summary, this application has the following beneficial effects: 1. The toothpaste of the present invention innovatively solves the problem of dental plaque formation by utilizing the efficient bactericidal properties of chlorine dioxide and combining the complexing and stabilizing effect of polyvinylpyrrolidone (PVP). Compared with traditional toothpaste, the toothpaste of the present invention not only has the effect of preventing caries and whitening teeth, but also has long-lasting and efficient bactericidal properties. In addition, the toothpaste prepared in this application does not contain fluoride, and prevents caries and dental plaque through the bactericidal ability of chlorine dioxide, avoiding the risk of dental fluorosis. The preparation process involved is simple and convenient for industrial production. At the same time, because there is no fluoride, the toothpaste of the present invention has less effect on the beneficial bacteria in the oral cavity and is healthier.

[0024] 2. In this application, the present solution is preferably used to achieve the precise controlled release of chlorine dioxide in the oral cavity through microencapsulation technology, thereby ensuring its strong antibacterial effect and enhancing the ability of toothpaste to clean and protect teeth. At the same time, it alleviates the discomfort caused by high concentrations of chlorine dioxide to the oral cavity, and slowly releases it during brushing, achieving an effective sterilization effect while bringing a good user experience.

[0025] 3. The method of the present application not only simplifies the production process of traditional toothpaste, but also makes the toothpaste unnecessary to add acid for activation during use, thereby simplifying the use process and improving the convenience of use. DETAILED DESCRIPTION

[0026] The present application is further described in detail below with reference to the embodiments.

[0027] If the specific conditions are not specified in the examples, the experiments were carried out under conventional conditions or conditions recommended by the manufacturer. If the manufacturers of the reagents or instruments are not specified, they are all conventional products that can be purchased commercially.

[0028] Poly(N-isopropylacrylamide) was purchased from Hubei Tosoh Chemical Technology Co., Ltd., CAS No.: 25189-55-3, density 0.879 g / cm 3 Sodium polyacrylate was purchased from Renqiu Shuangcheng Chemical Products Factory, model 0687, density 0.80 g / cm 3 ; Polyvinyl pyrrolidone was purchased from Jinan Huijinchuan Trading Co., Ltd., model K30; polyvinyl alcohol was purchased from Wuhan Kangqiong Biopharmaceutical Technology Co., Ltd., model PVA-217.

[0029] Preparation examples of raw materials and / or intermediates Preparation Example 1 An organic chlorine dioxide solution, the preparation of which comprises the following steps: (1) dissolving 140 g of sodium chlorite in 800 g of purified water and heating to 50° C., slowly adding 65 g of citric acid monohydrate and stirring to react, slowly washing the generated gas with water twice at 35° C., and then passing it into purified water until the concentration of chlorine dioxide in the purified water reaches 650 ppm, thereby obtaining a solution containing chlorine dioxide gas; (2) 840 g of a 10% polyvinyl pyrrolidone solution was heated to 50° C., 100 g of the obtained solution containing chlorine dioxide gas was added and stirred evenly, then the temperature was lowered to below 37° C., 20 g of sodium dodecyl sulfate was added and stirred thoroughly to obtain a stable organic chlorine dioxide solution.

[0030] Preparation Example 2 An organic chlorine dioxide solution, the preparation of which comprises the following steps: (1) dissolving 150 g of sodium chlorite in 770 g of purified water and heating to 45° C., slowly adding 70 g of citric acid monohydrate and stirring to react, slowly washing the generated gas with water twice at 20° C., and then passing it into purified water until the concentration of chlorine dioxide in the purified water reaches 700 ppm, thereby obtaining a solution containing chlorine dioxide gas; (2) 825 g of a 10% polyvinyl pyrrolidone solution was heated to 55° C., 90 g of the obtained solution containing chlorine dioxide gas was added and stirred evenly, then the temperature was lowered to below 37° C., 25 g of sodium dodecyl sulfate was added and stirred thoroughly to obtain a stable organic chlorine dioxide solution.

[0031] Preparation Example 3 An organic chlorine dioxide solution, the preparation of which comprises the following steps: (1) dissolving 160 g of sodium chlorite in 785 g of purified water and heating to 45° C., slowly adding 60 g of citric acid monohydrate and stirring to react, slowly washing the generated gas with water twice at 15° C., and then passing it into purified water until the concentration of chlorine dioxide in the purified water reaches 600 ppm, thereby obtaining a solution containing chlorine dioxide gas; (2) 855 g of a 10% polyvinyl pyrrolidone solution was heated to 45° C., 95 g of the obtained solution containing chlorine dioxide gas was added and stirred evenly, then the temperature was lowered to below 37° C., 30 g of sodium dodecyl sulfate was added and stirred thoroughly to obtain a stable organic chlorine dioxide solution.

[0032] Preparation Example 4 A microencapsulated organic chlorine dioxide, which is different from Preparation Example 1 in that a temperature-sensitive material and polyvinyl alcohol are added to the organic chlorine dioxide solution of this Preparation Example: specifically comprising the following steps: (1) dissolving 140 g of sodium chlorite in 800 g of purified water and heating to 50° C., slowly adding 65 g of citric acid monohydrate and stirring to react, slowly washing the generated gas with water twice at 35° C., and then passing it into purified water until the concentration of chlorine dioxide in the purified water reaches 650 ppm, thereby obtaining a solution containing chlorine dioxide gas; (2) 840 g of a 10% polyvinyl pyrrolidone solution was heated to 50° C., 100 g of the obtained solution containing chlorine dioxide gas was added and stirred evenly, then the temperature was lowered to below 37° C., 20 g of sodium dodecyl sulfate was added and stirred well, 420 g of poly(N-isopropylacrylamide) and 1008 g of polyvinyl alcohol were added and stirred evenly to obtain a chlorine dioxide gel solution, and the chlorine dioxide gel solution was freeze-dried to obtain microencapsulated organic chlorine dioxide.

[0033] Preparation Example 5 A microencapsulated organic chlorine dioxide, which is different from Preparation Example 4 in that 672 g of poly(N-isopropylacrylamide) is added in this Preparation Example.

[0034] Preparation Example 6 A microencapsulated organic chlorine dioxide, which is different from Preparation Example 4 in that 546 g of poly(N-isopropylacrylamide) is added in this Preparation Example.

[0035] Preparation Example 7 A microencapsulated organic chlorine dioxide, which is different from Preparation Example 4 in that no polyvinyl alcohol is added in this Preparation Example. Example

[0036] Example 1 A novel anti-caries toothpaste containing chlorine dioxide, the preparation of which comprises the following steps: (1) 50 g of sodium polyacrylate was added to 950 g of the organic chlorine dioxide solution prepared in Preparation Example 1 and stirred at high speed to completely dissolve the sodium polyacrylate, and water was added to adjust the viscosity to 6500 mPa.s ± 10% to obtain a high molecular viscous paste, which was soaked for 12 hours and homogenized to obtain a toothpaste mixture; (2) filling, sealing and packaging the prepared polymer viscous paste mixture to obtain a finished chlorine dioxide toothpaste.

[0037] Example 2 A novel anti-caries toothpaste containing chlorine dioxide, the preparation of which comprises the following steps: (1) 35 g of xanthan gum was added to 965 g of the organic chlorine dioxide solution prepared in Preparation Example 1 and stirred at high speed to completely dissolve the sodium polyacrylate, and water was added to adjust the viscosity to 6500 mPa.s ± 10% to obtain a high molecular viscous paste, which was soaked for 13 h and homogenized to obtain a toothpaste mixture; (2) filling, sealing and packaging the prepared polymer viscous paste mixture to obtain a finished chlorine dioxide toothpaste.

[0038] Example 3 A novel anti-caries toothpaste containing chlorine dioxide, the preparation of which comprises the following steps: (1) adding 20 g of sodium polyacrylate to 980 g of the organic chlorine dioxide solution prepared in Preparation Example 1 and stirring at high speed to completely dissolve the sodium polyacrylate, adding water to adjust the viscosity to 6500 mPa.s±10% to obtain a high molecular viscous paste, and soaking for 15 hours to obtain a toothpaste mixture after homogenization; (2) filling, sealing and packaging the prepared polymer viscous paste mixture to obtain a finished chlorine dioxide toothpaste.

[0039] Example 4 A novel anti-caries toothpaste containing chlorine dioxide is different from Example 1 in that the organic chlorine dioxide solution added in this example is prepared in Preparation Example 2.

[0040] Example 5 A novel anti-caries toothpaste containing chlorine dioxide, which is different from Example 1 in that the organic chlorine dioxide solution added in this example is prepared in Preparation Example 3.

[0041] Example 6 A novel anti-caries toothpaste containing chlorine dioxide is different from Example 1 in that the organic chlorine dioxide solution added in this example is the microencapsulated organic chlorine dioxide prepared in Preparation Example 4.

[0042] Example 7 A novel anti-caries toothpaste containing chlorine dioxide is different from Example 1 in that the organic chlorine dioxide solution added in this example is the microencapsulated organic chlorine dioxide prepared in Preparation Example 5.

[0043] Example 8 A novel anti-caries toothpaste containing chlorine dioxide is different from Example 1 in that the organic chlorine dioxide solution added in this example is the microencapsulated organic chlorine dioxide prepared in Preparation Example 6.

[0044] Example 9 A novel anti-caries toothpaste containing chlorine dioxide, which is different from Example 6 in that the organic chlorine dioxide solution added in this example is the microencapsulated organic chlorine dioxide prepared in Preparation Example 7.

[0045] Example 10 A novel anti-caries toothpaste containing chlorine dioxide, which is different from Example 6 in that the paste base material used in this example is xanthan gum.

[0046] Embodiment 11 A novel anti-caries toothpaste containing chlorine dioxide, which is different from Example 6 in that the paste base material used in this example is sodium carboxymethyl cellulose.

[0047] Comparative Example Comparative Example 1 A caries-preventing toothpaste containing chlorine dioxide, comprising the following preparation steps: (1) dissolving 140 g of sodium chlorite in 800 g of purified water and heating to 50° C., slowly adding 65 g of citric acid monohydrate and stirring to react, slowly washing the generated gas with water twice at 35° C., and then passing it into purified water until the concentration of chlorine dioxide in the purified water reaches 650 ppm, thereby obtaining a solution containing chlorine dioxide gas; (2) After heating 840 g of water to 50° C., 100 g of the prepared solution containing chlorine dioxide gas was added and stirred evenly, then the temperature was lowered to below 37° C., 20 g of sodium dodecyl sulfate was added and stirred thoroughly to obtain a stable organic chlorine dioxide solution; (3) 50 g of sodium polyacrylate was added to 950 g of the organic chlorine dioxide solution prepared in Preparation Example 1 and stirred at high speed to completely dissolve the sodium polyacrylate, and water was added to adjust the viscosity to 6500 mPa.s ± 10% to obtain a high molecular viscous paste, which was soaked for 12 h and homogenized to obtain a toothpaste mixture; (4) filling, sealing and packaging the prepared polymer viscous paste mixture to obtain a finished chlorine dioxide toothpaste.

[0048] Performance testing Detection method / test method Stability test: The test is carried out in accordance with the relevant provisions of the room temperature sample retention method as shown in 2.2.3.2.2 of the 2002 edition of the standard "Technical Specifications for Disinfection". The temperature is placed in an environment of 25±2℃. On the last day of the two-year validity period, samples are taken to measure the content of active ingredients, calculate the rate of decrease in the content of active ingredients, and record it to indicate the stability of the toothpaste.

[0049] Antibacterial performance test: According to the method shown in 2.1.1 Disinfectant Microbial Killing Test in the 2002 edition of the standard "Technical Specifications for Disinfection", Staphylococcus aureus was used. The 5th generation of the test bacteria on the nutrient agar medium slant culture (24h) was washed with 5mL 0.03mol / L phosphate buffer (hereinafter referred to as PBS) and diluted with the above PBS to make a concentration of 5×10 4 cfu / mL of bacterial suspension. Take 1g of each toothpaste prepared in the example and the comparative example, mix them evenly with 5mL of pure water respectively, as the sample liquid, take 5mL of the sample liquid and the control sample liquid (containing only the paste base material). Add 100uL of the above bacterial suspension to each sample liquid respectively, mix evenly, start the timing for 30s, 3min, and 20min, use a sterile pipette to take the mixed sample liquid (0.5mL) and put it into a test tube containing 5mL PBS, mix it thoroughly, take 0.5mL respectively, place it in two plates, pour 15mL of nutrient agar culture medium cooled to 40-50℃, rotate the plate to make it fully uniform, turn the plate over after the agar solidifies, and culture it at 35℃±2℃ for 48h to count the live bacterial colonies. The test was repeated 3 times, and the antibacterial rate was calculated according to the following formula: X = (AB) / A × 100%; Where: X is the inhibition rate, A is the average colony count of the control sample, and B is the average colony count of the test sample.

[0050] Skin and mucous membrane irritation test: According to the Technical Requirements for Hygiene and Safety Evaluation of Disinfection Products (WS628-2018), the toothpaste prepared in the examples and comparative examples was subjected to a complete skin irritation test (each sample was tested on 3 rabbits): about 24 hours before the experiment, the hair on both sides of the back spine of the rabbit was removed without damaging the skin. The hair removal range was about 3cmx3cm on the left and right. 0.5ml of the test sample was applied to the skin, and then covered with two layers of gauze and one layer of cellophane, and fixed with adhesive tape. 0.5ml of distilled water was applied to the other side of the skin as a blank control. The application time was 2 hours, and the test substance was rinsed with warm water for 1min to remove the test substance. The local skin reaction was observed 1 hour, 24 hours, and 48 hours after the test substance was removed, and the skin irritation reaction was scored according to Table 1. The rabbits used were New Zealand rabbits with intact skin, female, weighing 2.0-2.5kg, and fed with ordinary rabbit maintenance feed, with a temperature of 20-26℃ and a relative humidity of 40%-70%.

[0051] Table 1 Table 2 Test results Combining Examples 1-3 and Comparative Example 1 and Table 2, it can be seen that the test data of Examples 1-3 are better than those of Comparative Example 1, indicating that the complexation with polyvinyl pyrrolidone can improve the stability of chlorine dioxide in toothpaste, improve the activity and long-term effect of chlorine dioxide, and prepare a toothpaste with long-lasting and stable bactericidal effect.

[0052] Combining Examples 1-8 and the data in Table 2, it can be seen that the initial antibacterial rate of Example 1-5 at 30s is higher than that of Example 6-8, and the remaining experimental data of Example 6-8 are better than that of Example 1-5. Due to the slow release of the material encapsulation, Example 6-8 reduces the stimulation of high-concentration chlorine dioxide and is completely released within 3 minutes, achieving a good and complete antibacterial effect. This shows that adding thermosensitive materials and polyvinyl alcohol to the organic chlorine dioxide solution to microencapsulate it can further improve the stability of chlorine dioxide, control the release in a direction, and synchronize the release of chlorine dioxide with the brushing behavior, thereby enhancing its immediate effect and improving the bactericidal effect.

[0053] Combining Example 6 with Example 9 and Table 2, it can be seen that the various test data of Example 6 are better than those of Example 9, indicating that polyvinyl alcohol and the temperature-sensitive material work synergistically to improve the stability of the material and obtain a better sterilization effect.

[0054] Combining Example 1 with Examples 10-11 and Table 2, it can be seen that the various test data of Example 1 are better than those of Examples 10-11, indicating that the selection of sodium polyacrylate as the paste-based material has better compatibility with microencapsulated organic chlorine dioxide, which is beneficial to the uniform distribution of chlorine dioxide in the toothpaste and improves the antibacterial effect.

[0055] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make modifications to the present embodiment without any creative contribution as needed, but such modifications are protected by the patent law as long as they are within the scope of the claims of the present application.

Claims

1. A novel anti-caries toothpaste containing chlorine dioxide, characterized in that: The invention comprises active ingredients and cream-based materials. The active ingredients are a solution containing chlorine dioxide gas and a polyvinyl pyrrolidone solution to obtain a stable organic chlorine dioxide solution.

2. A novel anti-caries toothpaste containing chlorine dioxide according to claim 1, characterized in that: The toothpaste comprises 95-98 parts of organic chlorine dioxide solution and 2-5 parts of paste base material.

3. A novel anti-caries toothpaste containing chlorine dioxide according to claim 1, characterized in that: The preparation of the organic chlorine dioxide solution comprises the following steps: (1) preparing chlorine dioxide gas by reacting sodium chlorite with citric acid monohydrate, washing it twice with water, and then introducing it into purified water until the concentration of chlorine dioxide in the purified water reaches 600-700 ppm, thereby obtaining a solution containing chlorine dioxide gas; (2) Heat a 10% polyvinyl pyrrolidone solution to 45-55°C, add the prepared solution containing chlorine dioxide gas and stir evenly, cool to below 37°C, add sodium dodecyl sulfate and stir thoroughly to obtain a stable organic chlorine dioxide solution.

4. A novel anti-caries toothpaste containing chlorine dioxide according to claim 1, characterized in that: The organic chlorine dioxide solution may also be added with a temperature-sensitive material and polyvinyl alcohol to prepare microcapsules which are added to the toothpaste, specifically comprising the following steps: After adding sodium dodecyl sulfate and stirring evenly, adding the temperature-sensitive material and polyvinyl alcohol and stirring evenly to obtain chlorine dioxide gel solution, and freezing and drying the chlorine dioxide gel solution to obtain microencapsulated organic chlorine dioxide.

5. A novel anti-caries toothpaste containing chlorine dioxide according to claim 4, characterized in that: The paste-based material is sodium polyacrylate.

6. A novel anti-caries toothpaste containing chlorine dioxide according to claim 4, characterized in that: The weight ratio of the polyvinyl pyrrolidone solution, the temperature-sensitive material and the polyvinyl alcohol added to the organic chlorine dioxide solution is 1:0.5-0.8:1.

2.

7. A novel anti-caries toothpaste containing chlorine dioxide according to claim 1, characterized in that: The temperature-sensitive material is poly(N-isopropylacrylamide).

8. A method for preparing a novel anti-caries toothpaste containing chlorine dioxide according to any one of claims 1 to 7, characterized in that: The steps include: (1) Add an appropriate amount of sodium polyacrylate to an organic chlorine dioxide solution and stir at high speed to obtain a high molecular viscous paste, soak for 12-15 hours and homogenize to obtain a toothpaste mixture; (2) Filling, sealing and packaging the prepared toothpaste mixture to obtain a finished anti-caries toothpaste containing chlorine dioxide.