Gingiva protecting and tooth strengthening toothpaste containing bioactive glass and preparation method thereof
By combining modified bioactive glass powder with chitosan-polyphenol microspheres, a toothpaste matrix was prepared, which solved the problem of toothpaste lacking bio-repair function and achieved excellent gum protection and tooth strengthening effects with tooth remineralization and anti-sensitivity properties.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-13
- Publication Date
- 2026-03-31
AI Technical Summary
Existing toothpaste products lack active biological repair functions and cannot effectively promote the remineralization of tooth hard tissues and the self-healing of microcracks, making it difficult to solve problems such as early tooth decay and dentin hypersensitivity.
Strontium-reinforced bioactive glass powder was modified with a silane coupling agent, and then reacted with L-lysine and furfural to prepare modified bioglass. This modified bioglass was then combined with chitosan-polyphenol microspheres to prepare a toothpaste matrix. Finally, dicalcium phosphate and surfactants were added to form a toothpaste containing bioactive glass for gum protection and tooth strengthening.
It significantly improves antibacterial activity against oral pathogens, promotes enamel remineralization, reduces tooth sensitivity, improves gum health, provides long-lasting oral protection, enhances teeth's resistance to acid erosion, and promotes the repair of oral soft and hard tissues.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of oral care, specifically to a toothpaste containing bioactive glass for gum protection and tooth strengthening, and its preparation method. Background Technology
[0002] As one of the most promising bioactive materials of the 21st century, bioglass has undergone nearly fifty years of rapid development since Larry Hill invented 45S5 bioglass in 1970. Strontium-reinforced bioactive glass, representing the third generation of bioglass, has a unique chemical composition containing basic components such as silicon dioxide, sodium oxide, calcium oxide, and phosphorus oxide. The doping of strontium ions significantly enhances the material's bioactivity and osteoinductive properties. This material can rapidly form a hydroxyapatite layer in the body fluid environment, chemically bonding with human hard tissue to achieve true biobonding.
[0003] Existing toothpaste products have many limitations in terms of technology, which seriously restricts their effectiveness in maintaining oral health and treating diseases. Traditional toothpaste mainly relies on fluoride to prevent cavities and mechanical abrasives for cleaning, lacking active biological repair functions. It cannot effectively promote the remineralization of tooth hard tissues and the self-healing of microcracks, making it difficult to fundamentally solve problems such as early caries and dentin hypersensitivity. Summary of the Invention
[0004] This invention discloses a toothpaste containing bioactive glass for protecting and strengthening gums and its preparation method. The toothpaste containing modified bioactive glass prepared by this invention is cost-effective, effectively antibacterial and protects gums, provides excellent comfort, exhibits superior remineralization and desensitization properties, is long-lasting, continuously releases functional ions, provides long-lasting oral protection, improves oral health, and solves the technical problem of poor enamel repair function in existing toothpastes.
[0005] This invention protects a toothpaste for protecting and strengthening gums containing bioactive glass. The toothpaste is prepared by modifying strontium-reinforced bioactive glass powder with a silane coupling agent, reacting it with L-lysine and furfural to obtain modified bioglass, preparing chitosan-polyphenol microspheres, mixing the modified bioglass, chitosan-polyphenol microspheres, glycerin, sorbitol, carbomer, calcium hydrogen phosphate, and sodium fluoride to obtain the toothpaste base, adding surfactants, preservatives, sweeteners, and fragrances, and then vacuum degassing the mixture.
[0006] Preferably, the modified bioglass is prepared through the following specific steps: S1. Strontium-reinforced bioactive glass powder was ultrasonically dispersed in anhydrous ethanol, 3-aminopropyltriethoxysilane was added, and the mixture was reacted at 80°C for 4 hours under nitrogen protection. After filtration, the precipitate was washed three times with anhydrous ethanol and dried under vacuum at 60°C for 2 hours to obtain the intermediate. S2. The intermediate was dispersed in toluene, L-lysine and furfural were added, and the mixture was reacted at 110°C for 6 hours. After filtration, the modified bioglass was obtained.
[0007] Preferably, the chitosan-polyphenol microspheres are prepared by the following specific steps: dissolving chitosan in a 3% acetic acid solution, adding tannic acid, stirring at 800 r / min for 30 min, adjusting the pH to 4.5 with 1M sodium hydroxide solution, reacting at 25~35℃ for 2 h, spray drying, and sieving through a 100-mesh sieve to obtain chitosan-polyphenol complex microspheres.
[0008] Preferably, in S1, the weight ratio of the strontium-reinforced bioactive glass powder, anhydrous ethanol, and 3-aminopropyltriethoxysilane is 15~20:200:2~3.
[0009] Preferably, in S2, the weight ratio of the intermediate, toluene, L-lysine and furfural is 15~20:150:1.5~2:1~1.5.
[0010] Preferably, the weight ratio of chitosan, 3% acetic acid solution and tannic acid is 2~3:100:1.5~2.
[0011] Preferably, the specific conditions for spray drying are: inlet air temperature set to 150°C, outlet air temperature set to 80°C, and feed rate set to 5 mL / min.
[0012] This invention also protects a method for preparing the above-mentioned gum-protecting and tooth-strengthening toothpaste, specifically comprising the following steps: Step 1: Mix glycerin, sorbitol and carbomer 934P and stir at 800 rpm for 45 minutes. Add modified bioglass, chitosan-polyphenol microspheres, dicalcium phosphate and sodium fluoride, and stir at 800 rpm for 30 minutes to obtain the toothpaste base. Step 2: Add sodium lauryl ether sulfate and cocamidopropyl betaine to the toothpaste base, stir at 600 r / min for 20 minutes, then add sodium benzoate, sodium saccharin and peppermint oil, stir evenly, and perform vacuum degassing treatment at -0.06 MPa for 15-20 minutes to obtain gum-protecting and tooth-strengthening toothpaste.
[0013] Preferably, in step one, the weight ratio of glycerol, sorbitol, carbomer 934P, modified bioglass, chitosan-polyphenol microspheres, dicalcium phosphate, and sodium fluoride is 12:8~10:2~3:8~10:4~5:6~8:0.2~0.3.
[0014] Preferably, in step two, the weight ratio of sodium lauryl ether sulfate, cocamidopropyl betaine, toothpaste base, sodium benzoate, sodium saccharin and peppermint oil is 1~1.5:0.5~1:40:0.1~0.2:0.2~0.3:0.3~0.4.
[0015] The present invention has the following beneficial effects: (1) This invention uses modified bioglass as the core component. Strontium-reinforced bioactive glass powder is modified with a silane coupling agent and reacted with L-lysine and furfural to obtain modified bioglass, which significantly improves the antibacterial activity against oral pathogens. The modified bioglass can continuously release Ca 2+ PO4 3- Beneficial ions promote the remineralization process of tooth enamel, effectively repairing early caries. At the same time, the introduction of strontium ions enhances the bioactivity of bone tissue, promotes periodontal health, and is safe, environmentally friendly, and has no side effects. Meanwhile, the modified bioglass, through surface functionalization, significantly improves its biocompatibility and stability in the oral environment. It can exchange ions with calcium and phosphorus ions in saliva to form a bone-like apatite deposit layer, which can not only seal dentinal tubules and reduce tooth sensitivity, but also release antibacterial ions for a long time, maintain the oral microecological balance, and effectively prevent the occurrence of caries and gingivitis.
[0016] (2) The chitosan-polyphenol microspheres prepared by the present invention have good sustained-release properties and contain rich active functional groups. They can not only buffer and regulate the pH of the oral cavity, but also continuously release antioxidant active substances, remove free radicals in the oral cavity, and play an anti-inflammatory and gingival protection role, thereby improving symptoms such as gingival bleeding and swelling, and improving oral health.
[0017] (3) In the composite formula used in this invention, dicalcium phosphate is used as a mild abrasive, which works synergistically with modified bioglass and chitosan-polyphenol microspheres. It has the characteristics of moderate raw material cost and stable performance. Dicalcium phosphate can provide appropriate cleaning power. At the same time, the composite system can form a protective film on the tooth surface, improve the microstructure of tooth enamel, enhance the tooth's resistance to acid erosion, reduce the incidence of tooth decay, promote the repair of oral soft and hard tissues, activate local immune defense, prevent the occurrence of oral infectious diseases, and relieve local inflammation caused by gingivitis. It also has the functions of promoting periodontal tissue regeneration, promoting the healing of oral ulcers, enhancing saliva secretion, and promoting oral blood circulation.
[0018] (4) The modified bioglass prepared in this invention undergoes surface modification treatment, so that the powder surface has active functional groups such as amino and carboxyl groups. The amino groups can bind with the chitosan molecular chain, and the carboxyl groups can chelate with calcium ions, thereby promoting the uniform dispersion of the modified powder in the toothpaste matrix, so that the functional components can be evenly distributed in the oral cavity, thereby enhancing the antibacterial effect and improving the remineralization efficiency.
[0019] (5) The toothpaste product of the present invention is mainly composed of bioactive components. This composite toothpaste containing modified bioglass has excellent rheological properties and stability. The paste is delicate and smooth, and the user experience is comfortable. It has significant antibacterial, gum-protecting and tooth-strengthening effects, good durability, and moderate bioactive component content. During daily brushing, the modified bioglass can effectively release functional ions into the oral environment. Through the ion exchange mechanism, it forms a protective layer on the tooth surface and continues to play a role. It achieves the purpose of cleaning the oral cavity and also achieves the effect of long-term care. The release process is gentle and continuous and will not irritate the oral mucosa. The natural surfactants added to the toothpaste formula ensure good foaming and cleaning power. At the same time, the taste is fresh after use, which improves the user experience and the effect of use.
[0020] (6) The toothpaste containing modified bioglass prepared by this invention has a reasonable cost, can effectively protect gums and has excellent comfort, excellent remineralization and antisensitivity performance, strong durability, continuous release of functional ions, provides long-lasting oral protection, improves oral health, is loved by consumers and is worth promoting. Detailed Implementation
[0021] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.
[0022] The strontium-reinforced bioactive glass powder used in this application's embodiments is from Jiangsu Qiuzheng New Material Technology Co., Ltd., model QZ-0020, with a mesh size of 12,500; the chitosan used is from Zhejiang Jinke Pharmaceutical Co., Ltd., with a molecular weight of 100,000 to 300,000 DA; the sodium lauryl ether sulfate used is from Hubei Kangdis Chemical Co., Ltd., CAS number 9004-82-4; the cocamidopropyl betaine used is from Suzhou Minghua Sugar Alcohol Co., Ltd., CAS number 4292-10-8; and the carbomer 934P used is from Shaanxi Benhe Bioengineering Co., Ltd., CAS number 9007-20-9.
[0023] Example 1 Step 1: Preparation of modified bioglass: Take 17.5 parts of strontium-reinforced bioactive glass powder and ultrasonically disperse it in 200 parts of anhydrous ethanol. The ultrasonic frequency is set to 40 kHz and the ultrasonic time is 30 minutes. Add 2.5 parts of 3-aminopropyltriethoxysilane and react at 80℃ for 4 hours under nitrogen protection. During the reaction, maintain the stirring speed at 300 r / min. After the reaction is completed, filter and wash the precipitate three times with anhydrous ethanol, 50 mL each time. Dry under vacuum at 60℃ for 2 hours with a vacuum degree of -0.08 MPa to obtain an intermediate. Disperse 17.5 parts of the intermediate in 150 parts of toluene, add 1.75 parts of L-lysine and 1.25 parts of furfural, and react at 110℃ for 6 hours. During the reaction, maintain the stirring speed at 200 r / min and nitrogen protection. After the reaction is completed, filter and wash twice with toluene. Dry under vacuum at 60℃ for 3 hours to obtain modified bioglass.
[0024] Step 2: Preparation of chitosan-polyphenol microspheres: Dissolve 2.5 parts of chitosan in 100 parts of 3% acetic acid solution and stir at room temperature for 2 hours until completely dissolved. Add 1.75 parts of tannic acid and stir at 800 r / min for 30 minutes. Adjust the pH to 4.5 with 1M sodium hydroxide solution. After reacting at 30℃ for 2 hours, spray dry the product. Set the inlet air temperature to 150℃, the outlet air temperature to 80℃, and the feed rate to 5 mL / min. Sieve through a 100-mesh sieve to obtain chitosan-polyphenol complex microspheres.
[0025] Step 3: Toothpaste base preparation: Mix 12 parts glycerin, 9 parts sorbitol and 2.5 parts carbomer 934P, and stir at 800 r / min for 45 minutes. Add 9 parts modified bioglass, 4.5 parts chitosan-polyphenol microspheres, 7 parts dicalcium phosphate and 0.25 parts sodium fluoride, and stir at 800 r / min for 30 minutes to obtain the toothpaste base.
[0026] Step 4: Final product preparation: Add 1.25 parts of sodium lauryl ether sulfate and 0.75 parts of cocamidopropyl betaine to 40 parts of toothpaste base, stir at 600 r / min for 20 minutes, add 0.15 parts of sodium benzoate, 0.25 parts of sodium saccharin and 0.35 parts of peppermint oil, stir evenly, and perform vacuum degassing treatment at -0.06 MPa for 18 minutes to obtain gum-protecting and tooth-strengthening toothpaste.
[0027] Example 2 Step 1: Preparation of modified bioglass: Take 15 parts of strontium-reinforced bioactive glass powder and ultrasonically disperse it in 200 parts of anhydrous ethanol. The ultrasonic frequency is set to 40 kHz and the ultrasonic time is 30 minutes. Add 2 parts of 3-aminopropyltriethoxysilane and react at 80℃ for 4 hours under nitrogen protection. During the reaction, maintain the stirring speed at 300 r / min. After the reaction is completed, filter and wash the precipitate three times with anhydrous ethanol, 50 mL each time. Dry under vacuum at 60℃ for 2 hours with a vacuum degree of -0.08 MPa to obtain an intermediate. Disperse 15 parts of the intermediate in 150 parts of toluene, add 1.5 parts of L-lysine and 1 part of furfural, and react at 110℃ for 6 hours. During the reaction, maintain the stirring speed at 200 r / min and nitrogen protection. After the reaction is completed, filter and wash twice with toluene. Dry under vacuum at 60℃ for 3 hours to obtain modified bioglass.
[0028] Step 2: Preparation of chitosan-polyphenol microspheres: Dissolve 2 parts of chitosan in 100 parts of 3% acetic acid solution and stir at room temperature for 2 hours until completely dissolved. Add 1.5 parts of tannic acid and stir at 800 r / min for 30 minutes. Adjust the pH to 4.5 with 1M sodium hydroxide solution. After reacting at 25℃ for 2 hours, spray dry the product. Set the inlet air temperature to 150℃, the outlet air temperature to 80℃, and the feed rate to 5 mL / min. Sieve through a 100-mesh sieve to obtain chitosan-polyphenol complex microspheres.
[0029] Step 3: Toothpaste base preparation: Mix 12 parts glycerin, 8 parts sorbitol and 2 parts carbomer 934P, stir at 800 r / min for 45 minutes, add 8 parts modified bioglass, 4 parts chitosan-polyphenol microspheres, 6 parts dicalcium phosphate and 0.2 parts sodium fluoride, stir at 800 r / min for 30 minutes to obtain the toothpaste base.
[0030] Step 4: Final product preparation: Add 1 part sodium lauryl ether sulfate and 0.5 parts cocamidopropyl betaine to 40 parts toothpaste base, stir at 600 r / min for 20 minutes, add 0.1 parts sodium benzoate, 0.2 parts sodium saccharin and 0.3 parts peppermint oil, stir evenly, and perform vacuum degassing treatment at -0.06 MPa for 15 minutes to obtain gum-protecting and tooth-strengthening toothpaste.
[0031] Example 3 Step 1: Preparation of modified bioglass: Take 20 parts of strontium-reinforced bioactive glass powder and ultrasonically disperse it in 200 parts of anhydrous ethanol. The ultrasonic frequency is set to 40 kHz and the ultrasonic time is 30 minutes. Add 3 parts of 3-aminopropyltriethoxysilane and react at 80℃ for 4 hours under nitrogen protection. During the reaction, maintain the stirring speed at 300 r / min. After the reaction is completed, filter and wash the precipitate three times with anhydrous ethanol, 50 mL each time. Dry under vacuum at 60℃ for 2 hours with a vacuum degree of -0.08 MPa to obtain an intermediate. Disperse 20 parts of the intermediate in 150 parts of toluene, add 2 parts of L-lysine and 1.5 parts of furfural, and react at 110℃ for 6 hours. During the reaction, maintain the stirring speed at 200 r / min and nitrogen protection. After the reaction is completed, filter and wash twice with toluene. Dry under vacuum at 60℃ for 3 hours to obtain modified bioglass.
[0032] Step 2: Preparation of chitosan-polyphenol microspheres: Dissolve 3 parts of chitosan in 100 parts of 3% acetic acid solution and stir at room temperature for 2 hours until completely dissolved. Add 2 parts of tannic acid and stir at 800 r / min for 30 minutes. Adjust the pH to 4.5 with 1M sodium hydroxide solution. After reacting at 35℃ for 2 hours, spray dry the product. Set the inlet air temperature to 150℃, the outlet air temperature to 80℃, and the feed rate to 5 mL / min. Sieve through a 100-mesh sieve to obtain chitosan-polyphenol complex microspheres.
[0033] Step 3: Toothpaste base preparation: Mix 12 parts glycerin, 10 parts sorbitol and 3 parts carbomer 934P, stir at 800 r / min for 45 minutes, add 10 parts modified bioglass, 5 parts chitosan-polyphenol microspheres, 8 parts dicalcium phosphate and 0.3 parts sodium fluoride, stir at 800 r / min for 30 minutes to obtain the toothpaste base.
[0034] Step 4: Final product preparation: Add 1.5 parts of sodium lauryl ether sulfate and 1 part of cocamidopropyl betaine to 40 parts of toothpaste base, stir at 600 r / min for 20 minutes, add 0.2 parts of sodium benzoate, 0.3 parts of sodium saccharin and 0.4 parts of peppermint oil, stir evenly, and perform vacuum degassing treatment at -0.06 MPa for 20 minutes to obtain gum-protecting and tooth-strengthening toothpaste.
[0035] Example 4 Step 1: Preparation of modified bioglass: Take 16 parts of strontium-reinforced bioactive glass powder and ultrasonically disperse it in 200 parts of anhydrous ethanol. The ultrasonic frequency is set to 40 kHz and the ultrasonic time is 30 minutes. Add 2.2 parts of 3-aminopropyltriethoxysilane and react at 80℃ for 4 hours under nitrogen protection. During the reaction, maintain the stirring speed at 300 r / min. After the reaction is completed, filter and wash the precipitate three times with anhydrous ethanol, 50 mL each time. Dry under vacuum at 60℃ for 2 hours with a vacuum degree of -0.08 MPa to obtain an intermediate. Disperse 16 parts of the intermediate in 150 parts of toluene, add 1.6 parts of L-lysine and 1.1 parts of furfural, and react at 110℃ for 6 hours. During the reaction, maintain the stirring speed at 200 r / min and nitrogen protection. After the reaction is completed, filter and wash twice with toluene. Dry under vacuum at 60℃ for 3 hours to obtain modified bioglass.
[0036] Step 2: Preparation of chitosan-polyphenol microspheres: Dissolve 2.2 parts of chitosan in 100 parts of 3% acetic acid solution and stir at room temperature for 2 hours until completely dissolved. Add 1.6 parts of tannic acid and stir at 800 r / min for 30 minutes. Adjust the pH to 4.5 with 1M sodium hydroxide solution. After reacting at 28℃ for 2 hours, spray dry the product. Set the inlet air temperature to 150℃, the outlet air temperature to 80℃, and the feed rate to 5 mL / min. Sieve through a 100-mesh sieve to obtain chitosan-polyphenol complex microspheres.
[0037] Step 3: Toothpaste base preparation: Mix 12 parts glycerin, 8.5 parts sorbitol and 2.2 parts carbomer 934P, and stir at 800 r / min for 45 minutes. Add 8.5 parts modified bioglass, 4.2 parts chitosan-polyphenol microspheres, 6.5 parts dicalcium phosphate and 0.22 parts sodium fluoride, and stir at 800 r / min for 30 minutes to obtain the toothpaste base.
[0038] Step 4: Final product preparation: Add 1.1 parts of sodium lauryl ether sulfate and 0.6 parts of cocamidopropyl betaine to 40 parts of toothpaste base, stir at 600 r / min for 20 minutes, add 0.12 parts of sodium benzoate, 0.22 parts of sodium saccharin and 0.32 parts of peppermint oil, stir evenly, and perform vacuum degassing treatment at -0.06 MPa for 16 minutes to obtain gum-protecting and tooth-strengthening toothpaste.
[0039] Example 5 Step 1: Preparation of modified bioglass: Take 18 parts of strontium-reinforced bioactive glass powder and ultrasonically disperse it in 200 parts of anhydrous ethanol. The ultrasonic frequency is set to 40 kHz and the ultrasonic time is 30 minutes. Add 2.8 parts of 3-aminopropyltriethoxysilane and react at 80℃ for 4 hours under nitrogen protection. During the reaction, maintain the stirring speed at 300 r / min. After the reaction is completed, filter and wash the precipitate three times with anhydrous ethanol, 50 mL each time. Dry under vacuum at 60℃ for 2 hours with a vacuum degree of -0.08 MPa to obtain an intermediate. Disperse 18 parts of the intermediate in 150 parts of toluene, add 1.8 parts of L-lysine and 1.3 parts of furfural, and react at 110℃ for 6 hours. During the reaction, maintain the stirring speed at 200 r / min and nitrogen protection. After the reaction is completed, filter and wash twice with toluene. Dry under vacuum at 60℃ for 3 hours to obtain modified bioglass.
[0040] Step 2: Preparation of chitosan-polyphenol microspheres: Dissolve 2.8 parts of chitosan in 100 parts of 3% acetic acid solution and stir at room temperature for 2 hours until completely dissolved. Add 1.8 parts of tannic acid and stir at 800 r / min for 30 minutes. Adjust the pH to 4.5 with 1M sodium hydroxide solution. After reacting at 32℃ for 2 hours, spray dry the product. Set the inlet air temperature to 150℃, the outlet air temperature to 80℃, and the feed rate to 5 mL / min. Sieve through a 100-mesh sieve to obtain chitosan-polyphenol complex microspheres.
[0041] Step 3: Toothpaste base preparation: Mix 12 parts glycerin, 9.5 parts sorbitol and 2.8 parts carbomer 934P, and stir at 800 r / min for 45 minutes. Add 9.5 parts modified bioglass, 4.8 parts chitosan-polyphenol microspheres, 7.5 parts dicalcium phosphate and 0.28 parts sodium fluoride, and stir at 800 r / min for 30 minutes to obtain the toothpaste base.
[0042] Step 4: Final product preparation: Add 1.3 parts of sodium lauryl ether sulfate and 0.7 parts of cocamidopropyl betaine to 40 parts of toothpaste base, stir at 600 r / min for 20 minutes, add 0.18 parts of sodium benzoate, 0.28 parts of sodium saccharin and 0.38 parts of peppermint oil, stir evenly, and perform vacuum degassing treatment at -0.06 MPa for 17 minutes to obtain gum-protecting and tooth-strengthening toothpaste.
[0043] Comparative Example 1: Compared with Example 1, no 3-aminopropyltriethoxysilane was added during the preparation of the modified bioglass.
[0044] Step 1: Preparation of modified bioglass: Take 17.5 parts of strontium-reinforced bioactive glass powder, disperse it in 150 parts of toluene, add 1.75 parts of L-lysine and 1.25 parts of furfural, react at 110℃ for 6 hours, maintain a stirring speed of 200 r / min during the reaction, and protect with nitrogen. After the reaction is completed, filter, wash twice with toluene, and dry under vacuum at 60℃ for 3 hours to obtain modified bioglass.
[0045] Step 2: Preparation of chitosan-polyphenol microspheres: Dissolve 2.5 parts of chitosan in 100 parts of 3% acetic acid solution and stir at room temperature for 2 hours until completely dissolved. Add 1.75 parts of tannic acid and stir at 800 r / min for 30 minutes. Adjust the pH to 4.5 with 1M sodium hydroxide solution and react at 30℃ for 2 hours. Spray dry the mixture with an inlet air temperature of 150℃, an outlet air temperature of 80℃, and a feed rate of 5 mL / min. Sieve through a 100-mesh sieve to obtain chitosan-polyphenol complex microspheres.
[0046] Step 3: Toothpaste base preparation: Mix 12 parts glycerin, 9 parts sorbitol and 2.5 parts carbomer 934P, and stir at 800 r / min for 45 minutes. Add 9 parts modified bioglass, 4.5 parts chitosan-polyphenol microspheres, 7 parts dicalcium phosphate and 0.25 parts sodium fluoride, and stir at 800 r / min for 30 minutes to obtain the toothpaste base.
[0047] Step 4: Final product preparation: Add 1.25 parts of sodium lauryl ether sulfate and 0.75 parts of cocamidopropyl betaine to 40 parts of toothpaste base, stir at 600 r / min for 20 minutes, add 0.15 parts of sodium benzoate, 0.25 parts of sodium saccharin and 0.35 parts of peppermint oil, stir evenly, and perform vacuum degassing treatment at -0.06 MPa for 18 minutes to obtain gum-protecting and tooth-strengthening toothpaste.
[0048] Comparative Example 2: Compared with Example 1, no L-lysine was added during the preparation of the modified bioglass.
[0049] Step 1: Preparation of modified bioglass: Take 17.5 parts of strontium-reinforced bioactive glass powder and ultrasonically disperse it in 200 parts of anhydrous ethanol. The ultrasonic frequency is set to 40 kHz and the ultrasonic time is 30 minutes. Add 2.5 parts of 3-aminopropyltriethoxysilane and react at 80℃ for 4 hours under nitrogen protection. During the reaction, maintain the stirring speed at 300 r / min. After the reaction is completed, filter and wash the precipitate three times with anhydrous ethanol, 50 mL each time. Dry under vacuum at 60℃ for 2 hours with a vacuum degree of -0.08 MPa to obtain an intermediate. Disperse 17.5 parts of the intermediate in 150 parts of toluene and add 1.25 parts of furfural. React at 110℃ for 6 hours, maintaining the stirring speed at 200 r / min and nitrogen protection during the reaction. After the reaction is completed, filter and wash twice with toluene. Dry under vacuum at 60℃ for 3 hours to obtain modified bioglass.
[0050] Step 2: Preparation of chitosan-polyphenol microspheres: Dissolve 2.5 parts of chitosan in 100 parts of 3% acetic acid solution and stir at room temperature for 2 hours until completely dissolved. Add 1.75 parts of tannic acid and stir at 800 r / min for 30 minutes. Adjust the pH to 4.5 with 1M sodium hydroxide solution. After reacting at 30℃ for 2 hours, spray dry the product. Set the inlet air temperature to 150℃, the outlet air temperature to 80℃, and the feed rate to 5 mL / min. Sieve through a 100-mesh sieve to obtain chitosan-polyphenol complex microspheres.
[0051] Step 3: Toothpaste base preparation: Mix 12 parts glycerin, 9 parts sorbitol and 2.5 parts carbomer 934P, and stir at 800 r / min for 45 minutes. Add 9 parts modified bioglass, 4.5 parts chitosan-polyphenol microspheres, 7 parts dicalcium phosphate and 0.25 parts sodium fluoride, and stir at 800 r / min for 30 minutes to obtain the toothpaste base.
[0052] Step 4: Final product preparation: Add 1.25 parts of sodium lauryl ether sulfate and 0.75 parts of cocamidopropyl betaine to 40 parts of toothpaste base, stir at 600 r / min for 20 minutes, add 0.15 parts of sodium benzoate, 0.25 parts of sodium saccharin and 0.35 parts of peppermint oil, stir evenly, and perform vacuum degassing treatment at -0.06 MPa for 18 minutes to obtain gum-protecting and tooth-strengthening toothpaste.
[0053] Comparative Example 3: Compared with Example 1, no furfural was added during the preparation of the modified bioglass.
[0054] Step 1: Preparation of modified bioglass: Take 17.5 parts of strontium-reinforced bioactive glass powder and ultrasonically disperse it in 200 parts of anhydrous ethanol. The ultrasonic frequency is set to 40 kHz and the ultrasonic time is 30 minutes. Add 2.5 parts of 3-aminopropyltriethoxysilane and react at 80℃ for 4 hours under nitrogen protection. During the reaction, maintain the stirring speed at 300 r / min. After the reaction is completed, filter and wash the precipitate three times with anhydrous ethanol, 50 mL each time. Dry under vacuum at 60℃ for 2 hours with a vacuum degree of -0.08 MPa to obtain an intermediate. Disperse 17.5 parts of the intermediate in 150 parts of toluene and add 1.75 parts of L-lysine. React at 110℃ for 6 hours, maintaining the stirring speed at 200 r / min and nitrogen protection during the reaction. After the reaction is completed, filter and wash twice with toluene. Dry under vacuum at 60℃ for 3 hours to obtain modified bioglass.
[0055] Step 2: Preparation of chitosan-polyphenol microspheres: Dissolve 2.5 parts of chitosan in 100 parts of 3% acetic acid solution and stir at room temperature for 2 hours until completely dissolved. Add 1.75 parts of tannic acid and stir at 800 r / min for 30 minutes. Adjust the pH to 4.5 with 1M sodium hydroxide solution. After reacting at 30℃ for 2 hours, spray dry the product. Set the inlet air temperature to 150℃, the outlet air temperature to 80℃, and the feed rate to 5 mL / min. Sieve through a 100-mesh sieve to obtain chitosan-polyphenol complex microspheres.
[0056] Step 3: Toothpaste base preparation: Mix 12 parts glycerin, 9 parts sorbitol and 2.5 parts carbomer 934P, and stir at 800 r / min for 45 minutes. Add 9 parts modified bioglass, 4.5 parts chitosan-polyphenol microspheres, 7 parts dicalcium phosphate and 0.25 parts sodium fluoride, and stir at 800 r / min for 30 minutes to obtain the toothpaste base.
[0057] Step 4: Final product preparation: Add 1.25 parts of sodium lauryl ether sulfate and 0.75 parts of cocamidopropyl betaine to 40 parts of toothpaste base, stir at 600 r / min for 20 minutes, add 0.15 parts of sodium benzoate, 0.25 parts of sodium saccharin and 0.35 parts of peppermint oil, stir evenly, and perform vacuum degassing treatment at -0.06 MPa for 18 minutes to obtain gum-protecting and tooth-strengthening toothpaste.
[0058] Comparative Example 4: Compared with Example 1, chitosan powder was used instead of chitosan-polyphenol microspheres in the final component.
[0059] Step 1: Preparation of modified bioglass: Take 17.5 parts of strontium-reinforced bioactive glass powder and ultrasonically disperse it in 200 parts of anhydrous ethanol. The ultrasonic frequency is set to 40 kHz and the ultrasonic time is 30 minutes. Add 2.5 parts of 3-aminopropyltriethoxysilane and react at 80℃ for 4 hours under nitrogen protection. During the reaction, maintain the stirring speed at 300 r / min. After the reaction is completed, filter and wash the precipitate three times with anhydrous ethanol, 50 mL each time. Dry under vacuum at 60℃ for 2 hours with a vacuum degree of -0.08 MPa to obtain an intermediate. Disperse 17.5 parts of the intermediate in 150 parts of toluene, add 1.75 parts of L-lysine and 1.25 parts of furfural, and react at 110℃ for 6 hours. During the reaction, maintain the stirring speed at 200 r / min and nitrogen protection. After the reaction is completed, filter and wash twice with toluene. Dry under vacuum at 60℃ for 3 hours to obtain modified bioglass.
[0060] Step 2: Preparation of chitosan powder: Dissolve 2.5 parts of chitosan in 100 parts of 3% acetic acid solution, stir at room temperature for 2 hours until completely dissolved, spray dry at an inlet air temperature of 150℃ and an outlet air temperature of 80℃, feed rate of 5mL / min, and sieve through a 100-mesh sieve to obtain chitosan powder.
[0061] Step 3: Toothpaste base preparation: Mix 12 parts glycerin, 9 parts sorbitol and 2.5 parts carbomer 934P, and stir at 800 r / min for 45 minutes. Add 9 parts modified bioglass, 4.5 parts chitosan powder, 7 parts dicalcium phosphate and 0.25 parts sodium fluoride, and stir at 800 r / min for 30 minutes to obtain the toothpaste base.
[0062] Step 4: Final product preparation: Add 1.25 parts of sodium lauryl ether sulfate and 0.75 parts of cocamidopropyl betaine to 40 parts of toothpaste base, stir at 600 r / min for 20 minutes, add 0.15 parts of sodium benzoate, 0.25 parts of sodium saccharin and 0.35 parts of peppermint oil, stir evenly, and perform vacuum degassing treatment at -0.06 MPa for 18 minutes to obtain gum-protecting and tooth-strengthening toothpaste.
[0063] Performance testing 1. Antibacterial performance test: Prepare standard strains of Streptococcus mutans (S. mutans) and Porphyromonas gingivalis, prepare bacterial suspensions, and adjust the concentration to 10. 6 CFU / mL, the bacterial suspension was evenly spread on MH agar medium, 27 filter paper discs with a diameter of 16 mm were prepared, 20 μL of each group of toothpaste samples were added, and the samples were incubated at 37℃ for 24 hours. The diameter of the inhibition zone was measured. Three parallel samples were set up for each group, and the average value was taken.
[0064] 2. Calcium and Phosphorus Ion Release Test: Prepare artificial saliva solution (pH=7.4). For each example and comparative example, weigh 1g of toothpaste sample and add it to 100mL of artificial saliva. Incubate at 37℃ with shaking. Take 5mL samples at 24h, 72h, and 168h respectively, and use ICP-OES to detect Ca ions. 2+ and PO4 3- For ion concentration, three parallel samples were set up at each time point, and the average value was taken.
[0065] 3. Enamel remineralization test: Bovine tooth enamel blocks with dimensions of 4x4x2mm were prepared, polished, and demineralized with 0.1M lactic acid solution for 24 hours to prepare initial caries lesions. After treatment with toothpaste of each group for 3 minutes, they were remineralized in artificial saliva for 24 hours. The demineralization-remineralization cycle was repeated for 7 days. The surface hardness change was measured with a microhardness tester. Ten samples were taken from each group, and the average value was taken.
[0066] Test Result Data Table Table 1. Results of antibacterial performance test
[0067] Table 2. Results of calcium and phosphorus ion release test
[0068] Table 3. Results of enamel remineralization test
[0069] Data Analysis As can be seen from Table 1, the toothpaste prepared by the technical solution of the present invention has good antibacterial properties.
[0070] As can be seen from Table 2, the toothpaste prepared by the technical solution of the present invention has good calcium and phosphorus ion release performance.
[0071] As can be seen from Table 3, the toothpaste prepared by the technical solution of the present invention has a good effect on repairing tooth enamel.
[0072] Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the present invention. All equivalent changes and improvements made within the scope of the present invention should still fall within the patent coverage of the present invention.
Claims
1. A toothpaste containing bioactive glass for gum protection and tooth strengthening, characterized in that, The modified bioglass was prepared by modifying strontium-reinforced bioactive glass powder with silane coupling agent, reacting it with L-lysine and furfural, and then preparing chitosan-polyphenol microspheres. The modified bioglass, chitosan-polyphenol microspheres, glycerin, sorbitol, carbomer, dicalcium phosphate and sodium fluoride were mixed to prepare toothpaste matrix. After adding surfactants, preservatives, sweeteners and fragrances, the toothpaste was degassed under vacuum.
2. The gum-protecting and tooth-strengthening toothpaste according to claim 1, characterized in that, The modified bioglass is prepared through the following specific steps: S1. Strontium-reinforced bioactive glass powder was ultrasonically dispersed in anhydrous ethanol, 3-aminopropyltriethoxysilane was added, and the mixture was reacted at 80°C for 4 hours under nitrogen protection. After filtration, the precipitate was washed three times with anhydrous ethanol and dried under vacuum at 60°C for 2 hours to obtain the intermediate. S2. The intermediate was dispersed in toluene, L-lysine and furfural were added, and the mixture was reacted at 110°C for 6 hours. After filtration, the modified bioglass was obtained.
3. The toothpaste for protecting gums and strengthening teeth according to claim 1, characterized in that, The chitosan-polyphenol microspheres were prepared by the following specific steps: chitosan was dissolved in a 3% acetic acid solution, tannic acid was added, and the mixture was stirred at 800 r / min for 30 min. The pH was adjusted to 4.5 with 1M sodium hydroxide solution, and the mixture was reacted at 25~35℃ for 2 h. After spray drying, the mixture was sieved through a 100-mesh sieve to obtain chitosan-polyphenol complex microspheres.
4. The gum-protecting and tooth-strengthening toothpaste according to claim 2, characterized in that, In S1, the weight ratio of the strontium-reinforced bioactive glass powder, anhydrous ethanol, and 3-aminopropyltriethoxysilane is 15~20:200:2~3.
5. The gum-protecting and tooth-strengthening toothpaste according to claim 2, characterized in that, In S2, the weight ratio of the intermediate, toluene, L-lysine and furfural is 15~20:150:1.5~2:1~1.
5.
6. The gum-protecting and tooth-strengthening toothpaste according to claim 3, characterized in that, The weight ratio of chitosan, 3% acetic acid solution and tannic acid is 2~3:100:1.5~2.
7. The gum-protecting and tooth-strengthening toothpaste according to claim 3, characterized in that, The specific conditions for spray drying are: inlet air temperature set to 150℃, outlet air temperature set to 80℃, and feed rate set to 5mL / min.
8. A method for preparing a toothpaste for protecting gums and strengthening teeth as described in any one of claims 1 to 7, characterized in that, Specifically, the following steps are included: Step 1: Mix glycerin, sorbitol and carbomer 934P and stir at 800 rpm for 45 minutes. Add modified bioglass, chitosan-polyphenol microspheres, dicalcium phosphate and sodium fluoride, and stir at 800 rpm for 30 minutes to obtain the toothpaste base. Step 2: Add sodium lauryl ether sulfate and cocamidopropyl betaine to the toothpaste base, stir at 600 r / min for 20 minutes, then add sodium benzoate, sodium saccharin and peppermint oil, stir evenly, and perform vacuum degassing treatment at -0.06 MPa for 15-20 minutes to obtain gum-protecting and tooth-strengthening toothpaste.
9. The preparation method according to claim 8, characterized in that, In step one, the weight ratio of glycerol, sorbitol, carbomer 934P, modified bioglass, chitosan-polyphenol microspheres, dicalcium phosphate, and sodium fluoride is 12:8~10:2~3:8~10:4~5:6~8:0.2~0.
3.
10. The preparation method according to claim 8, characterized in that, In step two, the weight ratio of sodium lauryl ether sulfate, cocamidopropyl betaine, toothpaste base, sodium benzoate, sodium saccharin and peppermint oil is 1~1.5:0.5~1:40:0.1~0.2:0.2~0.3:0.3~0.4.