Sterilizing gingiva-protecting tooth cleaning water and preparation method thereof
Through the combination and process optimization of tea polyphenols, chitosan derivatives and β-cyclodextrin-embedded essential oils, the problems of insufficient synergies, irritation and stability of existing oral care products have been solved, and the multiple effects of efficient sterilization, gum protection and teeth cleaning have been achieved.
Patent Information
- Application Number
- CN202510505149.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-22
- Publication Date
- 2025-08-01
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
Existing oral care products have problems such as insufficient antibacterial ingredient synergy, irritation problems, limited gingival repair function, low stain removal efficiency and poor ingredient stability, especially traditional chemical synthetic antibacterial agents have a negative impact on oral microecological balance.
Tea polyphenols, chitosan derivatives and β-cyclodextrin-embedded essential oils are combined, combined with ammonium glycyrrhizine, sodium hyaluronate and collagen hydrolysate, organic matter is decomposed by pectinase and nanosilicon dioxide particles are used, combined with gradient warming crosslinking and ultrasonic assisted extraction technology to form multi-dimensional antibacterial, gingival protection and tooth cleaning effects.
It has achieved efficient inhibition of oral pathogenic bacteria, repair gingival inflammation, and remove tooth stains, while reducing irritation to oral mucosa, improving the safety, effectiveness and stability of the product.
Abstract
Description
Technical Field
[0001] The present invention relates to the field of oral care, in particular to a sterilization, gum protection and tooth cleaning water and a preparation method thereof. Background Art
[0002] Oral health is a crucial component of human well-being. Gingivitis, plaque, and tooth stains affect over 60% of the global population. Traditional oral care products (such as toothpaste and mouthwash) often rely on synthetic chemical antimicrobials (such as chlorhexidine and triclosan) or highly alkaline detergents. While these can inhibit bacteria in the short term, long-term use can disrupt the oral microbiome and cause side effects such as mucosal irritation and taste changes. Therefore, the development of safe, effective, and natural oral care products has become an industry trend.
[0003] Currently, natural antibacterial ingredients (such as tea polyphenols, chitosan, and plant essential oils) are widely studied due to their low toxicity and high biocompatibility. However, existing technologies still have the following drawbacks:
[0004] Insufficient synergy of antibacterial ingredients: The antibacterial spectrum of a single ingredient is narrow and is easily affected by the complex environment of the oral cavity (such as salivary proteins and enzymes), resulting in unstable effects.
[0005] Irritation problem: Direct use of plant essential oils (such as thyme essential oil) can easily cause a burning sensation in the mucous membrane, limiting its clinical application.
[0006] Limited gum protection and repair functions: Traditional products focus on cleaning and sterilization, and have few targeted ingredients for gum inflammation repair and cell regeneration.
[0007] Low stain removal efficiency: Conventional abrasives (such as calcium carbonate) can easily damage tooth enamel, and enzyme preparations (such as amylase) have limited effects on organic stains (such as smoke stains and coffee stains).
[0008] Poor ingredient stability: Nanomaterials (such as silica) are prone to agglomeration, and chitosan derivatives have low solubility in acidic environments, affecting product homogeneity and shelf life.
[0009] To address these issues, existing technologies have attempted to improve upon them through ingredient compounding or process optimization. For example, Chinese patent CN103932914B discloses a chitosan mouthwash and its preparation method, but fails to address the irritation issue of plant essential oils. CN108324661B discloses a β-cyclodextrin-based antibacterial, anti-inflammatory, and breath-removing mouthwash and its preparation method. This method primarily utilizes the adsorption properties of β-cyclodextrin to absorb oral odor, whereas the β-cyclodextrin-encapsulated target of this application is plant essential oils, aiming to reduce their volatility and irritation. Furthermore, traditional methods for preparing collagen hydrolyzates can easily destroy their biological activity, and the complex cross-linking and modification process of chitosan derivatives makes industrial production difficult. Summary of the Invention
[0010] Through the collaborative design of multiple components and precise process control, the present invention breaks through the bottlenecks of existing technologies:
[0011] Optimization of the antibacterial system: The compounding of tea polyphenols, chitosan derivatives and β-cyclodextrin-embedded essential oils is adopted to expand the antibacterial spectrum and reduce irritation;
[0012] Strengthening of gum protection and repair: Ammonium glycyrrhizinate for anti-inflammatory, sodium hyaluronate for moisturizing, and collagen hydrolysate for promoting regeneration are introduced to form multi-dimensional protection;
[0013] Upgrading of tooth cleaning technology: Pectinase is used to decompose organic substances, combined with nano-silica modified by polyethylene glycol to enhance physical adsorption, achieving mild stain removal;
[0014] Process innovation: Through technologies such as gradient temperature rise cross-linking and ultrasonic-assisted extraction, the stability and dispersibility of components are improved to ensure uniform product performance.
[0015] In summary, the antibacterial and gum-protecting tooth cleaning water provided by the present invention is significantly superior to existing products in terms of safety, effectiveness and stability, and has broad market application prospects.
[0016] To solve the above technical problems, the present invention provides an antibacterial and gum-protecting tooth cleaning water, which comprises the following components in mass percentage:
[0017] Natural antibacterial components: tea polyphenols (3% - 8%), chitosan derivatives (2% - 5%), plant essential oil (0.5% - 2%); Gum protection and repair components: ammonium glycyrrhizinate (1% - 3%), sodium hyaluronate (0.5% - 2%), collagen hydrolysate (1% - 3%); Tooth cleaning and stain removal components: pectinase (0.5% - 2%), nano-silica particles (0.5% - 3%); The balance is deionized water.
[0018] Further, the plant essential oil is a mixed essential oil prepared by compounding thyme essential oil and peppermint essential oil in a ratio of 1:2, and is embedded by β-cyclodextrin by ultrasonic method to reduce irritation.
[0019] Further, the preparation method of the collagen hydrolysate is as follows: Gelatin is added to deionized water and stirred in a water bath at 40 - 50°C. After the gelatin is completely dissolved, the pH value is adjusted to 7.5 - 8.0 with 0.1M NaOH solution or 0.05M HCl solution, and trypsin is added. The reaction is carried out for 2 - 4h. After the reaction ends, the stirring is stopped. The solution is heated to 80°C with an electric heating mantle for 20min. An appropriate amount of activated carbon is added to the solution after inactivating the enzyme, and stirred for 10 - 15min to adsorb impurities. Then, it is filtered under vacuum while it is hot to remove the activated carbon and impurities, obtaining the collagen hydrolysate. The above raw materials are in a mass ratio of gelatin: deionized water: trypsin: activated carbon = 1:20 - 50:0.001 - 0.01:1 - 5.
[0020] Further, the particle size of the nano-sized silica microparticles is 50 - 100 nm, and the surface is modified with polyethylene glycol to improve the co-dispersibility with pectinase.
[0021] Further, the preparation method of the chitosan derivative includes the following steps:
[0022] (1) Mix chitosan powder with 1% - 3% dilute acetic acid solution at a mass ratio of 1:10 - 1:20, and stir at 30 - 40 °C until completely dissolved to form a homogeneous colloidal solution;
[0023] (2) Add a crosslinking agent and a modifier to the solution in step (1) in sequence. The crosslinking agent is glutaraldehyde or epichlorohydrin, and the modifier is glycidyl methacrylate or acrylamide. Under nitrogen protection, control the reaction temperature at 40 - 60 °C, and continuously stir and react at a speed of 200 - 400 rpm for 4 - 8 hours. The addition amount of glutaraldehyde is 0.8% - 1.5% of the mass of chitosan, the addition amount of glycidyl methacrylate is 2% - 3.5% of the mass of chitosan, the addition amount of epichlorohydrin is 1.2% - 2.8% of the mass of chitosan, and the addition amount of acrylamide is 3% - 4.5% of the mass of chitosan;
[0024] (3) Filter and separate the reaction solution in step (2) through a Buchner funnel, wash it with absolute ethanol and deionized water in sequence until neutral, and obtain the chitosan derivative after vacuum freeze-drying;
[0025] In step (2), the stirring reaction adopts a gradient temperature-rising process. Control the temperature at 40 - 45 °C in the first 2 hours to promote molecular pre-crosslinking, and raise the temperature to 50 - 60 °C in the next 2 - 6 hours to complete the graft modification reaction.
[0026] Further, a preparation method of a bactericidal and gum-protecting dental rinse includes the following steps:
[0027] Step 1: Mix tea polyphenols, chitosan derivative and plant essential oil, and perform ultrasonic-assisted extraction for 30 - 60 minutes to obtain an antibacterial composite liquid;
[0028] Step 2: Under stirring conditions, add the antibacterial composite liquid, ammonium glycyrrhizinate, sodium hyaluronate and collagen hydrolysate to deionized water, and stir until completely dissolved;
[0029] Step 3: Add pectinase and nano-sized silica microparticles, and continue stirring for 30 minutes to ensure uniform dispersion;
[0030] Step 4: Add citric acid, adjust the pH to 6.0 - 7.0, filter through a 0.22 μm filter membrane to remove impurities and microorganisms, fill and seal, and store refrigerated at 4 °C.
[0031] The germicidal and gum-protecting dental rinse provided by the present invention achieves multiple oral care effects through the synergistic action of multiple components. Its core function lies in efficiently inhibiting oral pathogenic bacteria (such as Streptococcus mutans and Porphyromonas gingivalis), while repairing gum inflammation and removing dental stains. The natural antibacterial components, tea polyphenols, chitosan derivatives, and plant essential oils encapsulated by β-cyclodextrin form a triple antibacterial network, which destroys the bacterial cell membrane and inhibits biofilm formation; the gum-protecting and repairing components, ammonium glycyrrhizinate, can inhibit the secretion of inflammatory factors, and sodium hyaluronate and collagen hydrolysates promote the regeneration of gum cells and mucosal moisturization; the dental stain-removing component, pectinase, decomposes organic stains, and nano-scale silica particles enhance the cleaning power through physical adsorption, and the surface-modified polyethylene glycol improves the dispersibility and avoids damaging tooth enamel.
[0032] Its mechanism of action is based on precise molecular design and process control. The β-cyclodextrin encapsulation technology wraps thymol and menthol essential oil molecules in the hydrophobic cavity, reducing direct contact with the mucosa. At the same time, chitosan derivatives form a three-dimensional network structure through cross-linking modification, further stabilizing the inclusion complex and delaying release, ensuring continuous low-concentration sterilization of the essential oil in the oral cavity. The polyethylene glycol surface-modified nano-scale silica particles and pectinase form a synergistic dispersion system, enhancing the penetration and decomposition efficiency of the enzyme on dental stains. The positive charge property of chitosan derivatives enables them to target and adsorb on the surface of negatively charged bacteria, enhancing antibacterial specificity. In addition, ammonium glycyrrhizinate reduces the gum inflammation reaction by inhibiting the NF-κB signaling pathway, and the high moisturizing property of sodium hyaluronate and the repair-promoting effect of collagen hydrolysates jointly maintain the health of the oral mucosa. The overall formula achieves a balance among safety, effectiveness, and stability through ingredient compounding and process optimization.
[0033] In summary, the germicidal and gum-protecting dental rinse of the present invention realizes multiple effects of efficient sterilization, gum protection and repair, and dental stain removal through the synergistic action of natural antibacterial components, the promoting action of gum-protecting and repairing components, and innovative preparation processes, while reducing the irritation to the oral mucosa and meeting the high requirements of modern consumers for oral care products. Detailed implementation manners
[0034] To make the objectives, technical solutions, and advantages of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are some but not all of the embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.
[0035] The following specifically describes a germicidal and gum-protecting dental rinse provided by the present invention and its preparation method through embodiments.
[0036] Example 1:
[0037] Components:
[0038] Formulation:
[0039] Tea polyphenols: 3%;
[0040] Chitosan derivative: 2%;
[0041] Plant essential oil (thyme essential oil and peppermint essential oil are compounded in a ratio of 1:2 and embedded in β-cyclodextrin by ultrasonic method): 0.5%;
[0042] Ammonium glycyrrhizinate: 1%;
[0043] Sodium hyaluronate: 0.5%;
[0044] Collagen hydrolysate: 1%;
[0045] Pectinase: 0.5%;
[0046] Nanoscale silica microparticles: 0.5%, the particle size of the nanoscale silica microparticles is 100 nm, and the surface is modified with polyethylene glycol to improve the synergistic dispersibility with pectinase;
[0047] The balance is deionized water.
[0048] The preparation method of the collagen hydrolysate is as follows: Add gelatin to deionized water, place it in a water bath at 50 °C, stir until the gelatin is completely dissolved, adjust the pH value to 7.6 with 0.1 M NaOH solution or 0.05 M HCl solution, add trypsin, and react for 4 h. After the reaction is completed, stop stirring. Heat the solution to 80 °C with an electric heating mantle for 20 min, add an appropriate amount of activated carbon to the solution after inactivating the enzyme, stir for 15 min to adsorb impurities, and perform vacuum filtration while it is hot to remove the activated carbon and impurities to obtain the collagen hydrolysate. Based on the mass ratio, gelatin: deionized water: trypsin: activated carbon = 1:50:0.01:3.
[0049] The preparation method of the chitosan derivative includes the following steps:
[0050] (1) Mix chitosan powder with 2% dilute acetic acid solution in a mass ratio of 1:5, and stir at 40 °C until completely dissolved to form a homogeneous colloidal solution;
[0051] (2) Add crosslinking agent glutaraldehyde and modifier glycidyl methacrylate to the solution in step (1) in sequence. Under nitrogen protection, control the reaction temperature and continuously stir and react at 400 rpm for 8 hours, wherein the addition amount of glutaraldehyde is 1% of the mass of chitosan, and the addition amount of epichlorohydrin is 1.5% of the mass of chitosan.
[0052] (3) Filter and separate the reaction solution from step (2) through a Buchner funnel, wash it successively with absolute ethanol and deionized water until neutral, and obtain the chitosan derivative after vacuum freeze-drying;
[0053] Among them, the stirring reaction in step (2) adopts a gradient temperature-rising process. The temperature is controlled at 40 °C in the first 2 hours to promote molecular pre-crosslinking, and then the temperature is raised to 50 °C in the next 6 hours to complete the grafting modification reaction.
[0054] A preparation method of a bactericidal and gum-protecting tooth-cleaning water, comprising the following steps:
[0055] Step 1: Mix tea polyphenols, chitosan derivative and plant essential oil, and perform ultrasonic-assisted extraction for 60 minutes to obtain an antibacterial composite liquid;
[0056] Step 2: Under stirring conditions, add the antibacterial composite liquid, ammonium glycyrrhizinate, sodium hyaluronate and collagen hydrolysate to deionized water, and stir until completely dissolved;
[0057] Step 3: Add pectinase and nano-sized silica particles, and continue stirring for 30 minutes to ensure uniform dispersion;
[0058] [[ID=communicate]]Step 4: Add citric acid, adjust the pH to 7, filter through a 0.22 μm filter membrane to remove impurities and microorganisms, fill and seal, and store in a refrigerator at 4 °C.
[0059] Example 2:
[0060] Formula:
[0061] Tea polyphenols: 5%;
[0062] Chitosan derivative: 3%;
[0063] Plant essential oil (a compound of thyme essential oil and mint essential oil in a ratio of 1:2, β-cyclodextrin inclusion by ultrasonic method): 1%;
[0064] Ammonium glycyrrhizinate: 2%;
[0065] Sodium hyaluronate: 1%;
[0066] Collagen hydrolysate: 2%;
[0067] Pectinase: 1%; <communicate>
[0068] Nano-sized silica particles: 1%, the particle size of the nano-sized silica particles is 50 nm, and the surface is modified with polyethylene glycol to improve the synergistic dispersion with pectinase;
[0069] The balance is deionized water.
[0070] Preparation method: The same as in Example 1.
[0071] Example 3:
[0072] Formula:
[0073] Tea polyphenols: 8%;
[0074] Chitosan derivative: 5%;
[0075] Plant essential oil (thyme essential oil and peppermint essential oil compounded at 1:2): 2%;
[0076] Ammonium glycyrrhizinate: 3%;
[0077] Sodium hyaluronate: 2%;
[0078] Collagen hydrolysate: 3%;
[0079] Pectinase: 2%;
[0080] Nanoscale silica microparticles: 3%, the particle size of the nanoscale silica microparticles is 50 nm, and the surface is modified with polyethylene glycol to improve the synergistic dispersibility with pectinase;
[0081] The balance is deionized water;
[0082] Preparation method: the same as Example 1.
[0083] Example 4:
[0084] Formula:
[0085] Tea polyphenols: 4%;
[0086] Chitosan derivative: 2.5%;
[0087] Plant essential oil (thyme essential oil and peppermint essential oil compounded at 1:2): 0.8%;
[0088] Ammonium glycyrrhizinate: 1.5%;
[0089] Sodium hyaluronate: 0.8%;
[0090] Collagen hydrolysate: 1.5%;
[0091] Pectinase: 0.8%;
[0092] Nanoscale silica microparticles: 0.8%, the particle size of the nanoscale silica microparticles is 100 nm, and the surface is modified with polyethylene glycol to improve the synergistic dispersibility with pectinase;
[0093] The balance is deionized water.
[0094] Preparation method: the same as Example 1.
[0095] Example 5:
[0096] Formula:
[0097] Tea polyphenols: 6%;
[0098] Chitosan derivative: 4%;
[0099] Plant essential oil (a compound of thyme essential oil and peppermint essential oil in a ratio of 1:2): 1.5%;
[0100] Ammonium glycyrrhizinate: 2.5%;
[0101] Sodium hyaluronate: 1.5%;
[0102] Collagen hydrolysate: 2.5%;
[0103] Pectinase: 1.5%;
[0104] Nanoscale silica microparticles: 2%, the particle size of the nanoscale silica microparticles is 50 nm, and the surface is modified with polyethylene glycol to improve the synergistic dispersibility with pectinase;
[0105] The balance is deionized water.
[0106] The preparation method of the collagen hydrolysate is as follows: Add gelatin to deionized water, place it in a water bath at 50 °C, stir until the gelatin is completely dissolved, adjust the pH value to 8 with 0.1 M NaOH solution or 0.05 M HCl solution, add trypsin, react for 4 h, and stop stirring after the reaction ends. Heat the solution to 80 °C with an electric heating mantle for 20 min, add an appropriate amount of activated carbon to the solution after inactivating the enzyme, stir for 15 min to adsorb impurities, and perform vacuum filtration while it is hot to remove the activated carbon and impurities to obtain the collagen hydrolysate. Based on the mass ratio of the above raw materials, gelatin: deionized water: trypsin: activated carbon = 1:35:0.01:2.
[0107] The preparation method of the chitosan derivative includes the following steps:
[0108] (1) Mix chitosan powder with 3% dilute acetic acid solution at a mass ratio of 1:12, stir at 38 °C until completely dissolved to form a homogeneous colloidal solution;
[0109] (2) Add a crosslinking agent and a modifier to the solution in step (1) in sequence. The crosslinking agent is epichlorohydrin, and the modifier is acrylamide. Under nitrogen protection, control the reaction temperature at 50 °C, continuously stir and react at 400 rpm for 6 h. The addition amount of glycidyl methacrylate is 2.5% of the mass of chitosan, and the addition amount of epichlorohydrin is 2% of the mass of chitosan;
[0110] (3) Filter and separate the reaction solution in step (2) through a Buchner funnel, wash it with absolute ethanol and deionized water in sequence until neutral, and obtain the chitosan derivative after vacuum freeze-drying;
[0111] In step (2), the stirring reaction adopts a gradient heating process. The temperature is controlled at 40°C in the first 2 hours to promote molecular pre-crosslinking, and then the temperature is raised to 50°C in the next 4 hours to complete the graft modification reaction.
[0112] A method for preparing an antibacterial and gum-protecting dental rinse, comprising the following steps:
[0113] Step 1: Mix tea polyphenols, chitosan derivatives, and plant essential oils, and perform ultrasonic-assisted extraction for 60 minutes to obtain an antibacterial composite solution;
[0114] Step 2: Under stirring conditions, add the antibacterial composite solution, ammonium glycyrrhizinate, sodium hyaluronate, and collagen hydrolysate to deionized water, and stir until completely dissolved;
[0115] Step 3: Add pectinase and nano-sized silica particles, and continue stirring for 30 minutes to ensure uniform dispersion;
[0116] Step 4: Add citric acid to adjust the pH to 7, filter through a 0.22 μm filter membrane to remove impurities and microorganisms, fill and seal, and store refrigerated at 4°C.
[0117] Performance test:
[0118] Experiment 1: Verification of antibacterial effect (comparing with commercially available chlorhexidine-containing mouthwash)
[0119] Materials and methods:
[0120] Test strains: Streptococcus mutans (ATCC 25175), Porphyromonas gingivalis (ATCC 33277);
[0121] Experimental group: formulation of Example 1;
[0122] Control group: commercially available 0.12% chlorhexidine mouthwash, blank deionized water.
[0123] Method: The minimum inhibitory concentration (MIC) was determined by the microbroth dilution method, and the biofilm inhibition rate was quantified by the fluorescence staining method.
[0124] Table 1 Verification of antibacterial effect
[0125] Group MIC of Streptococcus mutans (μg / mL) Biofilm inhibition rate (Porphyromonas gingivalis) Blank deionized water — 0% Commercially available chlorhexidine 25 85.3% Example 1 30 82.7%
[0126] Conclusion: Although the MIC value of Example 1 is slightly higher than that of commercially available chlorhexidine, the biofilm inhibition rates are similar, and the overall antibacterial effects are comparable. The natural antibacterial system has an antibacterial effect similar to that of chemical bacteriostatic agents.
[0127] Experiment 2: Evaluation of gum repair function
[0128] Materials and models:
[0129] Cell model: Human gingival epithelial cells (HGEC);
[0130] Experimental group: The dentifrice solution diluted in Example 1 (1:10);
[0131] Control group: Blank group without added repair components, commercially available restorative mouthwash;
[0132] Steps:
[0133] 1. Use lipopolysaccharide (LPS) to induce the HGEC inflammation model;
[0134] 2. Treat with the experimental group and the control group respectively for 24 hours;
[0135] 3. Use ELISA method to detect the release amounts of inflammatory factors IL-6 and TNF-α, and use CCK-8 method to measure cell viability.
[0136] Table 2 Verification of gingival repair function
[0137] Group IL-6 decline rate TNF-α decline rate Cell survival rate Blank control group 0 0 62.5 Commercially available restorative mouthwash 48.3% 51.2% 85.7% Example 1 67.8% 73.5% 93.2%
[0138] Conclusion: The dentifrice in Example 1 has significantly better effects than commercially available restorative mouthwash in reducing inflammatory factors and promoting cell survival.
Claims
1. A bactericidal and gum-protecting tooth cleaning water, characterized in that, Comprising components with the following mass percentages: Natural antibacterial components: tea polyphenols (3% - 8%), chitosan derivatives (2% - 5%), plant essential oil (0.5% - 2%); Gingival protection and repair components: ammonium glycyrrhizinate (1% - 3%), sodium hyaluronate (0.5% - 2%), collagen hydrolysate (1% - 3%); Tooth cleaning and stain removing components: pectinase (0.5% - 2%), nano-sized silica particles (0.5% - 3%); The balance is deionized water.
2. The sterilizing and gum-protecting tooth cleaning water according to claim 1, characterized in that, The plant essential oil is a mixed essential oil prepared by compounding thyme essential oil and mint essential oil in a ratio of 1:2, and is embedded by β-cyclodextrin using the ultrasonic method to reduce irritation.
3. The antibacterial gingival protection and tooth cleaning water according to claim 1, wherein The preparation method of the collagen hydrolysate is as follows: Add gelatin to deionized water, place it in a water bath at 40 - 50 °C and stir. After the gelatin is completely dissolved, adjust the pH value to 7.5 - 8.0 with 0.1M NaOH solution or 0.05M HCl solution, add trypsin, and react for 2 - 4 h. After the reaction ends, stop stirring. Heat the solution to 80 °C with an electric heating mantle and heat for 20 min. Add an appropriate amount of activated carbon to the solution after inactivating the enzyme, stir for 10 - 15 min to adsorb impurities, and perform vacuum filtration while it is hot to remove the activated carbon and impurities to obtain the collagen hydrolysate. Based on the mass ratio of the above raw materials, gelatin: deionized water: trypsin: activated carbon = 1:20 - 50:0.001 - 0.01:1 - 5.
4. The sterilizing and gum-protecting tooth cleaning water according to claim 1, characterized in that, The particle size of the nano-sized silica particles is 50 - 100 nm, and the surface is modified with polyethylene glycol to improve the synergistic dispersibility with pectinase.
5. The sterilizing and gum-protecting tooth cleaning water according to claim 1, wherein The preparation method of the chitosan derivative includes the following steps: (1) Mix chitosan powder with a 1% - 3% dilute acetic acid solution in a mass ratio of 1:10 - 1:20, and stir at 30 - 40 °C until completely dissolved to form a homogeneous colloidal solution; (2) Add a crosslinking agent and a modifier to the solution in step (1) in sequence. The crosslinking agent is glutaraldehyde or epichlorohydrin, and the modifier is glycidyl methacrylate or acrylamide. Under nitrogen protection, control the reaction temperature at 40 - 60 °C, and continuously stir and react at 200 - 400 rpm for 4 - 8 hours. The addition amount of glutaraldehyde is 0.8% - 1.5% of the mass of chitosan, the addition amount of glycidyl methacrylate is 2% - 3.5% of the mass of chitosan, the addition amount of epichlorohydrin is 1.2% - 2.8% of the mass of chitosan, and the addition amount of acrylamide is 3% - 4.5% of the mass of chitosan; (3) Filter and separate the reaction solution in step (2) through a Buchner funnel, wash it with absolute ethanol and deionized water in sequence until neutral, and obtain the chitosan derivative after vacuum freeze-drying; Among them, the stirring reaction in step (z) adopts a gradient heating process. The temperature is controlled at 40 - 45 °C in the first 2 hours to promote molecular pre-crosslinking, and the temperature is raised to 50 - 60 °C in the next 2 - 6 hours to complete the graft modification reaction.
6. A preparation method of the antibacterial and gum-protecting tooth cleaning water according to any one of claims 1 to 5, characterized in that, Including the following steps: Step 1: Mix tea polyphenols, chitosan derivatives, and plant essential oils, and perform ultrasonic-assisted extraction for 30 to 60 minutes to obtain an antibacterial composite solution; Step 2: Under stirring conditions, add the antibacterial composite solution, ammonium glycyrrhizinate, sodium hyaluronate, and hydrolyzed collagen product to deionized water and stir until completely dissolved; Step 3: Add pectinase and nano-sized silica particles, and continue stirring for 30 minutes to ensure uniform dispersion; Step 4: Add citric acid to adjust the pH to 6.0 - 7.0, filter through a 0.22 μm filter membrane to remove impurities and microorganisms, fill and seal, and store in a refrigerator at 4°C.
Citation Information
Patent Citations
Chitosan mouthwash and preparation method thereof
CN103932914B
Antibacterial, anti-inflammatory, and breath-freshening mouthwash based on β-cyclodextrin and its preparation method
CN108324661B