A toothpaste for strengthening teeth and gums and its preparation method

Abstract

This invention provides a toothpaste for strengthening teeth and gums, belonging to the field of oral hygiene technology. It comprises the following components in parts by weight: 40-80 parts gallic acid extract, 1-5 parts antibacterial agent, 3-6 parts xanthate-crosslinked chitosan resin, 330-400 parts abrasive, and humectants, surfactants, and binders in a weight ratio of (100-300):(5-50):(5-40), with water added to bring the total to 1000 parts. The toothpaste for strengthening teeth and gums provided by this application contains gallic acid extract rich in active substances. Its various biological activities, including anti-inflammatory, antioxidant, antibacterial, and antiviral properties, can strengthen teeth and gums, kill bacteria, and relieve pain, showing significant efficacy in preventing and treating oral diseases such as periodontitis and oral mucosal ulcers. It also contains xanthate-crosslinked chitosan resin, which can better exert the efficacy of chitosan, improve the oral environment through adsorption, reduce damage to teeth from excessive friction, and help improve the anti-sensitivity and anti-inflammatory effects of the toothpaste.

Description

Technical Field

[0001] This invention relates to the field of oral hygiene products technology, and in particular to a toothpaste for strengthening teeth and gums and its preparation method. Background Technology

[0002] Teeth are the hardest and most sensitive organs in the human body, and oral health is an important part of overall health. Toothpaste is currently the most common oral cleaning and care product on the market.

[0003] Periodontitis is a chronic infectious disease caused by dental plaque biofilm that affects four types of tooth supporting tissues (gingiva, periodontal ligament, alveolar bone, and cementum). It often leads to inflammatory destruction of periodontal supporting tissues, formation of periodontal pockets, progressive attachment loss, and alveolar bone resorption, eventually resulting in tooth loosening and loss. Periodontitis mainly occurs in adults, and once it develops, the condition deteriorates rapidly. If treatment is not timely, it often leads to premature tooth loosening and loss.

[0004] Traditional toothpaste typically consists of a mixture of abrasives, humectants, thickeners, foaming agents, flavorings, water, and functional ingredients used to improve oral health. Among these, the types of functional ingredients added to commercially available toothpastes are numerous, and their anti-sensitivity and anti-inflammatory effects vary considerably. While abrasives, which act directly on the tooth surface, can mechanically abrade teeth to achieve a whitening effect, they can also cause excessive wear on tooth enamel. This increases the surface area for bacteria and other microorganisms to adhere to, making gums more sensitive and exacerbating periodontitis, and even leading to various oral diseases such as oral mucosal ulcers.

[0005] Existing technologies also provide some functional toothpastes. For example, patent CN18969456A provides a whitening and anti-inflammatory toothpaste that uses oyster shell as a whitening and anti-inflammatory ingredient; patent CN114469777A provides a toothpaste for improving periodontitis and its preparation method, which uses antibacterial agents to kill and inhibit bacteria, improving problems such as periodontitis, bleeding and swollen gums, and bad breath. However, the effectiveness of existing toothpastes and current oral care products in improving oral health still needs improvement. Summary of the Invention

[0006] To address the aforementioned problems, this invention aims to provide a toothpaste that can clean the oral cavity through adsorption, reduce enamel wear, significantly soothe tooth sensitivity, improve oral problems such as periodontitis and oral mucosal ulcers, and enhance the effect of strengthening teeth and gums.

[0007] On one hand, this application provides a toothpaste for strengthening teeth and gums, comprising the following components in parts by weight:

[0008] Galla extract 40-80 parts, antibacterial agent 1-5 parts, xanthan acid-crosslinked chitosan resin 3-6 parts, abrasive 330-400 parts, humectant, surfactant and adhesive in a mass ratio of (100-300):(5-50):(5-40), water to make up to 1000 parts;

[0009] The moisturizer is selected from one or more of glycerin, sorbitol, sodium alginate, propylene glycol, and sodium hyaluronate.

[0010] The surfactant is selected from one or more of polyvinylpyrrolidone, sodium dodecyl sulfonate, cocamidopropyl betaine, sodium dodecyl sulfate-ethoxylate, and sodium lauryl ether sulfate.

[0011] The adhesive is selected from one or more of sodium carboxymethyl cellulose, hydroxypropyl methyl cellulose, hydroxypropyl cellulose, and xanthan gum.

[0012] It is understood that the "water" mentioned in this application may be the water used in existing commercial oral care products, such as deionized water.

[0013] It is understood that the total mass of the toothpaste in this application is calculated in units of 1000.

[0014] It is understood that the xanthan acid-crosslinked chitosan resin and gallic acid extract used in this application can be commercially available products or can be prepared in-house.

[0015] Preferably, the gallnut extract can be an extract obtained from a variety of extractants, such as an aqueous extract and / or an organic solvent extract, and preferably an alcohol extract.

[0016] Understandably, chitosan has promising applications in oral care products: as a biological hemostatic agent, it can effectively repair gingival bleeding and quickly eliminate gingival inflammation; its excellent adsorption properties allow it to rapidly bind to bacterial cell membranes, decompose dental plaque on the enamel surface, inhibit the proliferation of harmful bacteria including Helicobacter pylori, and improve the anti-sensitivity and anti-inflammatory properties of tooth supporting tissues. However, chitosan has poor water solubility and poor stability when compounded with other water-soluble components and matrix water, easily leading to separation or leakage, which limits its application in toothpaste products.

[0017] This application converts chitosan into xanthate-crosslinked chitosan resin, which significantly improves its water solubility, thereby enhancing the solubility of chitosan in the toothpaste components provided in this application and during the use of toothpaste, i.e., the brushing process, and thus better exerting the efficacy of chitosan.

[0018] Furthermore, the numerous hydroxyl, carboxyl, and thiol groups in xanthan acid-crosslinked chitosan resin can provide electrons, thus giving it excellent adsorption properties. On the one hand, it can adsorb oral impurities and odors, helping to improve breath; on the other hand, it can better combine with the oral microbiota, reducing dental plaque and other harmful bacteria through adsorption without damaging tooth enamel, thus further improving the oral microbiota environment and protecting oral health.

[0019] At the same time, the appropriate addition of xanthan acid-crosslinked chitosan resin can also adsorb the abrasive in the modified toothpaste. Its lubricating effect on the abrasive can also reduce the damage of excessive wear of tooth enamel by the abrasive while maintaining a good friction effect, thereby improving the damage of mechanical wear to tooth enamel and tooth supporting tissues, and preventing the gums from becoming more sensitive.

[0020] In one embodiment, the friction agent is a mixture of dicalcium phosphate and hydrated silica in a mass ratio of (340-360):(5-25).

[0021] Preferably, the dicalcium phosphate has a mesh size of 325-400 mesh; and the hydrated silica has a mesh size of 2000-3000 mesh.

[0022] Both dicalcium phosphate and hydrated silica are abrasives with good cleaning power and less irritation to the oral mucosa. Furthermore, hydrated silica also has excellent compatibilizing, thickening, and dispersing properties, enabling better and more uniform mixing of the abrasive and xanthate-crosslinked chitosan resin, thus improving its process stability.

[0023] In one embodiment, the gallnut extract is an ethanol extract of gallnut, and the extraction method is as follows:

[0024] Step a: Add the dry matter of gallnut to anhydrous ethanol at a material-to-liquid ratio of 1:(1-5), and perform ultrasonic extraction at 40-45℃ for 1-3 hours with an ultrasonic frequency of 20kHz and a power of 300-800W to obtain crude gallnut extract.

[0025] Step b: The crude extract of gallnut is concentrated by rotary evaporation to remove ethanol and obtain gallnut concentrate. The gallnut concentrate is diluted with an aqueous solution of 1,3-butanediol with a mass concentration of 70% at a mass ratio of 1:(0.5-1) and stored.

[0026] Among them, gallic acid contains a variety of active substances such as gallic acid, polyphenols, tannins, and flavonoids, and has a variety of biological activities such as anti-inflammatory, antioxidant, antibacterial, and antiviral. It can strengthen teeth and gums, kill bacteria and relieve pain. It has a good preventive and therapeutic effect on tooth sensitivity, weak chewing, loosening and displacement, bleeding gums, swollen and painful gums and bad breath caused by periodontal disease.

[0027] The toothpaste component of this application contains a significant proportion of gallnut extract prepared using the above method. On one hand, the above preparation method uses ultrasonic extraction to rupture the cell walls and release a large amount of active substances, thereby increasing the extraction rate. A suitable temperature is also used to ensure that the active substances are fully dissolved in ethanol without being oxidized by high temperatures. Furthermore, the concentrate is dissolved in a 1,3-butanediol solution to further extend the storage time and prevent oxidation and deterioration. Therefore, this method can obtain gallnut extracts with a richer variety and higher content. On the other hand, the gallnut extract prepared using the above method is used in a larger quantity in this application, which can improve periodontal inflammation and achieve the effect of strengthening teeth and gums.

[0028] However, the gallic acid alcohol extract prepared by the above method has excellent water solubility and is easily soluble in an aqueous matrix, but its compatibility with the other active ingredient, chitosan, and other thickening components is poor, resulting in a short shelf life of the final paste. This application, based on the preparation of chitosan into xanthate-crosslinked chitosan resin, further optimizes the types and proportions of humectants, surfactants, and adhesives to improve the uniformity and stability of the final product.

[0029] In one embodiment, the moisturizer is sorbitol, glycerin and sodium alginate in a mass ratio of (130-150):(80-100):(10-20).

[0030] Preferably, the toothpaste comprises 130-150 parts of sorbitol, 80-100 parts of glycerin and 10-20 parts of sodium alginate by weight.

[0031] Optionally, the "sorbitol" described in this application may be added in the form of a 70% aqueous solution of sorbitol.

[0032] In one embodiment, the surfactant is sodium dodecyl sulfonate, cocamidopropyl betaine, and polyvinylpyrrolidone in a mass ratio of (15-20):(10-20):(5-10).

[0033] Preferably, the toothpaste comprises, by weight, 15-20 parts sodium dodecyl sulfonate, 10-20 parts cocamidopropyl betaine and 5-10 parts polyvinylpyrrolidone.

[0034] In one embodiment, the adhesive is sodium carboxymethyl cellulose, hydroxypropyl methyl cellulose and xanthan gum in a mass ratio of (10-20):(5-15):(1-5).

[0035] Preferably, the toothpaste comprises, by weight, 10-20 parts sodium carboxymethyl cellulose, 5-15 parts hydroxypropyl methyl cellulose and 1-5 parts xanthan gum.

[0036] The adhesives used in the aforementioned types and proportions provide a more easily dispersed thickening and binding matrix for gallic acid extract, xanthan acid-crosslinked resin, and abrasives. The humectants used in the aforementioned types and proportions enhance the stability of gallic acid extract and improve the water solubility of xanthan acid-crosslinked chitosan resin, thereby improving their compatibility and dispersibility. The surfactants used in the aforementioned types and proportions significantly improve the dispersion uniformity of gallic acid extract and xanthan acid-crosslinked chitosan resin in the thickening and binding matrix and in a large aqueous matrix. Furthermore, sodium dodecyl sulfate and cocamidopropyl betaine in the surfactants can also act as foaming agents to generate foam during toothpaste use. Therefore, with the optimization of the overall component ratio, a toothpaste product with better uniformity and stability can ultimately be obtained.

[0037] In one embodiment, the antibacterial agent is selected from one or two of chlorhexidine acetate and sodium fluoride, preferably chlorhexidine acetate.

[0038] Chlorhexidine acetate, an antibacterial agent, possesses disinfectant and antiseptic properties, exhibiting high sensitivity against Staphylococcus, Streptococcus mutans, Streptococcus salivarius, Candida albicans, Escherichia coli, and anaerobic propionibacteria; moderate sensitivity against Haemophilus influenzae; and low sensitivity against Proteus spp., Pseudomonas spp., Klebsiella spp., and Gram-negative cocci (such as Veillonella spp.). Chlorhexidine acetate demonstrates stronger antibacterial activity against both Gram-positive and Gram-negative bacteria than disinfectants such as benzalkonium bromide, and remains effective even in the presence of serum and blood. The chlorhexidine acetate added in this application can synergistically exert antibacterial and anti-inflammatory effects with gallic acid extract, further improving oral diseases.

[0039] In one embodiment, the toothpaste further includes 0.5 to 2 parts of preservative, 1 to 5 parts of cooling agent, 0.5 to 5 parts of sweetener, and 0.1 to 10 parts of pH adjuster.

[0040] The preservative is selected from one or more of ethylparaben, propylparaben, sodium benzoate, and sodium butylparaben, preferably ethylparaben;

[0041] The cooling agent is selected from one or more of menthol, menthol, and peppermint oil, preferably menthol;

[0042] The sweetener is selected from one or more of xylitol, sodium saccharin, and stevia, preferably xylitol;

[0043] The pH adjuster is selected from one or more of sodium citrate, lactic acid, and phosphoric acid, preferably sodium citrate.

[0044] Optionally, the toothpaste provided in this application has a pH value of 8 to 10.

[0045] On the other hand, this application also provides a method for preparing the toothpaste for strengthening teeth and gums, including the following steps:

[0046] Step 1) Weigh xanthan acid-crosslinked chitosan resin and abrasive according to the mass fraction, mix them under high shear to obtain material A;

[0047] Weigh out the humectant and adhesive by weight, mix them, and stir evenly to obtain material B;

[0048] Weigh out the antibacterial agent and surfactant according to the mass fractions, dissolve them in an appropriate amount of water, add gallnut extract and mix well to obtain material C;

[0049] Step 2) Mix materials A, B and C, homogenize and stir to form a semi-transparent mixture D, add sweetener, cooling agent, preservative and pH adjuster, mix and add water to a total of 1000 parts by weight, homogenize and stir to form a paste, test and package.

[0050] In one embodiment, the high-shear stirring speed in step 1) is 2000–3000 r / min; and / or,

[0051] In step 2), the temperature of the homogenizing stirring is 35℃~40℃, and the rotation speed is 30~60r / min.

[0052] Among them, high shear enables the raw materials to mix quickly and has a certain emulsifying effect, which makes the xanthan acid-crosslinked chitosan resin have better lubricity for friction agents and reduces excessive wear.

[0053] On the other hand, this application also provides the use of the toothpaste in the preparation of anti-allergic and anti-inflammatory oral care products.

[0054] This application has at least the following beneficial effects:

[0055] 1. The toothpaste for strengthening teeth and gums provided in this application contains gallnut extract rich in active substances. Its various biological activities, including anti-inflammatory, antioxidant, antibacterial, and antiviral properties, can strengthen teeth and gums, kill bacteria and relieve pain. It has significant effects on the prevention and treatment of oral diseases such as periodontitis and oral mucosal ulcers.

[0056] 2. The toothpaste for strengthening teeth and gums provided in this application also contains xanthate-crosslinked chitosan resin, which can not only better exert the effects of chitosan, but also improve the oral environment through adsorption, while reducing the damage to teeth caused by excessive friction, and help improve the anti-sensitivity and anti-inflammatory effects of the toothpaste.

[0057] 3. The toothpaste for strengthening teeth and gums provided in this application is prepared using a specific preparation method and supplemented with optimized toothpaste base raw materials, resulting in a paste with better transparency, uniformity, stability and less susceptibility to deterioration. It is suitable for mass production in the daily chemical industry and has a longer shelf life. Detailed Implementation

[0058] To more clearly illustrate the overall concept of this application, a detailed description is provided below by way of embodiments. Numerous specific details are set forth in the following description to provide a more thorough understanding of this application. However, it will be apparent to those skilled in the art that this application can be implemented without one or more of these details. In other instances, to avoid confusion with this application, some technical features well-known in the art have not been described.

[0059] Unless otherwise specified, in the following embodiments, reagents or instruments whose manufacturers are not indicated are all conventional products that can be purchased commercially.

[0060] In the following embodiments, the "high shear" is a high shear dispersing emulsifier provided by Zhejiang Sangtian Fluid Automation Equipment Co., Ltd. The "homogenization" is a homogenizing emulsifier provided by Changzhou Li'anbao Machinery Equipment Technology Co., Ltd.

[0061] Unless otherwise specified in the examples, the conditions shall be performed in accordance with the standard conditions or the conditions recommended by the manufacturer.

[0062] Unless otherwise specified, all components of the compositions used in this application are commercially available and are of cosmetic or food grade purity. The dicalcium phosphate and hydrated silica in the abrasive were provided by Hunan Chenguang New Material Technology Co., Ltd., with mesh sizes of 400 mesh and 3000 mesh, respectively. The sorbitol in the moisturizer is a 70% aqueous solution of sorbitol; in the following examples, the mass of the sorbitol used is based on the mass of the 70% aqueous solution.

[0063] In the following embodiments, the ingredient "water" is deionized water used in existing commercial oral care products.

[0064] In the following examples, the gallnut extract used was a self-made ethanol extract of gallnut, and the extraction method was as follows:

[0065] Step a: Add the dry matter of gallnut to anhydrous ethanol at a material-to-liquid ratio of 1:3, and perform ultrasonic extraction at 42℃ for 3 hours with an ultrasonic frequency of 20kHz and a power of 600W to obtain crude gallnut extract.

[0066] Step b: The crude extract of gallnut is concentrated by rotary evaporation to remove ethanol and obtain gallnut concentrate. The gallnut concentrate is diluted with an aqueous solution of 70% 1,3-butanediol at a mass ratio of 1:0.5 and stored to obtain the raw material for toothpaste made from gallnut extract.

[0067] In the following examples, the weight of gallic acid extract refers to the weight of the concentrate before dilution. The actual weight of the raw material for toothpaste can be calculated from its dilution ratio. For example, if the toothpaste contains 80g of gallic acid extract, the raw material diluted with a mass ratio of gallic acid extract to 70% 1,3-butanediol aqueous solution of 1:0.5 should be weighed as 80 / 1.5 = 120g.

[0068] The xanthan acid-crosslinked chitosan resin used in this application can be a commercially available product or it can be prepared in-house. In the following examples, a self-prepared xanthan acid-crosslinked chitosan resin is used, and the preparation method is as follows:

[0069] Weigh 1.0 g of chitosan (molecular weight 50–90 kDa, degree of deacetylation 86.6%) into a 250 mL three-necked flask, add 50 mL of 10% NaOH solution, and allow to swell for 0.5 h. Then add 2.5 mL of carbon disulfide (added dropwise in an ice-water bath using a dropping funnel), stir and react for several hours, add an appropriate amount of glutaraldehyde for cross-linking, centrifuge to remove unreacted raw materials, precipitate with anhydrous ethanol, filter and wash, and dry in a 50 °C oven to obtain the final product.

[0070] Example 1

[0071] An embodiment of this application provides a toothpaste for strengthening teeth and gums, comprising the following components in parts by weight:

[0072] Galla extract 40-80 parts, antibacterial agent 1-5 parts, xanthan acidified cross-linked chitosan resin 3-6 parts, abrasive 330-400 parts, humectant 100-300 parts, surfactant 5-50 parts, adhesive 8-40 parts, preservative 0.5-2 parts, cooling agent 1-5 parts, sweetener 0.5-5 parts, pH adjuster 0.1-10 parts, deionized water to make up to 1000 parts.

[0073] The method for preparing the above toothpaste includes the following steps:

[0074] Step 1) Weigh xanthan acid-crosslinked chitosan resin and abrasive according to the mass fraction, and mix them at a high shear emulsification stirring speed of 2500 r / min for 0.5 to 3 hours to obtain material A;

[0075] Weigh out the humectant and adhesive by mass and mix them. Then, at 35°C, stir homogenously at 30 r / min for 1 to 5 hours to obtain material B.

[0076] Weigh out the antibacterial agent and surfactant according to the mass ratio, dissolve them in water at a mass ratio of 1:1, add gallnut extract and mix, then homogenize and stir at 30 r / min at 35℃ for 0.5 to 2 hours to obtain material C.

[0077] Step 2) Mix materials A, B and C, and homogenize them at 40°C and 60 r / min to form a semi-transparent mixture D. Add sweetener, cooling agent, preservative and pH adjuster, mix and add water to a total of 1000 parts by weight. Continue to homogenize and stir for 1 to 8 hours to make a paste, and then test and package it.

[0078] Specifically, in the toothpaste provided in this embodiment, the following raw materials are weighed out in grams, based on a total mass of 1000g:

[0079] Galla extract 80g, chlorhexidine acetate 3g, xanthan acid-crosslinked chitosan resin 5g, abrasive 330-400g, humectant 100-300g, surfactant 5-50g, adhesive 8-40g, ethylparaben 1g, menthol 2g, xylitol 2g, sodium citrate 1g, deionized water to 1000g.

[0080] The above raw materials were processed into a paste using the above method. The composition and dosage of some raw materials were adjusted appropriately to obtain a series of toothpaste compositions. Suitable components were screened based on the homogeneity, dispersibility, and stability of the materials and the paste. Homogeneity was mainly observed to determine if the paste was uniform and whether there were large particles or obvious agglomerates of abrasives. Dispersibility was mainly observed to determine if the components in the paste were uniformly dispersed and whether any agglomerated particles or suspended matter were observed. The stability testing method appropriately referenced the national standard document "GB / T 8372-2017 Toothpaste," and the specific method is as follows:

[0081] stability

[0082] Instrument: Refrigerator: Accuracy ±1℃.

[0083] Electric thermostatic incubator: accuracy ±1℃.

[0084] Test procedure: Take 200g of the sample paste, divide it into two portions of 100g each, and place each portion into a transparent aluminum-plastic toothpaste tube. Seal the tubes. Store one tube at room temperature, and place the other tube in a refrigerator at -8℃±1℃ for 8 hours. After 8 hours, remove the tubes and allow them to return to room temperature. Observe the tubes after standing; there should be no layering or droplet precipitation. When the tubes are opened, the paste should not overflow. When the tubes are inverted, no liquid should drip from the opening within 10 seconds. After the paste is squeezed out, compare the samples stored at room temperature; their aroma and color should be normal.

[0085] The results are shown in Table 1:

[0086] Table 1

[0087]

[0088] As shown in Table 1, when using the gallic extract and other components and proportions provided in this application, as well as the same preparation method, the form of chitosan addition, the type and proportion of abrasive, and the mass ratio of humectant to surfactant and binder all have a significant impact on the uniformity, dispersibility, and stability of the final toothpaste. Example 7 shows the best toothpaste properties, but its uniformity and stability still need improvement.

[0089] The following example uses the basic component dosage of Example 7 (gallic acid extract 80g, chlorhexidine acetate 3g, xanthate-crosslinked chitosan resin 5g, dicalcium phosphate 350g, hydrated silica 18g, sorbitol 260g, sodium dodecyl sulfate 50g, sodium carboxymethyl cellulose 35g, ethylparaben 1g, menthol 2g, xylitol 2g, sodium citrate 1g, deionized water to make up to 1000g) as an example. Further adjustments were made from the perspective of optimizing the types of moisturizers, surfactants, and adhesives to further improve the paste's properties. The results are shown in Table 2.

[0090] Table 2

[0091]

[0092]

[0093] As shown in Table 2, when all other components and preparation methods are exactly the same, the specific types and proportions of the humectant, surfactant, and adhesive have a significant impact on the properties of the final paste. Among them, Examples 11 and 12 are the most preferred embodiments, and the toothpaste prepared from them has the best uniformity, dispersibility, and stability, making them effective formulations suitable for industrial production.

[0094] Example 11 comprises: 80g gallnut extract, 3g chlorhexidine acetate, 5g xanthan acid-crosslinked chitosan resin, 350g dicalcium phosphate, 18g hydrated silica, 150g sorbitol, 80g glycerin, 10g sodium alginate, 15g sodium dodecyl sulfate, 20g cocamidopropyl betaine, 10g polyvinylpyrrolidone, 15g sodium carboxymethyl cellulose, 10g hydroxypropyl methylcellulose, 5g xanthan gum, 1g ethylparaben, 2g menthol, 2g xylitol, 1g sodium citrate, and deionized water to bring the total to 1000g.

[0095] Example 12 consists of: 80g gallnut extract, 3g chlorhexidine acetate, 5g xanthan acid-crosslinked chitosan resin, 350g dicalcium phosphate, 18g hydrated silica, 130g sorbitol, 100g glycerin, 20g sodium alginate, 20g sodium dodecyl sulfonate, 10g cocamidopropyl betaine, 5g polyvinylpyrrolidone, 15g sodium carboxymethyl cellulose, 10g hydroxypropyl methylcellulose, 5g xanthan gum, 1g ethylparaben, 2g menthol, 2g xylitol, 1g sodium citrate, and deionized water to bring the total to 1000g.

[0096] Example 2: Efficacy Experiment

[0097] Examples 11 and 12 in Example 1 were used as Experiment 1 and Experiment 2, respectively. A commercially available anti-inflammatory and soothing toothpaste was used as Control Example 1, and the gallnut extract prepared in this application was used as Control Example 2. Dexamethasone was used as a positive control. The test sample was prepared with distilled water, and the following experiments were conducted.

[0098] I. Improvement of oral inflammation

[0099] Experimental Methods: Macrophages were stimulated with phorbol ester to induce a respiratory burst. Reactive oxygen species generated during the respiratory burst were detected by chemiluminescence analysis and electron paramagnetic resonance. The expression levels of inflammatory factors IL-1β and TNFα were measured to evaluate the anti-inflammatory effects of each sample. The results are shown in Table 3.

[0100] Table 3

[0101] sample Dosage (mg / mL) IL-1β TNFα normal group - 25.74±1.59 18.26±2.33 Model group - 172.65±0.77 121.32±1.68 Dexamethasone group 0.1 112.39±3.82 95.46±1.57 Example 11 (High-dose group) 5 56.21±2.46 48.82±6.24 Example 11 (Medium-dose group) 3 108.93±4.95 103.15±3.72 Example 11 (Low-dose group) 1 137.45±0.64 110.24±4.86 Example 12 (High-dose group) 5 73.96±5.75 39.68±2.58 Example 12 (Medium-dose group) 3 124.57±1.58 87.43±0.96 Example 12 (Low-dose group) 1 159.72±2.27 104.58±3.79 Compare with Example 1 5 163.35±3.25 114.65±1.26 Compare with Example 2 5 50.28±5.41 63.54±7.83

[0102] Note: Compared with the normal group, P < 0.05; compared with the model group, P < 0.01

[0103] As shown in Table 3, Examples 11 and 12 prepared in this application have good anti-inflammatory effects at low, medium and high doses.

[0104] II. Improvement of oral mucosal ulcers

[0105] The antibacterial properties of each sample and its effectiveness in preventing and treating oral mucosal ulcers were determined by conducting antibacterial tests on Staphylococcus aureus, hemolytic streptococci, and Pseudomonas aeruginosa, common pathogens of oral ulcers. The results are shown in Table 4.

[0106] Table 4

[0107]

[0108] As shown in Table 4, Examples 11 and 12 provided in this application have a significant inhibitory effect on common oral bacteria, and thus can play a certain role in the prevention and treatment of oral mucosal ulcers.

[0109] III. Effects of using toothpaste

[0110] Experimental methods:

[0111] Sixty patients with periodontitis and oral mucosal ulcers (34 males and 26 females, mean age 45 ± 1.2 years) were randomly divided into three groups of 20 patients each. Each group used toothpaste prepared according to Example 3, Comparative Example 1, and Comparative Example 3, respectively. All patients used the toothpaste for 15 days, applying it three times daily after meals with a toothbrush, at a dosage of 2g / time / approximately 60kg. Specific experimental results are shown in Table 5 (calculated results are rounded to the nearest integer).

[0112] Table 5

[0113]

[0114] As shown in Table 5, the toothpastes provided in Examples 11 and 12 of this application reduced inflammation, healed ulcers, and significantly reduced pain after use by patients. As oral care products for strengthening teeth and gums, they have good application prospects and market value.

[0115] The above description is merely an embodiment of this application and is not intended to limit the scope of this application. Various modifications and variations can be made to this application by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this application should be included within the scope of the claims of this application.

Claims

1. A toothpaste for strengthening teeth and gums, characterized in that, The components include the following parts by weight: Galla extract 40-80 parts, antibacterial agent 1-5 parts, xanthate-crosslinked chitosan resin 3-6 parts, abrasive 330-400 parts, humectant, surfactant and adhesive in a mass ratio of (100-300):(5-50):(8-40), water to make up to 1000 parts. The preparation method of the xanthate-crosslinked chitosan resin is as follows: take chitosan, add 10% NaOH solution, swell, then add carbon disulfide, stir and react, add glutaraldehyde for crosslinking, centrifuge to remove unreacted raw materials, precipitate with anhydrous ethanol, filter and wash, and dry to obtain the product. The friction agent is composed of dicalcium phosphate and hydrated silica in a mass ratio of (340~360):(5~25); The moisturizer is composed of sorbitol, glycerin and sodium alginate in a mass ratio of (130~150):(80~100):(10~20); The surfactant is sodium dodecyl sulfate, cocamidopropyl betaine and polyvinylpyrrolidone in a mass ratio of (15~20):(10~20):(5~10); The adhesive is sodium carboxymethyl cellulose, hydroxypropyl methyl cellulose and xanthan gum in a mass ratio of (10~20):(5~15):(1~5).

2. The toothpaste according to claim 1, characterized in that, The gallnut extract is an ethanol extract of gallnut, and the extraction method is as follows: Step a: Add the dry matter of gallnut to anhydrous ethanol at a material-to-liquid ratio of 1: (1~5), and perform ultrasonic extraction at 40~45℃ for 1~3h, with an ultrasonic frequency of 20kHz and a power of 300~800W to obtain crude gallnut extract. Step b: The crude extract of gallnut is concentrated by rotary evaporation to remove ethanol and obtain gallnut concentrate. The gallnut concentrate is diluted with an aqueous solution of 1,3-butanediol with a mass concentration of 70% at a mass ratio of 1:(0.5~1) and stored.

3. The toothpaste according to claim 1, characterized in that, The antibacterial agent is selected from one or two of chlorhexidine acetate and sodium fluoride.

4. The toothpaste according to claim 3, characterized in that, The antibacterial agent is chlorhexidine acetate.

5. The toothpaste according to claim 1, characterized in that, It also includes 0.5 to 2 parts of preservative, 1 to 5 parts of cooling agent, 0.5 to 5 parts of sweetener, and 0.1 to 10 parts of pH adjuster; The preservative is selected from one or more of ethylparaben, propylparaben, sodium benzoate, and sodium butylparaben; The cooling agent is selected from one or more of menthol, menthol, and peppermint oil; The sweetener is selected from one or more of xylitol, sodium saccharin, and stevia; The pH adjuster is selected from one or more of sodium citrate, lactic acid, and phosphoric acid.

6. The toothpaste according to claim 5, characterized in that, The preservative is ethylparaben.

7. The toothpaste according to claim 5, characterized in that, The cooling agent is menthol.

8. The toothpaste according to claim 5, characterized in that, The sweetener is xylitol.

9. The toothpaste according to claim 5, characterized in that, The pH adjuster is sodium citrate.

10. The method for preparing the toothpaste for strengthening teeth and gums as described in any one of claims 1-9, characterized in that, Includes the following steps: Step 1) Weigh xanthan acid-crosslinked chitosan resin and abrasive according to the mass fraction, mix them under high shear to obtain material A; Weigh out the humectant and adhesive by weight, mix them, and stir evenly to obtain material B; Weigh out the antibacterial agent and surfactant according to the mass fractions, dissolve them in an appropriate amount of water, add gallnut extract and mix well to obtain material C; Step 2) Mix materials A, B and C, and homogenize them to form a semi-transparent mixture D. Add sweetener, cooling agent, preservative and pH adjuster, mix and add water to a total of 1000 parts by weight, homogenize and stir to form a paste, and then test and package.

11. The preparation method according to claim 10, characterized in that, In step 1), the high-shear stirring speed is 2000~3000 r / min; and / or, In step 2), the temperature for homogenizing and stirring is 35℃~40℃, and the rotation speed is 30~60r / min.

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