Toothpaste with biological activity and deodorization function and preparation method thereof

By using modified tourmaline deodorizing modified materials and vitamin E inclusions in toothpaste, the problem of poor deodorization performance of toothpaste is solved, achieving better antibacterial performance and oral ulcer healing effect.

CN119564518APending Publication Date: 2025-03-07YIWU AISHANG COMMODITY

Patent Information

Application Number
CN202510112459.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-01-24
Publication Date
2025-03-07

AI Technical Summary

Technical Problem

Existing toothpastes have poor deodorization performance and are difficult to effectively solve oral ulcers and bad breath problems.

Method used

Triclosan, an antibacterial agent modified on the surface of tourmaline powder, was prepared and the vitamin E inclusion was added to the toothpaste to improve deodorization and antibacterial properties and promote the healing of oral ulcers.

Benefits of technology

It significantly improves the deodorization and antibacterial properties of toothpaste, can effectively inhibit the growth of a variety of oral bacteria, reduce the production of oral odor, and promote the healing of oral ulcers.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the technical field of toothpaste, and discloses toothpaste with biological activity and deodorization and a preparation method thereof, the toothpaste comprises the following raw materials: sucralose, glycerin, sorbitol, benzyl alcohol, sodium dihydrogen phosphate, water, hydrated silica, sodium carboxymethyl cellulose, xanthan gum, a deodorization modification material, a vitamin E inclusion compound, a foaming agent and essence; wherein the deodorizing modified material is obtained by modifying an antibacterial agent triclosan on the surface of tourmaline powder, so that the toothpaste is endowed with excellent antibacterial and deodorizing performance; the vitamin E clathrate compound is a protamine derivative coating vitamin E. In the use process, positive charges carried by protamine and mucous membranes with negative charges are utilized to generate an electrostatic adsorption effect, and the vitamin E clathrate compound is adhered to ulcers, so that the effects of positioning, slow-release and targeting are achieved, ulcer healing is promoted, and the healthy environment in the oral cavity is protected.
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Description

Technical Field

[0001] The invention relates to the technical field of toothpaste, and in particular to a toothpaste with biological activity and deodorization and a preparation method thereof. Background Art

[0002] Toothpaste is a commonly used oral cleaning product in daily life. It is composed of abrasives, moisturizers, thickeners, surfactants, sweeteners, etc. Its main function is to assist the toothbrush to remove food debris and plaque in the mouth, make the teeth white and beautiful, and maintain oral health.

[0003] With the rapid development of science and technology and the continuous improvement of people's living standards, ordinary toothpaste can no longer meet the diversified and high value-added market demand. Therefore, the functional development of toothpaste has become an important trend in the development of the industry. Ordinary toothpaste has the defect of poor deodorization performance. Bad breath is a common symptom, which is usually caused by volatile sulfides produced when bacteria in the mouth decompose food residues, saliva and other substances. These compounds, such as hydrogen sulfide and methyl mercaptan, have strong odors and are the main causes of bad breath. On the one hand, the volatile sulfides in bad breath will increase the permeability of the gingival sulcus epithelium, allowing bacterial enzymes, various toxins and metabolites to invade the underlying connective tissue, causing tissue damage and inducing inflammatory reactions. It can also affect the metabolism of fibronectin and bone in the periodontal tissue. It is beneficial to the maintenance and regeneration of bone tissue. On the other hand, bad breath destroys the healthy environment in the oral cavity, causing a large number of bacteria and fungi to remain in the mouth, causing serious harm to physical health. In addition, with the accelerated pace of modern life, people are facing greater mental stress and unhealthy eating habits. These factors work together to lead to a high incidence of oral ulcers. When oral ulcers occur, patients will feel severe burning pain, which not only affects their diet, but may also cause other physical symptoms, such as gum discomfort, swollen lymph nodes or fever, etc., which seriously affect the patient's health and daily life. The current toothpaste mainly plays a role in cleaning and health care, and has limited effect in solving the problem of oral ulcers. Therefore, it is of great significance to further improve the deodorization performance of toothpaste and the treatment of oral ulcers.

[0004] Based on this, the present invention provides a method for preparing a deodorizing toothpaste, which can solve the problems existing in the prior art. Summary of the invention

[0005] In order to solve the problems mentioned in the background technology, the object of the present invention is to provide a toothpaste with biological activity and a preparation method thereof.

[0006] The purpose of the present invention can be achieved through the following technical solutions: A toothpaste with biological activity and deodorization comprises the following raw materials in parts by weight: 0.2-0.6 parts of sucralose, 5-10 parts of glycerol, 30-40 parts of sorbitol, 0.1-0.3 parts of benzyl alcohol, 1-2 parts of sodium dihydrogen phosphate, 15-25 parts of hydrated silica, 0.4-0.6 parts of sodium carboxymethyl cellulose, 0.4-0.8 parts of xanthan gum, 3-5 parts of deodorization modification materials, 4-6 parts of vitamin E inclusion compound, 2-3 parts of foaming agent, 0.5-1.5 parts of flavor, and the balance of deionized water.

[0007] As a further embodiment of the present invention, the preparation method of the deodorizing modified material comprises the following steps: Step D1: ultrasonically disperse the tourmaline powder in acetone, add 2-bromoisobutyryl bromide and triethylamine to the formed dispersion under nitrogen protection, stir at room temperature for 4-6 hours, separate and collect the solid material, and obtain a modified tourmaline powder intermediate; Step D2: Mix the modified tourmaline powder intermediate with N,N-dimethylformamide, and ultrasonically disperse for 20-40 minutes. Under continuous nitrogen conditions, continue to add triclosan and catalyst to the system, raise the system temperature to 70-80°C under stirring conditions, and keep warm for 5-8 hours. After the material is naturally cooled, the solid material is separated by centrifugation, the solid material is washed, and vacuum dried to obtain a deodorized modified material.

[0008] As a further solution of the present invention, in step D1, the average particle size of the tourmaline powder is 5 μm.

[0009] As a further embodiment of the present invention, in step D2, the catalyst is any one of sodium carbonate, potassium carbonate or sodium bicarbonate.

[0010] It can be inferred that the principle of the above scheme is: in step D1, the tourmaline powder surface contains hydroxyl groups, which can react with the acyl bromide groups in the 2-bromoisobutyryl bromide structure under the action of triethylamine, thereby modifying the halogen functional groups on the surface of the tourmaline powder to obtain a modified tourmaline powder intermediate; in step D2, the halogen functional groups on the surface of the modified tourmaline powder intermediate are used as active sites. Under the action of a catalyst, the halogen functional groups can react with the hydroxyl groups in the triclosan structure to graft triclosan onto the surface of the tourmaline powder to obtain a deodorizing modified material.

[0011] As a further embodiment of the present invention, the method for preparing the vitamin E inclusion compound comprises the following steps: Step DD1: adding protamine and palmitic acid to a mixed solution of dimethyl sulfoxide and purified water, mechanically stirring the mixture, adding an activator and a condensing agent, stirring the mixture for 6-10 hours at room temperature, the whole process being carried out under nitrogen protection, and removing the solvent by distillation under reduced pressure to obtain an intermediate material; Step DD2: adding the intermediate material prepared in step DD1 to the ethanol aqueous solution, stirring at a stirring rate of 400-600 r / min for 20-40 min to obtain an intermediate material solution; Step DD3: Under stirring, add vitamin E to the intermediate material solution, set the stirring rate to 100-200r / min, and after stirring to form a uniform liquid, adjust the rotation speed to 600-1000r / min, and under continuous stirring, add the uniform liquid dropwise into deionized water at a rate of 5-20mL / min, let stand for 1-3h, and obtain a vitamin E inclusion complex through reduced pressure concentration and freeze-drying.

[0012] As a further embodiment of the present invention, in step DD1, the activator is any one of 4-dimethylaminopyridine, N-hydroxysuccinimide or 1-hydroxybenzotriazole.

[0013] As a further embodiment of the present invention, in step DD1, the condensing agent is any one of N,N-dicyclohexylcarbodiimide, 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide or N,N'-diisopropylcarbodiimide.

[0014] As a further embodiment of the present invention, in step DD2, the mass fraction of the ethanol aqueous solution is 20%-80%.

[0015] As a further solution of the present invention, in step DD3, the volume ratio of the uniform liquid material to deionized water is 1:3-4.

[0016] It can be inferred that the principle of the above scheme is: in step DD1, the amino group in the protamine structure can react with the carboxyl group in the palmitic acid structure under the action of the activator and the condensing agent, so that the palmitic acid is grafted into the structure of the protamine to obtain an intermediate material; in step DD3, vitamin E is insoluble in water but soluble in ethanol. When the uniform liquid material is added to deionized water, the intermediate material and vitamin E are quickly precipitated due to the increase in the water content in the solution. Since the intermediate material contains a large number of hydrophilic groups and hydrophobic long fatty chains, it has amphiphilicity and can form a cavity structure with internal hydrophobicity and external hydrophilicity, and the precipitated hydrophobic vitamin E will enter the cavity, thereby achieving effective encapsulation of vitamin E to obtain a vitamin E inclusion complex.

[0017] A method for preparing a toothpaste with biologically active deodorizing properties comprises the following steps: Step 1: Add sucralose, glycerol, sorbitol, benzyl alcohol, sodium dihydrogen phosphate and deionized water into a liquid premixing pot and stir evenly to obtain premix A; Step 2: Put hydrated silica, sodium carboxymethyl cellulose, xanthan gum, deodorizing modified material, vitamin E inclusion compound and foaming agent into a powder premixing pot, start a stirrer to mix, and obtain premix B; Step 3: Start the paste making machine, open the feed valve, suck the premix A into the paste making machine with vacuum, close the feed valve, and then turn on the vacuum pump to suck the premix B into the paste making machine. After sucking, close the feed valve, and then turn on the vacuum pump to stir. Stir until the paste begins to slowly drop and stabilize without rising, continue stirring for 15-25 minutes, and finally open the flavor inlet valve to suck the flavor into the paste pot. After sucking, close the flavor inlet valve, stir until the paste begins to slowly drop and stabilize without rising, continue stirring for 10-20 minutes, then stop double stirring, continue to stir with a scraper for 4-6 minutes, discharge the material, and obtain toothpaste.

[0018] Beneficial effects of the present invention: (1) The present invention prepares a deodorant modified material by modifying the surface of tourmaline powder with the antibacterial agent triclosan. On the one hand, the tourmaline powder can quickly remove exogenous oral odor, so that the prepared toothpaste has good deodorant performance. On the other hand, the deodorant modified material contains the broad-spectrum antibacterial agent triclosan, which can give the toothpaste excellent antibacterial performance and inhibit the growth of various oral bacteria, thereby reducing the generation of oral odor and further improving the deodorant performance of the toothpaste. In addition, the chemical connection method can avoid the precipitation and volatilization of the antibacterial agent, thereby protecting the healthy environment in the oral cavity and preventing bacteria and fungi from remaining in the oral cavity and causing harm to human health.

[0019] (2) The vitamin E inclusion compound prepared by the present invention is a protamine derivative coated with vitamin E. During the use of toothpaste, the positive charge of protamine is electrostatically adsorbed to the negatively charged mucosa, so that the vitamin E inclusion compound adheres to the ulcer surface, thereby playing a role in positioning and sustained release targeting. After the vitamin E is coated, the stability of the vitamin E in the oral environment can be improved, and a sustained release effect can be produced, thereby greatly improving the utilization rate of the vitamin E. When the vitamin E acts on the ulcer surface, it can promote the proliferation of capillaries and small blood vessels, improve the blood circulation around the oral ulcer surface, increase local tissue oxygen supply, and create good conditions for the healing of the ulcer surface. At the same time, it can help repair the oral mucosa, promote ulcer healing, and form a protective film on the ulcer surface to relieve pain and accelerate ulcer healing. In addition, protamine has antibacterial activity, can inhibit the growth and reproduction of various bacteria and viruses, alleviate infection symptoms, create favorable conditions for the healing of ulcers, and avoid problems such as gum discomfort, lymph node swelling or fever caused by oral ulcers.

[0020] Of course, any product implementing the present invention does not necessarily need to achieve all of the advantages described above at the same time. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings required for describing the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other accompanying drawings can be obtained based on these accompanying drawings without paying creative work.

[0022] Figure 1 This is the infrared spectrum test chart of the deodorizing modified material prepared by the present invention. DETAILED DESCRIPTION

[0023] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0024] Embodiment 1, Preparation of toothpaste Step 1: Add 0.2 g sucralose, 5 g glycerol, 30 g sorbitol, 0.1 g benzyl alcohol, 1 g sodium dihydrogen phosphate, and 38.4 g deionized water into a liquid premixing pot, stir evenly, and obtain premix A; Step 2: 15 g of hydrated silica, 0.4 g of sodium carboxymethyl cellulose, 0.4 g of xanthan gum, 3 g of deodorizing modified material, 4 g of vitamin E inclusion compound and 2 g of sodium dodecyl sulfate are put into a powder premixing pot, and a stirrer is turned on to mix to obtain premix B; Step 3: Start the paste making machine, open the feed valve, suck the premix A into the paste making machine with vacuum, close the feed valve, and then turn on the vacuum pump to suck the premix B into the paste making machine. After sucking, close the feed valve, and then turn on the vacuum pump to stir. Stir until the paste begins to slowly drop and stabilize without rising, continue stirring for 15 minutes, and finally open the flavor inlet valve to suck 0.5g of spearmint into the paste pot. After sucking, close the flavor inlet valve, stir until the paste begins to slowly drop and stabilize without rising, continue stirring for 10 minutes, then stop double stirring, control the vacuum degree to -0.098MPa, continue to stir with a scraper for 4 minutes, discharge the material, and obtain toothpaste.

[0025] Embodiment 2, Preparation of toothpaste Step 1: Add 0.4 g sucralose, 8 g glycerol, 35 g sorbitol, 0.2 g benzyl alcohol, 1.5 g sodium dihydrogen phosphate, and 20.3 g deionized water into a liquid premixing pot, stir evenly, and obtain premix A; Step 2: Add 20 g of hydrated silica, 0.5 g of sodium carboxymethyl cellulose, 0.6 g of xanthan gum, 4.5 g of deodorizing modified material, 5.5 g of vitamin E inclusion compound and 2.5 g of sodium lauryl sulfate into a powder premixing pot, start a stirrer to mix, and obtain premix B; Step 3: Start the paste making machine, open the feed valve, suck the premix A into the paste making machine with vacuum, close the feed valve, and then turn on the vacuum pump to suck the premix B into the paste making machine. After sucking, close the feed valve, and then turn on the vacuum pump to stir. Stir until the paste begins to slowly drop and stabilize without rising, continue stirring for 20 minutes, and finally open the flavor inlet valve to suck 1g of spearmint into the paste pot. After sucking, close the flavor inlet valve, stir until the paste begins to slowly drop and stabilize without rising, continue stirring for 15 minutes, then stop double stirring, control the vacuum degree to -0.098MPa, continue to stir with a scraper for 5 minutes, discharge the material, and obtain toothpaste.

[0026] Embodiment 3, Preparation of toothpaste Step 1: Add 0.6 g sucralose, 10 g glycerol, 40 g sorbitol, 0.3 g benzyl alcohol, 2 g sodium dihydrogen phosphate, and 5.2 g deionized water into a liquid premixing pot, stir evenly, and obtain premix A; Step 2: Add 25 g of hydrated silica, 0.6 g of sodium carboxymethyl cellulose, 0.8 g of xanthan gum, 5 g of deodorizing modified material, 6 g of vitamin E inclusion compound and 3 g of sodium dodecyl sulfate into a powder premixing pot, start a stirrer to mix, and obtain premix B; Step 3: Start the paste making machine, open the feed valve, suck the premix A into the paste making machine with vacuum, close the feed valve, and then turn on the vacuum pump to suck the premix B into the paste making machine. After sucking, close the feed valve, and then turn on the vacuum pump to stir. Stir until the paste begins to slowly drop and stabilize without rising, continue stirring for 25 minutes, and finally open the flavor inlet valve to suck 1.5g of spearmint into the paste pot. After sucking, close the flavor inlet valve, stir until the paste begins to slowly drop and stabilize without rising, continue stirring for 20 minutes, then stop double stirring, control the vacuum degree to -0.098MPa, continue to stir with a scraper for 6 minutes, discharge the material, and obtain toothpaste.

[0027] Comparative Example 1 Preparation of toothpaste Step 1: Add 0.4 g sucralose, 8 g glycerol, 35 g sorbitol, 0.2 g benzyl alcohol, 1.5 g sodium dihydrogen phosphate, and 20.3 g deionized water into a liquid premixing pot, stir evenly, and obtain premix A; Step 2: Add 20 g of hydrated silica, 0.5 g of sodium carboxymethyl cellulose, 0.6 g of xanthan gum, 4.5 g of deodorizing modified material and 2.5 g of sodium lauryl sulfate into a powder premixing pot, start the stirrer to mix, and obtain premix B; Step 3: Start the paste making machine, open the feed valve, suck the premix A into the paste making machine with vacuum, close the feed valve, and then turn on the vacuum pump to suck the premix B into the paste making machine. After sucking, close the feed valve, and then turn on the vacuum pump to stir. Stir until the paste begins to slowly drop and stabilize without rising, continue stirring for 20 minutes, and finally open the flavor inlet valve to suck 1g of spearmint into the paste pot. After sucking, close the flavor inlet valve, stir until the paste begins to slowly drop and stabilize without rising, continue stirring for 15 minutes, then stop double stirring, control the vacuum degree to -0.098MPa, continue to stir with a scraper for 5 minutes, discharge the material, and obtain toothpaste.

[0028] Comparative Example 2 Preparation of toothpaste Step 1: Add 0.4 g sucralose, 8 g glycerol, 35 g sorbitol, 0.2 g benzyl alcohol, 1.5 g sodium dihydrogen phosphate, and 20.3 g deionized water into a liquid premixing pot, stir evenly, and obtain premix A; Step 2: Add 20 g of hydrated silica, 0.5 g of sodium carboxymethyl cellulose, 0.6 g of xanthan gum, 5.5 g of vitamin E inclusion compound and 2.5 g of sodium lauryl sulfate into a powder premixing pot, start a stirrer to mix, and obtain premix B; Step 3: Start the paste making machine, open the feed valve, suck the premix A into the paste making machine with vacuum, close the feed valve, and then turn on the vacuum pump to suck the premix B into the paste making machine. After sucking, close the feed valve, and then turn on the vacuum pump to stir. Stir until the paste begins to slowly drop and stabilize without rising, continue stirring for 20 minutes, and finally open the flavor inlet valve to suck 1g of spearmint into the paste pot. After sucking, close the flavor inlet valve, stir until the paste begins to slowly drop and stabilize without rising, continue stirring for 15 minutes, then stop double stirring, control the vacuum degree to -0.098MPa, continue to stir with a scraper for 5 minutes, discharge the material, and obtain toothpaste.

[0029] Comparative Example 3 Preparation of toothpaste Step 1: Add 0.4 g sucralose, 8 g glycerol, 35 g sorbitol, 0.2 g benzyl alcohol, 1.5 g sodium dihydrogen phosphate, and 20.3 g deionized water into a liquid premixing pot, stir evenly, and obtain premix A; Step 2: Add 20 g of hydrated silica, 0.5 g of sodium carboxymethyl cellulose, 0.6 g of xanthan gum, 4.5 g of deodorizing modified material, 4.5 g of protamine, 1 g of vitamin E and 2.5 g of sodium lauryl sulfate into a powder premixing pot, start a stirrer to mix, and obtain premix B; Step 3: Start the paste making machine, open the feed valve, suck the premix A into the paste making machine with vacuum, close the feed valve, and then turn on the vacuum pump to suck the premix B into the paste making machine. After sucking, close the feed valve, and then turn on the vacuum pump to stir. Stir until the paste begins to slowly drop and stabilize without rising, continue stirring for 20 minutes, and finally open the flavor inlet valve to suck 1g of spearmint into the paste pot. After sucking, close the flavor inlet valve, stir until the paste begins to slowly drop and stabilize without rising, continue stirring for 15 minutes, then stop double stirring, control the vacuum degree to -0.098MPa, continue to stir with a scraper for 5 minutes, discharge the material, and obtain toothpaste.

[0030] Comparative Example 4 Preparation of toothpaste Step 1: Add 0.4 g sucralose, 8 g glycerol, 35 g sorbitol, 0.2 g benzyl alcohol, 1.5 g sodium dihydrogen phosphate, and 20.3 g deionized water into a liquid premixing pot, stir evenly, and obtain premix A; Step 2: Add 20 g of hydrated silica, 0.5 g of sodium carboxymethyl cellulose, 0.6 g of xanthan gum and 2.5 g of sodium lauryl sulfate into a powder premixing pot, start the stirrer to mix, and obtain premix B; Step 3: Start the paste making machine, open the feed valve, suck the premix A into the paste making machine with vacuum, close the feed valve, and then turn on the vacuum pump to suck the premix B into the paste making machine. After sucking, close the feed valve, and then turn on the vacuum pump to stir. Stir until the paste begins to slowly drop and stabilize without rising, continue stirring for 20 minutes, and finally open the flavor inlet valve to suck 1g of spearmint into the paste pot. After sucking, close the flavor inlet valve, stir until the paste begins to slowly drop and stabilize without rising, continue stirring for 15 minutes, then stop double stirring, control the vacuum degree to -0.098MPa, continue to stir with a scraper for 5 minutes, discharge the material, and obtain toothpaste.

[0031] The deodorizing modified materials in the above examples and comparative examples were prepared by the following method: Step D1: ultrasonically disperse 5 g of tourmaline powder with an average particle size of 5 μm in acetone, add 1.2 g of 2-bromoisobutyryl bromide and 0.05 g of triethylamine to the resulting dispersion under nitrogen protection, stir at room temperature for 5 h, separate and collect the solid material, and obtain a modified tourmaline powder intermediate; Step D2: Mix 5 g of modified tourmaline powder intermediate with N,N-dimethylformamide, and ultrasonically disperse for 30 min. Under continuous nitrogen conditions, continue to add 1.4 g of triclosan and 0.08 g of sodium carbonate to the system, raise the system temperature to 75 ° C under stirring conditions, and keep warm for 7 h. After the material is naturally cooled, the solid material is separated by centrifugation, the solid material is washed, and vacuum dried to obtain a deodorized modified material.

[0032] The deodorant modified material was tested by infrared using the TENSOR 27 Fourier transform infrared spectrometer produced by BRUKER, Germany. Figure 1 As shown, analysis shows that in the infrared spectrum of the deodorizing modified material, The absorption peak of the ester group C=O appears at The absorption peak of ether bond COC appears at The absorption peak of the carbon-hydrogen bond in the benzene ring appears at The absorption peak of C-Cl appears at

[0033] The vitamin E inclusion compounds in the above examples and comparative examples were prepared by the following method: Step DD1: add 6 g of protamine and 2.4 g of palmitic acid to a mixed solution of dimethyl sulfoxide and purified water in a volume ratio of 1:1, stir mechanically to obtain an intermediate material, add 0.1 g of 4-dimethylaminopyridine and 0.06 g of N,N-dicyclohexylcarbodiimide, and continue stirring at room temperature for 8 h. The whole process is carried out under nitrogen protection, and the solvent is removed by reduced pressure distillation to obtain an intermediate material. Step DD2: adding the intermediate material prepared in step DD1 to 50 ml of 60% by mass ethanol aqueous solution, stirring at a stirring rate of 500 r / min for 30 min to obtain an intermediate material solution; Step DD3: Under stirring, add 5 g of vitamin E to the intermediate material solution, set the stirring rate to 150 r / min, and after stirring to form a uniform liquid, adjust the speed to 800 r / min, and under continuous stirring, add the uniform liquid dropwise to 200 ml of deionized water at a rate of 15 mL / min, let it stand for 2 hours, and obtain a vitamin E inclusion compound through reduced pressure concentration and freeze-drying.

[0034] The prepared vitamin E inclusion complex was added into 50 ml of anhydrous ethanol, shaken thoroughly with a vortex shaker, washed by centrifugation, the supernatant was collected, the solvent was removed by rotary evaporation, and the vitamin E in the supernatant was collected. The embedding rate was calculated according to the formula P=[(T-T1) / T]×100%, where P is the embedding rate, %; T is the total mass of vitamin E, g; T1 is the mass of vitamin E in the supernatant, g; after calculation, the embedding rate of vitamin E was 70.4%.

[0035] Performance Testing Antibacterial performance test The toothpastes prepared in Examples 1 to 3 and Comparative Examples 1 to 4 of the present invention were tested for antibacterial performance according to WS / T650-2019 "Antibacterial and Antibacterial Effect Evaluation Method", and a quantitative antibacterial test was performed by carrier immersion. The test strains were Staphylococcus aureus (ATCC6538), Escherichia coli (8099), Candida albicans (ATCC10231), and Porphyromonas gingivalis (ATCC33277). The specific test results are shown in Table 1: Table 1 - Antibacterial performance test

[0036] It can be seen from the test results in Table 1 that the toothpastes prepared in Examples 1 to 3 of the present invention have good antibacterial properties; the toothpaste prepared in Comparative Example 1 does not add the vitamin E inclusion compound, and compared with the examples, the antibacterial performance of the toothpaste is average; the toothpaste prepared in Comparative Example 2 does not add the deodorant modifier, and the antibacterial performance of the toothpaste is not as good as that of the examples; the toothpaste prepared in Comparative Example 3 adds protamine, vitamin E and a deodorant modifier, and the antibacterial performance of the toothpaste is good; the toothpaste prepared in Comparative Example 4 does not add the deodorant modifier and the vitamin E inclusion compound, so the antibacterial performance of the toothpaste is poor.

[0037] Deodorization performance test 35 subjects aged 20-45 were randomly divided into seven groups. The subjects had more than 20 teeth in their mouths, no oral mucosal diseases, no digestive system diseases, no periodontal treatment in the past three weeks, no regular drinking and smoking habits, and women who were not menstruating, with a breath value of more than 130. The subjects did not brush their teeth in the morning and were on an empty stomach. The breath value was detected by a 4170 hydrogen sulfide analyzer, and the test was performed three times, and the average was recorded as T1; then the toothpaste prepared in Examples 1-3 and Comparative Examples 1-4 was used for brushing teeth, the toothpaste dosage was 1g, and it was ensured that the brushing was completed within 3 minutes. The breath value was measured immediately after brushing teeth, and the test was performed three times, and the average was recorded as T2. The deodorization rate T was calculated, T=T1-T2 / T1. The specific test results are shown in Table 2: Table 2- Deodorization performance test

[0038] It can be seen from the test results in Table 2 that the toothpastes prepared in Examples 1 to 3 of the present invention, Comparative Examples 1 and 3 have good deodorizing properties; the toothpaste prepared in Comparative Example 2 does not add a deodorizing modifier, and compared with the examples, the deodorizing performance of the toothpaste is average; the toothpaste prepared in Comparative Example 4 does not add a deodorizing modifier and a vitamin E inclusion compound, so the deodorizing performance of the toothpaste is the worst.

[0039] Mouth ulcer test 70 male rats weighing 250±5g were randomly divided into seven groups. The lower end of a plastic dropper (with an inner diameter of 3mm) with a phenol cotton ball was placed flat on the buccal membrane about 1mm from the left corner of the mouth of the rat and burned for 40 seconds, that is, a white wound with a diameter of about 3mm appeared at the site, which was the ulcer. Then, the toothpaste prepared in Examples 1-3 and Comparative Examples 1-4 was used to cover the ulcer surface, and washed with water after 3 minutes. The diameter of the ulcer surface of the rat was measured and photographed on the 3rd, 5th and 7th days of treatment. The ulcer surface was treated with toothpaste twice a day. The specific test results are shown in Table 3: Table 3 - Oral ulcer test

[0040] It can be seen from the test results in Table 3 that the toothpaste with added deodorant modifier and vitamin E inclusion compound has a good therapeutic effect on the ulcer surface of rats, and the rats can basically recover on the 7th day; the toothpaste in Comparative Example 1 does not add vitamin E inclusion compound, and the healing process of the ulcer surface of the rat is slow. The ulcer surface is still not completely healed on the 7th day, and the therapeutic effect is poor; the toothpaste in Comparative Example 2 does not add deodorant modifier, and the healing effect of the ulcer surface is average compared with the embodiment; the toothpaste in Comparative Example 3 uses protamine and vitamin E to replace the vitamin E inclusion compound. Compared with the embodiment, the healing effect of the ulcer surface is average, which may be because vitamin E is directly added without coating, and cannot play a role in positioning, sustained-release and targeting, resulting in a decrease in the therapeutic effect on oral ulcers; the toothpaste prepared in Comparative Example 4 does not add deodorant modifier and vitamin E inclusion compound, so the healing effect of the ulcer surface is poor.

[0041] The above contents are merely examples and explanations of the concept of the present invention. The technicians in this technical field may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the concept of the invention or exceed the scope defined by the claims, they should all fall within the protection scope of the present invention.

Claims

1. A toothpaste with biologically active deodorant, characterized in that: The invention comprises the following raw materials in parts by weight: 0.2-0.6 parts of sucralose, 5-10 parts of glycerol, 30-40 parts of sorbitol, 0.1-0.3 parts of benzyl alcohol, 1-2 parts of sodium dihydrogen phosphate, 15-25 parts of hydrated silica, 0.4-0.6 parts of sodium carboxymethyl cellulose, 0.4-0.8 parts of xanthan gum, 3-5 parts of deodorizing modified materials, 4-6 parts of vitamin E inclusion compound, 2-3 parts of foaming agent, 0.5-1.5 parts of flavor and the balance of deionized water.

2. A toothpaste with biologically active deodorant according to claim 1, characterized in that: The preparation method of the deodorizing modified material comprises the following steps: Step D1: ultrasonically disperse the tourmaline powder in acetone, add 2-bromoisobutyryl bromide and triethylamine to the formed dispersion under nitrogen protection, stir at room temperature for 4-6 hours, separate and collect the solid material, and obtain a modified tourmaline powder intermediate; Step D2: Mix the modified tourmaline powder intermediate with N,N-dimethylformamide, and ultrasonically disperse for 20-40 minutes. Under continuous nitrogen conditions, continue to add triclosan and catalyst to the system, raise the system temperature to 70-80°C under stirring conditions, and keep warm for 5-8 hours. After the material is naturally cooled, the solid material is separated by centrifugation, the solid material is washed, and vacuum dried to obtain a deodorized modified material.

3. A toothpaste with biologically active deodorant according to claim 2, characterized in that: In step D1, the average particle size of the tourmaline powder is 5 μm.

4. A toothpaste with biologically active deodorant according to claim 2, characterized in that: In step D2, the catalyst is any one of sodium carbonate, potassium carbonate or sodium bicarbonate.

5. A toothpaste with biologically active deodorant according to claim 1, characterized in that: The preparation method of the vitamin E inclusion compound comprises the following steps: Step DD1: adding protamine and palmitic acid to a mixed solution of dimethyl sulfoxide and purified water, mechanically stirring the mixture, adding an activator and a condensing agent, stirring the mixture for 6-10 hours at room temperature, the whole process being carried out under nitrogen protection, and removing the solvent by distillation under reduced pressure to obtain an intermediate material; Step DD2: adding the intermediate material prepared in step DD1 to the ethanol aqueous solution, stirring at a stirring rate of 400-600 r / min for 20-40 min to obtain an intermediate material solution; Step DD3: Under stirring, add vitamin E to the intermediate material solution, set the stirring rate to 100-200r / min, and after stirring to form a uniform liquid, adjust the rotation speed to 600-1000r / min, and under continuous stirring, add the uniform liquid dropwise into deionized water at a rate of 5-20mL / min, let stand for 1-3h, and obtain a vitamin E inclusion complex through reduced pressure concentration and freeze-drying.

6. A toothpaste with biologically active deodorant according to claim 5, characterized in that: In step DD1, the activator is any one of 4-dimethylaminopyridine, N-hydroxysuccinimide or 1-hydroxybenzotriazole.

7. A toothpaste with biologically active deodorant according to claim 5, characterized in that: In step DD1, the condensing agent is any one of N,N-dicyclohexylcarbodiimide, 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide or N,N'-diisopropylcarbodiimide.

8. A toothpaste with biologically active deodorant according to claim 5, characterized in that: In step DD2, the mass fraction of the ethanol aqueous solution is 20%-80%.

9. A toothpaste with biologically active deodorant according to claim 5, characterized in that: In step DD3, the volume ratio of the uniform liquid material to deionized water is 1:3-4.

10. A method for preparing a toothpaste having biological activity and deodorizing properties as claimed in claim 1, characterized in that: The following steps are involved: Step 1: Add sucralose, glycerol, sorbitol, benzyl alcohol, sodium dihydrogen phosphate and deionized water into a liquid premixing pot and stir evenly to obtain premix A; Step 2: Put hydrated silica, sodium carboxymethyl cellulose, xanthan gum, deodorizing modified material, vitamin E inclusion compound and foaming agent into a powder premixing pot, start a stirrer to mix, and obtain premix B; Step 3: Start the paste making machine, open the feed valve, suck the premix A into the paste making machine with vacuum, close the feed valve, and then turn on the vacuum pump to suck the premix B into the paste making machine. After sucking, close the feed valve, and then turn on the vacuum pump to stir. Stir until the paste begins to slowly drop and stabilize without rising, continue stirring for 15-25 minutes, and finally open the flavor inlet valve to suck the flavor into the paste pot. After sucking, close the flavor inlet valve, stir until the paste begins to slowly drop and stabilize without rising, continue stirring for 10-20 minutes, then stop double stirring, continue to stir with a scraper for 4-6 minutes, discharge the material, and obtain toothpaste.

Citation Information

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