Oral care composition

Abstract

The invention discloses an oral care composition. The oral care composition comprises amino-modified porous silicon dioxide particles, povidone iodine distributed in internal pores of the porous silicon dioxide particles, and beta-cyclodextrin which is distributed on the surfaces of the porous silicon dioxide particles and completely coats the porous silicon dioxide particles. The oral care composition is safe and stable and can be directly used for producing oral care products, povidone iodine in the oral care composition is distributed in internal pores of porous silicon dioxide and coated with beta-cyclodextrin, and the influence of illumination, oxygen and water on active iodine sterilization components in the oral care composition is reduced. Amino groups on the surface of the porous silicon dioxide and hydroxyl groups in the coated beta-cyclodextrin can form more stable chemical bond combination, so that the stability of the composition is further improved, and the composition has long service life and stability. When the composition is used for the oral care agent, the effective iodine content is high, the rapid sterilization effect and the slow release effect can be achieved, and the effective use time of the antibacterial agent is prolonged.

Description

Technical Field

[0001] The invention belongs to the field of oral care, and in particular relates to an oral care composition, which can make the contained povidone iodine stable and effective for a long time without deliberately avoiding light and sealing conditions, and can be quickly used in the production of oral care products. Background Art

[0002] The presence of bacteria, viruses, fungi, algae and other microorganisms in nature will not only cause pollution of daily necessities such as medicines and food, but also induce infectious diseases, posing a direct threat to human health. Antibacterial is essential for people's daily lives. Iodine is a strong oxidant that can destroy the structure of proteins, thereby playing a bactericidal role. Iodine-containing antibacterial materials stand out among many antibacterial materials with their broad-spectrum and efficient bactericidal ability. Among most iodine-containing antibacterial agents, free iodine and hypoiodous acid are the main contributors to the antibacterial effect. However, iodine is insoluble in water and has the disadvantages of strong oxidizing properties, easy blooming, and toxicity, and there are many restrictions on its use alone. Polyvinylpyrrolidone (PVP) is a non-ionic surfactant that has no antibacterial effect itself, but can increase the solubility of iodine, help improve the wetting and penetration ability of iodine solution on objects, enhance the affinity of effective iodine to cell membranes, and can directly introduce effective iodine into the cell membrane and cytoplasm of bacteria, killing bacteria immediately within a few seconds, thereby enhancing the bactericidal ability of iodine. Povidone-iodine (PVP-I) is a yellow-brown to reddish-brown amorphous powder. It is an amorphous complex iodine formed by the complexation of polyvinylpyrrolidone and iodine. It is a soluble complex in solvents such as water and ethanol. Preparations containing povidone-iodine can gradually release active iodine and produce strong antibacterial and antimicrobial activity after contacting the skin or mucous membranes. It is a new type of topical disinfectant with high efficiency, broad spectrum and low toxicity.

[0003] The common povidone iodine dosage forms on the market are mainly solutions, gels, ointments, suppositories, film coatings, patches, and aerosols. Water or organic solvents such as ethanol often appear during use. Although povidone iodine is water-soluble, the polyvinyl pyrrolidone in its structure is a high-molecular polymer, which is easy to clump when dissolved in water and has poor dispersibility, resulting in a long dissolution process and uneven dispersion during the preparation of mouthwashes, gels, etc. At the same time, iodine will undergo a series of chemical reactions in the water environment system, making povidone iodine unstable in the water environment in real life, and the effective iodine content continues to decrease, which limits its application to a certain extent. The stability of povidone-iodine solution is affected by many factors such as temperature, pH value, light, and concentration. It has little effect on the antibacterial property of the system when it is prepared and used in the short term. However, when the solution system needs to be stored for a long time so that oral care products can be manufactured at any time, the current povidone-iodine solution system will inevitably decompose and sublimate iodine, and organic matter such as proteins, polysaccharides, and lipids will consume a large amount of effective iodine, resulting in a decrease in the content of effective iodine, and failing to reach an effective bactericidal concentration, resulting in product failure. When using povidone-iodine solution to produce oral care products, the stability is often improved by adjusting pH and introducing stabilizers, but the long-term stability of povidone-iodine solution cannot be guaranteed, especially when it is not necessary to deliberately avoid light and is sealed for a long time, which is not conducive to the production of sterilization and disinfection products using this solution. For example, CN1626066A discloses a povidone-iodine toothpaste, which uses silicon dioxide as an abrasive and uses sodium dihydrogen phosphate or disodium hydrogen phosphate buffer to adjust the pH to a range suitable for povidone-iodine, thereby ensuring the stability of the quality of povidone-iodine and avoiding the loss of activity of povidone-iodine due to a decrease in the effective iodine content under alkaline conditions; CN1481812A discloses a povidone-iodine spray, which contains an active agent, povidone-iodine, potassium iodate and / or potassium iodide, glycerol and / or propylene glycol, a flavoring agent and water, wherein potassium iodate can be used as a stabilizer. It is a strong oxidant that oxidizes the reduced product of free iodine, iodine anions, into iodine, thereby maintaining the bactericidal activity.Potassium iodide can form a soluble complex with iodine, and play a role in solubilization, and make iodine stable and not easy to volatilize; CN102657600A discloses a veterinary povidone-iodine gel, which is composed of povidone-iodine, a moisturizing lubricant, a gel matrix, a stabilizer potassium iodate, a buffer solution containing sodium dihydrogen phosphate and disodium hydrogen phosphate, and sterile water. According to the preparation process, the pH value and the ratio are adjusted to form the povidone-iodine gel. After the gel is made, the effective iodine of the povidone-iodine is more stable, which achieves the purpose of sustained release and high efficiency; a stabilizer and a buffer solution are added to the gel to stabilize the effective iodine; CN102919269A discloses a povidone-iodine gel. A ketone-iodine disinfectant comprises povidone-iodine (PVP-I), potassium iodate and potassium iodide. Citric acid and sodium hydroxide are used to adjust the pH of the solution. The povidone-iodine solution of the present invention contains potassium iodide and potassium iodate. In an acidic environment, potassium iodide and potassium iodate in the solution react to produce molecular iodine, which increases the effective iodine concentration in the solution and promotes the slow release of active iodine, thereby increasing the bactericidal effect time of the povidone-iodine disinfectant. CN118252873A discloses a povidone-iodine solution, which is composed of the following components in mass percentage: 1% to 10% of povidone-iodine, 0.1% to 0.5% of potassium iodate, and polyvinyl pyrrolidone. The invention discloses a novel povidone-iodine solution comprising 5% to 20% ketone, 1% to 5% patchouli extract, 2% to 10% emollient, 0.1% to 0.5% pH buffer and the balance being water. Patchouli extract is added to the povidone-iodine solution, and the spatial steric hindrance of the patchouli extract and povidone-iodine is utilized to prolong the release time of the effective iodine, enhance the stability of the povidone-iodine solution and make the efficacy of the povidone-iodine solution more durable. Meanwhile, polyvinylpyrrolidone, as a carrier of the patchouli extract, further improves the stability of the patchouli extract. The patchouli extract and povidone-iodine work synergistically, significantly improving the disinfection effect and stability of the povidone-iodine solution. CN117618330A discloses an antibacterial composition with improved dispersibility, stability and iodine delivery efficiency, including povidone iodine and poloxamer, wherein poloxamer can reduce interfacial tension and promote the opening of polyvinyl pyrrolidone chains and dispersion in water; it also includes sodium hyaluronate with a molecular weight greater than 600,000, which can increase the adhesion of effective iodine, improve the utilization rate of effective iodine, and at the same time avoid the attenuation of effective iodine caused by poloxamer, thereby improving the inhibition of oral microorganisms; CN117959247A discloses a foaming povidone iodine solution, which at least includes povidone iodine, a surfactant, a stabilizer package and a pH regulator package. An anionic surfactant is added to make the povidone-iodine solution have both cleaning and disinfection effects; citric acid and sodium hydroxide are used as pH regulators, surfactant nonylphenol polyether is used as a stabilizer to protect the polymer, and potassium iodide is used as a stabilizer to reduce the decomposition of effective iodine; CN108451903A discloses a povidone-iodine solution, which is composed of povidone-iodine, potassium dihydrogen phosphate, dipotassium hydrogen phosphate, potassium iodate, glycerin, aloe polysaccharide zinc and sodium citrate.The potassium iodate added to the povidone-iodine solution can inhibit the reaction of iodate ions in water, effectively avoid or slow down the dissociation of povidone-iodine, and increase the stability of the povidone-iodine preparation. There are also a small amount of polar groups such as hydroxyl and carboxyl groups in the molecular structure of aloe polysaccharide zinc, which can form hydrogen bonds with water molecules, or the hydroxyl groups in glycerol react with the zinc ions in the aloe polysaccharide zinc to form a mutually cross-linked network structure, which can prevent the contact between iodine ions and hydrogen ions in water, and can further reduce the dissociation of povidone-iodine.

[0004] It can be seen that in view of the above problems, it is necessary to develop an oral care composition containing povidone-iodine as an antibacterial agent, which is low-cost, easy to store and use, and can be stable for a long time in a natural environment. Summary of the invention

[0005] In order to solve the defects of the prior art povidone-iodine solution, such as poor stability, the need for sealed storage away from light, and a significant decrease in effective iodine content after long-term storage, the present invention provides an oral care composition, which comprises amino-modified porous silica particles, povidone-iodine distributed in the pores inside the porous silica particles, and β-cyclodextrin distributed on the surface of the porous silica particles and completely coating the porous silica particles. The composition of this specific structure achieves double protection for the antibacterial agent povidone iodine, that is, it is effectively dispersed into the internal pores of the porous silica particles, and at the same time, the outside is completely coated by β-cyclodextrin, which effectively isolates factors such as air and water, and avoids the decomposition and failure of active iodine before use. At the same time, the "hydrophilic outside and hydrophobic inside" structure of β-cyclodextrin itself can effectively coat non-polar silica particles in the hydrophobic cavity. At the same time, in order to further strengthen the above-mentioned force, amino modification is performed on the surface of the porous silica particles, so that during the coating process, the amino groups on the surface of the porous silica particles interact with the hydroxyl groups on the β-cyclodextrin to form hydrogen bonds, so that the connection between the coating layer and the silica particle molecules is more closely intertwined, and the infiltration of external gas, water, etc. is effectively reduced, the stability of the composition is enhanced, the stability of the antibacterial substance povidone iodine is improved, and its high effective iodine content is maintained. In addition, β-cyclodextrin can be degraded by digestive enzymes and microorganisms in the human body. As a common carbohydrate, it participates in the body's metabolism without accumulation. It is an ideal inclusion carrier and is safe and non-toxic to use. At the same time, β-cyclodextrin also has certain antibacterial properties. When the composite material is used in oral care agents, such as toothpaste or mouthwash, β-cyclodextrin will gradually destroy the integrity of the coating layer under the action of friction or digestive enzymes in saliva, so that the internal povidone iodine effective ingredient contacts water and gradually releases effective iodine for sterilization and disinfection. That is, the composition has a certain slow-release effect of antibacterial substances, which can ensure a better disinfection and sterilization effect.

[0006] As a further improvement of the present invention, the amino-modified porous silica particles are prepared by the following method: 10 to 20 parts by weight of methyl orthosilicate are dissolved in ethanol to obtain solution A; 3 to 5 parts by weight of ammonia water and 1 to 2 parts by weight of hexadecyltrimethylammonium chloride are dissolved in deionized water to obtain solution B; solution B is added dropwise to solution A, heated to 50 to 80° C., stirred for reaction for 1 to 3 hours, filtered, washed, dried, calcined at 400 to 500° C. for 1 hour, and then naturally cooled to obtain porous silica; porous silica is uniformly mixed with trimethoxyaminopropylsilane and isopropanol in a mass ratio of 1:1:6 to 8, stirred for reaction at 85 to 95° C. and 200 to 300 r / min for 3 to 5 hours, solids are collected by centrifugation, rinsed with deionized water, and dried at 90 to 100° C. for 2 to 4 hours to obtain amino-modified porous silica.

[0007] As a further improvement of the present invention, the diameter of the porous silica particles is 50 to 300 nm. Preferably, the diameter of the porous silica particles can be 100 to 300 nm, 150 to 250 nm, 180 to 200 nm, etc., but not limited thereto. The average pore size of the porous silica particles can be 1 to 70 nm. Preferably, it can be 5 to 60 nm, 7 to 50 nm, 10 to 50 nm, 10 to 30 nm, 7 to 30 nm, etc., but not limited thereto. The porous silica particle diameter here refers to the size diameter of the porous silica particles in the final composition, not the diameter of the amino-modified porous silica particles obtained by direct synthesis of the present invention.

[0008] As a further improvement of the present invention, the porous silica particles have a BET specific surface area of ​​200 to 1000 m 2 Preferably, the porous silica particles have a BET specific surface area of ​​200 to 900 m 2 / g, more preferably, 200 to 700 m 2 / g, 200~600m 2 / g, 250~550m 2 / g, 300~500m 2 / g, etc., but not limited thereto, so that the povidone-iodine powder can be completely dispersed therein.

[0009] As a further improvement of the present invention, the mass ratio of the porous silica particles to povidone iodine is 10-30:0.5-1. Preferably, the mass ratio of the porous silica particles to povidone iodine is 10-30:0.8-1, more preferably 10-20:0.8-1, 10-15:0.8-1.

[0010] As a further improvement of the present invention, the mass ratio of the porous silica particles to β-cyclodextrin is 1:0.5-3.

[0011] The present invention also provides a method for preparing the oral care composition, which can obtain the oral care composition of the present invention that solves the existing problems. The composition can be a final product that can be directly used for oral care, or it can be an intermediate raw material for preparing oral care products. The preparation method of the oral care composition comprises the following steps: 1) preparing amino-modified porous silica particles: dissolving 10 to 20 parts by weight of methyl orthosilicate in ethanol to obtain solution A; dissolving 3 to 5 parts by weight of ammonia water and 1 to 2 parts by weight of hexadecyltrimethylammonium chloride in deionized water to obtain solution B; dropping solution B into solution A, heating to 50 to 80° C., stirring for reaction for 1 to 3 hours, filtering, washing, drying, calcining at 400 to 500° C. for 1 hour, and then cooling naturally to obtain porous silica; mixing porous silica, trimethoxyaminopropylsilane and isopropanol uniformly in a mass ratio of 1:1:6 to 8, stirring for reaction at 85 to 95° C. and 200 to 300 r / min for 3 to 5 hours, collecting solids by centrifugation, rinsing with deionized water, and drying at 90 to 100° C. for 2 to 4 hours to obtain amino-modified porous silica;

[0012] 2) Weighing amino-modified porous silica particles and povidone-iodine powder in a mass ratio of 10-30:0.5-1, mixing and putting into a ball mill, so that the povidone-iodine powder is completely dispersed in the pores inside the amino-modified porous silica particles; during the ball milling process, the particle size of the porous silica particles is further reduced, so that the non-polar porous silica particles in the subsequent β-cyclodextrin coating can more smoothly enter the β-cyclodextrin hydrophobic cavity to achieve coating. In this step, whether the povidone-iodine powder is completely dispersed in the amino-modified porous silica particles is determined by performing a SEM test on the particles after ball milling to observe whether there are small powder particles attached to the surface of the spherical silica particles. If not, it means that the povidone-iodine powder is completely dispersed in the porous silica particles; if yes, continue ball milling;

[0013] 3) Take 200 mg of the ball-milled powder and disperse it in 10 mL of anhydrous ethanol, ultrasonically disperse it for 30 minutes, add 100-600 mg of β-cyclodextrin under stirring conditions, heat to 40-70° C. under a nitrogen atmosphere and react for 5-10 hours. After the reaction is completed, centrifuge the solution, discard the supernatant, and vacuum dry it at 50° C. for 24 hours to obtain the product.

[0014] As a further improvement of the present invention, in step 1), the volume ratio of solution A to solution B is 2 to 5:1.

[0015] As a further improvement of the present invention, the method for preparing the oral care composition comprises the following steps: 1) preparing amino-modified porous silica particles: dissolving 15 parts by weight of methyl orthosilicate in 300 mL of ethanol to obtain solution A; dissolving 3 parts by weight of ammonia water and 2 parts by weight of hexadecyltrimethylammonium chloride in 100 mL of deionized water to obtain solution B; adding solution B dropwise into solution A, heating to 70° C., stirring for reaction for 2 hours, filtering, washing, drying, calcining at 500° C. for 1 hour, and then cooling naturally to obtain porous silica; mixing porous silica, trimethoxyaminopropylsilane and isopropanol uniformly in a mass ratio of 1:1:8, stirring for reaction at 85° C. and 300 r / min for 5 hours, collecting solids by centrifugation, rinsing with deionized water, and drying at 100° C. for 4 hours to obtain amino-modified porous silica;

[0016] 2) Weighing amino-modified porous silica particles and povidone-iodine powder in a mass ratio of 20:1, mixing and placing in a ball mill, so that the povidone-iodine powder is completely dispersed in the pores inside the amino-modified porous silica particles;

[0017] 3) Take 200 mg of the ball-milled powder and disperse it in 10 mL of anhydrous ethanol, ultrasonically disperse it for 30 min, add 300 mg of β-cyclodextrin under stirring, heat to 50° C. under a nitrogen atmosphere and react for 8 h. After the reaction is completed, centrifuge the solution, discard the supernatant, and vacuum dry it at 50° C. for 24 h.

[0018] Compared with the prior art, the technical solution of the present invention has the following beneficial effects:

[0019] 1. The oral care composition provided by the present invention is safe and non-toxic, makes full use of the bactericidal effect of povidone-iodine, does not use toxic raw materials, is safe and environmentally friendly, and can maintain the effective iodine content for a long time, such as 2 to 5 years without special treatment;

[0020] 2. The composition of the present invention can effectively disperse povidone iodine into the internal pores of silica, and by modifying the porous silica groups, a more stable hydrogen bond is formed between the hydroxyl groups on the surface of the coating material. Compared with the untreated coating relying solely on intermolecular forces, the stability of the composition is further improved. At the same time, the present invention provides double protection for the povidone iodine in the composition through a specific structure, effectively isolating factors such as air and water, avoiding the decomposition and failure of active iodine before use, and making it have long-life stability;

[0021] 3. The raw material β-cyclodextrin can be degraded by digestive enzymes and microorganisms in the human body. As a common carbohydrate, it participates in the body's metabolism, has no accumulation effect, and is safe and non-toxic. At the same time, β-cyclodextrin also has certain antibacterial properties. The composite material has high stability, good overall antibacterial properties, and has a certain sustained-release effect, which increases the effective use time of the antibacterial agent. DETAILED DESCRIPTION

[0022] In order to make the technical problems solved by the present invention, the technical solutions adopted and the technical effects achieved clearer, the technical solutions of the embodiments of the present invention are further described in detail below. 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 those skilled in the art without creative work are within the scope of protection of the present invention.

[0023] It should be noted that the reference to "embodiment" in this document means that the specific features, structures or characteristics described in conjunction with the embodiment may be included in at least one embodiment of the present application. The appearance of this phrase in various places in the specification does not necessarily refer to the same embodiment, nor is it an independent or alternative embodiment that is mutually exclusive with other embodiments. It is explicitly and implicitly understood by those skilled in the art that the embodiments described herein may be combined with other embodiments.

[0024] The experimental methods in the following examples are conventional methods unless otherwise specified. The materials and reagents used in the following examples are all commercially available unless otherwise specified. Povidone-iodine powder was purchased from BASF PVP-Iodine 30 / 60M10 (with an effective iodine content of 10.5%), and β-cyclodextrin was purchased from China Pharmaceutical (Group) Shanghai Chemical Reagent Company.

[0025] Active iodine test of the composition: according to the principle of 0.25g of povidone iodine, weigh the composition into an iodine volumetric bottle, add 75ml of purified water to dissolve, and titrate with sodium thiosulfate titrant (0.01mol / L) according to the potentiometric titration method. Calculate the active iodine content according to the dosage.

[0026] Example 1

[0027] An oral care composition comprises amino-modified porous silica particles, povidone-iodine distributed in the inner pores of the porous silica particles, and beta-cyclodextrin distributed on the surface of the porous silica particles and completely covering the porous silica particles. The preparation method of the oral care composition is as follows: 1) preparing amino-modified porous silica particles: dissolving 10 parts by weight of methyl orthosilicate in 200 mL of ethanol to obtain solution A; dissolving 3 parts by weight of ammonia water and 1 part by weight of hexadecyltrimethylammonium chloride in 100 mL of deionized water to obtain solution B; dropping solution B into solution A, heating to 50° C., stirring for reaction for 1 hour, filtering, washing, drying, calcining at 400° C. for 1 hour, and then cooling naturally to obtain porous silica; mixing porous silica, trimethoxyaminopropylsilane and isopropanol uniformly in a mass ratio of 1:1:6, stirring for reaction at 85° C. and 200 r / min for 3 hours, collecting solids by centrifugation, rinsing with deionized water, and drying at 90° C. for 2 hours to obtain amino-modified porous silica;

[0028] 2) Weighing amino-modified porous silica particles and povidone-iodine powder in a mass ratio of 10:1, mixing and placing in a ball mill for ball milling, so that the povidone-iodine powder is completely dispersed in the pores inside the amino-modified porous silica particles;

[0029] 3) Take 200 mg of the ball-milled powder and disperse it in 10 mL of anhydrous ethanol, ultrasonically disperse it for 30 minutes, add 100 mg of β-cyclodextrin under stirring conditions, heat to 40°C under a nitrogen atmosphere and react for 5 hours. After the reaction is completed, centrifuge the solution, discard the supernatant, and vacuum dry it at 50°C for 24 hours to obtain the product.

[0030] After testing, the diameter of the porous silica particles in the final composition is 50-300 nm, and the specific surface area of ​​the porous silica particles is 200-500 m 2 / g, the initial effective iodine content is 10.4%. The composition is placed in a natural environment without shading and sealing for 90 days, and the effective iodine content is tested to be 10.3%; the composition is placed in a natural environment without shading and sealing for 180 days, and the effective iodine content is tested to be 10.1%; the composition is placed in a natural environment without shading and sealing for 360 days, and the effective iodine content is tested to be 10.0%; the composition is placed in a natural environment without shading and sealing for 720 days, and the effective iodine content is tested to be 9.8%.

[0031] Example 2

[0032] An oral care composition comprises amino-modified porous silica particles, povidone-iodine distributed in the inner pores of the porous silica particles, and beta-cyclodextrin distributed on the surface of the porous silica particles and completely covering the porous silica particles. The preparation method of the oral care composition is as follows: 1) preparing amino-modified porous silica particles: dissolving 20 parts by weight of methyl orthosilicate in 500 mL of ethanol to obtain solution A; dissolving 5 parts by weight of ammonia water and 2 parts by weight of hexadecyltrimethylammonium chloride in 100 mL of deionized water to obtain solution B; dropping solution B into solution A, heating to 80°C, stirring for reaction for 3 hours, filtering, washing, drying, calcining at 500°C for 1 hour, and then cooling naturally to obtain porous silica; mixing porous silica, trimethoxyaminopropylsilane and isopropanol uniformly in a mass ratio of 1:1:8, stirring for reaction at 95°C and 300 r / min for 5 hours, collecting solids by centrifugation, rinsing with deionized water, and drying at 100°C for 4 hours to obtain amino-modified porous silica;

[0033] 2) Weighing amino-modified porous silica particles and povidone-iodine powder at a mass ratio of 60:1, mixing and placing in a ball mill for ball milling, so that the povidone-iodine powder is completely dispersed in the pores inside the amino-modified porous silica particles;

[0034] 3) Take 200 mg of the ball-milled powder and disperse it in 10 mL of anhydrous ethanol, ultrasonically disperse it for 30 minutes, add 600 mg of β-cyclodextrin under stirring conditions, heat to 70°C under a nitrogen atmosphere and react for 10 hours. After the reaction is completed, centrifuge the solution, discard the supernatant, and vacuum dry it at 50°C for 24 hours to obtain the product.

[0035] After testing, the diameter of the porous silica particles in the final composition is 50-300 nm, and the specific surface area of ​​the porous silica particles is 300-700 m 2 / g, the initial effective iodine content is 10.5%. The composition is placed in a natural environment without shading and sealing for 90 days, and the effective iodine content is tested to be 10.5%; the composition is placed in a natural environment without shading and sealing for 180 days, and the effective iodine content is tested to be 10.3%; the composition is placed in a natural environment without shading and sealing for 360 days, and the effective iodine content is tested to be 10.2%; the composition is placed in a natural environment without shading and sealing for 720 days, and the effective iodine content is tested to be 9.9%.

[0036] Example 3

[0037] An oral care composition comprises amino-modified porous silica particles, povidone-iodine distributed in the inner pores of the porous silica particles, and beta-cyclodextrin distributed on the surface of the porous silica particles and completely covering the porous silica particles. The preparation method of the oral care composition is as follows: 1) preparing amino-modified porous silica particles: dissolving 15 parts by weight of methyl orthosilicate in 300 mL of ethanol to obtain solution A; dissolving 3 parts by weight of ammonia water and 2 parts by weight of hexadecyltrimethylammonium chloride in 100 mL of deionized water to obtain solution B; dropping solution B into solution A, heating to 70°C, stirring for reaction for 2 hours, filtering, washing, drying, calcining at 500°C for 1 hour, and then cooling naturally to obtain porous silica; mixing porous silica, trimethoxyaminopropylsilane and isopropanol uniformly in a mass ratio of 1:1:8, stirring for reaction at 85°C and 300 r / min for 5 hours, collecting solids by centrifugation, rinsing with deionized water, and drying at 100°C for 4 hours to obtain amino-modified porous silica;

[0038] 2) Weighing amino-modified porous silica particles and povidone-iodine powder in a mass ratio of 20:1, mixing and placing in a ball mill, so that the povidone-iodine powder is completely dispersed in the pores inside the amino-modified porous silica particles;

[0039] 3) Take 200 mg of the ball-milled powder and disperse it in 10 mL of anhydrous ethanol, ultrasonically disperse it for 30 min, add 300 mg of β-cyclodextrin under stirring, heat to 50° C. under a nitrogen atmosphere and react for 8 h. After the reaction is completed, centrifuge the solution, discard the supernatant, and vacuum dry it at 50° C. for 24 h.

[0040] After testing, the diameter of the porous silica particles in the final composition is 50-300 nm, and the specific surface area of ​​the porous silica particles is 300-800 m 2 / g, the initial effective iodine content is 10.5%. The composition is placed in a natural environment without shading and sealing for 90 days, and the effective iodine content is tested to be 10.4%; the composition is placed in a natural environment without shading and sealing for 180 days, and the effective iodine content is tested to be 10.2%; the composition is placed in a natural environment without shading and sealing for 360 days, and the effective iodine content is tested to be 10.1%; the composition is placed in a natural environment without shading and sealing for 720 days, and the effective iodine content is tested to be 10.0%.

[0041] Comparative Example 1

[0042] The difference from Example 3 is that in step 2), porous silica particles and povidone iodine powder are weighed at a mass ratio of 5:1, and 80 mg of β-cyclodextrin is added in step 3). After testing, the diameter of the porous silica particles in the final composition is 50-200 nm, and the specific surface area of ​​the porous silica particles is 300-800 m 2 / g, the initial effective iodine content is 9.8%. The composition is placed in a natural environment without shading and sealing for 90 days, and the effective iodine content is 7.8% after testing; the composition is placed in a natural environment without shading and sealing for 180 days, and the effective iodine content is 6.2% after testing; the composition is placed in a natural environment without shading and sealing for 360 days, and the effective iodine content is 5.7% after testing; the composition is placed in a natural environment without shading and sealing for 720 days, and the effective iodine content is 5.2% after testing.

[0043] Comparative Example 2

[0044] The difference from Example 3 is that in step 2), ball milling is not performed, and conventional stirring is used for mixing. After testing, the diameter of the porous silica particles in the final composition is 50 to 1000 nm, and the specific surface area of ​​the porous silica particles is 300 to 800 m 2 / g, the initial effective iodine content is 10.1%. The composition is placed in a natural environment without shading and sealing for 90 days, and the effective iodine content is tested to be 9.3%; placed in a natural environment without shading and sealing for 180 days, and the effective iodine content is tested to be 8.4%; placed in a natural environment without shading and sealing for 360 days, and the effective iodine content is tested to be 6.9%; placed in a natural environment without shading and sealing for 720 days, and the effective iodine content is tested to be 6.1%.

[0045] Comparative Example 3

[0046] The difference from Example 3 is that porous silica is not introduced, and only the povidone-iodine particles are coated with β-cyclodextrin. After testing, the initial effective iodine content is 7.6%. The composition is placed in a natural environment without shading or sealing for 90 days, and after testing, its effective iodine content is 3.1%; after being placed in a natural environment without shading or sealing for 180 days, the effective iodine content is 1.2%; after being placed in a natural environment without shading or sealing for 360 days, there is basically no effective iodine.

[0047] Comparative Example 4

[0048] The difference from Example 3 is that cyclodextrin coating was not performed. After testing, the initial available iodine content was 10.3%. The composition was placed in a natural environment without shading and sealing for 90 days, and after testing, the available iodine content was 8.6%; after testing, it was placed in a natural environment without shading and sealing for 180 days, and the available iodine content was 5.1%; after testing, it was placed in a natural environment without shading and sealing for 360 days, and the available iodine content was 4.3%.

[0049] Comparative Example 5

[0050] The difference from Example 3 is that the porous silica obtained in step 1) is not subjected to surface amino modification and is directly used for subsequent ball milling. After testing, the diameter of the porous silica particles in the final composition is 50-300 nm, and the specific surface area of ​​the porous silica particles is 300-800 m 2 / g, the initial effective iodine content is 10.5%. The composition is placed in a natural environment without shading and sealing for 90 days, and the effective iodine content is tested to be 10.1%; placed in a natural environment without shading and sealing for 180 days, and the effective iodine content is tested to be 9.5%; placed in a natural environment without shading and sealing for 360 days, and the effective iodine content is tested to be 7.8%; placed in a natural environment without shading and sealing for 720 days, and the effective iodine content is tested to be 6.2%.

[0051] Comparative Example 6

[0052] PVP-Iodine 30 / 60M10 purchased from BASF was tested. The effective iodine content was 10.5%. After being placed in a sealed container without shielding from light for 90 days in a natural environment, the effective iodine content was tested to be 2.1%. After being placed in a sealed container without shielding from light for 180 days, there was basically no effective iodine.

[0053] From the test results in the above embodiments and comparative examples, it can be seen that the composition obtained in the embodiments of the present application has a high effective iodine retention rate, and can maintain a high effective iodine content even after being placed in an unshaded environment for 2 years. It can be seen that the product structure obtained by the specific method of the present application can achieve effective protection of the antibacterial agent povidone iodine, so that povidone iodine can be protected from the influence of light, oxygen, heat, water, etc. in the environment, and has high stability. The purchased commercial povidone iodine powder is affected by moisture and light in the air, and free iodine is continuously released and consumed from povidone iodine, resulting in a decrease in its effective iodine, and after a period of time, there is basically no effective iodine; the composition treated only with the partial method of the present invention also has a certain retention of effective iodine, but it cannot maintain a high effective iodine activity for a long time.

[0054] The above is a detailed introduction to an oral care agent composition. The above content is a further detailed description of the present invention in combination with specific preferred embodiments. It cannot be determined that the specific implementation of the present invention is limited to these descriptions. For ordinary technicians in the technical field to which the present invention belongs, without departing from the concept of the present invention, its architecture can be flexible and can derive a series of products. Just making a few simple deductions or substitutions should be regarded as belonging to the patent protection scope of the present invention determined by the submitted claims.

Claims

1. An oral care composition, characterized in that The oral care composition comprises amino-modified porous silica particles, povidone-iodine distributed in the inner pores of the porous silica particles, and beta-cyclodextrin distributed on the surface of the porous silica particles and completely covering the porous silica particles.

2. The oral care composition according to claim 1, characterized in that The amino-modified porous silica is prepared by the following method: 10 to 20 parts by weight of methyl orthosilicate is dissolved in ethanol to obtain solution A; 3 to 5 parts by weight of ammonia water and 1 to 2 parts by weight of hexadecyltrimethylammonium chloride are dissolved in deionized water to obtain solution B; solution B is added dropwise to solution A, heated to 50 to 80° C., stirred for reaction for 1 to 3 hours, filtered, washed, dried, calcined at 400 to 500° C. for 1 hour, and then naturally cooled to obtain porous silica; porous silica is uniformly mixed with trimethoxyaminopropylsilane and isopropanol in a mass ratio of 1:1:6 to 8, stirred for reaction at 85 to 95° C. and 200 to 300 r / min for 3 to 5 hours, solids are collected by centrifugation, rinsed with deionized water, and dried at 90 to 100° C. for 2 to 4 hours to obtain amino-modified porous silica.

3. The oral care composition according to claim 1, characterized in that The porous silica particles have a diameter of 50 to 300 nm.

4. The oral care composition according to claim 1 or 2, characterized in that The specific surface area of ​​the porous silica particles is 200 to 1000 m 2 / g.

5. The oral care composition according to claim 1, characterized in that The mass ratio of the porous silicon dioxide particles to povidone iodine is 10-30:0.5-1.

6. The oral care composition according to claim 1, characterized in that The mass ratio of the porous silica particles to beta-cyclodextrin is 1:0.5-3.

7. A method for preparing the oral care composition according to claim 1, characterized in that: The method comprises the following steps: 1) preparing amino-modified porous silica particles: dissolving 10 to 20 parts by weight of methyl orthosilicate in ethanol to obtain solution A; dissolving 3 to 5 parts by weight of ammonia water and 1 to 2 parts by weight of hexadecyltrimethylammonium chloride in deionized water to obtain solution B; dropping solution B into solution A, heating to 50 to 80° C., stirring for reaction for 1 to 3 hours, filtering, washing, drying, calcining at 400 to 500° C. for 1 hour, and then cooling naturally to obtain porous silica; uniformly mixing porous silica with trimethoxyaminopropylsilane and isopropanol in a mass ratio of 1:1:6 to 8, stirring for reaction at 85 to 95° C. and 200 to 300 r / min for 3 to 5 hours, collecting solids by centrifugation, rinsing with deionized water, and drying at 90 to 100° C. for 2 to 4 hours to obtain amino-modified porous silica; 2) Weighing amino-modified porous silica particles and povidone-iodine powder in a mass ratio of 10-30:0.5-1, mixing and putting into a ball mill for ball milling, so that the povidone-iodine powder is completely dispersed in the pores inside the amino-modified porous silica particles; 3) Take 200 mg of the ball-milled powder and disperse it in 10 mL of anhydrous ethanol, ultrasonically disperse it for 30 minutes, add 100-600 mg of β-cyclodextrin under stirring conditions, heat to 40-70° C. under a nitrogen atmosphere and react for 5-10 hours. After the reaction is completed, centrifuge the solution, discard the supernatant, and vacuum dry it at 50° C. for 24 hours to obtain the product.

8. The preparation method according to claim 7, characterized in that: In the step 1), the volume ratio of solution A to solution B is 2-5:1.