Remineralized composition, preparation method thereof and oral care product

Abstract

The invention belongs to the technical field of oral care, and particularly relates to a remineralized composition, a preparation method thereof and an oral care product. Comprising the following components in parts by mass: 1-5 parts of a film-forming agent, 0.05-0.15 part of fluoride, 0.01-1 part of a neutralizing agent, 40-80 parts of a humectant, 3-8 parts of a dispersing agent, 0.1-1 part of a thickening agent, 0.1-5 parts of a sweetening agent, 10-20 parts of a friction agent, 0.1-1 part of a preservative, 1-3 parts of a foaming agent, 0.5-1.5 parts of essence, 0-1 part of a pH regulator and a plurality of parts of water, wherein the remineralized composition is an ethanol-free system; and the film forming agent exists in the remineralized composition in any one of a fully neutralized state and a semi-neutralized state; according to the remineralized composition, the preparation method thereof and the oral care product, the film-forming agent is completely or partially neutralized by the neutralizer, so that the hydrophobic property of the film-forming agent is reduced, and the hydrophilic property is shown, so that the film-forming agent and fluoride form a stable form in a water-based system, and the remineralization effect is continuously exerted; and the dental caries occurrence rate of the oral care product is reduced.

Description

Technical Field

[0001] The invention belongs to the technical field of oral care, and in particular relates to a remineralization composition and a preparation method thereof, and an oral care product. Background Art

[0002] Caries, commonly known as "tooth decay", is a chronic progressive destructive disease that occurs on the hard tissues of the tooth under the action of bacteria and other factors. If not treated in time, it can cause tooth defects, residual crowns and roots, and further development of the disease can lead to pulpitis, apical periodontitis, etc., which can cause pain and discomfort to the patient.

[0003] Tooth enamel is the hardest tissue in the human body. Mature tooth enamel contains about 96% hydroxyapatite (HAP), 3% water, and 1% protein and lipid by weight. As the outermost layer of the tooth, tooth enamel is subject to various physical and chemical attacks, such as biting (up to 700N), friction, wear, and acid erosion from diet and bacteria.

[0004] The outermost layer of tooth enamel is in close contact with saliva and plaque fluid, and the HAP on its surface is in a dynamic balance of dissolution and redeposition. Oral cariogenic bacteria decompose food residues on the surface of teeth to produce acid, causing the demineralization and loss of hard tissues such as tooth enamel, dentin and cementum, which in turn leads to the formation of a series of oral diseases such as caries, tooth sensitivity, gingivitis, and gingivitis.

[0005] Fluoride is the most widely known active ingredient for preventing dental caries. During the process of brushing with fluoride toothpaste, fluoride can be delivered to many places in the oral cavity, including the tooth surface, saliva, soft tissue, and residual dental plaque. Fluoride can form CaF2-like deposits on the tooth surface, which can act as a "reservoir" of fluoride to protect the underlying enamel from acid erosion. At low pH values, CaF2-like deposits release fluoride ions, thereby inhibiting demineralization in the local microenvironment. As the pH value increases, fluoride ions can promote the formation of minerals. Therefore, fluoride can act as both an inhibitor of demineralization and a promoter of remineralization.

[0006] Fluoride can significantly reduce the dissolution rate of tooth minerals and promote the remineralization of demineralized teeth, thereby effectively preventing the occurrence of dental caries. Studies have shown that regular use of fluoride toothpaste can effectively reduce the incidence of dental caries and promote oral health.

[0007] Existing fluoride-containing oral care products have the problem of short fluoride retention time and inability to achieve long-term remineralization. Therefore, how to provide a remineralizing oral care product that can remain on the enamel surface for a long time is a technical problem that urgently needs to be solved in this field.

[0008] It should be noted that the above information disclosed in this background technology section is only used to understand the background technology of the present application concept, and therefore, the above description is not considered to constitute information of the prior art. Summary of the invention

[0009] The embodiments of the present disclosure at least provide a remineralizing composition and a preparation method thereof, and an oral care product.

[0010] In a first aspect, an embodiment of the present disclosure provides a remineralization composition, comprising the following components in parts by weight: 1-5 parts of a film former, 0.05-0.15 parts of a fluoride, 0.01-1 parts of a neutralizer, 40-80 parts of a humectant, 3-8 parts of a dispersant, 0.1-1 parts of a thickener, 0.1-5 parts of a sweetener, 10-20 parts of an abrasive, 0.1-1 parts of a preservative, 1-3 parts of a foaming agent, 0.5-1.5 parts of a flavor, 0-1 parts of a pH adjuster, and several parts of water; wherein the remineralization composition is an ethanol-free system; and the film former is present in the remineralization composition in any of the forms of complete neutralization and semi-neutralization.

[0011] In an optional embodiment, the film-forming agent is an acrylic resin copolymer.

[0012] In an optional embodiment, the film former is an acrylate octyl acrylamide copolymer.

[0013] In an alternative embodiment, the film former has a neutralization degree of 50% to 100% in the remineralizing composition.

[0014] In an optional embodiment, the neutralizing agent includes any one of triethanolamine and aminomethyl propanol or a combination of both.

[0015] In an optional embodiment, the fluoride includes any one or more combinations of sodium fluoride, sodium monofluorophosphate, stannous fluoride and olaflur.

[0016] In an alternative embodiment, the pH value of the remineralizing composition is 5.5-7.5.

[0017] In a second aspect, the embodiments of the present disclosure also provide a method for preparing the remineralized composition as described above, comprising the following steps: step S1, adding water, a moisturizer and a film-forming agent to a reactor respectively, and stirring and mixing them evenly at 200-500 rpm; step S2, adding a neutralizer to the reactor, and stirring and mixing them evenly; step S3, using a dispersant to disperse the thickener into a uniform material body and then adding it to the reactor, stirring and mixing them evenly; step S4, adding a sweetener, a fluoride, a preservative and a pH adjuster to the reactor respectively, stirring and mixing them evenly until they are completely dissolved; step S5, adding a friction agent to the reactor, stirring and mixing them evenly to obtain a paste; step S6, adding a foaming agent and a flavor to the reactor respectively, mixing and stirring them evenly, and then discharging, testing, filling and packaging in sequence to obtain the remineralized composition.

[0018] In a third aspect, the embodiments of the present disclosure also provide an oral care product, comprising the remineralizing composition as described above.

[0019] In an optional embodiment, the oral care product is any one of toothpaste, tooth powder, and oral cleaning care solution.

[0020] The beneficial effect of the present invention is that the remineralizing composition and its preparation method, and the oral care product completely or partially neutralize the film-forming agent through a neutralizing agent to reduce the hydrophobicity of the film-forming agent and show hydrophilicity, so that it forms a stable form with fluoride in an aqueous system and then continuously exerts a remineralizing effect, thereby improving the oral care product's ability to reduce the incidence of caries.

[0021] Other features and advantages of the present invention will be described in the following description, and partly become apparent from the description, or understood by practicing the present invention. The purpose and other advantages of the present invention are realized and obtained by the structures particularly pointed out in the description and claims.

[0022] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, preferred embodiments are given below for detailed description as follows. DETAILED DESCRIPTION

[0023] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution of the present invention will be described clearly and completely below. Obviously, the described embodiments are 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] As used herein, the phrases "in one embodiment," "according to one embodiment," "in some embodiments," and the like generally refer to the fact that the particular feature, structure, or characteristic following the phrase may be included in at least one embodiment of the present disclosure. Therefore, a particular feature, structure, or characteristic may be included in more than one embodiment of the present disclosure, so that these phrases do not necessarily refer to the same embodiment. As used herein, the terms "example," "exemplary," and the like are used to "serve as an example, instance, or illustration." Any implementation, aspect, or design described herein as "example" or "exemplary" is not necessarily to be construed as preferred or superior to other implementations, aspects, or designs. On the contrary, the use of the terms "example," "exemplary," and the like is intended to present concepts in a concrete manner.

[0025] In this document, as used herein, expressions such as "at least one of..." when following a list of elements modify the entire list of elements rather than modifying the individual elements in the list. For example, the expression "at least one of a, b, and c" should be understood to include only a, only b, only c, both a and b, both a and c, both b and c, or all of a, b, and c.

[0026] The terms used herein are only used to describe specific exemplary configurations and are not intended to be limited. As used herein, the singular articles "one", "an" and "the" may also be intended to include plural forms, unless it is clearly indicated above that this is not the case. The terms "comprise", "include" and "have" are inclusive, and therefore specify the presence of features, steps, operations, elements and / or components, but do not exclude the presence or addition of one or more other features, steps, operations, elements, components and / or combinations thereof. The method steps, processes and operations described herein should not be interpreted as necessarily requiring them to be performed in the specific order discussed or shown, unless specifically identified as an execution order. Additional or alternative steps may be adopted.

[0027] Chinese patent CN202410245563.0 discloses an anhydrous anti-caries gel and its preparation method and application, a tubular anhydrous anti-caries gel, which comprises a film-forming hydrophobic polymer and fluoride, and bioactive glass. In order to avoid the direct reaction of soluble fluoride and calcium in the aqueous solution system to form insoluble calcium and fluoride, the gel is an anhydrous matrix, and the hydrophobic polymer is dissolved in the matrix using anhydrous ethanol, that is, the film-forming agent is completely present in the matrix in a hydrophobic form. During use, when the gel meets water, the hydrophobic properties of the film-forming agent cause it to form a film on the surface of the teeth, that is, through this physical film-forming method, the slow release of the active ingredients is controlled to improve the remineralization effect of the anhydrous caries gel.

[0028] Similarly, Chinese invention patent CN202410283166.2 applies film-forming agents and whitening agent peroxides to tooth patch dosage forms, which improves the retention of active substances and the whitening effect by physically forming a film on the tooth surface.

[0029] The inventors found that although the physical film formed by the unneutralized film-forming agent in anhydrous ethanol using the hydrophobic property objectively delays the release of the active ingredient, the retention time is still not ideal.

[0030] On the other hand, the unneutralized film-forming polymer only exhibits hydrophobic properties. Therefore, during the use of anhydrous gel or tooth patch, the film-forming polymer quickly forms a film on the surface of teeth, oral mucosa, etc. when it encounters saliva: a. It causes a foreign body sensation in the mouth; b. After film formation, the polymer still has a waterproof function and is difficult to remove in a short time; c. The solvent ethanol in the anhydrous gel contacts the oral mucosa for a long time, which will cause mucosal irritation. These factors undoubtedly reduce the use experience of anhydrous gel and tooth patch dosage forms.

[0031] The defects existing in the above solutions are the results obtained by the inventor after practice and careful research. Therefore, the discovery process of the above problems and the solutions proposed by the present disclosure for the above problems below should be the contributions made by the inventor to the present disclosure during the disclosure process.

[0033] Some embodiments of the present invention are described in detail below. In the absence of conflict, the following embodiments and features in the embodiments can be combined with each other.

[0034] An embodiment of the present disclosure provides a remineralization composition, comprising the following components in parts by mass: 1-5 parts of a film former, 0.05-0.15 parts of a fluoride, 0.01-1 parts of a neutralizer, 40-80 parts of a humectant, 3-8 parts of a dispersant, 0.1-1 parts of a thickener, 0.1-5 parts of a sweetener, 10-20 parts of an abrasive, 0.1-1 parts of a preservative, 1-3 parts of a foaming agent, 0.5-1.5 parts of a flavor, 0-1 parts of a pH adjuster, and several parts of water; wherein the remineralization composition is an ethanol-free system; and the film former is present in the remineralization composition in any form of complete neutralization or semi-neutralization.

[0035] In some embodiments, specifically, the film-forming agent is an acrylic resin copolymer.

[0036] In some embodiments, specifically, the film former is an acrylate octyl acrylamide copolymer.

[0037] Specifically, the film-forming agent is preferably DERMACRYL 79 from Nouryon, which is a white powder with high hydrophobicity, water resistance, color dispersion, and the ability to form a thin film. It is often used in alcohol-based sunscreen systems to help keep the active ingredients on the skin active without affecting the viscosity of the formula.

[0038] In some embodiments, specifically, the neutralization degree of the film former in the remineralized composition is 50%-100%. When the film former is not neutralized, it shows hydrophobic properties and is soluble in ethanol. This solubility property makes it very suitable for alcohol-based sunscreen spray products; after the film former is neutralized, it shows hydrophilic properties and is water-soluble. It can be used to formulate various waterproof emulsions, which can increase the static SPF value of the formula and can still maintain the SPF value after being immersed in water for 80 minutes.

[0039] In some embodiments, specifically, the neutralizing agent includes any one or a combination of two of triethanolamine and aminomethyl propanol.

[0040] In some embodiments, specifically, the fluoride includes any one or more combinations of sodium fluoride, sodium monofluorophosphate, stannous fluoride and olafluor, and the mass fraction of the fluoride is calculated based on the fluorine contained therein.

[0041] In some embodiments, specifically, the pH value of the remineralization composition is 5.5-7.5. When HAP dissolves at pH < 5.5, this process is called demineralization. When HAP is at pH > 5.5 and high concentrations of calcium and phosphorus ions, the reaction equilibrium will proceed toward the direction of calcium phosphate deposition, thereby remineralizing demineralized teeth.

[0042] The disclosed embodiments also provide a method for preparing the remineralized composition as described above, comprising the following steps: step S1, adding water, a moisturizing agent and a film-forming agent to a reactor respectively, and stirring and mixing them evenly at 200-500 rpm; step S2, adding a neutralizing agent to the reactor, and stirring and mixing them evenly; step S3, using a dispersant to disperse the thickener into a uniform body and then adding the body to the reactor, and stirring and mixing them evenly; step S4, adding a sweetener, a fluoride, a preservative and a pH adjuster to the reactor respectively, and stirring and mixing them evenly until they are completely dissolved; step S5, adding an abrasive to the reactor, and stirring and mixing them evenly to obtain a paste; step S6, adding a foaming agent and a flavor to the reactor respectively, and stirring and mixing them evenly, and then discharging, testing, filling and packaging in sequence to obtain the remineralized composition.

[0043] The present disclosure also provides an oral care product, comprising the remineralizing composition as described above.

[0044] In some embodiments, specifically, the oral care product is any one of toothpaste, tooth powder, and oral cleaning care solution.

[0045] Example 1: The beneficial effects of film formers on promoting the remineralization of fluoride. The component parts of Examples A1-A3 and B1-B3 are shown in Table 1 below.

[0046] Table 1

[0047]

[0048] Preparation method:

[0049] Step S1: adding water, moisturizing agent and film-forming agent into the reactor in sequence, and stirring and mixing them uniformly at 200-500 rpm;

[0050] Step S2: adding a neutralizing agent and stirring to mix evenly;

[0051] Step S3: using a dispersant to disperse the thickener into a uniform body, and then adding it into the reactor, stirring and mixing evenly;

[0052] Step S4: adding the sweetener, fluoride, preservative, and pH adjuster into the reactor in sequence and stirring and mixing them evenly to ensure that they are dissolved;

[0053] Step S5: adding the friction agent into the reaction pot, stirring and mixing evenly, and completing the paste making process;

[0054] Step S6: Add the foaming agent and flavor into the reactor, and mix and stir evenly;

[0055] Step S7: discharging, testing, filling and packaging the mixture in the reactor in sequence.

[0056] Enamel remineralization test method (hardness test method):

[0057] Select in vitro bovine tooth enamel blocks that are close to human enamel, cut the bovine enamel into 5mm*5mm*2mm enamel blocks, and finally prepare them into 1cm*1cm*1cm enamel blocks after resin embedding, inlaying, polishing, etc. Use a hardness tester to test the initial hardness of the enamel HV0, put the enamel block into a citric acid solution to simulate the enamel acid etching process, and use a hardness tester to test the hardness after acid etching HV1.

[0058] Sample test: toothpaste and water were diluted at a ratio of 1:1.6 (mass ratio) to prepare toothpaste slurry, which was then poured into a customized device containing enamel. Under certain load conditions, an electric toothbrush was used to brush the surface of the enamel block for 2 minutes to complete one test. The enamel treated with the sample to be tested was then placed in simulated saliva and stored in a constant temperature incubator at 37°C.

[0059] The above test steps were repeated 6 times (in vitro simulation of 3 days of use), and the enamel hardness measured for the 6th time was HV6.

[0060] Repeat the above test steps 14 times (in vitro simulation of 7 days of use), the enamel hardness measured for the 14th time is HV 14 .

[0061] After 6 uses, the change in enamel hardness value (△HV) is calculated as follows: △HV = HV6 - HV1

[0062] After 14 times of use, the change in enamel hardness value (△HV) is calculated as follows: △HV = HV 14 —HV1

[0063] The test results are shown in Table 2 below:

[0064] Table 2

[0065] Hardness change value A1 A2 A3 B1 B2 B3 △HV: 3d 20.12 78.54 22.43 88.45 96.80 98.74 △HV: 7d 30.14 88.43 29.54 98.54 110.53 115.63 △HV: 3d (compared with A1) 1.00 3.90 1.11 4.40 4.81 4.91 △HV: 7d (compared with A1) 1.00 2.93 0.98 3.27 3.67 3.84 △HV: 3d (compared with A2) 0.26 1.00 0.29 1.13 1.23 1.26 △HV: 7d (compared with A2) 0.34 1.00 0.33 1.11 1.25 1.31

[0066] After the samples were treated, the effect of fluoride A2 on improving hardness was 3.90 times (3d) and 2.93 times (7d) that of the blank control group A1. That is, after the enamel was demineralized by acid etching and then treated with fluoride toothpaste A2, fluoride formed complex fluorapatite on the surface of the enamel, which was more acid-resistant and formed a protective layer, thereby improving the hardness of the enamel.

[0067] Specifically, the hardness of tooth enamel of toothpaste B1, toothpaste B2 and toothpaste B3 using "Dermacryl 79 + fluoride" was 3-5 times that of the blank control group A1. After 3 days of treatment, the hardness improvement was more obvious, all exceeding 4 times.

[0068] Specifically, compared with toothpaste A2 containing only fluoride, after treatment with toothpaste B1, the hardness change value increased by 13% (3d) and 11% (7d); after treatment with toothpaste B2, the hardness change value increased by 23% (3d) and 25% (7d); after treatment with toothpaste B3, the hardness change value increased by 26% (3d) and 31% (7d), that is, with the increase of the content of film-forming agent Dermacryl 79 and the same amount of fluoride added, the enamel repair ability gradually improved, ranging from 10% to 30%, which means that Dermacryl 79 helps to improve the remineralization efficiency of fluoride. However, the improvement of hardness of A3 using only Dermacryl 79 is almost the same as that of the blank control group A1, which means that the use of film-forming agents alone has no obvious or no effect on improving the hardness of enamel.

[0069] Example 2: Mineralization of different polymers. The component parts of Examples B2 and C2 are shown in Table 2 below.

[0070] Table 2

[0071]

[0072] Specifically, PVM / MA polymer is a linear polymer formed by the polymerization of methyl vinyl ether and maleic anhydride. It has excellent film-forming properties and can be directly used in oral care products to deliver and retain active ingredients on the oral mucosa. After brushing, the bioadhesiveness of PVM / MA polymer provides a polymer barrier film for teeth, protecting them from acid corrosion in food. PVM / MA polymer has multiple functions in toothpaste formulas, which can significantly improve the performance of toothpaste, increase the bioavailability of active substances, form a film on the surface of teeth, maintain the acid-base balance in the mouth, and protect teeth.

[0073] The test data of tooth enamel hardness are shown in Table 4 below:

[0074] Table 4

[0075] Hardness change value B2 C1 A1 A2 △HV: 3d 96.80 74.80 20.12 78.54 △HV: 7d 110.53 90.01 30.14 88.43 △HV: 3d (compared with A1) 4.81 3.62 1.00 3.90 △HV: 7d (compared with A1) 3.67 2.79 1.00 2.93 △HV: 3d (compared with A2) 1.23 0.95 0.26 1.00 △HV: 7d (compared with A2) 1.25 1.04 0.34 1.00

[0076] Specifically, after the treatment of the test samples, compared with the blank control group A1, the test samples B2, C1, and A2 all had significant hardness changes, and their hardness change values ​​were all more than 2.5 times, indicating the remineralization potential of fluoride toothpaste. By analyzing sample C1, after 3 days of treatment, its hardness change value was close to or slightly less than that of fluoride toothpaste A2, but after 7 days of treatment, compared with A2, the hardness value change of C1 increased from 0.95 times to 1.04 times, which means that with the extension of use time, the combination of PVM / MA polymer + fluorine shows the possibility of improving the remineralization effect, which also verifies the application characteristics of PVM / MA polymer toothpaste. Compared with A2, the hardness change values ​​of B2 are more than 1.2 times, which means that under the same conditions, the remineralization rate and efficiency of B2 are better than those of C1, indicating that the combination of film-forming agent Dermacryl 79 + fluoride is significantly better than the combination of PVM / MA polymer + fluoride in the speed of improving enamel hardness. The combination of film-forming agent Dermacryl 79 + fluoride can be used as a better and more efficient remineralization solution.

[0077] Example 3: In comparison with other remineralizing agents, the component parts of Examples B2, D1 and D2 are shown in Table 5 below.

[0078] Table 5

[0079]

[0080] Specifically, bioactive materials include bioglass, glass ceramics, and bioceramics, which have been widely studied as bone transplant materials. Bioglass is a type of bioactive material whose main components are calcium, sodium, phosphorus, and silicon. When bioglass comes into contact with body fluids, it can deposit calcium phosphate on the surface of the material. Similarly, when bioglass comes into contact with saliva, the sodium ions (Na + ) and the hydrogen ions (H + or H3O + ) is exchanged, releasing calcium ions (Ca 2+ ) and phosphate ions (PO4 3- ), thus forming a silicon-rich layer rich in silanol (Si-OH) on the surface of the bioglass, which can serve as a nucleation growth site for calcium phosphate. As calcium and phosphorus ions continue to dissolve from the bioglass, the concentration of calcium and phosphorus ions and the pH value in the saliva continue to increase, which prompts calcium phosphate to deposit and grow on the surface of the bioglass using the silicon-rich layer as a nucleation site.

[0081] The test data of tooth enamel hardness are shown in Table 6 below:

[0082] Table 6

[0083] Hardness change value B2 D1 D2 A1 A2 △HV: 3d 96.80 40.54 85.43 20.12 78.54 △HV: 7d 110.53 48.25 96.43 30.14 88.43 △HV: 3d (compared with A1) 4.81 2.01 4.25 1.00 3.90 △HV: 7d (compared with A1) 3.67 1.60 3.20 1.00 2.93 △HV: 3d (compared with A2) 1.23 0.52 1.09 0.26 1.00 △HV: 7d (compared with A2) 1.25 0.55 1.09 0.34 1.00

[0084] Specifically, after the samples to be tested are processed, it can be seen from the data that in terms of the change in enamel hardness, B2>D2>A2>D1>A1. That is, D1, which only uses active glass, has a weaker effect on enamel than A2, which only uses fluoride, while D2, which uses bioactive glass + fluoride, has a slightly better effect on improving hardness than A2. This means that as a remineralizing agent, bioactive glass promotes remineralization by increasing the calcium ions and phosphate ions in the oral environment, but its effect on improving the hardness of enamel and its acid resistance is weaker than that of fluoroapatite, which leads to no significant difference in hardness improvement compared with A2. Therefore, through the analysis of commercially available toothpaste, the main function of using toothpaste containing bioglass is to use bioglass particles to be deposited on the surface of tooth dentin and to block the dental tubules by inducing the generation of HAP-like materials to achieve the function of tooth anti-sensitivity. That is, the more effective effect of bioglass is reflected in blocking dentinal tubules and resisting tooth sensitivity. This group of data further illustrates the advantages of the combination of film-forming agent Dermacryl 79 + fluoride B2 in improving the hardness of tooth enamel, and can be used as a new form to protect teeth and prevent the formation of caries.

[0085] Example 4: Study on the neutralization degree of the neutralizer. The component parts of Examples B2, E1 and E2 are shown in Table 7 below.

[0086] Table 7

[0087]

[0088] The film-forming agent Dermacryl 79 is hydrophobic in its unneutralized state, insoluble in ethanol, and soluble in ethanol. When it comes into contact with water, it quickly forms a film on the surface, blocking the transfer of external substances such as water in the form of a physical barrier. This property of the film-forming agent Dermacryl 79 is usually used in products that require high waterproofness, such as sunscreen and mascara. When the film-forming agent Dermacryl 79 is neutralized, it shows hydrophilicity, and its polymer dissolves in the aqueous system, showing a certain charge characteristic. This example is studied based on this characteristic to evaluate the effect of improving the hardness of tooth enamel when used in combination with fluoride under different characteristics.

[0089] The enamel hardness test data are shown in Table 8 below:

[0090] Table 8

[0091] Hardness change value B2 E1 E2 A1 A2 Neutralization 100％ 50％ 0％ \ \ △HV: 3d 96.80 82.83 80.23 20.12 78.54 △HV: 7d 110.53 90.23 85.78 30.14 88.43 △HV: 3d (compared with A1) 4.81 4.12 3.99 1.00 3.90 △HV: 7d (compared with A1) 3.67 2.99 2.85 1.00 2.93 △HV: 3d (compared with A2) 1.23 1.05 1.02 0.26 1.00 △HV: 7d (compared with A2) 1.25 1.02 0.97 0.34 1.00

[0092] It can be seen from Table 8 that with the decrease of neutralization degree, compared with A2, the hardness change value △HV(3d) decreases from 1.23 (neutralization degree 100%) to 1.05 (neutralization degree 50%) and 1.02 (neutralization degree 0%), and the hardness change value △HV(7d) decreases from 1.25 (neutralization degree 100%) to 1.02 (neutralization degree 50%) and 0.97 (neutralization degree 0%). In terms of hardness performance: B2>E1>E2≈A2>A1. That is, as the degree of neutralization decreases, the improvement of the enamel hardness by the combination of film-forming agent Dermacryl 79 + fluoride decreases. When the degree of neutralization is 0, there is no significant difference in the improvement effect on hardness (3d and 7d) compared with the control group A2. This means that in the combination of film-forming agent Dermacryl 79 + fluoride, the neutralization degree of the film-forming agent Dermacryl 79 (the form of the film-forming agent) has a direct impact on the improvement effect on hardness. When the degree of neutralization is above 50% (that is, it exists in a semi-neutralized to completely neutralized form), there is a significant difference compared with the control group A2.

[0093] Example 5: The promoting effect of different fluorine contents. The component parts of Examples A2, B2, A4, F1, A5 and F2 are shown in Table 9 below.

[0094] Table 9

[0095]

[0096] Specifically, Examples 1, 2, 3, and 4 all demonstrate that the combination of Dermacryl 79 and fluoride is beneficial to promoting the remineralization effect of fluoride. Therefore, this group of examples explores the remineralization effect of Dermacryl 79 under different fluoride addition amounts.

[0097] The enamel hardness test data of A2 and B2 are shown in Table 10 below: (Fluoride addition amount: 1450ppm, calculated as fluorine)

[0098] Table 10

[0099] Hardness change value A2 B2 Fluorine content (measured in fluorine) 1450ppm 1450ppm △HV: 3d 78.54 96.80 △HV: 7d 88.43 110.53 △HV: 3d (compared with A2) 1.00 1.23 △HV: 7d (compared with A2) 1.00 1.25

[0100] Specifically, at a fluorine addition of 1450 ppm, compared with A2 without the film-forming agent Dermacryl 79, the combination B2 of "Dermacryl 79+F" increased the enamel hardness change value by 23% at 3d and by 25% at 7d.

[0101] The enamel hardness test data of A4 and F1 are shown in Table 11 below: (Fluoride addition amount: 1042ppm, calculated as fluorine)

[0102] Table 11

[0103] Hardness change value A4 F1 Fluorine content (measured in fluorine) 1042ppm 1042ppm △HV: 3d 65.23 75.34 △HV: 7d 77.58 95.12 △HV: 3d (compared with A4) 1.00 1.15 △HV: 7d (compared with A4) 1.00 1.23

[0104] Specifically, at a fluorine addition of 1042 ppm, compared with A4 without the film-forming agent Dermacryl 79, the combination F1 of "Dermacryl 79+F" increased the enamel hardness change value by 15% at 3d and 23% at 7d.

[0105] The enamel hardness test data of A5 and F2 are shown in Table 12 below: (Fluoride addition amount: 634 ppm, calculated as fluoride)

[0106] Table 12

[0107] Hardness change value A5 F2 Fluorine content (measured in fluorine) 634ppm 634ppm △HV: 3d 48.24 53.45 △HV: 7d 56.76 62.23 △HV: 3d (compared with A5) 1.00 1.11 △HV: 7d (compared with A5) 1.00 1.10

[0108] Specifically, at a fluorine addition of 634 ppm, compared with A4 without the film-forming agent Dermacryl 79, the combination F2 of "Dermacryl79+F" increased the enamel hardness change value by 11% at 3d and 10% at 7d.

[0109] It can be seen that under different fluorine contents, the film-forming agent Dermacryl 79 has a significant effect in promoting remineralization. When the amount of fluorine added is increased, the synergistic remineralization effect brought about by the combination of Dermacryl 79 and fluorine is more significant.

[0110] Example 6: Taste comparison test, the component parts of Examples A2, B2, and G1 are shown in Table 13 below.

[0111] Table 13

[0112]

[0113]

[0114] Taste test: 40 testers were screened for this taste test and randomly divided into 4 groups, with 10 patients in each group, including 23 male patients and 17 female patients. The oldest was 42 years old and the youngest was 21 years old.

[0115] Usage: A2, B2, G1 are used in the same way as toothpaste. Take an appropriate amount of paste, brush your teeth for 2 minutes according to the correct brushing method, then rinse your mouth with water and spit it out. G2 is used in the same way as gel. Take an appropriate amount of gel, apply it to the tooth surface for 10-20 minutes, then rinse your mouth with water and spit it out.

[0116] The taste test results are shown in Table 14 below:

[0117] Table 14

[0118]

[0119] It can be seen from the taste test results that the product use effect of B2 is the same as that of ordinary toothpaste A2, without any discomfort or abnormal feedback. Compared with B2, G1 with an anhydrous formula and ethanol system performs poorly in terms of rinsing and refreshing feeling. This is due to the film-forming agent in the product quickly forming a film when it encounters water in the mouth, and during use, the film-forming agent repeatedly forms a film, resulting in a foreign body sensation. The product attribute of G2 is a gel, and the use time is longer than that of toothpaste. Therefore, compared with toothpaste, it is not ideal in terms of rinsing, refreshing degree, and foreign body sensation. In terms of overall comfort, B2 is the same as ordinary toothpaste A2, and is better than G1 and G2. This embodiment solves the pain points of the film-forming agent in the sense of use in the anhydrous system.

[0120] Specifically, in oral care products, through the above embodiments, the film former Dermacryl 79 as one of the acrylic resin film formers, especially as an acrylate / octyl acrylate copolymer, can encapsulate fluoride and exist in the dosage form in hydrophobic and hydrophilic forms after neutralization.

[0121] When using toothpaste B1, B2, B3, F1, F2:

[0122] Specifically, acrylic resin copolymer film formers such as Dermacryl 79 can stay on the negatively charged tooth surface, and the inherent properties of the film former make it resistant to scouring and washing. Through neutralization, the film former shows hydrophilicity and charge properties. In an aqueous system, the hydrophilicity of the film former enables it to physically encapsulate fluoride, and the charge properties of the film former enable it to form a stable form with fluoride. Through these two methods, the remineralization effect is further and continuously exerted on the tooth surface, thereby improving the utilization of fluoride, improving the remineralization efficiency of fluoride, and promoting the remineralization of fluoride.

[0123] Specifically, the molecular properties of the film-forming agent Dermacryl 79 enable it to bind and adhere to the acquired salivary protein film on the tooth surface, that is, the neutralized Dermacryl 79 exhibits bioadhesion properties and can bind and adhere to the salivary protein film, rather than existing on the tooth surface as a hydrophobic film in a physically retained manner. That is, the bioadhesion properties further enhance the retention effect of fluoride and transmit it to the enamel surface, promoting the remineralization of fluoride in the weakly acidic environment of the oral cavity.

[0124] Specifically, the film-forming agent Dermacryl 79 can form a film on the surface of teeth. On the one hand, it can prevent the acidic substances produced by the metabolism of oral pathogens (such as Streptococcus mutans) from corroding the enamel, resulting in a decrease in the hardness of the teeth due to acid erosion and demineralization; on the other hand, it can wrap more fluoride through the hydrophobic properties of the film-forming agent, remain on the surface of the enamel, and then continue to remineralize.

[0125] Specifically, compared with other film-forming agents, such as PVM / MA copolymer, polyvinyl pyrrolidone, etc., the retention of fluoride is promoted only by physical encapsulation of polymer molecular chains. This is compared with the acrylic resin copolymer film-forming agent, which can form a stable form with fluoride ions through the charge characteristics after neutralization. It only reduces the remineralization effect and rate of fluoride by physically encapsulating fluoride ions. For example, in Example 2, after 3d and 7d of treatment, the remineralization rate and effect of B2 are significantly better than those of C1.

[0126] During the use of fluoride toothpaste A2, fluoride exists in a free form. In the absence of film-forming agents or polymers, fluoride ions are spit out in large quantities during the flushing process such as rinsing the mouth and the action of foaming agents (surfactants), thereby reducing the utilization rate of fluoride and limiting the effect of improving the hardness of tooth enamel.

[0127] In summary, the remineralizing composition and preparation method thereof, and the oral care product completely or partially neutralize the film-forming agent through a neutralizing agent to reduce the hydrophobicity of the film-forming agent and show hydrophilicity, so that it forms a stable form with fluoride in the aqueous system and continuously exerts a remineralizing effect, thereby improving the oral care product's ability to reduce the incidence of caries.

[0128] Based on the above ideal embodiments of the present invention, the relevant staff can make various changes and modifications without departing from the technical concept of the present invention through the above description. The technical scope of the present invention is not limited to the contents of the specification, and its technical scope must be determined according to the scope of the claims.

Claims

1. A remineralizing composition, characterized in that The composition includes the following components in parts by weight: 1-5 parts of film former, 0.05-0.15 parts of fluoride, 0.01-1 parts of neutralizer, 40-80 parts of humectant, 3-8 parts of dispersant, 0.1-1 parts of thickener, 0.1-5 parts of sweetener, 10-20 parts of abrasive, 0.1-1 parts of preservative, 1-3 parts of foaming agent, 0.5-1.5 parts of flavor, 0-1 parts of pH adjuster, and some parts of water; in The remineralizing composition is an ethanol-free system; and The film-forming agent is present in the remineralizing composition in any form of fully neutralized or semi-neutralized.

2. The remineralizing composition according to claim 1, characterized in that: The film-forming agent is an acrylic resin copolymer.

3. The remineralizing composition according to claim 2, characterized in that: The film former is an acrylate octyl acrylamide copolymer.

4. The remineralizing composition according to claim 1, characterized in that: The degree of neutralization of the film former in the remineralizing composition is 50% to 100%.

5. The remineralizing composition according to claim 1, characterized in that: The neutralizing agent includes any one of triethanolamine and aminomethyl propanol or a combination of the two.

6. The remineralizing composition according to claim 1, characterized in that: The fluoride includes any one or more combinations of sodium fluoride, sodium monofluorophosphate, stannous fluoride and olafluor.

7. The remineralizing composition according to claim 1, characterized in that: The pH of the remineralizing composition is 5.5-7.

5.

8. A method for preparing the remineralized composition according to any one of claims 1 to 7, characterized in that: The steps include: Step S1, adding water, moisturizing agent and film-forming agent into a reactor respectively, and stirring and mixing at 200-500 rpm; Step S2, adding a neutralizing agent into the reactor and stirring to mix evenly; Step S3, using a dispersant to disperse the thickener into a uniform material body, and then adding the material into the reactor, stirring and mixing evenly; Step S4, adding the sweetener, fluoride, preservative and pH adjuster into the reactor respectively, and stirring and mixing them evenly until they are completely dissolved; Step S5, adding the friction agent into the reactor, stirring and mixing evenly to obtain a paste; Step S6, adding the foaming agent and the flavor into the reactor respectively, mixing and stirring evenly, and then discharging, testing, filling and packaging in sequence to obtain the remineralized composition.

9. An oral care product, characterized in that: A remineralizing composition comprising the remineralizing composition of any one of claims 1 to 8.

10. The oral care product according to claim 9, characterized in that The oral care product is any one of toothpaste, tooth powder and oral cleaning care liquid.

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