Oral care composition for middle-aged and elderly people and preparation method of oral care composition

Abstract

The invention discloses an oral care composition for middle-aged and elderly people and a preparation method thereof, and belongs to the technical field of oral care compositions. The oral care composition is used for solving the technical problems that the oral care composition in the prior art cannot adopt a proper carrier to load antibacterial and anti-inflammatory active substances and how to improve the tooth hardness of middle-aged and elderly people. The oral care composition for middle-aged and elderly people comprises a blood coagulation preparation, repair type permeable resin, peppermint oil and deionized water. The amylopectin is crosslinked with sodium trimetaphosphate, and corn starch after primary crosslinking is obtained; cetylpyridinium chloride is added into the starch emulsion for secondary crosslinking, and the crosslinked starch carrier is prepared. Uniformly mixing the adsorbent resin, calcium phosphate, magnolol and ultrapure water, and reacting to prepare the repair type permeable resin; the adsorption resin is obtained by reaction of formaldehyde, 2-(trifluoromethyl) hydroquinone, 4-bromine-1-butene and the like. The oral care composition for the middle-aged and elderly people has the advantages of being antibacterial, high in stability and capable of enhancing tooth strength.

Description

Technical Field

[0001] This invention relates to the field of oral care composition technology, specifically to an oral care composition for middle-aged and elderly people and its preparation method. Background Technology

[0002] Gum health is the foundation of oral health. With the continuous progress of society, people's life pressures are increasing; irregular eating habits, improper oral hygiene practices, and especially the declining immunity of middle-aged and elderly people, all contribute to various gum problems. The oral cavity is a complex and complete micro-ecosystem; the interaction and balance among oral microorganisms maintain oral health. When this balance is disrupted, it can lead to various oral diseases, including tooth decay and periodontal disease.

[0003] Patent application CN104023700A discloses an oral care or cleaning composition containing a dissolved magnolol analogue and PPG-1-PEG-9 lauryl glycol ether. The oral care composition using the aforementioned dissolved analogue can provide antibacterial activity and prevent inflammation. How to select a suitable carrier to load the above-mentioned active substances, thereby improving the stability of the active substances, is an urgent technical problem to be solved. In addition, how to enhance the hardness of teeth in middle-aged and elderly people is also a technical problem that urgently needs to be solved in oral care compositions for this age group.

[0004] To address this technical deficiency, a solution is proposed. Summary of the Invention

[0005] The purpose of this invention is to provide an oral care composition for middle-aged and elderly people and its preparation method, which solves the technical problems in the prior art where existing oral care compositions fail to use suitable carriers to load antibacterial and anti-inflammatory active substances and how to improve the hardness of teeth in middle-aged and elderly people.

[0006] The objective of this invention can be achieved through the following technical solutions: An oral care composition for middle-aged and elderly people, comprising, by weight, 10-15 parts of a coagulation agent, 10-20 parts of a restorative penetrating resin, 1-3 parts of peppermint oil and 50-60 parts of deionized water.

[0007] Furthermore, the method for preparing the coagulation agent includes the following steps: A1. Sodium trimetaphosphate is added to deionized water and stirred to dissolve, yielding a surfactant solution. Amylopectin is added to the surfactant solution and mixed well to obtain a mixture. Sodium carbonate powder is added to the mixture to adjust the pH to 9.5-10.5, and the mixture is reacted at 55-65℃ for 60-80 minutes. After filtration, corn starch with one cross-linking is obtained. Water is added to the corn starch with one cross-linking until a starch emulsion with a content of 30-40%wt is formed. A2. Add cetylpyridinium chloride to starch emulsion to obtain reactants; add NaOH solution dropwise to adjust the pH value to 7-8, and carry out secondary cross-linking at 60-65℃ to prepare cross-linked starch carriers; Sodium trimetaphosphate can undergo esterification with the hydroxyl groups in starch molecules to form phosphate ester bonds, thereby generating cross-linked starch. Sodium ions may also form ionic bonds with starch hydroxyl groups, further enhancing the cross-linked structure. The primary cross-linked corn starch undergoes electrostatic adsorption with cetylpyridinium chloride for secondary cross-linking, thus producing the prepared cross-linked starch carrier.

[0008] A3. Cross-linked starch carrier and Bletilla striata powder were mixed and centrifuged. The Bletilla striata powder was then encapsulated at room temperature to obtain the product. The product was washed with distilled water and dried to prepare a coagulation preparation.

[0009] Further, in step A1, the ratio of sodium trimetaphosphate to deionized water is 10-20g:300-325mL, and the ratio of surfactant solution to amylopectin is 300-330mL:100-150g.

[0010] Further, in step A2, the weight ratio of starch emulsion to cetylpyridinium chloride is 100:3-10, and the duration of secondary cross-linking is 30-60 min; in step A3, the ratio of cross-linked starch carrier to Bletilla striata powder is 10-20 g:20-30 g; the centrifugation speed is 4000-5000 r / min, the centrifugation time is 15-20 min, the standing time is 40-60 min; the drying temperature is 60-70℃, and the drying time is 30-50 min.

[0011] Furthermore, the preparation method of the repair-type penetrating resin includes the following steps: B1. Formaldehyde and 2-(trifluoromethyl)hydroquinone were mixed at -20~-22℃ to obtain the reactants; HCl solution was added dropwise to adjust the pH of the reactants to 3-4; the reaction was then carried out at 80-90℃ for 6-8 hours to synthesize the product; the formaldehyde was removed from the product by rotary evaporation to prepare the intermediate product. Under acidic conditions, 2-(trifluoromethyl)hydroquinone and formaldehyde undergo a condensation polymerization reaction to synthesize an intermediate product, as shown in the following reaction formula: B2, intermediate product, 4-bromo-1-butene and ethanol are blended to obtain a composition; NaOH solution is added dropwise to the composition to adjust the pH value of the composition to 8-9; the composition is then heated to 85-90℃ and reacted at this temperature for 3-4 hours; peracetic acid is then added and an oxidation reaction is carried out at 65-75℃ for 2-3 hours; finally, the composition is filtered through a filter membrane and the ethanol is removed by rotary evaporation to synthesize the adsorption resin. Under alkaline conditions, the intermediate product undergoes a nucleophilic substitution reaction with 4-bromo-1-butene, as shown in the following reaction formula: Further catalytic oxidation is performed to synthesize the adsorption resin; the structural formula of the adsorption resin is as follows: B3. Mix the adsorption resin, calcium phosphate, magnolol and ultrapure water, transfer to a water bath shaker, and react at 25-30℃ and 120-150 r / min for 100-120 min. After filtration, collect the solid. Dry the solid under vacuum at 60-70℃ to constant weight to prepare the repair-type penetrating resin.

[0012] The adsorption resin, calcium phosphate, and magnolol were transferred to a water bath shaker for centrifugation to obtain a repair-type permeable resin containing the adsorption active composition of calcium phosphate and magnolol.

[0013] Further, in step B1, the ratio of formaldehyde to 2-(trifluoromethyl)hydroquinone is 40-60 mL: 9-18 g, and the rotary evaporation temperature is 40-45 °C; in step B2, the ratio of intermediate product, 4-bromo-1-butene, ethanol, and peracetic acid is 12-20 g: 10-15 mL: 200 mL: 2.5-3 mL; the pore size of the filter membrane is 20-30 μm, and the rotary evaporation temperature is 50-60 °C.

[0014] Furthermore, in step B3, the ratio of adsorption resin, calcium phosphate, magnolol, and ultrapure water is 20-30g:2-5g:3-5g:200mL.

[0015] As another aspect of the present invention, a coagulation agent, a repair-type penetrating resin, peppermint oil and deionized water are mixed to obtain an oral care composition for middle-aged and elderly people.

[0016] The present invention has the following beneficial effects: 1. The oral care composition for middle-aged and elderly people prepared in this invention is a solvent-based composition, using a coagulation agent and a repair-type penetrating resin as active substances, and adding peppermint oil to remove odor. This invention uses amylopectin as a carrier. Amylopectin contains multiple hydroxyl functional groups, and its terminal carbon atoms contain free α-hydroxyl groups, possessing reducing ends. Oxidation with sodium trimetaphosphate yields primary cross-linked corn starch. Cetylpyridinium chloride itself can act as an antibacterial agent and can undergo secondary cross-linking with starch emulsion, thereby preparing a cross-linked starch carrier. After secondary cross-linking, the amylopectin has a denser particle structure, thus improving its stability against heat, acid, and shear stress, resulting in higher chemical stability and multi-functional group modification. Bletilla striata is rich in polysaccharides (multi-hydroxyl), flavonoids (phenolic hydroxyl), saponins (hydroxycarboxyacetyl), and other active ingredients, possessing multiple effects such as hemostasis, anti-inflammation, tissue regeneration, and promoting tissue regeneration. By adsorbing active substances, the cross-linked starch carrier encapsulates modified Bletilla striata powder, thereby preparing a coagulation agent for oral care compositions.

[0017] 2. 2-(trifluoromethyl)hydroquinone and formaldehyde undergo condensation polymerization under acidic conditions, followed by a nucleophilic substitution reaction with 4-bromo-1-butene, oxidizing the double bonds to epoxy groups. This yields an adsorption resin rich in fluorine and epoxy functional groups. Calcium phosphate and magnolol, active substances, are adsorbed onto the surface of the adsorption resin, preparing a restorative penetrating resin. The fluorine-grafted adsorption resin reduces the solubility of tooth enamel and promotes enamel remineralization. Adding calcium phosphate to the adsorption resin replenishes calcium and phosphate ions; calcium phosphate maintains and enhances the activity of free calcium and phosphate ions, preventing enamel demineralization. Magnolol, the active ingredient of magnolia bark, possesses antibacterial, anti-inflammatory, and antioxidant biological properties, inhibiting various pathogens such as Streptococcus mutans. The synthesized penetrating resin has a high permeability coefficient, making it easier to penetrate the micropores of lesions beneath the enamel surface, allowing the resin filling the micropores to form a barrier within the damaged enamel. However, the strength of the penetrating resin is low. By filling the penetrating resin with a fluoride-calcium phosphate composition, the hardness of the synthetic penetrating resin can be improved, and the problems of polymerization shrinkage and aging can be mitigated. Coagulation agents, repair penetrating resin and peppermint oil are added to deionized water to prepare a nursing composition with antibacterial and coagulation functions. Detailed Implementation

[0018] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0019] The amylopectin used in Examples 1-3 of this invention was purchased from Anaiji Chemical, CAS No. 9037-22-3, item number A0456-25G; the Bletilla striata powder used in Examples 1-3 of this invention was purchased from Bozhou Zhoumubai Pharmaceutical Co., Ltd., item number 066; the magnolol used in Examples 4-6 of this invention was purchased from Shaanxi Xintianyu Biotechnology Co., Ltd., item number XTYHP; the peracetic acid used in Examples 4-6 of this invention was purchased from Yunnan Tianfeizi Pharmaceutical Co., Ltd., mesh size 400; the calcium phosphate used in Examples 4-6 of this invention was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd., product number B300164; the magnolol used in Examples 4-6 of this invention was purchased from Sichuan Hongen Plant Technology Co., Ltd.; the peppermint oil used in Examples 7-9 of this invention was purchased from Hubei Kangchun Fragrance Co., Ltd., item number 002.

[0020] Example 1 This embodiment provides a method for preparing a coagulation agent for oral care compositions for middle-aged and elderly people, including the following steps: A1. Add 10g of sodium trimetaphosphate to 300mL of deionized water and stir to dissolve, obtaining a surfactant solution. Add 100g of amylopectin to 300mL of the surfactant solution and mix well to obtain a mixture. Add sodium carbonate powder to the mixture to adjust the pH to 9.5, react at 55℃ for 60min, and then filter to obtain the first-crosslinked corn starch. Continue to add water to the first-crosslinked corn starch until a 30%wt starch emulsion is formed.

[0021] A2. According to the weight, add 3 parts of cetylpyridinium chloride to 100 parts of starch emulsion to obtain the reactant. Add NaOH solution dropwise to the reactant to adjust the pH to 7, and carry out secondary cross-linking at 60℃ for 30 min to prepare the cross-linked starch carrier.

[0022] A3. Add 10g of cross-linked starch carrier and 20g of Bletilla striata powder to a 200mL centrifuge tube, then centrifuge the tube at 4000r / min for 15min. Let the centrifuge tube stand at room temperature for 40min to encapsulate the active substance, Bletilla striata powder, to obtain the product. Wash the product three times with distilled water and dry it at 60℃ for 30min to obtain the prepared coagulation agent.

[0023] Example 2 This embodiment provides a method for preparing a coagulation agent for oral care compositions for middle-aged and elderly people, including the following steps: A1. Add 15g of sodium trimetaphosphate to 315mL of deionized water and stir to dissolve, obtaining a surfactant solution. Add 130g of amylopectin to 320mL of the surfactant solution and mix well to obtain a mixture. Add sodium carbonate powder to the mixture to adjust the pH to 10, react at 60℃ for 70min, and then filter to obtain the first-crosslinked corn starch. Continue to add water to the first-crosslinked corn starch until a 35%wt starch emulsion is formed.

[0024] A2. According to the weight, add 6 parts of cetylpyridinium chloride to 100 parts of starch emulsion to obtain the reactant. Add NaOH solution dropwise to the reactant to adjust the pH to 7.7, and carry out secondary cross-linking at 62℃ for 50 min to prepare the cross-linked starch carrier.

[0025] A3. Add 15g of cross-linked starch carrier and 25g of Bletilla striata powder to a 200mL centrifuge tube, then centrifuge the tube at 4500r / min for 18min. Let the centrifuge tube stand at room temperature for 50min to encapsulate the active substance, Bletilla striata powder, to obtain the product. Wash the product three times with distilled water and dry it at 65℃ for 40min to obtain the prepared coagulation agent.

[0026] Example 3 This embodiment provides a method for preparing a coagulation agent for oral care compositions for middle-aged and elderly people, including the following steps: A1. Add 20g of sodium trimetaphosphate to 325mL of deionized water and stir to dissolve, obtaining a surfactant solution. Add 150g of amylopectin to 330mL of the surfactant solution and mix well to obtain a mixture. Add sodium carbonate powder to the mixture to adjust the pH to 10.5, react at 65℃ for 80min, and then filter to obtain corn starch after one cross-linking. Continue to add water to the corn starch after one cross-linking until a starch emulsion with a concentration of 40% wt is formed.

[0027] A2. According to the weight, add 10 parts of cetylpyridinium chloride to 100 parts of starch emulsion to obtain the reactant. Add NaOH solution dropwise to the reactant to adjust the pH to 8, and carry out secondary cross-linking at 65℃ for 60 min to prepare the cross-linked starch carrier.

[0028] A3. Add 20g of cross-linked starch carrier and 30g of Bletilla striata powder to a 200mL centrifuge tube, then centrifuge the tube at 5000r / min for 20min. Let the centrifuge tube stand at room temperature for 60min to encapsulate the active substance, Bletilla striata powder, to obtain the product. Wash the product three times with distilled water and dry it at 70℃ for 50min to obtain the prepared coagulation agent.

[0029] Example 4 This embodiment provides a method for preparing a restorative penetrating resin for oral care compositions for middle-aged and elderly people, including the following steps: B1. Transfer a 500 mL four-necked flask to a cold water bath. Add 60 mL of formaldehyde solvent to the flask at -22 °C, followed by 18 g of 2-(trifluoromethyl)hydroquinone. Mix well to obtain the reactant. Then, add 0.1 mol / L HCl solution dropwise to the flask to adjust the pH of the reactant to 4. Transfer the flask to a warm water bath and react at 90 °C for 8 h to synthesize the product. Remove the formaldehyde solvent from the product by rotary evaporation at 45 °C to obtain the intermediate product.

[0030] B2, 20 g of the intermediate product, 15 mL of 4-bromo-1-butene, and 200 mL of ethanol were added to a 500 mL four-necked flask to obtain the composition. 0.1 mol / L NaOH solution was added dropwise to the composition to adjust the pH to 9. The composition was heated to 90 °C and reacted at this temperature for 4 h. Then, 3 mL of peracetic acid was added to the four-necked flask, and an oxidation reaction was carried out at 75 °C for 3 h. The mixture was then filtered through a 30 μm pore size filter membrane, and the ethanol solvent was removed by rotary evaporation at 60 °C to synthesize the adsorption resin.

[0031] B3. Add 30g of adsorption resin, 5g of calcium phosphate, 5g of magnolol, and 200mL of ultrapure water to a 500mL Erlenmeyer flask and stir thoroughly with a glass rod. Then transfer the Erlenmeyer flask to a water bath shaker and react at 30℃ and 150r / min for 120min. After filtration, collect the solid. Dry the solid under vacuum at 70℃ to constant weight, which is the prepared remedial penetrating resin.

[0032] Example 5 This embodiment provides a method for preparing a restorative penetrating resin for oral care compositions for middle-aged and elderly people, including the following steps: B1. Transfer a 500 mL four-necked flask to a cold water bath. Add 50 mL of formaldehyde solvent to the flask at -20 °C, followed by 15 g of 2-(trifluoromethyl)hydroquinone. Mix well to obtain the reactant. Then, add 0.1 mol / L HCl solution dropwise to the flask to adjust the pH of the reactant to 4. Transfer the flask to a warm water bath and react at 85 °C for 7 h to synthesize the product. Remove the formaldehyde solvent from the product by rotary evaporation at 42 °C to obtain the intermediate product.

[0033] B2, 18 g of the intermediate product, 12 mL of 4-bromo-1-butene, and 200 mL of ethanol were added to a 500 mL four-necked flask to obtain the composition. 0.1 mol / L NaOH solution was added dropwise to adjust the pH of the composition to 9. The composition was heated to 88 °C and reacted at this temperature for 3.6 h. Then, 2.5 mL of peracetic acid was added to the four-necked flask, and an oxidation reaction was carried out at 70 °C for 2.5 h. The mixture was then filtered through a 25 μm pore size filter membrane, and the ethanol solvent was removed by rotary evaporation at 55 °C to synthesize the adsorption resin.

[0034] B3. Add 26g of adsorption resin, 3g of calcium phosphate, 4g of magnolol, and 200mL of ultrapure water to a 500mL Erlenmeyer flask and stir thoroughly with a glass rod. Then transfer the Erlenmeyer flask to a water bath shaker and react at 28℃ and 130r / min for 110min. After filtration, collect the solid. Dry the solid under vacuum at 65℃ to constant weight, which is the prepared remedial penetrating resin.

[0035] Example 6 This embodiment provides a method for preparing a restorative penetrating resin for oral care compositions for middle-aged and elderly people, including the following steps: B1. Transfer a 500 mL four-necked flask to a cold water bath. Add 60 mL of formaldehyde solvent to the flask at -22 °C, followed by 18 g of 2-(trifluoromethyl)hydroquinone. Mix well to obtain the reactant. Then, add 0.1 mol / L HCl solution dropwise to the flask to adjust the pH of the reactant to 4. Transfer the flask to a warm water bath and react at 90 °C for 8 h to synthesize the product. Remove the formaldehyde solvent from the product by rotary evaporation at 45 °C to obtain the intermediate product.

[0036] B2, 20 g of the intermediate product, 15 mL of 4-bromo-1-butene, and 200 mL of ethanol were added to a 500 mL four-necked flask to obtain the composition. 0.1 mol / L NaOH solution was added dropwise to the composition to adjust the pH to 9. The composition was heated to 90 °C and reacted at this temperature for 4 h. Then, 3 mL of peracetic acid was added to the four-necked flask, and an oxidation reaction was carried out at 75 °C for 3 h. The mixture was then filtered through a 30 μm pore size filter membrane, and the ethanol solvent was removed by rotary evaporation at 60 °C to synthesize the adsorption resin.

[0037] B3. Add 30g of adsorption resin, 5g of calcium phosphate, 5g of magnolol, and 200mL of ultrapure water to a 500mL Erlenmeyer flask and stir thoroughly with a glass rod. Then transfer the Erlenmeyer flask to a water bath shaker and react at 30℃ and 150r / min for 120min. After filtration, collect the solid. Dry the solid under vacuum at 70℃ to constant weight, which is the prepared remedial penetrating resin.

[0038] Example 7 This embodiment provides a method for preparing an oral care composition for middle-aged and elderly people, including the following steps: The oral care composition for middle-aged and elderly people is prepared by mixing 10 parts of the coagulation preparation prepared in Example 1, 10 parts of the repair-type penetrating resin prepared in Example 4, 1 part of peppermint oil and 50 parts of deionized water according to the weight.

[0039] Example 8 This embodiment provides a method for preparing an oral care composition for middle-aged and elderly people, including the following steps: The oral care composition for middle-aged and elderly people is prepared by mixing 12 parts of the coagulation preparation prepared in Example 2, 15 parts of the repair-type penetrating resin prepared in Example 5, 2 parts of peppermint oil and 55 parts of deionized water according to the weight.

[0040] Example 9 This embodiment provides a method for preparing an oral care composition for middle-aged and elderly people, including the following steps: The oral care composition for middle-aged and elderly people is prepared by mixing 15 parts of the coagulation preparation prepared in Example 3, 20 parts of the repair-type penetrating resin prepared in Example 6, 3 parts of peppermint oil and 60 parts of deionized water according to the weight.

[0041] Comparative Example 1 The difference between this comparative example and Example 9 lies in the method of preparing the coagulation agent, which specifically includes the following steps: A1. Add 20g of sodium trimetaphosphate to 325mL of deionized water and stir to dissolve, obtaining a surfactant solution. Add 150g of amylopectin to 330mL of the surfactant solution and mix well to obtain a mixture. Add sodium carbonate powder to the mixture to adjust the pH to 10.5, react at 65℃ for 80min, and then filter to obtain the first-crosslinked corn starch, which is the prepared crosslinked starch carrier.

[0042] A2. Add 20g of cross-linked starch carrier, 10 parts of cetylpyridinium chloride, and 30g of Bletilla striata powder to a 200mL centrifuge tube. Centrifuge the tube at 5000r / min for 20min. Then, let the centrifuge tube stand at room temperature for 60min to encapsulate the active substance, Bletilla striata powder, to obtain the product. Wash the product three times with distilled water and dry it at 70℃ for 50min to obtain the prepared coagulation preparation.

[0043] Comparative Example 2 The difference between this comparative example and Example 9 is that step A3 is omitted. 20g of cross-linked starch carrier and 30g of Bletilla striata powder are added to a 200mL centrifuge tube, and then the centrifuge tube is centrifuged at 5000r / min for 20min to obtain the product. The product is washed three times with distilled water and dried at 70℃ for 50min to obtain the prepared coagulation preparation.

[0044] Comparative Example 3 The difference between this comparative example and Example 9 is that, in step B1, 2-(trifluoromethyl)hydroquinone is replaced with an equal mass of hydroquinone when preparing the repair-type penetrating resin.

[0045] Performance testing: Seven patients aged 60 years were selected. All patients consented to participate in this study and signed informed consent forms. They were diagnosed with enamel demineralization according to the "Fourth National Oral Health Epidemiological Survey Report." The seven patients were divided into three groups: Example Groups 1-3, Comparative Groups 1-3, and a blank control group. Extracted carious teeth were preserved, and 2 mm of enamel was removed by fine sandpaper to create molar specimens. The molar specimens from Example Groups 1-3 and Comparative Groups 1-3 were sequentially immersed in the oral care compositions for middle-aged and elderly individuals prepared in Examples 7-9 and Comparative Groups 1-3, respectively. The solid-liquid ratio was 60 g / L, the immersion time was 5 minutes, the immersion frequency was twice daily, and the total number of immersions was 4. The blank control group received no treatment.

[0046] 1. Three points were randomly measured on the molar specimen, and the surface microhardness was taken as the average value of the tooth samples. The hardness value of the tooth before and after the test was calculated using a microhardness tester, and the corresponding difference was calculated and recorded as ∆SMH.

[0047] 2. The oral care compositions for middle-aged and elderly people prepared in Examples 7-9 and Comparative Examples 1-3 were heated at 60°C for 10 minutes. Then, the molar specimens of Examples 1-3 and Comparative Examples 1-3 were sequentially immersed in the oral care compositions for middle-aged and elderly people prepared in Examples 7-9 and Comparative Examples 1-3, with a solid-liquid ratio of 60 g / L, an immersion time of 5 minutes, an immersion frequency of 2 times / day, and a total of 4 immersions. The ∆SMH was then measured according to the method of Test 1. The blank control group was not treated.

[0048] 3. Remove the nutrient agar plates from the anaerobic incubator at 37℃. Use a loop pick to collect one colony larger than 1 mm in diameter. Mix the colony in 2 mL of 0.85% NaCl solution, transfer it to a cuvette, and adjust the bacterial concentration to 1 × 10⁻⁶ using a UV spectrophotometer. 5 CFU / mL of E. coli bacterial suspension was placed in a 100mL beaker, and then the beaker was ultrasonically treated in an ultrasonic cleaner for 1 hour. After ultrasonic treatment, 50μL of oral care composition for middle-aged and elderly people was added to the surface of a nutrient agar plate, spread evenly using a smear stick, and incubated in a constant temperature anaerobic incubator at 37℃ for 24 hours. Colony counts and sterilization rates were calculated. The blank control group did not apply oral care composition for middle-aged and elderly people after ultrasonic treatment. Specific test results are shown in the table below: Table 1. Sample performance test data Data Analysis: By comparing and analyzing the data in the table above, the oral care composition for middle-aged and elderly people prepared in this invention can significantly improve the microhardness of teeth. This is demonstrated by the significant increase in hardness after teeth are immersed in the oral care compositions for middle-aged and elderly people prepared in Examples 7-9. However, in Comparative Example 3, when preparing the restorative penetrating resin, hydroquinone was used in place of 2-(trifluoromethyl)hydroquinone, resulting in a lack of fluoride in the prepared oral care composition for middle-aged and elderly people. Fluoride can promote enamel remineralization, thereby enhancing tooth hardness.

[0049] In Comparative Example 1, when preparing the coagulation preparation, cetylpyridinium chloride was not added to the starch emulsion for secondary cross-linking. Instead, the starch emulsion was directly mixed with cetylpyridinium chloride as a cross-linking starch carrier, which reduced the stability of the prepared oral care composition for the middle-aged and elderly.

[0050] In Comparative Example 2, when preparing the coagulation preparation, the cross-linked starch carrier and Bletilla striata powder were directly mixed and centrifuged without allowing the Bletilla striata powder to stand and be sealed in the cross-linked starch carrier. This resulted in the rapid inactivation of the Bletilla striata powder, which manifested as a decrease in the bactericidal rate against Escherichia coli.

[0051] The above description is merely an example and illustration of the structure of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described, or use similar methods to replace them, as long as they do not deviate from the structure of the invention or exceed the scope defined in the claims, all of which should fall within the protection scope of the present invention.

[0052] In the description of this specification, references to terms such as "an embodiment," "example," "specific example," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the invention. In this specification, illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0053] The preferred embodiments of the present invention disclosed above are merely illustrative of the invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the invention to specific implementations. Clearly, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of the invention, thereby enabling those skilled in the art to better understand and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims

1. An oral care composition for middle-aged and elderly people, characterized in that, By weight, it includes 10-15 parts of coagulation preparation, 10-20 parts of repairing penetrating resin, 1-3 parts of peppermint oil, and 50-60 parts of deionized water.

2. The oral care composition for middle-aged and elderly people according to claim 1, characterized in that, The method for preparing the coagulation agent includes the following steps: A1. Sodium trimetaphosphate is added to deionized water and stirred to dissolve, yielding a surfactant solution. Amylopectin is added to the surfactant solution and mixed well to obtain a mixture. Sodium carbonate powder is added to the mixture to adjust the pH to 9.5-10.5, and the mixture is reacted at 55-65℃ for 60-80 minutes. After filtration, corn starch with one cross-linking is obtained. Water is added to the corn starch with one cross-linking until a starch emulsion with a content of 30-40%wt is formed. A2. Add cetylpyridinium chloride to starch emulsion to obtain reactants; add NaOH solution dropwise to adjust the pH value to 7-8, and carry out secondary cross-linking at 60-65℃ to prepare cross-linked starch carriers; A3. Cross-linked starch carrier and Bletilla striata powder were mixed and centrifuged. The Bletilla striata powder was then encapsulated at room temperature to obtain the product. The product was washed with distilled water and dried to prepare a coagulation preparation.

3. The oral care composition for middle-aged and elderly people according to claim 2, characterized in that, In step A1, the ratio of sodium trimetaphosphate to deionized water is 10-20g:300-325mL, and the ratio of surfactant solution to amylopectin is 300-330mL:100-150g.

4. The oral care composition for middle-aged and elderly people according to claim 2, characterized in that, In step A2, the weight ratio of starch emulsion to cetylpyridinium chloride is 100:3-10; in step A3, the ratio of cross-linked starch carrier to Bletilla striata powder is 10-20g:20-30g, the centrifugation speed is 4000-5000r / min, the centrifugation time is 15-20min, the standing time is 40-60min; the drying temperature is 60-70℃, and the drying time is 30-50min.

5. The oral care composition for middle-aged and elderly people according to claim 1, characterized in that, The preparation method of the reparative penetrating resin includes the following steps: B1. Formaldehyde and 2-(trifluoromethyl)hydroquinone were mixed at -20~-22℃ to obtain the reactants; HCl solution was added dropwise to adjust the pH of the reactants to 3-4; the reaction was then carried out at 80-90℃ for 6-8 hours to synthesize the product; the formaldehyde was removed from the product by rotary evaporation to prepare the intermediate product. B2, intermediate product, 4-bromo-1-butene and ethanol are blended to obtain a composition; NaOH solution is added dropwise to the composition to adjust the pH value of the composition to 8-9; the composition is then heated to 85-90℃ and reacted at this temperature for 3-4 hours; peracetic acid is then added and an oxidation reaction is carried out at 65-75℃ for 2-3 hours; finally, the composition is filtered through a filter membrane and the ethanol is removed by rotary evaporation to synthesize the adsorption resin. B3. Mix the adsorption resin, calcium phosphate, magnolol and ultrapure water, transfer to a water bath shaker, and react at 25-30℃ and 120-150 r / min for 100-120 min. After filtration, collect the solid. Dry the solid under vacuum at 60-70℃ to constant weight to prepare the repair-type penetrating resin.

6. The oral care composition for middle-aged and elderly people according to claim 5, characterized in that, In step B1, the ratio of formaldehyde to 2-(trifluoromethyl)hydroquinone is 40-60 mL: 9-18 g, and the rotary evaporation temperature is 40-45 °C. In step B2, the ratio of intermediate product, 4-bromo-1-butene, ethanol, and peracetic acid is 12-20 g: 10-15 mL: 200 mL: 2.5-3 mL. The filter membrane has a pore size of 20-30 μm and a rotary evaporation temperature of 50-60 °C.

7. The oral care composition for middle-aged and elderly people according to claim 5, characterized in that, In step B3, the ratio of adsorption resin, calcium phosphate, magnolol, and ultrapure water is 20-30g:2-5g:3-5g:200mL.

8. A method for preparing an oral care composition for middle-aged and elderly people, characterized in that, The process includes the following steps: mixing a coagulation agent, a repair-type penetrating resin, peppermint oil, and deionized water to prepare an oral care composition for middle-aged and elderly people.

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