Long-acting anti-sensitive medical tooth desensitization paste and preparation method thereof

Abstract

The invention relates to a long-acting anti-sensitive medical tooth desensitization paste and a preparation method thereof, and belongs to the technical field of daily necessities. The long-acting anti-allergy medical tooth desensitization paste provided by the invention is prepared from the following raw materials: bioactive glass, glycerol, polyethylene glycol, sorbitol, carboxymethyl cellulose sodium, xanthan gum, lauryl sodium sulfate, calcium carbonate, hydroxyapatite, silicon dioxide, titanium dioxide, saccharin sodium, sodium pyrophosphate, N, 2, 4-trimethyl-1, 3-pentanediol monoisobutyrate and a proper amount of water. The cleaning agent is prepared from 2, 3, 3-trimethyl-2-isopropyl butyramide, spearmint essence, sodium benzoate and purified water. The silanized bioactive glass with the calcium phosphate layer attached to the surface and the carboxylated hydroxyapatite are introduced, so that the silanized bioactive glass with the calcium phosphate layer attached to the surface is obtained, a mineralization reaction in saliva is promoted, and the surface of teeth is helped to be re-deposited to obtain a mineralized layer; on the basis, sodium pyrophosphate is combined to synergistically form a physical composite closed structure in a dentin tubule to block stimulation conduction, so that tooth sensitivity is reduced.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of daily necessities, and relates to a long-acting anti-sensitive medical tooth desensitizing paste and a preparation method thereof. BACKGROUND

[0002] Tooth sensitivity, also known as dentin hypersensitivity, is a common oral problem, which is manifested as short-term and sharp pain of teeth when subjected to cold, heat, acid, sweet or mechanical stimulation, and the root cause is that dentin tubules are exposed, so that external stimulation can directly act on the pulp nerve, and typical symptoms include short-term stinging when drinking ice water, eating sweets or brushing teeth, and in severe cases, it can even affect normal diet and oral hygiene maintenance, and due to its high recurrence and universality, in addition to clinical treatment, daily care products such as desensitizing toothpaste become the most commonly used solution. SUMMARY

[0003] The application aims to provide a long-acting anti-sensitive medical tooth desensitizing paste and a preparation method thereof, and the medical tooth desensitizing paste prepared by the application has the synergistic effect of various components and has long-acting anti-sensitive efficacy.

[0004] The object of the application can be achieved by the following technical solutions. A long-acting anti-sensitive medical tooth desensitizing paste, raw materials of the medical tooth desensitizing paste comprise, by weight fraction, 0.1-0.3 parts of bioactive glass, 9-11 parts of glycerol, 4.5-5.5 parts of polyethylene glycol, 44-46 parts of sorbitol, 0.2-0.4 parts of sodium hydroxymethyl cellulose, 0.2-0.4 parts of xanthan gum, 2.3-2.7 parts of sodium dodecyl sulfate, 0.05-0.15 parts of calcium carbonate, 4.8-5.2 parts of hydroxyapatite, 13-17 parts of silicon dioxide, 0.2-0.4 parts of titanium dioxide, 0.2-0.4 parts of sodium saccharin, 0.04-0.06 parts of sodium pyrophosphate, 0.2-0.4 parts of N,2,3-trimethyl-2-isopropylbutyramide, 0.8-1.2 parts of spearmint essence, 0.18-0.22 parts of sodium benzoate and 13.5-15.5 parts of purified water.

[0005] Further, the bioactive glass is silanized bioactive glass with a surface-attached calcium phosphate layer, and a preparation method of the silanized bioactive glass with a surface-attached calcium phosphate layer comprises the following steps: X1, the bioactive glass is added into a coupling solution, stirred at 58-62 DEG C for 2-3 h, centrifuged, washed with anhydrous ethanol, and vacuum dried at 80 DEG C to obtain silanized bioactive glass; X2, the silanized bioactive glass is immersed in a calcium chloride solution for 8-12 min, taken out and immersed in a sodium phosphate dibasic solution for 8-12 min, taken out after repeating for multiple times, and placed at 36-38℃ for 24-36 h, and vacuum dried at 60℃ to obtain the silanized bioactive glass with a calcium phosphate layer attached to the surface.

[0006] Further, the mass ratio of the bioactive glass and the coupling solution in step X1 is 1:4.5-5.5; the coupling solution is obtained by compounding 1-2 wt% KH-550 and the rest of ethanol.

[0007] Further, the calcium chloride solution in step X2 is a 0.05-0.15 M calcium chloride solution with a pH of 7.2-7.6; and the sodium phosphate dibasic solution is a 0.05-0.15 M sodium phosphate dibasic solution.

[0008] Further, the hydroxyapatite is carboxylated hydroxyapatite, and the preparation method of the carboxylated hydroxyapatite comprises the following steps: Y1, the hydroxyapatite is dispersed in a citric acid solution, an ultrasonic frequency of 30-50 kHz and an ultrasonic power of 500-700 W are set, ultrasonic treatment is performed for 20-30 min, centrifugation is performed, washing is performed until neutral, and spray drying is performed to obtain the carboxylated hydroxyapatite.

[0009] Further, the mass ratio of the hydroxyapatite and the citric acid solution in step Y1 is 1:18-22; and the citric acid solution is a citric acid solution with a mass concentration of 4.5-5.5 wt%.

[0010] Further, the calcium carbonate and the silicon dioxide are sieved through a 400-mesh screen after ball milling.

[0011] Further, the preparation method of the long-acting anti-sensitive medical tooth desensitizing paste comprises the following steps: Z1, the stirring speed of the stirring equipment is set to 20-30 rpm; Z2, purified water, sorbitol, glycerol, polyethylene glycol, sodium saccharin, sodium benzoate and sodium pyrophosphate are sequentially added to the stirring equipment in proportion, and stirring is performed for 8-12 min to obtain material one; Z3, carboxymethyl cellulose sodium and xanthan gum are sequentially added to the material one, the temperature is increased to 80-90℃, and after uniform stirring, heat preservation is performed for 25-35 min to obtain material two; Z4, the temperature is decreased to 35-45℃, bioactive glass, hydroxyapatite, silicon dioxide, titanium dioxide, calcium carbonate, sodium dodecyl sulfate, N,2,3-trimethyl-2-isopropylbutyramide and spearmint flavor are sequentially added, and stirring is performed for 25-35 min.

[0012] The beneficial effects of the present application are: This invention provides a long-lasting anti-sensitivity medical tooth desensitizing paste, which incorporates silanized bioactive glass with a calcium phosphate layer on its surface and carboxylated hydroxyapatite. By silanizing the surface of the bioactive glass and combining it with calcium ions in a calcium chloride solution, a calcium-rich layer is formed. Subsequently, the calcium ions and hydrogen phosphate ions in disodium hydrogen phosphate mutually adsorb each other, promoting the formation of amorphous calcium phosphate precursors. Through multiple cycles of treatment, the layers are stacked through alternating ion adsorption. Finally, after standing and drying, a silanized bioactive glass with a calcium phosphate layer on its surface is obtained, which in turn promotes the mineralization reaction in saliva and helps to redeposit a mineralized layer on the tooth surface. By carboxylating hydroxyapatite, the negative charge on its surface is enhanced, increasing its binding capacity with calcium ions. This helps hydroxyapatite penetrate and fill the mineralized layer formed by silanized bioactive glass with a calcium phosphate layer attached to its surface, preventing the mineralized layer from easily falling off during tooth cleaning. Furthermore, sodium pyrophosphate is combined to synergistically form a physical composite sealing structure within the dentinal tubules, blocking stimulus transmission and thus reducing tooth sensitivity. In addition, this application reduces the particle size of silica and calcium carbonate through ball milling, minimizing wear on the mineralized layer caused by large particles, further improving the adhesion of the mineralized layer and achieving long-lasting anti-sensitivity effects. Detailed Implementation

[0013] To further illustrate the technical means and effects of the present invention in achieving its intended purpose, the following detailed description of the specific implementation methods, structures, features, and effects of the present invention, in conjunction with embodiments, is provided below.

[0014] In all embodiments and comparative examples of this invention, the bioactive glass (CAS No. 65997-18-4), calcium chloride, disodium hydrogen phosphate, hydroxyapatite (CAS No. 1306-06-5), and citric acid were purchased from Hubei Yamaide Biomedical Co., Ltd.; KH-550 was purchased from Wuhan Lingfan Technology Co., Ltd.

[0015] Example 1 A long-lasting anti-sensitivity medical tooth desensitizing paste, wherein the raw materials of the medical tooth desensitizing paste, by weight, include 0.1 parts bioactive glass, 9 parts glycerin, 4.5 parts polyethylene glycol, 44 parts sorbitol, 0.2 parts sodium carboxymethyl cellulose, 0.2 parts xanthan gum, 2.3 parts sodium dodecyl sulfate, 0.05 parts calcium carbonate, 4.8 parts hydroxyapatite, 13 parts silica, 0.2 parts titanium dioxide, 0.2 parts sodium saccharin, 0.04 parts sodium pyrophosphate, 0.2 parts N,2,3-trimethyl-2-isopropylbutyramide, 0.8 parts spearmint flavoring, 0.18 parts sodium benzoate, and 13.5 parts purified water.

[0016] The bioactive glass is a silanized bioactive glass with a calcium phosphate layer attached to its surface. The preparation method of the silanized bioactive glass with a calcium phosphate layer attached to its surface includes the following steps: X1. Add bioactive glass to the coupling solution, stir at 58°C for 2 hours, centrifuge, wash with anhydrous ethanol, and dry under vacuum at 80°C to obtain silanized bioactive glass. X2. Immerse the silanized bioactive glass in calcium chloride solution for 8 minutes, then remove it and immerse it in disodium hydrogen phosphate solution for 8 minutes. Repeat this process several times, then remove the glass and let it stand at 36°C for 24 hours. Finally, vacuum dry it at 60°C to obtain silanized bioactive glass with a calcium phosphate layer attached to its surface.

[0017] The mass ratio of the bioactive glass to the coupling solution in step X1 is 1:4.5; the coupling solution is prepared by mixing 1 wt% KH-550 and the remainder ethanol.

[0018] The calcium chloride solution mentioned in step X2 is a 0.05M calcium chloride solution with a pH of 7.2; the disodium hydrogen phosphate solution is a 0.05M disodium hydrogen phosphate solution.

[0019] The hydroxyapatite is carboxylated hydroxyapatite, and the preparation method of carboxylated hydroxyapatite includes the following steps: Y1. Disperse hydroxyapatite in citric acid solution, set the ultrasonic frequency to 30kHz and the ultrasonic power to 500W, sonicate for 20min, centrifuge, wash until neutral, spray dry to obtain carboxylated hydroxyapatite.

[0020] The mass ratio of hydroxyapatite to citric acid solution in step Y1 is 1:18; the citric acid solution is a citric acid solution with a mass concentration of 4.5 wt%.

[0021] The calcium carbonate and silicon dioxide were ball-milled and then passed through a 400-mesh sieve.

[0022] The preparation method of the long-acting anti-sensitivity medical dental desensitizing paste includes the following steps: Z1. Set the stirring speed of the mixing equipment to 20 rpm; Z2. Add purified water, sorbitol, glycerol, polyethylene glycol, sodium saccharin, sodium benzoate, and sodium pyrophosphate into the mixing equipment in proportion and stir for 8 minutes to obtain material one. Z3. Add sodium carboxymethyl cellulose and xanthan gum to material one in sequence, heat to 80°C, stir evenly and keep warm for 25 minutes to obtain material two. Z4. Cool to 35℃, then add bioactive glass, hydroxyapatite, silicon dioxide, titanium dioxide, calcium carbonate, sodium dodecyl sulfate, N,2,3-trimethyl-2-isopropylbutyramide, and spearmint flavoring in sequence. Stir for 25 minutes to obtain the final product.

[0023] Example 2 A long-lasting anti-sensitivity medical tooth desensitizing paste, wherein the raw materials of the medical tooth desensitizing paste, by weight, include 0.15 parts bioactive glass, 9.6 parts glycerin, 4.8 parts polyethylene glycol, 44.7 parts sorbitol, 0.25 parts sodium carboxymethyl cellulose, 0.25 parts xanthan gum, 2.4 parts sodium dodecyl sulfate, 0.08 parts calcium carbonate, 4.9 parts hydroxyapatite, 14 parts silica, 0.25 parts titanium dioxide, 0.25 parts sodium saccharin, 0.04 parts sodium pyrophosphate, 0.25 parts N,2,3-trimethyl-2-isopropylbutyramide, 0.9 parts spearmint flavor, 0.19 parts sodium benzoate, and 13.8 parts purified water.

[0024] The bioactive glass is a silanized bioactive glass with a calcium phosphate layer attached to its surface. The preparation method of the silanized bioactive glass with a calcium phosphate layer attached to its surface includes the following steps: X1. Add bioactive glass to the coupling solution, stir at 58°C for 2.3 h, centrifuge, wash with anhydrous ethanol, and dry under vacuum at 80°C to obtain silanized bioactive glass. X2. Immerse the silanized bioactive glass in calcium chloride solution for 9 minutes, then immerse it in disodium hydrogen phosphate solution for 9 minutes. Repeat this process several times. After immersion, remove the glass and let it stand at 36°C for 27 hours. Then, vacuum dry it at 60°C to obtain silanized bioactive glass with a calcium phosphate layer attached to its surface.

[0025] The mass ratio of the bioactive glass to the coupling solution in step X1 is 1:4.8; the coupling solution is prepared by mixing 1.2 wt% KH-550 and the balance ethanol.

[0026] The calcium chloride solution mentioned in step X2 is a 0.08M calcium chloride solution with a pH of 7.2; the disodium hydrogen phosphate solution is a 0.08M disodium hydrogen phosphate solution.

[0027] The hydroxyapatite is carboxylated hydroxyapatite, and the preparation method of carboxylated hydroxyapatite includes the following steps: Y1. Disperse hydroxyapatite in citric acid solution, set the ultrasonic frequency to 30kHz and the ultrasonic power to 500W, sonicate for 24min, centrifuge, wash until neutral, spray dry to obtain carboxylated hydroxyapatite.

[0028] The mass ratio of hydroxyapatite to citric acid solution in step Y1 is 1:19; the citric acid solution is a citric acid solution with a mass concentration of 4.8 wt%.

[0029] The calcium carbonate and silicon dioxide were ball-milled and then passed through a 400-mesh sieve.

[0030] The preparation method of the long-acting anti-sensitivity medical dental desensitizing paste includes the following steps: Z1. Set the stirring speed of the mixing equipment to 20 rpm; Z2. Add purified water, sorbitol, glycerol, polyethylene glycol, sodium saccharin, sodium benzoate, and sodium pyrophosphate into the mixing equipment in proportion and stir for 8 minutes to obtain material one. Z3. Add sodium carboxymethyl cellulose and xanthan gum to material one in sequence, heat to 80°C, stir evenly and keep warm for 25 minutes to obtain material two. Z4. Cool to 35℃, then add bioactive glass, hydroxyapatite, silicon dioxide, titanium dioxide, calcium carbonate, sodium dodecyl sulfate, N,2,3-trimethyl-2-isopropylbutyramide, and spearmint flavoring in sequence. Stir for 25 minutes to obtain the final product.

[0031] Example 3 A long-lasting anti-sensitivity medical tooth desensitizing paste, wherein the raw materials of the medical tooth desensitizing paste, by weight, include 0.2 parts bioactive glass, 10 parts glycerin, 5 parts polyethylene glycol, 45 parts sorbitol, 0.3 parts sodium carboxymethyl cellulose, 0.3 parts xanthan gum, 2.5 parts sodium dodecyl sulfate, 0.1 parts calcium carbonate, 5 parts hydroxyapatite, 15 parts silica, 0.3 parts titanium dioxide, 0.3 parts sodium saccharin, 0.05 parts sodium pyrophosphate, 0.3 parts N,2,3-trimethyl-2-isopropylbutyramide, 1 part spearmint flavoring, 0.2 parts sodium benzoate, and 14.5 parts purified water.

[0032] The bioactive glass is a silanized bioactive glass with a calcium phosphate layer attached to its surface. The preparation method of the silanized bioactive glass with a calcium phosphate layer attached to its surface includes the following steps: X1. Add bioactive glass to the coupling solution, stir at 60°C for 2.5 h, centrifuge, wash with anhydrous ethanol, and dry under vacuum at 80°C to obtain silanized bioactive glass. X2. Immerse the silanized bioactive glass in calcium chloride solution for 10 min, then remove it and immerse it in disodium hydrogen phosphate solution for 10 min. Repeat this process several times, then remove the glass and let it stand at 37°C for 30 h. Finally, vacuum dry it at 60°C to obtain silanized bioactive glass with a calcium phosphate layer attached to its surface.

[0033] The mass ratio of the bioactive glass and the coupling solution in step X1 is 1:5; the coupling solution is prepared by mixing 1.5wt% KH-550 and the remainder ethanol.

[0034] The calcium chloride solution mentioned in step X2 is a 0.1M calcium chloride solution with a pH of 7.4; the disodium hydrogen phosphate solution is a 0.1M disodium hydrogen phosphate solution.

[0035] The hydroxyapatite is carboxylated hydroxyapatite, and the preparation method of carboxylated hydroxyapatite includes the following steps: Y1. Disperse hydroxyapatite in citric acid solution, set the ultrasonic frequency to 40kHz and the ultrasonic power to 600W, sonicate for 25min, centrifuge, wash until neutral, spray dry to obtain carboxylated hydroxyapatite.

[0036] The mass ratio of hydroxyapatite to citric acid solution in step Y1 is 1:20; the citric acid solution is a citric acid solution with a mass concentration of 5wt%.

[0037] The calcium carbonate and silicon dioxide were ball-milled and then passed through a 400-mesh sieve.

[0038] The preparation method of the long-acting anti-sensitivity medical dental desensitizing paste includes the following steps: Z1. Set the stirring speed of the mixing equipment to 25 rpm; Z2. Add purified water, sorbitol, glycerin, polyethylene glycol, sodium saccharin, sodium benzoate, and sodium pyrophosphate into the mixing equipment in proportion and stir for 10 minutes to obtain material one. Z3. Add sodium carboxymethyl cellulose and xanthan gum to material one in sequence, heat to 85°C, stir evenly and keep warm for 30 minutes to obtain material two. Z4. Cool to 40℃, then add bioactive glass, hydroxyapatite, silicon dioxide, titanium dioxide, calcium carbonate, sodium dodecyl sulfate, N,2,3-trimethyl-2-isopropylbutyramide, and spearmint flavoring in sequence. Stir for 30 minutes to obtain the final product.

[0039] Example 4 A long-lasting anti-sensitivity medical tooth desensitizing paste, wherein the raw materials of the medical tooth desensitizing paste, by weight, include 0.25 parts bioactive glass, 10.4 parts glycerin, 5.3 parts polyethylene glycol, 45.3 parts sorbitol, 0.35 parts sodium carboxymethyl cellulose, 0.35 parts xanthan gum, 2.6 parts sodium dodecyl sulfate, 0.12 parts calcium carbonate, 5.1 parts hydroxyapatite, 16 parts silica, 0.35 parts titanium dioxide, 0.35 parts sodium saccharin, 0.06 parts sodium pyrophosphate, 0.35 parts N,2,3-trimethyl-2-isopropylbutyramide, 1.1 parts spearmint flavor, 0.21 parts sodium benzoate, and 15.1 parts purified water.

[0040] The bioactive glass is a silanized bioactive glass with a calcium phosphate layer attached to its surface. The preparation method of the silanized bioactive glass with a calcium phosphate layer attached to its surface includes the following steps: X1. Add bioactive glass to the coupling solution, stir at 62°C for 2.8 h, centrifuge, wash with anhydrous ethanol, and dry under vacuum at 80°C to obtain silanized bioactive glass. X2. Immerse the silanized bioactive glass in calcium chloride solution for 11 min, then remove it and immerse it in disodium hydrogen phosphate solution for 11 min. Repeat this process several times, then remove the glass and let it stand at 38°C for 32 h. Finally, vacuum dry it at 60°C to obtain silanized bioactive glass with a calcium phosphate layer attached to its surface.

[0041] The mass ratio of the bioactive glass to the coupling solution in step X1 is 1:5.3; the coupling solution is prepared by mixing 1.7wt% KH-550 and the balance ethanol.

[0042] The calcium chloride solution mentioned in step X2 is a 0.012M calcium chloride solution with a pH of 7.6; the disodium hydrogen phosphate solution is a 0.12M disodium hydrogen phosphate solution.

[0043] The hydroxyapatite is carboxylated hydroxyapatite, and the preparation method of carboxylated hydroxyapatite includes the following steps: Y1. Disperse hydroxyapatite in citric acid solution, set the ultrasonic frequency to 50kHz and the ultrasonic power to 700W, sonicate for 28min, centrifuge, wash until neutral, spray dry to obtain carboxylated hydroxyapatite.

[0044] The mass ratio of hydroxyapatite to citric acid solution in step Y1 is 1:21; the citric acid solution is a citric acid solution with a mass concentration of 5.2 wt%.

[0045] The calcium carbonate and silicon dioxide were ball-milled and then passed through a 400-mesh sieve.

[0046] The preparation method of the long-acting anti-sensitivity medical dental desensitizing paste includes the following steps: Z1. Set the stirring speed of the mixing equipment to 30 rpm; Z2. Add purified water, sorbitol, glycerol, polyethylene glycol, sodium saccharin, sodium benzoate, and sodium pyrophosphate into the mixing equipment in proportion and stir for 12 minutes to obtain material one. Z3. Add sodium carboxymethyl cellulose and xanthan gum to material one in sequence, heat to 90°C, stir evenly and keep warm for 35 minutes to obtain material two. Z4. Cool to 45℃, then add bioactive glass, hydroxyapatite, silicon dioxide, titanium dioxide, calcium carbonate, sodium dodecyl sulfate, N,2,3-trimethyl-2-isopropylbutyramide, and spearmint flavoring in sequence. Stir for 35 minutes to obtain the final product.

[0047] Example 5 A long-lasting anti-sensitivity medical tooth desensitizing paste, wherein the raw materials of the medical tooth desensitizing paste, by weight, include 0.3 parts bioactive glass, 11 parts glycerin, 5.5 parts polyethylene glycol, 46 parts sorbitol, 0.4 parts sodium carboxymethyl cellulose, 0.4 parts xanthan gum, 2.7 parts sodium dodecyl sulfate, 0.15 parts calcium carbonate, 5.2 parts hydroxyapatite, 17 parts silica, 0.4 parts titanium dioxide, 0.4 parts sodium saccharin, 0.06 parts sodium pyrophosphate, 0.4 parts N,2,3-trimethyl-2-isopropylbutyramide, 1.2 parts spearmint flavoring, 0.22 parts sodium benzoate, and 15.5 parts purified water.

[0048] The bioactive glass is a silanized bioactive glass with a calcium phosphate layer attached to its surface. The preparation method of the silanized bioactive glass with a calcium phosphate layer attached to its surface includes the following steps: X1. Add bioactive glass to the coupling solution, stir at 62℃ for 3h, centrifuge, wash with anhydrous ethanol, and dry under vacuum at 80℃ to obtain silanized bioactive glass. X2. Immerse the silanized bioactive glass in calcium chloride solution for 12 min, then remove it and immerse it in disodium hydrogen phosphate solution for 12 min. Repeat this process several times, then remove the glass and let it stand at 38°C for 36 h. Finally, vacuum dry it at 60°C to obtain silanized bioactive glass with a calcium phosphate layer attached to its surface.

[0049] The mass ratio of the bioactive glass to the coupling solution in step X1 is 1:5.5; the coupling solution is prepared by mixing 2wt% KH-550 and the remainder ethanol.

[0050] The calcium chloride solution mentioned in step X2 is a 0.15M calcium chloride solution with a pH of 7.6; the disodium hydrogen phosphate solution is a 0.15M disodium hydrogen phosphate solution.

[0051] The hydroxyapatite is carboxylated hydroxyapatite, and the preparation method of carboxylated hydroxyapatite includes the following steps: Y1. Disperse hydroxyapatite in citric acid solution, set the ultrasonic frequency to 50kHz and the ultrasonic power to 700W, sonicate for 30min, centrifuge, wash until neutral, spray dry to obtain carboxylated hydroxyapatite.

[0052] The mass ratio of hydroxyapatite to citric acid solution in step Y1 is 1:22; the citric acid solution is a citric acid solution with a mass concentration of 5.5 wt%.

[0053] The calcium carbonate and silicon dioxide were ball-milled and then passed through a 400-mesh sieve.

[0054] The preparation method of the long-acting anti-sensitivity medical dental desensitizing paste includes the following steps: Z1. Set the stirring speed of the mixing equipment to 30 rpm; Z2. Add purified water, sorbitol, glycerol, polyethylene glycol, sodium saccharin, sodium benzoate, and sodium pyrophosphate into the mixing equipment in proportion and stir for 12 minutes to obtain material one. Z3. Add sodium carboxymethyl cellulose and xanthan gum to material one in sequence, heat to 90°C, stir evenly and keep warm for 35 minutes to obtain material two. Z4. Cool to 45℃, then add bioactive glass, hydroxyapatite, silicon dioxide, titanium dioxide, calcium carbonate, sodium dodecyl sulfate, N,2,3-trimethyl-2-isopropylbutyramide, and spearmint flavoring in sequence. Stir for 35 minutes to obtain the final product.

[0055] Example 6 Based on Example 3, the silanized bioactive glass with the calcium phosphate layer attached to its surface was removed and replaced with an equal weight of bioactive glass, while other conditions remained the same as in Example 3.

[0056] Example 7 Based on Example 3, the carboxylated hydroxyapatite was removed and replaced with an equal weight of hydroxyapatite, while other conditions remained the same as in Example 3.

[0057] Example 8 Based on Example 3, the silanized bioactive glass and carboxylated hydroxyapatite with the calcium phosphate layer attached to the surface were removed and replaced with bioactive glass and hydroxyapatite of equal weight, while other conditions remained the same as in Example 3.

[0058] Comparative Example 1 Based on Example 3, while keeping other conditions consistent, the preparation method of bioactive glass was changed to the following steps: X1. Add bioactive glass to the coupling solution, stir at 58°C for 2.3 h, centrifuge, wash with anhydrous ethanol, and dry under vacuum at 80°C to obtain bioactive glass.

[0059] Comparative Example 2 Based on Example 3, while keeping other conditions consistent, the preparation method of bioactive glass was changed to the following steps: X1. Immerse the bioactive glass in calcium chloride solution for 9 minutes, then immerse it in disodium hydrogen phosphate solution for 9 minutes. Repeat this process several times. After immersion, remove the glass and let it stand at 37°C for 27 hours. Then, vacuum dry it at 60°C to obtain the bioactive glass.

[0060] Comparative Example 3 Based on Example 3, while keeping other conditions the same, calcium carbonate and silicon dioxide were ball-milled and then passed through a 200-mesh sieve.

[0061] Comparative Example 4 Based on Example 3, while keeping other conditions the same, the calcium carbonate and silicon dioxide were not ball-milled.

[0062] Using the medical tooth desensitizing pastes prepared in Examples 1-8 and Comparative Examples 1-4 as samples, 60 volunteers with tooth sensitivity were selected, half male and half female, aged 20-50 years, and randomly divided into 12 groups. They used the samples to brush their teeth once in the morning and once in the evening, and each brushing lasted for 2 minutes. After 2 months of continuous use, the tooth sensitivity before use and the tooth sensitivity after 2 months of use were tested with probe sensitivity. The scores were scored after the test, and the average scores were recorded as shown in Table 1 below. The probe sensitivity test method is as follows: an electronic pressure-sensitive probe is used to test the tooth sensitivity index. The probe contacts the exposed dentin on the buccal surface of the selected tooth and is placed at the enamel-dentin junction. The contact force of the probe is set to 50g. The scoring criteria for probe sensitivity testing are 0-3 points, where 0 indicates no pain upon probe contact, 1 indicates slight discomfort upon probe contact with minimal pain, 2 indicates pain upon probe contact with tolerable pain, and 3 indicates severe pain upon probe contact with intolerable pain.

[0063] As shown in Table 1, the long-lasting anti-sensitivity medical tooth desensitizing paste prepared by the present invention can significantly improve tooth sensitivity after use and has a good anti-sensitivity effect.

[0064] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any indirect modifications, equivalent changes, and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A long-lasting, desensitizing medical tooth desensitizing paste, characterized in that: The raw materials of the medical dental desensitizing paste, by weight, include 0.1-0.3 parts bioactive glass, 9-11 parts glycerin, 4.5-5.5 parts polyethylene glycol, 44-46 parts sorbitol, 0.2-0.4 parts sodium carboxymethyl cellulose, 0.2-0.4 parts xanthan gum, 2.3-2.7 parts sodium dodecyl sulfate, 0.05-0.15 parts calcium carbonate, 4.8-5.2 parts hydroxyapatite, 13-17 parts silica, 0.2-0.4 parts titanium dioxide, 0.2-0.4 parts sodium saccharin, 0.04-0.06 parts sodium pyrophosphate, 0.2-0.4 parts N,2,3-trimethyl-2-isopropylbutyramide, 0.8-1.2 parts spearmint flavor, 0.18-0.22 parts sodium benzoate, and 13.5-15.5 parts purified water.

2. The long-lasting desensitizing medical toothpaste according to claim 1, characterized in that: The bioactive glass is a silanized bioactive glass with a calcium phosphate layer attached to its surface. The preparation method of the silanized bioactive glass with a calcium phosphate layer attached to its surface includes the following steps: X1. Add bioactive glass to the coupling solution, stir at 58-62℃ for 2-3 hours, centrifuge, wash with anhydrous ethanol, and dry under vacuum at 80℃ to obtain silanized bioactive glass. X2. Immerse the silanized bioactive glass in a calcium chloride solution for 8-12 minutes, then remove it and immerse it in a disodium hydrogen phosphate solution for 8-12 minutes. Repeat this process several times. After removing the glass, let it stand at 36-38℃ for 24-36 hours and then vacuum dry it at 60℃ to obtain silanized bioactive glass with a calcium phosphate layer attached to its surface.

3. The long-lasting desensitizing medical tooth desensitizing paste according to claim 2, characterized in that: The mass ratio of the bioactive glass to the coupling solution in step X1 is 1:4.5-5.5; the coupling solution is prepared by mixing 1-2 wt% KH-550 and the balance ethanol.

4. The long-lasting desensitizing medical tooth desensitizing paste according to claim 2, characterized in that: The calcium chloride solution in step X2 is a 0.05-0.15M calcium chloride solution with a pH of 7.2-7.6; the disodium hydrogen phosphate solution is a 0.05-0.15M disodium hydrogen phosphate solution.

5. The long-lasting desensitizing medical tooth desensitizing paste according to claim 1, characterized in that: The hydroxyapatite is carboxylated hydroxyapatite, and the preparation method of the carboxylated hydroxyapatite includes the following steps: Y1. Disperse hydroxyapatite in citric acid solution, set the ultrasonic frequency to 30-50kHz and the ultrasonic power to 500-700W, sonicate for 20-30min, centrifuge, wash until neutral, spray dry to obtain carboxylated hydroxyapatite.

6. The long-lasting desensitizing medical toothpaste according to claim 5, characterized in that: In step Y1, the mass ratio of hydroxyapatite to citric acid solution is 1:18-22; the citric acid solution is a citric acid solution with a mass concentration of 4.5-5.5 wt%.

7. The long-lasting desensitizing medical tooth desensitizing paste according to claim 1, characterized in that: The calcium carbonate and silicon dioxide were ball-milled and then passed through a 400-mesh sieve.

8. A method for preparing a long-acting desensitizing medical toothpaste as described in any one of claims 1-7, characterized in that: The preparation method of the long-acting anti-sensitivity medical dental desensitizing paste includes the following steps: Z1. Set the stirring speed of the mixing equipment to 20-30 rpm; Z2. Add purified water, sorbitol, glycerin, polyethylene glycol, sodium saccharin, sodium benzoate, and sodium pyrophosphate into the mixing equipment in the following proportions, and stir for 8-12 minutes to obtain material one; Z3. Add sodium carboxymethyl cellulose and xanthan gum to material one in sequence, heat to 80-90℃, stir evenly, and keep warm for 25-35 minutes to obtain material two. Z4. Cool to 35-45℃, then add bioactive glass, hydroxyapatite, silicon dioxide, titanium dioxide, calcium carbonate, sodium dodecyl sulfate, N,2,3-trimethyl-2-isopropylbutyramide, and spearmint flavoring in sequence. Stir for 25-35 minutes to obtain the final product.

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