CN117771271A

CN117771271A - Quick-acting visual tooth desensitizer and preparation method thereof

Info

Publication number: CN117771271A
Application number: CN202410204783.9A
Authority: CN
Inventors: 徐延; 刘美霞; 周林曦; 孙浩; 张桂荣; 阎旭; 刘文彬; 吴嘉锜; 丛芳; 王逸琳; 郭恒; 徐浩楠; 赵娜
Original assignee: Shenyang Hengyuan Pharmaceutical Co ltd; Shenyang Stomatological Hospital; Institute of Metal Research of CAS
Current assignee: Shenyang Hengyuan Pharmaceutical Co ltd; Shenyang Stomatological Hospital; Institute of Metal Research of CAS
Priority date: 2024-02-26
Filing date: 2024-02-26
Publication date: 2024-03-29
Anticipated expiration: 2044-02-26
Also published as: CN117771271B

Abstract

The invention provides a quick-acting visual tooth desensitizer and a preparation method thereof. A quick-acting visual tooth desensitizer consists of the following components in percentage by weight: 0.5 to 10 percent of dyed selenium-containing bioactive glass, 3 to 40 percent of glycerol, 0.5 to 10 percent of silicon dioxide, 0.2 to 10 percent of mixture of carboxymethyl cellulose and xanthan gum, 0.2 to 7 percent of cocamidopropyl betaine, 10 to 40 percent of polyethylene glycol, 0.1 to 10 percent of xylitol or sorbitol, 0.01 to 2 percent of essence and the balance of purified water. The invention also provides a preparation method of the quick-acting visual tooth desensitizer. The visual tooth desensitizer adopts modified dyed selenium-containing bioactive glass, improves the sealing rate of dental tubules, has better visual effect and remineralization effect, has excellent biocompatibility and antibacterial effect, prevents early caries, can promote the growth of epidermal cells, repairs the wound surface of dental ulcer, and is safe to use without adding fluorine and strontium.

Description

Quick-acting visual tooth desensitizer and preparation method thereof

Technical Field

The invention relates to the technical field of tooth desensitizers, in particular to a quick-acting visual tooth desensitizer and a preparation method thereof.

Background

Tooth desensitizers are used to alleviate tooth sensitivity symptoms caused by dentinal exposure. Tooth desensitizers can be classified into three categories according to their mechanism of action: inorganic filler/remineralizing type, collagen denaturation blocking type, and film blocking type. However, in practical use, existing tooth desensitizers suffer from the following disadvantages:

(1) The existing potassium salt desensitizing method commonly used for the tooth desensitizing agent can take effect after 3-5 days, and the acting time is longer;

(2) Fluorine (sodium fluoride) and strontium are often added into the existing tooth desensitizer, the fluorine has a certain influence on the pine cone of a human body, and the strontium has an influence on the kidneys of children, so that certain potential safety hazards exist in using the desensitizer;

(3) The existing tooth desensitizer contains hydroxyapatite and is mainly used for remineralizing (reconstructing) tooth structures and repairing tooth enamel. However, the mineralization effect is short because the mineralization agent is easy to fall off after remineralization;

(4) The coverage of the existing tooth desensitizer on the tooth surface can not be quantified. In the use process of a patient, it is difficult to ensure that the desensitizer can uniformly cover each sensitive area, so that a better desensitizing effect is achieved.

Disclosure of Invention

In order to solve the technical problems, the invention aims to provide a quick-acting visualized tooth desensitizer and a preparation method thereof.

The above object of the present invention is achieved by the following technical solutions: a quick-acting visual tooth desensitizer consists of the following components in percentage by weight: 0.5 to 10 percent of dyed selenium-containing bioactive glass, 3 to 40 percent of glycerol, 0.5 to 10 percent of silicon dioxide, 0.2 to 10 percent of mixture of carboxymethyl cellulose and xanthan gum, 0.2 to 7 percent of cocamidopropyl betaine, 10 to 40 percent of polyethylene glycol, 0.1 to 10 percent of xylitol or sorbitol, 0.01 to 2 percent of essence and the balance of purified water.

Further, the rapid-acting visual tooth desensitizer consists of the following components in percentage by weight: 0.5% of dyed selenium-containing bioactive glass, 3% of glycerol, 0.5% of silicon dioxide, 0.2% of a mixture of carboxymethyl cellulose and xanthan gum, 0.2% of cocamidopropyl betaine, 10% of polyethylene glycol, 0.1% of xylitol or sorbitol, 0.01% of essence and the balance of purified water.

Further, the rapid-acting visual tooth desensitizer consists of the following components in percentage by weight: 10% of dyed selenium-containing bioactive glass, 20% of glycerol, 10% of silicon dioxide, 5% of carboxymethyl cellulose and xanthan gum mixture, 7% of cocamidopropyl betaine, 20% of polyethylene glycol, 10% of xylitol or sorbitol, 2% of essence and the balance of purified water.

Further, the rapid-acting visual tooth desensitizer consists of the following components in percentage by weight: 10% of dyed selenium-containing bioactive glass, 15% of glycerol, 5% of silicon dioxide, 10% of a mixture of carboxymethyl cellulose and xanthan gum, 1% of cocamidopropyl betaine, 40% of polyethylene glycol, 20% of xylitol or sorbitol, 0.1% of essence and the balance of purified water.

Further, the rapid-acting visual tooth desensitizer consists of the following components in percentage by weight: 6% of dyed selenium-containing bioactive glass, 40% of glycerol, 2% of silicon dioxide, 2% of a mixture of carboxymethyl cellulose and xanthan gum, 1% of cocamidopropyl betaine, 20% of polyethylene glycol, 1% of xylitol or sorbitol, 1% of essence and the balance of purified water.

Further, in the mixture of carboxymethyl cellulose and xanthan gum, the weight ratio of the carboxymethyl cellulose to the xanthan gum is 4:1.

further, the dyed selenium-containing bioactive glass is prepared by the following preparation method:

(1) Preparing an inorganic solution: siO is made of ₂ 、Na ₂ O、CaO、MgO、P ₂ O ₅ Mixing according to the weight percentages of 33%, 1%, 44%, 4.5% and 17.5% respectively to form an inorganic mixture, and adding the inorganic mixture into a tetrahydrate calcium nitrate aqueous solution to prepare an inorganic solution, wherein the mass ratio of the inorganic mixture to the tetrahydrate calcium nitrate aqueous solution is 1:3, the tetrahydrate calcium nitrate aqueous solution is a mixed solution of tetrahydrate calcium nitrate and water, and the molar ratio of water to tetrahydrate calcium nitrate is 6:1;

(2) Preparing an ethyl orthosilicate-ethanol organic solution: dissolving Tetraethoxysilane (TEOS) in absolute ethyl alcohol to prepare a solution with the concentration of 1.0 mol/L;

(3) Preparing sol: adding the inorganic solution prepared in the step (1) into the ethyl orthosilicate-ethanol organic solution prepared in the step (2), stirring while adding, dropwise adding 2mol/L nitric acid as a catalyst, dropwise adding until the pH of the solution is 2-4, and stirring for 50min to obtain sol;

(4) Preparation of xerogel: removing ethanol and water in the sol obtained in the step (3), and aging for 48 hours to obtain xerogel;

(5) Preparing bioactive glass powder: calcining the xerogel obtained in the step (4) at 700-800 ℃ for 2 hours, and sieving and purifying to obtain bioactive glass powder, wherein the particle size of the bioactive glass powder is 50 mu m;

(6) Preparing a test solution A: mixing the bioactive glass powder obtained in the step (5) with polyethylene glycol according to the weight ratio of 3:2, and adding purified water which is 2 times of the total weight of the bioactive glass powder and the polyethylene glycol to prepare a test solution A;

(7) Preparing a test solution B: tween-80 and Na ₂ SeO ₃ Mixing, emulsifying for 40 min to obtain test solution B; wherein Tween-80 and Na ₂ SeO ₃ The weight ratio of (2) is 200:1;

(8) Preparing a biological staining gel: biological staining gel The composite material consists of the following components in percentage by weight: acetic acid 2%, phycoerythrin B1.0%, sodium persulfate 0.5%, sodium alginate 1.6%, caCl ₂ 1.6% of purified water 93.3%;

the preparation method specifically comprises the following steps: taking the components in the proportion, firstly, respectively fully dissolving acetic acid, phycoerythrin B, sodium persulfate and purified water according to the weight percentage, standing for precipitation, and taking supernatant; then the supernatant is mixed with sodium alginate and CaCl ₂ Fully mixing, standing for 6 hours, and taking precipitated gel for standby, thus obtaining the biological staining gel;

(9) Preparing dyed selenium-containing bioactive glass: slowly adding the test solution A obtained in the step (6) into the test solution B obtained in the step (7), wherein the weight ratio of the test solution A to the test solution B is 1:1, obtaining a mixed solution, adding the biological dyeing gel obtained in the step (8) into the mixed solution, stirring for 2 hours, wherein the addition amount of the biological dyeing gel is 1% -5% of the total weight of the mixed solution, then adding glacial acetic acid serving as a catalyst, wherein the addition amount of the glacial acetic acid is 1.9% of the total weight of the mixed solution, continuing stirring for 1 hour, filtering, washing with absolute ethyl alcohol until oil is free, and drying to obtain the dyed selenium-containing bioactive glass.

Further, the xerogel is prepared in the step (4) by removing ethanol and water in the sol under the vacuum condition at 50-80 ℃.

Further, in the step (9), the drying is carried out for 24 hours at 50-80 ℃.

The invention also provides a preparation method of the visualized tooth desensitizer with rapid effect, which comprises the following steps:

s1, preparing dyed selenium-containing bioactive glass microcapsules: taking a mixture of carboxymethyl cellulose and xanthan gum and a part of polyethylene glycol as wall materials, wherein the weight ratio of the mixture to the xanthan gum is 10:3.5, using the dyed selenium-containing bioactive glass and glycerin as core materials, and using a high-pressure microcapsule embedding method to manufacture dyed selenium-containing bioactive glass microcapsules; the weight of the mixture of the carboxymethyl cellulose and the xanthan gum is 25 percent of the weight of the dyed selenium-containing bioactive glass, and the weight of the polyethylene glycol is 8 times of the weight of the mixture of the carboxymethyl cellulose and the xanthan gum;

s2, preparing an aqueous phase: uniformly mixing silicon dioxide, the rest mixture of carboxymethyl cellulose and xanthan gum and xylitol in the formula amount, adding purified water, stirring for 0.5 hour under the condition of the rotating speed of 60r/min, and obtaining a water phase after the mixture of carboxymethyl cellulose and xanthan gum is completely dissolved for later use;

s3, preparing an oil phase: stirring cocoamidopropyl betaine, the other part of polyethylene glycol, essence and the rest of glycerol for 0.5 hours under the conditions that the vacuum degree is more than or equal to 0.06MPa and the rotating speed is 60r/min until the mixture is uniform to obtain an oil phase for later use; the weight ratio of polyethylene glycol to cocamidopropyl betaine is 1:1;

S4, mixing and emulsifying: mixing and emulsifying the dyed selenium-containing bioactive glass microcapsule obtained in the step S1, the water phase obtained in the step S2, the oil phase obtained in the step S3 and the rest polyethylene glycol for 2 hours until uniformity, and obtaining the visual tooth desensitizer.

The invention has the beneficial effects that:

1. the visual tooth desensitizer adopts modified dyed selenium-containing bioactive glass, can react with saliva rapidly, continuously hydrolyzes calcium ions and phosphate ions, simultaneously releases a large amount of hydroxide ions, increases the pH value in a local environment to 8-10, further promotes calcium and phosphorus plasma to deposit on the tooth surface, is adsorbed on the tooth surface, forms calcium and phosphorus compound, simultaneously forms a silica-rich gel layer, and aggregates to form a hydroxyapatite layer similar to dental bone tissue, finally forms a stable crystalline hydroxyapatite layer in enamel defect, sensitive area or dentin tubule, improves the sealing rate of the tubule, and seals the tubule to achieve desensitization effect.

2. The addition of the dyed selenium-containing bioactive glass enhances the effect of the dyed selenium-containing bioactive glass on gram-positive bacteria in an alkaline environment, and the adhesion between the dyed selenium-containing bioactive glass and protein and soft tissues is poor, so that the defect of overlarge dyeing range in the color development process is overcome, and the tooth desensitizer has a good visual effect.

3. The preparation process of the visualized tooth desensitizer adopts a microcapsule wrapping process, delays the release of ions after the dyed selenium-containing bioactive glass reacts with purified water in a formula, and avoids weakening and remineralizing effects.

4. The invention adopts the dyed selenium-containing bioactive glass, can efficiently remove dental plaque, simultaneously improves the contact area of the desensitizer and the dental plaque, reduces the influence of the occupation of the dental plaque on the mineralization effect, accelerates the remineralization time, optimizes the mineralization effect and achieves better desensitization effect.

5. The selenium element in the dyed selenium-containing bioactive glass can increase the antibacterial property of the bioactive glass, promote the proliferation and migration of epidermal cells, promote the proliferation of fibroblasts, and the dyed selenium-containing bioactive glass has excellent biocompatibility and antibacterial (streptococcus mutans) effect, prevents early caries, can promote the growth of the epidermal cells, and can repair the wound surface of dental ulcer.

6. The visual tooth desensitizer disclosed by the invention is free from adding fluorine and strontium, does not bring potential safety hazards to human pine cone bodies and kidneys of children, and is safe to use.

Drawings

FIG. 1 is a diagram of a white light interference microscope in the surface detection of remineralized isolated dental samples;

FIG. 2 is a view of SEM scanning electron microscope in surface detection of remineralized isolated tooth samples;

FIG. 3 is a graph of the detection result of the inhibition zone in the evaluation of the inhibition effect;

FIG. 4 is a graph showing the detection result of the antibacterial effect by the direct contact method in the evaluation of the antibacterial effect;

FIG. 5 is a scan of a confocal laser scanning microscope for biofilm observation in the evaluation of bacteriostatic effects;

FIG. 6 is a graph showing the comparison of stained and removed sensitive teeth of a user of a visual dental desensitizing agent prepared according to the second embodiment of the present invention;

FIG. 7 is a graph showing the comparison of stained and removed sensitive teeth of a user of a visual dental desensitizing agent prepared according to example two of the present invention.

Detailed Description

The details of the invention and its embodiments are further described below with reference to the accompanying drawings and examples.

A quick-acting visual tooth desensitizer consists of the following components in percentage by weight: 0.5 to 10 percent of dyed selenium-containing bioactive glass, 3 to 40 percent of glycerol, 0.5 to 10 percent of silicon dioxide, 0.2 to 10 percent of mixture of carboxymethyl cellulose and xanthan gum, 0.2 to 7 percent of cocamidopropyl betaine, 10 to 40 percent of polyethylene glycol, 0.1 to 10 percent of xylitol or sorbitol, 0.01 to 2 percent of essence and the balance of purified water;

In the mixture of the carboxymethyl cellulose and the xanthan gum, the weight ratio of the carboxymethyl cellulose to the xanthan gum is 4:1.

the dyed selenium-containing bioactive glass is prepared by the following preparation method:

(8) Preparing a biological staining gel: the biological staining gel comprises the following components in percentage by weight: acetic acid 2%, phycoerythrin B1.0%, sodium persulfate 0.5%, sodium alginate 1.6%, caCl ₂ 1.6% of purified water 93.3%;

And (3) preparing xerogel in the step (4), namely removing ethanol and water in the sol under the vacuum condition at 50-80 ℃.

In the step (9), the drying is carried out for 24 hours at 50-80 ℃.

The preparation method of the quick-acting visual tooth desensitizer specifically comprises the following steps:

Example 1

The visual tooth desensitizer with quick effect comprises the following components in parts by weight: 0.5g of selenium-containing bioactive glass, 3g of glycerol, 0.5g of silicon dioxide, 0.2g of carboxymethyl cellulose and xanthan gum mixture, 0.2g of cocamidopropyl betaine, 10g of polyethylene glycol, 0.1g of xylitol, 0.01g of essence and 85.49g of purified water;

(1) Preparing an inorganic solution: siO is made of ₂ 、Na ₂ O、CaO、MgO、P ₂ O ₅ Mixing according to the weight ratio of 33g, 1g, 44g, 4.5g and 17.5g respectively to form an inorganic mixture 100g, adding the inorganic mixture into a tetrahydrate calcium nitrate aqueous solution to prepare an inorganic solution, wherein the inorganic mixture and the tetrahydrate calcium nitrate aqueous solutionThe mass ratio of the calcium nitrate tetrahydrate aqueous solution is 1:3, the calcium nitrate tetrahydrate aqueous solution is a mixed solution of calcium nitrate tetrahydrate and water, and the molar ratio of the water to the calcium nitrate tetrahydrate is 6:1;

(3) Preparing sol: adding the inorganic solution prepared in the step (1) into the ethyl orthosilicate-ethanol organic solution prepared in the step (2), stirring while adding, dropwise adding 2mol/L nitric acid as a catalyst, dropwise adding until the pH of the solution is 2, and stirring for 50min to obtain sol;

(4) Preparation of xerogel: removing ethanol and water in the sol obtained in the step (3) under the vacuum condition at 50 ℃ and aging for 48 hours to obtain xerogel;

(5) Preparing bioactive glass powder: calcining the xerogel obtained in the step (4) at 700 ℃ for 2 hours, and sieving and purifying to obtain bioactive glass powder, wherein the particle size of the bioactive glass powder is 50 mu m;

(8) Preparing a biological staining gel: the biological staining gel comprises the following components in parts by weight: acetic acid 2g, phycoerythrin B1.0g, sodium persulfate 0.5g, sodium alginate 1.6g, caCl ₂ 1.6g of purified water 93.3g;

the preparation method specifically comprises the following steps: taking the components in the proportion, firstly, respectively fully dissolving acetic acid, phycoerythrin B, sodium persulfate and purified water according to the weight, standing for precipitation, and taking supernatant; then the supernatant is mixed with sodium alginate and CaCl ₂ Fully mixing, standing for 6 hours, and taking precipitated gel for standby, thus obtaining the biological staining gel;

(9) Preparing dyed selenium-containing bioactive glass: slowly adding the test solution A obtained in the step (6) into the test solution B obtained in the step (7), wherein the weight ratio of the test solution A to the test solution B is 1:1, obtaining a mixed solution, adding the biological dyeing gel obtained in the step (8) into the mixed solution, stirring for 2 hours, wherein the addition amount of the biological dyeing gel is 1% of the total weight of the mixed solution, then adding the catalyst glacial acetic acid, wherein the addition amount of the glacial acetic acid is 1.9% of the total weight of the mixed solution, continuously stirring for 1 hour, filtering, washing to be oilless by using absolute ethyl alcohol, and drying for 24 hours at 50 ℃ to obtain the dyed selenium-containing bioactive glass.

Example two

The preparation method of the quick-acting visualized tooth desensitizer in the first embodiment specifically comprises the following steps:

s1, preparing dyed selenium-containing bioactive glass microcapsules: taking 0.125g of carboxymethyl cellulose and xanthan gum mixture and 1.0g of polyethylene glycol as wall materials, taking 0.5g of dyed selenium-containing bioactive glass and 0.175g of glycerol as core materials, and preparing dyed selenium-containing bioactive glass microcapsules by using a high-pressure microcapsule embedding method (the high-pressure microcapsule embedding method is a known technology and is not repeated here);

s2, preparing an aqueous phase: uniformly mixing 0.5g of silicon dioxide, the rest 0.075g of mixture of carboxymethyl cellulose and xanthan gum and 0.1g of xylitol, adding 85.49g of purified water, stirring for 0.5 hours at a rotating speed of 60r/min, and obtaining a water phase after the mixture of carboxymethyl cellulose and xanthan gum is completely dissolved for later use;

s3, preparing an oil phase: stirring 0.2g of cocamidopropyl betaine, 0.2g of polyethylene glycol, 0.01g of essence and the rest 2.825g of glycerin for 0.5 hour to be uniform under the conditions that the vacuum degree is more than or equal to 0.06MPa and the rotating speed is 60r/min to obtain an oil phase for later use;

s4, mixing and emulsifying: mixing and emulsifying the dyed selenium-containing bioactive glass microcapsule obtained in the step S1, the water phase obtained in the step S2, the oil phase obtained in the step S3 and the rest 8.8g of polyethylene glycol for 2 hours until uniformity, and obtaining the visual tooth desensitizer.

Example III

The visual tooth desensitizer with quick effect comprises the following components in parts by weight: 5g of selenium-containing bioactive glass, 20g of glycerol, 10g of silicon dioxide, 5g of carboxymethyl cellulose and xanthan gum mixture, 7g of cocamidopropyl betaine, 20g of polyethylene glycol, 10g of xylitol, 2g of essence and 21g of purified water;

(1) Preparing an inorganic solution: siO is made of ₂ 、Na ₂ O、CaO、MgO、P ₂ O ₅ Mixing according to the weight ratio of 33g, 1g, 44g, 4.5g and 17.5g respectively to form an inorganic mixture of 100g, and adding the inorganic mixture into a tetrahydrate calcium nitrate aqueous solution to prepare an inorganic solution, wherein the mass ratio of the inorganic mixture to the tetrahydrate calcium nitrate aqueous solution is 1:3, the tetrahydrate calcium nitrate aqueous solution is a mixed solution of tetrahydrate calcium nitrate and water, and the molar ratio of water to tetrahydrate calcium nitrate is 6:1;

(3) Preparing sol: adding the inorganic solution prepared in the step (1) into the ethyl orthosilicate-ethanol organic solution prepared in the step (2), stirring while adding, dropwise adding 2mol/L nitric acid as a catalyst, dropwise adding until the pH value of the solution is 4, and stirring for 50min to obtain sol;

(4) Preparation of xerogel: removing ethanol and water in the sol obtained in the step (3) under the vacuum condition at 80 ℃ and aging for 48 hours to obtain xerogel;

(5) Preparing bioactive glass powder: calcining the xerogel obtained in the step (4) at 800 ℃ for 2 hours, and sieving and purifying to obtain bioactive glass powder, wherein the particle size of the bioactive glass powder is 50 mu m;

(9) Preparing dyed selenium-containing bioactive glass: slowly adding the test solution A obtained in the step (6) into the test solution B obtained in the step (7), wherein the weight ratio of the test solution A to the test solution B is 1:1, obtaining a mixed solution, adding the biological dyeing gel obtained in the step (8) into the mixed solution, stirring for 2 hours, wherein the addition amount of the biological dyeing gel is 5% of the total weight of the mixed solution, then adding the catalyst glacial acetic acid, wherein the addition amount of the glacial acetic acid is 1.9% of the total weight of the mixed solution, continuously stirring for 1 hour, filtering, washing to be oilless by using absolute ethyl alcohol, and drying for 24 hours at 80 ℃ to obtain the dyed selenium-containing bioactive glass.

Example IV

The preparation method of the quick-acting visualized tooth desensitizer in the third embodiment specifically comprises the following steps:

s1, preparing dyed selenium-containing bioactive glass microcapsules: taking 1.25g of carboxymethyl cellulose and xanthan gum mixture and 10g of polyethylene glycol as wall materials, taking 5g of dyed selenium-containing bioactive glass and 1.75g of glycerol as core materials, and preparing the dyed selenium-containing bioactive glass microcapsules by using a high-pressure microcapsule embedding method (the high-pressure microcapsule embedding method is a known technology and is not repeated here);

S2, preparing an aqueous phase: uniformly mixing 10g of silicon dioxide, the rest 3.75g of mixture of carboxymethyl cellulose and xanthan gum and 10g of xylitol, adding 21g of purified water, stirring for 0.5 hour at the rotating speed of 60r/min, and obtaining a water phase after the mixture of carboxymethyl cellulose and xanthan gum is completely dissolved for later use;

s3, preparing an oil phase: stirring 7g of cocamidopropyl betaine, 7g of polyethylene glycol, 2g of essence and the rest 18.25g of glycerol for 0.5 hours under the conditions that the vacuum degree is more than or equal to 0.06MPa and the rotating speed is 60r/min to be uniform to obtain an oil phase for later use;

s4, mixing and emulsifying: and (3) mixing and emulsifying the dyed selenium-containing bioactive glass microcapsule obtained in the step (S1), the water phase obtained in the step (S2), the oil phase obtained in the step (S3) and the rest 3g of polyethylene glycol for 2 hours until uniformity, and obtaining the visual tooth desensitizer.

Example five

The visual tooth desensitizer with quick effect comprises the following components in parts by weight: 10g of dyed selenium-containing bioactive glass, 15g of glycerol, 5g of silicon dioxide, 10g of carboxymethyl cellulose and xanthan gum mixture, 1g of cocamidopropyl betaine, 40g of polyethylene glycol, 2g of sorbitol, 0.1g of essence and 16.9g of purified water;

(3) Preparing sol: adding the inorganic solution prepared in the step (1) into the ethyl orthosilicate-ethanol organic solution prepared in the step (2), stirring while adding, dropwise adding 2 mol/L nitric acid as a catalyst, dropwise adding until the pH of the solution is 3, and stirring for 50min to obtain sol;

(4) Preparation of xerogel: removing ethanol and water in the sol obtained in the step (3) under the vacuum condition at 60 ℃, and aging for 48 hours to obtain xerogel;

(5) Preparing bioactive glass powder: calcining the xerogel obtained in the step (4) at 750 ℃ for 2 hours, and sieving and purifying to obtain bioactive glass powder, wherein the particle size of the bioactive glass powder is 50 mu m;

(9) Preparing dyed selenium-containing bioactive glass: slowly adding the test solution A obtained in the step (6) into the test solution B obtained in the step (7), wherein the weight ratio of the test solution A to the test solution B is 1:1, obtaining a mixed solution, adding the biological dyeing gel obtained in the step (8) into the mixed solution, stirring for 2 hours, wherein the addition amount of the biological dyeing gel is 2% of the total weight of the mixed solution, then adding the catalyst glacial acetic acid, wherein the addition amount of the glacial acetic acid is 1.9% of the total weight of the mixed solution, continuously stirring for 1 hour, filtering, washing to be oilless by using absolute ethyl alcohol, and drying for 24 hours at 60 ℃ to obtain the dyed selenium-containing bioactive glass.

Example six

The preparation method of the quick-acting visualized tooth desensitizer in the fifth embodiment specifically comprises the following steps:

s1, preparing dyed selenium-containing bioactive glass microcapsules: taking 2.5g of carboxymethyl cellulose and xanthan gum mixture and 20g of polyethylene glycol as wall materials, taking 10g of dyed selenium-containing bioactive glass and 3.5g of glycerol as core materials, and preparing the dyed selenium-containing bioactive glass microcapsules by using a high-pressure microcapsule embedding method (the high-pressure microcapsule embedding method is a known technology and is not repeated here);

s2, preparing an aqueous phase: uniformly mixing 5g of silicon dioxide, the rest 7.5g of mixture of carboxymethyl cellulose and xanthan gum and 2g of sorbitol, adding 16.9g of purified water, stirring for 0.5 hour at the rotating speed of 60r/min, and obtaining a water phase after the mixture of carboxymethyl cellulose and xanthan gum is completely dissolved for later use;

s3, preparing an oil phase: stirring 1g of cocamidopropyl betaine, 1g of polyethylene glycol, 0.1g of essence and the rest 11.5g of glycerin for 0.5 hour under the conditions that the vacuum degree is more than or equal to 0.06MPa and the rotating speed is 60r/min to be uniform to obtain an oil phase for later use;

s4, mixing and emulsifying: and (3) mixing and emulsifying the dyed selenium-containing bioactive glass microcapsule obtained in the step (S1), the water phase obtained in the step (S2), the oil phase obtained in the step (S3) and the rest 19g of polyethylene glycol for 2 hours until the mixture is uniform, and thus obtaining the visual tooth desensitizer.

Example seven

The visual tooth desensitizer with quick effect comprises the following components in parts by weight: 6g of dyed selenium-containing bioactive glass, 40g of glycerol, 2g of silicon dioxide, 2g of carboxymethyl cellulose and xanthan gum mixture, 1g of cocamidopropyl betaine, 20g of polyethylene glycol, 1g of sorbitol, 1g of essence and 27g of purified water;

(4) Preparation of xerogel: removing ethanol and water in the sol obtained in the step (3) under the vacuum condition at 70 ℃ and aging for 48 hours to obtain xerogel;

the preparation method specifically comprises the following steps: taking the components in the proportion, firstly, respectively and fully dissolving acetic acid, phycoerythrin B, sodium persulfate and purified water according to the weight, and standingStanding for precipitation, and collecting supernatant; then the supernatant is mixed with sodium alginate and CaCl ₂ Fully mixing, standing for 6 hours, and taking precipitated gel for standby, thus obtaining the biological staining gel;

(9) Preparing dyed selenium-containing bioactive glass: slowly adding the test solution A obtained in the step (6) into the test solution B obtained in the step (7), wherein the weight ratio of the test solution A to the test solution B is 1:1, obtaining a mixed solution, adding the biological dyeing gel obtained in the step (8) into the mixed solution, stirring for 2 hours, wherein the addition amount of the biological dyeing gel is 3% of the total weight of the mixed solution, then adding the catalyst glacial acetic acid, wherein the addition amount of the glacial acetic acid is 1.9% of the total weight of the mixed solution, continuously stirring for 1 hour, filtering, washing to be oilless by using absolute ethyl alcohol, and drying for 24 hours at 70 ℃ to obtain the dyed selenium-containing bioactive glass.

Example eight

The preparation method of the quick-acting visualized tooth desensitizer in the seventh embodiment specifically comprises the following steps:

s1, preparing dyed selenium-containing bioactive glass microcapsules: taking 1.5g of carboxymethyl cellulose and xanthan gum mixture and 12g of polyethylene glycol as wall materials, taking 6g of dyed selenium-containing bioactive glass and 2.1g of glycerol as core materials, and preparing the dyed selenium-containing bioactive glass microcapsules by using a high-pressure microcapsule embedding method (the high-pressure microcapsule embedding method is a known technology and is not repeated here);

S2, preparing an aqueous phase: uniformly mixing 2g of silicon dioxide, the rest 0.5g of mixture of carboxymethyl cellulose and xanthan gum and 1g of sorbitol, adding 27g of purified water, stirring for 0.5 hour at the rotating speed of 60r/min, and obtaining a water phase after the mixture of carboxymethyl cellulose and xanthan gum is completely dissolved for later use;

s3, preparing an oil phase: stirring 1g of cocamidopropyl betaine, 1g of polyethylene glycol, 1g of essence and the rest 37.9g of glycerol for 0.5 hour under the conditions that the vacuum degree is more than or equal to 0.06MPa and the rotating speed is 60r/min to be uniform to obtain an oil phase for later use;

s4, mixing and emulsifying: and (3) mixing and emulsifying the dyed selenium-containing bioactive glass microcapsule obtained in the step (S1), the water phase obtained in the step (S2), the oil phase obtained in the step (S3) and the rest 7g of polyethylene glycol for 2 hours until uniformity, and obtaining the visual tooth desensitizer.

The application method of the visual tooth desensitizer comprises the following steps: and (3) taking the visual tooth desensitizer on a cotton swab or a soft hair toothbrush, repeatedly smearing the visual tooth desensitizer on the surface of the teeth for 3-5 minutes, and then rinsing with clean water to remove the teeth. Meanwhile, a user can clean the corresponding parts with emphasis according to the plaque chromogenic indication.

The visual dental desensitizers obtained in examples one to eight were characterized and had substantially the same properties, and thus were tested as follows:

1. And (3) physical detection:

1. sample treatment: collecting 48 premolars of oral hospitals in Shenyang city in 2023 and 8 months, soaking in physiological saline, changing physiological saline once a day, and storing in refrigerator at 4deg.C for use. The inclusion criteria were: the surface of the isolated enamel was examined under a stereomicroscope (x 20) for no caries, no crack, no undergrowth of enamel, and complete root development.

2. Preparation of reagents: preparing 45S5 bioactive glass sol with the concentration of 5%, dyed selenium-containing bioactive glass sol with the concentration of 5% and sodium fluoride solution with the concentration of 5%;

(1) the preparation method of the 45S5 bioactive glass sol with the concentration of 5 percent comprises the following steps: 0.8g 45S5 bioactive glass, 0.08g xanthan gum and 1.42g glycerol are weighed, 13.6mL sterile water is weighed and added into a vial sterilized in advance, the vial is stirred uniformly until the vial is completely dissolved, and after ultraviolet sterilization for 2 hours, the vial is preserved in a dark place at 4 ℃.

(2) The preparation method of the dyed selenium-containing bioactive glass sol with the concentration of 5 percent comprises the following steps: weighing 0.8g of dyed selenium-containing bioactive glass, 0.08g of xanthan gum and 1.42g of glycerol, weighing 13.6mL of sterile water, adding into a vial sterilized in advance, stirring uniformly to dissolve completely, sterilizing by ultraviolet for 2 hours, and preserving in dark at 4 ℃.

(3) Sodium fluoride solution with concentration of 5% is commercially available and is added into a vial sterilized in advance and stored at 4 ℃ in a dark place.

3. Preparation of ex-vivo tooth samples: cleaning and sterilizing 48 in-vitro premolars, removing bacterial plaque, coloring and periodontal fibrous soft tissues on root surfaces, performing ultrasonic vibration for 10min by using deionized water, cutting off roots below 5mm of enamel cementum boundary by using a high-speed mobile phone and a diamond drilling needle, and removing dental pulp tissues. Polishing of the enamel surface was performed with a polisher to obtain a flat enamel surface, after which the sample was rinsed with deionized water in an ultrasonic bath for 5min. After the treatment was completed, it was divided into two in the labial lingual direction of the isolated tooth to obtain 96 samples.

4. Grouping of adjacent surface test pieces and establishment of an early adjacent surface caries model:

grouping: the 96 samples were randomly divided on average into four groups (n=24), labeled as group a (45S 5 bioactive glass group), group B (sodium fluoride group), group C (blank control group), group D (stained selenium containing bioactive glass group). After the isolated tooth sample is dried, embedding the part below the cementum boundary in self-setting resin, exposing the adjacent surface of the isolated tooth sample, defining a 5mm 3mm area on the adjacent surface as an experimental area, sealing enamel outside the experimental area for 3 times by acid-resistant nail polish, and after the enamel is completely solidified, performing ultrasonic oscillation washing for 15 minutes. The sample is stored in artificial saliva and placed in an incubator at 37 ℃ for standby.

Ore removal treatment: taking out 96 samples stored in the artificial saliva, respectively soaking in 100mL of artificial ore removal liquid for ore removal, 10 times per day for 5min, replacing fresh liquid each time, flushing the artificial saliva at intervals, and continuously soaking for 10d within 12 h. After demineralization, the model was sonicated in deionized water for 5min to form an early model of early caries (success standard for caries model establishment: chalky change of the surface of the adjacent enamel, surface roughness was observed under electron microscopy with honeycomb structure generation).

5. After the adjacent caries model is established successfully, remineralizing treatment is carried out on the adjacent caries model: A. b, C, D the four groups of samples were respectively subjected to remineralization coating treatment for 5min (45S 5 bioactive glass sol with 5% experimental zone coating concentration in group a, sodium fluoride solution with 5% experimental zone coating concentration in group B, dyed selenium-containing bioactive glass sol with 5% experimental zone coating concentration in group D, and 5min for group C) and after the above treatment, were rinsed with neutral buffer solution for 3min, and then immersed in artificial saliva, the above operations were performed 2 times a day for 5min for a total of 15 days. During the non-treatment period, the samples are soaked in a 37 ℃ incubator containing the artificial saliva for preservation, the artificial saliva is prepared and used at present, the artificial saliva is replaced once a day, and deionized water is used for washing for 1min before the artificial saliva is replaced.

6. Surface detection of remineralised ex vivo tooth samples: dividing the four groups of samples of the group A, the group B, the group C and the group D into three subgroups (n=8), and randomly taking 5 samples from the subgroups (n=8) of the samples of each group for detection of a white light interference microscope and observation of surface morphology change and dent depth of the samples by an SEM;

(1) White light interference microscopy: the detection results of the remineralized sample three-dimensional morphology change by adopting a white light interference scanning electron microscope are shown in the figure 1, the rough surface and pit-shaped structure of the C group (blank group) enamel after demineralization are visually observed from the figure, and the uneven surface of the enamel layer and the demineralized pit structure with large area and different concavity can be observed from the three-dimensional morphology. Group B shows dense demineralization pores on the enamel surface, and relatively uniform spherical deposits on the enamel surface with thinner deposit layers. Group a shows irregular lamellar deposits with denser enamel surface. The group D visible lamellar deposits extend along the demineralization recesses, and the remineralization effect of the group D is better.

(2) SEM scanning electron microscopy: after carrying out metal spraying treatment on the remineralized sample, detecting by adopting an SEM scanning electron microscope, wherein the obtained SEM scanning electron microscope is shown as a figure 2, and as can be seen from the figure 2, a 45S5 bioactive glass group (A group) shows that irregular lamellar sediment is piled up on the enamel surface, and scattered pores exist among the sediment; the sodium fluoride group (B group) shows that enamel surfaces are scattered in pores, and flaky and spherical sediments are accumulated on the surfaces; the blank control group (group C) shows the disappearance of the normal morphology of the enamel surface and shows large-area honeycomb-shaped depressions; the surface of the dyed selenium-containing bioactive glass group (group D) enamel has tiny pores, and the sediment is uniformly arranged in a net shape; thus, SEM electron microscopy showed that the sample deposit coated with the dyed selenium-containing bioactive glass of the present invention was more uniform.

(3) Determination of calcium-phosphorus ratio of remineralized isolated tooth samples:

the four groups of samples of the A group, the B group, the C group and the D group are respectively divided into three subgroups (n=8), 5 samples are respectively and randomly taken from the subgroups (n=8) of the samples of each group, four points are randomly taken from each sample, the calcium-phosphorus ratio of the selected point of each group of samples is detected by adopting a Si (li) detector, the measurement result of each group of samples is averaged, the measurement result is shown in the table 1, the significant difference (P < 0.05) of the calcium-phosphorus ratios among the groups can be seen, the calcium-phosphorus ratio of the dyed selenium-containing bioactive glass group (D group) is the highest, the calcium-phosphorus ratio is higher than that of the normal enamel surface (1.9-2.1), the remineralization effect is better than that of the calcium-phosphorus ratio of the A group (45S 5 bioactive glass group) and the B group (sodium fluoride group), the calcium-phosphorus ratio of the blank group (C group) is lower than that of the normal enamel surface (1.9-2.1), and the calcium-phosphorus ratio of the blank group (C group) is the lowest than that of the normal enamel surface.

TABLE 1 calcium phosphorus ratio measurement results

2. Evaluation of bacteriostatic Effect

1. Antibacterial effect is detected to antibacterial ring

The method for judging the antibacterial potency of the reagent to be tested according to the size of the antibacterial zone comprises the steps of dispersing the reagent to be tested in a flat plate, so that the reagent to be tested has an antibacterial effect on surrounding bacteria to form the antibacterial zone, and detecting by adopting a perforation method in the experiment.

Reagent preparation and grouping: 45S5 bioactive glass sol with the concentration of 35mg/mL, dyed selenium-containing bioactive glass sol with the concentration of 35mg/mL and sodium fluoride solution with the concentration of 3mg/mL are prepared. The method comprises the steps of marking 1 group, 2 groups and 0 group respectively, wherein the 0 group is a control group sodium fluoride group, the 1 group is an observation group 45S5 bioactive glass sol, and the 2 group is a test group for dyeing selenium-containing bioactive glass sol; the preparation method of each reagent is as follows:

(1) the preparation method of the 45S5 bioactive glass sol with the concentration of 35mg/mL comprises the following steps: 0.5g 45S5 bioactive glass, 0.08g xanthan gum and 1.42g glycerol are weighed, 12.2ml sterile water is weighed and added into a vial sterilized in advance, the mixture is stirred uniformly until the mixture is completely dissolved, and after ultraviolet sterilization for 2 hours, the mixture is preserved in a dark place at 4 ℃.

(2) The preparation method of the dyed selenium-containing bioactive glass sol with the concentration of 35mg/mL comprises the following steps: weighing 0.5g of dyed selenium-containing bioactive glass, 0.08g of xanthan gum and 1.42g of glycerol, weighing 12.2ml of sterile water, adding into a vial sterilized in advance, stirring uniformly to dissolve completely, sterilizing by ultraviolet for 2 hours, and preserving in dark at 4 ℃.

(3) The preparation method of the sodium fluoride solution with the concentration of 3mg/mL comprises the following steps: 10mg of sodium fluoride is weighed, 3.32ml of sterile water is weighed, added into a vial sterilized in advance, stirred uniformly until the solution is completely dissolved, sterilized by ultraviolet rays for 2 hours, and stored at 4 ℃ in a dark place.

(2) The experimental steps are as follows: 100uL of Streptococcus mutans suspension (bacterial liquid concentration after liquid passage is about 1.0X10) ⁸ cfu/mL, diluted to a concentration of about 1.0X10 with BHI broth ⁵ cfu/mL of bacterial suspension for later use) are uniformly smeared on a BHI solid culture dish for 2 times, the plate is rotated by 90 degrees after each smearing, and finally the plate is smeared around the edge of the plate for one circle. Three holes (the positions of which are arranged on a flat plate at equal intervals in an equilateral triangle shape and marked) are punched on the culture dish by using a puncher, 80uL of prepared 1 group, 2 group and 0 group of reagents are respectively added into the three holes, after the culture is performed for 48 hours under anaerobic conditions, the diameter of a bacteriostasis ring is measured by using a vernier caliper, and a uniformly and completely sterile growth bacteriostasis ring is selected for measurement, wherein the diameter of the bacteriostasis ring is defined by the outer edge of the bacteriostasis ring. This procedure was repeated three times (three dishes were taken for parallel experiments, and the above procedure was repeated, with groups 1, 2, and 0 each giving three sets of data, which were averaged after measurement). The detection result of the inhibition ring is shown in figure 3, and the diameter of the inhibition ring is measured by a vernier caliper, and the diameter of the inhibition ring is positively correlated with the inhibition effect. The measurement results are shown in table 2, and it can be seen that the dyed selenium-containing bioactive glass (group 2) of the invention has a diameter larger than that of the control group (group 0) and the observation group (group 1), and has good antibacterial effect (the diameter is larger than 7mm, the diameter is smaller than 7mm, and the antibacterial effect is not determined).

TABLE 2 diameter measurement results of inhibition ring

Group of	Diameter of inhibition ring (mm)
		1	12.10 ^*
2	18.3 ^*
		0	7.57 ^*

(note: n=3, ^* represents P < 0.01)

2. Method for detecting antibacterial effect by direct contact method

(1) Reagent preparation and grouping: preparing 45S5 bioactive glass sol with the concentration of 70mg/mL, dyed selenium-containing bioactive glass sol with the concentration of 70mg/mL and sodium fluoride solution with the concentration of 6mg/mL, and marking the solution as 1 group, 2 groups and 0 groups respectively as reagent groups, wherein the 0 group is a control group, the 1 group is an observation group and the 2 groups are test groups; the preparation method of each reagent is as follows:

(1) the preparation method of the bioactive glass sol with the concentration of 70mg/mL comprises the following steps: 1.0g45S5 bioactive glass, 0.08g xanthan gum and 1.42g glycerol are weighed, 11.7mL sterile water is weighed and added into a vial sterilized in advance, the mixture is stirred uniformly until the mixture is completely dissolved, and after ultraviolet sterilization for 2 hours, the mixture is stored in a dark place at 4 ℃.

(2) The preparation method of the dyed selenium-containing bioactive glass sol with the concentration of 70mg/mL comprises the following steps: 1.0g of dyed selenium-containing bioactive glass, 0.08g of xanthan gum and 1.42g of glycerol are weighed, 11.7mL of sterile water is weighed and added into a vial sterilized in advance, the mixture is stirred uniformly until the mixture is completely dissolved, and after ultraviolet sterilization for 2 hours, the mixture is preserved in a dark place at 4 ℃.

(3) The preparation method of the sodium fluoride solution with the concentration of 6mg/mL comprises the following steps: weighing 20mg of sodium fluoride, weighing 3.32mL of sterile water, adding into a vial sterilized in advance, stirring uniformly to dissolve completely, sterilizing by ultraviolet for 2 hours, and preserving at 4 ℃ in dark place.

(2) The experimental steps are as follows:

A. a 24-well cell culture plate was taken, partitioned and labeled. Partitions in 24-well plates were as follows: the method comprises the steps of taking 6 holes from 1 group, 2 group and 0 group of reagent groups respectively, taking 6 holes on a 24-hole cell culture plate at the same time, setting a positive group and a blank control group, and taking 3 holes from the positive group and the blank control group respectively (the purpose of designing the positive group is that if turbidity or biofilm grows out, bacteria can grow normally under the given nutrition condition, the purpose of designing the blank control group is that the bacteria should be clear normally, if turbidity or biofilm grows out, bacteria are infected due to improper personal operation is represented);

B. reagents were added to 24-well cell culture plates:

(1) reagent set: into 6 wells of group 1, group 2 and group 0, 0.8 mL of BHI brain heart infusion broth culture medium and 0.2. 0.2 mL Streptococcus mutans suspension (Streptococcus mutans suspension after liquid passage, concentration of about 1.0X10) were added ⁸ cfu/mL), adding 1mL of the reagents of the 1 group, the 2 group and the 0 group respectively after fully mixing;

(2) positive group: 1.6mL of BHI brain heart infusion broth medium and 0.4. 0.4 mL Streptococcus mutans suspension (Streptococcus mutans suspension after liquid passage, concentration of about 1.0X10) were added to each well ⁸ cfu/mL）；

(3) Blank control group: 2mL of BHI brain heart infusion broth culture medium was added to each well;

C. The reagents in each well of the 24-well cell culture plate after anaerobic culture for 24 hours at 37 ℃ are uniformly mixed, 10 mu L of the uniformly mixed culture solution is inoculated on a BHI agar plate, after anaerobic culture for 48 hours, a photo is shown in fig. 4, colony counting is carried out, the experiment is repeated three times (the whole operation totally uses 3 24-well culture plates, the steps are repeated 3 times, and finally three culture dishes with colonies are obtained in groups 1, 2 and 0, and after the respective counting, the colony numbers in the table 3 are obtained by respectively taking the average value of the data of the groups 1, 2 and 0), so as to reduce errors.

TABLE 3 direct contact colony plate count statistics

Group of	Colony count (number)
		1	80.33 ^*
2	10 ^*
		0	255.33

(note: n=3, ^* represents P < 0.01 between any two groups

3. Observing the biomembrane by a laser confocal microscope:

the laser confocal adopts a laser light source, a confocal technology and a point scanning technology, can perform high-resolution nondestructive tomography on thicker samples, selects SYTO9/PI according to the difference of the permeability of dead and living cell membranes, marks the cells of the bacteria, and can directly observe the activity change of the bacteria through confocal. SYTO9 will give out green fluorescence after staining live bacteria, PI will give out red fluorescence after staining dead bacteria, and yellowish green indicates the overlapping place of live bacteria and dead bacteria. The test judges the activity of the thallus by directly observing the fluorescent staining condition of the thallus, and further judges the antibacterial action of the reagent to be tested, namely, the greater the dead bacteria ratio is, the stronger the antibacterial capability is as the red and yellowish green in the visual field are more obvious (the image analysis software used for the test is NIS-Elements Viewer).

(1) Reagent preparation and grouping: preparing 45S5 bioactive glass sol with the concentration of 35mg/mL, dyed selenium-containing bioactive glass sol with the concentration of 35mg/mL and sodium fluoride solution with the concentration of 3mg/mL, and respectively marking the solution as a group A, a group B and a group C as reagent groups, wherein the group C is a control group, the group A is an observation group, and the group B is a test group; the preparation method of each reagent comprises the following steps:

(2) The experimental steps are as follows: after 24-well cell slide was placed in a 24-well cell culture plate, 1.8mL of BHI brain heart infusion broth medium and 0.2mL of Streptococcus mutans suspension (Streptococcus mutans suspension after liquid passage, concentration was about 1.0X10) were added to each well ⁸ cfu/mL), after culturing for 72h at 37 ℃, obtaining simulated streptococcus mutans biomembrane, sucking the supernatant in the culture dish, only retaining the climbing slices and the biomembrane attached to the climbing slices, partitioning the 24-hole cell culture plate and marking, taking 6 holes of A group, B group and C group of the reagent group respectively, taking 6 holes as D group in addition, and taking the D group as blank group (the purpose of setting the blank group: no detection reagent is added for observing the growth condition of the biological film in a normal state);

adding 500 mu L of corresponding reagents of the A group, the B group and the C group into 6 holes of the A group, the B group and the C group respectively, adding no reagent into 6 holes of a blank group, placing a 24-hole cell culture plate into a 37 ℃ incubator for 20min, absorbing and discarding supernatant, flushing 2 times by PBS, fixing for 20min by tissue fixing liquid, adding 20 mu L of prepared live/dead bacterial fluorescent dye (SYTO 9/PI), incubating for 20min in a dark place, and rinsing by PBS to remove redundant dye.

And then observing the biological film under a laser scanning confocal microscope, wherein an excitation light source is 486nm/638nm, observing that living bacteria are stained by SYTO9 and emit green fluorescence, and dead bacteria are stained by PI and emit red fluorescence, wherein SYTO9 and PI staining are overlapped to form orange or yellowish green to represent overlapping parts of the living bacteria and the dead bacteria.

The scanning diagram of the confocal laser microscope is shown in fig. 5, bacteria are respectively dyed into red and green by observing under the confocal laser microscope after fluorescent dyeing, the red represents dead bacteria, the green shows all living bacteria, and orange or yellowish green are overlapped. The green fluorescence in group D (blank) without reagent is almost full of the whole visual field, and compared with group C (sodium fluoride solution), the red fluorescence in group A (45S 5 bioactive glass sol) and group B (dyed selenium-containing bioactive glass sol) are in a certain proportion and are partially overlapped to be orange or yellowish green, wherein the red fluorescence in group B is more in proportion, and the orange or yellowish green area is more obvious, so that the dyed selenium-containing bioactive glass has better antibacterial and sterilizing effects.

The evaluation results of the three antibacterial effects show that: the antibacterial capability of the sodium fluoride solution is weaker, and compared with the sodium fluoride solution, the antibacterial and bactericidal effects of the dyed selenium-containing bioactive glass are more remarkable. Meanwhile, due to the addition of selenium, compared with the conventional 45S5 bioactive glass, the dyed selenium-containing bioactive glass has better antibacterial effect, so that the selenium can synergistically strengthen the antibacterial performance of the bioactive glass, and a new thought is provided for clinical medication.

3. Dentin tubule blockage rate test

The dentinal tubule blocking rate of the tooth desensitizer prepared by the ordinary process method and the tooth desensitizer prepared by the preparation method in the second embodiment of the invention were detected by using YY/T1829-2022 dentinal tubule blocking effect in vitro evaluation method, and the detection results are shown in Table 4 in parallel for 3 times.

Wherein, the steps of preparing the tooth desensitizer by the common process method are as follows: the prescribed amount of dyed selenium-containing bioactive glass, glycerin, silicon dioxide, a mixture of sodium carboxymethyl cellulose and xanthan gum, xylitol or sorbitol was dissolved in purified water (85% of the weight of the formula amount of purified water) with stirring in the main pot of the emulsifying machine to obtain a mixture a. The prescribed amount of polyethylene glycol, cocamidopropyl betaine, and essence were dissolved with stirring in the remaining purified water (15% by weight of the prescribed amount of purified water) to prepare solution a. Mixing: adding the solution A into the mixture A, and stirring until the mixture A is uniform to obtain the visual tooth desensitizer.

TABLE 4 dentinal tubule occlusion rate measurement results

As can be seen from the data in Table 4, the dentinal tubule blocking rate of the desensitizer prepared by the second preparation method of the present invention is 92.8%, which is higher than that of the dentinal tubule blocking rate of 85.7% of the conventional process. Therefore, the preparation method of the second embodiment of the invention delays the release of ions after the dyed selenium-containing bioactive glass reacts with water in the formula, and improves the sealing rate of the dental tubules.

4. Visual effect detection

12 cases of users are selected, the ages of the users are 10 to 48 years, the average ages of the users (29.0+/-19) are all free of dental caries, dental caries and filling bodies, dental pulp, root tips and periodontal conditions are good, and selected patients have no treatment history of dentin hypersensitiveness, no treatment history of systematic diseases and drug hypersensitiveness, good periodontal conditions and no caries.

The detection method comprises the following steps: a proper amount of the visualized tooth desensitizer prepared in the second embodiment of the invention is repeatedly smeared on each surface of teeth of a user for 3-5 minutes on a cotton swab or a soft brush, and then the visualized tooth desensitizer is rinsed with clean water after cleaning.

The visual effect of the tooth desensitizer of the invention was observed by recording 12 photographs of the users after staining and photographs of the users after rinsing with clear water. The comparison photos of 12 users show that the stained dental plaque after the tooth desensitizer is coated can be intuitively seen, the color development of the dental plaque is greatly reduced after the tooth desensitizer is coated, the residual pigment amount of the gum and mouth part is smaller, the detection results are similar, 2 users (the age of the first user is 44 years old, the sex woman, the age of the second user is 35 years old, and the sex woman) are taken as examples, as shown in fig. 6 and 7, the dental plaque is intuitively seen to be stained after the tooth desensitizer is coated on the first user and the second user, the color development of the dental plaque is greatly reduced after the tooth desensitizer is coated on the clean water, and the residual pigment amount of the gum and mouth part is smaller.

The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.

Claims

1. The quick-acting visual tooth desensitizer is characterized by comprising the following components in percentage by weight: 0.5 to 10 percent of dyed selenium-containing bioactive glass, 3 to 40 percent of glycerol, 0.5 to 10 percent of silicon dioxide, 0.2 to 10 percent of mixture of carboxymethyl cellulose and xanthan gum, 0.2 to 7 percent of cocamidopropyl betaine, 10 to 40 percent of polyethylene glycol, 0.1 to 10 percent of xylitol or sorbitol, 0.01 to 2 percent of essence and the balance of purified water.

2. A rapid onset visual dental desensitizing agent according to claim 1, consisting of the following components in weight percent: 0.5% of dyed selenium-containing bioactive glass, 3% of glycerol, 0.5% of silicon dioxide, 0.2% of a mixture of carboxymethyl cellulose and xanthan gum, 0.2% of cocamidopropyl betaine, 10% of polyethylene glycol, 0.1% of xylitol or sorbitol, 0.01% of essence and the balance of purified water.

3. A rapid onset visual dental desensitizing agent according to claim 1, consisting of the following components in weight percent: 10% of dyed selenium-containing bioactive glass, 20% of glycerol, 10% of silicon dioxide, 5% of carboxymethyl cellulose and xanthan gum mixture, 7% of cocamidopropyl betaine, 20% of polyethylene glycol, 10% of xylitol or sorbitol, 2% of essence and the balance of purified water.

4. A rapid onset visual dental desensitizing agent according to claim 1, consisting of the following components in weight percent: 10% of dyed selenium-containing bioactive glass, 15% of glycerol, 5% of silicon dioxide, 10% of a mixture of carboxymethyl cellulose and xanthan gum, 1% of cocamidopropyl betaine, 40% of polyethylene glycol, 20% of xylitol or sorbitol, 0.1% of essence and the balance of purified water.

5. A rapid onset visual dental desensitizing agent according to claim 1, consisting of the following components in weight percent: 6% of dyed selenium-containing bioactive glass, 40% of glycerol, 2% of silicon dioxide, 2% of a mixture of carboxymethyl cellulose and xanthan gum, 1% of cocamidopropyl betaine, 20% of polyethylene glycol, 1% of xylitol or sorbitol, 1% of essence and the balance of purified water.

6. A rapid onset visual dental desensitizing agent according to claim 1 or 2 or 3 or 4 or 5, wherein said mixture of carboxymethylcellulose and xanthan gum comprises, by weight, 4:1.

7. a rapid onset visual dental desensitizing agent according to claim 1 or 2 or 3 or 4 or 5, wherein said stained selenium containing bioactive glass is prepared by the process of:

(2) Preparing an ethyl orthosilicate-ethanol organic solution: dissolving tetraethoxysilane in absolute ethyl alcohol to prepare a solution with the concentration of 1.0 mol/L;

8. A rapid onset visual dental desensitizing agent according to claim 7, wherein said xerogel prepared in step (4) is prepared by removing ethanol and water from a sol under vacuum at 50 ℃ to 80 ℃.

9. A rapid onset visual dental desensitizing agent according to claim 7, wherein said step (9) is performed at 50 ℃ to 80 ℃ for 24 hours.

10. A method of preparing a rapid onset visual dental desensitizing agent according to claim 1 or 2 or 3 or 4 or 5, comprising the specific steps of: