CN116585214A - Bi-component tooth whitening gel and preparation method thereof - Google Patents

Abstract

The invention discloses a double-component tooth whitening gel and a preparation method thereof, belonging to the technical field of dental materials, wherein the whitening gel is a double-component material and comprises a component A and a component B, and the proportion is 4:1, a step of; wherein the a component comprises a thickener, peroxide or peroxide complex; the component B is a component containing casein phosphopeptide-amorphous calcium phosphate CPP-ACP. The double-component tooth whitening gel and the preparation method thereof can be stored at room temperature, and have the characteristics of rapid and efficient bleaching effect, low sensitivity, neutral PH value and good remineralization effect.

Description

A kind of two-component teeth whitening gel and preparation method thereof

technical field

The invention relates to the technical field of dental materials, in particular to a two-component tooth whitening gel and a preparation method thereof.

Background technique

Over the past 100 years, oral care has become an important part of people's daily health maintenance as the link between tooth and gum health and overall health has become increasingly apparent. A healthy smile has become a representative of personal image and even social status. Currently commonly used tooth whitening mainly includes three methods: whitening toothpaste, tooth whitening gel and whitening porcelain veneer resin restoration. Among them, whitening toothpaste is difficult to see the whitening effect in a short period of time. Although the effect of whitening porcelain veneer is obvious, part of the teeth must be ground away, which will cause certain damage to the teeth. Whitening gels include office whitening and home whitening. In the dental office, it only takes 30 minutes or 1 hour for the dentist to use the whitening agent to achieve the whitening effect visible to the naked eye. The main component of whitening agents is peroxide. Since peroxide is unstable and sensitive to light and heat, whitening products on the market must be stored in the dark and refrigerated. It takes a certain period of time for the patient to wait for the gel to return to room temperature before it can be applied, which brings a lot of inconvenience to the dentist clinically. At the same time, due to the strong oxidation of peroxide, the viscosity of the whitening gel will change significantly with time and temperature, resulting in a shorter validity period of the gel.

The whitening of teeth by peroxide is essentially a bleaching process of redox reaction with pigment, which can achieve obvious bleaching effect in a short period of time, and has attracted extensive attention from domestic and foreign researchers and related industries. However, high concentration of hydrogen peroxide will increase the sensitivity of teeth, and the reaction will demineralize the enamel at the same time. How to reduce tooth sensitivity and achieve whitening effect in a short time is the most important part of the office whitening process. Therefore, there is an urgent need to develop a whitening gel that can be stored for a long time at room temperature and can relieve postoperative tooth sensitivity.

Contents of the invention

The purpose of the present invention is to provide a two-component tooth whitening gel and its preparation method, using self-made casein phosphopeptide-amorphous calcium phosphate CPP-ACP can release active calcium and phosphate ions, easy to form hydroxyapatite, On the one hand, it can remineralize the demineralized enamel, on the other hand, it can block some dentine tubules, assist CPP-ACP to penetrate into the tooth tissue better, and combine with each other to form amorphous calcium fluoride with stronger remineralization ability Can more effectively relieve postoperative tooth sensitivity. The prepared whitening gel can be stored at room temperature, and has the characteristics of fast and efficient bleaching effect, low sensitivity, neutral pH value and good remineralization effect.

In order to achieve the above purpose, the present invention provides a two-component tooth whitening gel, which is a two-component material, including A component and B component, the ratio is 4:1; wherein A component includes whitening gel thickener and at least one peroxide or peroxide complex; component B is a component containing casein phosphopeptide-amorphous calcium phosphate CPP-ACP.

Preferably, the thickener is a high molecular polymer or copolymer with sulfonic acid groups in side groups.

Further optimization of Clariant's polymers series of thickeners, including: /> BLV; /> ACL; /> TAC.

Preferably, the A component also includes a component A desensitizer, a component A moisturizing agent and a stabilizer; the B component also includes a catalyst, a viscosity modifier, nanoparticles, preservatives, and a B component moisturizing agent , PH regulator and flavoring agent.

Preferably, the A component includes 30-50 parts of whitening agent, 0.0001-0.1 part of stabilizer, 0.5-3 parts of thickener, 0.5-5 parts of A component desensitizer, 5-20 parts A component moisturizing agent, the balance is water; the B component includes, 0.0003-0.0005 parts of catalyst, 1-5 parts of viscosity modifier, 1-5 parts of nanoparticles, 0.5-5 parts of B group Desensitizing agent, 0.1-1 part of preservative, 5-20 parts of B component moisturizing agent, 0.5-5 part of pH regulator, 0.05-1 part of flavoring agent, and the balance is water.

Preferably, the whitening agent is one or more of organic and inorganic peroxides that release active oxygen.

It is further preferred that polyvinylpyrrolidone-hydrogen peroxide polymer is the whitening component, and Ashland's Peroxydone polymer is selected. Peroxydone polymer is a drug slow-release agent that can slowly release hydrogen peroxide, which can reduce the external conditions due to temperature and light. The resulting hydrogen peroxide decomposes rapidly, is stable in most solvents, and has good affinity, bioadhesion, film-forming and formulation thickening effects.

Preferably, the stabilizer used is sodium stannate, sodium citrate, disodium edetate, sodium hydrogen phosphate, sodium dihydrogen phosphate, sodium phosphate, tripolyphosphate, sodium metaphosphate, tartaric acid, phytic acid, N -One or more of hydroxyethylethylenediaminetriacetic acid, aminotriacetic acid, organic polyphosphate, aliphatic polyoxyethylene ether;

The desensitizer of component A is fluoride (sodium fluoride, stannous fluoride, sodium monofluorophosphate), potassium ion (potassium nitrate, potassium citrate, potassium hydroxide, potassium stannate), casein phosphopeptide - one or more of amorphous calcium phosphate CPP-ACP, strontium chloride, sodium monofluorophosphate;

Further preferred: composite stabilizer, the stability of the composite stabilizer to peroxides is greater than the ability to use a single stabilizer, pyrophosphate is preferably used in conjunction with magnesium salt or tin salt while adding a chelating agent such as EDTA-2Na or EDTA -4Na can effectively stabilize peroxides. The addition amount is between 0.0001% and 0.1%. Too much addition will further promote the decomposition of peroxide; the desensitizers used in component A are potassium nitrate and sodium fluoride, and the addition amount of potassium nitrate is 0.5%- 3%, an appropriate concentration of potassium nitrate can effectively relieve tooth sensitivity, too high a concentration will lead to a higher osmotic gradient, causing the liquid to flow outward, resulting in pain in the gums. The amount of sodium fluoride added is 0.05%-0.1%; fluoride can promote the ability of enamel remineralization, but when the concentration is greater than 0.1%, it can no longer improve the degree of enamel remineralization.

The moisturizing agent of the A component is one or more of polyethylene glycol, sorbitol, glycerin, and propylene glycol.

Preferably, the catalyst is an organic or nonpolar reagent that promotes the Fenton reaction of the peroxide.

Preferably, the viscosity regulator is carboxypolymethylene polymer Acrylic acid/C10-C30 alkyl acrylate copolymer/> Polyoxyethylene/polyoxypropylene block copolymer/> and hydroxypropylcellulose/> one or more of.

Preferably, the nanoparticles are one or more of 10-100nm hydroxyapatite, 10-100nm nano-zirconia powder, and 10-100nm silicon dioxide.

Preferably, the casein phosphopeptide-amorphous calcium phosphate CPP-ACP is mixed with sodium fluoride to form component B desensitizer; wherein the casein phosphopeptide-amorphous calcium phosphate CPP-ACP is a laboratory-made product, which The preparation process is as follows: first, add 50g of high-purity CPP to 150g of buffer solution, stir at 50°C to dissolve completely, adjust the pH to neutral, then add 150g of calcium ions, stir evenly without obvious precipitation, and dry for later use.

Preferably, the moisturizing agent of the B component is one or more of polyethylene glycol, sorbitol, glycerin, and propylene glycol;

Preferably, the pH regulator is one or more of sodium hydroxide, sodium carbonate, triethanolamine, sodium citrate, sodium phosphate, sodium dihydrogen phosphate, sodium trihydrogen phosphate, sodium pyrophosphate, EDTA-4Na kind.

The present invention provides a kind of preparation method of two-component teeth whitening gel, and its preparation method is as follows:

S1. Configuration of component A: Dissolve the desensitizer and stabilizer of component A with deionized water, then add a certain amount of deionized water and whitening agent, add thickener and moisturizing agent of component A under low temperature stirring, after proper stirring Let stand for a period of time, and then centrifuge to remove air bubbles in the production process.

S2. Configure B component: Mix catalyst, B component desensitizer, PH regulator, preservative, B component humectant with a certain amount of deionized water, add viscosity modifier and fragrance after dissolving, stir at high speed and add Nanoparticles, so that the nanoparticles are evenly distributed in the gel system, and then centrifuged to remove the air bubbles during the production process.

S3. Filling components A and B: use 2.5ml, 4:1 double-barreled syringes for filling, the part of the thick tube is filled with the gel of component A, and the part of the thin tube is filled with the gel of component B, stored at room temperature, used When changing the 4:1 mixing needle, the pH value of the mixed system is between 6-8.

Therefore, the present invention adopts the above-mentioned two-component tooth whitening gel and its preparation method. The whitening gel of the present invention does not need to be stored at low temperature and its viscosity will not decrease with the influence of time and temperature. It can be stored in an oven at 50°C. After more than 14 days, the active oxygen only decreased by about 0.3%, and the viscosity decreased by only about 5%. At the same time, the bleaching gel of the present invention has low sensitivity and remineralization effect on teeth, and the use of homemade casein phosphopeptide-amorphous calcium phosphate (CPP-ACP) can effectively reduce the sensitivity of teeth in the bleaching process. Among them, the PH value of the gel after mixing is 6-8, which can avoid acid corrosion damage to the teeth on the basis of ensuring the whitening effect, so that the teeth after bleaching have better gloss and the color can be stable for a long time.

The technical solutions of the present invention will be described in further detail below with reference to the accompanying drawings and embodiments.

Description of drawings

Fig. 1 is a kind of two-component tooth whitening gel of the present invention and its preparation method embodiment cell viability after different extracts are cultured for 30min, 2h, 24h;

Fig. 2 is a picture before bleaching of isolated teeth in the embodiment of a two-component tooth whitening gel and its preparation method of the present invention;

Fig. 3 is a picture of an isolated tooth after bleaching in an embodiment of a two-component tooth whitening gel and its preparation method according to the present invention.

Detailed ways

The technical solutions of the present invention will be further described below through the accompanying drawings and embodiments.

In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments It is a part of embodiments of the present invention, but not all embodiments. The components of the embodiments of the invention generally described and illustrated in the figures herein may be arranged and designed in a variety of different configurations.

The invention provides a two-component tooth whitening gel, which is a two-component material, including A component and B component, the ratio is 4:1; wherein A component includes a thickener and at least one A peroxide or a peroxide complex; component B is a component containing casein phosphopeptide-amorphous calcium phosphate CPP-ACP.

The thickener is a polymer or copolymer with sulfonic acid groups in the side group, which is sodium acrylate/sodium acryloyl dimethyl taurate copolymer; ammonium acryloyl dimethyl taurate/behenyl polyether -25 Methacrylate Crosspolymer; Hydroxyethyl Acrylate/Sodium Acryloyldimethyltaurate Copolymer; Ammonium Acryloyldimethyltaurate/Vinylpyrrolidone Copolymer; Acryloyldimethyltaurate One or more of sodium sulfonate/vinylpyrrolidone copolymer; sodium acrylate/sodium acryloyldimethyltaurate copolymer; ammonium acryloyldimethyltaurate/carboxyethyl acrylate crosspolymer species; further preferred Clariant's polymers series of thickeners, including: /> BLV; /> ACL; /> TAC.

The A component includes whitening agent: 30-50 parts by weight; stabilizer: 0.0001-0.1 parts by weight; thickener: 0.5-3 parts by weight; Component desensitizer: 0.5-5 parts by weight; component A moisturizing agent: 5-20 parts by weight; the balance is water;

Whitening agents include hydrogen peroxide, carbamide peroxide, alkali metal peroxides, alkali metal percarbonates, alkali metal perborates, alkali metal persulfates, polyvinylpyrrolidone-hydrogen peroxide polymers; methacrylic acid One or more of allyl ester crosslinked polymer/hydrogen peroxide complexes, organic peroxyacids, and other organic and inorganic peroxides and peroxide complexes that can release active oxygen. It is further preferred that polyvinylpyrrolidone-hydrogen peroxide polymer is the whitening component, and Ashland's Peroxydone polymer is selected. Peroxydone polymer is a drug slow-release agent that can slowly release hydrogen peroxide, which can reduce the external conditions due to temperature and light. The resulting hydrogen peroxide decomposes rapidly, is stable in most solvents, and has good affinity, bioadhesion, film-forming and formulation thickening effects.

Stabilizers are sodium stannate, sodium citrate, disodium edetate, sodium hydrogen phosphate, sodium dihydrogen phosphate, sodium phosphate, tripolyphosphate, sodium metaphosphate, tartaric acid, phytic acid, N-hydroxyethyl One or more of ethylenediaminetriacetic acid, hydroxyethylidene diphosphate, aminotriacetic acid, organic polyphosphate, aliphatic polyoxyethylene ether; A component desensitizer is fluoride (sodium fluoride, fluoride Stannous chloride, sodium monofluorophosphate), potassium ions (potassium nitrate, potassium citrate, potassium hydroxide, potassium stannate), casein phosphopeptide-amorphous calcium phosphate CPP-ACP, strontium chloride, sodium monofluorophosphate One or more of salt;

The stability of compound stabilizers to peroxides is greater than the ability to use a single stabilizer. Pyrophosphate is preferably used in conjunction with magnesium salts or tin salts. Adding a chelating agent such as EDTA-2Na or EDTA-4Na can effectively stabilize peroxides. oxide. The addition amount is between 0.0001% and 0.1%. Too much addition will further promote the decomposition of peroxide; the desensitizers used in component A are potassium nitrate and sodium fluoride, and the addition amount of potassium nitrate is 0.5%- 3%, an appropriate concentration of potassium nitrate can effectively relieve tooth sensitivity, too high a concentration will lead to a higher osmotic gradient, causing the liquid to flow outward, resulting in pain in the gums. The amount of sodium fluoride added is 0.05%-0.1%; fluoride can promote the ability of enamel remineralization, but when the concentration is greater than 0.1%, it can no longer improve the degree of enamel remineralization.

The moisturizer of component A is one or more of polyethylene glycol, sorbitol, glycerin, and propylene glycol.

The B component includes: catalyst: 0.0003-0.0005 parts by weight; viscosity regulator: 1-5 parts by weight; nanoparticles: 1-5 parts by weight; B Component desensitizer: 0.5-5 parts by weight; preservative: 0.1-1 parts by weight; component B moisturizing agent: 5-20 parts by weight; pH adjustment Agent: 0.5-5 parts by weight; flavoring agent: 0.05-1 part by weight; the balance is water. The catalyst is sodium tripolyphosphate, tripotassium phosphate, manganese gluconate, ferric nitrate, manganese sulfate, sodium bicarbonate, sodium carbonate, sodium hypochlorite, potassium hypochlorite, calcium hypochlorite, barium hypochlorite, etc., which can promote the generation of peroxide. Organic or non-polar reagents for Dundon reactions. Viscosity modifier is carboxypolymethylene polymer Acrylic acid/C10-C30 alkyl acrylate copolymer/> Polyoxyethylene/polyoxypropylene block copolymer/> and hydroxypropylcellulose/> one or more of. The nanoparticles are one or more of 10-100nm hydroxyapatite, 10-100nm nano-zirconia powder, and 10-100nm silicon dioxide.

Component B desensitizer is a mixture of casein phosphopeptide-amorphous calcium phosphate CPP-ACP and sodium fluoride at a ratio of 1:0.1; among them, casein phosphopeptide-amorphous calcium phosphate CPP-ACP is a laboratory-made product , the preparation process is as follows: First, add 50g of high-purity CPP to 150g of buffer solution, stir at 50°C to dissolve completely, adjust the pH to neutral, then add 150g of calcium ions, stir evenly without obvious precipitation, and dry for later use.

The moisturizing agent of component B is one or more of polyethylene glycol, sorbitol, glycerin, propylene glycol, sorbitol, etc.;

The pH adjusting agent is one or more of sodium hydroxide, sodium carbonate, triethanolamine; sodium citrate; sodium phosphate, sodium dihydrogen phosphate, sodium trihydrogen phosphate, sodium pyrophosphate, and EDTA-4Na.

The present invention provides a kind of preparation method of two-component teeth whitening gel, and its preparation method is as follows:

S1. Configuration of component A: Dissolve the desensitizer and stabilizer of component A with deionized water, then add a certain amount of deionized water and whitening agent, add thickener and moisturizing agent of component A under low temperature stirring, after proper stirring Let it stand for a period of time to make the thickener fully swell into a gel state, and then centrifuge to remove the air bubbles in the production process.

S2. Configure B component: Mix catalyst, B component desensitizer, PH regulator, preservative, B component humectant with a certain amount of deionized water, add viscosity modifier and fragrance after dissolving, stir at high speed and add Nanoparticles, so that the nanoparticles are evenly distributed in the gel system, and then centrifuged to remove the air bubbles during the production process.

S3. Filling component A and component B: use a 2.5ml, 4:1 double-barreled syringe imported from Switzerland to fill, the thick tube part is filled with component A gel, and the thin tube part is filled with component B gel, at room temperature Store, replace the 4:1 mixing needle when using, the pH value of the mixed system is between 6-8.

Example 1

A component raw material formula:

Whitening agent: polyvinylpyrrolidone-hydrogen peroxide polymer 30-50%;

Stabilizer: EDTA-2Na, magnesium chloride, sodium metaphosphate ratio: 1:0.5:1, addition amount: 0.0001%-0.1%;

Thickener: BLV: 2-3%;

A component desensitizer: potassium nitrate: 3%, sodium fluoride: 0.1%;

A component humectant: polyethylene glycol 400: 10-20%;

Deionized water: 10%-50%;

B component raw material formula:

Catalyst: Manganese Gluconate: 0.0003%

Viscosity modifier: EZ-5 Polymer: 3%;

Nanoparticles: Hydroxyapatite: 1%; Zirconia: 1%; Fumed Silica: 0.5%;

B component desensitizer: self-made fluorine-containing CPP-ACP: 1%;

Preservatives: Sodium Benzoate: 0.5%;

Component B humectant: polyethylene glycol 400: 5%-10%;

PH regulator: sodium hydroxide and sodium bicarbonate: 0.5%-5%

Fragrance: mint flavor: 0.1%;

Deionized water: 10%-50%.

Process flow:

First prepare component A gel: dissolve component A desensitizer and stabilizer with deionized water in a clean PP or PE container, then add a certain amount of deionized water and whitening agent and add thickener and whitening agent under low temperature stirring Component A moisturizer, after proper stirring, let it stand for 8 hours to make the thickener fully swell into a gel state, and then centrifuge to remove the air bubbles in the production process. The preparation process of component B gel is similar to that of component A. First, mix the catalyst, component B desensitizer, pH regulator, preservative, and B component moisturizer with a certain amount of deionized water, and then add Viscosity modifier and flavoring agent, add nanoparticles by high-speed stirring to ensure that the nanoparticles are evenly distributed in the gel system, and then centrifuge to remove air bubbles during the production process.

Use a 2.5ml, 4:1 double-barreled syringe imported from Switzerland for filling. The thick tube is filled with component A gel, and the thin tube is filled with component B gel. Store at room temperature, no need to refrigerate, just replace the 4:1 mixing needle when using.

Other embodiment and comparative example technological process are the same as embodiment 1

Example 2

A component raw material formula:

Whitening agent: polyvinylpyrrolidone-hydrogen peroxide polymer: 30-50%;

Stabilizer: EDTA-4Na, magnesium chloride, sodium dihydrogen phosphate ratio: 1:0.5:1, the addition amount is 0.0001%-0.1%;

Thickener: TAC: 2-3%;

A component desensitizer: potassium nitrate: 0.5%, sodium fluoride: 0.1%;

A component humectant: glycerin: 5-20%;

Deionized water: 10%-50%.

B component raw material formula:

Catalyst: manganese gluconate: 0.0003%;

Viscosity modifier: EZ-5 Polymer: 3%

Nanoparticles: Hydroxyapatite: 1%; Zirconia: 1%; Fumed Silica: 0.5%;

B component desensitizer: self-made fluorine-containing CPP-ACP: 1%;

Preservatives: Sodium Benzoate: 0.5%;

Component B humectant: polyethylene glycol 400: 5%-10%;

PH regulator: sodium hydroxide and sodium bicarbonate: 0.5-5%

Fragrance: mint flavor: 0.1%;

Deionized water: 10%-50%;

Example 3

A component raw material formula:

Whitening agent: polyvinylpyrrolidone-hydrogen peroxide polymer: 30-50%;

Stabilizer: sodium stannate, phytic acid, sodium metaphosphate ratio: 1:1:1, the addition amount is 0.0001%-0.1%;

Thickener: BLV: 2-3%;

A component desensitizer: potassium nitrate: 0.5%, sodium fluoride: 0.25%;

A component humectant: polyethylene glycol 400: 10-20%;

Deionized water: 10%-50%.

B component raw material formula:

Catalyst: manganese sulfate: 0.0003%;

Viscosity modifier: Pluronic F127: 3%;

Nanoparticles: Hydroxyapatite: 1%; Zirconia: 1%; Fumed Silica: 0.5%;

B component desensitizer: self-made fluorine-containing CPP-ACP: 1%;

Preservatives: Sodium Benzoate: 0.5%;

Component B humectant: polyethylene glycol 400: 5%-10%;

PH regulator: sodium hydroxide and triethanolamine: 0.5%-5%

Fragrance: mint flavor: 0.1%;

Deionized water: 10%-50%;

Technical process is the same as embodiment 1

Example 4

A component raw material formula:

Whitening agent: polyvinylpyrrolidone-hydrogen peroxide polymer: 30-50%;

Stabilizer: sodium stannate, magnesium chloride, sodium metaphosphate ratio: 1:0.5:1, the addition amount is 0.0001%-0.1%;

Thickener: BLV: 2-3%;

A component desensitizer: potassium nitrate: 3%, sodium fluoride: 0.1%;

Moisturizing agent of component A: polyethylene glycol 400 10-20%;

Deionized water: 10%-50%.

B component raw material formula:

Catalyst: 0.0003% ferric nitrate;

Viscosity Modifier: Hydroxypropyl Cellulose HF Pharm, HXF Pharm: 3%;

Nanoparticles: Hydroxyapatite: 1%; Zirconia: 1%; Fumed Silica: 0.5%;

B component desensitizer: self-made fluorine-containing CPP-ACP: 1%;

Preservatives: Sodium Benzoate: 0.5%;

Component B humectant: polyethylene glycol 400: 5%-10%;

PH regulator: sodium hydroxide and sodium citrate: 0.5%-5%

Fragrance: mint flavor: 0.1%;

Deionized water: 10%-50%.

Comparative example 1

A component raw material formula:

Whitening agent: 30-50% hydrogen peroxide;

Stabilizer: EDTA-2Na, magnesium chloride, sodium metaphosphate ratio: 1:0.5:1, adding amount: 0.00001%;

Thickener: BLV: 2-3%;

A component desensitizer: potassium nitrate 3%, sodium fluoride: 0.1%;

A component humectant: polyethylene glycol 400: 10-20%;

Deionized water: 10%-50%.

B component raw material formula:

Catalyst: manganese gluconate: 0.0003%;

Viscosity modifier: EZ-5 Polymer: 3%;

Nanoparticles: Hydroxyapatite: 1%; Zirconia: 1%; Fumed Silica: 0.5%;

B component desensitizer: self-made fluorine-containing CPP-ACP: 1%;

Preservatives: Sodium Benzoate: 0.5%;

Component B humectant: polyethylene glycol 400: 5%-10%;

PH regulator: sodium hydroxide and sodium bicarbonate: 0.5%-5%

Fragrance: mint flavor: 0.1%;

Deionized water: 10%-50%.

Comparative example 2

A component raw material formula:

Whitening agent: polyvinylpyrrolidone-hydrogen peroxide polymer: 30-50%;

Stabilizer: EDTA-2 sodium, magnesium chloride, sodium metaphosphate ratio: 1:0.5:1, the addition amount is 0.0001%-0.1%;

Thickener: BLV: 0.1-0.3%;

A component desensitizer: potassium nitrate 3%, sodium fluoride: 0.1%;

A component humectant: polyethylene glycol 400: 10-20%;

Deionized water: 10%-50%.

B component raw material formula:

Catalyst: manganese gluconate: 0.0003%;

Viscosity modifier: EZ-5 Polymer: 3%;

Nanoparticles: hydroxyapatite 1%; zirconia 1%; fumed silica: 0.5%;

B component desensitizer: Potassium nitrate: 1%;

Preservatives: Sodium Benzoate: 0.5%;

Component B humectant: polyethylene glycol 400: 5%-10%;

PH regulator: sodium hydroxide and sodium bicarbonate: 0.5-5%

Fragrance: mint flavor: 0.1%;

Deionized water: 10%-50%.

Comparative example 3

A component gel raw material formula:

Whitening agent: polyvinylpyrrolidone-hydrogen peroxide polymer 10-20%;

Stabilizer: EDTA-2 sodium, magnesium chloride, sodium metaphosphate ratio: 1:0.5:1, the addition amount is 0.0001%-0.1%;

Thickener: BLV: 2-3%;

A component desensitizer: potassium nitrate: 3%, sodium fluoride: 0.1%

Component A Humectant: Polyethylene Glycol 400: 10-20%

Deionized water: 10%-50%

Group B gel ingredient formula:

Catalyst: manganese gluconate: 0.0003%;

Viscosity modifier: EZ-5 Polymer: 3%

Nanoparticles: hydroxyapatite 1%; zirconia 1%; fumed silica: 0.5% B component desensitizer: fluorine-containing CPP-ACP: 1%;

Preservatives: Sodium Benzoate: 0.5%

Component B humectant: Polyethylene glycol 400: 5%-10%

PH regulator: sodium hydroxide and sodium bicarbonate: 0.5%-5%

Fragrance: Mint Flavor: 0.1%

Deionized water: 10%-50%

Comparative example 4

A component gel raw material formula:

Whitening agent: polyvinylpyrrolidone-hydrogen peroxide polymer: 30-50%;

Stabilizer: magnesium chloride: 0.0001%-0.1%;

Thickener: BLV: 2-3%;

A component desensitizer: potassium nitrate 3%, sodium fluoride: 0.1%

Component A Humectant: Polyethylene Glycol 400: 10-20%

Deionized water: 10%-50%

Group B gel ingredient formula:

Catalyst: manganese gluconate: 0.0003%;

Viscosity modifier: EZ-5 Polymer: 3%

Nanoparticles: hydroxyapatite 1%; zirconia 1%; fumed silica: 0.5% B component desensitizer: fluorine-containing CPP-ACP: 1%;

Preservatives: Sodium Benzoate: 0.5%

Component B humectant: Polyethylene glycol 400: 5%-10%

PH regulator: sodium hydroxide and sodium bicarbonate: 0.5%-5%

Fragrance: Mint Flavor: 0.1%

Deionized water: 10%-50%

Comparative example 5

A component gel raw material formula:

Whitening agent: polyvinylpyrrolidone-hydrogen peroxide polymer 30-50%;

Stabilizer: EDTA-2 sodium, magnesium chloride, sodium metaphosphate ratio: 1:0.5:1, the addition amount is 0.0001%-0.1%;

Thickener: BLV: 2-3%;

Desensitizer: potassium nitrate 3%, sodium fluoride: 0.1%

Moisturizer: Macrogol 400: 10-20%

Deionized water: 10%-50%

B component gel raw material formula:

Catalyst: manganese gluconate: 0.0003%;

Viscosity modifier: EZ-5 Polymer: 3%

Nanoparticles: Hydroxyapatite 1%; Zirconia 1%; Fumed Silica: 0.5%

B component desensitizer: self-made fluorine-containing CPP-ACP: 0.1%;

Preservatives: Sodium Benzoate: 0.5%

Component B humectant: Polyethylene glycol 400: 5%-10%

PH regulator: sodium hydroxide and sodium bicarbonate: 0.5%-5%

Fragrance: Mint Flavor: 0.1%

Deionized water: 10%-50%

Comparative example 6

A component gel raw material formula:

Whitening agent: polyvinylpyrrolidone-hydrogen peroxide polymer 30-50%;

Stabilizer: the ratio of EDTA-2Na, magnesium chloride, and sodium metaphosphate: 1:0.5:1, the addition amount is 0.0001%-0.1%;

Thickener: BLV: 2-3%;

A component desensitizer: potassium nitrate 3%, sodium fluoride: 0.1%

Component A Humectant: Polyethylene Glycol 400: 10-20%

Deionized water: 10%-50%

B component gel raw material formula:

Catalyst: manganese gluconate: 0.0001%;

Viscosity modifier: EZ-5 Polymer: 3%;

Nanoparticles: hydroxyapatite 1%; zirconia 1%; fumed silica: 0.5%;

B component desensitizer: self-made fluorine-containing CPP-ACP: 1%;

Preservatives: Sodium Benzoate: 0.5%;

Component B humectant: polyethylene glycol 400: 5%-10%;

PH regulator: sodium hydroxide and sodium bicarbonate: 0.5%-5%;

Fragrance: mint flavor: 0.1%;

Deionized water: 10%-50%

1. Active oxygen content test test:

Refer to YY T0632-2008 tooth bleaching peroxide content test. The experimental process is as follows:

Weigh a certain amount of whitening gel into a 50mL beaker, add 20mL deionized water, put the beaker on a magnetic stirrer and stir evenly, then transfer it to a 250mL iodine bottle. Add 5 mL of glacial acetic acid, rinse the beaker with 100 mL of deionized water and transfer it to an iodine flask, add 2 g of potassium iodide and 2 drops of 10% ammonium molybdate, and the solution is orange-yellow. After standing in the dark for 10 minutes, take it out and titrate with the above-mentioned calibrated sodium thiosulfate. When the end point is near, add 3mL of 10% starch and continue titrating until the solution is colorless (it does not change color within 30s), and record the consumed sodium thiosulfate. The amount of standard solution, while doing a blank test.

Experimental results:

Embodiment 1-4 peroxide content: 38%

Comparative example 1-2, 4-6 peroxide content: 38%

Comparative example 3 is peroxide content: 18%

Commercially available whitening gel 1 peroxide content: 37%

Commercially available whitening gel 2 peroxide content: 40%

2. Aging test:

Examples 1-4, Comparative Examples 1-6, commercially available whitening gel 1, and commercially available whitening gel 2 were stored in an oven at 50°C for 14 days for aging experiments, and the changes in hydrogen peroxide content before and after the experiment were tested. Brookfield rotational viscometer measured the viscosity change of the sample before and after aging, and the results are shown in Table 1.

Table 1 Comparison Table of Active Oxygen Content and Viscosity Data of Examples, Comparative Examples, and Commercially Available Whitening Gels After Aging

Experimental results: Tube burst phenomenon occurred after 3 days of aging in comparative example 1, and the aging experiment could be completed for other samples. After aging, the active oxygen content of Examples 1-4 and Comparative Examples 2-6 decreased by 0.2-3.5%; the active oxygen content of commercially available whitening gel 1 decreased by 4.5%; the active oxygen content of commercially available whitening gel 2 decreased by 2%.

After aging, the viscosity of Example 1-4 decreased by 4.5-5.8%; the viscosity of Comparative Example 2-6 decreased by 5.5-23.6%; the active oxygen content of commercially available whitening gel 1 decreased by 10.3%; the active oxygen content of commercially available whitening gel 2 decreased by 14.6% %.

3. Sensitive in vitro cell experiments:

The healthy third molars extracted in outpatient service were taken, and after the teeth were repeatedly cleaned with PBS solution containing double antibodies, the pulp was separated under aseptic conditions, cut into pieces of about 1.0 mm ³ and spread on a six-well plate in α-MEM culture medium Inside;

Cultivate in an incubator at 37°C and 5% CO ₂ , and change the medium every 3 days; dilute the mixed whitening gel extract to 10%, 5%, and 2% dilutions and add them dropwise to the above medium. After culturing for 30 min, 2 h, and 24 h, the cell viability was observed, and the results are shown in Figure 1.

4. Bleaching test:

Taking isolated teeth extracted in outpatient clinics as the experimental object, the staining solution was prepared with coffee, black tea, FeCl ₃ and mucin, etc., and stained on a tooth staining machine for 7 days, thereby forming a layer of exogenous stains on the surface of the teeth. The formation mechanism and composition are close to the real stain. Then the whitening gel is mixed and applied to the surface of the teeth. After staying for 8 minutes, remove the gel with deionized water and apply it repeatedly 4 times. Use the vita color chart to compare the color changes before and after bleaching. The results are shown in Figure 2-3, which can be clearly seen After 32 minutes of whitening, it is obviously whiter than the original sample.

Therefore, the present invention adopts the above-mentioned two-component tooth whitening gel and its preparation method, adopts self-made casein phosphopeptide-amorphous calcium phosphate CPP-ACP to release active calcium and phosphate ions, and easily forms hydroxyapatite, On the one hand, it can remineralize the demineralized enamel, and on the other hand, it can block some dentine tubules, thereby reducing tooth sensitivity. Due to the existence of fluoride ions in the system, it can assist CPP-ACP to better penetrate the tooth tissue, and combine with each other to form amorphous calcium phosphate fluoride with stronger remineralization ability, which can more effectively relieve postoperative tooth sensitivity. The prepared whitening gel can be stored at room temperature, and has the characteristics of fast and efficient bleaching effect, low sensitivity, neutral pH value and good remineralization effect.

Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit them. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: it still Modifications or equivalent replacements can be made to the technical solutions of the present invention, and these modifications or equivalent replacements cannot make the modified technical solutions deviate from the spirit and scope of the technical solutions of the present invention.

Claims (10)

1. A two-component tooth whitening gel, characterized in that: the whitening gel is a bi-component material, and comprises a component A and a component B in a proportion of 4:1, a step of; wherein the a component comprises a thickener, peroxide or peroxide complex; the component B is a component containing casein phosphopeptide-amorphous calcium phosphate CPP-ACP.

2. The two-component tooth whitening gel according to claim 1, wherein the thickener is a polymer or copolymer having a sulfonic acid group on a side group.

3. A two-component tooth whitening gel according to claim 2, characterized in that: the component A also comprises a component A desensitizer, a component A humectant and a stabilizer; the component B also comprises a catalyst, a viscosity regulator, nano particles, a preservative, a component B humectant, a PH regulator and a flavoring agent.

4. A two-component tooth whitening gel according to claim 3, characterized in that: the A component comprises, by weight, 30-50 parts of a whitening agent, 0.0001-0.1 part of a stabilizing agent, 0.5-3 parts of a thickening agent, 0.5-5 parts of an A component desensitizing agent, 5-20 parts of an A component humectant and the balance of water; the component B comprises 0.0003-0.0005 part of catalyst, 1-5 parts of viscosity modifier, 1-5 parts of nano particles, 0.5-5 parts of component B desensitizer, 0.1-1 part of preservative, 5-20 parts of component B humectant, 0.5-5 parts of PH modifier, 0.05-1 part of flavoring agent and the balance of water.

5. The two-component tooth whitening gel according to claim 4, wherein the whitening agent is one or more of an organic peroxide and an inorganic peroxide which release active oxygen;

the stabilizer is one or more of sodium stannate, sodium citrate, disodium edetate, sodium hydrogen phosphate, sodium dihydrogen phosphate, sodium phosphate, tripolyphosphate, sodium metaphosphate, tartaric acid, phytic acid, N-hydroxyethyl ethylenediamine triacetic acid, amino triacetic acid, organic polyphosphate and aliphatic polyoxyethylene ether;

the desensitizer of the A component is one or more of fluoride, potassium ion, casein phosphopeptide-amorphous calcium phosphate CPP-ACP, strontium chloride and sodium monofluorophosphate;

the A-component humectant is one or more of polyethylene glycol, sorbitol, glycerol and propylene glycol.

6. A two-part tooth whitening gel according to claim 5, characterized in that: the fluoride is as follows: one or more of sodium fluoride, stannous fluoride and sodium monofluorophosphate, wherein the potassium ions are one or more of potassium nitrate, potassium citrate, potassium hydroxide and potassium stannate.

7. The two-component tooth whitening gel according to claim 6, wherein: the catalyst is an organic or inorganic reagent for promoting the Fenton reaction of peroxide;

the viscosity modifier is one or more of carboxyl polymethylene polymer, acrylic acid/C10-C30 alkyl acrylate copolymer, polyoxyethylene/polyoxypropylene segmented copolymer and hydroxypropyl cellulose.

8. The two-component tooth whitening gel according to claim 7, wherein said nanoparticles are one or more of 10-100nm hydroxyapatite, 10-100nm nano zirconia powder, 10-100nm silica.

9. A two-component tooth whitening gel according to claim 8, characterized in that: the casein phosphopeptide-amorphous calcium phosphate CPP-ACP is mixed with sodium fluoride to form a B component desensitizer;

the component B humectant is one or more of polyethylene glycol, sorbitol, glycerol and propylene glycol;

the PH regulator is one or more of sodium hydroxide, sodium carbonate, triethanolamine, sodium citrate, sodium phosphate, sodium dihydrogen phosphate, sodium pyrophosphate and EDTA-4 Na.

10. The preparation method of the bi-component tooth whitening gel is characterized by comprising the following steps of:

s1, configuring a component A: dissolving the desensitizer and the stabilizer of the component A by deionized water, adding a certain amount of deionized water and the whitening agent, adding the thickener and the humectant of the component A under low-temperature stirring, standing for a period of time after proper stirring to enable the thickener to fully swell into a gel state, and centrifuging to remove bubbles in the production process;

s2, configuring a component B: mixing the catalyst, the component B desensitizer, the PH regulator, the preservative and the component B humectant with a certain amount of deionized water, adding the viscosity regulator and the flavoring agent after dissolving, adding the nano particles by high-speed stirring, and centrifuging to remove bubbles in the production process;

s3, filling the component A and the component B: filling with 2.5ml and 4:1 double-barrel syringe, packaging with a thick tube part containing component A and a thin tube part containing component B, storing at normal temperature, and replacing 4:1 mixed needle head when in use.