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

Bi-component tooth whitening gel and preparation method thereof Download PDF

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Publication number
CN116585214A
CN116585214A CN202310526400.5A CN202310526400A CN116585214A CN 116585214 A CN116585214 A CN 116585214A CN 202310526400 A CN202310526400 A CN 202310526400A CN 116585214 A CN116585214 A CN 116585214A
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CN
China
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component
sodium
humectant
tooth whitening
whitening gel
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Chinese (zh)
Inventor
闫鹏涛
张强
吴慧
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Sino Dentex Co ltd
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Sino Dentex Co ltd
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Priority to CN202310526400.5A priority Critical patent/CN116585214A/en
Publication of CN116585214A publication Critical patent/CN116585214A/en
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/64Proteins; Peptides; Derivatives or degradation products thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04Dispersions; Emulsions
    • A61K8/042Gels
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/24Phosphorous; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/02Stomatological preparations, e.g. drugs for caries, aphtae, periodontitis
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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

Bi-component tooth whitening gel and preparation method thereof
Technical Field
The invention relates to the technical field of dental materials, in particular to a bi-component tooth whitening gel and a preparation method thereof.
Background
Over the last 100 years, oral care has become an important part of people's daily health maintenance as the link between dental and gingival health and overall health has become more and more apparent. A healthy smile has become representative of personal figures and even social status. Tooth whitening currently in common use mainly involves three modes: whitening toothpaste, tooth whitening gel and whitening porcelain veneering resin repair. The whitening toothpaste has the advantages that the whitening effect is difficult to be seen in a short time, and the whitening porcelain veneer has obvious effect, but partial teeth are ground off, so that the whitening toothpaste has certain harm to the teeth. The whitening gel comprises two modes of consulting room whitening and home whitening. In a dental office, a dentist can use the whitening agent for only 30 minutes or 1 hour to achieve a macroscopic whitening effect. The main component of the whitening agent is peroxide, and the peroxide is unstable and sensitive to light and heat, so that the whitening products on the market must be stored in a cold storage way in a dark place. The gel can be applied after a certain time is needed before the gel is used by a patient, and a plurality of inconveniences are brought to dentists clinically. Meanwhile, the viscosity of the whitening gel can be obviously changed along with time and temperature due to the strong oxidizing property of the peroxide, so that the effective period of the gel is shorter.
The peroxide is a bleaching process of oxidation-reduction reaction with pigment, which can reach obvious bleaching effect in short time, and gets the extensive attention of researchers and related industries at home and abroad. However, the high concentration of hydrogen peroxide can increase the sensitivity of teeth, the reaction can simultaneously demineralize the enamel, how to reduce the sensitivity of teeth, and the whitening effect can be achieved in a short time, so that the method is the most important part of the whitening process in a consulting room. Therefore, there is an urgent need to develop a whitening gel that can be stored for a long period of time at room temperature and can relieve the sensitivity of the teeth after the operation.
Disclosure of Invention
The invention aims to provide a bi-component tooth whitening gel and a preparation method thereof, wherein self-made casein phosphopeptide-amorphous calcium phosphate CPP-ACP can release active calcium and phosphate ions, and hydroxyapatite is easy to form, so that demineralized enamel can be remineralized on one hand, and partial dentinal tubules are blocked on the other hand, CPP-ACP is assisted to better permeate dental tissues, and amorphous calcium phosphate fluoride with stronger remineralization capability is combined with each other to effectively relieve postoperative tooth sensitivity. The prepared whitening gel can be stored at room temperature, and has the characteristics of rapid and efficient bleaching effect, low sensitivity, neutral pH value and good remineralization effect.
In order to achieve the above purpose, the invention provides a two-component tooth whitening gel, which is a two-component material and comprises a component A and a component B, wherein the proportion is 4:1, a step of; wherein the a component comprises a thickener and at least one peroxide or peroxide complex; the component B is a component containing casein phosphopeptide-amorphous calcium phosphate CPP-ACP.
Preferably, the thickener is a high molecular polymer or copolymer with a sulfonic acid group on a side group.
Further preferred is CraienA polymer series thickener comprising: />BLV;/> ACL;/> TAC。
Preferably, the A component further comprises an A component desensitizer, an A component 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.
Preferably, the A component comprises 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 of 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.
Preferably, the whitening agent is one or more of organic and inorganic peroxides releasing active oxygen.
The polyvinylpyrrolidone-hydrogen peroxide polymer is further preferable as a whitening component, and the peroxdone polymer of the leishmania is selected as a drug sustained release agent capable of slowly releasing hydrogen peroxide, so that the rapid decomposition of hydrogen peroxide caused by external conditions of temperature illumination can be reduced, the whitening composition can be stabilized in most solvents, and the whitening composition has good affinity, bioadhesion, film forming property and formula thickening effect.
Preferably, 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, aminotriacetic acid, organic polyphosphate and aliphatic polyoxyethylene ether;
the desensitizer of the A component is one or more of fluoride (sodium fluoride, stannous fluoride and sodium monofluorophosphate), potassium ions (potassium nitrate, potassium citrate, potassium hydroxide and potassium stannate), casein phosphopeptide-amorphous calcium phosphate CPP-ACP, strontium chloride and sodium monofluorophosphate;
further preferred is: complex stabilizers, which have a stability to peroxide greater than the ability of a single stabilizer, pyrophosphates are preferably used in combination with magnesium or tin salts and chelating agents such as EDTA-2Na or EDTA-4Na are added to effectively stabilize the peroxide. The addition amount is between 0.0001% and 0.1%, and excessive addition amount can further promote the decomposition of peroxide; the desensitizer used in the component A is potassium nitrate and sodium fluoride, the addition amount of the potassium nitrate is 0.5-3%, the proper concentration of the potassium nitrate can effectively relieve tooth sensitivity, and the excessive concentration can lead to higher osmotic gradient, so that liquid flows outwards, and the gum is painful. The addition amount of sodium fluoride is 0.05% -0.1%; fluoride can promote the ability of enamel to remineralize but at concentrations greater than 0.1% it can no longer promote the extent of enamel remineralization.
The A-component humectant is one or more of polyethylene glycol, sorbitol, glycerol and propylene glycol.
Preferably, the catalyst is an organic or electrodeless reagent that promotes the Fenton reaction of the peroxide.
Preferably, the viscosity modifier is a carboxypolymethylene polymerAcrylic acid/C10-C30 alkyl acrylate copolymer +.>Polyoxyethylene/polyoxypropylene block copolymer->Hydroxypropyl cellulose->One or more of the following.
Preferably, the nano particles are one or more of hydroxyapatite with the wavelength of 10-100nm, nano zirconia powder with the wavelength of 10-100nm and silicon dioxide with the wavelength of 10-100 nm.
Preferably, the casein phosphopeptide-amorphous calcium phosphate CPP-ACP is mixed with sodium fluoride to form a B component desensitizer; the casein phosphopeptide-amorphous calcium phosphate CPP-ACP is a self-made product in a laboratory, and the preparation process is as follows: firstly, 50g of high-purity CPP is added with 150g of buffer solution, stirred at 50 ℃ for complete dissolution, pH is adjusted to be neutral, then 150g of calcium ions are added, stirred uniformly and no obvious precipitate exists, and dried for standby.
Preferably, the humectant of the component B is one or more of polyethylene glycol, sorbitol, glycerol 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 pyrophosphate and EDTA-4 Na.
The invention provides a preparation method of a bi-component tooth whitening gel, which comprises the following steps:
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, and centrifuging to remove bubbles in the production process.
S2, configuring a component B: the catalyst, the component B desensitizer, the PH regulator, the preservative and the component B humectant are mixed with a certain amount of deionized water, the viscosity regulator and the flavoring agent are added after the components are dissolved, the nano particles are added by high-speed stirring, so that the nano particles are uniformly distributed in a gel system, and then the air bubbles in the production process are removed by centrifugation.
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 A component gel and a thin tube part containing B component gel, storing at normal temperature, and replacing 4:1 mixing needle when in use, wherein the pH value of the mixed system is between 6 and 8.
Therefore, the double-component tooth whitening gel and the preparation method thereof are adopted, the whitening gel does not need to be stored at low temperature, the viscosity does not decrease along with the influence of time and temperature, the gel can be stored for more than 14 days after being placed in a 50 ℃ oven, the active oxygen only decreases by about 0.3%, and the viscosity decreases by about 5%. Meanwhile, the bleaching gel has low sensitivity and remineralization on teeth, and home-made casein phosphopeptide-amorphous calcium phosphate (CPP-ACP) can effectively reduce the sensitivity of the teeth in the bleaching process, and the pH value of the gel after mixing is 6-8 in the use process, so that the whitening effect is ensured, acid corrosion injury to the teeth is avoided, and the bleached teeth have better glossiness and long-time stable color.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 shows cell viability after culturing different extracting solutions for 30min, 2h and 24h in a two-component tooth whitening gel and a preparation method thereof according to an embodiment of the invention;
FIG. 2 is a photograph of a two-component tooth whitening gel according to an embodiment of the present invention before bleaching of an in vitro tooth;
fig. 3 is a photograph of a bi-component tooth whitening gel according to an embodiment of the present invention after bleaching of an in vitro tooth.
Detailed Description
The technical scheme of the invention is further described below through the attached drawings and the embodiments.
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
The invention provides a bi-component tooth whitening gel which 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 and at least one peroxide or peroxide complex; the component B is a component containing casein phosphopeptide-amorphous calcium phosphate CPP-ACP.
The thickener is a high molecular polymer or copolymer with a sulfonic acid group on a side group, and is a sodium acrylate/sodium acryloyldimethyl taurate copolymer; ammonium acryloyldimethyl taurate/behenate polyether-25 methacrylate cross-linked polymer; hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer; ammonium acryloyldimethyl taurate/vinyl pyrrolidone copolymer; sodium acryloyldimethyl taurate/vinyl pyrrolidone copolymer; sodium acrylate/sodium acryloyldimethyl taurate copolymer; one or more of the ammonium acryloyldimethyl taurate/carboxyethyl acrylate cross-linked polymers; further preferred is CraienA polymer series thickener comprising: /> BLV;/>ACL;/>TAC。
The A component comprises a whitening agent: 30-50 parts by weight; stabilizing agent: 0.0001-0.1 part by weight; and (3) a thickening agent: 0.5-3 parts by weight; a desensitizer of the A component: 0.5-5 parts by weight; a component A humectant: 5-20 parts by weight; the balance being water;
whitening agents include hydrogen peroxide, carbamide peroxide, alkali metal peroxides, alkali metal percarbonates, alkali metal perborates, alkali metal persulfates, polyvinylpyrrolidone-hydrogen peroxide polymers; allyl methacrylate crosslinked polymer/hydrogen peroxide complex, organic peroxide capable of releasing active oxygen, or one or more of organic peroxide and peroxide complex. The polyvinylpyrrolidone-hydrogen peroxide polymer is further preferable as a whitening component, and the peroxdone polymer of the leishmania is selected as a drug sustained release agent capable of slowly releasing hydrogen peroxide, so that the rapid decomposition of hydrogen peroxide caused by external conditions of temperature illumination can be reduced, the whitening composition can be stabilized in most solvents, and the whitening composition has good affinity, bioadhesion, film forming property and formula thickening effect.
The stabilizer is one or more of sodium stannate, sodium citrate, disodium ethylenediamine tetraacetate, sodium hydrogen phosphate, sodium dihydrogen phosphate, sodium phosphate, tripolyphosphate, sodium metaphosphate, tartaric acid, phytic acid, N-hydroxyethyl ethylenediamine triacetic acid, hydroxyethylidene diphosphate, aminotriacetic acid, organic polyphosphate and aliphatic polyoxyethylene ether; the desensitizer of the component A is one or more of fluoride (sodium fluoride, stannous fluoride and sodium monofluorophosphate), potassium ions (potassium nitrate, potassium citrate, potassium hydroxide and potassium stannate), casein phosphopeptide-amorphous calcium phosphate CPP-ACP, strontium chloride and sodium monofluorophosphate;
the stability of the compound stabilizer to peroxide is greater than that of a single stabilizer, and pyrophosphate is preferably used in combination with magnesium salt or tin salt while chelating agent such as EDTA-2Na or EDTA-4Na is added to effectively stabilize peroxide. The addition amount is between 0.0001% and 0.1%, and excessive addition amount can further promote the decomposition of peroxide; the desensitizer used in the component A is potassium nitrate and sodium fluoride, the addition amount of the potassium nitrate is 0.5-3%, the proper concentration of the potassium nitrate can effectively relieve tooth sensitivity, and the excessive concentration can lead to higher osmotic gradient, so that liquid flows outwards, and the gum is painful. The addition amount of sodium fluoride is 0.05% -0.1%; fluoride can promote the ability of enamel to remineralize but at concentrations greater than 0.1% it can no longer promote the extent of enamel remineralization.
The humectant of the component A is one or more of polyethylene glycol, sorbitol, glycerol and propylene glycol.
The component B comprises a catalyst: 0.0003 to 0.0005 weight portions; viscosity modifier: 1-5 parts by weight; nanoparticles: 1-5 parts by weight; b component desensitizer: 0.5-5 parts by weight; preservative: 01-1 parts by weight; and (3) a B-component humectant: 5-20 parts by weight; pH regulator: 0.5-5 parts by weight of a lubricant; flavoring agent: 0.05-1 part by weight; the balance being water. The catalyst is an organic or electrodeless reagent which can promote the Fenton reaction of peroxide, such as sodium tripolyphosphate, tripotassium phosphate, manganese gluconate, ferric nitrate, manganese sulfate, sodium bicarbonate, sodium carbonate, sodium hypochlorite, potassium hypochlorite, calcium hypochlorite, barium hypochlorite and the like. The viscosity modifier is carboxyl polymethylene polymerAcrylic acid/C10-C30 alkyl acrylate copolymer +.>Polyoxyethylene/polyoxypropylene block copolymer->Hydroxypropyl cellulose->One or more of the following. The nanometer particles are one or more of hydroxyapatite of 10-100nm, nanometer zirconia powder of 10-100nm and silicon dioxide of 10-100 nm.
The desensitizer of the component B is a mixture of casein phosphopeptide-amorphous calcium phosphate CPP-ACP and sodium fluoride in a mixing ratio of 1:0.1; the casein phosphopeptide-amorphous calcium phosphate CPP-ACP is a self-made product in a laboratory, and the preparation process is as follows: firstly, 50g of high-purity CPP is added with 150g of buffer solution, stirred at 50 ℃ for complete dissolution, pH is adjusted to be neutral, then 150g of calcium ions are added, stirred uniformly and no obvious precipitate exists, and dried for standby.
The humectant of the component B is one or more of polyethylene glycol, sorbitol, glycerin, propylene glycol, sorbitol and the like;
the PH regulator is sodium hydroxide, sodium carbonate and triethanolamine; sodium citrate; sodium phosphate, sodium dihydrogen phosphate, sodium pyrophosphate, EDTA-4 Na.
The invention provides a preparation method of a bi-component tooth whitening gel, which comprises the following steps:
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: the catalyst, the component B desensitizer, the PH regulator, the preservative and the component B humectant are mixed with a certain amount of deionized water, the viscosity regulator and the flavoring agent are added after the components are dissolved, the nano particles are added by high-speed stirring, so that the nano particles are uniformly distributed in a gel system, and then the air bubbles in the production process are removed by centrifugation.
S3, filling the component A and the component B: filling with 2.5ml double-barrel syringe with 4:1 inlet of Switzerland, packaging with coarse tube part containing A component gel and fine tube part containing B component gel, storing at normal temperature, and replacing 4:1 mixing needle when in use, wherein pH value of the mixed system is 6-8.
Example 1
The formula of the raw materials of the component A comprises the following components:
whitening agent: 30-50% of polyvinylpyrrolidone-hydrogen peroxide polymer;
stabilizing agent: EDTA-2Na, magnesium chloride and sodium metaphosphate in the following proportion: 1:0.5:1, and the addition amount is 0.0001% -0.1%;
and (3) a thickening agent: BLV:2-3%;
a desensitizer of the A component: potassium nitrate: 3%, sodium fluoride: 0.1%;
a component A humectant: polyethylene glycol 400:10-20%;
deionized water: 10% -50%;
the formula of the raw materials of the component B comprises the following steps:
catalyst: manganese gluconate: 0.0003%
Viscosity modifier:EZ-5 Polymer: 3%;
nanoparticles: hydroxyapatite: 1%; zirconia: 1%; fumed silica: 0.5%;
b component desensitizer: homemade fluorine-containing CPP-ACP:1%;
preservative: sodium benzoate: 0.5%;
and (3) a B-component humectant: polyethylene glycol 400:5% -10%;
pH regulator: sodium hydroxide and sodium bicarbonate: 0.5 to 5 percent
Flavoring agent: mint flavor: 0.1%;
deionized water: 10% -50%.
The process flow comprises the following steps:
first, a component A gel is prepared: dissolving the desensitizer and the stabilizer of the component A in clean PP or PE containers by using 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 8 hours after proper stirring to enable the thickener to fully swell into a gel state, and centrifuging to remove bubbles in the production process. The preparation flow of the component B gel is similar to that of the component A, a catalyst, a component B desensitizer, a PH regulator, a preservative and a component B humectant are mixed with a certain amount of deionized water, after the mixture is fully dissolved, a viscosity regulator and an essence flavoring agent are added, nano particles are added by high-speed stirring, the nano particles are ensured to be uniformly distributed in a gel system, and then air bubbles in the production process are removed by centrifugation.
Filling with 2.5ml double syringe of 4:1, coarse tube part containing A component gel, and fine tube part containing B component gel. The needle is stored at normal temperature without refrigeration, and the 4:1 mixed needle is replaced when in use.
Other examples and comparative examples Process flows are the same as in example 1
Example 2
The formula of the raw materials of the component A comprises the following components:
whitening agent: polyvinylpyrrolidone-hydrogen peroxide polymer: 30-50%;
stabilizing agent: EDTA-4Na, magnesium chloride and sodium dihydrogen phosphate: the addition amount of 1:0.5:1 is 0.0001% -0.1%;
and (3) a thickening agent: TAC:2-3%;
a desensitizer of the A component: potassium nitrate: 0.5 percent of sodium fluoride: 0.1%;
a component A humectant: glycerol: 5-20%;
deionized water: 10% -50%.
The formula of the raw materials of the component B comprises the following steps:
catalyst: manganese gluconate: 0.0003%;
viscosity modifier:EZ-5 Polymer: 3%
Nanoparticles: hydroxyapatite: 1%; zirconia: 1%; fumed silica: 0.5%;
b component desensitizer: homemade fluorine-containing CPP-ACP:1%;
preservative: sodium benzoate: 0.5%;
and (3) a B-component humectant: polyethylene glycol 400:5% -10%;
pH regulator: sodium hydroxide and sodium bicarbonate: 0.5-5%
Flavoring agent: mint flavor: 0.1%;
deionized water: 10% -50%;
example 3
The formula of the raw materials of the component A comprises the following components:
whitening agent: polyvinylpyrrolidone-hydrogen peroxide polymer: 30-50%;
stabilizing agent: the proportion of sodium stannate, phytic acid and sodium metaphosphate is as follows: the addition amount of 1:1:1 is 0.0001% -0.1%;
and (3) a thickening agent: BLV:2-3%;
a desensitizer of the A component: potassium nitrate: 0.5 percent of sodium fluoride: 0.25%;
a component A humectant: polyethylene glycol 400:10-20%;
deionized water: 10% -50%.
The formula of the raw materials of the component B comprises the following steps:
catalyst: manganese sulfate: 0.0003%;
viscosity modifier: pluronic F127:3%;
nanoparticles: hydroxyapatite: 1%; zirconia: 1%; fumed silica: 0.5%;
b component desensitizer: homemade fluorine-containing CPP-ACP:1%;
preservative: sodium benzoate: 0.5%;
and (3) a B-component humectant: polyethylene glycol 400:5% -10%;
pH regulator: sodium hydroxide and triethanolamine: 0.5 to 5 percent
Flavoring agent: mint flavor: 0.1%;
deionized water: 10% -50%;
process flow is the same as in example 1
Example 4
The formula of the raw materials of the component A comprises the following components:
whitening agent: polyvinylpyrrolidone-hydrogen peroxide polymer: 30-50%;
stabilizing agent: the proportion of sodium stannate, magnesium chloride and sodium metaphosphate is as follows: the addition amount of 1:0.5:1 is 0.0001% -0.1%;
and (3) a thickening agent: BLV:2-3%;
a desensitizer of the A component: potassium nitrate: 3%, sodium fluoride: 0.1%;
a component A humectant: polyethylene glycol 40010-20%;
deionized water: 10% -50%.
The formula of the raw materials of the component B comprises the following steps:
catalyst: 0.0003% of ferric nitrate;
viscosity modifier: hydroxypropyl celluloseHF Pharm,HXF Pharm:3%;
Nanoparticles: hydroxyapatite: 1%; zirconia: 1%; fumed silica: 0.5%;
b component desensitizer: homemade fluorine-containing CPP-ACP:1%;
preservative: sodium benzoate: 0.5%;
and (3) a B-component humectant: polyethylene glycol 400:5% -10%;
pH regulator: sodium hydroxide and sodium citrate: 0.5 to 5 percent
Flavoring agent: mint flavor: 0.1%;
deionized water: 10% -50%.
Comparative example 1
The formula of the raw materials of the component A comprises the following components:
whitening agent: 30-50% of hydrogen peroxide;
stabilizing agent: EDTA-2Na, magnesium chloride and sodium metaphosphate in the following proportion: 1:0.5:1, the addition amount is 0.00001%;
and (3) a thickening agent: BLV:2-3%;
a desensitizer of the A component: potassium nitrate 3%, sodium fluoride: 0.1%;
a component A humectant: polyethylene glycol 400:10-20%;
deionized water: 10% -50%.
The formula of the raw materials of the component B comprises the following steps:
catalyst: manganese gluconate: 0.0003%;
viscosity modifier:EZ-5 Polymer: 3%;
nanoparticles: hydroxyapatite: 1%; zirconia: 1%; fumed silica: 0.5%;
b component desensitizer: homemade fluorine-containing CPP-ACP:1%;
preservative: sodium benzoate: 0.5%;
and (3) a B-component humectant: polyethylene glycol 400:5% -10%;
pH regulator: sodium hydroxide and sodium bicarbonate: 0.5 to 5 percent
Flavoring agent: mint flavor: 0.1%;
deionized water: 10% -50%.
Comparative example 2
The formula of the raw materials of the component A comprises the following components:
whitening agent: polyvinylpyrrolidone-hydrogen peroxide polymer: 30-50%;
stabilizing agent: EDTA-2 sodium, magnesium chloride and sodium metaphosphate in the following proportion: the addition amount of 1:0.5:1 is 0.0001% -0.1%;
and (3) a thickening agent: BLV:0.1-0.3%;
a desensitizer of the A component: potassium nitrate 3%, sodium fluoride: 0.1%;
a component A humectant: polyethylene glycol 400:10-20%;
deionized water: 10% -50%.
The formula of the raw materials of the component B comprises the following steps:
catalyst: manganese gluconate: 0.0003%;
viscosity modifier:EZ-5 Polymer: 3%;
nanoparticles: 1% of hydroxyapatite; zirconia 1%; fumed silica: 0.5%;
b component desensitizer: potassium nitrate: 1%;
preservative: sodium benzoate: 0.5%;
and (3) a B-component humectant: polyethylene glycol 400:5% -10%;
pH regulator: sodium hydroxide and sodium bicarbonate: 0.5-5%
Flavoring agent: mint flavor: 0.1%;
deionized water: 10% -50%.
Comparative example 3
The gel raw material formula of the component A comprises the following components:
whitening agent: 10-20% of polyvinylpyrrolidone-hydrogen peroxide polymer;
stabilizing agent: EDTA-2 sodium, magnesium chloride and sodium metaphosphate in the following proportion: the addition amount of 1:0.5:1 is 0.0001% -0.1%;
and (3) a thickening agent: BLV:2-3%;
a desensitizer of the A component: potassium nitrate: 3%, sodium fluoride: 0.1%
A component A humectant: polyethylene glycol 400:10-20%
Deionized water: 10 to 50 percent of
The formula of the component raw materials of the gel group B comprises:
catalyst: manganese gluconate: 0.0003%;
viscosity modifier:EZ-5 Polymer: 3%
Nanoparticles: 1% of hydroxyapatite; zirconia 1%; fumed silica: 0.5% of a B component desensitizer: fluorine-containing CPP-ACP:1%;
preservative: sodium benzoate: 0.5%
And (3) a B-component humectant: polyethylene glycol 400:5 to 10 percent
pH regulator: sodium hydroxide and sodium bicarbonate: 0.5 to 5 percent
Flavoring agent: mint flavor: 0.1%
Deionized water: 10 to 50 percent of
Comparative example 4
The gel raw material formula of the component A comprises the following components:
whitening agent: polyvinylpyrrolidone-hydrogen peroxide polymer: 30-50%;
stabilizing agent: magnesium chloride: 0.0001% -0.1%;
and (3) a thickening agent: BLV:2-3%;
a desensitizer of the A component: potassium nitrate 3%, sodium fluoride: 0.1%
A component A humectant: polyethylene glycol 400:10-20%
Deionized water: 10 to 50 percent of
The formula of the component raw materials of the gel group B comprises:
catalyst: manganese gluconate: 0.0003%;
viscosity modifier:EZ-5 Polymer: 3%
Nanoparticles: 1% of hydroxyapatite; zirconia 1%; fumed silica: 0.5% of a B component desensitizer: fluorine-containing CPP-ACP:1%;
preservative: sodium benzoate: 0.5%
And (3) a B-component humectant: polyethylene glycol 400:5 to 10 percent
pH regulator: sodium hydroxide and sodium bicarbonate: 0.5 to 5 percent
Flavoring agent: mint flavor: 0.1%
Deionized water: 10 to 50 percent of
Comparative example 5
The gel raw material formula of the component A comprises the following components:
whitening agent: 30-50% of polyvinylpyrrolidone-hydrogen peroxide polymer;
stabilizing agent: EDTA-2 sodium, magnesium chloride and sodium metaphosphate in the following proportion: the addition amount of 1:0.5:1 is 0.0001% -0.1%;
and (3) a thickening agent: BLV:2-3%;
desensitizing agent: potassium nitrate 3%, sodium fluoride: 0.1%
Humectant: polyethylene glycol 400:10-20%
Deionized water: 10 to 50 percent of
The formula of the gel raw materials of the component B comprises the following steps:
catalyst: manganese gluconate: 0.0003%;
viscosity modifier:EZ-5 Polymer: 3%
Nanoparticles: 1% of hydroxyapatite; zirconia 1%; fumed silica: 0.5%
B component desensitizer: homemade fluorine-containing CPP-ACP:0.1%;
preservative: sodium benzoate: 0.5%
And (3) a B-component humectant: polyethylene glycol 400:5 to 10 percent
pH regulator: sodium hydroxide and sodium bicarbonate: 0.5 to 5 percent
Flavoring agent: mint flavor: 0.1%
Deionized water: 10 to 50 percent of
Comparative example 6
The gel raw material formula of the component A comprises the following components:
whitening agent: 30-50% of polyvinylpyrrolidone-hydrogen peroxide polymer;
stabilizing agent: the proportion of EDTA-2Na, magnesium chloride and sodium metaphosphate is as follows: the addition amount of 1:0.5:1 is 0.0001% -0.1%;
and (3) a thickening agent: BLV:2-3%;
a desensitizer of the A component: potassium nitrate 3%, sodium fluoride: 0.1%
A component A humectant: polyethylene glycol 400:10-20%
Deionized water: 10 to 50 percent of
The formula of the gel raw materials of the component B comprises the following steps:
catalyst: manganese gluconate: 0.0001%;
viscosity modifier:EZ-5 Polymer: 3%;
nanoparticles: 1% of hydroxyapatite; zirconia 1%; fumed silica: 0.5%;
b component desensitizer: homemade fluorine-containing CPP-ACP:1%;
preservative: sodium benzoate: 0.5%;
and (3) a B-component humectant: polyethylene glycol 400:5% -10%;
pH regulator: sodium hydroxide and sodium bicarbonate: 0.5% -5%;
flavoring agent: mint flavor: 0.1%;
deionized water: 10 to 50 percent of
1. Reactive oxygen content test:
reference YY T0632-2008 extradental bleaching peroxide content test. The experimental procedure was as follows:
a certain amount of whitening gel is weighed into a 50mL beaker, 20mL deionized water is added, the beaker is placed on a magnetic stirrer and stirred uniformly, and the beaker is transferred into a 250mL iodometric bottle. 5mL glacial acetic acid was added, the beaker was rinsed with 100mL deionized water and transferred to an iodometric flask, 2g potassium iodide was added, 2 drops of 10% amine molybdate, and the solution was orange-yellow. After 10min of placement in the dark, the solution was taken out and titrated with the calibrated sodium thiosulfate, 3mL of 10% starch was added near the end point, the titration was continued until the solution was colorless (no discoloration within 30 s), the amount of the consumed sodium thiosulfate standard solution was recorded, and a blank test was performed.
Experimental results:
examples 1-4 peroxide content: 38%
Comparative examples 1-2,4-6 peroxide content: 38%
Comparative example 3 is peroxide content: 18%
Commercial whitening gel 1 peroxide content: 37%
Commercial whitening gel 2 peroxide content: 40 percent of
2. Aging test:
the products of examples 1 to 4, comparative examples 1 to 6, and commercial whitening gel 1 and commercial whitening gel 2 were stored in an oven at 50℃for 14 days to conduct an aging test, the changes in hydrogen peroxide content before and after the test were measured, and the changes in viscosity before and after aging were measured using a Brookfield rotational viscometer, bohler, america, and the results are shown in Table 1.
Table 1 comparative table of active oxygen content and viscosity data of examples, comparative examples and commercial whitening gels after aging
Experimental results: the tube explosion phenomenon occurs after the comparative example 1 is aged for 3 days, and other samples can complete the aging experiment. The active oxygen content of examples 1-4 and comparative examples 2-6 decreases by 0.2-3.5% after aging; the active oxygen content of the commercial whitening gel 1 is reduced by 4.5 percent; the active oxygen content of the commercial whitening gel 2 is reduced by 2 percent.
The viscosity of examples 1-4 decreased by 4.5-5.8% after aging; comparative examples 2-6 decreased in viscosity by 5.5-23.6%; the active oxygen content of the commercial whitening gel 1 is reduced by 10.3 percent; the active oxygen content of the commercial whitening gel 2 is reduced by 14.6 percent.
3. Sensitive in vitro cell assay:
taking healthy third molar for outpatient extraction, repeatedly cleaning teeth with PBS solution containing double antibodies, separating dental pulp under aseptic condition, and cutting into pieces of about 1.0mm 3 Is flatly paved in a six-hole plate of alpha-MEM culture solution;
37℃、5%CO 2 culturing in incubator (1 time after every 3 days; the mixed whitening gel extract was diluted to 10%, 5% and 2% and then added dropwise to the above culture medium, and the cell viability was observed after culturing for 30min, 2h and 24h, and the results are shown in fig. 1.
4. Bleaching test:
taking the isolated tooth removed in clinic as an experimental object, and using coffee, black tea and FeCl 3 And mucin, etc., to form a stain, and staining the stain on a dental dyeing machine for 7 days, thereby forming an exogenous stain on the surface of the tooth, the formation mechanism and the composition of which are similar to those of a true stain. And then the whitening gel is mixed and smeared on the tooth surface, the gel is removed by deionized water after the mixture stays for 8min, the repeated smearing is carried out for 4 times, the color change before and after bleaching is compared by using a vita color chart, and the result is shown in fig. 2-3, so that the whitening sample is obviously whiter than the initial sample after 32min of whitening.
Therefore, the double-component tooth whitening gel and the preparation method thereof are adopted, and self-made casein phosphopeptide-amorphous calcium phosphate CPP-ACP can release active calcium and phosphate ions, so that hydroxyapatite is easy to form, on one hand, demineralized enamel can be remineralized, and on the other hand, part of dentin tubules are blocked, so that tooth sensitivity is reduced. Because of the existence of fluoride ions in the system, CPP-ACP can be assisted to better permeate dental tissues and be combined with each other to form amorphous calcium phosphate fluoride with stronger remineralization capability, so that postoperative tooth sensitivity can be effectively relieved. The prepared whitening gel can be stored at room temperature, and has the characteristics of rapid and efficient bleaching effect, low sensitivity, neutral pH value and good remineralization effect.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the 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.
CN202310526400.5A 2023-05-11 2023-05-11 Bi-component tooth whitening gel and preparation method thereof Pending CN116585214A (en)

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