CN111759751B - Whitening toothpaste excited by blue light LED and preparation method thereof - Google Patents
Whitening toothpaste excited by blue light LED and preparation method thereof Download PDFInfo
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- CN111759751B CN111759751B CN202010653528.4A CN202010653528A CN111759751B CN 111759751 B CN111759751 B CN 111759751B CN 202010653528 A CN202010653528 A CN 202010653528A CN 111759751 B CN111759751 B CN 111759751B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/29—Titanium; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/41—Amines
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/81—Preparation or application process involves irradiation
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/82—Preparation or application process involves sonication or ultrasonication
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/84—Products or compounds obtained by lyophilisation, freeze-drying
Abstract
The invention provides a whitening toothpaste excited by a blue light LED and a preparation method thereof. The toothpaste product takes titanium dioxide as a main whitening agent, can quickly generate oxidation-reduction reaction on discolored teeth under the excitation of blue light, and simultaneously has the following technical advantages: 1. can respond to visible light, can generate oxidation-reduction action without ultraviolet excitation, and is more healthy and safe. 2. The method has the advantages of simple and safe process, no need of adding organic solvent, simple operation method, low requirement on equipment and suitability for large-scale production and industrial popularization.
Description
The application is a divisional application of a patent application entitled whitening toothpaste with visible light excited redox reaction and a preparation method thereof, and the application date of the original application is 2017, 08 and 03 months, and the application number is 201710655705.0.
Technical Field
The invention relates to the technical field of toothpaste preparation, and simultaneously relates to the technical field of tooth whitening, in particular to whitening toothpaste excited by blue light LEDs and a preparation method thereof
Background
Tooth whitening has become a common cosmetic requirement because the color and luster of teeth directly affect the facial appearance, and with the development of medical technology, a plurality of repair means for discolored teeth are formed in recent years, wherein the applications of covering whitening and chemical bleaching are common. The main methods of masked whitening include veneering and full crown restoration, both of which require extensive grinding of the teeth and thus irreversible damage to the structure of the teeth themselves. The chemical bleaching method is relatively safe, but depends on chemical reaction, so the reaction design is very important, and if the reactant components are not reasonable, the whitening effect is not ideal, and even side effects can be generated.
The cold light whitening is a chemical bleaching technology based on a photocatalytic reaction, and the method uses 480-520 nm wavelength high-intensity blue light to irradiate a reagent which takes hydrogen peroxide or carbamide peroxide as a main component to generate an oxidation-reduction reaction, and removes pigments attached to the surface and the deep layer of teeth through dentin tubules, thereby achieving the whitening effect. Although this method has shown a good tooth-cleaning effect, there are side effects such as enamel demineralization, soft tissue irritation, tooth sensitivity, acute pulpitis, etc. in practical use because the reactive ingredients are not safe enough. Therefore, how to provide a whitening toothpaste which is catalyzed by mild light and has safe and effective ingredients is a technical problem which needs to be solved urgently by the technical personnel in the field.
Disclosure of Invention
The invention aims to provide whitening toothpaste with oxidation-reduction reaction excited by visible light and a preparation method thereof aiming at overcoming the technical defects in the prior art, and aims to solve the technical problem that the whitening effect is poor due to unreasonable reactant design in the prior art for tooth bleaching by photocatalytic oxidation reaction.
Another technical problem to be solved by the present invention is that tooth bleaching by photocatalytic oxidation in the prior art has damage to enamel due to unreasonable design of reactants.
The invention also aims to solve the technical problem that tooth bleaching by photocatalytic oxidation reaction in the prior art can only be carried out under the excitation of blue light or ultraviolet rays, and the light has strong irritation to human bodies.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a whitening toothpaste capable of exciting redox reaction by visible light, wherein the visible light is yellow light, the toothpaste contains porous zinc oxide with the mass fraction of 3%, the average pore diameter of the porous zinc oxide is 5 μm, and the average particle size of the porous zinc oxide is 15 μm. In this technical solution, the yellow light is strictly defined as light having a wavelength in the range of 580nm to 595 nm.
A preparation method of the whitening toothpaste with the oxidation-reduction reaction excited by visible light comprises the following steps:
1) With Zn (NO) 3 ) 2 ·6H 2 O、NH 3 ·H 2 In a ratio of 10 3 ) 2 ·6H 2 O、NH 3 ·H 2 Dissolving O and hexamethylenetetramine in deionized water, and stirring for 10min;
2) Then reacting the product obtained in the step 1) for 15min at a constant temperature of 65 ℃;
3) Adding sodium citrate and hydroxypropyl methyl cellulose into the mixture according to the proportion that the dosage of the sodium citrate, the hydroxypropyl methyl cellulose and the deionized water in the step 1) is 0.14;
4) And then, carrying out vacuum freeze drying on the product obtained in the step 3), and then placing the product into a microwave oven for microwave treatment for 15min to obtain the whitening toothpaste with visible light excited redox reaction.
Preferably, zn (NO) in step 1) 3 ) 2 ·6H 2 O、NH 3 ·H 2 The adding sequence of O and hexamethylenetetramine to the deionized water is NH in sequence 3 ·H 2 O、Zn(NO 3 ) 2 ·6H 2 O, hexamethylene tetramine.
Preferably, the isothermal reaction in step 2) and the isothermal reaction in step 3) are both performed under water bath conditions.
Preferably, the container in which the system is positioned is sealed by a cover during the stirring in the step 1) and the isothermal reaction in the step 2).
Preferably, step 1) is performed after stirring for 10min until the solution is clear, and step 2) is performed.
The other whitening toothpaste is formed by exciting a redox reaction by visible light, wherein the visible light is blue light, and the toothpaste contains 5% of titanium dioxide by mass. In this solution, the blue light is strictly defined as light having a wavelength in the range of 450 to 480 nm.
A preparation method of the whitening toothpaste with the oxidation-reduction reaction excited by visible light comprises the following steps:
1) Uniformly mixing the nano titanium dioxide, the dopamine hydrochloride and the pure water in a container according to the proportion of 0.08;
2) Adding hexamethylenetetramine into the solution, ultrasonically oscillating for 5min, sealing the container, and then carrying out water bath at 90 ℃ for 3h; the addition amount of the hexamethylene tetramine is 10 times of the weight of the dopamine hydrochloride in the step 1);
3) Washing the product obtained in the step 2) with pure water for 2 times, then washing with absolute ethyl alcohol for 2 times, then washing with pure water for 2 times, and freeze-drying to obtain the whitening toothpaste with visible light excited redox reaction.
Preferably, the container in step 1) is a conical flask.
Preferably, the toothpaste can be directly dissolved in water for use, and can also be prepared into gel, paste and the like by adding pharmaceutical excipients.
In the above technical scheme, the visible light-excited redox reaction is a photocatalytic reaction, and specifically belongs to an oxidation reaction catalyzed by visible light.
The invention provides whitening toothpaste with visible light excited redox reaction and a preparation method thereof. The toothpaste product contains porous zinc oxide, can rapidly generate oxidation-reduction reaction on discolored teeth under the excitation of yellow light, and simultaneously has the following technical advantages: 1. has porosity and good adsorption effect. 2. Can respond to yellow light, can generate redox action without ultraviolet excitation, and is safer to use because yellow light is milder and has less stimulation to eyes. 3. The method has the advantages of simple and safe process, no need of adding organic solvent, simple operation method, low requirement on equipment and suitability for large-scale production and industrialization.
In addition, the invention further provides another whitening toothpaste which is formed by exciting redox reaction by visible light and a preparation method thereof. The toothpaste product takes titanium dioxide as a main whitening agent, can quickly generate oxidation-reduction reaction on discolored teeth under the excitation of blue light, and simultaneously has the following technical advantages: 1. can respond to visible light, can generate oxidation-reduction action without ultraviolet excitation, and is more healthy and safe. 2. The process is simple and safe, organic solvent is not required to be added, the operation method is simple, the requirement on equipment is low, and the method is suitable for large-scale production and industrialization.
Drawings
FIG. 1 is a graph showing the results of an experiment in example 3 of the present invention; wherein, part a is a real object diagram of a toothbrush (which can be used with the toothpaste of the invention) capable of emitting yellow light; parts b to d are respectively a whitening effect graph of the toothpaste prepared in the example 1 after the toothpaste is used for treating experimental teeth for different action time; the insets at the upper right corners of the parts b to d are colony growth diagrams obtained by plating the substances on the surfaces of the experimental teeth; section e is a scanning electron micrograph of the tooth enamel in section b; part f is a scanning electron micrograph of the tooth enamel in part d, and part g is a scanning electron micrograph of the tooth enamel after 3h treatment with a conventional cold light whitening method; part h is a partial enlarged view of a square in part e; part i is a partial enlarged view at a frame in part f; the portion j is a partially enlarged view of the square in the portion g.
FIG. 2 is a graph showing the results of an experiment in example 4 of the present invention; wherein, a part a is a whitening effect graph of the toothpaste prepared in the example 2 after the toothpaste is used for treating experimental teeth for different action time; section b is a scanning electron micrograph of experimental tooth enamel 4h after treatment without treatment and with the toothpaste prepared in example 2, respectively.
Detailed Description
Hereinafter, specific embodiments of the present invention will be described in detail. Well-known structures or functions may not be described in detail in the following embodiments in order to avoid unnecessarily obscuring the details.
Approximating language, as used herein in the following examples, may be applied to identify quantitative representations that could permissibly vary in number without resulting in a change in the basic function. Accordingly, a value modified by a language such as "about", "left or right" is not to be limited to the precise value per se. In some embodiments, "about" indicates that the value allowed for correction varies within plus or minus ten percent (10%), for example, "about 100" indicates that any value between 90 and 110 is possible. Further, in the expression "about a first value to a second value", both the first and second values are corrected at about the same time. In some cases, the approximating language may be related to the precision of a measuring instrument.
Unless defined otherwise, technical and scientific terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Example 1
1. The precursor solution was prepared from 50mM zinc nitrate hexahydrate (Zn (NO) 3 ) 2 ·6H 2 O), 80mM ammonia (NH) 3 ·H 2 O, O) and 25mM Hexamethylenetetramine (HMT) in 100ml deionized water, covering the container with a cover, and fully stirring for 10min until the solute is completely dissolved and clarified for later use, wherein in order to avoid the precursor solution from generating early precipitation, the adding sequence is NH 3 ·H 2 O、Zn(NO 3 ) 2 ·6H 2 O, HMT and the container is always sealed with a lid.
2. When the temperature of the water bath kettle reaches 65 ℃, the precursor liquid container covered with the cover is put into the water bath kettle and is ensured to be fully immersed, and the reaction lasts for 15min.
3. 0.14g of sodium citrate and 0.1g of hydroxypropyl methyl cellulose are respectively added into the solution, and the mixture is put into a water bath kettle with the temperature of 85 ℃ for reaction for 12 hours.
4. And putting the obtained product into a vacuum freeze dryer, drying, and putting into a household microwave oven for pyrolysis for 15min to obtain a finished product.
Example 2
1. Putting 0.08g of nano titanium dioxide and 0.01g of dopamine hydrochloride into a 100ml conical flask, adding 50ml of pure water, and uniformly mixing by oscillation;
2. adding 0.1g of hexamethylenetetramine, ultrasonically oscillating for 5min, sealing the container, and then putting the container into a water bath kettle at 90 ℃ for reaction for 3h;
3. washing the obtained product with pure water for 2 times, washing with anhydrous ethanol for 2 times, washing with pure water for 2 times, putting the product into a vacuum freeze dryer, and freeze-drying to obtain the final product.
Example 3
The whitening effect can be seen by dissolving the finished product in example 1 in water, dipping the solution with a toothbrush, turning on an LED to have yellow light and brushing teeth for three minutes.
Meanwhile, the experimental teeth were treated with the toothpaste prepared in example 1 for various times by immersing the experimental teeth in the aqueous solution of the toothpaste prepared in example 1 and continuously irradiating with LED yellow light, and the experimental results are shown in fig. 1.
As shown in the parts b-d of fig. 1, the treatment effect is obvious after half an hour, and the tooth stain in the tooth socket is well cleaned. As can be seen from the interpolated graphs in the upper right corners of each of b-d. The teeth treated by the toothpaste in the embodiment 1 have almost no bacteria growing on the surface, and can effectively inhibit the breeding of oral bacteria. As shown in fig. 1, sections e to j, it can be seen from the scanning electron microscope that the toothpaste of example 1 has almost no damage to enamel even after 3 hours of treatment, and the damage of enamel is clearly seen on the tooth surface treated with the cold light whitening under the same conditions, and thus the toothpaste provided in example 1 is safe and effective.
Example 4
The whitening effect can be seen by dissolving the finished product in example 2 in water, dipping the solution with a toothbrush, turning on the LED to emit blue light and brushing teeth for three minutes.
Meanwhile, the experimental teeth were treated with the toothpaste prepared in example 2 for different periods of time by immersing the experimental teeth in the aqueous solution of the toothpaste prepared in example 2 and continuously irradiating with LED blue light, and the experimental results are shown in fig. 2.
As shown in a part of fig. 2, after the titanium dioxide is treated by blue light irradiation, a whitening effect is remarkably achieved in a half hour. As shown in part b of fig. 2, no significant change was observed in the enamel surface over 4 hours, and thus it was seen that the toothpaste provided in example 2 was safe and effective.
The embodiments of the present invention have been described in detail, but the description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. Any modification, equivalent replacement, and improvement made within the scope of the present application shall be included in the protection scope of the present application.
Claims (1)
1. The whitening toothpaste excited by the blue light LED is characterized in that the blue light is the blue light with the wavelength of 450-480 nm, and the toothpaste contains 5% of polydopamine-coated titanium dioxide by mass;
the preparation method of the whitening toothpaste excited by the blue light LED comprises the following steps:
1) Uniformly mixing the nano titanium dioxide, the dopamine hydrochloride and the pure water in a container according to the proportion of 0.08;
2) Adding hexamethylene tetramine into the mixture, ultrasonically oscillating for 5min, sealing the container, and then carrying out water bath for 3h at 90 ℃; the addition amount of the hexamethylene tetramine is 10 times of the weight of the dopamine hydrochloride in the step 1);
3) Washing the product obtained in the step 2) with pure water for 2 times, then washing with absolute ethyl alcohol for 2 times, then washing with pure water for 2 times, and freeze-drying to obtain the whitening toothpaste.
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| CN201710655705.0A CN107582415B (en) | 2017-08-03 | 2017-08-03 | Whitening toothpaste with visible light excited oxidation-reduction reaction and preparation method thereof |
| CN202010653528.4A CN111759751B (en) | 2017-08-03 | 2017-08-03 | Whitening toothpaste excited by blue light LED and preparation method thereof |
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| CN110215305A (en) * | 2018-03-02 | 2019-09-10 | 张家港环纳环保科技有限公司 | A kind of tooth whitening suit and tooth whitening method |
| CN110464674A (en) * | 2019-08-19 | 2019-11-19 | 南京理工大学 | Tooth whitening products containing piezoelectric material |
| CN111494230B (en) * | 2020-04-30 | 2021-09-17 | 江西师范大学 | Cold light tooth whitening gel, preparation method and application |
| CN111646495A (en) * | 2020-06-24 | 2020-09-11 | 南昌大学 | Double-light response type zinc oxide, preparation method thereof and photosensitive coating with antibacterial osteogenesis property |
| CN112957385A (en) * | 2021-04-30 | 2021-06-15 | 镇江市许布医疗器械有限公司 | Preparation process of carbonized moxa/zinc oxide composite material with near-infrared light/yellow light responsiveness and responsiveness determination method thereof |
| CN113440423B (en) * | 2021-06-25 | 2022-06-17 | 水羊化妆品制造有限公司 | Modified titanium dioxide particle, preparation method thereof and skin care product |
| CN115252777B (en) * | 2022-06-09 | 2023-08-29 | 南昌大学 | In-situ whitening caries-preventing gel and preparation method thereof |
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| CN103006445A (en) * | 2012-12-28 | 2013-04-03 | 美晨集团股份有限公司 | Toothpaste for simultaneously cleaning, whitening and restoring teeth and preparation method of toothpaste |
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| CN1255322A (en) * | 1998-12-02 | 2000-06-07 | 中国科学院光电技术研究所 | Oral cavity cleaning instrument and its cleaning toothpaste |
| US7354448B2 (en) * | 2001-11-29 | 2008-04-08 | Palomar Medical Technologies, Inc. | Dental phototherapy methods and compositions |
| CN101311119B (en) * | 2007-05-25 | 2010-09-08 | 中国科学院合肥物质科学研究院 | Reticular nano hole zinc oxide micron hollow ball and preparation method thereof |
| CN101292943B (en) * | 2008-06-20 | 2010-04-14 | 陕西太和科技股份有限公司 | Nanometer zinc oxide toothpaste |
| CN101880054A (en) * | 2009-05-08 | 2010-11-10 | 中国科学院兰州化学物理研究所 | Method for preparing hollow zinc oxide microspheres |
| CN102058904A (en) * | 2010-12-31 | 2011-05-18 | 重庆大学 | Biological functionalized nano titanium material and preparation method thereof |
| CN102614090A (en) * | 2012-04-24 | 2012-08-01 | 苏州维蒂卡科技有限公司 | Toothpaste composition |
| CN102659168A (en) * | 2012-04-27 | 2012-09-12 | 哈尔滨理工大学 | Method for preparing zinc oxide nanoshuttle |
| KR20150124919A (en) * | 2014-04-29 | 2015-11-06 | 포항공과대학교 산학협력단 | Oral composition and method for preparing thereof |
| CN105232378A (en) * | 2015-10-27 | 2016-01-13 | 丹东康齿灵牙膏有限公司 | Whitening toothpaste not added with oxidizing agent and bleaching agent and preparation |
| CN105434304A (en) * | 2015-12-10 | 2016-03-30 | 青岛拓联信息技术有限公司 | Whitening toothpaste |
| CN105617460B (en) * | 2016-01-15 | 2019-07-19 | 厦门大学 | A method of nontoxic method antimicrobial coating is prepared on medical embedded material surface |
| CN105903076A (en) * | 2016-05-23 | 2016-08-31 | 北京科技大学 | Preparation method of dental implant and composite surface thereof |
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| CN103006445A (en) * | 2012-12-28 | 2013-04-03 | 美晨集团股份有限公司 | Toothpaste for simultaneously cleaning, whitening and restoring teeth and preparation method of toothpaste |
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| CN111759751A (en) | 2020-10-13 |
| CN107582415A (en) | 2018-01-16 |
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