Manganese tungstate nanoparticle / hydrogen peroxide composition for tooth whitening and preparation method thereof

The modified manganese tungstate nanoparticles prepared with hydrogen peroxide combined with hydrogen peroxide and ultrasonic catalyzed reactive oxygen generation solves the problem of insufficient enamel erosion and biocompatibility in traditional tooth whitening technology, achieving efficient, safe and long-lasting teeth Whitening effect.

CN119424258AActive Publication Date: 2025-02-14JIANGNAN UNIV

Patent Information

Application Number
CN202411599149.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-11
Publication Date
2025-02-14
Estimated Expiration
2044-11-11

AI Technical Summary

Technical Problem

In the existing teeth whitening technology, traditional whitening agents such as hydrogen peroxide and their derivatives have problems with enamel erosion, oral soft tissue damage and tooth sensitivity, and inorganic sound-sensitizers are insufficient in biocompatibility and stability in oral environments. , it is difficult to effectively remove exogenous pigments on the surface of teeth.

Method used

Manganese tungstate nanoparticles are prepared by modification of polyethylene glycol derivatives, as an inorganic sound-sensitizer, combined with hydrogen peroxide, and catalyzed reactive oxygen generation under ultrasound to achieve teeth whitening, while inhibiting electrons through catalase-like activity -Hole recombination to improve reactive oxygen yield.

Benefits of technology

This method significantly improves the yield of reactive oxygen species under ultrasound, achieves efficient, safe and long-lasting teeth whitening effect, while not damaging the enamel, and has good biocompatibility and water suspension stability.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the technical field of oral products, and particularly discloses a manganese tungstate nanoparticle / hydrogen peroxide composition for tooth whitening and a preparation method thereof. The preparation method comprises the following steps: preparing manganese tungstate nano-particles, dispersing tungsten hexacarbonyl and a surfactant in a first organic solvent, adding an oleic acid / oleylamine ligand pair under a first reaction condition, and then carrying out stirring reaction, cooling, centrifuging, washing and drying under a second reaction condition to prepare the manganese tungstate nano-particles. And preparing a manganese tungstate nanoparticle / polyethylene glycol composite material, dispersing the manganese tungstate nanoparticles and a polyethylene glycol derivative in a second organic solvent, uniformly stirring, and carrying out nitrogen drying to prepare the manganese tungstate nanoparticle / polyethylene glycol composite material. The manganese tungstate nanoparticle / polyethylene glycol composite material is dissolved in artificial saliva, a hydrogen peroxide solution is added and mixed, and the manganese tungstate nanoparticle / hydrogen peroxide composition for tooth whitening is prepared.
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Description

Technical Field

[0001] The invention relates to the technical field of oral products, and in particular to a manganese tungstate nanoparticle / hydrogen peroxide composition for teeth whitening and a preparation method thereof. Background Art

[0002] In the field of dental aesthetics, the aesthetic value of tooth color is not only affected by the inherent color of the teeth themselves, but also by the exogenous stains accumulated on the tooth surface. These exogenous stains mainly come from environmental factors such as smoking habits, daily diet and exposure to specific chemicals (such as cationic agents). In response to this, most tooth whitening technologies rely on hydrogen peroxide and its derivatives (such as carbamide peroxide) as whitening agents. However, although such traditional whitening agents can effectively remove pigments, they have potential side effects - including enamel erosion, oral soft tissue damage and tooth sensitivity problems.

[0003] As an emerging non-invasive treatment method, sonodynamic therapy uses sonosensitizers with the assistance of ultrasound to induce the production of highly reactive active oxygen, thereby decomposing exogenous pigments on the tooth surface to achieve tooth whitening. Among the key components of sonodynamic therapy, the selection and optimization of sonosensitizers play a vital role in improving the treatment effect.

[0004] Sonosensitizers are mainly divided into two categories: organic sonosensitizers and inorganic sonosensitizers. Organic sonosensitizers are chemically unstable and have potential biological toxicity, especially in the complex environment of the oral cavity, which can easily cause tissue damage. Inorganic sonosensitizers have excellent chemical stability and good biocompatibility.

[0005] How to obtain an inorganic sonosensitizer for use in sonodynamic therapy to achieve better therapeutic effects is a technical problem that needs to be solved urgently. Summary of the invention

[0006] In view of the above problems, an object of the present invention is to provide a method for preparing a manganese tungstate nanoparticle / hydrogen peroxide composition for tooth whitening. Manganese tungstate nanoparticles modified with polyethylene glycol derivatives, as an inorganic sonosensitizer, not only show good water suspension stability and biocompatibility in aqueous solution, but also show efficient reactive oxygen generation ability under ultrasound. Its oxygen-deficient structure provides an ideal site for electron capture, effectively inhibits the recombination of electron-hole pairs, thereby significantly improving the yield of reactive oxygen. In addition, manganese tungstate nanoparticles also have catalase-like activity, which can catalyze the decomposition of hydrogen peroxide into more reactive oxygen. The synergistic effect of this sonodynamic force and chemical kinetics achieves a more efficient, safe and lasting tooth whitening effect.

[0007] The second object of the present invention is to provide a manganese tungstate nanoparticle / hydrogen peroxide composition for tooth whitening. Manganese tungstate nanoparticles with oxygen vacancies are prepared by a simple and effective method, hydrophilically modified to increase their water suspension stability, and combined with a hydrogen peroxide solution of appropriate concentration to achieve whitening of teeth without damaging tooth enamel.

[0008] The first technical solution adopted by the present invention is: a method for preparing a manganese tungstate nanoparticle / hydrogen peroxide composition for tooth whitening, comprising the following steps:

[0009] Step 1: preparing manganese tungstate nanoparticles, dispersing tungsten hexacarbonyl and a surfactant in a first organic solvent, adding an oleic acid / oleylamine ligand pair under a first reaction condition, and then stirring the reaction under a second reaction condition, cooling, centrifuging, washing, and drying to obtain manganese tungstate nanoparticles;

[0010] Step 2: preparing a manganese tungstate nanoparticle / polyethylene glycol composite material, dispersing the manganese tungstate nanoparticle and the polyethylene glycol derivative in a second organic solvent, stirring evenly, and drying with nitrogen to obtain a manganese tungstate nanoparticle / polyethylene glycol composite material;

[0011] Step 3: dissolving the manganese tungstate nanoparticle / polyethylene glycol composite material in artificial saliva, adding hydrogen peroxide solution and mixing, so as to prepare a manganese tungstate nanoparticle / hydrogen peroxide composition for teeth whitening.

[0012] Preferably, the first organic solvent is dibenzyl ether;

[0013] The second organic solvent is chloroform.

[0014] Preferably, the surfactant is 1,2-dodecanediol.

[0015] Preferably, the volume ratio of oleic acid to oleylamine in the oleic acid / oleylamine ligand pair is 1:1, and the added amount of the oleic acid / oleylamine ligand pair is 1-2 mL.

[0016] Preferably, the polyethylene glycol derivative is distearoyl phosphatidylethanolamine-methoxy polyethylene glycol.

[0017] Preferably, the manganese tungstate concentration in the manganese tungstate nanoparticle / hydrogen peroxide composition is 150-200 μg / mL, and the hydrogen peroxide concentration is 0.5-1 wt %.

[0018] Preferably, the washing conditions in step 1 are: washing with a cyclohexane-ethanol mixture, wherein the volume ratio of cyclohexane to ethanol in the cyclohexane-ethanol mixture is 1:(1.5-3).

[0019] Preferably, the first reaction condition is: the reaction environment is a nitrogen atmosphere, and the reaction temperature is 110-130°C.

[0020] Preferably, the second reaction condition is: heating the reaction temperature to 250-270° C., adding manganese acetylacetonate, the molar ratio of the hexacarbonyl tungsten to the manganese acetylacetonate is 1:1, and the reaction time is 0.5-2 h.

[0021] The second technical solution adopted by the present invention is: a manganese tungstate nanoparticle / hydrogen peroxide composition for teeth whitening.

[0022] Beneficial effects of the above technical solution:

[0023] (1) The preparation method of the manganese tungstate nanoparticle / hydrogen peroxide composition provided by the present invention is simple and effective. The present invention can prepare manganese tungstate nanoparticles with uniform morphology and oxygen vacancies by a high-temperature organic phase synthesis method, coat DSPE-PEG on the surface of the manganese tungstate nanoparticles, perform hydrophilic modification on the manganese tungstate nanoparticles to increase their water suspension stability, and then combine with hydrogen peroxide to achieve the effect of whitening teeth without damaging tooth enamel.

[0024] (2) The manganese tungstate nanoparticle / hydrogen peroxide composition provided by the present invention can catalyze water and dissolved oxygen to produce active oxygen under the action of ultrasound and catalyze hydrogen peroxide to produce active oxygen, thereby achieving the effect of degrading pigments and whitening teeth. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1a This is a transmission electron microscope (TEM) image of 100nm pixel of manganese tungstate nanoparticles;

[0026] Figure 1b This is a transmission electron microscope (TEM) pixel 20nm image of manganese tungstate nanoparticles;

[0027] Figure 2a This is the energy dispersive spectroscopic (EDS) overall element distribution diagram of manganese tungstate nanoparticles;

[0028] Figure 2b Energy dispersive spectrometry (EDS) oxygen element distribution diagram of manganese tungstate nanoparticles;

[0029] Figure 2c Energy dispersive spectrometry (EDS) distribution diagram of manganese element in manganese tungstate nanoparticles;

[0030] Figure 2d Energy dispersive spectroscopy (EDS) tungsten element distribution diagram of manganese tungstate nanoparticles;

[0031] Figure 3a This is the overall X-ray photoelectron spectroscopy (XPS) spectrum of manganese tungstate nanoparticles;

[0032] Figure 3b This is the oxygen element spectrum of the X-ray photoelectron spectroscopy (XPS) of manganese tungstate nanoparticles;

[0033] Figure 3c This is the X-ray photoelectron spectroscopy (XPS) tungsten element spectrum of manganese tungstate nanoparticles;

[0034] Figure 3d This is the X-ray photoelectron spectroscopy (XPS) manganese element spectrum of manganese tungstate nanoparticles;

[0035] Figure 4 is the X-ray diffraction (XRD) pattern of manganese tungstate nanoparticles;

[0036] Figure 5 This is the infrared spectrum of the manganese tungstate nanoparticles / polyethylene glycol composite material;

[0037] Figure 6a It is a transmission electron microscope (TEM) pixel 50nm image of the manganese tungstate nanoparticle / hydrogen peroxide composition;

[0038] Figure 6b This is a transmission electron microscope (TEM) pixel 10nm image of a manganese tungstate nanoparticle / hydrogen peroxide composition;

[0039] Figure 7a For tooth color pictures;

[0040] Figure 7b This is a statistical chart of L values ​​measured by a tooth colorimeter;

[0041] Figure 8 This is a graph showing the survival rate of human gingival fibroblasts after being treated with different concentrations of manganese tungstate nanoparticles;

[0042] Figure 9a This is a photo of the color of tooth enamel after hydrogen peroxide treatment;

[0043] Figure 9b This is a scanning electron microscope (SEM) image of normal tooth enamel;

[0044] Fig.9c This is the scanning electron microscope (SEM) image of tooth enamel after 8 hours of treatment with manganese tungstate nanoparticles, hydrogen peroxide and ultrasound;

[0045] Figure 9d This is a scanning electron microscope (SEM) image of tooth enamel treated with 20 wt % hydrogen peroxide for 30 minutes. DETAILED DESCRIPTION

[0046] The following is a further detailed description of the implementation methods of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than an exhaustive list of all the embodiments. It should be noted that the embodiments and features in the embodiments of the present application can be combined with each other without conflict.

[0047] The terms "first", "second", etc. (if any) in the specification and claims are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. It should be understood that the terms used in this way are interchangeable where appropriate so that the embodiments described herein can be implemented in an order other than that illustrated or described herein. In addition, the terms "including" and "having" and any variations thereof are intended to cover non-exclusive inclusions, for example, a process, method, system, product, or device that includes a series of steps or units is not necessarily limited to those steps or units that are clearly listed, but may include other steps or units that are not clearly listed or inherent to these processes, methods, products, or devices.

[0048] It should be understood that the term "and / or" used in this article is only a description of the association relationship of associated objects, indicating that there can be three relationships. For example, A and / or B can represent: A exists alone, A and B exist at the same time, and B exists alone. In addition, the character " / " in this article generally indicates that the associated objects before and after are in an "or" relationship.

[0049] Embodiment 1

[0050] (1) Preparation of manganese tungstate nanoparticles

[0051] 352 mg of hexacarbonyl tungsten and 1.5 g of 1,2-dodecanediol were dispersed in 20 mL of dibenzyl ether, heated to 120 °C in a nitrogen atmosphere, and then 1 mL of oleic acid and 1 mL of oleylamine were added; then the mixture was heated to 260 °C, and 352 mg of manganese acetylacetonate was added. The mixture was stirred for 1 h, cooled to room temperature, and then excess ethanol was added and centrifuged (10 min, 10000 rpm). Then, the mixture was dissolved in 10 mL of cyclohexane, and then 15 mL of ethanol was added and mixed, and then centrifuged (10 min, 10000 rpm). The mixture was repeated three times, and finally dried in a 60 °C oven.

[0052] The prepared manganese tungstate nanoparticles were photographed by transmission electron microscopy (TEM), and the results are as follows: Figure 1a and 1b As shown, it can be seen that the size of the prepared manganese tungstate nanoparticles is about 4-8nm. The prepared manganese tungstate nanoparticles were subjected to energy dispersive spectrometer (EDS) element mapping, and the results are as follows Figure 2a to 2dAs shown, it shows that the Mn, W and O elements are evenly distributed in the manganese tungstate nanoparticles. The prepared manganese tungstate nanoparticles were scanned by X-ray photoelectron spectroscopy (XPS), and the results are as follows Figure 3a to 3d As shown in the figure, by fitting the peaks of oxygen elements, it is found that there are oxygen vacancies and W in the material. 5+ and W 6+ The prepared manganese tungstate nanoparticles were subjected to X-ray diffraction (XRD) analysis, and the results were as follows: Figure 4 As shown, the XRD spectrum of manganese tungstate nanoparticles contains four characteristic diffraction peaks, corresponding to the lattice plane structures of (100), (001), (-111) and (002), respectively.

[0053] (2) Preparation of manganese tungstate nanoparticles / polyethylene glycol composites

[0054] 10 mg of manganese tungstate nanoparticles and 40 mg of DSPE-PEG were dispersed in 4 mL of chloroform and stirred for 1 h to obtain a mixed solution, which was then placed under a nitrogen blower for 2 h for nitrogen drying. After drying, a manganese tungstate nanoparticle / polyethylene glycol composite material was obtained.

[0055] The infrared spectrum of the prepared manganese tungstate nanoparticles / polyethylene glycol composite material was scanned. Figure 5 As shown in the figure, it can be seen that the spectrum of the prepared manganese tungstate nanoparticles / polyethylene glycol composite material is at 3400 cm -1 A broad OH band is shown near 1740 cm -1 A C=O stretching band is shown at 1740 cm -1 A stretching band of P=O, PO is shown at the center, which proves that DSPE-PEG is successfully coated on the surface of manganese tungstate nanoparticles.

[0056] (3) Preparation of manganese tungstate / hydrogen peroxide composition

[0057] Artificial saliva was prepared according to ISO / TR10271, that is, 0.4g NaCl, 0.4g KCl, 0.795g CaCl2·2H2O, 0.78g NaH2PO4·2H2O, 0.05g Na2S·2H2O, and 1g urea were dissolved in 1L deionized water. The manganese tungstate nanoparticle / polyethylene glycol composite material was dissolved in 25mL artificial saliva, and then mixed with 25mL 1wt% hydrogen peroxide solution to finally obtain 50mL manganese tungstate nanoparticle / hydrogen peroxide composition.

[0058] The prepared manganese tungstate nanoparticles / hydrogen peroxide composition was tested by transmission electron microscopy (TEM), and the results were as follows: Figure 6a and Figure 6bAs shown, it can be seen that the manganese tungstate nanoparticles are uniformly dispersed in the solution in the form of small aggregates with a diameter of about 20-30 nm.

[0059] Embodiment 2

[0060] (1) Preparation of manganese tungstate nanoparticles

[0061] 352 mg of hexacarbonyl tungsten and 1.5 g of 1,2-dodecanediol were dispersed in 20 mL of dibenzyl ether, heated to 130 °C in a nitrogen atmosphere, and then 1.5 mL of oleic acid and 1.5 mL of oleylamine were added; then heated to 270 °C, 352 mg of manganese acetylacetonate was added, and the reaction was stirred for 0.5 h. After cooling to room temperature, excess ethanol was added and centrifuged (10 min, 10000 rpm), and then dissolved in 10 mL of cyclohexane, 20 mL of ethanol was added and mixed, and then centrifuged (10 min, 10000 rpm), and repeated three times. Finally, it was placed in a 60 °C oven to dry.

[0062] (2) Preparation of manganese tungstate nanoparticles / polyethylene glycol composites

[0063] 10 mg of manganese tungstate nanoparticles and 50 mg of DSPE-PEG were dispersed in 4 mL of chloroform and stirred for 1 h to obtain a mixed solution, which was then placed under a nitrogen blower for 2 h for nitrogen drying. After drying, a manganese tungstate nanoparticle / polyethylene glycol composite material was obtained.

[0064] (3) Preparation of manganese tungstate / hydrogen peroxide composition

[0065] The manganese tungstate nanoparticle / polyethylene glycol composite material was dissolved in 25 mL of artificial saliva, and then mixed with 25 mL of 2 wt % hydrogen peroxide solution to finally obtain 50 mL of manganese tungstate nanoparticle / hydrogen peroxide composition.

[0066] Embodiment 3

[0067] (1) Preparation of manganese tungstate nanoparticles

[0068] 352 mg of hexacarbonyl tungsten and 1.5 g of 1,2-dodecanediol were dispersed in 20 mL of dibenzyl ether, heated to 110 °C in a nitrogen atmosphere, and then 1.5 mL of oleic acid and 1.5 mL of oleylamine were added; then the mixture was heated to 250 °C, and 352 mg of manganese acetylacetonate was added. The mixture was stirred for 1.5 h, cooled to room temperature, and then excess ethanol was added and centrifuged (10 min, 10000 rpm). Then, 10 mL of cyclohexane was used to dissolve the mixture, and 30 mL of ethanol was added and mixed, followed by centrifugation (10 min, 10000 rpm). The mixture was repeated three times, and finally dried in a 60 °C oven.

[0069] (2) Preparation of manganese tungstate nanoparticles / polyethylene glycol composites

[0070] 10 mg of manganese tungstate nanoparticles and 30 mg of DSPE-PEG were dispersed in 3 mL of chloroform and stirred for 1 h to obtain a mixed solution, which was then placed under a nitrogen blower for 2 h for nitrogen drying. After drying, a manganese tungstate nanoparticle / polyethylene glycol composite material was obtained.

[0071] (3) Preparation of manganese tungstate / hydrogen peroxide composition

[0072] The manganese tungstate nanoparticle / polyethylene glycol composite material was dissolved in 25 mL of artificial saliva, and then mixed with 25 mL of 1 wt % hydrogen peroxide solution to finally obtain 50 mL of manganese tungstate nanoparticle / hydrogen peroxide composition.

[0073] Evaluation of tooth whitening performance of manganese tungstate nanoparticles / hydrogen peroxide compositions

[0074] (1) Establishment of tooth staining model

[0075] The enamel part of fresh human teeth was cut into two parts, then soaked in a black tea solution for one week for coloring, and then taken out and rinsed with deionized water to remove surface dirt.

[0076] (2) Teeth whitening experiment

[0077] The stained teeth were divided into four groups, namely, ultrasound only group, hydrogen peroxide plus ultrasound group, manganese tungstate nanoparticles plus ultrasound group, and manganese tungstate nanoparticles plus hydrogen peroxide plus ultrasound group. The ultrasound group was ultrasounded in artificial saliva for 8 hours (15-20kHz, 50% duty cycle); the manganese tungstate nanoparticles plus ultrasound group was ultrasounded in 200μg / mL manganese tungstate nanoparticle suspension for 8 hours, the hydrogen peroxide plus ultrasound group was ultrasounded in 0.5wt% hydrogen peroxide solution for 8 hours, and the manganese tungstate nanoparticles plus hydrogen peroxide plus ultrasound group was ultrasounded in 0.5wt% hydrogen peroxide and 200μg / mL manganese tungstate nanoparticle suspension for 8 hours. Among them, a new suspension was replaced every hour.

[0078] (3) Evaluation of whitening effect

[0079] Take pictures of the appearance and use a colorimeter to measure their brightness (L) values, such as Figure 7a and Figure 7b Compared with the ultrasound group, hydrogen peroxide plus ultrasound group, and manganese tungstate nanoparticles plus ultrasound group, the manganese tungstate nanoparticles plus hydrogen peroxide plus ultrasound group had a more obvious whitening effect, indicating that a better whitening effect can be achieved under the dual effects of manganese tungstate nanoparticles and hydrogen peroxide.

[0080] Biocompatibility testing of manganese tungstate nanoparticles

[0081] (1) Cell recovery and passaging

[0082] The cryopreserved tube containing human gingival fibroblasts (HGF-1) was quickly shaken and dissolved in a 37°C water bath, and then the cell cryopreserved solution was mixed with 9mL of complete culture medium (DMEM culture medium containing 15% fetal bovine serum and 1% penicillin-streptomycin double antibody), centrifuged at 1200rpm for 5min, the supernatant was discarded, and the tube was transferred to a T25 bottle containing 5-6mL of complete culture medium and placed in an incubator (37°C, 5% CO2 and 95% relative humidity) for 18h. If long spindle-shaped, irregularly edged adherent cells are observed under a microscope, the recovery is successful. To ensure cell activity, the cells are passaged when the cell density reaches more than 80%. For cell passaging, discard the old culture medium, wash twice with PBS, add 1-2 mL of trypsin (0.25% Trypsin + 0.02% EDTA) and incubate at 37°C for 1-2 min to detach the cells, then add 5-6 mL of complete culture medium to terminate digestion and centrifuge again to remove the supernatant. Re-add complete culture medium and blow evenly and divide the cell suspension into new culture dishes at a ratio of 1:2 for continued culture.

[0083] (2) Cytotoxicity assay

[0084] The CCK-8 method was used to measure the viability of HGF-1 cells to evaluate the cytotoxicity of the material. Cells were seeded in a 96-well plate at a density of 1×10 4 cells. After incubation for 24 hours, discard the old culture medium, add 100 μL of fresh culture medium containing manganese tungstate nanoparticles / polyethylene glycol composite materials with different concentrations of manganese tungstate nanoparticles (50-1500 μg / mL), and continue to culture at 37°C for 24 hours. After incubation, add 10 μL of CCK-8 reagent to each well, continue incubation for 1-2 hours, and measure the absorbance value at 450nm. The formula for calculating the survival rate of HGF-1 cells is: Cell activity = (A s -A b ) / (A c -A b )×100%, where A s , A b and A c The absorbances of the sample group, blank group and control group are shown in Figure 2. Each group of samples was tested 5 times in parallel (n=5). Figure 8 As shown, when the concentration of manganese tungstate nanoparticles is above 200 μg / mL, the cell survival rate reaches above 80%. Therefore, manganese tungstate nanoparticles at this concentration (or below) have good biocompatibility.

[0085] Test of tooth enamel surface damage by manganese tungstate nanoparticles / hydrogen peroxide composition

[0086] The stained teeth were soaked in 20wt% hydrogen peroxide solution for 30 minutes and then taken out, and the brightness (L) value was similar to that of the manganese tungstate nanoparticles plus hydrogen peroxide plus ultrasound group. Then, scanning electron microscopy (SEM) was used to photograph normal enamel, enamel treated with 20% hydrogen peroxide for 30 minutes, and enamel treated with manganese tungstate nanoparticles plus hydrogen peroxide plus ultrasound for 8 hours. Figures 9a to 9d As shown, the surface of tooth enamel treated with manganese tungstate nanoparticles, hydrogen peroxide and ultrasound for 8 hours was smooth, almost indistinguishable from normal tooth enamel, while the surface of tooth enamel treated with 20wt% hydrogen peroxide solution for 30 minutes had obvious damage.

[0087] Obviously, the above embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not limitations on the implementation methods of the present invention. For ordinary technicians in the relevant field, other different forms of changes or modifications can be made on the basis of the above description. It is impossible to list all the implementation methods here. All obvious changes or modifications derived from the technical solution of the present invention are still within the protection scope of the present invention.

Claims

1. A method for preparing a manganese tungstate nanoparticle / hydrogen peroxide composition for tooth whitening, characterized in that: The steps include: Step 1: preparing manganese tungstate nanoparticles, dispersing tungsten hexacarbonyl and a surfactant in a first organic solvent, adding an oleic acid / oleylamine ligand pair under a first reaction condition, and then stirring the reaction under a second reaction condition, cooling, centrifuging, washing, and drying to obtain manganese tungstate nanoparticles; Step 2: preparing a manganese tungstate nanoparticle / polyethylene glycol composite material, dispersing the manganese tungstate nanoparticle and the polyethylene glycol derivative in a second organic solvent, stirring evenly, and drying with nitrogen to obtain a manganese tungstate nanoparticle / polyethylene glycol composite material; Step 3: dissolving the manganese tungstate nanoparticle / polyethylene glycol composite material in artificial saliva, adding hydrogen peroxide solution and mixing, so as to prepare a manganese tungstate nanoparticle / hydrogen peroxide composition for teeth whitening.

2. The method for preparing the manganese tungstate nanoparticle / hydrogen peroxide composition for tooth whitening according to claim 1, characterized in that: The first organic solvent is dibenzyl ether; The second organic solvent is chloroform.

3. The method for preparing the manganese tungstate nanoparticle / hydrogen peroxide composition for tooth whitening according to claim 1, characterized in that: The surfactant is 1,2-dodecanediol.

4. The method for preparing the manganese tungstate nanoparticle / hydrogen peroxide composition for tooth whitening according to claim 1, characterized in that: The volume ratio of oleic acid to oleylamine in the oleic acid / oleylamine ligand pair is 1:1, and the added amount of the oleic acid / oleylamine ligand pair is 1-2 mL.

5. The method for preparing the manganese tungstate nanoparticle / hydrogen peroxide composition for tooth whitening according to claim 1, characterized in that: The polyethylene glycol derivative is distearoyl phosphatidylethanolamine-methoxy polyethylene glycol.

6. The method for preparing the manganese tungstate nanoparticle / hydrogen peroxide composition for tooth whitening according to claim 1, characterized in that: The manganese tungstate nanoparticle / hydrogen peroxide composition has a manganese tungstate concentration of 150-200 μg / mL and a hydrogen peroxide concentration of 0.5-1 wt %.

7. The method for preparing the manganese tungstate nanoparticle / hydrogen peroxide composition for tooth whitening according to claim 1, characterized in that: The washing condition in the step 1 is: washing with a cyclohexane-ethanol mixture, wherein the volume ratio of cyclohexane to ethanol in the cyclohexane-ethanol mixture is 1:(1.5-3).

8. The method for preparing the manganese tungstate nanoparticle / hydrogen peroxide composition for teeth whitening according to claim 1, characterized in that: The first reaction condition is: the reaction environment is a nitrogen atmosphere, and the reaction temperature is 110-130°C.

9. The method for preparing the manganese tungstate nanoparticle / hydrogen peroxide composition for tooth whitening according to claim 1, characterized in that: The second reaction condition is: heating the reaction temperature to 250-270° C., adding manganese acetylacetonate, the molar ratio of the hexacarbonyl tungsten to the manganese acetylacetonate is 1:1, and the reaction time is 0.5-2 hours.

10. A manganese tungstate nanoparticle / hydrogen peroxide composition for tooth whitening prepared by the preparation method according to any one of claims 1 to 9.

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