Hydrogel tooth socket loaded with whitening factors and preparation method of hydrogel tooth socket

Abstract

The invention discloses a whitening factor-loaded hydrogel tooth socket, which comprises a soft tooth socket, the inner layer of the soft tooth socket is provided with whitening factor-containing hydrogel, and the soft tooth socket is prepared from the following raw material components in parts by mass: 30-60 parts of polydimethylsiloxane and 3.0-6.0 parts of a curing agent; the whitening factor is prepared from the following raw material components in parts by weight: 0.01-0.1 part of metal salt, 0.5-1.5 parts of a binding agent, 20-40 parts of a dispersing agent I, 1.0-3.5 parts of a pH regulator and 0.2-0.8 part of an oxidizing agent, the hydrogel comprises the following raw material components in parts by weight: 0.5-1.5 parts of gelatin, 20-25 parts of a dispersing agent II and 0.1-0.5 part of a colloid stabilizer. The invention further discloses a preparation method of the hydrogel brace loaded with the whitening factors. According to the invention, tooth injury caused by direct use of traditional peroxide is avoided. Meanwhile, the preparation method is simple in process, personalized adjustment can be carried out according to the tooth condition of a patient, the prepared hydrogel tooth socket is perfectly matched with the tooth form of the patient, and in-situ release of the whitening factors is achieved.

Description

Technical Field

[0001] The invention relates to the technical field of tooth whitening, and in particular to a hydrogel dental cap loaded with whitening factors and a preparation method thereof. Background Art

[0002] With the continuous improvement of living standards, people pay more and more attention to dental beauty, among which teeth whitening is particularly prominent. Existing teeth whitening can be achieved by using whitening strips, laser whitening, cold light whitening and other methods, but these methods will cause different degrees of irritation to the teeth, leading to discomfort such as tooth sensitivity. In comparison, removable whitening braces have the advantages of low irritation and no damage to the tooth surface. In addition, removable whitening braces can be removed at any time according to the patient's needs, without affecting tooth cleaning and eating, and are more convenient.

[0003] Currently, the chemical ingredients used for teeth whitening are mainly peroxides, such as hydrogen peroxide, carbamide peroxide, sodium percarbonate, etc. The principle is that peroxides can produce active oxygen to oxidatively bleach tooth enamel. Currently, the more commonly used blue light technology can accelerate the release of active oxygen and does not require grinding of tooth enamel. However, due to the strong oxidizing properties of peroxides, a series of side effects may occur during the operation: (1) demineralization of tooth enamel; (2) brittle teeth; (3) users generally have uncomfortable reactions such as tooth sensitivity and gum irritation; (4) uncontrollable chemical oxidation leads to mucosal damage; (5) causing gingival swelling and pain, and acute pulpitis.

[0004] Publication No. CN108289860A discloses a preparation for sticking on teeth or the peripheral part of teeth, and the preparation for sticking includes: a hardened paste-like oral composition and a medicinal ingredient for delivery into the oral cavity. The invention solves the problem of delivering drugs to teeth and the edges of teeth, but the preparation for sticking directly on teeth or the peripheral part of teeth may irritate the teeth and cause tooth sensitivity.

[0005] Publication No. CN116650363A discloses a tooth whitening adhesive patch and a preparation method thereof, the adhesive patch comprises the following raw materials in mass percentage: peroxide: 1-5%; adhesive: 10-20%; moisturizer: 40-50%; antiallergic agent: 1-2%; catalyst: 0.01-0.5%; stabilizer: 0.1-1%; water: balance; the adhesive is mainly obtained by reacting raw materials including carbomer, hydroxyethyl cellulose and chitosan fiber at 30-100°C, the mass ratio of carbomer, hydroxyethyl cellulose and chitosan fiber is 10:(2-4):(1-3), and the reaction pH value is 5-6. The tooth whitening adhesive patch contains peroxide, and the direct use of the peroxide will cause tooth damage and multiple side effects. Summary of the invention

[0006] In order to solve the above technical problems, the present invention provides a hydrogel dental cap loaded with whitening factors, which enables the whitening factors to respond quickly, release slowly and evenly and exert their effects in the teeth.

[0007] A hydrogel brace loaded with whitening factors, comprising a soft brace, wherein the inner layer of the soft brace has a hydrogel containing whitening factors, and the hydrogel contains the whitening factors in parts by mass.

[0008] The raw material components of the soft braces are 30-60 parts of polydimethylsiloxane and 3.0-6.0 parts of curing agent;

[0009] The raw material components of the whitening factor are 0.01-0.1 parts of soluble metal salt, 0.5-1.5 parts of combining agent, 20-40 parts of dispersant I, 1.0-3.5 parts of pH adjusting agent, and 0.2-0.8 parts of oxidant;

[0010] The oxidant in the present invention provides a peroxide bond, which can react with a soluble metal salt under alkaline conditions to generate a whitening factor. The whitening factor is not easily decomposed under normal conditions, but after contacting with moisture in the oral cavity, the whitening factor is hydrolyzed to form hydrogen peroxide. Hydrogen peroxide undergoes an oxidation reaction to release active oxygen that penetrates tooth enamel and dentin, reacts with pigment groups to decompose into small molecules and emits to the tooth surface, thereby changing the color of the teeth to achieve tooth whitening.

[0011] The raw material components of the hydrogel are 0.5-1.5 parts of gelatin, 20-25 parts of dispersant II, and 0.1-0.5 parts of colloid stabilizer;

[0012] The mass ratio of the whitening factor to the hydrogel is 0.4-0.6:1.

[0013] The whitening factor of the present invention can slowly release hydrogen peroxide in the acidic environment of the oral cavity to act on tooth enamel and oxidatively decompose pigments. By attaching the highly sensitive acid-responsive whitening factor to the hydrogel, its release rate can be controlled, so that the whitening factor can achieve rapid response, slow and uniform release and exert its effect in the tooth area. This characteristic reduces the incidence of side effects to a certain extent.

[0014] The present invention uses polydimethylsiloxane as the core raw material to make transparent soft braces. After curing treatment, the braces show excellent transparency, elasticity and strong toughness, can adapt to different conditions of teeth, and can maintain good morphological stability during wearing, without fear of deformation, and have excellent durability.

[0015] The present invention uses gelatin as the basic raw material of the hydrogel. Since gelatin is a protein extracted by collagen hydrolysis, it has good biocompatibility. As a highly hydrophilic new biomaterial, gelatin hydrogel can absorb a large amount of water in a liquid state without dissolving, so that it can fit the braces and teeth tightly in the braces application, promoting the whitening factor to play a better role.

[0016] Among the whitening factors,

[0017] Preferably, the soluble metal salt is at least one of manganese salt, sodium salt, calcium salt, zinc salt, iron salt and copper salt.

[0018] The combined agent is at least one of polyvinyl alcohol, polyvinyl pyrrolidone and copovidone.

[0019] The combining agent in the present invention is used as a ligand for synthesizing the whitening factor. The use of the combining agent can prevent the whitening factor from aggregating, so as to synthesize the whitening factor with a smaller and uniform particle size, thereby controlling the decomposition rate of the whitening factor.

[0020] Preferably, the dispersant I is at least one of ethanol, methanol, ethylene glycol and acetone.

[0021] Preferably, the pH adjuster is at least one of sodium hydroxide, ammonia water and sodium carbonate.

[0022] Preferably, the oxidant is at least one of sodium peroxide, hydrogen peroxide and peracetic acid.

[0023] Further preferably, in the whitening factor, the soluble metal salt is a calcium salt, and the oxidant is hydrogen peroxide.

[0024] Preferably, soluble calcium salt reacts with hydrogen peroxide under alkaline conditions to generate a whitening factor containing calcium peroxide. Calcium peroxide, as a stable active oxygen provider, can be hydrolyzed to generate hydrogen peroxide under the physiological conditions of the oral cavity. The active oxygen released by the oxidation reaction of hydrogen peroxide can penetrate the tooth enamel, oxidatively decompose the pigment groups, and thus exert a whitening effect. Compared with the same mass of peroxide, calcium peroxide provides more hydrogen peroxide and has better stability. Since teeth themselves contain calcium, the use of calcium salts will not introduce other additional substances.

[0025] In the hydrogel,

[0026] Preferably, the dispersant II is at least one of ethanol, methanol, water and propylene glycol.

[0027] Preferably, the colloidal stabilizer is at least one of zinc pyrrolidone hydroxyapatite, copper pyrrolidone hydroxyapatite and sodium pyrrolidone hydroxyapatite.

[0028] The present invention also provides a method for preparing the above-mentioned hydrogel braces loaded with whitening factors. The preparation method is simple and can be personalized according to the patient's dental condition. The prepared hydrogel braces perfectly match the patient's tooth shape and realize the in situ release of the whitening factors.

[0029] A method for preparing a hydrogel dental cap loaded with whitening factors, characterized in that it comprises the following steps:

[0030] (1) According to the patient's tooth arrangement, a digital dental model is obtained by full-mouth dental scanning, and a target model with a positioning mark base is printed using 3D printing technology. A transparent brace is obtained by molding and laser cutting;

[0031] (2) Mixing polydimethylsiloxane and curing agent in a certain proportion, placing the mixture in a vacuum drying oven for vacuum degassing, pouring the mixture into the transparent braces obtained in step (1), pressing to discharge the excess mixture, and finally placing the mixture in a vacuum drying oven for solidification and demolding to obtain a soft braces;

[0032] (3) dissolving the soluble metal salt and the combining agent in the dispersant I and mixing them evenly, adjusting the pH value with a pH adjusting agent, injecting an oxidant through a microinjection pump, centrifuging and washing the mixed solution, and obtaining a whitening factor;

[0033] (4) dissolving gelatin and a colloidal stabilizer in a dispersant II, mixing and stirring to obtain a hydrogel;

[0034] (5) The whitening factor obtained in step (3) is mixed with the hydrogel obtained in step (4) to obtain a hydrogel loaded with the whitening factor, and the hydrogel is evenly dripped into the soft braces obtained in step (2) to obtain a hydrogel braces loaded with the whitening factor.

[0035] Preferably, in step (2), the coagulation temperature is 60-80° C. and the coagulation time is 20-30 min.

[0036] Preferably, in step (3), the pH value is adjusted to 7-11.

[0037] Preferably, in step (3), the centrifugal speed is 8000-11000 rpm, and the centrifugal time is 10-30 min.

[0038] The present invention provides a simple preparation process, which can be adjusted individually according to the patient's dental condition. The prepared hydrogel dental cap perfectly matches the patient's tooth shape, achieving rapid response, precise and slow release of whitening factors at the site of action.

[0039] Compared with the prior art, the present invention has the following beneficial effects:

[0040] (1) The present invention uses polydimethylsiloxane as the core raw material to make transparent braces. After curing, the braces show excellent transparency, elasticity and strong toughness, can fit tightly to the tooth surface, and can adapt to different conditions of teeth, providing an ideal platform for the efficient action of whitening hydrogel, thereby promoting the maximization of tooth whitening effect.

[0041] (2) The whitening factor in the present invention is loaded on a highly sensitive acid-responsive hydrogel, which has significant advantages over the application of traditional peroxides in tooth whitening. Based on the characteristics of the hydrogel, it can achieve rapid response, precise and slow release at the site of action, and can reduce the health hazards caused by the direct release of traditional peroxide whitening factors. BRIEF DESCRIPTION OF THE DRAWINGS

[0042] Figure 1 This is an appearance diagram of the soft braces prepared in Example 1.

[0043] Figure 2 This is a transmission electron microscopy image of the whitening factor prepared in Example 1.

[0044] Figure 3 This is a schematic diagram of the process of uniformly dripping whitening hydrogel into the bracket of the soft braces in Example 1.

[0045] Figure 4 The figure is a comparison chart of the whitening factor solution prepared in Example 1 and the blank control solution.

[0046] Figure 5 This is a comparison chart of the whitening effect produced by the whitening factor prepared in Example 1 releasing H2O2.

[0047] Figure 6 This is a curve chart of the amount of H2O2 produced by the whitening factor prepared in Example 1 within 3 hours.

[0048] Figure 7 These are images of the hydrogel dental cap loaded with whitening factors prepared in Example 1 0 hour before use and 12 hours after use, wherein A is the image 0 hour before use and 12 hours after use, and B is an enlarged view of the left image in A. DETAILED DESCRIPTION

[0049] The present invention will be further described in detail below in conjunction with the examples, but the embodiments of the present invention are not limited to the following examples.

[0050] The raw materials used in the present invention are all commercially available.

[0051] Example 1

[0052] (1) According to the patient's tooth arrangement, 3D printing technology is used to print out a target model with a positioning mark base, and a transparent brace is obtained by molding and laser cutting;

[0053] (2) Using the above-obtained transparent dental brace as a template, 30 parts of the basic components of Dow Corning SYLGARD 184 material and 3 parts of the curing agent were mixed evenly, placed in a vacuum drying oven for vacuum degassing, and then poured into the transparent dental brace, and the excess mixed material was pressed out, and finally placed in a vacuum drying oven for solidification and demolding to obtain the following Figure 1 Soft braces shown;

[0054] (3) 0.05 parts of anhydrous calcium chloride and 1.5 parts of polyvinyl pyrrolidone were dissolved in 20 parts of methanol to form a mixed component, and the pH value of the mixed component was adjusted to 9 with 1.5 parts of sodium hydroxide. Then, 0.5 parts of hydrogen peroxide was injected into the mixed component through a microinjection pump, and the mixture was centrifuged at 10,000 rpm for 10 minutes and washed several times to obtain a whitening factor. The transmission electron microscopy image of the whitening factor is shown in FIG. Figure 2 shown.

[0055] (4) dissolving 0.8 parts of gelatin and 0.4 parts of sodium pyrrolidone hydroxyapatite in 20 parts of water, stirring and allowing to stand to obtain a hydrogel;

[0056] (5) Mix the whitening factor and the hydrogel in a ratio of 2:5 to obtain a hydrogel loaded with the whitening factor, and evenly drip the hydrogel loaded with the whitening factor into the bracket of the soft braces. Figure 3 As shown, a hydrogel dental cap loaded with whitening factors was obtained.

[0057] Example 2

[0058] (1) According to the patient's tooth arrangement, 3D printing technology is used to print out a target model with a positioning mark base, and a transparent brace is obtained by molding and laser cutting;

[0059] (2) Using the above-obtained transparent dental brace as a template, 30 parts of the basic components of Dow Corning SYLGARD 184 material and 3 parts of the curing agent were mixed evenly, placed in a vacuum drying oven for vacuum degassing, and then poured into the transparent dental brace, and the excess mixed material was pressed out, and finally placed in a vacuum drying oven for solidification and demolding to obtain a soft dental brace;

[0060] (3) 0.05 parts of anhydrous sodium chloride and 1.5 parts of polyvinyl alcohol were dissolved in 20 parts of methanol to form a mixed component, and the pH value of the mixed component was adjusted to 9 with 1.5 parts of sodium hydroxide. Then, 0.5 parts of sodium peroxide was injected into the mixed component through a microinjection pump, centrifuged at 10,000 rpm for 10 minutes, and washed several times to obtain a whitening factor;

[0061] (4) dissolving 0.8 parts of gelatin and 0.4 parts of sodium pyrrolidone hydroxyapatite in 20 parts of water, stirring and allowing to stand to obtain a hydrogel;

[0062] (5) The whitening factor and the hydrogel are mixed in a ratio of 2:5 to obtain a hydrogel loaded with the whitening factor, and the hydrogel loaded with the whitening factor is evenly dripped into the bracket of the soft braces to obtain a hydrogel braces loaded with the whitening factor.

[0063] Example 3

[0064] (1) According to the patient's tooth arrangement, 3D printing technology is used to print out a target model with a positioning mark base, and a transparent brace is obtained by molding and laser cutting;

[0065] (2) Using the above-obtained transparent dental brace as a template, 30 parts of the basic components of Dow Corning SYLGARD 184 material and 3 parts of the curing agent were mixed evenly, placed in a vacuum drying oven for vacuum degassing, and then poured into the transparent dental brace, and the excess mixed material was pressed out, and finally placed in a vacuum drying oven for solidification and demolding to obtain a soft dental brace;

[0066] (3) 0.1 parts of anhydrous zinc chloride and 1.5 parts of polyvinyl alcohol were dissolved in 20 parts of methanol to form a mixed component, and the pH value of the mixed component was adjusted to 9 with 1.5 parts of sodium hydroxide. Then, 0.5 parts of sodium peroxide was injected into the mixed component through a microinjection pump, centrifuged at 10000 rpm for 10 minutes, and washed several times to obtain a whitening factor;

[0067] (4) dissolving 0.8 parts of gelatin and 0.4 parts of sodium pyrrolidone hydroxyapatite in 20 parts of water, stirring and allowing to stand to obtain a hydrogel;

[0068] (5) The whitening factor and the hydrogel are mixed in a ratio of 2:5 to obtain a hydrogel loaded with the whitening factor, and the hydrogel loaded with the whitening factor is evenly dripped into the bracket of the soft braces to obtain a hydrogel braces loaded with the whitening factor.

[0069] Example 4

[0070] (1) According to the patient's tooth arrangement, 3D printing technology is used to print out a target model with a positioning mark base, and a transparent brace is obtained by molding and laser cutting;

[0071] (2) Using the above-obtained transparent dental brace as a template, 30 parts of the basic components of Dow Corning SYLGARD 184 material and 3 parts of the curing agent were mixed evenly, placed in a vacuum drying oven for vacuum degassing, and then poured into the transparent dental brace, and the excess mixed material was pressed out, and finally placed in a vacuum drying oven for solidification and demolding to obtain a soft dental brace;

[0072] (3) 0.05 parts of anhydrous zinc chloride and 1.5 parts of polyvinyl alcohol were dissolved in 20 parts of methanol to form a mixed component, and the pH value of the mixed component was adjusted to 9 with 1.5 parts of sodium hydroxide. Then, 0.5 parts of sodium peroxide was injected into the mixed component through a microinjection pump, and the mixture was centrifuged at 10,000 rpm for 10 minutes, and washed several times to obtain a whitening factor;

[0073] (4) dissolving 0.8 parts of gelatin and 0.4 parts of copper pyrrolidone hydroxyapatite in 25 parts of water, stirring and allowing to stand to obtain a hydrogel;

[0074] (5) The whitening factor and the hydrogel are mixed in a ratio of 3:5 to obtain a hydrogel loaded with the whitening factor, and the hydrogel loaded with the whitening factor is evenly dripped into the bracket of the soft braces to obtain a hydrogel braces loaded with the whitening factor.

[0075] Performance test: The performance test of the hydrogel dental cap loaded with whitening factor obtained in Example 1 was carried out, specifically:

[0076] (1) The morphology of the whitening factor prepared in Example 1 was characterized using a transmission electron microscope:

[0077] like Figure 2 As shown in FIG. 1 , the whitening factor is spherical or quasi-spherical under a transmission electron microscope, with a relatively uniform size and good dispersion. The appearance of the whitening factor solution is compared with that of the blank control, as shown in FIG. Figure 4 As shown, the whitening factor has good dispersion performance in water.

[0078] (2) Detecting the ability of the whitening factor prepared in Example 1 to release H2O2:

[0079] The production of H2O2 is detected by potassium titanium oxalate. H2O2 can form an orange complex with potassium titanium oxalate in an acidic solution. The higher the H2O2 content, the darker the color of the complex. Figure 5 As shown, the prepared whitening factor solution is easy to compare with the blank control, and the color becomes darker, indicating that the whitening factor solution can produce H2O2 and has good whitening performance. Figure 6 As shown, the H2O2 content generated in the whitening factor solution increased slowly and approached equilibrium within two hours, indicating that the whitening factor can slowly release H2O2.

[0080] (3) Testing the whitening ability of the hydrogel dental cap loaded with whitening factors prepared in Example 1:

[0081] Weigh 5g of black tea leaves and soak them in 20ml of hot water. Soak the tooth mold in the black tea water until the water completely covers the teeth. After soaking for 3 days, yellow stains will form on the surface of the tooth mold. Figure 7The hydrogel dental cap loaded with whitening factor was prepared according to the method of Example 1, and the photo was taken after 12 hours of use.

[0082] Figure 7 The images of the hydrogel dental cap loaded with whitening factors prepared in Example 1 are shown 0 hours before use and 12 hours after use, wherein Figure 7 As shown, after the tooth mold was soaked in black tea, obvious yellow stains formed on the tooth surface. After using the hydrogel cap loaded with whitening factors prepared in Example 1 for 12 hours, the yellow stains on the teeth disappeared, the appearance was improved, and the whitening effect was obvious.

[0083] The embodiments described above provide a detailed description of the technical solutions of the present invention. It should be understood that the above are only specific examples of the present invention and are not intended to limit the present invention. Any modifications, supplements or similar substitutions made within the scope of the principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A hydrogel brace loaded with whitening factors, including a soft brace, characterized in that: The inner layer of the soft braces has a hydrogel containing whitening factors, which is calculated by weight. The raw material components of the soft braces are 30-60 parts of polydimethylsiloxane and 3.0-6.0 parts of curing agent; The raw material components of the whitening factor are 0.01-0.1 parts of soluble metal salt, 0.5-1.5 parts of combining agent, 20-40 parts of dispersant I, 1.0-3.5 parts of pH adjusting agent, and 0.2-0.8 parts of oxidant; The raw material components of the hydrogel are 0.5-1.5 parts of gelatin, 20-25 parts of dispersant II, and 0.1-0.5 parts of colloid stabilizer; The mass ratio of the whitening factor to the hydrogel is 0.4-0.6:

1.

2. The hydrogel dental cap loaded with whitening factors according to claim 1, characterized in that: Among the whitening factors, The soluble metal salt is at least one of a manganese salt, a sodium salt, a calcium salt, a zinc salt, an iron salt, and a copper salt; The combined agent is at least one of polyvinyl alcohol, polyvinyl pyrrolidone and copovidone; The dispersant I is at least one of ethanol, methanol, ethylene glycol and acetone; The pH regulator is at least one of sodium hydroxide, ammonia water and sodium carbonate; The oxidant is at least one of sodium peroxide, hydrogen peroxide and peracetic acid.

3. The hydrogel dental cap loaded with whitening factors according to claim 2, characterized in that: In the whitening factor, the soluble metal salt is a calcium salt and the oxidant is hydrogen peroxide.

4. The hydrogel dental cap loaded with whitening factors according to claim 1, characterized in that: In the hydrogel, The dispersant II is at least one of ethanol, methanol, water and propylene glycol; The colloidal stabilizer is at least one of zinc pyrrolidone hydroxyapatite, copper pyrrolidone hydroxyapatite and sodium pyrrolidone hydroxyapatite.

5. The method for preparing the hydrogel dental cap loaded with whitening factors according to any one of claims 1 to 4, comprising the following steps: (1) According to the patient's tooth arrangement, a digital dental model is obtained by full-mouth dental scanning, and a target model with a positioning mark base is printed using 3D printing technology. A transparent brace is obtained by molding and laser cutting; (2) Mixing polydimethylsiloxane and curing agent in proportion, and after vacuum degassing, pouring the mixed material into the transparent braces obtained in step (1), pressing to expel excess mixed material, and demolding after solidification to obtain a soft braces; (3) dissolving the soluble metal salt and the combining agent in the dispersant I and mixing them evenly, adjusting the pH value with a pH adjusting agent, injecting the oxidant through a microinjection pump, and centrifuging and washing the mixed solution to obtain the whitening factor; (4) dissolving gelatin and a colloidal stabilizer in a dispersant II, mixing and stirring to obtain a hydrogel; (5) The whitening factor obtained in step (3) is mixed with the hydrogel obtained in step (4) to obtain a hydrogel loaded with the whitening factor, and the hydrogel is evenly dripped into the soft braces obtained in step (2) to obtain a hydrogel braces loaded with the whitening factor.

6. The method for preparing the hydrogel dental braces according to claim 5, characterized in that: In step (2), the coagulation temperature is 60-80°C and the coagulation time is 20-30 minutes.

7. The method for preparing the hydrogel dental cap according to claim 5, characterized in that: In step (3), the pH value is adjusted to 7-11.

8. The method for preparing the hydrogel dental cap according to claim 5, characterized in that: In step (3), the centrifugal speed is 8000-11000 rpm, and the centrifugal time is 10-30 min.

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