CN110302067B - Adjuvant with tooth whitening and repairing functions and preparation method thereof - Google Patents
Adjuvant with tooth whitening and repairing functions and preparation method thereof Download PDFInfo
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- CN110302067B CN110302067B CN201810229333.XA CN201810229333A CN110302067B CN 110302067 B CN110302067 B CN 110302067B CN 201810229333 A CN201810229333 A CN 201810229333A CN 110302067 B CN110302067 B CN 110302067B
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- bioactive glass
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Images
Classifications
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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
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
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- 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
- A61K8/25—Silicon; Compounds thereof
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- 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
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- 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
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- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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- 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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- Veterinary Medicine (AREA)
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Abstract
The invention discloses an adjuvant with tooth whitening and repairing functions and a preparation method thereof. The adjuvant can prevent the whitening agent carbamide peroxide from generating chemical reaction with the bioactive glass repair material to be inactivated. In the using process, the natural water-soluble polymer coating can disintegrate in water to slowly release bioglass components, so that the dual effects of tooth whitening and tooth restoration are realized; meanwhile, toothpaste tube expansion caused by the reaction of the bioactive glass and the carbamide peroxide is avoided, the stability of the product is improved, and the shelf life of the product is prolonged. The adjuvant has the advantages of simple preparation method, wide raw material source, low cost and convenient operation, and is beneficial to industrial production. The adjuvant can be used for various whitening and tooth cleaning objects for oral cavity, such as toothpaste, chewing gum, embrocation tooth powder, tooth paste, bleaching gel and the like, and has good application prospect.
Description
Technical Field
The invention belongs to the technical field of oral care, and particularly relates to an adjuvant with tooth whitening and repairing functions and a preparation method thereof.
Background
In China, various influences are caused on teeth along with age change, long-term diet and poor living habits, and one of the most common results is tooth discoloration, such as tooth darkening, yellowing, blackening and the like. The most common staining of teeth, caused by overeating some easily stained foods such as tea, coffee, dark foods and smoking, is mainly manifested by extrinsic pigments or deposits of pigments produced by bacteria in the oral cavity. If certain drugs are taken during tooth development, excessive fluoride intake, or the use of tooth restoration materials can cause staining, such as tetracycline pigmentation, dental fluorosis, incomplete development of enamel, and the like. However, it is an everyday pursuit of beauty to have a healthy white set of teeth, and tooth whitening is becoming a basic requirement of modern people for high quality life. Bleaching is the simplest cosmetic treatment for most people, with up to a million people receiving dentist bleaching treatments each year in china, and there may be more people purchasing commercially available products to try to perform tooth bleaching themselves.
In practice, in-office bleaching is usually carried out directly using higher concentrationsThe hydrogen peroxide solution is used as an oxidation bleaching agent, and meanwhile, the decomposition of the hydrogen peroxide is accelerated by means of illumination, ultrasound and the like. Household tooth bleaching gels typically use urea peroxide as the oxidizing active of the bleaching gel. Carbamide Peroxide (CP) is one of the most widely used preparations for tooth whitening. 10% of CP is a common drug for household bleaching, CP can be decomposed into 6.4% of urea and 3.6% of Hydrogen Peroxide (HP), and HP is decomposed into water, oxygen and superoxide radical HO-The free radicals undergo oxidation reactions with the pigment molecules of the teeth. The urea released by CP is alkaline, and can raise pH value in oral cavity and tray, and reduce side effect of bleaching agent. Urea also has anticarious effect, and can be used for treating root caries and improving oral hygiene. CP causes less adverse reaction clinically and is more stable than HP. In view of these advantages of CP, research on its use in the field of tooth whitening has been actively conducted.
The carbamide peroxide has good stability and is convenient to store, and can release hydrogen peroxide molecules at a certain speed under a certain condition to realize the bleaching of teeth. However, the above-mentioned methods also simultaneously "bleach" the enamel and dentin during the bleaching of the tooth surface, i.e., the bleaching agent destroys the organic substances in the enamel and dentin at the same time, resulting in tooth damage. In the bleaching of living pulp teeth, it is most likely that the gums are in contact due to the bleaching agent spillage. Numerous studies have shown that: the hydrogen peroxide produced by the bleaching agent is toxic to human gingival fibroblasts. Moreover, excessive hydrogen peroxide can also stimulate oral mucosa, throat mucosa and possible swallowing stomach mucosa, thus causing damage to digestive tract tissues.
The whitening toothpaste is used most frequently in households to whiten teeth, and the principle of the whitening toothpaste is to add bleaching substances such as carbamide peroxide into the toothpaste to bleach the teeth. The whitening toothpaste has the same bleaching principle as the whitening gel, and effectively avoids the damage to teeth, gums and oral cavity caused by directly using the whitening agent. However, some common raw materials in the toothpaste formula, such as bioglass with good tooth tissue restoration ability, are not well compatible with carbamide peroxide, and they accelerate the oxidation of carbamide peroxide, especially, the moisture in the toothpaste can promote the oxidation reaction to accelerate the release of active oxygen, thereby losing the whitening effect on teeth, and causing the problems of toothpaste tube expansion and preparation segregation. Therefore, there is a need for a method for preparing a whitening and repairing adjuvant having a tooth damage repairing function, which can effectively prevent toothpaste from expanding without weakening the whitening effect of toothpaste and can also serve as a technique for repairing tooth tissues.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, prevent the inactivation of whitening agent carbamide peroxide and bioactive glass repair materials due to chemical reaction, avoid toothpaste tube expansion caused by the reaction of bioactive glass and carbamide peroxide, and provide a tooth whitening repair adjuvant with tooth injury repair function.
The invention also aims to provide a preparation method of the tooth whitening and repairing adjuvant.
The invention also aims to provide application of the tooth whitening and repairing adjuvant.
The purpose of the invention is realized by the following technical scheme:
a tooth whitening repair adjuvant comprising: encapsulating bioactive glass and carbamide peroxide. The encapsulated bioactive glass is formed by a natural water-soluble polymer film and enwraps the bioactive glass.
The natural water-soluble polymer and the bioactive glass in the encapsulated bioactive glass are preferably mixed according to the mass ratio of 1: 1-3: 1.
The encapsulated bioactive glass is preferably prepared by a reverse microemulsion method.
The natural water-soluble polymer is preferably a surface sizing agent, alginic acid and water-soluble derivatives thereof, modified cellulose and modified chitosan.
The surface sizing agent can be one or at least two of natural starch, vegetable gum, animal gum (casein), chitin and the like.
The modified cellulose can be one or at least two of carboxymethyl cellulose, methyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose and the like.
The modified chitosan can be one or at least two of carboxymethyl chitosan, chitosan oligosaccharide, chitosan hydrochloride, chitosan quaternary ammonium salt, chitosan lactate, chitosan glutamate, chitosan sulfate, hyaluronic acid-like chitosan and the like.
The bioactive glass refers to an inorganic glass substance having silicon oxide as its main component and capable of bonding with a growing tissue when reacting with a physiological solution. For example, the bioactive glass of the present invention is a glass composition that will form a layer of hydroxyapatite in vitro when placed in simulated body fluid. The bioactive glass of the present invention is also biocompatible so that it does not elicit an overwhelming adverse immune response in vivo, for example, in the oral cavity.
The bioactive glass is well known to those skilled in the art and contains inorganic active ions such as K, Na, Sr, Mg, Mn, Fe, Si, Ca, Ag and the like; such as bioactive glass powder.
The preparation method of the tooth whitening and repairing adjuvant comprises the following steps:
(1) preparing a mixed solution: dissolving natural water-soluble polymer to obtain natural water-soluble polymer solution; dispersing bioactive glass in the natural water-soluble polymer solution, and removing bubbles by ultrasonic to obtain a mixed solution;
(2) preparing the encapsulated bioactive glass: preparing the encapsulated bioactive glass by a reverse micro-emulsion method based on the mixed solution in the step (1), cleaning and drying;
(3) and (3) uniformly mixing the encapsulated bioactive glass prepared in the step (2) with a certain amount of carbamide peroxide to obtain the tooth whitening and repairing adjuvant.
The natural water-soluble polymer and the bioactive glass in the step (1) are preferably mixed according to the mass ratio of 1: 1-3: 1; further preferably 1.5: 1.
The natural water-soluble polymer solution and the mixed solution in the step (1) are preferably prepared at 1-4 ℃.
The reversed-phase microemulsion method in the step (2) is preferably realized by a spray dryer, and the mixed solution in the step (1) is sprayed into an oil phase by using an atomizer.
The drying in step (2) is preferably freeze-drying.
The application of the tooth whitening and repairing adjuvant is added into a whitening dentifrice for oral cavity.
The tooth cleaning substance comprises toothpaste, chewing gum, brushing tooth powder, tooth paste, bleaching gel and the like.
The application method specifically comprises the following steps: adjusting the pH value of the dentifrice to 6.4-7 by using a pH value regulator, adding the tooth whitening and repairing adjuvant into the dentifrice, and uniformly stirring.
The pH value regulator is preferably sodium citrate.
The addition amount of the tooth whitening and repairing adjuvant is preferably 3-10% of the mass fraction of the encapsulated bioactive glass in the tooth cleaning product.
Compared with the prior art, the invention has the following advantages and effects:
the invention achieves better tooth restoration effect by the slow release function of the encapsulated bioactive glass (natural water-soluble polymer film/bioactive glass microspheres); the natural water-soluble polymer coating prevents urea peroxide from being directly contacted with bioactive glass to generate chemical reaction and inactivation, effectively prevents the toothpaste from expanding, and prolongs the shelf life of the whitening toothpaste. Meanwhile, in the using process, the natural water-soluble polymer coating is disintegrated when meeting water, and bioactive glass components are slowly released, so that the effect of repairing the tooth tissue is effectively achieved; the aim of repairing tooth tissues is achieved on the basis of not weakening the whitening effect of the toothpaste.
Meanwhile, the method has the advantages of wide raw material source, low cost and convenient operation, and is beneficial to industrial production.
Drawings
FIG. 1 is a scanning electron micrograph of the bioactive glass and the encapsulated bioactive glass of example 1.
Fig. 2 is a photograph showing the effect of the whitening effect test of example 6; the control group is on the left side, and the experimental group is on the right side.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1 preparation of whitening repair adjuvant
1. Preparation of Natural Water-soluble Polymer film/bioactive glass Mixed solution (taking Chitosan as an example)
Dissolving chitosan powder in 1% acetic acid solution to prepare chitosan solution with the concentration of 2% -5%, and after the chitosan is uniformly dissolved, enabling the bioglass to be in a ratio of m (bioglass): dissolving m (chitosan) in a ratio of 1: 1-3: 1 in a chitosan solution, ultrasonically removing bubbles from the obtained chitosan/bioglass mixed solution, and storing at 4 ℃ for later use.
2. Preparation of encapsulated bioactive glass by reverse micro-emulsion method
Preparing the chitosan/bioglass mixed solution prepared in the step 1 into microspheres by using a spray dryer, wherein the specific conditions are as follows: the inlet temperature is 220 ℃, the outlet temperature is 130 ℃, the air inlet pressure is 0.3MPa, and the air inlet ratio is 90 percent. And then the prepared encapsulated bioactive glass is dried in vacuum at normal temperature for standby.
3. Preparation of whitening repair adjuvant
And (3) mixing the encapsulated bioactive glass obtained in the step (2) with a certain amount of carbamide peroxide to obtain the whitening repair adjuvant.
By the preparation method, various groups of encapsulated bioactive glass in the table 1 are prepared according to the formula:
TABLE 1
Example 2 morphological Observation of Encapsulated bioactive glasses
The surface appearance of the encapsulated bioactive glass-1 is observed by adopting an S-570 scanning electron microscope of Hitachi company, gold is uniformly sprayed on the surface of a sample by adopting an ion spray coating method, and then the sample is placed on an electron microscope stage for observation. The technological parameters are as follows: accelerating and pressurizing by voltage of 20kV, current of 0.5mA and incident angle of 10-20 degrees; the results are shown in FIG. 1.
As can be seen from fig. 1, the bioactive glass exhibits irregular particle morphology before being coated with the chitosan film; after the chitosan film is wrapped, the chitosan film presents a regular spherical shape and is regular and ordered.
Example 3 colloidal stability assay
Colloidal stability measurements were made for the different dentifrice colloidal compositions of the components.
The control group selects common toothpaste in the market; the experimental group 1 is that urea peroxide with the mass ratio of 1 percent and bioactive glass (CaO. P) with the mass ratio of 3 percent are added into common toothpaste2O5·Na2O·SiO2) (ii) a The experimental group 2 is the common toothpaste added with 1% by mass of carbamide peroxide and 3% by mass of the encapsulated bioactive glass-1 prepared in the example 1; the colloids obtained from the control group, experimental group 1, and experimental group 2 were encapsulated in the sealing tape, the volume of gas generated in the sealing bag was measured, and the gas generation was observed at different intervals (using different numbers of + to represent), with the results shown in table 2:
TABLE 2
As can be seen from Table 2, the gas generation of the encapsulated bioactive glass of the present invention was much lower than that of experimental group 1 at the same time interval of treatment, and thus it was found that the colloidal stability of the dentifrice colloidal composition to which the encapsulated bioactive glass of the present invention was added was greatly improved; effectively prevents the expansion of the toothpaste and prolongs the shelf life of the whitening toothpaste.
Example 4 colloidal stability assay
Colloidal stability measurements were performed on the different dentifrice colloidal compositions of the components.
The control group selects common toothpaste in the market; the experimental group 1 is that urea peroxide with the mass ratio of 1 percent and bioactive glass (CaO. P) with the mass ratio of 3 percent are added into common toothpaste2O5·K2O·SiO2) (ii) a Experimental group 2 is a common toothpaste with 1% by weight of carbamide peroxide and 3% by weight of the encapsulated bioactive glass-2 prepared in example 1. The gels obtained from the control group, experimental group 1, and experimental group 2 were packed in a sealing tape, and the gas generation amounts (expressed by + different amounts) were observed at different intervals, and the results are shown in table 3:
TABLE 3
As can be seen from Table 3, the gas generation of the encapsulated bioactive glass of the present invention was much lower than that of experimental group 1 at the same time interval of treatment, and thus it was found that the colloidal stability of the dentifrice colloidal composition to which the encapsulated bioactive glass of the present invention was added was greatly improved; effectively prevents the toothpaste from expanding and prolongs the shelf life of the whitening toothpaste.
Example 5 colloidal stability assay
Colloidal stability measurements were performed on the different dentifrice colloidal compositions of the components. The control group selects common toothpaste in the market; the experimental group 1 is that urea peroxide with the mass ratio of 1 percent and bioactive glass (CaO. P) with the mass ratio of 3 percent are added into common toothpaste2O5·K2O·SiO2) (ii) a Experimental group 2 was a general toothpaste containing 1% by mass of carbamide peroxide and 3% by mass of the encapsulated bioactive glass-3 prepared in example 1. The control, experimental 1 and experimental 2 groups were encapsulated in a sealing tape, and the gas generation amounts (expressed by + different amounts) were observed at different intervals, and the results are shown in table 4:
TABLE 4
As can be seen from Table 4, the gas generation of the encapsulated bioactive glass of the present invention was much lower than that of experimental group 1 at the same time interval of treatment, and thus it was found that the colloidal stability of the dentifrice colloidal composition to which the encapsulated bioactive glass of the present invention was added was greatly improved; effectively prevents the toothpaste from expanding and prolongs the shelf life of the whitening toothpaste.
Example 6 whitening Effect test
Whitening effect tests were performed on different dentifrice gel compositions in terms of composition. The control group selects common toothpaste in the market; the experimental group is that urea peroxide with the mass ratio of 1% and the encapsulated bioactive glass-1 prepared in the example 1 with the mass ratio of 3% are added into common toothpaste. Bovine teeth were selected as whitening samples for the experiments. Each group was asked to brush the teeth evenly and quickly over the tooth surface using the same volume of toothpaste or gel composition on each brush, and to brush the stained area of the teeth repeatedly for 2 minutes, once a day, morning and evening. The end of test statistics are shown in table 5 (whitening effect is represented by different numbers of +:
TABLE 5
As shown in fig. 2 and table 5, the whitening effect of the experimental group added with the encapsulated bioactive glass-1 of the present invention was considerably improved compared to the control group; wherein, the left side of the graph 2 is a control group, the color and luster whiteness is poor, and the right side is an experimental group, the color and luster whiteness is obviously better.
Example 7 whitening Effect test
Whitening effect tests were performed on different dentifrice gel compositions. The control group selects common toothpaste in the market; the experimental group is that 1% of carbamide peroxide and 3% of the encapsulated bioactive glass-2 prepared in the example 4 are added into common toothpaste. Bovine teeth were selected as whitening samples for the experiments. Each group was asked to brush the teeth evenly and quickly over the tooth surface using the same volume of toothpaste or gel composition on each brush, and to brush the stained area of the teeth repeatedly for 2 minutes, once a day, morning and evening. The end of test statistics are shown in table 6 (whitening effect is represented by different numbers of +:
TABLE 6
As shown in table 6, the whitening effect of the experimental group added with the encapsulated bioactive glass of the present invention was significantly improved as compared with the control group.
Example 8 cytotoxicity assay
Cytotoxicity tests were conducted by the agar diffusion method in the biological evaluation of YY/T0127.9-2014 oral medical instruments, and the cytotoxicity of colloidal compositions of different components (i.e., the composition of encapsulated bioactive glass and carbamide peroxide in Table 7) was evaluated, and 2.5X 10 cells were prepared from L929 cell line (mouse fibroblast) and growth medium5The cell suspension was pipetted 10mL and added to the culture dish for 24 h. Then sucking out the culture solution, adding 10mL of new agar, adding neutral red staining solution after the agar culture medium is solidified, preserving for 30min, and sucking off the excess staining solution. The colloidal composition and control group (growth medium as negative control group, filter membrane soaked in phenol solution as positive control group) were uniformly coated on the filter membrane, and placed in a petri dish. 5% carbon dioxide, and culturing at 37 deg.C in dark for 24 h. The discolored area around the experimental and control materials was observed with an inverted microscope and the results are shown in table 7.
TABLE 7 colloidal composition agar diffusion method test results
As shown in Table 7, the combination of the encapsulated bioactive glass of the present invention and carbamide peroxide all showed slight cytotoxicity compared with the control sample; urea peroxide alone showed moderate cytotoxicity; the results indicate that the addition of encapsulated bioactive glass helps to improve the cytotoxicity of carbamide peroxide.
The above examples prove that the invention not only prevents the inactivation of whitening agent carbamide peroxide caused by chemical reaction with bioactive glass type repairing materials, but also effectively realizes the tooth repairing effect of bioactive glass without weakening the whitening effect of toothpaste; and also reduces the cytotoxicity of carbamide peroxide; effectively prevents the toothpaste from expanding, prolongs the shelf life of the whitening toothpaste and has good application prospect. Meanwhile, after the bioactive glass is compounded and encapsulated, the cytotoxicity is lower than that of the carbamide peroxide used alone. Therefore, the implementation of the invention can help to develop novel toothpaste additives; improving the technical progress in the field of tooth whitening and restoration.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. A preparation method of a tooth whitening and repairing adjuvant is characterized by comprising the following steps:
(1) preparing a mixed solution: dissolving natural water-soluble polymer to obtain natural water-soluble polymer solution; dispersing bioactive glass in the natural water-soluble polymer solution, and removing bubbles by ultrasonic to obtain a mixed solution; the natural water-soluble polymer and the bioactive glass are mixed according to the mass ratio of 1: 1-3: 1; the natural water-soluble polymer is natural starch, hydroxypropyl methylcellulose or carboxymethyl chitosan;
(2) preparing the encapsulated bioactive glass: preparing the encapsulated bioactive glass by a reverse micro-emulsion method based on the mixed solution in the step (1), cleaning and drying;
(3) and (3) uniformly mixing the encapsulated bioactive glass prepared in the step (2) with a certain amount of carbamide peroxide to obtain the tooth whitening and repairing adjuvant.
2. The method for preparing the adjuvant for tooth whitening and restoration according to claim 1, wherein:
and (2) preparing the natural water-soluble polymer solution and the mixed solution in the step (1) at 1-4 ℃.
3. A tooth whitening and repairing adjuvant is characterized in that: prepared by the preparation method of any one of claims 1-2.
4. The use of the adjuvant for tooth whitening restoration according to claim 3 in the preparation of a product for tooth whitening restoration, characterized in that:
the application is that the whitening toothpaste is added into a whitening toothpaste for oral cavity.
5. The use of the adjuvant for tooth whitening repair according to claim 4, characterized in that:
the dentifrice is selected from toothpaste, chewing gum, brushing dentifrice, tooth paste or bleaching gel.
6. The use of the adjuvant for tooth whitening repair according to claim 4, characterized in that:
the application method specifically comprises the following steps: adjusting the pH value of the dentifrice to 6.4-7 by using a pH value regulator, adding the tooth whitening and repairing adjuvant into the dentifrice, and uniformly stirring.
7. The use of the adjuvant for tooth whitening repair according to claim 4, characterized in that:
the addition amount of the tooth whitening and repairing adjuvant is 3-10% of the mass fraction of the encapsulated bioactive glass in the tooth cleaning substance.
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