CN113509394A - Mineralized glycerin gel, preparation method and application - Google Patents
Mineralized glycerin gel, preparation method and application Download PDFInfo
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- CN113509394A CN113509394A CN202110793310.3A CN202110793310A CN113509394A CN 113509394 A CN113509394 A CN 113509394A CN 202110793310 A CN202110793310 A CN 202110793310A CN 113509394 A CN113509394 A CN 113509394A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/15—Compositions characterised by their physical properties
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/831—Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
- A61K6/838—Phosphorus compounds, e.g. apatite
Abstract
The invention relates to mineralized glycerin gel, a preparation method and application thereof, wherein the preparation method comprises the following steps: dissolving a cation source in a glycerol solution to obtain a first solution; dissolving an anion source in a glycerol solution to obtain a second solution; and adding the second solution into the first solution for mixing to form mineralized glycerin gel. The method has the advantages that the mineralized glycerin gel can be prepared by directly mixing the glycerin solution containing the cation source and the glycerin solution containing the anion source, the preparation method is simple, no additional additive is needed, the types and the using amount of raw materials are reduced, and the production cost is greatly reduced; the prepared mineralized glycerin gel contains glycerin and mineral substances, is in a gel state below 50 ℃, is convenient to store, transport and use, and reduces the use cost; the mineralized glycerin gel can remineralize the tooth surface, repair enamel, and prevent the tooth decay from developing again.
Description
Technical Field
The invention relates to the technical field of tooth restoration, in particular to mineralized glycerin gel, a preparation method and application.
Background
Dental caries is a high incidence disease which is harmful to human health and can be generally divided into superficial caries, middle caries and deep caries. Among them, superficial caries occurring in the enamel layer of teeth surface is common. If superficial caries is not treated in time, it is easy to cause deep caries cavity and further damage dentin, dental pulp, etc.
The common superficial caries treatment method at present is to fill with dental resin, however, the method is easy to form gaps at the interface of the resin and the tooth after treatment, and causes the caries to develop again. In addition, the dental resin has large difference with teeth and mismatched mechanical properties, so that the restoration effect and functional reconstruction are not very ideal.
The main component of tooth is hydroxyapatite which is a kind of calcium phosphate substance, and the dental caries is caused by the loss of calcium phosphate component. Through tooth surface remineralization, a new calcium phosphate layer is formed, the microstructure of the calcium phosphate layer is the same as or similar to that of tooth enamel, and the calcium phosphate layer is an ideal tooth enamel restoration strategy. In recent years, some dental restorative products have appeared on the market, which can help minerals on the surface of teeth to achieve a certain degree of restoration, but at present, products which perfectly achieve the above strategies have not yet appeared.
At present, no effective solution is provided for the problems of incapability of remineralizing and low mineralization efficiency of tooth surfaces and the like in the related technology.
Disclosure of Invention
The present application aims to overcome the defects in the prior art, and provides a mineralized glycerin gel, a preparation method and an application thereof, so as to solve at least the problems that the tooth surface cannot be remineralized and the mineralization efficiency is low in the related technologies.
In order to achieve the purpose, the technical scheme adopted by the application is as follows:
in a first aspect, the present invention provides a method for preparing a mineralized glycerol gel, comprising:
dissolving a cation source in a glycerol solution to obtain a first solution;
dissolving an anion source in a glycerol solution to obtain a second solution;
adding the second solution into the first solution for mixing to form mineralized glycerin gel;
wherein the mineralized glycerol gel is in a gel state within 50 ℃;
wherein the cation source is water-soluble mineral salt, and the anion source is water-soluble inorganic acid and/or water-soluble inorganic acid salt;
wherein, in the mixed solution, the concentration of the cation source is 0.01-10 mol/L, the concentration of the anion source is 0.01-10 mol/L, and the molar ratio of the cation source to the anion source is 0.1-5: 1.
in some of these embodiments, the mineralized glycerol gel is gelatinous up to 45 ℃.
In some of these embodiments, the mineralized glycerol gel is gelatinous up to 40 ℃.
In some of these embodiments, the mineralized glycerol gel is gelatinous up to 38 ℃.
In some of these embodiments, the mineralized glycerol gel is gel-like at 4-38 ℃.
In some of these embodiments, the mineralized glycerol gel has a viscosity of 2500 mPa-s or greater.
In some embodiments, the cation source is one or a combination of calcium ion and magnesium ion.
In some embodiments, the cation source is one or more of a water-soluble calcium salt, a water-soluble magnesium salt.
In some embodiments, the cation source is one or more of calcium chloride, calcium nitrate, calcium acetate, magnesium chloride, magnesium nitrate, and magnesium acetate.
In some embodiments, the anion source is one or a combination of phosphate ion, sulfate ion, and carbonate ion.
In some embodiments, the anion source is one or more of water-soluble phosphate, water-soluble sulfate, and water-soluble carbonate.
In some of these embodiments, the anion source is a water soluble sodium salt comprising phosphate, a water soluble potassium salt comprising phosphate, a water soluble ammonium salt comprising phosphate, a water soluble sodium salt comprising sulfate, a water soluble potassium salt comprising sulfate, a water soluble ammonium salt comprising sulfate, a water soluble sodium salt comprising carbonate, a water soluble potassium salt comprising carbonate, a water soluble ammonium salt comprising carbonate.
In some of these embodiments, the anion source is one or a combination of phosphoric acid, sodium phosphate, sodium monohydrogen phosphate, sodium dihydrogen phosphate, potassium monohydrogen phosphate, potassium dihydrogen phosphate, ammonium monohydrogen phosphate, ammonium dihydrogen phosphate, sodium sulfate, sodium bisulfate, potassium sulfate, potassium bisulfate, ammonium sulfate, ammonium bisulfate, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, ammonium carbonate, and ammonium bicarbonate.
In some of these embodiments, the glycerol solution is a pure glycerol solution or a glycerol solution containing water;
wherein, in the glycerol solution containing water, the mass percent of the water is less than 50 percent.
In some of these embodiments, the method of adding the second solution to the first solution for mixing comprises:
a stirring method; and/or, ultrasonic methods; and/or, a vortex oscillation method.
In some of these embodiments, the method of agitating comprises:
the stirring time is more than 1s, and the stirring speed is 40-10000 r/min.
In some of the embodiments, the second solution is added to the first solution at a dropping speed of 0.1 to 10000 ml/min.
In some of these embodiments, the temperature at which the second solution is added to the first solution is 0 to 60 ℃.
In some of these embodiments, the temperature at which the second solution is added to the first solution is 0 to 50 ℃.
In a second aspect, the present invention provides a mineralized glycerol gel, prepared by the preparation method of the first aspect, comprising minerals and glycerol;
wherein the mineralized glycerol gel is in a gel state within 50 ℃;
the viscosity of the mineralized glycerin gel is more than or equal to 2500mPa & s.
In some embodiments, the mineral is 0.1-5% by weight.
In some embodiments, the water further comprises water, and the water accounts for 20% or less by mass.
In some embodiments, the mineral is one or more of calcium phosphate, calcium carbonate, calcium sulfate, magnesium phosphate, magnesium carbonate, and magnesium sulfate.
In a third aspect, the present invention provides the use of a mineralised glycerol according to the second aspect for repairing teeth.
Compared with the related technology, the mineralized glycerol gel, the preparation method and the application provided by the embodiment of the application can be used for preparing the mineralized glycerol gel by directly mixing the glycerol solution containing the cation source and the glycerol solution containing the anion source, the preparation method is simple, no additional additive is needed, the types and the using amount of raw materials are reduced, and the production cost is greatly reduced; the prepared mineralized glycerin gel contains glycerin and mineral substances, is in a gel state below 50 ℃, is convenient to store, transport and use, and reduces the use cost; the mineralized glycerin gel can remineralize the tooth surface, repair enamel, and prevent the tooth decay from developing again.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
FIG. 1A is a schematic representation of a mineralized glycerogel containing calcium phosphate according to the present invention;
FIG. 1B is a schematic of a pure glycerol solvent;
FIG. 2A is a schematic representation of a mineralized glycerogel containing calcium phosphate according to the present invention; (ii) a
FIG. 2B is a schematic representation of a mineralized glycerol gel containing calcium carbonate according to the present invention;
FIG. 2C is a schematic representation of a mineralized glycerol gel containing magnesium carbonate according to the present invention;
FIG. 2D is a schematic representation of a mineralized glycerol gel containing calcium sulfate in accordance with the present invention;
FIG. 2E is a schematic representation of a mineralized glycerol gel containing magnesium sulfate in accordance with the present invention;
FIG. 3 is a transmission electron micrograph of a mineralized glycerol gel according to the invention;
FIG. 4A is a scanning electron micrograph of a decayed tooth surface;
FIG. 4B is a scanning electron micrograph of an eroded tooth surface coated with a mineralized glycerol gel according to the invention for 1 h;
FIG. 4C is a scanning electron micrograph of an eroded tooth surface coated with a mineralized glycerol gel according to the invention for 24 h;
FIG. 4D is a scanning electron micrograph of an eroded tooth surface coated with calcium phosphate tribasic for 24 h;
FIG. 5A is a scanning electron micrograph of a tooth surface exposing dentinal tubules;
fig. 5B is a scanning electron micrograph of the tooth surface of exposed dentinal tubules coated with a mineralized glycerogel of the present invention for 24 h.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the present application will be described and illustrated below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present application and are not intended to limit the present application. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments provided in the present application without any inventive step are within the scope of protection of the present application.
It is obvious that the drawings in the following description are only examples or embodiments of the present application, and that it is also possible for a person skilled in the art to apply the present application to other similar contexts on the basis of these drawings without inventive effort. Moreover, it should be appreciated that in the development of any such actual implementation, as in any engineering or design project, numerous implementation-specific decisions must be made to achieve the developers' specific goals, such as compliance with system-related and business-related constraints, which may vary from one implementation to another.
Reference in the specification to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the specification. The appearances of the phrase in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. Those of ordinary skill in the art will explicitly and implicitly appreciate that the embodiments described herein may be combined with other embodiments without conflict.
Unless defined otherwise, technical or scientific terms referred to herein shall have the ordinary meaning as understood by those of ordinary skill in the art to which this application belongs. Reference to "a," "an," "the," and similar words throughout this application are not to be construed as limiting in number, and may refer to the singular or the plural. The present application is directed to the use of the terms "including," "comprising," "having," and any variations thereof, which are intended to cover non-exclusive inclusions; for example, a process, method, system, article, or apparatus that comprises a list of steps or modules (elements) is not limited to the listed steps or elements, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus. Reference to "connected," "coupled," and the like in this application is not intended to be limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. The term "plurality" as referred to herein means two or more. "and/or" describes an association relationship of associated objects, meaning that three relationships may exist, for example, "A and/or B" may mean: a exists alone, A and B exist simultaneously, and B exists alone. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship. Reference herein to the terms "first," "second," "third," and the like, are merely to distinguish similar objects and do not denote a particular ordering for the objects.
Example 1
This example is an illustrative embodiment of the present invention, and relates to mineralized glycerol gels, methods of preparation, and uses thereof.
A method of preparing a mineralized glycerol gel comprising:
step S102, dissolving a cation source in a glycerol solution to obtain a first solution;
step S104, dissolving an anion source in a glycerol solution to obtain a second solution;
and S106, adding the second solution into the first solution, and mixing to form mineralized glycerin gel.
Wherein the mineralized glycerin gel is in a gel state within 50 ℃;
wherein the cation source is water-soluble mineral salt, and the anion source is water-soluble inorganic acid and/or water-soluble inorganic acid salt;
wherein, in the mixed solution, the concentration of the cation source is 0.01-10 mol/L, the concentration of the anion source is 0.01-10 mol/L, and the molar ratio of the cation source to the anion source is 0.1-5: 1.
preferably, the mineralized glycerol gel is in the form of a gel at temperatures up to 45 ℃; preferably, the mineralized glycerol gel is in the form of a gel at temperatures up to 40 ℃; the mineralized glycerin gel is in a gel state within 38 ℃; the mineralized glycerin gel is in a gel state within 4-38 ℃.
In some of these embodiments, the mineralized glycerol gel has a viscosity of 2500mPa · s or greater.
In some of these embodiments, the cation source is one or a combination of calcium and magnesium ions.
In some embodiments, the cation source is one or more of a water-soluble calcium salt, a water-soluble magnesium salt.
In some of these embodiments, the cation source is one or a combination of calcium chloride, calcium nitrate, calcium acetate, magnesium chloride, magnesium nitrate, and magnesium acetate.
In some of these embodiments, the anion source is one or a combination of phosphate, sulfate, and carbonate ions.
In some of these embodiments, the source of anions is one or a combination of water soluble phosphates, water soluble sulfates, water soluble carbonates.
In some of these embodiments, the source of anions is a water soluble sodium salt comprising phosphate, a water soluble potassium salt comprising phosphate, a water soluble ammonium salt comprising phosphate, a water soluble sodium salt comprising sulfate, a water soluble potassium salt comprising sulfate, a water soluble ammonium salt comprising sulfate, a water soluble sodium salt comprising carbonate, a water soluble potassium salt comprising carbonate, a water soluble ammonium salt comprising carbonate.
In some of these embodiments, the source of anions is one or a combination of phosphoric acid, sodium phosphate, sodium monohydrogen phosphate, sodium dihydrogen phosphate, potassium monohydrogen phosphate, potassium dihydrogen phosphate, ammonium monohydrogen phosphate, ammonium dihydrogen phosphate, sodium sulfate, sodium hydrogen sulfate, potassium hydrogen sulfate, ammonium hydrogen sulfate, sodium carbonate, sodium hydrogen carbonate, potassium hydrogen carbonate, ammonium hydrogen carbonate.
In some of these embodiments, the glycerol solution is a pure glycerol solution or a glycerol solution containing water;
wherein, in the glycerol solution containing water, the mass percent of the water is less than 50 percent.
In some of these embodiments, the method of adding the second solution to the first solution for mixing comprises:
a stirring method; and/or, ultrasonic methods; and/or, a vortex oscillation method.
In some of these embodiments, the method of agitating comprises:
the stirring time is more than 1s, and the stirring speed is 40-10000 r/min.
In some of the embodiments, the second solution is added to the first solution at a dropping rate of 0.1 to 10000 ml/min.
In some of these embodiments, the second solution is added to the first solution at a temperature of 0 to 60 ℃. Preferably, the temperature for adding the second solution into the first solution and mixing is 0-50 ℃.
Preferably, the concentration of the cation source in the mixed solution is 0.1-8 mol/L; preferably, the concentration of the cation source in the mixed solution is 0.2-6 mol/L; preferably, the concentration of the cation source in the mixed solution is 0.5-4 mol/L; preferably, the concentration of the cation source in the mixed solution is 0.5-2 mol/L.
Preferably, the concentration of the anion source in the mixed solution is 0.1-8 mol/L; preferably, the concentration of the anion source in the mixed solution is 0.2-6 mol/L; preferably, the concentration of the anion source in the mixed solution is 0.5-4 mol/L; preferably, the concentration of the anion source in the mixed solution is 0.5-2 mol/L.
Preferably, the molar ratio of the cation source to the anion source is 0.2-4: 1; more preferably, the molar ratio of the cation source to the anion source is 0.2 to 3: 1; more preferably, the molar ratio of the cation source to the anion source is 0.3-2: 1; most preferably, the molar ratio of the cation source to the anion source is 0.5-2: 1.
in some of these embodiments, the method of adding the second solution to the first solution for mixing comprises:
a stirring method; and/or, ultrasonic methods; and/or, a vortex oscillation method; and/or, a resting method.
In some of these embodiments, the method of agitating comprises:
the stirring time is more than 1s, and the stirring speed is 40-10000 r/min.
In some of the embodiments, the second solution is added to the first solution at a dropping rate of 0.1 to 10000 ml/min.
Further, the preparation method also comprises the following steps:
and step S108, under the condition that the mixed solution does not form a gel state, removing impurities in the mixed solution to obtain mineralized glycerin gel.
In step S108, the removed impurities are non-mineral water-soluble inorganic salts after the cation source and the anion source are reacted.
In addition, impurities may also include sources of unreacted cations and anions.
In some embodiments, the method of removing impurities of the mixed solution includes:
a high speed centrifugation method; and/or, chromatographic methods; and/or, a dialysis method.
Wherein in the high-speed centrifugation method, the centrifugation rotating speed is 5000-20000 rpm.
Wherein, the chromatography method includes but is not limited to gel chromatography, thin layer chromatography, ion exchange chromatography, adsorption chromatography and partition chromatography.
In this embodiment, in step S106, the mixed solution may be used as it is (i.e., without removing the impurities), or may be used after removing the impurities. The reason for this is that the unreacted cation source, anion source and soluble inorganic salt produced by the reaction are non-toxic water-soluble substances, and in actual use, these substances are dissolved by the aqueous solution and flow along with the flow of the aqueous solution, and do not cause deposition, adsorption and other effects.
The prepared mineralized glycerin gel comprises mineral substances and glycerin, wherein the mineral substances account for 0.1-5% by mass.
The mineralized glycerin gel may be contaminated or may be free of contaminants.
Preferably, the mineralized glycerol gel is a mineralized glycerol gel free of impurities.
As shown in fig. 1A to 1B and fig. 2A to 2E, the mineralized glycerin gel prepared by the present invention is in a gel state at 50 ℃ or lower and has a viscosity of 2500mPa · s or higher, compared to the glycerin solvent, and the mineralized glycerin gel does not shift when the container storing the mineralized glycerin gel is turned over.
According to the preparation method, the mineralized glycerin gel comprises minerals and glycerin. As shown in FIG. 3, the minerals are extremely small sized particles (average particle size less than 10 nm).
In some of these embodiments, the mineralized glycerol gel further comprises water, wherein the water is present in an amount of 20% by weight or less.
Preferably, the mass percent of water is less than or equal to 15%; preferably, the mass percent of water is less than or equal to 10%; preferably, the mass percent of water is less than or equal to 5%; preferably, the mass percent of the water is 0.2-2%.
As for the above-mentioned mineralized glycerin gel, it can be applied to repair tooth hard tissue.
Specifically, the mineralized glycerin gel may be used as a single component, or may be used in combination with other components.
As shown in fig. 4A-4D, the mineralized glycerin gel prepared according to the present invention was applied to the tooth surface damaged by erosion and enamel. Compared with fig. 4A, a good restoration result can be obtained in a short time (fig. 4B), and the restoration result can penetrate into gaps and ravines generated on the surface of the corroded tooth and form a hydroxyapatite nano-rod mineralized layer; the coated tooth surface was more smooth and the restoration effect was more effective over a long period of time (fig. 4C). In contrast, after ordinary calcium phosphate treatment of eroded enamel, there were still significant gaps and gullies, which did not effectively repair eroded enamel (fig. 4D).
As shown in fig. 5A-5B, the mineralized glycerin gel prepared according to the present invention was applied to the tooth surface exposed to dentinal tubules due to erosion. Compared with fig. 5A, a dense mineralized layer can be generated in a short time (fig. 5B), covering the dentinal tubules, and thus a good repairing effect is obtained.
The method has the advantages that the mineralized glycerin gel can be prepared by directly mixing the glycerin solution containing the cation source and the glycerin solution containing the anion source, the preparation method is simple, no additional additive is needed, the types and the using amount of raw materials are reduced, and the production cost is greatly reduced; the prepared mineralized glycerin gel is in a gel state at the temperature of below 50 ℃, is convenient to store, transport and use, and reduces the use cost; the mineralized glycerin gel is filled in gaps of tooth interfaces, so that the decayed tooth is prevented from developing again; the mineralized glycerin gel contains minerals and can remineralize the tooth surface.
Example 2
This embodiment is a specific embodiment of the present invention.
Preparing 50mL of 0.04mol/L sodium phosphate dodecahydrate glycerol solution as a first solution;
preparing 10mL of 0.3mol/L calcium chloride dihydrate glycerol solution as a second solution;
and uniformly mixing the second solution and the first solution, and standing for 24 hours at 37 ℃ to obtain the mineralized glycerin gel.
Below 50 ℃, the mineralized glycerin gel is gelatinous, white and has no obvious fluidity.
In the mineralized glycerin gel, the mass percentages of the mineral substance, the water and the glycerin are respectively 0.4%, 0.7% and 98.9%.
The mineralized glycerol gel had a viscosity of 14000 mPas.
Example 3
This embodiment is a specific embodiment of the present invention.
Preparing 50mL of 0.08mol/L sodium phosphate dodecahydrate glycerol solution as a first solution;
preparing 10mL of 0.6mol/L calcium chloride dihydrate glycerol solution as a second solution;
and uniformly mixing the second solution and the first solution, and standing for 24 hours at 37 ℃ to obtain the mineralized glycerin gel.
Below 50 ℃, the mineralized glycerin gel is gelatinous, white and has no obvious fluidity.
In the mineralized glycerin gel, the mass percentages of the mineral substance, the water and the glycerin are respectively 0.8%, 1.4% and 97.8%.
The viscosity of the mineralized glycerol gel was 44000 mPas.
Example 4
This embodiment is a specific embodiment of the present invention.
Preparing 50mL of 0.08mol/L sodium phosphate dodecahydrate glycerol solution as a first solution;
preparing 10mL of 0.6mol/L magnesium chloride hexahydrate glycerol solution as a second solution;
and uniformly mixing the second solution and the first solution, and standing for 24 hours at 37 ℃ to obtain the mineralized glycerin gel.
Below 50 ℃, the mineralized glycerin gel is gelatinous, white and has no obvious fluidity.
In the mineralized glycerin gel, the mass percentages of the mineral substance, the water and the glycerin are respectively 0.6%, 2.0% and 97.4%.
The mineralized glycerol gel had a viscosity of 13000 mPas.
Example 5
This embodiment is a specific embodiment of the present invention.
Preparing 50mL of 0.04mol/L sodium phosphate dodecahydrate glycerol solution as a first solution;
preparing 10mL of 0.3mol/L magnesium chloride hexahydrate glycerol solution as a second solution;
and uniformly mixing the second solution and the first solution, and standing for 24 hours at 37 ℃ to obtain the mineralized glycerin gel.
Below 50 ℃, the mineralized glycerin gel is gelatinous, white and has no obvious fluidity.
In the mineralized glycerin gel, the mass percentages of the mineral substance, the water and the glycerin are respectively 0.3%, 1.0% and 98.7%.
The mineralized glycerol gel had a viscosity of 6600 mPas.
Example 6
This embodiment is a specific embodiment of the present invention.
Preparing 50mL of 0.08mol/L glycerol solution of sodium sulfate decahydrate as a first solution;
preparing 10mL of 0.4mol/L calcium chloride dihydrate glycerol solution as a second solution;
and uniformly mixing the second solution and the first solution, and standing for 24 hours at 37 ℃ to obtain the mineralized glycerin gel.
Below 50 ℃, the mineralized glycerin gel is gelatinous, white and has no obvious fluidity.
In the mineralized glycerin gel, the mass percentages of the mineral substance, the water and the glycerin are respectively 0.5%, 0.2% and 97.3%.
The mineralized glycerol gel had a viscosity of 25000 mPas.
Example 7
This embodiment is a specific embodiment of the present invention.
Preparing 50mL of 0.08mol/L glycerol solution of sodium sulfate decahydrate as a first solution;
preparing 10mL of 0.6mol/L calcium chloride dihydrate glycerol solution as a second solution;
and uniformly mixing the second solution and the first solution, and standing for 24 hours at 37 ℃ to obtain the mineralized glycerin gel.
Below 50 ℃, the mineralized glycerin gel is gelatinous, white and has no obvious fluidity.
In the mineralized glycerin gel, the mass percentages of the mineral substance, the water and the glycerin are respectively 0.7%, 1.1% and 98.2%.
The mineralized glycerol gel had a viscosity of 24000 mPas.
Example 8
This embodiment is a specific embodiment of the present invention.
Preparing 50mL of 0.08mol/L sodium carbonate glycerol solution as a first solution;
preparing 10mL of 0.6mol/L magnesium chloride glycerol solution as a second solution;
and uniformly mixing the second solution and the first solution, and standing for 24 hours at 37 ℃ to obtain the mineralized glycerin gel.
Below 50 ℃, the mineralized glycerin gel is gelatinous, white and has no obvious fluidity.
In the mineralized glycerin gel, the mass percentages of the mineral substance, the water and the glycerin are respectively 0.4%, 0.6% and 99%.
The viscosity of the mineralized glycerol gel was 32000 mPas.
Example 9
This embodiment is a specific embodiment of the present invention.
Preparing 50mL of 0.08mol/L sodium sulfate glycerol solution as a first solution;
preparing 10mL of 0.6mol/L magnesium chloride glycerol solution as a second solution;
and uniformly mixing the second solution and the first solution, and standing for 24 hours at 37 ℃ to obtain the mineralized glycerin gel.
Below 50 ℃, the mineralized glycerin gel is gelatinous, white and has no obvious fluidity.
In the mineralized glycerin gel, the mass percentages of the mineral substance, the water and the glycerin are respectively 0.6%, 1.4% and 98%.
The mineralized glycerol gel had a viscosity of 22000 mPas.
Example 10
This embodiment is a specific embodiment of the present invention.
50mL of a 0.1mol/L glycerol solution of potassium phosphate was prepared as a first solution;
preparing 10mL of 0.6mol/L calcium acetate glycerol solution as a second solution;
and uniformly mixing the second solution and the first solution, and standing for 24 hours at 37 ℃ to obtain the mineralized glycerin gel.
Below 50 ℃, the mineralized glycerin gel is gelatinous, white and has no obvious fluidity.
In the mineralized glycerin gel, the mass percentages of the mineral substance, the water and the glycerin are respectively 0.9%, 0.5% and 98.4%.
The mineralized glycerol gel had a viscosity of 14500 mPas.
Example 11
This embodiment is a specific embodiment of the present invention.
Preparing 50mL of 0.08mol/L glycerol solution of potassium sulfate as a first solution;
preparing 10mL of 0.6mol/L glycerin solution of calcium nitrate tetrahydrate as a second solution;
and uniformly mixing the second solution and the first solution, and standing for 24 hours at 37 ℃ to obtain the mineralized glycerin gel.
Below 50 ℃, the mineralized glycerin gel is gelatinous, white and has no obvious fluidity.
In the mineralized glycerin gel, the mass percentages of the mineral substance, the water and the glycerin are respectively 0.6%, 0.8% and 98.6%.
Example 12
This embodiment is a specific embodiment of the present invention.
Preparing 50mL of 0.1mol/L potassium carbonate glycerol solution as a first solution;
preparing 10mL of 0.4mol/L glycerin solution of magnesium nitrate hexahydrate as a second solution;
and uniformly mixing the second solution and the first solution, and standing for 24 hours at 37 ℃ to obtain the mineralized glycerin gel.
Below 50 ℃, the mineralized glycerin gel is gelatinous, white and has no obvious fluidity.
In the mineralized glycerin gel, the mass percentages of the mineral substance, the water and the glycerin are respectively 0.5%, 0.8% and 98.3%.
Example 13
This embodiment is a specific embodiment of the present invention.
Preparing 50mL of 0.1mol/L ammonium phosphate glycerol solution as a first solution;
preparing 10mL of 0.5mol/L glycerol solution of magnesium acetate tetrahydrate as a second solution;
and uniformly mixing the second solution and the first solution, and standing for 24 hours at 37 ℃ to obtain the mineralized glycerin gel.
Below 50 ℃, the mineralized glycerin gel is gelatinous, white and has no obvious fluidity.
In the mineralized glycerin gel, the mass percentages of the mineral substance, the water and the glycerin are respectively 0.5%, 1.0% and 98.5%.
Example 14
This embodiment is a specific embodiment of the present invention.
Preparing 50mL of 0.12mol/L ammonium sulfate glycerol solution as a first solution;
preparing 10mL of 0.7mol/L calcium acetate monohydrate glycerol solution as a second solution;
and uniformly mixing the second solution and the first solution, and standing for 24 hours at 37 ℃ to obtain the mineralized glycerin gel.
Below 50 ℃, the mineralized glycerin gel is gelatinous, white and has no obvious fluidity.
In the mineralized glycerin gel, the mass percentages of the mineral substance, the water and the glycerin are respectively 1.0%, 0.6% and 98.4%.
Example 15
This embodiment is a specific embodiment of the present invention.
Preparing 50mL of 0.12mol/L ammonium carbonate glycerol solution as a first solution;
preparing 10mL of 0.9mol/L magnesium acetate glycerol solution as a second solution;
and uniformly mixing the second solution and the first solution, and standing for 24 hours at 37 ℃ to obtain the mineralized glycerin gel.
Below 50 ℃, the mineralized glycerin gel is gelatinous, white and has no obvious fluidity.
In the mineralized glycerin gel, the mass percentages of the mineral substance, the water and the glycerin are respectively 1.6%, 0.5% and 97.9%.
Example 16
This embodiment is a specific embodiment of the present invention.
Preparing 50mL of 0.1mol/L glycerol solution of sodium monohydrogen phosphate dodecahydrate as a first solution;
preparing 10mL of 0.6mol/L magnesium chloride hexahydrate glycerol solution as a second solution;
and uniformly mixing the second solution and the first solution, and standing for 24 hours at 37 ℃ to obtain the mineralized glycerin gel.
Below 50 ℃, the mineralized glycerin gel is gelatinous, white and has no obvious fluidity.
In the mineralized glycerin gel, the mass percentages of the mineral substance, the water and the glycerin are respectively 0.8%, 0.6% and 97.4%.
Example 17
This embodiment is a specific embodiment of the present invention.
Preparing 50mL of 0.15mol/L potassium bisulfate glycerol solution as a first solution;
preparing 10mL of 0.5mol/L calcium acetate glycerol solution as a second solution;
and uniformly mixing the second solution and the first solution, and standing for 24 hours at 37 ℃ to obtain the mineralized glycerin gel.
Below 50 ℃, the mineralized glycerin gel is gelatinous, white and has no obvious fluidity.
In the mineralized glycerin gel, the mass percentages of the mineral substance, the water and the glycerin are respectively 0.7%, 0.8% and 98.5%.
Example 18
This embodiment is a specific embodiment of the present invention.
Preparing 50mL of 0.12mol/L ammonium bicarbonate glycerol solution as a first solution;
preparing 10mL of 0.6mol/L calcium chloride glycerol solution as a second solution;
and uniformly mixing the second solution and the first solution, and standing for 24 hours at 37 ℃ to obtain the mineralized glycerin gel.
Below 50 ℃, the mineralized glycerin gel is gelatinous, white and has no obvious fluidity.
In the mineralized glycerin gel, the mass percentages of the mineral substance, the water and the glycerin are respectively 1%, 0.8% and 98.2%.
Example 19
This embodiment is a specific embodiment of the present invention.
50mL of 0.12mol/L potassium bisulfate glycerol solution was prepared as a first solution;
preparing 10mL of 0.8mol/L magnesium chloride glycerol solution as a second solution;
and uniformly mixing the second solution and the first solution, and standing for 24 hours at 37 ℃ to obtain the mineralized glycerin gel.
Below 50 ℃, the mineralized glycerin gel is gelatinous, white and has no obvious fluidity.
In the mineralized glycerin gel, the mass percentages of the mineral substance, the water and the glycerin are respectively 1.2%, 0.6% and 98.2%.
Example 20
This example is a control experiment of the restorative material of the present invention and related art in restoring hard tissue of teeth.
A piece of enamel of 5X 3mm from the center of the labial and buccal surfaces of the dental crown was cut out by a diamond cutter. Exposing an enamel interface after resin embedding, gradually polishing by using 800-2000 # abrasive paper, cleaning by using ethanol, and drying. Then etching with 37% phosphoric acid for 60s, washing with deionized water and drying in air for standby.
Respectively coating the mineralized glycerin gel prepared in the example 2 and the repair material in the related technology on an enamel interface subjected to acid etching, and soaking an enamel sample to be repaired in simulated saliva; placing the sample soaked with the simulated saliva in a constant-temperature oven at 37 ℃ for 24 hours and then taking out; and (5) flushing under running water for 1 minute, removing impurities on the enamel interface repairing layer and then airing.
As shown in fig. 4A to 4D, compared with the initial interface after enamel acid etching, the enamel surface coated with the present invention can form a relatively dense hydroxyapatite nanorod mineralized layer within about 1h, and the repair layer is more smooth and dense after 24 h. In contrast, ordinary calcium phosphate was not effective in repairing eroded enamel (fig. 4D).
Example 21
This example is a control experiment of the restorative material of the present invention and related art in restoring hard tissue of teeth.
And cutting a dentin sheet 1mm above a pulp chamber at the crown part of the tooth by using a diamond cutting machine, soaking the dentin sheet in a 10% ethylene diamine tetraacetic acid solution for 5 minutes, performing ultrasonic treatment for 10 minutes, and washing the dentin sheet by using deionized water to obtain a dentin sample with exposed tubules.
Respectively coating the mineralized glycerin gel prepared in the example 2 and the repair material in the related technology on an enamel interface subjected to acid etching, and soaking an enamel sample to be repaired in simulated saliva; placing the sample soaked with the simulated saliva in a constant-temperature oven at 37 ℃ for 24 hours and then taking out; and (5) flushing under running water for 1 minute, removing impurities on the enamel interface repairing layer and then airing.
As shown in fig. 5A-5B, the samples before treatment clearly exposed the dentinal tubules (fig. 5A); however, the sample surface treated with the prepared mineralized glycerogel produced a dense mineralized layer covering the dentinal tubules in a short time (fig. 5B), resulting in good restoration results.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present application, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the concept of the present application, which falls within the scope of protection of the present application. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A method of preparing a mineralized glycerol gel, comprising:
dissolving a cation source in a glycerol solution to obtain a first solution;
dissolving an anion source in a glycerol solution to obtain a second solution;
adding the second solution into the first solution for mixing to form mineralized glycerin gel;
wherein the mineralized glycerol gel is in a gel state at a temperature below 50 ℃;
wherein the cation source is water-soluble mineral salt, and the anion source is water-soluble inorganic acid and/or water-soluble inorganic acid salt;
wherein, in the mixed solution, the concentration of the cation source is 0.01-10 mol/L, the concentration of the anion source is 0.01-10 mol/L, and the molar ratio of the cation source to the anion source is 0.1-5: 1.
2. the method according to claim 1, wherein the mineralized glycerol gel has a viscosity of 2500 mPa-s or more.
3. The preparation method according to claim 1 or 2, wherein the cation source is one or more of calcium ion and magnesium ion.
4. The preparation method according to any one of claims 1 to 3, wherein the anion source is one or a combination of phosphate ions, sulfate ions and carbonate ions.
5. The production method according to any one of claims 1 to 4, wherein the glycerin solution is a pure glycerin solution or a glycerin solution containing water;
wherein, in the glycerol solution containing water, the mass percent of the water is less than 50 percent.
6. A mineralized glycerol gel prepared by the preparation method of the mineralized glycerol gel according to any one of claims 1 to 5, and is characterized by comprising minerals and glycerol;
wherein the mineralized glycerol gel is in a gel state within 50 ℃;
the viscosity of the mineralized glycerin gel is more than or equal to 2500mPa & s.
7. The mineralized glycerol gel according to claim 6, wherein the mineral is present in an amount of 0.1 to 5% by weight.
8. The mineralized glycerol gel according to claim 6 or 7, further comprising water in an amount of 20% or less by mass.
9. The mineralized glycerol gel according to any one of claims 6 to 8, wherein the minerals are one or more of calcium phosphate, calcium carbonate, calcium sulfate, magnesium phosphate, magnesium carbonate, and magnesium sulfate.
10. Use of a mineralized glycerol gel according to any one of claims 6 to 9 for the restoration of teeth.
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| WO2023185212A1 (en) * | 2022-03-29 | 2023-10-05 | 上海市第十人民医院 | Mineralized collagen material, preparation method therefor, and application thereof |
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