CN115024988B - Preparation and application of antibacterial enamel remineralizing liquid - Google Patents
Preparation and application of antibacterial enamel remineralizing liquid Download PDFInfo
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Abstract
The invention discloses preparation and application of an antibacterial enamel remineralizing solution, and particularly relates to the field of oral care. An antibacterial enamel remineralizing solution includes a water-in-oil-in-water emulsion containing a soluble calcium, zinc and silver mixed salt; a water-in-oil-in-water emulsion containing a soluble phosphate salt; water-in-oil-in-water emulsions containing a soluble base. According to the invention, zinc and silver are loaded on the surface of the dental enamel in a loading mode, so that the dental enamel has antibacterial and anti-inflammatory effects, and meanwhile, the washing-off water-in-oil-in-water emulsion avoids renal metabolic toxicity caused by oral administration of zinc oxide and silver oxide, so that the oral administration is safe and reliable.
Description
Technical Field
The invention belongs to the technical field of daily chemical, hard tissue medical treatment, nursing and cleaning products, in particular to medical treatment and oral cleaning nursing products, and more particularly relates to preparation and application of antibacterial enamel remineralizing liquid.
Background
The human enamel is rich in 96% of inorganic hydroxyapatite, and researches show that enamel columns in the enamel are in a core-shell structure, organic liposome and other inorganic elements are mainly concentrated in the inner cores of the enamel columns, and the shell structure of the enamel columns is mainly made of the inorganic hydroxyapatite.
Hydroxyapatite (HAP) is a sparingly soluble substance, so that dental bodies present a dissolution remineralization process in oral saliva, and methods for achieving enamel remineralization by providing calcium, phosphorus ions have been demonstrated.
The tooth enamel is easily demineralized through acidic substances generated by diet and bacteria, so that white spots are formed, and finally the tooth enamel evolves into decayed teeth; damaged enamel can be repaired to a certain extent by adding calcium and phosphorus ions. However, the remineralization process of enamel is limited due to the bacteria on the enamel surface and the bacterial film formed thereby, the bacteria continue to grow and continuously produce acid, resulting in a final enamel demineralization rate far exceeding the remineralization rate and tooth erosion. Therefore, effectively inhibiting the bacteria from growing on the enamel surface and loading the anti-acid substance on the tooth body are ideal strategies for effectively solving the problem of enamel acid etching and ore removal.
The antibacterial and antiviral properties of zinc ions and silver ions and the safety performance thereof in use in human bodies have been widely confirmed, and particularly zinc oxide, zinc chloride, zinc lactate and other compounds rich in zinc elements have been commonly used in toothpastes, however, bacteria continuously grow in the oral cavity, the tooth brushing time is very limited (usually 3 minutes), silver ions and zinc ions can be directly added into the toothpastes to kill part of the bacteria in the process of using the toothpastes, but acid-producing bacteria still exist continuously and damage the teeth in a period of time after tooth brushing; therefore, zinc oxide and silver ions with antibacterial property are directly loaded on tooth enamel, and continuous inhibition of bacteria breeding on teeth is an ideal strategy for effectively solving the problem of enamel acid etching and demineralization.
Disclosure of Invention
Therefore, the invention provides preparation and application of an antibacterial enamel remineralization liquid, which are used for solving the problem that the existing oral care products have poor effects on enamel remineralization, antibacterial and antiviral effects.
The invention aims to prepare water-in-oil-in-water emulsion with internal water phases of free calcium ions, phosphate ions, zinc ions and silver ions respectively, mix the three emulsions according to different proportions, demulsify the tooth enamel surface by using a toothbrush, and deposit zinc and silver elements on the tooth enamel in the remineralization process of the tooth enamel to play a role.
In order to achieve the above object, the present invention provides the following technical solutions:
according to a first aspect of the present invention there is provided an antibacterial enamel remineralisation liquid comprising:
water-in-oil-in-water emulsions containing soluble calcium, zinc and silver salts simultaneously;
a water-in-oil-in-water emulsion containing a soluble phosphate salt;
water-in-oil-in-water emulsions containing a soluble base.
Wherein the soluble calcium, zinc and silver mixed salt is a mixed solution of soluble calcium salt, soluble silver salt and soluble zinc salt.
The invention adopts the compartmentalized calcium, zinc and silver mixed metal ions, phosphate ions and hydroxide ions as raw materials to avoid direct contact reaction among the ions before application, and in the application process, the calcium, zinc and silver mixed metal ions, the phosphate ions and the hydroxide ions are demulsified and released on the surface of enamel, and calcium phosphate ions are instantly provided by taking a tooth body as a seed crystal to form a supersaturated solution of calcium phosphate so as to promote remineralization of enamel, and meanwhile, zinc and silver ions react with OH-in the remineralization process to form enamel/zinc oxide and enamel/silver oxide mixed materials.
Further, the preparation method of the water-in-oil-in-water emulsion containing soluble calcium, salt and silver mixed salt/soluble phosphate/soluble alkali comprises the following steps:
mixing an aqueous solution containing soluble calcium, zinc and silver mixed salt with an oil phase containing solid particles according to the volume ratio (1-3): (1-19) mixing, stirring for 0.5-120 minutes at the temperature of 30-80 ℃ and the rotation speed of 10-24000 r/min to obtain water-in-oil emulsion containing soluble calcium, zinc and silver salts; and then the water-in-oil emulsion containing the soluble calcium, zinc and silver mixed salt and the water phase containing solid particles are mixed according to the volume ratio (1-3): (1-19) mixing, stirring for 0.5-120 minutes at the temperature of 30-80 ℃ and the rotating speed of 10-24000 r/min, and obtaining the water-in-oil-in-water emulsion containing the soluble calcium, zinc and silver mixed salt.
The method for preparing the water-in-oil-in-water emulsion containing the soluble phosphate and the water-in-oil-in-water emulsion containing the soluble alkali are identical to the method for preparing the water-in-oil-in-water emulsion containing the soluble calcium, zinc and silver mixed salt, except that the soluble salt is used, and the soluble calcium, zinc and silver mixed salt used in the preparation of the water-in-oil-in-water emulsion containing the soluble calcium, zinc and silver mixed salt is correspondingly replaced by the soluble phosphate, or the soluble alkali can be prepared into the water-in-oil-in-water emulsion containing the soluble phosphate and the water-in-oil-in-water emulsion containing the soluble alkali.
Further, the concentration of each of calcium, zinc and silver ions in the aqueous solution containing the soluble calcium, zinc and silver mixed salt is 0.001-2.5mol/l;
and/or the concentration of phosphate ions in the aqueous solution containing soluble phosphate is 0.001-1.5mol/l;
and/or the concentration of hydroxide ions in the aqueous solution containing the soluble alkali is 0.001-2mol/l.
Further, the preparation method of the oil phase containing the solid particles comprises the following steps: the mass ratio of the solid particles to the grease is (0.1-25): 100, mixing at 30-80deg.C;
and/or the preparation method of the water phase containing the solid particles comprises the following steps: the mass ratio of the solid particles to water is (0.1-25): 100.
Further, the soluble calcium salt is a substance which can be dissolved in water and alcohols and can generate free calcium ions. As examples, the soluble calcium salt includes, but is not limited to, one or more of calcium chloride, calcium hydroxide, calcium oxide, calcium nitrate, calcium gluconate, calcium bicarbonate, calcium lactate, calcium citrate, calcium acetate.
Further, the soluble silver salt is a substance which can be dissolved in water and alcohols and can generate free silver ions; as an example, the soluble silver salts include, but are not limited to, one or more of nitrate, silver fluoride, silver chlorate, silver perchlorate;
further, the soluble zinc salt is a substance which can be dissolved in water and alcohols and can generate free zinc ions; as an example, the soluble silver salts include, but are not limited to, one or more of nitrate, silver fluoride, silver chlorate, silver perchlorate;
further, the soluble phosphate is a compound capable of generating free phosphate, hydrogen phosphate or dihydrogen phosphate ions. As examples, the soluble phosphate salts include, but are not limited to, one or more of potassium phosphate, sodium phosphate, ammonium phosphate, potassium phosphate monobasic, sodium phosphate monobasic, ammonium phosphate monobasic.
Further, the soluble base is a substance that is soluble in water and is capable of generating hydroxide ions in a free state. By way of example, the soluble base includes, but is not limited to, one or more of sodium hydroxide, potassium hydroxide, lithium hydroxide, calcium hydroxide.
Further, the solid particles are organic micro-nano particles and/or inorganic micro-nano particles. By way of example, the solid particles include, but are not limited to, one or more of calcium carbonate, aluminum oxide, silicon dioxide, calcium phosphate, magnesium aluminum silicate, lignocellulose, protein particles.
Further, the grease is a water agent, a gel agent, a natural grease of all plant sources, animal sources and mineral sources for preparing toothpaste, mouthwash or enamel restoration gel for oral treatment, or a synthetic grease processed by petrochemical products and natural extraction raw materials. By way of example, the grease includes, but is not limited to, one or more of triglycerides, peanut oil, canola oil, lard, tallow, shea butter, sunflower oil, walnut oil, soybean oil.
According to the preparation method of the antibacterial enamel remineralizing solution provided by the second aspect of the invention, the water-in-oil-in-water emulsion containing soluble calcium, zinc and silver salts, the water-in-oil-in-water emulsion containing soluble phosphate and the water-in-oil-in-water emulsion containing soluble alkali are mixed to obtain the antibacterial enamel remineralizing solution.
According to a third aspect of the present invention there is provided the use of an antibacterial enamel remineralisation as described above in an oral care product which is a toothpaste, mouthwash or gel.
According to a fourth aspect of the present invention there is provided an oral care implement comprising an antibacterial enamel remineralisation solution as described above.
According to a fifth aspect of the present invention there is provided a method of loading zinc silver on enamel for daily brushing with an antibacterial enamel remineralizing solution as described above or an oral care implement as described above, or for simulating daily brushing in artificial saliva.
In some preferred embodiments, efficacy is achieved by daily brushing of teeth to deposit elemental zinc silver on the enamel during remineralization of the enamel. Or the isolated enamel is embedded by epoxy resin to expose the enamel surface, and the remineralized enamel surface is loaded with zinc and silver by simulating daily tooth brushing process in artificial saliva.
It will be appreciated that in order to provide a high level of zinc and silver loading on the enamel, the oral care implement preferably contains an abrasive such as silica or calcium carbonate or dibasic calcium phosphate dihydrate.
The invention has the following advantages:
according to the invention, water phase is water-in-oil-in-water emulsion of free calcium, zinc, silver ions, phosphate ions and hydroxyl ions respectively, the water phase is mixed according to different proportions, and a toothbrush is used for demulsification on the surface of dental enamel, so that zinc and silver elements can be loaded on the surface of remineralized dental enamel in the process of remineralizing dental enamel, the hardness of teeth is enhanced, and meanwhile, nano zinc oxide and silver with antibacterial, anti-inflammatory and efficacy can be loaded on the dental enamel of a human body (living body or in vitro); thereby enhancing the antibacterial property of the tooth surface and enabling the efficacy of zinc oxide and silver oxide in organisms to be applied to human bodies.
According to the invention, zinc and silver are loaded on the surface of the dental enamel in a loading mode, so that the dental enamel has antibacterial and anti-inflammatory effects, and meanwhile, the washing-off water-in-oil-in-water emulsion avoids renal metabolic toxicity caused by oral administration of zinc oxide and silver oxide, so that the oral administration is safe and reliable.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It will be apparent to those of ordinary skill in the art that the drawings in the following description are exemplary only and that other implementations can be obtained from the extensions of the drawings provided without inventive effort.
The structures, proportions, sizes, etc. shown in the present specification are shown only for the purposes of illustration and description, and are not intended to limit the scope of the invention, which is defined by the claims, so that any structural modifications, changes in proportions, or adjustments of sizes, which do not affect the efficacy or the achievement of the present invention, should fall within the ambit of the technical disclosure.
FIG. 1 is a scanning electron microscope image of the mineralization of the surface of an enamel module provided by the invention; wherein a is non-demineralized enamel; b is demineralized enamel, c is remineralized enamel after sample 2 is brushed and d is remineralized enamel after sample 1 is brushed;
FIG. 2 is a graph showing the distribution of elements of zinc successfully loaded on the enamel surface;
FIG. 3 is a graph showing the distribution of elements of a silver element successfully loaded on the enamel surface according to the present invention;
FIG. 4 is a graph of biofilm thickness grown on non-demineralized enamel surfaces provided by the present invention;
FIG. 5 is a graph showing the thickness of biofilm growing on the surface of remineralized enamel after brushing of sample 2 provided by the present invention;
FIG. 6 is a graph of biofilm thickness grown on the surface of remineralized enamel after brushing of sample 1 provided by the present invention.
Detailed Description
Other advantages and advantages of the present invention will become apparent to those skilled in the art from the following detailed description, which, by way of illustration, is to be read in connection with certain specific embodiments, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Preparing a water-in-oil-in-water emulsion containing a soluble calcium, zinc and silver mixed salt:
1) Adding 20g of calcium carbonate into 300g of triglyceride, and uniformly stirring to prepare an oil phase for later use; 15g of calcium carbonate is added into 180g of water, heated to 40 ℃ and stirred uniformly to prepare a water phase for standby.
2) Mixing 50ml of calcium chloride aqueous solution with calcium ion concentration of 0.1mol/L, 10ml of silver nitrate aqueous solution with silver ion concentration of 0.1mol/L and 5ml of zinc chloride aqueous solution with zinc ion concentration of 0.1mol/L uniformly, adding into 200ml of oil phase, heating to 60 ℃, and stirring for 1 minute at 5000 revolutions per minute by using a high-speed dispersing machine to obtain water-in-oil emulsion containing soluble calcium, zinc and silver mixed salt;
3) 100ml of the water-in-oil emulsion was added to 200ml of the aqueous phase, heated to 40℃and stirred with a high speed disperser at 2000 rpm for 2 minutes to obtain a water-in-oil-in-water emulsion containing the soluble calcium, zinc and silver mixed salts.
Preparing a water-in-oil-in-water emulsion containing a soluble phosphate salt:
1) Adding 20 silicon dioxide into 500g peanut oil, and uniformly stirring to prepare an oil phase for later use; 20g of calcium carbonate is added into 500g of water, heated to 40 ℃ and stirred uniformly to prepare a water phase for standby.
2) Adding 100ml of dipotassium hydrogen phosphate aqueous solution with phosphate ion concentration of 0.1mol/L into 300ml of oil phase, heating to 70 ℃, and stirring for 10 minutes at 3000 rpm by using a high-speed dispersing machine to obtain water-in-oil emulsion containing soluble phosphate;
3) 100ml of the water-in-oil emulsion was added to 300ml of the aqueous phase, heated to 45℃and stirred with a high speed disperser at 2000 rpm for 2 minutes to obtain the water-in-oil-in-water emulsion containing soluble phosphate.
Preparing a water-in-oil-in-water emulsion containing a soluble base:
1) Adding 10g of calcium carbonate into 200g of triglyceride, and uniformly stirring to prepare an oil phase for later use; 15g of calcium carbonate is added into 300g of water, heated to 50 ℃ and stirred uniformly to prepare a water phase for standby.
2) 10ml of sodium hydroxide aqueous solution with hydroxide ion concentration of 0.15mol/L is added into 50ml of oil phase, heated to 40 ℃, and stirred for 4 minutes at 3000 rpm by a high-speed dispersing machine to obtain water-in-oil emulsion containing soluble alkali;
3) 50ml of the water-in-oil emulsion was added to 200ml of the aqueous phase, heated to 45℃and stirred with a high speed disperser at 1000 rpm for 3 minutes to obtain the water-in-oil-in-water emulsion containing the soluble base.
The preparation method of the antibacterial enamel remineralizing solution provided by the embodiment is as follows:
the water-in-oil-in-water emulsion containing the soluble calcium, zinc and silver mixed salt, the water-in-oil-in-water emulsion containing the soluble phosphate and the water-in-oil-in-water emulsion containing the soluble alkali are mixed according to the volume ratio of 6:3:1.
Example 2
Preparing a water-in-oil-in-water emulsion containing a soluble calcium, zinc and silver mixed salt:
1) Adding 20g of magnesium aluminum silicate into 300g of soybean oil, and uniformly stirring to prepare an oil phase for later use; 30g of magnesium aluminum silicate is added into 500g of water, heated to 60 ℃ and stirred uniformly to prepare a water phase for standby.
2) 100ml of calcium nitrate aqueous solution with the calcium ion concentration of 0.5mol/L, 20ml of silver nitrate aqueous solution with the silver ion concentration of 0.01mol/L and 50ml of zinc chloride aqueous solution with the zinc ion concentration of 0.01mol/L are added into 300ml of oil phase after being uniformly mixed, heated to 50 ℃, and stirred for 3 minutes at 3000 revolutions per minute by a high-speed dispersing machine to obtain water-in-oil emulsion containing soluble calcium salt;
3) 100ml of the water-in-oil emulsion was added to 300ml of the aqueous phase, heated to 60℃and stirred with a high speed disperser at 1000 rpm for 5 minutes to obtain a water-in-oil-in-water emulsion containing the soluble calcium salt.
Preparing a water-in-oil-in-water emulsion containing a soluble phosphate salt:
1) Adding 10g of silicon dioxide into 200g of peanut oil, and uniformly stirring to prepare an oil phase for later use; 20g of calcium carbonate is added into 300g of water, heated to 55 ℃ and stirred uniformly to prepare a water phase for standby.
2) Adding 100ml of dipotassium hydrogen phosphate aqueous solution with phosphate ion concentration of 0.3mol/L into 200ml of oil phase, heating to 50 ℃, and stirring for 2 minutes at 2000 revolutions per minute by using a high-speed dispersing machine to obtain water-in-oil emulsion containing soluble phosphate;
3) 100ml of the water-in-oil emulsion was added to 300ml of the aqueous phase, heated to 45℃and stirred with a high speed disperser at 3000 rpm for 3 minutes to obtain the water-in-oil-in-water emulsion containing soluble phosphate.
Preparing a water-in-oil-in-water emulsion containing a soluble base:
1) Adding 20g of calcium carbonate into 200g of triglyceride, and uniformly stirring to prepare an oil phase for later use; 15g of calcium carbonate is added into 300g of water, heated to 45 ℃ and stirred uniformly to prepare a water phase for standby.
2) Adding 10ml of potassium hydroxide aqueous solution with hydroxide ion concentration of 0.01mol/L into 30ml of oil phase, heating to 40 ℃, and stirring for 3 minutes at 3000 rpm by using a high-speed dispersing machine to obtain water-in-oil emulsion containing soluble alkali;
3) 20ml of the water-in-oil emulsion was added to 80ml of the aqueous phase, heated to 50℃and stirred with a high speed disperser at 1000 rpm for 5 minutes to obtain the water-in-oil-in-water emulsion containing the soluble base.
The preparation method of the antibacterial enamel remineralizing solution provided by the embodiment is as follows:
the water-in-oil-in-water emulsion containing the soluble calcium salt, the water-in-oil-in-water emulsion containing the soluble phosphate and the water-in-oil-in-water emulsion containing the soluble alkali are mixed according to the volume ratio of 8:5:2.
Example 3
Preparing a water-in-oil-in-water emulsion containing a soluble calcium, zinc and silver mixed salt:
1) Adding 30g of calcium carbonate into 300g of triglyceride, and uniformly stirring to prepare an oil phase for later use; 20g of calcium carbonate is added into 500g of water, heated to 65 ℃ and stirred uniformly to prepare a water phase for standby.
2) 100ml of calcium nitrate aqueous solution with the calcium ion concentration of 0.01mol/L, 10ml of silver nitrate aqueous solution with the silver ion concentration of 0.01mol/L and 20ml of zinc nitrate aqueous solution with the zinc ion concentration of 0.01mol/L are added into 300ml of oil phase after being uniformly mixed, heated to 50 ℃, and stirred for 3 minutes at 3000 revolutions per minute by a high-speed dispersing machine to obtain water-in-oil emulsion containing soluble calcium salt;
3) 100ml of the water-in-oil emulsion was added to 400ml of the aqueous phase, heated to 40℃and stirred with a high speed disperser at 3000 rpm for 3 minutes to obtain a water-in-oil-in-water emulsion containing the soluble calcium salt.
Preparing a water-in-oil-in-water emulsion containing a soluble phosphate salt:
1) Adding 25g of silicon dioxide into 300g of peanut oil, and uniformly stirring to prepare an oil phase for later use; 20g of calcium carbonate is added into 500g of water, heated to 55 ℃ and stirred uniformly to prepare a water phase for standby.
2) Adding 100ml of dipotassium hydrogen phosphate aqueous solution with phosphate radical ion concentration of 0.01mol/L into 300ml of oil phase, heating to 45 ℃, and stirring for 3 minutes at 3000 rpm by using a high-speed dispersing machine to obtain water-in-oil emulsion containing soluble phosphate;
3) 100ml of the water-in-oil emulsion was added to 400ml of the aqueous phase, heated to 45℃and stirred with a high speed disperser at 5000 rpm for 2 minutes to obtain the water-in-oil-in-water emulsion containing soluble phosphate.
Preparing a water-in-oil-in-water emulsion containing a soluble base:
1) Adding 10g of calcium carbonate into 100g of triglyceride, and uniformly stirring to prepare an oil phase for later use; 20g of calcium carbonate is added into 300g of water, heated to 50 ℃ and stirred uniformly to prepare a water phase for standby.
2) 10ml of sodium hydroxide aqueous solution with hydroxide ion concentration of 0.01mol/L is added into 40ml of oil phase, heated to 40 ℃, and stirred for 3 minutes at 3000 rpm by a high-speed dispersing machine to obtain water-in-oil emulsion containing soluble alkali;
3) 20ml of the water-in-oil emulsion was added to 80ml of the aqueous phase, heated to 40℃and stirred with a high speed disperser at 4000 rpm for 3 minutes to obtain the water-in-oil-in-water emulsion containing the soluble base.
The preparation method of the antibacterial enamel remineralizing solution provided by the embodiment is as follows:
the water-in-oil-in-water emulsion containing the soluble calcium, zinc and silver mixed salt, the water-in-oil-in-water emulsion containing the soluble phosphate and the water-in-oil-in-water emulsion containing the soluble alkali are mixed according to the volume ratio of 13:7:2.
Test example 1
Sample 1: 10g of the antibacterial enamel remineralization liquid of example 1 was added to 120g of Yunnan white drug powder ilex toothpaste for whitening and uniformly mixed.
Sample 2: yunnan white drug powder ilex toothpaste for whitening skin.
Brushing the enamel module by adopting toothpaste of a sample 1 and a sample 2 respectively, wherein the brushing is carried out 3 times per day for 3 minutes each time, and after 15 days, a mineralization chart of the enamel surface observed by a scanning electron microscope is shown in a figure 1, wherein a is non-demineralized enamel; b is demineralized enamel, c is remineralized enamel after sample 2 is brushed and d is remineralized enamel after sample 1 is brushed; it can be seen that the load of zinc and silver enhances the remineralization degree of enamel; the distribution display diagrams of elements of zinc and silver elements successfully loaded on the enamel surface are shown in fig. 2 and 3 respectively, and fig. 2 is a distribution display diagram of elements of zinc successfully loaded on the enamel surface; fig. 3 is a graph showing the elemental distribution of silver successfully supported on the enamel surface.
As can be seen from fig. 1, 2 and 3, zinc and silver elements are successfully loaded on the enamel surface.
Test example 2
Experiment for inhibiting dental caries bacteria (Streptococcus mutans)
The enamel module after brushing in experimental group of test example 1 was placed in wells of a 24-well tissue culture plate (one module in each well, the module was not accessible to the walls of the wells), coated with normal human sterile saliva (1.0 mL/well) at 37 ℃ for 4h, and rinsed 2 times with 1.0mL PBS. Streptococcus mutans was inoculated at 37℃for two generations to a logarithmic growth phase (bacterial concentration 107 cfu/mL), and cultured for 24 hours to form a biofilm.
The dental module was rinsed 2-3 times with 1.0mL of sterile PBS (soak time for 10s per rinse) in sequence to remove non-adherent bacteria; non-invasive confocal imaging was performed using a TCSSP2 confocal microscope mounted on a 488nm Ar/Ar-Kr laser scanning head on a vibration-free platform. The objective lens used was 40×, the image was three-fold magnified; LIVE/DEAD staining of samples was performed using RBacLightTM bacterial viability kit. Dyeing time is (9+ -1) min, dyeing ratio is 1:1, obtaining the dye at corresponding wavelength [ Syto9:515 nm-530 nm; propidium Iodide (PI): an optimal fluorescence signal at >600nm ]; these measurements were performed by selecting at least 3 independent and representative locations on the biofilm-covered dental module. Within each zone, the thickest point is measured by determining the upper and lower limits of the biofilm. As shown in fig. 4, 5 and 6, wherein fig. 4 is the non-demineralized enamel biofilm thickness; FIG. 5 is the thickness of remineralized enamel biofilm after sample 2 brushing; figure 6 is the thickness of remineralized enamel biofilm after sample 1 brushing.
From fig. 4, fig. 5 and fig. 6, the bacterial film thickness of the enamel surface which can be remineralized by compartmentalization of calcium phosphate ions is equivalent to that of the original enamel, the bacterial film thickness of the enamel surface mineralized by the zinc and silver-loaded remineralizing solution is obviously reduced, and the phenomenon of bacterial death occurs, which indicates that the zinc and silver-loaded remineralizing enamel surface has antibacterial performance.
While the invention has been described in detail in the foregoing general description and specific examples, it will be apparent to those skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
Claims (7)
1. An antibacterial enamel remineralizing solution, comprising:
a water-in-oil-in-water emulsion containing a soluble calcium, zinc and silver mixed salt;
a water-in-oil-in-water emulsion containing a soluble phosphate salt;
a water-in-oil-in-water emulsion containing a soluble base;
the preparation method of the water-in-oil-in-water emulsion containing the soluble calcium, zinc and silver mixed salt/soluble phosphate/soluble alkali comprises the following steps:
mixing an aqueous solution containing soluble calcium, zinc and silver mixed salt/phosphate/alkali with an oil phase containing solid particles according to the volume ratio (1-3): (1-19) mixing, stirring for 0.5-120 minutes at the temperature of 30-80 ℃ and the rotation speed of 10-24000 r/min to obtain water-in-oil emulsion containing soluble calcium, zinc and silver mixed salt/phosphate/alkali; the water-in-oil emulsion containing soluble calcium, zinc and silver mixed salts/phosphate/alkali is then mixed with an aqueous phase containing solid particles in a volume ratio (1-3): (1-19) mixing, stirring for 0.5-120 minutes at the temperature of 30-80 ℃ and the rotation speed of 10-24000 r/min to obtain the water-in-oil-in-water emulsion containing the soluble calcium, zinc and silver mixed salt/phosphate/alkali;
the concentration of each of calcium, zinc and silver ions in the water solution containing the soluble calcium, zinc and silver mixed salt is 0.001-2.5mol/l;
the concentration of phosphate ions in the water solution containing the soluble phosphate is 0.001-1.5mol/l;
the concentration of hydroxide ions in the aqueous solution containing the soluble alkali is 0.001-2mol/l;
the solid particles are selected from one or more of calcium carbonate, aluminum oxide, silicon dioxide, calcium phosphate, magnesium aluminum silicate, lignocellulose and protein particles.
2. The antibacterial enamel remineralizing solution according to claim 1, wherein,
the soluble calcium salt is one or more selected from calcium chloride, calcium hydroxide, calcium oxide, calcium nitrate, calcium gluconate, calcium bicarbonate, calcium lactate, calcium acetate and calcium citrate;
the soluble silver salt is selected from one or more of nitrate, silver fluoride, silver chlorate and silver perchlorate;
the soluble zinc salt is selected from one or more of zinc nitrate, zinc chloride, zinc sulfate and zinc acetate;
and/or the soluble phosphate is selected from one or more of potassium phosphate, sodium phosphate, ammonium phosphate, potassium phosphate monobasic, sodium phosphate monobasic, ammonium phosphate monobasic;
and/or the soluble alkali is selected from one or more of sodium hydroxide, potassium hydroxide, lithium hydroxide and calcium hydroxide.
3. The antibacterial enamel remineralizing solution according to claim 1, wherein,
the preparation method of the oil phase containing the solid particles comprises the following steps: the mass ratio of the solid particles to the grease is (0.1-25): 100, mixing at 30-80deg.C;
and/or the preparation method of the water phase containing the solid particles comprises the following steps: the mass ratio of the solid particles to water is (0.1-25): 100.
4. An antibacterial enamel remineralizing solution according to claim 3, wherein said grease is selected from one or more of triglycerides, peanut oil, rapeseed oil, lard, tallow, shea butter, sunflower oil, walnut oil, soybean oil.
5. The method for preparing antibacterial enamel remineralizing solution according to any one of claims 1 to 4, wherein said water-in-oil-in-water emulsion containing soluble calcium, zinc and silver salts, water-in-oil-in-water emulsion containing soluble phosphate, water-in-oil-in-water emulsion containing soluble alkali are mixed.
6. Use of an antibacterial enamel remineralizing solution according to any one of claims 1-4, in the manufacture of an oral care product, wherein said oral care product is a toothpaste, mouthwash or gel.
7. An oral care product comprising the antibacterial enamel remineralizing solution according to any one of claims 1-4.
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