Tubule-closing materials from silicon dioxide for tooth care preparations

FIELD: chemistry.

SUBSTANCE: group of inventions relates to precipitated materials from silicon dioxide for application as abrasive substances or thickening agents in preparations for tooth care, which are simultaneously efficient for closing dentinal tubules in order to reduce dentin sensitivity. The claimed precipitated material from silicon dioxide has an average size of particles from 1 to 5 microns and contains a metal adduct, present on at least a part of its surface for formation of a metal adduct-processed precipitated material from silicon dioxide, which demonstrates more than 10% reduction of zeta-potential in comparison with precipitated material from silicon dioxide of the same structure but without the metal adduct. Also claimed are: versions of tooth care preparation, containing the said precipitated material from silicon dioxide and a method of processing teeth of a mammal with application of such preparations.

EFFECT: claimed precipitated material from silicon dioxide has sufficiently small size of particles and a definite ionic charge, which provides long-term adhesion of the said materials to dentin surface and efficient accumulation inside the dentinal tubules in processing teeth with tooth care preparations, containing the said material.

19 cl, 11 tbl, 10 ex, 6 dwg

Reference to related applications

This application claims the priority filing date of the provisional application U.S. No. 61/196,732, filed August 25, 2008, entitled "Materials of silicon dioxide covering the tubules, for money to care for your teeth", the disclosure of which is included in this description in its entirety by reference.

The technical field

This invention relates to precipitated materials from silicon dioxide for use as abrasive agents or thickeners in the care of the teeth, more specifically, to such deposited materials from silicon dioxide, which simultaneously close the dentinal tubules.

The level of technology

Materials of silicon dioxide is particularly useful in vehicles for the care of teeth, such as tooth pastes, where they function as abrasive substances and thickeners. In addition to these functions, the materials of silicon dioxide, especially amorphous precipitated materials from silicon dioxide, also have the advantage compared to other abrasive substances such as aluminum oxide and calcium carbonate, in care of the teeth, which is that they have a relatively high compatibility with active ingredients such as sources of fluoride, including sodium fluoride, sodium monitoroff etc. Mate is ialy of silicon dioxide is particularly suitable for use in vehicles for the care of the teeth, they provide good cleansing properties and moderate abrasion of dentin, which allows the user to effectively clean the teeth without substantial destruction of the tooth surface. The ability to provide thickening agent compatible with fluoride to toothpaste is also an important advantage for the consumer and the manufacturer.

Tooth sensitivity has recently become a problem in the field of money to care for your teeth, especially because of the loss of the protection of tooth enamel due to different dietary habits and methods of cleaning teeth in a certain circle of persons In addition to the aforementioned advantages, which give the materials from silicon dioxide means for care of teeth (grinding and thickening properties), the drafters of the compositions for certain special funds for care of teeth include certain materials, which are useful to reduce the sensitivity of the teeth to a certain extent. In particular, the toothpastes that help reduce tooth sensitivity to cold and heat and have additional benefits, such as polysaccharide sweetener that reduces pain and/or discomfort associated with unwanted feelings.

Although the causes of tooth sensitivity are not known precisely, consider that the sensitivity due to exposed dentinal tubules. This is the bone, which contain fluid and cellular patterns that emerge from the pulp of the teeth to the surface or boundary of tooth enamel. According to some theories, a lack of proper dental hygiene and/or medical conditions can lead to loss of enamel or gum recession on tooth surfaces. Depending on the severity of the loss of enamel or gum recession, the outer parts of the tubules can be exposed to the environment of the mouth. When these open tubules in contact with certain stimulants, such as, for example, hot or cold liquid, dentinal fluid can expand or contract, causing a pressure difference inside of the tooth, which leads to discomfort and possibly pain in humans.

Previous attempts to solve the problem of tooth sensitivity were aimed at blocking the pump ion channels potassium/sodium responsible for the direction of the pain impulse to the brain. Consider, without being limited to any particular theory, this chemical mechanism is created in the patient due to the inclusion of nitrate in preparations for the care of teeth. However, this alternative prevents the pain impulse to the brain, the pain still exists, but it is not felt by the patient. This illusory effect is temporary and is a waste of time, which then requires constant is e the use of toothpaste, contains potassium nitrate, to maintain the effect. Other attempts at reducing tooth sensitivity was closed channel open to the outside. This closing of the tubules was achieved by coating or filling the tubules certain types of materials from silicon dioxide. However, obtaining such "closing" materials typically involved control of particle size, which should be such as to at least partially close the channel. However, in most cases, the choice of covering material based on particle size is not by itself sufficient to ensure adequate closure to achieve a satisfactory reduction of sensitivity. Usually this covers the material has no affinity for the tooth surface and therefore does not have sufficient adhesion to remain inside, on or around the tubule in sufficient time to reduce the sensitivity to the desired level of pain and/or discomfort, to prevent or reduce pain. For example, the standard of precipitated materials from silicon dioxide may be close tubules temporarily, provided that they have a relatively small particle size for such closure tubules, but they will be easily removed, for example, when rinsing the mouth with water after brushing. The poet is mu there is a need for new materials from silicon dioxide, which would have sufficient compatibility with sources of fluoride (at some sources of fluoride), a sufficiently small particle size for effective penetration into the dentinal tubules, have a static charge for long-term stability when introduced into the dentinal tubules and the ability to transfer to the tooth and in dentinal tubules so that they could be introduced into the oral cavity and in contact with the tooth surface during normal brushing. To date such materials based on silicon dioxide, which would provide these benefits, have been created.

The invention

A significant advantage of the invention is sufficient affinity precipitated materials from silicon dioxide-treated adducts, with dentinal surface for long-lasting adhesion of these materials on the dentinal surface, which allows to introduce such materials into dentinal tubules and fill them. Another advantage of the invention is the ability to include such deposited materials from silica-treated adducts, means for care of the teeth as or abrasive agents, or thickening agents, and cleaning teeth such deposited materials from silica-treated adducts, will pass from the means to care is and the teeth on the surface of the teeth and close the dentinal tubules.

In accordance with one embodiments of the invention the means for care of teeth contains precipitated material from a silicon dioxide having an average particle size of from 1 to 5 microns and containing adduct is present at least on part of its surface, forming a precipitated material from silicon dioxide-treated adduct, which has a Zeta potential (electrokinetic potential), which is more than 10% below the Zeta-potential of deposited material from the silicon dioxide of the same structure, but without the adduct. The invention also includes means for care of teeth, containing such deposited material from silicon dioxide-treated adduct, as a thickening agent, an abrasive agent, or both, and containing at least one other component, such as a solvent, preservative, surfactant, or abrasive or thickening agent that is different from the specified precipitated material from silicon dioxide-treated adduct.

The invention also covers a method of treatment of a teeth of a mammal, comprising the following operations:

a) receiving means for care of teeth, containing precipitated material from a silicon dioxide having an average particle size of from 1 to 5 microns and containing adduct is present at least on part of its surface, the image of the store sediment from silicon dioxide, the treated adduct, which detects decrease in Zeta-potential of more than 10% compared to the precipitated material from the silicon dioxide of the same structure, but without adduct;

(b) the application of this tool for the care of teeth on the teeth of a mammal; and

c) brushing way to care for your teeth, put on stage “b”, ensuring the closure of the dentinal tubules precipitated material from silicon dioxide-treated adduct.

A brief description of graphic materials

Figure 1 shows the micrograph showing the test results on the use of funds for care of teeth on the control sample, illustrating its ability to close the dentinal tubules.

Figure 2 presents a micrograph showing the test results on the use of funds for care of teeth on the comparative sample 1, illustrating its ability to close the dentinal tubules.

Figure 3 presents a micrograph showing the test results on the use of funds for care of teeth on the sample of Example 6, illustrating its ability to close the dentinal tubules.

4 shows a micrograph showing the test results on the use of funds for care of teeth on the comparative sample 4, illustrating its ability to close the den the other tubules.

Figure 5 presents a micrograph showing the test results on the use of funds for care of teeth on the comparative sample 5, illustrating its ability to close the dentinal tubules.

Figure 6 presents a micrograph showing the test results on the use of funds for care of teeth on the comparative sample 2, illustrating its ability to close the dentinal tubules.

Detailed description of the invention

All parts, percentages and ratios are mass, unless otherwise specified. All cited documents are included in this description by reference.

Precipitated materials from silicon dioxide for use in the compositions of the means to care for your teeth were designed so that they have high affinity to the teeth of a mammal, as a result, they firmly adhere to the surface of the teeth and provide a better closure of the dentinal tubules. Not limited to any theory, believe that the increased affinity precipitated material from silicon dioxide to the teeth is a consequence of the reduction of the negative charge on the surface of the deposited material from silicon dioxide; this reduction is due to the presence of the adduct of at least part of the surface of silicon dioxide.

The charge on the surface of the oxide credit the deposits and the change of this charge is a well studied area, but in this discussion (see, for example, Ralph K. Her, The Chemistry of silica: Solubility, Polymerization, Colloid and Surface Properties and Biochemistry of silica, pp.659-672). The use of certain adducts previously discussed in the patent literature, for example in patents US 3,967,563 and US 4,122,160 on the name of the Wason, although such materials from silicon dioxide was treated metal adducts exclusively for the purposes of their ability to form transparent abrasive substances having a large particle size for the money to care for teeth.

Thus, in accordance with one variant of the invention, the precipitated material from silicon dioxide has an average particle size of from 1 to 5 microns and contains the adduct is present at least on part of its surface, forming a precipitated material from silicon dioxide-treated adduct, which provides a reduction of the Zeta potential of more than 10% compared to the Zeta-potential of the precipitated material from the silicon dioxide of the same structure, but without the adduct.

In accordance with one variant of the invention, the adduct is a metal. In accordance with another variant of the adduct is a metal selected from transition metals and poslepechatnykh metals (metals that are located in the Periodic system of the elements to the right of the transition metals). Examples of potholesinmylawn include aluminum, zinc, tin, strontium, iron, copper and mixtures thereof. Precipitated material from silicon dioxide-treated adduct formed by adding the adduct in the form of a water-soluble metal salt in the process of formation of deposited material from silicon dioxide. Any salt that is soluble in the acidic environment is suitable, for example the nitrates, chlorides, sulfates, etc.

In accordance with one variant of the invention, the precipitated material from silicon dioxide-treated adduct, reduces the Zeta potential of more than 15% compared to the Zeta-potential of the precipitated material from the silicon dioxide of the same structure, but without the adduct. In accordance with another variant of the decreasing Zeta potential more than 20%. In accordance with yet another option is reducing the Zeta-potential of more than 25%.

In accordance with one variant of the invention, the precipitated material from silicon dioxide-treated adduct receive the following way. An aqueous solution of alkali silicate such as sodium silicate, is loaded into a reactor equipped with mixing means, which is adequate to obtain a homogeneous mixture. In the reactor a solution of alkali silicate is heated to a temperature between about 65 º C and about 100ºC. Rast is the PR alkali silicate may have a concentration of approximately from 8.0 to 35 wt.%, including the range from 8.0 to about 20 wt.%. The alkali silicate may be a sodium silicate with a ratio of SiO₂:Na₂O from about 1 to about 3.5, including the range from about 2.4 to about 3.4. Alkaline silicate is loaded into the reactor, usually in an amount of about 5 wt.% to 100 wt.% all of the silicate used in the loop. Optionally, the reaction mixture was added electrolyte, such as sodium sulphate solution. Mixing can be performed under conditions of high shear.

Then to the reactor sequentially add: (1) an aqueous solution of acidifying agent or acid, such as sulfuric acid; (2) an additional amount of an aqueous solution containing the same alkali silicates, as in a reactor, such an aqueous solution is heated to a temperature from about 65 º C to about 100ºC. To a solution of acidifying agent added compound adduct before the introduction of the solution, acidifying agent into the reactor. The connection of the pre-adduct is mixed with solution of acidifying agent in a concentration of from about 0.002 to about 0.185 mol, preferably from about 0,074 to about 0,150 mol per 1 liter of the solution acidifying agent. Perhaps, if you require a higher concentration of the adduct in the besieged material of silicon dioxide, the treated adduct, instead of the acid to be used an aqueous solution of the compound adduct.

Preferred acidifying agent is in solution in a concentration of from about 6 to 35 wt.%, for example, from about 9.0 to about 20 wt.%. After all the solution of alkali silicate is introduced into the reactor, enter solution acidifying agent until, until you reach the desired pH values.

Loaded in the reactor substances leave to stand or "digested" for 5-30 minutes at the prescribed reaction temperature at a constant pH. After completion of the reaction, the reaction mixture was filtered, washed with water to remove excess inorganic salts side up until the wash water from the precipitate of silicon dioxide on the filter will not have conductivity 2000 mcmo (µs). Since the conductivity of the filtrate from washing the precipitate of silicon dioxide is proportional to the concentration of inorganic salts side, if you maintain the conductivity of the filtrate is less than 2000 mcmo, it is possible to obtain the desired low concentration of inorganic salts, such as Na₂SO₄in the sediment on the filter. The precipitate of silicon dioxide on the filter is suspended in water, then dried by conventional methods, such as spray drying, to obtain the precipitated material from silicon dioxide-treated adduct containing from about 3 wt.% to about 50 wt.% the moisture. Precipitated material of silicon dioxide, and less the p adduct, you can then grind to get the desired particle size between about 1 μm and 5 μm. Such particle size required to give a useful abrasive and/or thickening properties to the means for care of teeth and also provides the desired closure of the dentinal tubules to reduce pain and discomfort to the patient.

For the purposes of the present description, the term "means for care of teeth" has the meaning given in the document Oral Hygiene Products and Practice, Morton Pader, Consumer Science and Technology Series, Vol.6, Marcel Dekker, NY 1988, p.200, which is included in this description by reference. More specifically, the means to care for your teeth" means "... a substance that is used in conjunction with a toothbrush to clean the accessible surfaces of the teeth. Means for care of the teeth mainly consist of water, detergent, hygroscopic substance, a binder, corrigentov and finely ground abrasive powder as the main ingredient.... is that the way to care for teeth is abrasive-containing dosage form for delivery agents from and against decay to the teeth." Means for care of the teeth contain ingredients which must be dissolved before the introduction of tools for the care of teeth (for example, agents against dental caries, such as sodium fluoride, sodium phosphate, corrigentov, such as saccharin).

With the introduction of the besieged m the material of silicon dioxide, the treated adduct, means for care of the teeth, it can be present in amounts of from 0.01 to about 25% by weight of the total composition means for care of the teeth. If the deposited material from silicon dioxide-treated adduct is abrasive by nature, its amount may be from 0.05 to about 15 wt.% (this substance can only act as an abrasive, or to have a double action, i.e. at the same time to ensure closure of the tubules after brushing your teeth). If the deposited material from silicon dioxide-treated adduct, is a modifier viscosity (thickening agent), its amount may be from 0.05 to about 10 wt.%. Precipitated material from silicon dioxide-treated adduct, where the metal adduct is present in it to modify the Zeta-potential, is at the same time to ensure the modification of the viscosity and the long closing tubules. However, the precipitated material from silicon dioxide-treated adduct are not required to provide other properties, in addition to the closure of the tubules. Its quantity in the product to take care of your teeth may be in the range specified above, such materials will not give a significant degree of thickening or abrasiveness means to care for your teeth, but will only provide closure tubules. Such means is La care of teeth can contain salts of potassium nitrate as one of the examples of other material, ensure the reduction of tooth sensitivity, if necessary.

The compositions and methods described above will be better understood from reference to the following non-limiting examples.

Examples

To study the effect of the adduct on the affinity of silicon dioxide to the teeth mammals adding adduct to deposited materials from silicon dioxide were made examples of. In the first series of parties for the experimental setup was prepared several samples containing metal adduct Al₂About₃while one comparative sample contained only trace amounts of aluminum and other metals, as shown in Table 1. Samples were prepared as follows.

Amounts of reactants and conditions are presented in Table 1 below. First, in a reactor at 400 gallons (approximately 1514 liters)heated to 87º, downloaded 67 l of an aqueous solution containing 19.5 wt.% sodium silicate (molar ratio of SiO₂:Na₂O=3,32), and 167 liters of water during recirculation 30 Hz and stirring at 60 rpm Then simultaneously added an aqueous solution of sulfuric acid (having a concentration of 17.1 wt.% and containing aluminum in a concentration shown in Table 1 below) and an aqueous solution of sodium silicate (with a concentration of 19.5 wt.%, the molar ratio of SiO₂:Na₂O=3,32, the solution was heated to 85 º C) with a speed of 12.8 l/min (for the forces of the kata) and 1.2 l/min (for sulfuric acid) for 47 minutes. 47 minutes adding silicate was stopped, and the addition of acid is continued up until the pH of the mixture has not dropped to 5.5. The temperature of the reaction mixture maintained at 87º within 10 minutes that was the reaction. Then mix with the silica was filtered, washed, received the precipitate on the filter with a conductivity of about 1500 mcmo (µs). Then the residue is suspended in water, was dried with a spray dried product was ekranizirovali suitable way, including jet milling or grinding in the flow of air to particle sizes of about 3 μm. A comparative sample of precipitated silica (Comparative sample 2) was obtained from material of Example 6 using a hammer mill to particle sizes of about 10 μm. The materials obtained are then tested for the presence of several metal oxide, the concentrations of which are presented in Table 1.

The analysis of the materials according to the invention for closing tubules and other characteristics

Various materials described here from silicon dioxide were investigated as follows, unless otherwise indicated.

The surface of silicon dioxide on CTAB was determined by adsorption of CTAB (cetyltrimethylammonium bromide) on the surface of silicon dioxide, the excess was separated by centrifugation and was determined by titration with sodium lauryl using surfactants the electrode (ion-seletive electrode for the titration of surfactants). The area of the outer surface of the silica was determined by the amount of absorbed CTAB (analysis of CTAB before and after adsorption).

In particular, approximately 0.5 g of silicon dioxide accurately weighed and placed in a glass of 250 ml of 100.00 ml of CTAB solution (5.5 g/l, brought to pH 9,0±0,2), mixed on the plate with an electric mixer for 30 minutes, then centrifuged for 15 minutes at 10000 Rev/min To 5.0 ml of clear supernatant was added to 1.0 ml of 10% Triton X-I00 in a glass of 250 ml pH was brought up to 3.0-3.5 with a solution of 0.1 N HCl and the sample was titrated with a solution 0,0100 M sodium lauryl using a surfactant electrode (Brinkmann SURI50I-DL) to determine the endpoint.

Absorbance values of the oils were determined using the method of rubbing. This method is based on the principle of mixing Flaxseed oil and silicon dioxide by rubbing with a spatula on a smooth surface to produce a dense, type of filler paste. On the basis of measuring the amount of oil that is required to obtain a paste, which will form a curl when it is loading, you can calculate the value of oil absorption of the silica - value, which represents the volume of oil required per unit mass of silicon dioxide to saturate the absorbing surface of the silicon dioxide. A higher level of absorption of the oil indicates that b is more high structure precipitated silica; similarly, a low value is indicative of what is called low structure precipitated silica. The absorbance value of the oil is calculated by the following formula:

The oil absorption=ml absorbed oil X 100

weight of silicon dioxide with grams

=ml oil/100 g of silicon dioxide

The average particle size was determined using a device with a light-diffusing laser model LA-930 (or LA-300 or equivalent) from the company Horiba Instruments, Boothwyn, PA.

The percentage of residue of silicon dioxide on sieve No. 325 was determined using a standard sieve No. 325 on the U.S. standard with the holes 44 microns or 0,0017 inch (stainless steel mesh), by weighing 10.0 g of the sample with an accuracy of 0.1 grams per Cup mixer 1 quart Hamilton model No. 30, was added approximately 170 ml of distilled or deionized water and was stirred suspension of at least 7 minutes. The mixture was transferred to a sieve No. 325, sprayed water on a sieve under pressure of 20 psi for 2 minutes, and the spray head was kept at a distance of 4-6 inches from the sieves. The remaining balance was transferred to the sight glass was dried in a thermostat at 150 º C for approximately 15 minutes, then cooled and weighed on an analytical balance.

The pH of the reaction mixtures (5%suspension), you can control any electrical the om for pH measurement.

For measuring the brightness of the samples were pressed into a cuvette with a smooth surface and was measured on the meter Technidyne brightness Brightmeter S-5/BC. This device has a dual optical system, where the samples irradiated under an angle of 45º, and the reflected light look angle of 0º.

Table 2 presents the results of measurements of these properties for the materials received.

Zeta potential is a measure of the charge on the outer surface of the particles suspended in the solution. Particles with Zeta-potentials of the same charge will repel, and particles with Zeta-potentials of opposite charge will be attracted. Historically, the Zeta-potential was measured by the method of microelectrophoresis, which made the electric field through the dispersion of particles and measured the rate of migration of the particles toward the electrode of opposite charge. Particles that migrate with greater speed towards the electrode of opposite charge, will have a large amount of charge on their surface. Alternatively, the Zeta-potential can be determined by the method of electrokinetic sonic amplitude (ESA). ESA measures the electrokinetic properties of the particles electroacoustic method. The electric field of high frequency to make the dispersion of the particles. Particles will move in an alternating field in proportion to their charge on the surface. When the particles move in the same direction, the fluid will move in the opposite direction. If there is a difference in density between the particles and the liquid medium will be generated acoustic wave at the interface between the electrode and the liquid dispersion in the movement of the fluid and particles. The generated acoustic wave can be measured, and the intensity of this wave to bodysuitiodine the magnitude of the Zeta-potential. Zeta-potential is usually measured in the range of pH, as a result of receiving information about how the surface charge of suspended particles varies with pH (Greenwood, R. "Review of the measurement of zeta-potential concentration in aqueous suspensions using electroacoustics" Advances in Colloid and Interface Science, 2003, 106, 55-81 included in this description by reference). We measured the Zeta-potentials of comparative sample 1 and Examples 1 to 6, the results are presented in Table 3. From Table 3 we can see that the negative charge (as measured by Zeta-potential) on the surface of the silicon dioxide was lower in Example 6 at pH means for care of the teeth (i.e. between about 7 and about 9)than in the comparative sample 1 (comparative samples and the samples of Examples 1-10 were investigated by Zeta-potential method ESA in Colloid measurement Systems LLC).

It was found that the presence of metal adduct affects the amount of negative charge on the surface of the silicon dioxide.

Next, we determined the affinity of the samples of silicon dioxide to bovine teeth (which are similar to the teeth of all mammals) using atomic force microscopy to measure the strength of adhesion. Using atomic force microscopy (“AFM”) is a new method for this purpose. Since its development began over 20 years ago (see Its G.; spatial resolution of an F. F. Phys. Rev. Lett., 56, 930 (1986)), the AFM used for a wide range of engineering problems, including those areas as microelectronics (for example, see Douheret et al., Progress in Photovoltaics: Research and Applications, 15, 713, 2007), chemistry [e.g., S. Manne et al., Science, 251, 183 (1991)] and particularly biological science [see especially C. Drake et al., Science 243, 1586 (1989)]. The diversity of methods AFM due to several factors, among which the fact that AFM, unlike the non-optical microscopies, such as electron or transmission electron microscopy (“EAT” or “THEMES”) and scanning electron microscopy (“SEM”), does not require vacuum and special treatment of the samples (for example, spraying or coating a conductive material layer). And the M is also unique in its ability to provide true three-dimensional measurements and images.

Sample preparation for AFM was pressing silicon dioxide in the form of tablets 1.25 inches using a tablet press model Angstrom (40000 pounds, the aging time is 3 minutes). The resulting tablet was then installed on the drive for samples of size 15 mm, using double-sided adhesive strips. Then the prepared sample was mounted on an XY-scanner of the AFM or by using magnetic sample holder, or in a vacuum holder directly on the scanner.

Bovine teeth were obtained from the University's dental school Indiana in the solution of thymol. Before using them sterilized in an autoclave and kept in ethanol. Before any operations of cutting or grinding the teeth were dried. Needle cantilevers for AFM (type DNP, A cantilever, k=0.58 N/m value) was prepared by grinding bovine tooth high speed Dremel attachment #191 rotating apparatus Dremel 400|XPR. To place a drop of epoxy resin (supermicrosurgery resin Elmers Pro Bond) at the end of the cantilever used single copper wire (Hex Wix Fine Braid, # W76-10). Another piece of copper wire used to select the piece of tooth (roughly spherical, roughly ~ 20-30 µm in diameter) and place it on a drop of epoxy resin. Then the AFM cantilever was dried at room temperature overnight.

The tip of the AFM cantilever was placed n the standard holder (the holder of the cantilever model Veeco Model # DCHNM) or in the liquid holder (liquid holder cantilever model Veeco Model # DTFML-DD), and installed on the head of a scanning probe (SPM) of the AFM. All measurements were performed according to the manufacturer's instructions and using a digital instrument Dimension 3100 installed inside the acoustic hood for vibration isolation. The device operates under program control NanoScope Ilia version 4.32r3. All data is exported in units and converted to produce a force in NN in the spreadsheet. Transformation was performed using the following equation presented in the user manual Veeco Dimension 3100:

Force (NN)=Deflection (In)×Sensitivity deviation (nm·^-1)×k (NN·nm^-1),

where the deviation is the deviation of the measured intensity curve, sensitivity deviation is the slope of the curve deflection versus voltage Z when the sample is in contact, and k is the spring constant of the cantilever.

The measurements were performed in air and in liquid medium. In the case of a liquid medium used liquid holder cantilever for AFM. To eliminate variations that could occur due to the difference of the constants of the spring at different cantilevers and/or differences in the size and shape of fragments of teeth attached to the cantilevers used the same cantilever for all dimensions in a particular experiment. Estimated comparative sample 1 and the silicon dioxide obtained in the Example is 6. To simplify the strength of adhesion for the comparative samples was taken as 100%, and values for the samples were determined, respectively. The results are presented in Table 4

It was found that the sample according to the invention of Example 6 containing aluminum adduct has a greater adhesion force to the fragment of the bovine tooth for measurements in air and liquid.

In order to additionally verify that these results indeed confirm that these effects are the result of forces of attraction between particles of the teeth on the cantilever and the particles dioxide silicon tested, which used a commercially available cantilevers. As the substrate used cut pieces of bovine teeth about the size of 1×1 mm tubules oriented an angle of about 90º to the surface. We selected two different cantilever, one modified spherical particle SiO₂size 5 μm (NovaScan PT.SiO₂.SI.S) and the other is the modified spherical particle of Al₂About₃size 5 μm (NovaScan PT.CUST.SI), and measurements of affinity. The results of these measurements are presented in Tables 5 and 6.

It was found that the use of aluminum particles increased affinity compared with particles of silicon dioxide in air and in liquid medium. It should be noted that for AFM measurements of samples in each of Tables 4, 5 and 6 used a different cantilevers, therefore, the apparent difference in results is due to differences of the cantilevers.

To investigate the impact of load adduct were testing samples of silicon dioxide with increasing loading of the adduct. Physical and chemical analysis of these samples are presented in tables 1 and 2, the results of determination of affinity by AFM are presented in Table 6. It was found that the material of Example 6 had the highest affinity for the needle to which Talavera, modified bovine tooth, and that adding aluminum adduct increased the affinity of the silica particles teeth.

To study the effects of different adducts prepared samples as follows. 410 ml silicate (13.3%, and 1,112 g/ml, the molar ratio of 3.32) were loaded into a reactor and were heated to 85 º C under stirring speed 300 rpm Then simultaneously added silicate (13.3%, and 1,112 g/ml, the molar ratio of 3.32) and sulfuric acid (11.4%, and 1,078 g/ml) with speed and 82.4 ml/min and 24 8 ml/min for 47 minutes. After 47 minutes, the flow of silicate was stopped and the pH was brought to 5.5 by continuing the addition of an acid. After reaching a pH of 5.5 was leaving the reaction mixture to reaction for 10 minutes at 90ºC. After this time the reaction mixture was filtered, washed approximately 6 l of deionized water, dried at 105º during the night.

These samples of silicon dioxide was tested for the presence of certain other oxides of metals concentrations presented in table 7. Were also measured some other physical properties of these materials, the results are presented in table 8.

The samples were pressed into pellets and analyzed by AFM, as described above. It was found that the materials of silicon oxide containing a metal adducts, had a higher adhesion than the CPA the enforcement of silicon dioxide, cooked without metal adducts (or only trace amounts of adducts). In particular, all materials of silicon dioxide from 1.4% cu, 3.6% of Sn and 2.0% Al showed the strength of adhesion is higher than silicon dioxide of comparative sample 3, containing adducts.

For additional confirmation of the results obtained using the method of AFM, were held complement the performance communications experiments using test affinity in solution.

Bovine tooth was cut in half along its length tool Dremel 400|XPR equipped with a flexible shaft and a diamond disk No. 545. Then the enamel scraped from the surface of the tooth to treat dentin same Dremel tool fitted with an abrasive stone No. 8193 aluminum oxide. After removal of the enamel to the dentin surface was polished with sandpaper, 200 and 400 grit sanding paper with silicon carbide McMaster-Carr). Then the dentin was polished with a slurry of 50% silicon dioxide (US Silica). Then it was washed with deionized water, again polished with a slurry of 50% calcium carbonate (HUBERCAL® 950). After polishing the sample tooth was irradiated with ultrasound for 2 minutes in 0.5 M HCl solution and washed with deionized water.

Teflon tape is cut to half length and was wrapped around her middle part of the polished sample of a tooth with getting two open areas and one closed. The closed area was used as a control in testing. The tooth is grasped with tweezers along its side and immersed in the aqueous suspension of silicon dioxide (10.0 g silicon dioxide, glass, 150 ml, 90 ml of deionized H₂O), which was stirred with a magnetic stirrer Thomas Magnematic 15 model installed on the value of 5, for 4 minutes. During this time the tooth was moving in suspension, and the dentin was oriented in the incoming stream of particles dioc the IDA silicon. After a mixing time the tooth was removed from the solution and washed with deionized water for 2 seconds in bottles of 500 ml with inside. After washing, cut the tooth was dried at room temperature. After drying Teflon tape was carefully removed, and the tooth was analyzed by scanning electron microscope (SEM).

Comparative sample 1 and the sample of Example 6 was analyzed using test affinity in solution. The tests were repeated several times, the results are presented in figure 2 (Comparative 1) and figure 3 (Example 6 with silicon dioxide). Figure 2 and 3 pictures on the left side show the closed area of the tooth, pictures in the center of the boundary region between the closed and open areas, pictures on the right side show the open area of the tooth.

It was found that the tooth is treated with silicon dioxide according to Example 6 (2% aluminum adduct), had greater coverage than the Comparative sample 1, the processed without the adduct. These results obtained with a test for the affinity in solution, consistent with the results of the test on the affinity using AFM that silicon dioxide with adduct is more effective to close the tubules in the teeth of mammals.

Making preparations for the care of teeth and analysis of its impact on the tooth surface

The samples according to the invention, are selected is cooked, as described above, was inserted in the means for care of the teeth according to the information presented in table 10.

These compositions were analyzed for thickening ability to determine whether the materials according to the invention with small particles to provide sufficient viscosity in the care of teeth, if they will be included with abrasive precipitated by silica (Zeodent 113). Specific values of viscosity are presented in table 10. These results show that there is no difference in thickening ability when using precipitated materials from silicon dioxide-treated adduct (not all compositions were measured for viscosity at each time interval as noted below).

To determine the effect of particle size on the ability of deposited materials from silicon dioxide according to the invention to close the dentinal tubules, as well as on the ability of these materials to leave money to care for the teeth in the teeth (and fill tubules)were undertaken following tests similar to the test for the affinity in solution, described above, however, the results were shown after 1 minute of brushing your teeth 2 grams of funds for care of teeth (from Table 9), which were applied to bovine teeth (“test affinity tools for care of teeth”). In the same test affinity in solution, as described above, a piece of tape of TEFLON® (DuPont) x half inch cut along and turned them to the middle of the tooth, providing a 3 zone - 2 open and one closed. The closed area is the internal standard in the testing process.

Has been evaluated by 5 samples in the test for affinity tools for care of teeth: one control sample, the Comparative sample 1, Example 6, Comparative sample 4, Comparative sample 5. Figure 1 - 5 shows the results of this test on the affinity of funds for the care of teeth. Zone of the teeth were cleaned with a brush (soft, normal brush company Oral-B) using funds for care of teeth for 1 minute. After cleaning the memory is washed with deionized water until as there was a visible residue on the tooth (about 10 seconds).

Brief description of figures

All figures 1-6 image as follows: 1) the pictures on the left side show the closed area of the tooth, 2) pictures in the center of the boundary region between the closed and open areas, and 3) pictures on the right side show the open area of the tooth.

Images in figures 1-6 show that the materials of silicon dioxide according to Example 6 (Figure 3) demonstrate a greater affinity and covering the dentinal surface, and the area around and inside the tubules, compared with the control and comparative examples. These data correlate well with data obtained using AFM, in that silicon dioxide-treated adduct, is better suited to close the tubules of the teeth, and also the test for the affinity in solution, which showed the same phenomenon. Figures 1 and 2 show very little coverage of this type, or no show. Figures 4 and 5 show a greater degree of coverage than figures 1 and 2. In addition, samples with smaller particle size (figures 3-5) explicitly provide greater coverage than 6 (particles of silicon dioxide, the treated metal adduct, in a larger size). Even with present metal adduct the particle sizes are too large, to ensure adequate coverage within the dentinal tubules; has only been observed a certain degree of adhesion to the dentinal surface. As can be seen in Fig.6, only some small particles present along with larger particles really are inside of some tubules. However, most of the particles are too large, so that it can provide a sufficient effect closing of the tubules. 6, in particular, shows that only need granulometrical composition can provide a result that is in the delivery of large quantities of material from silicon dioxide, its adhesion and filling the dentinal tubules to reduce tooth sensitivity.

Although the invention is described in detail with respect to its specific options, it is assumed that specialists in this field of technology can be made various changes, variations and equivalents of these options. Accordingly, the scope of the invention defined by the claims and any equivalents.

1. Precipitated material from a silicon dioxide having an average particle size of from 1 to 5 microns and containing metal adduct is present at least on part of its surface for the formation of a processed metal adduct precipitated material from silicon dioxide, which detects decrease in Zeta-potential of more than 10% compared to the precipitated material ismixed silicon of the same structure, but without metal adduct.

2. Precipitated material from silicon dioxide according to claim 1, where the metal adduct includes cations and/or oxides of the metal.

3. Precipitated material from silicon dioxide according to claim 2, where the metal is selected from transition metals and poslepechatnykh metals.

4. Precipitated material from silicon dioxide according to claim 3, where the metal is selected from the group consisting of aluminum, zinc, tin, strontium, iron, copper and mixtures thereof.

5. Precipitated material from silicon dioxide according to claim 1, where the deposited material from silicon dioxide, the treated metal adduct, detects the decrease in Zeta-potential of more than 15% compared with the precipitated material from the silicon dioxide of the same structure, but without the metal adduct.

6. Precipitated material from silicon dioxide according to claim 1, where the deposited material from silicon dioxide, the treated metal adduct, detects the decrease in Zeta-potential by more than 20% compared to the precipitated material from the silicon dioxide of the same structure, but without the metal adduct.

7. Precipitated material from silicon dioxide according to claim 1, where the deposited material from silicon dioxide, the treated metal adduct, detects the decrease in Zeta-potential by more than 25% compared to the precipitated material from the silicon dioxide of the same structure, but without the metal and the product.

8. Means for care of teeth, containing precipitated material from silicon dioxide, the treated metal adduct, according to claim 1 and at least one additional component selected from the group consisting of at least one abrasive substance that is different from the specified precipitated material from silicon dioxide, the treated metal adduct, at least one thickening agent that is different from the specified precipitated material from silicon dioxide, the treated metal adduct, at least one solvent, at least one preservative and at least one surfactant, where the deposited material from silicon dioxide, the treated metal the adduct is present as an abrasive agent, thickening agent, or both in the means to care for teeth.

9. Means for care of teeth, containing precipitated material from silicon dioxide, the treated metal adduct, according to claim 5 and at least one additional component selected from the group consisting of at least one abrasive substance that is different from the specified precipitated material from silicon dioxide, the treated metal adduct, at least one thickening agent that is different from the specified precipitated material from silicon dioxide, examined what about the metal adduct, at least one solvent, at least one preservative and at least one surfactant, where the deposited material from silicon dioxide, the treated metal adduct is present as an abrasive agent, thickening agent, or both in the means to care for teeth.

10. Means for care of teeth, containing precipitated material from silicon dioxide, the treated metal adduct, according to claim 6 and at least one additional component selected from the group consisting of at least one abrasive substance that is different from the specified precipitated material from silicon dioxide, the treated metal adduct, at least one thickening agent that is different from the specified precipitated material from silicon dioxide, the treated metal adduct, at least one solvent, at least one preservative and at least one surfactant, where the deposited material from silicon dioxide, the treated metal the adduct is present as an abrasive agent, thickening agent, or both in the means to care for teeth.

11. Means for care of teeth, containing precipitated material from silicon dioxide, the treated metal adduct, according to claim 7 and at least one additional component selected is from the group consisting of at least one abrasive substance that is different from the specified precipitated material from silicon dioxide-treated adduct, at least one thickening agent that is different from the specified precipitated material from silicon dioxide-treated adduct, at least one solvent, at least one preservative and at least one surfactant, where the deposited material from silicon dioxide-treated adduct is present as an abrasive agent, thickening agent, or both in the means to care for teeth.

12. The processing method of teeth of a mammal, comprising the following operations:
a) receiving means for care of teeth, containing precipitated material from a silicon dioxide having an average particle size of from 1 to 5 microns and containing metal adduct is present at least on part of its surface for the formation of a processed metal adduct precipitated material from silicon dioxide, which detects decrease in Zeta-potential of more than 10% compared to the precipitated material from the silicon dioxide of the same structure, but without the metal adduct;
(b) the application of this tool for the care of teeth on the teeth of a mammal; and
c) brushing way to care for your teeth, put on with the adiya's "b".

13. The method according to item 12, where the means to care for your teeth, get on stage "a"further comprises at least one other component selected from the group consisting of at least one abrasive substance that is different from the specified precipitated material from silicon dioxide, the treated metal adduct, at least one thickening agent that is different from the specified precipitated material from silicon dioxide, the treated metal adduct, at least one solvent, at least one preservative and at least one surfactant, where the deposited material from silicon dioxide, the treated metal the adduct is present as an abrasive agent, thickening agent, or both in the means to care for teeth.

14. The method according to item 12, where the deposited material from silicon dioxide, the treated metal adduct, in stage "a" detects the decrease in Zeta-potential of more than 15% compared with the precipitated material from the silicon dioxide of the same structure, but without the metal adduct.

15. The method according to item 12, where the deposited material from silicon dioxide, the treated metal adduct, in stage "a" detects the decrease in Zeta-potential by more than 20% compared to the precipitated material from silicon dioxide, the same structure is tours, but without metal adduct.

16. The method according to item 12, where the deposited material from silicon dioxide, the treated metal adduct, in stage "a" detects the decrease in Zeta-potential by more than 25% compared to the precipitated material from the silicon dioxide of the same structure, but without the metal adduct.

17. The method according to item 13, where the deposited material from silicon dioxide, the treated metal adduct, in stage "a" detects the decrease in Zeta-potential of more than 15% compared with the precipitated material from the silicon dioxide of the same structure, but without the metal adduct.

18. The method according to 17, where the deposited material from silicon dioxide, the treated metal adduct, in stage "a" detects the decrease in Zeta-potential by more than 20% compared to the precipitated material from the silicon dioxide of the same structure, but without the metal adduct.

19. The method according to 17, where the deposited material from silicon dioxide, the treated metal adduct, in stage "a" detects the decrease in Zeta-potential by more than 25% compared to the precipitated material from the silicon dioxide of the same structure, but without the metal adduct.