KR20040021954A - Composition of Whitening Toothpaste - Google Patents

Abstract

PURPOSE: A whitening toothpaste composition using titanium dioxide fine powders is provided. The adhesion of the titanium dioxide fine powders on the surface of teeth exhibits teeth whitening effects. The formulation and package of the final product of the composition is provided with the shape of a conventional tubed ointment(paste phase). CONSTITUTION: The whitening toothpaste composition contains 0.1 to 10.0% by weight of titanium dioxide fine powders having a particle size of 10 to 200nm as a whitening agent. It also contains 0.05 to 0.15% by weight of fluoride and 5 to 50% by weight of a polishing agent, based on the total weight of the composition. The polishing agents are one or more selected from the group consisting of precipitated silica, silica gel, zirconium silicate, dicalcium phosphate dihydrate, dicalcium phosphate anhydrous, hydrous alumina, light calcium carbonate, heavy calcium carbonate, potassium pyrophosphate, insoluble metaphosphate and aluminium silicate.

Description

Whitening Toothpaste Composition {Composition of Whitening Toothpaste}

The present invention relates to a whitening toothpaste composition having a safe and aesthetic function to the human body. Specifically, the present invention relates to a stable and effective toothpaste composition containing titanium dioxide microparticles in a toothpaste composition having a whitening effect.

In general, tooth discoloration may be classified into exogenous discoloration and endogenous discoloration. Exogenous tooth discoloration can be caused by food debris, nicotine and tar components of tobacco, or coffee black tea deposited on the tooth surface, or soft deposits on the tooth surface by staining with pigment components. Or tetracycline antibiotics or aging.

Tooth whitening toothpaste has been commercialized and used for a long time to prevent discoloration and discoloration of discolored teeth caused by these various causes. Looking at the teeth whitening technology commercialized to date, the most classic method is the method of strong polishing and the corrosion of the tooth surface by adjusting the pH of the product to strong acidity.

However, the strong polishing method is to physically polish the surface of the tooth to make the surface smooth and expect a whitening effect.However, it is the first in the area where the tooth and gum are connected with the thinnest enamel area due to excessive wear of the tooth over a long period of use. It is obvious that abrasion can cause cervical abrasion. The method of corrosive tooth surface by adjusting the pH of the product to strong acidity also presupposes that the surface of the tooth is corroded. Therefore, the damage of the tooth caused by this corrosion decreases the hardness of the tooth, which increases the speed of tooth decay and causes irritable teeth. There is a problem that can be done.

Therefore, it is difficult to expect the actual whitening effect with the technology that only smoothes the tooth surface. Such action is expected to be effective for the coloring material due to the exogenousness mentioned above, but for the coloring by the endogenous pigmentation in the tooth surface. The effect is considered to be very weak. Therefore, the use of peroxides is essential to have a whitening effect on such endogenous pigmentation, but it has been pointed out that it is difficult to stabilize such peroxides in toothpaste for a long time, and the safety issue for the human body is excessively controversial. .

In addition, when the peroxide is used in the toothpaste composition, not only the compatibility with the general ingredients used in the toothpaste is not good, but the peroxide itself is very unstable, and there is a problem that the concentration of active oxygen decreases rapidly over time. In order to overcome this problem, Korean Patent Nos. 103,344, US Patent Nos. 4,687,663, and 5,020,694, etc. used a double container system to separate peroxides to stabilize the peroxides over time, and US Pat. No. 5,122,365 provided three separate packages. In the first step, the tooth surface is treated with acid corrosion, the second step is bleaching with peroxide and the third step is smoothing the tooth surface with abrasive and titanium oxide. And second stage In this case, the safety of the human body is questioned, and if it is commercialized based on this principle, it is expected to be troublesome to use and increase the packaging cost of the manufacturer. Numerous studies have been conducted on the safety of peroxides in toothpaste for many years, but until now, no clear conclusions have been made about such safety.

Another technique applied to the whitening toothpaste is a method of inhibiting the generation of the causative agent by blocking the polyvalent metal cations (cations such as Ca and Fe) known as the cause of discoloration using phosphates including sodium pyrophosphate. However, the effect by phosphates is difficult to expect the actual whitening effect and there is a problem that the side effects causing irritation to the oral mucosa when using a large amount of phosphate.

On the other hand, as another approach to tooth whitening effect, US Patent No. 4,986,981 attempted tooth whitening using papain, a plant proteolytic enzyme, without using peroxide. The effect was also evaluated to be very weak.

Therefore, the present inventors have determined that the whitening substance known to date has limitations in using a toothpaste composition to have a safe whitening effect on the human body. Thus, the present inventors consistently performed a collection evaluation on a new whitening substance and used it as a tooth whitening material in the toothpaste composition. The present invention was completed as a result of finding a new material that has not been made and researching and studying a prescription of a whitening toothpaste that is safe for the human body that can realize stabilization and whitening efficacy in the product for this material. The whitening toothpaste composition of the present invention can also be provided in the form of the final product formulation and packaging in the form of a tube of the conventional ointment (paste).

The whitening toothpaste composition of the present invention is characterized in that it uses a new type of whitening substance, that is, titanium dioxide fine powder. The molecular formula of titanium dioxide is expressed as TiO2 and its size has an average particle size of about 10 ~ 200nm. When titanium dioxide fine powder is used, titanium dioxide fine powder fills the tooth surface by adsorption action on the damaged and rough tooth surface, which can whiten the tooth surface, resulting in tooth whitening effect. In addition, by using the whitening toothpaste composition of the present invention by filling the damaged tooth surface of the fine powder of titanium dioxide it can be observed that the hardness of the tooth surface is increased.

Titanium dioxide is not soluble in water, but exists in a dispersed state in the toothpaste composition. Titanium dioxide is known to lighten by light scattering and is used as a brightener to increase whiteness in various products. There is an example that is used in toothpaste, but its purpose has been to improve the appearance quality of toothpaste by increasing the whiteness of toothpaste, and even in the particle size of titanium dioxide used, it is generally used as a powder having an average particle size of 200 nm or more. It was difficult to expect whitening on the teeth.

Another characteristic of titanium dioxide is that it is generally compatible with the ingredients used in toothpaste, so the final product is manufactured in the existing ointment (paste) and provided to the consumer in one package (tube, etc.). It is possible.

Considering the characteristics of the titanium dioxide fine powder, the comparison of the whitening effect with the other whitening components showed that the stability over time and the whitening effect were excellent. The higher the content of the toothpaste composition, the higher the whitening effect was, but the synergistic effect was less than 10%, and the effect was small in products containing less than 0.1%.

The types and amounts of abrasives used in the present invention are precipitated silica, silica gel, zirconium silicate, calcium dihydrogen phosphate, calcium dihydrogen phosphate, hydrous alumina, hard calcium carbonate, heavy calcium carbonate, calcium pyrophosphate, insoluble metaphosphate, and Using 5 to 50% by weight of at least one selected from aluminum silicates, the abrasiveness of the final product is represented to a value of 30 to 100 so as to avoid tooth wear due to excessive polishing. The particle size also varies depending on the type of abrasive, but the average particle size Its diameter was 20 microns or less. In general, the polishing value starts at 0 and represents a relative polishing degree with a standard toothpaste of 100. In general, most products have a value of 200 or less.

The use of humectants in toothpaste compositions is an essential base ingredient in the preparation of ointment formulations, which prevents toothpaste from drying and solidifying when exposed to air. Play a role. In the present invention, the entire toothpaste composition using concentrated glycerin (98%), glycerin (85%), sorbitol aqueous solution (70%), amorphous sorbitol aqueous solution (70%), xylitol, polyethylene glycol, and propylene glycol at least one type 20 to 70% by weight based on weight is used.

In addition, in general toothpaste compositions, suitable medicinal ingredients can be used according to the purpose of use. The use of fluoride, which is widely known as a tooth decay prevention component, is understood as an essential ingredient of toothpaste today. , At least one of amine fluoride and tin fluoride was used as fluorine to be less than 1,500 ppm in the product. In addition to the above components, enzymes may be used together for the purpose of suppressing and removing cationic surfactants or plaques for the purpose of sterilizing oral bacteria. In addition, in order to prevent periodontal disease, water-soluble salts such as sodium chloride or sodium bicarbonate having high osmotic pressure, aminocapronic acid, allantoin and allantoin derivatives having hemostatic action, and various vitamins may be used simultaneously.

In addition, the use of a binder in the toothpaste composition is essential in the ointment toothpaste to ensure that the solid powder and liquid components are not separated, and may be used as long as it is a water-soluble polymer. Commonly used components include sodium carboxymethylcellulose synthesized from cellulose of wood, carrageenan extracted from seaweed, xanthan gum obtained from metabolism of microorganisms, and the like.

The use of foaming agent enhances the feeling of use of the product, helps cleansing action, facilitates the dispersal and penetration of other active ingredients, and reduces the interfacial tension, thereby easily removing foreign substances in the oral cavity. As the foaming agent, sodium lauryl sulfate, an anionic surfactant, is mainly used, and a copolymer of polyoxyethylene polyoxypropylene (poloxamer), polyoxyethylene hardened castor oil, and polyoxy, which is auxiliary nonionic surfactant depending on the characteristics of the formulation. Ethylene sorbitan fatty acid ester is used.

In addition, in order to improve the feeling of use of the toothpaste composition according to the present invention can be used flavors, sweeteners and pigments, etc. The fragrance used for this purpose is necessary to use edible edible flavors, peppermint oil, spearmint oil, Sage, eucalyptol, methyl salicylate and fruit extract can be used. Sodium saccharin is the most commonly used sweetener, and food coloring is mainly used.

As a result of comparing and evaluating the effect and stability of the composition of the present invention consisting of the above components and the existing commercially available whitening toothpaste in various aspects, the toothpaste composition according to the present invention was much superior (Tables 3, 4 and 5) It was thus confirmed that the inventors achieved the intended effect.

Hereinafter, the present invention will be described in more detail based on the following Examples and Comparative Examples. However, this is only to help the understanding of the present invention, but the scope of the present invention in any sense is not limited thereto.

Examples 1 to 10 and Comparative Examples 1 to 4

Toothpaste compositions according to the present invention (Examples 1 to 10) and conventional toothpaste compositions (Comparative Examples 1 to 4) for comparison thereto were prepared at the composition ratios shown in Tables 1 and 2 below.

The manufacturing method is as follows.

1) After mixing and dispersing the binder and other additives in the humectant, the abrasive and the whitening agent were added and stirred for about 30 minutes.

2) Finally, after adding the foaming agent, the resultant was stirred for 20 minutes in a vacuum state to obtain a final product.

division Name Example 1 Example 2 Example 3 Example 4 Example 5 Comparative Example 1 Comparative Example 2 Comparative Example 3 Precipitated silica 20.0 15.0 - - 5.0 20.0 5.0 20.0 abrasive Calcium dihydrogen phosphate - - 45.0 - - - - - Hydrous alumina - - 5.0 - - - - - Hard calcium carbonate - - - - 25.0 - 25.0 - Calcium Pyrophosphate - - - 30.0 - - - - Silica gel - 3.0 - 5.0 - - - - Concentrated glycerin (98%) 45.0 - 20.0 - - 20.0 45.0 - Humectant Sorbitol aqueous solution (70%) - 60.0 10.0 38.0 20.0 20.0 - 30.0 Zyritol - - - - 3.0 - - 3.0 Foam Sodium Lauryl Sulfate 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 Poloxamer - - - 1.0 2.0 - - 2.0 Binder Carboxymethyl Cellulose Sodium 1.2 1.0 0.9 0.5 - 0.9 1.0 - Carrageenan - - - 0.5 0.8 - - 0.8 Titanium Dioxide (100nm) 0.1 1.0 5.0 10.0 15.0 - - - Whitening agent Sodium pyrophosphate - - - - - 4.0 - 15.0 And Hydrogen peroxide (30%) - - - - - 1.0 - 5.0 Medicinal agents Sodium Fluoride 0.76 0.38 0.76 - 0.76 0.76 0.76 0.76 Sodium fluoride 0.11 0.11 - 0.22 - - - - Spices 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 additive Saccharin 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 Purified water 29.73 16.41 10.24 11.68 25.34 30.24 20.14 20.34

division Name Example 6 Example 7 Example 8 Example 9 Example 10 Comparative Example 4 abrasive Precipitated silica 17.0 17.0 17.0 17.0 17.0 17.0 Silica gel 3.0 3.0 3.0 3.0 3.0 3.0 Humectant Sorbitol aqueous solution (70%) 60.0 60.0 60.0 60.0 60.0 60.0 Foam Sodium Lauryl Sulfate 2.0 2.0 2.0 2.0 2.0 2.0 Binder Carboxymethyl Cellulose Sodium 1.0 1.0 1.0 1.0 1.0 1.0 Whitening agent Titanium Dioxide (10nm) 1.0 Titanium Dioxide (30nm) 1.0 Titanium Dioxide (100nm) 1.0 And Titanium Dioxide (150nm) 1.0 Titanium Dioxide (200nm) 1.0 Medicinal agents Titanium Dioxide (250nm) 1.0 Sodium Fluoride 0.38 0.38 0.38 0.38 0.38 0.38 Sodium fluoride 0.11 0.11 0.11 0.11 0.11 0.11 Spices 1.0 1.0 1.0 1.0 1.0 1.0 additive Saccharin 0.1 0.1 0.1 0.1 0.1 0.1 Purified water 14.41 14.41 14.41 14.41 14.41 14.41

Experimental Example 1: Evaluation test for whitening effect using human teeth

The stain removal effect of the toothpaste composition of Examples 1-10 and Comparative Examples 1-3 was evaluated by the following method. Tobacco, coffee, tea, sugar and calcium are mixed into gel and then transferred to the bottom container of a motorized device for rotation, and tooth specimens extracted from healthy people in their 20s to 30s are epoxy resins. After fixing the specimen to make the exposed area horizontal X length = 2mm X 2mm, it was attached to the rotating plate and operated for 3 days.

At this time, incandescent lamps were installed in the center of the rotating plate to dry the stains attached to the specimens, thereby promoting adhesion of the stains. Remove the stained specimen on the last day and measure the whiteness using a color difference meter (Model: SZ, Nippon Denshoku), fix the specimen on a specially designed abrasive force meter to allow reciprocating motion, and then move the soft brush head. It is fixed to the shaft so that it can rub against the specimen. At this time, each of the Example and Comparative Example composition on the brush head 0.5g by putting the same composition for 30 minutes to reciprocate 90 times per minute, and then take out the specimen again using a colorimeter (b) After measuring the degree of increase in whiteness (△ L, ba) is shown in Tables 3 and 4 below.

division Example 1 Example 2 Example 3 Example 4 Example 5 Comparative Example 1 Comparative Example 2 Comparative Example 3 Increase in whiteness (△ L) 59.5 74.9 84.7 95.6 96.7 37.5 20.5 46.8

division Example 6 Example 7 Example 8 Example 9 Example 10 Comparative Example 4 Increase in whiteness (△ L) 65.5 71.6 76.8 69.5 62.3 32.2

As can be seen from Table 3, the toothpaste composition according to the present invention was evaluated to have a better whitening effect (increase in whiteness) than the composition of Comparative Example.

As can be seen from Table 4, the whitening effect (increase in whiteness) was different according to the average particle size of titanium dioxide used, and showed a greater whitening effect in fine particles of 200 nm or less.

Experimental Example 2: Whitening effect test through clinical trial

In order to see the more obvious whitening effect of the toothpaste composition according to the present invention, the whitening effect of the toothpaste composition of Examples 2, 3, 8 and Comparative Examples 1, 3, 4 was evaluated by direct human use for 3 months.

Forty people with relatively yellow teeth were selected and the color tone of the incisor plane was measured before starting the experiment, and the average value of the color tone was measured using a Trubyte Bioform colorimeter in a room with constant lighting. Each group of toothpaste was divided into six groups (10 people each) to be almost identical, and each toothpaste composition was distributed and brushed according to a usual brushing habit.

In order to confirm the increase of the brightness of teeth, 10 kinds of sensory identifications were selected from the 24 standard standards of brightness of the Trubyte Bioform colorimeter, and in order of increasing brightness for each An evaluation score was added to 10 points.

Before using the experimental toothpaste, the tooth brightness value of each group was evaluated to the first digit after the decimal point based on the above criteria, the brightness value after brushing for 3 months was evaluated, and then the increase rate of the average brightness value was calculated.

division Example 2 Example 3 Example 8 Comparative Example 1 Comparative Example 3 Comparative Example 4 Average brightness value (before experiment) 4.1 4.0 4.1 4.1 4.0 4.0 Average brightness value (after 3 months use) 8.1 8.7 8.2 5.4 6.2 4.8 % Increase in brightness 97.6 117.5 100.0 31.7 55.0 20.0

As can be seen from the results, the toothpaste composition using the titanium dioxide fine powder according to the present invention was evaluated to have a better whitening effect (increasing effect of brightness) than the general whitening toothpaste composition of the comparative example.

Experimental Example 3 Comparative Evaluation of Time-lapse Quality of Toothpaste Composition

The toothpaste compositions of Examples 1 to 5 and Comparative Examples 1 to 3 were stored at room temperature and 40 ° C., and the state stability of the toothpaste compositions was evaluated at regular intervals according to the following criteria.

<< evaluation criteria >>

◎ Very good: smooth surface, no phase separation, normal toothpaste

○ Relatively good: Only the surface is slightly rough or the tube entrance is slightly bad

▽ Relatively bad: Phase separation and slight discoloration and gas generation

× Very bad: severe phase separation and gas generation or hardening

time lapse Example 1 Example 2 Example 3 Example 4 Example 5 Comparative Example 1 Comparative Example 2 Comparative Example 3 1 month Room temperature ◎ ◎ ◎ ◎ ◎ ◎ ◎ ◎ 40 degrees ◎ ◎ ◎ ◎ ◎ ▽ ◎ × 3 months Room temperature ◎ ◎ ◎ ◎ ◎ ▽ ◎ ▽ 40 degrees ◎ ◎ ◎ ◎ ◎ × ○ × 5 months Room temperature ◎ ◎ ◎ ◎ ◎ ▽ ○ × 40 degrees ○ ○ ○ ○ ▽ × ▽ × 8 months Room temperature ◎ ◎ ◎ ◎ ◎ × ▽ × 40 degrees ○ ○ ▽ ▽ × × × ×

As shown in the above results, the toothpaste composition according to the present invention is superior to conventional whitening toothpaste composition, that is, a comparative example toothpaste composition containing peroxide and pyrophosphate as a whitening agent, and is thought to be advantageous in terms of commodity value. It was more severe as time passed.

The present invention relates to a toothpaste composition having a tooth whitening effect, by using a titanium dioxide micropowder in the toothpaste composition, the fine powder of titanium dioxide is attached to the tooth surface to show the tooth whitening effect, the whitening toothpaste composition of the present invention is a formulation of the final And the packaging form can also be provided in the form of the tube in the conventional ointment (paste phase).

Claims (3)

A whitening toothpaste composition, wherein the whitening toothpaste composition contains 0.1 to 10.0% by weight of titanium dioxide (TiO 2) as a whitening agent, and has an average particle size of 10 to 200 nm. The fluoride used in the toothpaste composition contains 0.05 to 0.15% by weight of the entire toothpaste composition as fluorine using at least one selected from sodium phosphate, sodium fluoride, amine fluoride, and tin fluoride. Whitening toothpaste composition characterized in. The abrasive used in the toothpaste composition is a precipitated silica, silica gel, zirconium silicate, calcium dihydrogen phosphate, calcium dihydrogen phosphate, hydrous alumina, hard calcium carbonate, heavy calcium carbonate, calcium pyrophosphate, insoluble meta A whitening toothpaste composition comprising 5 to 50% by weight of at least one selected from phosphates and aluminum silicates.