KR20100085344A - Toothpaste composition comprising poorly water soluble dye dispersed bead - Google Patents

Abstract

PURPOSE: A toothpaste composition containing bead in which water-insoluble pigment is dispersed is provided to improve stability and efficiency and to prevent color shift phenomenon. CONSTITUTION: A toothpaste composition comprises a bead having core particles and coating materials. The coating material contains 35-99.99 weight parts of cellulose, 4-60 weight parts of mannitol, 0.5-10 weight parts of hydroxylpropyl methyl cellulose, and 0.01-2.5 weight parts of water-insoluble pigment. The composition contains 0.01-5 weight parts of bead based on 100 weight parts of total composition. The average particle diameter of the bead is 0.1-10 mm. The bead additionally contains functional effective ingredient or perfume ingredient.

Description

Toothpaste composition comprising beads dispersed in poorly water-soluble pigments {TOOTHPASTE COMPOSITION COMPRISING POORLY WATER SOLUBLE DYE DISPERSED BEAD}

The present invention relates to a dentifrice composition comprising beads in which a poorly water-soluble pigment is dispersed on the surface, and more particularly, to a dentifrice composition having excellent aging stability and effectiveness.

In the field of toothpaste manufacturing, techniques for producing toothpaste capable of expressing two or more colors different from each other have been studied in various directions for the purpose of stimulating the purchasing desire of the general consumer due to the appearance beauty of the product.

In order to express two or more colors having different colors in the toothpaste composition, a color pigment for expressing different colors must be included in each medium. By the way, in each medium containing different colored pigments, since there exists a difference in the concentration of the pigments at the interface between which they are in contact with each other, the colored pigments contained in one medium are diffused into the other medium in contact with each other. Penetration of the colored pigment by such diffusion is apparently observed as a color bleeding phenomenon in which the boundary between toothpaste mediums in contact with each other becomes unclear. For this reason, when the toothpaste is discharged from the inside of the toothpaste container, the sharp color separation as the user desires does not appear, and when the color bleeding is excessively progressed, the toothpaste product may be recognized as dirty. Therefore, the color bleeding phenomenon in toothpaste that expresses two or more colors is a significant factor to reduce the buyer's desire to purchase a product.

In order to solve this problem, a method of distinguishing the toothpaste container in which the toothpaste is stored to discharge toothpaste of different colors together, or mixing the pigment in a water-insoluble resin such as polyethylene or encapsulating the pigment in wax has been attempted. The manufacturing cost of the container is excessively increased, or the inherent odor contained in the toothpaste is reduced due to the wax, and wax and the like are difficult to commercialize due to low economical efficiency as an expensive material.

On the other hand, in the field of toothpaste manufacturing, there have been attempts to improve various functional effects by using a toothpaste composition containing beads.

Korean Patent Laid-Open Publication No. 2002-56224 describes a toothpaste composition in which jojoba beads are formulated so as to know a proper brushing time. When brushing for a certain time, the jojoba bead breaks down finely due to the friction between the toothbrush and the teeth, and can recognize the particle color at the beginning of brushing. It is possible to know a sufficient brushing time. However, these dentifrice compositions only make it possible to recognize sufficient dentition time and could not have sufficient hardness for use in toothpaste prevention and toothpaste of coatings containing pigments.

In addition, Korean Patent Publication No. 10-2005-0058069 discloses a toothpaste composition containing the active ingredient. It is effective for oral diseases and treatments by improving the ocular stability and effectiveness of oily ingredients in soft beads. However, these dentifrice compositions have only increased the stability of the active ingredient and are not related to preventing color bleeding.

Therefore, there is a need for research on the development of a toothpaste composition having no long-term color bleeding effectively without adding a separate manufacturing device, having sufficient hardness for use in toothpaste, and having excellent stability in the formulation.

The present invention is to provide a toothpaste composition having a sufficient hardness when used for the manufacture of toothpaste and gargle without the color bleeding for a long time.

The present invention also provides a dentifrice composition having improved stability in the formulation of the dentifrice composition while including the functional active ingredient and flavor in the beads.

The present invention includes beads comprising a core particle and a coating material surrounding the core material, wherein the coating material provides a dentifrice composition comprising cellulose, mannitol, hydroxypropylmethylcellulose, and a poorly water-soluble pigment.

The present invention also the coating material is a) 35 to 99.99 parts by weight of cellulose, b) 4 to 60 parts by weight of mannitol, c) 0.5 to 10 parts by weight of hydroxypropylmethylcellulose, based on 100 parts by weight of the total weight of the coating material, and d) provides a dentifrice composition comprising 0.01 to 2.5 parts by weight of a poorly water-soluble pigment.

Hereinafter, the present invention will be described in more detail.

The present inventors have found that the toothpaste prepared by adding the beads improves the stability and effectiveness over time so that the pigment does not spread in the toothpaste while including the pigment, the functional active ingredient and the flavor.

In particular, the toothpaste composition of the present invention is characterized in that it comprises a bead (Bead) homogeneously dispersed coating material containing a poorly water-soluble pigment. The beads include pigments, functional active ingredients, and fragrances, but improve time stability and effectiveness so that the pigments do not spread in the toothpaste. In addition, the beads are not broken even during toothpaste manufacture, and can be delivered to every corner of the oral cavity while the functionally effective ingredients and fragrances are sufficiently broken during brushing.

The toothpaste composition of the present invention comprises a bead consisting of the core particles and a coating material surrounding the coating material, the coating material comprises cellulose, mannitol, hydroxypropylmethyl cellulose, and poorly water-soluble pigments.

The toothpaste composition of the present invention comprises beads in an amount of 0.01 to 5 parts by weight, preferably 0.1 to 2 parts by weight, based on 100 parts by weight of the total weight of the total composition.

The beads are first composed of core particles and a coating material surrounding the beads, and may be prepared by coating a coating material including a poorly water-soluble pigment using the core particles as a support.

The beads may be coated by coacervation method, spray drying method, spray cooling method, crystallization method, co-crystallization method, and fluidized bed method. Among these, the fluidized bed method is most preferable. The fluidized bed method uses a fluidized bed gutter consisting of unit processes of raw material conveying, mixing, coalescing, granulation and drying. That is, a coating of the beads is made by spraying the coating material solution through the spray nozzle while flowing the core particles by the flowing air using a fluidized bed coater.

In the bead manufacturing process, the core particle is used as a support for coating a coating material with a particle diameter sufficient for preparing a bead, and if it can serve as a support, it can be prepared including all ingredients known to be used in the toothpaste composition. have.

The core particle may have an average particle diameter of 0.01 to 1 mm, preferably 0.02 to 0.08 mm, and the particle diameter of the core particle in the above range in terms of providing sufficient hardness and color development characteristics to the coated beads. It is desirable to maintain.

In a preferred embodiment of the present invention, the core particles may be prepared in the same composition as the coating material. More preferably, it may include one or more selected from the group consisting of cellulose, mannitol, hydroxypropylmethyl cellulose, and poorly water-soluble pigments, and may be prepared by further comprising a functional active ingredient, a fragrance component, and the like. The beads of the present invention are completed by uniformly dispersing the coating material using the components thus mixed as a core.

In particular, the core particles are based on 100 parts by weight of the total core particles, 35 to 99.99 parts by weight of cellulose, 0 to 60 parts by weight of mannitol, 0 to 10 parts by weight of hydroxypropylmethylcellulose, and 0.01 to 2.5 parts by weight of poorly water-soluble pigments. It may include one or more selected from the group consisting of.

In another preferred embodiment of the present invention, the core particles are based on 100 parts by weight of the total core particles, 60 to 99.99 parts by weight of cellulose, 5 to 15 parts by weight of mannitol, 0.5 to 5 parts by weight of hydroxypropylmethylcellulose, And 0.01 to 2.5 parts by weight of poorly water-soluble pigments.

On the other hand, the present invention uses a poorly water-soluble pigment that does not dissolve in water, which is the main solvent in the toothpaste, there is no color bleeding in the toothpaste. In particular, as the poorly water-soluble pigments, blue 201 (D & C Blue No. 6), red 226 (D & C Red No. 30), red 202 (D & C Red No. 7), green 201 (D & C Green No. 5) , Green No.202 (D & C Green No.6), Orange No.201 (D & C Orange No.5), Orange No.206 (D & C Orange No.10), Purple No.201 (D & C Violet No.2), Yellow No.201 (D & C Yellow No. 7), titanium oxide, or the like can be used as one or more kinds, and from the standpoint of light stability, Blue 201 (D & C Blue No. 6), Red 226 (D & C Red No. 30), titanium oxide, and the like are preferred. Can be used.

In order to properly express the bead color, it is desirable to allow the coating material to be uniformly dispersed during the manufacturing process.

In the present invention, the poorly water-soluble pigment is used by encapsulating it with an insoluble or poorly soluble coating agent. In particular, as the coating agent, cellulose, mannitol, and hydroxypropylmethylcellulose, which are insoluble or poorly soluble in water and having a rigid structure that is destroyed by mechanical stimulation, are used. Cellulose is a water-insoluble substance that plays a role in preserving the form of beads in juicy toothpaste. In addition, mannitol and hydroxypropylmethylcellulose increase the binding strength of the beads and prevent swelling by water. Therefore, the hardness of the beads and the stability in the toothpaste may vary depending on the content of cellulose, mannitol, and hydroxypropylmethylcellulose.

In a preferred embodiment of the invention, the coating material is a) 35 to 99.99 parts by weight, preferably 60 to 99.99 parts by weight of cellulose based on 100 parts by weight of the total weight of the coating material; b) 4 to 60 parts by weight, preferably 5 to 15 parts by weight of mannitol; c) 0.5 to 10 parts by weight of hydroxypropylmethylcellulose, preferably 0.5 to 5 parts by weight; And d) 0.01 to 2.5 parts by weight of the poorly water-soluble pigment, preferably 0.10 to 2.00 parts by weight.

In the present invention, the beads may further include a functional active ingredient or a flavor component in addition to, and may be included in each of the core particles and the coating material.

As the functional active ingredient, one or more selected from the group consisting of tocopherol acetate, sodium chloride, tranexamic acid, aminocaproic acid, pyridoxine hydrochloride, tranexamic acid, triclosan, vitamin A, allantoin, and palmitic acid may be used. have.

As the fragrance component, all compounds known to be generally usable in the dentifrice composition may be used, and are not particularly limited thereto.

In addition, the beads include fluorides such as water-soluble sodium fluoride, sodium fluoride phosphate, amine fluoride and tin fluoride, pyrophosphates such as sodium pyrophosphate, potassium pyrophosphate and sodium pyrophosphate, cationic surfactants, enzymes, sodium chloride or hydrogen carbonate. It may further include an active ingredient such as water-soluble salts such as sodium, aminocaproic acid, allantoin and allantoin derivatives having a hemostatic action, and various vitamins.

In addition, in the present invention, the beads may have an average hardness of 100 to 1000 g, preferably 300 to 900 g, and more preferably 500 to 800 g, depending on the content of the coating material. . At this time, as a method of measuring the hardness, it can be measured using a compression tester (FGC-01 Shimpo, Japan) and the average value can be obtained. If the hardness of the bead is less than 100 g may cause color bleeding phenomenon when the toothpaste is manufactured, if more than 1000 g may feel a lot of foreign body due to the bead at the time of brushing, may cause inconvenience during use.

The beads may have an average particle diameter of 0.1 mm to 10 mm, preferably 0.2 mm to 8 mm, more preferably 0.3 mm to 2 mm. In particular, the diameter of the beads is 0 to 10% by weight of more than 1.0 mm to 20 mm in diameter, 50 to 100% by weight of more than 0.425 mm to less than 1.0 mm in diameter, 0.425 mm or less to 0.01 mm or more relative to the total weight of the beads It may be from 0 to 50% by weight, preferably from 95% or more of particles having a diameter of 0.425 mm to 1.00 mm of all beads. The diameter of the beads in the dentifrice composition of the present invention is preferably maintained in the above range in terms of ensuring excellent stability in the dentifrice composition and excellent sensory evaluation when brushing.

The toothpaste composition of the present invention may be prepared by mixing components other than beads, such as abrasives, wetting agents, binders, foaming agents, and the like, which are generally known to be usable in toothpaste compositions.

The abrasive may be selected from among dental type silica, 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 aluminum silicate. Use at least one kind. Among them, abrasives such as dental type silica, precipitated silica, silica gel and zirconium silicate can be preferably used. The abrasive is preferably included in an amount of 5 to 30 parts by weight based on the toothpaste composition.

The humectant is an essential base ingredient in the preparation of the toothpaste formulation, which prevents the toothpaste from drying and solidifying when exposed to the air and provides a gloss on the surface of the toothpaste, and also serves to sweeten the toothpaste according to the type. In the toothpaste composition of the present invention, 20 to 75 of at least one selected from concentrated glycerin (98%), glycerin (85%), aqueous sorbitol solution (70%), aqueous amorphous sorbitol solution (70%), polyethylene glycols and propylene glycol Used in parts by weight.

The binder serves to prevent the solid powder and liquid components from being separated. Any kind of water-soluble polymer may be used, and examples of commonly used components include sodium carboxymethyl cellulose, carrageenan, xanthan gum, and the like.

The foaming agent acts to easily remove foreign substances in the oral cavity by enhancing the feeling of use of the product, aiding the cleaning action, speeding up the dispersion and penetration of other active ingredients, and reducing the interfacial tension. As the foaming agent, sodium lauryl sulfate which is an anionic surfactant, a copolymer of polyoxyethylene-polyoxypropylene (poloxamer), polyoxyethylene hardened castor oil, polyoxyethylene sorbitan fatty acid ester and the like can be used.

Flavors, sweeteners and pigments may be used in order to improve the usability in addition to the above ingredients, and as the fragrance used for this purpose, the use of edible edible flavors is essential. Sodium saccharin is most commonly used as a sweetener, and food coloring is preferably used as a pigment.

In addition, in the present invention, in addition to the functional active ingredient added to the beads, a suitable functional active ingredient may be added directly to the dentifrice composition, depending on the purpose of use. As such functional active ingredients, water-soluble fluorides, pyrophosphates, cationic surfactants, active ingredients and the like can be used.

The water-soluble fluorides include sodium fluoride, sodium phosphate, amine fluoride and tin fluoride. The pyrophosphates include sodium pyrophosphate, potassium pyrophosphate, and acid pyrophosphate. It is used for the purpose of sterilizing bacteria, and the active ingredient is sodium bicarbonate, tocopherol acetate, sodium chloride, tranexamic acid, aminocapronic acid, pyridoxine hydrochloride, tranexamic acid, triclosan, vitamin A, allantoin, palmitic acid Etc.

In addition, the present invention can provide a stabilization method for improving the stability in the formulation of the composition for oral cavity by encapsulating a pigment, a functional active ingredient and a flavor component with the coating agent.

In the present invention, matters other than those described above can be added or subtracted as required, and therefore, the present invention is not particularly limited thereto.

The present invention can be used to prevent the color bleeding for a long time by using the beads (Bead) in which the poorly water-soluble pigments are effectively dispersed on the surface, to ensure sufficient hardness that can be used in the manufacture and brushing of toothpaste, and for the functional active ingredient and flavor component It is effective to secure excellent stability.

Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the scope of the present invention is not limited to the following examples.

Example  1-3

To prepare a coating material with a composition as shown in Table 1, after preparing the core particles having an average particle diameter of 0.2 mm in the same composition as the coating material, the coating material is coated on the core particles using a fluidized bed coater to average particle diameter 0.7 mm of beads were prepared. The unit in Table 1 below is weight percent.

In Examples 1 to 3, blue 201, red 226, and titanium oxide, which are poorly water-soluble dyes, were added, respectively.

division Example 1 Example 2 Example 3 cellulose 90 90 90 Mannitol 5 5 5 Hydroxypropylmethylcellulose 2 2 2 Blue 201 One - - Red 226 - One - Titanium oxide - - One Blue No. 1 Menthol flavor One One One Tocopherol Acetate One One One

Based on the total weight of the composition, 0.2% by weight of the beads thus prepared, 20% by weight of abrasive dental type silica, 1.5% by weight of binder carboxymethylcellulose sodium, 50% by weight of aqueous solution of wetting agent sorbitol (70%), foaming agent la Toothpaste composition was prepared by mixing 2.0 wt% sodium uryl sulfate, 0.2 wt% sodium saccharin sweetener, and the balance of purified water.

Comparative example  One

A toothpaste composition was prepared in the same manner as in Example 1, except that blue No. 1, which was not a poorly water-soluble dye, was added instead of blue 201, which is a poorly water-soluble dye.

Comparative example  2

A toothpaste composition was prepared in the same manner as in Example 1, except that blue 201 pigment, which is a poorly water-soluble pigment, was added to the beads and mixed directly in an amount of 0.2% by weight based on the total weight of the composition. It was.

Comparative example  3

A toothpaste composition was prepared in the same manner as in Example 1, except that the crude jojoba beads including the blue pigment 201 were prepared and used.

Comparative example  4

A toothpaste composition was prepared in the same manner as in Example 1, except that the blue 201 pigment was encapsulated with a wax.

Comparative example  5

A toothpaste composition was prepared in the same manner as in Example 1, except that a lake pigment having a yellow 203 lake pigment attached to the alumina carrier was used.

Experimental Example  One

For the toothpaste compositions of Examples 1 to 3 and Comparative Examples 1 to 5 were tested as follows to evaluate the change over time in the dentifrice formulation.

First, the toothpaste compositions prepared according to Examples 1 to 3 and Comparative Examples 1 to 5 were treated under conditions of 0 ° C., room temperature (22-25 ° C.), 40 ° C., and 50 ° C. for 1 week and 1 month, respectively. For color bleeding after storage in a greenhouse, the color bleeding is defined as the color bleeding around the beads contained in the transparent toothpaste, and the appearance evaluation was performed based on the following criteria.

Color bleeding  Appearance Evaluation Criteria

Stable: No color bleeding in beads or toothpaste

Unstable: Has color bleeding in beads or toothpaste

The evaluation results of the color change over time for the toothpaste compositions of Examples 1 to 3 and Comparative Examples 1 to 5 are shown in Table 2 below.

division Evaluation temperature (℃) 0 Room temperature 40 50 Example 1 1 week stability stability stability stability 1 month stability stability stability stability Example 2 1 week stability stability stability stability 1 month stability stability stability stability Example 3 1 week stability stability stability stability 1 month stability stability stability stability Comparative Example 1 1 week stability Instability Instability Instability 1 month Instability Instability Instability Instability Comparative Example 2 1 week stability Instability Instability Instability 1 month stability Instability Instability Instability Comparative Example 3 1 week stability stability Instability Instability 1 month stability Instability Instability Instability Comparative Example 4 1 week stability stability stability stability 1 month stability stability stability Instability Comparative Example 5 1 week stability stability stability stability 1 month stability stability Instability Instability

As can be seen in Table 2, it was found that the toothpaste compositions of Examples 1 to 3 according to the present invention are all stable in the toothpaste formulation without color bleeding in the toothpaste even after a long time of one month or more.

Example  4

Toothpaste composition was prepared in the same manner as in Example 1, except that the bead content was changed to 1% by weight with the composition as shown in Table 3 below. The units in Table 3 below are by weight.

Comparative example  6 ~ 7

Example 1 and using the same content as the one added to the beads of Example 4, except for directly mixing the functional active ingredient and the flavor component, respectively, without the addition of separate beads in a composition as shown in Table 3 below Toothpaste compositions were prepared in the same manner. The units in Table 3 below are by weight.

division Example 4 Comparative Example 6 Comparative Example 7 Dental Type Silica 20 20 20 Carboxymethyl Cellulose Sodium 1.5 1.5 1.5 Sorbitol aqueous solution (70%) 50 50 50 Sodium Lauryl Sulfate 2.0 2.0 2.0 Zaccarin Sodium 0..2 0..2 0..2 Beads (prepared according to Example 1) 1.0 - - Menthol flavor - 0.01 Tocopherol Acetate - - 0.01 Purified water Balance Balance Balance

Experimental Example  2

In the toothpaste compositions of Example 4 and Comparative Example 6, the following tests were performed to evaluate the change over time of the menthol flavor content in the toothpaste formulation.

First, the toothpaste compositions prepared according to Example 4 and Comparative Example 6, under the conditions of 0 ℃, room temperature (22 ~ 25 ℃), 40 ℃, 50 ℃, constant temperature room for 1 week, 1 month, 3 months respectively The residual content of menthol flavor was compared after storage at. The content of menthol flavor was confirmed by chromatographic analysis, which is expressed as weight% relative to the initial blend amount.

The menthol flavor content evaluation results for the dentifrice compositions of Example 4 and Comparative Example 6 are shown in Table 4 below.

Temperature
(℃) Example 4 Comparative Example 6 1 week 1 month 3 months 1 week 1 month 3 months 0 99.7% 99.7% 99.6% 99.6% 99.5% 99.2% Room temperature 99.5% 99.2% 98.7% 99.3% 99.0% 98.1% 40 99.1% 97.7% 96.2% 98.8% 97.2% 95.4% 50 98.7% 96.5% 95.4% 97.6% 95.2% 92.1%

As can be seen in Table 4, the toothpaste composition of Example 4 containing the beads in the present invention is more stable than the toothpaste composition of Comparative Example 6 to which menthol flavor was added directly, as shown in Table 4 above. It can be seen.

Experimental Example 3

The toothpaste compositions of Example 4 and Comparative Example 7 were tested as follows to evaluate the change over time of the content of tocopherol acetate in the toothpaste formulation.

First, the toothpaste compositions prepared according to Example 4 and Comparative Example 7 in a constant temperature room for 1 week, 1 month, 3 months under the conditions of 0 ℃, room temperature (22 ~ 25 ℃), 40 ℃, 50 ℃, respectively After storage at to compare the residual content of tocopherol acetate. The content of tocopherol acetate was confirmed by chromatographic analysis, which is expressed as weight% relative to the initial blending amount.

Tocopherol acetate content over time evaluation results for the dentifrice compositions of Example 4 and Comparative Example 7 are shown in Table 5 below.

Temperature
(℃) Example 4 Comparative Example 7 1 week 1 month 3 months 1 week 1 month 3 months 0 99.6% 99.4% 99.2% 99.5% 99.4% 99.2% Room temperature 99.0% 98.7% 98.1% 99.0% 98.5% 97.8% 40 ℃ 98.9% 97.8% 96.0% 98.5% 97.0% 94.9% 50 ℃ 98.7% 96.7% 95.6% 97.8% 95.6% 92.5%

As can be seen in Table 5, the toothpaste composition of Example 4 containing the bead of the present invention is more stable than the toothpaste composition of Comparative Example 7 to which tocopherol acetate was directly added. It can be seen.

Example  5 and Comparative example  8-9

A bead was prepared in the same manner as in Example 1, except that the coating material described in the composition as shown in Table 6 was prepared, and a core particle having an average particle diameter of 0.2 mm was prepared in the same composition as the coating material. . The units in Table 6 below are by weight.

division Example 5 Comparative Example 8 Comparative Example 9 cellulose 90 92 95 Mannitol 5 5 0 Hydroxypropylmethylcellulose 2 0 2 Blue 201 One One One Menthol flavor One One One Tocopherol Acetate One One One

The beads thus prepared had a diameter distribution and an average particle diameter as shown in Table 7 below, and a toothpaste composition was prepared in the same manner as in Example 1, except that beads were added in this diameter distribution.

At this time, the diameter of the beads was measured by the following method using 18 (eye size 1000 μm), 40 (eye size 425 μm) mesh or the like.

Bead diameter measurement method

(1) 10 g of beads were accurately weighed.

(2) The body is arranged so that the larger the mesh value is below.

(3) Put the weighed beads on the body and shake as much as possible. At this time, under the 40 mesh sieve (Mesh sieve) was able to pick up the flowed granules, this process was repeated about 10 times each minute.

(5) The weight of the granules remaining in each body was measured and converted into percentages.

The diameter distribution measured by the above method with respect to the beads prepared according to Example 5 and Comparative Examples 8 to 9 is as shown in Table 7 below.

division Example 5 Comparative Example 8 Comparative Example 9 Bead Count 100 100 100 Average particle diameter (mm) 0.72 0.05 13 1.0mm or more in diameter (% by weight) 2 0 90 0.425-1.0mm or more in diameter (% by weight) 88 10 9 0.425 mm or less in diameter (% by weight) 10 90 One

Experimental Example  4

About the beads manufactured according to Example 5 and Comparative Examples 8 to 9, the hardness of the beads was measured using a compression tester (FGC-01 Shimpo, Japan), and the average value was obtained. The measurement results are shown in Table 8 below.

division Example 5 Comparative Example 8 Comparative Example 9 Bead Count 100 100 100 Hardness range (g) 310 to 970 40 to 80 20 to 30 Average hardness (g) 565 ± 165 50 ± 13 27 ± 9

As can be seen in Table 8, it can be seen that the beads prepared according to Example 5 of the present invention have superior hardness compared to the beads of Comparative Examples 8 and 9 to which hydroxypropylmethylcellulose or mannitol is not added. .

Experimental Example  5

With respect to the toothpaste composition prepared according to Example 5 and Comparative Examples 8 to 9, it was observed whether the bead breaks during toothpaste preparation.

In the toothpaste manufacturing process, the beads of the coating material containing poorly water-soluble pigments were broken and the color of the entire toothpaste was visually observed, and the results are shown in Table 9 below.

division Example 5 Comparative Example 8 Comparative Example 9 Toothpaste color variations No color change Turns blue Turns blue

As can be seen in Table 9, the beads of Example 5 containing hydroxypropylmethylcellulose and mannitol in the coating material of the beads with a poorly water-soluble pigment in accordance with the present invention without breaking the beads during the toothpaste manufacturing process You can see that there is no color change in the toothpaste.

However, Comparative Examples 8 and 9, which contain only poorly water-soluble pigments without containing hydroxypropylmethylcellulose or mannitol, respectively, in the coating material of the beads, the bead hardness is significantly lower than the hardness required to prepare the dentifrice composition. You can see that the beads are broken and color bleeding occurs at.

Experimental Example  6

For toothpaste compositions prepared according to Example 5 and Comparative Examples 8-9, the sensory rejection according to the diameter of the beads was evaluated.

First, the toothpaste compositions of Examples 5 and Comparative Examples 8 to 9 were brushed for 3 minutes to 20 test subjects (10 males and 10 females of 25-35 years of age) after one week of preparation. In addition, sensory evaluation was performed to determine the degree of rejection of the teeth in the toothpaste due to fractures. The evaluation results are shown in Table 10 below.

Sensory evaluation result Example 7 Comparative Example 8 Comparative Example 9 No feeling 4 18 One I feel massage when brushing my teeth 15 2 6 Severe rejection One 0 13

As can be seen in Table 10, the toothpaste composition of Example 5 according to the present invention can be seen that the bead does not give a sense of rejection even while brushing the bead when feeling the massage.

On the contrary, the toothpaste composition of Comparative Example 8 using beads having a diameter of 0.425 mm or less but 90% by weight did not give a sense of rejection in brushing the teeth, but there was no sensory feeling. Although the toothpaste composition of 9 was evaluated to have a feeling of bead massage when brushing teeth in some sense, it can be seen that the majority is evaluated as giving a rejection in the gargle, it is difficult to practically commercialize.

According to the present invention, by using beads having a uniformly dispersed coating material including a poorly water-soluble pigment on the surface, a toothpaste composition having a hardness sufficient for use in preparing toothpaste, brushing teeth, or the like without prolonged color bleeding in toothpaste can be prepared. have. In particular, the bead in the present invention can be secured in the formulation of the toothpaste composition while containing a functional active ingredient and flavor, it can be said that the industrial applicability is very large.

Claims (11)

A bead consisting of core particles and a coating material surrounding the same, The coating material comprises a cellulose, mannitol, hydroxypropyl methyl cellulose, and poorly water-soluble pigment. The method of claim 1, Toothpaste composition comprising the beads in an amount of 0.01 to 5 parts by weight based on 100 parts by weight of the total composition. The method of claim 1, The poorly water-soluble pigments include blue No. 201 (D & C Blue No. 6), red No. 226 (D & C Red No. 30), red No. 202 (D & C Red No. 7), green No. 201 (D & C Green No. 5), green 202 (D & C Green No.6), Orange 201 (D & C Orange No.5), Orange 206 (D & C Orange No.10), Purple 201 (D & C Violet No.2), Yellow 201 (D & C Yellow No. .7) and at least one toothpaste composition selected from the group consisting of titanium oxides. The method of claim 1, The beads have an average particle diameter of 0.1 mm to 10 mm. The method of claim 1, The core particle has an average particle diameter of 0.01 mm to 1 mm. The method of claim 1, The beads may be from 0 to 10% by weight of more than 1.0 mm to 20 mm in diameter, from 50 to 100% by weight of more than 0.425 mm and less than 1.0 mm in diameter, and from 0 to 10 mm or more in diameter from 0.425 mm or less, based on the total weight of the beads. Toothpaste composition to be 50% by weight. The method of claim 1, The bead is a toothpaste composition having an average hardness of 100 g to 1,000 g measured using a compression tester. The method of claim 1, The coating material is based on 100 parts by weight of the total weight of the coating material a) 35 to 99.99 parts by weight of cellulose, b) 4 to 60 parts by weight of mannitol, c) 0.5 to 10 parts by weight of hydroxypropylmethylcellulose, and d) 0.01 to 2.5 parts by weight of poorly water-soluble pigments Toothpaste composition comprising a. The method of claim 1, Toothpaste composition further comprises a functional active ingredient or flavor component. The method of claim 1, The beads further comprise at least one functional active ingredient selected from the group consisting of tocopherol acetate, sodium chloride, tranexamic acid, aminocaproic acid, pyridoxine hydrochloride, tranexamic acid, triclosan, vitamin A, allantoin, and palmitic acid. Toothpaste composition comprising. The method of claim 1, The composition of the toothpaste composition further comprises at least one selected from the group consisting of abrasives, wetting agents, binders, foaming agents, flavoring agents, sweeteners, colorants, functional active ingredients.