Pump-Type Toothpaste Composition

Abstract

The present disclosure relates to a pump-type toothpaste composition capable of being provided as contained in a pumping type container, and to a pump-type toothpaste composition improving the spreading property to a tooth as the toothpaste composition discharged to a toothbrush penetrates into the toothbrush and having an effect of ultimately delivering a medicinal ingredient continuously for a long time in the oral cavity.

In addition, the present disclosure relates to a pump-type toothpaste composition with excellent commercial value, which can ensure discharge stability without hardening and accordingly, can be used in a pump-type container equipped with a dispenser pump (dip pump), which has a remarkable problem of hardening in the discharge port due to free movement of external air because of properties of the container, and thus can ensure even the convenient use.

Claims

1. A pump-type toothpaste composition contained in a pump-type container, comprising a non-ionic surfactant having an HLB value of 16 or less, wherein a viscosity of the pump-type toothpaste composition is from 5,000 cP to 40,000 cP when being measured with BrookField, RVT type No. 7 spindle or RV-5, under the conditions of 25 C., 20 rpm, and 5 cycle.

2. The pump-type toothpaste composition according to claim 1, wherein the non-ionic surfactant having an HLB value of 16 or less is one or more selected from the group consisting of glyceryl monostearate, polyoxyethylene monooleate, polyoxyethylene monostearate, potassium oleate, sodium oleate, sorbitan monolaurate, sorbitan monopalmitate, sorbitan monostearate, sorbitan tristearate, sorbitan monooleate, sorbitan trioleate, triethanolamine oleate, polyoxyethylene sorbitan monolaurate, polyoxyethylene sorbitan monopalmitate, polyoxyethylene sorbitan monostearate, polyoxyethylene sorbitan tristearate, polyoxyethylene sorbitan monooleate, polyoxyethylene sorbitan trioleate, and mixtures thereof.

3. The pump-type toothpaste composition according to claim 1, wherein the content of the non-ionic surfactant having an HLB value of 16 or less is 0.1 to 10% by weight based on the total weight of the composition.

4. The pump-type toothpaste composition according to claim 1, wherein the composition is in a suspended state in which a hydrophobic array is formed.

5. The pump-type toothpaste composition according to claim 1, wherein the content of an abrasive comprised in the composition is 40% by weight or less based on the total weight of the composition.

6. The pump-type toothpaste composition according to claim 1, wherein the pump of the pump-type container is a dip pump.

7. The pump-type toothpaste composition according to claim 1, wherein the toothpaste composition exhibits the compression strength of 5 g or less, when the compression strength is measured with a 0.4 to 2 cm probe after drying the toothpaste composition at 60 C. for 5 hours using a texture analyzer.

8. A pump-type toothpaste comprising the pump-type toothpaste composition according to claim 1, and a pump-type container in which the pump-type toothpaste composition is contained.

9. The pump-type toothpaste according to claim 8, wherein the pump-type toothpaste exhibits the discharge pressure of 3 kg or less, when the pump pressure is measured using a texture analyzer, after discharging toothpaste and then drying it at 60 C. for 6 hours, for the pump-type toothpaste.

10. The pump-type toothpaste composition according to claim 1, wherein the composition is in a gel form.

11. The pump-type toothpaste composition according to claim 1, wherein the composition further comprises 25% by weight or more of liquid polyol based on the total weight of the composition.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0104] The following drawings accompanied herein illustrate preferable examples of the present invention, and serve to further understand the technical idea of the present disclosure together with the aforementioned disclosure, and thus the present disclosure should not be construed as being limited to the matters described in such drawings.

[0105] The FIGURE is a graph showing the values of evaluating the bubble satisfaction and bubble texture satisfaction of the compositions (Example 7, Example 8, and Comparative example 1) prepared according to Preparative example 2 of the following II. Pump-type toothpaste composition.

MODE FOR INVENTION

[0106] Hereinafter, the present disclosure will be described with reference to the following examples and the like to describe the present disclosure in more detail. However, the examples according to the present disclosure can be modified into various other forms, and the scope of the present disclosure should not be construed as being limited to the examples described below. The examples of the present disclosure are provided illustratively in order to facilitate a specific understanding of the present invention.

I. Preparative Example 1 of Pump-Type Toothpaste Composition

[0107] The toothpaste compositions of Examples and Comparative example were prepared with ingredients and composition ratios shown in the following Table 1. Powder ingredients such as purified water, liquid polyol, flavoring, a pharmaceutical agent, a surfactant, a binder, saccharine were completely dispersed to mix primarily, and then an abrasive such as silica and the like and a pharmaceutical agent were added and mixed in a vacuum to prepare toothpaste compositions.

TABLE-US-00001 TABLE 1 Comparative Example Example Example Example Example example 1 2 3 4 5 1 Precipitated 15.00 15.00 15.00 15.00 15.00 15.00 silica Glycerin 50.00 50.00 50.00 50.00 50.00 50.00 Sodium lauryl 2.20 2.20 2.20 2.20 2.20 2.20 sulfate Sodium 0.20 0.20 0.20 0.20 0.20 0.20 saccharine Sodium 0.22 0.22 0.22 0.22 0.22 0.22 fluoride Vitamin E 0.20 0.20 0.20 0.20 0.20 0.20 Sodium 0.60 0.50 0.50 0.40 1.50 2.50 carboxy methyl cellulose Xanthan 0.20 gum Sodium polyacrylic 0.50 0.20 acid Sodium 0.50 0.20 alginate Flavoring 1.00 1.00 1.00 1.00 1.00 1.00 Purified 30.68 30.18 30.18 30.18 39.68 28.68 water

Experimental Example 1-1. Viscosity of Prepared Toothpaste (Measurement of Viscosity Using Brookfield Viscometer)

[0108] For the toothpaste prepared as Examples 1 to 5 and Comparative example 1 of Table 1, in order to measure the viscosity at a room temperature (25 C.), the viscosity values were measured by rotating at a rotation speed of 20 rotations per minute using spindle No. 7 with Brookfield viscometer RVT type.

TABLE-US-00002 TABLE 2 Comparative Example Example Example Example Example example 1 2 3 4 5 1 Viscosity 5.5 12 13 15 40 60 (1,000 cP)

[0109] Comparative example 1 showed the high viscosity, but on the other hand, Examples 1 to 5 showed a viscosity in a range of 5,500 to 40,000 cP.

Experimental Example 1-2. Degree of Penetrating into Toothbrush Bristles

[0110] For the toothpaste prepared as Examples 1 to 5 and Comparative example 1 of Table 1, the toothpaste compositions in a gel phase of Examples 1 to 5 were put in pump-type containers, and the toothpaste composition in a paste phase of Comparative example 1 was put in a tube, and they were discharged to a toothbrush having a hole interval (interval between a toothbrush bristle and a bristle) of 1.5 mm, and the toothpaste safely arrived on the bristles, and in 10 seconds, the penetration depth at which the toothpaste extended from the top to the bottom of the toothbrush bristles was measured, and the result was as the following Table 3.

TABLE-US-00003 TABLE 3 Comparative Example Example Example Example Example example 1 2 3 4 5 1 Penetrating 2 1 1 1 1 No depth penetrating (mm)

[0111] It could be seen that the paste toothpaste according to Comparative example 1 did not penetrate into the bristles, while Examples 1 to 5 penetrated into the bristles in a depth of 1-2 mm in the spaces among the bristles.

[0112] In addition, for the toothpaste prepared as Examples 1 to 5 and Comparative example 1 of Table 1, the toothpaste compositions in a gel phase of Examples 1 to 5 were put in pump-type containers, and the toothpaste composition in a paste phase of Comparative example 1 was put in a tube, and they were discharged to a toothbrush having a hole interval (interval between a toothbrush bristle and a bristle) of 2 mm, and the toothpaste safely arrived on the toothbrush bristles, and in 10 seconds, the penetration depth was measured, and the result was as the following Table 4.

TABLE-US-00004 TABLE 4 Comparative Example Example Example Example Example example 1 2 3 4 5 1 Penetrating 4 3 2 5 1.5 No depth penetrating (mm)

[0113] It could be seen that the paste toothpaste according to Comparative example 1 did not penetrate into the bristles, while Examples 1 to 5 penetrated into the bristles in a depth of 1.5-5 mm in the spaces among the bristles.

[0114] As could be seen by the results of Table 3 and Table 4, as a toothbrush having a large hole interval was used, the difference in penetration into the toothbrush bristles between Comparative example and Examples were remarkably shown.

[0115] As could be seen by the results of Table 3 and Table 4, it could be seen that the toothpaste according to Examples 1-5 penetrated into the toothbrush bristles well when contained in a pump-type container and discharged to a toothbrush, and thus it had an effect of delivering a medicinal ingredient to the oral cavity continuously during brushing, compared to Comparative example 1.

II. Preparative Example 2 of Pump-Type Toothpaste Composition

[0116] The toothpaste compositions of Examples and Comparative examples were prepared with ingredients and composition ratios shown in the following Table 5. Powder ingredients such as purified water, liquid polyol, flavoring, a pharmaceutical agent, a surfactant, a binder, saccharine were completely dispersed to mix primarily, and then an abrasive such as silica and the like and a pharmaceutical agent were added and mixed in a vacuum to prepare toothpaste compositions.

TABLE-US-00005 TABLE 5 Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- ple ple ple ple ple ple ple ple ple ple ple ple ple ple 1 2 3 4 5 6 7 8 9 10 11 12 13 14 Precipitated 15 15 15 15 15 15 15 15 15 15 15 15 15 15 silica Glycerin 50 50 50 50 50 50 50 50 50 50 50 50 50 50 Sodium 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2 lauryl sulfate Sodium 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 saccharine Sodium 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 fluoride Vitamin E 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 PVM/MA 1 1 0.1 0.5 2 PVP 1 1 0.1 0.5 2 HPMC 1 1 0.1 0.5 HPC Sodium 0.5 0.8 0.5 0.5 0.5 0.8 0.5 0.5 0.5 0.8 0.5 carboxy methyl cellulose Xanthan 0.5 0.5 0.5 gum Flavoring 1 1 1 1 1 1 1 1 1 1 1 1 1 1 Purified 29.68 29.68 30.28 30.18 28.68 29.68 29.68 30.28 30.18 28.68 29.68 29.68 30.28 30.18 water Example Example Example Example Example Example Example 15 16 17 18 19 20 21 Precipitated 15 15 15 15 15 15 15 silica Glycerin 50 50 50 50 50 50 50 Sodium 2.2 2.2 2.2 2.2 2.2 2.2 2.2 lauryl sulfate Sodium 0.2 0.2 0.2 0.2 0.2 0.2 0.2 saccharine Sodium 0.22 0.22 0.22 0.22 0.22 0.22 0.22 fluoride Vitamin E 0.2 0.2 0.2 0.2 0.2 0.2 0.2 PVM/MA 1 PVP HPMC 2 HPC 1 1 0.1 0.5 2 Sodium 0.5 0.5 0.8 0.5 0.5 carboxy methyl cellulose Xanthan 0.5 gum Flavoring 1 1 1 1 1 1 Purified 28.68 29.68 29.68 30.28 30.18 28.68 31.18 water Compar- Compar- Compar- Compar- ative ative ative ative Example Example Example example example example example 22 23 24 1 2 3 4 Precipitated 15 15 15 15 15 15 15 silica Glycerin 50 50 50 50 50 50 50 Sodium 2.2 2.2 2.2 2.2 2.2 2.2 2.2 lauryl sulfate Sodium 0.2 0.2 0.2 0.2 0.2 0.2 0.2 saccharine Sodium 0.22 0.22 0.22 0.22 0.22 0.22 0.22 fluoride Vitamin E 0.2 0.2 0.2 0.2 0.2 0.2 0.2 PVM/MA PVP 1 HPMC 1 HPC 1 Sodium 1 0.5 carboxy methyl cellulose Xanthan 1 0.5 3 gum Flavoring 1 1 1 1 Purified 31.18 31.18 31.18 30.18 30.18 30.18 28.18 water

Experimental Example 2-1. Viscosity of Prepared Toothpaste (Measurement of Viscosity Using Brookfield Viscometer)

[0117] For the toothpaste prepared as Examples 1 to 24 and Comparative examples 1 to 4 of Table 5, in order to measure the viscosity at a room temperature (25 C.), the viscosity values were measured by rotating at a rotation speed of 20 rotations per minute using spindle No. 7 with Brookfield viscometer RVT type, and the result was as the following Table 6.

TABLE-US-00006 TABLE 6 Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- ple ple ple ple ple ple ple ple ple ple ple ple ple ple 1 2 3 4 5 6 7 8 9 10 11 12 13 14 Viscosity 20 15 15 12 28 16 11 11 8 24 17 12 12 9 (1,000 cP) Com- Com- Com- Com- parative parative parative parative Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- ple ple ple ple ple ple ple ple ple ple ple ple ple ple 15 16 17 18 19 20 21 22 23 24 1 2 3 4 Viscosity 25 23 18 18 15 30 10 5 6 12 20 18 15 50 (1,000 cP)

[0118] Comparative examples 1 to 4 and Examples 1 to 24 showed the viscosity in a range of 40,000 cP or less all.

Experimental Example 2-2. Degree of Penetrating into Toothbrush Bristles

[0119] The toothpaste prepared as Examples 1 to 24 and Comparative examples 1 to 4 of Table 5 were put in pump-type containers, and they were discharged to a toothbrush having a hole interval (interval between a toothbrush bristle and a bristle) of 11.5 mm, and the toothpaste safely arrived on the toothbrush bristle, and in 10 seconds, the penetration depth at which the toothpaste extended from the top to the bottom of the toothbrush bristle was measured, and the result was as the following Table 7.

TABLE-US-00007 TABLE 7 Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- ple ple ple ple ple ple ple ple ple ple ple ple ple ple 1 2 3 4 5 6 7 8 9 10 11 12 13 14 Penetrating 4 4 4 4 1.5 4.5 4.5 4.5 4.5 2 2.5 3.5 3.5 4.5 depth (mm) Com- Com- Com- Com- parative parative parative parative Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- ple ple ple ple ple ple ple ple ple ple ple ple ple ple 15 16 17 18 19 20 21 22 23 24 1 2 3 4 Pene- 2 2 2.5 2.5 3 1.5 4.5 5 5 3.5 1 1 1 No trating pene- depth trating (mm)

[0120] The paste toothpaste according to Comparative examples 1-4 showed an appropriate viscosity, but the penetrating depth was significantly decreased, compared to Examples 1 to 24. Through this, it was expected that Comparative examples 1 to 4 had a high elastic modulus.

Experimental Example 2-3. Tan (Loss Modulus (G)/Elastic Modulus (G)

[0121] The amplitude sweep oscillation test was conducted using Paar Physica rheology measuring instrument, and the elastic modulus and viscosity coefficient were read when the shear stress was 1, and Tan values for them were obtained.

TABLE-US-00008 TABLE 8 Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- ple ple ple ple ple ple ple ple ple ple ple ple ple ple 1 2 3 4 5 6 7 8 9 10 11 12 13 14 Tan 0.5 0.5 0.5 0.5 0.8 0.55 0.55 0.55 0.55 0.85 0.4 0.45 0.45 0.55 Com- Com- Com- Com- parative parative parative parative Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- ple ple ple ple ple ple ple ple ple ple ple ple ple ple 15 16 17 18 19 20 21 22 23 24 1 2 3 4 Tan 0.85 0.75 0.75 0.75 0.45 0.65 0.55 0.9 0.9 0.65 0.25 0.35 0.3 0.01

[0122] Although the larger the value of Tan , the higher the viscosity of the toothpaste by using a polymer having a high viscosity coefficient, it means that a structure with flowability can be produced. According to the Table 8, it can be seen that Examples have higher values of Tan , compared to Comparative examples.

Experimental Example 2-4. Measurement of Rich Feeling

[0123] After using the toothpaste according to Examples 7 and 8 and Comparative example 1 for the evaluation group, the evaluation questionnaire was progressed about the attribute that was the evaluation scale of rich feeling during brushing. The questionnaire was progressed on a 5-point scale, and it was evaluated as 1-point was low in texture and 5-point was high.

[0124] As a result, as shown in the FIGURE, it was confirmed that the bubble texture and satisfaction of bubbles in case of using Examples were higher than Comparative example.

III. Preparative Example 3 of Pump-Type Toothpaste Composition

[0125] The toothpaste compositions of Examples and Comparative examples were prepared with ingredients and composition ratios shown in the following Table 9. Purified water, liquid polyol, flavoring, a pharmaceutical agent, xanthan gum, saccharine, a preservative, and powder ingredients such as a surfactant were completely dispersed to mix primarily, and then an abrasive such as silica and the like and a pharmaceutical agent were added and mixed in a vacuum to prepare toothpaste compositions.

TABLE-US-00009 TABLE 9 Comparative Comparative Comparative Example Example Example Example Example Example example example example 1 2 3 4 5 6 1 2 3 Precipitated 10.00 20.00 30.00 40.00 10.00 20.00 30.00 silica Calcium 20.00 carbonate Calcium 20.00 hydrogen phosphate Glycerin 80.00 70.00 60.00 50.00 70.00 70.00 45.00 45.00 45.00 Sodium 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 2.00 lauryl sulfate Sodium 0.20 0.20 0.20 0.20 0.20 0.20 0.20 0.20 0.20 saccharine Xanthan 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 gum Sodium 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 fluoride Vitamin E 0.20 0.20 0.20 0.20 0.20 0.20 0.20 0.20 0.20 Flavoring 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 Purified 5.38 5.38 5.38 5.38 5.38 5.38 40.38 30.38 20.38 water

Experimental Example 3-1. Time to Harden after Discharging Pump-Type Toothpaste

[0126] The toothpaste compositions prepared as Examples and Comparative examples of Table 9 were filled to a 24 well plate, and then were dried in a dry oven equipped with a fan at 60 C. for 48 hours. Then, the degree of hardening when applying pressure to the toothpaste using a probe-rod (round-shaped pen) was determined to evaluate the degree of hardening of the toothpaste.

[0127] For the degree of hardening, it was marked as hardened when contents were hardened to the extent that they were not scratched, and it was marked as not hardened when contents were scratched or the probe-rod was inserted into the contents. The result was described in Table 10.

TABLE-US-00010 TABLE 10 Comparative Comparative Comparative Example Example Example Example Example Example example example example 1 2 3 4 5 6 1 2 3 Degree Not Not Not Not Not Not Hardened Hardened Hardened of hardened hardened hardened hardened hardened hardened hardening

[0128] As could be seen from the result, Comparative examples 1 to 3 were shown as hardened all, while Examples 1 to 6 were shown as not hardened.

Experimental Example 3-2. Compression Strength Test

[0129] The toothpaste compositions prepared as Examples and Comparative examples of Table 9 were filled in a 24 well plate and were dried at 60 C. for 48 hours, and then the compression strength of the toothpaste was measured with a 0.4-2 cm probe, using a texture analyzer. It was confirmed that one showing 5 g or less in the measurement was not hardened, and it was confirmed that the compression strength increased due to hardening of the surface in case of receiving a force of 5 g or more. The result was described in Table 11.

TABLE-US-00011 TABLE 11 Comparative Comparative Comparative Example Example Example Example Example Example example example example 1 2 3 4 5 6 1 2 3 Compression 5 g or 5 g or 5 g or 5 g or 5 g or 5 g or 9 g 15 g 50 g strength less less less less less less

[0130] As could be seen from the result, Examples 1 to 6 showed the compression strength of 5 g or less all, while Comparative examples 1 to 3 showed the compression strength of 5 g or more and therefore it was shown that their surfaces were hardened.

Experimental Example 3-3. Test for Observing Hardening of Pump Inlet

[0131] The toothpaste compositions prepared as Examples and Comparative examples of Table 9 were put in a pump-type container, and after the contents of this pump-type toothpaste was discharged, the pump was dried at 60 C. for 6 hours. Then, the pump pressure was measured using a texture analyzer. The result was described in Table 12.

TABLE-US-00012 TABLE 12 Comparative Comparative Comparative Example Example Example Example Example Example Example example example example 1 2 3 4 5 6 7 1 2 3 Compression 2.6 kg 2.6 kg 2.6 kg 2.6 kg 2.6 kg 2.6 kg 2.6 kg 3.2 kg 3.7 kg Impossible strength to discharge

[0132] As a result, Examples 1 to 6 showed the discharge pressure of 3 kg or less all, while Comparative examples 1 to 3 showed the discharge pressure of 3 kg or more, and therefore it could be seen that their inlets were hardened and thereby the discharge pressure increased.

IV. Preparative Example 4 of Pump-Type Toothpaste Composition

[0133] The toothpaste compositions of Examples and Comparative examples were prepared with ingredients and composition ratios shown in the following Table 13. Purified water, liquid polyol, flavoring, a pharmaceutical agent, xanthan gum, saccharine, a preservative, powder ingredients such as a surfactant (HCO40, HLB 12.5; TWEEN 60, HLB 14.9; and SPAN 80, HLB 4.3) were completely dispersed to mix primarily, and then an abrasive such as silica and the like and a pharmaceutical agent were added and mixed in a vacuum to prepare toothpaste compositions.

TABLE-US-00013 TABLE 13 Com- Com- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- parative parative ple ple ple ple ple ple ple ple ple ple ple ple example example 1 2 3 4 5 6 7 8 9 10 11 12 1 2 Precip- 15 15 15 15 15 15 15 15 15 15 15 15 15 15 itated silica Glycerin 40 40 40 40 40 40 40 40 40 40 40 40 40 40 Sodium 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2 2.2 lauryl sulfate Sodium 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 saccharine Xanthan 1 1 1 1 1 1 1 1 1 1 1 1 1 1 gum Sodium 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 fluoride Vitamin E 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 HCO 40 0.05 0.2 0.5 1 5 10 0.5 0.1 0.5 20 TWEEN 1 0.5 0.5 0.1 0.5 60 SPAN 80 1 0.5 0.1 0.5 Flavoring 1 1 1 1 1 1 1 1 1 1 1 1 1 1 Purified 40.13 39.98 39.68 39.18 35.18 30.18 39.18 39.18 39.18 39.18 39.88 38.68 40.18 20.18 water

Experimental Example 4-1. Phase Stability

[0134] Comparative example 2 comprising an excessive amount of surfactant did not maintain the phase of toothpaste and was modified. Thus, the evaluation itself was impossible in subsequent experiments.

Experimental Example 4-2. Time to Harden after Discharging Pump-Type Toothpaste

[0135] The toothpaste compositions prepared as Examples and Comparative examples of Table 13 were filled to a 24 well plate, and then were dried in a dry oven equipped with a fan at 60 C. for 48 hours. Then, the degree of hardening when applying pressure to the toothpaste using a probe-rod (round-shaped pen) was determined to evaluate the degree of hardening of the toothpaste.

[0136] For the degree of hardening, it was marked as hardened when contents were hardened to the extent that they were not scratched, and it was marked as not hardened when contents were scratched or the probe-rod was inserted into the contents. The result was described in Table 14.

TABLE-US-00014 TABLE 14 Example Example Example Example Example Example Example Example 1 2 3 4 5 6 7 8 Evaluation Not Not Not Not Not Not Not Not result hardened hardened hardened hardened hardened hardened hardened hardened Comparative Comparative Example Example Example Example example example 9 10 11 12 1 2 Evaluation Not Not Not Not Hardened Not result hardened hardened hardened hardened measurable

[0137] As could be seen from the result, Comparative example 1 was shown as hardened, while Examples 1 to 12 were shown as not hardened.

Experimental Example 4-3. Compression Strength TEST

[0138] The toothpaste compositions prepared as Examples and Comparative examples of Table 13 were filled in a 24 well plate and were dried at 60 C. for 48 hours, and then the compression strength of the toothpaste was measured with a 0.4-2 cm probe, using a texture analyzer. It was confirmed that one showing 5 g or less in the measurement was not hardened, and it was confirmed that the compression strength increased due to hardening of the surface in case of receiving a force of 5 g or more. The result was described in Table 15.

TABLE-US-00015 TABLE 15 Com- Com- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- parative parative ple ple ple ple ple ple ple ple ple ple ple ple example example 1 2 3 4 5 6 7 8 9 10 11 12 1 2 Evalu- 5 g 5 g 5 g 5 g 5 g 5 g 5 g 5 g 5 g 5 g 5 g 5 g 7 g Not ation or or or or or or or or or or or or measurable result less less less less less less less less less less less less

[0139] As could be seen from the result, Examples 1 to 12 showed the compression strength of 5 g or less all, while Comparative example 1 showed the compression strength of 5 g or more and therefore it was shown that its surface was hardened.

Experimental Example 4-4. Test for Observing Hardening of Pump Inlet

[0140] The toothpaste compositions prepared as Examples and Comparative examples of Table 13 were put in a pump-type container, and after the contents of this pump-type toothpaste was discharged, the pump was dried at 60 C. for 6 hours. Then, the pump pressure was measured using a texture analyzer. The result was described in Table 16.

TABLE-US-00016 TABLE 16 Com- Com- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- parative parative ple ple ple ple ple ple ple ple ple ple ple ple example example 1 2 3 4 5 6 7 8 9 10 11 12 1 2 Evaluation 2.9 2.8 2.7 2.6 2.5 2.4 2.5 2.5 2.5 2.5 2.6 2.5 3.2 Not result kg kg kg kg kg kg kg kg kg kg kg kg kg meaurable

[0141] As a result, Examples 1 to 12 showed the discharge pressure of 3 kg or less all, while Comparative example 1 showed the discharge pressure of 3 kg or more, and therefore it could be seen that its inlet was hardened and thereby the discharge pressure increased.

V. Preparative Example 5 of Pump-Type Toothpaste Composition

[0142] The toothpaste compositions of Examples and Comparative examples were prepared with ingredients and composition ratios shown in the following Table 17. Purified water, liquid polyol, flavoring, a pharmaceutical agent, xanthan gum, saccharine, a preservative, powder ingredients such as a surfactant were completely dispersed to mix primarily, and then an abrasive such as silica and the like and a pharmaceutical agent were added and mixed in a vacuum to prepare toothpaste compositions.

TABLE-US-00017 TABLE 17 Comparative Comparative Comparative Example Example Example Example Example Example Example example example example 1 2 3 4 5 6 7 1 2 3 Precipitated 15.00 15.00 15.00 15.00 15.00 15.00 15.00 15.00 15.00 15.00 silica Glycerin 45.00 45.00 45.00 45.00 45.00 45.00 45.00 45.00 45.00 45.00 Sodium 1.00 1.00 2.00 2.00 2.00 2.00 2.00 2.00 lauryl sulfate Organic 0.50 1.00 1.00 2.00 5.00 10.00 20.00 30.00 oil Sodium 0.20 0.20 0.20 0.20 0.20 0.20 0.20 0.20 0.20 0.20 saccharine Xanthan 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 gum Sodium 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 fluoride Vitamin 0.20 0.20 0.20 0.20 0.20 0.20 0.20 0.20 0.20 0.20 E Flavoring 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 0.50 Purified 36.38 35.88 34.88 33.88 31.10 26.10 15.83 37.88 35.88 7.88 water

Experimental Example 5-1. Phase Stability

[0143] Comparative example 3 comprising an excessive amount of oil only without a surfactant had a problem in stability. Thus, the evaluation itself was impossible in subsequent experiments.

Experimental Example 5-2. Time to Harden after Discharging Pump-Type Toothpaste

[0144] The toothpaste compositions prepared as Examples and Comparative examples of Table 17 were filled to a 24 well plate, and then were dried in a dry oven equipped with a fan at 60 C. for 48 hours. Then, the degree of hardening when applying pressure to the toothpaste using a probe-rod (round-shaped pen) was determined to evaluate the degree of hardening of the toothpaste.

[0145] For the degree of hardening, it was marked as hardened when contents were hardened to the extent that they were not scratched, and it was marked as not hardened when contents were scratched or the probe-rod was inserted into the contents. The result was described in Table 18.

TABLE-US-00018 TABLE 18 Comparative Comparative Comparative Example Example Example Example Example Example Example example example example 1 2 3 4 5 6 7 1 2 3 Degree Not Not Not Not Not Not Not Hardened Hardened Not of hardened hardened hardened hardened hardened hardened hardened hardened hardening

[0146] As could be seen from the result, Comparative examples 1 and 2 were shown as hardened, while Examples 1 to 7 were shown as not hardened.

Experimental Example 5-3. Compression Strength TEST

[0147] The toothpaste compositions prepared as Examples and Comparative examples of Table 17 were filled in a 24 well plate and were dried at 60 C. for 48 hours, and then the compression strength of the toothpaste was measured with a 0.4-2 cm probe, using a texture analyzer. It was confirmed that one showing 5 g or less in the measurement was not hardened, and it was confirmed that the compression strength increased due to hardening of the surface in case of receiving a force of 5 g or more. The result was described in Table 19.

TABLE-US-00019 TABLE 19 Comparative Comparative Comparative Example Example Example Example Example Example Example example example example 1 2 3 4 5 6 7 1 2 3 Compression 5 g or 5 g or 5 g or 5 g or 5 g or 5 g or 5 g or 9 g 7 g Not strength less less less less less less less measurable (Liquid separation)

[0148] As could be seen from the result, Examples 1 to 7 showed the compression strength of 5 g or less all, while Comparative examples 1 and 2 showed the compression strength of 5 g or more and therefore it was shown that their surfaces were hardened.

Experimental Example 5-4. Test for Observing Hardening of Pump Inlet

[0149] The toothpaste compositions prepared as Examples and Comparative examples of Table 17 were put in a pump-type container, and after the contents of this pump-type toothpaste was discharged, the pump was dried at 60 C. for 6 hours. Then, the pump pressure was measured using a texture analyzer. The result was described in Table 20.

TABLE-US-00020 TABLE 20 Comparative Comparative Comparative Example Example Example Example Example Example Example example example example 1 2 3 4 5 6 7 1 2 3 Compression 2.9 kg 2.8 kg 2.6 kg 2.6 kg 2.6 kg 2.6 kg 2.6 kg 3.2 kg 3.3 kg Not strength measurable (Liquid separation)

[0150] As a result, it could be seen that all Examples 1 to 7 showed the discharge pressure of 3 kg or less, while Comparative examples 1 and 2 showed the discharge pressure of 3 kg or more, and therefore the inlet was hardened and thereby the discharge pressure increased.