WO2020054996A1 - Foamable mouthwash solid formulation and preparation method therefor - Google Patents

Abstract

The present invention relates to a foamable mouthwash solid formulation and, more specifically, to a foamable mouthwash solid formulation, which: comprises a mixture of a grape extract, a green tea extract, a baikal skullcap extract, and a balloon flower extract as an active ingredient; exhibits an excellent effect on dentin remineralization and dentinal tubule occlusion; melts to generate bubbles when put into the mouth, thus not necessitating additional tooth-brushing; is excellent in a cleaning effect; and has anti-inflammatory, antibacterial, dental caries-preventing, halitosis-eliminating, and scaling effects.

Description

Effervescent solid agent for mouthwash and manufacturing method thereof

The present invention relates to a foamable solid agent for mouthwash, and more particularly, to a foamable solid agent for mouthwash comprising a mixture of grape extract, green tea extract, golden extract and bellflower extract as an active ingredient.

Toothpaste, also known as a dentifrice, is a detergent used in combination with a toothbrush to clean the tooth surface in the mouth when brushing, and is a quasi-drug. The primary purpose of toothpaste use is to effectively remove bacterial plaque attached to the tooth surface, and has been expanded for additional purposes such as dental caries, periodontal disease prevention, whitening effect, slowing perception, and bad breath suppression.

The main components of toothpaste include abrasives, water, moisturizers, detergents, binders, flavoring agents, sweeteners, prophylactic treatments, pigments and preservatives. Among them, antibacterial, antibacterial, neutralizing, and anti-enzymatic pharmacology As an effect, active ingredients such as drugs or chemicals that suppress dental caries and prevent periodontal disease are selectively added.

In general, toothpaste is composed of a paste, powder, gel, mucus, and liquid. Among them, the paste phase is the most widely distributed, but it is highly likely to cause damage to the tooth enamel layer by the abrasive component, and it is inconvenient to squeeze when used, and the remaining amount in a container that is discarded There is a problem that the toothpaste remains. In addition, the powdery phase has the disadvantage that it is inconvenient to use because the particles are sprayed or scattered during use, and the gel phase has low spreadability due to high viscosity and is not easily dispersed in the oral cavity. In addition, the liquid phase flows easily due to its low viscosity, and it is difficult to expect a sufficient cleaning effect due to lack of cleaning ingredients.

Accordingly, recently, various formulations of detergents have been developed for specific prescriptions for specific uses and targets, and techniques for re-mixing various components commonly used have been developed. For example, Korean Patent Publication No. 10-2012-0079537 discloses a sheet-type toothpaste, Korean Patent Publication No. 10-2015-0051296 discloses a foam-type toothpaste disclosed in Korean Patent Publication No. 10-2004-0008953. There is disclosed a pill form toothpaste. However, the developed toothpaste can stimulate consumer curiosity beyond the formulation of a general detergent, but there is a problem in that the conventional toothpaste simply deforms the formulation or has a poor cleaning effect, and still needs brushing. . Therefore, there is a need to develop a detergent that is convenient to use and has improved efficacy.

On the other hand, resveratrol, which is known as a natural extract that is harmless and safe to the human body, is a kind of polyphenols contained in plants of peanuts and grape extracts, and emits for self-defense when plants are exposed to external stresses such as ultraviolet rays and pathogens. It is one of the phytoalexin compounds (biological defense materials). Catechin, also known as green tea extract, belongs to flavan-3-ols of the flavonoid group and is a type of polyphenol. It is known to have anti-carcinogenic, arteriosclerotic, antiviral, anti-obesity, anti-diabetic, antibacterial, detoxifying, and anti-inflammatory effects, and particularly has dental caries prevention and bad breath prevention effects. Baikalin (baicalin) is one of the flavonoids contained in Lamiaceae and roots, and has efficacy such as anti-inflammatory and antioxidant, and is used in various forms in vivo.

Therefore, in the present invention, a foamable solid agent for mouthwash was developed that excludes harmful synthetic chemicals and contains only natural products as an active ingredient.

For reference, KR 10-1448283 B1, KR 10-2005-0086796 A, and KR 10-1056573 B1 were used as prior art documents.

In order to solve the above problems, the present invention includes a mixture of grape extract, green tea extract, golden extract and bellflower extract as an active ingredient, does not require tooth brushing, removes bad breath, gingivitis and effervescent foam for oral cleaning with anti-microbial efficacy The purpose is to provide siblings.

The present invention to achieve the above object,

In the foamable solid agent for mouthwash, there is provided a foamable solid agent for mouthwash comprising a mixture of grape extract, green tea extract, golden extract and bellflower extract as an active ingredient.

The grape extract contains resveratrol as an active ingredient, the green tea extract contains catechin as an active ingredient, the golden extract contains Baikalin as an active ingredient, and the bellflower extract is characterized by a long path.

The foamable solid agent for mouthwash includes sodium hydrogen carbonate as a foaming agent, and is characterized by further comprising a surfactant, a pH adjusting agent, a formulation agent, an abrasive, a disintegrant, a lubricant, a sweetener, and a fragrance.

The grape extract, the green tea extract, the golden extract and the bellflower extract is made of 1: 7: 2: 4 by weight, the blowing agent is characterized in that it comprises 20 parts by weight based on 100 parts by weight of the total composition.

The formulation agent is crystalline cellulose, the abrasive is calcium carbonate, the disintegrant is lactose and starch, the lubricant is magnesium stearate, the pH adjusting agent is DL-apple acid, and the surfactant is L-Lysin and olive oil It is characterized by.

The foamable solid agent for oral cleaning is foamed within 30 seconds after oral injection, and is characterized by having dentin remineralization and dentinal tubule closure.

In addition, in another aspect, the present invention, a step of mixing a mixture consisting of grape extract, green tea extract, golden extract and bellflower extract, surfactant, pH adjusting agent, formulation agent, abrasive, disintegrant, lubricant, sweetener and flavoring agent; Two steps of aging the mixture; 3 steps of tableting the aged mixture; Four steps of aging the tableted mixture; 5 steps of coating the aged mixture; 6 steps for drying the coated mixture; provides a method for preparing a foamable solid for mouthwash comprising a.

More specifically, the mixture of the grape extract, green tea extract, golden extract, and bellflower extract in step 1, and a surfactant, a pH adjusting agent, a formulation agent, an abrasive, a disintegrant, a lubricant, a sweetener and a fragrance, at a temperature of 22 ° C. or less and humidity It is preferable to mix for 15 minutes at a speed of 30 rpm or less under conditions of 40% or less, and the mixture is aged for 8 hours in a sealed state at a temperature of 25 ° C or less and a humidity of 60% or less. In addition, in the step 3, the aged mixture is preferably compressed to a pressure of 2,000 kg / cm 2 and a speed of 30 rpm under conditions of a temperature of 20 ° C. or less and a humidity of 40% or less, and the compressed mixture is temperature 25 ° C. or less and humidity 60 It is preferable to aged for 8 hours in a sealed state under a condition of% or less. The aged mixture was first coated at 1.5 rpm for 90 minutes and 2.5 rpm for 60 minutes under heat exchanger pressure of 0.2 Mpsi, air compressor pressure of 4 to 6 bar, and gun injection pressure of 5 bar, followed by 3.5 rpm for 60 minutes and 4.5. It is preferable to undergo a step of secondary coating for 30 minutes at rpm. It is preferable to dry the coated mixture for 8 hours in a sealed state at a temperature of 25 ° C. or less and a humidity of 60% or less.

The effervescent solid agent for oral cleaning according to the present invention is a new solid agent type, which is convenient to carry, and can be conveniently and easily administered to the mouth without water or a toothbrush when going out at home and regardless of the place. In addition, the abundant foam quickly penetrates to clean every corner, and the tooth protection and cleaning effect is faster than that of the prior art. Accordingly, it is effective for people with weak teeth and weak teeth or gums, and no residue remains after brushing. In addition, it has excellent dentin remineralization and ivory tubule closing effect, has anti-inflammatory and antibacterial functions in the oral cavity, and prevents tooth decay, bad breath removal, and scaling.

1 is a graph of changes in the gingival gingival index attached to the nipple margins.

2 is a graph of Talbott's gingivitis index change.

Figure 3 is a graph of the change in the surface area management ability index.

4 is a graph of changes in the rating criteria of the dental hygiene membrane.

5 is a halitosis change graph measured by a halitometer.

6 is a graph of sensory evaluation changes.

7 is an SEM image of remineralization of dentin artificial caries lesions.

8 is an SEM image of the artificial ivory tubule closing effect.

9 is a graph for testing the effect of removing bad breath according to the concentration of hydrogen sulfide.

10 is a graph for testing the effect of removing bad breath according to the concentration of methyl mercaptan.

Hereinafter, the foamable solid agent for oral cleaning of the present invention will be described in more detail.

The effervescent solid for oral cleaning of the present invention includes a mixture of grape extract, green tea extract, golden extract and bellflower extract as an active ingredient, the grape extract is resveratrol, the green tea extract is catechin, and the golden extract is Baikal It contains lean as an active ingredient, the bellflower extract is preferably long.

The resveratrol is a polyphenol-based material found in more than 70 species of plants such as peanuts, grapes, pine trees, and red wine, and exists in two forms, cis-resveratrol and trans-resveratrol, as shown in the structure shown below. In the 1970s, resveratrol was found to act as a phytoalexin, an antibiotic produced by plants to fight bacteria and fungi, and the anticancer effect of lasveratrol was reported in 1997. In 2003, it was announced that yeast activates the long-lived gene SIRT1. In addition, by Dr. Louis Doely of Imperial Real University in London, UK, resveratrol has been shown to be effective in treating asthma, chronic obstructive pulmonary disease (COPD) and arthritis due to its wide range of anti-inflammatory effects. According to it, resveratrol has several tens and hundreds of times more antioxidants than vitamins and minerals, and it can be used to help prevent and treat gum disease by Dr. Patiachandard of the University of Quebec-Siraval, Canada. As described above, resveratrol is effective in preventing and treating oral diseases as physiological activity effects such as anti-inflammatory, antioxidant, and gum disease prevention are reported.

The catechin is a type of polyphenol contained in green tea, and main catechins include EGCG (epigallocatechin gallate), EGC (epigallocatechin), ECG (epicatechin gallate), and EC (epicatechin). EGCG, which accounts for 40% of total polyphenols, is known to have the strongest physiological activity. Catechins have been reported to have excellent bactericidal effects against oral bacteria (The Korean Journal of Microbiology, Vol. 40, No. 4, 2004: 364-366), and antioxidant and antibacterial activity effects of catechins extracted from tea have been published ( Horticulture Environment and Biotechnology, Vol. 10, 2007: 114-114). In addition, it has been reported to suppress the activity of the causative agent causing plaque, contribute to the prevention of alveolar bone loss through the antioxidant effect and the healing of damaged gums, and has various physiological and pharmacological effects such as anti-cancer, bad breath removal, and tooth discoloration prevention. The structure of the catechin is shown below.

The baicalin is a type of flavonoids contained in the roots of Lamiaceae and Golden (Scutellaria baicalensis Georgi), and the reported major physiological activity is antibacterial and anti-inflammatory activity, and in addition, it has effects on antiviral, antioxidant, and anticancer effects. It was reported to indicate. As an example, it has been reported that the golden extract has antibacterial activity and anti-adhesion effect against Streptococcus mutans, the causative agent of dental caries (Journal of Dental Hygiene Science, Vol. 8, No. 4, 2008: 367-373), and accordingly Lean's bioactive effect can be used for periodontal disease prevention and oral care.

The Gilty (Platycodonis Radix) is an excellent alkaline food with various active ingredients such as proteins, sugars, lipids, minerals, vitamins and saponins, including abundant fiber, iron, and calcium. Gilkyung contains triterpenoid saponin and phytosterol components. Triterpenoid saponin has anti-inflammatory effect. In oriental medicine, it acts on the lungs to treat many symptoms of seawater and phlegm and uncomfortable breathing. It is used for sore throat, cough due to cold, phlegm, nasal congestion, asthma, bronchitis, pleurisy, headache, chills, tonsillitis. In addition, pharmacological action was reported as expectorant action, hypoglycemic action, cholesterol lowering action, and improved bacteriostatic action.

The grape extract, the green tea extract, the golden extract and the bellflower extract is preferably made of 1: 7: 2: 4 by weight.

The foamable solid agent for mouthwash preferably contains sodium hydrogen carbonate as the foaming agent for foaming, and the foaming agent preferably contains 20 parts by weight based on 100 parts by weight of the total composition. The sodium hydrogen carbonate has a soft abrasive power, has an excellent inhibitory effect on bacteria in the oral cavity, and has a tooth decay prevention effect by neutralizing the organic acid produced by plaque.

In addition, it is preferable that the solid agent further includes a surfactant, a pH adjusting agent, a formulation agent, an abrasive, a disintegrant, a lubricant, a sweetener, and a fragrance.

The surfactant is preferably L-Lysin and olive oil, and the pH adjusting agent is preferably DL-apple acid.

It is preferable that the formulation agent contains crystalline cellulose as a role for bonding foaming agents, abrasives, and the like, and is added for production into a solid.

The abrasive preferably contains calcium carbonate, and plays an important role in cleaning such as removal of plaque and food, and should not damage the enamel of teeth, and compatibility with other ingredients should be secured.

It is preferred that the disintegrant comprises lactose and starch.

The lubricant is added to prevent foreign substances from being caught in the punch of the tableting machine during the tableting process, and preferably contains magnesium stearate.

The sweetener is added to overcome the basic taste of the solid agent, and may be L-menthol, D-sorbitol, xylitol, or enzymatically treated stevia.

The fragrance is added to reinforce, modify or suppress the fragrance.

The solid agent foams within 30 seconds after oral administration, and has dentin remineralization and dentinal tubule closure.

In addition, the present invention, in another aspect, a mixture of a grape extract, green tea extract, golden extract and bellflower extract, surfactant, pH adjusting agent, formulation agent, abrasive, disintegrating agent, lubricant, sweetener and fragrance at a temperature of 22 ° C. or less and humidity Mixing for 15 minutes at a speed of 30 rpm or less at a condition of 40% or less; Aging the mixture in a sealed state at a temperature of 25 ° C. or less and a humidity of 60% or less for 8 hours; Compressing the aged mixture at a temperature of 20 ° C. or less and a humidity of 40% or less at a pressure of 2,000 kg / cm 2 and a speed of 30 rpm; Aging the compressed mixture in a sealed state at a temperature of 25 ° C. or less and a humidity of 60% or less for 8 hours; The aged mixture was first coated at 1.5 rpm for 90 minutes and 2.5 rpm for 60 minutes under conditions of heat exchanger pressure 0.2 Mpsi, air compressor pressure 4 to 6 bar, gun injection pressure 5 bar, and then 60 minutes at 3.5 rpm, 4.5 Second coating for 30 minutes at rpm; It provides a method for producing a foamable solid for oral cleaning comprising; drying the coated mixture for 8 hours in a sealed state at a temperature of 25 ° C. or less and a humidity of 60% or less.

Hereinafter, the present invention will be described in more detail through examples. However, the following examples are intended to illustrate the present invention, and the scope of the present invention is not limited thereto.

Example

After mixing the components according to Table 1 for 15 minutes at a speed of 30 rpm or less under a temperature of 22 ° C or less and a humidity of 40% or less using a ribbon mixer (V-Mixer), the temperature is 25 ° C or less and humidity It was aged for 8 hours in a sealed state at a condition of 60% or less. The aged raw material was compressed at a pressure of 2,000 kg / cm 2 and a speed of 30 rpm using a tablet press under conditions of a temperature of 20 ° C. or less and a humidity of 40% or less, and then sealed in a sealed condition at a temperature of 25 ° C. or less and a humidity of 60% or less Aged for an hour. Thereafter, the aged raw material was first coated with a heat exchanger pressure of 0.2 Mpsi, a main air compressor pressure of 4 to 6 bar, and a gun injection pressure of 5 bar using a coating machine. At this time, the exhaust temperature was 35 to 38 ° C, and 1.5 It was performed for 90 minutes at rpm and 60 minutes at 2.5 rpm. Subsequently, the second coating was performed under the same conditions as the first coating. At this time, the exhaust temperature was 45 to 48 ° C, and it was performed at 3.5 rpm for 60 minutes and 4.5 rpm for 30 minutes. Thereafter, the mixture was dried for 8 hours in a sealed state at a temperature of 25 ° C or lower and a humidity of 60% or lower.

	Ingredient name (main ingredient name)	Parts by weight	Weight (mg)
main ingredient	Green tea extract (catechin)	0.35	2.8
	Grape extract (resveratrol)	0.05	0.4
	Golden extract (Baikalin)	0.1	0.8
	Bellflower extract (Kilkyung)	0.2	1.6
Sweetener	Xylitol	27.48	219.84
	L-menthol	0.8	6.4
	D-sorbitol	14.1	112.8
	Enzyme Treatment Stevia	1.44	11.52
Surfactants	Olive oil	3.3	26.4
	L-Lysin	1.92	15.36
pH adjuster	DL-apple	13.1	104.8
Additive for formulation	Magnesium stearate	0.48	3.84
	Calcium carbonate	0.08	0.64
	Sodium hydrogen carbonate	20	160
	Crystalline cellulose	4.8	38.4
	Lactose	6	48
	Starch	5	40
Spices	Mint flavor powder	0.8	6.4

Comparative Example 1 (Comparative detergent)

It was prepared in the same manner except for the main component in the above example.

Comparative Example 2 (standard detergent)

Comparative Example 2 (standard detergent) was prepared, which consisted only of the components of a conventional detergent using dental type silica as a main component.

Comparative Example 3 (control detergent)

Only the basic components such as wetting agent, foaming agent, and fragrance were added to prepare Comparative Example 3 (control detergent), which is a standard brush solution.

Selection of test subjects and test methods

120 adult men and women aged 20 to 50 years with mild-to-moderate gingivitis symptoms were selected as test subjects, and the test subjects were tested in groups of 30 each after a one-week run-in period. , Comparative group, negative control group, divided into four groups of the positive control group, the test was conducted for 4 weeks, and test examples 1 to 4 were performed at intervals of 1 week, 2 weeks, and 4 weeks.

In order to create an oral environment with the same toothpaste, all four groups were subjected to brushing using the rotation method using Comparative Example 2 for 3 minutes after breakfast and after dinner every day. The test group was rinsed in Example after lunch, the comparative group was washed in Comparative Example 1 after lunch, and the positive control was washed in Comparative Example 3 after lunch, and the negative control was additionally washed after breakfast and after dinner. There was no.

At this time, in Example 1 and Comparative Example 1, tablets were placed in the mouth, masticated, and crushed using the tongue and lips to rub the gums, teeth, and tongue and spit them out by rubbing and gargle. . In Comparative Example 3, after lunch, an appropriate amount (10 cc) was kept in the mouth for about 1 minute, and was used as a spitting method.

Table 2 below shows the gender and age distribution of all subjects.

	Total age group	20's	30s	40s
Total sex	120	71	29	20
male	33	14	14	5
female	87	57	15	15

Test example  One. Gingivitis index  evaluation

1) Papillary Marginal Attached Gingival index (PMA index)

The gingival marginal gingival index was measured for the maxillary and mandibular anterior gingival teeth, which are shown in Table 3 and FIG. 1 below. The PMA index at week 0 before the test was not significantly different between the 4 groups (p> 0.05) in the test group 11.27, the comparison group 11.30, the negative control group 11.33, and the positive control group 11.30, and after one week, the PMA index was the test group 11.03, comparison group 11.07. , Negative control group 11.67, positive control group 11.10, and after 2 weeks, the PMA index was examined in the test group 10.93, comparison group 10.80, negative control group 11.63, and positive control group 10.80. On the other hand, after 4 weeks, the PMA index was examined as 10.20 in the test group, 11.07 in the comparison group, 11.90 in the negative control group, and 10.20 in the positive control group, and the test group and the positive control group were significantly lower in the PMA index than the negative control group (p < 0.05), it was confirmed that the PMA index of the test group and the positive control group decreased to a statistically significant level 4 weeks after the test (p <0.05). Through the above results, it was confirmed that the embodiment of the present invention showed a similar degree of gingivitis relief effect when using a conventional oral brushing solution.

	Week 0		Week 1		Week 2		Week 4
	Average	Standard Deviation	Average	Standard Deviation	Average	Standard Deviation	Average	Standard Deviation
Test group	11.27	2.95	11.03	2.89	10.93	2.42	10.20	2.30
Comparison	11.30	2.59	11.07	2.86	10.80	2.01	11.07	2.21
Eumseong Control	11.33	2.88	11.67	2.95	11.63	2.39	11.90	2.26
Positive control	11.30	2.63	11.10	2.81	10.80	1.95	10.20	2.27
p-value	1.000		0.805		0.401		0.011

2) Talbott, Mandel and Chilton's Gingival Index (GI)

The gingivitis index is divided into mesial, centrifugal, and central gingivitis, respectively, according to the rating criteria of the gingivitis of Loe modified by Talbott, Mandel and Chilton. Was calculated as the arithmetic mean. The gingivitis index of an individual was calculated by dividing the sum of the measured values of each part by the number of teeth to be examined. At this time, the total number of teeth to be tested was # 16, # 11, # 26, # 46, # 31, and # 36 teeth. Was made. The gingivitis rating criteria for each site of Loe are as follows, and the results are shown in Table 4 and FIG. 2 below.

[Based on the gingivitis rating for each part of Loe]

0: no inflammation

1: Minor gingivitis (slight change in color tone and weak edema)-No bleeding during periodontal perimetry

2: Moderate gingivitis (redness, edema)-bleeding during periodontal perimetry

3: High gingivitis (ulcer)-tends to bleed on its own

The pre-test Talbott's gingivitis index was 1.33 in the test group, 1.33 in the comparison group, 1.36 in the negative control group, and 1.35 in the positive control group. There was no significant difference between the 4 groups.Measurement after 1 week was 1.31 in the test group, 1.35 in the comparison group, and 1.37 in the negative control group. There was no significant difference between the 4 groups, which was investigated as the control group 1.31. Measurements after 2 weeks were examined as test group 1.24, control group 1.33, negative control group 1.41, and positive control group 1.22. Measurements after 4 weeks were examined as test group 1.19, control group 1.26, negative control group 1.44, and positive control group 1.12. After 4 weeks, it was confirmed that the gingivitis index of the test group and the positive control group was significantly lower than that of the test (p <0.05). In addition, the gingivitis index was higher in the negative control group after 4 weeks than in the test (p <0.05). There was no significant difference between the groups by period before and 4 weeks after the test (p> 0.05), but after 2 weeks, the test group and the positive control group had significantly lower gingival index than the control and negative control groups ( p <0.05), the gingivitis index was significantly lower in the control group than in the negative control group (p <0.05). On the other hand, after 4 weeks, the gingivitis index of the positive control group was the lowest, but it was not significantly different from the test group, and it was confirmed that there was a significant difference between the control group and the negative control group.

	Week 0		Week 1		Week 2		Week 4
	Average	Standard Deviation	Average	Standard Deviation	Average	Standard Deviation	Average	Standard Deviation
Test group	1.33	0.19	1.31	0.16	1.24	0.13	1.19	0.13
Comparative bacteria	1.33	0.17	1.35	0.15	1.33	0.11	1.26	0.12
Eumseong Control	1.36	0.15	1.37	0.10	1.41	0.09	1.44	0.10
Positive control	1.35	0.16	1.31	0.16	1.22	0.13	1.12	0.11
p-value	0.814		0.334		0.000		0.000

Test example  2. Dental hygiene membrane  evaluation

1) Dental Hygiene Performance Index (PHP index)

The degree of adhesion of the dental hygiene membrane was evaluated by the dental hygiene management ability index, and the teeth to be examined were # 16, # 11, # 26, # 46, # 31, and # 36 teeth.

As shown in Table 5 and Fig. 3, the pre-test PHP index was test group 2.23, comparative group 2.16, negative control group 2.16, positive control group 2.21, and after one week, the PHP index was test group 2.18, comparison group 2.07, negative control group 2.21, positive The control group 2.06, the PHP index after 2 weeks was tested in the test group 2.07, the comparison group 2.15, the negative control group 2.21, the positive control group 2.09, and the 4 weeks later the PHP index was tested in the test group 2.04, the comparison group 2.09, the negative control group 2.35, and the positive control group 2.08. There was no significant difference between the 4 groups before, 1 and 2 weeks after the test (p> 0.05), and the PHP index was significantly lower in the test group after 4 weeks than the negative control (p <0.05). . Through the above results, it was confirmed that the embodiment of the present invention has superior ability to inhibit the formation of dental bacterial membranes compared to the case where the mouth was not washed.

	Week 0		Week 1		Week 2		Week 4
	Average	Standard Deviation	Average	Standard Deviation	Average	Standard Deviation	Average	Standard Deviation
Test group	2.23	0.39	2.18	0.36	2.07	0.32	2.04	0.37
Comparison	2.16	0.49	2.07	0.45	2.15	0.35	2.09	0.43
Eumseong Control	2.16	0.37	2.21	0.30	2.21	0.36	2.35	0.35
Positive control	2.21	0.41	2.06	0.44	2.09	0.34	2.08	0.41
p-value	0.833		0.376		0.424		0.011

2) Tooth microbial membrane rating standard (Plaque index)

The degree of attachment of the dentifrice membrane was measured using Turesky-modified Quigley and Hein's dentifrice membrane rating criteria, and the teeth tested were # 15, # 13, # 26, # 44, # 32, and # 36 teeth.

As shown in Table 6 and Figure 4, Turesky's surface microbial index was tested before test group 2.58, comparison group 2.60, negative control group 2.55, positive control group 2.58, test group 2.53 after 1 week, comparison group 2.53, negative control group 2.56, Positive control group 2.51, 2 weeks later, test group 2.55, comparison group 2.47, negative control group 2.57, positive control group 2.49, and after 4 weeks, test group 2.44, control group 2.47, negative control group 2.67, and positive control group 2.45. There was no significant difference between the 4 groups before, 1 week, and 2 weeks after the test (p> 0.05), and after 4 weeks, the test group and the positive control group showed significantly lower dental plaque index than the negative control group ( p <0.05).

	Week 0		Week 1		Week 2		Week 4
	Average	Standard Deviation	Average	Standard Deviation	Average	Standard Deviation	Average	Standard Deviation
Test group	2.58	0.38	2.53	0.32	2.55	0.31	2.44	0.27
Comparison	2.60	0.36	2.53	0.29	2.47	0.29	2.47	0.30
Eumseong Control	2.55	0.35	2.56	0.28	2.57	0.22	2.67	0.26
Positive control	2.58	0.38	2.51	0.29	2.49	0.30	2.45	0.30
p-value	0.959		0.911		0.503		0.004

Test example  3. Bad breath evaluation

1) Bad breath meter

Halitosis evaluation was conducted using a bad breath meter BB Checker (Plustech, Daejeon, Korea), and the measured values are shown in Table 7 and FIG. 5 below.

As a result of the measurement, the test group before the test 81.4, the control group 82.3, the negative control group 82.3, the positive control group 81.3, the test group 78.7 after 1 week, the comparison group 81.5, the negative control group 83.8, the positive control group 77.4, the test group 77.2 after 2 weeks, the comparison group 82.2 , Negative control group 84.3, positive control group 76.7, and after 4 weeks, the test group 73.6, comparison group 78.5, negative control group 87.3, and positive control group 72.8 were investigated. There was no significant difference between the 4 groups before, 1 and 2 weeks after the test (p> 0.05), and after 4 weeks, the test group and the positive control group showed significantly lower halitosis than the negative control group ( p <0.05). It was also confirmed that the degree of bad breath in the test group and the positive control group decreased significantly after 4 weeks compared to before the test even with the difference over time (p <0.05). Through the above results, it was confirmed that the embodiment of the present invention has a similar degree of bad breath reduction effect as in the case of using a conventional mouthwash solution.

	Week 0		Week 1		Week 2		Week 4
	Average	Standard Deviation	Average	Standard Deviation	Average	Standard Deviation	Average	Standard Deviation
Example	81.4	11.7	78.7	16.3	77.2	14.9	73.6	14.1
Comparative Example 1	82.3	12.9	81.5	12.7	82.2	10.8	78.5	13.0
Comparative Example 2	82.3	14.1	83.8	14.9	84.3	9.3	87.3	14.3
Comparative Example 3	81.3	12.4	77.4	12.4	76.7	11.5	72.8	13.3
p-value	0.984		0.309		0.034		0.000

2) Visual analogue scale inspection

A bad breath evaluation was performed through a sensory test using a visual analogue scale, which is shown in Table 8 and FIG. 6 below.

As a result, it was confirmed that the degree of bad breath in the test group was low from 4.63 before the test to 4.27 after 4 weeks, and showed a lower value than the comparison group.

	Week 0		Week 1		Week 2		Week 4
	Average	Standard Deviation	Average	Standard Deviation	Average	Standard Deviation	Average	Standard Deviation
Test group	4.63	0.67	4.47	0.78	4.53	0.73	4.27	0.83
Comparison	4.67	0.66	4.57	0.57	4.50	0.68	4.30	0.79
Eumseong Control	4.60	0.67	4.50	0.63	4.73	0.78	4.60	0.56
Positive control	4.53	0.68	4.60	0.50	4.37	0.67	4.37	0.76
p-value	0.885		0.838		0.266		0.305

Test example  4. Stability evaluation

In order to evaluate the stability, adverse reactions that occurred after using the detergent were analyzed. After 2 and 4 weeks, the investigator was checked for the presence or absence of adverse reactions, and follow-up observations of all adverse reactions were conducted until the corresponding reaction disappeared, stabilized, or when the situation reached a descriptive point. . The relevance of an adverse reaction to a product for human application testing by the investigator is 'Possibly related', 'Probably related', 'Definitely related', 'Unknown' For the adverse reactions judged to have been evaluated as adverse reactions related to the product for human application testing, detailed information was presented separately. As a result of the evaluation, no adverse reaction was found in the tester during the entire test period.

Test Example 5. Evaluation of dentin artificial caries lesion remineralization

Dentin refers to the layer under the enamel, consisting of 70% inorganic, 20% organic, and 10% moisture. When the dentin is exposed, the sensitivity of the teeth increases because it is not protected from external stimuli, and as a result, all stimuli from the outside are transmitted to the nerves within the pulp and react more sensitively to the same stimuli. This can cause pain or tingling and tingling symptoms, such as hypersensitivity. Accordingly, remineralization of demineralized dentin is very important for root caries prevention and hypersensitivity treatment.

After testing the examples on the artificially created dental lesions, the surface of the dentin artificial caries lesion was observed through a scanning electron microscope (SEM), and the results are shown in FIG. 7. As a result of the observation, in the control group shown in FIG. 7 (a), it was possible to observe the demineralization pattern in which the dentin surface shape was irregular and the appearance was collapsed. It was observed that the caries lesion disappeared and the tooth surface lost due to remineralization was calcified again. In addition, as a result of measuring the dentin microhardness, it was found that the dentin surface microhardness increased to 140.26 HV (kg / mm ² ) to achieve calcification with a hard outer shape for dentin protection. Through this, it was confirmed that the embodiment of the present invention penetrated into the demineralized pores of dentin and had an excellent effect on remineralization.

Test Example 6. Evaluation of artificial ivory tubule closing effect and whitening effect

Ivory tubules can be a path of bacterial penetration if there is dental caries or are exposed, and if physical, chemical stimulation and thermal stimulation are applied while the ivory tubules are exposed, the liquid in the ivory tubules moves in and out at a very high rate. And the pressure created by the movement of the ivory fluid affects the cells in the pulp. As a result, as the cells are stretched or compressed, the nerve contacting the cells senses this change and feels pain. Accordingly, the exposed ivory tubules can be closed to protect the teeth from gum disease and tooth decay, and to relieve hard caries and hypersensitivity.

In order to evaluate the effect of closing the ivory tubules, an example was tested on an artificial dentinal tubule to observe the surface change through a scanning electron microscope, and the results are shown in FIG. 8. As a result, in the control group of FIG. 8 (a), while the ivory tubules were exposed, the artificial ivory tubules treated with the examples were observed to deposit inside the ivory tubules, so that the diameter of the ivory tubules was observed to be small, and the closure of 71.6% It showed that the closing effect of ivory customs was excellent. In addition, after processing the Examples, it was confirmed that the measurement value increased by 30.73 when the color was measured, and there was a whitening effect.

Test Example 7. Evaluation of bad breath removal effect

The causes of bad breath are mainly volatile sulfur compounds, and the main components are hydrogen sulfide (H ₂ S) and methyl mercaptan (CH ₃ SH). Accordingly, the concentration of hydrogen sulfide and methyl mercaptan in the oral cavity was measured to evaluate the efficacy of removing bad breath. Bad breath was measured 4 times in total after gas phase, immediately after washing, after 30 minutes of washing, and after 1 hour of washing. Comparative Example 1 was used as a control, and comparative analysis was conducted using a commercially available Gagreen as a comparative example. .

As shown in FIG. 9, as a result of measuring the concentration of hydrogen sulfide, it can be seen that the concentration of hydrogen sulfide is significantly reduced when washing the mouth through Examples and Comparative Examples compared to the control group. In addition, while the concentration immediately after using the comparative example was 393 ppb, the concentration immediately after using the example was 279 ppb, indicating that the bad breath removal rate was better when the example was used, and the comparative example was 346 ppb even after 1 hour. Compared to the example, the value of 174 ppb is shown, and it can be confirmed that the bad breath effect of the example of the present invention is better.

In addition, as shown in Figure 10, it can be seen that the concentration of methyl mercaptan is significantly lower when using Examples and Comparative Examples compared to the control group. In addition, the concentration of methyl mercaptan immediately after use of the example is 112 ppb, whereas the use of the comparative example shows 169 ppb immediately after use, which confirms that the deodorization rate is better when using the example, and maintains a low concentration even after a lapse of time. It can be confirmed through the bad breath removal effect.

Above, the present invention has been described by way of example, and those skilled in the art to which the present invention pertains will be capable of various modifications without departing from the essential characteristics of the present invention. Therefore, the embodiments disclosed herein are not intended to limit the present invention, but to explain the present invention, and the spirit and scope of the present invention are not limited by these embodiments. The scope of protection of the present invention should be interpreted by the following claims, and all technologies within the equivalent range should be interpreted as being included in the scope of the present invention.

According to the present invention, it is excellent in portability, easy to use, and has an industrial applicability because it can manufacture a foamable solid agent for mouthwash, which has excellent cleaning effect, bad breath removal, tooth decay prevention and other dental protection effects.

Claims (19)

1. In the foamable solid for oral cleaning, a foamable solid for oral cleaning comprising a mixture of grape extract, green tea extract, golden extract and bellflower extract as an active ingredient
2. According to claim 1, wherein the grape extract contains resveratrol as an active ingredient, the green tea extract contains catechin as an active ingredient, and the golden extract contains baikalin as an active ingredient, effervescent for mouthwash. Solids
3. According to claim 1, wherein the bellflower extract is effervescent solid foam for oral cleaning, characterized in that the long diameter
4. The foamable solid agent for mouthwash according to claim 1, wherein the foaming agent comprises sodium hydrogen carbonate.
5. The foamable solid agent for mouthwash according to claim 1, further comprising a surfactant, a pH adjusting agent, a formulation agent, an abrasive, a disintegrant, a lubricant, a sweetener and a fragrance.
6. According to claim 1, The grape extract, the green tea extract, the golden extract and the bellflower extract is a foaming solid agent for oral cleaning, characterized in that consisting of 1: 7: 2: 4 by weight.
7. 6. The foamable solid preparation for oral cleaning according to claim 5, wherein the formulation agent comprises crystalline cellulose, the abrasive is calcium carbonate, the disintegrant is lactose and starch, and the lubricant is magnesium stearate.
8. 6. The foamable solid preparation for mouthwash according to claim 5, wherein the pH adjusting agent is DL-apple acid.
9. The foamable solid preparation for oral cleaning according to claim 5, wherein the surfactant is L-Lysin and olive oil.
10. The foamable solid preparation for oral cleaning according to claim 1, characterized in that it is foamed within 30 seconds after oral input.
11. The foamable solid preparation for oral cleaning according to claim 1, wherein it has dentin remineralization and dentinal tubule closure.
12. According to claim 4, The blowing agent is a foamable solid agent for oral cleaning, characterized in that it comprises 20 parts by weight based on 100 parts by weight of the total composition
13. A first step of mixing a mixture of grape extract, green tea extract, golden extract and bellflower extract with a surfactant, pH adjusting agent, formulation agent, abrasive, disintegrating agent, lubricant, sweetener and flavoring agent;

    Two steps of aging the mixture;

    3 steps of tableting the aged mixture;

    Four steps of aging the tableted mixture;

    5 steps of coating the aged mixture;

    6 steps of drying the coated mixture; Method for manufacturing a foamable solid for mouthwash, comprising
14. The method according to claim 13, wherein the first step is mixing for 15 minutes at a speed of 30 rpm or less under conditions of a temperature of 22 ° C. or less and a humidity of 40% or less.
15. The method according to claim 13, wherein the second step is aged for 8 hours in a sealed state under a temperature of 25 ° C. or less and a humidity of 60% or less.
16. 15. The method of claim 13, wherein the third step is a production method characterized in that the pressure is 20 kg or less, and the pressure is 2000 kg / cm 2 and the speed is 30 rpm.
17. 14. The method of claim 13, wherein the fourth step is a manufacturing method characterized by aging for 8 hours in a sealed state under a temperature of 25 ° C or less and a humidity of 60% or less.
18. The heat exchanger pressure of 0.2 Mpsi, air compressor pressure of 4 to 6 bar, gun injection pressure of 5 bar is coated at 1.5 rpm for 90 minutes and 2.5 rpm for 60 minutes. 60 minutes, the manufacturing method characterized in that the coating for 30 minutes at 4.5 rpm
19. 15. The method of claim 13, wherein the step 6 is characterized in that the drying is performed for 8 hours in a sealed state under a temperature of 25 ° C or less and a humidity of 60% or less.

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