KR101723588B1 - Composition for mouth comprising camellia japonica l leaf extract and manufacturing method thereof - Google Patents

Abstract

The present invention relates to an oral composition containing an extract extracted from a camellia leaf and a method of preparing the same, wherein the oral composition of the present invention exhibits at least one of an antioxidative effect, an antimicrobial effect, and an oral cancer cell proliferation inhibitory effect.

Description

TECHNICAL FIELD The present invention relates to a composition for oral cavity including a camellia leaf extract, and a method for producing the same. BACKGROUND ART [0002]

The present invention relates to an oral composition comprising a camphor leaf extract, and a method for producing the same.

Oral diseases are 80% of adults in Korea and about 90% of elderly people over 60 are suffering from chronic diseases. Gingival disease is the third most common foreign disease, and its incidence is high and it is reported to increase every year.

Periodontal disease is closely related to the occurrence of systemic chronic diseases. The importance of eco-friendly and human-friendly natural materials is increasing day by day in the development of health supplements and hygiene products related to the medical and dental medicine fields. Especially, in order to prevent and improve periodontal diseases, Interest in phyto-materials is increasing in the materials.

Although 80% of domestic adults and 90% of the silver generation age are suffering from chronic oral diseases, the development and commercialization of auxiliary products that can be managed in advance preventive measures have not been made.

Functional detergents currently on the market include functional inhibition of plaque inhibition, inhibition of noxious bacteria in oral cavity, improvement of bad breath, and whitening effect. However, most products that do not take into account age, Inflammation is often exacerbated, and there is a demand for a product development technology to replace it.

A dentifrice composition comprising a camellia plant leaf as a main ingredient has been disclosed in Korean Patent No. 10-1391545 (entitled "Oriental herb extract and propolis-added toothpaste"). In this case, the camellia plant disclosed herein does not refer to camellia leaves. Since the number of plant species belonging to Camellia crassifolia is about 1,000, the camellia leaves used as a material in the present invention is one of 1,000 species It can not be said that the camelliace plants disclosed in the Japanese Patent Application No. 10-1391546 necessarily refer to the camellia leaves.

However, conventional toothpastes contain extracts extracted from leaves of Camellia crassifolia and various plant leaves or petals for the purpose of treatment of periodontal diseases and various oral diseases, but in this case, effects of treatment and prevention of various oral diseases , There is a problem that the dentifrice composition is deteriorated in color or the flavor is changed when the dentifrice is used for a long period of time, the effect of the medicinal effect contained in the dentifrice composition is reduced and the commercial properties of the dentifrice causing discomfort during use are decreased.

The present invention aims to provide a composition for a low-irritation and functional natural-type oral cavity using the extract extracted from camellia leaves and a method for providing the same.

The present invention relates to a composition for oral cavity which maintains the effect of a pharmacologically active agent contained in toothpaste and maintains the effect of the pharmacological effect contained in the toothpaste even when the color of toothpaste is maintained and the flavor thereof is changed by adding antioxidant power for inhibiting deterioration and flavor change and essential oil- And a manufacturing method thereof.

In one embodiment, the present invention provides an oral composition comprising an extract from camellia leaves.

In another embodiment, the present invention relates to a method for the treatment and / or prophylaxis of cancer, comprising 1 to 4% by weight of an extract from camellia leaves, 0.001 to 0.010% by weight of a pine needle extract, 0.001 to 0.010% by weight of an extract of corn oil, 0.001 to 0.010% % ≪ / RTI > by weight of the composition.

At this time, the composition for oral use was 0.25 to 0.50% by weight of enzyme-treated Stevia, 0.10 to 0.50% by weight of xylitol, 40 to 60% by weight of D-sorbitol solution, 15% by weight of dental type silica, 0.22% by weight of sodium fluoride, 0.05% by weight of pyridoxine hydrochloride, 0.50% by weight of sodium pyrophosphate, 2 to 3% by weight of vegetable glycerin, 0.05% by weight of hydroxyapatite, and 12.58 to 30% by weight of purified water.

In yet another embodiment, the present invention provides a composition comprising 1 to 4% by weight of an extract from camellia leaves, 0.001 to 0.010% by weight of essential oil, 0.001 to 0.010% by weight of an extract of corn oil, 0.001 to 0.010% Adding 0.20 to 0.80% by weight of the extract to the solvent; And 0.1 to 0.50% by weight of enzyme treated stevia, 0.10 to 0.50% by weight of xylitol, 40 to 60% by weight of D-sorbitol solution, 15% by weight of dental type silica, 0.22% by weight of sodium fluoride, 0.05% by weight of pyridoxine hydrochloride, 0.5 to 0.50% by weight of vegetable glycerin, 2 to 3% by weight of vegetable glycerin, 0.05% by weight of hydroxyapatite and 12.58 to 30% by weight of purified water to the solvent.

The camellia used in the above refers to camellias and Camellia japonica L as a plant taxonomic.

The composition of the present invention shows improvement of gingivitis, antioxidative activity, suppression of oral pest, bactericidal action, and dental calculus improving ability.

In addition, the composition of the present invention contains an extract extracted from camellia leaves, which is effective for oral health maintenance, to heal gum inflammation, prevent dental caries, prevent gum aging, and prevent dental deposition.

In addition, the composition of the present invention has antioxidant ability which suppresses alteration and fragrance change and essential oil-derived essential oil component, so that even if the color of the toothpaste is maintained and the flavor is changed, the effect of the pharmacologically active agent contained in the toothpaste is maintained, .

FIG. 1 shows the phenolic contents of ethanol extracts from Camellia japonica L. leaves in each month.
FIG. 2 shows DPPH radical scavenging activity of ethanol extracts from Camellia japonica leaves of ethanol extract of camellia leaves according to each month.
FIG. 3 shows the catalase activities of extracts of Camellia sinensis from various parts of camellia.
Fig. 4 shows the antimicrobial activity (① 20 mg / mL, ② 40 mg / mL, ③ 80 mg / mL, and ④ 100 mg / mL) of the extract extracted from camellia leaves against the carotid bacterium S. mutans.
Fig. 5 shows the antimicrobial activity (① 20 mg / mL, ② 40 mg / mL, ③ 80 mg / mL, and ④ 100 mg / mL) of the extract extracted from camellia leaves against dental caries-inducing S. sobrinus.
Figure 6 shows the antimicrobial activity of extracts from camellia leaves against the causative organism C. albicans (20 mg / mL, 40 mg / mL, 80 mg / mL, and 100 mg / mL).
Fig. 7 shows the antimicrobial activity (① 20 mg / mL, ② 40 mg / mL, ③ 80 mg / mL (1 mm), and 100 mg / mL (3 mm)) of the anticancer composition against the cavity-inducing S. mutans.
Fig. 8 shows the antimicrobial activity (① 20 mg / mL, ② 40 mg / mL, ③ 80 mg / mL, and ④ 100 mg / mL) of a cicatricial composition against dental caries-inducing S. sobrinus.
Fig. 9 shows the antimicrobial activity (① 20 mg / mL, ② 40 mg / mL, ③ 80 mg / mL, and ④ 100 mg / mL) of the anticancer composition against C. albicans causing the stomatitis.
FIG. 10 shows DPPH radical scavenging activity of ethanol extracts from Cornus officinalis of ethanol extract of camellia leaves.
Fig. 11 shows the SOD activity (HL / F) of the extract of corn oil.
Fig. 12 shows the antioxidant activity of extract oil from Agastache rugosa.
Figure 13 shows the antimicrobial activity of essential oil from the essential oil of herb against Staphylococcus epidermidis.
FIG. 14 shows the antimicrobial activity of essential oil depending on the concentration of essential oil. FIG. 14 shows the antimicrobial activity of essential oil depending on the concentration of essential oil in the staphylococcus epidermidis.
FIG. 15 shows the antimicrobial activity of essential oil from herb against Propionibacterium acnes (1).
FIG. 16 shows the antimicrobial activity of essential oil depending on the concentration of essential oil.
FIG. 17 shows the antimicrobial activity of essential oil from herbicide of Malassezia furfur.
Fig. 18 shows the results of antimicrobial activity of the extracts of the upper leaves (left side) and the extract of the mulberry bark (right side).

Hereinafter, some embodiments of the present invention will be described in detail with reference to exemplary drawings. It should be noted that, in adding reference numerals to the constituent elements of the drawings, the same constituent elements are denoted by the same reference numerals even though they are shown in different drawings. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted when it may make the subject matter of the present invention rather unclear.

In the present specification, the percentages may be% by volume or, if necessary,% by weight, unless otherwise specified.

The present invention provides an oral composition for oral hygiene and improvement of oral hygiene, an effect of inhibiting harmful bacteria in the oral cavity, a dentifrice thereof, and a preparation method thereof. The composition for oral use may be selected from the group consisting of a toothpaste composition, a mouthwash composition, an oral perfume composition, a dentifrice composition, a toothpick coating composition, a composition for dental coating, a mouth film composition, .

Oral has been considered as one of the important causes of oral and systemic diseases caused by pathogenic infectious strains and resident bacteria by providing a very easy environment for various microorganisms. In order to improve oral health by controlling the growth conditions of oral microorganisms, various researches and developments have been made. However, since the abuse and abuse of medicines and the resistance of medicines to the infectious organisms have become serious problems, .

Hereinafter, a method for producing an oral composition including an extract derived from camellia leaves and a composition thereof will be described in detail by way of specific examples, but it should be borne in mind that the scope of the present invention is not limited by these embodiments.

The present invention relates to a method for treating gum inflammation by containing an extract extracted from a camellia leaf which is effective for oral health maintenance and containing essential oil, essential oil, corn oil extract, The present invention relates to a composition for preventing dental caries, preventing premature aging of teeth and dental calculus, and a method of manufacturing the same, and particularly relates to a composition for improving gingivitis, antioxidant activity, inhibition and sterilization of oral noxious bacteria, To a composition for oral cavity which can prevent and improve gingivitis and other oral diseases by adding it as a main functional material, and a method for producing the same.

In addition, the composition of the present invention can be a detergent composed mainly of a low-stimulus natural material considering vulnerable oral conditions of infants and the elderly.

In order to accomplish the above object, the present invention provides a detergent composition comprising as an essential ingredient an extract extracted from camellia leaves, comprising 1 to 4% by weight of an extract derived from a camellia plant leaf, 0.001 to 0.010% by weight of essential oil, 0.001 to 0.010% by weight of the extract of corn oil, 0.001 to 0.010% by weight of the extract of Oriental herbal extract, 0.20 to 0.80% by weight of the leaf extract, 0.25 to 0.50% by weight of the enzyme-treated stevia, 0.10 to 0.50% by weight of xylitol, 15 wt% of dental type silica, 0.22 wt% of sodium fluoride, 0.05 wt% of pyridoxine hydrochloride, 0.50 wt% of sodium pyrophosphate, 2 to 3 wt% of vegetable glycerin, 0.05 wt% of hydroxyapatite, and 12.58 to 30 wt% of purified water And then mixed.

The extracts from Camellia sinensis leaf, essential oil, Sansori oil extract, Rhizoctonia soluum extract, and Mulberry leaf extract were concentrated alcohol extracted with alcohol.

The method for preparing a detergent composition using the extract extracted from the camellia leaves of the present invention is characterized by using a multi-mixer (LAB-NEO-V) capable of removing bubbles in the mixture by applying the principle of vacuum, 0.001 to 0.010% by weight of an essential oil, 0.001 to 0.010% by weight of an extract of corn oil, 0.001 to 0.010% by weight of an extract of Oriental herb extract, and 0.20 to 0.80% (JAC-4020) under the condition of 50 캜 before mixing with the purified water before adding to the pot of the mixer jar, 15% by weight of dental type silica in the multi-mixer jar, 15% by weight of sodium fluoride 0.22% by weight of sodium pyrophosphate, 0.50% by weight of sodium pyrophosphate, and 0.05% by weight of hydroxyapatite, and then mixed with the purified water for 20 minutes at room temperature. A third mixing step of adding 0.25 to 0.50 wt% of stevia, 0.10 to 0.50 wt% of xylitol, 40 to 60 wt% of D-sorbitol solution and 2 to 3 wt% of vegetable glycerin and uniformly mixing them at 50 캜 for 20 minutes, second mixing step and the fourth mixing stage for mixing the 30 minutes at the conditions of 50 ℃ uniform in addition to the tertiary mixture in accordance with the mixing step cheonyeonmulreul mixed in a primary mixing stage, and then finally mixed for 10 minutes at room temperature 10 ^{- And} a finishing step of removing air bubbles under a vacuum of ³ Torr.

The properties and efficacy of extracts from Camellia sinensis, essential oil, Rhizoctonia solanum L., and Mulberry leaf extract are examined below.

I. Main Ingredients of Oral Compositions

Extracts from camellia leaves

Camellia japonica L (Camellia japonica L) is an evergreen tree belonging to Camellia japonica and Camellia japonica. It is a species of Camellia japonica L. It is located in Jeolla province such as Gochang, Wando, Kangjin, Naju and Yeosu And Jeonnam region occupies 67% of the total planted area. According to recent reported results, there are pharmacological activities such as antioxidant action and antioxidant activity, inhibition of tartar formation, inhibition of alcohol absorption, whitening action, anti-inflammatory action and HIV-1 protease inhibitory activity, The active leaves have been used for long time in Korea and Japan. The main components contained in camellia include flowers such as leucoanthocyanin and anthocyanin. The fruit contains camelliagenin ABC, which is an aglycon of fatty oil, camellin, tsubaki-saponin and tsubaki-saponin. The leaves contain ι-epicatechol, d- catechol and so on. As described above, camellia contains a large amount of major active ingredients, and its physiological activity is various. However, studies for industrializing it into edible products and secondary processed products have not been conducted yet.

The Camellia japonica L belonging to Camellia and Camellia is a plant taxonomically disclosed in Korean Patent No. 10-1391545 (entitled "Herbal Extract and Propolis-Added Toothpaste"), . Namely, since the number of plant species belonging to Camellia crassifolia is 1,000, the camellia leaves used as a material in the present invention corresponds to only one of 1,000 species, and the camellia plant family disclosed in Korean Patent No. 10-1391546 (Camellia japonica L) belonging to Camellia and Camellia can not be referred to as plant taxonomically in the present invention.

1. Anti-microbial activity test

1) Antimicrobial activity test

The camellia used in this experiment was collected from the wild camellia which is native to Camellia japonica in Cheongbuksan, Jangheung - gun, Jeonnam Province, in February - March, young leaves in April - May, and young leaves in June - August Respectively. The antimicrobial activity of Gram positive bacteria was Bacillus subtillis , Streptomyces fradiae and Staphylococcus aureus were used, and Escherichia coli , Pseudomonas aeruginosa , Enterobacter spp. C1036 and Salmonella typhimurium , respectively. The green leaf samples of camellia were powdered to be suitable for extraction, methanol of 10 times the weight of the sample was added, extracted at 40 ° C for 5 to 6 hours, filtered, and the extract solvent was removed using a vacuum concentrator and dried using a freeze dryer And then used in the experiment.

A single colony of each pure strain was taken and platelets were taken in 10 ml of microbial broth and incubated for three times at a temperature of 18-24 hours. To prepare the plate culture medium for the antimicrobial activity test, 15 ml of each agar medium was sterilized, and 15 ml of each medium was dispensed into petridish to coagulate the medium for the base layer. The medium for medium layer to which 0.7% , 0.1 ml of a test suspension (a suspension of the bacteria in which the bacterial suspension was made to have an absorbance of 0.3 at 660 nm by making sterilized saline solution) was aseptically added and mixed well, and then the mixture was dispensed on the medium for the base layer And uniformly solidified to prepare a double-medium inoculated medium. The antimicrobial activity of camellia extract was determined by disc plate method (Piddocket, 1990; Bauer et al ., 1996). The filter paper discs (Toyo roshi kaisha, 8 mm) were sterilized by filtration with 0.45 μm membrane filter (Millipore Co., USA) at 1, 5, 10 and 15 mg / , The extract solvent was aseptically air-dried and completely blown. After culturing for 24 to 48 hours at the appropriate temperature of each microorganism, the diameter (mm) of the clear zone formed around the paper disc was measured to determine the antibacterial activity Were compared. At this time, the solvent and the surfactant used to dissolve each sample were tested.

The results of the experiment showed that the antimicrobial activity was increased as the concentration of the extracts of each part dropped on the disc. As the concentration increased, the size of the inhibition zone showing the antimicrobial activity was increased. For the B. subtilis , S. fradiae , P. aeruginosa , and S. typhimurium in the young leaf extract, inhibition at 13 mg / Ring. Therefore, it was confirmed that the extracts of young leaves in Camellia have wide antibacterial activity against Gram - positive bacteria and Gram - negative bacteria. Among them, S. aureus and E. coli reacted most sensitively and showed inhibitory effect of 10 ㎜ when 5 mg / ㎖ of young leaf extract was administered. In contrast, mature leaf extract showed a 15㎎ / ㎖ antimicrobial activity of the 6 ~ 10㎜ at concentrations only for P. aeruginosa, bud extract of P. aeruginosa and Enterobacter spp . C1036 strain at a concentration of 15 mg / ml, the inhibitory effect was 8 mm and 9 mm, respectively. Table 1 shows the antibacterial activity (Antibacterial activities of methanol extracts in different sections of Camellia japonica) in the extract from other parts of the Camellia (Camellia japonica).

       Microorganisms Conc.
(mg / ml) Size of inhibition zone (mm) YL ML FWB FW BK BH SD G (+) Bacillus subtilis  One - - - - - - -  5 9 - - - - - -  10 11 - - - - - -  15 13 - - - - - - Streptomyces  fradiae  One - - - - - - -  5 7 6 5 - - - -  10 12 8 7 - - - -  15 13 10 8 - - - - Staphylococcus aureus  One - - - - - - -  5 10 - 6 - - - -  10 11 - 8 - - - -  15 12 - 9 - - - - G (-) Escherichia coli  One - - - - - - -  5 10 - - - - - -  10 11 - - - - - -  15 12 - - - - - - Pseudomonas  aeroginosa  One - - - - - - -  5 9 - - - - - -  10 11 - - - - - -  15 13 - - - - - - Enterobacter spp. C1036  One - - - - - - -  5 8 - - - - - -  10 10 - - - - - -  15 12 - - - - - - Salmonella typhimurium  One - - - - - - -  5 - - - - - - -  10 8 - - - - - -  15 9 - - - - - -

In the present specification, it was found that the antimicrobial activity varies according to the content of the phenolic substance contained in the methanol extract of the camellia. As a result, the antimicrobial activity of young leaves extract of Camellia japonica differed according to the content of phenolic substances, and the higher the content of phenolic substances, the higher the antimicrobial activity. Thus, the use of natural antibacterial agent .

2. Antioxidant activity analysis to prevent premature aging of gum tissue

In this specification, the oxidative stress of the gum due to active oxygen species generated during the metabolism of cells serves as a cause of premature aging of the gum, and thus, one index for evaluating the antioxidative effect capable of improving or preventing the gum DPPH scavenging activity, antioxidant activity, and antioxidant enzyme activities were used.

1) Analysis of polyphenol contents

Phenolic compounds are one of the secondary metabolites widely distributed in plants and have various structures and molecular weights. Because they have a phenolic hydrowyl (OH) group, they bind easily with proteins and other macromolecules, and have various physiological activities such as antioxidant and anti-cancer. In this experiment, total phenol contents of extracts were measured with tannic acid as a reference material for each stage of maturity of camellia leaves.

The results showed that the highest phenolic content was found in camellia leaves collected in July, 740.6 ㎍ / ㎎, followed by 737.9 ㎍ / ㎎ in leaves collected in June, and leaves collected in August In leaves collected in May, and 733.6 ㎍ / ㎎ in leaves collected in May, and 368.2 ㎍ / ㎎ in leaves collected in March, and 333.6 ㎍ / 329.8 ㎍ / ㎎ in leaves collected, 327.4 ㎍ / ㎎ in leaves collected in February, and 291.5 ㎍ / ㎎ in leaves collected in December last year. From May to August, the content of phenol was relatively high, ranging from 721.6 to 740.6 ㎍ / ㎎, and the content of phenol was 291.5 ~ 368.2 ㎍ / ㎎ during December to April of last year.

1 and Table 2 show the phenolic contents of methanol extracts of camellia leaves (total phenolic contents of methanol extracts from each month of Camellia japonica L. leaves).

Sample Collection time Total phenolics (㎍ / mg) ^{1 )} Leaves
Dec. 2005 291.5 ± 8.21 ²⁾ Jan. 2006 329.8 ± 10.22 Feb. 2006 327.4 ± 8.45 Mar. 2006 368.2 ± 10.55 Apr. 2005 333.6 ± 18.35 May 2005 721.6 + 1.13 Jun. 2005 737.9 ± 11.03 Jul. 2005 740.6 + - 9.80 Aug. 2005 734.6 ± 10.45 Flower
Apr. 2005 635.5 ± 9.89 May 2005 649.7 ± 6.22

① Sample was analyzed using tannic acid as a standard.

②Each value is means ± SD (n = 3)

2) Analysis of DPPH radical scavenging ability

For each concentration, 160 μL of the sample was dissolved in methanol and mixed well with 40 μL of a DPPH solution dissolved in methanol at a concentration of 1.5 × 10 4 M. The reaction mixture was allowed to stand at room temperature for 30 minutes, and the absorbance was measured at 520 nm with a microplate reader spectrophotometer VERSAmax. The free radical scavenging activity was expressed as a percentage and the 50% scavenging concentration (IC50 expressed in μg / mL or μM) was calculated as compared to the control without the sample. The measured values were expressed as the average value obtained by three repeated experiments and compared with the conventional antioxidants Vit C, Vit E and BHT.

   The antioxidant activity of camellia leaf extracts was measured by DPPH method at 100 ㎍ / ㎖ concentration for each period (05.12 ~ 06.8). From December to February, it was less than 30% . However, the DPPH radical scavenging rate increased rapidly to 70.89% in March, and the scavenging rate was more than 90% in the camphor leaf extract collected from May to June, indicating the highest antioxidant activity . The antioxidant activity was similar to that of ascorbic acid (Vit C), which is a natural antioxidant, and showed much higher antioxidative activity than BHT which is a synthetic antioxidant.

2 and 3 show DPPH radical scavenging activity of methanol extracts from Camellia japonica leaves of methanol extract of camellia leaves according to each month.

Sample Collection time Scavenging activity (100 [mu] g / ml) IC ₅₀ (/ / ml) ^* Leaves Dec. 2005 28.79 ± 1.23 179.88 Jan. 2006 26.75 + - 0.83 184.32 Feb. 2006 24.97 ± 0.78 190.48 Mar. 2006 70.89 ± 1.02 57.85 Apr. 2006 84.49 + - 2.18 39.78 May 2006 92.54 + 0.16 ≤ 12.5 Jun. 2006 93.30 ± 0.04 ≤ 12.5 Jul. 2006 76.98 1.50 48.77 Aug. 2006 74.64 ± 1.12 46.73 ascorbic acid 96.19 + 0.04 ≤ 12.5 BHT 31.43 + - 1.29 198.93

3) Analysis of catalase activity of Camellia sinensis leaf extract

catalase is an antioxidant enzyme that rapidly treats harmful oxygen in vivo and protects cells. It is a typical enzyme that decomposes and eliminates antioxidant enzyme H ₂ O ₂ . Antioxidant enzyme-rich foods have been thought to reduce the likelihood of developing cancer or heart disease, and antioxidant enzymes have been reported to delay the aging of the body. These antioxidant enzyme-rich supplements include fat-soluble vitamin E such as alpha-tocopherol, beta-carotene, water-soluble vitamin C, selenium (Se), green tea, chlorella and greenish-yellow vegetables. Vitamin E is known to be the most important lipid-soluble antioxidant in humans because it is related to cell membranes. Vitamin C also plays a role in removing water-soluble peroxide radicals and regenerating reduced vitamin E.

In this experiment, catalase activity was measured by Aebi (1984) method. To 50 mM potassium phosphate (pH 7.0) was added 10 mM H ₂ O ₂ And a reaction enzyme solution were added thereto. The change in absorbance at 240 nm for 2 minutes was observed, and the amount of enzyme degrading 1 uM H ₂ O ₂ was set to 1 unit over 1 minute.

The catalase activities of the cambial larvae, young leaves, and mature leaves were investigated. The activities of green tea and camellia were the highest in leaf extracts, Showed almost similar activity. In the case of fresh leaves, the lowest activity was observed compared with green tea leaves. From these results, it is observed that camellia seedlings have higher activity than the green tea activity reported so far and contain substances with high H ₂ O ₂ removal ability.

FIG. 3 shows the catalase activities of extracts of Camellia sinensis from various parts of camellia.

3. Component analysis

1) Content analysis of camellia sinensis leaf

Total nitrogen was the highest in the first leaf (4.21%) and decreased in the third leaf and the fourth leaf after ripening. Total free amino acids were 2.12% and 2.27% in leaf and stem, respectively. The content of catechin was 17.8% in the first leaf and decreased as the leaf became very immature and maturation progressed. Vitamin C tended to increase slightly as the leaf width developed, then decreased again. Table 4 shows the content of leaf components in camellia sinensis (new leaf).

division Total nitrogen Total free amino acids Catechin Caffeine Vitamin C 1st leaf 4.21 0.52 17.80 2.61 33.27 Second leaf 4.13 0.59 17.63 2.52 58.91 Third leaf 4.10 0.69 17.28 2.44 69.63 Fourth leaf 4.11 0.73 16.48 2.43 51.97 Fifth leaf 4.09 0.82 16.26 2.35 64.98 6th leaf 4.06 0.86 14.96 2.29 43.31

2) Analysis of free sugar content of camellia leaves

The content of free sugar in Camellia japonica leaf was highest in sucrose content of 12.8 nmol / 0.1 mg, followed by fructose, glucose and maltos. Table 5 shows the content of free sugars of camellia leaf extracts (unit, nmol / 0.1 mg) of the extracts extracted from camellia leaves.

Glucose Fructose Sucrose Maltose Total 3.3 6.7 12.8 2.1 24.9

 4. Antimicrobial activity of extracts extracted from Camellia sinensis on oral harmful bacteria

S. mutans, which occurs frequently in the oral cavity of elderly people, is an early causative agent causing dental caries (dental caries). It is caused by the acid generated by the decomposition of sugar and starch by S. mutans, Damaged and cavities occur. Candidiasis, Thrush: Candida albicans infection causes grayish or milky spots on the surface of the oral mucosa. Especially in elderly denture users, consuming diseases or immunity patients.

The paper disc method was used to analyze the antimicrobial activity of the extracts from the camellia leaves and the toothpastes containing the extracts from the camellia leaves. A single colony of each isolate was isolated and inoculated into 10 ml of the broth culture medium. The broth was cultured for three times at a temperature of 18-24 hours at the appropriate temperature of the strain, and then used as an antimicrobial activity test strain. For the preparation of the plate culture medium for the antimicrobial activity test, 15 ml of agar was added to 15 ml of each agar medium, and 15 ml of the agar medium was added to the petri dish to coagulate the culture medium. , D) was 0.4 (10 ⁶ CFU / mL), and the mixture was aseptically added to a medium containing 0.7% agar. The mixture was then mixed on a medium for the bed, and then solidified uniformly. Medium was prepared. The sterilized 8 mm paper disc was placed on a solid medium which was sufficiently hard, and then 30 μl of each sample was absorbed into the disc. After incubation at 37 ° C for 24 hours, the clear zone around the disc was observed, Respectively.

 Fig. 4 shows the antimicrobial activity (① 20 mg / mL, ② 40 mg / mL, ③ 80 mg / mL, and ④ 100 mg / mL) of the extract extracted from camellia leaves against the carotid bacterium S. mutans.

Fig. 5 shows the antimicrobial activity (① 20 mg / mL, ② 40 mg / mL, ③ 80 mg / mL, and ④ 100 mg / mL) of the extract extracted from camellia leaves against dental caries-inducing S. sobrinus.

Figure 6 shows the antimicrobial activity of extracts from camellia leaves against the causative organism C. albicans (20 mg / mL, 40 mg / mL, 80 mg / mL, and 100 mg / mL).

Table 6 summarizes the antimicrobial activities of Camellia sinensis extracts from Camellia sinensis on C. suicide, S. sobrinus, C. albicans, and C. cannabis.

Clear zone of extract from camellia leaves (Unit: mm) Concentration Microbial strains S. mutans S. sobrinus C. albicans control - - - ① 20mg / ml 2 2 3 ② 40mg / ml 3 3 4 ③ 80mg / ml 4 4 5     ④ 100mg / ml 5 5 6

2. Antimicrobial activity of erectile composition against oral harmful bacteria

Fig. 7 shows the antimicrobial activity (① 20 mg / mL, ② 40 mg / mL, ③ 80 mg / mL (1 mm), and 100 mg / mL (3 mm)) of the anticancer composition against the cavity-inducing S. mutans.

Fig. 8 shows the antimicrobial activity (① 20 mg / mL, ② 40 mg / mL, ③ 80 mg / mL, and ④ 100 mg / mL) of a cicatricial composition against dental caries-inducing S. sobrinus.

Fig. 9 shows the antimicrobial activity (① 20 mg / mL, ② 40 mg / mL, ③ 80 mg / mL, and ④ 100 mg / mL) of the anticancer composition against C. albicans causing the stomatitis.

Table 7 summarizes the antimicrobial activity of the antiseptic composition against the carotid-inducing bacteria S. mutans, the dental caries-inducing bacteria S. sobrinus, and the causative organism of stomatitis C. albicans.

Clear zone of the sheath composition (unit: mm) Concentration Microbial strains S. mutans S. sobrinus C. albicans control - - - ① 20mg / ml - 3 3 ② 40mg / ml - 4 5 ③ 80mg / ml One 5 5     ④ 100mg / ml 3 6 6

Corn oil

Cornus officinalis is a deciduous broad-leaved arboreous tree belonging to the genus Cornaceae. It is a plant that lives in the vicinity of the mountainous region, and generally uses the flesh quality of the fruit as medicinal. Major efficacy has been reported to have antimicrobial action against skin incontinence, diabetes, hypotension, anticancer action, convergence, skin fungi (Staphylococcus aureus, yellow pseudomonas), auditory cell protection, tugging, antioxidant, Such as Morroniside, Loganin, Cornin (Verbenalin), Saponin, Tannin, Ursolic acid, Gallic acid, Malic acid, Tartaric acid, Vitamin A and others.

1. Antioxidant efficacy analysis to prevent premature aging of gum tissue

In this specification, the oxidative stress of the gum due to active oxygen species generated during the metabolism of cells serves as a cause of premature aging of the gum, and thus, one index for evaluating the antioxidative effect capable of improving or preventing the gum DPPH scavenging activity, antioxidant activity, and antioxidant enzyme activities were used.

 1) Polyphenol content of extract

Total polyphenol content was measured by Folin-Denis method. To 0.1 g of the extract isolated from corn oil, 10 ml of methanol was added, and the mixture was extracted at 70 ° C for 30 minutes and made into 1 mg / ml. 650 μl of distilled water was added to 50 μl of the sample solution, 50 μl of Folin-Denis reagent was added, and the mixture was reacted at room temperature for 3 minutes. After the reaction, 100 μl of a saturated solution of 10% Na ₂ CO ₃ was added, and 150 μl of distilled water was added to adjust the final volume to 1 ml. After reacting in a water bath at 37 ° C for 1 hour, the absorbance was measured at 725 nm using a UV-Vis spectrophotometer. In the blank test, the methanol solution was treated in place of the sample solution, and the standard curve was such that the concentration of tannic acid (Sigma Co., USA) was 0 to 500 μg / mL, and the total phenol content was determined therefrom.

 Analysis of polyphenol contents showed that 27.17 / / ml was contained as in Table 8 (total polyphenol content of the extract).

Plant name (Parts used) Total Polyphenolics (占 퐂 / ml) Corn oil (fruit) 27.17

2) Analysis of DPPH radical scavenging ability of extract

The antioxidant activity was measured by slightly modifying the Blois method for measuring the radical scavenging effect of the sample using the DPPH method. 100 μl of 1 × 10 ^-4 M DPPH and concentration-specific extracts were taken and incubated for 30 min in the dark, and the residual radical concentration was measured at 517 nm using an ELISA reader (Bio-RAD, USA). The amount of reducing power of the sample is expressed as a scavenging activity. RC ₅₀ is expressed as the amount (㎍) of the sample required to reduce the concentration of DPPH to 1/2. BHT (butylated hydroxytoluene) and Vit C (ascorbic acid) were compared.

DPPH radical scavenging activity (%) = (Ac-As) / Ac x 100

Where Ac is the absorbance of the control without addition of the sample and As is the absorbance of the reaction solution containing the sample.

As a result of DPPH radical scavenging activity of the extract, the RC ₅₀ value of the extract from corn syrup was 234.51 ug / ml.

10 and 9 show the DPPH radical scavenging activity of ethanol extracts from Cornus officinalis of the ethanol extract of camellia leaves.

name (Scientific name) Part used RC ₅₀ (ug / ml) Hosta lancifolia ) Flesh 234.51 BHT 101 Vit.C 6.8

2) SOD-like activity and CAT activity

10-6mM)를 참가하여 반응을 측정하였다. SOD 활성 측정은 550nm에 30초 단위로 5분간 흡광도를 측정하였다. SOD activity was measured by Beauchamp and Fridovich (1971). The solution containing 50 mM carbonic buffer (pH 10.2), 0.1 mM EDTA, 0.1 mM Xanthine, 0.025 mM nitroblue tetrazolium (NBT) and enzyme solution was reacted at 25 ° C for 10 minutes and then treated with Xanthine oxidase

10-6mM) was added to measure the response. SOD activity was measured by absorbance at 550 nm for 5 minutes in 30 second increments.

Catalase activity was measured by the Aebi (1984) method. To 50 mM potassium phosphate (pH 7.0) was added 10 mM H ₂ O ₂ And a reaction enzyme solution were added thereto. The change in absorbance at 240 nm for 2 minutes was observed, and the amount of enzyme degrading 1 uM H ₂ O ₂ was set to 1 unit over 1 minute.

As shown in Table 10, the SOD activity of the fermented soybean oil (17.8 U / mg) showed excellent enzyme activity. As a result of analysis of CAT activity, the fermented soybean oil had excellent activity as 13.9 U / mg.

Fig. 11 shows the SOD activity (HL / F) of the extract of corn oil.

Sample CAT activity (U / mg) SOD activity (U / mg) Corn oil 13.9 17.8

2. Analysis of sterility against oral harmful bacteria

In addition, the bactericidal effect of six kinds of oral disease - inducing bacteria was verified by MBC (Minimum Bactericidal Concentration) method.

Table 11 shows the minimum bactericidal concentration of extracts from Cornus officinalis fruits).

MBC (mg / mL) Aa  33384 Tf  43037 Fn  25586 Pi 25611 Pg  33277 Sm  25175 > 1 > 1 0.25 > 1 One > 1

* Aa 33384: Actinobacillus actinomycetem - comitans (invasive periodontitis, gum disease causing bacteria)

* Tf 43037: Tannerella forsythensis

* Fn 25586: Fusobacterium necrophorum (ulcerative stomatitis, periodontal disease, causing bad breath)

* Pi 25611: Prevotella intermedia (hormone-related periodontitis causing bacteria)

* Pg 33277: Porphyromonas gingivalis (major causative agent of periodontal disease)

* Sm 25175: Streptococcus mutans (a major cause of dental caries)

The fruit extract of Sanskrit showed excellent antimicrobial activity against Fusobacterium necrophorum, which acts as a causative organism of ulcerative stomatitis, periodontal disease and bad breath, and showed strong antiseptic effect against Porphyromonas gingivalis, a major pathogen of periodontal disease. In addition, Actinobacillus actinomycetemcomitans, a causative organism of dental caries and periodontal disease, Prevotella intermedia, a hormone-related periodontitis inducer, Streptococcus mutans, an early pathogen of dental caries, and Prevotella intermedia, were demonstrated at low levels.

Fried

Agastache rugosa (排草香Agastach in Korea Prime Encyclopedia rugosa O.Kuntze) is a perennial plant of Labiatae, also known as a fenugreek, hwakyeong, or tochuka, and is distributed geographically in East Asia such as Japan, China, Manchuria, and Taiwan. In our country, mountain wilderness, valleys, and some humid places in the country are alive. The main component of the syrup is phenylpropanoide essential oil component and its main component is methylchavicol. In addition, anethloe, ansialdehyde, and terpene essential oils contain α-limonene, β-methoxycinnamaldehyde and α-pinene. The pharmacological effect has an action of inhibiting the development of skin fungus, Staphylococcus aureus, Pseudomonas aeruginosa, Escherichia coli, Disease, hemolytic streptococcus, and pneumonia.

1. Refined oil extraction

The cleaned plant was cut into a predetermined size, put in a round flask together with distilled water, and steam distillation was performed using a steam distillation apparatus for 5 hours to obtain a transparent essential oil.

2. Antioxidant and antioxidant activity analysis

In this specification, the oxidative stress of the gum due to active oxygen species generated during the metabolism of cells serves as a cause of premature aging of the gum, and thus, one index for evaluating the antioxidative effect capable of improving or preventing the gum DPPH scavenging activity, antioxidant activity, and antioxidant enzyme activities were used.

1) Analysis of phenol content

The filtrate used in this specification was extracted with 500 ml of ethanol per 500 g of the sample for 5 hours under heating mentle. The extract was filtered with filter paper (No. 1, Advantec) and concentrated under reduced pressure at 50 ° C before use.

Total polyphenol content was measured by Folin-Denis method. 0.1 g of the extract was dissolved in 10 ml of methanol and diluted to 1 mg / ml. Add 650 μl of distilled water to 50 μl of the sample solution, add 50 μl of Folin-Denis reagent, and allow to react at room temperature for 3 minutes. After the reaction, 100 μl of a saturated solution of 10% Na ₂ CO ₃ was added, and 150 μl of distilled water was added to adjust the final volume to 1 ml. After reacting in a water bath at 37 ° C for 1 hour, absorbance was measured at 725 nm using a UV-Vis spectrophotometer (Pharmacia Biotech ultrospec-2000). For the blank test, the methanol solution was used instead of the sample solution, and the standard curve was such that the concentration of tannic acid (Sigma Co., USA) was 0 to 500 μg / mL, and the total phenol content was determined therefrom.

Polyphenolic compounds are aromatic compounds that give a specific color to a plant and act as a substrate in a redox reaction and have two or more phenolic hydroxyl (OH) groups in one molecule. Flavonoids and tannins are the main components. AIDS, antioxidant, and anti-cancer. Total polyphenol contents in each of the herbal extracts were measured using tannic acid as a reference. The content of polyphenol contained in the syrup was 51.91 占 4.64 占 퐂 / ml as shown in Table 12.

Scientific name Korean name Total phenolics (/ / ml) Agastache rugosa Fried 51.91 + - 4.64

2) Determination of antioxidant activity of essential oil

The antioxidant activity was determined by modifying the Blois method to measure the radical scavenging effect of the sample using the DPPH method. 100 μl of 1 × 10 ^-4 M DPPH and concentration-specific extracts were mixed and left to stand for 30 minutes in darkness. Residual radical concentrations were measured at 517 nm using an ELISA reader (Bio-RAD, USA). The amount of reducing power of the sample is expressed as a scavenging activity. RC ₅₀ is expressed as the amount (μg) of sample required to reduce the concentration of DPPH to 1/2. BHT (butylated hydroxytoluene), which is well known as an antioxidant, Vitamin C (ascorbic acid).

DPPH is a relatively stable free radical with a deep purple color. It is often used to search for antioxidants from various natural materials because it is reduced by aromatic compounds and aromatic amines. The antioxidative activity of each extract was measured by the DPPH method as follows.

Table 13 were compared with the antioxidant activity by the DPPH radical scavenging of the extract in an amount ₅₀ RC value of a sample required to decrease the DPPH radical concentration to 1/2, RC ₅₀ value of Agastache rugosa essential oil (essential oil) is a 700㎍ / ㎖ appear.

Fig. 12 shows the antioxidant activity of extract oil from Agastache rugosa.

sample  RC ₅₀ (占 퐂 / ml) Bleeding (AR) 700 Vit  C. (ascorbic acid) 9.08 BHT 95.68

3. Antimicrobial activity of essential oil

The paper disk diffusion method was used to confirm the antimicrobial activity of the ethanol extraction extract solution. As shown in Table 14, the results of the ethanol extracts of the foliar extracts showed strong antimicrobial activity against the four strains.

Table 14 shows the antimicrobial activities of essential oils from Agastache rugosa.

         Strains Inhibition zone (mm) 125 [mu] g / ml 250 [mu] g / ml 500 [mu] g / ml   Staphylococcus aureus - ^* - -   Bacillus amyloliquefaciens - - - Enterobacter spp. 20 30 50 Listeria monocytogenes 30 40 40 Pityrosporum oval e 30 40 50   Staphylococcus epidermidis 20 20 30 Candida albicams - - 20

 *: Not detected

4. Antimicrobial activity of essential oil

Propionibacterium The antimicrobial activity of acnes was 30 ~ 40%, and Staphylococcus epidermidis showed strong antimicrobial activity at 30% and 40% concentration. In addition, essential oil extracts were added to 10, 20, 30 and 40% concentration of Malassezia furfur The antimicrobial activity was measured by paper disc agar diffusion method, and the antimicrobial activity was observed at the concentration of 40%.

Figures 13 and 15 show the antimicrobial activity of essential oil from the herbicide essential oil from herb against Staphylococcus epidermidis .

Bacterium Antimicrobial activity (mm) 20% 30% 40% Staphylococcus epidermidis Blossom flower - +++ ++ Back ground top - + +

14 shows the essential oil antimicrobial activity Agastache rugosa (Antimicrobial activity of essential oil depending on various concentration against Staphylococcus epidermidis. Flowers Agastache rugosa A, B Agastache rugosa aerial part) according to the concentration of the (essential oil).

      sample
density. A. blossom flowers B. Bamboo ground top Essential oil 5 [mu] l + EtOH 35 [ 3.3 - Essential oil 10 μl + EtOH 30 μl 3.3 - Essential oil 20 [mu] l + EtOH 20 [ 5 3 Essential oil 30 [mu] l + EtOH 10 [ 6.3 - Essential oil 40 μl 8.6 2.6

15 is Agastache rugosa essential oil antimicrobial activity (Antimicrobial activity of (essential oil) of essential oil from herb against Propionibacterium acnes . 1. Blossom bloom 2. Above ground part.

Strains Antimicrobial activity (mm) 20% 30% 40% Propionibacterium acnes Blossom flower - + + Back ground top - + +

FIG. 16 shows the antimicrobial activity of essential oil depending on the concentration of essential oil.

    sample
density A. blossom flowers B. Bamboo ground top Essential oil 5 [mu] l + EtOH 35 [ 3 - Essential oil 10 μl + EtOH 30 μl 2.6 - Essential oil 20 [mu] l + EtOH 20 [ 3.3 2 Essential oil 30 [mu] l + EtOH 10 [ 4 2.6 Essential oil 40 μl 4.3 3.3

*: not available

FIG. 17 shows the antimicrobial activity of essential oil from herb against Malassezia furfur. Left: bamboo flower right: bamboo ground part).

Sample
Conc. Blossom flower Back ground top Essential oil 5 [mu] l + EtOH 35 [ 4.6 - Essential oil 10 μl + EtOH 30 μl 5.3 2.3 Essential oil 20 [mu] l + EtOH 20 [ 5.6 2.3 Essential oil 30 [mu] l + EtOH 10 [ 6 2.6 Essential oil 40 μl 6.3 4

The top  And morphine

The main bark is the root of bark belonging to Moracerae, and the top leaf is the leaf of mulberry. Its main effect is used for the treatment of noise, hypoglycemia, hypotension, antimicrobial action, anti-inflammatory action, prevention and treatment of diabetes, The compounds of the present invention may be used in combination with one or more of the following: rutin, quercetin, moracetin, b-sitosterol, campesterol, lupeol, myoinositol, inokosterone), and the like. In the present specification, the mulberry leaf extract comprises the mulberry bark extract.

1. Antimicrobial activity against oral bacteria

Using paper disc method, mulberry leaf and mulberry root extracts prepared by hot water extraction method were used to analyze the inhibitory effect of Streptococcus mutans acting as a causative organism of dental caries. The concentrations of extracts treated with S. mutans were 1, 10, 50, and 100 ㎎ / ㎖, and the results showed that the extracts of mulberry root (mulberry root shell) Inhibition of the antimicrobial activity of the mulberry leaf extracts was not observed in all concentration groups.

18 and 20 show the antimicrobial activity results of the extracts of the upper leaves (left side) and the extract of the mulberry bark (right side).

Sample concentration (mg / mL) The top Mallow Clear zone (mm) One - 1.5 10 - 1.8 50 1.3 3.2 100 1.6 6

In addition, in the case of the upper leaves, the minimum concentration of sterilization power was analyzed for six kinds of oral disease causing bacteria, and it showed excellent lethal power against three kinds of bacteria.

Table 21 shows the minimum bactericidal concentration of extracts from Morus alba L. leaves.

MBC (mg / mL)  Aa 33384 Tf 43037 Fn 25586 Pi 25611 Pg 33277 Sm 25175 > 2 0.5 0.125 0.125 <0.015 > 2

* Aa 33384: Actinobacillus actinomycetem - comitans (invasive periodontitis, gum disease causing bacteria)

* Tf 43037: Tannerella forsythensis

* Fn 25586: Fusobacterium necrophorum (ulcerative stomatitis, periodontal disease, causing bad breath)

* Pi 25611: Prevotella intermedia (hormone-related periodontitis causing bacteria)

* Pg 33277: Porphyromonas gingivalis (major causative agent of periodontal disease)

* Sm 25175: Streptococcus mutans (a major cause of dental caries)

II. toothpaste  Preparation of composition

1. Difference between toothpaste of synthetic raw material and toothpaste ingredient of natural raw material

The components of toothpaste, which is usually one of the oral compositions composed of synthetic raw materials, include synthetic abrasives, synthetic humectants, synthetic functional raw materials, artificial coloring and flavoring agents, and foaming agents for detergents.

On the other hand, the constituents of toothpaste which is one of the oral compositions composed of natural raw materials include natural abrasives, natural wetting agents, functional raw materials (plain white, herbal etc.), vegetable coloring agents and flavoring agents, and natural foaming agents.

 2. Characteristics and Function of Composition Component

The properties and functions of the composition components are shown in Table 22 below.

ingredient Features and Functions Wetting agent Preventing the hardening of the cream type cuticle chief ingredient Prevention of tooth decay, prevention of periodontal disease & antioxidant effect (Vitamin B6),
Prevention of calcification abrasive Removal of plaque Viscosity modifier Adjust the overall viscosity of the composition Brighteners By adjusting the color of the extract and increasing the composition,
Prevention of tooth discoloration by tooth Excipient
(hydroxyapatite) It is the same ceramic as human bone and main component, it is used as artificial bone and root, and it is possible to integrate with tissue with good bio-adaptability. Sweetener Adjusts the flavor and taste of the toothpaste with a sweetener whose sweetness is about 100 to 200 times that of sugar Foaming agent It is an additive used to uniformly disperse a liquid or solid that does not mix with each other uniformly in a liquid. It causes bubbles to increase the feeling of brushing and removes dirty substances.

3. Status of used ingredients by country

[Table 23] shows the ingredients used in each country of Sekishi.

Ingredient used by country
Classification domestic
(Standard manufacturing standard) Japan
(Standard manufacturing standard) United States of America
(FDA approved) Removal of plaque Calcium hydrogen phosphate, anhydrous calcium hydrogen phosphate, precipitated calcium carbonate, calcium carbonate, tricalcium phosphate, colloidal silicon dioxide, silicon dioxide, anhydrous calcium phosphate, hydrated silicon dioxide, dental type silica As an active ingredient
Do not accept As an active ingredient
Do not accept Gum disease prevention Sodium chloride, tocopherol acetate, pyridoxine hydrochloride, allantoin, allantoin chlorohydroxyaluminum, tranexamic acid, aminocaproic acid Sodium chloride, tocopherol acetate, pyridoxine hydrochloride, allantoin chlorohydroxy aluminum, chlorohexidine hydrochloride, lysozyme chloride, hinokitiol, polyoxyethylene laurelate, cetylpyridinium chloride, trichloroacid, etc. Triclosan Prevention of calcification Sodium pyrophosphate Zeolite,
Sodium pyrophosphate,
Sodium polyphosphate, etc. Caries prevention NaF, SnF, SMFP, AmF NaF, SnF, SMFP, AmF Cyrin relieves KNO₃ Removal of cigarette tar Sodium polyphosphate,
Polyethylene glycol,
Polyvinylpyrrolidone

3. Functional ingredients and amount of addition of oral composition

In order to prepare the toothpaste using the oral composition, at least one of a wetting agent, a main ingredient, an abrasive, a viscosity controlling agent, a brightening agent, an excipient and a sweetening agent may be added as a basic additive of the composition together with the extract extracted from the camellia leaves.

As described above, the detergent composition comprising the extract extracted from the camellia leaves of the present invention as a main material comprises 1 to 4% by weight of an extract extracted from camellia leaves, 0.001 to 0.010% by weight of essential oil, 0.001 to 0.010% by weight of the extract, 0.001 to 0.010% by weight of the extract of Oriental herbal extract, 0.20 to 0.80% by weight of the leaf extract, 0.25 to 0.50% by weight of Enzymatically Modified Stevia Glucosyl Stevia, 0.10 to 0.50% by weight of xylitol, 40 to 60 wt%, dental type silica 15 wt%, sodium fluoride 0.22 wt%, pyridoxine hydrochloride 0.05 wt%, sodium pyrophosphate 0.50 wt%, vegetable glycerin 2 to 3 wt%, hydroxyapatite 0.05 wt%, purified water 12.58 By weight to 30% by weight.

For example, the difference in the physical properties depending on the addition amount of the extract and the basic components extracted from the camellia leaves can be analyzed and the addition amounts of the respective components can be determined as shown in Table 24.

Raw material name Content (% by weight) Purpose of blending Extracts from camellia leaves 1.0 to 4.0 Main active ingredients (gingivitis, inhibition of oral bacteria, antioxidant activity, improvement of bad breath, improvement of toothache and gingival ulcer and oral disease, anti-inflammation) Essential oil 0.001 to 0.050 Corn oil extract 0.001 to 0.050 Ginseng extract 0.001 to 0.050 Leaf extract 0.20 to 0.80 D-sorbitol solution 40 to 60 Wetting agent Vegetable glycerin 2.0 to 3.0 Apple Wash 2.0 to 10.0 Natural foaming agent (vegetable surfactant) Dental type silica 15 abrasive Sodium fluoride
(Sodium fluoride) 0.22 Caries prevention Sodium pyrophosphate 0.50 Prevention of calcification Hydroxy
Apatite 0.05 Excipient Enzyme treatment Stevia 0.25-0.50 Sweetener Xylitol 0.10 to 0.50 Purified water To 100

As can be seen from Table 24, the oral composition according to one embodiment of the present invention contains D-sorbitol liquid and (concentrated) glycerin as a wetting agent in purified water as a solvent, dental type silica and sodium fluoride (sodium fluoride ), Pyridoxine hydrochloride and sodium pyrophosphate, PEG-1500 and titanium oxide as an abrasive, hydrated silicic acid as a viscosity regulator, hydroxyapatite as a brightener, stevia treated with an enzyme as an excipient, xylitol as a sweetener, But is not limited to these. The mouthpiece composition may contain SLS as a foaming agent, CMS as a viscosity modifier, Optamint 295901 as a flavoring agent, and L-menthol.

III. Clinical experiment

The present invention aims to evaluate the anti-stinging effect, anti-gingivitis effect and oral microbial reduction effect of oral composition containing camellia extract through clinical experimental studies.

1. Clinical research subjects

This study was approved by the Research Ethics Review Committee of Chosun University Dental Hospital and all subjects were limited to those who voluntarily agreed to participate in clinical trial research. The subjects were 20-59 year old adults with at least 18 natural teeth. (Patient Hygiene Performance; PHP Index: 1.5 or higher), which is thought to accumulate dental plaque.

In the results of the existing domestic studies, the reduction effect of the dental plaque membrane and the effect size of the control group were calculated in the group using the gingivitis reduction effective substance (sodium hydrogencarbonate-containing toothpaste). We calculated the average size of each effect in both studies, and the number of initial target samples was calculated as 25 for each group considering the power of Z distribution (Zα = 0.05, Zβ = 0.2, unilateral verification). In addition, considering the 4 - week study period, the dropout rate was determined as 10% and the final study subjects were 82.

The final study subjects were assigned to double-blind randomization by toothpaste group, and the sex, age, and dental flora of the subjects assigned to each tooth group were evenly distributed without statistically significant difference (p> 0.05, 25).

The toothpaste used in this study was a negative control group (toothpaste 'group') containing no extracts extracted from camellia leaves, a toothpaste group containing extracts extracted from camellia leaves , And commercial toothpaste (anti - plaque product), which showed the improvement of gingivitis.

division Toothpaste. Toothpaste. Anti-plague p-value Study subjects (persons) 24 (34.3) 24 (34.3) 22 (31.4) Gender (%) ^* man 5 (20.8) 10 (41.7) 11 (50.0) 0.10 ^* Woman 19 (79.2) 14 (58.3) 11 (50.0) Age (Mean ± sd) 30.65 ± 2.19 30.17 ± 2.14 31.86 + - 2.46 0.62 ^** PHP Index 1.76 + 0.16 1.72 + - 0.12 1.87 + - 0.13 0.56 ^{** *} Chi-square test ^** One-way ANOVA

 This study was conducted for a total of 6 months including 4 weeks of actual research period and research preparation and preparation period. The examiner selected 82 eligible subjects by judging whether or not they were eligible for the study by oral examination at the first visit. All subjects were instructed to take oral hygiene training and to brush their teeth twice a day or more during the study period according to their habits. The use of oral mouthrinse was limited

Contents Primary Secondary Third term 0 days 2 weeks 4 weeks evaluation Base-line
Saliva test
Gingivitis evaluation
Term evaluation Saliva test
Gingivitis evaluation
Term evaluation Saliva test
Gingivitis evaluation
Term evaluation Participants 82 people 70 people 70 people

2. Clinical evaluation

Subjects were evaluated clinically by saliva test, gingivitis index, and plaque index.

1) Saliva test

First, the subjects were asked to chew paraffin wax to generate irritating saliva, and then saliva was collected three times, baseline, two weeks, and four weeks later.

2) Evaluation of gingivitis

For the evaluation of gingivitis, the Le & Silness Gingival index was used in this study. In this evaluation method, the teeth in the upper right maxillary first molar, the maxillary right second incisor, the maxillary left first molar, the mandibular left first molar, the mandibular left second incisor, and the mandibular first premolar are used as index teeth.

3) Evaluation of plaque index

In this specification, the PHP (Patient Hygiene Performance, PHP) Index was used as the plaque index.

3. Statistical Analysis

The dental plaque indexes of each group were analyzed by Kolmogorov-Smirnov test. Repeated measure ANOVA was performed to determine whether there was a change in the number of Streptococcus mutans in the saliva, changes in the gingival index, and changes in the dental plaque membrane according to the duration of toothpaste use in each of the three experimental groups. Duncan's multiple comparison method was used for the post-test to determine the significant difference between the groups performing the ANOVA. A Paired t-test was used to compare the mean difference between before and after toothpaste use for each experimental group. Statistical analysis was performed using the SPSS 18.0 statistical package program (SPSS Inc., U.S.A.) with a significance level of 0.05.

4. Research Results

1) Gingivitis reduction effect

As can be seen from Table 27, the gingival index decreased with time after use in toothpaste, toothpaste, toothpaste, and anti-prage group. However, there was no decrease in the gingivitis index (p> 0.05). Toothpaste ',' group ',' toothpaste ', and' army 'group showed continuous decrease of gingivitis after 2 weeks and 4 weeks (p <0.05). In the case of toothpaste 'A', the reduction in gingivitis was 1.1 times and 1.5 times in the case of toothpaste 'I', respectively.

Classification and measurement timing Average difference
(MD + SE) p-value ^* p-value ^** 0 days after 2 weeks After 4 weeks Toothpaste. 1.60 + 0.06 1.43 + 0.06 - 0.17 ± 0.05 0.00 ^* <0.001 ^** - 1.43 + 0.06 1.31 + 0.07 0.13 + 0.04 0.01 ^* 1.60 + 0.06 - 1.31 + 0.07 0.29 ± 0.27 0.00 ^* Toothpaste. 1.61 + 0.06 1.38 + 0.06 - 0.24 ± 0.05 0.00 ^* - 1.38 + 0.06 1.22 + 0.06 0.16 ± 0.05 0.00 ^* 1.61 + 0.06 - 1.22 + 0.06 0.40 ± 0.05 0.00 ^* Anti-plague 1.58 + 0.07 1.42 ± 0.06 - 0.17 + 0.04 0.01 ^* - 1.42 ± 0.06 1.33 + 0.07 0.09 ± 0.05 0.10 1.58 + 0.07 - 1.33 + 0.07 0.26 + 0.04 0.07 ^* p < 0.05 obtained by paired t-test ^** p <0.05 obtained by Repeated measure ANOVA MD ± E denote Mean difference ± standard error

2) Inhibitory effect of bacterial membrane formation on tooth surface

As can be seen from Table 28, when the toothpaste was applied to the group, the toothpaste, the army, and the anti-prage group, the bacterial film index decreased after the use time.

However, there was no significant difference in the reduction of dental floss (p> 0.05). In the case of toothpaste 'I', the bacterial membrane was statistically decreased after 2 weeks of use and maintained for 4 weeks (p <0.05).

However, in the case of tooth group 'A', the bacterial count index decreased, but the value was not statistically significant (p> 0.05).

Classification and measurement timing Average difference
(MD + SE) p-value ^* p-value ^** 0 days after 2 weeks After 4 weeks Toothpaste. 1.74 + - 0.12 1.57 + - 0.14 - 0.17 + 0.14 0.22 <0.001 ^** - 1.57 + - 0.14 1.49 ± 0.12 0.08 ± 0.12 0.53 1.74 + - 0.12 - 1.49 ± 0.12 0.25 + 0.13 0.07 Toothpaste. 1.76 + 0.16 1.51 ± 0.16 - 0.24 0.10 0.03 ^* - 1.51 ± 0.16 1.49 ± 0.19 0.02 0.09 0.81 1.76 + 0.16 - 1.49 ± 0.19 0.26 ± 0.12 0.04 ^* Anti-plague 1.87 + - 0.13 1.58 ± 0.18 - 0.28 ± 0.15 0.07 - 1.58 ± 0.18 1.62 ± 0.16 -0.04 ± 0.12 0.76 1.87 + - 0.13 - 1.62 ± 0.16 0.24 0.11 0.03 ^{* *} p < 0.05 obtained by paired t-test ^** p <0.05 obtained by Repeated measure ANOVA MD ± E denote Mean difference ± standard error

According to the present invention, it is possible to provide a dentifrice composition, which is an oral composition, which contains gypsum salts, antioxidative activity, inhibition and sterilization of oral noxious bacteria, and extract of camellia leaves, essential oils, It has been found that the composition containing these natural substances can improve various oral diseases by adding extracts, ginseng extracts, and leaf extracts, and in particular, has proven gingivitis and periodontal disease improvement and therapeutic effects as a result of clinical trials.

According to the present invention, the dentifrice composition as an oral composition has the effect of maintaining the effect of the medicinal effect contained in the dentifrice even when the color of the dentifrice is maintained and the fragrance thereof is changed, and it is refreshing when used.

V. Other  Manufacture of oral composition

In addition to the dentifrice composition described above, the oral composition such as a composition of oral cleanser (oral cleanser), a composition of oral perfume, a composition of dentifrice cleanser, a composition for toothpick coating, a composition for dental coating, a composition for oral film, Depending on the type and purpose, the compounding ratio between the components may be slightly different, but the basic components are applied in accordance with the components of the above composition.

As described above, the composition for oral cavity comprises 1 to 4% by weight of the extract extracted from the camellia leaves, 0.001 to 0.010% by weight of essential oil, 0.001 to 0.010% by weight of the extract of corn oil, 0.001 to 0.010% The composition may further contain 0.20 to 0.80 wt% of a wetting agent, a natural foaming agent, a pH adjusting agent, a tooth decay prevention agent, an edible flavoring agent, a natural preservative, a dispersing agent, an emulsifying agent, a sweetening agent, and the like depending on the type and purpose of the formulation have.

The ingredient ratio and the purpose of compounding of the oral composition will be described below by way of example, but the present invention is not limited thereto.

1. Composition of Oral Cleanser (Oral Cleanser)

Raw material name content( weight% ) Purpose of blending Camellia leaf extract 1.0 to 4.0 Main active ingredients (gingivitis, inhibition of oral bacteria, antioxidant activity, improvement of bad breath, improvement of toothache and gingival ulcer and oral disease, anti-inflammation) Refined oil 0.001 to 0.050 Corn oil extract 0.001 to 0.050 Ginseng extract 0.001 to 0.050 Leaf extract 0.20 to 0.80 D-sorbitol solution 40 to 60 Wetting agent Vegetable glycerin 2.0 to 3.0 Coco Betaine 2.0 to 10.0 Natural foaming agent (natural surfactant derived from coconut) Citric acid (hydrate) 0.005 pH adjusting agent Sodium fluoride
(Sodium fluoride) 0.22 Caries prevention Mint scent 0.20 Edible flavoring agent Grapefruit seed extract 0.20 Natural preservative Enzyme treatment Stevia 0.25-0.50 Sweetener Xylitol 0.10 to 0.50 Purified water To 100

A mint scent is any flavoring agent that can impart a mint flavor.

2. Composition of oral perfume

Raw material name content( weight% ) Purpose of blending Camellia leaf extract 0.2 to 1.0 Main active ingredients (gingivitis, inhibition of oral bacteria, antioxidant activity, improvement of bad breath, improvement of toothache and gingival ulcer and oral disease, anti-inflammation) Refined oil 0.001 to 0.050 Corn oil extract 0.001 to 0.050 Ginseng extract 0.001 to 0.050 Leaf extract 0.20 to 0.80 D-sorbitol solution 10.00 Wetting agent Vegetable glycerin 2.0 to 3.0 Coconut oil 0.10 Natural surfactant Citric acid (hydrate) 0.005 pH adjusting agent Baking soda Removing plaque, whitening effect, removing bad breath Mint for gaggle incense 0.20 Edible flavoring agent Citrus 0.10 Natural edible preservative Olive oil wax 0.30 Natural emulsifier Enzyme treatment Stevia 0.050 Sweetener Xylitol 0.10 to 0.50 Purified water To 100

3. Composition of denture cleanser

Raw material name content( weight% ) Purpose of blending Camellia leaf extract 0.001 to 0.050 Main active ingredients (gingivitis, inhibition of oral bacteria, antioxidant activity, improvement of bad breath, improvement of toothache and gingival ulcer and oral disease, anti-inflammation) Refined oil 1.00 to 2.00 Corn oil extract 0.001 to 0.050 Ginseng extract 0.001 to 0.050 Leaf extract 0.001 to 0.050 Chlorhexidine 1.00 to 2.00 disinfectant Polysorbate 20 (Polysorbate 20) 0.30 to 1.00 Emulsifier, dispersant D-sorbitol solution 40 to 60 Wetting agent Mint for gaggle incense 0.20 Edible flavoring agent Grapefruit seed extract 0.20 Natural preservative Purified water To 100

Polysorbate 20 is polysorbate 20 is a partial ester mixture of sorbitol condensed with ethylene oxide at about 20 M and sorbitol anhydride, lauric acid for 1 M of 1 or 2 anhydrides of sorbitol or sorbitol.

4. Composition for toothpick coating

Raw material name content( weight% ) Purpose of blending Camellia leaf extract 1.0 to 4.0 Main active ingredients (gingivitis, inhibition of oral bacteria, antioxidant activity, improvement of bad breath, improvement of toothache and gingival ulcer and oral disease, anti-inflammation) Refined oil 0.001 to 0.050 Corn oil extract 0.001 to 0.050 Ginseng extract 0.001 to 0.050 Leaf extract 0.20 to 0.80 D-sorbitol solution 40 to 60 Wetting agent Sodium fluoride
(Sodium fluoride) 0.22 Caries prevention Mint flavor 0.20 Edible flavoring agent Grapefruit seed extract 0.20 Natural preservative Purified water To 100

5. Composition for dental floss coating

Raw material name content( weight% ) Purpose of blending Camellia leaf extract 1.0 to 4.0 Main active ingredients (gingivitis, inhibition of oral bacteria, antioxidant activity, improvement of bad breath, improvement of toothache and gingival ulcer and oral disease, anti-inflammation) Refined oil 0.001 to 0.050 Corn oil extract 0.001 to 0.050 Ginseng extract 0.001 to 0.050 Leaf extract 0.20 to 0.80 D-sorbitol solution 40 to 60 Wetting agent Sodium fluoride
(Sodium fluoride) 0.22 Caries prevention Mint flavor 0.20 Edible flavoring agent Grapefruit seed extract 0.20 Natural preservative Vegetable glycerin 5.00 Wetting agent Purified water To 100

6. Oral film composition (other than tooth whitening film)

Raw material name content( weight% ) Purpose of blending Camellia leaf extract 1.0 to 4.0 Main active ingredients (gingivitis, inhibition of oral bacteria, antioxidant activity, improvement of bad breath, improvement of toothache and gingival ulcer and oral disease, anti-inflammation) Refined oil 0.001 to 0.050 Corn oil extract 0.001 to 0.050 Ginseng extract 0.001 to 0.050 Leaf extract 0.20 to 0.80 D-sorbitol solution 10 to 40 Wetting agent Hydrogen peroxide 0.005 to 0.05 Tooth whitening effect Sodium fluoride
(Sodium fluoride) 0.22 Caries prevention Mint scent 0.20 Edible flavoring agent Grapefruit seed extract 0.20 Natural preservative Purified water To 100

7. Gel composition for protecting gums

Raw material name content( weight% ) Purpose of blending Camellia leaf extract 1.0 to 4.0 Main active ingredients (gingivitis, inhibition of oral bacteria, antioxidant activity, improvement of bad breath, improvement of toothache and gingival ulcer and oral disease, anti-inflammation) Refined oil 0.001 to 0.050 Corn oil extract 0.001 to 0.050 Ginseng extract 0.001 to 0.050 Leaf extract 0.20 to 0.80 D-sorbitol solution 40 to 60 Wetting agent Vegetable glycerin 5.00 Sodium fluoride
(Sodium fluoride) 0.22 Caries prevention Mint scent 0.20 Edible flavoring agent Grapefruit seed extract 0.20 Natural preservative gelatin 0.8 to 2.0 Seaweed derived gel Purified water To 100

According to the present invention, in the same manner as the dentifrice composition, an extract derived from camellia leaves and an essential oil, which have gingivitis improvement, antioxidative activity, inhibition and sterilization of oral pest bacteria, , Corn oil extract, ginseng extract, and mulberry leaf extract, it is understood that the composition containing these natural substances improves and treats various oral diseases, especially gingivitis and periodontal disease.

In addition, according to the present invention, the composition for oral use has the effect of maintaining the effect of the pharmacologically active agent contained in the dentifrice even when the hue of the composition is maintained and the fragrance thereof is changed, and it is refreshing when used.

The foregoing description is merely illustrative of the technical idea of the present invention, and various changes and modifications may be made by those skilled in the art without departing from the essential characteristics of the present invention. Therefore, the embodiments disclosed in the present invention are intended to illustrate rather than limit the scope of the present invention, and the scope of the technical idea of the present invention is not limited by these embodiments. The scope of protection of the present invention should be construed according to the following claims, and all technical ideas within the scope of equivalents should be construed as falling within the scope of the present invention.

Claims (12)

Wherein the extract comprises 1 to 4% by weight of an extract from camellia leaves, 0.001 to 0.010% by weight of essential oil, 0.001 to 0.010% by weight of an extract of corn oil, 0.001 to 0.010% Oral composition. The method according to claim 1,
The oral composition is a dentifrice composition or a detersive composition,
0.1 to 0.50% by weight of xylitol, 40 to 60% by weight of D-sorbitol, 15% by weight of dental type silica, 0.22% by weight of sodium fluoride, 0.05% by weight of pyridoxine hydrochloride, 0.50% by weight of sodium pyrophosphate Wherein the composition further comprises 2 to 3% by weight of vegetable glycerin, 0.05% by weight of hydroxyapatite, and 12.58 to 30% by weight of purified water. The method according to claim 1,
The oral composition is an oral or oral cleanser composition,
(Sodium hydrosulfite) 0.22% by weight, citric acid (hydrate) 0.005% by weight, mint flavor (mint), sodium dodecylbenzenesulfonate 0.20% by weight of scent, 0.20% by weight of grapefruit seed extract, 0.25-0.50% by weight of enzyme-treated stevia, 0.10-0.50% by weight of xylitol, and remaining purified water. The method according to claim 1,
The oral composition is an oral perfume composition,
D-sorbitol solution 10.00% by weight, vegetable glycerin 2.0-3.0% by weight, coconut oil 0.10% by weight, citric acid (hydrate) 0.005% by weight, mint flavor 0.20% by weight, citrus 0.10% by weight, olive oil wax 0.30% 0.065% stevia, 0.10-0.50% xylitol, and the remaining purified water. The method according to claim 1,
The oral composition is a denture cleanser composition,
1.00 to 2.00 wt% of chlorhexidine, 0.30 to 1.00 wt% of Polysorbate 20, 40 to 60 wt% of D-sorbitol solution, 0.20 wt% of mint flavor, 0.20 wt% of grapefruit seed extract, Further comprising an oral composition. The method according to claim 1,
The oral composition is a composition for toothpicking,
The oral composition further comprising 40 to 60% by weight of a D-sorbitol solution, 0.22% by weight of sodium fluoride (sodium fluoride), 0.20% by weight of a mint flavor, 0.20% by weight of a grapefruit seed extract, and the remaining purified water. The method according to claim 1,
The oral composition is a composition for dental coating,
The oral composition further comprising 40 to 60% by weight of D-sorbitol solution, 0.22% by weight of sodium fluoride (sodium fluoride), 0.20% by weight of mint flavor, 0.20% by weight of grapefruit seed extract, 5.00% by weight of vegetable glycerin, . The method according to claim 1,
The oral composition is an oral film or a tooth whitening film composition,
10 to 40 wt% of D-sorbitol solution, 0.005 to 0.05 wt% of hydrogen peroxide, 0.22 wt% of sodium fluoride (sodium fluoride), 0.20 wt% of mint flavor, 0.20 wt% of grapefruit seed extract, &Lt; / RTI &gt; The method according to claim 1,
The oral composition is a gel composition for protecting the gums,
, 0.20% by weight of mint flavor, 0.20% by weight of grapefruit seed extract, 0.8% by 2.0% by weight of gelatin, and 40% by weight of D-sorbitol solution, vegetable glycerin 5.00%, sodium fluoride (sodium fluoride) Further comprising an oral composition. 10. The method according to any one of claims 1 to 9,
Wherein the camellia is a Camellia japonica L plant taxonomically. 0.001 to 0.010% by weight of an essential oil, 0.001 to 0.010% by weight of an extract of corn oil, 0.001 to 0.010% by weight of an extract of Rhizoctonia solids, and 0.20 to 0.80% ; And
0.1 to 0.50% by weight of xylitol, 40 to 60% by weight of D-sorbitol, 15% by weight of dental type silica, 0.22% by weight of sodium fluoride, 0.05% by weight of pyridoxine hydrochloride, 0.50% by weight of sodium pyrophosphate Adding 2 to 3% by weight of botanical glycerin, 0.05% by weight of hydroxyapatite, and 12.58 to 30% by weight of purified water to the solvent. 12. The method of claim 11,
Wherein the camellia is a Camellia japonica L (Camellia japonica L) plant taxonomically.

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