JPS62142109A - Composition for removing foul breath and method therefor - Google Patents

Abstract

PURPOSE:To provide the titled composition containing copper gluconate and a polar solvent extract of plant of Camellia family, capable of completely eliminating foul breath composed of amine smell and sulfur compound smell by the use of an extremely small amount of the composition nd usable without causing color staining. CONSTITUTION:The objective composition contains (A) an extract produced by extracting leaf of a plant of Camellia family with a polar solvent, preferably with a 20-80% aqueous solution of glycerol at 50-100 deg.C and (B) copper gluconate. The amounts of the components A and B having deodorizing titer of (n) are nX(4.5-5.5)pts.wt. and 1pt.wt., respectively. The deodorizing titer is defined by the volume (m1) of 500ppm aqueous solution of the extract necessary to essentially eliminate the smell of 1ml of 1,000ppm aqueous solution of trimethylamine. The composition is added to mouth wash, chewing gum, candy, dentifrice, etc., at ratios of 0.0005-0.5wt% component A (in terms of 1.0 deodorizing titer) and 0.0001-0.1wt% component B.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a halitosis removing composition and a halitosis removing method,
More specifically, a breath odor removing composition containing as an active ingredient a synergistic composition of a polar solvent extract of a leaf of a Camellia plant and gluconic acid SP+, and a mouthwash, chewing gum, candy, and tablet confectionery containing the same. , relates to a method for removing bad breath that uses toothpaste or the like to deodorize the entire area of bad breath.

[Conventional technology]

It has been known that polar solvent extracts of plants of the Camellia family have a deodorizing effect (see Japanese Patent Publication No. 18098/1983). There is a review article on the removal of bad breath using an extract of green tea, which is made from the leaves of the tea tree, a representative plant of the Camellia family (Food Industry, Vol. 26, No. 16, 1983; Two Green Tea Flavonoids: Vol. 27, No. 1983). No. 8, 1984: Regarding green tea flavonoid entrance odor removal gum). Also, U.S. Patent No. 2,894,876; No. 3,044,939;
No. 12066 discloses the use of copper gluconate as a breath odor removing composition.

Add gluconic acid to the river Index 10th edition
On page 378, number 2629, cupric gluconate is described as a breath odor remover.

According to the above conventional technology, the deodorizing effect of green tea flavonoids is great against amine compounds (ammonia, trimethylamine, etc.), while the deodorizing effect of green tea flavonoids is strong against sulfur (arsenic compounds (hydrogen sulfide, methyl mercaptan, etc.)) due to the effect of chlorophyll. , and their combined use has been applied to chewing gum, etc. US Pat. No. 4,112,066 discloses the deodorizing effect of copper gluconate on sulfur monoxide.

On the other hand, halitosis is a general term for odorous substances from the oral cavity, including amines, alcohols, sulfur compounds, fatty acids, tridi-1-
It is thought that fan derivatives exist, among which,
The main components are when volatile sulfur compounds are generated from epithelial tissues, connective tissues, food afterburns, etc. through sulfur-containing amino acids through the action of enzymes, and sulfides and amines as odors coming from food and drink. In particular, methyl mercaptan and trimethylamine are thought to have a strong correlation with bad breath.

[Problem that the invention seeks to solve]

Therefore, a composition aimed at removing oral IX must be effective against both sulfur compounds (particularly methylmercapkun) and amines (particularly trimethylamine). When chlorophyll is used in combination with chlorophyll, the amount added must be 0.05 to 0.5% or more in order to produce an effect similar to that of sulfide odor due to chlorophyll. Addition (n) has the disadvantage that the color tone becomes dark green to black-rimmed and significantly lowers the product+i!fi value.

The inventors of the present invention have conducted repeated experiments on breath odor removing compositions that can be used in trace amounts and do not have the disadvantage of coloring, in view of the drawbacks of chlorophyll mentioned above. There have been no reports that it is suitable to use the leaf extract of Camellia plant in combination with gluconate sinuses, and surprisingly, a synergistic effect of 3 to 5 times can be obtained by combining the two, and the amount used is significantly reduced. The present invention was completed by discovering that the intended purpose could be achieved.

Therefore, the object of the present invention is to provide a halitosis removing composition that can completely remove bad breath consisting of both amine odor and sulfur compound odor by adding extremely small amounts of P, and that can freely adjust the color tone without coloring additives. It is on offer.

Another object of the present invention is to provide a method for removing bad breath, in which the entire area of bad breath is deodorized using a mouth-fitting product containing the halitosis removing composition according to the present invention.

[Means for solving problems]

In order to achieve the above object, in the present invention, in a polar solvent extract of leaves of a plant of the Camellia family, 1 mA of a 500 ppm aqueous solution of trimethylamine is required to substantially deodorize 1 mA of a 11000 ppm aqueous solution of trimethylamine. ．．
When the deodorizing power is defined as 0, the deodorizing power of the specified extract is 1i
nX (4,5~
5.5) Features a full-spectrum halitosis-removing Al11 composition containing as an active ingredient 11 parts by weight of gluconic acid and 11 parts by weight of gluconic acid.

There have already been many reports on the deodorizing effect of polar solvent extracts of leaves of Camelliaaceae plants, and it is thought that a group of flavonoids, which are the main components, play the leading role in deodorizing substances. This flavonoid is found in the present applicant's publication 191 that, for example, a polar solvent extract of black tea, which has been fermented with an autooxidizing enzyme from leaves of Camelliaaceae plants, has a stronger deodorizing effect than a green tea extract. This is where it pertains (
(See Japanese Unexamined Patent Publication No. 153778). In this way, the deodorizing effect of polar solvent extracts of leaves of Camellia family plants varies depending on the type of plant, the condition of the leaves (season, fermented, non-fermented), the type of solvent, the degree of purification, etc. Therefore, the amount used also varies. There must be. In the present invention, as shown in the experimental examples described below, an extract that is relatively rich in flavonoids and has a greater deodorizing effect than green tea is used as a standard, and the deodorizing power (ilfil, 0, i.e., trimethylamine) p m 500 extracts required to substantially deodorize 1 m72 of aqueous solution
1ml of ppm aqueous solution! The deodorizing potency should be inversely proportional to the flavonoid content and proportional to the amount added.

Representative plants of the Camellia family used in the present invention include tea plant, Ichiharu, sasanqua, and sakaki, and commercially available green tea such as bancha and sencha can be conveniently used. Of course, black tea and oolong tea can also be suitably used.

The polar solvents used include water, glycols (chrycerin, ethylene glycol, propylene glycol, etc.), lower alcohols (methyl alcohol, ethyl alcohol, isopropyl alcohol, etc.), and lower ketones (acetone, methyl ethyl ketone, etc.). ) or a mixture of these.Water has the disadvantage of extracting a lot of impurities such as sugars, proteins, and amino acids, while alcohols and ketones often extract substances other than chlorophyll, and flavonoids are relatively pure. For good extraction, it is preferable to extract with a 20-80% aqueous glycol solution at 50-100°C.

The halitosis-removing composition according to the present invention relates to both a halitosis-removing composition that is applied directly during the day and a raw material composition for preparing this halitosis-removing composition. The raw material composition is a mixture of a polar solvent extract of the leaves of the camellia plant and gluconic acid 111i1 in a predetermined ratio, which is prepared in a form 9 convenient for blending into a breath odor removing composition, and includes a liquid agent, It may be prepared into powders, granules, emulsions, etc. by conventional methods. However, the most important thing is the mixing ratio, and both components are prepared at a mixing ratio where the synergistic effect is most pronounced. That is, the deodorizing potency of the polar solvent extract of the leaves of the Camellia family plant to be used is determined by the method described in Examples below, and the deodorizing potency is n×(5±0.5):
],, A polar solvent extract of leaves of a Camellia plant and copper gluconate are blended in the ratio of O@Kawabe. Forms that can be used directly during the day include mouthwash, chewing gum, candy tablets, and dentifrice, and the proportions of both ingredients in these are of course the same as above. A single solvent extract of leaves of a plant of the family is selected in the range of 0.005 to 0.5% by weight and 0.0001 to 0.1@p% of copper gluconate.

[Example] Next, the bad breath removing composition according to the present invention will be specifically explained using Examples and Experimental Examples. Add 300 g of 20% glycerin aqueous solution, stir and extract at 50° C. for 3 hours, and collect the extract using a centrifuge. The same operation was repeated to cool the extract twice at 10'C for 124 hours, and the precipitated chlorophyll, wax, etc. were removed.The extract was condensed under reduced pressure, further filtered with a small amount of Celite, and then impurities were removed under high vacuum. After distillation, a 1% green tea extract containing green tea flavonoids as the main component was obtained.

Experimental Example 2 Camellia leaves were steamed by distillation and then dried under hot air at 60'C to obtain dried camellia leaves corresponding to green tea. 5 of this dried product
The same procedure as in Experimental Example 1 was carried out, except that 100 g of the pulverized material having a particle size of 0 mesohydrium or less was extracted with water to obtain an extract of 31.5%.

Experimental Example 3 The deodorizing effects of the green tea extract, camellia leaf extract, and glucone Mi obtained in Experimental Example 1.2 on methyl mercaptan and trimethylamine were measured.

Pour 1 ml of 25 ppm aqueous solution of methylmercapkun and 1000 ppm aqueous solution of trimethylamine into 100 mj2 wide-mouthed bottles, and add green tea extract, camellia leaf extract,
After adding 1 m6 of an aqueous solution of copper gluconate at a predetermined concentration and shaking for 5 minutes, the headspace gas was analyzed by gas chromatography.

Gas chromatographic analysis of trimethylamine; Column...inner diameter 3mm, length 3m glass tube; stationary phase liquid...5%
Ranpha (filler developed for amine compounds manufactured by Wako Pure Chemical Industries 91); fixed [formerly l (*
…Chromosorp W; Column temperature…75°C; Injection temperature…
75°C; Sample failure...300 μl; Carrier gas...Helium; Detector...Hydrogen flame ionization detector Methyl mercaptan gas chromatography Minutes tJi-: Minutes tJi-: Column...inside (+3 ***; length 5m; Teflon Tube; Stationary phase liquid...20% DOP, Stationary phase solid...Chromosorp W; Column temperature...75°C; Injection V+!L degree...120
°Cz Sample amount...300μl; Carry 1--Gas...Nitrogen; Detector...Tip photometric detector Analysis values are based on the integral needle display of the gas chromatograph for the peak of the gas chromatogram (depending on the relative area, the control analysis 1 shift is The deodorization rate was calculated based on the first shift of sample analysis.The results are shown in Table 1.

show.

From Table 1, it can be seen that the combination of copper gluconate and green tea extract or copper gluconate and camellia leaf extract synergistically increases the deodorizing effect compared to when each is used alone. Is recognized.

In addition, to completely deodorize 1 ml of methyl mercaptan 25 ppm water/8 solution, 1 ml of gluconic acid 60 ppm aqueous solution
m 12 or more, (copper gluconate 20 ppm water solution 0.
5mx+@, 1 tea extract 1100pp aqueous solution 0.5m#
) or more, or (copper gluconate 2 oppm water 1 volume skin 0
．． 5 mff + camellia leaf extract 10'r) m water/8 liquid 0.5 mff) or more, and trimethylamine 1100
To completely deodorize 1ml of 0pp aqueous solution, use 1ml of aqueous solution.
1 or more, 1 ml of camellia leaf extract 5X10 ppm aqueous solution,
or (0.5 mI of copper gluconate 20 ppm aqueous solution!+
LW tea extract 10100pp, 5m12) or more, or (gluconic acid ffi 20 ppm aqueous solution 0.5
mA + camellia leaf extract 10'pp m aqueous solution 0.5m#)
That's all.

By the way, the deodorizing effect of a polar solvent extract of a plant of the Camellia family can be considered to be proportional to its furanoboid content, but there are many types of extracts. Considering the relationship between Experimental Examples 1 and 2, it is recognized that the deodorizing effect of the camellia leaf extract is about 1/10 of that of the green tea extract. Therefore, in the present invention, it is preferable to uniformly process the green tea extract of Experimental Example 1, which is relatively rich in furanovoids, as a standard. That is, 1 ml of trimethylamine 11000 pp aqueous solution
According to gas chromatographic analysis of trimethylamine in Experimental Example 3, when A is substantially deodorized by 1 m6 of a 500 ppm aqueous solution of the extract, the deodorizing power is defined as 1.0.The deodorizing potency of a given extract is n. Once determined, the bad breath removing composition according to the present invention has nX (4,5 to 5.5) @9f
? 1 of extract and 1.0 part by weight of copper gluconate.

Actual) 6 Example 1 [''Powder raw material composition for preparing charcoal removal composition 1 part by weight of nigerconate, green tea extract of Experimental Example 1 (deodorizing power 1 and 1)
A solution of 5 parts by weight of dextrin and 14 parts by weight of dextrin heated to 9 parts by weight of water (100 parts by weight/g I) W L/ was spray-dried to obtain 20 parts by weight of a powder raw material and a dark blue composition.

Example 2 Granular raw material composition for 0 odor removing composition ill; copper gluconate 1 i [i placed part, camellia leaf extract obtained in Experimental Example 2 (deodorizing power + [1 IilO) 50 laid parts A mixture of 9 parts by weight of 1 powder and 1 part by weight of the powder was mixed well in a TW granule to obtain 1 part of granule 1' and 7-shaped 15 (preparation composition 60iJi).

Example 3 Breath odor removing composition for mouthwash; Mouthwash Freha-0.3 1n9 parts Pluronic P-85 (manufactured by Wyandoto Chemical Co.) 4.840 strength lamel 1% aqueous solution
1.0 Ethyl alcohol (95%) 20.3 Water 72.27 Sodium monofluorophosphate 0.7 Hinokitiol 1% alcohol solution 0.5 Composition of Example 1 0.09 Obtained mouthwash The deodorizing effect on methyl mercaptan and trimethylamine was measured per 1 mJ by the method described in Experimental Example 3.

As a result, 100% deodorizing effect on both methyl mercaptan and trimethylamine was confirmed. The headspace gas subjected to gas chromatography analysis was also determined to be substantially odorless by a sensory test conducted by an expert panel. This indicates that this mouthwash is an effective breath odor removing composition for all areas of halitosis.

Example 4 Chewing gum bad breath removal composition: Chewing gum base 20 @ Harube Sugar 55 Starch syrup 20 Fragrance 0.73 Composition of Example 2 0.27 Softener 4.0 Chewing gum was obtained using the above formulation in a conventional manner.

In order to examine the effectiveness of prototype chewing gum in removing bad breath, sensory tests were conducted on tobacco odor, garlic odor, and artificial odor. The evaluation criteria are shown in Table 2, and Table 3 shows the average of the evaluations by the five expert panels.

Smoking 3 Highlights at the same time for 3 minutes up to 2/3 of the cigarette odor causes 3 exhales! ! It is taken as bad breath immediately after smoking cigarettes,
Next, the prototype chewing gum Log was mixed for 3 minutes, and the breath 31 after chewing was taken out was taken to determine the bad breath immediately after tasting. The garlic smell is 100ml of garlic press juice diluted 200 times with water! ! The breath 31 after rinsing the mouth was taken to represent the garlic odor immediately after halitosis occurred, and the breath 31 after the chewing gum assembly was taken in the same manner as in the case of tobacco odor and was taken to represent the bad breath immediately after tasting. Artificial bad breath contains 10,100pp of hydrogen sulfide.
Methyl mercaptan sPpm.

After rinsing the mouth with 100 ml of an aqueous solution containing 10 ppm of dimethyl sulfide, the breath odor was collected in the same manner as for garlic odor.

Table 3 shows that this chewing gum is an effective breath odor removing composition across the entire spectrum of possible breath odor.

Example 5 Composition for removing bad breath from candy; Prescription: Sugar...50 parts by weight Starch syrup...50 Acidulant...0. 5 Orange flavor...0.1 Orange colorant..., tlIII amount Composition of Example 1...
0.1 Candies were obtained by blending the above formulation in a conventional manner. The deodorizing effect of eating one piece of this candy was measured in the same manner as the mouthwash of Example 3, and the same results were obtained. Also, unlike conventional methods that use chlorophyll, the fabric is virtually colorless, resulting in a beautiful orange color.

Example 6 Composition for removing bad breath from tablet confectionery: Prescription: Sugar...9.5 parts by weight Starch syrup...
1.0 Corn starch...0.5 Corn starch...0.5 10% gelatin aqueous solution...1.5 Appetizing agent...0.5 Yellow coloring agent...Lemon flavor in the right places... 0.1 Composition of Example 2……0
．． 1) The formulation described in 1 was blended in a conventional manner and compressed into tablets using two Jr. presses to obtain tablet confectionery. This tablet confectionery had exactly the same deodorizing effect as the candy of Example 5. Also, I was able to color it a beautiful lemon color.

Ta. Also, I was able to color it a beautiful lemon color.

Example 7 Bad breath removal composition for dentifrice: Formula Calcium diphosphate...50 rt 11 parts Glycerin...25 Water...19 Sodium lauryl sulfate...lCMC... ……………1
Satucalin sodium...0.2 Composition of Example 1...
.........0.15 The above formulation was thoroughly kneaded using a defoaming type n6 crusher to make a dentifrice. The deodorizing effect of this dentifrice was measured in the same manner as the chewing gum of Example 4, and as a result, similarly good deodorizing effect was obtained.

Then I bought toothpaste f4j. The deodorizing effect of this toothpaste was measured in the same manner as the chewing gum of Example 4, and the results were as follows:
Similarly, a good deodorizing effect was obtained.

〔Effect of the invention〕

According to the halitosis-removing composition of the present invention, it is possible to provide a halitosis-removing composition that can deodorize the entire area of halitosis substantially odorless by applying a very small amount, and does not stain or stain products.

Claims (1)

Scope of Claims: (1) A polar solvent extract of leaves of plants of the Camellia family that has a deodorizing potency of 1.0 when 1 ml of a 500 ppm aqueous solution of trimethylamine is required to substantially deodorize 1 ml of a 1000 ppm aqueous solution of trimethylamine. When stipulating that, the ratio of the blending amount n x (4.5 to 5.5) parts by weight of the specified extract to the deodorizing potency n of the specified extract and 1 part by weight of copper gluconate is used as the active ingredient. A halitosis removing composition that covers all areas of bad breath. (2) Leaves of plants in the Camellia family include tea plants, camellias, sasanqua flowers, and sakaki trees, including fresh leaves of these plants, leaves dried after heat inactivation of autooxidation enzymes, and fermented leaves treated with autooxidation enzymes. The bad breath removing composition according to claim 1. (3) Take 1 ml of a 1000 ppm aqueous solution of trimethylamine in a 100 ml wide-mouth bottle, add a predetermined amount of a 500 ppm aqueous solution of a leaf extract of a specified Camellia plant, shake for 5 minutes, and then analyze the headspace gas by gas chromatography (column: stationary phase liquid... 5% Lanpha, stationary phase support: Chromosorp W, inner diameter: 3 mm, length: 3 m glass tube, column temperature: 75°C, sample amount: 300 μl, carrier gas: helium, detector: hydrogen flame ionization detector). The predetermined amount nm that does not detect the peak of trimethylamine
Claim 1, in which the deodorizing potency n is determined by measuring l.
The bad breath removing composition described in Section 1. (4) The polar solvent extraction is thermal extraction using water, glycerin, ethylene glycol, propylene glycol, methyl alcohol, ethyl alcohol, isopropyl alcohol, acetone, methyl ethyl ketone, or a mixture thereof. A bad breath removing composition. (5) The leaf extract of the Camellia family is obtained by drying green tea to a moisture content of approximately 1%, pulverizing it to 50 mesh or less, heating and extracting it with a 20-80% glycerin aqueous solution, and separating the extract by centrifugation. The bad breath according to claim 1, which is an extract mainly composed of green tea flavonoids obtained by distilling off the solvent from the filtrate from which chlorophyll etc. have been removed by cooling the extracted liquid at 10° C. for 24 hours. Removal composition. (6) Regarding polar solvent extracts of leaves of Camelliaaceae plants, when 1 ml of a 500 ppm aqueous solution of the extract required to substantially deodorize 1 ml of a 1000 ppm aqueous solution of trimethylamine is defined as a deodorizing potency of 1.0. Bad breath over the entire range of halitosis containing as an active ingredient a blending amount n x (4.5 to 5.5) parts by weight of a given extract relative to the deodorizing potency n of the given extract and 1 part by weight of copper gluconate. A method for removing bad breath, which deodorizes the entire area of bad breath by using a mouth application selected from the group consisting of a mouthwash, chewing gum, candy, tablets, and toothpaste containing a removal composition. (7) In a polar solvent extract of leaves of Camelliaaceae plants, 0.0005 to 0.5% by weight of the extract and 0.0 copper gluconate per 1.0 of its deodorizing potency.
7. The method for removing bad breath that deodorizes the entire area of bad breath, which comprises a mouthwash, chewing gum, candy, tablets, and toothpaste containing 0.001 to 0.1% by weight.