JPH0712374B2 - Liquid deodorant composition - Google Patents

Description

TECHNICAL FIELD The present invention relates to a liquid deodorant composition exhibiting a good deodorizing effect on methyl mercaptan and the like, and is particularly less colored and does not cause stains or tingling. The present invention relates to a deodorant composition.

[Conventional technology]

It has been conventionally practiced to extract a plant containing a component having a deodorant action with various solvents and use the obtained plant extract as a deodorant. For example, Lamiaceae plants (JP-A-57-204278) and clove (JP-A-58-39615).
No.), Daihuang, Eleuthero, Japanese radish, Japanese koboku, Japanese cypress (leaf), Suhou, Renja, Purple root, Crustacea, Bractum, Burkki, Japanese pepper, Carrot grass, Japanese moss (JP-A-60-77763), White birch , Itohimehagi, pomegranate, Achillea millefolium, Linden, Coptis, Coptis (JP-A-61-2409)
It is known to use the plant extract of No. 60) as a deodorant. In addition, leaves, buds and dried products of Salixaceae plants such as weeping willow and poplar (JP-A-60-111659), Pinaceae plants (60-119951), Cedar plants (60-119952).
No.), eucalyptus, etc.
It is also known to use extracts of quince (No. 60-119954) and fennel (No. 61-260012).

However, the above method is a method in which a specific plant is extracted with a specific solvent, and if the extract is stored for a long period of time, there is a problem that it is colored or tingling or dull occurs. .

[Problems to be solved by the invention]

Therefore, it is an object of the present invention to provide a deodorant composition containing, as a deodorant component, a plant extract that does not become colored even if stored for a long period of time and does not cause stagnation or sediment.

[Means for solving problems]

The present invention, after extracting a plant containing a deodorant component with water or an aqueous lower alcohol, a specific solvent is added to color, nigori, and if a substance causing ori is forcibly precipitated and removed,
This was done based on the finding that the above problems can be effectively solved.

That is, the present invention contains water or aqueous lower alcohol solvent extract from a plant containing a deodorant component, which is obtained by adding a lower alcohol having a higher alcohol concentration than the extraction solvent and removing the generated precipitate. A characteristic liquid deodorant composition is provided.

In the present invention, any plant can be used as long as it contains a deodorant component, and various parts such as plant flowers, leaves, stems and bark, preferably dried products thereof can be used. Specific examples of such plants include Lamiaceae plants, cloves, rhubarb,
Eleuthero, Chinese cabbage, Japanese cabbage, Japanese lacquer tree, Suho, Lianx, Purple root, Cicada bark, Bamboo bark, Burdock, Japanese pepper, Carrot grass, Pleurotus cornucopiae, Birch, Itohimehagi, Pomegranate, Sawtooth orchid, Linden, Coleoptera, Cercis chinensis and more. Examples include Salixaceae plants such as poplar, Pinaceae plants, Cryptomeriaceae plants, Eucalyptus plants such as Eucalyptus plants, Scutellariae plants, Fennel, Killi, Holly oyster daisies, butterflies, dokudami, purple oxalis and the like.
In the present invention, the target plant is not limited to these, and various other plants can be used. Among these plants, it is particularly preferable to use Lamiaceae plants such as sorghum, Clove, Eleuthero, lacquer grass, and primrose grass.

In order to obtain the deodorant component used in the present invention, the above plant is first extracted with water or an aqueous lower alcohol. For example, the amount is 3 to 20 times (weight) with respect to the dry powder of the plant, more preferably 5
~ 10 times amount of water / lower alcohol is 100/0 ~ 10/90 (weight ratio), preferably 70/30 ~ 30/70 solvent is used, extraction is carried out at 10 ~ 50 ° C, and the extraction residue is filtered off. Obtain the extract. Examples of the lower alcohol include alcohols having 1 to 3 carbon atoms, and ethanol is particularly preferably used.

In the present invention, with respect to the extract, an aqueous lower alcohol having a higher alcohol concentration than the extract used for the extraction or
Add 100% lower alcohol. As the aqueous lower alcohol, it is preferable to use one having a concentration of 10 to 100% by weight (hereinafter, abbreviated as%). By such an operation, the alcohol concentration in the extract is 5 to 98%, preferably 20%.
It is increased by -40% to forcibly precipitate a coloring component and a component that causes dust and slag, and this is filtered to obtain an extract used in the present invention.

The amount of the above extract to be added to the deodorant composition is arbitrary,
It is preferably 0.0001 to 50%, particularly 0.001 to 5% of the total composition.

In the present invention, the above deodorant active ingredient can be used alone, but can also be used in combination with other active ingredients.

The deodorant composition of the present invention can be used in various forms as long as it is in a liquid state, and other appropriate components can be mixed depending on the application. For example, when preparing a mouthwash, a thickener, a surfactant, a sweetener, a flavoring agent, a preservative, a coloring agent, etc. are used, and further lysozyme chloride, dextranase, lytic enzyme, mutanase, chlorhexidine or Its salt, sorbic acid, alexidine, hinokitiol, cetylpyridinium chloride, alkylglycine, alkyldiaminoethylglycine salt, allantoin, ε-aminocaproic acid, tranexamic acid, azulene, vitamin E, sodium monofluorophosphate, sodium fluoride, fluorinated Active ingredients such as stannous tin, water-soluble or dibasic phosphates, quaternary ammonium compounds, and sodium chloride can also be added.

Also, in the case of household and industrial deodorants, depending on the type,
Ingredients usually used in liquid deodorants can be added, for example, antioxidants, surfactants, and fragrances can be added.

〔The invention's effect〕

The present invention provides a stable deodorant composition that is free from the stagnation and tingling that occur during long-term storage at low temperatures, which has been a conventional defect while maintaining a high deodorizing power.

Therefore, the liquid deodorant composition of the present invention can be used as a mouthwash, a liquid mouth freshener such as a breath freshening spray, a liquid oral composition such as a liquid toothpaste, for garbage, for refrigerators, for indoor use, Widely used as a domestic deodorant for cars, toilets, etc., an industrial deodorant that removes offensive odors generated from sewage treatment plants, fish processing plants, fish meal manufacturing plants, livestock manure and chicken manure drying plants, pulp mills, etc. To be done.

Next, the present invention will be described with reference to examples, but the present invention is not limited thereto.

〔Example〕

 An example of producing the plant extract used in the examples is shown below.

Production Example To a powder of clove leaf, 5 times amount of water / ethanol mixture for extraction was added to the powder amount, and the mixture was subjected to shaking extraction at room temperature for 1 hour. Then, the extract was centrifugally filtered with a 200-mesh filter cloth, and the filtrate was further naturally filtered with Toyo filter paper No. 2. The same amount of purified water / ethanol mixed solution was added to this filtrate, and the mixture was stirred for 30 minutes. The precipitate generated at this time was removed by filtering again with Toyo filter paper No. 2.

Accurately take a portion (about 3 g) of this filtrate in a weighing bottle,
After drying at 0 ° C. for 5 hours, the dry solid content was calculated from the weight loss.
Based on the calculated dry solid content, the same extraction water and ethanol mixed solution as described above were added to the filtrate to give a dry solid content of 2
Adjusted to be%.

Each of the extracts was obtained in the same manner as the above method using Rhodophyllum japonicus or Eleuthero rhizome instead of the clove leaves.

Example 1 According to the above method, the deodorant active ingredient liquid purified (inventive products 1 to 3) and the plant extracted deodorant active ingredient liquid not purified for comparison (comparative products 4 to 6 are all dried solids). Minute 2
%), And the deodorizing power, the degree of coloring, and the occurrence of sediment were evaluated by the following methods.

Deodorizing power 25μ of deodorant active ingredient liquid (dry solid content 2%) obtained by the above method and 0.975ml of purified water in a test tube with an internal capacity of about 22-23ml.
Add 1 ml of purified water for control, and
The pH was adjusted to 7.5 by adding 0.1 M phosphate buffer solution. To this was added 0.5 ml of a 10% by volume aqueous ethanol solution containing 1 μg / ml of methyl mercaptan (0.5 μg of methyl mercaptan), a silicon stopper was immediately added, and the mixture was vigorously stirred for 1 minute. Then, after standing still at 37 ° C. for 6 minutes, 5 ml of air was injected into the test tube by piercing the silicon stopper with a gas syringe for gas chromatography. After vigorously stirring for 30 seconds, 5 ml of gas was similarly sampled from the head space with a gas syringe and immediately injected into the gas chromatograph, the integral count of methyl mercaptan was measured, and the deodorization rate was calculated from the following formula. The gas chromatograph used was Hitachi 163.

C: Integrated count of control S: Integrated count of sample Degree of coloring Deodorant active ingredient liquid obtained by the above method (dry solid content 2%)
Mix 100μ with 10ml of purified water, and add 400
The absorbance at nm was measured by an absorbance meter (UV-260 manufactured by Shimadzu Corporation) using a quartz cell having a thickness of 1 cm, and the degree of coloring was evaluated from the measured value.

Occurrence of sediment Deodorant active ingredient liquid obtained by the above method (dry solid content 2%)
Was added to a mouthwash having the following composition.

Mouthwash Ethanol 10% by weight Glycerin 5 Perfume 1 Deodorant active ingredient solution 2 Saccharin 0.01 Polyoxyethylene propylene glycol 2 Methyl paraoxybenzoate 0.5 Water Residual 100.0% by weight Then, this mouthwash was stored at -5 ° C for 3 months. After that, the occurrence state of the cage was visually observed and evaluated according to the following criteria.

Evaluation criteria for occurrence of sediment +: Presence of sediment can be confirmed by tilting the container.

±: When the container is tilted and the liquid surface touches the bottom of the container, the presence of the sediment can be confirmed.

-: The orientation cannot be confirmed.

The results are summarized in Table 1.

From the results in Table 1, the deodorant active ingredient liquids (No. 4 to 6) without purification treatment by addition of ethanol have a high absorbance measurement value and a large degree of coloring, and when blended in a mouthwash, they can be used at low temperatures for a long time. While storage causes slag, deodorant active ingredient liquid purified by adding ethanol (No. 1 ~
It was confirmed that 3) had an excellent deodorizing power and had a small degree of coloring, and that even if it was added to a mouthwash and stored at a low temperature for a long period of time, almost no sediment was generated.

Example 2 To a dry powder of thyme leaves, which is a Lamiaceae plant, was added a mixed solution of an extraction solvent water: ethanol (1: 1) in an amount of 8 times the powder weight, and the mixture was shake-extracted at room temperature for 1 hour. Then extract 20
After centrifugal filtration with a 0 mesh filter cloth, the filtrate was further naturally filtered through Toyo filter paper No. 2. To this filtrate, 1/4 amount of 99% methanol as a solvent for purification was added and stirred for 30 minutes. The resulting precipitate was removed by filtering with Toyo Filter Paper No. 2. This was prepared in the same manner as above so that the dry solid content was 2%.

This extract is also a defect of conventional unrefined products while maintaining high deodorizing power, which is caused by long-term storage at low temperature,
It was confirmed that a stable deodorant composition without stagnation can be provided.

Example 3 To a dried powder of rosemary leaves, which is a Lamiaceae plant, was added an 8-fold amount of extraction water: ethanol (2: 1) mixture to the powder amount, and the mixture was shake-extracted at room temperature for 1 hour. Then, the extract was centrifugally filtered with a 200-mesh filter cloth, and the filtrate was further filtered with Toyo Filter Paper N.
It was gravity filtered at o.2. 1/5 amount of purification solvent for this filtrate
99% Propanol was added and stirred for 30 minutes. The resulting precipitate was filtered off with Toyo Filter Paper No. 2 and removed, and then the dry solid content was adjusted to 2%.

This extract is also a defect of conventional unrefined products while maintaining high deodorizing power, which is caused by long-term storage at low temperature,
It was confirmed that a stable deodorant composition without stagnation can be provided.

Example 4 Various composition liquids were prepared using the deodorant active ingredient liquids (invention products 1 to 3) used in Example 1.

Deodorant spray Ethanol 50% Dichlorodifluoromethane 45 Clove extract (Invention product 1) 5 Total 100% Liquid deodorant No. 1 Ethanol 50% Fragrance 1 Ogon extract (Invention product 2) 20 Water Residual 100% Liquid deodorant No.2 Ethanol 30% Fragrance 1 Eleuthero extract (Invention product 3) 10 Benzethonium chloride 0.02 Water Residual 100% Mouthwash No.1 Ethanol 30% Glycerin 15 Polyoxyethylene sorbitan monooleate (Twin 8
0) 1 Saccharin 0.1 Fragrance 1 Heavyweight 0.8 Clove extract (Product 1 of the present invention) 0.5 Water Residual 100% Mouthwash No. 2 Ethanol 20% Solbit 5 Polyexethylene ethylene hydrogenated castor oil 2 Fragrance 1 Saccharin 0.1 Sardine extract ( Inventive product 2) 3 Water Residual 100% Mouthwash No.3 Ethanol 25% Perfume 1 Polyoxyethylene propylene glycol 3 Saccharin 0.05 Methyl paraoxybenzoate 0.5 Sodium hydroxide 0.001 Sodium fluoride 0.1 Eleuthero extract (Inventive product 3 ) 1 Blue No. 1 0.001 Water 100% remaining

Claims (1)

[Claims] 1. A solution obtained by adding a lower alcohol having a higher alcohol concentration than the extraction solvent to a water or aqueous lower alcohol solvent extraction solution from a plant containing a deodorant component and removing the formed precipitate. A characteristic liquid deodorant composition.