JP6031902B2 - Two-layer separated liquid oral composition - Google Patents

Description

  The present invention relates to a two-layer separated type liquid oral composition that is improved in oil irritation during use and stickiness after use, and has excellent palatability and is particularly suitable as a mouthwash.

  Conventionally, it is a two-layer formulation that consists of an oil layer and a water layer containing water, and has a beautiful appearance and enjoyment. The liquid composition is separated into two layers when allowed to stand and is used by shaking. Is known, and Patent Document 1 (Japanese Patent Laid-Open No. 11-79962) proposes a two-phase liquid composition for oral cavity.

  However, a two-layer liquid oral composition composed of an oil layer and an aqueous layer, particularly when applied to the oral cavity as a mouthwash, is irritated by the oil during use, and after use, stickiness is found in the oral cavity. The remaining problem was in palatability.

JP-A-11-79962

  The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a two-layer separated liquid oral composition having improved palatability after use and improved stickiness after use. And

As a result of intensive studies to achieve the above object, the inventors of the present invention contain an oil agent (A) that is liquid at 25 ° C., and include menthol (B), thymol (C-1), and carvacrol (C -2) Oil layer containing one or more selected from 2) and one or more components (D) selected from rose, lavender, chamomile, jasmine, oris and violet; It has been found that by separating the layers, the oil irritation at the time of use and the stickiness after use are improved, and a two-layer separated liquid oral composition excellent in palatability can be obtained.
Furthermore, by adding one or more components (E) selected from organic acids, orthophosphoric acids and salts thereof to the water layer, the stickiness after use is further improved, and the interface between the two layers is cleaner. Found to separate.

Liquid oral compositions such as mouthwashes generally rarely contain a large amount of oil, but according to the present invention, two layers of an oil layer and an aqueous layer are separated upon standing. In the two-layer separating agent type liquid composition that mixes by shaking when used, the oil layer is selected from the component (B), the component (C-1) and the component (C-2) together with the oil agent (A). In combination with component (D) in combination with one or more of the above, even when the oil agent is blended in an amount of 10% by mass or more, the feeling of irritation at the time of use, which has been a drawback of the conventional two-layered type Thus, it is possible to provide a two-layer separated liquid oral composition that can reduce stickiness in the oral cavity after use, has excellent palatability, and can be suitably prepared especially as a mouthwash.
In addition, the applicant has separated two layers of an oil layer containing an oil agent that is liquid at 25 ° C. and an aqueous layer containing condensed phosphoric acid or a salt thereof into PCT / JP2012 / 55617, A two-layer separation type liquid oral composition that has a high effect of removing dirt from the teeth and has reduced oily feeling and astringent feeling because the content of the oil agent and the ratio of the oil agent to condensed phosphoric acid or a salt thereof are in an appropriate range. This was intended to reduce the oily feeling of the oil agent by condensed phosphoric acid or a salt thereof, and to reduce the astringent feeling of condensed phosphoric acid or salt thereof by the oil agent. Component (B), component (C) of the present invention -1) and the combination of the component selected from the component (C-2) and the component (D) are technically different from improvement of oil irritation and stickiness.

  Accordingly, the present invention contains an oil agent (A) that is liquid at 25 ° C., and at least one selected from menthol (B), thymol (C-1), and carvacrol (C-2). Two layers characterized by separating two layers, an oil layer containing at least one component (D) selected from rose, lavender, chamomile, jasmine, oris and violet, and an aqueous layer Provided is a separate liquid oral composition, wherein the aqueous layer contains one or more components (E) selected from organic acids, orthophosphoric acid and salts thereof, and the above two-layer liquid oral composition. .

  ADVANTAGE OF THE INVENTION According to this invention, the irritation | stimulation feeling of the oil at the time of use and the stickiness after use can be improved, and the two-layer separated type liquid oral cavity composition which has the outstanding palatability can be provided.

The present invention will be described in further detail below. The two-layer separated type liquid oral composition of the present invention comprises an oil layer and an aqueous layer separated into two layers. The oil layer comprises 10 to 60% by mass of an oil agent (A), menthol (B), thymol (C -1) and with one or more selected from carvacrol (C-2), rose, lavender, Ri Na contain the chamomile and Jasumi down or al least one component selected (D), Mass ratio with respect to the following component (A) is (D) / (A) = 0.00001-0.005, and when (B) component is included, (B) / (A) = 0.0001-01 .006, and when the component (C) is included, (C) / (A) = 0.00003 to 0.0006 .

Here, the two-layer separation type is separated into two layers of an aqueous layer and an oil layer at the time of standing, and when lightly shaken at the time of use, the two layers easily mix and become an emulsion, and then leave the original when left to stand. It is a preparation in a form that returns to two layers.
More specifically, here, the two-layer separation type preparation has an appearance that separates into two layers of an aqueous layer and an oil layer when left standing, and the two layers are easily mixed by shaking lightly during use. It becomes an emulsion, and after use it is shaken and left to stand, then it returns to the state separated into two layers. In this case, the product is left shaken and left to stand and separated into two layers within one hour at the latest. Just go back to. Furthermore, when this preparation is used after shaking, if the container is left standing without shaking or stirring, the two-layer separation state of the oil layer and the aqueous layer is stabilized and maintained. After that, they are mixed again, so that they can be used in an emulsion when used.

  Here, separating into two layers is as follows. When 60 mL of the composition is put into a 100 mL Epton tube and shaken up and down for 5 seconds at a rate of 3 times per second, when the shaking is stopped and the mixture is left to stand, the composition is generally composed of two layers. May have an oil layer at the boundary between the two layers, a dispersion layer of milky white water or fine particles of oil that are different in appearance from the water layer, etc. This is the case of 5% or less of the total volume of the water layer and the oil layer.

  The oil agent (A) contained in the oil layer is a liquid oil agent at 25 ° C., and is a component that gives the appearance characteristics of the product as a preparation separated into two layers. Here, the liquid at 25 ° C. means a liquid having a viscosity of 100 mPa · s or less when the viscosity is measured using a BL type viscometer in a 25 ° C. environment.

  Examples of the oil agent (A) include hydrocarbons, fatty acid esters of glycerin, fatty acid esters of alcohol, and silicones. Specifically, medium chain fatty acid triglycerides such as tri (caprylic acid / capric acid) glyceryl composed of fatty acids having 6 to 12 carbon atoms contained in liquid paraffin, coconut oil, palm kernel oil, milk, breast milk, jojoba oil, Examples include isopropyl myristate, octyldodecyl myristate, isopropyl palmitate, octyldodecyl palmitate, decyl oleate, dimethylpolysiloxane represented by the following formula (1), methylpolysiloxane, and the like, and one or more of these Is used. Among them, liquid paraffin, medium-chain fatty acid triglyceride, and isopropyl myristate are particularly preferable because they are less irritating.

（式中、ｍは１〜１０，０００の整数である。）

(In the formula, m is an integer of 1 to 10,000.)

  The blending amount of the component (A) is preferably 10 to 60% (mass%, the same applies hereinafter) of the whole composition, and more preferably 20 to 40%. When 10% or more is blended, the two layers become clear, and 60% or less is preferable for improving irritation and stickiness and improving palatability.

  In this invention, the irritation | stimulation in use by mix | blending combining 1 type, or 2 or more types chosen from a component (B), a component (C-1), and a component (C-2), and a component (D). The feeling and stickiness after use can be improved. When component (B), component (C-1) and component (C-2) are absent, or when component (D) is absent, irritation during use and stickiness after use cannot be improved.

As the menthol of component (B), in addition to synthetic menthol and natural menthol, menthol-containing essential oils such as peppermint oil and peppermint oil may be used. Synthetic menthol is good in terms of improving stickiness after use. For example, those manufactured by Takasago International Corporation can be used.
The amount of component (B) menthol is preferably 0 to 0.2% of the total composition, more preferably 0.005 to 0.2%, and still more preferably 0.01 to 0.1%. The stickiness can be improved as the blending amount increases, but it is preferably 0.2% or less because the feeling of irritation does not become a problem.

  Moreover, when mix | blending a component (B), (B) / (A) is preferably 0.0001-0.006 as a mass ratio with respect to a component (A), More preferably, it is 0.0003-0.004. It mixes in the ratio which becomes. A ratio of 0.0001 or more is suitable for improving stickiness and irritation, and a ratio of 0.006 or less is preferable because irritation does not cause a problem.

Component (C) is thymol (C-1) and / or carvacrol (C-2), and either thymol (C-1) or carvacrol (C-2) may be blended alone, Or you may mix | blend combining 2 types.
Component (C) thymol and carvacrol include synthetic products, natural isolated products, and essential oils containing thymol and / or carvacrol, such as thyme oil, oregano oil, origanum oil, ajowan oil, marjoram oil, etc. It may be used.
The amount of component (C) (thymol (C-1) and / or carvacrol (C-2)) is preferably 0 to 0.02%, more preferably 0.001 to 0.02 of the total composition. %, More preferably 0.002 to 0.01%. The stickiness can be improved as the blending amount increases, but it is preferably 0.02% or less because the feeling of irritation does not become a problem.

  Moreover, when mix | blending a component (C), (C) / (A) is preferably 0.00003-0.0006 as a mass ratio with respect to a component (A), More preferably, 0.00006-0.0004 It mixes in the ratio which becomes. It is suitable for improvement of stickiness and irritation to be 0.00003 or more, and is preferably 0.0006 or less because irritation does not cause a problem.

  In addition, a component (B), a component (C-1), and a component (C-2) may mix | blend any or a component (B) and a component (C-1) and / or in the point of an effect expression. You may use a component (C-2) together.

The component (D) is one or more components selected from rose, lavender, chamomile, jasmine, oris and violet, and among them, rose, lavender, chamomile and jasmine are particularly preferable for suppressing irritation. In particular, rose is more preferable from the viewpoint of reducing irritation during use.
Component (D), when combined with one or more selected from component (B), component (C-1) and component (C-2), greatly improves the feeling of irritation during use and stickiness after use. .

  Ingredient (D) is obtained by steam distillation or solvent extraction of all or part (flowers, leaves, stems, roots, etc.) of plants of rose, lavender, chamomile, jasmine, orris or violet. It is generally called oil, absolute, concrete, etc. Specific examples of the fragrance component used as the component (D) include rose oil, rose absolute, lavender oil, lavender absolute, chamomile oil, jasmine absolute, oris oil, oris concrete, violet absolute, and the like.

  The amount of component (D) is preferably 0.0002 to 0.1%, more preferably 0.002 to 0.05% of the entire composition. The greater the blending amount, the better the irritation feeling can be improved, but the range of 0.1% or less is preferable because the irritation feeling and stickiness do not become a problem.

  Component (D) is blended in such a ratio that (D) / (A) is preferably 0.00001 to 0.005, more preferably 0.00006 to 0.002 as a mass ratio with respect to component (A). . It is suitable for improvement of stickiness and irritation to be 0.00001 or more, and is preferably 0.005 or less because irritation does not cause a problem.

  In the oil layer, in addition to the components (A), (B), (C), and (D), other known oil-soluble components can be blended as necessary as long as the effects of the present invention are not hindered. For example, a fragrance | flavor, a pigment | dye, an active ingredient etc. are mentioned. Specifically, as the fragrance, a known amount other than the above components (B), (C) and (D) may be added in a normal amount within a range not impeding the effects of the present invention. ), Even in the case of a natural fragrance containing the component (C), the components (B) and (C) in the composition can be blended within a range in which the appropriate amounts are obtained. Examples of such perfumes include anise oil, eucalyptus oil, winter green oil, cassia oil, clove oil, sage oil, lemon oil, orange oil, cardamom oil, coriander oil, mandarin oil, lime oil, rosemary oil, Natural fragrances such as laurel oil, caraway oil, bay oil, lemongrass oil, pine needle oil, neroli oil, orange flower, and processing of these natural fragrances (front reservoir cut, rear reservoir cut, fractional distillation, liquid Liquid extraction, essence, powdered fragrance, etc.) and carvone, anethole, cineol, methyl salicylate, cinnamic aldehyde, eugenol, 3-l-menthoxypropane-1,2-diol, linalool, linalyl acetate , Limonene, menthone, menthyl acetate, N-substituted-paramentane-3-cal Xamide, pinene, octylaldehyde, citral, pulegone, carbyl acetate, anisaldehyde, ethyl acetate, ethyl butyrate, methyl anthranilate, vanillin, undecalactone, hexanal, ethyl alcohol, propyl alcohol, butanol, isoamyl alcohol, hexenol Well-known perfume materials used for oral compositions such as single product perfume such as dimethyl sulfide, cycloten, furfural, trimethylpyrazine, ethyl lactate, and ethylthioacetate can be used.

  Examples of the dye include oil-soluble dyes such as Red No. 215, Red No. 225, Yellow No. 201, and Yellow No. 204. Examples of the active ingredient include isopropylmethylphenol, triclosan, tocopherol acetate and the like. The blending amount of these optional components can be a normal amount as long as the effects of the present invention are not hindered.

In the present invention, it is preferable to further blend a component (E) selected from organic acids, orthophosphoric acid and salts thereof in the aqueous layer, and by blending the component (E), the stickiness after use can be further improved, Further, the interface between the two layers when allowed to stand can be separated more finely without causing emulsion-like white turbidity, thereby improving the appearance of the preparation.
Component (E) is an organic acid or a salt thereof, orthophosphoric acid or a salt thereof. Examples of the organic acid include citric acid, malic acid, and a sodium salt thereof, and orthophosphoric acid includes a hydrogen salt, and examples thereof include phosphoric acid, a sodium salt thereof, and a hydrogen phosphate salt. Specific examples include citric acid, sodium citrate, malic acid, sodium malate, sodium monohydrogen phosphate, sodium dihydrogen phosphate, trisodium phosphate, and the like. These 1 type can be used individually or in combination of 2 or more types from the point of effect expression.
In addition, the orthophosphoric acid of the component (E) is different from the condensed phosphoric acid, and the condensed phosphoric acid may not be contained in the present invention.

  When mix | blending a component (E), 0.01-2% of the compounding quantity is preferable with respect to the whole composition, More preferably, it is 0.05-1%. When it is 0.01% or more, the stickiness after use can be further improved, the interface between the two layers becomes cleaner, and the appearance of the preparation can be improved. It is suitable for suppressing irritation to be 2% or less.

  In the aqueous layer, a known water-soluble component other than the component (E) can be further blended as necessary within a range not impeding the effects of the present invention. For example, wetting agents, thickeners, sweeteners, pigments, preservatives, water-soluble fragrances, active ingredients and the like can be mentioned. In the present invention, the surfactant does not need to be blended, and when the surfactant is not included, the two layers are separated cleanly while the upper and lower layers are transparent, and the appearance of the preparation is further improved.

  Specific examples of the wetting agent include sugar alcohols such as sorbit, xylit, maltitol, and erythritol, and polyhydric alcohols such as glycerin, propylene glycol, polyethylene glycol, hexylene glycol, and butylene glycol.

  As thickeners, cellulose derivatives such as sodium carboxymethylcellulose, hydroxyethylcellulose, hydroxypropylcellulose, hydroxypropylmethylcellulose, methylcellulose, polyethylene glycol, xanthan gum, carrageenan, guar gum, sodium alginate, propylene glycol alginate, agar, sodium polyacrylate, Polyvinyl alcohol, polyvinyl pyrrolidone, gellan gum, pectin and the like can be mentioned.

  As sweeteners, sodium saccharin, aspartame, sucralose, acesulfame K, xylitol, stevia extract, etc. As dyes, red No. 2, red No. 3, red No. 106, red No. 102, yellow No. 4, yellow No. 5, orange No. 205, Examples of water-soluble dyes such as Blue No. 1 and Green No. 3 and preservatives include paraoxybenzoic acid esters such as methylparaben, sodium benzoate, and the like.

Active ingredients include: fluorides such as sodium fluoride, sodium monofluorophosphate, tin fluoride, enzymes such as epsilon aminocaproic acid, dextranase, mutanase, tranexamic acid, allantochlorohydroxyaluminum, hinokitiol, lauroyl sarcosine sodium, Ascorbic acid, dihydrocholesterol, α-bisabolol, chlorhexidine salts, azulene, dipotassium glycyrrhizinate, copper chlorophyllin sodium, chlorophyll, copper gluconate and other copper compounds, aluminum lactate, strontium chloride, potassium nitrate, berberine, zinc citrate, buckwheat extract, Examples include chamomile, clove, rosemary, ougon, safflower extracts.
These optional components can be blended in a usual amount as long as the effects of the present invention are not impaired.

The solvent is usually water, but a lower monohydric alcohol such as ethanol may be further blended within a range that does not hinder the effects of the present invention.
Moreover, it is preferable to adjust pH in 25 degreeC to 6.5-8.5 for the two-layer separated type liquid oral cavity composition of this invention.

  The ratio of the water layer to the oil layer (water layer / oil layer) in the two-layer separated liquid oral composition is preferably 0.6 to 9, more preferably 0.6 to 6, and still more preferably 1 to 1 in terms of mass ratio. 5. A value of 0.6 or more is preferred for improving the feeling of irritation and stickiness, and a value of 9 or less is preferred from the viewpoint of easily recognizing that there are two layers.

  The two-layer separated liquid oral composition of the present invention is separated into two layers of an aqueous layer and an oil layer when left standing, but the two layers are easily mixed by shaking lightly during use. Thus, it can be applied to the oral cavity in this state, and it is preferably applied by rinsing the mouth.

  EXAMPLES Hereinafter, although an Example and a comparative example are shown and this invention is demonstrated concretely, this invention is not restrict | limited to the following Example. In the following examples, “%” means “% by mass” unless otherwise specified.

Examples and comparative examples
Two-layer separated liquid oral compositions having the compositions shown in Tables 1 to 8 were prepared by the following method. The following evaluation was performed about the obtained 2 layer separation type liquid oral cavity composition. The results are shown in the table.

<Method for Preparing Two-layer Separable Liquid Oral Composition>
Dissolve water-soluble components (sodium saccharin, glycerin, organic acid, etc.) in water, dissolve oil-soluble components (menthol (B), component (C), component (D), methylparaben, etc.) in oil agent (A), and Were mixed at a fixed ratio. The composition of the comparative example was prepared according to the above.

<Evaluation method>
(1) Evaluation of lack of irritation The composition shown in the table was lightly shaken at the time of use, and the two layers were mixed, and 20 mL of this composition was contained in the mouth. Evaluation was made in 5 stages, and the average score of 10 people was shown in the table as ◎, ○, Δ, × according to the following criteria.
Criterion 5: No irritation was observed.
4: The irritation was hardly recognized.
3: Slight irritation was observed.
2: A feeling of irritation was observed.
1: Strong irritation was recognized.
Evaluation criteria A: Average point of 4.0 points or higher B: Average point of 3.0 points or higher and lower than 4.0 points Δ: Average point of 2.0 points or higher and lower than 3.0 points Less than 0

(2) Evaluation of non-stickiness after use The composition shown in the table was lightly shaken at the time of use, and the two layers were mixed, and 20 ml of this composition was included in the mouth, and the mouth was rinsed for 30 seconds. The average score of 10 people was shown in the table with ☆, ◎, ○, Δ, × according to the following criteria.
Criterion 5: Stickiness was not recognized.
4: Stickiness was hardly recognized.
3: Slight stickiness was recognized.
2: Stickiness was recognized.
1: Strong stickiness was recognized.
Evaluation criteria ☆: Average point 4.5 points or more ◎: Average point 4.0 points or more and less than 4.5 points ○: Average point 3.0 points or more and less than 4.0 points △: Average point 2.0 points or more Less than 0 ×: Average score 1.0 or more and less than 2.0

(3) Evaluation of cleanliness of interface between two layers 50 mL of the composition shown in the table was put into a PET cylindrical shape (diameter 40 mm × height 120 mm) and shaken and mixed at a speed of 20 times for 10 seconds. Then, after standing still for 30 minutes, the state of the interface between the oil layer and the water layer was observed from the side surface, evaluated in the following four stages, and indicated by ◎, ○, Δ, and × in the table.
Judgment criteria A: Emulsion-like white turbidity is not recognized at the interface.
○: Emulsion-like white turbidity is slightly observed at the interface, but it is at a level that causes no problem in appearance.
Δ: Emulsion white turbidity is slightly observed at the interface.
X: Emulsion-like cloudiness is observed at the interface.

Details of the raw materials used are shown below.
Liquid paraffin: manufactured by Sanko Chemical Co., Ltd., liquid paraffin No. 70S
Tri (caprylic acid / capric acid) glyceryl: NOF Corporation, Panacet 810
Isopropyl myristate: NOF Corporation, IPM-R
Isopropyl palmitate: NOF Corporation, IPP-R
Menthol: manufactured by Takasago International Corporation, menthol JP
Thymol: Takasago International Corporation Carvacrol: Takasago International Corporation Rose Absolute: Hasegawa Inc. Lavender Oil: Takasago International Inc. Chamomile Oil: Ve Manfis Inc. Jasmine Absolute: Ve Manfis Fragrance Co., Ltd. Oris Concrete: Hasegawa Fragrance Co., Ltd. Violet Absolute: Hasegawa Fragrance Co., Ltd.

＊；（Ｂ）、（Ｃ）、（Ｄ）成分を含まない香料。

*: A fragrance not containing the components (B), (C), and (D).

Claims (7)

Containing 10-60 mass% of oil agent (A) which is liquid at 25 ° C,
One or more selected from menthol (B), thymol (C-1) and carvacrol (C-2);
Rose, the oil layer comprising lavender, and chamomile and Jasumi down or al least one component selected (D),
Are two layers name separated with the aqueous layer, the mass ratio following components (A),
(D) / (A) = 0.0001-0.005,
When (B) component is included,
(B) / (A) = 0.0001 to 0.006,
When (C) component is included,
(C) / (A) = 0.00003-0.0006
Two layers separated liquid oral composition, characterized in that it.   The two-layer separated liquid oral composition according to claim 1, wherein the oil agent of component (A) is at least one selected from hydrocarbons, fatty acid esters of glycerin, fatty acid esters of alcohol and silicones. The content of the oil component (A) is a 2 0-4 0% by weight of the total composition according to claim 1 or 2 2-layer separation type liquid oral composition according.   The two-layer separated liquid oral composition according to claim 1, 2 or 3, wherein the content of the menthol of component (B) is 0.005 to 0.2 mass% of the whole composition.   The two layers according to any one of claims 1 to 4, wherein the content of thymol (C-1) and / or carvacrol (C-2) is 0.001 to 0.02 mass% of the entire composition. Separable liquid oral composition.   The two-layer separated liquid oral composition according to any one of claims 1 to 5, wherein the content of the component (D) is 0.0002 to 0.1 mass% of the entire composition.   The two-layer separated liquid oral composition according to any one of claims 1 to 6, wherein the aqueous layer further contains one or more components (E) selected from organic acids, orthophosphoric acids and salts thereof.