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JP2015086149A - Fine emulsion composition for oral cavity and liquid composition for oral cavity containing the same - Google Patents

Fine emulsion composition for oral cavity and liquid composition for oral cavity containing the same Download PDF

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JP2015086149A
JP2015086149A JP2013224306A JP2013224306A JP2015086149A JP 2015086149 A JP2015086149 A JP 2015086149A JP 2013224306 A JP2013224306 A JP 2013224306A JP 2013224306 A JP2013224306 A JP 2013224306A JP 2015086149 A JP2015086149 A JP 2015086149A
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oral cavity
fine emulsion
composition
emulsion composition
components
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直紀 金子
Naoki Kaneko
直紀 金子
由紀 ▲柳▼
由紀 ▲柳▼
Yuki Yanagi
金華 李
Kinka Ri
金華 李
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Cosmos Technical Center Co Ltd
Nikko Chemicals Co Ltd
Nippon Surfactant Industries Co Ltd
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Cosmos Technical Center Co Ltd
Nikko Chemicals Co Ltd
Nippon Surfactant Industries Co Ltd
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Abstract

PROBLEM TO BE SOLVED: To prepare an aqueous fine emulsion composition in which a fine emulsion can be stably and easily blended in a liquid composition for an oral cavity.SOLUTION: When an oily component is dispersed in a water phase as a fine emulsion, an oily component, a surfactant and a polyol are blended in a specific ratio to obtain an excellent stability. That is, there is provided: a fine emulsion composition having an average particle diameter of 100 nm or less which contains the following components (A) to (D) as essential components and in which the ratio (mass ratio) of the components (A) to (C) is (A)/(B)=70/30 to 30/70 and [(A)+(B)]/(C)=90/10 to 60/40; and a liquid composition for an oral cavity obtained by blending the above components. (A) An oily component, (C) A polyoxyethylene cured castor oil, (B) A polyol and (D) Water.

Description

本発明は、液体口腔用組成物に安定に配合する事が可能な平均粒子径100nm以下の微細エマルション組成物および、この微細エマルション組成物を配合する液体口腔用組成物に関する。   The present invention relates to a fine emulsion composition having an average particle diameter of 100 nm or less that can be stably blended in a liquid oral composition, and a liquid oral composition containing the fine emulsion composition.

近年、洗口剤、マウスウォッシュ等の液体口腔用組成物に関して、エマルションタイプの口腔用組成物の配合成分や製造プロセスについての種々の検討がなされている。たとえば特許文献1には、油性成分を油相に含む特定成分のエマルションを別に調製し、エタノールを含有する液体口腔用組成物に添加することにより、エタノール由来の刺激を抑制し、なおかつ安定性も良好な液体口腔用組成物を得る方法が提案されている。特許文献2には、油性成分、ノニオン界面活性剤、エタノールを混合した油性混合液と、アニオン界面活性剤をクラフト点以上の温度で水に溶解させて調製したアニオン界面活性剤水溶液をそれぞれ調製し、これらを混合することにより、外観の経時安定性に優れた液体口腔用組成物を得る方法が提案されている。さらに、特許文献3には、特定の比率の有効成分、多価アルコール、(ポリ)グリセリン脂肪酸エステル、(ポリ)グリセリン脂肪酸エステルに該当しないノニオン界面活性剤及びアニオン界面活性剤とを混合してなる油相を水相中に投入してエマルションとすることを特徴とする口腔用組成物の製造方法が提案されている。   In recent years, regarding liquid oral compositions such as mouthwashes, mouthwashes, and the like, various studies have been made on the components and manufacturing processes of emulsion-type oral compositions. For example, in Patent Document 1, an emulsion of a specific component containing an oily component in an oil phase is separately prepared and added to a liquid oral composition containing ethanol, thereby suppressing irritation derived from ethanol and also having stability. A method for obtaining a good liquid oral composition has been proposed. In Patent Document 2, an oily mixed solution in which an oily component, a nonionic surfactant and ethanol are mixed, and an anionic surfactant aqueous solution prepared by dissolving an anionic surfactant in water at a temperature above the Kraft point are prepared. There has been proposed a method for obtaining a liquid oral composition having excellent appearance stability over time by mixing them. Further, Patent Document 3 is a mixture of an active ingredient having a specific ratio, a polyhydric alcohol, a (poly) glycerin fatty acid ester, a nonionic surfactant and an anionic surfactant that do not correspond to the (poly) glycerin fatty acid ester. There has been proposed a method for producing an oral composition characterized in that an oil phase is introduced into an aqueous phase to form an emulsion.

特開2005−179231号公報JP 2005-179231 A 特開2007−197411号公報JP 2007-197411 A 特開2011−168506号公報JP 2011-168506 A

しかしながら、特許文献1〜3に記載の方法の場合には、配合工程が多く、製造プロセスが煩雑であり、さらには高圧ホモジナイザーなどの高剪断タイプの乳化装置を使用する必要があるなどの問題点がある。また、これらの方法で得られた口腔用組成物は、経時的に濁りやオリ、クリーミングが生じる場合があり、安定性が十分ではなかった。
本発明は、上記実状に鑑み、安定性が良好でなおかつ簡便に液体口腔用組成物へ配合することができる水系の微細エマルション組成物を調製することを目的とした。
However, in the case of the methods described in Patent Documents 1 to 3, there are many compounding steps, the manufacturing process is complicated, and further, it is necessary to use a high shear type emulsifier such as a high pressure homogenizer. There is. Moreover, the composition for oral cavity obtained by these methods may generate turbidity, orientation and creaming over time, and its stability is not sufficient.
The present invention has been made in view of the above circumstances, and an object thereof is to prepare an aqueous fine emulsion composition that has good stability and can be easily blended into a liquid oral composition.

本発明者らは鋭意研究を重ねた結果、水相中に油性成分を微細エマルションとして分散させる際、油性成分、界面活性剤およびポリオールを特定の比率で配合することにより、優れた安定性が得られることを見出した。なおかつこの微細エマルションの調製方法は非常に簡便であり、上記課題が解決されることを見出し、本発明を完成するに至った。   As a result of intensive studies, the present inventors have obtained excellent stability by mixing the oil component, surfactant and polyol in a specific ratio when dispersing the oil component as a fine emulsion in the aqueous phase. I found out that And the preparation method of this fine emulsion is very simple, discovered that the said subject was solved, and came to complete this invention.

本発明は、特定成分の組合せにより、安定な微細エマルション組成物としてあらかじめ調製することにより、従来では安定に配合が困難であった液体口腔用組成物にも容易に配合することが可能な、口腔用微細エマルション組成物である。本口腔用微細エマルション組成物の調製には、高圧ホモジナイザーのような高剪断タイプの乳化装置を使用する必要がなく、またこの口腔用微細エマルション組成物を用いて調製した液体口腔用組成物は、従来の調製方法で調製した液体口腔用組成物と比較して、その処方成分が同じであるにもかかわらず、経時的にクリーミングや層分離等を生じず、非常に安定であった。   The present invention provides an oral cavity that can be easily blended into a liquid oral composition, which has been difficult to be blended stably in the past, by preparing in advance as a stable fine emulsion composition by combining specific components. It is a fine emulsion composition. The preparation of this oral fine emulsion composition does not require the use of a high shear type emulsifying device such as a high-pressure homogenizer, and the liquid oral composition prepared using this fine oral emulsion composition comprises: Compared with the composition for liquid oral cavity prepared by the conventional preparation method, although the formulation components were the same, it did not cause creaming or layer separation over time and was very stable.

本発明に使用される成分(A)の油性成分としては、任意に選択することができる。具体例としては、スクワラン、流動パラフィン、エステル油等が挙げられ、一種を単独で用いても良く、二種以上を併用しても良い。また、必要に応じてトリクロサン、イソプロピルメチルフェノール等の殺菌剤、メントール、ペパーミント油等の香料成分、天然精油成分等の、液体口腔用組成物の構成成分として重要な成分を配合しても良い。   The oil component of the component (A) used in the present invention can be arbitrarily selected. Specific examples include squalane, liquid paraffin, ester oil and the like. One kind may be used alone, or two or more kinds may be used in combination. Moreover, you may mix | blend an important component as components of liquid oral compositions, such as fungicides, such as a triclosan and isopropylmethylphenol, fragrance | flavor components, such as menthol and peppermint oil, and a natural essential oil component, as needed.

本発明に使用される成分(B)のポリオキシエチレン硬化ヒマシ油としては、平均ポリオキシエチレン付加モル数が10〜40モルであることを特徴とし、具体的にはNIKKOL HCO−10、HCO−20、HCO−30、HCO−40、HCO−40(医薬用)(日光ケミカルズ社製)などが挙げられ、これらの1種または2種以上を組み合わせて使用することができる。   The polyoxyethylene hydrogenated castor oil as the component (B) used in the present invention is characterized in that the average polyoxyethylene addition mole number is 10 to 40 moles, specifically, NIKKOL HCO-10, HCO- 20, HCO-30, HCO-40, HCO-40 (for pharmaceutical use) (manufactured by Nikko Chemicals Co., Ltd.) and the like, and one or more of these can be used in combination.

本発明に使用される成分(C)のポリオールとしては、プロピレングリコール、1,3−ブチレングリコール、ジプロピレングリコール、ペンチレングリコール、グリセリン、ソルビトールなどがあり、特に好ましくは1,3−ブチレングリコール、ジプロピレングリコール、ペンチレングリコールである。   Examples of the polyol of component (C) used in the present invention include propylene glycol, 1,3-butylene glycol, dipropylene glycol, pentylene glycol, glycerin, sorbitol, and the like, particularly preferably 1,3-butylene glycol, Dipropylene glycol and pentylene glycol.

本発明において、成分(A)〜(C)の比率(質量比)は、(A)/(B)=70/30〜30/70かつ[(A)+(B)]/(C)=90/10〜60/40の範囲にあるとき、さらに好ましくは(A)/(B)=60/40〜40/60かつ[(A)+(B)]/(C)=90/10〜70/30の範囲において、口腔用微細エマルション組成物がより安定に調製できる。
なお、(A)/(B)=70/30より上の比率では、油性成分に対して界面活性剤量の割合が少なすぎて、安定な口腔用微細エマルション組成物を得ることができず、逆に(A)/(B)=30/70より下の比率では、界面活性剤が水中で形成する高次分子集合体が強固なゲルとなり、調製時に強い機械力が必要となってしまう。
また、[(A)+(B)]/(C)=90/10より上の比率では、前述と同様に界面活性剤が水中で高次分子集合体を形成してしまい、強固なゲル構造を分散させるために強い機械力が必要となり、逆に[(A)+(B)]/(C)=60/40よりも下の比率では、ポリオールが界面活性剤の溶剤として機能してしまい、安定な口腔用微細エマルション組成物を形成することができない。
In the present invention, the ratio (mass ratio) of the components (A) to (C) is (A) / (B) = 70/30 to 30/70 and [(A) + (B)] / (C) = When in the range of 90/10 to 60/40, more preferably (A) / (B) = 60/40 to 40/60 and [(A) + (B)] / (C) = 90/10 In the range of 70/30, the fine emulsion composition for oral cavity can be prepared more stably.
In the ratio above (A) / (B) = 70/30, the ratio of the surfactant amount to the oil component is too small to obtain a stable fine oral emulsion composition. On the other hand, when the ratio is lower than (A) / (B) = 30/70, the higher-order molecular assembly formed by the surfactant in water becomes a strong gel, and a strong mechanical force is required during preparation.
In addition, when the ratio is higher than [(A) + (B)] / (C) = 90/10, the surfactant forms a high-order molecular assembly in water as described above, and a strong gel structure. In order to disperse the polymer, a strong mechanical force is required. Conversely, at a ratio lower than [(A) + (B)] / (C) = 60/40, the polyol functions as a solvent for the surfactant. A stable oral fine emulsion composition cannot be formed.

本発明の微細エマルション組成物は、成分(A)〜(D)のみで構成されてもよく、あるいは本発明の効果を損なわない範囲において、一般に化粧料に使用される界面活性剤、高級アルコール、アルキルグリセリルエーテル、脂肪酸、油性原料、活性成分、保湿成分、抗菌成分、粘度調整剤、安定化剤、色素、香料などを併用することもできる。   The fine emulsion composition of the present invention may be composed of only components (A) to (D), or a surfactant generally used in cosmetics, a higher alcohol, as long as the effects of the present invention are not impaired. Alkyl glyceryl ethers, fatty acids, oily raw materials, active ingredients, moisturizing ingredients, antibacterial ingredients, viscosity modifiers, stabilizers, pigments, fragrances and the like can also be used in combination.

本発明の口腔用微細エマルション組成物は、成分(A)〜(D)やその他の任意の原料をあらかじめ融解混合して均一な混合物とし、それを攪拌しながら室温まで冷却することで、半透明〜微白色乳化組成物として得ることができる。   The fine emulsion composition for oral cavity of the present invention is semitransparent by melting and mixing components (A) to (D) and other arbitrary raw materials in advance to form a uniform mixture and cooling it to room temperature while stirring. -It can be obtained as a slightly white emulsion composition.

上記成分により構成される本発明の口腔用微細エマルション組成物は、平均粒子径が100nm以下であり、好ましくは80nm以下である。100nmを超える平均粒子径では、油性成分と水性成分との比重差により、クリーミングを生じてしまう場合があり、十分な経時安定性を確保することが難しい。
本発明の口腔用微細エマルション組成物は、シスメックス株式会社製の粒度分布測定装置(ZETASIZER Nano−S)を使用して平均粒子(質量平均)を測定できる。
The oral emulsion fine emulsion composition of the present invention composed of the above components has an average particle size of 100 nm or less, preferably 80 nm or less. When the average particle diameter exceeds 100 nm, creaming may occur due to the difference in specific gravity between the oily component and the aqueous component, and it is difficult to ensure sufficient stability over time.
The fine emulsion composition for oral cavity of this invention can measure an average particle (mass average) using the particle size distribution measuring apparatus (ZETASIZER Nano-S) by Sysmex Corporation.

本発明の口腔用微細エマルション組成物は、0.1〜20質量%の範囲において、任意の液体口腔用組成物に簡便かつ安定に配合することが可能である。より好ましくは1〜10%である。20%を超えて配合すると、べたつきが増す、油臭さが増す等、嗜好性が悪くなる恐れがある。上記液体口腔用組成物は、液体歯磨剤、液状歯磨剤、洗口剤、マウスウォッシュ等であり、これらの製剤に簡便に、かつ安定に配合することができる。   The fine oral emulsion composition of the present invention can be easily and stably blended with any liquid oral composition in the range of 0.1 to 20% by mass. More preferably, it is 1 to 10%. If it exceeds 20%, the stickiness may increase, the oily odor may increase, and the like may deteriorate. The liquid oral composition is a liquid dentifrice, liquid dentifrice, mouthwash, mouthwash, and the like, and can be easily and stably blended into these preparations.

以下に実施例を挙げて本発明を更に具体的に説明するが、本発明はこれらによって限定されるものではない。   The present invention will be described more specifically with reference to the following examples, but the present invention is not limited thereto.

口腔用微細エマルション組成物の調製と評価
(1)口腔用微細エマルション組成物の調製
攪拌機および真空ポンプを装備した2リッターガラス製乳化器に、あらかじめ均一溶解した表に示す各成分を、合計で1Kgになるように仕込んだ。乳化器内を20〜30mmHgに減圧し、1時間攪拌・混合を行ない、本発明品1〜7および比較品1〜4の口腔用微細エマルション組成物を得た。これらの組成を表1および2に示す。

Figure 2015086149

Figure 2015086149
Preparation and Evaluation of Oral Fine Emulsion Composition (1) Preparation of Oral Fine Emulsion Composition Each component shown in the table uniformly dissolved in advance in a 2-liter glass emulsifier equipped with a stirrer and a vacuum pump is 1 kg in total. It was prepared to become. The inside of the emulsifier was decompressed to 20 to 30 mmHg, and stirred and mixed for 1 hour to obtain fine emulsion compositions for oral cavity of the present invention products 1 to 7 and comparative products 1 to 4. Their compositions are shown in Tables 1 and 2.

Figure 2015086149

Figure 2015086149

(2)安定性評価
本発明品を45℃、5℃、−5〜45℃のサイクル恒温槽に1ヶ月間放置し、外観を目視にて観察し、さらに粒子径を測定した(シスメックス株式会社製粒度分布測定装置:ZETASIZER Nano−S)。これらの結果を表3〜4に示す。
○:外観の変化が認められず
×:濁りまたは分離・クリーミングが認められた

Figure 2015086149

Figure 2015086149
(2) Stability evaluation The product of the present invention was left in a 45 ° C., 5 ° C., and −5 to 45 ° C. cycle thermostatic bath for one month, the appearance was visually observed, and the particle size was further measured (Sysmex Corporation). Particle size distribution measuring device: ZETASIZER Nano-S). These results are shown in Tables 3-4.
○: No change in appearance was observed ×: Turbidity or separation / creaming was observed

Figure 2015086149

Figure 2015086149

実施例1で得た本発明品2を配合した液体歯磨剤
1.実施例1で得られた本発明品2 3.0質量%
2.ポリオキシエチレン硬化ヒマシ油(60E.O.) 1.0
3.エタノール 10.0
4.クエン酸 0.05
5.クエン酸三ナトリウム 0.2
6.グリセリン 3.0
7.キシリトール 5.0
8.防腐剤 適量
9.精製水で100.0質量%とする。
調製法 : 2〜9を攪拌、混合し、均一になったところで1を添加し、さらに撹拌し、均一になったところで調製を終了する。
安定性 : 調製品を45℃、5℃および−5℃〜45℃のサイクル恒温槽にて1ヶ月間保存した後、目視にて外観を観察したところ、変化は認められず、安定であった。
1. Liquid dentifrice containing the product 2 of the present invention obtained in Example 1. Invention product 2 obtained in Example 1 3.0% by mass
2. Polyoxyethylene hydrogenated castor oil (60 EO) 1.0
3. Ethanol 10.0
4). Citric acid 0.05
5. Trisodium citrate 0.2
6). Glycerin 3.0
7). Xylitol 5.0
8). Preservative appropriate amount 9. It is made 100.0 mass% with purified water.
Preparation method: 2 to 9 are stirred and mixed, 1 is added when the mixture becomes uniform, and further stirred, and the preparation is completed when the mixture becomes uniform.
Stability: After the preparation was stored for 1 month in a 45 ° C, 5 ° C, and -5 ° C to 45 ° C cycle thermostat, the appearance was visually observed. No change was observed and the product was stable. .

実施例1で得た本発明品4を配合した洗口剤
1.実施例1で得た本発明品4 5.0質量%
2.ポリオキシエチレン硬化ヒマシ油(60E.O.) 0.5
3.トリクロサン 0.05
4.エタノール 10.0
5.キシリトール 3.0
6.ラウリル硫酸ナトリウム 0.1
7.クエン酸 0.01
8.クエン酸三ナトリウム 0.1
9.香料 適量
10.防腐剤 適量
11.精製水で100.0質量%とする。
調製法 : 2〜11を攪拌、混合し、均一になったところで1を添加し、さらに撹拌し、均一になったところで調製を終了する。
安定性 : 調製品を45℃、5℃および−5℃〜45℃のサイクル恒温槽にて1ヶ月間保存した後、目視にて外観を観察したところ、変化は認められず、安定であった。
1. A mouthwash containing the product 4 of the present invention obtained in Example 1. Invention product 4 obtained in Example 1 5.0 mass%
2. Polyoxyethylene hydrogenated castor oil (60 EO) 0.5
3. Triclosan 0.05
4). Ethanol 10.0
5. Xylitol 3.0
6). Sodium lauryl sulfate 0.1
7). Citric acid 0.01
8). Trisodium citrate 0.1
9. Perfume appropriate amount10. Preservative appropriate amount11. It is made 100.0 mass% with purified water.
Preparation method: 2 to 11 are stirred and mixed, 1 is added when the mixture becomes uniform, and the mixture is further stirred, and the preparation is completed when the mixture becomes uniform.
Stability: After the preparation was stored for 1 month in a 45 ° C, 5 ° C, and -5 ° C to 45 ° C cycle thermostat, the appearance was visually observed. No change was observed and the product was stable. .

実施例1で得た本発明品6を配合したマウスウォッシュ
1.実施例1で得た本発明品6 20.0質量%
2.ポリオキシエチレン硬化ヒマシ油(60E.O.) 2.0
3.エタノール 20.0
4.サッカリンナトリウム 0.2
5.安息香酸ナトリウム 0.1
6.着色剤 適量
7.ペパーミント油 0.05
8.メントール 0.05
9.防腐剤 適量
10.精製水で100.0質量%とする。
調製法 : 2〜10を攪拌、混合し、均一になったところで1を添加し、さらに撹拌し、均一になったところで調製を終了する。
安定性 : 調製品を45℃、5℃および−5℃〜45℃のサイクル恒温槽にて1ヶ月間保存した後、目視にて外観を観察したところ、変化は認められず、安定であった。
1. Mouthwash containing the product 6 of the present invention obtained in Example 1. Invention product 6 obtained in Example 1 20.0% by mass
2. Polyoxyethylene hydrogenated castor oil (60 EO) 2.0
3. Ethanol 20.0
4). Saccharin sodium 0.2
5. Sodium benzoate 0.1
6). Colorant appropriate amount 7. Peppermint oil 0.05
8). Menthol 0.05
9. Preservative appropriate amount10. It is made 100.0 mass% with purified water.
Preparation method: 2 to 10 are stirred and mixed, 1 is added when the mixture becomes uniform, and further stirred, and the preparation is completed when the mixture becomes uniform.
Stability: After the preparation was stored for 1 month in a 45 ° C, 5 ° C, and -5 ° C to 45 ° C cycle thermostat, the appearance was visually observed. No change was observed and the product was stable. .

Claims (4)

次の成分(A)〜(D)を必須成分として含有し、成分(A)〜(C)の比率(質量比)が、(A)/(B)=70/30〜30/70かつ[(A)+(B)]/(C)=90/10〜60/40であることを特徴とする、平均粒子径100nm以下の口腔用微細エマルション組成物。
(A)油性成分
(B)ポリオキシエチレン硬化ヒマシ油
(C)ポリオール
(D)水
The following components (A) to (D) are contained as essential components, and the ratio (mass ratio) of the components (A) to (C) is (A) / (B) = 70/30 to 30/70 and [ (A) + (B)] / (C) = 90 / 10-60 / 40, The fine emulsion composition for oral cavity with an average particle diameter of 100 nm or less.
(A) Oil component (B) Polyoxyethylene hydrogenated castor oil (C) Polyol (D) Water
成分(B)ポリオキシエチレン硬化ヒマシ油の酸化エチレン付加モル数が、10〜40モルであることを特徴とする、請求項1に記載の口腔用微細エマルション組成物。 The fine emulsion composition for oral cavity according to claim 1, wherein the number of moles of ethylene oxide added to the component (B) polyoxyethylene hydrogenated castor oil is 10 to 40 moles. 成分(C)ポリオールが、プロピレングリコール、1,3−ブチレングリコール、ジプロピレングリコール、ペンチレングリコールより選ばれる1種または2種以上からなる、請求項1又は2に記載の口腔用微細エマルション組成物。 The fine emulsion composition for oral cavity according to claim 1 or 2, wherein the component (C) polyol comprises one or more selected from propylene glycol, 1,3-butylene glycol, dipropylene glycol, and pentylene glycol. . 請求項1〜3のいずれか1項に記載の口腔用微細エマルション組成物を0.1〜20質量%含有する液体口腔用組成物。 The liquid oral cavity composition which contains 0.1-20 mass% of oral fine emulsion compositions of any one of Claims 1-3.
JP2013224306A 2013-10-29 2013-10-29 Fine emulsion composition for oral cavity and liquid composition for oral cavity containing the same Pending JP2015086149A (en)

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