KR20170117406A - Liquid oral composition - Google Patents

Liquid oral composition Download PDF

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KR20170117406A
KR20170117406A KR1020177021898A KR20177021898A KR20170117406A KR 20170117406 A KR20170117406 A KR 20170117406A KR 1020177021898 A KR1020177021898 A KR 1020177021898A KR 20177021898 A KR20177021898 A KR 20177021898A KR 20170117406 A KR20170117406 A KR 20170117406A
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liquid oral
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oral composition
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KR102491340B1 (en
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유미코 히라시마
야스히로 아카바네
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라이온 가부시키가이샤
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/40Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/44Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/49Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/86Polyethers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses

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  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Cosmetics (AREA)

Abstract

(A) 질산칼륨 및 (B) 염화세틸피리디늄을 배합한 에탄올 무배합의 액체 구강용 조성물에, (C) 비이온 계면활성제 및 (D) 양성 계면활성제를 배합하고, (E) 수분량을 55질량% 이상 92질량% 미만으로 하고, 조성물의 pH를 6.8 이상 8.0 미만으로 하고, (A) 및 (B) 염화세틸피리디늄의 병용에 의해 생기는 불용성 침전물의 석출이 억제되고, 지각 과민 억제 효과 및 우식 억제 효과가 우수한 액체 구강용 조성물을 제공한다.(C) a nonionic surfactant and (D) an amphoteric surfactant in an ethanol-free liquid oral composition containing (A) potassium nitrate and (B) cetylpyridinium chloride, By mass or more and less than 92% by mass and the pH of the composition is set to 6.8 or more and less than 8.0, and precipitation of insoluble precipitates formed by the combination of (A) and (B) cetylpyridinium chloride is suppressed, A liquid oral composition having excellent caries inhibiting effect is provided.

Description

액체 구강용 조성물Liquid oral composition

본 발명은, 지각(知覺) 과민 억제 효과 및 구강내의 부유균(浮遊菌) 살균 효과가 우수한, 질산칼륨을 함유하는 에탄올 무배합의 액체 구강용 조성물에 관한 것이다.The present invention relates to a liquid oral composition containing no potassium nitrate, which is excellent in an inhibitory effect on perceived hypersensitivity and a sterilizing effect of floating bacteria in the oral cavity.

상아질 지각 과민증의 예방책으로서, 유효성분으로서 공지(公知)인 질산칼륨이 구강용 조성물에 배합된다(특허 문헌 1, 2). 이 질산칼륨은, 구강용 조성물에 일반적으로 배합되는 라우릴황산나트륨 존재하에서 불용성 석출물을 생성한다는 문제가 있고, 특허 문헌 3에서는, 질산칼륨 및 라우릴황산나트륨 함유의 구강용 조성물에 다가알코올, 양성 계면활성제를 배합함에 의해, 라우릴황산칼륨의 석출을 방지하고, 저온 석출을 억제하여 있다.As a preventive measure for dentin hypersensitivity, potassium nitrate known as an effective ingredient is incorporated into an oral composition (Patent Documents 1 and 2). This potassium nitrate has a problem that insoluble precipitates are formed in the presence of sodium lauryl sulfate generally contained in oral compositions. Patent Document 3 discloses that potassium hydroxide and sodium lauryl sulfate are added to oral compositions containing polyhydric alcohol, amphoteric surfactant , Precipitation of potassium lauryl sulfate is prevented and low-temperature precipitation is suppressed.

또한, 특히 액체 구강용 조성물에서의 지각 과민의 억제에는, 점막 자극이 적고 저자극성인 논알코올 타입의 액체 제제가 보다 알맞다.In addition, in particular, in the liquid oral composition, a non-alcohol type liquid preparation having less mucosal irritation and hypotonicity is more suitable for suppressing the sensory hyperactivity.

한편, 카티온성 살균제인 염화세틸피리디늄은, 구강내의 부유 세균에의 살균 효과가 우수하고, 우식 등의 구강 질환의 예방 또는 억제에 유효하지만, 계면활성제의 영향을 받기 쉽다. 특허 문헌 4에는, 비구아니드계의 카티온성 살균제와 비이온성 계면활성제를 함유하는 구강용 조성물에 특정 화합물을 첨가하여, 비이온성 계면활성제에 의한 카티온성 살균제의 실활(失活)을 방지하고 안정화 배합한 기술이 제안되어 있다.On the other hand, cetylpyridinium chloride, which is a cationic fungicide, has an excellent germicidal effect against airborne bacteria in the oral cavity and is effective for preventing or inhibiting oral diseases such as caries, but is easily affected by surfactants. Patent Document 4 discloses that a specific compound is added to an oral composition containing a cationic fungicide of the acetophenone type and a nonionic surfactant to prevent inactivation of the cationic fungicide by the nonionic surfactant, One technique has been proposed.

특허 문헌 1 : 미국 특허 제3,863,006호Patent Document 1: U.S. Patent No. 3,863,006 특허 문헌 2 : 일본국 특개평7-101842호 공보Patent Document 2: JP-A-7-101842 특허 문헌 3 : 일본국 특개2005-68071호 공보Patent Document 3: JP-A-2005-68071 특허 문헌 4 : 일본국 특개소60-255717호 공보Patent Document 4: Japanese Patent Application Laid-Open No. 60-255717 특허 문헌 5 : 일본국 특개2013-35792호 공보Patent Document 5: JP-A-2013-35792 특허 문헌 6 : 일본국 특개2007-84471호 공보Patent Document 6: Japanese Patent Application Laid-Open No. 2007-84471

따라서 질산칼륨을 배합한 논알코올 타입의 액체 구강용 제제에서 지각 과민을 억제하고, 또한 동시에 구강내 부유균에 대해 높은 살균력을 발휘시킬 수 있으면, 구강 질환의 예방 또는 억제에 보다 유효하지만, 지금까지의 기술에서는 어려운 것이 현재의 상태이고, 이와 같은 우수한 특성을 갖는 액체 구강용 제제의 개발이 요망되었다.Therefore, it is more effective in preventing or suppressing oral diseases, if it is possible to inhibit the hypersensitivity in a non-alcohol type liquid oral preparation containing potassium nitrate and at the same time to exhibit a high sterilizing power against the floating bacteria in the oral cavity. And it has been desired to develop liquid oral preparations having such excellent properties.

본 발명은, 상기 사정을 감안하여 이루어진 것으로, 지각 과민 억제 효과 및 구강내의 부유균 살균 효과가 우수한, 질산칼륨을 함유하는 에탄올 무배합의 액체 구강용 조성물을 제공하는 것을 목적으로 한다.The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a liquid oral composition containing no potassium nitrate, which is excellent in inhibiting the hypersensitivity and sterilizing the floating bacteria in the oral cavity.

본 발명자들은, 상기 목적을 달성하기 위해 예의 검토를 행한 결과, (A) 질산칼륨과 (B) 염화세틸피리디늄을 배합한 에탄올 무배합의 액체 구강용 조성물에, (C) 비이온 계면활성제 및 (D) 양성 계면활성제를 배합하고, (E) 수분량을 55질량% 이상 92질량% 미만으로 하고, 조성물의 pH를 6.8 이상 8.0 미만으로 함에 의해, (A), (B)성분의 병용에 의해 생기는 불용성 침전물의 석출이 억제되고, 지각 과민 억제 효과 및 구강내의 부유균 살균 효과가 우수한 논알코올 타입의 액체 구강용 조성물을 얻을 수 있고, 지각 과민 및 우식의 억제에 알맞게 사용할 수 있는 것을 지견하여, 본 발명을 이루는데 이르렀다.The inventors of the present invention have found that (A) a nonionic surfactant (C) and a nonionic surfactant (B) are added to a liquid oral composition having no ethanol blended with potassium nitrate (B) and cetylpyridinium chloride (A) and (B) by combining the component (D) and the amphoteric surfactant (E) with the water content of 55 mass% or more and less than 92 mass% It is possible to obtain a non-alcoholic liquid oral composition which suppresses the precipitation of insoluble precipitates that are produced and has an effect of inhibiting the hypersensitivity and sterilization of floating bacteria in the oral cavity, and can be used to suppress the hypersensitivity and caries, The present invention has been accomplished.

즉, 질산칼륨 함유의 액체 구강용 조성물에, 카티온성 살균제인 염화세틸피리디늄을 배합함에 의해 지각 과민 억제 효과 및 구강내의 부유균 살균 효과를 부여할 수 있다고 예상되었지만, 질산칼륨과 염화세틸피리디늄을 에탄올 함유 액체 구강용 조성물 중에 배합하는 경우는 특단의 문제가 생기지 않음에도 불구하고, 저자극의 에탄올 무배합의 액체 구강용 조성물에 질산칼륨과 염화세틸피리디늄을 병용하고 배합하면, 불용성 침전물이 산생(産生)되어 석출하고, 이에 의해, 지각 과민 억제 효과가 저하되고, 살균 효과도 충분히 발현하지 않게 된다는 문제가 생기는 것을 지견하였다. 이 때문에, 에탄올 무배합의 액체 구강용 조성물 중에서 질산칼륨과 염화세틸피리디늄을 불용성 침전물의 석출 없이 병용하고, 질산칼륨 및 염화세틸피리디늄의 작용 효과를 만족하게 발휘시킨다는 새로운 과제가 부상하였다. 그래서, 이들의 과제를 해결하기 위해, 본 발명자들이 더욱 검토를 진행한 결과, (C) 비이온 계면활성제와 (D) 양성 계면활성제를 조합시켜서 첨가하고, 조성물 중의 수분량, pH를 상기 범위 내로 함에 의해, 상기한 (A), (B)성분의 병용에 의해 생기는 불용성 침전물의 석출이 경시(經時)에서도 억제되고, 높은 지각 과민 억제 효과 및 부유균 살균 효과를 동시에 부여할 수 있고, 또한, 외관을 안정하게 유지하고, 쓴맛(苦味)을 억제하여 양호한 사용감을 주는 것도 가능하였다. 이 경우, 염화세틸피리디늄은 비이온 계면활성제 등의 계면활성제에 의한 영향을 받고 실활되기 쉬음에도 불구하고, 본 발명에서는, (C), (D)성분인 계면활성제의 조합이, 조성물 중의 수분량(水分量), pH가 특정 범위 내에서 특이적으로 작용하여, 상기 각별하면서 현저한 작용 효과를 준다.In other words, it was expected that by adding cetylpyridinium chloride, which is a cationic fungicide, to a liquid oral composition containing potassium nitrate, it is possible to impart a sensory hypersensitivity effect and a germicidal effect in the oral cavity, but potassium nitrate and cetylpyridinium chloride Is mixed with an ethanol-containing liquid oral composition does not cause any particular problem, when potassium nitrate and cetylpyridinium chloride are used in combination with a liquid oral composition having no ethanol-containing low-polarity, insoluble precipitates It was found that the effect of inhibiting the hypersensitivity is lowered and the sterilizing effect is not sufficiently manifested. For this reason, a new problem has arisen in that potassium nitrate and cetylpyridinium chloride are used in combination in an ethanol-free liquid oral composition without precipitation of an insoluble precipitate to exert satisfactorily the action effects of potassium nitrate and cetylpyridinium chloride. In order to solve these problems, the inventors of the present invention have conducted further investigations. As a result, they have found that (C) a nonionic surfactant and (D) an amphoteric surfactant are added in combination, The precipitation of insoluble precipitates caused by the combined use of the above components (A) and (B) is suppressed even in the course of time, and a high antinociception inhibitory effect and a sterilizing effect of a floating bacteria can be simultaneously given, It was possible to maintain the appearance stably and to suppress the bitter taste (bitterness) to give a good feeling of use. In this case, although cetylpyridinium chloride is susceptible to being influenced by a surfactant such as a nonionic surfactant and inactivated, in the present invention, the combination of the surfactants (C) and (D) (Water content) and pH of the water-absorbing agent specifically function within a specific range to give distinct and remarkable action effects.

따라서, 본 발명의 에탄올 무배합의 액체 구강용 조성물은, 후술하는 실시례로부터도 분명한 바와 같이, 액체 구강용 조성물을 조제하여 4주간 경과해도 불용성 침전물의 석출이 거의 없고 외관이 경시로 안정하고, 지각 과민 억제 효과 및 구강내의 부유균 살균 효과가 높고, 또한, 사용 후의 쓴맛이 억제되어 맛이 좋은 양호한 사용감을 갖는다.Therefore, the liquid oral composition containing no ethanol in the present invention has substantially no precipitation of insoluble precipitates even after 4 weeks from the preparation of a composition for oral cavity as evidenced by the later-described examples, the appearance is stable with time, A hypersensitive hypersensitive effect and a germicidal effect in the oral cavity are high, and a bitter taste after use is suppressed, so that a good taste is obtained with good taste.

또한, 특허 문헌 3은, 구강용 조성물에서 질산칼륨 및 라우릴황산나트륨의 병용에 의해 생기는 라우릴황산칼륨의 석출을 억제하는 것이고, 또한, 특허 문헌 4는, 비이온 계면활성제에 의한 카티온성 살균제의 실활 방지이고, 카티온성 살균제를 질산칼륨에 병용하는 것에 대해 언급되어 있지 않다. 특허 문헌 5, 6에는, 질산칼륨, 염화세틸피리디늄을 배합한 액체 구강용 조성물이 기재되어 있지만, 이들은 에탄올 배합 조성이다. 특허 문헌 3∼6으로부터, 에탄올 무배합의 액체 구강용 조성물에서의 질산칼륨과 염화세틸피리디늄과의 병용에 의해 생기는 불용성 침전물의 석출 억제는 예측할 수가 없다.Patent Document 3 is directed to inhibiting the precipitation of potassium lauryl sulfate caused by the combined use of potassium nitrate and sodium lauryl sulfate in the oral composition and Patent Document 4 discloses that the cationic fungicide There is no mention of the prevention of inactivation and the use of a cationic bactericide in combination with potassium nitrate. Patent Documents 5 and 6 disclose liquid oral compositions containing potassium nitrate and cetylpyridinium chloride, but these are ethanol blended compositions. Patent Literatures 3 to 6 show that inhibition of precipitation of insoluble precipitates caused by the combined use of potassium nitrate and cetylpyridinium chloride in a liquid oral composition without ethanol is unpredictable.

따라서 본 발명은, 하기한 액체 구강용 조성물 및 그 조성물에서의 불용성 침전물의 석출 억제 방법을 제공한다.Accordingly, the present invention provides the liquid oral composition described below and a method for inhibiting the precipitation of insoluble precipitates in the composition.

[1][One]

(A) 질산칼륨 및 (B) 염화세틸피리디늄을 배합한 에탄올 무배합의 액체 구강용 조성물에, (C) 비이온 계면활성제 및 (D) 양성 계면활성제를 배합하고, (E) 수분량을 55질량% 이상 92질량% 미만으로 하고, 조성물의 pH를 6.8 이상 8.0 미만으로 한 것을 특징으로 하는 액체 구강용 조성물.(C) a nonionic surfactant and (D) an amphoteric surfactant in an ethanol-free liquid oral composition containing (A) potassium nitrate and (B) cetylpyridinium chloride, By mass to less than 92% by mass, and the pH of the composition is set to 6.8 or more and less than 8.0.

[2][2]

(C) 비이온 계면활성제가 폴리옥시에틸렌경화피마자유이고, (D) 양성 계면활성제가 알킬아미드베타인 또는 그 염인 [1] 기재의 액체 구강용 조성물.(C) the liquid non-ionic surfactant is a polyoxyethylene hardened castor oil, and (D) the amphoteric surfactant is an alkylamide betaine or a salt thereof.

[3][3]

(C) 비이온 계면활성제가, 에틸렌옥사이드의 평균부가몰수가 40∼100몰의 폴리옥시에틸렌경화피마자유이고, (D) 양성 계면활성제가, 야자유지방산아미드프로필베타인인 [1] 또는 [2] 기재의 액체 구강용 조성물.1] or [2], wherein the nonionic surfactant (C) is a polyoxyethylene hydrogenated castor oil having an average addition mole number of ethylene oxide of 40 to 100 moles, (D) the amphoteric surfactant is coconut fatty acid amide propyl betaine, ≪ / RTI >

[4][4]

(C)성분을 0.1∼2질량%, (D)성분을 0.1∼2질량% 배합한 [1], [2] 또는 [3] 기재의 액체 구강용 조성물.The liquid oral composition according to [1], [2] or [3], wherein 0.1 to 2 mass% of component (C) and 0.1 to 2 mass% of component (D) are combined.

[5][5]

(A)성분을 0.01∼10질량%, (B)성분을 0.001∼0.1질량% 배합한 [1]∼[4]의 어느 하나에 기재된 액체 구강용 조성물.The liquid oral composition according to any one of [1] to [4], wherein the content of the component (A) is 0.01 to 10 mass% and the content of the component (B) is 0.001 to 0.1 mass%.

[6][6]

세구제(洗口劑)인 [1]∼[5]의 어느 하나에 기재된 액체 구강용 조성물.A liquid oral composition according to any one of [1] to [5], which is a mouth rinse.

[7][7]

지각 과민 및 우식 억제용인 [1]∼[6]의 어느 하나에 기재된 액체 구강용 조성물.The liquid oral composition according to any one of [1] to [6], which is suitable for inhibiting the hypersensitivity and dental caries.

[8][8]

(A) 질산칼륨 및 (B) 염화세틸피리디늄을 배합한 에탄올 무배합의 액체 구강용 조성물에, (C) 비이온 계면활성제 및 (D) 양성 계면활성제를 배합하고, (E) 수분량을 55질량% 이상 92질량% 미만으로 하고, 조성물의 pH를 6.8 이상 8.0 미만으로 하는 것을 특징으로 하는, 상기 액체 구강용 조성물에서의 (A) 질산칼륨 및 (B) 염화세틸피리디늄의 병용에 의해 생기는 불용성 침전물의 석출 억제 방법.(C) a nonionic surfactant and (D) an amphoteric surfactant in an ethanol-free liquid oral composition containing (A) potassium nitrate and (B) cetylpyridinium chloride, (A) nitric acid potassium and (B) cetylpyridinium chloride in the liquid oral composition, wherein the composition has a pH of not less than 92 mass% and a pH of the composition of not less than 6.8 and less than 8.0. A method for inhibiting precipitation of insoluble precipitates.

[9][9]

액체 구강용 조성물이 세구제인, [8] 기재의 액체 구강용 조성물에서의 (A) 질산칼륨 및 (B) 염화세틸피리디늄의 병용에 의해 생기는 불용성 침전물의 석출 억제 방법.A method for inhibiting the precipitation of an insoluble precipitate caused by the combined use of (A) potassium nitrate and (B) cetylpyridinium chloride in a liquid oral composition according to [8], wherein the composition for liquid oral use is a detergent.

본 발명에 의하면, 지각 과민 억제 효과 및 구강내의 부유균 살균 효과가 우수한 질산칼륨 함유의 에탄올 무배합의 액체 구강용 조성물을 제공할 수 있다.INDUSTRIAL APPLICABILITY According to the present invention, it is possible to provide a composition for oral administration of potassium nitrate-free ethanol-free formulation having an excellent inhibitory effect on hypersensitivity and a germicidal effect in the oral cavity.

이하, 본 발명에 관해 더욱 상세히 기술한다. 본 발명의 액체 구강용 조성물은, (A) 질산칼륨, (B) 염화세틸피리디늄, (C) 비이온 계면활성제, (D) 양성 계면활성제, (E) 물(水)을 함유하고, 에탄올 무배합(無配合)이다.Hereinafter, the present invention will be described in more detail. The liquid oral composition of the present invention is characterized by containing (A) potassium nitrate, (B) cetylpyridinium chloride, (C) a nonionic surfactant, (D) an amphoteric surfactant, (E) water (water) (No blending).

(A) 질산칼륨은, 상아질 지각 과민증을 예방 또는 치료하기 위한 유효성분으로서 배합되는 것이고, 지각 과민 억제제이다.(A) Potassium nitrate is compounded as an active ingredient for preventing or treating dental hypersensitivity, and is a hypersensitivity inhibitor.

(A)성분인 질산칼륨의 배합량은, 조성물 전체의 0.01∼10%(질량%, 이하, 마찬가지.)가 바람직하고, 보다 바람직하게는 0.1∼7%이다. 배합량이 많을수록 지각 과민 억제 효과는 높아지지만, 10% 이하인 것이, 충분한 석출 억제, 쓴맛의 억제에는 보다 알맞다.The blending amount of potassium nitrate as the component (A) is preferably 0.01 to 10% (mass%, the same applies hereinafter), more preferably 0.1 to 7% of the whole composition. The more the compounding amount is, the higher the inhibitory effect of inhibiting the hypersensitivity, but the less than 10% is more suitable for inhibiting sufficient precipitation and suppressing the bitter taste.

(B) 염화세틸피리디늄은, 카티온성 살균제이고, 구강내 부유균에 대한 살균제이다. 염화세틸피리디늄은, 시판(市販)의 것을 사용할 수 있다.(B) Cetylpyridinium chloride is a cationic fungicide and a disinfectant for oral bacteria. Cetylpyridinium chloride may be commercially available.

(B)성분인 염화세틸피리디늄의 배합량은, 조성물 전체의 0.001∼0.1%가 바람직하고, 보다 바람직하게는 0.005∼0.1%, 더욱 바람직하게는 0.01∼0.05%이다. 많이 배합할수록 살균 효과가 높아지지만, 0.1% 이하인 것이, 충분한 석출 억제, 쓴맛의 억제에는 보다 알맞다.The blending amount of cetylpyridinium chloride as the component (B) is preferably 0.001 to 0.1%, more preferably 0.005 to 0.1%, and still more preferably 0.01 to 0.05% of the whole composition. The greater the blending ratio, the higher the bactericidal effect. However, the blending amount of 0.1% or less is more suitable for inhibiting sufficient precipitation and suppressing the bitter taste.

본 발명에서는, (C) 비이온 계면활성제 및 (D) 양성 계면활성제를 조합시켜서 배합하는 것이 효과 발현에 중요하다. (C)성분 또는 (D)성분을 결여하면, 불용성 침전물이 석출하고, 지각 과민 억제 효과 및 부유균 살균 효과가 뒤떨어진다. 또한, 쓴맛이 억제되지 않고 사용감이 뒤떨어진다.In the present invention, the combination of (C) a nonionic surfactant and (D) an amphoteric surfactant is important for manifesting the effect. If the component (C) or the component (D) is not used, an insoluble precipitate is precipitated, and the effect of suppressing the hypersensitivity and the effect of sterilizing the floating bacteria are poor. Also, the bitter taste is not suppressed and the feeling of use is poor.

(C) 비이온 계면활성제로서는, 폴리옥시에틸렌경화피마자유, 폴리옥시에틸렌알킬에테르, 폴리글리세린지방산에스테르를 들 수 있고, 이들의 1종 또는 2종 이상을 사용할 수 있는데, 특히, 에틸렌옥사이드(E.O.)의 평균부가몰수가 40∼100몰, 특히 60∼100몰의 폴리옥시에틸렌경화피마자유, 알킬기의 탄소수가 16∼18이고 E.O.의 평균부가몰수가 10∼40몰, 특히 20∼40몰의 폴리옥시에틸렌알킬에테르, 지방산의 탄소수가 12∼18, 특히 12∼14의 데카글리세린모노지방산에스테르폴리글리세린지방산에스테르가 바람직하고, 그 중에서도 E.O.의 평균부가몰수가 40∼100몰의 폴리옥시에틸렌경화피마자유가 바람직하다.Examples of the nonionic surfactant (C) include polyoxyethylene hydrogenated castor oil, polyoxyethylene alkyl ether, and polyglycerin fatty acid ester. One or more of these surfactants may be used. In particular, ethylene oxide (EO Polyoxyethylene hydrogenated castor oil having an average addition mole number of 40 to 100 mol, in particular 60 to 100 mol, of alkyl groups having 16 to 18 carbon atoms and an average addition molar number of EO of 10 to 40 mol, especially 20 to 40 mol, of poly Oxyethylene alkyl ethers, and decaglycerol mono fatty acid ester polyglycerin fatty acid esters having 12 to 18 carbon atoms, particularly 12 to 14 carbon atoms. Among them, polyoxyethylene hydrogenated castor oil having an average addition mole number of EO of 40 to 100 mol desirable.

구체적으로는, 상품화되어 있는 하기에 나타내는 바와 같은 시판품을 사용할 수 있다.Concretely, commercially available products such as those shown below that are commercialized can be used.

폴리옥시에틸렌경화피마자유 ;Polyoxyethylene hydrogenated castor oil;

닛코우케미칼즈사제의 NIKKOL HCO계, 니혼에멀션사제의 에마렉스HC계, 니혼유지 사제의 유니옥스HC계NIKKOL HCO series manufactured by Nikko Chemicals Co., Emarex HC series manufactured by Nippon Emulsion Co., Uniox HC series manufactured by Nippon Oil &

폴리옥시에틸렌알킬에테르 ;Polyoxyethylene alkyl ethers;

닛코우케미칼즈사제의 NIKKOL BC계, NIKKOL BS계, 니혼에멀션사제의 에마렉스100계, 에마렉스600계NIKKOL BC series manufactured by Nikko Chemicals Co., NIKKOL BS series, Emarex 100 series manufactured by Nihon Emulsion Co., Emarex 600 series

데카글리세린모노지방산에스테르 ;Decaglycerol mono fatty acid esters;

닛코우케미칼즈사제의 NIKKOL Decagln계, 미쯔비시화학푸드사제의 료토(등록상표) 포리구리에스테르 D시리즈NIKKOL Decagln series manufactured by Nikko Chemicals Co., Ltd., Ryogo (registered trademark) polyglycol ester D series manufactured by Mitsubishi Chemical Foods Co.,

(C)성분인 비이온 계면활성제의 배합량은, 조성물 전체의 0.1∼2%가 바람직하고, 보다 바람직하게는 0.1∼1%, 더욱 바람직하게는 0.2∼0.5%이다. 0.1% 이상 배합하면, 충분한 석출 억제 효과, 지각 과민 억제 효과 및 부유균 살균 효과를 이루고, 또한, 쓴맛을 충분히 억제할 수 있다. 2% 이하인 것이, 지각 과민 억제 효과 및 부유균 살균 효과가 저하되는 것을 방지하는데는 보다 알맞다.The blending amount of the nonionic surfactant as the component (C) is preferably from 0.1 to 2%, more preferably from 0.1 to 1%, and still more preferably from 0.2 to 0.5% based on the whole composition. When the content is 0.1% or more, sufficient precipitation inhibiting effect, crustal hypersensitivity inhibiting effect and floating bacteria germicidal effect are achieved, and the bitter taste can be sufficiently suppressed. 2% or less is more suitable for preventing the hypersensitivity inhibiting effect and the sterilizing effect of the floating bacteria from being deteriorated.

(D) 양성 계면활성제로서는, 야자유지방산아미드프로필베타인 등의 알킬아미드베타인 또는 그 염, 라우릴디메틸아미노아세트산베타인 등의 아세트산베타인형, N-지방산아실-N-카르복시메틸-N-히드록시에틸에틸렌디아민염 등의 이미다졸린형, N-지방산아실-L-알기네이트염 등의 아미노산형 등을 들 수 있고, 이들의 1종 또는 2종 이상을 사용할 수 있는데, 특히, 알킬아미드베타인 또는 그 염이 바람직하고, 그 중에서도, 야자유지방산아미드프로필베타인이 알맞다.Examples of the amphoteric surfactant (D) include alkyl amide betaine or salts thereof such as palm oil fatty amide propylbetaine, betaine acetate type such as lauryldimethylaminoacetic acid betaine, N-fatty acid acyl-N-carboxymethyl- And amino acid types such as imidazoline type and N-fatty acid acyl-L-alginate salt, and the like, and they may be used alone or in combination of two or more. In particular, alkylamide beta Phosphorus or a salt thereof is preferable, and palm oil fatty amide propyl betaine is particularly suitable.

구체적으로는, 야자유지방산아미드프로필베타인(데구사사제의 TEGO Betain CK OK(30% 수용액), 가오(주)제의 안히토루5AB(30% 수용액)) 등의 시판품을 사용할 수 있다.Specifically, commercially available products such as coconut oil fatty acid amide propyl betaine (TEGO Betaine CK OK (30% aqueous solution) manufactured by Degussa Corporation, Anichtor 5AB (30% aqueous solution) manufactured by Kao Corporation) and the like can be used.

(D)성분인 양성 계면활성제의 배합량은, 조성물 전체의 0.1∼2%가 바람직하고, 보다 바람직하게는 0.1∼1%, 더욱 바람직하게는 0.2∼0.5%이다. 0.1% 이상 배합하면, 충분한 석출 억제 효과, 지각 과민 억제 효과 및 부유균 살균 효과를 이루고, 또한, 쓴맛을 충분히 억제할 수 있다. 2% 이하인 것이, 지각 과민 억제 효과 및 부유균 살균 효과가 저하되는 것을 방지하는데는 보다 알맞다.The blending amount of the amphoteric surfactant as the component (D) is preferably from 0.1 to 2%, more preferably from 0.1 to 1%, and still more preferably from 0.2 to 0.5%, based on the whole composition. When the content is 0.1% or more, sufficient precipitation inhibiting effect, crustal hypersensitivity inhibiting effect and floating bacteria germicidal effect are achieved, and the bitter taste can be sufficiently suppressed. 2% or less is more suitable for preventing the hypersensitivity inhibiting effect and the sterilizing effect of the floating bacteria from being deteriorated.

본 발명의 액체 구강용 조성물은, (E) 물의 함유량, 즉 조성물 중의 수분량이, 조성물 전체의 55% 이상 92% 미만이고, 바람직하게는 60% 이상 91% 이하, 보다 바람직하게는 60% 이상 70% 이하이다. 수분량이 상기 범위 내이면, 불용성 침전물을 석출 억제할 수 있고, 우수한 지각 과민 억제 효과 및 쓴맛 억제 효과를 부여할 수 있다. 55% 미만이면, 석출 억제할 수가 없고, 지각 과민 억제 효과 및 부유균 살균 효과가 뒤떨어진다. 92% 이상이면, 석출 억제 효과가 뒤떨어지고, 지각 과민 억제 효과 및 부유균 살균 효과도 뒤떨어지고, 쓴맛을 억제할 수도 없다.The liquid oral composition of the present invention is characterized in that (E) the content of water, that is, the water content in the composition, is 55% or more and less than 92%, preferably 60% or more and 91% or less, more preferably 60% or more, % Or less. When the water content is within the above range, the insoluble precipitate can be inhibited from being precipitated, and a superior antihyperglycemic effect and a bitter taste suppressing effect can be imparted. If it is less than 55%, precipitation can not be inhibited and the effect of suppressing the hypersensitivity and the effect of sterilizing the floating bacteria are inferior. If it is more than 92%, the precipitation inhibiting effect is inferior, the perineal hypersensitivity inhibiting effect and the sterilizing effect of the floating bacteria are also inferior, and the bitter taste can not be suppressed.

본 발명에서, 액체 구강용 조성물의 pH는 6.8 이상 8.0 미만이고, 바람직하게는 pH6.8∼7.8, 보다 바람직하게는 pH6.8∼7.5이다. 상기 범위 내이면, 석출 억제 효과, 지각 과민 억제 효과 및 쓴맛 억제 효과가 우수하다. pH6.8 미만 또는 pH8.0 이상이면, 석출 억제할 수가 없고, 지각 과민 억제 효과 및 부유균 살균 효과가 뒤떨어진다.In the present invention, the pH of the liquid oral composition is from 6.8 to less than 8.0, preferably from 6.8 to 7.8, more preferably from 6.8 to 7.5. Within this range, the precipitation inhibiting effect, the perineal hypersensitive inhibiting effect and the bitter taste suppressing effect are excellent. If the pH is less than 6.8 or the pH is 8.0 or more, precipitation can not be inhibited, and the effect of suppressing the hypersensitivity and the effect of sterilizing the floating bacteria are inferior.

또한, pH는, 조성물을 조제 직후에 도아전파공업사제의 pH미터(형번 Hm-30S)를 이용하여 측정하고, 25℃, 3분 후의 값이다(이하, 마찬가지.).The pH value was measured by using a pH meter (model number Hm-30S) manufactured by Doi Kagaku Kogyo Co., Ltd. immediately after preparation, and the value after 3 minutes at 25 캜 (the same applies hereinafter).

본 발명에서는, 조성물의 pH를 상기 범위 내로 조정하는데, 공지의 pH 조정제를 첨가하여도 좋다. 예를 들면 인산2수소나트륨 등의 인산수소알칼리금속염, 수산화나트륨 등의 알칼리금속의 수산화물 등을 들 수 있다.In the present invention, a known pH adjuster may be added to adjust the pH of the composition within the above range. For example, an alkali metal hydrogen phosphate such as sodium dihydrogenphosphate and an alkali metal hydroxide such as sodium hydroxide.

본 발명의 액체 구강용 조성물은, 에탄올 무배합이다. 여기서, 「에탄올 무배합」이란, 에탄올이 배합되지 않는 것이지만, 액체 구강용 조성물에서는, 조성물 중에 배합되는 향료 중에 원료 유래의 에탄올이 미량 포함되는 경우 등이 있기 때문에, 이들의 이유를 고려하여서, 향료 중 등에 미량 함유되는 에탄올 이외에 에탄올을 포함하지 않는 것이다. 또한, 이 경우, 조성물 중의 에탄올량은 조성물 전체에 대해 바람직하게는 100ppm 이하, 보다 바람직하게는 50ppm 이하, 더욱 바람직하게는 10ppm 이하이고, 0ppm이라도 좋다.The liquid oral composition of the present invention is ethanol-free. Herein, " no ethanol blended " means that ethanol is not blended. However, in the liquid oral composition, there is a case where a trace amount of ethanol derived from the raw material is contained in the perfume blended in the composition. Therefore, It does not contain ethanol in addition to ethanol which is contained in a trace amount. In this case, the amount of ethanol in the composition is preferably 100 ppm or less, more preferably 50 ppm or less, further preferably 10 ppm or less, and 0 ppm in the composition.

본 발명에서는, 이와 같은 에탄올 무배합의 조성에서, 불용성 침전물의 석출을 억제하고, 우수한 지각 과민 억제 효과 및 부유균 살균 효과를 이룬다.In the present invention, precipitation of an insoluble precipitate is suppressed in the ethanol-free formulation, and an excellent inhibitory effect on hypersensitivity and a sterilization effect of a floating bacteria are achieved.

본 발명의 액체 구강용 조성물은, 특히 세구제로서 알맞다. 또한, 본 발명 조성물에는, 상기 성분에 더하여, 필요에 응하여 기타의 공지 성분을, 본 발명의 효과를 방해하지 않는 범위에서 배합할 수 있다. 구체적으로는, 습윤제, 용제, 또한 필요에 의해 감미제, 착색제, 방부제, 향료, 유효성분 등이 배합된다.The liquid oral composition of the present invention is particularly suitable as a detergent. In addition to the above-mentioned components, other known components may be added to the composition of the present invention within a range that does not interfere with the effect of the present invention. Specifically, a wetting agent, a solvent and, if necessary, a sweetening agent, a coloring agent, an antiseptic, a fragrance, and an active ingredient are blended.

또한, 액체 구강용 조성물, 특히 세구제에는, 연마제 등이 가용화하지 않는 고형 성분은 통상 배합되지 않고, 연마제는 포함하지 않는 것이 바람직하다.In the composition for liquid oral cavity, particularly, the cleansing agent, it is preferable that a solid component not to be solubilized by an abrasive or the like is not ordinarily compounded, but does not contain an abrasive.

또한, 계면활성제로서는, (C) 비이온 계면활성제 및 (D) 양성 계면활성제 이외의 계면활성제는 배합하지 않아도 좋지만, 배합하는 경우는 0.5% 이하(0∼0.5%), 특히 0.05∼0.2%가 바람직하다.As the surfactant, a surfactant other than the nonionic surfactant (C) and the amphoteric surfactant (D) may not be blended, but in the case of blending, 0.5% or less (0 to 0.5%), particularly 0.05 to 0.2% desirable.

습윤제로서는, 예를 들면 소르비톨 등의 당(糖)알코올, 글리세린, 폴리에틸렌글리콜 등의 다가알코올을 들 수 있다. 이들 습윤제의 배합량은, 통상, 1∼40%, 특히 2∼40%이다.Examples of the wetting agent include sugar alcohols such as sorbitol, and polyhydric alcohols such as glycerin and polyethylene glycol. The blending amount of these wetting agents is usually 1 to 40%, particularly 2 to 40%.

용제로서는, 정제수가 일반적으로 사용되고, 조성물 중의 수분량이 상기 범위 내에서 첨가할 수 있다. 또한, 에탄올 등의 탄소수 1∼3의 저급 1가 알코올, 프로필렌글리콜 등을 배합하여도 좋다.As the solvent, purified water is generally used, and the water content in the composition can be added within the above range. Further, lower monohydric alcohols having 1 to 3 carbon atoms such as ethanol, propylene glycol and the like may be blended.

감미제로서는, 크실리톨, 말티톨, 사카린, 사카린나트륨, 스테비오사이드, 아스파르탐 등을 배합할 수 있다. 착색제로서, 청색1호, 녹색3호, 황색4호, 적색105호 등, 안전성이 높은 수용성 색소를 첨가할 수 있다. 방부제로서는, 파라옥시안식향산에스테르, 안식향산 또는 그 염을 들 수 있다.As the sweetening agent, xylitol, maltitol, saccharin, sodium saccharin, stevioside, aspartame and the like can be mixed. As the coloring agent, a water-soluble coloring matter having high safety such as Blue No. 1, Green No. 3, Yellow No. 4, and Red No. 105 can be added. Examples of the preservative include paraoxybenzoic acid ester, benzoic acid and salts thereof.

향료로서는, 페퍼민트유, 스피어민트유, 유칼리유, 윈터그린유, 클로브유, 타임유, 세이지유, 카르다몬유, 로즈마리유, 마조람유, 레몬유, 너트메그유, 라벤더 유, 파라크레스유 등의 천연정유, 및 l-멘톨, l-카르본, 신나믹알데히드, 오렌지 오일, 아네톨, 1,8-시네올, 메틸살리실레이트, 오이게놀, 티몰, 리날로올, 리모넨, 멘톤, 멘틸아세테이트, 시트랄, 캠퍼, 보르네올, 피넨, 스필란톨 등의 상기 천연정유 중에 포함된 향료 성분, 또한, 에틸아세테이트, 에틸부틸레이트, 이소 아밀아세테이트, 헥사날, 헥세날, 메틸안트라닐레이트, 에틸메틸페닐글리시데이트, 벤즈알데히드, 바닐린, 에틸바닐린, 프라네올, 말톨, 에틸말톨 감마/델타데카락톤, 감마/델타운데카락톤, N-에틸-p-멘탄-3-카르복사미드, 멘틸락테이트, 에틸렌글리콜-l-멘틸카보네이트 등의 향료 성분, 나아가서는, 몇가지의의 향료 성분이나 천연정유를 조합시켜서 이루어지는, 애플, 바나나, 스트로베리, 블루베리, 멜론, 피치, 파인애플, 포도, 무스카트, 와인, 체리, 스쿼시, 커피, 브랜디, 요구르트 등의 조합 플레이버의 1종 또는 2종 이상을, 조성물 중 0.00001∼3%로, 본 발명의 효과를 방해하지 않는 범위에서 사용할 수 있다.Examples of the perfume include natural essential oils such as peppermint oil, spearmint oil, eucalyptus oil, wintergreen oil, clove oil, time oil, sage oil, cardamon oil, rosemary oil, marzam oil, lemon oil, nutmeg oil, lavender oil, paracrine oil Methylene salicylate, eugenol, thymol, linalool, limonene, menthone, menthyl acetate, lauric acid, lauric acid, A perfume ingredient contained in the natural essential oils such as citral, camphor, borneol, pinene, spilan tall and the like, and a perfume ingredient such as ethyl acetate, ethyl butyrate, isoamyl acetate, hexanal, hexenyl, methyl anthranilate, Ethyl-p-menthane-3-carboxamide, menthyllactate, ethyleneglycol, ethyleneglycol, ethyleneglycol, trimethylolpropane, -l-menthyl carbonate and the like And furthermore it is also possible to use a flavoring agent such as apple, banana, strawberry, blueberry, melon, pitch, pineapple, grape, muscat, wine, cherry, squash, coffee, brandy, yogurt One or two or more kinds of combine flavors may be used in an amount of 0.00001 to 3% in the composition so long as they do not interfere with the effect of the present invention.

유효성분으로서는, 질산칼륨, 염화세틸피리디늄에 더하여, 이소프로필메틸페놀 등의 살균제, 트라넥삼산, 입실론아미노카프론산 등의 항염증제, 덱스트라나제 등의 효소, 불화나트륨, 모노플루오로인산나트륨 등의 불화물, 알란토인, 비타민C 등의 비타민류, 구리 화합물, 식물 추출물 등을 들 수 있다. 또한, 이들의 유효성분의 첨가량은, 본 발명의 효과를 방해하지 않는 범위로 할 수 있다.Examples of the active ingredient include, in addition to potassium nitrate and cetylpyridinium chloride, fungicides such as isopropylmethylphenol, antiinflammatory agents such as tranexamic acid and epsilon aminocaproic acid, enzymes such as dextranase, sodium fluoride, sodium monofluorophosphate , Allantoin, vitamins such as vitamin C, copper compounds, and plant extracts. The amount of the active ingredient to be added may be within a range that does not hinder the effect of the present invention.

실시례Example

이하, 실시례 및 비교례, 처방례를 나타내어, 본 발명을 구체적으로 설명하지만, 본 발명은 하기한 실시례로 제한되는 것이 아니다. 또한, 하기한 예에서 %는 특히 단서가 없는 한 모두 질량%를 나타낸다. 또한, pH는 상기한 바와 마찬가지로 25℃에서 측정하였다.Hereinafter, the present invention will be described in detail by way of examples, comparative examples, and formulations, but the present invention is not limited to the following examples. In the following examples,% represents mass% unless otherwise specified. The pH was measured at 25 캜 as described above.

[실시례, 비교례][Practical example, comparative example]

표 1, 2에 표시하는 조성의 액체 구강용 조성물(세구제)을 일상 방법에 의해 조제하였다. 얻어진 세구제에 관해, 하기한 방법 및 기준에 의해 평가를 행한 바, 표 1, 2와 같은 결과가 얻어졌다.A liquid oral composition (salve) having the compositions shown in Tables 1 and 2 was prepared by a routine method. The results are shown in Tables 1 and 2, with respect to the obtained curing agent, by the following methods and criteria.

(1) 외관 안정성(석출 억제 효과)의 평가 방법(1) Evaluation method of appearance stability (precipitation inhibiting effect)

표에 기재된 각 세구제를 100㎖의 페트병 중에 80㎖ 넣고, 25℃ 항온조 중에 정치(靜置) 보존하고, 4주간 후의 외관을 하기한 평점 기준에 따라 육안으로 판정하였다. 5샘플의 평균치를 구하고, 하기한 평가 기준에 따라 평가하였다.80 mL of each of the tax remedies listed in the table was placed in a 100 mL PET bottle and stored in a constant temperature bath at 25 ° C. The appearance after 4 weeks was judged visually according to the following criteria. The average value of 5 samples was obtained and evaluated according to the following evaluation criteria.

평점 기준 :Rated by:

4점 : 석출물이 전혀 없었다4 points: There was no precipitate

3점 : 석출물이 근소하게 있었다3 point: The precipitate was slightly

2점 : 석출물이 약간 있었다2 points: There were some precipitates

1점 : 석출물이 상당히 있었다1 point: There was considerable precipitate

외관 안정성(석출 억제 효과)의 평가 기준 :Evaluation criteria for appearance stability (precipitation inhibiting effect):

◎ : 평균점 3.5점 이상 4.0점 이하◎: Average point 3.5 or more and 4.0 or less

○ : 평균점 3.0점 이상 3.5점 미만○: 3.0 points or more and less than 3.5 points

△ : 평균점 2.0점 이상 3.0점 미만△: Average point of 2.0 points or more and less than 3.0 points

× : 평균점 2.0점 미만X: Average point less than 2.0 point

(2) 지각 과민 억제 효과의 평가 방법(2) Evaluation method of inhibiting the hypersensitive hypersensitivity

표에 기재된 각 세구제를, 상아질 지각 과민을 갖는 사람 5명에게 1개월간, 통상의 방법으로 세구(洗口)하여 사용시키고, 지각 과민의 억제 효과를 하기 평점 기준으로 판정하였다. 피험 5명의 평균치를 구하고, 하기한 평가 기준에 따라 평가하였다.Each of the cigarette removers listed in the table was used for five months to dentine sensitive hypoglycemia for one month in a conventional manner, and the suppressive effect of the hypersensitivity was evaluated on the basis of the following criteria. The average value of 5 subjects was obtained and evaluated according to the following evaluation criteria.

지각 과민 억제 효과의 평점 기준 :Rating criteria for inhibiting the hypersensitivity:

3점 : 통증을 느끼지 않게 되었다3 points: I did not feel any pain

2점 : 거의 통증을 느끼지 않게 되었다2 points: I almost did not feel any pain.

1점 : 통증을 느낀다1 point: I feel pain

지각 과민 억제 효과의 평가 기준 :Evaluation criteria for inhibiting hypersensitivity:

◎ : 2.5점 이상 3.0점 이하◎: 2.5 points or more and 3.0 points or less

○ : 2.0점 이상 2.5점 미만○: 2.0 points or more and less than 2.5 points

△ : 1.5점 이상 2.0점 미만?: 1.5 or more and less than 2.0 points

× : 1.5점 미만×: less than 1.5 points

(3) 구강내 부유균에 대한 살균 효과의 평가 방법(3) Evaluation method of sterilization effect on airborne bacteria in oral cavity

사용한 균액(菌液)은, 배양액으로서 트립티케이스 소이 브로트(Difco사제) 30g을 1ℓ의 정제수에 용해한 것을, 구강 상재(常在) 세균으로서 ?읗?렙토코쿠스 뮤탄스ATCC10449주(株)를 사용하고, 37℃, 혐기 조건하(5용량% 탄산가스, 95용량% 질소)로 1일 배양한 액의 550㎚에서의 투과도(透過度)가 20이 되도록 생리식염수를 가하여 조제하였다. 샘플(액체 구강용 조성물) 2.7㎖에 균액 0.3㎖을 가하고, 교반 후, 37℃로 1분간 반응시키고, 재차 교반 후, 미리 2.7㎖의 배양액이 들어간 시험관을 5개 준비하고, 그 1번째의 시험관에, 상기 균액을 가한 샘플 0.3㎖을 가하고, 교반하였다. 이 액 0.3㎖을 채취하고, 2번째의 시험관에 가하여, 교반하였다. 이 조작을 마찬가지로 3∼5번째의 시험관에 차례로 행하였다. 1, 3, 5번째의 시험관 중의 배양액을 교반 후, 10% 면양(綿羊) 탈섬혈(脫殲血) 함유 트립티케이스 소이 한천 평판(Difco사제)에 50㎕ 도말(塗沫)하고, 혐기 조건하에서 배양하였다. 생육한 콜로니를 계측하고, 잔존하는 ?읗?렙토코쿠스 뮤탄스균(菌)의 생균수(生菌數)(cfu)를 구하고, 하기한 기준에 따라, 부유균 살균 효과를 판정하였다.The bacterial solution to be used was prepared by dissolving 30 g of a tryptic case soy broth (Difco) as a culture solution in 1 L of purified water to prepare a bacterial suspension containing 10 mg of Lactococcus mutans ATCC10449 Co., Ltd. as an oral bacterium , And was prepared by adding physiological saline so that the permeability (permeability) at 550 nm of the liquid cultured for 1 day under anaerobic conditions (5 volume% carbonic acid gas, 95 volume% nitrogen) was 20 at 37 ° C. 0.3 ml of the bacterial solution was added to 2.7 ml of the sample (liquid oral composition), and the mixture was stirred and reacted at 37 占 폚 for 1 minute. After stirring again, five test tubes containing 2.7 ml of the culture solution were prepared in advance, , 0.3 ml of the sample to which the bacterial solution was added was added and stirred. 0.3 ml of this solution was sampled, added to a second test tube, and stirred. This operation was likewise carried out successively in the third to fifth test tubes. The culture medium in the 1st, 3rd and 5th test tubes was stirred and then 50 쨉 l of a tryptic case soybean agar plate (Difco) containing 10% sheep desensitized blood was smoothed, Lt; / RTI > The grown colonies were counted and the viable cell count (cfu) of the remaining Leptococcus mutans bacteria was determined. The bactericidal effect of the floating bacteria was determined according to the following criteria.

판정 기준 :Criteria :

◎ : 생균수가 102 미만&Amp; cir &: Less than 10 < 2 &

○ : 생균수가 102 이상 103 미만○: Number of living cells 10 2 or more and less than 10 3

△ : 생균수가 103 이상 104 미만?: The number of viable cells was 10 3 or more and less than 10 4

× : 생균수가 104 이상×: number of viable bacteria is 10 4 or more

(4) 사용감(쓴맛의 없음)의 평가 방법(4) Evaluation method of feelings (no bitterness)

표에 기재된 각 세구제 10㎖을 입에 머금고, 30초간 헹군 후, 세구 후의 쓴맛에 관해 판정사 5명이 하기한 평점 기준에 의해 판정하였다. 5명의 평균치를 구하고, 하기한 평가 기준에 따라 평가하였다.Ten milliliters of each corticosteremic agent listed in the table was placed in the mouth and rinsed for 30 seconds. Five judges of the bitter taste after the cuffing were judged according to the following criteria. The average value of 5 persons was obtained and evaluated according to the following evaluation criteria.

평점 기준 :Rated by:

4점 : 쓴맛이 없었다4 points: There was no bitter taste.

3점 : 쓴맛이 거의 없었다3 points: Almost no bitter taste.

2점 : 쓴맛이 약간 있었다.2 points: There was bitter taste.

1점 : 쓴맛이 상당히 있었다1 point: There was a bitter taste.

사용감(세구 후의 쓴맛의 없음)의 평가 기준 :Feeling of use (no bitterness after categorization) Evaluation criteria:

◎ : 평균점 3.5점 이상 4.0점 이하◎: Average point 3.5 or more and 4.0 or less

○ : 평균점 3.0점 이상 3.5점 미만○: 3.0 points or more and less than 3.5 points

△ : 평균점 2.0점 이상 3.0점 미만△: Average point of 2.0 points or more and less than 3.0 points

× : 평균점 2.0점 미만X: Average point less than 2.0 point

사용 원료의 상세를 하기에 나타낸다.Details of the raw materials used are shown below.

(A) 질산칼륨 ; 질산칼륨 슈퍼 태블릿(오쓰카식품화학사제)(A) potassium nitrate; Potassium nitrate super tablet (manufactured by Otsuka Food Chemical Co., Ltd.)

(B) 염화세틸피리디늄 ; 염화세틸피리디늄(와코순약공업사제)(B) cetylpyridinium chloride; Cetylpyridinium chloride (manufactured by Wako Pure Chemical Industries, Ltd.)

(C) 폴리옥시에틸렌(100)경화피마자유 ;(C) polyoxyethylene (100) hardened castor oil;

에틸렌옥사이드의 평균부가몰수 100(닛코우케미칼즈사제)Average addition mole number 100 of ethylene oxide (manufactured by Nikko Chemicals Co., Ltd.)

폴리옥시에틸렌(40)경화피마자유 ;Polyoxyethylene (40) hardened castor oil;

에틸렌옥사이드의 평균부가몰수 40(닛코우케미칼즈사제)Average addition mole number 40 of ethylene oxide (manufactured by Nikko Chemicals)

(D) 알킬아미드베타인 ;(D) alkylamide betaine;

야자유지방산아미드프로필베타인의 30% 수용액, TEGO Betain CK OK(데구사사제)30% aqueous solution of palm oil fatty amide propyl betaine, TEGO Betain CK OK (manufactured by Degussa)

또한, 표 중도 포함하여, 알킬아미드베타인의 배합량은, 순분 환산치이다(이하, 마찬가지.).Incidentally, the compounding amount of the alkylamide betaine in the tables is the net conversion value (the same applies hereinafter).

[표 1][Table 1]

Figure pct00001
Figure pct00001

[표 2][Table 2]

Figure pct00002
Figure pct00002

* ; 비교례 8의 에탄올 배합 조성에서는, (A), (B)성분이 배합되어 있어도 불용성 침전물의 석출이 없고, 지각 과민 억제 효과, 부유균 살균 효과가 저하되는 일도 없었다.*; In the ethanol-blended composition of Comparative Example 8, there was no precipitation of insoluble precipitates, and the effect of suppressing the hypersensitivity and the sterilizing effect of the floating bacteria were not lowered even when the components (A) and (B) were blended.

이하, 처방례를 나타낸다. 사용 원료는 상기와 마찬가지이다. 이 세구제는, 외관 안정성(석출 억제 효과), 지각 과민 억제 효과, 부유균 살균 효과, 사용감(쓴맛의 없음)이 전부 우수하였다.Hereinafter, a prescription example is shown. The materials used are the same as above. These three remedies were all excellent in appearance stability (precipitation inhibiting effect), retarding hypersensitivity effect, sterilizing effect of floating bacteria, and feeling of use (no bitter taste).

[처방례] 세구제[Prescription]

(A) 질산칼륨 5.0%(A) Potassium nitrate 5.0%

(B) 염화세틸피리디늄 0.05(B) cetylpyridinium chloride 0.05

(C) 폴리옥시에틸렌(60)경화피마자유 0.5(C) Polyoxyethylene (60) Hardened castor oil 0.5

(D) 알킬아미드베타인 0.3(D) Alkyl amide betaine 0.3

글리세린 3.0Glycerin 3.0

프로필렌글리콜 8.0Propylene glycol 8.0

사카린나트륨 0.1Sodium saccharin 0.1

인산2수소 나트륨 0.5Sodium dihydrogen phosphate 0.5

수산화나트륨 0.16Sodium hydroxide 0.16

향료 0.2Fragrance 0.2

(E) (E) 정제수Purified water 82.19 82.19

합계 100.0%Total 100.0%

pH 6.8pH 6.8

Claims (9)

(A) 질산칼륨 및 (B) 염화세틸피리디늄을 배합한 에탄올 무배합의 액체 구강용 조성물에, (C) 비이온 계면활성제 및 (D) 양성 계면활성제를 배합하고, (E) 수분량을 55질량% 이상 92질량% 미만으로 하고, 조성물의 pH를 6.8 이상 8.0 미만으로 한 것을 특징으로 하는 액체 구강용 조성물.(C) a nonionic surfactant and (D) an amphoteric surfactant in an ethanol-free liquid oral composition containing (A) potassium nitrate and (B) cetylpyridinium chloride, By mass to less than 92% by mass, and the pH of the composition is set to 6.8 or more and less than 8.0. 제1항에 있어서,
(C) 비이온 계면활성제가 폴리옥시에틸렌경화피마자유이고, (D) 양성 계면활성제가 알킬아미드베타인 또는 그 염인 것을 특징으로 하는 액체 구강용 조성물.
The method according to claim 1,
(C) the nonionic surfactant is a polyoxyethylene hardened castor oil, and (D) the amphoteric surfactant is an alkylamide betaine or a salt thereof.
제1항 또는 제2항에 있어서,
(C) 비이온 계면활성제가, 에틸렌옥사이드의 평균부가몰수가 40∼100몰의 폴리옥시에틸렌경화피마자유이고, (D) 양성 계면활성제가, 야자유지방산아미드프로필베타인인 것을 특징으로 하는 액체 구강용 조성물.
3. The method according to claim 1 or 2,
(C) the nonionic surfactant is polyoxyethylene hydrogenated castor oil having an average addition mole number of ethylene oxide of 40 to 100 moles, and (D) the amphoteric surfactant is palm oil fatty acid amide propyl betaine. Composition.
제1항 내지 제3항 중 어느 한 항에 있어서,
(C)성분을 0.1∼2질량%, (D)성분을 0.1∼2질량% 배합한 것을 특징으로 하는 액체 구강용 조성물.
4. The method according to any one of claims 1 to 3,
, 0.1 to 2 mass% of component (C), and 0.1 to 2 mass% of component (D).
제1항 내지 제4항 중 어느 한 항에 있어서,
(A)성분을 0.01∼10질량%, (B)성분을 0.001∼0.1질량% 배합한 것을 특징으로 하는 액체 구강용 조성물.
5. The method according to any one of claims 1 to 4,
0.01 to 10 mass% of component (A) and 0.001 to 0.1 mass% of component (B).
제1항 내지 제5항 중 어느 한 항에 있어서,
세구제인 것을 특징으로 하는 액체 구강용 조성물.
6. The method according to any one of claims 1 to 5,
Or a salt thereof.
제1항 내지 제6항 중 어느 한 항에 있어서,
지각 과민 및 우식 억제용인 것을 특징으로 하는 액체 구강용 조성물.
7. The method according to any one of claims 1 to 6,
Wherein the composition is for inhibiting hypersensitivity and dental caries.
(A) 질산칼륨 및 (B) 염화세틸피리디늄을 배합한 에탄올 무배합의 액체 구강용 조성물에, (C) 비이온 계면활성제 및 (D) 양성 계면활성제를 배합하고, (E) 수분량을 55질량% 이상 92질량% 미만으로 하고, 조성물의 pH를 6.8 이상 8.0 미만으로 하는 것을 특징으로 하는, 상기 액체 구강용 조성물에서의 (A) 질산칼륨 및 (B) 염화세틸피리디늄의 병용에 의해 생기는 불용성 침전물의 석출 억제 방법.(C) a nonionic surfactant and (D) an amphoteric surfactant in an ethanol-free liquid oral composition containing (A) potassium nitrate and (B) cetylpyridinium chloride, (A) nitric acid potassium and (B) cetylpyridinium chloride in the liquid oral composition, wherein the composition has a pH of not less than 92 mass% and a pH of the composition of not less than 6.8 and less than 8.0. A method for inhibiting precipitation of insoluble precipitates. 액체 구강용 조성물이 세구제인 것을 특징으로 하는, 제8항에 기재된 액체 구강용 조성물에서의 (A) 질산칼륨 및 (B) 염화세틸피리디늄의 병용에 의해 생기는 불용성 침전물의 석출 억제 방법.A method for inhibiting the precipitation of an insoluble precipitate caused by the combined use of (A) potassium nitrate and (B) cetylpyridinium chloride in the liquid oral composition according to claim 8, wherein the liquid oral composition is a three-part cleansing agent.
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