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KR101472304B1 - Nano emulsion with stable and uniform particle size distribution - Google Patents

Nano emulsion with stable and uniform particle size distribution Download PDF

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KR101472304B1
KR101472304B1 KR1020070141288A KR20070141288A KR101472304B1 KR 101472304 B1 KR101472304 B1 KR 101472304B1 KR 1020070141288 A KR1020070141288 A KR 1020070141288A KR 20070141288 A KR20070141288 A KR 20070141288A KR 101472304 B1 KR101472304 B1 KR 101472304B1
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신홍주
안순애
권이경
조준철
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(주)아모레퍼시픽
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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
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04Dispersions; Emulsions
    • A61K8/06Emulsions
    • 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
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
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    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8141Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • A61K8/8152Homopolymers or copolymers of esters, e.g. (meth)acrylic acid esters; Compositions of derivatives of such polymers
    • 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
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    • 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
    • A61K8/89Polysiloxanes
    • 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/413Nanosized, i.e. having sizes below 100 nm

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Abstract

본 발명은 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 블록공중합체와 보조 계면활성제를 유화 안정화제로 사용하여 안정화한 나노에멀젼, 이의 제조방법 및 이를 함유하는 화장료 조성물에 관한 것이다. 보다 상세하게는 폴리카프로락톤-폴리에틸렌글리콜 블록공중합체와 보조계면활성제로 고분자계 계면활성제인 이눌린라우릴카바메이트, 폴록사머 또는 이들의 혼합물을 사용하여 대단히 균일한 입도 분포와 높은 안정도를 가지는 나노에멀젼을 제공하는 것이 특징이다.The present invention relates to a nanoemulsion stabilized by using a polycaprolactone-polyethylene glycol (PCL-PEG) block copolymer and a cosurfactant as emulsion stabilizers, a process for producing the same, and a cosmetic composition containing the same. More particularly, the present invention relates to a method for producing a nano emulsion having a very uniform particle size distribution and high stability by using a polycaprolactone-polyethylene glycol block copolymer and an anionic surfactant such as inulin lauryl carbamate, poloxamer, .

나노 에멀젼, 에멀젼, 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 블록공중합체, 고분자계 계면활성제 Nano emulsion, emulsion, polycaprolactone-polyethylene glycol (PCL-PEG) block copolymer, high-molecular surfactant

Description

안정하고 균일한 입도분포를 가지는 나노에멀젼{A stable nano-emulsion with narrow particle size distribution}A stable nano-emulsion with narrow particle size distribution has a stable and uniform particle size distribution.

본 발명은 양친매성고분자를 함유한 안정하고 균일한 입도분포를 가지는 나노에멀젼, 이의 제조방법 및 이를 함유하는 화장료 조성물에 관한 것이다. 보다 상세하게는 양친매성고분자로 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 블록공중합체와 보조 계면활성제로 주안정화제로서 양친매성 고분자인 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 블록공중합체와 보조 계면활성제로서 이눌린라우릴카바메이트, 폴록사머 또는 이들의 혼합물을 포함하는 것을 특징으로 한다. The present invention relates to a nanoemulsion having a stable and uniform particle size distribution containing an amphipathic polymer, a method for producing the same, and a cosmetic composition containing the same. (PCL-PEG) block copolymer as an amphipathic polymer and a polycaprolactone-polyethylene glycol (PCL-PEG) block copolymer as an auxiliary surfactant as amphipathic polymer Characterized in that it comprises inulin lauryl carbamate, poloxamer or mixtures thereof as a surfactant.

에멀젼은 하나의 액상에 섞이지 않는 하나 이상의 액상이 분산되어 있는 액-액 분산계를 말하는데, 일반적으로 0.1 마이크로미터(mm)에서 수십 마이크로미터(mm)의 크기 분포를 가진다. 이와 같은 매크로에멀젼은 열역학적으로 불안정 상태이며 응집(Flocculation), 침강(Sedimentation), 크리밍(Creaming), 입자성장(Ostwald ripening), 유착(Coalescence) 등과 같은 다양한 경로로 종국에는 분리되려는 성질을 가지고 있다. 이때 분산상의 에멀젼 입자의 크기가 나노 크기로 작아지면 입자간의 브라운 운동에 의해 동역학적(Kinetic) 측면에서 에멀젼의 안정도 를 크게 향상시킬 수 있고, 내상의 함량이 높은 저점도의 에멀젼을 제조할 수 있기 때문에 다양한 사용감을 가진 화장료를 만들 수 있을 뿐만 아니라 입자크기가 작아 피부에 유효성분을 효과적으로 전달할 수 있는 장점이 있다. An emulsion refers to a liquid-liquid dispersion system in which one or more liquid phases are dispersed in one liquid phase, and generally has a size distribution of 0.1 to several tens of micrometers (mm). These macroemulsions are thermodynamically unstable and are eventually separated by various routes such as flocculation, sedimentation, creaming, Ostwald ripening, coalescence, and the like . If the size of the emulsion particle of the dispersed phase is reduced to the nano size, the stability of the emulsion can be greatly improved in terms of kinetic by the Brownian motion between the particles, and a low viscosity emulsion having a high internal phase content can be produced Therefore, it is possible not only to make a cosmetic having various feeling of use but also to have an effect of effectively transmitting an effective ingredient to the skin because of its small particle size.

문헌에 따라 조금씩 차이는 있으나 일반적으로 분산상의 입자의 평균 직경이 20~500nm인 액-액 분산계를 나노에멀젼이라고 하는데(Flockhart, I. R. etc, Nanoemulsions derived from lanolin show promising drug delivery properties, J. Pharm. pharmacol., 50(Supplement)1998, 141), 보통 고압유화법나 PIT 유화법을 사용하고 있다. 고압유화법는 인지질을 주계면활성제로 사용하고 적당한 보조 계면활성제(co-surfactant)를 병용하여 고압(예를 들어, 약 800 ~ 1,500 기압)의 유화기(High pressure homogenizer)를 사용하여 입자를 나노 크기로 쪼개주는 방법인데, 인지질의 고온 불안정성(예를 들어, 오일분리, 크리밍, 등)으로 인해 변취나 고온 안정도가 떨어지며, 특히 분산상의 입도 분포가 상대적으로 넓어 제조 로트마다 균질한 품질을 확보하기 어려운 단점이 있었다. 그리고 PIT 법은 PIT(Phase Transition Temperature 혹은 HLB temperature)를 가지는 특정 계면활성제 시스템에 한정되며, 계면활성제에 따라 온도 범위가 좁거나 넓을 수 있기 때문에 제조가 제한적이고 어렵다는 문제를 가지고 있었다. Although liquid-liquid dispersion systems having an average diameter of 20 to 500 nm in dispersed phase particles are called nanoemulsions (Flockhart, IR et al., Nanoemulsions derived from lanolin show promising drug delivery properties, J. Pharm. Pharmacol ., 50 (Supplement) 1998, 141), usually using high-pressure emulsification or PIT emulsification. The high-pressure emulsification method uses a phospholipid as the main surfactant and a suitable co-surfactant in combination with a high pressure homogenizer at high pressure (for example, about 800 to 1,500 atm) (Eg, oil separation, creaming, etc.), the stability and stability at high temperatures are deteriorated. Particularly, since the particle size distribution of the dispersed phase is relatively wide, it is possible to obtain a homogeneous quality per production lot There were difficult disadvantages. The PIT method is limited to a specific surfactant system having a PIT (Phase Transition Temperature or HLB temperature). Since the temperature range may be narrow or wide depending on the surfactant, the PIT method has a problem of being limited and difficult to manufacture.

이에 본 발명자들은 제조 중 발생할 수 있는 변취 문제 해결 및 제조된 나노에멀젼의 고온 안정성을 확보하고 더 나아가 균일한 입도 분포를 가져 품질의 균질성을 높일 수 있는 방법에 대해 지속적인 연구를 통해 양친매성 고분자인 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 블록공중합체를 주안정화제로 포함하고 보조 계 면활성제로 이눌린라우릴카바메이트, 폴록사머 혹은 이의 혼합물을 포함하는 나노 에멀젼은 제조 중 발생되는 변취의 문제와 나노 에멀젼의 고온 안정성을 획기적으로 개선할 수 있을 뿐만 아니라 균일한 입도분포를 가지는 것을 확인하였다. Therefore, the inventors of the present invention have continued to investigate a method of solving the problem of mangling during manufacturing and securing the high temperature stability of the prepared nanoemulsion and further increasing the homogeneity of quality by having a uniform particle size distribution, A nanoemulsion containing caprolactone-polyethylene glycol (PCL-PEG) block copolymer as a desizing agent and an auxiliary surfactant including inulin lauryl carbamate, poloxamer, or a mixture thereof, It was confirmed that not only the stability of the emulsion at high temperature can be remarkably improved, but also the particle size distribution is uniform.

본 발명이 이루고자 하는 기술적 과제는 제조 중 발생할 수 있는 변취 문제를 해결하고 균일한 입도 분포를 가지면서 고온에서 안정한 나노에멀젼 및 이를 함유하는 화장료 조성물을 제공하는데 있다. 이를 위해 다양한 종류의 양친매성 물질들과 오일의 종류 및 함량에 따른 나노에멀젼 양친매성 고분자인 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 블록공중합체를 주안정화제로 사용하고 보조 계면활성제로 이눌린라우릴카바메이트, 폴록사머 혹은 이의 혼합물로 제조되는 나노 에멀젼은 제조 중 발생되는 변취의 문제와 나노 에멀젼의 고온 안정성을 획기적으로 개선할 수 있을 뿐만 아니라 균일한 입도분포를 가지는 것을 확인하고 본 발명을 완성하게 되었다.Disclosure of Invention Technical Problem [8] Accordingly, the present invention has been made in view of the above problems, and an object of the present invention is to provide a nano emulsion which has a uniform particle size distribution and stable at a high temperature and a cosmetic composition containing the nano emulsion. For this purpose, a variety of amphipathic materials, polycaprolactone-polyethylene glycol (PCL-PEG) block copolymer, which is a nano-emulsion amphipathic polymer according to the kind and content of oil, is used as a desizing agent, The nanoemulsion prepared from a carbamate, poloxamer or a mixture thereof can remarkably improve the stability of the nano-emulsion at the high temperature and the problem of the manganese produced during the production, and has a uniform particle size distribution. .

따라서 본 발명의 목적은 균일한 입도분포를 가지는 안정한 나노에멀젼 및 이를 함유하는 화장료 조성물을 제공하는 것이다. Accordingly, an object of the present invention is to provide a stable nanoemulsion having a uniform particle size distribution and a cosmetic composition containing the same.

상기의 목적을 달성하기 위해 주안정화제로서 양친매성 고분자인 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 블록공중합체와 보조 계면활성제로서 이눌린라우릴카바메이트, 폴록사머 또는 이들의 혼합물을 포함하는 본 발명에 따른 나노에멀젼은 나노에멀젼 총 중량에 대하여 주안정화제인 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 블록공중합체를 0.1내지 10중량%, 바람직하게는 0.1 내지 3 중량%를 사용하고 보조 계면활성제인 이눌린라우릴카바메이트, 폴록사머 및 이들의 혼합물 을 0.01내지 10중량%, 바람직하게는 0.1 내지 3 중량%를 사용하는 것을 특징으로 한다. 주안정화제인 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 블록공중합체는 PCL(폴리카프로락톤)과 PEG(폴리에틸렌글리콜)의 중량비가 1:2에서 12:1인 것인바, 보다 바람직하게는 1:1에서 4:1이고, 분자량이 2,000에서 60,000 달톤 정도가 가능한 바, 보다 바람직하게는 분자량이 4,000에서 20,000 달톤인 블록공중합체를 말하며, 예를 들어 상품명 PCG-101이 예시된다.In order to achieve the above objects, the present invention provides a method for producing a polyurethane foam, which comprises a polycaprolactone-polyethylene glycol (PCL-PEG) block copolymer, which is an amphipathic polymer, as a diazotizing agent and an inulin laurylcarbamate, poloxamer, Is used in an amount of 0.1 to 10% by weight, preferably 0.1 to 3% by weight, based on the total weight of the nano emulsion, of a polycaprolactone-polyethylene glycol (PCL-PEG) 0.01 to 10% by weight, preferably 0.1 to 3% by weight, of an inorganic lauryl carbamate, poloxamer, and a mixture thereof. The weight ratio of PCL (polycaprolactone) to PEG (polyethylene glycol) is 1: 2 to 12: 1, more preferably 1: 1 to 4: 1, a molecular weight of 2,000 to 60,000 daltons, and more preferably a molecular weight of 4,000 to 20,000 daltons, for example, trade name PCG-101.

폴록사머로는 화학식 1로 표시되는 폴리옥시에틸렌과 폴리옥시프로필렌 공중합체가 사용되었고, 예를 들면 상품명 Lutrol F-127(폴록사머 407)을 들 수 있다.As the poloxamer, polyoxyethylene and polyoxypropylene copolymer represented by the general formula (1) are used, and for example, trade name Lutrol F-127 (Poloxamer 407) can be mentioned.

[화학식 1][Chemical Formula 1]

Figure 112007094919610-pat00001
Figure 112007094919610-pat00001

상기 화학식 1에서, X = 2 내지 128, Y = 16 내지 67, Z = 2 내지 128이다.In Formula 1, X = 2 to 128, Y = 16 to 67, and Z = 2 to 128.

또한 본 발명에 따른 나노에멀젼은 실리콘 오일, 에스테르계 오일, 하이드로카본계 오일, 식물성 오일, 자외선차단오일 및 이들의 혼합물을 0.1 내지 60 중량%, 바람직하게는 5 내지 30 중량%를 사용하는 것을 특징으로 한다. 실리콘 오일은 옥타메틸사이클로테트라실록산 및 데카메틸사이클로펜타실록산 등과 같이 하기 화학식 2로 표시되는 사이클로메치콘형 실리콘 오일을 사용하는 것이 바람직하다: The nanoemulsion according to the present invention is characterized in that 0.1 to 60% by weight, preferably 5 to 30% by weight, of a silicone oil, an ester oil, a hydrocarbon oil, a vegetable oil, an ultraviolet barrier oil and a mixture thereof is used . The silicone oil is preferably a cyclomethicon type silicone oil represented by the following formula (2) such as octamethylcyclotetrasiloxane and decamethylcyclopentasiloxane and the like:

[화학식 2](2)

Figure 112007094919610-pat00002
Figure 112007094919610-pat00002

또한 비휘발성 실리콘 오일로는 디메치콘 및 폴리페트리닐메치콘; 탄화수소계 오일로는 스쿠알란, 유동파라핀 및 하이드로제네이티드 C6-14 올레핀폴리머; 에스테르계 오일로는 부틸렌글라이콜디카프릴레이트-디카프레이트, C14-18 알킬에틸헥사노에이트, 디카프릴릴카보네이트, 세틸옥타노에이트 및 옥틸도데실미리스테이트; 식물성 오일로는 메도폼씨드오일, 올리브오일 및 호호바오일;자외선 차단오일로는 에틸헥실메톡시신나메이트, 옥틸살리실레이트, 에틸헥실트리아진 및 비스-에틸헥실옥시페놀메톡시페닐트리아진을 예로 들 수 있으나 이에만 한정되는 것은 아니다.Non-volatile silicone oils also include dimethicone and polypetryinyl methicone; Hydrocarbon-based oils include squalane, liquid paraffin, and hydrogenated C6-14 olefin polymers; Examples of ester-based oils include butyleneglycol dicaprylate-dicaprate, C14-18 alkyl ethylhexanoate, dicaprylyl carbonate, cetyl octanoate and octyldodecyl myristate; Examples of the vegetable oil include methoform seed oil, olive oil and jojoba oil, and examples of the ultraviolet barrier oil include ethylhexylmethoxycinnamate, octyl salicylate, ethylhexyltriazine, and bis-ethylhexyloxyphenol methoxyphenyltriazine But is not limited thereto.

또한 본 발명의 나노에멀젼에는 나노 입자의 계면막 강화를 위해 C12~C22의 지방산 알코올을 에멀젼 총 중량에 대하여 0.1 내지 10 중량%를 함유하는 포함할 수 있으며, 보조성분으로 색소, 향, 방부제, 점증제 등을 나노에멀젼 총 중량에 대하여 0 내지 20 중량%을 함유할 수 있다. In addition, the nanoemulsion of the present invention may contain 0.1 to 10% by weight of C12 to C22 fatty acid alcohols based on the total weight of the emulsion for enhancing the interfacial film of the nanoparticles, and may contain pigments, fragrances, preservatives, And the like may be contained in an amount of 0 to 20% by weight based on the total weight of the nano emulsion.

상기 지방산 알코올로는 세토스테아릴알코올, 비헤닐알코올 등이 예시되며, 점증제로는 에칠아크릴레이트/소듐아크릴로일디메칠타우레이트코폴리머, 카보머, 폴리아크릴레이트-13 등이 예시된다. Examples of the fatty alcohol include cetostearyl alcohol, biphenyl alcohol and the like. Examples of the fatty alcohol include ethyl acrylate / sodium acryloyldimethyltaurate copolymer, carbomer, and polyacrylate-13.

본 발명에서 제공하는 나노에멀젼은 수성상과 유성상을 50℃~ 80℃의 온도에서 균일하게 혼합/용해시킨 후 이를 500~2500 bar의 압력에서 균질화하여 제조할 수 있다. The nanoemulsion provided in the present invention can be prepared by uniformly mixing / dissolving the aqueous phase and the oil phase at a temperature of 50 ° C to 80 ° C and homogenizing the mixture at a pressure of 500 to 2500 bar.

본 발명에 따른 나노에멀젼의 제조방법은 상세하게는 수상성분을 50 내지 80℃에서 교반하면서 안정화제인 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 공중합체를 포함하는 유상성분을 첨가하여 프리에멀젼을 제조하는 단계; 상기 프리에멀젼을 고압유화기에서 500 내지 2500bar의 압력에서 균질화하는 단계; 를 포함하며, 보조 계면활성제로서 이눌린라우릴카바메이트를 상기 수상성분에 포함하거나, 폴록사머를 상기 유상성분에 포함하거나, 또는 이들 보조 계면활성제로 이눌린라우릴카바메이트를 상기 수상성분에 포함하고 폴록사머를 상기 유상성분에 포함하는 것을 특징으로 한다.The method for preparing a nanoemulsion according to the present invention comprises: preparing a pre-emulsion by adding an oil component containing a copolymer of poly (caprolactone-polyethylene glycol) (PCL-PEG) ; Homogenizing the pre-emulsion in a high-pressure emulsifier at a pressure of 500 to 2500 bar; , Wherein inulin lauryl carbamate as an auxiliary surfactant is included in the aqueous phase component, poloxamer is contained in the oil phase component, or inulin lauryl carbamate is included in the aqueous phase component with these cosurfactants, Characterized in that the oil component is contained in the oil component.

본 발명에 따른 나노에멀젼을 함유하는 화장료 조성물의 제형에는 특별한 제한은 없으나 피부, 점막, 두피 또는 모발 등에 사용할 수 있는 것으로서, 상기 화장료 조성물은 유연화장수, 영양화장수, 로션, 크림, 팩, 젤, 패치 또는 스프레이(미스트)으로부터 선택되는 기초 화장료 조성물, 립스틱, 메이크업베이스, 또는 파운데이션으로부터 선택되는 색조 화장료 조성물, 샴푸, 린스, 바디클렌저, 치약, 구강 청정제로부터 선택되는 세정료 조성물, 또는 헤어토닉, 젤, 무스 등의 정발제, 양모제, 염모제로부터 선택되는 모발용 화장료 조성물을 포함하며, 또한 로션, 연고, 겔, 크림, 패취 또는 분무제와 같은 의약품 및 의약부외품 등으로 폭넓게 적 용할 수 있다. The formulation of the cosmetic composition containing the nanoemulsion according to the present invention is not particularly limited, but it can be used for skin, mucous membrane, scalp or hair, and the cosmetic composition can be used as a softener, a lotion, a cream, A cleaning composition selected from basic cosmetic compositions, lipsticks, makeup bases or foundations selected from the group consisting of cosmetics, cosmetics, perfumes, cosmetics, perfumes, Hair cosmetic compositions selected from hair growth agents, hair growth agents, hair growth promoters, hair growth promoters, hair growth promoters, hair growth promoters, hair growth promoters, antioxidants, antioxidants, antioxidants and antioxidants.

양친매성 고분자인 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 블록공중합체를 주안정화제로 사용하고 보조 계면활성제로 이눌린라우릴카바메이트, 폴록사머 혹은 이의 혼합물을 사용하여 제조된 본 발명에 따른 나노에멀젼 혹은 이를 함유하는 화장료 조성물은 제조 중 발생되는 변취의 문제와 고온 안정성을 획기적으로 개선할 수 있을 뿐만 아니라 균일한 입도분포를 가지고 있어서 로트별 품질 균질성을 극대화 할 수 있는 효과가 있다. The nanoemulsion according to the present invention, prepared by using an amphipathic polymer, a polycaprolactone-polyethylene glycol (PCL-PEG) block copolymer as a desalting agent and an auxiliary surfactant using inulin lauryl carbamate, poloxamer, Or a cosmetic composition containing the cosmetic composition can remarkably improve the problem of extraction and high-temperature stability during production, and has a uniform particle size distribution, thereby maximizing quality uniformity per lot.

이하, 실시예 및 시험예를 들어 본 발명을 보다 상세하게 설명하기로 한다. 그러나, 본 발명의 범위가 하기 실험예 및 시험예 등으로 한정되는 것은 아니다. Hereinafter, the present invention will be described in more detail with reference to examples and test examples. However, the scope of the present invention is not limited to the following experimental examples and test examples.

[제조예][Manufacturing Example]

표 1에 기재된 유상성분을 혼합하여 60℃~ 70℃로 가온한 후 완전 용해하였으며, 표1에 기재된 수상성분을 혼합하여 용해한 후 60℃~ 70℃로 가온하였다. 상기 상기 수상성분을 호모게나이저(Homogenizer)를 이용하여 7000rpm으로 교반하면서 60℃~70℃에서 상기 유상성분을 서서히 첨가하여 유화하여 프리에멀젼(pre-emulsion)을 제조하였다. 제조된 프리에멀젼을 고압유화기(High pressure homogenizer)를 사용하여 1,000bar에서 1회 이상 재순환 처리하여 나노에멀젼을 제 조하였하였다. The oil components shown in Table 1 were mixed and heated to 60 ° C to 70 ° C and then completely dissolved. The aqueous components listed in Table 1 were mixed and dissolved, and then heated to 60 ° C to 70 ° C. The aqueous phase component was gradually added at 60 to 70 ° C while stirring at 7000 rpm using a homogenizer to emulsify the pre-emulsion. The prepared preemulsion was recycled at a rate of 1,000 bar once using a high pressure homogenizer to prepare a nanoemulsion.

[표-1][Table 1]

Figure 112007094919610-pat00003
Figure 112007094919610-pat00003

[ 실시예 ] 나노에멀젼 안정도 및 평균 입자크기 및 분포 [ Example ] Nano emulsion stability and average particle size and distribution

표1에 기재된 조성에 의하여 제조된 제조예 1 내지 제조예 3 및 비교예 1 내지 비교예 3의 나노에멀젼을 30도, 45도, 순환 항온조에서 크리밍이나 오일 분리와 같은 에멀젼 안정도를 관찰하고, 에멀젼의 평균입도와 입도 분포는 동적 레이저 광산란법(Dynamic Light Scattering, 기기 모델: Zetasizer 300HS, Malvern, UK)을 이용하여 측정하였다. 이때 산란각은 90도로 고정하고 측정온도는 25도로 유지하였다. 표-2에서 보는 바와 같이 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 블록공중합체를 주안정화제로 사용하면서 이눌린라우릴카바메이트, 폴록사머 혹은 이의 혼합물을 같이 배합할 경우 고온 안정도를 확보할 수 있음을 알 수 있다. 그러나 이에 반해 종래의 인지질을 사용한 나노에멀젼의 경우 고온에서 내용물의 변취나 오일 분리가 발생, 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 블록공중합체 단독으로 사용할 경우에도 나노에멀젼의 변취 문제는 해결되지만 고온 안정성이 떨어지는 것을 알 수 있다. 또한 도 1에서 보는 바와 같이 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 블록공중합체를 주안정화제로 사용하면서 이눌린라우릴카바메이트이나 폴록사머를 배합할 경우 균일한 입자크기를 가진 나노에멀젼을 얻을 수 있고, 특히 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 블록공중합체, 이눌린라우릴카바메이트, 그리고 폴록사머를 동시에 사용할 경우 평균 입자크기가 200nm 이하이면서 입도분포가 대단히 균일한 나노에멀젼을 제조할 수 있음을 알 수 있다. The emulsion stability of the nanoemulsion of Production Examples 1 to 3 and Comparative Examples 1 to 3 prepared according to the composition shown in Table 1 was observed at 30 degrees and 45 degrees in a circulating thermostat such as creaming and oil separation, The average particle size and particle size distribution of the emulsion were measured using Dynamic Light Scattering (instrument model: Zetasizer 300HS, Malvern, UK). At this time, the scattering angle was fixed at 90 degrees and the measurement temperature was maintained at 25 degrees. As shown in Table 2, when the polycaprolactone-polyethylene glycol (PCL-PEG) block copolymer is used as the eye-cleansing agent, inulin lauryl carbamate, poloxamer, or a mixture thereof can be used to secure high temperature stability . On the other hand, conventional nanoemulsions using phospholipids cause changes in contents or oil separation at high temperatures, and even when using a polycaprolactone-polyethylene glycol (PCL-PEG) block copolymer alone, the problem of nanoemulsion removal can be solved It can be seen that the high temperature stability is poor. Also, as shown in FIG. 1, when a polycaprolactone-polyethylene glycol (PCL-PEG) block copolymer is used as a desalting agent and inulin lauryl carbamate or poloxamer is blended, a nano emulsion having a uniform particle size can be obtained In particular, when a polycaprolactone-polyethylene glycol (PCL-PEG) block copolymer, inulin lauryl carbamate, and poloxamer are simultaneously used, a nano emulsion having an average particle size of 200 nm or less and a very uniform particle size distribution can be produced .

[표-2] 온도/시간에 따른 실시예와 비교예의 나노에멀젼 안정도 변화 [Table 2] Changes in stability of nanoemulsion in Examples and Comparative Examples according to temperature / time

Figure 112007094919610-pat00004
Figure 112007094919610-pat00004

도 1은 본 발명에 따른 나노에멀젼 입도분포이다.1 is a particle size distribution of the nano emulsion according to the present invention.

Claims (12)

주안정화제로서 양친매성 고분자인 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 블록공중합체와 보조 계면활성제로서 이눌린라우릴카바메이트, 폴록사머 또는 이들의 혼합물 및 실리콘 오일과 하이드로카본계 오일의 혼합물을 포함하는 나노에멀젼.Polycaprolactone-polyethylene glycol (PCL-PEG) block copolymer which is an amphipathic polymer as a main cleaning agent and a mixture of inulin lauryl carbamate, poloxamer or a mixture thereof and a silicone oil and a hydrocarbon oil as an auxiliary surfactant Nano emulsion. 제 1항에 있어서, The method according to claim 1, 나노에멀젼 총 중량에 대하여 주안정화제인 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 블록공중합체 0.1 내지 10중량%, 보조 계면활성제인 이눌린라우릴카바메이트, 폴록사머 또는 이들의 혼합물 0.01 내지 3중량% 및 실리콘 오일과 하이드로카본계 오일의 혼합물 0.1 내지 60 중량%를 포함하는 것을 특징으로 하는 나노에멀젼. 0.1 to 10% by weight of a polycaprolactone-polyethylene glycol (PCL-PEG) block copolymer as a shampooing agent based on the total weight of the nano emulsion, 0.01 to 3% by weight of an auxiliary surfactant inulin lauryl carbamate, poloxamer, And 0.1 to 60% by weight of a mixture of a silicone oil and a hydrocarbon-based oil. 삭제delete 삭제delete 삭제delete 제 1항에 있어서, The method according to claim 1, 나노에멀젼 총 중량에 대하여 C12~C22의 지방산 알코올 0.1 내지 10 중량%를 함유하는 것을 특징으로 하는 나노에멀젼.And 0.1 to 10% by weight of fatty alcohol of C12 to C22 with respect to the total weight of the nano emulsion. 제 1항에 있어서, The method according to claim 1, 색소, 향, 방부제, 점증제로부터 선택되는 1 이상의 보조성분을 총 중량에 대하여 나노에멀젼 총 중량에 대하여 0 내지 20 중량%을 함유하는 나노에멀젼.At least one auxiliary component selected from pigments, fragrances, preservatives and thickeners in an amount of 0 to 20% by weight based on the total weight of the total nano emulsion. 제 1항 내지 제 2항, 제 6항 및 제 7항에서 선택되는 어느 한 항에 따른 나노에멀젼을 함유하는 화장료 조성물.A cosmetic composition comprising a nanoemulsion according to any one of claims 1 to 6, 제 8 항에 있어서,9. The method of claim 8, 상기 화장료 조성물은 유연화장수, 영양화장수, 로션, 크림, 팩, 젤, 패치 또는 스프레이(미스트)으로부터 선택되는 기초 화장료 조성물, 립스틱, 메이크업베이스, 또는 파운데이션으로부터 선택되는 색조 화장료 조성물, 샴푸, 린스, 바디클렌저, 치약, 구강 청정제로부터 선택되는 세정료 조성물, 또는 헤어토닉, 젤, 무스 등의 정발제, 양모제, 염모제로부터 선택되는 모발용 화장료 조성물인 것을 특징으로 하는 화장료 조성물.The cosmetic composition may comprise at least one of a cosmetic composition selected from a cosmetic composition selected from softening longevity, nutrition lotion, lotion, cream, pack, gel, patch or spray (mist), lipstick, makeup base or foundation, shampoo, rinse, A cosmetic composition for hair which is selected from a cleansing composition selected from a cleanser, a toothpaste and an oral cleansing agent, or a hair cleansing agent such as a hair tonic, a gel and a mousse, a hair cleanser, and a hair dye. 수상성분을 50 내지 80℃에서 교반하면서 안정화제인 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 블록공중합체 및 실리콘 오일과 하이드로카본계 오일의 혼합물을 포함하는 유상성분을 첨가하여 프리에멀젼을 제조하는 단계;Preparing a pre-emulsion by adding an oil component comprising a mixture of a polycaprolactone-polyethylene glycol (PCL-PEG) block copolymer and a silicone oil and a hydrocarbon-based oil as stabilizers while stirring the aqueous phase components at 50 to 80 ° C ; 상기 프리에멀젼을 고압유화기에서 500 내지 2500bar의 압력에서 균질화하는 단계;Homogenizing the pre-emulsion in a high-pressure emulsifier at a pressure of 500 to 2500 bar; 를 포함하며,/ RTI > 보조 계면활성제로서 이눌린라우릴카바메이트를 상기 수상성분에 포함하거나, 폴록사머를 상기 유상성분에 포함하는 것을 특징으로 하는 나노에멀젼의 제조방법.Characterized in that inulin lauryl carbamate is contained in the aqueous phase component as an auxiliary surfactant or poloxamer is contained in the oil phase component. 제 10항에 있어서,11. The method of claim 10, 나노에멀젼 총 중량에 대하여 주안정화제인 폴리카프로락톤-폴리에틸렌글리콜(PCL-PEG) 블록공중합체 0.1 내지 10중량%, 보조 계면활성제인 이눌린라우릴카바메이트, 폴록사머 또는 이들의 혼합물 0.01 내지 3중량% 및 실리콘 오일과 하이드로카본계 오일의 혼합물 0.1 내지 60 중량%를 포함하는 것을 특징으로 하는 나노에멀젼의 제조방법. 0.1 to 10% by weight of a polycaprolactone-polyethylene glycol (PCL-PEG) block copolymer as a shampooing agent based on the total weight of the nano emulsion, 0.01 to 3% by weight of an auxiliary surfactant inulin lauryl carbamate, poloxamer, And 0.1 to 60% by weight of a mixture of a silicone oil and a hydrocarbon-based oil. 제 11항에 있어서,12. The method of claim 11, 상기 유상성분에 나노에멀젼 총 중량에 대하여 C12~C22의 지방산 알코올 0.1 내지 10 중량%를 더 함유하는 것을 특징으로 하는 나노에멀젼의 제조방법.Wherein the oil component further contains 0.1 to 10% by weight of C12 to C22 fatty acid alcohol based on the total weight of the nano emulsion.
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