KR20240015891A - Manufacturing method of double matrix capsule - Google Patents
Manufacturing method of double matrix capsule Download PDFInfo
- Publication number
- KR20240015891A KR20240015891A KR1020220093703A KR20220093703A KR20240015891A KR 20240015891 A KR20240015891 A KR 20240015891A KR 1020220093703 A KR1020220093703 A KR 1020220093703A KR 20220093703 A KR20220093703 A KR 20220093703A KR 20240015891 A KR20240015891 A KR 20240015891A
- Authority
- KR
- South Korea
- Prior art keywords
- ingredient
- capsule
- oil
- mixing
- liquid crystal
- Prior art date
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Images
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0295—Liquid crystals
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/06—Emulsions
- A61K8/062—Oil-in-water emulsions
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/11—Encapsulated compositions
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/41—Particular ingredients further characterized by their size
- A61K2800/413—Nanosized, i.e. having sizes below 100 nm
Abstract
본 발명에 따른 2중 매트릭스 캡슐의 제조방법은,
유상성분을 준비하는 유상성분제공단계;
수상성분을 준비하는 수상성분제공단계;
상기 유상성분과 상기 수상성분을 혼합하는 제1혼합단계;
상기 제1혼합단계 후의 혼합물에 유효성분을 혼합하여 제1혼합용액을 제조하는 유효성분제공단계;
상기 제1혼합용액을 100 내지 1000bar의 고압으로 나노믹서에 통과하여 상기 유효성분이 내부에 포집된 다층 라멜라 액정구조의 나노입자를 포함하는 수중유형 액정 에멀젼을 형성하는 1차캡슐화단계;
상기 액정 에멀젼과 고분자가 용해된 수상의 고분자용액을 혼합하여 제2혼합용액을 제조하는 제2혼합단계; 및
상기 제2혼합용액을 노즐에 통과시키고 드롭핑하여 상기 액정구조의 나노입자를 내부에 포함하는 고분자 매트릭스를 가지는 2중 매트릭스캡슐입자를 얻는 2차캡슐화단계; 를 포함하는 것을 특징으로 한다. The method for manufacturing a double matrix capsule according to the present invention is,
Oil ingredient provision step of preparing oil ingredients;
An aqueous ingredient provision step of preparing an aqueous ingredient;
A first mixing step of mixing the oil phase component and the aqueous phase component;
An active ingredient providing step of preparing a first mixed solution by mixing the active ingredient with the mixture after the first mixing step;
A first encapsulation step of passing the first mixed solution through a nanomixer at a high pressure of 100 to 1000 bar to form an oil-in-water liquid crystal emulsion containing nanoparticles with a multilayer lamellar liquid crystal structure with the active ingredient trapped therein;
A second mixing step of preparing a second mixed solution by mixing the liquid crystal emulsion and the aqueous polymer solution in which the polymer is dissolved; and
A secondary encapsulation step of passing the second mixed solution through a nozzle and dropping it to obtain double matrix capsule particles having a polymer matrix containing the liquid crystal structure nanoparticles therein; It is characterized by including.
Description
본 발명은 안정도를 증가하면서 경피흡수를 용이 하게 하는 이중 매트릭스 캡슐의 제조방법에 관한 것이다. The present invention relates to a method for manufacturing a double matrix capsule that facilitates transdermal absorption while increasing stability.
일반적으로, 화장품은 식품과는 다르게 제품을 장기간 사용해야 하는 특성으로 안정성을 확보하는 것이 무엇보다도 중요하다. 최근에는 화장품산업에 있어서, 용기나 내용물 속에 캡슐이나, 비드 등을 함유시켜서 아름다움을 표현하고, 보다 고품질화를 위한 적용 사례가 다수 있다. In general, unlike food, cosmetics require long-term use, so ensuring safety is of the utmost importance. Recently, in the cosmetics industry, there are many application cases to express beauty and improve quality by incorporating capsules or beads into containers or contents.
또한, 화장료에 있어서, 장기간 안정성을 유지하기 어려운 불안정한 유효성분은 단순하게 안정화제를 투입하거나, 다중 에멀젼으로 봉입하는 방법, 특수한 용기를 개발하는 방법, 리포좀 같은 베지클에 단순 캡슐화하여 유효성분을 안정화하는 방법이 적용되고 있다. In addition, in cosmetics, unstable active ingredients that are difficult to maintain long-term stability can be stabilized by simply adding a stabilizer, encapsulating them in multiple emulsions, developing special containers, or simply encapsulating them in vesicles such as liposomes. The method is being applied.
그러나 이러한 방법들은 유효성분을 봉입하는 양이 그다지 많지 않으며, 우수한 안정성을 확보하는 것도 한계가 있다. 최근에는 비드모양의 그래뉼 형태로 만들어 유효성분을 안정화하거나, 색소와 함께 사용하여 외관적으로 차별화되도록 발전시키는 방법도 상품화되고 있다. 또한, 폴리머 형태의 매트릭스를 가지면서 단순한 모노머 형태의 캡슐화방법도 소개되고 있다. However, these methods do not encapsulate a large amount of active ingredients, and there are limitations in ensuring excellent stability. Recently, methods of stabilizing the active ingredients by making them into bead-shaped granules or using them with pigments to differentiate them in appearance have also been commercialized. In addition, a simple monomer-type encapsulation method with a polymer-type matrix has also been introduced.
그러나 이러한 방법들은 단순한 외관적으로만 사용되고 있을 뿐, 고함량의 유효성분을 안정화시키는데 어려움이 따르고, 경시변화에 따라 약물을 피부 속으로 흡수시키는데 한계를 가진다.However, these methods are only used for simple appearance, have difficulty stabilizing high amounts of active ingredients, and have limitations in absorbing drugs into the skin due to changes over time.
상기한 바와 같은 종래 기술의 문제점을 해결하기 위하여, 본 발명은 고함량의 유효성분을 안정화시키고, 경시변화에 따라 약물을 피부 속으로 흡수시킬 수 있는 이중 매트릭스캡슐의 제조방법을 제공한다. In order to solve the problems of the prior art as described above, the present invention provides a method for manufacturing a double matrix capsule that can stabilize a high content of the active ingredient and allow the drug to be absorbed into the skin according to changes over time.
2중 매트릭스캡슐이 형성되는 물질과 최적 조성에 의해 안정한 구상의 캡슐을 제공하여 유효성이 있는 약물을 안정하게 봉입하도록 할 수 있도록 한다.The material from which the double matrix capsule is formed and the optimal composition provide a stable spherical capsule to enable stable encapsulation of an effective drug.
본 발명에 따른 2중 매트릭스 캡슐 제조방법은,The method for manufacturing a double matrix capsule according to the present invention,
유상성분을 준비하는 유상성분제공단계;Oil ingredient provision step of preparing oil ingredients;
수상성분을 준비하는 수상성분제공단계;An aqueous ingredient provision step of preparing an aqueous ingredient;
상기 유상성분과 상기 수상성분을 혼합하는 제1혼합단계;A first mixing step of mixing the oil phase component and the aqueous phase component;
상기 제1혼합단계 후의 혼합물에 유효성분을 혼합하여 제1혼합용액을 제조하는 유효성분제공단계;An active ingredient providing step of preparing a first mixed solution by mixing the active ingredient with the mixture after the first mixing step;
상기 제1혼합용액을 100 내지 1000bar의 고압으로 나노믹서에 통과하여 상기 유효성분이 내부에 포집된 다층 라멜라 액정구조의 나노입자를 포함하는 수중유형 액정 에멀젼을 형성하는 1차캡슐화단계;A first encapsulation step of passing the first mixed solution through a nanomixer at a high pressure of 100 to 1000 bar to form an oil-in-water liquid crystal emulsion containing nanoparticles with a multilayer lamellar liquid crystal structure with the active ingredient trapped therein;
상기 액정 에멀젼과 고분자가 용해된 수상의 고분자용액을 혼합하여 제2혼합용액을 제조하는 제2혼합단계; 및A second mixing step of preparing a second mixed solution by mixing the liquid crystal emulsion and the aqueous polymer solution in which the polymer is dissolved; and
상기 제2혼합용액을 노즐에 통과시키고 드롭핑하여 상기 액정구조의 나노입자를 내부에 포함하는 고분자 매트릭스를 가지는 2중 매트릭스캡슐입자를 얻는 2차캡슐화단계; 를 포함하는 것을 특징으로 한다. A secondary encapsulation step of passing the second mixed solution through a nozzle and dropping it to obtain double matrix capsule particles having a polymer matrix containing the liquid crystal structure nanoparticles therein; It is characterized by including.
이 때, 상기 2중 매트릭스캡슐입자의 크기는 0.1㎛~5mm인 것이 바람직하다. At this time, the size of the double matrix capsule particles is preferably 0.1㎛ ~ 5mm.
또한, 상기 유상성분은 1차캡슐을 형성하기 위한 계면활성제와 다가알코올, 및 오일성분을 포함하는 것이 바람직하다. In addition, the oil phase component preferably includes a surfactant, polyhydric alcohol, and an oil component to form the primary capsule.
또한, 상기 수상성분은 정제수, 점증제, 피부자극완화 성분, 피부보습성분, 보존제성분등이 포함되는 것이 바람직하다. In addition, the water-based ingredients preferably include purified water, a thickener, a skin irritation relieving ingredient, a skin moisturizing ingredient, and a preservative ingredient.
또한, 상기 유효성분은 GHK-Cu, AHK-Cu, 피세틴, 쿼세틴, 이데베논, 비타민류, 라스베라트롤, 카페인, 아데노신, 코디세핀, 니아신아마이드, 및 제니스테인로 구성되는 군에서 선택되는 하나 또는 2이상의 물질일 수 있다. Additionally, the active ingredient is one selected from the group consisting of GHK-Cu, AHK-Cu, fisetin, quercetin, idebenone, vitamins, rasveratrol, caffeine, adenosine, cordycepin, niacinamide, and genistein It may be two or more substances.
또한, 상기 고분자는 피이지-240/에이치디아이코폴리머비스-데실테트라데세스-20에터인 것이 바람직하다. In addition, the polymer is preferably PEG-240/HDI copolymer bis-decyltetradeceth-20 ether.
본 발명에 따른 이중 매트릭스 캡슐을 가지는 화장료 조성물은 유효성분의 장기보존 안정성을 월등히 증가시킬 수 있고, 외관이 미적으로 아름답게 보일 수 있으며, 유효성분, 예컨대 GHK-Cu, AHK-Cu, 피세틴, 쿼세틴, 이데베논, 비타민류, 라스베라트롤, 카페인, 아데노신, 코디세핀, 니아신아마이드, 제니스테인을 수중유적형의 액정 나노입자의 중심부에 안정하게 봉입되도록 하여, 안정화가 장기간 유지되도록 할 수 있다. The cosmetic composition having a double matrix capsule according to the present invention can significantly increase the long-term storage stability of the active ingredients, have an aesthetically pleasing appearance, and contain active ingredients such as GHK-Cu, AHK-Cu, fisetin, and quercetin. , idebenone, vitamins, resveratrol, caffeine, adenosine, cordycepin, niacinamide, and genistein are stably encapsulated in the center of the oil-in-water liquid crystal nanoparticles, so that stabilization can be maintained for a long period of time.
또한 액정 나노입자를 고분자 매트릭스 폴리머로 봉입하여 이중캡슐화하여 안정화할 수 있도록 하고, 이것을 이용하여 효능을 극대화하여, 외관이 미적으로 아름답게 보일 수 있도록 한다.In addition, liquid crystal nanoparticles are encapsulated in a high molecular matrix polymer to double encapsulate and stabilize them, and this is used to maximize efficacy and make the exterior look aesthetically pleasing.
도 1은 본 발명의 일 실시예에 따른 2중 매트릭스 캡슐의 제조방법을 나타낸 순서도이다.
도 2는 본 발명의 일 실시예에 따른 2중 매트릭스 캡슐의 구조도이다.
도 3은 본 발명의 일 실시예에 따른 다층 라멜라 구조의 나노입자에 유효성분이 봉입되는 상태를 보이는 구조도이다.
도 4는 본 발명의 실시예3을 편광현미경으로 관찰한 사진이다.
도 5는 본 발명의 일 실시예에 따른 2중 매트릭스캡슐의 제조된 후 사진이다.
도 6은 본 발명의 일 실시예에 따른 2중매트릭스캡슐화가 가능한 화장료 조성물에 대한 피부보습력 결과를 나타낸 그래프이다.
도 7은 실시예들에 따른 2중 매트릭스 캡슐화된 시료의 경피흡수 모식도이다.
도 8은 본 발명의 일 실시예에 따른 2중 매트릭스캡슐화가 가능한 화장료 조성물에 대한 경피흡수효과를 나타낸 그래프이다.
도 9는 본 발명의 일 실시예에 따른 2중 매트릭스캡슐화가 가능한 화장료 조성물에 대한 안정도 결과를 나타낸 그래프이다.1 is a flowchart showing a method of manufacturing a double matrix capsule according to an embodiment of the present invention.
Figure 2 is a structural diagram of a double matrix capsule according to an embodiment of the present invention.
Figure 3 is a structural diagram showing a state in which an active ingredient is encapsulated in nanoparticles with a multilayer lamellar structure according to an embodiment of the present invention.
Figure 4 is a photograph of Example 3 of the present invention observed with a polarizing microscope.
Figure 5 is a photograph after manufacturing a double matrix capsule according to an embodiment of the present invention.
Figure 6 is a graph showing the results of skin moisturizing power for a cosmetic composition capable of double matrix encapsulation according to an embodiment of the present invention.
Figure 7 is a schematic diagram of transdermal absorption of a double matrix encapsulated sample according to examples.
Figure 8 is a graph showing the transdermal absorption effect of a cosmetic composition capable of double matrix encapsulation according to an embodiment of the present invention.
Figure 9 is a graph showing the stability results for a cosmetic composition capable of double matrix encapsulation according to an embodiment of the present invention.
본 발명은 다양한 변경을 가할 수 있고, 여러 가지 실시예를 가질 수 있는 바, 특정 실시예들을 도면에 예시하고, 상세하게 설명하고자 한다. 그러나, 이는 본 발명을 특정한 실시 형태에 대해 한정하려는 것이 아니고, 본 발명의 기술 사상 및 기술 범위에 포함되는 모든 변경, 균등물 내지 대체물을 포함하는 식으로 이해되어야 하고, 여러 가지 다른 형태로 변형될 수 있으며, 본 발명의 범위가 하기 실시예에 한정되는 것은 아니다. 이하, 첨부된 도면을 참조하여 본 발명에 따른 실시예를 상세히 설명하며, 도면 부호에 관계없이 동일하거나 대응하는 구성요소에 대해서는 동일한 참조 번호를 부여하고, 이에 대해 중복되는 설명을 생략하기로 한다. Since the present invention can be subject to various changes and can have various embodiments, specific embodiments will be illustrated in the drawings and described in detail. However, this is not intended to limit the present invention to specific embodiments, but should be understood to include all changes, equivalents, and substitutes included in the technical idea and scope of the present invention, and may be modified into various other forms. The scope of the present invention is not limited to the following examples. Hereinafter, embodiments according to the present invention will be described in detail with reference to the attached drawings, and identical or corresponding components will be assigned the same reference numerals regardless of the reference numerals, and redundant description thereof will be omitted.
본 발명은 다양한 변경을 가할 수 있고, 여러 가지 실시예를 가질 수 있는 바, 특정 실시예들을 도면에 예시하고, 상세하게 설명하고자 한다. 그러나 이는 본 발명을 특정한 실시 형태에 대해 한정하려는 것이 아니고, 본 발명의 기술사상 및 기술범위에 포함되는 모든 변경, 균등물 내지 대체물을 포함하는 식으로 이해되어야 하고, 여러 가지 다른 형태로 변형될 수 있으며, 본 발명의 범위가 하기 실시예에 한정되는 것은 아니다. 또한, 본 발명에 사용된 주요 외래어에 대한 정의를 다음과 같이 표현하여 이해를 명확히 하고자 한다. Since the present invention can be subject to various changes and can have various embodiments, specific embodiments will be illustrated in the drawings and described in detail. However, this is not intended to limit the present invention to specific embodiments, but should be understood to include all changes, equivalents, and substitutes included in the technical idea and scope of the present invention, and may be modified into various other forms. The scope of the present invention is not limited to the following examples. In addition, the definitions of major foreign words used in the present invention are expressed as follows to clarify understanding.
본 발명의 일측면에 따른 이중 매트릭스 캡슐을 제조하는 방법은, 유상성분제공 단계; 수상성분제공단계; 제1혼합단계; 유효성분제공단계; 1차캡슐화단계; 제2혼합단계; 2차캡슐화단계; 및 세정단계;를 포함한다. 도 1은 본 발명의 실시예에 따른 2중 매트릭스캡슐화 방법을 도시한 순서도이다 A method of manufacturing a double matrix capsule according to one aspect of the present invention includes the step of providing an oily component; Water component provision step; First mixing step; Active ingredient provision step; First encapsulation step; Second mixing step; Secondary encapsulation step; and a cleaning step. 1 is a flowchart showing a double matrix encapsulation method according to an embodiment of the present invention.
유상성분제공단계는 이중매트릭스 캡슐 제조에 사용되는 유상성분을 준비하는 단계이다. 본 실시예에서 유상성분은 1차캡슐을 형성하기 위한 계면활성제와 다가알코올, 오일성분을 포함한다. 유상성분은 75 내지 90℃로 가온용해하여 디스퍼미서로 500~1500rpm으로 10 내지 20 분간 교반하여 잘 분산시킨다. The oily ingredient provision step is a step of preparing the oily ingredient used to manufacture double matrix capsules. In this example, the oil component includes a surfactant, polyhydric alcohol, and oil component to form the primary capsule. The oil phase component is dissolved by heating to 75 to 90°C and stirred with a dispermiser at 500 to 1,500 rpm for 10 to 20 minutes to disperse well.
유상성분은 예를 들면, 수크로오스폴리코튼씨데이트, 폴리글리세릴-10베헤네이트/에이코사디오에이트, 세테아릴알코올, 연꽃꽃왁스이다. Oily ingredients include, for example, sucrose polycotton seed date, polyglyceryl-10 behenate/eicosadioate, cetearyl alcohol, and lotus flower wax.
수상성분제공단계는 수중유 타입의 에멀젼 형성을 위한 수상성분을 준비하는 단계로서, 수상성분은 정제수, 점증제, 피부자극완화 성분, 피부보습성분, 보존제성분등이 포함된다. 수상성분은 800 ~1200rpm으로 교반하면서 75 내지 85 ℃로 5 내지 10분간 가온 용해한다. 수상성분은 예를 들면, 글리세롤, 정제수, 1,2-헥산다이올, 에틸헥실글리세린이다. The aqueous ingredient provision step is a step of preparing aqueous ingredients to form an oil-in-water type emulsion. The aqueous ingredients include purified water, thickeners, skin irritation relieving ingredients, skin moisturizing ingredients, and preservative ingredients. The aqueous component is dissolved by heating at 75 to 85°C for 5 to 10 minutes while stirring at 800 to 1200 rpm. The aqueous phase components are, for example, glycerol, purified water, 1,2-hexanediol, and ethylhexylglycerin.
제1혼합단계는 유상성분과 수상성분을 혼합하는 단계이다. 수상성분에 유상성분을 서서히 투입하여 호모믹서로 혼합할 수 있다. 유상성분과 수상성분은 1 : 7 혹은 1 : 5 비율로 혼합하고, 75 내지 85 ℃에서 2 내지 10분간 호모믹서로 1000~4600rpm으로 교반한다. The first mixing step is a step of mixing the oil phase component and the aqueous phase component. The oil phase components can be gradually added to the water phase components and mixed using a homomixer. The oil phase component and the aqueous phase component are mixed in a ratio of 1:7 or 1:5, and stirred at 1000-4600 rpm with a homomixer at 75-85°C for 2-10 minutes.
유효성분제공단계는 유효성분을 전술한 혼합단계의 유상성분과 수상성분의 혼합물에 유효성분을 혼합하여 제1혼합용액을 제조하는 단계이다. 유효성분 45 내지 60℃까지 냉각하여 유효성분을 투입하여 2,000~4000rpm으로 2 내지 5분간 교반한다. The active ingredient provision step is a step of preparing a first mixed solution by mixing the active ingredient with the mixture of the oil phase component and the aqueous phase component of the mixing step described above. Active ingredient: Cool to 45 to 60°C, add the active ingredient, and stir at 2,000 to 4000 rpm for 2 to 5 minutes.
유효성분은 수용성, 유용성 모두 적용이 가능하며 예를 들어, 이 때 유효성분은 GHK-Cu, AHK-Cu, 피세틴, 쿼세틴, 이데베논, 비타민류, 라스베라트롤, 카페인, 아데노신, 코디세핀, 니아신아마이드, 및 제니스테인로 구성되는 군에서 선택되는 하나 또는 2이상의 물질이 사용될 수 있다. The active ingredients can be both water-soluble and oil-soluble. For example, the active ingredients include GHK-Cu, AHK-Cu, fisetin, quercetin, idebenone, vitamins, rasveratrol, caffeine, adenosine, cordycepin, One or two or more substances selected from the group consisting of niacinamide and genistein may be used.
여기서 GHK-Cu는 구리펩타이드-1이라고도 칭하며, 아미노산인 글라이신-히스티딘-라이신으로 연결된 구조에 구리 이온이 결합되어 착물을 형성하는 화합물을 말하며, AHK-Cu는 구리펩타이드-3라고도 칭하며, 아미노산인 알라닌-히스티딘-라이신으로 연결된 구조에 구리 이온이 결합되어 착물을 형성하는 화합물을 말한다. 이는 통상 탈모방지에 효능을 가진 약물로, 헤어케어 및 스킨케어 화장품에 항노화 성분으로 알려진 활성성분이다.Here, GHK-Cu is also called copper peptide-1, and refers to a compound that forms a complex by combining copper ions with a structure linked to the amino acids glycine-histidine-lysine. AHK-Cu is also called copper peptide-3, and refers to a compound containing the amino acids alanine. -Refers to a compound in which a copper ion is bonded to a structure linked by histidine-lysine to form a complex. This is a drug that is effective in preventing hair loss, and is an active ingredient known as an anti-aging ingredient in hair care and skin care cosmetics.
1차캡슐화단계는 유효성분이 혼합된 제1혼합용액을 100 내지 1000bar의 고압 나노믹서에 통과하여 나노 입자화하는 단계이다. 이 때 생성되는 액정 나노입자는 수중유적형 (O/W타입: Oil-in-Water)으로 라멜라 액정 구조를 가져 유효성분이 내부에 포집되며, 평균입경은 10~500nm 이다. The first encapsulation step is a step in which the first mixed solution containing active ingredients is passed through a high-pressure nanomixer at 100 to 1000 bar to form nanoparticles. The liquid crystal nanoparticles produced at this time are of the oil-in-water type (O/W type: Oil-in-Water) and have a lamellar liquid crystal structure in which the active ingredients are captured inside, and the average particle diameter is 10 to 500 nm.
도 3은 본 발명의 일 실시예에 따른 다층 라멜라 구조의 나노입자에 유효성분이 봉입되는 상태를 보이는 구조도로서, 다층 라멜라 구조내 친수성영역과 친유성영역에 유친수성 유효성분 및 친유성 유효성분이 봉입되는 것을 도시한다. 또한 다층 라멜라 구조의 나노입자는 수중유형 액정 에멀젼을 형성하여 외상이 수상으로 형성되어 있고, 그 안에 수중유형의 입자가 분산된다. Figure 3 is a structural diagram showing a state in which an active ingredient is encapsulated in a nanoparticle with a multilayer lamellar structure according to an embodiment of the present invention, in which an oleophilic active ingredient and a lipophilic active ingredient are encapsulated in the hydrophilic region and the lipophilic region within the multilayer lamellar structure. shows that In addition, nanoparticles with a multi-layered lamellar structure form an oil-in-water liquid crystal emulsion, in which the outer layer is formed as an aqueous phase, and oil-in-water particles are dispersed within it.
생성되는 수중유형(O/W형) 액정 에멀젼은, 예를 들면, 액정 에멀젼의 전체 중량을 기준으로, 0.1~10중량%의 수크로오스폴리코튼씨데이트, 0.5~8중량%의 폴리글리세릴-10베헤네이트/에이코사디오에이트, 0.1~12중량%의 세테아릴알코올, 0.01~3중량%의 연꽃꽃왁스, 0.1~45중량%의 글리세린, 1~70중량%의 정제수를 혼합하여 형성할 수 있다.The resulting oil-in-water (O/W type) liquid crystal emulsion contains, for example, 0.1 to 10% by weight of sucrose polycotton seed date and 0.5 to 8% by weight of polyglyceryl-10, based on the total weight of the liquid crystal emulsion. It can be formed by mixing behenate/eicosadioate, 0.1 to 12% by weight of cetearyl alcohol, 0.01 to 3% by weight of lotus flower wax, 0.1 to 45% by weight of glycerin, and 1 to 70% by weight of purified water. there is.
이 때, 예를 들어, 액정 에멀젼의 전체 중량을 기준으로, 0.001~3중량%의 GHK-Cu, 0.001~1중량%의 AHK-Cu, 3중량%의 피세틴, 2중량%의 쿼세틴, 2중량%의 이데베논, 0.001~5중량%의 비타민류(레티놀, 아스코르빅애씨드, 토코페롤), 1중량%의 라스베라트롤, 1중량%의 카페인, 1중량%의 아데노신, 1중량%의 코디세핀, 3중량%의 니아신아마이드, 2중량%의 제니스테인 중에서 어느 하나 또는 다수가 유효성분으로 상기 1중 O/W 액정 에멀젼에 봉입될 수 있다. At this time, for example, based on the total weight of the liquid crystal emulsion, 0.001 to 3% by weight of GHK-Cu, 0.001 to 1% by weight of AHK-Cu, 3% by weight of fisetin, 2% by weight of quercetin, 2% by weight. % by weight idebenone, 0.001~5% by weight vitamins (retinol, ascorbic acid, tocopherol), 1% by weight resveratrol, 1% by weight caffeine, 1% by weight adenosine, 1% by weight coordination. Any one or more of sepin, 3% by weight of niacinamide, and 2% by weight of genistein may be encapsulated in the single O/W liquid crystal emulsion as an active ingredient.
제2혼합단계는 전술한 단계에서 제조된 액정 에멀젼과 고분자가 용해된 수상의 고분자용액을 혼합하는 단계이다. 수상겔화가 이루어지는 고분자를 계량하여 정제수에 넣고 50~60℃로 가온하여 디스퍼믹서로 1,000~2,000rpm으로 7~12분간 교반하여 잘 분산시켜 고분자 용액을 만들고, 다음으로 이것을 60℃내지 40℃로 냉각하고, 액정 에멀젼에 첨가하여 pH는 4.5~7.5에서, 호모믹서로 1,000~2,000rpm으로 교반하여 안정하게 분산시켜 제2혼합용액을 제조한다. The second mixing step is a step of mixing the liquid crystal emulsion prepared in the above-described step with the aqueous polymer solution in which the polymer is dissolved. Weigh the polymer in which aqueous gelation occurs, add it to purified water, heat to 50-60℃, stir with a disper mixer at 1,000-2,000 rpm for 7-12 minutes to disperse well, and then heat it to 60℃-40℃. Cool, add to the liquid crystal emulsion, stir at pH 4.5 to 7.5, and stir at 1,000 to 2,000 rpm with a homomixer to prepare a second mixed solution by stably dispersing it.
이 때 사용되는 고분자는 수상겔화가 이루어지는 고분자로는, 예를 들어, 피이지-240/에이치디아이코폴리머비스-데실테트라데세스-20에터를 사용할 수 있다. 고분자는 2차캡슐화 에멀젼 용액의 0.05 내지 1중량%로 포함되는 것이 바람직하다. The polymer used at this time is a polymer that undergoes water gelation, for example, PEG-240/HDI copolymer bis-decyltetradeceth-20 ether can be used. The polymer is preferably included in 0.05 to 1% by weight of the secondary encapsulation emulsion solution.
또한 제2혼합용액은 계면활성제를 포함한다. 계면활성제로는 제한이 없으나, 폴리글리세릴-10스테아레이트(Polygleceryl-10 Stearate) 와 폴리글리세릴-10 올리에이트 (Polygleceryl-10 Oleate)를 혼합하여 사용하는 것이 바람직하다. 계면활성제는 2차캡슐화 에멀젼 용액의 0.1 내지 7중량%, 바람직하게는 0.5 내지 5 중량%로 포함되는 것이 바람직하다. Additionally, the second mixed solution contains a surfactant. There are no restrictions on the surfactant, but it is preferable to use a mixture of Polyglyceryl-10 Stearate and Polygleceryl-10 Oleate. The surfactant is preferably included in 0.1 to 7% by weight of the secondary encapsulation emulsion solution, preferably 0.5 to 5% by weight.
그 외에 제2혼합용액은, 향료, 글리세린, 부틸렌글라이콜, 피이지-240/에이치디아이코폴리머비스-데실테트라데세스-20에터, 하이드로라이즈드콜라겐이나 아가 등을 더 포함할 수 있고, 콜라겐은 하이드롤라이즈드콜라겐 등이 사용될 수 있고, 정제수는 30중량% 내지 80중량%로 포함된다. In addition, the second mixed solution may further include fragrance, glycerin, butylene glycol, PEG-240/HDI copolymer bis-decyltetradeceth-20 ether, hydrolyzed collagen, agar, etc. Collagen such as hydrolyzed collagen can be used, and purified water is included at 30% to 80% by weight.
보다 상세하게는 0.05~0.3중량%의 피이지-240/에이치디아이코폴리머비스-데실테트라데세스-20에터, 0.05~0.2중량%의 하이드로라이즈드콜라겐, 혹은 0.1~3중량%의 아가를 단일 혹은 2종 이상의 혼합된 성분으로 이루어져 최종 물질이 그래뉼처럼 구상의 매트릭스 캡슐을 형성하는 것을 특징으로 하는 조성물이 여기에 해당된다.More specifically, 0.05 to 0.3% by weight of PEG-240/HDI copolymer bis-decyltetradeceth-20 ether, 0.05 to 0.2% by weight of hydrolyzed collagen, or 0.1 to 3% by weight of agar as a single Alternatively, this includes compositions that are composed of two or more mixed ingredients, and the final material forms a spherical matrix capsule like granules.
제2캡슐화단계는 제2혼합용액을 노즐에 통과시키고 드롭핑하여 그래뉼 타입의 2중 매트릭스캡슐입자를 얻는 단계이다. 또한 2중 매트릭스 캡슐 입자에 천연색소를 배합하여 외관이 다양한 색상을 가지도록 할 수 있다. The second encapsulation step is to obtain granule-type double matrix capsule particles by passing the second mixed solution through a nozzle and dropping it. In addition, natural pigments can be mixed into the double matrix capsule particles to give them a variety of colors.
제2혼합용액을 내경이 0.1~15mm의 노즐에 통과시키고, 노즐을 통과한 용액이 오일층을 통하여 하층으로 드롭핑시키면 혼합용액이 굳어지면서 2중 매트릭스캡슐입자가 형성된다. When the second mixed solution is passed through a nozzle with an inner diameter of 0.1 to 15 mm, and the solution that has passed through the nozzle is dropped to the lower layer through the oil layer, the mixed solution hardens and double matrix capsule particles are formed.
이 때, 노즐의 크기에 따라 다양한 크기의 입자로 만들 수 있다. 오일층을 통과할 경우 묻어 있는 오일을 세정하는 공정이 포함될 수 있다. At this time, particles of various sizes can be made depending on the size of the nozzle. When passing through the oil layer, a process of cleaning the remaining oil may be included.
즉, 제2캡슐화단계에서 1차 캡슐된 액정나노입자는 고분자 매트릭스로 2차캡슐화되어, 2중 매트릭스캡슐구조를 이룬다. 도 2는 1중 액정에멀젼이 고분자 매트릭스 안에 봉입되어 2차캡슐화단계 후의 2중 매트릭스캡슐입자를 도시한다. 이 때 2중 매트릭스캡슐입자의 크기는 0.1um~5mm의 그래뉼 형태이다. That is, in the second encapsulation step, the first encapsulated liquid crystal nanoparticles are secondarily encapsulated with a polymer matrix, forming a double matrix capsule structure. Figure 2 shows double-matrix capsule particles after a secondary encapsulation step in which a single-layer liquid crystal emulsion is encapsulated in a polymer matrix. At this time, the size of the double matrix capsule particles is in the form of granules of 0.1um to 5mm.
2중 매트릭스 캡슐은 내부의 1중 캡슐을 안정하게 보존하는 기능을 하며, 피부에 도포할 경우 부드럽게 펴발라지면서 빠르게 흡수되는 장점을 가진다. The double-layer matrix capsule has the function of stably preserving the single-layer capsule inside, and has the advantage of being absorbed quickly while spreading smoothly when applied to the skin.
따라서 2중 매트릭스 캡슐은 손으로 문지르거나, 펌프를 통과하여 토출될 경우 부드럽게 깨짐으로써 피부에 흡수될 수 있다. 내경이 0.1~15mm의 노즐 그리고 노즐을 통과한 내용물이 오일층을 통하여 하층으로 침강하면서 굳어지는 것을 특징으로 하는 것일 수 있다. Therefore, the double matrix capsule can be absorbed into the skin by rubbing it by hand or by gently breaking it when discharged through a pump. It may be characterized by a nozzle with an inner diameter of 0.1 to 15 mm and the content passing through the nozzle sinking to the lower layer through the oil layer and hardening.
제2캡슐화단계에서 2중 매트릭스캡슐입자의 드롭핑시에 오일층을 통과할 경우 묻어 있는 오일을 세정하는 세정단계가 더 포함될 수 있다.In the second encapsulation step, when the double matrix capsule particles pass through the oil layer during dropping, a cleaning step of cleaning the remaining oil may be further included.
이렇게 하여 얻어진 생성물은 장기간 안정성이 우수하고 경피흡수를 보다 효과적으로 할 수 있으며, 확대 응용으로써 기초화장품, 색조화장품 및 헤어케어 제품에 응용하여 외관적으로는 아름답고 다양한 색상으로 만들어 고급감을 부여하고, 사용감 측면으로도 부드러우며, 촉촉한 느낌을 가질 수 있도록 다양한 제형으로 만들 수 있도록 하는 것일 수 있다.The product obtained in this way has excellent long-term stability and can be absorbed more effectively through the skin. As an expanded application, it can be applied to basic cosmetics, color cosmetics, and hair care products, making it beautiful in appearance and in various colors to give a sense of luxury and a feeling of use. It may be possible to make it into various formulations so that it can have a soft and moist feeling.
<실시예 ><Example>
<실시예 1> 1중 O/W 나노 액정 에멀젼의 제조<Example 1> Preparation of single O/W nano liquid crystal emulsion
유상성분을 계량하여 가온 용해하여 디스퍼믹서로 10분이상 교반하면서(500~1500rpm) 잘 분산시킨다. 다음으로 수상부를 계량하여 가온용해하여 교반(800~1200rpm) 하면서 분산시킨다. 다음으로 수상성분에 유상성분을 서서히 투입하여 호모믹서로 1000~4000rpm으로 5분간 교반한다. 다음으로 50℃까지 냉각하여 유효성분을 투입하여 2,000~4000rpm으로 3분간 교반한다. 다음으로 고압 나노셀에 통과하여 나노 액정입자를 만든다. 최종적으로 진공 탈포를 한 다음 제조를 완료하였다. 사용된 각 성분의 함량은 표 1에 정리되었다. Weigh the oil phase ingredients, dissolve them by heating, and disperse them well while stirring (500-1500 rpm) for more than 10 minutes using a disper mixer. Next, the aqueous phase is weighed, dissolved by heating, and dispersed while stirring (800-1200 rpm). Next, slowly add the oil phase ingredients to the water phase components and stir with a homomixer at 1000-4000 rpm for 5 minutes. Next, cool to 50°C, add the active ingredient, and stir at 2,000-4000 rpm for 3 minutes. Next, it passes through a high-pressure nanocell to create nano liquid crystal particles. Finally, vacuum degassing was performed and manufacturing was completed. The content of each ingredient used is summarized in Table 1.
<실시예 2 내지 10><Examples 2 to 10>
표 1 및 표 2의 함량의 차이를 제외하고는 동일하게 실시예 1과 같이 제조하였다. 실시예 6 내지 실시예 10은 유효성분을 1종의 물질만을 포함시켰다. It was prepared in the same manner as in Example 1, except for the difference in content in Tables 1 and 2. Examples 6 to 10 included only one type of active ingredient.
폴리글리세릴-10베헤네이트/에이코사디오에이트
세테아릴알코올
연꽃꽃왁스Sucrose Poly Cotton Sea Date
Polyglyceryl-10behenate/eicosadioate
Cetearyl alcohol
lotus flower wax
2
5
3One
2
5
3
1.5
5
32
1.5
5
3
1
5
33
One
5
3
0.5
5
34
0.5
5
3
0.1
5
35
0.1
5
3
정제수
1,2-헥산다이올
에틸헥실글리세린glycerol
Purified water
1,2-hexanediol
Ethylhexylglycerin
33.81
2
0.140
33.81
2
0.1
43.90
2
0.130
43.90
2
0.1
51.90
2
0.120
51.90
2
0.1
53.90
2
0.110
53.90
2
0.1
41.77
2
0.15
41.77
2
0.1
AHK-Cu
피세틴
쿼세틴
이데베논
비타민류
라스베라트롤
카페인
아데노신
코디세핀
니아신아마이드
제니스테인GHK-Cu
AHK-Cu
fisetin
quercetin
Idebenone
Vitamins
rasveratrol
Caffeine
Adenosine
Cordycepin
Niacinamide
genistein
0.01
5
5
3
0.01
0.01
0.01
0.01
0.01
0.01
0.010.01
0.01
5
5
3
0.01
0.01
0.01
0.01
0.01
0.01
0.01
0.5
3
3
2
0.5
0.5
0.5
0.5
0.5
0.5
0.50.5
0.5
3
3
2
0.5
0.5
0.5
0.5
0.5
0.5
0.5
1
2
2
1
1
1
1
1
1
1
1One
One
2
2
One
One
One
One
One
One
One
One
5
1
1
1
2
1
1
0.5
1
2
15
5
One
One
One
2
One
One
0.5
One
2
One
10
0.01
0.01
0.01
3
2
2
1
2
5
310
10
0.01
0.01
0.01
3
2
2
One
2
5
3
폴리글리세릴-10베헤네이트/에이코사디오에이트
세테아릴알코올
연꽃꽃왁스
카프릴릭/카프릭트리글리세라이드Sucrose Poly Cotton Sea Date
Polyglyceryl-10behenate/eicosadioate
Cetearyl alcohol
lotus flower wax
Caprylic/Capric Triglyceride
2
5
3
53
2
5
3
5
2
5
3
53
2
5
3
5
2
5
3
53
2
5
3
5
2
5
3
53
2
5
3
5
2
5
3
53
2
5
3
5
정제수
1,2-헥산다이올
에틸헥실글리세린glycerol
Purified water
1,2-hexanediol
Ethylhexylglycerin
48.9
2
0.130
48.9
2
0.1
48.9
2
0.130
48.9
2
0.1
48.9
2
0.130
48.9
2
0.1
48.9
2
0.130
48.9
2
0.1
48.9
2
0.130
48.9
2
0.1
AHK-Cu
피세틴
쿼세틴
이데베논GHK-Cu
AHK-Cu
fisetin
quercetin
Idebenone
-
-
-
-One
-
-
-
-
1
-
-
--
One
-
-
-
-
1
-
--
-
One
-
-
-
-
1
--
-
-
One
-
-
-
-
1-
-
-
-
One
<실시예 11 내지 15><Examples 11 to 15>
먼저 표 3에서와 같은 조성으로 Solubil ORG-1300에 향료, 글리세린, 부틸렌글라이콜, 피이지-240/에이치디아이코폴리머비스-데실테트라데세스-20에터, 하이드롤라이즈드콜라겐, 아가를 정제수에 잘 용해하여 고분자용액을 만들었다. 제조된 고분자 용액에 표 1의 실시예 3을 혼합하여 잘 교반함으로써 이중 매트릭스 캡슐화를 진행하였다. First, with the composition as shown in Table 3, fragrance, glycerin, butylene glycol, PEG-240/HDI copolymer bis-decyltetradeceth-20 ether, hydrolyzed collagen, and agar were added to Solubil ORG-1300 with purified water. It was dissolved well to create a polymer solution. Double matrix encapsulation was performed by mixing Example 3 in Table 1 with the prepared polymer solution and stirring well.
향료
글리세린
부틸렌글라이콜
피이지-240/에이치디아이코폴리머비스-데실테트라데세스-20에터
하이드롤라이즈드콜라겐
아가
정제수Solubil ORG-1300
Spices
glycerin
Butylene glycol
PEG-240/HDI copolymer bis-decyltetradeceth-20 ether
Hydrolyzed Collagen
baby
Purified water
0.1
3
8
0.1
0.2
0.2
67.90.5
0.1
3
8
0.1
0.2
0.2
67.9
0.1
2
8
0.1
0.2
0.5
58.1One
0.1
2
8
0.1
0.2
0.5
58.1
0.1
3
8
0.1
0.2
0.8
46.31.5
0.1
3
8
0.1
0.2
0.8
46.3
0.1
4
8
0.1
0.2
1
33.63
0.1
4
8
0.1
0.2
One
33.6
0.1
5
8
0.1
0.2
3
78.65
0.1
5
8
0.1
0.2
3
78.6
캡슐underwater type
capsule
캡슐underwater type
capsule
캡슐underwater type
capsule
캡슐underwater type
capsule
캡슐underwater type
capsule
한편 도 5는 전술한 실시예 들을 1mm와 3mm 크기로 그래뉼 타입의 캡슐로 제조한 사진이다. 이와 같이 2중 캡슐화된 알갱이 형태로 존재하며 본 발명에서 이루고자 한 최종 완성물이다. 이것은 스킨, 로션, 에센스, 크림, 파운데이션, 썬블록크림 등 다양한 제형에 적용이 가능하고, 헤어제품의 샴푸, 린스, 엠플, 염모제 등에도 적용이 가능하다. Meanwhile, Figure 5 is a photograph of the above-described examples manufactured as granule-type capsules in sizes of 1 mm and 3 mm. As such, it exists in the form of double-encapsulated granules and is the final product sought to be achieved in the present invention. This can be applied to various formulations such as skin, lotion, essence, cream, foundation, and sunblock cream, and can also be applied to hair products such as shampoo, rinse, ampoule, and hair dye.
<처방예 ><Prescription example>
<처방예 1~3>에센스<Prescription Examples 1-3> Essence
수상을 계량하여 50~60℃로 가온하여 용해한다. 이것을 40℃ 이하로 냉각하고, 여기에 첨가1을 혼합 교반한다. 여기에 중화제를 넣고 혼합한다. 여기에 첨가 2를 넣어 혼합한다.Weigh the water phase and dissolve it by heating to 50~60℃. This is cooled to 40°C or lower, and Addition 1 is mixed and stirred. Add neutralizer here and mix. Add Addition 2 here and mix.
글리세린
부틸렌글라이콜
다이프로필렌글라이콜
EDTA-2Na
알란토인
카보머-941 (2%용액)
정제수Solubil ORG-1300
glycerin
Butylene glycol
Dipropylene glycol
EDTA-2Na
allantoin
Carbomer-941 (2% solution)
Purified water
5
5
3
0.02
0.1
10
75.08One
5
5
3
0.02
0.1
10
75.08
5
5
3
0.02
0.1
10
75.08One
5
5
3
0.02
0.1
10
75.08
5
5
3
0.02
0.1
10
65.08One
5
5
3
0.02
0.1
10
65.08
병풀추출물Purslane extract
Centella asiatica extract
-5
-
5-
5
55
5
정제수Arginine 10% solution
Purified water
2One
2
2One
2
2One
2
실시예 18Example 12
Example 18
0.30.2
0.3
0.30.2
0.3
0.30.2
0.3
<처방예 1~3>크림<Prescription Examples 1-3> Cream
수상을 계량하여 80~90℃로 가온하여 용해한다. 유상을 계량 80~90℃로 가온하여 용해한다. 이것을 혼합하여 호모믹서로 교반한다. 중화제를 넣고 교반한다. 30℃까지 냉각 하7여 첨가제를 넣는다. 탈기하여 제조를 완료한다.Weigh the water phase and dissolve it by heating to 80~90℃. Dissolve the oil phase by heating it to 80~90℃. This is mixed and stirred with a homomixer. Add neutralizer and stir. Cool to 30℃ and add additives. Manufacturing is completed by degassing.
글리세린
부틸렌글라이콜
다이프로필렌글라이콜
EDTA-2Na
알란토인
카보머-940 (2%용액)
정제수Solubil ORG-1300
glycerin
Butylene glycol
Dipropylene glycol
EDTA-2Na
allantoin
Carbomer-940 (2% solution)
Purified water
5
5
3
0.02
0.1
20
to 100One
5
5
3
0.02
0.1
20
to 100
5
5
3
0.02
0.1
10
to 100One
5
5
3
0.02
0.1
10
to 100
5
5
3
0.02
0.1
10
to 100One
5
5
3
0.02
0.1
10
to 100
쉐어버터
마이크로크리스탈라인왁스
Solubil ORG-1300
글리세릴모노스테아레이트
세틸에틸헥사노에이트
식물성스쿠알란
트레에틸헥사노인Cetearyl alcohol
shea butter
Micro Crystal Line Wax
Solubil ORG-1300
Glyceryl Monostearate
Cetyl Ethyl Hexanoate
Vegetable squalane
Treethylhexanoin
2
1
5
1
3
5
33
2
One
5
One
3
5
3
2
1
5
1
3
5
33
2
One
5
One
3
5
3
2
1
5
1
3
5
33
2
One
5
One
3
5
3
정제수Arginine 10% solution
Purified water
22
2
22
2
22
2
실시예 13Example 12
Example 13
-10
-
10-
10
55
5
<처방예: 샴푸><Prescription example: Shampoo>
폴리퉈터늄-10Purified water
Polytuternium-10
0.2550.3
0.25
0.2550.3
0.25
0.2550.3
0.25
구아하이드록시프로필트리모늄클로라이드
다이소듐이디티에이
베타인
판테놀glycerin
Guahydroxypropyltrimonium chloride
Disodium EDTA
Betaine
panthenol
0.25
0.05
0.25
0.22
0.25
0.05
0.25
0.2
0.25
0.05
0.25
0.22
0.25
0.05
0.25
0.2
0.25
0.05
0.25
0.22
0.25
0.05
0.25
0.2
코코-베타인
코카마이드미파
프로필렌글라이콜라우레이트 Sodium C14-16 Olefin Sulfonate
Coco-Betaine
cocamide mifa
propylene glycol laurate
20
0.25
0.5522
20
0.25
0.55
20
0.25
0.5522
20
0.25
0.55
20
0.25
0.5522
20
0.25
0.55
0.30.9
0.3
0.30.9
0.3
0.30.9
0.3
실시예 17Example 16
Example 17
0One
0
10
One
0.50.5
0.5
<처방예: 린스><Prescription example: rinse>
다이소듐이디티에이
프로필렌글라이콜
판테놀
베타인
세트리모늄클로라이드Purified water
Disodium EDTA
propylene glycol
panthenol
Betaine
Cetrimonium chloride
0.05
2
0.2
1
370.95
0.05
2
0.2
One
3
0.05
2
0.2
1
370.95
0.05
2
0.2
One
3
0.05
2
0.2
1
370.95
0.05
2
0.2
One
3
세틸알코올
사이클로펜타실록세인
스테아트라이모늄클로라이드
베헨트라이모늄클로라이드Stearamidopropyldimethylamine
cetyl alcohol
Cyclopentasiloxane
steartrimonium chloride
behentrimonium chloride
6.5
2.5
2
11.5
6.5
2.5
2
One
6.5
2.5
2
11.5
6.5
2.5
2
One
6.5
2.5
2
11.5
6.5
2.5
2
One
하이드롤라이즈드콜라겐Amodimethicone
Hydrolyzed Collagen
2.74
2.7
2.74
2.7
2.74
2.7
카프릴릴글라이콜1,2-hexanediol
caprylyl glycol
0.30.5
0.3
0.30.5
0.3
0.30.5
0.3
실시예 13Example 12
Example 13
0One
0
10
One
0.50.5
0.5
<처방예: 탈모예방 엠플><Prescription example: Hair loss prevention ampoule>
피이지-75라놀린
알란토인
부틸렌글라이콜
판테놀
사이클로덱스트린
소듐구아이아줄렌설포네이트&치자추출물
알지닌Purified water
PEG-75 Lanolin
allantoin
Butylene glycol
panthenol
Cyclodextrin
Sodium guaiazulenesulfonate & Gardenia extract
arginine
0.3
0.1
2
0.2
0.2
0.05
0.3182.24
0.3
0.1
2
0.2
0.2
0.05
0.31
0.3
0.1
2
0.2
0.2
0.05
0.3182.24
0.3
0.1
2
0.2
0.2
0.05
0.31
0.3
0.1
2
0.2
0.2
0.05
0.3182.24
0.3
0.1
2
0.2
0.2
0.05
0.31
멘톨
살리실릭애씨드
트라이에틸시트레이트ethanol
menthol
Salicylic Acid
Triethyl citrate
0.3
0.25
15
0.3
0.25
One
0.3
0.25
15
0.3
0.25
One
0.3
0.25
15
0.3
0.25
One
피이지-60하이드로제네이티드캐스터오일
부틸렌글라이콜
향료ethanol
PEG-60 Hydrogenated Castor Oil
Butylene glycol
Spices
0.3
0.25
15
0.3
0.25
One
0.3
0.25
15
0.3
0.25
One
0.3
0.25
15
0.3
0.25
One
실시예 13Example 12
Example 13
0One
0
10
One
0.50.5
0.5
<실험예><Experimental example>
<실험예 1> 수중유형의 입자구조분석<Experimental Example 1> Particle structure analysis of underwater type
도 4는 실시예 3을 가지고 편광현미경으로 입자를 관찰한 결과이다. 편광현미경으로 1,000배율 관찰이 가능한 대물렌즈를 장착시켜 입경의 모양을 관찰하였다. 도 4에 따르면 흰색의 동그란 입자 안에 십자로 모양의 구조가 형성되는 것을 알 수 있고 이것은 다중 라멜라형 구조를 형성한다는 것을 의미한다. 이 안에 다양한 약물을 봉입하여 안정도를 높일 수 있는 방법으로 사용될 수 있다.Figure 4 shows the results of observing particles using a polarizing microscope in Example 3. The shape of the particle size was observed using a polarizing microscope with an objective lens capable of observing at 1,000x magnification. According to Figure 4, it can be seen that a cross-shaped structure is formed within the white round particles, which means that a multi-lamellar structure is formed. It can be used as a way to increase stability by encapsulating various drugs within it.
<실험예 2> 이중 고분자 매트릭스 캡슐의 장기안정성 평가<Experimental Example 2> Long-term stability evaluation of double polymer matrix capsules
표 5는 이중 고분자 매트릭스캡슐 안에 피세틴 2%를 캡슐화하여 장기안정성을 측정한 결과를 나타낸 그래프이다. 3개의 시료 모두 각각 피세틴 2%를 함유하는 시료로 동일한 조건에서의 안정성을 관찰하였다. 수중유형의 2중 캡슐화 피센틴 2%함유한 실시예 18, 비캡슐한 피세틴 2%의 비교예 1, 1중액정에멀젼화 시료 비교예 2를 45℃ 인큐베이터에서 30일 경과한 후, HPLC로 정량 분석한 결과이다.Table 5 is a graph showing the results of measuring long-term stability by encapsulating 2% of fisetin in a double polymer matrix capsule. The stability of all three samples, each containing 2% fisetin, was observed under the same conditions. Example 18 containing 2% of oil-in-water double encapsulated ficentin, Comparative Example 1 of non-encapsulated ficentin 2%, and Comparative Example 2 of single-layer liquid crystal emulsification sample were analyzed by HPLC after 30 days in an incubator at 45°C. This is the result of quantitative analysis.
(비캡슐)underwater type
(non-capsule)
(1중캡슐)underwater type
(single capsule)
피세틴2%1 layer liquid crystal capsule
Fisetin 2%
피세틴2% Double matrix capsule
Fisetin 2%
비교예 1, 비교예 2, 실시예 18의 경우 제조 즉시에는 2%로 동일한 함량을 보이고 있었다. 비교예 1, 비교예 2의 경우 4주 후의 안정성은 급격히 하락하여 피세틴의 잔존량이 34%와 56%로 나타났다. 반면, 본 발명의 실시예 18의 경우 제조 즉시에는 2%, 4주후의 피세틴의 함량은 1.95%로 97.5%의 잔존량을 보였다. 이 결과로 보아, 비캡슐과 1중캡슐화한 조성물보다 2중 매트릭스 캡슐화한 것에서 월등히 우수한 안정성을 보였다.In the case of Comparative Example 1, Comparative Example 2, and Example 18, the content was the same at 2% immediately after manufacturing. In the case of Comparative Examples 1 and 2, the stability after 4 weeks decreased rapidly, with the remaining amounts of fisetin reaching 34% and 56%. On the other hand, in the case of Example 18 of the present invention, the fisetin content was 2% immediately after manufacture and 1.95% after 4 weeks, showing a residual amount of 97.5%. Based on these results, the double matrix encapsulated composition showed significantly better stability than the non-encapsulated and single encapsulated composition.
<실험예 3> 일반 O/W유화 평가<Experimental Example 3> General O/W oil painting evaluation
일반유화와 2중 캡슐의 성능적 차이점을 실험하여 더욱 설득력 있는 성능적 차별점을 설명하기 위하여 비교예 3~7을 제시하였다. 이에 유상부를 계량하여 가온 용해하여 디스퍼믹서로 500~1500rpm으로 10분간 교반하여 잘 분산시키고, 수상부를 가온용해 하고, 수상에 유상을 서서히 투입하여 호모믹서로 4000rpm으로 5분간 교반한 후, 중화제를 투입하여 호모믹서로 4000rpm으로 5분간 교반한다. 이후 50℃까지 냉각하여 유효성분을 투입하여 4000rpm으로 2분간 교반하고, 30℃까지 냉각하여 진공 탈포를 한 다음 비교예 3 내지 7의 제조를 완료하였다.Comparative Examples 3 to 7 were presented to demonstrate the performance differences more convincingly by testing the performance differences between general emulsions and double capsules. Accordingly, the oil phase was weighed, heated and dissolved, and stirred with a disper mixer at 500-1,500 rpm for 10 minutes to disperse well. The aqueous phase was heated and dissolved. The oil phase was slowly added to the aqueous phase, stirred with a homomixer at 4,000 rpm for 5 minutes, and then a neutralizer was added. Add and stir with a homomixer at 4000 rpm for 5 minutes. Afterwards, the mixture was cooled to 50°C, the active ingredient was added, stirred at 4000 rpm for 2 minutes, cooled to 30°C, vacuum degassed, and the preparation of Comparative Examples 3 to 7 was completed.
여기에서는 가장 일번적으로 사용중인 폴리솔베이트-60과 PEG-60하이드로제네이티드캐스터오일을 적용하였다. 비교예4의 외관은 점도가 높은 크림이었으며, pH=5.8, 비중은 0.998이었다. 유화입자는 평균 8.9㎛이었다.Here, the most commonly used polysorbate-60 and PEG-60 hydrogenated castor oils were applied. The appearance of Comparative Example 4 was a cream with high viscosity, pH = 5.8, and specific gravity was 0.998. The average emulsion particle size was 8.9㎛.
하이드로제네이티드폴리데센
세테아릴알코올
마이크로크리스탈라인왁스
폴리솔베이트-60
PEG-60하이드로제네이티드캐스터오일Caprylic/Capric Triglyceride
Hydrogenated polydecene
Cetearyl alcohol
Micro Crystal Line Wax
Polysorbate-60
PEG-60 Hydrogenated Castor Oil
5
3
2
3
25
5
3
2
3
2
5
3
2
3
25
5
3
2
3
2
5
3
2
3
25
5
3
2
3
2
5
3
2
3
25
5
3
2
3
2
5
3
2
3
25
5
3
2
3
2
다이프로필렌글라이콜
1,2-헥산다이올
에틸헥실글리세린
카보머-940 (2%용액)
정제수 glycerol
Dipropylene glycol
1,2-hexanediol
Ethylhexylglycerin
Carbomer-940 (2% solution)
Purified water
3
2
0.1
15
45.47
3
2
0.1
15
45.4
3
2
0.1
15
45.47
3
2
0.1
15
45.4
3
2
0.1
15
45.47
3
2
0.1
15
45.4
3
2
0.1
15
45.47
3
2
0.1
15
45.4
3
2
0.1
15
45.47
3
2
0.1
15
45.4
정제수Arginine 10% solution
Purified water
51.5
5
51.5
5
51.5
5
51.5
5
51.5
5
AHK-Cu
피세틴
쿼세틴
코디세핀GHK-Cu
AHK-Cu
fisetin
quercetin
Cordycepin
-
-
-
-One
-
-
-
-
1
-
-
--
One
-
-
-
-
1
-
--
-
One
-
-
-
-
1
--
-
-
One
-
-
-
-
1-
-
-
-
One
<실험예 4> 보습력평가<Experimental Example 4> Moisturizing power evaluation
도 6은 피부보습력평가를 나타낸 그래프이다. 보습력평가는 20~50대의 남녀 20명을 대상으로 하여 보습력 측정기로 측정한 결과이다. 비교예 4와 실시예17을 가지고 보습력의 차이를 측정하였다. 도포 즉시에는 두 시료 모두 58%대로 급격히 증가하는 것을 알 수 있었다. 비교예4의 경우 시간이 경과하면서 보습력은 급격히 감소하여 도포전과 비슷한 수준으로 낮아짐을 알 수 있었다. 그러나 실시예17의 경우 4시간 경과 후에는 25,8%, 6시간경과 후에는 21.6%, 8시간 경과 후에는 15.8%로 도포전보다는 5배정도 우수한 효과를 보였다. Figure 6 is a graph showing skin moisturizing power evaluation. The moisturizing power evaluation is the result of measuring 20 men and women in their 20s to 50s using a moisturizing power meter. The difference in moisturizing power was measured between Comparative Example 4 and Example 17. Immediately after application, both samples were found to rapidly increase to 58%. In the case of Comparative Example 4, it was found that the moisturizing power decreased rapidly over time, lowering to a level similar to that before application. However, in Example 17, the effect was 25.8% after 4 hours, 21.6% after 6 hours, and 15.8% after 8 hours, which was about 5 times better than before application.
<실험예 5> 경피흡수평가<Experimental Example 5> Transdermal absorption evaluation
도 7은 실시예들에 따른 2중 매트릭스 캡슐화된 시료의 경피흡수 모식도이다. 이에 다르면, 실시예들은 경피흡수를 용이하게 하기 때문에 화장품 피부학적으로 많은 강점이 있다. 유효성분을 장기간동안 안정성을 확보할 수 있고, 외관적으로 아름답게 표현할 수 있으며, 피부 흡수가 빠르게 할 수 있어 적은 량으로도 효능을 낼 수 있는 것이 장점인 예이다. Figure 7 is a schematic diagram of transdermal absorption of a double matrix encapsulated sample according to examples. According to this, the embodiments have many advantages in cosmetic dermatology because they facilitate transdermal absorption. An example of an advantage is that the stability of the active ingredient can be secured for a long period of time, the appearance can be expressed beautifully, and the skin can be absorbed quickly, so even a small amount can be effective.
도 8은 실시예를 통하여 경피흡수력 실험을 나타낸 그래프이다. 경피흡수력 평가는 프렌츠셀을 이용하여 인조 피부를 장착시킨 후 그 위에 시료를 도포하고 10시간까지 경과에 따라 샘플링하여 HPLC정량 분석을 통하여 경피흡수가 어느 정도 가능한가를 측정한 결과를 나타내었다. 측정지표의 약물은 AHK-Cu를 정량분석하여 백분율로 나타내었다. 비교예4의 경우 1시간경과 후에는 0.05%, 10시간경과 후에는 1.28%의 흡수력을 보여주고 있다. 반면에 실시예 17은 1시간경과 후에는 1.96%, 10시간경과 후에는 9.52%의 흡수력을 보여주고 있다. 이것은 일반 유화의 경우 유화입경이 크고 거칠어서 인조피부층을 통과하지 못하는 것으로 해석되며, 실시예17은 2중 캡슐이 부드럽에 깨져서 나오는 1중의 액정입자는 나노입자를 형성하기 때문에 인조피부를 쉽게 통과하는 것으로 해석된다. Figure 8 is a graph showing transdermal absorption tests through examples. For the evaluation of transdermal absorption, artificial skin was mounted using a Frenzcell, a sample was applied on top, and sampling was conducted over up to 10 hours, and the extent to which transdermal absorption was possible was measured through HPLC quantitative analysis. The drug in the measurement index was expressed as a percentage by quantitative analysis of AHK-Cu. In the case of Comparative Example 4, the absorption power was 0.05% after 1 hour and 1.28% after 10 hours. On the other hand, Example 17 shows an absorption capacity of 1.96% after 1 hour and 9.52% after 10 hours. This is interpreted as the fact that in the case of general emulsification, the emulsion particle diameter is large and rough, so it cannot pass through the artificial skin layer. In Example 17, the double-layer capsule is soft, and the single liquid crystal particles that come out form nanoparticles that easily pass through the artificial skin. It is interpreted that
<실험예 6> 2중 캡슐의 안정성 평가<Experimental Example 6> Stability evaluation of double capsule
도 9는 2중캡슐의 안정성을 평가한 그래프이다. 비교예 4와, 실시예 7의 1중 캡슐과 실시예13의 2중 캡슐에 대하여 45℃ 인큐베이터에 3개월동안 보관한 샘플을 HPLC 정량분석을 통하여 잔존량을 분석하고 안정성을 백분율로 환산하여 측정하였다. 비교예4의 경우 지표물질이 약 12.6% 존재하였으며, 1중캡슐인 실시예7은 61.5%, 2중캡슐인 실시예13은 98.5%로 2중 캡슐이 다른 시료군에 비하여 월등하게 우수한 안정성을 보였다. 이것은 고분자매트릭스 캡슐이 1중 캡슐의 액정 입자를 코팅하고 있어서 외부와의 접촉이 없으며, 산소와 차단되어 산폐되지 않고 안정한 상태로 유지되고 있다는 것을 반증해 주고 있는 의미 있는 결과이다. Figure 9 is a graph evaluating the stability of the double capsule. For Comparative Example 4, the single capsule of Example 7, and the double capsule of Example 13, samples stored in an incubator at 45°C for 3 months were analyzed for residual amount through HPLC quantitative analysis, and stability was measured by converting it into a percentage. did. In the case of Comparative Example 4, about 12.6% of the indicator substance was present, Example 7, which was a single-layer capsule, contained 61.5%, and Example 13, which was a double-layer capsule, contained 98.5%, showing that the double-layer capsule had significantly better stability than other sample groups. It seemed. This is a meaningful result that disproves that the polymer matrix capsule coats the liquid crystal particles of the single-layer capsule, so there is no contact with the outside, and it is blocked from oxygen and is maintained in a stable state without oxidation.
이와 같이 본 발명에 대해서 첨부된 도면을 참조하여 설명하였으나, 본 발명의 기술적 사상을 벗어나지 않는 범위 내에서 다양한 수정 및 변형이 이루어질 수 있음은 물론이다. 그러므로, 본 발명의 범위는 설명된 실시례에 한정되어서는 아니되며, 후술하는 특허 청구범위 뿐만아니라 이러한 특허청구범위와 균등한 것들에 의해 정해져야 한다.Although the present invention has been described with reference to the accompanying drawings, it goes without saying that various modifications and variations can be made without departing from the technical spirit of the present invention. Therefore, the scope of the present invention should not be limited to the described embodiments, but should be determined by the patent claims described below as well as equivalents to these claims.
Claims (6)
수상성분을 준비하는 수상성분제공단계;
상기 유상성분과 상기 수상성분을 혼합하는 제1혼합단계;
상기 제1혼합단계 후의 혼합물에 유효성분을 혼합하여 제1혼합용액을 제조하는 유효성분제공단계;
상기 제1혼합용액을 100 내지 1000bar의 고압으로 나노믹서에 통과하여 상기 유효성분이 내부에 포집된 다층 라멜라 액정구조의 나노입자를 포함하는 수중유형 액정 에멀젼을 형성하는 1차캡슐화단계;
상기 액정 에멀젼과 고분자가 용해된 수상의 고분자용액을 혼합하여 제2혼합용액을 제조하는 제2혼합단계; 및
상기 제2혼합용액을 노즐에 통과시키고 드롭핑하여 상기 액정구조의 나노입자를 내부에 포함하는 고분자 매트릭스를 가지는 2중 매트릭스캡슐입자를 얻는 2차캡슐화단계; 를 포함하는 2중 매트릭스 캡슐의 제조방법. Oil ingredient provision step of preparing oil ingredients;
An aqueous ingredient provision step of preparing an aqueous ingredient;
A first mixing step of mixing the oil phase component and the aqueous phase component;
An active ingredient providing step of preparing a first mixed solution by mixing the active ingredient with the mixture after the first mixing step;
A first encapsulation step of passing the first mixed solution through a nanomixer at a high pressure of 100 to 1000 bar to form an oil-in-water liquid crystal emulsion containing nanoparticles with a multilayer lamellar liquid crystal structure with the active ingredient trapped therein;
A second mixing step of preparing a second mixed solution by mixing the liquid crystal emulsion and the aqueous polymer solution in which the polymer is dissolved; and
A secondary encapsulation step of passing the second mixed solution through a nozzle and dropping it to obtain double matrix capsule particles having a polymer matrix containing the liquid crystal structure nanoparticles therein; Method for manufacturing a double matrix capsule comprising.
상기 2중 매트릭스캡슐입자의 크기는 0.1㎛~5mm인 2중 매트릭스 캡슐의 제조방법.According to paragraph 1,
A method of manufacturing a double matrix capsule wherein the size of the double matrix capsule particles is 0.1㎛ ~ 5mm.
상기 유상성분은 1차캡슐을 형성하기 위한 계면활성제와 다가알코올, 및 오일성분을 포함하는 2중 매트릭스 캡슐의 제조방법.According to paragraph 1,
A method of producing a double matrix capsule wherein the oil phase component includes a surfactant, polyhydric alcohol, and an oil component to form the primary capsule.
상기 수상성분은 정제수, 점증제, 피부자극완화 성분, 피부보습성분, 보존제성분등이 포함되는 2중 매트릭스 캡슐의 제조방법.According to paragraph 1,
A method of manufacturing a double matrix capsule in which the aqueous ingredients include purified water, a thickener, a skin irritation relieving ingredient, a skin moisturizing ingredient, and a preservative ingredient.
상기 유효성분은 GHK-Cu, AHK-Cu, 피세틴, 쿼세틴, 이데베논, 비타민류, 라스베라트롤, 카페인, 아데노신, 코디세핀, 니아신아마이드, 및 제니스테인로 구성되는 군에서 선택되는 하나 또는 2이상의 물질인 2중 매트릭스 캡슐의 제조방법.According to paragraph 1,
The active ingredient is one or two or more selected from the group consisting of GHK-Cu, AHK-Cu, fisetin, quercetin, idebenone, vitamins, resveratrol, caffeine, adenosine, cordycepin, niacinamide, and genistein. Method for manufacturing a double matrix capsule material.
상기 고분자는 피이지-240/에이치디아이코폴리머비스-데실테트라데세스-20에터인 2중 매트릭스 캡슐의 제조방법.
According to paragraph 1,
A method of manufacturing a double matrix capsule wherein the polymer is PEG-240/HDI copolymer bis-decyltetradeceth-20 ether.
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