KR101610246B1 - Stable non-epispastic vitamin C cosmetic composition having high skin-transmissivity - Google Patents

Stable non-epispastic vitamin C cosmetic composition having high skin-transmissivity Download PDF

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KR101610246B1
KR101610246B1 KR1020140134457A KR20140134457A KR101610246B1 KR 101610246 B1 KR101610246 B1 KR 101610246B1 KR 1020140134457 A KR1020140134457 A KR 1020140134457A KR 20140134457 A KR20140134457 A KR 20140134457A KR 101610246 B1 KR101610246 B1 KR 101610246B1
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김병욱
장동일
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(주)폭스앤플래닛
장동일
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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
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/67Vitamins
    • A61K8/676Ascorbic acid, i.e. vitamin C
    • 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
    • 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
    • A61K8/67Vitamins
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin

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Abstract

Provided in the present invention is a cosmetic composition comprising vitamin C as an active component, wherein vitamin C is dissolved in a mixed solvent obtained by mixing propanediol, pentylene glycol, butylene glycol, diethoxy ethyl succinate, dimethyl isosorbide, bis-ethoxy diglycol, cyclohexane 1,4- dicarboxylate, and peppermint oil. The composition according to the present invention improves stability of vitamin C, and increases skin transmissivity, thereby being used as an antioxidant cosmetic composition. Also, the composition according to the present invention is anhydrous, so the composition not only effectively removes a problem of vitamin C easily decomposed by an external environment such as water, temperature, sunray, and the like, by an innovative method controlling the decomposition of vitamin C caused by the oxidation and other problems occurring in an aqueous phase, but also controls the growth of pathogen and microorganisms causing the decomposition propagated through water.

Description

비타민 C를 함유하는 안정화되고 피부 투과율이 높은 화장료 조성물{Stable non-epispastic vitamin C cosmetic composition having high skin-transmissivity}[0001] The present invention relates to a stabilized non-epispastic vitamin C cosmetic composition having high skin-transmissivity,

본 발명은 비타민 C를 함유하는 화장료 조성물에 관한 것으로서, 더욱 상세하게는 비타민 C를 안정화시켜 비타민 C가 물, 온도, 광선 등의 외부환경에 의해 산화되는 것을 효과적으로 억제할 수 있으면서 비타민 C의 피부 투과량을 향상시킨 화장료 조성물에 관한 것이다.The present invention relates to a cosmetic composition containing vitamin C, and more particularly, to a cosmetic composition containing vitamin C by stabilizing vitamin C and effectively inhibiting oxidation of vitamin C by an external environment such as water, temperature, To an improved cosmetic composition.

비타민 C(ascorbic acid)는 인체의 면역기능을 높여주고 피부, 연골, 모세혈관, 근육 등의 구성요소인 콜라겐(collagen)의 생성을 촉진하며 자외선이 피부에 침투하여 생기는 화학물질을 파괴하여 피부손상을 막아주는 역할을 한다. 또한 주름을 방지하고, 건강하게 피부를 유지시키며, 상처 난 피부 조직의 치료를 돕고 알레르기 반응을 일으키는 것으로 알려진 히스타민(histamin)의 형성 및 노화 과정 중에 피부를 퇴색시키는 멜라민(melamine)의 형성을 막아주는 노화방지제로서 알려져 있다.Vitamin C (ascorbic acid) enhances the immune function of the human body and promotes the production of collagen, which is a component of skin, cartilage, capillary blood vessels and muscles, and destroys chemical substances generated by penetration of ultraviolet rays into skin, . It also helps prevent wrinkles, maintain healthy skin, help to heal damaged skin tissues, prevent the formation of histamine, which is known to cause allergic reactions, and the formation of melamine, which fades skin during the aging process. Are known as antioxidants.

그러나 비타민 C는 γ-락톤과 유사한 구조로서 불안정하여 물과 공기, 특히 산소와 열, 그리고 빛과 같은 외부환경에 민감하게 반응하여 쉽게 산화되는 문제점이 있다. 비타민 C의 산화반응은 대게 연속적인 두 개의 전자 전이과정(electron transfer process)인 수소이온의 해리로 인한 비타민 C의 산화 중간체(intermediate)인 디하이드로아스코벨이트 라디칼이 만들어지며 이는 반응성이 풍부하고 그 자체가 2 분자로 반응해서 1 분자의 비타민 C와 디하이드로아스코르빈산을 생산한다고 알려져 있다. However, vitamin C is unstable due to its structure similar to γ-lactone, and is easily oxidized due to sensitivity to external environment such as water and air, especially oxygen, heat, and light. Oxidation of vitamin C produces dihydro-ascorbate radicals, an intermediate of vitamin C due to the dissociation of hydrogen ions, which are usually two consecutive electron transfer processes, which are rich in reactivity It is known that it itself reacts with two molecules to produce one molecule of vitamin C and dihydroacercubic acid.

비수용액 중에서는 극소량이 용해되는 반면 수용액 중에서는 많은 양이 용해되지만 빠른 산화 작용으로 인하여 충분한 양의 비타민 C가 안정화되지 못하기 때문에, 의약, 식품, 화장품 등에서는 활성물질(active ingredient)로서 소량의 비타민 C만이 사용 가능한 것으로 보고되어 있다.A very small amount is dissolved in a non-aqueous solution, whereas a large amount is dissolved in an aqueous solution. However, since a sufficient amount of vitamin C can not be stabilized due to rapid oxidation, a small amount of active ingredient Only vitamin C has been reported to be available.

이러한 비타민 C 고유의 문제점을 보완하고 안정성을 향상시키기 위하여 비타민 C 유도체(ascorbic acid derivative)를 사용하는 방안이 제안되어 있지만 효율 면에서 열등한 단점이 있었다.A method of using an ascorbic acid derivative to complement the inherent problems of vitamin C and to improve its stability has been proposed, but it has a disadvantage in terms of efficiency.

한편, 최근 들어, 비타민 C의 산화를 방지하기 위한 방법으로서 무수상태의 비타민 C를 제형의 측면에서 안정화시키고자, 다가 알코올(POLYOLS)을 용매로서 사용하여 비타민C를 용해하였지만, 종래의 기술은 8%가 최대로, 가장 효과적인 20%에는 크게 못 미치고 있다.In recent years, as a method for preventing the oxidation of vitamin C, vitamin C has been dissolved by using polyhydric alcohol (POLYOLS) as a solvent in order to stabilize anhydrous vitamin C in terms of formulation. However, % Is the largest, far below the most effective 20%.

미국 특허 등록 US 7,179,841 B2US Patent No. 7,179,841 B2

본 발명자들은 연구를 거듭한 결과, 용매로서 프로판디올, 펜틸렌글라이콜, 부틸렌글라이콜, 디에톡시에칠석시네이트, 디메칠이소소바이드, 비스-에톡시디글라이콜 사이클로헥산1,4-디카복실레이트, 페퍼민트오일의 이상적인 배합을 통하여, 화장품의 피부 투과율을 높이면서도, 화장품으로 사용할 시 가장 적합한 비타민 C의 용해도(20%)를 가지도록 하여 상술한 종래기술의 문제점 해결에 성공하였다.As a result of extensive research, the inventors of the present invention have found that, as a solvent, propane diol, pentylene glycol, butylen glycol, diethoxyethane monostearate, dimethicone ssobide, bis-ethoxydiglycol cyclohexane 1,4- Dicarboxylate, and peppermint oil, the solubility of vitamin C (20%), which is most suitable for use as a cosmetic product, is increased while enhancing the skin permeability of cosmetics and succeeding in solving the problems of the prior art described above.

따라서 본 발명의 목적은 비타민 C를 유효성분으로 하면서 효과적으로 안정되고 피부 투과율이 높은 화장료 조성물을 제공하는 것이다.Accordingly, an object of the present invention is to provide a cosmetic composition which is effectively stabilized and has high skin permeability while containing vitamin C as an active ingredient.

상기 기술적 과제를 달성하기 위하여, 본 발명은According to an aspect of the present invention,

비타민 C를 프로판디올, 펜틸렌글라이콜, 부틸렌글라이콜, 디에톡시에칠석시네이트, 디메칠이소소바이드, 비스-에톡시디글라이콜 사이클로헥산1,4-디카복실레이트 및 페퍼민트오일을 배합한 혼합 용매에 용해시킨 활성성분으로 비타민 C를 포함하는 화장료 조성물을 제공한다.
Vitamin C may be formulated with propanediol, pentaerythritol, butyleneglycol, diethoxylated monostearate, dimethicone isobarbide, bis-ethoxydiglycol cyclohexane 1,4-dicarboxylate and peppermint oil A cosmetic composition comprising vitamin C as an active ingredient dissolved in one mixed solvent is provided.

상술한 바와 같은 본 발명에 따른 조성물은 상기 비타민 C를 15 내지 25중량% 함유하고, 잔부는 상기 혼합 용매일 수 있다.
The composition according to the present invention as described above contains 15 to 25% by weight of the vitamin C, and the balance may be the daily for mixing.

상술한 바와 같은 본 발명에 있어서, 제 1항 또는 제 2항에 있어서, 상기 혼합 용매는 프로판디올 60 ~ 70중량%, 펜틸렌글라이콜 10 ~ 20중량%, 부틸렌글라이콜 5.0 ~ 15중량%, 디에톡시에칠석시네이트 2.5 ~ 7.5중량%, 디메칠이소소바이드 1.0 ~ 4.0중량%, 비스-에톡시디글라이콜 사이클로헥산1,4-디카복실레이트 1.0 ~ 3.0중량%, 페퍼민트오일 0.05 ~ 0.15중량% 포함할 수 있으며, 바람직하게는 프로판디올 66.6중량%, 펜틸렌글라이콜 14중량%, 부틸렌글라이콜 10중량%, 디에톡시에칠석시네이트 5중량%, 디메칠이소소바이드 2.3중량%, 비스-에톡시디글라이콜 사이클로헥산1,4-디카복실레이트 2중량%, 페퍼민트오일 0.1중량%로 구성될 수 있다.In the present invention as described above, the mixed solvent may include 60 to 70% by weight of propanediol, 10 to 20% by weight of pentaerythritol, 5.0 to 15% by weight of butylene glycol, 2.5 to 7.5% by weight of diethoxy stannate, 1.0 to 4.0% by weight of dimethicone isobaride, 1.0 to 3.0% by weight of bis-ethoxydiglycol cyclohexane 1,4-dicarboxylate, 0.15% by weight, preferably 66.6% by weight of propanediol, 14% by weight of pentylene glycol, 10% by weight of butylene glycol, 5% by weight of diethoxy tin dilaurate, 2.3% by weight of dimethicone isobaride 2% by weight of bis-ethoxydiglycol cyclohexane 1,4-dicarboxylate, and 0.1% by weight of peppermint oil.

상술한 바와 같이, 본 발명에 따른 조성물은 비타민 C의 안정성을 향상시키고 피부 투과율을 높인 것으로서, 항산화 화장료 조성물로서 유용하게 사용할 수 있다.As described above, the composition according to the present invention improves the stability of vitamin C and increases the skin permeability, and thus can be usefully used as an antioxidant cosmetic composition.

또한 본 발명에 따른 조성물은 무수상이기 때문에 수상에서 발생되는 산화 및 기타의 문제로 인해 비타민 C가 분해되는 것을 억제하는 획기적인 방법으로, 물, 온도, 광선 등의 외부환경에 의해 쉽게 분해되는 비타민 C의 문제를 효과적으로 해결하였을 뿐만 아니라, 물로 인하여 증식되는 병원성 세균, 부패의 원인이 되는 미생물의 성장도 억제할 수 있다.In addition, the composition according to the present invention is an innovative method for inhibiting the decomposition of vitamin C due to oxidation and other problems occurring in a water phase due to its non-aqueous phase, and is a vitamin C easily decomposed by external environment such as water, temperature, Not only effectively solved the problem of microbial growth, but also inhibited the growth of pathogenic microbes, which are caused by water, and microorganisms which are responsible for decay.

도 1은 비타민 C 피부 투과 시험을 위한 HPLC의 사진이다.
도 2는 비타민 C 피부 투과 시험을 위한 Side-by-side diffusion cell의 사진이다.
도 3은 비타민 C 피부 투과 시험 결과를 도시한 그래프이다.
Figure 1 is a photograph of HPLC for vitamin C skin permeation test.
2 is a photograph of a side-by-side diffusion cell for vitamin C skin permeation test.
3 is a graph showing the results of vitamin C skin permeation test.

본 발명을 상세하게 설명하기로 한다.The present invention will be described in detail.

본 발명자들은 연구를 거듭한 결과, 용매로서 프로판디올, 펜틸렌글라이콜, 부틸렌글라이콜, 디에톡시에칠석시네이트, 디메칠이소소바이드, 비스-에톡시디글라이콜 사이클로헥산1,4-디카복실레이트, 페퍼민트오일의 이상적인 배합을 통하여, 화장품의 피부 투과율을 높이면서도, 화장품으로 사용할 시 가장 적합한 비타민 C의 용해도 20%를 가지도록 하여 상술한 종래기술의 문제를 해결하였으며, 이에 따라서 본 발명의 목적은 비타민 C를 유효성분으로 하면서 효과적으로 안정되고 피부 투과율이 높은 화장료 조성물을 제공하는 것이다.As a result of extensive research, the inventors of the present invention have found that, as a solvent, propane diol, pentylene glycol, butylen glycol, diethoxyethane monostearate, dimethicone ssobide, bis-ethoxydiglycol cyclohexane 1,4- Dicarboxylate and peppermint oil, the solubility of vitamin C is 20%, which is most suitable for use as a cosmetic product, while improving the skin permeability of cosmetics and solving the problems of the prior art. Is to provide a cosmetic composition which is effectively stabilized and has high skin permeability while containing vitamin C as an active ingredient.

이러한 기술적 과제를 달성하기 위하여, 본 발명은 비타민 C를 프로판디올, 펜틸렌글라이콜, 부틸렌글라이콜, 디에톡시에칠석시네이트, 디메칠이소소바이드, 비스-에톡시디글라이콜 사이클로헥산1,4-디카복실레이트 및 페퍼민트오일을 배합한 혼합 용매에 용해시킨 활성성분으로 비타민 C를 포함하는 화장료 조성물을 제공한다.
In order to accomplish this technical object, the present invention relates to a pharmaceutical composition comprising vitamin C in combination with propanediol, pentaerythritol, butyleneglycol, diethoxylated monostearate, dimethylysosobide, bis-ethoxydiglycolcyclohexane 1 , 4-dicarboxylate, and peppermint oil. The present invention also provides a cosmetic composition comprising vitamin C as an active ingredient.

상술한 바와 같은 본 발명에 따른 조성물은 상기 비타민 C를 15 내지 25중량% 함유할 수 있으며, 상기 혼합 용매는 프로판디올 60 ~ 70중량%, 펜틸렌글라이콜 10 ~ 20중량%, 부틸렌글라이콜 5.0 ~ 15중량%, 디에톡시에칠석시네이트 2.5 ~ 7.5중량%, 디메칠이소소바이드 1.0 ~ 4.0중량%, 비스-에톡시디글라이콜 사이클로헥산1,4-디카복실레이트 1.0 ~ 3.0중량%, 페퍼민트오일 0.05 ~ 0.15중량% 포함할 수 있으며, 바람직하게는 프로판디올 66.6중량%, 펜틸렌글라이콜 14중량%, 부틸렌글라이콜 10중량%, 디에톡시에칠석시네이트 5중량%, 디메칠이소소바이드 2.3중량%, 비스-에톡시디글라이콜 사이클로헥산1,4-디카복실레이트 2중량%, 페퍼민트오일 0.1중량% 로 구성될 수 있다.
The composition according to the present invention may contain 15 to 25% by weight of the vitamin C, and the mixed solvent may include 60 to 70% by weight of propanediol, 10 to 20% by weight of pentylene glycol, 5.0 to 15% by weight of diethoxy stannate, 2.5 to 7.5% by weight of diethoxy stannanesulfonate, 1.0 to 4.0% by weight of dimethicone isobaride, 1.0 to 3.0% by weight of bis-ethoxydiglycol cyclohexane 1,4-dicarboxylate, , 0.05 to 0.15% by weight of peppermint oil, and preferably 66.6% by weight of propanediol, 14% by weight of pentylene glycol, 10% by weight of butylene glycol, 5% by weight of diethoxy- 2.3% by weight of isobarbide, 2% by weight of bis-ethoxydiglycolcyclohexane 1,4-dicarboxylate and 0.1% by weight of peppermint oil.

이하 실시예 및 실험예를 통하여 본 발명을 상세하게 설명하기로 한다. 후술하는 실시예와 실험예에 의해 본 발명이 한정되는 것이 아님은 명백하다.
Hereinafter, the present invention will be described in detail with reference to Examples and Experimental Examples. It is apparent that the present invention is not limited by the following examples and experimental examples.

<본 발명에 따른 조성물의 제조>&Lt; Preparation of composition according to the present invention >

하기 표 1과 같은 성분과 배합 비율을 가지도록 혼합용매를 제조한 후에 이 혼합 용매와 비타민 C 배합 비율은 하기 표 2와 같이 하여 본 발명에 따른 조성물을 하였다.After preparing a mixed solvent having a mixing ratio with the components shown in Table 1, the composition according to the present invention was prepared as shown in Table 2 below.

성분ingredient 배합비(중량%)Compounding ratio (% by weight) 프로판디올Propanediol 66.6 66.6 펜틸렌글라이콜Pentyleneglycol 14 14 부틸렌글라이콜Butylene glycol 10 10 디에톡시에칠석시네이트Diethoxy-fumarate 5 5 디메칠이소소바이드Dimethyldisoside 2.3 2.3 비스-에톡시디글라이콜사이클로헥산1,4-디카복실레이트Bis-ethoxydiglycol cyclohexane 1,4-dicarboxylate 2 2 페퍼민트오일Peppermint oil 0.1 0.1


성분

ingredient
함량비(중량%)Content ratio (% by weight)
샘플 1Sample 1 샘플 2Sample 2 샘플 3Sample 3 비타민 CVitamin C 1515 2525 2020 혼합용매Mixed solvent 8585 7575 8080

<< 비교예의Comparative example 조성물 제조> Composition Preparation>

하기 표 3의 배합 비율을 가지도록 비교예의 조성물을 제조하였다.The compositions of Comparative Examples were prepared so as to have the blending ratios shown in Table 3 below.


성분

ingredient
함량비(중량%)Content ratio (% by weight)
비교 샘플 1Comparative Sample 1 비교 샘플 2Comparative Sample 2 비타민 CVitamin C 1515 2020 정제수Purified water 8585 8080

<조성물의 피부 투과 시험: 피부 투과 연구>&Lt; Skin permeation test of composition: Skin permeation study >

1. 시험 방법1. Test Method

상기 실시예에서 제조한 본 발명에 따른 조성물 및 비교예의 조성물 각각 side-bi-side diffusion cell의 donor phase에 넣은 뒤, 1, 3, 6, 9, 12, 24 시간 동안 diffusion cell의 receptor phase로 투과된 ascorbic acid의 양을 HPLC를 이용하여 정량하여 피부 투과 시험을 실시하였다.The composition according to the present invention prepared in the above example and the composition according to the comparative example were put into the donor phase of the side-bi-side diffusion cell and permeated into the receptor phase of the diffusion cell for 1, 3, 6, 9, The amount of ascorbic acid was quantified by HPLC and skin permeation test was performed.

상기 HPLC에 대한 사진은 도 1로 첨부하였다. A photograph of the above HPLC is attached in Fig.

2. 시험시설 및 장비2. Testing facilities and equipment

NO.NO. 시험시설 및 장비명 Test facility and equipment name 규 격 standard 제조사 정보 Manufacturer Information 용 도 Usage 1One Side-by-side diffusion cell
(도 2)
Side-by-side diffusion cell
(Fig. 2)
내용량 1 ㎖ 투과면적 0.57 cm2 Contents 1 ml Transmission area 0.57 cm 2 유일과학(주), Busan,
Korea
Unique Science Co., Ltd., Busan,
Korea
피부투과실험용Experimental skin permeation
22 HPLC system (도 1)The HPLC system (Figure 1) -- Futecs, Daejeon, Korea Futecs, Daejeon, Korea 정량분석용For quantitative analysis 33 pH meter (Model 320pH meter (Model 320 Digital typeDigital type Corning, NY, USA Corning, NY, USA pH 측정pH measurement 44 Vortex (G-560)Vortex (G-560) Hz 60Hz 60 Scientific Industries Inc.,
NY, USA
Scientific Industries Inc.,
NY, USA
시약 혼합Reagent mixing
55 Deep Freezer (MDF-
U2086S)
Deep Freezer (MDF-
U2086S)
216 ℓ216 L SANYO Co., Osaka, Japan SANYO Co., Osaka, Japan 초저온 냉동고Cryogenic freezer

3. 실험 방법3. Experimental Method

(1) (One) HairlessHairless mousemouse skinskin 준비  Ready

8 주령의 hairless mouse의 full-thickness skin을 사용하였다. Mouse를 CO2 gas로 희생시킨 뒤 피부를 박리한 후 피부 안쪽의 피하지방을 제거하여 -70℃ deep freezer에 보관하였다가 실험 직전 상온에서 녹여 피부에 상처나 긁힌 흔적이 없는 부분을 사용하였다. Full-thickness skin of 8-week-old hairless mice was used. The mice were sacrificed with CO 2 gas, and the skin was peeled off. The subcutaneous fat inside the skin was removed and stored in a deep freezer at -70 ° C. Then, the skin was melted at room temperature just before the experiment, and the skin was scratched or scratched.

Side-by-side diffusion cell (내용량 1 ㎖, 투과면적 0.57 cm2) 사이에 hairless mouse의 피부를 놓고 clamp로 고정시켜 사용하였다 (도 2 참조).
The skin of the hairless mouse was placed between the side-by-side diffusion cell (content of 1 ml, permeation area of 0.57 cm 2 ) and fixed with a clamp (see FIG. 2).

(2) (2) 실험군Experimental group

Diffusion cell의 donor phase쪽에 상기 실시예에서 표 2에 따른 본 발명의 조성물들을 각각 1㎖씩 넣고, receptor phase 쪽에는 PBS (phosphate buffer saline, pH 7.4, acetonitrile 2% (v/v) 함유) 용액을 1㎖ 채운 다음 투과실험을 실시하였다. 1 ml each of the compositions of the present invention as shown in Table 2 in the above examples was added to the donor phase of the diffusion cell and a solution of PBS (phosphate buffer saline, pH 7.4, containing 2% (v / v) acetonitrile) And then permeation experiments were carried out.

본 연구에서는 ascorbic acid의 안정성을 샘플링 시간 동안 유지하기 위해, 실험에 사용한 모든 PBS(phosphate buffer saline, pH 7.4)용액 내에 acetonitrile을 2% (v/v) 첨가하였다. In this study, 2% (v / v) acetonitrile was added to all PBS (phosphate buffer saline, pH 7.4) solution to maintain the stability of ascorbic acid during the sampling time.

1, 3, 6, 9, 12, 24시간 후에 diffusion cell의 receptor phase쪽의 용액을 각각 모두 취해 검액으로 사용하였고, 즉시 새로운 PBS 용액으로 receptor cell에 1㎖를 채워 넣었다. After 1, 3, 6, 9, 12, and 24 hours, each of the solutions in the receptor phase of the diffusion cell was used as the sample solution and immediately filled with 1 ml of the new PBS solution into the receptor cell.

검액 내에 있는 ascorbic acid의 정량은 high-performance liquid chromatography (HPLC; Futecs, Daejeon, Korea)를 이용하였다. High-performance liquid chromatography (HPLC, Futecs, Daejeon, Korea) was used for the determination of ascorbic acid in the test solution.

Column은 5 μm C18 (4.6 x 250 mm, CAPCELL PAK, Shiseido)을 사용하였으며 oven의 온도는 36.5℃를 유지하였다. 각각의 개체 수는 5로 하였다. Columns were 5 μm C18 (4.6 x 250 mm, CAPCELL PAK, Shiseido) and the oven temperature was maintained at 36.5 ° C. The number of individuals was 5.

(4) 대조군 ((4) Control ( CellexCellex -c) -c)

Diffusion cell의 donor phase쪽에 표 3에 따른 비교예의 조성물들을 각각 1㎖를 넣고, receptor phase 쪽에는 PBS 용액 1㎖를 채운 다음 투과 실험을 실시하였다. In the donor phase of the diffusion cell, 1 ml of each of the comparative compositions according to Table 3 was added, and 1 ml of PBS solution was filled in the receptor phase.

1, 3, 6, 9, 12, 24시간 후에 diffusion cell의 receptor phase쪽의 용액을 각각 모두 취해 검액으로 사용하였고, 즉시 새로운 PBS 용액으로 receptor cell에 1㎖를 채워 넣었다. 검액 내에 있는 ascorbic acid는 HPLC로 정량하였다. 각각의 개체 수는 5로 하였다.
After 1, 3, 6, 9, 12, and 24 hours, each of the solutions in the receptor phase of the diffusion cell was used as the sample solution and immediately filled with 1 ml of the new PBS solution into the receptor cell. The ascorbic acid in the sample solution was quantified by HPLC. The number of individuals was 5.

4. 시험결과 및 분석4. Test Results and Analysis

(1) 본 발명에 따른 조성물(표 2의 조성물)을 사용하여 1, 3, 6, 9, 12, 24시간 동안의 피부를 통한 ascorbic acid 투과를 측정한 결과 비교예의 조성물(표 3의 조성물) 사용한 대조군에 비하여 큰 투과량 증가를 나타내었다. (1) The composition of the comparative example (composition of Table 3) was determined by measuring the permeation of ascorbic acid through the skin for 1, 3, 6, 9, 12 and 24 hours using the composition according to the present invention And the increase of the permeability was larger than that of the control group.

(2) 본 발명에 따른 샘플 1을 사용하여 실험하였을 경우 6시간 후 20.467 ㎍/cm2, 24시간 후 50.483 ㎍/cm2의 피부투과를 나타내어 비교 샘플 1을 사용한 대조군 (6시간 후 15.862 ㎍/cm2, 24시간 후 32.232 ㎍/cm2)에 비해 각 시간에서 1.29배, 1.57배의 투과량이 증가함을 관찰하였다. (2) When hayeoteul experiment using the sample 1 according to the invention after 6 hours 20.467 ㎍ / cm 2, 24 hours after the image shows a skin permeation of 50.483 ㎍ / cm 2 Comparative Sample control group with 1 (3 hours after 15.862 ㎍ / cm 2 , and 32.232 ㎍ / cm 2 after 24 hours), respectively.

(3) 본 발명에 따른 샘플 2를 사용하여 실험하였을 경우 6시간 후 34.855 μg/cm2, 24시간 후 136.783 ㎍/cm2의 피부투과를 나타내어 비교 샘플 1을 사용한 대조군 (6시간 후 15.862 ㎍/cm2, 24시간 후 32.232 ㎍/cm2)에 비해 각 시간에서 2.20배, 4.24배의 투과량이 증가함을 관찰하였다. (3) hayeoteul experiment using the sample 2 of the present invention after 6 hours 34.855 μg / cm 2, 24 hours after 136.783 ㎍ / image shows a skin permeation of cm 2 Comparative Sample control group with 1 (3 hours after 15.862 ㎍ / cm 2 , and 32.232 ㎍ / cm 2 after 24 hours), respectively.

(4) 본 발명에 따른 샘플 3을 사용하여 실험하였을 경우 6시간 후 59.869 ㎍/cm2, 24시간 후 183.981 ㎍/cm2의 피부투과를 나타내어 비교 샘플 1을 사용한 대조군 (6시간 후 15.862 ㎍/cm2, 24시간 후 32.232 ㎍/cm2)에 비해 각 시간에서 3.77배, 5.71배의 투과량이 증가함을 관찰하였다. (4) When hayeoteul experiment with a sample 3 according to the invention after 6 hours 59.869 ㎍ / cm 2, 24 hours after the image shows a skin permeation of 183.981 ㎍ / cm 2 Comparative Sample control group with 1 (3 hours after 15.862 ㎍ / cm 2 , and 32.232 ㎍ / cm 2 after 24 hours), respectively.

(5) 본 발명에 따른 샘플 1을 사용하여 실험하였을 경우 6시간 후 20.467 ㎍/cm2, 24시간 후 50.483 ㎍/cm2의 피부투과를 나타내어 비교 샘플 2를 사용한 대조군(6시간 후 16.369 ㎍/cm2, 24시간 후 39.372 μg/cm2)에 비해 1.25배, 1.28배의 투과량이 증가함을 관찰하였다. (5) When hayeoteul experiment using the sample 1 according to the invention after 6 hours 20.467 ㎍ / cm 2, 24 hours after 50.483 ㎍ / cm Control 2 indicated a skin permeation using a comparative sample 2 (6 hours after 16.369 ㎍ / cm 2 and 39.372 μg / cm 2 after 24 hours), respectively.

(6) 본 발명에 따른 샘플 2를 사용하여 실험하였을 경우 6시간 후 34.855 μg/cm2, 24시간 후 136.783 μg/cm2의 피부투과를 나타내어 비교 샘플 2를 사용한 대조군 (6시간 후 16.369 μg/cm2, 24시간 후 39.372 ㎍/cm2)에 비해 각 시간에서 2.13배, 3.47배의 투과량이 증가함을 관찰하였다. (6) hayeoteul experiment using the sample 2 of the present invention after 6 hours 34.855 μg / cm 2, 24 hours after 136.783 represented by the skin permeation of μg / cm 2 Comparative Sample control group with 2 (6 hours of 16.369 μg / cm 2 and 39.372 ㎍ / cm 2 after 24 hours), respectively.

(7) 본 발명에 따른 샘플 3을 사용하여 실험하였을 경우 6시간 후 59.869 ㎍/cm2, 24시간 후 183.981 ㎍/cm2의 피부투과를 나타내어 비교 샘플 2를 사용한 대조군 (6시간 후 16.369 ㎍/cm2, 24시간 후 39.372 ㎍/cm2)에 비해 3.66배, 4.67배의 투과량이 증가함을 관찰하였다. (7) If hayeoteul experiment with a sample 3 according to the invention after 6 hours 59.869 ㎍ / cm 2, 24 hours after the image shows a skin permeation of 183.981 ㎍ / cm 2 Comparative Sample control group with 2 (3 hours after 16.369 ㎍ / cm 2 and 39.372 ㎍ / cm 2 after 24 hours), respectively.

(8) 실험 결과는 도 3으로 정리하여 나타냈다.
(8) Experimental results are summarized in FIG.

<조성물의 안정성 시험: 비타민 C의 &Lt; Stability test of composition: Vitamin C 역가Potency 측정> Measurement>

상기 실시예에서 표 2와 표 3에 따라 제조된 조성물에 대하여 비타민 C의 역가 유지능을 알아보기 위해 비타민 C의 초기 역가를 100으로 하고, 1개월 후의 비타민 C의 역가를 25℃와 45℃에서 측정하였으며, 그 결과를 하기 표 5에 나타내었다. 측정은 Waters사의 SunFire C18 5,100A, 150X4.6mm 컬럼을 이용하였다. 이때, 검출기의 파장은 254nm으로 하고, 이동상은 25mM KH2PO4 buffer(pH2.5)를 이용하였으며, 0.6㎖/min의 유속으로 측정하였다.To evaluate the potency of vitamin C to maintain the potency of the composition prepared according to Tables 2 and 3, the initial potency of vitamin C was set at 100, and the activity of vitamin C after 1 month was measured at 25 ° C and 45 ° C The results are shown in Table 5 below. The measurement was performed using a Waters SunFire C18 5,100 A, 150 X 4.6 mm column. At this time, the wavelength of the detector was 254 nm, and the mobile phase was measured with a flow rate of 0.6 ml / min using 25 mM KH 2 PO 4 buffer (pH 2.5).

비고Remarks 샘플 1Sample 1 샘플 2Sample 2 샘플 3Sample 3 비교 샘플 1Comparative Sample 1 비교 샘플 2Comparative Sample 2 25℃25 ℃ 9999 9999 9999 9999 9999 45℃45 ° C 9797 9696 9797 8282 7979

상기 표 5에서 알 수 있듯이, 본 발명에 따른 화장료 조성물과 종래 기술로 제조된 화장품에 비해서, 비타민 C의 역가는 비교적 안정적임을 확일할 수 있었다. 따라서 본 발명에 따른 조성물은 종래 기술의 조성물보다 더욱 안정한 조성물임을 알 수 있다.
As can be seen from Table 5, the reversibility of vitamin C was relatively stable compared to the cosmetic composition according to the present invention and the cosmetics prepared according to the prior art. Therefore, it can be seen that the composition according to the present invention is a more stable composition than the composition of the prior art.

<조성물의 안정성 시험: 변색, &Lt; Stability test of composition: Discoloration, 변취Fling >>

상기 실시예에서 표 2와 표 3에 따라 제조된 조성물에 대하여 제형 안정성을 알아보기 위해 45℃로 일정하게 유지되는 항온조에서 불투명 초자 용기에 담아 12주 동안 보관하고, 또한 4℃로 일정하게 유지되는 완전히 차광된 냉장고 내에서 불투명 초자 용기에 담아 12주 동안 보관한 후, 변색 및 변취 정도를 비교 측정하였다. 그 결과는 하기 표 6에 나타냈다.The compositions prepared according to Tables 2 and 3 in the above Examples were stored in an opaque glass container in a thermostat kept constant at 45 DEG C for 12 weeks and kept at 4 DEG C In a completely shaded refrigerator, it was stored in an opaque glazed container for 12 weeks. The results are shown in Table 6 below.

이때, 제품 변색 및 변취 정도는 다음의 6등급으로 분류하여 평가하였다.At this time, the degree of product discoloration and degree of detachment was classified into the following six grades and evaluated.

0 : 변화없음 1 : 극히 조금 0: No change 1: Extremely small

2 : 조금 3 : 조금 심하게 2: a little bit 3: a bit badly

4 : 심하게 5 : 극히 심하게 4: Severely 5: Extremely severe

변색discoloration 변취Fling
샘플 1

Sample 1
45℃45 ° C 0.10.1 0.150.15
4℃4 00 00
샘플 2

Sample 2
45℃45 ° C 0.10.1 0.150.15
4℃4 00 00
샘플 3

Sample 3
45℃45 ° C 0.10.1 0.10.1
4℃4 00 00
비교 샘플 1

Comparative Sample 1
45℃45 ° C 33 44
4℃4 ℃ 1One 22
비교 샘플 2

Comparative Sample 2
45℃45 ° C 55 44
4℃4 ℃ 22 22

상기 표 6에 나타난 바와 같이, 본 발명은 종래의 기술에 따른 화장료 조성물 보다 45℃에서 변색이나 변취 현상이 거의 없음을 알 수 있었다. 따라서 종래 기술의 화장료 조성물보더 더욱 안정한 조성물임을 알 수 있다.As shown in Table 6, it was found that the present invention has almost no discoloration or detachment phenomenon at 45 ° C as compared with the cosmetic composition according to the prior art. Therefore, it can be understood that the composition of the prior art cosmetic composition is more stable composition.

이상에서 살펴본 바와 같이 본 발명에 따른 조성물을 비타민 C를 15 내지 25중량%까지 충분히 용해시킬 수 있으면서도 피부 투과율이 높으면서도 화학적 안정성까지도 뛰어난 조성물임을 알 수 있다.As described above, it can be seen that the composition according to the present invention can dissolve vitamin C in an amount of 15 to 25% by weight, and is superior in chemical stability even when the skin permeability is high.

Claims (4)

비타민 C를 프로판디올, 펜틸렌글라이콜, 부틸렌글라이콜, 디에톡시에칠석시네이트, 디메칠이소소바이드, 비스-에톡시디글라이콜 사이클로헥산1,4-디카복실레이트 및 페퍼민트오일을 배합한 혼합 용매에 용해시킨 활성성분으로 비타민 C를 포함하는 화장료 조성물.
Vitamin C may be formulated with propanediol, pentaerythritol, butyleneglycol, diethoxylated monostearate, dimethicone isobarbide, bis-ethoxydiglycol cyclohexane 1,4-dicarboxylate and peppermint oil A cosmetic composition comprising vitamin C as an active ingredient dissolved in a mixed solvent.
제 1항에 있어서, 조성물 전체에 대하여 상기 비타민 C가 15 내지 25중량% 함유되며, 잔부는 혼합 용매인 것을 특징으로 활성성분으로 비타민 C를 포함하는 화장료 조성물.
The cosmetic composition according to claim 1, wherein the composition contains vitamin C in an amount of 15 to 25% by weight and the balance is a mixed solvent.
제 1항 또는 제 2항에 있어서, 상기 혼합 용매는 프로판디올 60 ~ 70중량%, 펜틸렌글라이콜 10 ~ 20중량%, 부틸렌글라이콜 5.0 ~ 15중량%, 디에톡시에칠석시네이트 2.5 ~ 7.5중량%, 디메칠이소소바이드 1.0 ~ 4.0중량%, 비스-에톡시디글라이콜 사이클로헥산1,4-디카복실레이트 1.0 ~ 3.0중량%, 페퍼민트오일 0.05 ~ 0.15중량%로 구성되는 것을 특징으로 하는 활성성분으로 비타민 C를 포함하는 화장료 조성물.
The method according to claim 1 or 2, wherein the mixed solvent comprises 60 to 70% by weight of propanediol, 10 to 20% by weight of pentylene glycol, 5.0 to 15% by weight of butyleneglycol, , 1.0 to 4.0% by weight of dimethicone isobaride, 1.0 to 3.0% by weight of bis-ethoxydiglycolcyclohexane 1,4-dicarboxylate, and 0.05 to 0.15% by weight of peppermint oil. And vitamin C as an active ingredient.
제 3항에 있어서, 상기 혼합 용매는 프로판디올 66.6중량%, 펜틸렌글라이콜 14중량%, 부틸렌글라이콜 10중량%, 디에톡시에칠석시네이트 5중량%, 디메칠이소소바이드 2.3중량%, 비스-에톡시디글라이콜 사이클로헥산1,4-디카복실레이트 2중량%, 페퍼민트오일 0.1중량%로 구성되는 것을 특징으로 하는 활성성분으로 비타민 C를 포함하는 화장료 조성물.4. The method according to claim 3, wherein the mixed solvent comprises 66.6% by weight of propanediol, 14% by weight of pentylene glycol, 10% by weight of butylene glycol, 5% by weight of diethoxy-terephthalic acid, 2.3% , Bis-ethoxydiglycol cyclohexane 1,4-dicarboxylate 2% by weight, and peppermint oil 0.1% by weight.
KR1020140134457A 2014-10-06 2014-10-06 Stable non-epispastic vitamin C cosmetic composition having high skin-transmissivity KR101610246B1 (en)

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Publication number Priority date Publication date Assignee Title
KR102035260B1 (en) * 2018-04-26 2019-10-22 (주)뷰애드 Stable non-epispastic vitamin C cosmetic composition having high skin-transmissivity

Citations (1)

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KR100425260B1 (en) 1999-01-09 2004-03-30 한국콜마 주식회사 Functional Cosmetic Compound of Powder type

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100425260B1 (en) 1999-01-09 2004-03-30 한국콜마 주식회사 Functional Cosmetic Compound of Powder type

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102035260B1 (en) * 2018-04-26 2019-10-22 (주)뷰애드 Stable non-epispastic vitamin C cosmetic composition having high skin-transmissivity

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