KR20060113612A - Cosmetic composition with high concentration of stable pure vitamin c in aqueous system - Google Patents
Cosmetic composition with high concentration of stable pure vitamin c in aqueous system Download PDFInfo
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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
- A61K8/04—Dispersions; Emulsions
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
- A61K8/65—Collagen; Gelatin; Keratin; Derivatives or degradation products thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/67—Vitamins
- A61K8/676—Ascorbic acid, i.e. vitamin C
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- A61K8/00—Cosmetics or similar toiletry preparations
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- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
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- 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
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Abstract
Description
본 발명은 수계에서도 안정한 고농도 순수 비타민 C를 함유한 유화 화장료 조성물에 관한 것으로 비타민 C는 대표적인 수용성 비타민으로 피부, 혈액 및 조직에서 강력한 생체 항산화제로 생체 내에서 반응성이 높은 활성산소, 자유 라디칼등의 과산화물에 의해 산화되는 것을 차단하여 피부 노화를 방지하는 항산화 작용을 갖고 있다. 또한 비타민 C는 인체의 면역기능을 높여주고, 피부, 연골, 모세혈관, 근육 등의 구성요소인 콜라겐(Collagen)의 생성을 촉진하여 주름을 방지하고 건강하게 피부를 유지시키며 상처난 피부조직의 재생을 돕고 알레르기 반응을 일으키는 것으로 알려진 히스타민(Histamin)형성 촉진시켜 주는 역할도 한다.The present invention relates to an emulsified cosmetic composition containing a high concentration of pure vitamin C, which is stable even in aquatic systems. Vitamin C is a representative water-soluble vitamin and is a powerful bio-oxidant in skin, blood, and tissues. It has an antioxidant action that prevents skin aging by blocking the oxidation by. In addition, vitamin C enhances the body's immune function, promotes the production of collagen, which is a component of skin, cartilage, capillaries, and muscles, prevents wrinkles, maintains healthy skin, and regenerates damaged skin tissue. It also helps to promote the formation of histamine, known to cause allergic reactions.
비타민 C에 의한 간접적인 자외선 차단 효과를 가지고 있는데 기존의 자외선 차단제와는 같이 자외선을 직접 흡수하는 기능은 없으나 UVB에 의해 유발되는 홍반 및 부종을 충분히 감소시켜주는 작용을 갖고 있다. It has an indirect sunscreen effect by vitamin C. Like conventional sunscreens, it does not absorb UV light directly, but it has a function of sufficiently reducing erythema and edema caused by UVB.
또한, 비타민 C는 피부 내 멜라닌 형성의 주요 효소인 타이로시나제 활성을 억제하고, 산화 과정에 의해 형성된 산화형 멜라닌을 다시 환원시켜 환원형멜라닌으로 변화시킴으로써 피부 색소 침착증을 개선시키는 효과를 가지고 있다.In addition, vitamin C has an effect of improving skin pigmentation by inhibiting tyrosinase activity, which is a major enzyme of melanin formation in the skin, and reducing oxidized melanin formed by oxidation to reduce melanin. .
상기의 이러한 여러 생물학적 기능을 갖고 있는 비타민 C는 일단 피부내로 흡수되면 저장되는 효능이 있어서 사용을 중단해도 장시간 그 효능이 유지되는 장점이 있다.Vitamin C having these various biological functions has the advantage of being stored once absorbed into the skin, thus maintaining its efficacy for a long time even after discontinuing use.
그러나, 비타민 C는 감마-락톤과 유사한 구조로 매우 불안정하여 공기, 특히 산소, 열 및 빛과 같은 외부환경에 민감하게 반응하여 쉽게 분해 되는 문제점이 있다. 이와 같은 현상은 주로 비타민 C의 산화반응으로 전자전이과정(Electron transfer process)인 수소 이온이 해리되어 탈수소-L-아스코르빈산(Dehydro-L-ascorbic acid)형태로 라디칼로 쉽게 산화되는 당 유사구조(Sugar like structure)를 갖고 있기 때문이다. 비수용액 중에서는 극소량이 용해되는 반면 수용액 중에서는 많은 양이 용해되지만 빠른 산화 작용으로 인해 충분한 양의 비타민 C가 안정화 되지 못하기 때문에 의약, 식품, 화장품 등에서 소량 사용되고 있거나 또는 비수계 시스템(Non-aqueous system)에서 사용되고 있는 실정이다.However, vitamin C has a problem in that it is very unstable in a structure similar to gamma-lactone and is easily decomposed by being sensitive to air, particularly oxygen, heat, and external environment such as light. This phenomenon is mainly due to the oxidation reaction of vitamin C, the sugar-like structure that is easily oxidized to radical in the form of dehydro-L-ascorbic acid by dissociating hydrogen ions which are electron transfer process. (Sugar like structure). Very small amount is dissolved in the non-aqueous solution, while a large amount is dissolved in the aqueous solution, but a sufficient amount of vitamin C cannot be stabilized due to the rapid oxidation, and thus a small amount is used in medicine, food, cosmetics, or a non-aqueous system. system).
대한민국특허 등록번호 제 10-158102호에서는 글루코실 L-아스코르빈산 유도체로 합성하여 안정화하였고, 대한민국특허 등록번호 제 10-230653호에서는 L-아스코르빈산과 3-아미노프로판인산을 반응시킨 유도체로 안정화한 특허등이 있으며, 대한민국특허 공개번호 제 10-2002-23574에서는 다가알콜을 사용하여 비타민 C를 용해한 후 오일상과 유화한 유중다가알콜형 비수계 에멀젼을 미국특허 제4,983,382호에서는 물과 에탄올 등 유기용매를 매질로서 함께 사용하는 방법을, 미국특허 제 5,981,578호에서는 아스코르빈산을 포함하는 비수성 용액과 물을 함유하는 화장수나 로션 등 다른 제품을 동시 적용하는 방법을 기재하였다.In Korean Patent Registration No. 10-158102, it was synthesized and stabilized with a glucosyl L-ascorbic acid derivative. In Korean Patent Registration No. 10-230653, a derivative obtained by reacting L-ascorbic acid and 3-aminopropane acid. In Korea Patent Publication No. 10-2002-23574, a water-soluble polyhydric alcohol-type non-aqueous emulsion that is dissolved in vitamin C using polyhydric alcohol and then emulsified in water and ethanol is disclosed in US Patent No. 4,983,382. A method of using an organic solvent together as a medium, US Patent No. 5,981,578 describes a method of simultaneously applying a non-aqueous solution containing ascorbic acid and other products such as a lotion or lotion containing water.
그러나, 상기 특허에서는 사용하는 비타민 C의 유도체인 경우 피부 흡수문제와 활성부분의 가수분해의 어려움 등이 있어 생리활성면에서 순수 비타민 C 자체에 비해 미약하고, 비수계 형태의 제형의 경우 경피흡수의 어려움으로 인해 피부 전달과정이 비효율적이어서 효과 발현의 효율성이 낮고 사용성면에서 끈적임이 많이 남는 단점이 있다.However, in the patent, the derivative of vitamin C used has a problem of skin absorption and difficulty in hydrolysis of the active part, so that it is weaker than pure vitamin C in terms of physiological activity. Due to the difficulty, the skin delivery process is inefficient, resulting in low efficiency of expression and stickiness in usability.
본 발명은 일반적인 화장료 유화물과 같은 우수한 사용감을 가지면서 장기간 안정한 순수비타민 C를 함유한 유화물로 상기된 문제점들을 극복하였다.The present invention overcomes the problems described above with emulsions containing pure vitamin C, which are stable over a long period of time with excellent usability, such as common cosmetic emulsions.
또한 일반적인 유중수형에멀젼의 특징인 피부 안전성과 피부 흡수가 우수하한 장점을 가지고 있다.In addition, it has the advantages of excellent skin safety and skin absorption, which are characteristic of general water-in-oil emulsions.
본 발명자들은 열이나 빛, 산소등에 매우 불안정하여 대기중에 변색,변취가 발생하여 피부 안전성 및 제형 안정성의 문제가 발생되고 역가가 급격히 감소되는 문제점을 갖고 있는 비타민 C의 안정성 문제를 고농도가 함유된 수계(aqueous system)에서 안정화하여 상기의 문제점들과 피부 도포시 끈적임이 없는 사용감이 우수한 화장료을 개발할 수 있었다. 따라서, 본 발명은 수계(Aqueous system)에서 안정하면서도 고농도 순수 비타민 C 함유한 화장료 조성을 제공하는 것이다.The present inventors are very unstable to heat, light, oxygen, etc., causing discoloration and discoloration in the air, causing problems of skin safety and formulation stability, and the stability problem of vitamin C, which has a problem in that the titer is drastically reduced. By stabilizing in an (aqueous system) it was possible to develop a cosmetic excellent in the above problems and a feeling of non-sticky when applying skin. Accordingly, the present invention is to provide a cosmetic composition containing a high concentration of pure vitamin C while being stable in an aqueous system.
본 발명은 순수 비타민 C 3~20 중량%, 극성용매 0.5~20중량%,계면활성제 0.1~10중량%,실리콘오일 0.1~30중량% 및 기타 첨가물과 물과 이루어지는 수계 유화 화장료 조성물을 제공하고자 한다.The present invention is to provide an aqueous emulsion cosmetic composition consisting of 3 to 20% by weight of pure vitamin C, 0.5 to 20% by weight of a polar solvent, 0.1 to 10% by weight of surfactant, 0.1 to 30% by weight of silicone oil and other additives and water. .
본 발명의 화장료 조성물은 순수 비타민C를 고농도로 안정화시킨 베이스를 친수파트에 첨가함으로써 안정한 수계 유화 제형을 제조함을 특징으로 한다.The cosmetic composition of the present invention is characterized in that a stable aqueous emulsion formulation is prepared by adding a base stabilized at a high concentration of pure vitamin C to a hydrophilic part.
본 발명의 화장료 조성물에 사용되는 비타민C는 피부를 맑고, 깨끗하게 해주며, 화장료 조성물 총중량에 대하여 3~20중량% 포함한다. 만일 비타민C가 20중량%를 초과하면 낮은 pH로 인해 박피 현상 등의 피부 자극이 우려되고, 3중량% 미만이면 피부개선효과가 적다.Vitamin C used in the cosmetic composition of the present invention is clear and clean skin, and contains 3 to 20% by weight based on the total weight of the cosmetic composition. If the vitamin C exceeds 20% by weight, skin irritation such as peeling phenomenon is concerned due to the low pH, and less than 3% by weight of the skin improvement effect is less.
< 실험예 1> : 안정한 고농도 비타민C 베이스 제조Experimental Example 1 Preparation of Stable High Concentration Vitamin C Base
구체적인 제조 예는 다음과 같다.Specific manufacturing examples are as follows.
하기 표1과 같은 조성으로 실온에서 L-Ascorbic Acid 20중량%, 기타 첨가제, 히아루론산나트륨(1%)3.0중량%를 정제수에 아지믹서로 혼합하여 용해시킨 후 Sodium Hydroxide(20%) 3.5중량%를 서서히 투입하면서 혼합시킨다.20 wt% L-Ascorbic Acid, other additives, and 3.0% by weight of sodium hyaluronate (1%) at room temperature with a composition as shown in Table 1 were dissolved by mixing in purified water with an azimixer and 3.5 wt% of Sodium Hydroxide (20%). Mix slowly while adding.
실시 예 1~2의 화장료 조성물의 조성비는 중량%이다.The composition ratio of the cosmetic composition of Examples 1-2 is weight%.
상기 실시 예1~2를 실온, 37℃, 45℃,일광에서 보관 후 변색, 변취안정성 및 HPLC를 이용하여 순수 비타민 C 잔존율을 측정하여 (표 2)와(표 3)에 나타내었다. Examples 1 and 2 were stored at room temperature, 37 ° C., 45 ° C., daylight, and measured pure vitamin C residual ratios using discoloration, odor stability, and HPLC, and are shown in Tables 2 and 3.
변색, 변취 안정성 결과( 변색, 변취 없음 : ○, 변색, 변취 : X) Discoloration, deodorant stability results (discoloration, no odor: ○, discoloration, odor: X)
L-Ascorbic Acid (비타민 C)잔존율 측정 Residual L-Ascorbic Acid (Vitamin C)
L-Ascorbic Acid(비타민 C)의 산화안정성을 보다 정확히 조사하기 위해 상기 실험에1에서 제조한 조성물을 실온, 항온조(37℃,45℃),일광에서 경시변화에 따른 L-Ascorbic Acid의 잔존율을 HPLC로 측정하였다. In order to more accurately investigate the oxidation stability of L-Ascorbic Acid (Vitamin C), the composition prepared in the above Experiment 1 was subjected to the residual rate of L-Ascorbic Acid according to the change over time in room temperature, thermostat (37 ℃, 45 ℃) and sunlight. Was measured by HPLC.
HPLC에 의한 L-Ascorbic Acid의 정량분석 조건은 칼럼은 Phenomenex 00G-4252-EO Luan 5u C18(2) 100A(size 250 *4.60 mm)을 사용하였으며 상기 실시 예에서 준비한 샘플 용액 20㎕를 유속 0.7㎖/min으로 240nm의 자외선 흡광광도계 조건에서 검출하였다. 또한 이동상은 0.025M 인산수소칼륨용액(pH 2.5)을 사용하였다.As a column for quantitative analysis of L-Ascorbic Acid by HPLC, Phenomenex 00G-4252-EO Luan 5u C18 (2) 100A (size 250 * 4.60 mm) was used. It was detected at 240 nm ultraviolet absorbance spectrometer at / min. In addition, 0.025 M potassium hydrogen phosphate solution (pH 2.5) was used for the mobile phase.
(표 2),(표 3)에서 나타낸 바와 같이 본 발명의 실시 예 1,2를 비교하여 보면 실시 예 1이 가혹 조건에서도 변색, 변취가 발생하지 않았으며, 비타민 C 잔존율에서도 실시 예2에 비해 높은 잔존율을 보이고 있으며, 기능성화장품법상에서 요구하는 안정성 기준(95%이상)보다도 높은 결과를 보이고 있다. As shown in Table 2 and Table 3, when comparing Examples 1 and 2 of the present invention, Example 1 did not cause discoloration and discoloration even under severe conditions, and in Example 2 in vitamin C residual ratio, It shows a higher residual rate than the stability standard (95% or more) required by the functional cosmetics law.
이런 안정한 실시 예1을 이용하여 대표적인 제형인 크림 및 스킨 제형에서의 변색, 변취 및 L-Ascorbic Acid잔존율을 경시 및 온도 등의 조건에 따른 실험결과는 다음과 같다.Experimental results of discoloration, discoloration, and L-Ascorbic Acid residual ratio in the cream and skin formulations, which are representative formulations, according to the stabilization and temperature, are as follows.
<실험 예 2> 비타민C 3% 함유 크림 및 유연화장수 제조Experimental Example 2 Preparation of Cream and Soft Cosmetics Containing 3% of Vitamin C
상기 제형 예 1은 유중수형에멀젼타입의 크림 조성으로 제조방법은 다음과 같다. 오일파트와 물파트를 각각 80℃까지 온도를 상승시켜 균일하게 용해시킨 후 물파트를 오일파트에 천천히 부어주면서 혼합한 후 원하는 점도를 형성시킨 다음 실온까지 냉각시켜 제조한다.Formulation Example 1 is a water-in-oil emulsion type cream composition is as follows. The oil parts and the water parts are heated to 80 ° C., respectively, to be uniformly dissolved, and then the water parts are slowly poured into the oil parts, mixed and mixed to form a desired viscosity, followed by cooling to room temperature.
상기 제형 예 2는 물파트와 알콜파트의 각 성분을 용해시킨 후 알콜파트를 물파트에 서서히 투입하면서 혼합 믹싱한 다음 실시 예 1을 최종 첨가하여 제조한다.Formulation Example 2 is prepared by dissolving each component of the water part and the alcohol part and mixing and mixing the alcohol part into the water part gradually, followed by the final addition of Example 1.
(표 4)제형 예 1,2의 변색, 변취 안정성 결과Table 4 Discoloration and malodor stability results of Formulation Examples 1 and 2
(변색, 변취 없음 : ○ 변색, 변취 : X) (Discoloration, no odor: ○ discoloration, odor: X)
(표 5) 제형 예 1,2의 L-Ascorbic Acid(비타민 C) 잔존율 측정 Table 5 Measurement of L-Ascorbic Acid (Vitamin C) Retention Rate of Formulation Examples 1,2
상기 (표 4)및 (표 5)에서 나타낸 바와 같이 본 발명의 제형 예 1,2 모두 가혹 조건에서도 변색, 변취가 발생하지 않았으며, 비타민 C 잔존율에서도 실시 예2에 비해 높은 잔존율을 보이고 있으며, 기능성화장품법상에서 요구하는 안정성 기준(95%이상)보다도 높은 결과를 보이고 있다.As shown in (Table 4) and (Table 5), the formulation examples 1 and 2 of the present invention did not discolor or deteriorate even under severe conditions, and showed a higher residual rate in the vitamin C residual rate than Example 2. The results are higher than the stability criteria (95% or more) required by the Functional Cosmetics Act.
(표 4)와(표 5)에서의 실험조건은 (표 2)와 (표 3)에서 시행한 조건과 동일한 조건에서 실험하였다.Experimental conditions in (Table 4) and (Table 5) were tested under the same conditions as in (Table 2) and (Table 3).
<실험 예 3> 피부자극도 측정Experimental Example 3 Measurement of Skin Irritability
건강한 남녀 실험자 50명의 팔 하박부에 상기 각 실시예의 시료를 폐쇄 첩포 시험 방법에 따라, 1일 1회씩 도포 후 외부와의 차단을 위해 플라스틱 캡을 씌운 다음 1일 후, 3일 후, 7일 후에 다음의 판정 방법에 따라 자극 정도를 관찰하였다. 자극 정도의 판단 기준은 하기 (표 6)에 나타나 있다.50 healthy male and female experimenters applied the samples of each of the above examples to the lower arm of the arm under the closed patch test method, and then covered with a plastic cap for blocking from the outside once a day, then 1 day, 3 days, and 7 days later. The degree of stimulation was observed according to the following judgment method. Criteria for the degree of stimulation are shown in Table 6 below.
각 피험자의 자극 정도를 측정한 후 피험자의 수로 나누어 그 평균 자극 정도를 계산하였다. 하기 (표 7)에 나타난 결과는 상기의 판정 방법에 의해 산출된 자극의 평균치이다.The stimulus degree of each subject was measured, and the average stimulus degree was calculated by dividing by the number of subjects. The result shown in following (Table 7) is an average value of the stimulus computed by the said determination method.
상기 제형 예 1과 제형 예 2의 전 시료에 있어 피부 자극은 없음을 알 수 있다. 이러한 결과는 본 발명에서 제공되는 비타민C 3% 함유 일반제형에서도 피부자극이 거의 없는 상태에서 제형화가 가능함을 확인해 주는 결과이다. It can be seen that there is no skin irritation in all samples of Formulation Example 1 and Formulation Example 2. This result is a result confirming that the formulation can be provided in a state with almost no skin irritation even in the general formulation containing 3% vitamin C provided in the present invention.
이상에서 본 발명의 실험 예, 제형 예를 살펴보았다.The experimental examples, formulation examples of the present invention have been described above.
이상에서 볼 수 있는 바와 같이, 본 발명에 의해 제공되는 비타민 C안정화 방법이 물이 80%이상 함유된 수계(Aqueous System)에서 물리화학적으로 안정한 상태를 장기간 유지하는 특징이 있으며, 특히, 일반 제형에서 피부 자극 없이 안전하게 사용할 수 있다는 장점이 있다.As can be seen from the above, the vitamin C stabilization method provided by the present invention is characterized by maintaining a long period of physicochemically stable state in an aqueous system containing 80% or more of water. It can be used safely without skin irritation.
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