KR890001694B1 - Process for preparing emulsion of microcrystalline ascorbic fatty acid ester pearl and its preparation - Google Patents
Process for preparing emulsion of microcrystalline ascorbic fatty acid ester pearl and its preparation Download PDFInfo
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- KR890001694B1 KR890001694B1 KR1019860004191A KR860004191A KR890001694B1 KR 890001694 B1 KR890001694 B1 KR 890001694B1 KR 1019860004191 A KR1019860004191 A KR 1019860004191A KR 860004191 A KR860004191 A KR 860004191A KR 890001694 B1 KR890001694 B1 KR 890001694B1
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- ascorbyl
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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
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/37—Esters of carboxylic acids
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- 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
Abstract
Description
본 발명은 아스코르빌팔미테이트, 아스코르빌스테아레이트, 아스코르빌디팔미테이트등의 아스코르빌지방산에스텔을 미세결정화한 펄 유화액의 제조방법 및 이를 이용한 펄효과가 있는 액상 화장료에 관한 것이다.The present invention relates to a method for preparing a pearl emulsion obtained by microcrystallization of ascorbyl fatty acid esters such as ascorbyl palmitate, ascorbyl stearate, ascorbyl dipalmitate, and a liquid cosmetic having a pearl effect using the same.
이를 좀더 상세히 설명하면, 폴리옥시에칠렌소르비탄스테아레이트, 폴리옥시에칠렌세틸에텔, 폴리옥시에칠렌경화피마자유, 폴리옥시에칠렌스테아레이트, 폴리옥시에틸렌콜레스테롤에텔, 소디움라우릴설페이트, 소디움라우릴에텔설페이트등의 에이취.엘.비(Hydrophilic Lipophilic Balance)가 10 이상인 계면활성제 0.2-5.0% 수용액에 아스코르빌지방산에스텔을 0.2-5.0% 가하고, 이를 60-90℃로 가열 용해시킨 다음 냉각하면 일정온도에서 아스코르빌지방산에스텔과 계면활성제로 형성된 젤이 형성된다. 이를 더욱 냉각하면 아스코르빌지방산에스텔은 펄효과가 있는 미세결정의 유화액이 된다. 이때 아스코르빌지방산에스텔의 안정화를 위하여 구연산, 호박산, 젖산등을 가하여 pH 3.5-6.5로 조정하고, 또 에칠렌디아민테트라초산나트륨, 메타인산나트륨등의 킬레이트제 0.005-0.2%, 아황산수소나트륨, 몰식자산프로필등의 수용성 항산화제를 0.01-0.1%를 가한다. 이렇게 만들어진 아스코르빌지방산에스텔의 펄을 이용하여 일반적인 수용성 상태의 화장품에 첨가하면 펄효과가 있는 제품을 만들수 있다.In more detail, polyoxyethylene sorbitan stearate, polyoxy ethylene cetyl ether, polyoxy ethylene hardened castor oil, polyoxy ethylene stearate, polyoxyethylene cholesterol ether, sodium lauryl sulfate, sodium lauryl ether sulfate, etc. 0.2-5.0% of ascorbyl fatty acid ester was added to a 0.2-5.0% aqueous solution of H.H.B. (Hydrophilic Lipophilic Balance) of 10 or more. Gels formed from corville fatty acid esters and surfactants are formed. When this is further cooled down, ascorbyl fatty acid ester becomes an emulsion of fine crystals having a pearl effect. At this time, to stabilize the ascorbyl fatty acid ester, add citric acid, succinic acid, and lactic acid to adjust the pH to 3.5-6.5, and chelating agents 0.005-0.2% of sodium ethylenediaminetetraacetate, sodium metaphosphate, sodium hydrogen sulfite, molar asset 0.01-0.1% of water-soluble antioxidants such as propyl are added. The pearls of ascorbyl fatty acid ester made in this way can be added to general water-soluble cosmetics to make products with a pearl effect.
일반적으로 펄은 그 외관이 독특하고 미려하므로 화장품등에 널리 응용되고 있으며 여기에 사용되는 물질로는 운모티탄류의 합성펄이나, 구아닌등의 천연펄 또는 지방산류를 결정화시켜 사용하고 있다. 그러나 운모티탄류의 합성펄은 펄의 안정성과 펄효과는 우수하지만 비중이 크기 때문에 고점성을 갖는 제품외에는 사용하기 어려우며 구아닌 펄은 가격이 비싸고 또 일정크기의 펄입자를 분리하기 힘들며 지방산류 결정펄은 시간경과에 따라 결정입자가 커져 안정화가 힘들고 또 펄효과가 그다지 우수하지 못하다는 단점이 있다.In general, since pearls are unique and beautiful in appearance, they are widely used in cosmetics and the like. The materials used therein are crystallized synthetic pearls of mica titanium, natural pearls such as guanine, or fatty acids. However, synthetic pearls of mica titanium have excellent pearl stability and pearl effect, but because they have high specific gravity, they are difficult to use except for products with high viscosity.Guanine pearls are expensive and difficult to separate pearl particles of a certain size. The disadvantage is that the crystal grains become larger with time and stabilization is difficult and the pearl effect is not so good.
그러나, 본 발명에 의하여 아스코르빌지방산에스텔로 제조된 미세결정 형태의 펄은 그 펄효과가 우수할 뿐만 아니라 시간경과에 따라 결정 성장속도가 느려 안정할 뿐 아니라 보다 중요한 것은 아스코르빈산 유도체를 미세결정화시켜 사용함으로써 수동액에서 안정화시킬 수 있으며, 또 많은 양을 사용할 수 있다는 잇점이 있다.However, the pearl of the microcrystalline form made of ascorbyl fatty acid ester according to the present invention not only has excellent pearl effect, but also slows down the crystal growth rate over time, and more importantly, fine ascorbic acid derivatives are fine. By crystallization and use, it can be stabilized in a passive liquid, and there is an advantage in that a large amount can be used.
아스코르빈산 지방산에스텔은 화장품등에서 피부 미백효과 및 기미 제거등의 멜라닌 색소 침착방지에 효과가 있는데, 이것은 아스코르빈산이 강한 환원성 물질로서 피부의 멜라닌 생성 억제작용이 있기 때문인 것으로 알려져 있다. 그러나 아스코르빈산은 수용액에서 안정성이 나빠 분해되기 쉽고 또 피부흡수가 거의 되지 않으므로 화장품등 피부의용제로 사용될 경우 아스코르빈산에 지방산을 가하여 에스텔화시킨 아스코르빌지방산에스텔이 주로 사용되고 있다. 그러나, 아스코르빌지방산에스텔은 물에 대한 용해성이 극히 나쁘고 또 오일류에도 용해성이 나쁜 단점이 있다. 그리고 수용액에서 안정성이 아스코르빈산 보다는 양호하지만 이것 역시 강한 환원성 물질로서 안정성이 나쁘므로 분말자체로 사용하는 경우외에는 화장품에 첨가할 경우에는 그 사용량이 크게 제한되며 특히 화장수나 팩류등에는 물에 대한 용해성이 극히 나빠 아주 소량밖에 첨가할 수 없었다.Ascorbic acid fatty acid ester is effective in preventing melanin pigmentation, such as skin whitening effect and blemish removal in cosmetics, etc. This is because ascorbic acid is a strong reducing substance and is known to have melanin production inhibitory effect on the skin. However, ascorbic acid has poor stability in aqueous solution and is easily decomposed and almost no skin absorption. Therefore, ascorbyl fatty acid ester which is esterified by adding fatty acid to ascorbic acid when used as a skin solvent such as cosmetics is mainly used. However, ascorbyl fatty acid ester has disadvantages of extremely poor solubility in water and poor solubility in oils. In addition, its stability in aqueous solution is better than that of ascorbic acid, but it is also a strong reducing substance, and its stability is poor. Therefore, its use is greatly limited when added to cosmetics, except when used as powder itself. It was so bad that only a very small amount could be added.
그러나 본 발명자는 에이취.엘.비가 10 이상인 계면활성제를 이용하여 아스코르빌지방산에스텔을 물에 일단 용해시킨 다음 이를 냉각하여 미세결정상으로 만듬으로써 아스코르빌지방산에스텔을 수용액에서 고체상으로 존재하게 함으로써 안정성을 증가시킬 수 있었으며 아울러 이 미세결정은 펄효과가 우수하며 우수한 펄효과를 갖는 화장품을 만들수 있었다. 그리고 아스코르빌지방산에스텔 자체를 펄로 사용함으로서 화장품에 그 첨가량을 증가시킬 수 있었다. 즉, 수용액에서 안정성이 나쁜 아스코르빌지방산에스텔을 펄로 만듬으로써 안정성과 첨가량을 증가시키고 또 펄효과도 갖는 제품을 만들 수 있다.However, the present inventors dissolve the ascorbyl fatty acid ester in water using a surfactant having an H.L. ratio of 10 or more, and then cool it to form a microcrystalline phase, thereby making the ascorbyl fatty acid ester exist in a solid state in an aqueous solution. In addition, the microcrystals were able to make cosmetics with excellent pearl effect and excellent pearl effect. In addition, ascorbyl fatty acid ester itself was used as a pearl to increase the amount of cosmetics added. That is, by making pearl of ascorbyl fatty acid ester having poor stability in aqueous solution, it is possible to make a product having increased stability and addition amount and also having a pearl effect.
[실시예 1]Example 1
물 90중량부(이하부는 중량부임)에 아스코르빌팔미테이트 3.0부 폴리옥시에칠렌경화피마자유 2.5부 에칠렌디아민테트라 초산나트륨 0.02부, 아황산수소나트륨 0.03부, 파라옥시안식향산메칠 0.3부를 가하고 교반한후 구연산으로 pH를 3.5로 조절하고, 전체가 100부가 되게 물을 가하고 60℃로 가열교반하여 용액으로 한다음 실온까지 서서히 냉각하여 미세결정의 아스코르빌팔미테이트 펄 유화액을 제조하였다.To 90 parts by weight of water (hereinafter referred to as parts by weight), 3.0 parts of ascorbyl palmitate, 3.0 parts of polyoxyethylene hardened castor oil, 2.5 parts of ethylenediaminetetrasodium acetate, 0.03 parts of sodium bisulfite, and 0.3 parts of paraoxybenzoic acid methyl were added, followed by stirring. The pH was adjusted to 3.5 with citric acid, water was added to 100 parts in total, and stirred at 60 ° C. to make a solution, followed by cooling slowly to room temperature to prepare microcrystalline ascorbyl palmitate pearl emulsion.
[실시예 2]Example 2
물 90부에 아스코르빌디팔미테이트 1.0부, 폴리옥시에칠렌스테아레이트 0.7부, 에칠렌디아민테트라초산나트륨 0.007부, 아황산수소나트륨 0.05부, 파라옥시안식향산메칠 0.2부를 가하고 교반한 후 구연산으로 pH를 4.5로 조절하고 전체가 100부가 되게 물을 가하고 70℃로 가열 교반하여 용해시킨 다음 실온까지 서서히 냉각하여 미세결정의 아스코르빌디팔미테이트 펄 유화액을 제조하였다.To 90 parts of water, 1.0 part of ascorbyl dipalmitate, 0.7 parts of polyoxyethylene stearate, 0.007 parts of sodium ethylenediaminetetraacetate, 0.05 parts of sodium bisulfite, 0.2 parts of methyl paraoxybenzoate are stirred, and the pH is adjusted to 4.5 with citric acid. Water was added to adjust the total amount to 100 parts, dissolved by heating and stirring at 70 ° C., and then slowly cooled to room temperature to prepare a microcrystalline ascorbyl dipalmitate pearl emulsion.
[실시예 3]Example 3
물 90부에 아스코르빌스테아레이트 3.0부, 폴리옥시에틸렌소르비탄스테아레이트 3.0부, 메타인산나트륨 0.01부, 아황산수소나트륨 0.07부, 파라옥시안식향산메칠 0.15부를 가하고 교반한 후 젖산으로 pH를 5.5로 조절하고 전체가 100부가 되게 물을 가하고 80℃로 가열교반하여 용액으로한 다음 실온까지 서서히 냉각하여 미세결정의 아스코르빌스테아레이트 펄 유화액을 제조하였다.To 90 parts of water, add 3.0 parts of ascorbyl stearate, 3.0 parts of polyoxyethylene sorbitan stearate, 0.01 part of sodium metaphosphate, 0.07 part of sodium hydrogen sulfite, 0.15 part of methyl paraoxybenzoate and stir to pH 5.5 with lactic acid. Water was added to adjust the total amount to 100 parts, and the mixture was heated and stirred at 80 ° C. to prepare a solution, and then cooled slowly to room temperature to prepare a microcrystalline ascorbyl stearate pearl emulsion.
[실시예 4]Example 4
물 90부에 아스코르빌팔미테이트 2.0부, 아스코르빌스테아레이트 2.0부, 폴리옥시에칠렌세틸에텔 4.0부, 에칠렌디아민테트라초산나트륨 0.03부, 몰식자산프로필 0.15부, 파라옥시안식향산메칠 0.2부를 가하고 교반한 후 젖산으로 pH를 6.5로 조절하고 전체가 100부가 되게 물을 가하고 90℃로 가열교반하여 용액으로한 다음 실온까지 서서히 냉각하여 미세결정의 아스코르빌팔미테이트 및 아스코르빌스테아레이트 펄 유화액을 제조하였다.To 90 parts of water, 2.0 parts of ascorbyl palmitate, 2.0 parts of ascorbyl stearate, 4.0 parts of polyoxyethylene cetyl ether, 0.03 parts of sodium ethylenediaminetetraacetic acid, 0.15 part of methacrylatepropyl, 0.2 part of paraoxybenzoic acid methyl, and stirred After adjusting the pH to 6.5 with lactic acid, adding water to 100 parts in total, stirring the mixture at 90 ° C., heating the solution to form a solution, and then slowly cooling to room temperature to prepare microcrystalline ascorbyl palmitate and ascorbyl stearate pearl emulsions. It was.
[실시예 5]Example 5
유연화장수 제조방법Flexible Cosmetic Manufacturing Method
제조방법 : 원료 14에 원료 1-8을 가하여 수상으로 하고 원료 12에 원료 9-11을 가하여 알코올상으로 한다. 알코올상을 수장에 서서히 가하면서 교반 혼합한후 원료 13을 가하여 조색한다.Method of Preparation: Add water 1-8 to raw material 14 to form an aqueous phase, and add raw material 9-11 to raw material 12 to obtain an alcohol phase. The alcohol phase is gradually added to the water column, stirred and mixed, and then raw material 13 is added to color.
[실시예 6]Example 6
농축화장수 제조방법How to make concentrated concentrated water
제조방법 : 원료 14에 원료 1-8을 가하여 수상으로 한다. 원료 12에 원료 9-11을 가하여 알코올상으로 한다. 알코올상을 수상에 서서히 가하여 교반 혼합하고 원료 10을 가하여 조색한다.Manufacturing Method: Add water 1-8 to raw material 14 to obtain an aqueous phase. Raw material 9-11 is added to raw material 12 to obtain an alcohol phase. The alcohol phase is gradually added to the aqueous phase, stirred and mixed, and the raw material 10 is added to color.
[실시예 7]Example 7
팩제조방법How to pack
제조방법 : 원료 13에 원료 1-7을 가하여 혼합하고 여기에 원료 11에 원료 8-10을 용해시킨 것을 서서히 가하면서 교반하고 원료 12을 가하여 조색한다Method of Preparation: Raw material 1-7 was added to the raw material 13, mixed, and the raw material 8-10 dissolved in the raw material 11 was slowly added while stirring, and raw material 12 was added to color.
[실시예 8]Example 8
하이드로 퀴논 제재 제조방법Hydroquinone preparation method
제조방법 : 원료 11에 원료 1-10을 가하여 교반 혼합한다.Preparation Method: Raw material 1-10 was added to the raw material 11, followed by stirring and mixing.
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KR1019860004191A KR890001694B1 (en) | 1986-05-28 | 1986-05-28 | Process for preparing emulsion of microcrystalline ascorbic fatty acid ester pearl and its preparation |
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KR1019860004191A KR890001694B1 (en) | 1986-05-28 | 1986-05-28 | Process for preparing emulsion of microcrystalline ascorbic fatty acid ester pearl and its preparation |
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KR890001694B1 true KR890001694B1 (en) | 1989-05-18 |
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