KR101473925B1 - Antiseptic compositions comprising Magnolia grandiflora extract and cosmetic compositions containing the same - Google Patents
Antiseptic compositions comprising Magnolia grandiflora extract and cosmetic compositions containing the same Download PDFInfo
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Abstract
본 발명은 태산목 추출물을 함유하는 항균 및 방부용 조성물에 관한 것으로서, 구체적으로는 태산목 추출물과 카프릴릴 글리세릴 에테르 화합물의 상승작용에 의하여 그 항균 및 방부활성이 우수하여 화장품의 보존제로 유용하게 사용할 수 있는 항균 및 방부용 조성물 및 그 제조방법에 관한 것이다. 상기 항균 및 방부용 조성물은 태산목 추출 파우더 0.1~3.0 중량%, 50~65℃로 가온한 정제수 10~40 중량%, 및 글리세린 10~30 중량%를 혼합하면서 용해시키는 단계; 부틸렌글리콜, 프로필렌 글리콜 및 헥산디올로 이루어지는 군으로부터 선택된 적어도 하나의 글리콜 5~40 중량%를 혼합하는 단계; 카프릴릴 글리세릴 에테르(carprylyl glyceryl ether) 10~40 중량%를 혼합하는 단계; 및 상기 혼합물을 여과하는 단계를 포함하는 항균 및 방부용 조성물의 제조방법에 의하여 제조될 수 있다.The present invention relates to an antimicrobial and antidandruff composition containing a perennial plant extract. Specifically, the antimicrobial and antimicrobial composition of the present invention is excellent in antimicrobial and preservative activity by synergistic action of a perennial extract and a caprylyl glyceryl ether compound. And to a method for preparing the same. Wherein the antimicrobial and antidandruff composition comprises 0.1 to 3.0% by weight of a magnolia extract powder, 10 to 40% by weight of purified water heated to 50 to 65 캜, and 10 to 30% by weight of glycerin; Mixing 5 to 40% by weight of at least one glycol selected from the group consisting of butylene glycol, propylene glycol and hexanediol; Mixing 10 to 40% by weight of carpyryl glyceryl ether; And filtering the mixture. The antimicrobial and antidandruff compositions of the present invention can be prepared by a method comprising the steps of:
Description
본 발명은 태산목 추출물을 함유하는 항균 및 방부용 조성물에 관한 것으로서, 구체적으로는 태산목 추출물과 카프릴릴 글리세릴 에테르 화합물의 상승작용에 의하여 그 항균 및 방부활성이 우수하여 화장품의 보존제로 유용하게 사용할 수 있는 항균 및 방부용 조성물에 관한 것이다.The present invention relates to an antimicrobial and antidandruff composition containing a perennial plant extract, and more particularly, to a composition for antimicrobial and antimicrobial use containing a perennial plant extract, which is excellent in antimicrobial and preservative activity by synergistic action of a perennial extract and a caprylyl glyceryl ether compound, Gt; antimicrobial < / RTI >
식품이나 화장품의 보존기간을 늘리기 위해서는 항균 또는 방부활성을 가지는 물질을 함께 첨가하여야 한다. 특히 화장품은 물, 수용성 성분과, 오일, 왁스류 및 지용성 성분이 포함되는데, 이러한 제품 내 수분과 각종 유기물 성분들은 세균이나 곰팡이의 좋은 영양분으로 작용하여 미생물이 쉽게 번식할 수 있는 환경을 제공하므로 보존성을 높이는 것이 중요하다. 미생물에 오염된 화장품은 성분의 변질에 따른 기능저하는 물론 피부 발진, 염증 등 피부 트러블과 미생물 감염의 위험성을 내포한다. 따라서 대부분의 화장품은 미생물의 증식을 억제하거나 사멸할 목적으로 방부제를 포함하고 있다. 특히 제품의 특성상 사용기간이 수 개월에서 수 년까지 매우 길기 때문에 화장품 조성에 있어서 이들 방부제의 역할은 더욱 중요하다.In order to increase the shelf life of food or cosmetics, substances with antibacterial or antiseptic properties should be added together. In particular, cosmetics include water, water-soluble components, oils, waxes and lipid-soluble components. Moisture and various organic components of these products act as good nutrients for bacteria and fungi, . Cosmetics contaminated with microorganisms have a risk of skin troubles and microbial infections such as skin rash and inflammation, as well as functional deterioration due to the deterioration of components. Therefore, most cosmetics contain preservatives for the purpose of suppressing or killing microbial growth. Especially, the use period of these preservatives is more important in cosmetic composition because the period of use is very long from several months to several years due to the characteristics of the product.
상기의 화장품의 특성에 의해 고려되어야 하는 방부제의 기본 조건으로는 넓은 항균 스펙트럼을 가지며, 사용 및 제조가 용이하고, 피부 자극이 없어야 한다. 또한 범용적으로 사용가능하기 위해서, 제품의 산도(pH)에 영향을 받지 않고, 제품 성분의 효과를 저하시키지 않으며, 다루기가 용이해야 한다. 이러한 조건을 충족시키기 위해, 화장품 및 의약품 등에 일반적으로 사용되는 방부제로는 파라옥시안식향산에스텔과 파라벤류가 주로 쓰이며, 살균의 목적으로 염화벤잘코늄(Benzalkonium Chloride), 글루콘산 클로로헥시딘(chlorohexidine gluconic acid) 및 트리클로로 카르바닐리드 등이 사용되고 있다. 그러나 이들 인공방부제들은 소량의 사용에 의해서도 피부 자극, 피부 알러지 등을 유발하고, 암이나 유전자 변이 유발의 가능성까지 대두되고 있다. 이에 따라 기존의 화학합성 방부제가 가지는 부작용을 해결하고 제품의 안전성을 위해 천연성분의 방부제의 필요성이 대두되었다.The basic condition of the preservative to be considered by the characteristics of the above-mentioned cosmetics is that it has a broad antibacterial spectrum, is easy to use and manufacture, and has no skin irritation. In addition, since it is universally usable, it is not affected by the pH of the product, does not deteriorate the effect of the product components, and should be easy to handle. Preservatives commonly used in cosmetics and pharmaceuticals to meet these requirements are paraoxybenzoates and parabens. For the purpose of sterilization, benzalkonium chloride, chlorohexidine gluconic acid, acid and trichlorocarbonylide are used. However, these artificial preservatives cause skin irritation, skin allergy, etc., even with a small amount of use, and the possibility of inducing cancer or gene mutation is emerging. As a result, the need for natural preservatives has emerged for solving the side effects of conventional chemical synthetic preservatives and for the safety of the products.
이러한 예로서 대한민국 공개특허 제2004-0080717호 "방부 및 항균 활성을 갖는 키토산 및 자몽종자 추출물을함유한 기능성 화장료 조성물"에는 키토산(chitosan) 및 자몽종자 추출물을 필수적으로 포함하며 포도씨 추출물, 겨자씨 추출물, 편백나무 추출물 및 목련 추출물로부터 선택된 추출물을 추가적으로 포함하는 기능성 화장료 조성물이 개시되어 있다.As an example of such an example, Korean Patent Publication No. 2004-0080717 entitled " Functional Cosmetic Composition Containing Chitosan and Grapefruit Seed Extract with Antiseptic and Antimicrobial Activity ", chitosan and grapefruit seed extract are essential, and grape seed extract, mustard seed extract, A functional cosmetic composition is further disclosed which further comprises an extract selected from Clostridium botulinum extract and Magnoliae extract.
본 발명자들은 항균 및 방부활성을 가지는 다양한 식물추출물들을 탐색하였으며, 그 중 태산목추출물을 선정하여 그 항균 및 방부활성을 높이는 방법에 대하여 연구하던 중 특정화합물과 함께 사용하는 경우 그 상승작용에 의하여 그 항균 및 방부활성이 증가한다는 것을 발견하여 본 발명을 완성하였다.The present inventors have searched various plant extracts having antimicrobial and antiseptic activities. Among them, when studying a method for enhancing the antimicrobial and preservative activity of a selected product of the extract of the magnolius, when used in combination with a specific compound, And an antiseptic activity are increased, thus completing the present invention.
본 발명은 항균 및 방부활성이 우수한 태산목 추출물함유 항균 및 방부용 조성물을 제공하는 것을 목적으로 한다.An object of the present invention is to provide a composition for antimicrobial and antidandruff containing antioxidant and antioxidant activity.
또한 본 발명은 상기 항균 및 방부용 조성물의 제조방법을 제공하는 것을 다른 목적으로 한다.Another object of the present invention is to provide a method for producing the composition for antibacterial and antidandruff.
또한, 본 발명은 상기 태산목 추출물 함유 항균 및 방부용 조성물을 이용한 화장료 조성물을 제공하는 것을 또 다른 목적으로 한다.It is still another object of the present invention to provide a cosmetic composition using the antimicrobial and nasal composition containing the black tea extract.
상기 목적을 달성하기 위하여 본 발명에 따르면, 태산목추출물과 카프릴릴 글리세릴 에테르(carprylyl glyceryl ether)를 함유하는 항균 및 방부용 조성물이 제공된다. 바람직하게는 상기 태산목추출물은 태산목의 열수추출물이다. 상기 태산목추출물과 카프릴릴 그리세릴 에테르(carprylyl glyceryl ether)는 0.1~3.0:10~40의 중량비로 혼합되는 것이 바람직하다. 상기 다른 목적을 달성하기 위하여 본 발명에 따르면, 태산목 추출 파우더 0.1~3.0 중량%, 50~65℃로 가온한 정제수 10~40 중량%, 및 글리세린 10~30 중량%를 혼합하면서 용해시키는 단계; 부틸렌글리콜, 프로필렌 글리콜 및 헥산디올로 이루어지는 군으로부터 선택된 적어도 하나의 글리콜 5~40 중량%를 혼합하는 단계; 카프릴릴 글리세릴 에테르(carprylyl glyceryl ether) 10~40 중량%를 혼합하는 단계; 및 상기 혼합물을 여과하는 단계를 포함하는 항균 및 방부용 조성물의 제조방법이 제공된다. 이때, 상기 태산목 추출파우더는 태산목의 열수추출물인 것이 바람직하다. 상기 또 다른 목적을 달성하기 위하여 본 발명에 따르면, 상기 항균 및 방부용 조성물을 화장료 조성물의 전체 중량에 대하여 0.0001 ~ 50 중량%만큼 함유하여 그 보존성이 우수한 화장료조성물이 제공된다.According to the present invention, there is provided an antimicrobial and antidandruff composition comprising a perennial plant extract and carpyryl glyceryl ether. Preferably, the Magnolia plant extract is a hydrothermal extract of Magnoliaceae. It is preferable that the black tea extract and the carpyryl glyceryl ether are mixed at a weight ratio of 0.1 to 3.0: 10 to 40. According to another aspect of the present invention, there is provided a method for preparing a microcrystalline cellulose, which comprises dissolving, in a mixture, 0.1 to 3.0% by weight of magnolia extract powder, 10 to 40% by weight of purified water heated to 50 to 65 캜, and 10 to 30% Mixing 5 to 40% by weight of at least one glycol selected from the group consisting of butylene glycol, propylene glycol and hexanediol; Mixing 10 to 40% by weight of carpyryl glyceryl ether; And filtering the mixture. ≪ IMAGE > At this time, the magnolia seed extract powder is preferably a hydrothermal extract of magnolia. According to the present invention, there is provided a cosmetic composition comprising the antimicrobial and anticorrosion composition in an amount of 0.0001 to 50% by weight based on the total weight of the cosmetic composition, and having excellent preservability.
상기 화장료조성물은 유연화장수, 영양화장수, 마사지크림, 영양크림, 팩, 젤, 피부 점착타입의 화장료, 립스틱, 메이컵 베이스, 파운데이션, 샴푸, 린스, 바디크렌저, 비누, 치약, 구강청정제, 로션, 연고, 겔, 크림, 패취 또는 분무제의 제형으로 적용될 수 있다.The cosmetic composition of the present invention can be used in cosmetics such as soft longevity, nutritional lotion, massage cream, nutritional cream, pack, gel, skin stick type cosmetic, lipstick, makeup base, foundation, shampoo, rinse, body cleanser, soap, toothpaste, Ointments, gels, creams, patches or spray formulations.
본 발명의 항균 및 방부용 조성물은 천연추출물을 함유하여 안전하며, 각 성분의 상승작용에 의하여 그 항균 및 방부활성이 크게 증가되어 화장료의 보존제로 사용되는 경우 장기간 안정한 상태로 유지시키므로 유용하다.The antimicrobial and antidandruff compositions of the present invention are safe because they contain natural extracts, and their antimicrobial and preservative activities are greatly increased by the synergistic action of the respective components, so that they are useful for keeping the composition stable for a long period of time when it is used as a preservative for cosmetics.
이하 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail.
태산목(Magnolia grandiflora)은 목련목의 식물로서 원산지는 북아메리카이고 높이가 약 30m까지 자란다. 양옥란(洋玉蘭)이라고도 하며, 가지와 겨울눈에 털이 난다. 잎은 어긋나고 긴 타원형이거나 긴 달걀을 거꾸로 세워놓은 모양이고 길이 10∼20cm, 너비 5∼10cm이다. 끝이 둔하고 혁질(革質:가죽 같은 질감)이다. 겉면은 짙은 녹색으로서 윤기가 있고 뒷면에는 갈색 털이 빽빽이 나며 가장자리가 밋밋하다. 잎자루는 길이 2∼3cm이다. 꽃은 5∼6월에 흰색으로 피는데, 지름 15∼20cm이고 가지 끝에 위를 향하여 1개씩 달린다. 향기가 강하고 꽃받침은 3개, 꽃잎은 9∼12개이다. 암술과 수술은 많으며 수술대는 자주색이다. 열매는 골돌과로서 9월에 익는데, 타원형이고 짧은 털이 나며 붉은 종자가 2개씩 나와서 붉은 실로 매달린다. 북아메리카원산이며 관상용으로 심는다. 미국에서는 잎을 크리스마스장식용으로 쓴다. 꽃과 나무 껍질을 약용하는 데 생약명은 하화옥란이다. 외감풍한, 두통비색, 완복창통, 구토복사, 편두통, 고혈압을 치료하는데 효능이 있는 것으로 알려져 있다. 대한민국특허 공개 제2009-0020870호에는 태산목 추출물이 식물병 방제에 사용될 수 있음이 개시되어 있다.Magnolia grandiflora is a plant of Magnoliaceae, native to North America and growing to a height of about 30 meters. It is also known as Yangyoran (洋 玉蘭), hairy in branches and winter eyes. Leaves are alternate long oval or long egg in inverted shape, length 10 ~ 20cm, width 5 ~ 10cm. It is dull and swollen (leather: leather-like texture). The surface is dark green with shiny, with brown hairs on the back and plain edges. The petiole is 2 ~ 3cm long. Flowers bloom in May-June, white, 15 ~ 20cm in diameter, one branch runs on the end of the branch. It has strong aroma, 3 calyxes, and 9-12 petals. There are many pistils and stamens, and the operating table is purple. The fruit is oolongid, ripening in September, oval, short hairs, two red seeds, hanging in red thread. It is native to North America and is planted for ornamental purposes. In the United States, leaves are used for Christmas decorations. Flowers and bark are medicinal herbs are Hwanghae Ran. It is known to be efficacious in treating externalities, headache coloration, dandruff, vomiting, migraine, and hypertension. Korean Patent Laid-Open Publication No. 2009-0020870 discloses that a perennial plant extract can be used for controlling plant diseases.
본 발명자들은 상기 태산목 추출물에 항균 및 방부활성이 있음을 확인하여, 다양한 방법으로 추출물을 제조하였다. 물, 에탄올, 아세톤, 클로로포름 등의 다양한 용매를 사용하여 추출하여 본 결과, 각 추출물에 다양한 세균에 대한 항균활성이 있는 것을 확인하였으며, 그 중에서도 태산목의 열수추출물의 경우에 그 활성이 가장 우수한 것을 확인하였다. 상기 태산목 추출물은 태산목의 잎, 줄기 또는 그 혼합 추출물인 것이 바람직하다. 또한, 상기 태산목 추출물에 카프릴릴 글리세릴 에테르(carprylyl glyceryl ether)를 특정비율로 혼합하는 경우에 그 활성이 크게 증가하는 것을 발견하였다. 따라서 본 발명은 태산목 추출물과 카프릴릴 글리세릴 에테르(carprylyl glyceryl ether)를 함유하는 조성물이 그 상승작용에 의하여 항균 및 방부활성이 우수하다는 것을 이용한 것이다. 바람직하게는 상기 태산목추출물과 카프릴릴 글리세릴 에테르를 0.1~3.0:10~40의 중량비의 비율로 혼합하는 경우에 그 활성이 가장 우수하게 나타났다.The present inventors confirmed that the above-mentioned Magnoliaceae extract had antimicrobial and antiseptic activity, and thus, the extract was prepared by various methods. As a result of extracting with various solvents such as water, ethanol, acetone, and chloroform, it was confirmed that each extract had antimicrobial activity against various bacteria. Among them, hydrothermal extract of Respectively. It is preferable that the magnolia berry extract is leaf, stem or a mixed extract thereof of magnolia. In addition, it has been found that the activity is greatly increased when carprylyl glyceryl ether is mixed with the black tea extract at a specific ratio. Accordingly, the present invention utilizes the fact that a composition containing a perennial extract and a carpyryl glyceryl ether is superior in antibacterial and antiseptic activity due to its synergistic action. Preferably, the activity is most excellent when the grape seed extract and caprylyl glyceryl ether are mixed at a weight ratio of 0.1 to 3.0: 10 to 40.
상기 방부용 조성물은 다음과 같은 방법에 의하여 제조할 수 있다. 본 발명의 일 구체예에 따르면, 먼저 태산목 열수 추출 파우더 0.1~3.0 중량%를 50~65℃로 가온한 정제수 10~40 중량%, Glycerin 10~30 중량%와 혼합하면서 용해한다. 여기에 부틸렌 글리콜(Butylene glycol), 프로필렌 글리콜(Propylene glycol), 헥산디올(Hexanediol)과 같은 글리콜을 5~40 중량%을 혼합한다. 이어서 카프릴릴 글리세릴 에테르(Carprylyl glyceryl ether) 10~40 중량%을 혼합하여 교반한다. 상기 혼합물을 필터지를 사용하여 여과하여 제조한다. The anticorrosive composition can be prepared by the following method. According to one embodiment of the present invention, 0.1 to 3.0% by weight of the hydrothermal extracted powder is mixed with 10 to 40% by weight of purified water heated to 50 to 65 캜 and 10 to 30% by weight of glycerin. 5 to 40% by weight of glycols such as butylene glycol, propylene glycol, and hexanediol are mixed. 10 to 40% by weight of Carprylyl glyceryl ether is then mixed and stirred. The mixture is prepared by filtration using filter paper.
이와 같이 제조된 항균 및 방부용 조성물은 E. Coli, S. Aureus, P. auruginosa, C. Albicans, A. Niger와 같은 세균에 대하여 우수한 항균활성을 가짐을 확인할 수 있었다. 또한, 상기 항균 및 방부용 조성물을 화장료 전체조성물에 대하여 0.0001 ~ 50 중량% 함유하는 화장료를 제조하여 그 성상 안정성을 시험한 결과 그 성상안정성이 우수함을 확인할 수 있었다. 그러므로 태산목 추출물과 카프릴릴 글리세릴 에테르(Carprylyl glyceryl ether)를 함유하는 상기 항균 및 방부용 조성물은 화장품의 보존제로서 유용하게 사용될 수 있다. 상기 화장료는 유연화장수, 영양화장수, 마사지크림, 영양크림, 팩, 젤, 피부 점착타입의 화장료, 립스틱, 메이컵 베이스, 파운데이션, 샴푸, 린스, 바디크렌저, 비누, 치약, 구강청정제, 로션, 연고, 겔, 크림, 패취 또는 분무제의 제형으로 적용될 수 있다.
The antibacterial and antidandruff compositions thus prepared were found to have excellent antibacterial activity against bacteria such as E. coli, S. aureus, P. auruginosa, C. albicans and A. niger. Further, cosmetic compositions containing the antimicrobial and antidandruff composition in an amount of 0.0001 to 50% by weight based on the total composition of the cosmetic composition were prepared and tested for stability, and as a result, it was confirmed that the stability of the composition was excellent. Therefore, the antimicrobial and antidandruff composition containing the perennial extract and Carprylyl glyceryl ether can be usefully used as a preservative in cosmetics. The above-mentioned cosmetics can be used as cosmetics such as softening longevity, nutritional lotion, massage cream, nutritional cream, pack, gel, skin adhesive type, lipstick, makeup base, foundation, shampoo, rinse, body cleanser, soap, toothpaste, , Gels, creams, patches or spray formulations.
[실시예][Example]
이하 실시예 및 시험예를 통하여 본 발명을 더욱 상세히 설명하지만, 본 발명이 하기의 예에 의하여 제한되지는 않는다.
Hereinafter, the present invention will be described in more detail by way of examples and test examples, but the present invention is not limited by the following examples.
제조예 1: 태산목 에탄올 추출물 제조Production Example 1: Production of ethanol extract of magnolia
건조된 태산목 잎, 줄기 100g을 95% EtOH 1Kg, 65℃에서 4시간 추출하였다. 추출 과정을 마무리한 후, 여과 과정을 거친다. 여과액을 감압증류하여 태산목 95% EtOH 추출 파우더 5.1g을 얻었다.
100g of dried leaves and stem were extracted with 1Kg of 95% EtOH at 65 ℃ for 4 hours. After the extraction process is completed, the filtration process is performed. The filtrate was distilled under reduced pressure to obtain 5.1 g of a magnesia extract of 95% EtOH.
제조예 2: 태산목 아세톤 추출물 제조Production Example 2: Preparation of an extract of perennial acetone
건조된 태산목 잎, 줄기 100g을 Acetone 1Kg, 65℃에서 환류냉각하여 4시간 추출하였다. 추출 과정을 마무리한 후, 여과 과정을 거친다. 여과액을 감압증류하여 태산목 Acetone 추출 파우더 6.8g을 얻었다.
Dried leaves of Magnoliaceae and 100g of stem were extracted with 1Kg of Acetone under reflux at 65 ℃ for 4 hours. After the extraction process is completed, the filtration process is performed. The filtrate was distilled under reduced pressure to obtain 6.8 g of Acetone extract powder of Magnoliaceae.
제조예 3: 태산목 열수 추출물 제조Production Example 3: Production of hot pepper extract of magnolia
건조된 태산목 잎, 줄기 100g을 정제수 1Kg, 80℃에서 4시간 추출하였다. 추출 과정을 마무리한 후, 여과 과정을 거친다. 여과액을 감압증류하여 태산목 열수 추출 파우더 17.8g을 얻었다.
Dried leaves and stem of 100g of Magnoliaceae were extracted with 1Kg of purified water at 80 ℃ for 4 hours. After the extraction process is completed, the filtration process is performed. The filtrate was distilled under reduced pressure to obtain 17.8 g of a hydrothermally extracted powder of magnolia.
제조예 4: 태산목 클로로포름 추출물 제조Production Example 4: Preparation of chloroform-extract of peroxidase
건조된 태산목 잎, 줄기 100g을 CHCl3(클로로포름) 1Kg, 65℃에서 환류냉각하여 4시간 추출하였다. 추출 과정을 마무리한 후, 여과 과정을 거친다. 여과액을 감압증류하여 태산목 CHCl3(클로로포름) 추출 파우더 9.6g을 얻었다.
100 g of dried peduncle leaves and stem were extracted with 1 Kg of CHCl 3 (chloroform) at 65 ° C under refluxing for 4 hours. After the extraction process is completed, the filtration process is performed. The filtrate was distilled under reduced pressure to obtain 9.6 g of a magnolia tree extract CHCl 3 (chloroform) -extracted powder.
시험예 1: 항균활성 시험(MIC TEST)Test Example 1: Antimicrobial activity test (MIC TEST)
상기 제조예의 태산목 추출물 및 카프릴릴 글리세릴 에테르(Carprylyl glyceryl ether)의 항균활성을 확인하였다. 세균의 발육을 억제할 수 있는 최소한의 항생제(항균제)의 농도를 측정하는 MIC(minimal inhibitory concentration) 테스트로 이를 확인하였다.The antimicrobial activity of the extract of the perennial plant and the carpyryl glyceryl ether of the above-mentioned production example was confirmed. This was confirmed by the MIC (minimal inhibitory concentration) test, which measures the concentration of the minimum antibiotic (antibacterial agent) that can inhibit bacterial growth.
먼저 하기 표 1과 같은 미리 배양된 사용 균주를 준비하였다(세균: 2 ~ 4×107CFU/mL, 진균: 2 ~ 4×106CFU/mL). Microtube에 시험하고자 하는 시료를 세균용, 진균용 따로 담았다(시험하고자 하는 농도를 결정하여 무게를 단다). 시료를 담고 세균용은 NB(nutrient broth)로 진균용은 PDB(potato dextrose broth)를 담아 vortexing하여 섞어주고 sonication하여 확실히 녹여주었다. 이 때 잘 녹지 않는 시료는 희석된 DMSO에 녹인 후 배지로 희석하여 사용하였다. 96 well plate에 labeling 하고 맨 위 칸에 준비한 시료를 0.1 ml씩 넣어주었다(세균용과 진균용을 구분하여 넣어준다). 균을 96 well plate 전체에 0.1 mL씩 채운 후, 96 well plate에 시료와 균 액 준비가 완료되면 맨 위칸부터 1/2씩 희석하면서 내려간다. 맨 아래칸은 시료와 희석하지 않고 균액만 두어 blank로 사용하였다. 이어 96 well plate를 37℃에서 배양하였다.(Bacteria: 2-4 × 10 7 CFU / mL, fungus: 2-4 × 10 6 CFU / mL) were prepared as shown in Table 1 below. The microtube contains the sample to be tested separately for bacterial and fungal (weighing to determine the concentration to be tested). The samples were vortexed with NB (nutrient broth) for bacteria, PDB (potato dextrose broth) for fungi, and mixed by sonication. At this time, samples that did not dissolve were dissolved in diluted DMSO and diluted with medium. Label in a 96-well plate and add 0.1 ml of the prepared sample to the top of the well (separate for both germ and fungi). Fill the plate with 0.1 mL of the whole 96-well plate, then dilute with 1/2 dilution from the top of the plate. The bottom column was used as a blank with no dilution of the sample and a homogeneous solution. Then, 96 well plate was incubated at 37 ℃.
세균 확인은 18 ~ 24hr, C.albicans의 경우 32 ~ 56hr, A.niger의 경우 36 ~ 72 hr 후에 꺼내어 spectrophometer로 흡광도를 측정하여 균의 성장 여부를 확인하였다. Bacteria were identified in 18-24hrs, C.albicans in 32-56hrs, A.niger in 36-72hrs, and the absorbance was measured by spectrophotometer.
그 결과를 하기의 표 1에 나타내었다.The results are shown in Table 1 below.
상기 제조예의 태산목 추출물 가운데서 태산목 열수추출물의 경우 항균활성이 가장 우수하게 나타남을 확인할 수 있었다.
Among the extracts of the magnolius of the above example, it was confirmed that the hydrothermal extract of Magnolia is the most excellent antimicrobial activity.
실시예 1: 태산목 추출물 함유 항균 방부용 조성물제조Example 1: Preparation of antimicrobial composition containing a black tea extract
상기 제조예 3에서 제조된 태산목 열수 추출 파우더 1.0g을 60℃로 가온한 정제수 29g과 Glycerin 20g을 혼합하면서 용해하였다. 1, 2-Hexanediol 25g을 혼합하고, Carprylyl glyceryl ether 25g을 넣고 혼합하였다. 혼합을 마친 후, 1.0㎛ 필터지로 여과하여 항균 방부용 조성물을 제조하였다.
1.0 g of the hydrothermal extract of the magnolia prepared in Preparation Example 3 was dissolved while mixing 29 g of purified water heated to 60 ° C and 20 g of glycerin. 1, 2-hexanediol were mixed and 25 g of Carprylyl glyceryl ether was added and mixed. After completion of the mixing, the mixture was filtered through a 1.0 mu m filter paper to prepare an antimicrobial composition.
비교예 1:태산목 추출물 함유 항균 방부용 조성물제조COMPARATIVE EXAMPLE 1: Preparation of composition for antimicrobial antibacterial agent containing extract of Magnolia
상기 제조예 3에서 제조된 태산목 열수 추출 파우더 1.0g을 60℃로 가온한 정제수 40g과 Glycerin 34g을 혼합하면서 용해하였다. 1, 2-Hexanediol 25g을 넣고 혼합하였다. 혼합을 마친 후, 1.0㎛ 필터지로 여과하여 항균 방부용 조성물을 제조하였다.
1.0 g of the hydrothermal extracted gentle magnolia powder prepared in Preparation Example 3 was dissolved in 40 g of purified water heated to 60 캜 and 34 g of glycerin while mixing. 1, 2-hexanediol (25 g) were added and mixed. After completion of the mixing, the mixture was filtered through a 1.0 mu m filter paper to prepare an antimicrobial composition.
비교예 2:태산목 추출물 함유하지 않은 항균 방부용 조성물제조Comparative Example 2: Preparation of antimicrobial composition containing no extract of Magnolia
상기 제조예 3에서 제조된 태산목 열수 추출 파우더를 제외하고 60℃로 가온한 정제수 25g과 Glycerin 25g을 혼합하면서 용해하였다. 1, 2-Hexanediol 25g을 혼합하고, Carprylyl glyceryl ether 25g을 넣고 혼합하였다. 혼합을 마친 후, 1.0㎛ 필터지로 여과하여 항균 방부용 조성물을 제조하였다.
25 g of purified water heated to 60 ° C and 25 g of Glycerin were dissolved while mixing the hydrothermal extracted powder produced in Production Example 3. 1, 2-hexanediol were mixed and 25 g of Carprylyl glyceryl ether was added and mixed. After completion of the mixing, the mixture was filtered through a 1.0 mu m filter paper to prepare an antimicrobial composition.
시험예 2: 항균활성 시험(MIC TEST)Test Example 2: Antimicrobial activity test (MIC TEST)
상기 실시예 1의 조성물에 대한 항균활성 시험을 상기 시험예 1과 동일한 방법으로 수행하였으며, 그 결과를 하기 표 2에 나타내었다.The antibacterial activity of the composition of Example 1 was tested in the same manner as in Test Example 1, and the results are shown in Table 2 below.
상기 표 2에서 확인되는 바와 같이, 태산목 열수추출물과 Carprylyl glyceryl ether를 함유하는 실시예 1의 조성물은 각각의 항균활성보다 더욱 우수한 항균활성을 나타내는 것을 확인할 수 있었다.
As shown in Table 2, it was confirmed that the composition of Example 1 containing the hydrothermal extract of Magnolia sieboldii and Carprylyl glyceryl ether exhibited more excellent antibacterial activity than the respective antimicrobial activities.
실시예 2: 크림 제조Example 2: Cream production
하기 표 3의 조성을 가지는 크림을 통상의 방법으로 제조하였다.A cream having the composition shown in Table 3 was prepared by a conventional method.
시험예 3: 방부력 시험(CHALLENGE TEST)Test Example 3: CHALLENGE TEST
상기 실시예 2의 크림에 일정 수의 균을 접종한 후 잔존하는 생균수를 확인하는 방법으로 상기 실시예 1 조성물의 방부력을 다음과 같이 평가하였다.
The flushing force of the composition of Example 1 was evaluated as follows in order to confirm the number of viable bacteria remaining after inoculating a certain number of bacteria into the cream of Example 2 as follows.
시험균 준비Preparation of Test Bacteria
대장균(Escherichia coli ATCC 8739), 황색 포도상구균(Staphlyococcus aureus ATCC 6538), 녹농균(Pseudomonas aeruginosa ATCC 9027)등 3 종의 세균은 대두카제인 소화한천배지에 각각 접종하고, 캔디다 알비칸스(Candida albicans ATCC 10231)는 사부로 포도당 액체배지에 접종한다. 액체배지에 접종 된 4 종의 시험균을 30~35℃ shaking incubator에서 18시간 배양하여, 시험균으로 사용한다. 또한, 아스퍼질러스 니거(Aspergillus niger ATCC 16404)는 배양된 평판배지에서 멸균생리식염수를 이용하여 포자를 포집하여 시험균으로 사용한다.
Three bacteria such as Escherichia coli ATCC 8739, Staphlyococcus aureus ATCC 6538 and Pseudomonas aeruginosa ATCC 9027 were inoculated into soybean casein digest agar medium, respectively, and Candida albicans ATCC 10231, Is inoculated into Sabouraud glucose liquid medium. Four kinds of test bacteria inoculated in liquid medium are cultured for 18 hours in shaking incubator at 30 ~ 35 ℃ and used as test bacteria. In addition, Aspergillus niger ATCC 16404 is used as a test organism by collecting spores using sterilized physiological saline in a cultured plate medium.
시험균 접종 및 균수 측정Inoculation of the test bacteria and measurement of the number of bacteria
시료는 깨끗한 용기에 20g씩 평량한 다음, 대장균(Escherichia coli ATCC 8739), 황색 포도상구균(Staphlyococcus aureus ATCC 6538), 녹농균(Pseudomonas aeruginosa ATCC 9027), 아스퍼질러스 니거(Aspergillus niger ATCC 16404), 캔디다 알비칸스(Candida albicans ATCC 10231) 5종의 배양된 균액을 20g의 시료에 200㎕ 씩 각각 넣고 멸균된 스페츌라로 잘 혼합하여 균액이 시료에 잘 섞이도록 한다. 이때 세균은 시료 당 초기농도 106cfu/g되도록 혼합하고, 진균은 시료 당 초기농도 105cfu/g이 되도록 혼합한다. 시험균이 접종 된 시료는 25℃ 배양기에서 4주간 배양하면서, 1, 7, 14, 21, 28일째에 시료를 각각 1g씩 취하여 생균수를 측정한다. 생균수 측정용 배지로는 대두카제인 소화 한천 배지와 사부로포도당 한천배지를 사용하며, 세균은 30~35℃ 배양기에서 24~48시간, 진균은 25℃ 배양기에서 3~5일간 배양하여 평판배지에 검출되는 균수를 측정한다.
Samples were weighed 20 g each in a clean container and then weighed in an amount of 20 g each of Escherichia coli ATCC 8739, Staphlyococcus aureus ATCC 6538, Pseudomonas aeruginosa ATCC 9027, Aspergillus niger ATCC 16404, Add 200 μl of each of the cultures of 5 kinds of Candida albicans (ATCC 10231) to 20g of the sample, mix well with sterilized Spetula, and mix well. Bacteria are mixed at an initial concentration of 10 6 cfu / g per sample, and fungi are mixed at an initial concentration of 10 5 cfu / g per sample. The samples inoculated with the test bacteria are cultured for 4 weeks in an incubator at 25 ° C., and 1 g of each sample is taken on days 1, 7, 14, 21 and 28, and the viable cell count is measured. Bacteria were cultured for 24 to 48 hours at 30 ~ 35 ℃ in incubator, for 3 to 5 days at 25 ℃ in incubator, and detected on plate medium. The number of viable cells is measured.
방부력 판정Buoyancy determination
방부력 판정 기준은 CTFA기준을 적용하였으며 세균은 7일후 접종균수의 99.9% 이상이 사멸되고 4주간 더 이상의 균 증식이 없어야 하며, 진균은 7일후 접종균수의 90% 이상이 사멸되고 4주간 더 이상의 균 증식이 없어야 한다.
The criteria for buoyancy assessment were CTFA standard. After 7 days, more than 99.9% of inoculated bacteria were killed and no more than 4 weeks of bacterial proliferation. After 7 days, more than 90% of inoculated bacteria were killed and more than 4 weeks There should be no bacterial growth.
그 결과를 하기의 표 4에 나타내었다.The results are shown in Table 4 below.
reduction%
reduction
reduction%
reduction
reduction%
reduction
reduction%
reduction
방부력 시험 결과 세균에 대해서는 시험균 접종 7일 후 99.9% 이상의 사멸을 보였고 28일 까지 더 이상의 균증식이 없었으며, 진균에 대해서도 접종 7일후 90% 이상의 사멸율과 28일까지 더 이상의 균증식이 없어 세균과 진균 모두에서 방부력을 유지하고 있음을 확인할 수 있었다.
As a result of buoyancy test, the bacteria showed more than 99.9% death after 7 days of inoculation of the test organism, no further bacterial growth until 28th day, and more than 90% of dead organisms after 7 days of inoculation, And it was confirmed that the bacterium maintains buoyancy in both bacteria and fungi.
시험예 4: 성상안정성 시험Test Example 4: Stability test
상기 실시예 1 및 실시예 2의 조성물을 온도 Cycling Chamber에서(4℃↔45℃, 24시간 간격) 성상 변화를 관찰하였으며, 그 결과를 하기의 표 5에 나타내었다.The compositions of Examples 1 and 2 were observed in a temperature cycling chamber (4 ° C ↔45 ° C, every 24 hours), and the results are shown in Table 5 below.
(-;변화없음, +;약간 색의 변화, ++;색변화 혹 약간의 침전, +++;색변화와 침전 발생)(-; no change, +; slight color change, ++; color change or slight precipitation, +++; color change and precipitation)
상기 표 5에서 확인되는 바와 같이 실시예 1과 실시예 2의 조성물은 성상 안정화 시험에서 어떤 성상의 변화를 나타내지 않아 성상안정성이 높은 것을 확인할 수 있었다.
As shown in Table 5, the compositions of Example 1 and Example 2 did not show any change in properties in the property stabilization test, and it was confirmed that the composition stability was high.
Claims (7)
The cosmetic composition according to claim 6, wherein the cosmetic composition is at least one selected from the group consisting of softening agents, nutritional lotion, massage cream, nutritional cream, pack, gel, skin adhesive type cosmetic, lipstick, makeup base, foundation, shampoo, rinse, Soap, toothpaste, mouthwash, lotion, ointment, gel, cream, patch or spray agent.
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WO2022092453A1 (en) * | 2020-10-30 | 2022-05-05 | 주식회사 엑티브온 | Preservative comprising polylysine and caprylyl glyceryl ether for external-use skin formulations and cosmetics composition comprising same |
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WO2022092453A1 (en) * | 2020-10-30 | 2022-05-05 | 주식회사 엑티브온 | Preservative comprising polylysine and caprylyl glyceryl ether for external-use skin formulations and cosmetics composition comprising same |
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