KR102468216B1 - Cosmetic Composition For Hair With Preventing Hair Color Separation And Dyeing Hair Containing Cassia Tora Seed Extract As Active Ingredient - Google Patents

Cosmetic Composition For Hair With Preventing Hair Color Separation And Dyeing Hair Containing Cassia Tora Seed Extract As Active Ingredient Download PDF

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KR102468216B1
KR102468216B1 KR1020220065254A KR20220065254A KR102468216B1 KR 102468216 B1 KR102468216 B1 KR 102468216B1 KR 1020220065254 A KR1020220065254 A KR 1020220065254A KR 20220065254 A KR20220065254 A KR 20220065254A KR 102468216 B1 KR102468216 B1 KR 102468216B1
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hair
cosmetic composition
cassia tora
dyeing
extract
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신은진
최정연
이정노
박성민
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주식회사 코씨드바이오팜
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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
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/02Preparations for cleaning the hair
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/06Preparations for styling the hair, e.g. by temporary shaping or colouring
    • A61Q5/065Preparations for temporary colouring the hair, e.g. direct dyes

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  • Cosmetics (AREA)

Abstract

The present invention relates to a cosmetic composition for hair with a hair color separation prevention effect and a natural hair dyeing effect, by containing a Cassia tora seed extract as an active ingredient. More specifically, the present invention relates to a cosmetic composition for natural hair dye containing a Cassia tora seed extract. The cosmetic composition according to the present invention has a hair dyeing effect by allowing negative ionic natural components of a natural extract to adsorb to positive ions of hair cuticles through ionic bonding.

Description

결명자 추출물을 유효성분으로 포함하는 모발 색빠짐 방지 및 염색 효과를 갖는 모발용 화장료 조성물{Cosmetic Composition For Hair With Preventing Hair Color Separation And Dyeing Hair Containing Cassia Tora Seed Extract As Active Ingredient}Cosmetic composition for hair containing Cassia tora extract as an active ingredient and having hair color loss prevention and dyeing effects {Cosmetic Composition For Hair With Preventing Hair Color Separation And Dyeing Hair Containing Cassia Tora Seed Extract As Active Ingredient}

본 발명은 결명자 추출물을 유효성분으로 포함하여, 모발 색빠짐 방지 및 천연 염색 효과를 갖는 모발용 화장료 조성물에 관한 것으로, 더욱 상세하게는 결명자 추출물을 함유하는 모발용 화장료 조성물에 관한 것이다.The present invention relates to a cosmetic composition for hair containing Cassia tora extract as an active ingredient, which prevents hair color loss and has a natural dyeing effect, and more particularly, to a cosmetic composition for hair containing Cassia tora extract.

염모제는 칼라의 지속적인 상태에 따라 일시적, 반영구적, 영구적 염모제로 구별된다. 가장 보편적인 영구 염모제는 모발 염색이 모표피를 침투하여 모피질 안에 색소 분자를 침전시키도록 고안한 것이다. 영구적인 염모제는 염료에 따라 산화, 금속 및 식물성 염모제로 나눌 수 있으며 가장 자주 사용하는 염모제는 방향족 아미노 화합물과 같은 산화염료를 사용하는 산화 염모제이다. Hair dyes are classified into temporary, semi-permanent, and permanent hair dyes according to the continuous state of the color. The most common permanent hair dyes are designed so that the hair dye penetrates the cuticle and deposits the pigment molecules in the cortex. Permanent hair dyes can be divided into oxidation, metal and vegetable hair dyes according to dyes, and the most frequently used hair dyes are oxidation hair dyes using oxidation dyes such as aromatic amino compounds.

산화 염료는 일반적으로 염료인 1제와 산화제인 2제를 혼합하여 사용하는 산화형 염모제 형태이다. 1제의 알칼리제에 의해 큐티클층이 열리고, 2제인 산화제에 의해 모발 속 멜라닌 색소의 탈색과 함께 분자량이 작은 단량체 화합물인 염료성분들이 큐티클층을 통과하여 모발 중심부까지 들어가 중합반응이 일어나고 큐티클층이 닫히면서 염색이 된다.Oxidation dyes are generally in the form of oxidation-type hair dyes in which a first agent, which is a dye, and a second agent, which is an oxidizing agent, are mixed and used. The cuticle layer is opened by the alkali agent of the first agent, and the melanin pigment in the hair is bleached by the oxidizing agent of the second agent, and the dye components, which are monomeric compounds with a small molecular weight, pass through the cuticle layer and enter the center of the hair, where a polymerization reaction occurs and the cuticle layer is closed. It becomes dyed.

산화 염모제는 염모력이 우수하지만 모발 염착이 늦고 일광, 세척 등에 의해 변색되는 단점이 있으며, 모발을 팽윤시켜 염료의 침투를 용이하게 하고 모발 내부에서의 산화중합에 의해 염착이 되게 하는 강알칼리제, 모노에탄올아민 등과 같은 알칼리제를 함께 사용하기 때문에 모발의 윤기 및 광택이 없어지고 모발이 심하게 손상되는 경우가 있어 부자연스러운 색이 되기도 하고 피부 자극 및 피부 트러블을 유발하는 단점이 있다. 또한 염착력을 높이기 위하여 사용한 다량의 염료는 염모제의 안정성을 저하시키고 모발의 손상 및 강한 피부 자극을 유발한다. 특히 염모제로 인한 피부 트러블과 묻으면 잘 지워지지 않는다. 심한 경우에는 피부의 발적, 피부의 홍반 또는 전신에 두드러기와 같은 홍반이 발생하는 경우도 있고 눈이 아프기도 해서 민감한 사람들에게는 사용상에 한계가 더욱 많다. Oxidative hair dyes have excellent hair dyeing power, but have the disadvantage of slow hair dyeing and discoloration due to sunlight, washing, etc., strong alkali agents that swell the hair to facilitate the penetration of dyes and dye by oxidative polymerization inside the hair, mono Since the alkali agent such as ethanolamine is used together, the gloss and luster of the hair are lost and the hair may be severely damaged, resulting in an unnatural color and causing skin irritation and skin trouble. In addition, a large amount of dye used to increase dyeing power reduces the stability of the hair dye and causes hair damage and strong skin irritation. In particular, it does not erase well when it comes to skin troubles caused by hair dye. In severe cases, redness of the skin, erythema of the skin, or erythema such as hives may occur all over the body, and it may cause eye pain, so there are more limitations in use for sensitive people.

따라서, 이러한 염모제의 단점 및 불편함을 개선하기 위해서는 천연 염모성분이 다량 함유되고 두피 보호, 모발 보호 등의 효과가 우수하며 인체에 무해하고 사용이 간편한 천연 염모 소재의 개발 및 그 물질을 함유하는 사용이 용이한 염모제의 개발이 필수적이다. 본 발명의 염색을 하는 방법을 사용한다면 위에서 열거한 문제점들을 해결할 수 있으며 염색 후 샴푸에 의한 물빠짐이 적고 모근과 두피에 영양공급을 하는 것은 물론 염색까지 자연스럽게 된다. Therefore, in order to improve the disadvantages and inconveniences of these hair dyes, the development of natural hair dye materials that contain a large amount of natural hair dye ingredients, have excellent effects such as scalp protection and hair protection, are harmless to the human body and are easy to use, and use containing the materials The development of this easy hair dye is essential. If the dyeing method of the present invention is used, the problems listed above can be solved, and after dyeing, water loss by shampoo is reduced, and nutrition is supplied to the hair roots and scalp, as well as dyeing becomes natural.

염색제와 관련하여, 대한민국 등록특허 제10-1108783호 (2012.01.16.)는, 대황, 하오수, 결명자 혼합추출물을 함유하는 염모제를 개시한다.Regarding the dye, Korean Patent Registration No. 10-1108783 (2012.01.16.) discloses a hair dye containing a mixed extract of rhubarb, Haosu, and Cassia tora.

대한민국 등록특허 제10-1458877호 (2014.10.31.)는, 오배자, 함초, 감잎 혼합추출물의 천연성분을 함유하는 1제형 산화형 염모제 조성물을 개시한다.Korean Patent Registration No. 10-1458877 (October 31, 2014) discloses a one-part oxidative hair dye composition containing natural ingredients of gall nut, seaweed, and persimmon leaf mixed extract.

대한민국 등록특허 제10-2353526호 (2022.01.17)는, 오디열매, 상백피, 상엽 및 흑운모 혼합 추출물을 유효성분으로 함유하는 염모제 샴푸 조성물을 개시한다.Korean Patent Registration No. 10-2353526 (January 17, 2022) discloses a hair dye shampoo composition containing mixed extracts of mulberry fruit, moth bark, moth leaf, and biotite as active ingredients.

본 발명은 기존 산화 염모제의 단점 및 불편함을 개선하기 위해서 천연 염모성분이 다량 함유되고 두피 보호, 모발 보호 등의 효과가 우수하며 인체에 무해하고 사용이 간편한 천연 염모 소재의 개발 및 그 물질을 함유하는 일반 샴푸, 린스와 같은 조성물로 염모 및 색빠짐 방지 기능을 갖는 조성물을 제공하고자 한다. 특히, 본 발명에 따른 화장료 조성물은 헤어의 큐티클의 양이온에 천연추출물의 음이온성 천연성분이 이온결합하여 흡착함으로써 염색 효과를 갖는 화장료 조성물을 제공하고자 한다.In order to improve the disadvantages and inconveniences of existing oxidative hair dyes, the present invention contains a large amount of natural hair dye ingredients, has excellent effects such as scalp protection and hair protection, and develops natural hair dye materials that are harmless to the human body and easy to use, and contain the materials It is intended to provide a composition having a function of preventing hair dyeing and color loss with a composition such as a general shampoo or rinse. In particular, the cosmetic composition according to the present invention is intended to provide a cosmetic composition having a dyeing effect by ionically bonding and adsorbing anionic natural components of natural extracts to cations of hair cuticles.

상기한 과제는, 결명자 추출물을 유효성분으로 포함하는 모발 색빠짐 방지 및 염색 효과를 갖는 모발용 화장료 조성물에 의해 달성된다.The above object is achieved by a cosmetic composition for hair containing Cassia tora extract as an active ingredient and having a hair color loss prevention and dyeing effect.

바람직하게는, 상기 결명자 추출물은 화장료 조성물 총 중량 대비 0.01 내지 30.0 중량%로 포함될 수 있다.Preferably, the Cassia tora extract may be included in 0.01 to 30.0% by weight based on the total weight of the cosmetic composition.

또한 바람직하게는, 상기 결명자 추출물은 75.0 %(v/v) 농도의 에탄올 수용액으로 45℃에서 추출된 것일 수 있다.Also preferably, the Cassia tora extract may be extracted at 45° C. with an aqueous ethanol solution having a concentration of 75.0% (v/v).

또한 바람직하게는, 상기 모발용 화장료 조성물은 pH가 4.5 내지 7.5일 수 있다.Also preferably, the cosmetic composition for hair may have a pH of 4.5 to 7.5.

또한 바람직하게는, 상기 모발용 화장료 조성물은 샴푸, 린스 및 헤어토닉으로 이루어진 군에서 선택된 제형을 갖는 것일 수 있다. Also preferably, the cosmetic composition for hair may have a formulation selected from the group consisting of shampoo, rinse and hair tonic.

삭제delete

도 1은 본 발명의 추출조건에 따른 반응표면분석 결과이다.
도 2는 본 발명의 제조예 1~4와 비교제조예1에 따라 염색한 모발의 사진이다.
도 3은 본 발명의 실험예 2에 따라 염색한 모발의 현미경 사진이다.
도 4는 본 발명의 실험예 4에 따라 pH에 따라 염색한 모발의 사진이다.
도 5는 본 발명의 실험예 5에 따라 모발의 색빠짐 방지 효과를 보여주는 사진이다.
1 is a response surface analysis result according to the extraction conditions of the present invention.
Figure 2 is a photograph of hair dyed according to Preparation Examples 1 to 4 and Comparative Preparation Example 1 of the present invention.
3 is a photomicrograph of hair dyed according to Experimental Example 2 of the present invention.
4 is a photograph of hair dyed according to pH according to Experimental Example 4 of the present invention.
5 is a photograph showing the effect of preventing color loss of hair according to Experimental Example 5 of the present invention.

본 발명에서 사용되는 모든 기술용어는, 달리 정의되지 않는 이상, 하기의 정의를 가지며 본 발명의 관련 분야에서 통상의 당업자가 일반적으로 이해하는 바와 같은 의미에 부합된다. 또한, 본 명세서에는 바람직한 방법이나 시료가 기재되나, 이와 유사하거나 동등한 것들도 본 발명의 범주에 포함된다.All technical terms used in the present invention, unless otherwise defined, have the following definitions and correspond to the meanings commonly understood by those of ordinary skill in the art related to the present invention. In addition, although preferred methods or samples are described in this specification, those similar or equivalent thereto are also included in the scope of the present invention.

용어 "약"이라는 것은 참조 양, 수준, 값, 수, 빈도, 퍼센트, 치수, 크기, 양, 중량 또는 길이에 대해 30, 25, 20, 15, 10, 9, 8, 7, 6, 5, 4, 3, 2 또는 1% 정도로 변하는 양, 수준, 값, 수, 빈도, 퍼센트, 치수, 크기, 양, 중량 또는 길이를 의미한다.The term "about" means a reference amount, level, value, number, frequency, percentage, dimension, size, amount, weight or length of 30, 25, 20, 15, 10, 9, 8, 7, 6, 5, means an amount, level, value, number, frequency, percentage, dimension, size, quantity, weight or length that varies by 4, 3, 2 or 1%.

본 명세서를 통해, 문맥에서 달리 필요하지 않으면, "포함하다" 및 "포함하는"이라는 말은 제시된 단계 또는 구성요소, 또는 단계 또는 구성요소들의 군을 포함하나, 임의의 다른 단계 또는 구성요소, 또는 단계 또는 구성요소들의 군이 배제되지는 않음을 내포하는 것으로 이해하여야 한다.Throughout this specification, unless the context requires otherwise, the terms "comprise" and "comprising" include a given step or component, or group of steps or components, but any other step or component, or It is to be understood that steps or groups of components are not excluded.

본 발명은 결명자 추출물을 유효성분으로 포함하는 모발 색빠짐 방지 및 염색 효과를 갖는 모발용 화장료 조성물에 관한 것이다.The present invention relates to a cosmetic composition for hair containing Cassia tora extract as an active ingredient and having a hair color loss prevention and dyeing effect.

결명자(Cassia Tora Seed)는 키가 1∼1.5m로, 잎은 우상복엽이고 2∼4쌍의 도란형이며, 7∼8월에 잎의 겨드랑이에서 노란 꽃이 핀다. 잎이 진 뒤에 약 10㎝ 정도 되는 활모양의 꼬투리가 열린다. 꼬투리 속에 윤기가 나는 종자가 한 줄로 들어 있는데, 이것을 결명자라고도 하고 차로 마시거나 약용으로 쓰인다. 종자는 길이 3∼6㎜, 지름 2∼3.5㎜의 기둥 모양이고, 모가 나 있으며 양측면에는 엷은 황갈색의 세로줄 및 띠가 있다. 종자에는 구부러진 어두운 색깔의 떡잎이 있다. 원산지는 미국이며, 우리나라의 각지에서 재배하고 있다. Cassia Tora Seed is 1 to 1.5 m tall, has pinnate leaves and 2 to 4 pairs of obovate leaves, and yellow flowers bloom from the axils of the leaves in July to August. After the leaves fall, a bow-shaped pod about 10 cm long opens. There is a row of shiny seeds in the pod, which is also called gyeolmyeongja and is drunk as tea or used for medicinal purposes. Seeds are columnar with a length of 3-6mm and a diameter of 2-3.5mm, with hairs, and light yellowish brown vertical lines and bands on both sides. Seeds have curved, dark-colored cotyledons. The country of origin is the United States, and it is cultivated in various parts of Korea.

결명(決明)이라는 이름은 눈을 밝게 해준다는 뜻에서 유래되었는데, 약효성분으로는 에모딘(emodin), 오브투시훠린(obtusifolin), 오브투신(obtusin) 등이 함유되어 있다. 동물실험 결과 혈압을 내려주는 효과가 인정되었고, 두꺼비를 이용한 실험에서는 혈관을 수축시키고, 그밖에 포도상구균, 대장균, 인플루엔자균 등의 발육을 억제시키는 효과가 있는 것으로 밝혀졌다. 약성은 서늘하고, 맛은 달고 써서 간염치료에 유효하고, 간경화로 인한 복수에 쓰이며, 간장의 병변으로 인한 안질에도 효과가 뛰어나다. 따라서 눈이 충혈되거나 햇빛을 볼 수 없을 정도로 시거나 눈물이 나오는 증상에 이용된다. 또 급성결막염, 각막혼탁 증세에도 쓰인다. 그밖에 이뇨, 변비 등에도 효능이 있어서 습관성변비, 고혈압 등의 치료제로 알려져 있다. The name Gyeolmyeong is derived from the meaning of brightening the eyes. It contains emodin, obtusifolin, and obtusin as active ingredients. As a result of animal experiments, the effect of lowering blood pressure was recognized, and in experiments using toads, it was found that there was an effect of constricting blood vessels and inhibiting the growth of Staphylococcus aureus, Escherichia coli, and influenza. The medicinal properties are cool, the taste is sweet and bitter, and it is effective in treating hepatitis, used for ascites due to cirrhosis of the liver, and is also effective in eye disease caused by lesions of the liver. Therefore, it is used for symptoms of bloodshot eyes or sore eyes that cannot see sunlight or tears. It is also used for acute conjunctivitis and corneal opacity. In addition, it is effective for diuresis and constipation, so it is known as a treatment for habitual constipation and high blood pressure.

본 발명은 상기와 같은 특징이 있는 결명자 추출물을 포함하는 것을 특징으로 하는 모발 천연염색제 화장료 조성물을 제공한다. The present invention provides a natural hair dye cosmetic composition comprising a Cassia tora extract having the above characteristics.

상기 결명자 추출물은, 물, 탄소수 1 내지 4인 알코올, 프로필렌글리콜, 부틸렌글리콜, 글리세린, 아세톤, 에틸 아세테이트, 클로로포름, 부틸 아세테이트, 디에틸에테르, 디클로로메탄, 헥산 및 이들의 혼합물로 구성된 군으로부터 선택되는 추출용매를 이용하여, 용매 추출법, 초임계 추출법 및 초음파 추출법 중 선택되는 어느 하나의 추출법을 통해 결명자로부터 추출될 수 있다. 바람직하게, 탄소수 1 내지 4인 알코올, 탄소수 1 내지 4인 알코올 내지 물을 사용하여 추출하는 것이 바람직하고, 가장 바람직하게는 75.0 %(v/v) 농도의 에탄올을 사용하여 45℃에서 추출할 수 있다.The Cassia tora extract is selected from the group consisting of water, alcohol having 1 to 4 carbon atoms, propylene glycol, butylene glycol, glycerin, acetone, ethyl acetate, chloroform, butyl acetate, diethyl ether, dichloromethane, hexane, and mixtures thereof Using an extraction solvent that is, it can be extracted from Cassia tora through any one extraction method selected from solvent extraction, supercritical extraction and ultrasonic extraction. Preferably, extraction is preferably performed using alcohol having 1 to 4 carbon atoms, alcohol having 1 to 4 carbon atoms or water, and most preferably, extraction can be performed at 45° C. using ethanol having a concentration of 75.0% (v/v). have.

본 발명의 화장료 조성물에 있어서, 상기 결명자 추출물은 화장료 조성물 전체 중량에 대하여 0.1~80 중량%로 함유되는 것이 좋고, 바람직하게는 1~30 중량%로 함유되는 것이 좋다.In the cosmetic composition of the present invention, the Cassia tora extract is preferably contained in an amount of 0.1 to 80% by weight, preferably 1 to 30% by weight, based on the total weight of the cosmetic composition.

한편, 본 발명의 두발용 조성물은 당업계에서 통상적으로 제조되는 어떠한 제형으로도 제조될 수 있으며, 일례로 샴푸, 린스, 헤어토닉 등으로 제형화될 수 있다. 다만, 반드시 이에 한정되는 것은 아니다. On the other hand, the composition for hair of the present invention may be prepared in any formulation commonly prepared in the art, and may be formulated into, for example, shampoo, rinse, hair tonic, and the like. However, it is not necessarily limited thereto.

이하, 본 발명의 내용에 대해 하기 실시예에서 더욱 상세히 설명하고자 한다. 다만, 본 발명의 권리범위가 하기 실시예에만 한정되는 것은 아니고, 이와 등가의 기술적 사상의 변형까지를 포함한다.Hereinafter, the contents of the present invention will be described in more detail in the following examples. However, the scope of the present invention is not limited only to the following examples, and includes modifications of equivalent technical ideas.

실험예 1: 결명자 추출물의 최적의 추출 조건 확인Experimental Example 1: Confirmation of Optimal Extraction Conditions for Cassia tora Extract

결명자의 주 색소 성분은 안트라퀴논계의 에모딘(Emodin), 카로테노이드계의 카로틴(Carotin) 및 플라보노이드계의 캠페롤(Kaempherol)등이 알려져 있다. 그 중 결명자로부터 최대 함량의 에모딘를 추출하는 공정의 모델링과 최적화를 위해 3-level-3-factor 실험계획인 Box-Behnken design과 반응표면분석법을 이용하였다. 추출공정에 중요한 독립변수(Xn)로 고려되는 인자 즉, 에탄올 농도(ethanol Concentration(%) : X1), 추출 온도(temperature : X2), 원물과 추출 용매의 비율(ratio : X3)을 요인변수로 하여, 3단계(-1, 0, 1)로 부호화하였으며, Box-behnken design에 따라, 하기 표 1과 같이 15구간으로 설정하여 추출실험을 실시하였다. 또한, 상기의 독립변수에 영향을 받는 종속변수는 에모딘의 함량(Y1)으로 측정하여 회귀분석을 실시하였다.The main pigment components of Cassia tora are anthraquinone-based Emodin, carotenoid-based carotin, and flavonoid-based Kaempherol. Among them, Box-Behnken design and response surface analysis, a 3-level-3-factor experimental design, were used to model and optimize the process of extracting the maximum content of emodine from Cassia tora. Factors considered as important independent variables (Xn) in the extraction process, that is, ethanol concentration (ethanol concentration (%): X1), extraction temperature (temperature: X2), and the ratio of raw material to extraction solvent (ratio: X3) are factor variables. Therefore, it was coded in three stages (-1, 0, 1), and according to the Box-behnken design, an extraction experiment was conducted by setting it to 15 sections as shown in Table 1 below. In addition, regression analysis was performed by measuring the dependent variable affected by the independent variable as the content of emodine (Y1).

반응표면분석에서 독립변수의 종속변수에 대한 2차 회귀식은 다음과 같았다.In the response surface analysis, the second-order regression equation for the dependent variable of the independent variable was as follows.

[수학식 1][Equation 1]

Y = b0 + b1X1 + b2X2 + b3X3 + b11X12+ b21X2X1 + b22X22+ b31X3X1 + b32X3X2 + b33X32Y = b0 + b1X1 + b2X2 + b3X3 + b11X12+ b21X2X1 + b22X22+ b31X3X1 + b32X3X2 + b33X32

여기서, Y는 종속변수, X1, X2, X3은 독립변수, b0는 절편, bn은 회귀계수이다. 추출특성의 모니터링과 최적조건범위 예측은 각 종속변수의 반응표면(response surfaces)을 이용하여 분석하였다.Here, Y is the dependent variable, X1, X2, and X3 are the independent variables, b0 is the intercept, and bn is the regression coefficient. Monitoring of extraction characteristics and prediction of optimal condition range were analyzed using response surfaces of each dependent variable.

결명자로부터 에모딘(Emodin)의 최적 추출조건을 설정하기 위해 용매조건, 추출온도, 원물과 추출용매의 비율을 독립변수로 하여 Box-behnken design에 의해 설계된 15구간의 추출조건을 표 1에 나타내었다. 또한, 각 추출물로부터 얻어진 에모딘 함량 즉, 종속변수의 결과는 표 2에 나타내었다. 이러한 실험결과를 이용하여 반응표면 회귀분석을 실시하고 종속변수에 대한 회귀식을 얻었다. 또한, 종속변수에 대한 최적 추출조건과 이에 따른 에모딘 함량을 예측하여 표 3에 나타내었다. 그리고 추출조건인 정제수 농도, 추출온도, 원물과 추출용매의 비율이 에모딘 함량에 미치는 영향을 확인하기 위해, 도 1에 반응표면 곡선으로 나타내었다.Table 1 shows the extraction conditions of 15 sections designed by the Box-behnken design with the solvent conditions, extraction temperature, and the ratio of the raw material and the extraction solvent as independent variables to set the optimal extraction conditions for Emodin from the defect. . In addition, the emodine content obtained from each extract, that is, the results of the dependent variable are shown in Table 2. Response surface regression analysis was performed using these experimental results, and regression equations for dependent variables were obtained. In addition, the optimal extraction conditions for the dependent variable and the corresponding emodine content were predicted and shown in Table 3. In addition, in order to confirm the effect of the extraction conditions, the concentration of purified water, the extraction temperature, and the ratio of raw material and extraction solvent on the emodine content, a response surface curve is shown in FIG. 1.

Figure 112022056228764-pat00001
Figure 112022056228764-pat00001

Figure 112022056228764-pat00002
Figure 112022056228764-pat00002

Figure 112022056228764-pat00003
Figure 112022056228764-pat00003

Box-behnken design에 의한 추출 조건별 Emodin 함량은 표 2에 나타낸 바와 같았고, 결과에 대한 반응표면 회귀식은 아래 수학식 2와 같다.The Emodin content for each extraction condition according to the Box-behnken design was as shown in Table 2, and the response surface regression equation for the results is shown in Equation 2 below.

[수학식 2][Equation 2]

Emodin= -109.170 + 2.4600X1 -2.72917X2 + 5.34333 X3 -0.02577 X1 2 -0.00729 X2 2 -0.03366 X3 2 + 0.07750 X1 X2 - 0.00533 X1 X3 -4.50787X2 X3 Emodin= -109.170 + 2.4600X 1 -2.72917X 2 + 5.34333 X 3 -0.02577 X 1 2 -0.00729 X 2 2 -0.03366 X 3 2 + 0.07750 X 1 X 2 - 0.00533 X 1 X 3 -4.50787X 2 X

에모딘 함량에 대한 회귀식은 R2은 0.973로 높은 상관관계를 보였고, 5% 이내에서 유의성이 인정되었다(표 4).The regression equation for emodine content showed a high correlation with R2 of 0.973, and significance was recognized within 5% (Table 4).

Figure 112022056228764-pat00004
Figure 112022056228764-pat00004

도 1에 나타낸 반응표면 그래프를 보면, 추출조건 중 추출용매 (에탄올 농도)가 에모딘 함량에 가장 큰 영향을 주었으며, 에탄올 농도가 높아질수록, 즉, 정제수 함량이 낮아질수록 에모딘의 함량이 증가하는 경향을 나타내었다.Looking at the response surface graph shown in FIG. 1, the extraction solvent (ethanol concentration) among the extraction conditions had the greatest effect on the emodine content, and the higher the ethanol concentration, that is, the lower the purified water content, the higher the emodine content. showed a trend.

반응표면분석에 따라 예측된 에모딘의 최대값은 143.993 ppm으로 예측되었고, 이때의 추출조건은 시료에 대한 에탄올 농도 75.00 %(v/v), 추출온도 45℃, 추출시간 7.00h으로 각각 결정되었다. 즉, 100 %(v/v) 에탄올에 가까운 용매에 45℃에서 7시간 추출할 경우 가장 높은 수율의 에모딘을 얻을 수 있는 것으로 나타났다.The maximum value of emodine predicted according to the response surface analysis was predicted to be 143.993 ppm, and the extraction conditions at this time were determined as ethanol concentration of 75.00% (v / v), extraction temperature of 45 ° C, and extraction time of 7.00 h for the sample. . That is, it was found that the highest yield of emodin could be obtained when extraction was performed at 45° C. for 7 hours in a solvent close to 100% (v/v) ethanol.

이상의 결과로써, 결명자로부터 최대 에모딘 함량을 갖는 추출공정은 추출조건 즉, 에탄올 농도, 추출온도, 추출시간 비율에 영향을 받은 것으로 확인되었고, 특히 추출용매인 에탄올의 농도에 영향을 크게 받는 것으로 확인되었다. 또한, 추출조건에 따른 에모딘 함량을 설명하는 유의성을 가진 회귀식이 수립되었고, 에모딘 추출에 최적인 추출조건을 결정할 수 있었다.As a result of the above, it was confirmed that the extraction process with the maximum emodin content from Cassia tora was affected by the extraction conditions, that is, the ethanol concentration, extraction temperature, and extraction time ratio, and was particularly affected by the concentration of ethanol, the extraction solvent. It became. In addition, a regression equation with significance explaining the emodine content according to the extraction conditions was established, and the optimal extraction conditions for emodine extraction could be determined.

실시예 1~4: 결명자 추출물(Natural Hair Hybrid)의 제조Examples 1-4: Preparation of Cassia tora Extract (Natural Hair Hybrid)

결명자 200g을 분쇄하여 분쇄물을 제조하였다. 상기 분쇄물을 4개로 분리한 후, 30 %(v/v), 50 %(v/v), 75 %(v/v), 100 %(v/v) 농도의 에탄올 2000 g을 각각 첨가한 후, 냉각콘덴서가 부착된 추출기에서, 45℃ 온도로 7시간 동안 가열하여 추출하였다. 상기 각 추출물을 400메쉬(mesh) 여과포로 여과한 후, 와트만 2번 여과지로 다시 한 번 여과하였다. 그 후, 냉각콘덴서가 달린 증류장치로 40℃ 온도에서 감압 농축하였으며, 잔사에 대하여 동일한 조건으로 1회 더 반복 실시하여, 실시예 1~4의 결명자 추출물을 각각 제조하였다(표 5). 200 g of Cassia tora was pulverized to prepare a pulverized product. After separating the pulverized product into four pieces, 2000 g of ethanol at concentrations of 30% (v/v), 50% (v/v), 75% (v/v), and 100% (v/v) was added, respectively. Then, in an extractor equipped with a cooling condenser, extraction was performed by heating at 45° C. for 7 hours. After filtering each of the above extracts with a 400 mesh filter cloth, it was filtered again with Whatman No. 2 filter paper. After that, it was concentrated under reduced pressure at a temperature of 40 ° C using a distillation apparatus equipped with a cooling condenser, and the residue was repeated once more under the same conditions to prepare Cassia tora extracts of Examples 1 to 4, respectively (Table 5).

구분division 실시예 1Example 1 실시예 2Example 2 실시예 3Example 3 실시예 4Example 4 에탄올 농도ethanol concentration 75 %(v/v)75% (v/v) 100 %(v/v)100% (v/v) 50 %(v/v)50% (v/v) 30 %(v/v)30% (v/v)

실험예 1:Experimental Example 1: 결명자 추출물(Natural Hair Hybrid)의 에모딘 함량 분석Analysis of Emodin Content of Cassia tora Extract (Natural Hair Hybrid)

상기 실시예 1~4에서 제조된 결명자 추출물의 에모딘의 함량은 0.45μm 필터를 거친 추출물을 HPLC (Waters 2695)를 이용하여 분석하였다. 이때, 분석조건으로 컬럼은 Optimapak C18 250 - 4.6 μm, 이동상은 25% ACN, 75% DW, 유속은 1.0 ml/min, 검출기는 UV(254 nm)를 각각 사용하였다. 정량은 외부표준법으로 검량선을 작성하여 실시하였다. 즉, 표준물질 Emodin를 메탄올에 녹여 1000 ppm으로 한 후, 이 액을 희석하여 500, 250, 125 ppm별로 표준용액을 조제하고, HPLC로 분석한 후, 검량선을 작성하여 정량하였다. 측정 결과, 에탄올 농도가 75 (v/v)%인 실시예 1의 에모딘 함량이 가장 높았다.The content of emodin in the Cassia tora extracts prepared in Examples 1 to 4 was analyzed using HPLC (Waters 2695) for the extracts that had passed through a 0.45 μm filter. At this time, as the analysis conditions, Optimapak C18 250 - 4.6 μm was used as the column, 25% ACN and 75% DW as the mobile phase, 1.0 ml/min as the flow rate, and UV (254 nm) as the detector. Quantification was performed by creating a calibration curve using an external standard method. That is, after dissolving the standard substance Emodin in methanol to 1000 ppm, diluting this solution to prepare standard solutions for each 500, 250, and 125 ppm, analyzing by HPLC, and then preparing a calibration curve for quantification. As a result of the measurement, the emodin content of Example 1 having an ethanol concentration of 75 (v/v)% was the highest.

성분ingredient 실시예 1Example 1 실시예 2Example 2 실시예 3Example 3 실시예 4Example 4 에모딘 함량 (ppm)Emodine content (ppm) 148148 127127 124124 9898

실험예 2: 염색 효과 분석Experimental Example 2: Analysis of staining effect

상기 실시예 1~4에서 수득한 결명자 추출물을 1 중량%가 되도록 정제수로 희석하여 제조예 1~4를 각각 제조하였다. 또한, 에모딘(시그마알드리치, cas no. 518-82-1)을 1,000ppm 함유된 비교제조예 1을 제조하였다.Preparation Examples 1 to 4 were prepared by diluting the Cassia tora extract obtained in Examples 1 to 4 with purified water to 1% by weight. In addition, Comparative Preparation Example 1 containing 1,000 ppm of Emodin (Sigma Aldrich, cas no. 518-82-1) was prepared.

성분(중량%)Ingredients (% by weight) 제조예 1Preparation Example 1 제조예 2Preparation Example 2 제조예 3Preparation Example 3 제조예 4Production Example 4 비교제조예 1Comparative Preparation Example 1 실시예 1Example 1 1.01.0 -- -- -- -- 실시예 2Example 2 -- 1.01.0 -- -- -- 실시예 3Example 3 -- -- 1.01.0 -- -- 실시예 4Example 4 -- -- -- 1.01.0 -- 에모딘Emodin -- -- -- -- 1000 ppm1000 ppm 정제수Purified water 잔량balance 잔량balance 잔량balance 잔량balance 잔량balance total 100.0 100.0 100.0100.0 100.0100.0 100.0100.0 100.0100.0

백모(브랜드 TV헤어마트, OM2LSW)를 물로 세척한 후, 제조예 1~4와 비교제조예 1을 샴푸를 사용하는 방법으로 약 2분간 도포한 후 물로 헹군 뒤 건조하는 과정을 매일 1번씩 7일간 반복한 후 백모가 염색되는 효과를 확인하였다. 그 결과를 도 2에 나타냈다.After washing white hair (Brand TV Hair Mart, OM2LSW) with water, Preparation Examples 1 to 4 and Comparative Preparation Example 1 were applied using shampoo for about 2 minutes, then rinsed with water and dried once a day for 7 days. After repetition, the effect of dyeing gray hair was confirmed. The results are shown in FIG. 2 .

그 결과, 제조예 1>제조예 3>제조예 2=제조예 4>비교제조예 1(에모딘 1000ppm) 순으로 염색효과의 차이를 보이는 것을 확인하였다. 차이가 크진 않았지만, 에모딘 함량이 가장 많이 추출되는 조건으로 추출된 결명자 추출물을 포함하는 경우(제조예 1), 가장 좋은 염색 효과를 발휘하였다. As a result, it was confirmed that the difference in dyeing effect was shown in the order of Preparation Example 1> Preparation Example 3> Preparation Example 2 = Preparation Example 4> Comparative Preparation Example 1 (Emodin 1000ppm). Although the difference was not large, the best dyeing effect was exhibited when the Cassia tora extract extracted under the condition that the most emodin content was extracted (Preparation Example 1) was included.

또한, 도 3은 염색 전 백마와 제조예 1로 7일간 염색한 후의 모발의 현미경 사진이다. 도 3을 보면, 제조예 1을 7일간 사용한 후, 백모가 염색된 것을 확인할 수 있다.3 is a photomicrograph of hair after dyeing for 7 days with white horse before dyeing and Preparation Example 1. Referring to FIG. 3, after using Preparation Example 1 for 7 days, it can be confirmed that gray hair is dyed.

실험예 3: pH 변화에 따른 결명자 추출물(Natural Hair Hybrid)의 염색 효과Experimental Example 3: Dyeing effect of Cassia tora extract (Natural Hair Hybrid) according to pH change

결명자 추출물의 pH에 따른 염색 효과를 확인하기 위해, 산성, 중성, 염기성이 되도록 pH를 조절하여 염색 효과를 확인하였다. 각각의 pH 조정은 씨트릭산 및 염화나트륨을 이용하였다.In order to confirm the dyeing effect according to the pH of Cassia tora extract, the dyeing effect was confirmed by adjusting the pH to be acidic, neutral, or basic. Each pH adjustment used citric acid and sodium chloride.

실시예 1의 결명자 추출물이 1중량% 포함된 조성물을 pH별로 준비하고 탈색모에 2~3분간 도포한 후, 물로 헹군 뒤 건조하는 과정을 매일 1번씩 7일간 반복한 후 반복 사용에 따른 염색 효과를 확인하였다. 그 결과를 도 4에 나타냈다. 도 4를 보면, pH 7일 때, 염색 효과가 가장 우수한 것을 확인하였다. A composition containing 1% by weight of the Cassia tora extract of Example 1 was prepared by pH, applied to bleached hair for 2 to 3 minutes, rinsed with water, and then dried once a day for 7 days. After repeated use, the dyeing effect Confirmed. The results are shown in FIG. 4 . Referring to Figure 4, it was confirmed that the dyeing effect was the best when the pH was 7.

성분(중량%)Ingredients (% by weight) 제조예 5Preparation Example 5 제조예 6Preparation Example 6 제조예 7Preparation Example 7 결명자추출물
(실시예 1)
Cassia tora Extract
(Example 1)
1.01.0 1.01.0 1.01.0
씨트릭산/염화나트륨Citric Acid/Sodium Chloride 적량Appropriate amount 적량Appropriate amount -- 정제수Purified water 잔량balance 잔량balance 잔량balance total 100.0 100.0 100.0 100.0 100.0100.0 pH 측정값pH reading 4.04.0 7.07.0 10.010.0

제형예 1: 결명자 추출물(Natural Hair Hybrid)을 포함하는 샴푸 조성물 제조Formulation Example 1: Preparation of Shampoo Composition Containing Cassia tora Extract (Natural Hair Hybrid)

상기 실시예 1에서 수득한 결명자 추출물이 1 중량% 포함되고, 샴푸 제형으로 제조한 제형예 1을 하기 표 9에 나타냈다. Formulation Example 1 containing 1% by weight of Cassia tora extract obtained in Example 1 and prepared as a shampoo formulation is shown in Table 9 below.

성분(중량%)Ingredients (% by weight) 제형예 1Formulation example 1 결명자추출물
(실시예 1)
Cassia tora Extract
(Example 1)
1.01.0
다이소듐이디티에이Disodium EDT 0.030.03 폴리쿼터늄-10Polyquaternium-10 0.10.1 암모늄라우릴설페이트Ammonium Lauryl Sulfate 40.540.5 암모늄라우레스설페이트Ammonium Laureth Sulfate 15.515.5 코카미도프로필베타인Cocamidopropyl Betaine 6.06.0 프로필렌글라이콜propylene glycol 2.02.0 소듐크실렌설포네이트sodium xylene sulfonate 2.02.0 글라이콜다이스테아레이트Glycol Distearate 3.03.0 코카마이드디이에이Cocamide DEA 1.01.0 라우라마이드디이에이Lauramide DEA 1.01.0 살리실산salicylic acid 0.130.13 디메티콘dimethicone 3.03.0 방부제antiseptic 적량Appropriate amount incense 적량Appropriate amount 정제수Purified water 잔량balance total 100.0 100.0

실험예 4: 모발의 색빠짐 방지 효과Experimental Example 4: Effect of preventing color loss of hair

모발 염색은 시중에서 판매중인 백모를 TV헤어마트(카다로그번호,OM2LSW)를 통해 구입하였다. 시중에서 새치커버 흑갈색3.0(려 자양윤모)을 구매하여 산화형 염모제인 1제 염모제와 2제 산화제를 섞은 후 백모에 15분간 도포한 후 물로 헹군 뒤 건조하여 백모를 염색하였다. For hair dyeing, commercially available white hair was purchased through TV Hair Mart (catalog number, OM2LSW). Gray hair cover dark brown 3.0 (Ryo Jayangyunmo) was purchased on the market, and after mixing the first hair dye and the second oxidizing agent, which are oxidation-type hair dyes, it was applied to white hair for 15 minutes, rinsed with water, and dried to dye gray hair.

이후 일반 샴푸, 상기 제형예 1의 샴푸로 각각 세척한 후 흐르는 물로 맑은 물이 나올 때까지 헹구는 과정을 매일 2번씩 30일간 반복한 후 초기 색상과 색차계로 색상을 비교하여, 모발 색빠짐을 확인하였다. 색빠짐 결과를 도 5에 나타냈다. 도 5를 보면, 결명자 1.0 중량%를 포함하는 샴푸에서 색빠짐 방지 효과가 있는 걸로 확인하였다. 일반샴푸는 색빠짐이 증가하지만 결명자추출물을 함유한 샴푸의 경우 모발 코팅으로 인한 색빠짐방지 효과가 우수한 것을 확인하였다. Thereafter, after washing with the general shampoo and the shampoo of Formulation Example 1, the process of rinsing with running water until clear water came out was repeated twice a day for 30 days, and then the initial color was compared with the color difference meter to confirm hair color loss. . The color loss results are shown in FIG. 5 . Referring to Figure 5, it was confirmed that there is an effect of preventing color loss in the shampoo containing 1.0% by weight of Cassia tora. General shampoo increased color loss, but in the case of shampoo containing Cassia tora extract, it was confirmed that the effect of preventing color loss due to hair coating was excellent.

제형예 2: 결명자 추출물(Natural Hair Hybrid)을 포함하는 린스 조성물 제조Formulation Example 2: Preparation of rinse composition containing Cassia tora extract (Natural Hair Hybrid)

상기 실시예 1에서 수득한 결명자 추출물이 1.0 중량% 포함되고, 린스 제형으로 제조한 제형예 2를 하기 표 10에 나타냈다. Formulation Example 2 containing 1.0% by weight of Cassia tora extract obtained in Example 1 and prepared as a rinse formulation is shown in Table 10 below.

성분(중량%)Ingredients (% by weight) 제형예 2Formulation Example 2 결명자추출물
(실시예 1)
Cassia tora Extract
(Example 1)
1.01.0
다이소듐이디티에이Disodium EDT 0.020.02 하이드록시에틸셀룰로오스Hydroxyethyl Cellulose 0.20.2 판테놀panthenol 0.050.05 프로필렌글라이콜propylene glycol 1.51.5 글리세린glycerin 2.02.0 세틸알코올cetyl alcohol 3.53.5 스테아릴알코올Stearyl Alcohol 1.51.5 글리세릴스테아레이트에스이Glyceryl Stearate SE 0.50.5 디메치콘dimethicone 1.51.5 방부제antiseptic 적량Appropriate amount incense 적량Appropriate amount 정제수Purified water 잔량balance total 100.0 100.0

제형예 3: 결명자 추출물(Natural Hair Hybrid)을 포함하는 헤어토닉 조성물 제조Formulation Example 3: Preparation of hair tonic composition containing Cassia tora extract (Natural Hair Hybrid)

상기 실시예 1에서 수득한 결명자 추출물이 1.0 중량% 포함되고, 헤어토닉 제형으로 제조한 제형예 3을 하기 표 11에 나타냈다. Formulation Example 3 containing 1.0% by weight of Cassia tora extract obtained in Example 1 and prepared as a hair tonic formulation is shown in Table 11 below.

성분(중량%)Ingredients (% by weight) 제형예 3Formulation Example 3 결명자추출물
(실시예 1)
Cassia tora Extract
(Example 1)
1.01.0
다이소듐이디티에이Disodium EDT 0.020.02 판테놀panthenol 0.50.5 부틸렌글라이콜Butylene Glycol 10.010.0 에탄올ethanol 18.018.0 멘톨menthol 0.030.03 폴리솔베이트 80Polysorbate 80 1.01.0 이미다졸리디닐우레아imidazolidinyl urea 0.20.2 바이오틴biotin 0.10.1 incense 적량Appropriate amount 정제수Purified water 잔량balance total 100.0 100.0

실험예 5: 염색 효과와 색빠짐 방지 효과 만족도 조사Experimental Example 5: Investigation of Satisfaction with Dyeing Effect and Color Loss Prevention Effect

새치가 있는 피험자 30명을 2그룹으로 나누고, 제형예 1의 샴푸(실험군)와 일반 샴푸(대조군)를 30일간 사용하게 하고 염색효과와 색빠짐 방지 효과에 대한 결과에 대한 만족도 조사하였다. 그 결과는 아래의 표 12에 나타내었다. 표 12를 보면, 제형예 1의 샴푸를 사용한 그룹에서 다수의 사용자가 염색 효과와 색빠짐 방지 효과에서 “매우 좋음” 평가를 하였다. 30 subjects with gray hair were divided into 2 groups, and the shampoo (experimental group) and general shampoo (control group) of Formulation Example 1 were used for 30 days, and the satisfaction with the results of the dyeing effect and the color loss prevention effect was investigated. The results are shown in Table 12 below. Referring to Table 12, a number of users in the group using the shampoo of Formulation Example 1 gave a “very good” evaluation in the dyeing effect and color loss prevention effect.

구분 division 대조군control group 실험군experimental group 염색 효과dye effect 매우 좋음very good 00 1212 좋음good 44 1616 변화 없음no change 2626 22 색빠짐 방지 효과Color fading prevention effect 매우 좋음very good 22 1919 좋음good 1010 1010 변화 없음no change 1818 1One

Claims (5)

결명자 추출물을 유효성분으로 포함하는 모발용 화장료 조성물로서, 상기 모발용 화장료 조성물은 pH가 4.5 내지 7.5이고, 샴푸, 린스 및 헤어토닉으로 이루어진 군에서 선택된 제형을 갖는 것을 특징으로 하는 모발 색빠짐 방지 및 염색 효과를 갖는 모발용 화장료 조성물.A cosmetic composition for hair containing Cassia tora extract as an active ingredient, wherein the cosmetic composition for hair has a pH of 4.5 to 7.5 and has a formulation selected from the group consisting of shampoo, rinse and hair tonic, characterized in that it has a hair color loss prevention and dyeing effect A cosmetic composition for hair having a. 제1항에 있어서,
상기 결명자 추출물은 화장료 조성물 총 중량 대비 0.01 내지 30.0 중량%로 포함되는 것을 특징으로 하는 모발용 화장료 조성물.
According to claim 1,
The Cassia tora extract is a cosmetic composition for hair, characterized in that contained in 0.01 to 30.0% by weight relative to the total weight of the cosmetic composition.
제1항에 있어서,
상기 결명자 추출물은 75.0 %(v/v) 농도의 에탄올 수용액으로 45℃에서 추출된 것을 특징으로 하는 모발용 화장료 조성물.
According to claim 1,
The Cassia tora extract is a cosmetic composition for hair, characterized in that extracted at 45 ℃ with an ethanol aqueous solution of 75.0% (v / v) concentration.
삭제delete 삭제delete
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20100114649A (en) * 2009-04-16 2010-10-26 주식회사 더마랩 Hairdye
KR101663285B1 (en) * 2015-08-13 2016-10-06 정정임 Method for manufacturing herbal shampoo

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20100114649A (en) * 2009-04-16 2010-10-26 주식회사 더마랩 Hairdye
KR101663285B1 (en) * 2015-08-13 2016-10-06 정정임 Method for manufacturing herbal shampoo

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