KR102080940B1 - The active ingredient-adsorbed citrus biogel and the preparing method thereof - Google Patents

The active ingredient-adsorbed citrus biogel and the preparing method thereof Download PDF

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KR102080940B1
KR102080940B1 KR1020170160821A KR20170160821A KR102080940B1 KR 102080940 B1 KR102080940 B1 KR 102080940B1 KR 1020170160821 A KR1020170160821 A KR 1020170160821A KR 20170160821 A KR20170160821 A KR 20170160821A KR 102080940 B1 KR102080940 B1 KR 102080940B1
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citrus
cellulose gel
mask pack
adsorbed
hesperidin
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KR20190061925A (en
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김상숙
박경진
최영훈
안현주
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대한민국
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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
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/731Cellulose; Quaternized cellulose derivatives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0212Face masks
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
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    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/347Phenols
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/49Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/4973Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
    • A61K8/498Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom having 6-membered rings or their condensed derivatives, e.g. coumarin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/60Sugars; Derivatives thereof
    • A61K8/602Glycosides, e.g. rutin
    • 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
    • A61Q19/00Preparations for care of the skin

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Abstract

본 발명은 셀룰로오스겔을 포함하는 마스크팩에 있어서, 상기 마스크팩은 셀룰로오스겔의 표면에 꿩의 비름 추출물이 흡착된 마스크팩을 제공한다. 본 발명의 마스크팩은 뛰어난 항산화 활성을 갖는다. The present invention provides a mask pack comprising a cellulose gel, wherein the mask pack provides a mask pack in which the sperm extract of Pheasant is adsorbed on the surface of the cellulose gel. The mask pack of the present invention has excellent antioxidant activity.

Description

활성 성분이 흡착된 감귤 바이오겔 및 이를 생산하는 방법{The active ingredient-adsorbed citrus biogel and the preparing method thereof}The active ingredient-adsorbed citrus biogel and the preparing method

본 발명은 감귤 바이오겔에 활성 성분을 흡착시키는 방법 및 이러한 방법을 통해 활성 성분이 흡착된 감귤 바이오겔에 관한 것으로, 더욱 구체적으로 감귤 바이오겔에 항산화 성분을 흡착시켜 피부 투과율을 높일 수 있는 방법 및 이러한 감귤 바이오겔을 생산하는 방법에 것이다. The present invention relates to a method of adsorbing an active ingredient to a citrus biogel and a citrus biogel to which the active ingredient is adsorbed through such a method, and more particularly, a method of increasing the skin permeability by adsorbing an antioxidant component to the citrus biogel and It would be on the way to produce these citrus biogels.

셀룰로오스는 자연계에 가장 풍부한 생체 물질 자원으로 특히, 초산균이 생성하는 셀룰로오스는 식품의 첨가제뿐만 아니라, 고부가가치의 산업용 신소재로 많은 주목을 받고 있다. 초산균이 셀룰로오스를 생산한다는 사실이 보고된 이래(Brown. A. J., J. Chem. Soc., vol. 49, pp. 432-439,1986), 미생물에 의해 생산되는 셀룰로오스(Bacterial Cellulose)는 신소재로서 끊임없는 연구 대상이 되어 왔다. Cellulose is one of the most abundant biological materials in nature. In particular, cellulose produced by acetic acid bacteria has attracted much attention not only as an additive of food but also as a new value-added industrial new material. Since it has been reported that acetic acid bacteria produce cellulose (Brown. AJ, J. Chem. Soc., Vol. 49, pp. 432-439, 1986), cellulose produced by microorganisms (Bacterial Cellulose) is a new material. Has not been studied.

특히 초산균이 생성하는 셀룰로오스를 이용한 마스크팩은 화장품업계에서 고부가가치를 인정받고 있다. 셀룰로오스를 이용한 마스크팩은 피부 밀착력이 높고 자연유래 친환경소재로 수요자들에게 큰 호응을 얻고 있다. In particular, mask packs using cellulose produced by acetic acid bacteria have been recognized in the cosmetic industry for high added value. Cellulose mask packs have high skin adhesion and have a great response from consumers with nature-friendly eco-friendly materials.

한편 화장품 분야에서 시트(sheet) 타입의 마스크팩은 손으로 화장료를 바를 필요 없이 특정 형태로 제작된 시트를 인체에 붙이는 제품이다. Meanwhile, in the cosmetics field, a sheet type mask pack is a product that attaches a sheet made in a specific form to a human body without applying cosmetics by hand.

시트 타입의 팩은 일반적인 화장유액에 비해서 오랫동안 피부에 작용할 수 있도록 유액을 담지할 수 있는 지지체를 갖고 있고, 해당 지지체가 제공하는 폐쇄효과(Occlusive effect)에 의한 피부 효능 성분의 피부침투효과 증진으로 인해 보습효과, 피부미용효과가 탁월한 화장 제품이다. 사용감, 착용감, 효능 등에 있어서 차별화하기 위한 다양한 소재연구가 시도되고 있다.Sheet-type packs have a support that can hold the fluid so that it can act on the skin for a long time as compared to a general cosmetic emulsion, and due to the enhancement of the skin penetration effect of the skin efficacy ingredient by the occlusive effect provided by the support It is a cosmetic product with excellent moisturizing effect and skin beauty effect. Various materials research for differentiation in feeling of use, fit, efficacy, etc. has been attempted.

그러나 시트 타입의 마스크팩은 제조과정에서 투입된 유효성분이 마스크팩 1회 제공량에 모두 포함되지 못하고, 화장유액에 잔류한채로 버려지는 문제가 있다. However, the mask pack of the sheet type does not include all of the active ingredients introduced in the manufacturing process once the mask pack is provided, there is a problem that is discarded while remaining in the cosmetic oil.

따라서 본 발명이 이루고자 하는 기술적 과제는 활성 성분을 마스크팩에 흡착시켜 피부로 전달되는 활성성분의 양을 향상시키는 것을 목적으로 한다. Therefore, an object of the present invention is to improve the amount of the active ingredient is delivered to the skin by adsorbing the active ingredient in the mask pack.

본 발명은 항산화 활성이 뛰어난 활성 성분들을 감귤 바이오겔에 흡착시키는 방법을 제공하고자 한다. The present invention is to provide a method for adsorbing the active ingredient with excellent antioxidant activity to citrus biogel.

본 발명은 상기와 같은 문제점을 해결하기 위하여, 셀룰로오스겔에 활성 성분을 흡착시킨 것을 특징으로 하는 마스크팩을 제공하고자 한다. The present invention to solve the above problems, to provide a mask pack characterized in that the active ingredient is adsorbed on the cellulose gel.

본 발명은 셀룰로오스겔을 포함하는 마스크팩에 있어서, 셀룰로오스겔의 표면에 꿩의 비름 추출물이 흡착된 마스크팩을 제공하고자 한다. The present invention provides a mask pack containing a cellulose gel, wherein the pheasant extract of the pheasant is adsorbed on the surface of the cellulose gel.

바람직한 실시예에서, 본 발명은 셀룰로오스겔의 표면에 꿩의 비름 추출물, 바람직하게 폴리페놀, 카로티노이드 등의 성분, 더 바람직하게 헤스페리딘, 쿼세틴, 레스베라트롤, 이소플라본, 카테킨 등의 폴리페놀, 카로티노이드 등이 흡착된 마스크팩을 제공하고자 한다. In a preferred embodiment, the present invention is adsorbed on the surface of the cellulose gel adsorbed by the pheasant extract, preferably polyphenols, carotenoids and other components, more preferably hesperidin, quercetin, resveratrol, isoflavones, catechins and other polyphenols, carotenoids and the like To provide a mask pack.

상기 셀룰로오스겔은 감귤 유래 셀룰로오스겔일 수 있다. 셀룰로오스겔은 코코넛 유래 셀룰로오스겔 등이 존재하나, 특히 감귤 유래 셀룰로오스겔을 이용할 때 활성 성분의 흡착이 탁월한 것을 발견하고 본 발명을 완성하게 되었다. The cellulose gel may be a citrus cellulose gel. The cellulose gel is present in coconut-derived cellulose gel, etc., in particular, the use of citrus-derived cellulose gel was found to be excellent in the adsorption of the active ingredient to complete the present invention.

본 명세서에서 사용된 ‘흡착’은 셀룰로오스겔의 표면에 목적으로 하는 성분이 모여있는 현상을 의미하는 것으로 이해될 수 있다. 셀룰로오스겔의 기공(pore)의 영향으로 기공이 형성된 부분의 표면에 목적으로 하는 성분이 모여있는 것으로 보여질 수 있으므로 셀룰로오스겔의 내부에 목적으로 하는 성분이 포함될 수 있고, 이 경우도 본 발명의 범위에서 배제되지 않는 것으로 이해될 수 있다. As used herein, the term "adsorption" may be understood to mean a phenomenon in which a target component is collected on the surface of a cellulose gel. Due to the influence of pores of the cellulose gel, it can be seen that the target components are gathered on the surface of the portion where the pores are formed, the target components can be included in the interior of the cellulose gel, even in this case the scope of the present invention It can be understood that it is not excluded from.

본 명세서에서 사용된 ‘셀룰로오스겔’은 감귤 착즙액 또는 감귤 착즙 후 잔류하는 부산물을 이용하여 제조된 셀룰로오스겔을 의미하며, 예를 들어, 감귤 착즙액 또는 감귤 착즙 후 남은 남은 잔류물을 배지로 하여 상기 배지에 글루콘아세토박터 속(Gluconacetobacter sp.) gel_SEA623-2(KACC 91526P)를 접종하여 생산된 셀룰로오스겔을 의미하는 것으로 이해될 수 있다. 'Cellulose gel' as used herein refers to a cellulose gel prepared by using citrus juice or by-products remaining after citrus juice, and, for example, by using as a medium the residual residue remaining after citrus juice or citrus juice. Gluconacetobacter sp. Gel_SEA623-2 (KACC 91526P) inoculated in the medium can be understood to mean a cellulose gel produced.

본 발명의 발명자들은 꿩의 비름 추출물이 뛰어난 항산화 활성을 가지고 있음에도 마스크팩을 이용하여 전달이 용이하지 않다는 것을 확인하고 본 발명을 완성하게 되었다. The inventors of the present invention confirmed that the pheasant extract of Pheasant has excellent antioxidant activity, but it is not easy to deliver using a mask pack, and thus, the present invention has been completed.

본 발명의 발명자들은 셀룰로오스겔에 일정한 처리를 가하였을 때, 꿩의 비름 추출물이 셀룰로오스겔의 표면에 흡착되어 피부로 용이하게 전달할 수 있다는 것을 확인하고 본 발명을 완성하게 되었다. The inventors of the present invention have confirmed that when a certain treatment is applied to the cellulose gel, the sperm extract of the pheasant is adsorbed on the surface of the cellulose gel and can be easily delivered to the skin, thereby completing the present invention.

특히 감귤 유래 셀룰로오스겔은 겔의 탄력성이 뛰어나고, 쉽게 변형되지 않는 특성으로 인해 본 발명의 목적에 특히 탁월하다는 것을 확인하게 되었다. In particular, citrus-derived cellulose gel has been found to be particularly excellent for the purpose of the present invention because of the excellent elasticity of the gel and the property of not being easily deformed.

바람직하게 상기 꿩의 비름 추출물은 플라보노이드. 카포티노이드 등의 항산화 성분들을 다량 함유하고 있고, 특히 쿼세틴, 카로틴, 헤스페리딘 등을 다량 포함하며, 본 발명의 처리 방법을 통해 감귤 유래 셀룰로오스 겔 표면에 헤스페리딘의 흡착이 용이하다는 것을 확인하게 되었다. Preferably the sperm extract of the pheasant is a flavonoid. It contains a large amount of antioxidant components, such as capotenoid, and particularly contains a large amount of quercetin, carotene, hesperidin and the like, and it was confirmed that the adsorption of hesperidin on the citrus-derived cellulose gel surface through the treatment method of the present invention.

본 발명의 일 실시예를 통해서 헤스페리딘이 마스크팩 표면에 흡착되어 피부로 전달되는 마스크팩을 제공할 수 있다. Through one embodiment of the present invention it is possible to provide a mask pack in which hesperidin is adsorbed on the surface of the mask pack and delivered to the skin.

본 발명의 일 실시예에 따르면, 꿩의 비름 추출물 및 셀룰로오스겔을 포함하는 마스크팩을 제조하는 방법을 제공할 수 있다. According to one embodiment of the present invention, it is possible to provide a method of manufacturing a mask pack comprising a sperm extract and cellulose gel of pheasant.

바람직하게 상기 셀룰로오스겔은 S1) 셀룰로오스겔을 산성 용액에 침지시키는 단계, 및 (S2) 상기 (S1) 단계에서 침지된 셀룰로오스겔을 꿩의 비름 추출물이 함유된 화장료 조성물에 침지시키는 단계를 거칠 수 있다. Preferably, the cellulose gel may be subjected to a step of immersing S1) a cellulose gel in an acidic solution, and (S2) immersing the cellulose gel immersed in the step (S1) in a cosmetic composition containing the amaranth extract of Pheasant. .

추가로 (S3) 상기 (S2) 단계의 셀룰로오스겔을 90 내지 130℃의 온도로, 바람직하게는 95 내지 128 ℃의 온도로, 더 바람직하게는 98 내지 125℃의 온도로 가열하여 고온 처리할 수 있다. 상기 온도 범위에서 마스크팩에 흡착되는 꿩의 비름 추출물, 바람직하게 헤스페리딘의 양이 향상될 수 있다. Further (S3) the cellulose gel of step (S2) can be heated to a temperature of 90 to 130 ℃, preferably at a temperature of 95 to 128 ℃, more preferably to a temperature of 98 to 125 ℃ high temperature treatment have. In the above temperature range, the amount of sperm extract, preferably hesperidin of pheasant adsorbed on the mask pack may be improved.

바람직하게 상기 (S1) 단계의 산성 용액은 pH 2.5 내지 6일 수 있으며, 바람직하게는 pH 3.5 내지 5.5일 수 있으며, 더 바람직하게는 약 pH 4-5일 수 있다. Preferably the acidic solution of step (S1) may be pH 2.5 to 6, preferably pH 3.5 to 5.5, more preferably may be about pH 4-5.

마스크팩을 상기 pH 조건에서 침지시킬 때, 마스크팩에 흡착되는 꿩의 비름 추출물, 바람직하게 헤스페리딘의 양이 향상될 수 있다. When the mask pack is immersed in the above pH conditions, the amount of sperm extract, preferably hesperidin of the pheasant adsorbed to the mask pack can be improved.

마스크팩의 특성상 외부 오염원에 의해 감염의 우려가 있으므로 방부 처리 공정을 거칠 수 있다. 다만, 통상적인 마스크팩이 예를 들어, 페녹시에탄올(phenoxy ethanol), 메틸파라벤(methyl paraben), 에틸파라벤, 프로필파라벤, 부틸파라벤 및 1,2-헥산다이올 중 선택된 하나 이상을 이용하여 방부처리를 하는 것과 비교하여, 본 발명의 마스크팩은 꿩의 비름 추출물이 갖는 뛰어난 방부 효과 및 항산화 효과로 인해 상기와 같은 성분들을 실질적으로 포함하지 않는다Due to the nature of the mask pack, the contamination may be caused by an external contaminant. However, a conventional mask pack is emulsified using at least one selected from, for example, phenoxy ethanol, methyl paraben, ethyl paraben, propyl paraben, butyl paraben and 1,2-hexanediol. Compared to the treatment, the mask pack of the present invention is substantially free of such ingredients due to the excellent antiseptic and antioxidant effects of the Pheasant's amaranth extract

본 발명에 따른 바이오셀룰로오스 시트에 적용할 수 있는 화장료에는 특별한 제한이 없으며 항산화제, 안정화제, 용해화제, 비타민, 안료 및/또는 향료와 같은 통상적인 첨가제 등을 포함할 수 있다. 본 발명의 꿩의 비름 추출물 성분이 함유된 바이오셀룰로오스는 성형기 등을 이용하여 마스크 형태로 가공하여 얼굴용 마스크팩을 제조할 수 있다. The cosmetics applicable to the biocellulose sheet according to the present invention are not particularly limited and may include conventional additives such as antioxidants, stabilizers, solubilizers, vitamins, pigments and / or flavors. Biocellulose containing the amaranth extract component of the pheasant of the present invention can be processed in the form of a mask using a molding machine to produce a facial mask pack.

본 발명의 마스크팩은 화장용 마스크팩으로의 제조를 위해 필수공정인 성형, 접기, 삽입, 충진 및 포장 공정 단계를 추가로 거칠 수 있다. The mask pack of the present invention may be further subjected to molding, folding, inserting, filling, and packaging process steps, which are essential processes for manufacturing a cosmetic mask pack.

본 발명의 마스크팩은 뛰어난 항산화 활성을 갖는다. The mask pack of the present invention has excellent antioxidant activity.

본 발명의 마스크팩은 화장료 조성물에 포함된 항산화 활성 성분의 피부 전달율을 향상시킬 수 있다. The mask pack of the present invention can improve the skin delivery rate of the antioxidant active ingredient included in the cosmetic composition.

도 1은 꿩의 비름 추출물이 감귤 셀룰로오스겔에 흡착된 모습을 보여준다.
대조군은 추출물을 포함하지 않는 용액을 나타낸다.
도 2는 코코넛 셀룰로오스겔과 감귤 셀룰로오스겔을 비교한 사진이다.
Figure 1 shows the appearance of the pheasant extract adsorbed on the citrus cellulose gel.
Control refers to a solution that does not contain an extract.
2 is a photograph comparing the coconut cellulose gel and citrus cellulose gel.

이하, 본 발명의 이해를 돕기 위하여 실시예 등을 들어 상세하게 설명하기로 한다. 그러나, 본 발명에 따른 실시예들은 여러 가지 다른 형태로 변형될 수 있으며, 본 발명의 범위가 하기 실시예들에 한정되는 것으로 해석되어서는 안 된다. 본 발명의 실시예들은 당업계에서 평균적인 지식을 가진 자에게 본 발명을 보다 완전하게 설명하기 위해 제공되는 것이다.Hereinafter, examples and the like will be described in detail to help the understanding of the present invention. However, embodiments according to the present invention can be modified in many different forms, the scope of the invention should not be construed as limited to the following examples. Embodiments of the present invention are provided to more fully explain the present invention to those skilled in the art.

[감귤 Citrus 셀룰로오스겔의Cellulose gel 준비] Ready]

당도 10 brix, 산도 pH 3.0의 온주밀감 착즙액(10%(v/v))에 기탁번호 KACC 91526P인 글루콘아세토박터 속 SEA623-2 균주를 1 × 105cell/ml로 접종하였고, 25℃에서 20일간 호기성 조건에서 정치배양하였다. 그 결과, 균주의 초기 겔 생성 속도가 매우 뛰어나서 배양 2일부터 겔 막이 형성되기 시작하였으며, 약 8 mm 두께를 갖는 셀룰로오스겔을 이용하여 실험을 진행하였다. SEA623-2 strain of Gluconacetobacter sp., Deposited under accession number KACC 91526P, was inoculated at 1 × 10 5 cells / ml in a sugar concentration of 10 brix and an acidity pH 3.0 (10% (v / v)). Incubated at 20 days in aerobic conditions. As a result, the initial gel formation rate of the strain was very excellent, and the gel membrane was formed from the second day of the culture, and the experiment was performed using a cellulose gel having a thickness of about 8 mm.

실시예Example 1. 감귤  Citrus 바이오겔의Biogel pH 조성 확인  pH composition check

먼저 다양한 pH 환경을 조성하였다. pH는 3-10까지를 설정하였다. 정확한 pH 조건을 만들기 위해 First, various pH environments were created. pH was set to 3-10. To make accurate pH conditions

pH3, 4, 5 : sodium citrate buffer, pH 3, 4, 5: sodium citrate buffer,

pH 6,7,8: sodium phosphate buffer, pH 6,7,8: sodium phosphate buffer,

pH 9, 10: Glycine-NaOH buffer을 사용하였다. pH 9, 10: Glycine-NaOH buffer was used.

25% 글라이세롤을 포함하는 에탄올에 완충용액의 농도는 0.1M이 되도록 조성하였다. 카로틴, 헤스페리딘, 갈릭산, 비타민C를 이용하여 실험하였다.Ethanol containing 25% glycerol was prepared so that the concentration of the buffer solution to 0.1M. Carotene, hesperidin, gallic acid, vitamin C was used for the experiment.

감귤 바이오겔에 유용 성분 흡착을 위해 4개의 화합물을 처리하였다. 처리된 화합물은 카로틴, 헤스페리딘, 갈릭산, 비타민 C이다. 이들 화합물들은 5mg/mL의 농도로 감귤 바이오겔에 흡착 시켜 이후 의 흡착 정도를 확인하였다. Four compounds were treated for useful ingredient adsorption in citrus biogels. Compounds treated are carotene, hesperidin, gallic acid, vitamin C. These compounds were adsorbed onto citrus biogel at a concentration of 5 mg / mL to confirm the degree of subsequent adsorption.

실시예Example 2. pH에 따른 흡착력 확인 2. Check the adsorption power according to pH

조성된 조건의 pH에 사방 1cm가 되도록 자른 감귤 바이오겔을 넣은 후 25℃에서 밤새 방치 후 흡착력 확인을 위해 항산화 활성을 측정하였다. 흡착력 확인을 위해서는 연구에 사용된 화합물들이 항산화 활성이 우수한 화합물이므로 DPPH라디칼 소거활성으로 흡착력을 확인하고자 하였다.After putting the citrus biogel cut to 1cm in all directions to the pH of the composition conditions, and left at 25 ℃ overnight, the antioxidant activity was measured to confirm the adsorption capacity. In order to confirm the adsorption capacity, the compounds used in the study were compounds having excellent antioxidant activity.

DPPH라디칼 소거활성은 아래와 같은 방법으로 확인하였다.DPPH radical scavenging activity was confirmed by the following method.

흡착시험이 끝나면 증류수로 3회 세척 후 24웰 플레이트에 유용성분이 흡착된 감귤 바이오겔을 넣고 DPPH 반응액을 500 uL 넣어 10분간 반응 후 517nm에서 흡광도를 측정하였다. 이를 반복하여 활성이 유지되는 정도도 확인하였다. 6회 반복하여 활성을 유지하는 것을 확인하였다After the adsorption test was washed three times with distilled water and put the citrus biogel adsorbed in a useful component in a 24-well plate, 500 μL of DPPH reaction solution was added for 10 minutes and the absorbance was measured at 517 nm. This was repeated to confirm the degree of activity maintained. It was confirmed that the activity was maintained by repeating six times.

그 결과 pH4와 5에서 흡착력이 가장 우수하였으며, 6회 이상 반복하여도 흡착력이 유지되어 항산화 활성을 보이는 것을 확인 할 수 있었다. As a result, the adsorption power was the best at pH 4 and 5, it was confirmed that the adsorption power is maintained even after repeated six times or more to show the antioxidant activity.

pH pH beta carotenebeta carotene hesperidin hesperidin gallic acid gallic acid 비타민C Vitamin C
3

3
39.75  39.75 40.20  40.20 65.42  65.42 68.05  68.05

4

4
54.45  54.45 42.48  42.48 83.92  83.92 85.60  85.60

5

5
52.32  52.32 41.45  41.45 80.89   80.89 83.65  83.65

6

6
47.30  47.30 37.93  37.93 77.08  77.08 79.86  79.86

8

8
32.76  32.76 28.23  28.23 4.92  4.92 0.68  0.68

10

10
35.92  35.92 31.57  31.57 73.94  73.94 79.26 79.26

실시예Example 3. 흡착력이 우수한  3. Excellent adsorption pH인pH pH4와pH4 and 5의 조건에서 온도에 따른 흡착력 확인을 위해 25, 37, 50, 및 100℃(1기압), 그리고 121℃(1.5기압)의 조건에서 흡착력 확인 Adsorption force at 25, 37, 50, and 100 ° C (1 atm), and 121 ° C (1.5 atm) to confirm the adsorption power according to the temperature at 5

분자량이 작은 gallic acid와 vitaminC는 온도에 상관없이 흡착력이 높은 것을 확인할 수 있었고 vitaminC의 경우 열이 가해졌을 때 화합물의 안정성이 떨어지는 것으로 보인다. 그러나 분자량이 큰 카로틴과 헤스페리딘은 열을 가해 주었을 때 흡착력이 높아지는 것을 확인할 수 있었다. 적정 pH는 4, 5에서 흡착력이 가장 우수한 것을 확인할 수 있었다. Small molecular weight gallic acid and vitaminC showed high adsorption capacity regardless of temperature, and vitaminC seems to be less stable when heat is applied. However, carotene and hesperidin, which have high molecular weights, were found to increase their adsorption capacity when heated. It was confirmed that the proper pH was the best adsorption power at 4, 5.

온도별로 흡착정도를 확인하기 위해 흡착력이 우수한 pH 조건인 4와 5에서 시험을 수행하였고, 그 결과 온도가 올라갈수록 흡착력이 증가하였으며 100도에서 흡착력이 가장 우수하였다. 또한 압력이 가해질 경우 분자량이 큰 화합물의 흡착력이 증가하는 것을 확인할 수 있었다. In order to confirm the degree of adsorption by temperature, the tests were carried out at pH conditions 4 and 5, which were excellent in adsorption power. In addition, when the pressure is applied, it was confirmed that the adsorption power of the compound having a large molecular weight increases.

하기 표 2는 온도에 따른 카로틴과 헤스페리딘의 흡착 정도를 확인한 결과이다. Table 2 shows the results of confirming the adsorption degree of carotene and hesperidin according to the temperature.

pH4  pH4 pH5  pH5
온도(℃)

Temperature (℃)

beta carotene

beta carotene

hesperidin

hesperidin

beta carotene

beta carotene

hesperidin

hesperidin

25

25
54.45  54.45 42.48   42.48 39.75  39.75 41.45   41.45

37

37
56.53  56.53 56.72  56.72 50.98  50.98 53.19  53.19

50

50
61.13  61.13 58.93  58.93 58.47  58.47 58.23  58.23

100

100
69.73  69.73 68.4  68.4 60.11  60.11 66.6  66.6
121121 75.01  75.01 77.8  77.8 69.24  69.24 76.2  76.2 130130 40  40 38  38 37  37 35  35

하기 표 3은 갈릭산과 비타민C에 121℃ 열을 가했을 때 활성을 보여준다. Table 3 shows the activity when 121 ° C. heat was applied to gallic acid and vitamin C.


pH

pH
gallic acid  gallic acid ascorbic acid  ascorbic acid

3

3

93.75

93.75

41.29

41.29

4

4

93.58

93.58

47.48

47.48

5

5

92.07

92.07

46.20

46.20

6

6

93.15

93.15

41.47

41.47

8

8

75.12

75.12

45.12

45.12

10

10

93.07

93.07

40.30

40.30

실시예Example 4. 흡착된 화합물들의 온도에 따른 release 정도 확인을 상온(25℃)과 사람의  4. Check the release degree according to the temperature of the adsorbed compounds. 체온인(37℃)에서At body temperature (37 degrees Celsius) 확인 Confirm

또한 화합물의 release 정도 확인을 위해 상온과 피부온도에서 활성을 측정하였을 때 상온보다 20% 이상 release가 잘되는 것을 확인 할 수 있었다. 이는 피부에 밀착력이 우수한 바이오겔에 유용한 성분을 흡착 시켜 피부에 부착 시켰을 때 천천히 지속적으로 유용성분의 방출이 용이하리라고 여겨진다. In addition, when the activity was measured at room temperature and skin temperature to confirm the release degree of the compound, it was confirmed that the release was more than 20% better than room temperature. It is thought that it will be easy to release useful ingredients slowly and continuously when adsorbing useful ingredients to biogel with excellent adhesion to skin.

하기 표 4는 release 온도에 따른 활성을 보여준다. (DPPH를 이용하여 20분간 반응 후 활성 측정)Table 4 shows the activity according to the release temperature. (Measure activity after 20 minutes using DPPH)

25도(℃)  25 degrees (℃) 36.5도(℃)  36.5 degrees (℃)
pH

pH

beta carotene

beta carotene

hesperidin

hesperidin

beta carotene

beta carotene

hesperidin

hesperidin

4

4

54.45

54.45

42.48

42.48

67.13

67.13

53.46

53.46

5

5

39.75

39.75

41.45

41.45

59.65

59.65

61.10

61.10

실시예Example 5.  5. 바이오겔Biogel 내에 안정적인 흡착이 이루어진 것인지 여부에 대해 추가 실험 진행 Further experimentation as to whether or not stable adsorption was achieved within

바이오겔 표면에 일시적인 부착이 아니라는 점을 확인하기 위해 안정성 실험을 진행하였다. 4℃에서 70일간 방치 후 활성을 확인하였다. Stability experiments were conducted to confirm that there was no temporary adhesion to the biogel surface. After standing for 70 days at 4 ℃ activity was confirmed.

하기 표 5는 활성 성분을 흡착시킨 바이오겔을 70일간 4℃에서 방치 후 pH에 따른 흡착력 테스트 결과를 보여준다. Table 5 shows the results of adsorption test according to pH after leaving the biogel adsorbed the active ingredient at 4 ℃ for 70 days.

pH  pH beta carotene beta carotene hesperidin hesperidin gallic acid gallic acid ascorbic acid ascorbic acid
3

3

4,12

4,12

-

-

86.23

86.23

62.312

62.312

4

4

4.755

4.755

-

-

90.399

90.399

77.236

77.236

5

5

6.245

6.245

-

-

87.049

87.049

89.567

89.567

6

6

6.521

6.521

-

-

84.122

84.122

33.738

33.738

8

8

-

-

-

-

65.785

65.785

24.392

24.392

10

10

-

-

-

-

26.518

26.518

-

-

하기 표 6은 121℃, 1.5기압으로 처리된 셀룰로오스겔을 70일간 4℃ 방치 후 측정한 활성을 보여준다.Table 6 below shows the activity measured after standing at 4 ° C. for 70 days at 121 ° C. and treated with 1.5 atm.


pH

pH

beta carotene

beta carotene

hesperidin

hesperidin

gallic acid

gallic acid

ascorbic acid

ascorbic acid

3

3

40.322

40.322

2.331

2.331

87.231

87.231

89.635

89.635

4

4

73.681

73.681

13.804

13.804

90.134

90.134

90.139

90.139

5

5

71.371

71.371

11.43

11.43

88.183

88.183

87.674

87.674

6

6

60.664

60.664

7.114

7.114

85.453

85.453

90.961

90.961

8

8

59.641

59.641

1.962

1.962

68.059

68.059

72.290

72.290

10

10

-

-

5.058

5.058

37.216

37.216

52.982

52.982

본 발명의 조건으로 처리한 경우, 불안정한 헤스페리딘이 저온에서도 경시안정성을 갖는 것으로 확인되었다. When treated under the conditions of the present invention, it was confirmed that the unstable hesperidin has stability over time even at low temperatures.

실시예Example 6.  6. 꿩의 비름Pheasant's Purslane 추출물의 흡착 실험 Adsorption Experiment of Extract

이를 활용하여 항산화 활성이 우수한 꿩의비름 추출물을 바이오겔에 흡착시켰을 때 역시 pH4에서 가장 흡착력이 높아 항산화 활성이 우수하였으며, 항산화 활성을 6회 이상 반복하여 측정하여도 활성이 유지되는 것을 확인할 수 있었다. When the extract of pheasant with excellent antioxidant activity was adsorbed onto the biogel, the anti-oxidant activity was also excellent at pH 4, and the antioxidant activity was excellent. .

이상의 결과에서 확인할 수 있듯이, 일반적인 베타카로틴과 헤스페리딘은 비타민 C 및 갈산과 비교했을 때, 셀룰로오스겔에 쉽게 부착되지 않았으나, 베타카로틴과 헤스페리딘을 포함하는 수용액의 pH를 4-5로 조절하고, 121℃, 1.5기압에서 샘플을 가열하여 최적의 조건을 수립하였을 때, 높은 흡착율을 보였다. As can be seen from the above results, the general beta carotene and hesperidin was not easily attached to the cellulose gel when compared with vitamin C and gallic acid, but adjusted the pH of the aqueous solution containing beta carotene and hesperidin to 4-5, 121 ℃ When the optimum conditions were established by heating the sample at 1.5 atm, the adsorption rate was high.

또한 꿩의비름 추출물이 흡착된 바이오겔의 총 폴리페놀 함량 측정방법으로 꿩의 비름이 흡착되어 색이 변하는 바이오겔을 확인 할 수 있었다.In addition, as a method of measuring the total polyphenol content of the biogel adsorbed by the pheasant extract of the pheasant, it was possible to identify the biogel that changes color due to the adsorption of the pheasant.

실시예Example 7. 감귤  7. Citrus 셀룰로오스겔과With cellulose gel 코코넷Coconnet 셀룰로오스  cellulose 겔의Gel 비교 실험 Comparative experiment

코코넛 겔을 이용하여 제조한 마스크팩은 거칠고 이물질이 많아 마스크팩으로 이용하기 어려웠다. 또한 본 발명과 같이 유효성분을 흡착하기 어려웠다. The mask pack manufactured using the coconut gel was rough and had a lot of foreign substances, making it difficult to use as a mask pack. In addition, it was difficult to adsorb the active ingredient as in the present invention.

그러나 본 발명의 감귤 셀룰로오스겔은 겔의 입자가 가늘고 이물질이 없어 마스크팩으로 활용하기 적당하였다. However, the citrus cellulose gel of the present invention was suitable for use as a mask pack because the gel particles are thin and have no foreign matter.

Claims (10)

삭제delete 삭제delete 삭제delete 삭제delete 베타카로틴, 헤스페리딘, 또는 이들의 혼합물및 감귤 셀룰로오스겔을 포함하고, 상기 베타카로틴, 헤스페리딘, 또는 이들의 혼합물이 감귤 셀룰로오스겔에 흡착된 마스크팩을 제조하는 방법에 있어서,
(S1) 감귤 셀룰로오스겔을 산성 용액에 침지시키는 단계,
(S2) 상기 (S1) 단계에서 침지된 셀룰로오스겔을 베타카로틴, 헤스페리딘, 또는 이들의 혼합물이 함유된 화장료 조성물에 침지시키는 단계; 및
(S3) 상기 (S2) 단계의 감귤 셀룰로오스겔을 98 내지 125℃의 온도로 가열하는 단계를 포함하는 베타카로틴, 헤스페리딘, 또는 이들의 혼합물이 흡착된 마스크팩 제조 방법.
In the method for producing a mask pack containing beta carotene, hesperidin, or a mixture thereof and citrus cellulose gel, wherein the beta carotene, hesperidin, or a mixture thereof is adsorbed on the citrus cellulose gel,
(S1) immersing the citrus cellulose gel in an acidic solution,
(S2) immersing the cellulose gel immersed in the step (S1) in the cosmetic composition containing beta carotene, hesperidin, or a mixture thereof; And
(S3) Method for producing a mask pack adsorbed beta carotene, hesperidin, or a mixture thereof comprising heating the citrus cellulose gel of step (S2) to a temperature of 98 to 125 ℃.
삭제delete 제5항에 있어서, 상기 (S1) 단계의 산성 용액은 pH 2.5 내지 6인 것을 특징으로 하는 마스크팩 제조 방법. The method of claim 5, wherein the acidic solution of the step (S1) is a mask pack manufacturing method, characterized in that the pH 2.5 to 6. 제7항에 있어서, 상기 (S1) 단계의 산성 용액은 pH 3.5 내지 5.5인 것을 특징으로 하는 마스크팩 제조 방법. The method of claim 7, wherein the acidic solution of the step (S1) is a mask pack manufacturing method, characterized in that the pH 3.5 to 5.5. 삭제delete 삭제delete
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