KR20190078203A - A method of increasing bioactive compounds isolated from onion skin using subcritical water with carbon dioxide - Google Patents
A method of increasing bioactive compounds isolated from onion skin using subcritical water with carbon dioxide Download PDFInfo
- Publication number
- KR20190078203A KR20190078203A KR1020170179997A KR20170179997A KR20190078203A KR 20190078203 A KR20190078203 A KR 20190078203A KR 1020170179997 A KR1020170179997 A KR 1020170179997A KR 20170179997 A KR20170179997 A KR 20170179997A KR 20190078203 A KR20190078203 A KR 20190078203A
- Authority
- KR
- South Korea
- Prior art keywords
- quercetin
- extract
- onion skin
- extraction
- minutes
- Prior art date
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- 235000002732 Allium cepa var. cepa Nutrition 0.000 title claims abstract description 69
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Abstract
Description
본 발명은 이산화탄소를 첨가한 아임계수를 이용하여 양파껍질에서 분리되는 생리활성 성분을 증가시키는 방법에 관한 것이다.The present invention relates to a method for increasing physiologically active ingredients isolated from onion skin using carbon dioxide-added subcodes.
양파는 백합과에 속하는 다년생 식물로서, 다량 함유되어 있는 페놀화합물로 인하여 항산화, 항암, 항고혈압, 혈액지질 개선, 항염증 등 여러 생리활성이 있다. 양파 내 주요 페놀화합물은 퀘르세틴(quercetin)과 퀘르세틴(quercetin) 배당체로서, 퀘르세틴(quercetin) 배당체가 전체 페놀화합물 중 약 80%를 차지하며, 비가식부인 양파껍질의 퀘르세틴(quercetin) 함량은 208.8㎎%로 가식부인 양파 과육의 2.26㎎%에 비하여 92배 이상을 함유하고 있다.Onion is a perennial plant belonging to the lily family. It has many physiological activities such as antioxidant, anti-cancer, antihypertensive, blood lipid improvement, anti-inflammation due to the phenol compound contained in large quantity. The major phenolic compounds in onion were quercetin and quercetin glycosides. Quercetin glycosides accounted for about 80% of total phenolic compounds. The quercetin content of the non-fermented onion skin was 208.8 mg% , Which contains more than 92 times as much as the 2.26 ㎎% of onion pulp.
양파껍질에서의 페놀화합물은 프리폼(free form), 에스테르화 폼(esterified form), 그리고 비수용성 섬유질, 다당류, 리그닌(lignin) 등과 결합된 불용성 바운드폼(bound form)이 각각 44.2%, 20.9%, 34.9%의 비율로 존재하는데, 이러한 형태의 페놀화합물은 성분 분석을 목적으로 할 경우에는 주로 메탄올과 같은 유기용매로 추출하거나 산 또는 알칼리를 이용하여 가수분해한 후 추출한다. 그러나 이러한 추출 및 가수분해 방법은 사용 용매의 독성으로 인하여 양파 껍질을 이용한 가공식품의 개발이 주 목적인 경우에는 사용할 수가 없다는 문제점이 있고, 이러한 문제점을 해결하고자 하는 요구가 있었다. The phenolic compounds in the onion skin were 44.2%, 20.9%, and 50.0%, respectively, in free form, esterified form, and insoluble bound form combined with non-water soluble fibrous, polysaccharide, lignin, 34.9%. When this type of phenol compound is used for the purpose of component analysis, it is mainly extracted with an organic solvent such as methanol or hydrolyzed with an acid or an alkali. However, this extraction and hydrolysis method has a problem that it can not be used when the main purpose is to develop processed foods using onion skin due to the toxicity of the used solvent, and there has been a demand to solve such problems.
본 발명의 하나의 목적은, 이산화탄소가 첨가된 아임계수를 이용하여 양파로부터 분리되는 생리활성 성분을 증가시키는 방법을 제공하는 것이다.It is an object of the present invention to provide a method for increasing physiologically active ingredients separated from onion using carbon dioxide added limulus coefficient.
본 발명의 다른 목적은 상기 방법에 의한 수득한 양파껍질의 아임계수 추출물 또는 상기 양파껍질 추출물에서 분리한 생리활성 성분을 포함하는 항산화 식품조성물을 제공하는 것이다. Another object of the present invention is to provide an antioxidant food composition comprising an aseismic extract of onion skin obtained by the above method or a physiologically active ingredient isolated from the onion skin extract.
본 발명의 다른 목적은 상기 항산화 식품조성물을 포함하는 건강기능식품을 제공하는 것이다. Another object of the present invention is to provide a health functional food comprising the antioxidant food composition.
본 발명의 또 다른 목적은 상기 방법에 의해 수득한 양파껍질의 아임계수 추출물 또는 상기 양파껍질 추출물에서 분리한 생리활성 성분을 포함하는 항산화용 화장료 조성물을 제공하는 것이다.It is still another object of the present invention to provide an antioxidative cosmetic composition comprising an aseismic extract of onion skin obtained by the above method or a physiologically active ingredient isolated from the onion skin extract.
상기 목적을 달성하기 위하여 본 발명은 하나의 양태로, 양파껍질과 물을 아임계수 추출장치의 반응조에 투입하는 단계, 상기 반응조에 질소를 통과시켜 용존 산소를 제거하는 단계, 이산화탄소(CO2)를 상기 반응조에 50 내지 80bar의 압력으로 주입하고, 상기 반응조를 가열하는 단계, 105 내지 125℃의 온도 및 80 내지 300bar의 압력 조건에서 3 내지 13분 동안 추출하여 양파 껍질의 아임계수 추출물을 수득하는 단계, 상기 양파껍질의 아임계수 추출물에서 생리활성 성분을 분리하는 단계를 포함하는, 이산화탄소가 첨가된 아임계수를 이용하여 양파로부터 분리되는 생리활성 성분을 증가시키는 방법을 제공한다.According to one aspect of the present invention, there is provided a method for removing carbon dioxide (CO 2 ), comprising the steps of introducing an onion skin and water into a reaction tank of an asphaltene extraction apparatus, passing nitrogen through the reaction tank to remove dissolved oxygen, Heating the reaction vessel at a pressure of 50 to 80 bar and extracting the reaction vessel at a temperature of 105 to 125 DEG C and a pressure of 80 to 300 bar for 3 to 13 minutes to obtain an index factor extract of onion skin , And separating the physiologically active component from the limulus extract of the onion skin. The present invention also provides a method for increasing physiologically active components separated from onion using carbon dioxide-added limulus coefficient.
본 발명의 용어 “양파껍질”은 백합과에 속하는 다년생 식물인 양파의 외피를 의미한다. 상기 양파껍질은 건조된 것일 수 있으며, 열풍건조, 동결건조, 진공건조 등의 건조방법을 사용하여 건조된 것 일 수 있다. 상기 양파껍질은 추출과정을 진행함에 따라 추출용매와 접촉 면적을 최대로 증가시켜 추출 수율을 높이기 위해 분쇄할 수 있으며, 항산화 활성 물질을 최대한 유지시킨다는 목적을 위하여 추출단계를 수행하기 전까지 4 내지 -20℃에서 보관할 수 있다. The term " onion skin " of the present invention means the skin of an onion which is a perennial plant belonging to the lily family. The onion skin may be dried or dried using a drying method such as hot air drying, freeze drying, or vacuum drying. The onion peel may be pulverized to increase the extraction yield by maximally increasing the contact area with the extraction solvent as the extraction process proceeds. In order to keep the antioxidant active material as much as possible, Lt; 0 > C.
본 발명의 용어 “아임계수”는 온도 100 내지 374℃, 압력 4 내지 400bar 범위에서 액체 상태인 물이다. 일반적으로 물은 1 대기압에서의 끓는점은 100℃이다. 고압에서는 온도를 올려도 액체 상태인 물을 아임계수라고 하며, 온도를 374℃이상으로 올리면 초임계수 상태로 된다. 아임계수의 온도에 따른 유전상수(ε)가 15 ~ 50 범위 이내로 메탄올(ε= 32) 및 에탄올(ε= 24) 등 유기용매와 비슷하기 때문에 유기용매와 비슷한 용해특성을 갖는다. 상온 상압상태 물의 유전상수는 ε= 79로 상온 상압의 물에 용해되지 않는 물질도 아임계수 상태에서 용해, 추출될 수 있다The term " sub-coefficient " of the present invention is water in a liquid state at a temperature of 100 to 374 DEG C and a pressure of 4 to 400 bar. Generally, the boiling point of water at 1 atmospheric pressure is 100 ° C. At high pressure, the water in the liquid state is called as the ash factor even if the temperature is raised. When the temperature is raised to 374 ° C or higher, the supercritical water is obtained. The dielectric constant (ε) of the asymptotic coefficient varies with the organic solvent such as methanol (ε = 32) and ethanol (ε = 24) within the range of 15~50. The dielectric constant of water at normal temperature and pressure is ε = 79, and materials that are not soluble in water at normal temperature and pressure can be dissolved and extracted in the asymmetric state
본 발명의 용어 “추출”은 식물이나, 광물 등 여러 성분을 이루고 있는 물질에서 특정한 성분만을 녹여서 얻는 방법으로, 본 발명에서는 양파껍질에 이산화탄소가 첨가된 아임계수를 용매로 양파껍질내의 생리활성 물질을 녹여서 추출하는 것을 의미한다. The term " extraction " of the present invention refers to a method of dissolving only a specific component in a plant, mineral, or other constituent. In the present invention, the carbonation of the onion skin is controlled by the sub- It means melting and extracting.
본 발명의 “아임계수 추출장치”는 도 1에 도시된 바와 같이 밴드히터, 냉각조, 이산화탄소 탱크, 질소 탱크, 체크밸브, 인라인 필터, 고압펌프, 압력게이지, 반응조, 안전밸브, 온도게이지, 온도조절기, 온/오프(on/off) 밸브를 포함하고 있다.As shown in FIG. 1, the "apparatus for extracting the sub-coefficient" of the present invention includes a band heater, a cooling tank, a carbon dioxide tank, a nitrogen tank, a check valve, an inline filter, a high pressure pump, a pressure gauge, Regulator, and an on / off valve.
본 발명의 “양파껍질과 물을 아임계수 추출장치의 반응조에 투입하는 단계”는 양파껍질 및 물을 반응조(RV)에 투입하는 단계로, 상기 물은 증류수를 이용할 수 있으며, 양파껍질을 증류수에 분산시킨 후 상기 반응조(RV)에 투입할 수 있다.&Quot; Inoculating the onion skin and water into the reaction tank of the aseum extracting apparatus " of the present invention is a step of putting the onion skin and water into the reaction tank (RV), wherein the water can be distilled water, Dispersed and then introduced into the reaction tank (RV).
본 발명의 “용존 산소를 제거하는 단계”는 아임계수 추출장치의 질소탱크에 연결된 밸브(V2)와 반응조(RV)에 연결된 밸브(V4)를 열어 반응조(RV)의 질소가스를 주입하여 물 속의 용존된 산소를 제거하는 단계를 의미한다. 상기 질소의 주입 압력은 50bar 일 수 있으며, 아임계수의 용존산소 제거시 용존산소에 의한 생리활성 물질의 산화를 방지하는 장점이 있다. The "dissolved oxygen removing step" of the present invention is a step of removing dissolved oxygen by opening a valve V2 connected to a nitrogen tank and a valve V4 connected to a reaction tank RV by injecting a nitrogen gas in a reaction tank RV, And means to remove dissolved oxygen. The injection pressure of the nitrogen may be 50 bar, and oxidation of the physiologically active substance due to dissolved oxygen is advantageously prevented when the dissolved oxygen is removed.
본 발명의 “이산화탄소를 주입하는 단계”는 이산화탄소 탱크에 있는 상온에서 액체인 이산화탄소를 이산화탄소 탱크와 연결된 밸브(V1)와 반응조와 연결된 밸브(V4)를 열고 고압펌프(HPP)를 이용하여 반응조에 주입하는 단계이다. 주입압력은 50 내지 80bar이며, 상기 주입압력은 반응조에 연결된 밸브(V4)와 연결된 압력게이지를 통해 측정할 수 있다.In the "step of injecting carbon dioxide" of the present invention, carbon dioxide which is liquid at room temperature in a carbon dioxide tank is opened by opening a valve (V1) connected to a carbon dioxide tank and a valve (V4) connected to a reaction tank and injecting . The injection pressure is 50 to 80 bar, and the injection pressure can be measured through a pressure gauge connected to the valve (V4) connected to the reaction tank.
본 발명의 “반응조를 가열하는 단계”는 반응조 외곽에 형성된 밴드히터가 가열되어 반응조의 온도를 높이거나 일정한 온도로 유지하는 단계를 의미한다. 반응조 내부와 밴드히터에는 각각 온도게이지가 연결되어 있으며, 상기 온도게이지가 밴드히터와 연결된 온도조절기에 반응조 또는 밴드히터의 온도정보를 제공하며, 밴드히터에 연결된 온도조절기가 설정된 온도로 밴드히터를 가열하여 반응조의 추출 온도를 조절한다.The " step of heating the reaction tank " of the present invention means a step of heating the band heater formed on the outer side of the reaction tank to raise the temperature of the reaction tank or keep it at a constant temperature. A temperature gauge is connected to the inside of the reactor and a band heater respectively. The temperature gauge provides temperature information of the reaction tank or the band heater to the temperature controller connected to the band heater. The temperature controller connected to the band heater heats the band heater Thereby adjusting the extraction temperature of the reaction tank.
본 발명의 “아임계수 추출물을 수득하는 단계”에서 반응조 내부의 온도를 105 내지 125℃의 온도로 유지하였고, 반응조 내부에 연결된 압력게이지로 반응조내부의 압력을 측정하였으며, 추출이 진행되는 동안 80 내지 300bar의 일정한 압력을 유지하였다. 반응조 내부의 압력이 목표압력보다 높을 경우 밸브(V5)를 통해 기체를 배출시켜 조절하였고, 추출시간은 목표온도에 도달한 시점을 0분으로 측정하여, 3 내지 13분 동안 추출하였고, 추출이 끝난 뒤 상기 반응조를 냉각하여 추출물을 수득하였다. 또한 상기 추출물을 여과하는 단계를 더 포함할 수도 있다.In the "step of obtaining the limulus extract" of the present invention, the temperature inside the reaction tank was maintained at a temperature of 105 to 125 ° C., the pressure inside the reaction tank was measured with a pressure gauge connected to the inside of the reaction tank, A constant pressure of 300 bar was maintained. When the pressure inside the reactor was higher than the target pressure, the gas was discharged through the valve (V5). The extraction time was measured as 0 minutes when the target temperature was reached, and the extraction time was 3 to 13 minutes. Then, the reaction vessel was cooled to obtain an extract. The method may further comprise filtering the extract.
본 발명의 일실시예에서는 동일한 추출온도, 추출시간 조건에서 이산화탄소를 주입하지 않은 아임계수 추출물과 이산화탄소를 주입한 아임계수 추출물의 퀘르세틴(quercetin) 및 프로토카테츄산(protocatechuic acid)의 함량을 측정하였다. 이산화탄소 주입시 퀘르세틴(quercetin) 및 프로토카테츄산(protocatechuic acid)의 함량 모두 증가하는 것을 확인하였으나, 110℃에서 5분간 추출하였을 때 퀘르세틴(quercetin)은 2.89배 증가하였으나, 프로토카테츄산(protocatechuic acid)는 1.58배 증가하여 프로토카테츄산(protocatechuic acid)의 함량의 증가폭이 가장 작음을 확인하였다. 이를 보아 이산화탄소 65bar의 주입이 퀘르세틴(quercetin)이 프로토카테츄산(protocatechuic acid)으로 전환되는 것을 억제함을 확인하였다. In one embodiment of the present invention, the content of quercetin and protocatechuic acid in the extract of carbon dioxide-injected and carbon dioxide-injected subcodes were measured at the same extraction temperature and extraction time. The amount of quercetin and protocatechuic acid was increased when carbon dioxide was injected. However, when extracted at 110 ℃ for 5 minutes, the quercetin increased 2.89 times. Protocatechuic acid increased the content of quercetin and protocatechuic acid 1.58 fold, and the increase in the content of protocatechuic acid was the least. It was confirmed that the injection of 65 bar of carbon dioxide inhibited the conversion of quercetin to protocatechuic acid.
따라서 이산화탄소 주입에 의해, 프로토카테츄산(protocatechuic acid)의 생성을 억제할 수 있다.Therefore, the production of protocatechuic acid can be suppressed by the injection of carbon dioxide.
본 발명의 일실시예에서 이산화탄소를 65bar로 주입한 아임계수 추출물을 추출온도 및 추출시간에 따른 양파껍질 추출물의 생리활성 물질의 함량을 측정하였다. 생리활성 물질인 퀘르세틴-3,4’-디글루코사이드(quercetin-3,4’-diglucoside), 퀘르세틴-4’-글루코사이드(quercetin-4’-glucoside) 및 퀘르세틴(quercetin)의 함량을 측정한 결과 110℃에서 5 내지 10분간 추출한 추출물 및 120℃에서 5분간 추출한 추출물에서 상기 퀘르세틴-3,4’-디글루코사이드(quercetin-3,4’-diglucoside), 퀘르세틴-4’-글루코사이드(quercetin-4’-glucoside) 및 퀘르세틴(quercetin)의 함량이 우수하였다. 또한, 총페놀화합물 및 총플라보노이드의 함량을 측정한 경과 상기 110℃에서 5분 내지 10분간 추출한 추출물 및 120℃에서 5분간 추출한 추출물이 총페놀화합물 및 총플라보노이드의 함량이 우수하였다.In one embodiment of the present invention, the content of physiologically active substance of onion skin extract was measured according to the extracting temperature and extraction time of the ash extract extract which was injected with carbon dioxide at 65 bar. The content of quercetin-3,4'-diglucoside, quercetin-4'-glucoside and quercetin, which are physiologically active substances, was measured and found to be 110 (Quercetin-3,4'-diglucoside, quercetin-4'-glucoside, and quercetin-4'-glucoside) were extracted from the extracts extracted for 5 to 10 minutes at room temperature and for 5 minutes at 120 ° C, glucoside) and quercetin (quercetin). The contents of total phenolic compounds and total flavonoids were higher in the extracts extracted at 110 ° C for 5 minutes to 10 minutes and at 120 ° C for 5 minutes.
따라서 본 발명의 추출은 80 내지 300bar 압력조건에서 추출온도 110℃에서 추출시간 5 내지 10분, 또는 추출온도 120℃에서 추출시간 5분간 진행되는 것일 수 있다. Therefore, the extraction of the present invention may be carried out at an extraction temperature of 110 ° C for 5 to 10 minutes at 80 to 300 bar pressure, or at an extraction temperature of 120 ° C for 5 minutes.
또한, 본 발명의 생리활성 성분은 퀘르세틴-3,4’-디글루코사이드(quercetin-3,4’-diglucoside), 퀘르세틴-4’-글루코사이드(quercetin-4’-glucoside) 및 퀘르세틴(quercetin)으로 이루어진 군에서 선택되는 하나 이상을 포함하는 총페놀화합물 또는 총플라보노이드 화합물일 수 있다. In addition, the physiologically active ingredient of the present invention may be a quercetin-3,4'-diglucoside, a quercetin-4'-glucoside and a quercetin. Lt; RTI ID = 0.0 > phenol < / RTI > compound or a total flavonoid compound.
본 발명의 다른 양태로서, 상기 방법에 의해 수득한 양파껍질의 아임계수 추출물 또는 상기 양파껍질의 아임계수 추출물에서 분리한 생리활성 성분을 포함하는, 항산화용 식품조성물을 제공한다.In another aspect of the present invention, there is provided an antioxidant food composition comprising an aseismic extract of an onion skin obtained by the above method or a physiologically active ingredient isolated from an extract of an aseismic extract of the onion skin.
본 발명의 일실시예에서 이산화탄소를 첨가한 아임계수 추출물의 추출온도 및 추출시간에 따른 추출물의 DPPH 자유라디칼 소거활성 및 FRAP 활성을 확인하여 항산화 효과를 확인하였다. DPPH 자유라디칼 소거활성 및 FRAP 활성을 측정한 결과 추출온도 110℃에서 5 내지 10분간 추출한 추출물 및 120℃에서 5분간 추출한 추출물이 DPPH 자유라디칼 소거활성 및 FRAP 활성이 우수하여, 항산화 효과가 우수함을 확인하였다.In one embodiment of the present invention, DPPH free radical scavenging activity and FRAP activity of the extract according to the extracting temperature and extraction time of carbon dioxide-added index extract were confirmed and the antioxidative effect was confirmed. The DPPH free radical scavenging activity and FRAP activity were measured. The extracts obtained by extracting at 110 ° C for 5 to 10 minutes and the extracts for 5 minutes at 120 ° C showed excellent DPPH free radical scavenging activity and FRAP activity, Respectively.
따라서 본 발명의 양파껍질의 아임계수 추출물 또는 상기 양파껍질의 아임계수 추출물에서 분리한 생리활성 성분을 항산화용 식품조성물로 이용할 수 있다. Therefore, the physiologically active ingredient isolated from the sublingual extract of the onion skin of the present invention or the sublingual extract of the onion skin can be used as a food composition for antioxidation.
상기 항산화용 식품조성물은 식품제조시 통상적으로 첨가되는 성분, 예를 들면, 단백질, 탄수화물, 지방, 영양소, 조미제 및 향미제를 추가로 포함할 수 있다. The antioxidant food composition may further comprise ingredients commonly added in food production, for example, proteins, carbohydrates, fats, nutrients, seasonings and flavors.
상기 탄수화물의 예는 모노사카라이드, 예를 들어, 포도당, 과당 등; 디사카라이드, 예를 들어 말토스, 슈크로스, 올리고당 등; 및 폴리사카라이드, 예를 들어 덱스트린, 사이클로덱스트린 등과 같은 통상적인 당 및 자일리톨, 소르비톨, 에리트리톨 등의 당알콜이다. 향미제로서 천연 향미제[타우마틴, 스테비아 추출물 (예를 들어 레바우디오시드 A, 글리시르히진 등)] 및 합성 향미제(사카린, 아스파르탐 등)를 사용할 수 있다.Examples of such carbohydrates are monosaccharides, such as glucose, fructose, and the like; Disaccharides such as maltose, sucrose, oligosaccharides and the like; And polysaccharides such as dextrin, cyclodextrin and the like, and sugar alcohols such as xylitol, sorbitol and erythritol. Natural flavorings such as tau martin and stevia extract (e.g., rebaudioside A and glycyrrhizin) and synthetic flavors (saccharin, aspartame, etc.) may be used as flavorings.
예컨대, 본 발명의 식품 조성물이 드링크제로 제조되는 경우에는 구연산, 액 상과당, 설탕, 포도당, 초산, 사과산, 과즙, 두충 추출액, 대추 추출액, 감초 추출액 등을 추가로 포함시킬 수 있다.For example, when the food composition of the present invention is prepared as a drink, citric acid, liquid fructose, sugar, glucose, acetic acid, malic acid, juice, mulberry extract, jujube extract and licorice extract may be further added.
본 발명의 다른 양태로서, 상기 항산화용 식품조성물을 포함하는 건강기능식품일 수 있다. In another aspect of the present invention, the composition may be a health functional food containing the antioxidant food composition.
본 발명의 건강기능식품은 상기 식품조성물을 포함한 음료(알콜성 음료 포함), 과실 및 그의 가공식품(예: 과일통조림, 병조림, 잼, 마아말레이드 등), 어류, 육류 및 그 가공식품 (예: 햄, 소시지, 콘비이프 등), 빵류 및 면류(예: 우동, 메밀국수, 라면, 스파게티, 마카로니 등), 과즙, 각종 드링크, 쿠키, 엿, 유제품 (예: 버터, 치즈 등), 식용식물유지, 마아가린, 식물성 단백질, 레토르트 식품, 냉동식품, 각종 조미료(예: 된장, 간장, 소스 등) 등일 수 있다.The health functional food of the present invention can be used as a health functional food containing the above food composition such as beverage (including alcoholic beverage), fruit and its processed food (such as canned fruit, jar, jam, maarelade, etc.), fish, (Such as butter, cheese, etc.), edible plants (such as, for example, ham, sausage, and corn beef), breads and noodles (e.g., udon, buckwheat noodles, ramen noodles, spaghetti, macaroni, Vegetable protein, retort food, frozen food, various seasonings (e.g., miso, soy sauce, sauces, etc.).
또한, 본 발명의 건강기능식품은 정제, 환제, 산제, 과립제, 분말제, 캡슐제, 액제 제형 등으로 제형화된 것일 수도 있다. 이들은 담체, 희석제, 부형제 및 첨가제 중 하나 이상을 더 포함하여 제형화될 수 있다.In addition, the health functional food of the present invention may be formulated into tablets, pills, powders, granules, powders, capsules, liquid preparations and the like. These may be formulated further comprising one or more of carriers, diluents, excipients and additives.
상기 담체, 부형제, 희석제 및 첨가제의 구체적인 예로는 이에 한정하는 것은 아니나, 락토즈, 덱스트로즈, 슈크로즈, 솔비톨, 만니톨, 에리스리톨, 전분, 아카시아 고무, 인산칼슘, 알지네이트, 젤라틴, 칼슘 포스페이트, 칼슘 실리케이트, 미세결정성 셀룰로즈, 폴리비닐피롤리돈, 셀룰로즈, 폴리비닐피롤리돈, 메틸셀룰로즈, 물, 설탕시럽, 메틸셀룰로즈, 메틸 하이드록시 벤조에이트, 프로필하이드록시 벤조에이트, 활석, 스테아트산 마그네슘 및 미네랄 오일로 이루어진 그룹으로부터 선택된 1종 이상이 사용되는 것이 바람직하다.Specific examples of the carrier, excipient, diluent and additives include, but are not limited to, lactose, dextrose, sucrose, sorbitol, mannitol, erythritol, starch, acacia rubber, calcium phosphate, alginate, gelatin, calcium phosphate, calcium Silicate, microcrystalline cellulose, polyvinylpyrrolidone, cellulose, polyvinylpyrrolidone, methylcellulose, water, sugar syrup, methylcellulose, methylhydroxybenzoate, propylhydroxybenzoate, talc, magnesium stearate And a mineral oil are preferably used.
본 발명은 또 다른 양태로서, 상기 방법에 의해 수득한 양파껍질의 아임계수 추출물 또는 상기 양파껍질의 아임계수 추출물에서 분리한 생리활성 성분을 포함하는, 항산화용 화장료 조성물을 제공한다.According to still another aspect of the present invention, there is provided an antioxidant cosmetic composition comprising an asymptotic extract of the onion skin obtained by the above method or a physiologically active ingredient isolated from the extract of the asein extract of the onion skin.
상기 항산화용 화장료 조성물은 안정화제, 기용화제, 비타민, 안료 및 향료등과 같은 통상적인 보조제 및 담체를 더 포함할 수 있다. The antioxidant cosmetic composition may further contain conventional auxiliaries and carriers such as stabilizers, excipients, vitamins, pigments and fragrances.
본 발명의 화장료 조성물은 당업계에서 통상적으로 제조되는 어떠한 제형으로도 제조될 수 있으며, 예를 들어, 용액, 현탁액, 유탁액, 페이스트, 겔, 크림, 로션, 파우더, 비누, 계면활성제-함유 클린싱, 오일, 분말 파운데이션, 유탁액 파운데이션, 왁스 파운데이션 및 스프레이 등으로 제형화될 수 있으나, 이에 한정되는 것은 아니다. 보다 상세하게는, 영양 크림, 수렴 화장수, 유연 화장수, 로션, 에센스, 영양젤 또는 마사지 크림의 제형으로 제조될 수 있다.The cosmetic composition of the present invention can be prepared into any of the formulations conventionally produced in the art and can be used as a solution, a suspension, an emulsion, a paste, a gel, a cream, a lotion, a powder, a soap, , Oil, powder foundation, emulsion foundation, wax foundation and spray, but is not limited thereto. More specifically, it can be prepared as a nutritional cream, a convergent lotion, a soft lotion, a lotion, an essence, a nutritional gel or a massage cream.
본 발명의 제형이 페이스트, 크림 또는 겔인 경우에는 담체 성분으로서 동물성유, 식물성유, 왁스, 파라핀, 전분, 트라가칸트, 셀룰로오스 유도체, 폴리에틸렌 글리콜, 실리콘, 벤토나이트, 실리카, 탈크 또는 산화아연 등이 이용될 수 있다.When the formulation of the present invention is a paste, a cream or a gel, an animal oil, vegetable oil, wax, paraffin, starch, tragacanth, cellulose derivative, polyethylene glycol, silicone, bentonite, silica, talc or zinc oxide .
본 발명의 제형이 파우더 또는 스프레이인 경우에는 담체 성분으로서 토스, 탈크, 실리카, 알루미늄 히드록시드, 칼슘 실리케이트 또는 폴리아미드 파우더가 이용될 수 있고, 특히 스프레이인 경우에는 추가적으로 클로로플루오로히드로카본, 프로판/부탄 또는 디메틸 에테르와 같은 추진체를 포함할 수 있다.When the formulation of the present invention is a powder or a spray, tosse, talc, silica, aluminum hydroxide, calcium silicate or polyamide powder may be used as a carrier component. In the case of a spray, in particular, chlorofluorohydrocarbons, propane / Propane or dimethyl ether.
본 발명의 제형이 용액 또는 유탁액인 경우에는 담체 성분으로서 용매, 가용화제 또는 유탁화제가 이용되고, 예컨대 물, 에탄올, 이소프로판올, 에틸 카보네이트, 에틸 아세테이트, 벤질 알코올, 벤질 벤조에이트, 프로필렌 글리콜, 1,3-부틸글리콜 오일, 글리세롤 지방족 에스테르, 폴리에틸렌 글리콜 또는 소르비탄의 지방산 에스테르가 있다.When the formulation of the present invention is a solution or emulsion, a solvent, a solubilizing agent or an emulsifying agent is used as a carrier component, and examples thereof include water, ethanol, isopropanol, ethyl carbonate, ethyl acetate, benzyl alcohol, benzyl benzoate, , 3-butyl glycol oil, glycerol aliphatic ester, polyethylene glycol or sorbitan fatty acid esters.
본 발명의 제형이 현탁액인 경우에는 담체 성분으로서 물, 에탄올 또는 프로필렌 글리콜과 같은 액상의 희석제, 에톡실화 이소스테아릴 알코올, 폴리옥시에틸렌 소르비톨 에스테르 및 폴리옥시에틸렌 소르비탄 에스테르와 같은 현탁제, 미소결정성 셀룰로오스, 알루미늄 메타히드록시드, 벤토나이트, 아가 또는 트라가칸트 등이 이용될 수 있다.In the case where the formulation of the present invention is a suspension, a carrier such as water, a liquid diluent such as ethanol or propylene glycol, a suspending agent such as ethoxylated isostearyl alcohol, polyoxyethylene sorbitol ester and polyoxyethylene sorbitan ester, Cellulose, aluminum metahydroxide, bentonite, agar or tragacanth.
아임계수에 이산화탄소를 가하여, 생리활성물 성분이 증가된 양파 추출물을 얻을 수 있으며, 퀘르세틴(quercetin)이 고온에서는 열분해되어 항산화 활성이 낮은 프로토카테츄산(protocatechuic acid)으로 변환되는 것을 방지하여, 항산화 효과가 증가된 양파 추출물을 얻을 수 있어 양파를 이용한 기능성 식품의 개발, 식품 소재의 개발, 화장품 소재의 개발 등 다양한 산업분야에 활용될 수 있다.It is possible to obtain an onion extract with an increased amount of physiologically active components by adding carbon dioxide to the ash factor, and quercetin is prevented from being converted into protocatechuic acid which is pyrolyzed at high temperature to have a low antioxidative activity, Can be utilized in various industrial fields such as development of functional food using onion, development of food material, development of cosmetic material and the like.
도 1은 아임계수 추출장치의 도식이다(BH: 밴드히터, CB: 냉각조, CO2 TK: CO2 탱크, CV: 체크밸브, F: 인라인필터, HPP: 고압펌프, N2 TK: 질소탱크, P: 압력게이지, RV: 반응조, SV: 안전밸브, T: 온도게이지, TC: 온도조절기, V: 온/오프(on/off) 밸브).
도 2는 아임계수 추출장치에서 추출온도를 100 내지 150℃로 하여 5분간 추출한 후 추출물의 페놀화합물의 함량을 측정한 결과이다(a: 프로토카테츄산 (protocatechuic acid), b: 퀘르세틴-3,4’-디글루코사이드(quercetin-3,4’-diglucoside), c: 퀘르세틴-4’-글루코사이드(quercetin-4’-glucoside), d: 퀘르세틴(quercetin), e: 전체 페놀화합물(total)).
도 3은 양파껍질을 아임계수 추출장치에서 추출온도를 110 내지 130℃로 하며, 추출시간을 5 내지 20분으로 달리하여 추출한 추출물의 페놀화합물의 함량을 측정한 결과이다(a: 프로토카테츄산(protocatechuic acid), b: 퀘르세틴-3,4’-디글루코사이드(quercetin-3,4’-diglucoside), c: 퀘르세틴-4’-글루코사이드(quercetin-4’-glucoside), d: 퀘르세틴(quercetin), e: 전체 페놀화합물(total)).
도 4는 양파껍질을 아임계수 추출 장치에서 추출온도를 110 내지 130℃로 하며, 추출시간을 5 내지 20분으로 달리하여 추출한 추출물의 (A)총페놀의 함량, (B)총플라보노이드의 함량, (C)DPPT 자유라디칼 소거활성, (D)FRAP 활성을 측정한 결과이다.FIG. 1 is a diagram of an apparatus for extracting asymptotic coefficients (BH: band heater, CB: cooling tank, CO 2 TK: CO 2 tank, CV: check valve, F: inline filter, HPP: high pressure pump, N 2 TK: nitrogen tank , P: pressure gauge, RV: reaction tank, SV: safety valve, T: temperature gauge, TC: temperature regulator, V: on / off valve).
FIG. 2 shows the result of measuring the phenol compound content of the extract after extraction at an extraction temperature of 100 to 150 ° C for 5 minutes in the ash factor extracting apparatus (a: protocatechuic acid, b: quercetin-3,4 Quercetin-3,4'-diglucoside, c: quercetin-4'-glucoside, d: quercetin, e: total phenol compound (total)).
FIG. 3 shows the results of measuring the content of phenol compounds in the extracts obtained by extracting the onion skin at an extraction temperature of 110 to 130 ° C. and extracting the extracts at different extraction times of 5 to 20 minutes (a: protocatechuic acid protocatechuic acid, b: quercetin-3,4'-diglucoside, c: quercetin-4'-glucoside, d: quercetin, e: total phenol compound (total)).
FIG. 4 is a graph showing the content of total phenol, (A) total phenol content, (B) total flavonoid content, and total flavonoid content of the extract obtained by extracting the onion skin at an extraction temperature of 110 to 130 ° C. in an asymptotic counting apparatus, (C) DPPT free radical scavenging activity, and (D) FRAP activity.
이하, 본 발명을 실시예에 의해 보다 상세히 설명한다. 단, 하기 실시예는 본 발명을 예시하는 것일 뿐, 본 발명의 내용이 하기의 실시예에 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail by way of examples. However, the following examples are illustrative of the present invention, and the contents of the present invention are not limited to the following examples.
<비교예1> 아임계수를 이용한 양파껍질의 페놀화합물 추출물의 제조≪ Comparative Example 1 > Preparation of phenol compound extract of onion skin using subcriticality coefficient
양파는 시중 마트에서 구입하여 세척한 후 과육과 껍질을 분리하여 동결건조한 후 냉동 보관하였고, 아임계수 추출은 도 1의 아임계수 추출장치를 이용하였다. 동결건조한 양파껍질 2g과 증류수 100㎖를 300㎖ 반응조(RV)에 투입하고 뚜껑을 닫은 후 질소를 통과시켜 시료 용액 중의 용존 산소를 제거하였고, 밴드히터(BH)를 이용하여 100 내지 150℃의 온도로 가열하고, 5 내지 20분 동안 추출하였으며, 추출 후 수돗물을 이용하여 상온으로 냉각하였다. 반응조(RV)의 뚜껑을 개봉한 뒤 반응조(RV) 아래의 밸브(V6)를 열어 추출물을 회수하였고, 100㎖로 정용한 후 여과하여 성분 분석에 사용하였다.The onion was purchased from the market mart, washed, separated from the flesh and the skin, frozen and stored frozen, and the ash factor extraction was performed using the ash factor extraction device of Fig. 2 g of the lyophilized onion skin and 100 ml of distilled water were placed in a 300-ml reaction tank (RV), and the lid was closed. Then, nitrogen was passed through to remove dissolved oxygen in the sample solution and heated to 100 to 150 ° C And extracted for 5 to 20 minutes. After extraction, the solution was cooled to room temperature using tap water. After opening the lid of the reaction tank (RV), the valve (V6) under the reaction tank (RV) was opened to recover the extract.
비교예1의 추출온도와 추출시간은 하기 표 1과 같이 추출하였다.The extraction temperature and extraction time of Comparative Example 1 were extracted as shown in Table 1 below.
<실험방법1> 추출물의 개별 페놀화합물의 분석<Experimental Method 1> Analysis of individual phenol compounds of the extract
개별 페놀화합물의 함량은 고성능액체크로마토그래피(high performance liquid chromatography, HPLC)를 이용하여 분석하였다. 추출물은 2배로 희석한 후 시린지 필터(syringe filter)로 여과한 후 분석하였다. 피크의 분리는 Inertsil ODS-3V 컬럼(5㎛, 4.6 × 250㎜)을 이용하였고 컬럼 온도는 30℃, 유속은 1.0㎖/min, 시료 주입량은 10㎕이었다. 이동상의 용매A(solvent A)로 0.5% 포름산(formic acid) 수용액과 용매B(solvent B)로 아세토나이트릴(acetonitrile)을 사용하였고, 피크 분리를 위한 용매 구배는 0분, 15% B; 15분, 30% B; 30분, 35% B; 32 분, 70% B; 35분, 15% B이었다. 분리된 피크는 PDA 검출기를 이용하여 검출하였고, 분석파장은 280㎚와 360㎚이었다.The contents of the individual phenolic compounds were analyzed using high performance liquid chromatography (HPLC). The extract was diluted 2-fold and then filtered with a syringe filter and analyzed. The peak was separated using an Inertsil ODS-3V column (5 μm, 4.6 × 250 mm) at a column temperature of 30 ° C., a flow rate of 1.0 ml / min and a sample injection volume of 10 μl. The solvent phase for mobile phase A was 0.5% formic acid solution and acetonitrile was used for solvent B. The solvent gradient for peak separation was 0 min, 15% B; 15 min, 30% B; 30 min, 35% B; 32 min, 70% B; 35 minutes and 15% B, respectively. Separated peaks were detected using a PDA detector, and analysis wavelengths were 280 nm and 360 nm.
<실험방법2> 추출물의 총페놀 및 총플라보노이드의 함량 분석<
총페놀의 함량은 다음의 방법으로 측정하였다. 비교예 1-1 내지 1-15의 추출물을 8배로 희석한 추출물 100㎕, 증류수 900㎕, Folin-Ciocalteau's phenol reagent 100㎕를 혼합한 후 5분간 상온에서 반응시켰다. 여기에 20% Na2CO3 300㎕와 증류수를 가하여 2㎖로 정용하였고, 25℃에서 1시간 동안 반응시킨 후 760㎚에서 흡광도를 측정하였다. 총플라보노이드의 함량은 다음의 방법으로 측정하였다. 추출물 원액 200㎕에 에탄올 800㎕와 5% NaNO2 60㎕를 가한 후 5분간 실온에서 반응시켰다. 이 용액에 10% AlCl3를 60㎕ 가하여 실온에서 다시 5분간 반응시킨 후 1M NaOH 용액을 400㎕ 가하여 1분간 상온에서 반응시켰다. 그 뒤 증류수 500㎕를 가하여 균질화시킨 후 415㎚에서 흡광도를 측정하였다.The content of total phenol was measured by the following method. 100 쨉 l of the extract obtained by diluting the extracts of Comparative Examples 1-1 to 1-15 8 times, 900 쨉 l of distilled water and 100 쨉 l of Folin-Ciocalteau's phenol reagent were mixed and reacted at room temperature for 5 minutes. After adding 300 μl of 20% Na 2 CO 3 and distilled water, the mixture was adjusted to 2 ml. After reacting at 25 ° C for 1 hour, absorbance was measured at 760 nm. The content of total flavonoid was measured by the following method. To 200 원 of the extract solution, 800 에 of ethanol and 60 5 of 5% NaNO 2 were added, followed by reaction at room temperature for 5 minutes. To this solution, 60 μl of 10% AlCl 3 was added, reacted for 5 minutes at room temperature, 400 μl of 1 M NaOH solution was added, and the mixture was reacted at room temperature for 1 minute. After that, 500 μl of distilled water was added and homogenized, and the absorbance was measured at 415 nm.
<실험방법3> 항산화 활성의 측정<
항산화 활성을 측정하기 위해 DPPH 자유라디칼 소거활성 및 제2철염 감소 항산화 활성(Ferric reducing antioxidant power, FRAP)을 측정하였다. 4배로 희석한 추출물 0.1㎖에 0.2mM DPPH 용액 2.0㎖을 가하여 30분간 반응시킨 후 517㎚에서 흡광도를 측정하여 DPPH 자유라디칼 소거활성 측정하였고, FRAP은 다음의 방법으로 측정하였다. FRAP 용액은 20mM FeCl3·6H2O 용액, 300mM 아세테이트 버퍼(acetate buffer), 10mM 2,4,6-tripyridyl-s-triazine(TPTZ) 용액(in 40mM HCl)을 1:1:10의 부피비로(v/v)로 혼합하여 제조하였다. 상기 희석한 추출물 0.1㎖에 상기 FRAP 용액 3㎖, 증류수 0.3㎖를 가하여 30분간 37℃에서 반응시킨 후 595㎚에서 흡광도를 측정하였다.To determine antioxidant activity, DPPH free radical scavenging activity and ferric reducing antioxidant power (FRAP) were measured. 2.0 ml of 0.2 mM DPPH solution was added to 0.1 ml of the extract which was diluted four times, and reacted for 30 minutes. Then, the DPPH free radical scavenging activity was measured by measuring the absorbance at 517 nm, and FRAP was measured by the following method. The FRAP solution was prepared by mixing 20 mM FeCl 3 .6H 2 O solution, 300 mM acetate buffer and 10
<비교실험예1> 추출온도 및 추출시간에 따른 아임계수를 이용한 양파껍질의 개별 페놀화합물의 함량 측정<Comparative Experimental Example 1> Determination of content of individual phenol compounds of onion skin by using the subcodes according to extraction temperature and extraction time
양파껍질을 아임계수로 추출한 추출물의 개별 페놀화합물인 프로토카테츄산(protocatechuic acid), 퀘르세틴-3,4’-디글루코사이드(quercetin-3,4’-diglucoside), 퀘르세틴-4’-글루코사이드(quercetin-4’-glucoside), 퀘르세틴(quercetin) 및 이들 전체 페놀 화합물(total)의 함량이 높은 추출온도를 확인하고자, 추출온도별로 양파껍질 아임계수 추출물의 프로토카테츄산(protocatechuic acid), 퀘르세틴-3,4’-디글루코사이드(quercetin-3,4’-diglucoside), 퀘르세틴-4’-글루코사이드(quercetin-4’-glucoside), 퀘르세틴(quercetin)의 함량을 각각 측정하고, 이들의 함량의 합을 전체 페놀 화합물(total)로 계산하였다.The protocatechuic acid, quercetin-3,4'-diglucoside, quercetin-4'-glucoside, which are the individual phenolic compounds of the extract extracted from the onion skin with the limulus- 4'-glucoside, quercetin, and total phenolics (total) were investigated in order to investigate the extraction temperature of protocatechuic acid, quercetin-3,4 The content of quercetin-3,4'-diglucoside, quercetin-4'-glucoside and quercetin was measured, and the sum of these contents was used as the total phenol compound (total).
도 2는 양파껍질을 아임계수 추출장치에서 하기 표 2와 같이 추출온도를 100 내지 150℃로 하여 5분간 추출한 후 추출물의 프로토카테츄산(protocatechuic acid), 퀘르세틴-3,4’-디글루코사이드(quercetin-3,4’-diglucoside), 퀘르세틴-4’-글루코사이드(quercetin-4’-glucoside), 퀘르세틴(quercetin) 및 이들 페놀화합물 전체(total)의 함량을 측정한 결과이다.2 shows the results of extracting the onion skin from the extract of protocatechuic acid, quercetin-3, 4'-di-glucoside -3,4'-diglucoside, quercetin-4'-glucoside, quercetin, and the total amount of these phenol compounds.
전체 페놀함량은 추출온도 100℃에서 130℃로 증가함에 따라 증가하였고 추출온도 130℃에서 15.00㎎/g 건조시료(dry sample)로 100℃에 비해 3.13배 높았으며, 개별 페놀화합물의 함량을 보면 protocatechuic acid는 추출온도가 증가함에 따라 계속 증가하여 150℃에서 9.69㎎/g dry sample로 가장 높았다. quercetin-3,4’-diglucoside의 함량은 120℃에서 0.41 mg/g dry sample로 가장 높았고, quercetin-4’-glucoside의 함량은 120℃와 130℃에서 각각 2.35와 2.24 mg/g dry sample로 가장 높았다. quercetin의 함량은 130℃에서 5.56 mg/g dry sample로 가장 높았으며 100℃에 비해 3.19배 높았다. 특히 protocatechuic acid의 함량은 추출온도의 증가에 따라 계속 증가하였는데, 이는 고온에서 quercetin의 일부가 protocatechuic acid으로 전환되었기 때문이다.The total phenolic content increased with increasing extraction temperature from 100 ℃ to 130 ℃ and was 3.13 times higher than that of 100 ℃ at 15.00㎎ / g dry sample at extraction temperature of 130 ℃. The content of individual phenolic compounds was protocatechuic acid increased continuously as the extraction temperature increased and was the highest at 9.69mg / g dry sample at 150 ℃. The content of quercetin-3,4'-diglucoside was the highest at 0.41 mg / g dry sample at 120 ℃ and the content of quercetin-4'-glucoside was 2.35 and 2.24 mg / g dry sample at 120 ℃ and 130 ℃, respectively. Respectively. The content of quercetin was highest at 5.56 mg / g dry sample at 130 ℃ and 3.19 times higher than that at 100 ℃. In particular, the content of protocatechuic acid increased with increasing extraction temperature, because part of quercetin was converted to protocatechuic acid at high temperature.
protocatechuic acid의 항산화 활성은 quercetin보다 2.1 내지 3.9배 낮은 것으로 알려져 있다. 따라서 추출물의 quercetin의 함량이 높고 protocatechuic acid 함량이 낮을수록 우수한 추출조건이다.The antioxidant activity of protocatechuic acid is 2.1 to 3.9 times lower than that of quercetin. Therefore, the higher the content of quercetin in the extract and the lower the content of protocatechuic acid, the better the extraction condition.
quercetin-3,4’-diglucoside의 함량은 110 내지 130℃에서 높았고, quercetin-4’-glucoside 및 quercetin의 함량은 120 내지 130℃에서 높았으며, protocatechuic acid의 함량은 100 내지 120℃에서 적게 측정되었다.The content of quercetin-3,4'-diglucoside was high at 110 to 130 ° C, the content of quercetin-4'-glucoside and quercetin was high at 120 to 130 ° C, and the content of protocatechuic acid was low at 100 to 120 ° C .
결론적으로, 110 내지 130℃에서 quercetin-3,4’-diglucoside, quercetin-4’-glucoside, quercetin의 함량 높고, protocatechuic acid의 함량이 적어 quercetin의 일부가 protocatechuic acid로의 전환이 적은 것을 확인하여, 110 내지 130℃에서 양파껍질의 아임계수 추출이 우수함을 확인하였다.As a result, it was confirmed that quercetin-3,4'-diglucoside, quercetin-4'-glucoside, quercetin and protocatechuic acid content were low at 110 to 130 ° C, It was confirmed that the extraction of the onion peel was good at 130 ℃.
다음으로, 양파껍질의 아임계수의 추출온도 및 추출시간에 따른 개별 페놀화합물(protocatechuic acid, quercetin-3,4’-diglucoside, quercetin-4’-glucoside, quercetin)의 최적 추출조건을 확인하고자, 우수한 추출온도로 확인한 110 내지 130℃의 온도에서 추출시간을 5분 내지 20분으로 조절하여 추출한 추출물의 protocatechuic acid, quercetin-3,4’-diglucoside, quercetin-4’-glucoside, quercetin의 함량을 각각 측정하고, 이들의 함량의 합을 전체 페놀 화합물(total)로 계산하였다.Next, to determine the optimal extraction conditions of the individual phenolic compounds (protocatechuic acid, quercetin-3,4'-diglucoside, quercetin-4'-glucoside, quercetin) according to extraction temperature and extraction time of onion peel, The contents of protocatechuic acid, quercetin-3,4'-diglucoside, quercetin-4'-glucoside and quercetin in the extracts were measured at the temperature of 110 ~ 130 ℃ , And the sum of these contents was calculated as the total phenol compound (total).
도 3은 하기 표 3과 같이 양파껍질을 아임계수 추출장치에서 추출온도 110 내지 130℃로, 5 내지 20분간 추출한 추출물의 페놀화합물의 함량을 측정한 결과이다. FIG. 3 is a result of measuring the content of a phenol compound in an extract obtained by extracting an onion skin from an extracting apparatus at an extraction temperature of 110 to 130 ° C for 5 to 20 minutes, as shown in Table 3 below.
추출온도 110℃에서 전체 페놀화합물의 함량은 추출시간 15분에서 20.38 mg/g dry sample로 추출시간 5분에 비해 2.46배 높으며, protocatechuic acid의 함량은 추출시간의 증가에 따라 계속 증가하였고, quercetin-3,4’-diglucoside, quercetin-4’-glucoside 및 quercetin의 함량은 추출시간 15분에서 가장 높았으며, quercetin의 함량은 추출시간 15분에서 8.37 mg/g dry sample로 추출시간 5분에 비해 2.70배 높았다. At the extraction temperature of 110 ℃, the content of total phenolic compounds was 2.46 times higher than the extraction time of 5 minutes at 20.38 mg / g dry sample at the extraction time of 15 minutes. The content of protocatechuic acid increased continuously with the extraction time, and quercetin- The contents of 3,4'-diglucoside, quercetin-4'-glucoside and quercetin were the highest at the extraction time of 15 min. The content of quercetin was 8.37 mg / g dry sample at 15 min and 2.70 I was hungry.
추출온도 120℃에서의 전체 페놀화합물의 함량은 추출시간 10분에서 21.64 mg/g dry sample로 가장 높았으며, protocatechuic acid는 추출시간 10분 이상에서는 동일한 함량을 나타내었으며, quercetin-3,4’-diglucoside, quercetin-4’-glucoside, quercetin의 함량은 추출시간 10분에서 가장 높게 나타났다. quercetin의 함량은 추출시간 10분에서 8.87mg/g dry sample로 추출시간 5분에 비해 1.73배 높았다. The content of total phenolic compounds at the extraction temperature of 120 ° C was the highest at 21.64 mg / g dry sample at the extraction time of 10 minutes. The content of protocatechuic acid was the same at the extraction time of 10 minutes and the content of quercetin-3,4'- The content of diglucoside, quercetin-4'-glucoside and quercetin was the highest at the extraction time of 10 minutes. The content of quercetin was 1.73 times higher than the extraction time of 5 minutes at 8.87 mg / g dry sample at the extraction time of 10 minutes.
추출온도 130℃에서는 추출시간의 증가에 따라 potocatechuic acid를 제외하고는 모두 급격히 감소하였다. At the extraction temperature of 130 ℃, all the extracts except potocatechuic acid decreased rapidly with increasing extraction time.
이상의 결과로부터 양파껍질의 아임계수 추출물의 전체 페놀화합물의 함량은 추출온도 120℃에서 10분 동안 추출시 전체 페놀화합물 및 quercetin 추출 수율이 가장 우수함을 확인 하였다.From the above results, it was confirmed that the extraction yield of total phenolic compounds and quercetin was the highest in the total phenolic compound content of the extract of the onion peel during extraction at 120 ℃ for 10 min.
<비교실험예2> 추출온도 및 추출시간에 따른 아임계수를 이용한 양파껍질의 총페놀의 함량, 총플라보노이드의 함량 및 항산화 활성 측정<Comparative Experimental Example 2> Determination of total phenol content, total flavonoid content and antioxidative activity of onion skin by the sublimation coefficient according to extraction temperature and extraction time
다음으로 추출온도 및 추출시간에 따른 아임계수 양파껍질 추출물의 생리활성 성분의 양을 측정하고자, 총페놀의 함량, 총플라보노이드의 함량을 측정하였으며, 항산화 활성을 확인하고자, DPPH 자유라디칼 소거활성과 FRAP을 측정하였다.Then, total phenol contents and total flavonoid contents were measured. To investigate antioxidant activity, DPPH free radical scavenging activity and FRAP activity were investigated in order to determine the amount of physiologically active components of onion skin extracts Were measured.
도 4는 표 3과 같이 양파껍질을 아임계수 추출장치에서 추출온도를 110 내지 130℃, 추출시간을 5 내지 20분으로 달리하여 추출한 추출물의 총페놀의 함량(total phenolics contents, TPC), 총플라보노이드의 함량(total flavonoid contents, TFC) 및 항산화 활성을 측정한 결과이다. 추출온도 110℃와 120℃에서 추출시간에 따른 아임계수 추출물의 총페놀의 함량과 총플라보노이드의 함량의 변화는 개별 페놀화합물의 변화 양상과 유사한 경향을 나타내었다.FIG. 4 is a graph showing the total phenolics contents (TPC), total flavonoids (total phenolics contents), and total flavonoid contents of the extracts obtained by extracting the onion skin with an asymmetric index extracting apparatus at 110-130.degree. (Total flavonoid contents, TFC) and antioxidant activity. The changes of total phenol contents and total phenol contents of sub - extracts at the extraction temperatures of 110 ℃ and 120 ℃ were similar to those of the individual phenolic compounds.
추출온도 110℃에서는 추출시간이 증가할수록 총페놀의 함량이 증가하였으며, 추출시간 15분과 20분에서 각각 56.5와 56.7mg 갈륨산 등가물(gallic acid equivalents, GAE)/g dry sample로 가장 높았다. 총플라보노이드의 함량도 추출시간의 증가에 따라 증가하였으며, 추출시간 15분과 20분에서 각각 34.3와 35.3mg 퀘르세틴 등가물(quercetin equivalents, QE)/g dry sample로 가장 높았다.At the extraction temperature of 110 ℃, the total phenol content increased with increasing extraction time. The highest values were 56.5 and 56.7 mg gallic acid equivalents (GAE) / g dry sample at 15 min and 20 min, respectively. The content of total flavonoids increased with the increase of extraction time, and 34.3 and 35.3mg quercetin equivalents (QE) / g dry samples were the highest at 15 min and 20 min extraction time, respectively.
추출온도 120℃에서는 총페놀의 함량과 총플라보노이드의 함량이 추출시간 10분에서 각각 62.4mg GAE/g dry sample과 34.8mg QE/g dry sample로 가장 높았으며 그 이상의 추출시간에서는 감소하였다.At the extraction temperature of 120 ℃, total phenol contents and total flavonoid contents were highest at 62.4 mg GAE / g dry sample and 34.8 mg QE / g dry sample at 10 minutes of extraction time, respectively.
추출온도 130℃에서는 추출시간 5분에서 TPC와 TFC가 각각 37.8mg GAE/g dry sample과 23.0mg QE/g dry sample로 가장 높았으며, 그 이상의 추출시간에서는 감소하였다. At the extraction temperature of 130 ℃, TPC and TFC were the highest at 37.8 mg GAE / g dry sample and 23.0 mg QE / g dry sample at 5 min extraction time, respectively.
추출시간에 따른 항산화 활성은 TPC와 TFC의 변화 양상과 유사한 경향을 나타내었다. 추출온도 110℃에서의 DPPH 자유라디칼 소거활성과 FRAP는 추출시간이 증가에 따라 증가하여 추출시간 15분에서 각각 41.1mg 아스코르브산 등가물(ascorbic acid equivalents, AAE)/g dry sample과 78.8mmol Fe2+/100g dry sample로 가장 높았으며, 추출온도 120℃에서의 DPPH 자유라디칼 소거활성과 FRAP는 추출시간 10분에서 각각 43.9mg AAE/g dry sample과 80.2mmol Fe2+/100 g dry sample로 가장 높았고, 추출온도 130℃에서의 DPPH 자유라디칼 소거활성은 추출시간의 증가에 따라 증가하였고, FRAP은 추출시간의 증가에 따라 다소 감소하는 특이한 현상을 나타내었는데, 이는 페놀화합물의 영향이라기보다는 고온 열분해 생성물에 의한 것이다.The antioxidative activities of TPC and TFC were similar to those of TPC. The DPPH free radical scavenging activity and FRAP at the extraction temperature of 110 ° C increased with increasing extraction time and reached 41.1 mg ascorbic acid equivalents (AAE) / g dry sample and 78.8 mmol Fe 2+, respectively, / 100g dry sample, and the DPPH free radical scavenging activity and FRAP at the extraction temperature of 120 ° C were the highest at 43.9mg AAE / g dry sample and 80.2mmol Fe 2+ / 100g dry sample at 10 min extraction time, respectively , And the radical scavenging activity of DPPH at the extraction temperature of 130 ℃ increased with increasing extraction time. FRAP showed a slight decrease with increasing extraction time, .
이상의 결과로부터 추출온도 120℃에서 10분간 추출한 아임계수 추출물이 총페놀의 함량(total phenolics contents, TPC) 및 총플라보노이드의 함량(total flavonoid contents, TFC)이 높아 생리활성 성분의 함량이 우수하며, 항산화 활성이 우수함을 확인하였다.From the above results, the total phenolics contents (TPC) and the total flavonoid contents (TFC) of the ash extract extracts extracted at 120 ° C for 10 minutes were high, Activity.
<실시예1> 이산화탄소를 첨가한 아임계수를 이용한 양파껍질의 페놀화합물 추출물의 제조Example 1 Preparation of Phenol Compound Extract of Onion Peel Using Carbon Dioxide Additive Coefficient
아임계수에 의하여 페놀화합물 특히 비극성인 quercetin의 추출을 최대한 증가시킬 수 있을 것으로 기대하였으나, 비교실험예들에서 추출 및 가수분해에 의해 생성되었던 quercetin 중 상당량이 고온의 아임계수 처리로 인하여 quercetin과 비교하여 상대적으로 항산화 활성이 낮은 protocatechuic acid으로 전환되는 것을 알 수 있었다. 따라서 quercetin이 protocatechuic acid로의 전환을 방지하기 위해 최적 추출온도 및 추출시간을 낮출 필요가 있다. 이를 위하여 아임계수에 CO2를 첨가하여 양파껍질을 추출한 추출물을 제조하였다.It was expected that the extraction of phenolic compounds, especially non-polar quercetin, would be maximized by the submixture, but in comparative experiments a significant amount of quercetin, which was produced by extraction and hydrolysis, was compared with quercetin And it was converted to protocatechuic acid which is relatively low in antioxidative activity. Therefore, it is necessary to lower the optimum extraction temperature and extraction time to prevent the conversion of quercetin to protocatechuic acid. For this purpose, extracts of onion skin were prepared by adding CO 2 to sub -
물에 CO2를 첨가하면 탄산이 생성되며 탄산이 해리되면 수소이온이 유리되어 용액의 pH가 낮아지게 되므로, 결합형 페놀화합물이나 quercetin 배당체의 가수분해를 촉진하게 된다.When CO 2 is added to water, carbonic acid is formed. When carbonic acid dissociates, hydrogen ions are liberated and the pH of the solution is lowered, thereby promoting the hydrolysis of the bonded phenolic compound or quercetin glycoside.
따라서 비교예들에서 우수한 추출조건으로 확인한 120℃에서 10분간 추출하였을 때보다 낮은 온도, 짧은 시간 조건으로 확인하고자 110 내지 120℃에서 5 내지 10분간 추출하여 실시예를 제조하였다.Therefore, the extracts were prepared by extracting at 110 to 120 ° C for 5 to 10 minutes in order to confirm the conditions under which the extracting conditions were excellent at 120 ° C for 10 minutes and at a lower temperature and for a shorter time.
상온에서 액체 이산화탄소를 고압펌프(HPP)를 이용하여 반응조(RV)에 65bar로 주입하고, 추출온도 및 시간을 달리한 것을 제외하고 비교예1과 동일한 방법으로 양파껍질 추출물을 제조하였으며, 실시예1의 추출온도와 추출시간은 하기 표 4와 같이 추출물을 제조하였다.The onion skin extract was prepared in the same manner as in Comparative Example 1, except that the liquid carbon dioxide was injected at 65 bar into the reaction tank (RV) using a high-pressure pump (HPP) at room temperature and the extraction temperature and time were different. The extracts were prepared as shown in Table 4 below.
<실험예1> 추출온도 및 추출시간에 따른 이산화탄소 첨가 아임계수를 이용한 양파껍질의 개별 페놀화합물의 함량 측정<Experimental Example 1> Determination of content of individual phenolic compounds in onion skin using carbon dioxide addition index according to extraction temperature and extraction time
추출온도 및 추출시간에 따른 양파껍질을 이산화탄소를 첨가한 아임계수로 추출한 추출물의 개별 페놀화합물인 protocatechuic acid, quercetin-3,4’-diglucoside, quercetin-4’-glucoside, quercetin 및 이들 전체 페놀 화합물(total)의 함량이 높은 추출온도 및 추출시간을 확인하고자, 추출온도 110℃ 내지 120℃에서 5분 내지 10분 동안 추출한 추출물에서 상기 protocatechuic acid, quercetin-3,4’-diglucoside, quercetin-4’-glucoside, quercetin 및 이들 전체 페놀 화합물(total)의 함량을 측정하였다.Quercetin-4'-glucoside, quercetin-4'-glucoside, quercetin, and all of these phenolic compounds, which are the individual phenolic compounds of extracts extracted from the onion skin with carbon dioxide added by extraction temperature and extraction time quercetin-3,4'-diglucoside, quercetin-4'-deoxycholic acid, and quercetin-4'-diglucoside were extracted from the extracts extracted for 5 minutes to 10 minutes at an extraction temperature of 110 ° C to 120 ° C to confirm the extraction temperature and extraction time, glucoside, quercetin and total phenolic compounds (total) were measured.
CO2를 상온에서 65bar로 증류수에 가하여 110℃와 120℃에서 5분과 10분 동안 양파껍질을 처리한 추출물 및 동일조건에서 CO2를 첨가하지 않은 비교예의 protocatechuic acid, quercetin-3,4’-diglucoside, quercetin-4’-glucoside, quercetin 및 이들 전체 페놀 화합물(total)의 함량은 표 5와 같다.Comparative Examples was added to distilled water, the CO 2 to 65bar at room temperature without addition of CO 2 in the onionskin extract and process the same conditions for at 110 ℃ and 120 ℃ 5 minutes and 10 minutes protocatechuic acid, quercetin-3,4'-diglucoside , quercetin-4'-glucoside, quercetin and their total phenolic compounds (total) are shown in Table 5.
3,4’-diglucosideQuercetin-
3,4'-diglucoside
4’-glucosideQuercetin-
4'-glucoside
전체 페놀화합물의 함량을 보면, CO2를 첨가하고 110℃에서 5분간 추출하였을 때 18.43mg/g dry sample로 CO2를 첨가하지 않았을 때의 8.26mg/g dry sample보다 2.23배 높았다. 110℃에서 10분과 120℃에서 5분에서도 CO2를 첨가하였을 때는 CO2를 첨가하지 않았을 때보다 전체 페놀화합물의 함량이 각각 1.39배와 1.51배 높았다. 이는 CO2의 첨가로 아임계수의 pH가 낮아져 결합형 페놀화합물의 가수분해가 증가하고 낮은 pH로 인해 더 많은 페놀화합물이 추출된 것이다.The contents of total phenolic compounds were 2.23 times higher than 8.26mg / g dry sample without CO 2 at 18.43mg / g dry sample when CO 2 was added and extracted at 110 ° C for 5 minutes. At 110 ℃ in 10 minutes and 120 ℃ 5 bun in the amount of the total phenolic compounds were 1.39 times and 1.51 times respectively, than would not have the addition of CO 2, when the addition of CO 2. This is because the addition of CO 2 lowers the pH of the subcycle, increasing the hydrolysis of the coupled phenolic compounds and the extraction of more phenolic compounds due to the low pH.
개별 페놀화합물의 함량을 보면, CO2를 첨가한 아임계수 추출에서 추출온도 110℃에서 5분간 추출하였을 때, protocatechuic acid, quercetin-3,4’-diglucoside, quercetin-4’-diglucoside 및 quercetin의 함량은 CO2를 첨가하지 않았을 때보다 각각 1.58, 1.82, 2.38, 2.89배 증가하였으며, 이 중 quercetin의 증가율이 2.89배로 가장 높았으며 protocatechuic acid의 증가율이 1.58배로 가장 낮았다. 이로 보아 아임계수에 CO2 첨가로 인하여 quercetin이 protocatechuic acid로의 전환을 방지된 것을 확인할 수 있었다.The contents of the individual phenolic compounds were determined by extraction with CO 2 for 5 min at extraction temperature of 110 ° C. The content of protocatechuic acid, quercetin-3,4'-diglucoside, quercetin-4'-diglucoside and quercetin , 1.58, 1.82, 2.38 and 2.89 times higher than without CO 2 , respectively. Among them, quercetin increased 2.89 times and protocatechuic acid had the lowest growth rate 1.58 times. From this result, it was confirmed that the conversion of quercetin to protocatechuic acid was prevented due to the addition of CO 2 to the asymptotic coefficient.
CO2를 첨가한 아임계수 추출에서 추출온도 110℃에서 10분간 추출하였을 때와 CO2를 첨가하지 않았을 때 보다 개별 페놀화합물의 함량이 1.22 내지 1.54배 높았으며, 120℃에서 5분간 추출하였을 때, CO2를 첨가하지 않았을 때 보다 개별 페놀화합물의 함량이 1.26 내지 1.75배 높았다. 특히 이산화탄소를 첨가하고 110℃에서 10분간 추출한 양파껍질 추출물에서 quercetin의 함량은 9.23㎎/g으로 가장 높았다. 이 경우에도 quercetin의 증가율이 가장 높았고 protocatechuic acid의 증가율이 가장 낮았는데, 이로 보아 65bar의 CO2의 첨가가 아임계수 추출에서 quercetin이 protocatechuic acid로의 전환을 방지함을 확인하였다.When was the amount at the time when extracted for 10 minutes at
또한, 110℃에서 5분간 추출한 CO2 첨가에 의한 페놀화합물의 함량의 증가율은 다른 추출온도와 추출시간 보다 높았는데, 이는 저온에서 가수분해 및 추출되는 페놀화합물의 양이 작아 CO2 첨가에 의한 추출 수율의 향상효과가 상대적으로 크게 나타난 것이다. In addition, the rate of increase in the content of phenol compounds by CO 2 addition is extracted for 5 minutes at 110 ℃ is I was higher than other extraction temperature and extraction time, which is the amount of the phenol compound to be hydrolyzed and extracted from the low-temperature smaller extraction with CO 2 is added The improvement effect of the yield is relatively large.
결론적으로 아임계수에 CO2를 첨가하면, quercetin 및 이들 배당체의 최적 추출온도 120℃에서 110℃로 낮출 수 있으며, 최적 추출시간을 10분에서 5분으로 줄일 수 있고, quercetin의 파괴 및 protocatechuic acid로의 전환이 방지할 수 있으며, 양파껍질 추출물에서 생리활성 물질인 페놀화합물을 증가시킬 수 있다.In conclusion, the addition of CO 2 to the subcycle can lower the optimum extraction temperature of quercetin and these glycosides to 110 ° C at 120 ° C, reduce the optimum extraction time from 10 minutes to 5 minutes, and break down quercetin and protocatechuic acid The conversion can be prevented, and the phenolic compound, which is a physiologically active substance, can be increased in the onion skin extract.
<실험예2> 추출온도 및 추출시간에 따른 이산화탄소 첨가 아임계수를 이용한 양파껍질의 총페놀의 함량, 총플라보노이드의 함량 및 항산화 활성<Experimental Example 2> Total phenol content, total flavonoid content and antioxidant activity of onion skin using carbon dioxide addition index according to extraction temperature and extraction time
CO2를 상온에서 65bar로 증류수에 가하여 110℃와 120℃에서 5분과 10분 동안 양파껍질을 처리한 추출물 및 동일조건에서 CO2를 첨가하지 않은 비교예의 총페놀의 함량, 총플라보노이드의 함량, 항산화 활성(DPPH 자유라디칼 소거활성, FRAP)은 표 6과 같다. CO 2 and the reaction mixture in distilled water to 65bar at room temperature at 110 ℃ and 120 ℃ 5 minutes and 10 minutes onion skin treated with the extract, and the content of total phenolic comparative example without addition of CO 2 under the same conditions for the content of total flavonoids, antioxidants The activity (DPPH free radical scavenging activity, FRAP) is shown in Table 6.
(mg GAE/g)Total phenolic content
(mg GAE / g)
(mg QE/g)Total flavonoid content
(mg QE / g)
(mg AAE/g)DPPH
(mg AAE / g)
(mmol Fe2+/100 g)FRAP
(mmol Fe < 2 + > / 100 g)
65bar의 CO2를 첨가하였을 때는 CO2를 첨가하지 않았을 때보다 총페놀의 함량, 총플라보노이드의 함량, DPPH 자유라디칼 소거활성 및 FRAP 활성이 110℃에서 5분간 추출하였을 때 TPC는 3.17배, TFC는 2.97배, DPPH 자유라디칼 소거활성은 2.48배, FRAP은 2.54배 증가하였고, 110℃에서 10분간 추출 시 TPC는 1.96배, TFC는 1.78배, DPPH 자유라디칼 소거활성은 1.69배, FRAP은 1.70배 증가하였고, 120℃에서 5분간 추출시 TPC 2.18배, TFC 2.10, DPPH 자유라디칼 소거활성은 1.72, FRAP은 1.94배 증가하였다. CO2 첨가에 의한 TPC와 TFC의 증가 효과는 첨가한 CO2에 의해 생성된 탄산이 산 촉매로 작용하여 결합형 페놀화합물의 가수분해를 촉진하였기 때문이며, 이로 인하여 항산화 효과(DPPH 자유라디칼 소거활성, FRAP)도 증가하였다.When 65 bar CO 2 was added, total phenol content, total flavonoid content, DPPH free radical scavenging activity and FRAP activity were 3.17 times higher than that without CO 2 , 3.17 times at 110 ℃, TFC 2.97 times, DPPH free radical scavenging activity was increased 2.48 times and FRAP was increased 2.54 times. The TPC, TFC, and free radical scavenging activity were 1.96 times, 1.78 times, 1.69 times and 1.70 times, respectively TPC 2.18 times, TFC 2.10, DPPH free radical scavenging activity 1.72 and FRAP 1.94 times at the extraction temperature of 120 ℃ for 5 minutes. The increase of TPC and TFC by the addition of CO 2 is due to the fact that the carbonic acid produced by the added CO 2 acts as an acid catalyst to accelerate the hydrolysis of the coupled phenolic compounds and as a result the antioxidative effect (DPPH free radical scavenging activity, FRAP) also increased.
CO2 첨가에 의한 TPC, TFC, DPPH 자유라디칼 소거활성, FRAP 활성의 증가 효과는 110℃에서 5분간 추출한 추출물에서 가장 높았는데, 이는 110℃에서 5분간 추출하는 조건이 110℃에서 10분, 120℃에서 5분간 추출하는 조건에 비해 페놀화합물이 추출 및 가수분해되는 양이 적고 이로 인해 CO2 첨가에 의한 효과가 상대적으로 크게 나타난 것이다. 따라서 아임계수에 CO2를 가하면 보다 낮은 추출온도와 추출시간에서 높은 TPC와 TFC를 얻을 수 있었으며, 이로 인하여 항산화 활성(DPPH 자유라디칼 소거활성, FRAP)이 높은 추출물을 얻을 수 있었다.The increase of TPC, TFC, DPPH free radical scavenging activity and FRAP activity by CO 2 addition was the highest in extracts extracted at 110 ℃ for 5 min. The extraction and hydrolysis of the phenolic compounds was less than that of the extraction at 5 ° C for 5 minutes and the effect of CO 2 addition was relatively large. Therefore, when CO 2 was added to the asymmetry index, high TPC and TFC could be obtained at lower extraction temperature and extraction time, resulting in higher antioxidative activity (DPPH free radical scavenging activity, FRAP).
상기한 바와 같이, 본 발명인 CO2를 첨가한 아임계수를 이용하는 추출법을 특정 조건에서 수행하는 경우, 양파껍질 추출물의 생리활성 물질인 페놀화합물과 플라보노이드의 함량이 증가하였을 뿐만 아니라, 친환경 및 무독성 용매를 사용하므로 용매 제거를 위한 추가공정이 발생되지 아니하고, 환경문제도 발생되지 아니한다. 또한 추출온도를 낮추고, 추출시간을 줄일 수 있어 추출물 제조비용이 감소하여 경제적이다. 또한, 상기 본 발명의 방법은 우리나라 전역에 분포되어 있는 양파로부터 수득한 양파껍질을 이용하여 항산화 활성을 비롯한 여러 기능성이 우수한 물질인 퀘르세틴 및 이의 배당체들을 효율적으로 수득할 수 있는 방법이므로, 양파를 이용한 기능성 식품의 개발, 식품 소재의 개발, 화장품 소재의 개발 등 다양한 산업분야에 활용될 수 있을 것으로 기대된다.As described above, when the extraction method using the ash factor with CO 2 added according to the present invention is carried out under specific conditions, not only the content of the phenolic compounds and flavonoids, which are physiologically active substances of the onion skin extract, but also the environmentally and nontoxic solvents So that an additional process for removing the solvent does not occur and no environmental problems occur. In addition, since the extraction temperature can be lowered and the extraction time can be shortened, the manufacturing cost of the extract is reduced, which is economical. In addition, since the method of the present invention can efficiently obtain quercetin and its glycosides having various functions including antioxidative activity using onion peels obtained from onion distributed throughout Korea, It is expected to be used in various industrial fields such as development of functional food, development of food material, development of cosmetic material.
Claims (7)
상기 반응조에 질소를 통과시켜 용존 산소를 제거하는 단계;
이산화탄소를 상기 반응조에 50 내지 80bar의 압력으로 주입하고, 상기 반응조를 가열하는 단계;
105 내지 125℃의 온도 및 80 내지 300bar의 압력 조건에서 3 내지 13분 동안 추출하여 양파껍질의 아임계수 추출물을 수득하는 단계;
상기 양파껍질의 아임계수 추출물에서 생리활성 성분을 분리하는 단계를 포함하는, 이산화탄소가 첨가된 아임계수를 이용하여 양파로부터 분리되는 생리활성 성분을 증가시키는 방법.Introducing the onion skin and water into the reaction tank of the ash extraction apparatus;
Passing nitrogen through the reaction tank to remove dissolved oxygen;
Injecting carbon dioxide into the reaction tank at a pressure of 50 to 80 bar and heating the reaction tank;
Extracting for 3 to 13 minutes at a temperature of 105 to 125 DEG C and a pressure of 80 to 300 bar to obtain a subliming extract of onion skin;
Isolating the physiologically active component from the limulus extract of the onion skin. ≪ RTI ID = 0.0 > 11. < / RTI >
상기 추출은 80 내지 300bar 압력조건에서 110℃에서 5분 내지 10분, 또는 120℃에서 5분간 진행되는 것인, 양파로부터 분리되는 생리활성 성분을 증가시키는 방법.The method according to claim 1,
Wherein the extraction is carried out at 110 DEG C for 5 minutes to 10 minutes or at 120 DEG C for 5 minutes under a pressure of 80 to 300 bar.
상기 이산화탄소 주입에 의해, 프로토카테츄산(protocatechuic acid)의 생성을 억제하는 것인, 양파로부터 분리되는 생리활성 성분을 증가시키는 방법.The method according to claim 1,
Wherein the carbon dioxide injection inhibits the production of protocatechuic acid.
상기 생리활성 성분은 i) 퀘르세틴-3,4’-디글루코사이드(quercetin-3,4’-diglucoside), 퀘르세틴-4’-글루코사이드(quercetin-4’-glucoside) 및 퀘르세틴(quercetin)으로 이루어진 군에서 선택되는 하나 이상을 포함하는 총 페놀화합물; 또는 ii) 총 플라보노이드 화합물인 것인, 양파로부터 분리되는 생리활성 성분을 증가시키는 방법.The method of claim 1,
Wherein said physiologically active ingredient is selected from the group consisting of i) quercetin-3,4'-diglucoside, quercetin-4'-glucoside and quercetin A total phenolic compound comprising at least one selected; Or ii) is a total flavonoid compound.
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| 고민정. Subcritical water extraction of flavonol quercetin from onion skin. 이화여자대학교 석사학위논문(2010.05.12.)* * |
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