KR100511802B1 - Extraction Method of Resveratrol from Grape - Google Patents
Extraction Method of Resveratrol from Grape Download PDFInfo
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- KR100511802B1 KR100511802B1 KR10-2002-0044436A KR20020044436A KR100511802B1 KR 100511802 B1 KR100511802 B1 KR 100511802B1 KR 20020044436 A KR20020044436 A KR 20020044436A KR 100511802 B1 KR100511802 B1 KR 100511802B1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0261—Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
- B01D11/0265—Applying ultrasound
Abstract
본 발명은 포도의 송이가지를 원료로 하여 물/에탄올 혼합 용매와 초음파를 이용하여 레스베라트롤를 추출하는 방법에 관한 것으로서, 포도의 송이가지를 원료로 하여 1개월 동안 일광건조하고, 입도가 0.3∼0.5 mm\가 되도록 분쇄한 분쇄물을 추출원료로 하며, 물과 에탄올을 부피기준으로 2:8 내지 3:7 로 혼합한 혼합물을 용매로 하여 건조된 분쇄물 1 kg 당 용매를 5∼10 L 투입한 후, 실온에서 45∼50 kHz의 초음파를 상기 분쇄물이 투입된 1 L 의 용매당 0.03∼0.05 kW의 에너지 강도로 3∼5분간 처리하여 레스베라트롤을 추출함으로써 안전하면서도 추출 효과가 매우 양호한 장점을 갖는다.The present invention relates to a method for extracting resveratrol by using a water-ethanol mixed solvent and ultrasonic wave as a raw material of grapes as a raw material, which is sun-dried for 1 month using a pine branch of grapes as a raw material, and has a particle size of 0.3 to 0.5 mm The pulverized pulverized product as \ was used as an extraction material, and 5-10 L of solvent was added per kg of the dried pulverized product, using a mixture of water and ethanol at a volume basis of 2: 8 to 3: 7 as a solvent. Subsequently, the ultrasonic wave of 45-50 kHz at room temperature is treated for 3 to 5 minutes at an energy intensity of 0.03 to 0.05 kW per 1 L of the pulverized powder, thereby extracting resveratrol, which is safe and has an excellent extraction effect.
Description
본 발명은 포도로부터 레스베라트롤을 추출하는 방법에 관한 것으로서, 보다 상세하게는, 포도의 송이 가지를 원료로 하여 물/에탄올 혼합 용매와 초음파 처리에 의해 레스베라트롤를 추출하는 방법에 관한 것이다. The present invention relates to a method for extracting resveratrol from grapes, and more particularly, to a method for extracting resveratrol by using water / ethanol mixed solvent and sonication, using a cluster of grape branches as a raw material.
레스베라트롤(resveratrol, 3,4'5-trihydroxystilbene)은 포도 및 여러 식물에서 발견된 피토알렉신(phytoalexin)화합물로써 항암, 항혈전, 및 항염증 활성 등 여러 생리적·약리적작용을 지니고 있다. 특히, 레스베라트롤은 최근 여성호르몬 에스트로겐 유사작용이 있는 피토에스트로겐(phytoestrogen) 화합물로써 밝혀지면서 갱년기 이후 여성의 심장병, 골다공증, 치매증 및 여러 갱년기증상을 억제해주는 생리활성물질로써 새로이 각광을 받고 있다.Resveratrol (3,4'5-trihydroxystilbene) is a phytoalexin compound found in grapes and various plants and has various physiological and pharmacological effects including anticancer, antithrombotic, and anti-inflammatory activity. In particular, resveratrol has recently emerged as a phytoestrogen compound having a female hormone estrogen-like action, and has recently been in the spotlight as a bioactive substance that suppresses cardiac disease, osteoporosis, dementia and various menopausal symptoms after menopause.
종래에는 이러한 레스베라트롤을 수득하기 위해서, 포도의 덩굴, 또는 포도 과실의 껍질 및 씨를 원료로 하여 에탄올, 메탄올, 아세톤 등의 유기용매를 가온처리하여 레스베라트롤을 추출하는 방법이 사용되어 왔다. Conventionally, in order to obtain such resveratrol, a method of extracting resveratrol by heating an organic solvent such as ethanol, methanol, acetone, etc., using grape vines or grape fruit skin and seeds as raw materials has been used.
이러한 종래의 유기 용매에 의한 추출에 있어서는 30 ℃ 에서 20 시간 추출, 또는 60 ℃ 에서 30 분 추출조건이 최대 추출 조건으로 되어왔다. 이러한 종래의 추출방법에 있어서의 추출조건은 중저온 조건에서는 많은 추출시간이 소요되는 단점이 있고, 고온조건에서는 추출시간은 단축되나 유기용매의 폭발 위험이 매우 높은 단점이 있다. 한편, 추출조건이 지나치게 강하거나 추출시간이 필요 이상으로 길 경우 추출된 레스베라트롤이 오히려 분해되어 손실될 우려가 있었다.In the extraction by such a conventional organic solvent, the extraction conditions for 20 hours at 30 ° C or 30 minutes at 60 ° C have become the maximum extraction conditions. Extraction conditions in the conventional extraction method has a drawback that takes a lot of extraction time in the low and medium temperature conditions, extraction time is shortened in high temperature conditions, but there is a high risk of explosion of the organic solvent. On the other hand, if the extraction conditions are too strong or the extraction time is longer than necessary, there is a fear that the extracted resveratrol is rather decomposed and lost.
따라서 상기와 같은 종래의 유기용매를 이용한 포도로부터 레스베라트롤을 추출하는 방법에 있어서, 고온 추출시의 작업상의 위험 및 제품 분해 위험, 저온 추출시의 장시간의 작업으로 인한 공정 효율 저하를 해결할 있는 추출방안에 대한 필요가 제기되어 왔다.Therefore, in the method of extracting resveratrol from grapes using the conventional organic solvent as described above, there is an extraction scheme that can solve the operational risks and product decomposition risks at high temperature extraction, process efficiency degradation due to long time operation at low temperature extraction The need has been raised.
본 발명은 상기와 같은 문제를 해결하고자 안출된 것으로서, 포도를 유기 용매와 초음파를 이용하여 추출함으로써 레스베라트롤의 추출 효율이 높으면서도 안전한 공정 조건에서의 실시가 가능한 레스베라트롤 추출방법을 제공하기 위한 것이다. The present invention has been made to solve the above problems, it is to provide a resveratrol extraction method that can be carried out under safe process conditions while high extraction efficiency of resveratrol by extracting grapes using an organic solvent and ultrasonic waves.
포도에서 레스베라트롤을 추출함에 있어서, 본 발명은In extracting resveratrol from grapes, the present invention
a) 포도 송이가지를 건조시키는 단계;a) drying the grape cluster;
b) 상기 포도 송이가지를 분쇄하여 분쇄물을 수득하는 단계;b) grinding the grape cluster branches to obtain a pulverized product;
c) 상기 분쇄물을 용매에 투입하는 단계;c) introducing the milled product into a solvent;
d) 상기 분쇄물이 투입된 상기 용매를 초음파로 처리하는 단계d) ultrasonically treating the solvent into which the pulverized powder is added;
를 포함하는 방법으로 이루어진다. It consists of a method comprising a.
상기 포도는 통상의 포도를 사용할 수 있으며, 레스베라트롤의 함량이 많은 송이가지 부위를 사용하는 것이 바람직하다. The grape may be used as a normal grape, it is preferable to use a cluster branch site with a high content of resveratrol.
상기 건조는 건조기를 이용한 강제 건조 및 자연건조가 가능하나, 원료에 함유된 성분의 보존을 위해서 자연건조 하는 것이 바람직하고, 일광 건조하는 것이 보다 바람직하다. The drying may be forced drying using a dryer and natural drying, but for natural preservation of the ingredients contained in the raw material is preferably natural drying, more preferably daylight drying.
상기 포도원료의 분쇄는 본원 발명이 속하는 분야에서 통상적으로 사용하는 분쇄기를 사용할 수 있으며, 특별한 제한은 없다. 상기 분쇄물은 0.3 - 0.5 mm 의 입도를 가지는 것이 바람직하며, 이는 추출 용매 및 초음파에 의한 추출에 있어서 효율을 높이기 위한 것이다. 0.5 mm 를 초과시에는 용매의 추출효율이 낮아지며, 너무 작을 경우에는 작업성이 나쁘게 된다.The pulverization of the grape raw material may use a grinder commonly used in the field of the present invention, there is no particular limitation. The pulverized product preferably has a particle size of 0.3-0.5 mm, which is intended to increase efficiency in extraction by extraction solvent and ultrasonic waves. If it exceeds 0.5 mm, the extraction efficiency of the solvent becomes low, and if it is too small, workability becomes bad.
발명의 바람직한 실시에 있어서, 상기 용매는 물, 에탄올, 메탄올, 아세톤 등을 이용할 수 있으며, 물과 에탄올, 메탄올, 아세톤등을 혼합하여 사용하는 것이 바람직하며, 물과 에탄올을 혼합하여 사용하는 것이 가장 바람직하다. 발명의 한 바람직한 실시에서는 상기 분쇄물 1 kg 당 물과 에탄올을 부피기준으로 2:8 내지 3:7 로 혼합한 용매 5∼10 L 투입한다. In a preferred embodiment of the invention, the solvent may be water, ethanol, methanol, acetone and the like, it is preferable to use a mixture of water and ethanol, methanol, acetone, etc., it is most preferable to use a mixture of water and ethanol desirable. In a preferred embodiment of the invention, 5 to 10 L of a solvent mixed with water and ethanol at a volume basis of 2: 8 to 3: 7 is added per kg of the pulverized product.
상기 분쇄물이 투입된 용매를 초음파로 처리하여 추출효과를 높이는 것이 바람직하다. 초음파로 처리하지 않으면, 저온에서는 추출속도가 늦어지게 되며, 추출속도를 증가시키기 위해서는 이를 고온으로 가열하여야 하는 문제가 있다. It is preferable to increase the extraction effect by treating the solvent in which the pulverized product is added with ultrasonic waves. If it is not treated with ultrasonic waves, the extraction rate is slow at low temperatures, and there is a problem in that it is heated to a high temperature in order to increase the extraction rate.
초음파는 실온에서 45 ∼ 50 kHz의 범위로 1 ℓ의 용액당 0.03∼0.05 kW의 에너지 강도로 3∼5분간 처리하는 것이 레스베라트롤을 효율적인 추출을 위해서 보다 바람직하다. Ultrasound is more preferably treated for 3 to 5 minutes at room temperature with an energy intensity of 0.03 to 0.05 kW per 1 L solution in the range of 45 to 50 kHz for efficient extraction of resveratrol.
본 발명의 보다 용이한 실시를 위하여 하기의 실시예를 참조할 수 있으며, 하기 실시예가 발명의 범위를 한정하는 것으로 해석되지 않는다는 것은 본 발명이 속하는 분야에서 통상의 지식을 가지는 자에게 자명할 것이다.Reference may be made to the following examples for easier implementation of the invention, and it will be apparent to those skilled in the art that the following examples are not to be construed as limiting the scope of the invention.
[실시예]EXAMPLE
실시예 1Example 1
구입한 거봉 포도에서 송이가지를 분리하고, 1 개월간 일광건조를 실시하였다. 분쇄기를 이용하여 건조된 송이가지를 평균 0.4 mm 의 직경으로 분쇄한 후, 분쇄물 150 g 을 물 250 ml 와 에탄올 750 ml 를 혼합한 용액에 투입하였다. 초음파 발생기를 이용하여 실온에서 50 kHz 주파수의 초음파를 발생시켜 3 분간 처리하였다. Pine branches were isolated from the purchased grape grapes and sun-dried for 1 month. The dried clustered branches were crushed to an average diameter of 0.4 mm using a grinder, and then 150 g of the ground product was added to a solution in which 250 ml of water and 750 ml of ethanol were mixed. The ultrasonic generator was used to generate ultrasonic waves at a frequency of 50 kHz at room temperature and treated for 3 minutes.
수득된 레스베라트롤의 중량을 건조물 중량과 대비한 결과치를 측정하였다.The weight of the obtained resveratrol was measured as a result of comparing with the weight of the dry matter.
실시예 2Example 2
실시예 1 과 동일한 조건에서 초음파로 5 분간 실시하였다. It carried out for 5 minutes by ultrasonic waves under the same conditions as in Example 1.
실시예 3Example 3
켐벨포도를 이용하여 실시예 1 과 동일한 조건으로 실시하였다. It was carried out under the same conditions as in Example 1 using Campbell grapes.
실시예 4. Example 4.
켐벨 포도를 이용하여 실시예 2 와 동일한 조건으로 실시하였다.It was carried out under the same conditions as in Example 2 using Campbell grapes.
비교예 1Comparative Example 1
구입한 거봉 포도에서 송이가지를 분리하고, 1 개월간 일광건조를 실시하였다. 분쇄기를 이용하여 건조된 송이가지를 평균 0.4 mm 의 직경으로 분쇄한 후, 분쇄물 150 g 을 물 250 ml 와 에탄올 750 ml 를 혼합한 60 ℃ 용액에 투입하였다. 30 분후에 추출을 종료하고 수득된 레스베라트롤의 중량을 건조물 중량과 대비한 결과치를 측정하였다.Pine branches were isolated from the purchased grape grapes and sun-dried for 1 month. The dried clustered branches were pulverized to an average diameter of 0.4 mm using a grinder, and then 150 g of the ground product was added to a 60 ° C. solution in which 250 ml of water and 750 ml of ethanol were mixed. The extraction was terminated after 30 minutes and the weight of the resveratrol obtained was compared with the weight of the dry matter.
비교예 2Comparative Example 2
켐벨 포도를 이용하여 비교예 1 과 동일한 조건에서 실시하였다. Campbell grapes were used under the same conditions as in Comparative Example 1.
하기의 표 1은 본 발명에서 고안한 방법으로 포도의 송이가지를 원료로 하여 추출된 레스베라트롤의 추출량을 종래의 방법으로 추출된 양과 비교한 결과를 나타내고 있다.Table 1 below shows the results of comparing the extraction amount of resveratrol extracted by using the cluster of grapes as a raw material of the present invention with the amount extracted by the conventional method.
본 발명의 방법에 의해서 포도로부터 레스베라트롤 추출함에 있어서, 원료로서 레스베라트롤의 함량이 상대적으로 높은 송이가지를 사용하며, 이를 유기 용매와 초음파를 이용하여 추출함으로서 레스베라트롤의 추출 효율이 높으면서도 안전한 공정 조건에서의 실시가 가능한 레스베라트롤 추출방법과 이에 의해 추출된 레스베라트롤을 제공하도록 하였다. In extracting resveratrol from grapes by the method of the present invention, a pine branch having a relatively high content of resveratrol is used as a raw material, and extracted using an organic solvent and ultrasonic wave to extract resveratrol at a safe and safe process condition. It was to provide a resveratrol extraction method that can be carried out and the resveratrol extracted thereby.
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WO1999003816A1 (en) * | 1997-07-15 | 1999-01-28 | Caudalie | Compositions based on resveratrol |
KR20000000342A (en) * | 1999-10-13 | 2000-01-15 | 황재관 | Extraction of antibacterials from Curcuma xanthorrhiza Roxb. |
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WO1999003816A1 (en) * | 1997-07-15 | 1999-01-28 | Caudalie | Compositions based on resveratrol |
KR20000000342A (en) * | 1999-10-13 | 2000-01-15 | 황재관 | Extraction of antibacterials from Curcuma xanthorrhiza Roxb. |
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KR100893788B1 (en) * | 2007-10-11 | 2009-04-20 | 서원대학교산학협력단 | Method for purification of resveratrol from extract of grape twig |
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