KR20160072407A - Acorn separation and antioxidant capacity of the active ingredient - Google Patents
Acorn separation and antioxidant capacity of the active ingredient Download PDFInfo
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Abstract
Description
본 발명은 도토리의 유효성분을 추출,분리하여 이 유효성분의 함유한 천연항산화제 및 건강기능식품을 개발하는 것이다.The present invention is to extract natural acorn extracts and isolate them to develop natural antioxidants and health functional foods containing the active ingredients.
식용유지나 지방질식품의 가공 또는 저장 중에 있어서 품질을 저하시키는 원인중의 하나는 지질의 산화이며, 특히 불포화지방산을 많이 함유하는 식품은 쉽게 산화되어 과산화 지질을 형성하고 더욱 산화,분해,중합되어 불쾌한 냄새를 나타내거나 독성물질을 생성한다. 이같은 자동산화는 열,자외선,산소,금속이온에 의하여 촉진 되므로 산소,자외선 차단,항산화제 및 chelate지를 첨가하여 자동산화를 억제하고 있다.유지의 항산화제는 항산화력이 강한 합성 B.H.A , B.H.T , N.D.G.A등이 있지만 합성이므로 소비자로부터 기피되고 있으므로 천연항산화제의 연구개발이 필요한 현실이다.One of the causes of deterioration in quality during processing or storage of edible oil or fat foods is the oxidation of lipids, especially foods containing a large amount of unsaturated fatty acids, which are easily oxidized to form lipid peroxides, further oxidized, decomposed and polymerized to produce unpleasant odors Or produce toxic substances. These autoxidations are promoted by heat, ultraviolet rays, oxygen, and metal ions, thus inhibiting autoxidation by adding oxygen, ultraviolet light blocking, antioxidants, and chelate. Synthetic BHA, BHT, NDGA However, since it is synthetic, it is avoided from consumers, so research and development of natural antioxidants are necessary.
본 발명은 도토리에서 새로운 유효성분을 규명하고 이를 산업적으로 활용할 수 있는 방법을 제안 하고자 한다.The present invention discloses a new effective ingredient in acorns and proposes a method for industrial application thereof.
본발명은 국내에서 쉽게 채취할 수 있는 도토리에 유기용매를 처리하여 얻어진 추출물중 유효성분을 분리,동정하고 항산화 효과를 규명하여 산업적으로 응용하고자 한다. 또한 본 발명의 목적은 도토리 추출물의 유효성분을 유지산패 방지 첨가물이나 노화방지등을 하는 항산화제인 건강기능식품을 제공 하고자 한다.INDUSTRIAL APPLICABILITY The present invention aims to isolate and identify active ingredients among extracts obtained by treating organic acorns, which can be easily collected in Korea, and to identify the antioxidative effects and apply them industrially. It is also an object of the present invention to provide a health functional food, which is an antioxidant for preventing or treating rancidity, an antioxidant, or an anti-aging agent.
도토리추출물을 ethanol에 용해하여 조제용 TLC plate에 점적하고 chloroform:ethyl formate:formic acid(50:40:10)용매로 전개시켜 건조 후 UV lamp를 조사하였을 때 얻어진 chromatogram으로 확인할 수 있었다. The acorn extract was dissolved in ethanol and applied to TLC plate for preparation. The solution was developed with chloroform: ethyl formate: formic acid (50:40:10) solvent, dried and UV lamp was irradiated.
도토리추출물 중에는 gallic acid,digallic acid 및 gallotannin등과 Rf 0.35,0.66 및 0.81의 위치에 알 수 없는 성분이 함유되어 있어으며 gallic acid가 주종을 이루고 있었다.Among the acorn extracts, gallic acid, digallic acid, and gallotannin were found to contain unknown components at Rf 0.35, 0.66, and 0.81, and gallic acid was the main species.
TLC상의 Rf 0.51획분을 methol에 용해한 분획물은 HPLC의 Rt 2.98로 표준 gallic acid와 같았으며로 HPLC에 의해서도 도토리추출물 중에는 주로 gallic acid가 함유되어 있음을 확인하였다.The fractions obtained by dissolving Rf 0.51 fraction of TLC on methol were the same as those of standard gallic acid at Rt 2.98 of HPLC. It was confirmed by HPLC that acorn extract mainly contained gallic acid.
본 발명은 도토리추출물에 대한 새로운 생리적 효과를 규명하고 이를 산업적으로 활용할 방법을 제시하고자 한다.도토리추출물 유효성분이 항산력이 인증되는바 이 추출물을 분리 동정,정제하여 식용유지류나 지방질식품 가공류에 첨가하여 식품의 안전성을 유지 해 주는 활용방안과 건강기능식품의 소재로 이용된다면 산업적으로 부가가치를 창출할 수 있다.
The present invention discloses a new physiological effect of acorn extract and proposes a method of industrially utilizing it. Acorn extract has an antioxidant activity. The extract is isolated, identified, purified and added to edible oils and fat foods processing Therefore, it is possible to create added value by industrial use if it is used as a material for utilization of health functional food and a utilization method for maintaining the safety of food.
도 1은 도토리의 유효성분 추출과정이다.
도 2는 돈지유탁액에서 도토리추출물을 0.01% 및 0.02%의 농도가 되도록 첨가하여 60℃에서 저장하면서 POV를 측정한 결과이다.
도 3,4는 식용유지 유탁액에 0.02% 농도가 되도록 도토리추출물을 첨가하고 60℃에서 저장하면서 POV를 측정한 결과이다.
도 5는 마지막단계의 도토리추출물을 ethanol에 용해하고 조제용 TLC plate에 점적하여 전개시켜 얻어진 chromatogram이다.
도 6은 TLC상의 Rf 0.51획분을 methol에 용해한 것의 HPLC chromatogram이다.
도 7은 Rf 0.51인 gallic acid와 Rf 0.28인 digallic acid를 분취하여 일정농도로 돈지에 첨가하여 유탁액으로 한 다음 60℃에서 저장하면서 항산력을 측정한 결과이다.
도 8은 돈지유탁액에 gallic acid를 농도별로 첨가하여 저장에 따른 POV를 측정한 결과이다. 1 is a process for extracting an active ingredient of acorn.
FIG. 2 shows the result of measuring the POV while adding acorn extract to the concentration of 0.01% and 0.02% in lard emulsion and storing at 60 ° C.
3 and 4 show the result of POV measurement while adding acorn extract to 0.02% concentration of edible oil-in-water emulsion and storing at 60 ° C.
FIG. 5 is a chromatogram obtained by dissolving acorn extract at the last stage in ethanol and developing it by sprinkling on a preparative TLC plate.
Figure 6 is an HPLC chromatogram of the Rf 0.51 fraction on TLC dissolved in methol.
FIG. 7 shows the results of measuring the antioxidant activity by collecting gallic acid having an Rf of 0.51 and digallic acid having an Rf of 0.28 and adding it to lard at a certain concentration to prepare an emulsion and then storing it at 60 ° C.
FIG. 8 shows the result of measuring the POV according to storage by adding gallic acid to the lard emulsion.
1.항산화성분의 추출1. Extraction of antioxidants
분쇄한 도토리에 4배량의 acetone-water(1:1)를 가하여 실온에서 7시간 추출하고 잔사를 3∼4회 반복 추출하고, 전액을 여과한 후 40℃에서 감압농축하였다. 농축액에 2배량의 ethyl acetate 를 첨가하여 진탕하고 항산화성분을 ethyl acetate 층으로 이행시켰다. 이조작을 3회 반복하고 40℃에서 감압농축하여 분말상의 도토리추출물을 얻었다.Four times the amount of acetone-water (1: 1) was added to the crushed acorns, and the mixture was extracted at room temperature for 7 hours. The residue was extracted three to four times, and the whole was filtered and concentrated under reduced pressure at 40 ° C. Two times as much ethyl acetate was added to the concentrate to shake and the antioxidant component was transferred to the ethyl acetate layer. This experiment was repeated three times and concentrated under reduced pressure at 40 DEG C to obtain a powdered acorn extract.
2.항산화성분의 분리 및 확인2. Isolation and identification of antioxidant components
TLC에 의한 항산화성분의 분리는 도 1의 방법으로 조제한 도토리추출물을 ethanol에 용해하여 조제용 TLC plate에 점적하고 chloroform:ethyl formate:formic acid(50:40:10)용매로 전개시켜 건조 후 UV lamp를 조사하여 발색 band를 확인하였으며 각각의 band를 분취하여 ethanol에 용해하여 galls filter로 여과하여 돈지에 대한 항산화력을 측정하였다.In order to separate the antioxidant components by TLC, the acorn extract prepared by the method of FIG. 1 was dissolved in ethanol, applied to a preparation TLC plate, developed with a solvent of chloroform: ethyl formate: formic acid (50:40:10) . Each band was aliquoted, dissolved in ethanol and filtered with a galls filter to measure the antioxidative potential against lard.
HPLC에 의한 항산화성분의 확인은 도 1의 방법에서 조제한 도토리추출물을 methnol에 녹여 HPLC의 분석시료로 하였으며 표준품인 tannin,gallic acid와 비교하여 항산화성분을 확인 동정하였으며, HPLC 분석조건은 표 1과 같다.To confirm the antioxidant component by HPLC, the acorn extract prepared in the method of FIG. 1 was dissolved in methnol to prepare an analytical sample of HPLC. The antioxidant component was identified by comparing with the standard tannin and gallic acid, and the HPLC analysis conditions were as shown in Table 1 .
3.도토리추출물의 농도따른 항산화 효과3. Antioxidant effect of acorn extract concentration
돈지유탁액에서 도토리추출물을 0.01% 및 0.02%의 농도가 되도록 첨가하여 60℃에서 저장하면서 POV를 측정한결과 도 2와 같았다. 도토리추출물을 0.01%농도로 첨가하여 4일,8일 저장하였을 때의 POV는 12meq/kg, 60meq/kg, 0.02%농도로 첨가하였을 때의 POV는 8meq/kg, 30meq/kg으로 첨가농도가 증가함에 따라 항산화력이 높았으며 도토리추출물 0.02% 첨가구는 실용적인 농도로 인정되었다.From the lard dispenser, the acorn extract was added so as to have a concentration of 0.01% and 0.02%, and the POV was measured while being stored at 60 ° C. The result was as shown in FIG. The POV of 8 meq / kg, 30 meq / kg POV when added with 12 meq / kg, 60 meq / kg and 0.02% concentration of POV when stored at 4 days and 8 days with 0.01% , And the addition of 0.02% acorn extract was found to be a practical concentration.
4.식용유지에 대한 항산화 효과4. Antioxidant effect on edible oil
식용유지 유탁액에 0.02% 농도가 되도록 도토리추출물을 첨가하고 60℃에서 저장하면서 POV를 측정한 결과는 도 3,4와 같았다. 무첨가구에서 60℃,8일간 저장하였을 때, 돈지유탁액의 POV는 112meq/kg,우지유탁액 12meq/kg, 대두유탁액 14meq/kg 으로 산화속도는 돈지〉대두유〉우지유탁액의 순으로 나타났으며, BHA 0.01%첨가구에서는 돈지유탁액의 POV는 18meq/kg, 우지유탁액은 3meq/kg, 대두유유탁액은 2meq/kg으로 BHA는 돈지 대하여서는 항산화 효과가 낮았으나, 우지와 대두유유탁액에서는 14일 경과 후에도 POV의 변화가 적어 항산화 효과가 강하였다.The acorn extract was added to the edible oil-in-water emulsion at a concentration of 0.02%, and the POV was measured at 60 ° C while storing it. When stored at 60 ° C for 8 days, the POV of the lard emulsion was 112 meq / kg, the lard emulsion was 12 meq / kg, the soybean emulsion was 14 meq / kg, and the oxidation rate was in the order of lard> soybean oil> In the case of BHA 0.01%, the antioxidative effect of lard was lowered by 18 meq / kg of POV, 3 meq / kg of Wuji emulsion and 2 meq / kg of soybean oil emulsion. The antioxidative effect was strong because of little change in POV after 14 days.
도토리추출물 0.02%첨가구에서는 60에서 8일간 저장하였을 때,돈지유탁액의 POV는 31meq/kg,우지유탁액 7meq/kg, 대두유유탁액은 6meq/kg으로 항산화 효과가 높았다.When the acorn extract was stored at 60 ℃ for 8 days, the POV of the lard emulsion was increased to 31 meq / kg, the Wuji emulsion was 7 meq / kg, and the soybean oil emulsion was 6 meq / kg.
5.도토리추출물중에 gallic acid 함량 및 항산화 효과5. Gallic acid content and antioxidative effect in acorn extract
도토리추출물중의 gallic acid의 함량을 측정한 결과는 표 2와 같았다. gallic acid의 함량은 작은 품종의 것이 큰품종보다 높았으며 정제과정을 더해감에 따라 함량비가 증가하였다.The content of gallic acid in the acorn extract was measured as shown in Table 2. The content of gallic acid was higher in small varieties than in large varieties.
마지막단계의 도토리추출물을 ethanol에 용해하고 조제용 TLC plate에 점적하여 전개시켰을 때, chloroform:ethyl formate:formic acid(50:40:10)용매로 전개시켜 건조 후 UV lamp를 조사하였을 때 얻어진 chromatogram은 도 5과 같았다.TLC상의 Rf 0.51획분을 methol에 용해한 것의 HPLC chromatogram은 도 6과 같았으며 TLC상의 Rf 0.51 분획물은 HPLC의 Rt 2.98로 표준 gallic acid와 같았다.The final chromatographic extracts were dissolved in ethanol and developed on a preparative TLC plate. The developed chromatograms were developed with chloroform: ethyl formate: formic acid (50:40:10) The HPLC chromatogram of the Rf 0.51 fraction on the TLC dissolved in methol was as shown in FIG. 6. The Rf 0.51 fraction on the TLC had a Rt of 2.98 as the standard gallic acid.
Rf 0.51인 gallic acid와 Rf 0.28인 digallic acid를 분취하여 일정농도로 돈지에 첨가하여 유탁액으로 한 다음 60℃에서 저장하면서 항산력을 측정한 결과 도 7와 같았다. digallic acid 분취물 첨가구는 저장 6일째에는 gallic acid 분취물 첨가구와 비슷한 항산화력을 보였으나 8일째에는 digallic acid 첨가구의 POV가 상당히 증가하였으나 gallic acid 분취물은 강한 항산력을 나타내고 있다.The results are shown in FIG. 7, wherein gallic acid having a Rf of 0.51 and digallic acid having a Rf of 0.28 were aliquoted and added to lard at a constant concentration to prepare an emulsion. On the 6th day after storage, the antioxidative capacity of digallic acid was similar to that of gallic acid. On the 8th day, the POV of digallic acid was significantly increased, but the gallic acid fraction showed strong antioxidant capacity.
도 8은 돈지유탁액에 gallic acid를 농도별로 첨가하여 저장에 따른 POV를 측정한 것으로서 POV가 60meq/kg에 달하는데 요하는 시간은 무첨가구가 5일,gallic acid 0.005% 첨가구는 8일정도 소요되었으므며 8일경과했을 때 gallic acid 0.01%첨가구의 POV는 31meq/kg, 0.015%첨가구는 28meq/kg으로서 낮은 농도에서도 BHA와 비슷한 항산력을 나타내었다.FIG. 8 shows the POV measured by the addition of gallic acid to the lard emulsion. The time required for the POV to reach 60 meq / kg was 5 days for the non-additive group and 8 days for the additive group containing 0.005% of gallic acid After 8 days, the POV of gallic acid 0.01% was 31 meq / kg and the addition of 0.015% had 28 meq / kg.
POV,meq/kgPOV, meq / kg
Claims (3)
A composition comprising the antioxidant of claim 2 as an antioxidant and an inhibitor of aging by lipid oxidation of a food comprising an active ingredient.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200074469A (en) * | 2018-12-17 | 2020-06-25 | 대한민국(산림청 국립산림과학원장) | Antioxidant composition comprising acorn extract and use of the same |
| KR20200139893A (en) * | 2019-06-05 | 2020-12-15 | 대한민국(산림청 국립산림과학원장) | Antioxidnat and antibacterial composition comprising Quercus acuta Thunb acorn extract |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200074469A (en) * | 2018-12-17 | 2020-06-25 | 대한민국(산림청 국립산림과학원장) | Antioxidant composition comprising acorn extract and use of the same |
| KR20200139893A (en) * | 2019-06-05 | 2020-12-15 | 대한민국(산림청 국립산림과학원장) | Antioxidnat and antibacterial composition comprising Quercus acuta Thunb acorn extract |
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