KR100543809B1 - High quality grape granule tea containing antioxidative anthocyanins and catechins and method for preparation thereof - Google Patents
High quality grape granule tea containing antioxidative anthocyanins and catechins and method for preparation thereof Download PDFInfo
- Publication number
- KR100543809B1 KR100543809B1 KR1020040013512A KR20040013512A KR100543809B1 KR 100543809 B1 KR100543809 B1 KR 100543809B1 KR 1020040013512 A KR1020040013512 A KR 1020040013512A KR 20040013512 A KR20040013512 A KR 20040013512A KR 100543809 B1 KR100543809 B1 KR 100543809B1
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- South Korea
- Prior art keywords
- grape
- extract
- catechin
- grape seed
- juice
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- 150000008163 sugars Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 108010038851 tannase Proteins 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 229960000984 tocofersolan Drugs 0.000 description 1
- 235000010384 tocopherol Nutrition 0.000 description 1
- 229930003799 tocopherol Natural products 0.000 description 1
- 239000011732 tocopherol Substances 0.000 description 1
- 229960001295 tocopherol Drugs 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
- 235000014101 wine Nutrition 0.000 description 1
- 239000002076 α-tocopherol Substances 0.000 description 1
- 235000004835 α-tocopherol Nutrition 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61H—PHYSICAL THERAPY APPARATUS, e.g. DEVICES FOR LOCATING OR STIMULATING REFLEX POINTS IN THE BODY; ARTIFICIAL RESPIRATION; MASSAGE; BATHING DEVICES FOR SPECIAL THERAPEUTIC OR HYGIENIC PURPOSES OR SPECIFIC PARTS OF THE BODY
- A61H33/00—Bathing devices for special therapeutic or hygienic purposes
- A61H33/60—Components specifically designed for the therapeutic baths of groups A61H33/00
- A61H33/6005—Special constructive structural details of the bathtub, e.g. of the walls or supporting structure
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61H—PHYSICAL THERAPY APPARATUS, e.g. DEVICES FOR LOCATING OR STIMULATING REFLEX POINTS IN THE BODY; ARTIFICIAL RESPIRATION; MASSAGE; BATHING DEVICES FOR SPECIAL THERAPEUTIC OR HYGIENIC PURPOSES OR SPECIFIC PARTS OF THE BODY
- A61H33/00—Bathing devices for special therapeutic or hygienic purposes
- A61H33/06—Artificial hot-air or cold-air baths; Steam or gas baths or douches, e.g. sauna or Finnish baths
- A61H2033/068—Steam baths
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61H—PHYSICAL THERAPY APPARATUS, e.g. DEVICES FOR LOCATING OR STIMULATING REFLEX POINTS IN THE BODY; ARTIFICIAL RESPIRATION; MASSAGE; BATHING DEVICES FOR SPECIAL THERAPEUTIC OR HYGIENIC PURPOSES OR SPECIFIC PARTS OF THE BODY
- A61H2201/00—Characteristics of apparatus not provided for in the preceding codes
- A61H2201/02—Characteristics of apparatus not provided for in the preceding codes heated or cooled
- A61H2201/0207—Characteristics of apparatus not provided for in the preceding codes heated or cooled heated
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61H—PHYSICAL THERAPY APPARATUS, e.g. DEVICES FOR LOCATING OR STIMULATING REFLEX POINTS IN THE BODY; ARTIFICIAL RESPIRATION; MASSAGE; BATHING DEVICES FOR SPECIAL THERAPEUTIC OR HYGIENIC PURPOSES OR SPECIFIC PARTS OF THE BODY
- A61H2201/00—Characteristics of apparatus not provided for in the preceding codes
- A61H2201/10—Characteristics of apparatus not provided for in the preceding codes with further special therapeutic means, e.g. electrotherapy, magneto therapy or radiation therapy, chromo therapy, infrared or ultraviolet therapy
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- Health & Medical Sciences (AREA)
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
본 발명은 항산화성 안토시아닌 색소 및 카테킨을 함유한 고품질의 포도 과립차 및 그것의 제조방법에 관한 것으로, 볶은 포도씨를 헥산으로 탈지하여 얻은 잔사를 효소 처리한 후 에탄올로 열탕 추출하고 여과 및 농축하여 얻어진 포도씨추출물 엑기스와 포도 과실을 파쇄, 가온, 착즙, 여과 및 살균한 후 냉장처리한 다음 다시 여과 및 농축하여 얻은 포도 과즙 엑기스를 주성분으로 포함하는 포도 과립차를 제공하는 뛰어난 효과가 있다. 또한, 본 발명 포도 과즙 엑기스와 포도씨 엑기스는 각각 항산화성 카테킨 성분 및 안토시아닌 색소를 다량 함유하고 있어 암, 심장병, 고혈압 및 노화 등을 예방하는 기능성식품의 유효성분으로 사용될 수 있다.The present invention relates to a high-quality grape granular tea containing antioxidant anthocyanin pigment and catechin and a method for producing the same, wherein the residue obtained by degreasing roasted grape seeds with hexane is subjected to enzymatic treatment, followed by hot water extraction with ethanol, filtration and concentration. There is an excellent effect of providing a grape granules tea containing grape juice extract obtained by crushing, warming, juice, filtration and sterilization of the extract extract and grape fruit, and then filtered and concentrated again. In addition, the grape juice extract and grape seed extract of the present invention each contain a large amount of antioxidant catechin component and anthocyanin pigment can be used as an active ingredient of a functional food to prevent cancer, heart disease, high blood pressure and aging.
포도 과즙 엑기스, 포도씨 엑기스, 안토시아닌 색소, 카테킨, 포도 과립차Grape juice extract, grape seed extract, anthocyanin pigment, catechin, grape granule tea
Description
본 발명은 항산화성 안토시아닌 색소 및 카테킨을 함유한 고품질의 포도 과립차 및 그것의 제조방법에 관한 것이다. 보다 상세하게는, 본 발명은 생체 포도를 파쇄, 가온, 착즙, 여과, 살균 및 저온 숙성하여 여과한 후 농축하여 제조된 포도 과즙 엑기스와 건조 포도씨를 볶은 후 노르말-헥산으로 탈지하여 얻어진 유박을 효소처리한 후 에탄올을 가하여 가열 추출한 다음 여과 및 농축하여 만든 포도씨 엑기스를 혼합하여 만든 암, 고혈압, 심장병 및 노화의 예방 및 치료에 유용한 포도 과립차에 관한 것이다.The present invention relates to a high quality grape granule tea containing the antioxidant anthocyanin pigment and catechin and a method for producing the same. More specifically, the present invention is a grape juice extract prepared by crushing, warming, juice, filtration, sterilization and low temperature aging and then concentrated grape juice extract and roasted dried grape seeds after enzyme degreased the oil squeezed with normal-hexane The present invention relates to a grape granule tea useful for the prevention and treatment of cancer, hypertension, heart disease and aging made by mixing grape seed extract made by heating, extraction, filtration and concentration.
최근 급격한 산업사회의 발전에 따른 환경오염의 가속화와 더불어 식생활 패턴의 서구화로의 변모로 육류 소비가 크게 증가하면서 암을 비롯한 심장병, 고혈압, 동맥경화증, 당뇨병 및 치매 등 여러 만성적인 퇴행성질환이 크게 증가하고 있다. 따라서 현재 이러한 만성적인 질환을 예방 및 치료할 수 있는 천연물 유래의 새로운 생리활성물질을 개발하려는 연구가 활발히 진행되고 있으며, 특히 생체의 방어기구를 향상시켜 질병을 방지 및 회복시키거나, 면역기능 향상 및 노화 억제 등의 생체조절기능을 갖고 있는 천연 항산화물질에 대한 관심이 크게 고조되고 있다(Larson, A.L., Phytochemistry 27: 969-978, 1988; Richard Sies H., Oxidative Stress, Oxidants, and Antioxidants, Academic Press, New York, 1991).Recently, due to the rapid development of industrial society and the rapid change of eating patterns, the consumption of meat has increased due to the transformation of dietary patterns into Westernization, and many chronic degenerative diseases such as cancer, heart disease, hypertension, arteriosclerosis, diabetes and dementia have greatly increased. Doing. Therefore, researches are currently being actively conducted to develop new bioactive substances derived from natural products that can prevent and treat such chronic diseases. In particular, the defense mechanisms of the living body are improved to prevent and recover diseases, or to improve immune function and age. There is a great interest in natural antioxidants that have bioregulatory functions such as inhibition (Larson, AL, Phytochemistry 27: 969-978, 1988; Richard Sies H., Oxidative Stress, Oxidants, and Antioxidants, Academic Press, New York, 1991).
항산화물질은 불포화지방산의 자동산화과정에서 생성되는 활성카르보닐화합물 유래의 라디컬종(ROO·, RO·및 ROOH)을 포착 및 제거하여 지방을 함유한 식품의 산패를 억제해 줄 뿐 아니라 생체내에서 생성되는 활성산소 라디컬(1O2, O- 2, H2O2,·OH)에 의한 지질과산화반응을 억제하여 암, 심장병, 동맥경화증, 염증, 면역저하 및 노화를 예방해주는 생리활성물질로써 크게 각광을 받고 있다(Halliwell and Gutteridge, Lipid peroxidation. In: Free Radicala in Biology and Medicine. 2nd ed., Clarendon Press, Oxford, 1988; Emerit and Lippman, Free radicals and lipid peroxidation in cell pathology, pp. 177-18, Vol. 1, CRC Press, Boca Raton, USA, 1990). 현재 부틸화된 하이드록시아니솔(butylated hydroxyanisole(BHA)), 부틸화된 하이드록시톨루엔(butylated hydroxytoluene(BHT)) 및 프로필 갈레이트(propyl gallate (PG))와 같은 합성 항산화제와 α-토코페롤(tocopherol) 및 L-아스코르브산과 같은 천연항산화제가 식품, 화장품 및 의약품 산업에 널리 사용되고 있으나 합성 항산화제가 지니고 있는 독성 및 발암성 등의 안전성이 크게 문제시 되고 또한 천연 항산화제는 합성 항산화제 보다 항산화력이 낮을 뿐만 아니라 고가이므로 보다 안전하고 효과있는 천연 항산 화제의 개발이 요구되고 있다(Johnson, F.C.A. CRC Crit. Rev. Food Technol. 10: 267-273, 1971; Branen, A.L. J. Am. Oil Chem. Soc. 52: 59-65, 1975; Ito, N., Fukushima, S. and Fukushima, H., CRC Crit. Rev. Food Technol. 15: 109-114, 1985). Antioxidants capture and remove radical species (ROO, RO, and ROOH) derived from active carbonyl compounds produced during the automatic oxidation of unsaturated fatty acids, while suppressing the rancidity of fat-containing foods. Bioactive substance that prevents cancer, heart disease, arteriosclerosis, inflammation, immunosuppression and aging by inhibiting lipid peroxidation reaction by the produced free radical radicals ( 1 O 2 , O - 2 , H 2 O 2 , .OH) (Halliwell and Gutteridge, Lipid peroxidation.In: Free Radicala in Biology and Medicine.2nd ed., Clarendon Press, Oxford, 1988; Emerit and Lippman, Free radicals and lipid peroxidation in cell pathology, pp. 177 -18, Vol. 1, CRC Press, Boca Raton, USA, 1990). Currently, synthetic antioxidants such as butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT) and propyl gallate (PG) and α-tocopherol ( Although natural antioxidants such as tocopherol) and L-ascorbic acid are widely used in the food, cosmetics and pharmaceutical industries, the safety of toxicity and carcinogenic properties of synthetic antioxidants are greatly raised, and natural antioxidants are more effective than synthetic antioxidants. Not only is it low but also expensive, there is a need to develop safer and more effective natural antioxidants (Johnson, FCA CRC Crit. Rev. Food Technol . 10: 267-273, 1971; Branen, AL J. Am. Oil Chem. Soc 52: 59-65, 1975; Ito, N., Fukushima, S. and Fukushima, H., CRC Crit. Rev. Food Technol . 15: 109-114, 1985).
포도 (Vitis vinifera)는 갈대나무목 (Rhamnales) 포도과 (Vitaceae)에 속하는 낙엽성 덩굴식물로서 세계적으로 11속 약 700 여종이 분포되어 있으며, 주로 열대 및 아열대 지역에 자생하며 일부는 온대지방에까지 분포되어 있다. 포도는 1998년 현재 세계에서 거의 남한 크기인 약 7백 4십만 ha에서 5천8백만톤 가량이 생산되어 온대 과실 중에서는 가장 많이 재배되고 있는 과실의 하나이다. 한편, 1998년도 현재 국내의 포도 생산량은 397,800 MT으로서 감귤, 사과 다음으로 생산량이 많은 과실이며, 주로 미국종 (Vitis labrusca L.)인 캠벨얼리(Cambell Early) 품종이 대부분을 차지하고 있으며, 그 다음으로 거봉 및 새단 (Sheridan)과 그 외 이들 상호간의 교잡종 (Vitis labruscana B.)이 재배되고 있으며, 경북의 영천, 경산, 김천 및 상주와 충북의 영동 지역이 포도 생산량의 대부분을 차지하고 있다.Grape ( Vitis vinifera ) is a deciduous vine plant belonging to the Rhamnales family, Vitaceae , with about 700 genera distributed in 11 genera around the world, mainly native to tropical and subtropical regions, and partly to temperate regions. . Grapes are one of the most cultivated fruits of temperate fruit, producing about 58 million tons in about 4.8 million ha, the size of almost South Korea in 1998. On the other hand, as of 1998, the domestic grape production was 397,800 MT, the second largest fruit after citrus fruits and apples, mainly from the Campbell Early varieties, Vitis labrusca L., followed by Geobong. And Sheridan and other hybrids ( Vitis labruscana B.) are cultivated, and Yeongcheon, Gyeongsan, Gimcheon, and Sangju and Yeongdong of Chungbuk dominate the grape production.
포도는 당, 유기산 및 독특한 향기를 함유하고 있을 뿐만 아니라 페놀산, 플라보노이드(플라보놀(flavonols), 플라반-3-올스(flavan-3-ols) 및 플라바노놀스(flavanonols)), 레즈베라트롤(resveratrol) 및 안토시아닌 색소 등의 항암, 항고혈압, 항염증 및 항산화성 폴리페놀화합물을 다량 함유하고 있어 최근 포도 주스, 음료 및 포도주 등의 여러 가공식품의 소비가 크게 증가하고 있다 (Renauds, S. and Lorgeril, M. Lancet 339: 1523-1526, 1992; Kanner, J., Frankel, E., Granit, R., German, B. and Kinsella, J.E. J. Agric Food Chem. 42: 64-69, 1994; Frankel, E.N., J. Agric Food Chem. 43: 890-894, 1995; Tanahashi, H., Suwa, Y., Toyoda, Y. and Itakura, H., Am. J. Enol. Vitic. 46: 405-409, 1995). 특히 포도 과피에 다량 함유되어 있는 안토시아닌 색소는 생체내 활성산소에 의해 유도되는 세포막의 지질과산화반응을 효과적으로 억제할 수 있는 천연 항산화제로써 뿐만 아니라 지질단백질(LDL) 산화를 억제하는 항고혈압성 생리활성물질로써 현재 식품 착색료로써 뿐만 아니라 식이성 기능성식품 신소재로써 널리 사용되고 있다(Tsuda, T., Watanabe, M., Ohshima, K., Norinobu, S., Choi, S.W., Kawakishi, S. and Osawa, T. J. Agric. Food Chem. 42: 2407-2410, 1994; Tamura, H. and Yamagami, A. J. Agric Food Chem. 42: 1612-1615, 1994; Tsuda, T., Horio, F. and Osawa, T. Lipids 33: 583-588, 1998; Tsuda, T., Horio, F., Kitoh, J. and Osawa, T. Arch. Biochem. Biophys. 368: 361-366, 1999).Grapes not only contain sugars, organic acids and unique scents, but also phenolic acids, flavonoids (flavonols, flavan-3-ols and flavanonols), resveratrol (resveratrol) and anthocyanin pigments, such as anti-cancer, antihypertensive, anti-inflammatory and antioxidant polyphenol compounds in large amounts have recently increased the consumption of various processed foods, such as grape juice, beverages and wine (Renauds, S. and Lorgeril, M. Lancet 339: 1523-1526, 1992; Kanner, J., Frankel, E., Granit, R., German, B. and Kinsella, JE J. Agric Food Chem. 42: 64-69, 1994 Frankel, EN, J. Agric Food Chem. 43: 890-894, 1995; Tanahashi, H., Suwa, Y., Toyoda, Y. and Itakura, H., Am. J. Enol. Vitic. 46: 405 -409, 1995). In particular, anthocyanin pigments contained in grape skins are not only natural antioxidants that can effectively inhibit the lipid peroxidation of cell membranes induced by free radicals in vivo, but also antihypertensive biological activities that inhibit lipoprotein (LDL) oxidation. As a substance, it is widely used not only as a food coloring material but also as a dietary functional food new material (Tsuda, T., Watanabe, M., Ohshima, K., Norinobu, S., Choi, SW, Kawakishi, S. and Osawa, T) J. Agric.Food Chem . 42: 2407-2410, 1994; Tamura, H. and Yamagami, A. J. Agric Food Chem . 42: 1612-1615, 1994; Tsuda, T., Horio, F. and Osawa T. Lipids 33: 583-588, 1998; Tsuda, T., Horio, F., Kitoh, J. and Osawa, T. Arch. Biochem. Biophys . 368: 361-366, 1999).
한편, 포도씨는 포도 중량의 약 3-5%를 차지하며 지방(9-12%), 단백질(8-12%) 및 헤미셀룰로오스(hemicellulose)와 같은 식이성섬유소(약 45%)를 다량 함유하고 있을 뿐만 아니라 Ca, Mg 및 P과 같은 무기질의 함량이 높다(Kinsella, J.E., Food Technol. 28: 58-60, 1974; Fantozzi P., J. Am. Oil Chem. Soc. 58: 1027-1031, 1981; Fedeli E., J. Am. Oil Chem. Soc. 60(2): 404-406, 1983; Kamel, B.S., Dawson, H. and Kakuda, Y., J. Am. Oil Chem. Soc. 62: 881-883, 1985; Rao, P.U., Food Chem. 50: 379-382, 1994; Igartuburu, J.M., J. Nat. Prod. 61: 876-880, 1998). 또한, 포도씨는 포도과육과 달리 식물성스테롤, 토코페놀 뿐만 아 니라 카테킨(catechins) 및 프로시아니딘(procyanidins)과 같은 플라반-3-올스(flavan-3-ols) 화합물을 다량 함유하고 있어 기능성 식품, 화장품 및 의약품의 신소재로써 널리 사용되고 있다(Kinsella, J.E., Food Technol. 28: 58-60, 1974; Kinsella, J.E., Cosme. Toiletries 91: 19-24, 1976; Ricardo da Silva, J.M., Rigaud, J., Cheynier, V., Cheminat, A. and Moutounet, M., Phytochemistry 30: 1259-1264, 1991).Grape seeds, on the other hand, account for about 3-5% of the weight of grapes and contain large amounts of dietary fiber (about 45%) such as fat (9-12%), protein (8-12%) and hemicellulose. In addition, the content of minerals such as Ca, Mg and P is high (Kinsella, JE, Food Technol. 28: 58-60, 1974; Fantozzi P., J. Am. Oil Chem. Soc. 58: 1027-1031, 1981 Fedeli E., J. Am. Oil Chem. Soc. 60 (2): 404-406, 1983; Kamel, BS, Dawson, H. and Kakuda, Y., J. Am. Oil Chem. Soc. 62: 881-883, 1985; Rao, PU, Food Chem. 50: 379-382, 1994; Igartuburu, JM, J. Nat. Prod. 61: 876-880, 1998). In addition, grape seed, unlike grape flesh, contains not only vegetable sterols and tocophenols, but also flavan-3-ols compounds such as catechins and procyanidins, which are functional foods and cosmetics. And new materials for pharmaceuticals (Kinsella, JE, Food Technol. 28: 58-60, 1974; Kinsella, JE, Cosme. Toiletries 91: 19-24, 1976; Ricardo da Silva, JM, Rigaud, J., Cheynier, V., Cheminat, A. and Moutounet, M., Phytochemistry 30: 1259-1264, 1991).
한편, 포도씨추출물에는 5-20%의 카테킨화합물(프로안토시아니딘(proanthocyanidin), 소량체 및 다량체 폴리하이드록시플라반-3-올 유닛(oligo- meric and polymeric polyhydroxyflavan-3-ol units))를 함유하고 있으며, 그 중 일부 단량체 카테킨 (monomeric catechin: (+)-catechin 및 (-)-epicatechin) 성분과 이량체 (dimer), 삼량체 (trimer) 및 사량체 (tetramer) 등의 소량체 프로시아니딘(oligomeric procyanidin) 및 몰식자산 (gallic acid)이 에스테르화된 프로시아니딘 성분으로 대부분 구성되어 있다. 그리고 소량체 프로시아니딘 성분 중 55% 이상은 아직까지 확인되지 않은 다량체 프로시아니딘(polymeric procyanidins: 5개 이상의 단량체 유닛(more than five monomer units), 중합화도(polymerization degree): 2.3-15.1 또는 2.4-16.7) 성분으로 구성되어 있으며, 그 이외에도 미량의 가수분해형 탄닌성분들이 함유되어 있다(Ricardo da Silva, J.M., Rigaud, J., Cheynier, V., Cheminat, A. and Moutounet, M., Phytochemistry 30: 1259-1264, 1991; Teresa, E.B. Yolanda, G.F., Julian, C.R. and Celestino, S.B., J. Agric. Food Chem. 40: 1794-1799, 1992; Fuleki, T. and Ricardo Da Silva, J.M., J. Agric. Food Chem. 45: 1156-1160, 1997). 포도씨에 함유되어 있는 이들 카테킨화합물은 항암(Gali, H.U., Perchellet, E.M., Gao, X.M., Karchesy, J.J. and Perchellet, J.P., Planta Med. 60: 235-239, 1994; Zhao, J., Carcinogenesis 20(9): 1737-1745, 1999; Shirataki, Y., Kawase, M., Saito, S., Kurihara, T., Tanaka, W., Satoh, K., Sakagami, H., Motohashi, N., Anticancer Res. 20: 423-426, 2000; Sen, C.K. and Bagchi, D., Mol. Cell Biochem. 215: 1-7, 2001), 항고혈압 (Tebib, K., J. Nutr. 124: 2451-2457, 1994; Yamakoshi, J., Kataoka, S., Koga, T., Ariga, T., Atherosclerosis 142: 139-149, 1999; Fitzpatrick, D.F., Fleming, R.C., Bing, B., Maggi, D.A., O'Malley, R.M., J. Agric. Food Chem. 48: 6384-6390, 2000), 항균 (Palma, M., Taylor, L.T., Varela, R.M., Cutler, S.J., Cutler, H.G., J. Agric. Food Chem. 47: 5044-5048, 1999;), 항산화작용 (Ricardo, J.M., Darmon, N., Fernandez, Y. and Mitjavila, S., J. Agric. Food Chem. 39: 1549-1552, 1991; Bagchi, D., Garg, A., Krohn, R.L., Bagchi, M., Bagchi, D.J., Balmoori, J., Stohs, S.J., Gen. Pharmacol. 30(5): 771-776, 1998; Koga, T., Moro, K., Nakamori, K., Yamakoshi, J., Hosoyama, H., Kataoka, S. and Ariga, T. J. Agric. Food Chem. 47: 1892-1897, 1999; Yamaguchi, F., Yoshimura, Y., Nakazawa, H., Ariga, T., J. Agric. Food Chem. 47: 2544-2548, 1999; Koga, T., Moro, K., Nakamori, K., Yamakoshi, J., Hosoyama, H., Kataoka, S., Ariga, T., J. Agric. Food Chem. 47: 1892-1897, 1999; Castillo, J., Benavente-garcia, O., Lorente, J., Alcaraz, M., Redondo, A., Ortuno, A., Del Rio, J.A., J. Agric. Food Chem. 48: 1738-1745, 2000; Jayaprakasha, G.K., Singh, R.P. and Sakariah, K.K., Food Chem. 73: 285-290, 2001) 뿐만 아니라 항위궤양 (Saito, M., Hosoyama, H., Ariga, T., Kataoka, S., Yamaji, N., J. Agric. Food Chem. 46: 1460-1464, 1998), 눈 망막 보호작용 (Yamakoshi, J., Saito, M., Kataoka, S. and Tokutake, S., J. Agric. Food Chem. 50: 4983-4988, 2002), 장의 유용미생물 발육 촉진 효과 (Tebib, K., Besancon, P. and Rouanet, J.M., Nutrition Res. 16(1): 105-110, 1996) 그리고 피부미백 (德武昌一, 山越 純, New Food Industry 43(11): 1-9, 2001; 山越 純, 德武昌一, Food Style 6(12): 41-44, 2002) 작용 등 여러 가지 중요한 생리적 작용을 지니고 있다. 이와 같이 안토시아닌 색소를 다량 함유하고 있는 포도 과즙과 카테킨 및 프로시아니딘과 같은 폴리페놀화합물을 다량 함유하고 있는 포도씨추출물은 암, 고혈압, 심장병 및 노화와 같은 여러 만성적인 질병을 예방할 수 있는 기능성 식품, 화장품 및 의약품의 신소재로써 각광을 받고 있다 (Laparra, J., Michaud, J. and Masquelier, J., Bull. Soc. Pharm Bordeaux 118: 7-13, 1979; 식품첨가물 공전, 식품의약품안전청, 문영사, 서울, pp 967-968, 2001).On the other hand, grape seed extract contains 5-20% of the catechin compound (proanthocyanidin, small and multimeric polyhydroxyflavan-3-ol units). And some monomers such as monomeric catechins ((+)-catechin and (-)-epicatechin) and dimers such as dimers, trimers, and tetramers. Oligomeric procyanidin and gallic acid are mostly composed of esterified procyanidin components. In addition, more than 55% of the components of the small monomer procyanidins have not yet been identified as polymeric procyanidins (more than five monomer units, polymerization degree: 2.3-15.1 or 2.4-16.7). And other trace amounts of hydrolyzable tannins (Ricardo da Silva, JM, Rigaud, J., Cheynier, V., Cheminat, A. and Moutounet, M., Phytochemistry 30: 1259 -1264, 1991; Teresa, EB Yolanda, GF, Julian, CR and Celestino, SB, J. Agric.Food Chem. 40: 1794-1799, 1992; Fuleki, T. and Ricardo Da Silva, JM, J. Agric. Food Chem. 45: 1156-1160, 1997). These catechin compounds contained in grape seeds are anticancer agents (Gali, HU, Perchellet, EM, Gao, XM, Karchesy, JJ and Perchellet, JP, Planta Med. 60: 235-239, 1994; Zhao, J., Carcinogenesis 20 ( 9): 1737-1745, 1999; Shirataki, Y., Kawase, M., Saito, S., Kurihara, T., Tanaka, W., Satoh, K., Sakagami, H., Motohashi, N., Anticancer Res. 20: 423-426, 2000; Sen, CK and Bagchi, D., Mol. Cell Biochem. 215: 1-7, 2001), antihypertensive (Tebib, K., J. Nutr. 124: 2451-2457 1994; Yamakoshi, J., Kataoka, S., Koga, T., Ariga, T., Atherosclerosis 142: 139-149, 1999; Fitzpatrick, DF, Fleming, RC, Bing, B., Maggi, DA, O 'Malley, RM, J. Agric.Food Chem. 48: 6384-6390, 2000), antibacterial (Palma, M., Taylor, LT, Varela, RM, Cutler, SJ, Cutler, HG, J. Agric.Food Chem 47: 5044-5048, 1999;), antioxidant (Ricardo, JM, Darmon, N., Fernandez, Y. and Mitjavila, S., J. Agric Food Chem 39:.. 1549-1552, 1991; Bagchi, D., Garg, A., Krohn, RL, Bagchi, M., Bagchi, DJ, Balmoori, J., Stohs, SJ, Gen. Pharmacol. 30 (5): 77 1-776, 1998; Koga, T., Moro, K., Nakamori, K., Yamakoshi, J., Hosoyama, H., Kataoka, S. and Ariga, T. J. Agric. Food Chem. 47: 1892-1897, 1999; Yamaguchi, F., Yoshimura, Y., Nakazawa, H., Ariga, T., J. Agric. Food Chem. 47: 2544-2548, 1999; Koga, T., Moro, K., Nakamori, K., Yamakoshi, J., Hosoyama, H., Kataoka, S., Ariga, T., J. Agric. Food Chem. 47: 1892-1897, 1999; Castillo, J., Benavente-garcia, O., Lorente, J., Alcaraz, M., Redondo, A., Ortuno, A., Del Rio, JA, J. Agric. Food Chem. 48: 1738-1745, 2000; Jayaprakasha, GK, Singh, RP and Sakariah, KK, Food Chem. 73: 285-290, 2001) as well as anti-gastric ulcers (Saito, M., Hosoyama, H., Ariga, T., Kataoka, S., Yamaji, N., J. Agric.Food Chem. 46: 1460-1464 , 1998), protecting the eye retina (Yamakoshi, J., Saito, M., Kataoka, S. and Tokutake, S., J. Agric. Food Chem. 50: 4983-4988, 2002), promoting the growth of useful microorganisms in the intestines Effects (Tebib, K., Besancon, P. and Rouanet, JM, Nutrition Res. 16 (1): 105-110, 1996) and skin whitening (德 武昌 一, 山 越 越, New Food Industry 43 (11): 1 -9, 2001; 山 越, 德 武昌 一, Food Style 6 (12): 41-44, 2002). Grape juice extract containing a large amount of anthocyanin pigment and grape seed extract containing a large amount of polyphenolic compounds such as catechin and procyanidin are functional foods, cosmetics and cosmetics that can prevent many chronic diseases such as cancer, high blood pressure, heart disease and aging. It is in the spotlight as a new material for medicine (Laparra, J., Michaud, J. and Masquelier, J., Bull. Soc. Pharm Bordeaux 118: 7-13, 1979; Food Additives Code, Korea Food and Drug Administration, Moonyoungsa, Seoul , pp 967-968, 2001).
지금까지 포도 과피의 안토시아닌 색소 및 포도씨의 카테킨화합물을 효과적으로 추출 및 분리할 수 있는 기술 개발과 더불어 그를 이용한 기능성 식품 및 화장품의 개발이 활발히 이루어져 왔다(磐田化學工業(주), 일본 공개특허공보 제2001-292731호, Whiprowpdir(주), 일본 공개특허공보 제2000-125823호, 해태제과(주), 한국공개특허공보 제2000-0037080호). Ricardo da Silva 등은 (Phytochemistry 30: 1259-1264, 1991; J. Agric. Food Chem. 45: 1156-1160, 1997) 폴리아미드 칼럼 크로마토그래피 (polyamide column chromatography)를 사용하여 포도씨의 메탄올추출물로부터 카테킨 및 프로시아니딘 성분을 순수 분리할 수 있는 방법을 보고한 바가 있으며, Kalhithraka 등 (Phytochemical Analysis 6: 265-267, 1995)은 포도씨 페놀화합물의 추출에 필요한 최적 용매 조건을 조사한 바가 있다. 또한, Kovacer 등(Contempory Agric. 39: 5-17, 1991), Castillo 등(J. Agric. Food Chem. 48: 1738-1745, 2000) 및 Takashi 등 (J. Agric. Food Chem. 50: 1254-1259, 2002)은 XAD, Diaion HP-20 및 Amberlite와 같은 여러 이온수지를 이용하여 포도씨로부터 카테킨 및 프로안토시아니딘 화합물을 효과적으로 추출 및 분리할 수 있는 방법을 보고한 바가 있다. 한편, 포도씨추출물에 다량 함유된 카테킨 및 프로시아니딘과 같은 폴리페놀화합물은 특유의 떫은맛을 지니고 있을 뿐만 아니라 산화적 및 효소적 갈변반응에 의해 쉽게 산화되어 품질에 악영향을 미치기 때문에 (Oszmianski, J., Sapis, J.C. and Macheix, J.J., J. Food Sci. 50: 1505-1506, 1985; Romeyer, F.M., Macheix, J.J. and Sapis, J.C., Phytochemistry 25: 219-221, 1986; Robichaud, J.L. and Noble, A.C., J. Sci. Food Agric. 53: 343-353, 1990) 지금까지 그를 이용한 가공식품의 개발에 크게 제한을 받고 있다. 따라서 현재 탄나아제(tannase)와 같은 효소처리나 효모를 이용한 발효공학 기술을 통하여 포도씨추출물이 지니고 있는 갈변 색소 및 나쁜 맛 등 여러 품질 특성을 개선하려는 기술 개발이 활발히 이루어지고 있다(식품첨가물 공전, 식품의약품안전청, 문영사, 서울, pp 967-968, 2001; 일본특허, 2002-10-0292731). Up to now, the development of technology for effectively extracting and separating anthocyanin pigments and grape catechin compounds from grape skins and the development of functional foods and cosmetics using them have been actively carried out (磐田 化學 工業, JP 2001-2001) -292731, Whiprowpdir Co., Japanese Unexamined Patent Publication No. 2000-125823, Haitai Confectionery Co., Ltd., Korea Unexamined Patent Publication No. 2000-0037080). Ricardo da Silva et al. ( Phytochemistry 30: 1259-1264, 1991; J. Agric. Food Chem. 45: 1156-1160, 1997) from catechins and ethanol extracts of grape seeds using polyamide column chromatography. A method for pure separation of procyanidin components has been reported, and Kalhithraka et al. ( Phytochemical Analysis 6: 265-267, 1995) have investigated the optimum solvent conditions for the extraction of grape seed phenolic compounds. See also Kovacer et al. ( Contempory Agric . 39: 5-17, 1991), Castillo et al. ( J. Agric. Food Chem. 48: 1738-1745, 2000) and Takashi et al. ( J. Agric. Food Chem. 50: 1254- 1259, 2002) reported a method for effectively extracting and separating catechin and proanthocyanidin compounds from grape seeds using various ion resins such as XAD, Diaion HP-20 and Amberlite. On the other hand, polyphenolic compounds such as catechins and procyanidins contained in large amounts in grape seed extracts not only have a characteristic astringent taste but are easily oxidized by oxidative and enzymatic browning reactions and adversely affect the quality (Oszmianski, J., Sapis). , JC and Macheix, JJ, J. Food Sci. 50: 1505-1506, 1985; Romeyer, FM, Macheix, JJ and Sapis, JC, Phytochemistry 25: 219-221, 1986; Robichaud, JL and Noble, AC, J Sci. Food Agric. 53: 343-353, 1990) Until now, the development of processed foods using them has been greatly limited. Therefore, the development of technology to improve various quality characteristics such as browning pigment and bad taste of grape seed extract through enzyme treatment such as tannase or fermentation engineering technology using yeast has been actively conducted (food additives, Korea Food and Drug Administration, Moon Youngsa, Seoul, pp 967-968, 2001; Japanese Patent, 2002-10-0292731).
이와 같이 항산화성 안토시아닌 색소 및 카테킨을 함유하고 있는 포도추출물의 제조방법 및 이를 이용한 기능성 건강보조식품의 개발이 활발히 이루어져 왔으나 아직까지 고품질의 포도 즙액 및 포도씨추출물의 제조방법 및 그를 이용한 기능성 포도 과립차의 개발에 관한 연구는 거의 없는 실정이다.As such, the development of grape extracts containing antioxidant anthocyanin pigments and catechins and functional health supplements using them has been actively developed, but the development of high quality grape juice and grape seed extracts and the development of functional grape granule tea using the same There is very little research on.
이에 본 발명자들은 항산화성 안토시아닌 색소와 카테킨 화합물을 다량 함유하고 있는 유기농 포도를 이용하여 포도 과즙 및 포도씨 엑기스 제조 기술 개발과 더불어 그를 이용한 고부가가치의 포도 과립차를 개발하고자 하였다.Accordingly, the present inventors have attempted to develop grape juice and grape seed extract manufacturing technology using organic grapes containing a large amount of antioxidant anthocyanin pigment and catechin compound, and to develop high value-added grape granule tea using the same.
따라서, 본 발명의 목적은 항산화성 안토시아닌 색소와 카테킨 화합물을 다량 함유하고 있는 포도 과즙 엑기스 및 포도씨 엑기스를 제조하는 방법을 제공하고자 한다.Accordingly, an object of the present invention is to provide a method for producing grape juice extract and grape seed extract containing a large amount of antioxidant anthocyanin pigment and catechin compound.
본 발명의 다른 목적은 상기에서 제조된 포도 과즙 엑기스와 포도씨 엑기스를 이용한 암, 고혈압, 심장병 및 노화의 예방 및 치료에 효과가 탁월한 포도 과립차를 제공하고자 한다.Another object of the present invention is to provide a grape granule tea excellent in the prevention and treatment of cancer, hypertension, heart disease and aging using the grape juice extract and grape seed extract prepared above.
본 발명의 상기 목적은 유기농 포도에서 안토시아닌 색소의 함량을 측정하고, 포도씨의 총카테킨 및 4가지 카테킨 화합물의 함량을 측정한 후, 유기농 포도를 탈립, 파쇄, 가온, 착즙, 여과 및 살균한 후 냉장 처리한 다음 다시 여과 및 농축하여 포도 엑기스를 제조하고, 상기 과정에 얻은 포도씨를 건조시켜 건조된 포도씨를 볶은 후 노르말-헥산으로 탈지하여 포도씨 유박을 얻고 이를 이온수로 현탁시 킨 후 여기에 효소를 가하여 가수분해반응을 실시하고 효소처리한 포도씨 유박 수용액에 에탄올을 가하여 열탕 추출한 후 여과 및 농축하여 포도씨 엑기스를 얻은 다음, 상기에서 제조된 포도 과즙 엑기스와 포도씨 엑기스를 혼합하여 고품질의 기능성 포도 과립차를 제조함으로써 달성하였다.The object of the present invention is to measure the content of the anthocyanin pigment in organic grapes, and after measuring the total catechin and four catechins of grape seeds, the organic grapes are granulated, crushed, warmed, juiced, filtered and sterilized After filtration and concentrating again to prepare a grape extract, dried grape seed obtained in the above process, roasted dried grape seed, degreased with normal-hexane to obtain grape seed oil, suspended it in ionized water and add enzyme to it Hydrolysis was carried out, ethanol was added to an aqueous solution of enzyme-treated grape seed milk, extracted with hot water, filtered and concentrated to obtain grape seed extract, and then the grape juice extract prepared above was mixed with grape seed extract to prepare high quality functional grape granule tea. Achieved.
이하, 본 발명의 구성을 구체적으로 설명한다. EMBODIMENT OF THE INVENTION Hereinafter, the structure of this invention is demonstrated concretely.
본 발명은 포도의 안토시아닌 색소의 함량 측정 단계; 포도씨의 총카테킨 및 4가지 카테킨 화합물의 함량 측정 단계; 유기농 포도에서 포도 엑기스의 제조 단계; 건조 포도씨로부터 포도씨 유박을 얻는 단계; 포도씨 유박의 가수분해 및 에탄올 추출후 포도씨 엑기스를 얻는 단계; 상기의 포도 과즙 엑기스와 포도씨 엑기스를 혼합하여 고품질의 기능성 포도 과립차를 제조하는 단계로 구성된다.The present invention comprises the steps of measuring the content of anthocyanin pigment of grape; Determining the content of total catechin and four catechin compounds of grape seed; Preparation of grape extracts from organic grapes; Obtaining grape seed oil from dry grape seeds; Obtaining grape seed extract after hydrolysis and ethanol extraction of grape seed milk; The grape juice extract and grape seed extract are mixed to produce a high quality functional grape granule tea.
본 발명 포도 과립차의 제조방법은 다음 단계를 포함함을 특징으로 함:Method for producing grape granule tea of the present invention is characterized in that it comprises the following steps:
유기농 포도를 탈립, 파쇄, 가온, 착즙, 여과 및 살균한 후 냉장 처리한 다음 다시 여과 및 농축하여 포도 엑기스를 제조하고, Organic grapes are granulated, crushed, warmed, juiced, filtered and sterilized, then refrigerated, filtered and concentrated again to prepare grape extracts.
상기에서 얻은 포도씨를 건조하여 볶은 다음 분쇄하고 노르말-헥산으로 탈지하여 얻은 탈지박을 효소(비스코자임 L, Viscozyme L) 처리하고 에탄올로 가열추출한 다음 여과 및 농축하여 포도씨 에탄올추출물 엑기스를 제조하고,The grape seeds obtained above were dried, roasted, crushed, degreased with normal-hexane to be treated with enzymes (biscozyme L, Viscozyme L), heated and extracted with ethanol, filtered and concentrated to prepare grape seed ethanol extract extract,
상기 포도 과즙 엑기스 (60°Brix) 10 중량%와 포도씨 엑기스 (50°Brix) 5~15 중량%에 정제포도당 65~75 중량%, 유당 3.0 중량%, 말토덱스트린 2.0 중량%, 비타민C 4.0 중량% 및 구연산 1.0 중량%를 혼합하여 50 메쉬 크기의 과립으로 제조 함.10% by weight of the grape juice extract (60 ° Brix) and 5-15% by weight of grape seed extract (50 ° Brix) 65-75% by weight glucose, 3.0% by weight lactose, 2.0% by weight maltodextrin, 4.0% by weight vitamin C And 1.0% by weight of citric acid to prepare a granule of 50 mesh size.
이하, 본 발명의 구체적인 구성을 실시예를 들어 상세히 설명하지만 본 발명의 권리범위가 하기 실시예에만 제한되는 것은 아니다.Hereinafter, the specific configuration of the present invention will be described in detail with reference to Examples, but the scope of the present invention is not limited only to the following Examples.
[실시예]EXAMPLE
실시예 1: 포도 과피의 안토시아닌 색소 함량 측정Example 1 Determination of Anthocyanin Pigment Content in Grape Skin
포도 과립차 제조용 최적 포도를 선별하기 위하여 경북 상주, 김천, 경산 및 영천 그리고 충북 영동에서 노지 재배한 포도 캠벨얼리 품종을 2003년 8월 중순부터 9월 하순까지 최적 수확시기에 포도를 각각 수확한 후 포도의 생리활성물질의 지표가 되는 안토시아닌 색소 함량을 측정하였다.In order to select the optimal grapes for the manufacture of grape granule tea, grapes Campbell early varieties grown in open fields in Sangju, Gimcheon, Gyeongsan and Yeongcheon, Gyeongbuk, and Yeongdong, Chungbuk, were harvested at the optimal harvesting time from mid-August to late September 2003. Anthocyanin pigment content, which is an indicator of bioactive substances, was measured.
먼저, 산지별로 수확한 생체 포도를 손으로 파쇄하여 포도 과피, 과육 및 포도씨를 각각 따로 분리한 후 동결건조하였다. 포도 과피 5 g에 에탄올-1.5 N 염산(85:15) 100 mL를 가하여 균질기(homogenizer, Iuchi CM-100, 일본)로 마쇄한 후 여과하여 얻어진 여과액을 200 mL 정용 플라스크로 정용한 뒤 실온의 암소에서 2시간 방치 후 분광광도계(Cecil, UK)를 이용하여 535 nm에서 흡광도(O.D.)를 측정한 후 Fuleki와 Francis 방법(J. Food Sci. 33: 72-77, 1968a; J. Food Sci. 33: 78-83, 1968b)에 따라 다음의 식으로 총안토시아닌 색소 함량을 측정하고 그 결과를 표 1에 나타내었다.First, the living grapes harvested for each region were crushed by hand to separate grape skins, pulp and grape seeds, respectively, and then lyophilized. 100 g of ethanol-1.5 N hydrochloric acid (85:15) was added to 5 g of grape skin, and the mixture was crushed with a homogenizer (homogenizer, Iuchi CM-100, Japan), filtered and the filtrate was filtered into a 200 mL flask, and After 2 hours in the dark, absorbance (OD) was measured at 535 nm using a spectrophotometer (Cecil, UK), followed by Fuleki and Francis methods ( J. Food Sci . 33: 72-77, 1968a; J. Food Sci . 33: 78-83, 1968b), the total anthocyanin pigment content was measured by the following equation and the results are shown in Table 1.
총안토시아닌 색소(mg%) = 흡광도 × 200/시료량(g) × 1/85.1(흡광계수)Total anthocyanin pigment (mg%) = absorbance × 200 / sample amount (g) × 1 / 85.1 (absorption coefficient)
표 1에 나타난 바와 같이, 충북 영동, 경북 상주, 김천, 경산 및 영천에서 수확한 포도의 총안토시아닌 색소 함량은 각각 251.56, 250.82, 251.23, 253.23 및 252.76 mg% (생체 중)으로서 모두 비슷하게 나타났다. 반면, 상주 모동 지역에서 유기농법으로 재배한 포도의 총안토시아닌 함량은 295.12 mg%으로서 다른 포도 보다 함량이 높았다. 이와 같이 캠벨얼리 포도 과피의 안토시아닌 색소 함량은 산지에 따라 비슷하게 나타났으나 유기농 재배 포도는 일반재배 포도와 달리 총안토시아닌 색소의 함량이 높음을 알 수 있었다.As shown in Table 1, the total anthocyanin pigment contents of grapes harvested from Yeongdong, Gyeongbuk, Sangju, Gimcheon, Gyeongsan, and Yeongcheon, Chungbuk, were 251.56, 250.82, 251.23, 253.23 and 252.76 mg% (in vivo), respectively. On the other hand, the total anthocyanin content of organically grown grapes in Sangdong Modong area was 295.12 mg%, higher than other grapes. As described above, the anthocyanin pigment content of the Campbell early grape skin was similar depending on the region, but the organically grown grapes were found to have a high total anthocyanin pigment content, unlike the general cultured grapes.
실시예 2: 포도씨의 카테킨 함량 측정Example 2: Determination of Catechin Content in Grape Seeds
포도과립차 제조용 포도씨를 선별하기 위하여 위에서 얻어진 포도씨의 생리활성물질의 지표가 되는 총 카테킨 및 4가지 카테킨 조성 함량을 측정하였다.To select grape seeds for grape granulation tea, total catechin and four catechin composition contents, which are indicative of bioactive substances of grape seeds obtained above, were measured.
실험예 1: 총카테킨 함량 측정Experimental Example 1: Determination of Total Catechin Content
총 카테킨 함량 측정은 식품공전(식품의약품 안전청, 문영사, pp 330-331, 2000)에 따라 바닐린비색법에 의해 측정하였다. 즉, 건조 포도씨 10g을 분쇄한 다 음 80% 메탄올수용액 200 mL 가하여 울트라클리너(ultracleaner, 미국 브라소닉)에서 3시간 동안 2회 반복 추출한 후 감압여과 및 농축하여 포도씨추출물 (9.2 g)을 얻었다. 상기 추출물 0.2 g에 80% 메탄올수용액 100 mL을 가하여 녹인 후 여과하여 얻어진 여액 1 mL에 발색시약 (ο-vanillin 1 g을 메탄올 100 mL에 용해시키고 따로 메탄올의 8%가 되도록 진한 염산을 혼합하여 시험전에 바닐린 용액과 염산용액을 1:1로 혼합한 것) 5 mL를 넣고 30℃에서 20분간 반응시킨 후 자외선/가시광선 분광광도계(UV/vis spectrophotometer)(Digital ultraviolet spectrophotomer Cecil, cambridge, UK)를 이용하여 500 nm에서 흡광도를 측정하였다. 이때 표준용액 [(+)-카테킨을 메탄올에 녹여서 100~1,000 ㎍/mL로 한 것]은 위와 동일한 방법으로 실시하여 검량선을 작성한 후 시험용액 중의 카테킨 농도 (㎍/g)를 구한 후 다음 식에 따라 시료 중의 총 카테킨 함량 (mg/100g)을 구하였다. 이때 모든 자료는 3회 반복하여 측정한 값을 평균하여 나타내었다.Total catechin content was measured by vanillin colorimetry according to the Food Code (Food and Drug Administration, Moon Youngsa, pp 330-331, 2000). That is, 10 g of dry grape seed was pulverized, and 200 mL of 80% aqueous methanol solution was added thereto, followed by repeated extraction for 3 hours in an ultracleaner (ultracleaner, Brasonic, USA), followed by filtration under reduced pressure and concentration to obtain grape seed extract (9.2 g). To 0.2 g of the extract, add 100 mL of 80% aqueous methanol solution, dissolve, and filter 1 mL of the filtrate obtained by filtration. (1 g of ο-vanillin was dissolved in 100 mL of methanol, and concentrated hydrochloric acid was mixed to make 8% of methanol separately. 5 mL of a mixture of vanillin solution and hydrochloric acid solution 1: 1) and reacted at 30 ° C. for 20 minutes, followed by UV / vis spectrophotometer (Digital ultraviolet spectrophotomer Cecil, cambridge, UK). Absorbance at 500 nm was measured. At this time, the standard solution [dissolved in (+)-catechin in methanol to make 100 ~ 1,000 ㎍ / mL] was prepared by the same method as above, and prepared the calibration curve. Accordingly the total catechin content (mg / 100g) in the sample was obtained. At this time, all the data were shown by averaging the measured value repeatedly three times.
총 카테킨 함량 (mg/100 g) = C×(V ×N/W)×10/100Total catechin content (mg / 100 g) = C × (V × N / W) × 10/100
C: 시험용액중의 카테킨의 농도 (㎍/g)C: concentration of catechin in test solution (µg / g)
W: 시료채취량 (g)W: Sample volume (g)
V: 시험용액의 전량 (mL)V: total amount of test solution (mL)
N: 시험용액의 희석배수N: Dilution factor of test solution
포도 산지별 캠벨얼리 포도씨의 총 카테킨 함량을 비교한 결과는 표 2에 나타내었다.Table 2 shows the results of comparing the total catechin content of Campbell early grape seeds by grape regions.
표 2에 나타난 바와 같이, 충북 영동, 경북 상주, 김천, 경산 및 영천에서 수확한 포도씨의 총 카테킨 함량은 각각 3.87, 3.53, 3.85, 3.75 및 3.79% (건물 중)으로서 산지별에 따라 약간 차이가 있었으나 거의 비슷하였다. 반면, 상주 모동 지역에서 유기농법으로 재배한 포도의 총 카테킨 함량은 4.61%으로서 다른 포도 보다 함량이 높았다. 이와같이 위의 총 안토시아닌 색소 함량에서 보는 바와 같이 캠벨얼리 포도씨의 총 카테킨 함량은 산지에 따라 비슷하게 나타났으나 유기농 재배 포도는 일반재배 포도와 달리 총 카테킨 함량이 높음을 알 수 있었다.As shown in Table 2, the total catechin content of grape seeds harvested from Yeongdong, Gyeongbuk, Sangju, Gimcheon, Gyeongsan, and Yeongcheon, Chungbuk, was 3.87, 3.53, 3.85, 3.75, and 3.79%, respectively, which differed slightly depending on the region. But it was almost the same. On the other hand, the total catechin content of organically grown grapes in Sangdong Modong area was 4.61%, higher than that of other grapes. As shown in the above total anthocyanin pigment content, the total catechin content of the Campbell Early grape seed was similar depending on the region, but the organically grown grapes were found to have a higher total catechin content than the general cultured grapes.
실험예 2: 4가지 카테킨 조성 함량 측정Experimental Example 2: Determination of four catechin composition contents
HPLC에 의한 포도씨 메탄올추출물의 카테킨류 정량분석은 Ricardo da Silva의 방법(1990)을 변형한 최 등(문성옥, 이준영, 김은정, 최상원. 한국식품과학회지, 35: 576-585, 2003)의 방법에 따라 다음과 같이 실시하였다.Quantitative analysis of catechins of methanol extract of grape seed by HPLC was carried out by Choi et al. (Moon Sung-ok, Jun-young Lee, Eun-jung Kim, Sang-Won Choi. Korean Journal of Food Science and Technology, 35: 576-585, 2003). According to the following procedure.
즉, 포도씨추출물 0.2 g을 80% 메탄올수용액으로 용해시킨 후 100 mL로 정용하였다. 이 중 2.0 mL에 초순수 6.0 mL를 가하고 미리 20% 메탄올수용액으로 평형 화시켜 놓은 폴리아미드 카트리지 (polyamide cartridge)에 흡착시킨 후 같은 용액 (20 mL)으로 수세하였다. 다음으로, 80% 메탄올용액 (50 mL)으로 흡착된 카테킨류를 용출시킨 다음 농축한 후 여기에 내부표준물질로서 카테콜 (catechol 0.2 mg을 MeOH 1 mL에 녹인 액) 1 mL와 메탄올 1 mL 혼합액을 가하여 용해시킨 후 0.45 ㎛ 멤브레인 필터로 여과하여 HPLC로 4가지 카테킨류 [(+)-카테킨, 프로시아니딘 B2, (-)-에피카테킨, 및 (-)-에피카테킨 갈레이트]를 분석하였다. 이때 각 시료의 카테킨류 함량은 4가지 표준 카테킨 물질을 이용하여 별도로 작성한 검량선으로부터 측정하였다.That is, 0.2 g of grape seed extract was dissolved in 80% aqueous methanol solution, and then 100 mL was used. 6.0 mL of ultrapure water was added to 2.0 mL of this solution, and the resultant was adsorbed onto a polyamide cartridge previously equilibrated with 20% aqueous methanol solution and washed with the same solution (20 mL). Next, catechins adsorbed with 80% methanol solution (50 mL) were eluted, concentrated, and then mixed with 1 mL of catechol (0.2 mg of catechol dissolved in 1 mL of MeOH) and 1 mL of methanol as an internal standard. 4 catechins [(+)-catechin, procyanidin B 2 , (-)-epicatechin, and (-)-epicatechin gallate] were analyzed by HPLC by dissolving by adding a 0.45 μm membrane filter. At this time, the catechin content of each sample was measured from a calibration curve prepared separately using four standard catechin substances.
표 3에 나타난 바와 같이, 충북 영동, 경북 상주, 김천, 경산 및 영천에서 수확한 포도씨의 4가지 카테킨 조성 함량(건물 중)을 보면 (+)-카테킨 0.20%, (-)-프로시아니딘 0.1%, (-)-에피카테킨 0.29% 및 (-)-에피카테킨 갈레이트 0.02% 내외 로서 거의 비슷하게 나타났다. 반면, 상주 모동 지역에서 유기농법으로 재배한 포도의 4가지 카테킨 조성 함량을 보면 (+)-카테킨 0.22%, (-)-프로시아니딘 B2 0.14%, (-)-에피카테킨 0.40% 및 (-)-에피카테킨 갈레이트 0.03% 내외로서 다른 포도씨 보다 함량이 높았다. 이와같이 유기농 재배 포도씨의 4가지 주된 카테킨 조성 함량은 위의 총 안토시아닌 색소 및 총카테킨 함량에서 보는 바와 같이 일반재배 포도씨와 달리 총 카테킨 함량이 높음을 알 수 있었다.As shown in Table 3, the four catechin composition contents (in buildings) of grape seeds harvested from Yeongdong, Gyeongbuk, Sangju, Gimcheon, Gyeongsan, and Yeongcheon, Chungbuk, were found to be (+)-catechin 0.20%, (-)-procyanidine 0.1%, (-)-Epicatechin 0.29% and (-)-Epicatechin gallate were 0.02% around, almost similar. On the other hand, the contents of four catechins of organically grown grapes in Sangdong Modong area were 0.22% for (+)-catechin, 0.14% for (-)-procyanidin B 2 , 0.40% for (-)-epicatechin and (-)- Epicatechin gallate was about 0.03% higher than other grape seeds. As such, the four main catechin composition contents of the organically grown grape seeds were found to be higher in total catechin content than in general cultivated grape seeds as shown in the above total anthocyanin pigment and total catechin content.
실험예 3: 효소 및 비효소 처리에 의해 생산된 포도씨 엑기스의 카테킨 함량 비교Experimental Example 3: Comparison of catechin content of grape seed extract produced by enzyme and non-enzyme treatment
상기에서 효소 및 비효소 처리에 의해 생산된 포도씨 엑기스의 총 카테킨 및 4가지 카테킨 조성 함량을 상기 실시예 2의 방법에 따라 측정하고 그 결과를 표 4와 표 5에 나타내었다.The total catechin and four catechin composition contents of grape seed extract produced by the enzyme and non-enzyme treatment were measured according to the method of Example 2, and the results are shown in Tables 4 and 5.
표 4 및 표 5에 나타난 바와 같이, 효소 및 비효소 처리에 의해 생산된 포도씨 엑기스의 수율은 각각 약 13.2% 및 7.1%로서 효소 처리 엑기스의 수율이 비효소 처리구 보다 약 2.0배 높았다. 또한, 효소처리에 의해 생산된 포도씨 엑기스의 총카테킨 함량(건조 분말당)은 41.85%이었으며, 또한 4가지 카테킨 조성 함량을 보면 (+)-카테킨 6.18%, 프로시아니딘 B2 0.21%, (-)-에피카테킨 5.21% 및 (-)-에피카테킨 갈레이트 0.19%로 나타났다. 반면, 비효소 처리 포도씨 엑기스의 총 카테킨 함량은 65.98%이었으며, 그리고 4가지 주된 카테킨 조성 함량을 보면 (+)-카테킨 7.47%, 프로시아니딘 B2 0.43%, (-)-에피카테킨 6.74% 및 (-)-에피카테킨 갈레이트의 0.49% 이었다. 이와 같이 효소 처리에 의해 생산된 포도씨 엑기스는 비효소 처리 엑기스 보다 포도씨의 주된 생리활성물질인 총 카테킨 및 4가지 카테킨 조성 함량이 다소 낮지만 추출 수율이 높아서 결과적으로 건조 포도씨 100 g당 총 카테킨 함량은 5.52% 및 4.69%, 그리고 4가지 카테킨 조성 함량은 1.56% 및 1.08%로서 효소 처리한 포도씨 엑기스가 비효소 처리 엑기스 보다 함량이 높음을 알 수 있었다.As shown in Table 4 and Table 5, the yields of grape seed extract produced by enzyme and non-enzyme treatment were about 13.2% and 7.1%, respectively, and the yield of enzyme-treated extract was about 2.0 times higher than that of non-enzyme treatment. In addition, the total catechin content (per dry powder) of grape seed extract produced by the enzyme treatment was 41.85%, and the four catechin composition contents were (+)-catechin 6.18%, procyanidin B 2 0.21%, (-)- Epicatechin 5.21% and (-)-epicatechin gallate 0.19%. On the other hand, the total catechin content of the non-enzymatic grape seed extract was 65.98%, and the four main catechin contents were (+)-catechin 7.47%, procyanidin B 2 0.43%, (-)-epicatechin 6.74% and (-). 0.49% of epicatechin gallate. The grape seed extract produced by the enzyme treatment was slightly lower in total catechin and four catechins, which are the main bioactive substances of grape seeds, but the extraction yield was higher than the non-enzyme extract, resulting in a total catechin content per 100 g of dry grape seed. 5.52% and 4.69%, and the four catechin composition contents were 1.56% and 1.08%, indicating that the enzyme-treated grape seed extract was higher than the non-enzyme-treated extract.
실시예 3: 효소 및 비효소 처리에 의해 생산된 포도씨추출물 엑기스의 물리적 특성 측정Example 3 Determination of Physical Properties of Grape Seed Extract Extract Produced by Enzyme and Non-Enzyme Treatment
상기 실험예 3에서 효소 및 비효소 처리에 의해 생산된 포도씨 엑기스의 용해성, pH, 색상 및 맛 등의 물리적 특성을 측정하여 그 결과를 표 6에 나타내었다.In Experimental Example 3, physical properties such as solubility, pH, color and taste of grape seed extract produced by enzyme and non-enzyme treatment were measured, and the results are shown in Table 6.
표 6에 나타난 바와 같이, 효소처리에 의해 생산된 포도씨 엑기스는 수용성 및 알코올 수용성인데 반해 비효소 처리 엑기스는 80% 알코올 수용성을 지니고 있으며, pH는 각각 4.68 및 4.79로 비슷하였다. 그리고 효소처리구의 색상 (L=94.15, a=2.62 및 b=23.03)은 연한 갈색인 반면 비효소 처리구의 색상 (L=75.62, a=11.16 및 b=50.50)로 진한 갈색을 나타내었으며, 효소 처리구는 약간 쓴맛과 단맛을 지니고 있는 반면, 비효소 처리구는 강한 쓴맛을 보였다. 이와 같이 효소처리에 의해 생산된 포도씨 엑기스는 용해성, 색상 및 맛이 비효소 처리구 보다 우수함을 알 수 있었다.As shown in Table 6, the grape seed extract produced by enzymatic treatment was water soluble and alcohol soluble whereas the non-enzyme treated extract had 80% alcohol solubility, and the pH was similar at 4.68 and 4.79, respectively. The color of the enzyme treatment (L = 94.15, a = 2.62 and b = 23.03) was light brown while the color of the non-enzyme treatment (L = 75.62, a = 11.16 and b = 50.50) was dark brown. Was slightly bitter and sweet, while the non-enzyme treatment had a strong bitter taste. Thus, grape seed extract produced by the enzyme treatment was found that the solubility, color and taste is superior to the non-enzyme treatment.
실시예 4: 본 발명 포도 과립차의 제조Example 4 Preparation of the Invention Grape Granule Tea
상기 실시예 1∼3을 통해, 경북 상주 모동에서 유기농법으로 재배한 캠벨얼리 품종이 다른 지역에서 재배된 것보다 과실의 안토시아닌 색소 그리고 포도씨의 총 카테킨 및 4가지 카테킨화합물의 함량이 훨씬 높음을 알 수 있었다. 따라서 유기농으로 재배한 상주 모동 포도를 이용하여 다음과 같이 포도 과립차를 제조하였다. Through Examples 1 to 3, it was found that the Campbell early varieties cultivated by organic farming in Sangju, Gyeongsangbuk-do, were much higher in the content of anthocyanin pigment and grape catechin and four catechin compounds. there was. Therefore, grape granule tea was prepared using organically grown resident Modong grape as follows.
먼저, 포도 과즙 엑기스를 제조하기 위해 2002년 9월 초순경에 경북 상주 모동에서 수확한 봉지 씌운 캠벨얼리 생체 포도(10 kg)를 탈립하여 포도 줄기와 과실을 선별한 후 롤(Roll)기에 넣어 파쇄하고 80~90℃에서 10분간 가온한 후 착즙 및 여과하여 포도즙액과 잔사를 분리하였다. 즙액은 다시 100℃에서 1분간 살균처리한 후 1~5℃ 냉장고에 넣어 2주일간 보관하면서 침전하는 주석산을 감압여과하여 제거한 후 얻어진 여과액을 50℃ 이하에서 감압농축기를 사용하여 농축하여 포도 엑기스 (60°Brix, 3.5 kg)를 제조하였다(정의선, 대한민국 특허출원번호 제2001-0004553호, 2001년 1월).First, in order to manufacture the grape juice extract, the encapsulated Campbell early bio grapes (10 kg) were harvested in Sangdong, Gyeongsangbuk-do, at the beginning of September 2002, the grape stems and fruits were sorted, and then put into a roll machine for crushing. After heating for 10 minutes at 80 ~ 90 ℃ juice and filtered to separate the juice and the residue. The juice solution was sterilized again at 100 ° C. for 1 minute, and then stored in a 1-5 ° C. refrigerator for 2 weeks to remove the tartaric acid precipitated under reduced pressure. The filtrate was concentrated using a vacuum condenser at 50 ° C. or lower. 60 ° Brix, 3.5 kg) was prepared (Jeong-sun Jung, Korean Patent Application No. 2001-0004553, January 2001).
다음으로, 상기에서 얻은 포도 잔사를 물에 넣어 휘저어면서 상층으로 떠오르는 포도 과피 및 일부의 과육 잔사를 제거하고 아래에 침전된 포도씨를 체를 이용하여 수거하였다. 포도씨를 50~60℃로 조절된 강제순환식 열풍건조기에 넣어 이틀간 건조한 후 (수분 5% 이하까지) 다시 볶음기 (곡물온도 100℃, 솥온도 200℃, 동광유압, 서울, 한국)에 넣어 5분간 볶았다. 볶은 포도씨 (10 kg)를 조분쇄기로 분쇄한 후 여기에 노르말-헥산 (30 L)을 가하여 열탕에서 하룻 동안 교반하면서 탈 지한 후 여과 및 농축하여 포도씨 기름 (0.82 kg)과 유박 (oil cake, 9.18 kg)을 각각 얻었다. 유박을 미리 30℃로 가온한 이온수 (25 L)에 넣고 1시간 동안 교반한 후 여기에 효소 비스코자임 L (덴마크 노보자임) 1 kg을 가하여 혼합한 후 50~60℃로 가온한 다음 2시간 동안 효소반응을 실시하였다. 여기에 주정 에탄올 (75 L)을 가하여 80~90℃에서 환류냉각장치가 부착된 추출기에서 2회 반복 추출한 후 여과 및 농축하여 포도씨 엑기스(50°Brix, 22.1 kg)을 제조하였다.Next, the grape residue obtained in the above was stirred in water to remove the grape skin and some of the pulp residue rising to the upper layer, and the grape seed precipitated below was collected using a sieve. Grape seed was placed in a forced circulation hot air dryer controlled at 50 ~ 60 ℃, dried for 2 days (up to 5% of moisture), and then put again in a stirrer (grain temperature 100 ℃, pot temperature 200 ℃, Donggwang hydraulic, Seoul, Korea) 5 Roasted for a minute. Roasted grape seeds (10 kg) are crushed with a coarsely mill, and then normal-hexane (30 L) is added thereto, degreased with stirring in hot water for one day, filtered and concentrated to obtain grape seed oil (0.82 kg) and oil cake (9.18). kg) respectively. Put the oil gourd into the ionized water (25 L) warmed to 30 ℃ in advance and stirred for 1 hour, and then mixed with 1 kg of enzyme biscozyme L (Denmark Novozyme), and warmed to 50 ~ 60 ℃ and then for 2 hours Enzyme reaction was performed. Alcohol ethanol (75 L) was added thereto, followed by repeated extraction twice in an extractor equipped with a reflux condenser at 80-90 ° C., followed by filtration and concentration to prepare grape seed extract (50 ° Brix, 22.1 kg).
상기에서 제조된 포도 과즙 엑기스 및 포도씨 엑기스에 정제포도당, 유당, 말토덱스트린, 비타민 C 및 구연산을 표 7의 배합비에 따라 혼합한 후 과립기에 넣고 50 메쉬 크기의 포도과립차를 제조하였다. Purified glucose, lactose, maltodextrin, vitamin C, and citric acid were mixed in the grape juice extract and grape seed extract prepared according to the mixing ratio of Table 7, and then put into a granulator to prepare a 50 mesh size grape granule tea.
실험예 1: 본 발명 포도 과립차의 품질 특성 조사Experimental Example 1 Investigation of Quality Characteristics of the Grape Granule Tea of the Present Invention
상기의 재료 혼합비율에 따른 포도 과립차의 품질특성을 알아보기 위하여 위에서 제조한 포도 과립차 5 g를 100 mL 비이커에 취하고 비등수 50 mL를 가하여 스푼으로 저어면서 녹인 후 포도 과립차의 당도 (°Brix), 용해도, 색도 및 수율을 측정하였고, 또한 잘 훈련된 관능검사요원 10명으로 하여금 5점 척도법에 따라 색, 향, 맛 및 종합적인 기호도를 평가하여 그 결과를 표 8에 나타내었다.In order to determine the quality characteristics of the grape granule tea according to the mixing ratio of the ingredients, 5 g of the grape granulated tea prepared above was taken in a 100 mL beaker, and 50 mL of boiling water was added to the mixture, followed by stirring with a spoon to dissolve sugar (° Brix), Solubility, chromaticity and yield were measured, and 10 well-trained organoleptics evaluated color, aroma, taste and overall palatability according to the 5-point scale method and the results are shown in Table 8.
표 8에 나타난 바와 같이, 포도 과립차의 당도, 용해도, 색도 및 수율 등은 혼합비율에 따라 큰 차이를 보이지 않았으나 관능검사 결과에서는 포도 과즙 엑기스 및 정제포도당 등의 첨가량이 증가할수록 기호도가 증가하였으며, 특히 시료 3구가 가장 양호한 맛을 나타내었다.As shown in Table 8, the sweetness, solubility, color, and yield of grape granule tea did not show a significant difference according to the mixing ratio, but in sensory evaluation, the preference increased as the amount of added grape juice extract and purified glucose increased. Three samples showed the best taste.
이상의 결과로부터 포도 과즙 엑기스 및 포도씨 추출물 엑기스를 이용하여 제조된 포도 과립차는 항산화성 안토시아닌 색소와 카테킨 성분을 다량 함유하고 있어 암, 심장병, 고혈압 및 노화를 예방할 수 있는 기능성 건강식품으로서 각광을 받을 것으로 기대된다.From the above results, grape granulated tea prepared using grape juice extract and grape seed extract extract contains a large amount of antioxidant anthocyanin pigment and catechin, which is expected to attract attention as a functional health food that can prevent cancer, heart disease, high blood pressure and aging. do.
상기 실시예와 실험예를 통하여 설명한 바와 같이, 본 발명은 항산화성 안토시아닌 색소 및 카테킨을 함유한 고품질의 포도 과립차 및 그것의 제조방법에 관한 것으로, 볶은 포도씨를 헥산으로 탈지하여 얻은 잔사를 효소 처리한 후 에탄올로 열탕 추출하고 여과 및 농축하여 얻어진 포도씨추출물 엑기스와 포도 과실을 파쇄, 가온, 착즙, 여과 및 살균한 후 냉장처리한 다음 다시 여과 및 농축하여 얻어진 포도 과즙 엑기스를 주성분으로 포함하는 포도 과립차를 제공하는 뛰어난 효과가 있다. 또한, 본 발명 포도 과즙 엑기스와 포도씨 엑기스는 각각 항산화성 카테킨 성분 및 안토시아닌 색소를 다량 함유하고 있어 암, 심장병, 고혈압 및 노화 등을 예방하는 기능성식품의 유효성분으로 사용될 수 있어 기능성식품산업상 매우 유용한 발명이다.As described in the above Examples and Experimental Examples, the present invention relates to a high-quality grape granule tea containing an antioxidant anthocyanin pigment and catechin, and a method for preparing the same, wherein the residue obtained by degreasing roasted grape seeds with hexane is subjected to enzyme treatment. Grape granulated tea containing grape juice extract obtained by boiling water extraction with ethanol, filtration and concentration, grape fruit extract and grape fruit extract were crushed, warmed, juiced, filtered and sterilized, refrigerated, and then filtered and concentrated. There is an excellent effect to provide. In addition, the grape juice extract and grape seed extract of the present invention contain a large amount of antioxidant catechin component and anthocyanin pigment, respectively, can be used as an active ingredient of the functional food to prevent cancer, heart disease, high blood pressure and aging, which is very useful in the functional food industry Invention.
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| JP4601570B2 (en) * | 2006-03-20 | 2010-12-22 | 株式会社ロッテ | Antioxidant, method for producing the same, and food and drink containing the antioxidant |
| KR100878876B1 (en) * | 2007-05-16 | 2009-01-15 | 재단법인 전라북도생물산업진흥원 | Process for Preparing Granule using Rubi Fructus |
| KR100978140B1 (en) * | 2008-02-27 | 2010-08-25 | 옥천농업협동조합 | Anthocyanin Extraction Method Using Grape Skin |
| KR101023215B1 (en) * | 2008-02-27 | 2011-03-18 | 옥천농업협동조합 | How to extract procandine from grape seeds |
| WO2014083577A2 (en) | 2012-11-27 | 2014-06-05 | Tata Global Beverages Limited | Beverage with heart aid functional ingredients and process thereof |
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