KR100842448B1 - The method for manufacturing the cyanidin-3-glucoside derived from a mulberry with the food coloring powder - Google Patents
The method for manufacturing the cyanidin-3-glucoside derived from a mulberry with the food coloring powder Download PDFInfo
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- KR100842448B1 KR100842448B1 KR1020060127755A KR20060127755A KR100842448B1 KR 100842448 B1 KR100842448 B1 KR 100842448B1 KR 1020060127755 A KR1020060127755 A KR 1020060127755A KR 20060127755 A KR20060127755 A KR 20060127755A KR 100842448 B1 KR100842448 B1 KR 100842448B1
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- YTMNONATNXDQJF-UBNZBFALSA-N chrysanthemin Chemical compound [Cl-].O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC2=C(O)C=C(O)C=C2[O+]=C1C1=CC=C(O)C(O)=C1 YTMNONATNXDQJF-UBNZBFALSA-N 0.000 title claims abstract description 65
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- 240000000249 Morus alba Species 0.000 title claims description 10
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- 238000004519 manufacturing process Methods 0.000 title claims description 8
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- 239000000049 pigment Substances 0.000 claims abstract description 37
- 239000000546 pharmaceutical excipient Substances 0.000 claims abstract description 8
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 43
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 39
- 238000000605 extraction Methods 0.000 claims description 12
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- 238000004108 freeze drying Methods 0.000 claims description 2
- 230000003078 antioxidant effect Effects 0.000 abstract description 5
- 239000003963 antioxidant agent Substances 0.000 abstract description 4
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- 238000003306 harvesting Methods 0.000 description 8
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
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- 150000008131 glucosides Chemical class 0.000 description 2
- 229930182470 glycoside Natural products 0.000 description 2
- 150000002338 glycosides Chemical group 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- FUKUFMFMCZIRNT-UHFFFAOYSA-N hydron;methanol;chloride Chemical compound Cl.OC FUKUFMFMCZIRNT-UHFFFAOYSA-N 0.000 description 2
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- 239000000126 substance Substances 0.000 description 2
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- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 1
- TWCMVXMQHSVIOJ-UHFFFAOYSA-N Aglycone of yadanzioside D Natural products COC(=O)C12OCC34C(CC5C(=CC(O)C(O)C5(C)C3C(O)C1O)C)OC(=O)C(OC(=O)C)C24 TWCMVXMQHSVIOJ-UHFFFAOYSA-N 0.000 description 1
- PLMKQQMDOMTZGG-UHFFFAOYSA-N Astrantiagenin E-methylester Natural products CC12CCC(O)C(C)(CO)C1CCC1(C)C2CC=C2C3CC(C)(C)CCC3(C(=O)OC)CCC21C PLMKQQMDOMTZGG-UHFFFAOYSA-N 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
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- 229930014669 anthocyanidin Natural products 0.000 description 1
- 150000001452 anthocyanidin derivatives Chemical class 0.000 description 1
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- 235000007336 cyanidin Nutrition 0.000 description 1
- GVJHHUAWPYXKBD-UHFFFAOYSA-N d-alpha-tocopherol Natural products OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
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- 239000000706 filtrate Substances 0.000 description 1
- 235000013376 functional food Nutrition 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 235000021021 grapes Nutrition 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- PFOARMALXZGCHY-UHFFFAOYSA-N homoegonol Natural products C1=C(OC)C(OC)=CC=C1C1=CC2=CC(CCCO)=CC(OC)=C2O1 PFOARMALXZGCHY-UHFFFAOYSA-N 0.000 description 1
- 235000003642 hunger Nutrition 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
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- 235000004213 low-fat Nutrition 0.000 description 1
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- 239000000974 natural food coloring agent Substances 0.000 description 1
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- 229960001295 tocopherol Drugs 0.000 description 1
- 229930003799 tocopherol Natural products 0.000 description 1
- 235000010384 tocopherol Nutrition 0.000 description 1
- 239000011732 tocopherol Substances 0.000 description 1
- 230000004304 visual acuity Effects 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
- GVJHHUAWPYXKBD-IEOSBIPESA-N α-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-IEOSBIPESA-N 0.000 description 1
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L19/00—Products from fruits or vegetables; Preparation or treatment thereof
- A23L19/09—Mashed or comminuted products, e.g. pulp, purée, sauce, or products made therefrom, e.g. snacks
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/10—Natural spices, flavouring agents or condiments; Extracts thereof
- A23L27/14—Dried spices
-
- A23L3/44—
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/40—Colouring or decolouring of foods
- A23L5/42—Addition of dyes or pigments, e.g. in combination with optical brighteners
- A23L5/43—Addition of dyes or pigments, e.g. in combination with optical brighteners using naturally occurring organic dyes or pigments, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2250/00—Food ingredients
- A23V2250/02—Acid
- A23V2250/032—Citric acid
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- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
본 발명은 오디로부터 유래한 시아니딘-3-글루코사이드를 식용색소 분말로 제조하는 방법에 관한 것으로서, 상세하게는 오디에서 시아니딘-3-글루코사이드를 추출 및 농축하는 단계; 상기 농축물에 부형제를 첨가하여 시아니딘-3-글루코사이드를 안정화시키는 단계; 및 상기 안정화된 시아니딘-3-글루코사이드를 동결건조하여 분말화하는 단계를 포함하는 오디로부터 유래한 시아니딘-3-글루코사이드를 식용색소 분말로 제조하는 방법에 관한 것이다.The present invention relates to a method for preparing cyanidin-3-glucoside derived from audi as an edible pigment, specifically, the step of extracting and concentrating cyanidin-3-glucoside in Audi; Adding excipients to the concentrate to stabilize cyanidin-3-glucoside; And lyophilizing the stabilized cyanidin-3-glucoside to powder the cyanidin-3-glucoside derived from Audi.
오디, 시아니딘-3-글루코사이드, 천연 항산화색소 Audi, Cyanidin-3-glucoside, Natural Antioxidant
Description
도 1은 추출용매별 오디에 함유된 시아니딘-3-글루코사이드의 함량을 비교한 그래프이다.1 is a graph comparing the content of cyanidin-3-glucoside contained in Audi for each extraction solvent.
도 2는 에탄올 농도별 산 첨가시의 시아니딘-3-글루코사이드의 함량을 비교한 그래프이다.Figure 2 is a graph comparing the content of cyanidin-3-glucoside at the time of acid addition by ethanol concentration.
도 3은 추출 방법 및 그에 따른 시아니딘-3-글루코사이드 추출효율을 비교한 것이다.Figure 3 compares the extraction method and the resulting cyanidin-3-glucoside extraction efficiency.
도 4는 덱스트린 첨가 여부에 따른 색소 선명도를 나타내는 도면이다.4 is a view showing the sharpness of the pigment according to the addition of dextrin.
본 발명은 오디로부터 유래한 시아니딘-3-글루코사이드를 식용색소 분말로 제조하는 방법에 관한 것으로서, 상세하게는 오디에서 시아니딘-3-글루코사이드를 추출 및 농축하는 단계; 상기 농축물에 부형제를 첨가하여 시아니딘-3-글루코사이드를 안정화시키는 단계; 및 상기 안정화된 시아니딘-3-글루코사이드를 동결건조하 여 분말화하는 단계를 포함하는 오디로부터 유래한 시아니딘-3-글루코사이드를 식용색소 분말로 제조하는 방법에 관한 것이다.The present invention relates to a method for preparing cyanidin-3-glucoside derived from audi as an edible pigment, specifically, the step of extracting and concentrating cyanidin-3-glucoside in Audi; Adding excipients to the concentrate to stabilize cyanidin-3-glucoside; And lyophilizing the stabilized cyanidin-3-glucoside to powder the cyanidin-3-glucoside derived from Audi.
최근 건강 식품에 대한 소비자들의 선호도 증가와 더불어 인공합성색소의 안전성에 대한 논란으로 인하여 천연색소가 가지는 기능성 및 이용성에 대한 가치가 재조명됨에 따라 각종 작물에 함유된 색소 물질에 대한 연구가 활발히 진행되고 있다. 포도의 경우 껍질에 존재하는 안토시아닌 색소의 다양한 기능성이 알려지면서 생식용 이외에 포도주, 주스, 잼 등의 가공식품과 시력개선제 등 의약품으로 판매되고 있어 경제성이 매우 크다. 또한, 유색미, 검정콩, 검정 찰옥수수 등도 대표적인 안토시아닌 색소 함유 작물로 알려짐에 따라 그 이용성이 증대되고 있으며, 대부분의 과실이나 꽃에 존재하는 안토시아닌 색소를 이용하여 기능성을 높인 상품을 개발함으로써 고부가 가치 산업으로 활용하기 위한 방안들이 연구되고 있다.Recently, research on pigmented substances in various crops has been actively conducted as the value of natural pigments has been re-examined due to the increased consumer preference for health foods and controversy over the safety of artificial synthetic pigments. . In the case of grapes, various functionalities of anthocyanin pigments present in the skin are known, and as a result, they are sold as processed foods such as wine, juice, jam, and medicines such as visual acuity improvers. In addition, color rice, black soybeans, black waxy corn, etc. are also known as a representative anthocyanin pigment-containing crops, and its usability is increasing. Plans for their use are being studied.
뽕나무 오디는 동의보감 탕액편(湯液篇)에 '까만 오디는 뽕나무의 정령(精靈)이 모여 있는 것이며, 당뇨병에 좋고 오장에 이로우며 오래 먹으면 배고픔을 잊게 해준다'라고 하며, '귀와 눈을 밝게 한다'라고 했으며, '오디를 오래 먹으면 백발이 검게 변하고 노화를 방지한다'라고 기록되어 있어 그 기능성이 기대되는 작물이다.Mulberry-wood is said to be in the Dongsimbogam Tang liquid piece (湯 液 篇) 'black mulberry is the soul of the mulberry tree (精靈) gathered, it is good for diabetes, it is beneficial to the five chapters, and long eating will make you forget hunger.' 'And if you eat audio for a long time, white hair will turn black and prevent aging', so its functionality is expected crop.
뽕나무 오디에 함유된 천연색소는 안토시아닌 색소의 한 형태인 시아니딘-3-글루코사이드로서 단일 물질로 존재하여, 보다 안정적이며 분리방법이 간단할 뿐만 아니라, 과실 전체에 색소를 함유하여 그 함량이 높고 분리수율 또한 높다. 오디 에 함유된 안토시아닌 색소 시아니딘-3-글루코사이드(cyanidin-3-glucoside, C3G)는 노화 억제 효과가 있는 토코페롤보다 7배나 높은 노화 억제 효과를 보이며, 오디의 시아니딘-3-글루코사이드의 함량은 포도의 23배, 유색미의 2.3배에 달한다. 오디 추출물은 강한 항산화 물질을 가져 뇌손상뿐만 아니라 활성 산소에 대한 각종 만성 퇴행성 질환을 예방하는 것으로 알려져 있다.Natural pigment contained in mulberry mulberry is a form of anthocyanin pigment, cyanidin-3-glucoside, which is present as a single substance, which is more stable and simple to separate. Yield is also high. Anthocyanin pigment cyanidin-3-glucoside (C3G) contained in Audi showed 7 times higher anti-aging effect than tocopherol, which has anti-aging effect. 23 times, 2.3 times of the color taste. Audi extract has strong antioxidants and is known to prevent various chronic degenerative diseases for free radicals as well as brain damage.
일반적으로 안토시아닌 색소는 색소의 기분 골격(아글리콘)인 안토시아니딘(anthocyanidin)에 결합하는 당의 종류에 따라 색소의 배당체가 결정되며, 항산화 활성 등 생리적 효능에도 영향을 미치는 것으로 알려져 있다. 최근의 연구결과에 의하면 시아니딘(cyanidin)의 경우 항산화력이 2.24이지만 글루코오스(glucose) (3.49)와 람노 글루코오스(rhamnoglucose) (2.99)가 결합하면 항산화력이 증가한다. 안토시아닌 색소는 자연계에 배당체 형태로 존재하며 오디에 다량으로 함유된 시아니딘-3-글루코사이드는 여러 색소 중에서도 항산화력이 가장 뛰어난 것으로 알려져 있기 때문에 오디에 함유된 안토시아닌 색소인 시아니딘-3-글루코사이드(cyanidin-3-glucoside, C3G)는 천연색소 자원으로서 그 가치를 새롭게 인정받고 있다.In general, the anthocyanin pigment is a glycoside of the pigment is determined according to the type of sugar that binds to anthocyanidin, which is the mood skeleton (aglycone) of the pigment, and is known to affect physiological effects such as antioxidant activity. Recent studies have shown that cyanidins have an antioxidant capacity of 2.24, but the combination of glucose (3.49) and rhamnoglucose (2.99) increases antioxidant activity. Anthocyanin pigments are present in glycosides in nature, and cyanidin-3-glucosides contained in large amounts in Audi are known to have the highest antioxidant power among various pigments. -3-glucoside (C3G) is newly recognized for its value as a natural pigment resource.
그러나 색소 자체의 불안정성 때문에 조리 또는 가공 중에 쉽게 변색되는 등 문제점이 있다. However, there are problems such as discoloration during cooking or processing due to the instability of the pigment itself.
본 발명은 오디에 시아니딘-3-글루코사이드이 존재함을 발견하고 시아니딘-3-글루코사이드의 안정성을 유지하면서 인체에 유해하지 않은 천연 식용색소를 오 디로부터 유래한 시아니딘-3-글루코사이드를 식용색소 분말로 제조하는 방법을 제공하고자 한다.The present invention finds the presence of cyanidin-3-glucoside in the odyssey, and maintains the stability of cyanidin-3-glucoside while maintaining the stability of cyanidin-3-glucoside. It is intended to provide a method of making powder.
상기 목적을 달성하기 위하여, 본 발명은 오디에서 시아니딘-3-글루코사이드를 추출 및 농축하는 단계; 상기 농축물에 부형제를 첨가하여 시아니딘-3-글루코사이드를 안정화시키는 단계; 및 상기 안정화된 시아니딘-3-글루코사이드를 동결건조하여 분말화하는 단계를 포함하는 오디로부터 유래한 시아니딘-3-글루코사이드를 식용색소 분말로 제조하는 방법을 제공한다.In order to achieve the above object, the present invention comprises the steps of extracting and concentrating cyanidin-3-glucoside in Audi; Adding excipients to the concentrate to stabilize cyanidin-3-glucoside; And lyophilizing and drying the stabilized cyanidin-3-glucoside, thereby providing a method for preparing cyanidin-3-glucoside derived from Audi into an edible pigment.
바람직하게는 상기 시아니딘-3-글루코사이드를 추출하는 단계는 70%의 에탄올 및 0.1%의 구연산을 추출용매로 사용하는 오디로부터 유래한 시아니딘-3-글루코사이드를 식용색소 분말로 제조하는 방법을 제공한다.Preferably, the step of extracting cyanidin-3-glucoside provides a method for preparing cyanidin-3-glucoside from edible using 70% ethanol and 0.1% citric acid as an extraction solvent as an edible pigment powder. do.
또 바람직하게는 상기 부형제는 덱스트린 또는 말토덱스트린을 50중량%를 첨가하는 오디로부터 유래한 시아니딘-3-글루코사이드를 식용색소 분말로 제조하는 방법을 제공한다. Also preferably, the excipient provides a method for preparing cyanidin-3-glucoside derived from Audi, which adds 50% by weight of dextrin or maltodextrin, as an food coloring powder.
또 바람직하게는 상기 동결건조는 -85℃에서 5mTorr의 압력으로 48시간 동안 이루어지는 오디로부터 유래한 시아니딘-3-글루코사이드를 식용색소 분말로 제조하는 방법을 제공한다. Also preferably, the lyophilization provides a method of preparing cyanidin-3-glucoside derived from audi for 48 hours at a pressure of 5 mTorr at −85 ° C. as an food coloring powder.
또 바람직하게는 상기 오디는 수성뽕, 강선, 국광, 사방소, 태전조생, 절곡조생,부사, 팔청시평, 수원노상, 청노상, 천현노상, 죽천조생, 이대내1, 당상 7호 및 목상으로 이루어지는 그룹에서 하나 이상 선택되는 오디로부터 유래한 시아니딘-3-글루코사이드를 식용색소 분말로 제조하는 방법을 제공한다.In addition, the Audi is an aqueous mulberry, gangseon, kwanggwang, Sabangso, Taejeonjo, bending bending, adverbs, Palchungsipyeong, Suwon nosang, Cheongnosang, Cheonhyeonnosang, Jukcheonjosaeng, Idaenae 1, Dangsang 7 and Moksang Provided is a process for preparing cyanidin-3-glucoside derived from an Audi selected from at least one group consisting of food coloring powder.
이하, 본 발명인 오디로부터 유래한 시아니딘-3-글루코사이드를 식용색소 분말로 제조하는 방법에 관하여 상세히 설명한다.Hereinafter, a method for preparing cyanidin-3-glucoside derived from Audi of the present invention into food coloring powder will be described in detail.
<실시예 1> 뽕나무 오디의 과실적 특성 조사 및 우량 계통 선발<Example 1> Investigation of fruit characteristics and mulberry tree mulberry mulberry
한 그루의 오디 중 10% 정도 완숙된 때를 수확시기, 이로부터 미숙한 오디가 10% 미만 남아 있을 때까지를 수확성기, 10% 미만의 미숙한 오디가 남아 있을 때 이후를 수확종기라고 하는데, 한 그루에서 수확할 수 있는 총수량을 조사하기 위해 수확시기부터 수확종기까지의 성숙한 오디를 모두 수확한다. 계통당 공시주수는 2주로 하였다. 수확한 날짜별로 오디 무게를 측정한 후, 50과를 선별하여 과중, 과장, 과폭 및 과병장을 조사하였다. 당도 측정기(digital refractometer)를 이용하여 5℃에서 1시간 동안 정치시킨 과즙의 당도를 측정하였다. When the harvest time is about 10% of a single matured harvest, the harvest season is until there are less than 10% immature, and the harvest boils when there are less than 10% immature. Harvest all mature Audi from harvest to boil to investigate the total harvest from a single tree. The number of disclosures per line was 2 weeks. After the weight of the mulberry was measured by harvesting date, 50 fruits were screened to examine the fruit weight, fruit weight, fruit width and fruit disease. Using a digital refractometer, the sugar content of the juice was allowed to stand at 5 ° C. for 1 hour.
오디 생산용으로 적합한 품종을 육성하기 위하여 수량성, 오디의 크기, 당도 값을 고려하여 이들의 특성을 모두 만족시키는 계통을 우량계통으로 선발하였다(표 1).In order to cultivate varieties suitable for the production of Audi, a system that satisfies all of these characteristics was selected as a superior system in consideration of the quantity, size and sugar value (Table 1).
<실시예 2> 오디의 시아니딘-3-글루코사이드 함량 분석Example 2 Analysis of Cyanidin-3-glucoside Content of Audi
안토시아닌의 표준물질인 시아니딘-3-글루코사이드와 고성능 액체크로마토그래피 크로마토그램(HPLC chromatogram)을 비교하여 뽕나무 오디의 계통별 함량을 분석하였다. 각 시료에 대한 시아니딘-3-글루코사이드의 농도는 시아니딘-3-글루코사이드 표준물질의 농도를 기준으로 면적비로 계산하였으며, 표준물질인 시아니딘-3-글루코사이드는 제냐 프랑스(Genay France)사에서 구입하여 사용하였다. 지질이 제거된 각 계통 오디의 색소 추출물은 고성능 액체크로마토그래피 분석 조건에 따라 시마주 엘씨 시스템(shimadzu LC system)에 주입하여 538㎚에서 분석하였다. 컬럼(column)은 노바-팩 씨18(Nova-Pack C18) (300*3.9㎜)을 사용하였으며, 컬럼의 온도는 35℃를 유지하였다. 이동상으로는 H20:CH3CN:HoAC:H2PO4 = 81.7: 8.4: 8.4: 1.5(V/V)를 사용하였으며, 유량은 1.0㎖/min이 되도록 하였다.Cyanide-3-glucoside, an anthocyanin standard, and a high performance liquid chromatography chromatogram were analyzed to analyze the content of mulberry mulberry. The concentration of cyanidin-3-glucoside for each sample was calculated as the area ratio based on the concentration of the cyanidin-3-glucoside standard, and the standard cyanidin-3-glucoside was purchased from Genay France. Was used. The pigment extract of each of the lipids from which the lipid was removed was injected into the Shimadzu LC system according to high performance liquid chromatography analysis conditions and analyzed at 538 nm. As a column, Nova-Pack C18 (300 * 3.9 mm) was used, and the temperature of the column was maintained at 35 ° C. H20: CH3CN: HoAC: H2PO4 = 81.7: 8.4: 8.4: 1.5 (V / V) was used as the mobile phase, and the flow rate was 1.0 ml / min.
[표 1] 오디 유망 계통의 시아니딘-3-글루코사이드 함량TABLE 1 Cyanidin-3-glucoside content of Audi promising strains
<실시예 3> 오디에서 천연 시아니딘-3-글루코사이드 고함유 최적 추출조건 및 방법 규명Example 3 Identification of Optimal Extraction Conditions and Methods for High Content of Natural Cyanidin-3-glucoside in Audi
오디함유 천연색소 시아니딘-3-글루코사이드의 식용색소화 및 안정생산을 위한 최적 전처리 조건 중 먼저 오디 색소 추출용매를 선정하였다. 시아니딘-3-글루 코사이드 함량 분석에 사용하는 0.5% 염산-메탄올을 대조로 하여, 메탄올, 에탄올(주정) 및 물(증류수)을 이용하여 오디 색소를 추출하여 각 용매의 시아니딘-3-글루코사이드 함량을 분석한 결과, 0.5% 염산-메탄올(건물당 0.533%)> 메탄올(건물당 0.496%)> 에탄올(건물당 0.066%)> 물(건물당 0.006%) 순으로 높았으나, 이중 식용색소로 추출가능한 용매는 에탄올(주정)과 물(증류수)이었다. 그러나 오디 색소 추출물의 시아니딘-3-글루코사이드 함량이 에탄올 추출시 물 추출에 비해 10배 높았으므로 에탄올(주정)을 최적 용매로 선정하였다(도 1 참조). Among the optimal pretreatment conditions for food coloring and stable production of the natural pigment cyanidin-3-glucoside containing audi, an Audi pigment extraction solvent was first selected. With 0.5% hydrochloric acid-methanol used for cyanidin-3-glucoside content analysis as a control, the Audi pigment was extracted using methanol, ethanol (alcohol) and water (distilled water) to obtain cyanidin-3- Glucoside content was analyzed to be 0.5% hydrochloric acid-methanol (0.533% per building)> methanol (0.496% per building)> ethanol (0.066% per building)> water (0.006% per building). The solvents extracted with were ethanol (alcohol) and water (distilled water). However, since the cyanidin-3-glucoside content of the Audi pigment extract was 10 times higher than that of water extraction in ethanol extraction, ethanol (alcohol) was selected as an optimal solvent (see FIG. 1).
다음으로 오디 시아니딘-3-글루코사이드 추출용매로 선정된 에탄올의 최적 농도를 구하기 위해 에탄올의 농도를 10%, 20%, 30%, 50%, 70% 및 95%로 달리하여 오디 시아니딘-3-글루코사이드 함량을 분석하였다. Next, in order to determine the optimal concentration of ethanol selected as the odysyanidin-3-glucoside extractant, the concentration of ethanol was changed to 10%, 20%, 30%, 50%, 70%, and 95% to diocyanidine-3 Glucoside content was analyzed.
[표 2] 추출 용매 에탄올의 농도에 따른 시아니딘-3-글루코사이드 함량 분석Table 2 Analysis of Cyanidin-3-glucoside Content According to Concentration of Extraction Solvent Ethanol
상기 표 2에 의하면, 70% 에탄올로 추출하는 경우 가장 높은 시아니딘-3-글루코사이드 함량을 나타내었다(도 3 참조). According to Table 2, the highest content of cyanidin-3-glucoside when extracted with 70% ethanol (see Figure 3).
일반적으로 안토시아닌 색소는 수용액의 pH에 따라 색이 변하는 불안정한 특성을 갖는다. 즉 산성 용액에서 안정하여 적색을 띠며, 중성 용액에서는 자색(보라색), 염기성 용액에서는 녹색 또는 청색을 띠는 특성이 있으므로, 오디에 함유된 시아니딘-3-글루코사이드를 안정화시키기 위하여 오디 색소 추출 용매에 식품 제조시 널리 이용되는 구연산(citric acid)을 첨가하여 안토시아닌 색소 시아니딘-3-글루코사이드의 함량뿐만 아니라 식품에 대한 안정성 및 색소의 안정성을 증가시키고자 하였다. In general, anthocyanin pigments have unstable characteristics that change color depending on the pH of an aqueous solution. In other words, it is stable in acidic solution, reddish in neutral solution, and purple or violet in basic solution, and green or blue in basic solution. Therefore, it is applied to an audio pigment extraction solvent to stabilize cyanidin-3-glucoside in Audi. Citric acid, which is widely used in food production, was added to increase the content of anthocyanin pigment cyanidin-3-glucoside, as well as stability to food and pigment.
이에 구연산의 기능을 알아보기 위하여 에탄올 농도를 10%, 20%, 30%, 50%, 70%, 95%로 달리하여 각각 구연산 0.1%씩 첨가하여 오디 시아니딘-3-글루코사이드 함량을 분석하였다.In order to determine the function of citric acid, ethanol concentrations of 10%, 20%, 30%, 50%, 70%, and 95%, respectively, were added 0.1% citric acid, respectively, and analyzed the content of odysyanidin-3-glucoside.
[표 3] 구연산 첨가시의 시아니딘-3-글루코사이드 함량 TABLE 3 Cyanidin-3-glucoside content with citric acid addition
상기 표 3에 의하면, 70% 에탄올을 첨가하는 경우까지는 에탄올만 단독으로 추출한 것에 비해 0.1% 구연산을 더 첨가한 경우 오디의 시아니딘-3-글루코사이드의 함량이 증가하여 천연 항산화 색소 시아니딘-3-글루코사이드의 함량뿐만 아니라 식품에 대한 안정성을 증가시키는 것으로 나타났다.According to Table 3, when the amount of 70% ethanol is added, the content of cyanide-3-glucoside of the Audi is increased when 0.1% citric acid is added as compared to ethanol alone. It has been shown to increase the content of glucosides as well as the stability to food.
또한 구연산의 적정 농도를 규명하기 위하여 0.1% 구연산-70% 에탄올과 1% 구연산-80% 에탄올 추출시 오디 시아니딘-3-글루코사이드 함량을 분석하였다.In addition, in order to determine the proper concentration of citric acid, the content of odysyanidin-3-glucoside in 0.1% citric acid-70% ethanol and 1% citric acid-80% ethanol extraction was analyzed.
[표 4] 구연산 농도에 따른 시아니딘-3-글루코사이드 함량[Table 4] Cyanidin-3-glucoside content according to citric acid concentration
상기 표 4에 의하면, 에탄올에 첨가하는 구연산의 농도는 0.1%가 바람직한 것으로 판단하였다.According to Table 4, the concentration of citric acid added to ethanol was determined to be 0.1% preferred.
<실시예 4> 오디 색소의 추출 및 농축Example 4 Extraction and Concentration of Audi Pigments
생오디, 냉동 오디 및 동결건조된 오디를 오디 색소 시아니딘-3-글루코사이드의 최적추출조건인 0.1% 구연산, 70% 에탄올로 추출하여 여과하였다. 오디에 추출용매를 가한 후 손으로 직접 오디를 짓이겨 추출하는 방법과 진탕기(shaking incubator)를 이용하여 4℃에서 24시간 동안 추출하는 방법 사이에는 최종 농축물에 큰 차이가 없는 것으로 나타났다(도 3). Raw audio, frozen audio and lyophilized audio were filtered with 0.1% citric acid, 70% ethanol, which is the optimal extraction condition of the audio pigment cyanidin-3-glucoside. There was no significant difference in the final concentrate between the method of extracting by manually squeezing the audio after adding the extraction solvent to the Audi and the method of extracting at 4 ° C. for 24 hours using a shaking incubator (FIG. 3). ).
상기 추출된 여과액은 대용량 회전진공 농축기를 이용하여 40℃에서 85mbar, 50rpm으로 보다 경제적이며 대량으로 농축물을 분리하였다.The extracted filtrate was separated more economically and in bulk at 85 mbar, 50 rpm at 40 ℃ using a large-volume rotary vacuum concentrator.
<실시예 5><Example 5>
상기 오디 색소의 농축물을 -85℃에서 5mTorr로 48시간 동안 동결건조하여 오디 색소 분말을 제조하였다. 그러나 이 분말은 수분에 대한 흡습성이 높아 보관시 안정성에 대한 문제점이 있었다. 따라서 이 문제점을 해결하기 위하여 갈변에 대한 저항성을 보유하며, 저흡습성으로 수분흡수를 억제시키는 부형제인 덱스트린 또는 말토덱스트린을 농축물:덱스트린(말토덱스트린)= 1:1(무게비)로 첨가한다. 일반적으로 부형제로 사용한 덱스트린(말토덱스트린)은 식품가공분야에 널리 이용되고 있어 그 안정성에 대한 문제는 없으며, 저지방, 저칼로리 식품과 복합 탄수화물 섭취 수준을 향상시키는 기능성 식품소재이다.The concentrate of the Audi pigment was lyophilized for 48 hours at -85 ℃ 5mTorr to prepare an Audi pigment. However, this powder has a problem of stability during storage because of high hygroscopicity to moisture. Therefore, in order to solve this problem, dextrin or maltodextrin, which is an excipient having browning resistance and inhibits water absorption with low hygroscopicity, is added as a concentrate: dextrin (maltodextrin) = 1: 1 (weight ratio). In general, dextrin (maltodextrin) used as an excipient is widely used in the food processing field, there is no problem about its stability, and is a functional food material that improves low fat, low calorie food and complex carbohydrate intake levels.
덱스트린의 첨가 여부에 따른 색소의 선명도를 육안으로 관찰하였다(도 4).The sharpness of the pigment with or without dextrin was observed visually (FIG. 4).
도 4에 의하면 덱스트린을 사용한 경우는 덱스트린을 사용하지 않았을 때에 비해 색소의 선명도가 증가하였다.According to FIG. 4, the sharpness of the pigment was increased in the case of using dextrin, compared with the case of not using dextrin.
본 발명에 의한 오디로부터 유래한 시아니딘-3-글루코사이드 식용색소 분말은 안정적이므로, 적색의 색소를 첨가하여 제조하는 모든 식품에 이용할 수 있으므로 식품산업에 이용할 수 있다. 오디의 기능성과 천연 식용색소의 안정성으로 인해 최근 사용금지 또는 논란이 되고 있는 인공합성색소를 대체할 수 있으므로 소비자의 신뢰도를 높일 수 있다.Since the cyanidin-3-glucoside food coloring powder derived from the Audi of this invention is stable, it can be used for all the foods manufactured by adding a red pigment, and can be used for the food industry. Due to the functionality of Audi and the stability of natural food coloring, it is possible to replace artificial synthetic pigment, which has been banned or controversial recently, thereby increasing consumer confidence.
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| WO2013032087A1 (en) * | 2011-08-30 | 2013-03-07 | 가톨릭대학교 산학협력단 | Pharmaceutical composition including c3g or mulberry extracts containing c3g for preventing or treating diabetic impotence |
| KR101367995B1 (en) * | 2012-01-05 | 2014-02-28 | 대한민국 | Manufacturing method for semi-dried mulberry improved taste and semi-dried mulberry manufactured using the same |
| KR20200091766A (en) | 2019-01-23 | 2020-07-31 | 경상남도 산청군 | Method For Manufacturing Mulberry Powder |
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| KR101438790B1 (en) * | 2011-01-20 | 2014-09-05 | 농업회사법인 주식회사 헬스페이스 | Method for extracting mulberry |
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