KR101859688B1 - A manufacturing method of functional powder comprising abundant rutin ingredient - Google Patents
A manufacturing method of functional powder comprising abundant rutin ingredient Download PDFInfo
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- KR101859688B1 KR101859688B1 KR1020160080822A KR20160080822A KR101859688B1 KR 101859688 B1 KR101859688 B1 KR 101859688B1 KR 1020160080822 A KR1020160080822 A KR 1020160080822A KR 20160080822 A KR20160080822 A KR 20160080822A KR 101859688 B1 KR101859688 B1 KR 101859688B1
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- 239000000843 powder Substances 0.000 title claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 27
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 title claims abstract description 23
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 title claims abstract description 23
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 235000005493 rutin Nutrition 0.000 title claims abstract description 23
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 title claims abstract description 23
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229960004555 rutoside Drugs 0.000 title claims abstract description 23
- 239000004615 ingredient Substances 0.000 title claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 76
- 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 claims abstract description 23
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- 239000011343 solid material Substances 0.000 claims abstract description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 238000000605 extraction Methods 0.000 claims description 15
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- 238000001816 cooling Methods 0.000 claims description 3
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- 235000013305 food Nutrition 0.000 abstract description 11
- 241000255789 Bombyx mori Species 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 4
- 230000036541 health Effects 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 3
- 239000004006 olive oil Substances 0.000 abstract description 2
- 235000008390 olive oil Nutrition 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 20
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- 239000013543 active substance Substances 0.000 description 3
- 235000010208 anthocyanin Nutrition 0.000 description 3
- 229930002877 anthocyanin Natural products 0.000 description 3
- 239000004410 anthocyanin Substances 0.000 description 3
- 150000004636 anthocyanins Chemical class 0.000 description 3
- 229960003692 gamma aminobutyric acid Drugs 0.000 description 3
- BTCSSZJGUNDROE-UHFFFAOYSA-N gamma-aminobutyric acid Chemical compound NCCCC(O)=O BTCSSZJGUNDROE-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
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- 241000251468 Actinopterygii Species 0.000 description 2
- LXBIFEVIBLOUGU-UHFFFAOYSA-N Deoxymannojirimycin Natural products OCC1NCC(O)C(O)C1O LXBIFEVIBLOUGU-UHFFFAOYSA-N 0.000 description 2
- QNVSXXGDAPORNA-UHFFFAOYSA-N Resveratrol Natural products OC1=CC=CC(C=CC=2C=C(O)C(O)=CC=2)=C1 QNVSXXGDAPORNA-UHFFFAOYSA-N 0.000 description 2
- LUKBXSAWLPMMSZ-OWOJBTEDSA-N Trans-resveratrol Chemical compound C1=CC(O)=CC=C1\C=C\C1=CC(O)=CC(O)=C1 LUKBXSAWLPMMSZ-OWOJBTEDSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
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- 240000008067 Cucumis sativus Species 0.000 description 1
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- 206010012689 Diabetic retinopathy Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 description 1
- 239000004472 Lysine Substances 0.000 description 1
- 241000218213 Morus <angiosperm> Species 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 238000002347 injection Methods 0.000 description 1
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- 229910052760 oxygen Inorganic materials 0.000 description 1
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- 230000004304 visual acuity Effects 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 COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/40—Shaping or working of foodstuffs characterised by the products free-flowing powder or instant powder, i.e. powder which is reconstituted rapidly when liquid is added
-
- 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
- A23V2250/20—Natural extracts
- A23V2250/21—Plant extracts
-
- 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
- A23V2250/20—Natural extracts
- A23V2250/21—Plant extracts
- A23V2250/2116—Flavonoids, isoflavones
- A23V2250/2117—Rutin
-
- 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
- A23V2300/00—Processes
- A23V2300/14—Extraction
-
- 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
- A23V2300/00—Processes
- A23V2300/48—Ultrasonic treatment
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Botany (AREA)
- Mycology (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Saccharide Compounds (AREA)
Abstract
본 발명은 루틴 성분을 다량 함유한 기능성 분말의 제조방법에 관한 것이다.
본 발명의 루틴 성분을 다량 함유한 기능성 분말의 제조방법으로는, 오디을 에탄올 및 산에 넣고 추출하여 시아니딘-3-글루코사이드(C3G)가 제거된 고형물을 제조하는 제1단계, 상기 C3G가 제거된 고형물에 에탄올을 넣고 다시 추출한 다음 여과한 후, 걸러져 나온 추출액을 농축한 다음, 물을 넣고 용해하여 용해물을 제조하는 제2단계, 상기 용해물을 1~10℃에서 20~30시간동안 저온 정치한 후, 원심분리하여 침전된 잔사 고형물을 채취하는 제3단계 및, 상기 잔사 고형물을 동결건조하여 루틴성분을 주성분으로 함유한 기능성 분말을 제조하는 제4단계를 포함하는 것이 특징이다.
본 발명에 의해 제조된 루틴(rutin)의 함량이 증진된 기능성 분말을 식품에 적용함으로써 단순 식품에서 벗어나 고부가 제품 및 기능성이 증진된 제품을 개발하여 판매할 수 있으므로 양잠농가 및 가공업체의 소득증대 및 국민의 건강증진에 기여할 수 있게 된다.The present invention relates to a process for producing a functional powder containing a large amount of a routine component.
The method for producing a functional powder containing a large amount of the routine component of the present invention includes a first step of preparing a solid material from which cyanidin-3-glucoside (C3G) has been removed by adding an extract of an olive oil into ethanol and an acid, A second step in which ethanol is added to the solid matter and then extracted again, filtered, and the extracted solution is concentrated, and then water is added to dissolve to produce a dissolved product. The dissolved product is cooled at a temperature of 1 to 10 ° C for 20 to 30 hours A third step of centrifuging and collecting the precipitated residue, and a fourth step of lyophilizing the residue to prepare a functional powder containing a rutin component as a main component.
By applying the functional powder enhanced in the content of rutin produced by the present invention to foods, it is possible to develop and sell products with high value-added products and functionalities that are devoid of simple foods, thereby increasing the income of silkworm farmers and processing companies, And contribute to the health promotion of the people.
Description
본 발명은 루틴 성분을 다량 함유한 기능성 분말의 제조방법에 관한 것으로서, 보다 상세하게는 오디를 이용하여 기능성 성분 중 루틴의 함량이 다량 함유되는 기능성 분말의 제조방법에 관한 것이다.The present invention relates to a process for producing a functional powder containing a large amount of a rutin component, and more particularly, to a process for producing a functional powder containing a large amount of a rutin in a functional ingredient by using an ori.
뽕나무(Morus alba L.)는 누에고치 생산에 필요한 식물일 뿐만 아니라 전통적으로 약제로써 널리 사용되었으며, 뽕잎 뿐만 아니라 뿌리, 어린 가지, 잎의 흰 액즙 및 열매와 같은 부산물이 사용되고 뽕잎, 상백피, 오디의 생리활성에 대한 연구가 꾸준히 진행되고 있다.Mulberry ( Morus alba L. ) is not only a plant necessary for the production of silkworm cucumbers but has also been widely used as a medicament in tradition. It is used not only for mulberry leaves but also byproducts such as roots, young branches, white juice and fruits of leaves and mulberry leaves, Studies on physiological activity have been progressing steadily.
그 중, 오디는 뽕나무과에 속하는 뽕나무 또는 산뽕나무에 열리는 열매로서, 늦은 봄에서 이른 여름 사이에 익기 시작한다. 오디에는 다량의 비타민과 함께 활성산소를 제거하여 노화를 방지한다고 알려진 물질인 안토시아닌과 루틴(Rutin), 가바(GABA), 디엔제이(1-DNJ), 레스베라트롤(Resveratrol) 등 여러 가지 기능성 성분들이 들어있어 건강에 이로운 식품으로 알려져 있거나, 노화억제, 당뇨병성 망막장애의 치료 및 시력개선 효과, 항산화 작용 등 다양한 생리활성을 갖는 것으로 보고됨에 따라 인체에 무해한 기능성 소재로서 각광받고 있다.Among them, Audi is a mulberry tree belonging to the bract family, or a fruit that opens in mountain mulberry trees, and begins to ripen from late spring to early summer. There are many functional ingredients such as anthocyanins, Rutin, GABA, 1-DNJ and Resveratrol, which are substances known to prevent aging by eliminating active oxygen with large amounts of vitamins. Which is known as a food beneficial to health, has been reported to have various physiological activities such as inhibition of aging, treatment of diabetic retinopathy, improvement of visual acuity, and antioxidative action.
현재에는 뽕나무 유래 소재를 이용하여 용매처리별 루틴(rutin), GABA 및 1-DNJ 함량과 생리활성에 대한 연구는 일부 진행되었으나, 이러한 유용성분을 고농도로 추출하기 위한 연구는 제한적으로 이루어졌다. 특히, 기존의 식품소재를 위한 식물 추출방법에는 유용성분을 추출하는 가열, 농축 등의 과정에서 파괴가 발생되거나 식품으로 이용하기에 적합하지 않는 용매를 사용하기 때문에 유용성분의 파괴를 최소화함과 동시에 식용으로도 이용가능 하도록 하는 특정 제조방법에 대한 연구가 필요하다.Currently, studies on rutin, GABA and 1-DNJ contents and physiological activities of solvent treatment using mulberry-derived materials have been conducted, but studies for extracting such useful components at a high concentration have been limited. Particularly, since the plant extract method for existing food materials uses a solvent which is destroyed in the course of heating, concentration and the like for extracting useful components or is not suitable for use as food, the destruction of useful ingredients is minimized There is a need for studies on specific manufacturing methods that are also available for food.
본 발명의 목적은 오디를 이용하여 기능성 성분 중 루틴의 함량이 다량 함유되는 기능성 분말의 제조방법을 제공하는 데에 있다.It is an object of the present invention to provide a process for producing a functional powder in which the content of the rutin in the functional ingredient is large.
본 발명이 이루고자 하는 기술적 과제들은 이상에서 언급한 기술적 과제들로 제한되지 않으며, 언급되지 않은 다른 기술적 과제들은 아래의 기재로부터 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자에게 명확하게 이해될 수 있을 것이다.It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory and are not intended to limit the invention to the particular embodiments that are described. It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory and are not restrictive of the invention, There will be.
상기 목적을 달성하기 위한 본 발명의 루틴 성분을 다량 함유한 기능성 분말의 제조방법은, 오디를 에탄올 및 산에 넣고 추출하여 시아니딘-3-글루코사이드(C3G)가 제거된 고형물을 제조하는 제1단계, 상기 C3G가 제거된 고형물에 에탄올을 넣고 다시 추출한 다음 여과한 후, 걸러져 나온 추출액을 농축한 다음, 물을 넣고 용해하여 용해물을 제조하는 제2단계, 상기 용해물을 1~10℃에서 20~30시간동안 저온 정치한 후, 원심분리하여 침전된 잔사 고형물을 채취하는 제3단계 및, 상기 잔사 고형물을 동결건조하여 루틴성분을 주성분으로 함유한 기능성 분말을 제조하는 제4단계를 포함하는 것이 특징이다.In order to accomplish the above object, the present invention provides a method for producing a functional powder containing a large amount of a routine component, comprising the steps of: preparing a solid material from which cyanidin-3-glucoside (C3G) A second step of adding ethanol to the solid material from which the C3G has been removed and re-extracting the mixture, filtering, concentrating the extracted liquid, and then adding water to dissolve to prepare a lysate; A third step of collecting the precipitated residue by centrifugation after being left at low temperature for 30 hours and a fourth step of lyophilizing the residual solid to prepare a functional powder containing a rutin component as a main component Feature.
상기 제1단계 또는 제2단계의 에탄올은 50~95%(v/v)의 에탄올인 것이 특징이며, 상기 제1단계의 산은 0.1~1.0%(v/v)의 구연산인 것이 특징이다.The ethanol of the first or second step is ethanol of 50 to 95% (v / v), and the acid of the first step is 0.1 to 1.0% (v / v) of citric acid.
상기 제1단계 또는 제2단계에 적용된 추출방법으로 환류냉각추출방식을 적용하되, 80~95℃에서 1~4시간동안 이루어지거나, 상기 제1단계 또는 제2단계에 적용된 초음파추출방식을 적용하되, 60~70℃에서 1~2시간동안 이루어지는 것이 특징이다.The extraction method applied to the first step or the second step may be carried out at 80 to 95 ° C for 1 to 4 hours, or an ultrasonic extraction method applied to the first or second step may be applied. , And at 60 to 70 ° C for 1 to 2 hours.
또한, 상기 제3단계의 원심분리는 4~8℃, 1000~2000g에서 10~30분동안 이루어지며, 상기 제4단계의 동결건조는 35~38℃에서 24~48시간동안 이루어지는 것이 특징이다.The third stage centrifugation is performed at 4 ~ 8 ° C, 1000 ~ 2000g for 10 ~ 30 minutes, and the fourth stage freeze drying is performed at 35 ~ 38 ° C for 24 ~ 48 hours.
본 발명의 루틴 성분을 다량 함유한 기능성 분말은 상기 제조방법에 의해 제조되어, 루틴의 함량은 200~2000 mg/100g인 것이 특징이다.The functional powder containing a large amount of the routine component of the present invention is produced by the above-described production method, and the content of the routine is 200 to 2000 mg / 100 g.
본 발명에 의해 제조된 루틴(rutin)의 함량이 증진된 기능성 분말을 식품에 적용함으로써 단순 식품에서 벗어나 고부가 제품 및 기능성이 증진된 제품을 개발하여 판매할 수 있으므로 양잠농가 및 가공업체의 소득증대 및 국민의 건강증진에 기여할 수 있게 된다.By applying the functional powder enhanced in the content of rutin produced by the present invention to foods, it is possible to develop and sell products with high value-added products and functionalities that are devoid of simple foods, thereby increasing the income of silkworm farmers and processing companies, And contribute to the health promotion of the people.
도 1은 본 발명의 실시예1에 따른 루틴 성분을 다량 함유한 기능성 분말의 제조공정도를 나타낸 도면이다.
BRIEF DESCRIPTION OF DRAWINGS FIG. 1 is a view showing a process for producing a functional powder containing a large amount of a routine component according to Example 1 of the present invention. FIG.
이하, 본 발명을 상세하게 설명하며, 본 발명의 요지를 불필요하게 흐릴 수 있는 공지 기능 및 구성에 대한 상세한 설명은 생략한다.DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, the present invention will be described in detail, and a detailed description of known functions and configurations that may unnecessarily obscure the gist of the present invention will be omitted.
본 발명은 루틴 성분을 다량 함유한 기능성 분말의 제조방법에 관한 것으로서, 보다 상세하게는 루틴성분이 자체 함유되어 있는 오디를 대상하되, 이 루틴 성분을 극대화할 수 있는 특정 제조과정을 거침으로써, 루틴 성분이 다량 함유된 기능성 분말을 제공하는 것이 특징이다. The present invention relates to a process for producing a functional powder containing a large amount of a rutin component, and more particularly, to a process for preparing a functional powder containing a rutin component, It is characterized by providing a functional powder containing a large amount of components.
이를 위하여 오디의 시아니딘-3-글루코사이드(C3G) 색소를 제거한 뒤 이를 식품에 적용가능하도록 에탄올로 추출하므로서, 단순 식품에서 벗어나 고부가 제품 및 기능성이 증진된 제품을 개발하는데 사용할 수 있는 기능성 분말을 제조하는 것을 주요 골자로 한다.For this purpose, the cyanidin-3-glucoside (C3G) pigment of Audi is removed and then extracted with ethanol to be applicable to foods, so that a functional powder which can be used for development of high value-added products and functional products can be manufactured As the main focus.
하기, 본 발명의 루틴 성분을 다량 함유한 기능성 분말의 제조방법을 구체적으로 설명하면 다음과 같다.Hereinafter, a method for producing a functional powder containing a large amount of the routine components of the present invention will be described in detail.
1단계) 시아니딘-3-글루코사이드(C3G)가 제거된 고형물 제조Step 1) Production of solids from which cyanidin-3-glucoside (C3G) has been removed
먼저, 재료로 오디를 준비한다. First, prepare the audi for the material.
오디는 여러 생리활성물질을 함유하고 있다고 알려져 있으며, 그 중 주요 생리활성물질로는 안토시아닌, 레스베라트롤, 루틴, 유리당, 가바 등이 있는 것으로 보고된 바가 있다. Odi is known to contain various physiologically active substances. Among them, the major physiologically active substances are anthocyanin, resveratrol, rutin, free sugar, and GABA.
그 중 시아니딘-3-글루코사이드(C3G) 물질은 안토시아닌 색소의 한 형태로써 단순히 오디를 에탄올로 추출할 경우 상기 C3G 물질까지 함께 추출되어 루틴함량을 최대치로 분리해내는데 어려움이 있다.Among them, cyanidin-3-glucoside (C3G) is a form of anthocyanin pigment, and when oder is simply extracted with ethanol, it is difficult to extract the C3G material together to maximize the content of rutin.
이에, 먼저 추출 전 오디의 시아니딘-3-글루코사이드(C3G)를 제거해야 하며, 이때, 오디에 에탄올 및 산을 넣고 추출하는 방법을 적용하는 것으로써, 상기 추출방법은 등록특허 제10-0842448호인 본 발명의 발명자가 선출원한 “오디로부터 유래한 시아니딘-3-글루코사이드를 식용색소분말로 제조하는 방법”에 공지된 기술을 적용하는 것을 특징으로, 사용된 상기 에탄올은 50~95%(v/v)의 에탄올이며, 상기 산은 0.1~1.0%(v/v)의 구연산인 것이 특징이다.In this case, the cyanidin-3-glucoside (C3G) of the oder before extraction should be removed. In this case, by applying the method of extracting the oily ethanol and the acid, the extraction method is disclosed in Japanese Patent Application No. 10-0842448 Characterized in that the technique known in the " process for preparing cyanidin-3-glucoside from edible fats as edible color powder ", which was filed by the inventor of the present invention, is applied, wherein the ethanol used is 50-95% v) ethanol, and the acid is 0.1 to 1.0% (v / v) citric acid.
2단계) 용해물 제조2) Manufacture of lysine
본 단계에서는 증진된 루틴함량을 분리해 내기 위한 것으로써, 상기 C3G가 제거된 고형물에 에탄올을 넣고 다시 추출한 다음 여과한 후, 걸러져 나온 추출액을 농축한 다음, 물을 넣고 용해하여 용해물을 제조하는 것이 특징이다. In this step, ethanol is added to the solid substance from which the C3G has been removed, and then the mixture is filtered. After concentrating the filtered extract, water is added and dissolved to prepare a lysate .
이 때, 상기 적용된 추출방법으로 환류냉각추출방식을 적용하되, 80~95℃에서 1~4시간동안 이루어지거나, 상기 초음파추출방식을 적용하되, 60~70℃에서 1~2시간동안 이루어지는 것을 특징으로, 상기 온도 및 시간을 벗어날 경우에는 루틴함량이 충분히 추출되지 않거나, 오히려 성분파괴로 인해 본 발명이 목적하는 효과를 이루기 어렵게 된다.At this time, the reflux cooling extraction method is applied as the above extraction method, and it is performed at 80 to 95 ° C for 1 to 4 hours or at 60 to 70 ° C for 1 to 2 hours using the ultrasonic extraction method If the temperature and the time are out of the range, the rutin content is not sufficiently extracted, or rather, the desired effect of the present invention is not achieved due to the component breakage.
특히, 상기 에탄올의 종류로는 50~95%(v/v)의 에탄올을 사용하는 것으로써, 이는 50%(v/v) 미만이 에탄올을 사용할 경우 에탄올의 농도가 너무 낮아 루틴함량이 충분이 추출되지 않게 되며, 95%(v/v) 초과의 에탄올을 사용할 경우, 오히려 과도한 에탄올의 농도로 인해 루틴 성분이 파괴되는 문제가 발생된다.Particularly, the use of 50 to 95% (v / v) ethanol as the ethanol is less than 50% (v / v). When ethanol is used, the concentration of ethanol is too low, If the ethanol is used in an amount exceeding 95% (v / v), the concentration of excess ethanol may cause the problem that the routine component is destroyed.
이렇게 추출된 상기 에탄올 추출물은 식용가능한 식품의 소재로 적용하기 위해서는 반드시 농축과정을 통해 에탄올 성분을 제거하고, 남은 잔사고형물을 물에 용해시킴으로 인해 식품의 소재로의 이용가치를 높여주게 된다.In order to apply the extracted ethanol extract as a foodable food material, the ethanol component is necessarily removed through a concentration process, and the residual solids are dissolved in water, thereby increasing the value of the product as a food ingredient.
3단계) 잔사 고형물 채취Step 3) Collection of residue solid
본 단계에서는 상기 2단계에서 제조된 용해물을 1~10℃에서 20~30시간동안 저온 정치한 후, 원심분리하여 침전된 잔사 고형물을 채취한다. In this step, the liquor prepared in step 2 is allowed to stand at 1 to 10 ° C for 20 to 30 hours, and centrifuged to collect the precipitated residue.
이때, 상기 원심분리는 4~8℃, 1000~2000g에서 10~30분동안 이루어지는 것을 특징으로, 상기 조건을 벗어날 경우 고형물이 완전히 분리되지 않거나 원심분리과정으로 인해 오히려 성분파괴 될 우려가 있는 바, 상기 원심분리 조건은 기능성 분말 제조에 있어 생리활성물질의 손실을 최대한 방지하는 필수 조건이다.At this time, the centrifugation is performed at 4 to 8 ° C. and 1000 to 2000 g for 10 to 30 minutes. If the condition is exceeded, the solids may not be completely separated or the components may be destroyed due to the centrifugation process. The centrifugation conditions are a necessary condition to prevent the loss of physiologically active substances in the production of functional powder as much as possible.
4단계) 루틴성분을 주성분으로 함유한 기능성 분말 제조Step 4) Preparation of a functional powder containing a main component of a routine component
본 단계에서는 상기 잔사 고형물을 동결건조하여 루틴성분을 주성분으로 함유한 기능성 분말을 제조한다. In this step, the residue solid is lyophilized to produce a functional powder containing a rutin component as a main component.
이때, 상기 동결건조는 35~38℃에서 24~48시간동안 이루어지는 것이 특징으로, 이 또한, 생리활성물질의 손실을 최대한 방지하는 필수 조건인 것으로써, 상기 건조조건을 벗어날 경우 완전히 분말형태로 이루지 않게 되어 보관시 부패가 진행될 우려가 있게 되거나, 과건조로 인해 루틴 성분의 함량이 손실될 우려가 있게 된다.At this time, the freeze-drying is performed at 35 to 38 ° C for 24 to 48 hours. This is also an essential condition for preventing the loss of the physiologically active material to the utmost, so that when the drying condition is exceeded, There is a possibility that corruption may proceed during storage, or the content of the routine component may be lost due to overdrying.
이렇게 제조된 상기 기능성 분말은 오디 유래로 제조할 경우 루틴의 함량은 200~2000 mg/100g인 것이 특징으로, 이는 기존 오디 에탄올 추출물 대비 월등히 높은 루틴함량을 함유하고 있는 것인 바, 이를 통해 단순 식품소재에서 벗어나 고부가 제품 및 기능성이 증진된 제품을 개발하여 판매할 수 있는 기능성 소재로써의 이용가치가 있게 된다.The functional powder thus prepared is characterized in that the content of rutin is 200 to 2000 mg / 100 g when it is prepared from an audi, and it contains a much higher routine content than the conventional ODI ethanol extract, It is worth using as a functional material which can develop and sell a product with high value added and functionality that is out of the material.
이하에서는 실시예를 들어 본 발명에 관하여 더욱 상세하게 설명할 것이나, 이들 실시예는 단지 설명의 목적을 위한 것으로 본 발명의 보호 범위를 제한하고자 하는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to examples, but these examples are for illustrative purposes only and are not intended to limit the scope of protection of the present invention.
<< 실시예Example 1. 루틴 성분을 다량 함유한 기능성 1. Functionalities containing a large amount of a routine component 분말1Powder 1 제조> Manufacturing>
생오디 1kg에 70%(v/v)의 에탄올 2,000 ㎖와 0.1(v/v)의 구연산 2g을 넣고 진탕기(shaking incubator)를 이용하여 4℃에서 24시간동안 추출하였다.2,000 ml of 70% (v / v) ethanol and 2 g of 0.1 (v / v) citric acid were added to 1 kg of raw fish and extracted at 4 ° C for 24 hours using a shaking incubator.
이때, 제조된 추출액에 시아니딘-3-글루코사이드(C3G)성분이 포함된 상태로 추출되는 바, 이 추출액은 제거하고 남은 고형물을 획득하였다.At this time, the extract was extracted with the cyanidin-3-glucoside (C3G) component contained therein, and the extract was removed to obtain the remaining solid.
이렇게 C3G가 제거된 고형물에 다시 70%(v/v)의 에탄올 10,000 ㎖을 넣고 환류냉각추출방식을 적용하여 90℃에서 3시간동안 추출하였다.Then, 10,000 ml of 70% (v / v) ethanol was added to the C3G-free solids, and the mixture was subjected to extraction under reflux cooling at 90 ° C for 3 hours.
여기서 생성된 추출물을 여과처리하여 고형물은 제거하고 걸러져 나온 액상상태의 추출액만을 농축하여 농축물을 제조하였다.The extract thus formed was filtered to remove solids, and concentrated solids of the filtered liquid extract were concentrated.
제조된 농축물 380g에 물 3800㎖을 넣고 완전히 용해될 때까지 섞어 용해물을 제조하였다.3800 ml of water was added to 380 g of the prepared concentrate and mixed until completely dissolved to prepare a melt.
상기 용해물을 4℃에서 25시간동안 저온 정치한 후, 4℃, 2000g조건하에 20분동안 원심분리하여 침전된 잔사 고형물을 채취하였다. The lysate was allowed to stand at 4 캜 for 25 hours, and then centrifuged at 4 캜 and 2000 g for 20 minutes to collect precipitated solids.
이렇게 채취된 상기 잔사 고형물은 85℃에서 5mTorr의 압력으로 48시간동안 동결건조하여 본 발명인 루틴성분을 다량 함유한 기능성 분말1을 제조하였다.The residue solid thus obtained was lyophilized at 85 캜 for 48 hours at a pressure of 5 mTorr to prepare Functional Powder 1 containing a large amount of the routine component of the present invention.
<< 비교예Comparative Example 1. 오디 유래 기능성 1. Functionality derived from audi 분말1Powder 1 제조> Manufacturing>
상기 실시예 1과 같은 방법으로 제조하되, 상기 에탄올 대신 물을 이용하여 기능성 분말1을 제조하였다. The functional powder 1 was prepared in the same manner as in Example 1 except that water was used instead of ethanol.
<< 비교예Comparative Example 2. 오디 유래 기능성 2. Functionality derived from audi 분말2Powder 2 제조> Manufacturing>
상기 실시예 1과 같은 방법으로 제조하되, 상기 70%(v/v)의 에탄올 대신40%(v/v)의 에탄올을 이용하여 기능성 분말2를 제조하였다. (V / v) ethanol was used instead of 70% (v / v) ethanol to prepare Functional Powder 2.
<< 비교예Comparative Example 3. 오디 유래 기능성 3. Audi-derived functionality 분말3Powder 3 제조> Manufacturing>
상기 실시예 1과 같은 방법으로 제조하되, 상기 70%(v/v)의 에탄올 대신100%(v/v)의 에탄올을 이용하여 기능성 분말3을 제조하였다. (V / v) ethanol was used instead of the 70% (v / v) ethanol to prepare a functional powder 3.
<< 비교예Comparative Example 4. 오디 유래 기능성 4. Functionality from Audi 분말4Powder 4 제조> Manufacturing>
상기 실시예 1과 같은 방법으로 제조하되, 상기 구연산은 넣지 않고 기능성 분말4를 제조하였다. The functional powder 4 was prepared in the same manner as in Example 1 except that citric acid was not added.
<< 비교예Comparative Example 5. 오디 유래 기능성 5. Functionality from Audi 분말5Powder 5 제조-통상의 추출방식-에탄올 3회 추출> Manufacturing - Conventional extraction method - Ethanol three times extraction>
상기 비교예 4와 같은 방법으로 제조하되, 에탄올 추출과정을 1회 더 하여 총 3회의 에탄올 추출과정을 거쳐 기능성 분말5를 제조하였다. The process of Comparative Example 4 was repeated except that the ethanol extraction process was performed one time to perform a total of 3 times of ethanol extraction to prepare a functional powder 5.
<< 비교예Comparative Example 6. 오디 유래 기능성 6. Functionality from Audi 분말6Powder 6 제조-에탄올 1회 추출: 4℃> Manufacturing -Ethanol Extraction: 4 ° C>
생오디 1kg에 70%(v/v)의 에탄올 2,000㎖을 넣고 진탕기(shaking incubator)를 이용하여 4℃에서 30시간동안 추출하였다.2,000 ml of 70% (v / v) ethanol was added to 1 kg of raw fish and extracted at 4 ° C for 30 hours using a shaking incubator.
여기서 생성된 추출물을 여과처리하여 고형물은 제거하고 걸러져 나온 액상상태의 추출액만을 농축하여 농축물을 제조하였다.The extract thus formed was filtered to remove solids, and concentrated solids of the filtered liquid extract were concentrated.
제조된 농축물 53g에 물 530㎖을 넣고 완전히 용해될 때까지 섞어 용해물을 제조하였다.530 ml of water was added to 53 g of the prepared concentrate and mixed until completely dissolved to prepare a melt.
상기 용해물을 4℃에서 25시간동안 저온 정치한 후, 4℃, 2000g조건하에 20분동안 원심분리하여 침전된 잔사 고형물을 채취하였다. The lysate was allowed to stand at 4 캜 for 25 hours, and then centrifuged at 4 캜 and 2000 g for 20 minutes to collect precipitated solids.
이렇게 채취된 상기 잔사 고형물은 85℃에서 5mTorr의 압력으로 48시간동안 동결건조하여 기능성 분말5를 제조하였다.The residue solid thus obtained was lyophilized at 85 캜 for 48 hours at a pressure of 5 mTorr to prepare a functional powder 5.
<< 비교예Comparative Example 7. 오디 유래 기능성 7. Audi-derived functionality 분말7Powder 7 제조-에탄올 1회 추출: 90℃> Manufacturing - Ethanol 1 time extraction: 90 ° C>
상기 비교예 7과 같은 방법으로 제조하되, 4℃ 아닌 90℃에서 추출하여 기능성 분말7을 제조하였다.The functional powder 7 was prepared in the same manner as in Comparative Example 7 except that it was extracted at 90 ° C, not 4 ° C.
<< 실험예Experimental Example 1. 루틴 성분 확인> 1. Identify Routine Components>
1. 실험방법1. Experimental Method
처리별 뽕나무 오디의 rutin 함량 분석은 Waters Nova-Pak C18 column(300×3.9 ㎜)을 사용하여 HPLC로 분석하였다. 검출기는 Waters 486 Tunable Absorbance Detector를 사용하였으며, 파장은 355 ㎚에서 실시하였다. 이동상으로는 2.5％ acetic acid : methanol : acetonitrile = 70 : 10 : 20 (V:V:V)의 혼합용매를 사용하였으며, flow rate는 0.6 ㎖/min이 되도록 하였다. HPLC 분석용 시료의 주입량은 20 ㎕이 되도록 하였으며, 표준품은 Sigma 社의 것을 사용하였다.The rutin content of the mulberry seeds was analyzed by HPLC using a Waters Nova-Pak C18 column (300 × 3.9 mm). The detector was a Waters 486 Tunable Absorbance Detector and the wavelength was 355 ㎚. As a mobile phase, a mixed solvent of 2.5% acetic acid: methanol: acetonitrile = 70: 10: 20 (V: V: V) was used and the flow rate was 0.6 ml / min. The injection amount of the sample for HPLC analysis was set to 20 μl, and the standard product was purchased from Sigma.
2. 실험결과2. Experimental results
상기 실험결과 하기 표 1과 같이 나타났다.The results of the experiment are shown in Table 1 below.
상기 표 1에 나타나 있듯이, 비교예 1인 오디 유래 물 추출물에서는 루틴 성분이 166 mg/100g 인 반면, 같은 조건에서 에탄올로 추출한 본 발명인 실시예의 경우에는 그 성분이 약 3배 정도 증가됨을 알 수 있었다. As shown in Table 1, in the case of the extract according to the present invention obtained by extracting ethanol with the same conditions, the component of the extract was increased about 3 times .
또한, 오디를 대상으로 CG3를 제거하더라도 에탄올의 농도에 따라 루틴 성분이 다르게 나타나는 바, 비교예 2인 40%의 에탄올을 사용할 경우 98mg/100g으로 나타나며, 비교예 3인 100%의 에탄올을 사용할 경우에는 405mg/100g을 나타내는 바, 본 발명의 제조방법을 적용하더라도 적용되는 에탄올의 농도는 50~95%가 가장 적합함을 알 수 있었다. In addition, even when CG3 was removed from the sample of ODI, the routine components were different depending on the concentration of ethanol. In the case of using 40% ethanol as the comparative example 2, 98 mg / 100 g was used. When 100% ethanol as the comparative example 3 was used And 405 mg / 100 g in the case of applying the manufacturing method of the present invention, it is found that the concentration of ethanol applied is most preferably 50 to 95%.
또한, 비교예 4의 경우에는 구연산을 적용하지 않은 것인 바, 충분히 C3G 성분을 제거하지 못할 경우에 루틴 성분이 충분히 추출되지 못함을 확인하였다.In addition, in the case of Comparative Example 4, citric acid was not applied, and it was confirmed that the routine component could not be extracted sufficiently when the C3G component could not be sufficiently removed.
비교예 5의 경우에는 통상의 에탄올 추출방식으로써 수율을 높이기 위해 일반적으로 3회 추출 방식을 많이 적용하는 데, 이 또한, 루틴 성분이 300mg/100g으로 그 함량이 본 발명보다 낮게 나타나 추출횟수를 증가한다고 무조건 루틴성분이 많이 추출되는 것이 아님을 알 수 있다. In the case of Comparative Example 5, in order to increase the yield by the usual ethanol extraction method, a three-time extraction method is generally applied. In addition, the content of the routine component is 300 mg / 100 g, which is lower than that of the present invention, It can be seen that a lot of the routine components are not extracted.
이와 같이, 본 발명의 제조방법은 오디에서부터 루틴함량을 최대치로 추출해내기 위한 필수과정이며, 이 제조방법을 통해 제조된 기능성 분말의 경우 루틴의 함량이 가장 많이 함유하고 있는 바, 이 기능성 분말을 식품에 적용함으로써 단순 식품에서 벗어나 고부가 제품 및 기능성이 증진된 제품을 개발하여 판매할 수 있으므로 양잠농가 및 가공업체의 소득증대 및 국민의 건강증진에 기여할 수 있게 됨을 알 수 있다.As described above, the production method of the present invention is an essential process for extracting the maximum amount of the rutin content from Audi. The functional powder prepared through this production method contains the largest amount of the rutin, , It is possible to develop and sell high value added products and products with enhanced functionality, thereby contributing to the income increase of the silkworm farmers and processing companies and the health promotion of the people.
상기의 본 발명은 바람직한 실시예를 중심으로 살펴보았으며, 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자는 본 발명의 본질적 기술 범위 내에서 상기 본 발명의 상세한 설명과 다른 형태의 실시예들을 구현할 수 있을 것이다. 여기서 본 발명의 본질적 기술범위는 특허청구범위에 나타나 있으며, 그와 동등한 범위 내에 있는 모든 차이점은 본 발명에 포함된 것으로 해석되어야 할 것이다.It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the invention as defined by the appended claims. It will be possible. The scope of the present invention is defined by the appended claims, and all differences within the scope of the claims are to be construed as being included in the present invention.
Claims (9)
상기 C3G가 제거된 고형물에 50~95%(v/v)의 에탄올을 넣고 다시 추출한 다음 여과한 후, 걸러져 나온 추출액을 농축한 다음, 물을 넣고 용해하여 용해물을 제조하는 제2단계;
상기 용해물을 1~10℃에서 20~30시간동안 저온 정치한 후, 4~8℃, 1000~2000g에서 10~30분동안 원심분리하여 침전된 잔사 고형물을 채취하는 제3단계 및,
상기 잔사 고형물을 35~38℃에서 24~48시간동안 동결건조하여 오디 유래 루틴의 함량이 200~2000 mg/100g으로 함유하여 기존 오디 에탄올 추출물 대비 높은 루틴함량을 함유하는 기능성 분말을 제조하는 제4단계;를 포함하는,
루틴 성분을 다량 함유한 기능성 분말의 제조방법.
A first step of preparing cyanidin-3-glucoside (C3G) -solid solid by extracting ODI in 50 to 95% (v / v) ethanol and 0.1 to 1.0% (v / v) citric acid;
A second step of adding 50 to 95% (v / v) of ethanol to the solid material from which the C3G has been removed, reextracting it, filtering, concentrating the filtered extract, adding water and dissolving the ethanol to prepare a lysate;
A third step of allowing the solute to stand at a temperature of 1 to 10 ° C for 20 to 30 hours and then centrifuging at 4 to 8 ° C and 1000 to 2000 g for 10 to 30 minutes to collect the precipitated solids;
The residue solid was lyophilized at 35 to 38 ° C for 24 to 48 hours to prepare a functional powder containing a higher rutin content than that of the conventional ODI ethanol extract, containing rutin-derived rutin content of 200 to 2000 mg / Comprising:
A method for producing a functional powder containing a large amount of a routine component.
상기 제1단계 또는 제2단계에 적용된 추출방법으로 환류냉각추출방식을 적용하되, 80~95℃에서 1~4시간동안 이루어지는 것을 특징으로 하는,
루틴 성분을 다량 함유한 기능성 분말의 제조방법.
The method according to claim 1,
Wherein the extraction method applied to the first step or the second step is a reflux cooling extraction method and is performed at 80 to 95 ° C for 1 to 4 hours.
A method for producing a functional powder containing a large amount of a routine component.
상기 제1단계 또는 제2단계에 적용된 초음파추출방식을 적용하되, 60~70℃에서 1~2시간동안 이루어지는 것을 특징으로 하는,
루틴 성분을 다량 함유한 기능성 분말의 제조방법,
The method according to claim 1,
Wherein the ultrasonic extraction method applied to the first step or the second step is applied at 60 to 70 ° C for 1 to 2 hours.
A process for producing a functional powder containing a large amount of a routine component,
오디 유래 루틴의 함량이 200~2000 mg/100g인 것을 특징으로 기존 오디 에탄올 추출물 대비 높은 루틴함량을 함유하는 것이 특징인,
루틴 성분을 다량 함유한 기능성 분말.
5. A process for producing a polyimide precursor which is produced by the production method of any one of claims 1, 4 and 5,
And the content of rou- tine derived from the roots is 200 to 2000 mg / 100 g.
Functional powder containing a large amount of a routine ingredient.
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