KR20020000660A - Pigment extraction of chlorophyll and carotenoid from seaweed, crustacea and echinoderm using supercritical and subcritical CO2 with entrainer - Google Patents
Pigment extraction of chlorophyll and carotenoid from seaweed, crustacea and echinoderm using supercritical and subcritical CO2 with entrainer Download PDFInfo
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- KR20020000660A KR20020000660A KR1020000035638A KR20000035638A KR20020000660A KR 20020000660 A KR20020000660 A KR 20020000660A KR 1020000035638 A KR1020000035638 A KR 1020000035638A KR 20000035638 A KR20000035638 A KR 20000035638A KR 20020000660 A KR20020000660 A KR 20020000660A
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- chlorophyll
- supercritical
- carotenoid
- seaweeds
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- 239000000049 pigment Substances 0.000 title claims abstract description 25
- 241001474374 Blennius Species 0.000 title claims abstract description 24
- 229930002875 chlorophyll Natural products 0.000 title claims abstract description 15
- 235000019804 chlorophyll Nutrition 0.000 title claims abstract description 15
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 title claims abstract description 15
- 238000000605 extraction Methods 0.000 title claims abstract description 14
- 241000238424 Crustacea Species 0.000 title claims abstract description 12
- 235000021466 carotenoid Nutrition 0.000 title claims abstract description 12
- 150000001747 carotenoids Chemical class 0.000 title claims abstract description 12
- 241000258955 Echinodermata Species 0.000 title claims abstract description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical class O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 24
- 241000238557 Decapoda Species 0.000 claims abstract description 20
- 241000257465 Echinoidea Species 0.000 claims abstract description 17
- 241000258957 Asteroidea Species 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 239000001569 carbon dioxide Substances 0.000 claims description 20
- 239000006184 cosolvent Substances 0.000 claims description 7
- 239000006227 byproduct Substances 0.000 abstract description 11
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 241000251571 Ciona intestinalis Species 0.000 abstract 2
- 239000000470 constituent Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 241000251468 Actinopterygii Species 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 241000195493 Cryptophyta Species 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920001661 Chitosan Polymers 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 241000251555 Tunicata Species 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000000783 alginic acid Substances 0.000 description 1
- 229920000615 alginic acid Polymers 0.000 description 1
- 229960001126 alginic acid Drugs 0.000 description 1
- 235000010443 alginic acid Nutrition 0.000 description 1
- 150000004781 alginic acids Chemical class 0.000 description 1
- 230000003466 anti-cipated effect Effects 0.000 description 1
- 239000002537 cosmetic Substances 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
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 238000007602 hot air drying Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 235000014102 seafood Nutrition 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 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
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
Classifications
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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
- 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
-
- 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
- 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
- A23L5/44—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 using carotenoids or xanthophylls
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K35/00—Medicinal preparations containing materials or reaction products thereof with undetermined constitution
- A61K35/56—Materials from animals other than mammals
- A61K35/612—Crustaceans, e.g. crabs, lobsters, shrimps, krill or crayfish; Barnacles
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K35/00—Medicinal preparations containing materials or reaction products thereof with undetermined constitution
- A61K35/56—Materials from animals other than mammals
- A61K35/616—Echinodermata, e.g. starfish, sea cucumbers or sea urchins
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/02—Algae
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0403—Solvent extraction of solutions which are liquid with a supercritical fluid
- B01D11/0411—Solvent extraction of solutions which are liquid with a supercritical fluid the supercritical fluid acting as solvent for the solvent and as anti-solvent for the solute, e.g. formation of particles from solutions
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- 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
- A23V2200/00—Function of food ingredients
- A23V2200/04—Colour
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- 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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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Abstract
Description
일반적으로 해조류 및 수산가공부산물이라 함은 해조류를 채취하여 자연건조, 열풍건조, 냉풍건조 등의 방법을 통하여 가식부분을 상품화하고 남은 잔사물질 즉, 폐기되는 부분을 일컸는다. 그러나 이 페기되는 해조류 및 수산가공부산물에는 알긴산, 토코페롤, 지방산, 색소, 키토산 등의 활용 가능한 성분이 다량 함유되어 있어서 활용에 따라서는 매우 다양하게 이용될 수 있다. 그럼에도 불구하고 해조류 및 수산가공부산물은 다른 식품소재 또는 기타 산업에 소재로서 사용이 활발하지못하다. 그 이유는 해조류 및 수산가공 부산물의 활용 가능한 성분에 대한 인식도의 저하와 해조류 및 수산가공품의 이용 범위의 제한성, 생산시기의 제한성 때문이다. 한편 기존에 알려진 추출 방법인 유기용매 추출 법을 이용하여 유용성분들을 추출할 경우 불순물의 혼입이 많고 유해물질인 용매의 회수가 불가능함으로 제품의 품질에 대한 문제가 야기되고 있으며 몇 단계의 공정을 거치므로 공정이 복잡할 뿐 아니라 유용한 성분도 유실될 수가 있으며 화학약품에 의한 이물질의 혼입도 있을 수 있다. 이러한 문제점을 보완하기 위해 초임계 및 아임계 이산화탄소(CO2)와 보조용매를 이용하여 해조류 및 수산가공부산물로부터 클로로필 및 카로티노이드 색소 성분을 추출하기 위한 연구를 시도하여 본 발명에서 해조류 및 수산가공 부산물로부터 천연 색소를 얻을 수가 있었다.In general, seaweeds and fish processing by-products are used to collect the seaweed and commercialize the decorated part through natural drying, hot air drying, and cold air drying, and the remaining residues, that is, discarded parts. However, these discarded seaweeds and fish processing by-products contain a large amount of usable ingredients such as alginic acid, tocopherol, fatty acids, pigments, chitosan and the like, and can be used in various ways depending on the application. Nevertheless, seaweed and fish processing by-products are not actively used as materials in other food materials or other industries. The reason for this is the decrease in awareness of the available components of seaweed and fish processing by-products, the limitation of the use range of the seaweed and seafood processing products, and the timing of production. On the other hand, when useful components are extracted by using organic solvent extraction method, which is a known extraction method, there are many impurities, and it is impossible to recover harmful solvents. Therefore, not only is the process complicated, but also useful components may be lost and foreign substances may be mixed by chemicals. In order to solve this problem, a study for extracting chlorophyll and carotenoid pigment components from seaweeds and fishery by-products using supercritical and subcritical carbon dioxide (CO2) and cosolvents has been attempted. I could get a pigment.
이에 본 발명에서는 액상 및 분말상의 해조류와 수산 가공 부산물을 초임계 및 아임계 이산화탄소(CO2) 반응기에 넣고 압력, 온도 및 이산화탄소(CO2)와 보조용매의 유량을 조절하여 해조류 및 갑각류(게, 새우), 극피동물(유령멍게, 불가사리, 성게 등)로부터 클로로필 및 카로티노이드 색소를 추출하는 것이다. 본 발명은 기존에 알려진 열수 추출법과 중성염 추출 법이 용매의 회수에 대한 어려움이 따른다는 것과 그 외의 다른 용매 추출 법 또한 얻고자하는 순도의 제품 및 용매회수를 높이기 어려운 단점이 있는데 초임계 및 아임계 추출 법은 여러 단계의 공정을 거치지 않을 뿐 아니라, 원료의 상태를 유지하면서 효과적으로 색소를 추출하는 공정이기에 유용성분의 유실을 막을 수가 있는 장점을 가지고 있다. 초임계 및 아임계 이산화탄소(CO2)를 이용한 분리공정은 천연물질로부터 유용한 성분을 선택적으로 추출함으로서 기존의 재래식 추출 방법에서 야기되는 어려움을 해결할 수 있으므로 해조류 및 갑각류(게, 새우), 극피동물(유령멍게, 불가사리, 성게 등)로부터 색소 성분을 회수하여 식품 및 첨가물 산업분야에 적극 활용할 수 있을 것으로 예상된다.Therefore, in the present invention, the liquid and powdery seaweeds and fishery by-products are put in supercritical and subcritical carbon dioxide (CO2) reactors, and the pressure, temperature, and the flow rate of carbon dioxide (CO2) and the cosolvent are adjusted to control algae and crustaceans (crabs and shrimps). , Chlorophyll and carotenoid pigments are extracted from eukaryotic animals (ghost sea urchins, starfish, sea urchins, etc.). The present invention has the disadvantages that the known hot water extraction method and neutral salt extraction method has difficulty in recovering the solvent and other solvent extraction methods also have difficulty in increasing the purity of the product and solvent recovery to obtain. The critical extraction method does not go through several steps but also has the advantage of preventing the loss of useful components because it is a process of effectively extracting the pigment while maintaining the state of the raw material. Separation process using supercritical and subcritical carbon dioxide (CO2) solves the difficulties caused by conventional extraction methods by selectively extracting useful components from natural substances, so seaweeds, crustaceans (crabs, shrimps) and echinoderm (ghosts) It is expected to recover the pigment components from sea squirts, starfish, sea urchins, etc., and to utilize them in the food and additive industries.
이하 본 발명을 상세히 설명하면 다음과 같다. 본 발명은 액상 및 분말상인 해조류 및 갑각류(게, 새우), 극피동물(유령멍게, 불가사리, 성게 등)로부터 초임계 및 아임계 이산화탄소(CO2)와 보조용매를 이용한 클로로필 및 카로티노이드 색소 추출 방법에 관한 것이다. 본 발명에 따르면 액상 및 분말상의 해조류 및 갑각류(게, 새우), 극피동물(유령멍게, 불가사리, 성게 등)를 초임계 및 아임계 반응기에 투입한 후, 일정한 압력(50-500bar)으로 이산화탄소(CO2)를 통과시키면서 보조용매를 일정량[1-70%(v/v)]사용하여, 색소성분인 클로로필(Chlorophyll)과 카로티노이드-(Carotenoid)를 추출하는 것이다. 본 발명에서는 이산화탄소(CO2)를 추출용매로, 에탄올을 보조용매로 사용하였는데, 이산화탄소(CO2)는 추출 종료 후 곧 바로 휘발되기 때문에 제품 중에 잔존하지 않는 것이 용매로서의 큰 장점이며, 에탄올은 일반적인 방법으로 쉽게 제거할 수가 있다.이하 실시 예를 통하여 본 발명을 구체적으로 설명하고자하나, 다음의 실시 예에 의하여 본 발명이 한정되는 것은 아니다.Hereinafter, the present invention will be described in detail. The present invention relates to a chlorophyll and carotenoid pigment extraction method using supercritical and subcritical carbon dioxide (CO2) and co-solvent from liquid and powdered seaweeds and crustaceans (crabs, shrimps), echinoderm (ghost sea urchins, starfish, sea urchins, etc.) will be. According to the present invention, liquid and powdered seaweeds and crustaceans (crabs, shrimps), echinoderm (ghost sea urchins, starfish, sea urchins, etc.) are introduced into supercritical and subcritical reactors, and then, at a constant pressure (50-500 bar), carbon dioxide ( CO2) is used to extract chlorophyll and carotenoids (Carotenoid), which are pigments, by using a certain amount of co-solvent [1-70% (v / v)]. In the present invention, carbon dioxide (CO2) was used as an extraction solvent and ethanol as a co-solvent, but since carbon dioxide (CO2) is volatilized immediately after the end of extraction, it does not remain in the product, which is a great advantage as a solvent, and ethanol is a general method. Although the present invention will be described in detail with reference to the following examples, the present invention is not limited to the following examples.
실시 예 >Example>
기장 소재 해조류 가공회사로부터 제공받은 해조류 가공 부산물을 수분함량 10% 이하로 건조하여 초임계 추출기(국내제작, 일신엔지니어링) 반응기내에 30g을 넣고 이하의 방법으로 해조류 가공부산물 중에 잔존하는 클로로필 색소를 추출하였다. 클로로필 색소의 추출 조건은 반응기 내의 온도가 30-45℃, 압력이 1500-2500psi 였다. 이때 클로로필 색소의 추출 및 이취 성분을 효과적이고 신속하게 제거하기 위하여 보조용매를 1-5ml/min으로 조정하였다. 이와 같은 조건으로 처리된 해조류 가공 부산물은 이취가 없는 원형 그대로를 유지하고 있었다.The seaweed processing by-products provided by Gijang-based seaweed processing company were dried to 10% or less of water, and 30 g of the supercritical extractor (domestic production, Ilshin Engineering) reactor was put into the reactor to extract the remaining chlorophyll pigments from the seaweed processing by-products as follows. . The extraction conditions of the chlorophyll pigment | dye were 30-45 degreeC and pressure 1500-1500psi in the reactor. At this time, the co-solvent was adjusted to 1-5ml / min to effectively and quickly remove the chlorophyll pigment extraction and off-flavor components. Seaweed processing by-products treated under these conditions remained intact without odor.
도면 1은 초임계 이산화탄소를 이용하여 클로로필 색소를 추출하여 UV 스펙트럼으로 분석한 결과를 나타내었다. 이때 분석의 조건은 다음과 같다.Figure 1 shows the results of chlorophyll pigment extraction by using a supercritical carbon dioxide analysis by UV spectrum. The conditions of the analysis are as follows.
UV-spectrophotometer 분석조건UV-spectrophotometer analysis conditions
전술한 바와 같이 본 발명의 방법으로 제조한 해조류 및 갑각류(게, 새우), 극피동물(유령멍게, 불가사리, 성게 등)의 천연 색소는 그 활용도가 매우 높을 것으로 판단된다. 해조류 및 갑각류(게, 새우), 극피동물(유령멍게, 불가사리, 성게 등)로부터 추출한 천연 색소를 화장품 또는 기타 제품에 첨가제로 사용하거나 식품에 천연 색소를 첨가하여 그 제품의 상품성을 높일 수가 있을 것으로 예상되며 해조류 가공 부산물에서 색소와 같이 추출된 해조 추출물도 첨가제로서 사용될 것으로 생각된다.As described above, natural pigments of algae and crustaceans (crabs, shrimps) and echinoderms (ghost sea urchins, starfish, sea urchins, etc.) prepared by the method of the present invention are considered to have high utility. Natural pigments extracted from seaweeds, crustaceans (crabs, shrimps) and echinoderms (ghost sea urchins, starfish, sea urchins, etc.) may be used as additives in cosmetics or other products, or natural pigments may be added to foods to enhance the product's marketability. It is anticipated that seaweed extracts, such as pigments, extracted from seaweed processing by-products will also be used as additives.
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RU2469732C1 (en) * | 2011-07-05 | 2012-12-20 | Федеральное государственное бюджетное учреждение науки Тихоокеанский институт биоорганической химии им. Г.Б. Елякова Дальневосточного отделения Российской академии наук (ТИБОХ ДВО РАН) | Method of obtaining carotinoid complex from starfish |
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