KR102282510B1 - Extraction Mehtod of Lutein and Beta Carotene from Paprika Leaf Using a Supercritical Carbon Dioxide - Google Patents
Extraction Mehtod of Lutein and Beta Carotene from Paprika Leaf Using a Supercritical Carbon Dioxide Download PDFInfo
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- KR102282510B1 KR102282510B1 KR1020180088588A KR20180088588A KR102282510B1 KR 102282510 B1 KR102282510 B1 KR 102282510B1 KR 1020180088588 A KR1020180088588 A KR 1020180088588A KR 20180088588 A KR20180088588 A KR 20180088588A KR 102282510 B1 KR102282510 B1 KR 102282510B1
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- 229960005375 lutein Drugs 0.000 title claims abstract description 42
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C403/00—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone
- C07C403/06—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone having side-chains substituted by singly-bound oxygen atoms
- C07C403/08—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone having side-chains substituted by singly-bound oxygen atoms by hydroxy groups
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C403/00—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone
- C07C403/24—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone having side-chains substituted by six-membered non-aromatic rings, e.g. beta-carotene
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P20/00—Technologies relating to chemical industry
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Abstract
본 발명은 파프리카로부터 루테인을 추출하는 방법에 관한 것으로, 더욱 구체적으로 초임계 이산화탄소를 이용한 파프리카로부터 루테인 및 베타카로틴을 추출하는 방법 및 이에 따라 추출된 파프리카 루테인 및 베타카로틴에 관한 것이다.
본 발명의 파프리카로부터 루테인 및 베타카로틴을 추출하는 방법은 초임계 추출법을 이용하여 파프리카 잎으로부터 루테인 및 베타카로틴를 분리함으로써 각 물질의 생화학적 특성이 그대로 유지되면서도 신체에 유해한 유기 용매를 사용하지 않아 추출물의 신뢰성을 높일 수 있다.The present invention relates to a method for extracting lutein from paprika, and more particularly, to a method for extracting lutein and beta-carotene from paprika using supercritical carbon dioxide, and paprika lutein and beta-carotene extracted accordingly.
The method of extracting lutein and beta-carotene from paprika of the present invention is by separating lutein and beta-carotene from paprika leaves by using a supercritical extraction method, thereby maintaining the biochemical properties of each material as it is, and does not use an organic solvent harmful to the body reliability can be increased.
Description
본 발명은 파프리카로부터 루테인을 추출하는 방법에 관한 것으로, 더욱 구체적으로 초임계 이산화탄소를 이용한 파프리카로부터 루테인 및 베타카로틴을 추출하는 방법 및 이에 따라 추출된 파프리카 루테인 및 베타카로틴에 관한 것이다.The present invention relates to a method for extracting lutein from paprika, and more particularly, to a method for extracting lutein and beta-carotene from paprika using supercritical carbon dioxide, and paprika lutein and beta-carotene extracted accordingly.
파프리카 열매는 카로티노이드, 아스코르빈산, 토코페롤, 플라보노이드, 페놀성 화합물과 같은 영양소를 다수 포함한 채소로 널리 알려져 있다. Paprika fruit is widely known as a vegetable that contains many nutrients such as carotenoids, ascorbic acid, tocopherols, flavonoids and phenolic compounds.
신선한 파프리카는 국내에서 7년 동안 재배면적이 3배, 소비가 6배 가량 증가하였고, 또 재배기술의 발전에 따라 온실에서 재배되는 파프리카의 키는 4 내지 6m에 이르며, 과육의 생산량도 증가하고 있는 추세이다. For fresh paprika, the cultivated area has increased by 3 times and consumption by 6 times for 7 years in Korea. Also, with the development of cultivation technology, the height of paprika grown in greenhouses is 4 to 6 m, and the production of fruit is also increasing. is the trend
그러나, 이러한 재배기술의 발전에도 불구하고 파프리카 잎과 줄기의 영양적 가치와 그 평가가 제대로 이루어지지 않은 채 대부분 버려지고 있는 실정이며, 파프리카의 이용률을 높이기 위해서는 파프리카에 내재된 천연 기능성 물질들을 추출하여 그 이용률을 제고할 필요가 있다.However, despite the development of such cultivation technology, the nutritional value and evaluation of paprika leaves and stems are mostly thrown away without being properly evaluated. In order to increase the utilization rate of paprika, the natural functional substances inherent in paprika must be extracted. It is necessary to increase the utilization rate.
한편, 루테인은 식물, 예컨대 꽃, 특히 매리골드 (marigold)의 꽃과, 녹색 잎 채소에서 발견되는 잔토필 및 자연 발생 카로테노이드이다. 루테인은, 예를 들어 매리골드, 시금치, 케일 및 브로콜리의 꽃잎에서 추출될 수 있다. 매리골드는 특히 루테인이 풍부하며, 이는 지방산을 갖는 루테인 에스테르로서 발견된다. 루테인은 기능성 식품 및 헬스케어 제품과 같은 모든 유형의 조성물에서 황색 안료로서 사용될 수 있다. 루테인의 눈 질환과 관련된 약리학적 효과 및 적용은 널리 공지되어 있는데, 루테인을 섭취하면 황반색소의 밀도가 증가하여 눈 질환이 있는 환자들에게서 시각 기능을 개선시킬 수 있고, 눈의 유해활성산소에 의한 시세포 손상에 따른 노화과정을 효과적으로 억제함으로써 백내장이나 노인성 황반변성(Age-related macular degeneration)과 같은 안구질환의 발생율을 감소시킬 수 있음이 공지된 바 있다(Bernstein P.S. et al., Ophthalmology, 2002(109), 1780-1787; Kvansakul J. et al., Ophthalmic and Physiological Optics, 2006(26), 362-371). On the other hand, lutein is a xanthophyll and naturally occurring carotenoid found in plants, such as flowers, particularly those of marigolds and green leafy vegetables. Lutein can be extracted, for example, from the petals of marigold, spinach, kale and broccoli. Marigolds are particularly rich in lutein, which is found as lutein esters with fatty acids. Lutein can be used as a yellow pigment in all types of compositions, such as functional foods and healthcare products. The pharmacological effects and applications of lutein related to eye diseases are well known, and when lutein is ingested, the density of macular pigment increases, which can improve visual function in patients with eye diseases, and It has been known that the incidence of eye diseases such as cataracts or age-related macular degeneration can be reduced by effectively inhibiting the aging process caused by photocell damage (Bernstein PS et al., Ophthalmology, 2002 (109) ), 1780-1787;Kvansakul J. et al., Ophthalmic and Physiological Optics, 2006(26), 362-371).
천연 식물소재로부터 루테인을 추출하는 방법과 관련된 특허로, 특허공개 제10-2014-0137758호, ‘눈큰흑찰(흑찰거대배아미) 쌀겨로부터 추출된, 루테인, 비타민 E 및 베타-카로틴을 함유하는 지용성 조성물’, 특허등록 제10-1449379호 ‘ 녹차로부터 루테인의 추출 방법’등이 공개된 바 있으나, 아직까지 루테인을 천연소재로부터 상업적으로 충분하게 활용할 수 있을 만큼 고농도로 추출하는 방법에 대해 공개된 바 없다. A patent related to a method of extracting lutein from natural plant materials, Patent Publication No. 10-2014-0137758, 'Nunkeun Heukchal (Heukchal giant baeahmi), extracted from rice bran, Lutein, vitamin E and beta-A fat-soluble composition containing carotene ', Patent Registration No. 10-1449379, 'A method of extracting lutein from green tea', etc. have been disclosed, but a method for extracting lutein from natural materials at a high enough concentration to be commercially available from natural materials has not been disclosed. .
이에, 본 발명자들은 천연 식물소재에서 루테인과 베타카로틴을 추출하는 방법을 연구하던 중, 파프리카 잎을 소재로 하여 초임계 추출 방식을 적용하는 경우, 높은 수율로 천연 루테인 및 베타카로틴을 추출할 수 있음을 확인함으로써 본 발명을 완성하였다. Therefore, the present inventors were studying a method of extracting lutein and beta-carotene from natural plant materials, and when supercritical extraction method was applied using paprika leaves as a material, natural lutein and beta-carotene could be extracted with high yield. By confirming the present invention was completed.
따라서, 본 발명의 주된 목적은 파프리카 잎으로부터 높은 수율로 루테인 및 베타카로틴을 추출하는 방법을 제공하는 데 있다.Accordingly, the main object of the present invention is to provide a method for extracting lutein and beta-carotene in high yield from paprika leaves.
본 발명의 다른 목적 및 이점은 하기의 발명의 상세한 설명, 청구범위 및 도면에 의해 보다 명확하게 된다.Other objects and advantages of the present invention will become more apparent from the following detailed description of the invention, claims and drawings.
본 발명의 한 양태에 따르면, 본 발명은 1) 파프리카 잎을 동결건조 한 후, 0.5 내지 2 mm 크기로 분쇄하는 단계; 2) 상기 파프리카 잎 분쇄물을 초임계 이산화탄소를 사용하여 초임계 추출하는 단계; 및 3) 상기 초임계 추출물의 잔여물을 물 또는 알코올로 추출하여 분리 정제하는 단계;를 포함하는 파프리카 잎으로부터 루테인 및 베타카로틴을 추출하는 방법을 제공한다.According to one aspect of the present invention, the present invention comprises the steps of: 1) lyophilizing paprika leaves, then pulverizing them to a size of 0.5 to 2 mm; 2) supercritical extraction of the paprika leaf pulverized product using supercritical carbon dioxide; And 3) extracting the residue of the supercritical extract with water or alcohol to separate and purify; provides a method for extracting lutein and beta-carotene from paprika leaves, including.
본 발명에서 사용되는 용어 "파프리카(paprika, Capsicum annuum var. angulosum)는 쌍떡잎식물 통화식물목 가지과의 한해살이 식물을 의미한다. 본 발명에서 파프리카는 잎 부위에 루테인 및 베타카로틴과 함께 폴리페놀 화합물을 다량 함유하고 있기 때문에, 이에 따라 본 발명은 추출 원료로서 파프리카 잎을 사용하는 것을 특징으로 한다.As used in the present invention, the term "paprika (paprika, Capsicum annuum var. angulosum) refers to an annual plant of the Solanaceae family, a dicotyledonous plant. In the present invention, paprika contains a large amount of polyphenol compounds along with lutein and beta-carotene in the leaf part. Therefore, the present invention is characterized in that paprika leaves are used as an extraction raw material.
본 발명의 파프리카 잎으로부터 루테인 및 베타카로틴을 추출하는 방법에서, 상기 단계 1)은 파프리카 잎의 추출 효율을 증가시키기 위한 전처리 단계로, 상기 파프리카 잎을 동결건조하고 분쇄하는 방식으로 수행될 수 있으며, 파프리카 잎 건조물을 일정 크기로 분쇄시켜 파프리카 잎의 추출 효율을 증가시키기 위한 전처리 단계이다.In the method of extracting lutein and beta-carotene from paprika leaves of the present invention, step 1) is a pretreatment step for increasing the extraction efficiency of paprika leaves, and may be performed by freeze-drying and pulverizing the paprika leaves, This is a pre-treatment step for increasing the extraction efficiency of paprika leaves by grinding the dried paprika leaves to a predetermined size.
본 발명에서 상기 분쇄는 파프리카 잎을 0.5 내지 2 mm 크기로 분쇄하는 것이 바람직하다. 만일 상기 분쇄 시 입자 크기가 상기 범위 밖일 경우, 파프리카 잎의 추출 효율이 떨어지는 단점이 있다. 특히, 0.5 mm 미만의 입자 크기에서는 초임계 추출 시 압력 부하로 인하여 추출 효율이 떨어지게 되고 또한 휘발성 유효 성분이 분쇄 과정 중에 휘발되는 단점이 있다. 한편, 2 mm보다 큰 입자 크기에서는 입자 속에 포함되어 있는 유효 성분이 초임계 유체에 의해 외부로 추출되기 어려워 결과적으로 유효 성분의 추출 효율이 떨어지는 단점이 있다.In the present invention, the pulverization is preferably pulverizing paprika leaves to a size of 0.5 to 2 mm. If the particle size at the time of grinding is outside the above range, there is a disadvantage in that the extraction efficiency of paprika leaves is lowered. In particular, in the case of a particle size of less than 0.5 mm, extraction efficiency is lowered due to pressure load during supercritical extraction, and there is a disadvantage in that volatile active ingredients are volatilized during the grinding process. On the other hand, with a particle size larger than 2 mm, it is difficult for the active ingredient contained in the particle to be extracted to the outside by the supercritical fluid, and consequently the extraction efficiency of the active ingredient is lowered.
본 명세서에서 상기 용어 "초임계 추출법"은 임계온도 및 경계압력을 초과하는 상태의 유체인 초임계 유체를 사용하여 추출하는 방법을 의미한다. 기체는 임계온도이하에서는 어떤 압력을 초과하면 액화되지만 임계온도 이상에서는 저압에서 고압까지 연속한 상(phase)상태를 나타내고 기체와 액체의 성질을 구별할 수 없게 된다. 따라서, 초임계유체는 높은 밀도가 있으면서 낮은 점성과 액체의 백배가량이나 큰 확산능력이 있기 때문에 초임계 유체를 이용한 초임계 추출법은 액체추출법에 비교하면 효율이 높은 추출법이다. In the present specification, the term "supercritical extraction method" refers to a method of extraction using a supercritical fluid, which is a fluid in a state exceeding the critical temperature and boundary pressure. A gas is liquefied when a certain pressure is exceeded below the critical temperature, but above the critical temperature, it shows a continuous phase from low pressure to high pressure, and the properties of gas and liquid cannot be distinguished. Therefore, the supercritical fluid has a high density, low viscosity, and a 100 times greater diffusion capacity of a liquid. Therefore, the supercritical extraction method using the supercritical fluid is an extraction method with high efficiency compared to the liquid extraction method.
본 발명의 바람직한 구현예에 따르면, 상기 초임계 추출법은 이산화탄소를 초임계유체로 사용한 것이다. 또한 본 발명에서는 상기 초임계 유체 이외에 별도로 보조용매(co-solvent)를 사용하지 않는 것을 특징으로 한다. According to a preferred embodiment of the present invention, the supercritical extraction method uses carbon dioxide as a supercritical fluid. In addition, in the present invention, it is characterized in that a co-solvent is not used in addition to the supercritical fluid.
본 발명의 바람직한 구현예에 따르면, 상기 단계 2)의 초임계 추출은 40℃ 내지 60℃ 온도 및 200 bar 내지 400 bar의 압력 조건을 갖는 추출조와 45℃ 내지 55℃ 온도 및 20 bar 내지 40 bar의 압력 조건을 갖는 분리조에서 수행하는 것이 바람직하다.According to a preferred embodiment of the present invention, the supercritical extraction of step 2) is performed with an extraction tank having a temperature of 40°C to 60°C and a pressure of 200 bar to 400 bar, and a temperature of 45°C to 55°C and 20 bar to 40 bar. It is preferably carried out in a separation tank having pressure conditions.
또한, 본 발명의 파프리카 잎으로부터 루테인 및 베타카로틴을 추출하는 방법에서, 상기 단계 2)의 초임계 추출은, 초임계 이산화탄소를 사용하여 40㎖/min 내지 70 ㎖/min 유량으로 60분 내지 180분 동안 초임계 추출하는 것이 바람직하다.In addition, in the method of extracting lutein and beta-carotene from paprika leaves of the present invention, the supercritical extraction of step 2) is 60 to 180 minutes at a flow rate of 40 ml/min to 70 ml/min using supercritical carbon dioxide. During supercritical extraction is preferred.
본 발명의 일 실시예에 따르면 상기 단계 2)의 초임계 추출에서 3% 이상의 수율로 고농도의 루테인 및 베타카로틴이 추출된다.According to an embodiment of the present invention, high concentrations of lutein and beta-carotene are extracted in a yield of 3% or more in the supercritical extraction of step 2).
본 발명의 다른 양태에 따르면, 본 발명은 상기 파프리카 잎으로부터 루테인 및 베타카로틴을 추출하는 방법에 따라 추출된 루테인 및 베타카로틴을 제공한다.According to another aspect of the present invention, the present invention provides lutein and beta-carotene extracted according to the method for extracting lutein and beta-carotene from the paprika leaf.
본 발명의 파프리카 잎으로부터 추출된 루테인 및 베타카로틴은 상기 파프리카 잎으로부터 루테인 및 베타카로틴을 추출하는 방법에 따라 추출되어, 생화학적 특성이 그대로 유지되면서도 신체에 유해한 유기 용매를 사용하지 않아 추출물의 신뢰성을 높일 수 있는 장점이 있다. 본 발명의 파프리카 잎으로부터 추출된 루테인 및 베타카로틴은 상기 본 발명의 초임계 추출방법에 따라 추출되므로 과도한 설명을 피하기 위하여 이들 사이에 중복되는 내용에 대한 설명은 생략하도록 한다. Lutein and beta-carotene extracted from paprika leaves of the present invention are extracted according to the method of extracting lutein and beta-carotene from paprika leaves, and biochemical properties are maintained as they are, and organic solvents harmful to the body are not used. There are advantages to increasing it. Since lutein and beta-carotene extracted from paprika leaves of the present invention are extracted according to the supercritical extraction method of the present invention, the description of overlapping content therebetween will be omitted in order to avoid excessive description.
본 발명은 상기 수단을 통하여, 초임계 추출법을 이용하여 파프리카 잎으로부터 루테인 및 베타카로틴를 분리함으로써 각 물질의 생화학적 특성이 그대로 유지되면서도 신체에 유해한 유기 용매를 사용하지 않아 추출물의 신뢰성을 높일 수 있다.The present invention, through the above means, by separating lutein and beta-carotene from paprika leaves using a supercritical extraction method, while maintaining the biochemical properties of each material as it is, it does not use an organic solvent harmful to the body. It is possible to increase the reliability of the extract.
도 1은 파프리카 잎을 동결건조 하는 과정을 나타내는 사진이다.
도 2는 루테인 표준품(상)과 파프리카 잎의 초임계 추출물(하)의 HPLC 크로마토그램 그래프이다.
도 3은 베타카로틴 표준품(상)과 파프리카 잎의 초임계 추출물(하)의 HPLC 크로마토그램 그래프이다. 1 is a photograph showing the process of freeze-drying paprika leaves.
2 is an HPLC chromatogram graph of a lutein standard (top) and a supercritical extract of paprika leaves (bottom).
3 is an HPLC chromatogram graph of beta-carotene standard (top) and supercritical extract of paprika leaf (bottom).
이하, 실시예를 통하여 본 발명을 더욱 상세히 설명하기로 한다. 이들 실시예는 단지 본 발명을 예시하기 위한 것이므로, 본 발명의 범위가 이들 실시예에 의해 제한되는 것으로 해석되지는 않는다.Hereinafter, the present invention will be described in more detail through examples. These examples are only for illustrating the present invention, and therefore, the scope of the present invention is not to be construed as being limited by these examples.
실시예 1. 파프리카 잎으로부터 루테인 및 베타카로틴의 초임계 유체 추출Example 1. Supercritical fluid extraction of lutein and beta-carotene from paprika leaves
파프리카 잎 원물은 농업회사법인 해누리유한회사에서 재배한 잎을 사용하였으며, 세척 과정을 거친 후, 동결건조하여 0.5 ~ 2 mm 사이즈로 분쇄하여 밀봉 포장 후 냉장보관하면서 사용하였다(도 1 참조). As the raw material of paprika leaves, leaves grown by Haenuri Co., Ltd., an agricultural company, were used, and after washing, freeze-dried and crushed to a size of 0.5 to 2 mm, sealed and stored in a refrigerator (see FIG. 1).
초임계유체추출은 천연물로부터 선택적인 물질을 추출할 수 있으며 다양한 조건 즉, 온도, 압력, 입자크기, 보조용매 사용 등에 따라 추출수율 및 활성성분의 함량에 크게 영향을 미친다. Supercritical fluid extraction can extract selective substances from natural products and greatly affects the extraction yield and content of active ingredients according to various conditions, such as temperature, pressure, particle size, and the use of auxiliary solvents.
파프리카로부터 추출물을 획득하기 위해 초임계유체추출 장치(ISA-SCFE-0050-0100-080-re, 일신오토클레이브, 한국)를 이용하여 추출하였다. 추출조는 압력 350bar, 60℃ 및 400bar, 50℃의 두가지 조건으로 설정하였다. 유속은 60mL/min으로 하였고 분리조는 40bar 및 40℃의 조건을 120min 동안 유지하였으며, 보조용매는 사용하지 않고 추출하였다. 원료는 동결건조되어 분쇄된 파프리카 잎 200g을 주입하였고 시료 당 120분 동안 초임계 추출을 실시하였고, 추출물을 회수하였다.To obtain an extract from paprika, it was extracted using a supercritical fluid extraction device (ISA-SCFE-0050-0100-080-re, Ilshin Autoclave, Korea). The extraction tank was set to two conditions of pressure 350 bar, 60 ℃ and 400 bar, 50 ℃. The flow rate was 60 mL/min and the separation tank was maintained at 40 bar and 40° C. conditions for 120 min, and extraction was performed without using an auxiliary solvent. As a raw material, 200 g of freeze-dried and pulverized paprika leaves were injected, and supercritical extraction was performed for 120 minutes per sample, and the extract was recovered.
그 결과, 350bar, 60℃ 조건의 경우 파프리카잎 추출물의 추출량은 6.68g으로 측정되었고, 400bar, 50℃ 조건에서는 파프리카잎 추출물의 추출량이 7.12g으로 측정되어, 파프리카 잎 초임계 추출시 수율이 3% 이상임을 확인할 수 있었다. As a result, the extraction amount of the paprika leaf extract was measured to be 6.68 g in the case of 350 bar and 60 ℃ conditions, and the extraction amount of the paprika leaf extract was measured to be 7.12 g in the condition of 400 bar and 50 ℃, and the yield is 3% when supercritical extraction of paprika leaves is obtained. I could confirm that it was abnormal.
[표 1][Table 1]
실시예 2. 루테인 및 베타카로틴의 분석Example 2. Analysis of lutein and beta-carotene
루테인의 분석은 용매혼합용액으로 추출하고 에탄올로 희석한 용액을 자외분광광도계 446nm에서 총 카로티노이드 함량을 구하고 고속액체크로마토그래프/자외부흡광광도 검출기를 이용하여 분석하는 방법으로 최대흡수파장인 446nm에서 검출하여 정량 분석하였다. The analysis of lutein is a method of extracting a solution diluted with a solvent mixture and diluting it with ethanol, obtaining the total carotenoid content at 446 nm using an ultraviolet spectrophotometer, and analyzing it using a high-performance liquid chromatography/ultraviolet absorbance detector. It is detected at the maximum absorption wavelength of 446 nm. and quantitative analysis was performed.
또한, 베타카로틴 정량 방법은 검화과정을 거쳐 시료로부터 베타카로틴을 추출한 후 고속액체크로마토그래프/자외부흡광광도검출기를 이용하여 분석하는 방법으로 최대흡수파장인 450 nm에서 검출하여 정량하였다. In addition, the beta-carotene quantification method is a method of analyzing beta-carotene from the sample through a saponification process and then analyzing it using a high-performance liquid chromatography/ultraviolet absorbance detector. It was detected and quantified at 450 nm, the maximum absorption wavelength.
그 결과, 상기 실시예 1의 초임계 추출방법(400bar, 50℃)을 이용한 파프리카 잎의 초임계 추출물에 28.82mg/kg 함량의 루테인 및 1,628mg/kg 함량의 베타카로틴이 포함되어 있음을 확인할 수 있었다(도 2 및 도 3 참조). As a result, it can be confirmed that the supercritical extract of paprika leaf using the supercritical extraction method of Example 1 (400 bar, 50 ° C) contains lutein at a content of 28.82 mg/kg and beta-carotene at a content of 1,628 mg/kg. (see Figures 2 and 3).
[표 2][Table 2]
상기 실시예의 파프리카 잎의 초임계 추출물과는 달리 5배 부피의 100% 에탄올을 이용하여 60℃에서 4시간 동안 추출한 파프리카 잎의 에탄올 추출물에서는 루테인이 검출되지 않았고, 베타카로틴의 함량도 실시예 1의 초임계 추출물에 비해 50% 수준으로 나타났다. Unlike the supercritical extract of paprika leaves of the above example, lutein was not detected in the ethanol extract of paprika leaves extracted at 60° C. for 4 hours using 5 times the volume of 100% ethanol, and the content of beta-carotene was also It was found to be at a level of 50% compared to the supercritical extract.
상기와 같은 결과를 통해, 본 발명의 초임계 추출방법을 통해 파프리카 잎을 추출하는 경우, 보조용매의 사용 없이 루테인과 베타카로틴을 고농도로 손쉽게 추출할 수 있음을 확인할 수 있었다.Through the above results, it was confirmed that when paprika leaves are extracted through the supercritical extraction method of the present invention, lutein and beta-carotene can be easily extracted at high concentrations without the use of an auxiliary solvent.
Claims (5)
2) 상기 파프리카 잎 분쇄물을 초임계 이산화탄소를 사용하여 초임계 추출하는 단계; 및
3) 상기 초임계 추출물의 잔여물을 물 또는 알코올로 추출하여 분리 정제하는 단계;를 포함하되,
상기 단계 1)의 분쇄는 파프리카 잎을 0.5 내지 2 mm 크기로 분쇄하는 것을 특징으로 하고,
상기 단계 2)의 초임계 추출은 40℃ 내지 60℃ 온도 및 200 bar 내지 400 bar의 압력 조건을 갖는 추출조와 45℃ 내지 55℃ 온도 및 20 bar 내지 40 bar의 압력 조건을 갖는 분리조에서 수행하는 것을 특징으로 하며,
상기 단계 2)의 초임계 추출은 초임계 이산화탄소를 사용하여 40㎖/min 내지 70 ㎖/min 유량으로 60분 내지 180분 동안 초임계 추출하는 것을 특징으로 하는,
파프리카 잎으로부터 루테인 및 베타카로틴을 추출하는 방법.1) freeze-drying paprika leaves, then pulverizing them to a size of 0.5 to 2 mm;
2) supercritical extraction of the paprika leaf pulverized product using supercritical carbon dioxide; and
3) separating and purifying the residue of the supercritical extract by extracting it with water or alcohol;
The pulverization of step 1) is characterized in that the paprika leaves are pulverized to a size of 0.5 to 2 mm,
The supercritical extraction of step 2) is performed in an extraction tank having a temperature of 40°C to 60°C and a pressure of 200 bar to 400 bar, and a separation tank having a temperature of 45°C to 55°C and a pressure of 20 bar to 40 bar characterized by,
The supercritical extraction of step 2) is characterized in that supercritical extraction is performed for 60 to 180 minutes at a flow rate of 40 ml/min to 70 ml/min using supercritical carbon dioxide,
A method for extracting lutein and beta-carotene from paprika leaves.
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