KR101112053B1 - Method for obtaining purified lycopene and water-soluble lycopene from tomato - Google Patents
Method for obtaining purified lycopene and water-soluble lycopene from tomato Download PDFInfo
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- KR101112053B1 KR101112053B1 KR1020110059833A KR20110059833A KR101112053B1 KR 101112053 B1 KR101112053 B1 KR 101112053B1 KR 1020110059833 A KR1020110059833 A KR 1020110059833A KR 20110059833 A KR20110059833 A KR 20110059833A KR 101112053 B1 KR101112053 B1 KR 101112053B1
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- lycopene
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- OAIJSZIZWZSQBC-GYZMGTAESA-N lycopene Chemical compound CC(C)=CCC\C(C)=C\C=C\C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)\C=C\C=C(/C)CCC=C(C)C OAIJSZIZWZSQBC-GYZMGTAESA-N 0.000 title claims abstract description 115
- UPYKUZBSLRQECL-UKMVMLAPSA-N Lycopene Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1C(=C)CCCC1(C)C)C=CC=C(/C)C=CC2C(=C)CCCC2(C)C UPYKUZBSLRQECL-UKMVMLAPSA-N 0.000 title claims abstract description 111
- JEVVKJMRZMXFBT-XWDZUXABSA-N Lycophyll Natural products OC/C(=C/CC/C(=C\C=C\C(=C/C=C/C(=C\C=C\C=C(/C=C/C=C(\C=C\C=C(/CC/C=C(/CO)\C)\C)/C)\C)/C)\C)/C)/C JEVVKJMRZMXFBT-XWDZUXABSA-N 0.000 title claims abstract description 111
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- ZCIHMQAPACOQHT-ZGMPDRQDSA-N trans-isorenieratene Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/c1c(C)ccc(C)c1C)C=CC=C(/C)C=Cc2c(C)ccc(C)c2C ZCIHMQAPACOQHT-ZGMPDRQDSA-N 0.000 title claims abstract description 111
- 235000007688 Lycopersicon esculentum Nutrition 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 29
- 240000003768 Solanum lycopersicum Species 0.000 title description 30
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- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
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- 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
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/81—Solanaceae (Potato family), e.g. tobacco, nightshade, tomato, belladonna, capsicum or jimsonweed
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/22—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the construction of the column
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- 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
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
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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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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Abstract
Description
본 발명은 토마토 유래 정제 라이코펜 및 수용성 라이코펜의 수득방법에 관한 것으로, 더욱 상세하게는 저온 칼럼 추출법 및 반용매 용출법을 이용하여 고농도, 고수율 및 안정성을 구현할 수 있는 토마토 유래 정제 라이코펜 및 수용성 라이코펜의 수득방법에 관한 것이다.
The present invention relates to a method for obtaining tomato-derived lycopene and water-soluble lycopene, and more particularly, to a method for obtaining tomato-derived lycopene and water-soluble lycopene, which can realize high concentration, high yield and stability using low temperature column extraction and anti-solvent elution. It relates to a method of obtaining.
일반적으로 라이코펜(lycopene)은, 강렬한 붉은 색상을 갖으며, 특히 토마토와 수박에 풍부히 함유되어 있는 천연색소이다.In general, lycopene is a natural pigment, which has an intense red color and is particularly rich in tomatoes and watermelons.
최근들어 상기 토마토 유래 라이코펜의 전립선암의 방지와 치료에 대한 효과가 입증되면서 토마토와 라이코펜에 대한 관심도 증가하고 있는 추세이다.Recently, as the effects of the tomato-derived lycopene on the prevention and treatment of prostate cancer have been proved, interest in tomatoes and lycopene is also increasing.
상기 전립선 비대증은 혈액 내에서 테스토스테론(testosterone) 이 과다하게 존재하면 전립선에서 5알파-리덕테이스(reductase) 에 의해 DHT(De-Hydro-Testosterone)를 다량 합성하게 되고 합성된 DHT는 전립선 세포에 있는 남성호르몬수용체(androgen receptor)에 결합하여 전립선 비대를 유발하는데 라이코펜은 전립선 비대증 주요 발현 요소인 5알파-리덕테이스의 활성을 억제하여 전립선 비대증을 근원적으로 방지하며 개선하는 효과를 나타낸다.
The prostate hyperplasia is a large amount of DHT (De-Hydro-Testosterone) synthesized by 5 alpha-reductase in the prostate when excessive testosterone is present in the blood, and the synthesized DHT is present in the prostate cells. It binds to the male hormone receptor (androgen receptor) and causes prostatic hypertrophy. Lycopene inhibits the activity of 5 alpha-reductase, a major expression factor of prostatic hyperplasia, thereby preventing and improving prostatic hypertrophy.
그 외 토마토에는 라이코펜 이외에도 베타카로틴(β-carotene), 피 토엔(phytoene), 피 토플루엔(phytofluene) 등의 카로티노이드류를 다양하게 함유하고 있어 기능성이 매우 우수한 야채로 알려져 있다.
In addition to lycopene, tomatoes contain various carotenoids such as beta-carotene, phytoene, and phytofluene.
이와 같은 특성과 더불어 완전하고 유익한 효과 때문에, 라이코펜은 통상 올레오레진(oleoresin) 형태로, 즉 천연지질 중에 현탁액 형태로 색소제로서 식품산업에서 널리 사용되어왔다.Because of these properties and the complete and beneficial effect, lycopene has been widely used in the food industry as a colorant, usually in the form of oleoresin, ie in the form of a suspension in natural lipids.
이런 형태에서는 라이코펜의 산화(결정형 라이코펜은 아주 불안정하다)와 세균에 의한 변화가 방지되고, 대부분이 지질이기 때문이며, 천연 항산화제가 함유되어있다. 나아가 라이코펜은 항산화작용과 화학보호성질이 있어 식품보조제로서 사용 되었다.
This form prevents the oxidation of lycopene (crystalline lycopene is very unstable) and changes caused by bacteria, most of which are lipids, and contain natural antioxidants. Furthermore, lycopene has been used as a food supplement because of its antioxidant activity and chemical protective properties.
한편, 탈모 또한 테스토스테론이 과다하게 존재하면 모모세포에서 5알파-리덕테이스에 의해 DHT를 다량 합성하게 되고 합성된 DHT는 모모세포에 있는 남성호르몬수용체에 결합하여 모낭의 퇴화 및 탈모의 촉진을 유발하여 점증적으로 탈모가 진행되게 되는데 라이코펜의 5알파-리덕테이스의 활성 저해 작용은 탈모 방지 및 양모에 많은 도움을 줄 수 있다.
On the other hand, when hair loss is also excessive in testosterone, the hair cells synthesize DHT by 5 alpha-reductase in a large amount, and the synthesized DHT binds to the male hormone receptor in the hair cells, causing hair follicle degeneration and promoting hair loss. Hair loss progresses gradually, and lycopene 5 alpha-reductase activity inhibitory action can help a lot of hair loss prevention and wool.
현재까지 국내 외 모두 토마토에서 추출한 라이코펜을 이용한 탈모방지 및 양모 촉진 육모제 의약외품 및 두발전문화장품 소재와 이를 활용한 화장품 제형은 개발되지 않은 실정이다.
Until now, domestic and foreign domestic use of lycopene extracted from tomato prevents hair loss and promotes hair growth.
토마토의 경우 많은 양의 라이코펜을 함유하고 있으며, 활성성분 추출을 위한 전처리 과정이 수월하여 화장품 소재로의 활용이 유리한 원료이다.
Tomato contains a large amount of lycopene, and is easy to use as a cosmetic material since the pretreatment process for extracting the active ingredient is easy.
합성에 의하여 라이코펜을 제조할 수 있지만 [카렐등(Karrer et al.), Helv. Chim. Acta 33, 1349 (1950); 아이슬러등(Isler et al.), ibid. 39, 463 (1956)], 토마토(lycopersicum esculentum)에서 통상적으로 얻어질 수 있는 수준이었다.
Lycopene can be prepared by synthesis, but Karel et al., Helv. Chim. Acta 33, 1349 (1950); Isler et al., Ibid. 39, 463 (1956)], tomatoes (lycopersicum esculentum) was a level that can be obtained conventionally.
또한, 라이코펜은 친유성 천연색소로써 지용성이며 두발화장품 중 토닉, 앰플등의 수용성 화장 원료로써의 사용이 어려운 실정이므로 수용성 라이코펜으로의 전환이 필요하며, 토마토 유래 라이코펜 추출공정은 이와 같은 형태의 제품을 얻도록 감안하여야 될 것이다.
In addition, lycopene is lipophilic as a lipophilic natural pigment, and it is difficult to use it as a water-soluble cosmetic raw material such as tonic and ampoule among hair cosmetics, so it needs to be converted to water-soluble lycopene. You should consider to get.
관련 선행기술로써, 대한민국 공개특허공보 제10-2006-0070846호에는 초임계 이산화탄소를 추출 주용매로 하며 보조용매로 스쿠알렌을 투입하여 토마토 라이코펜 조추출물을 수득하는 방법이 공개되어 있다.
As a related prior art, Korean Patent Laid-Open Publication No. 10-2006-0070846 discloses a method for obtaining crude crude lycopene extract by adding supercritical carbon dioxide as an extraction main solvent and adding squalene as an auxiliary solvent.
하지만, 상기와 같은 종래기술의 경우, 라이코펜에 대한 초임계 이산화탄소의 용해도는 압력 40℃, 400bar 기준 용매 밀도가 약0.75로 헥산과 유사하다. However, in the prior art as described above, the solubility of supercritical carbon dioxide in lycopene is similar to hexane with a solvent density of about 0.75 at a pressure of 40 ° C. and 400 bar.
이는 라이코펜에 대한 용해도로써 실제 원료 토마토 분말로부터 추출수행 시에는 토마토 분말의 잔존 수분에 의한 초임계 용매 침투 저해 요인으로써 입자의 표면 및 내부 침투력이 약해지며, 반회분식 공정의 경우 용매 체류 시간이 짧아 유기 용매인 헥산보다 용해성이 떨어지는 문제점이 있다. This is the solubility in lycopene. When extraction is performed from the actual tomato powder, the surface and internal penetration of the particles are weakened as a factor of inhibiting supercritical solvent penetration by the residual moisture of the tomato powder. There is a problem that the solubility is inferior to the solvent hexane.
또한, 라이코펜 정제를 하기 위해선 초임계 유체 추출 후에도 후속공정으로 지질 제거 공정이 추가되어져야 하는 문제점이 있었다.In addition, in order to purify lycopene, there was a problem that a lipid removal process should be added as a subsequent process even after supercritical fluid extraction.
한편, 초임계 유체 추출의 추출수율 향상을 위해 보조 용매로써 라이코펜과 유사 분자 구조를 갖는 스쿠알렌을 채택하여 용해도를 높일려고 하였으나, 라이코펜의 경우 탄소수가 40개, 스쿠알렌의 경우 탄소수가 30개로써 초임계 이산화탄소의 분배계수가 라이코펜보다 스쿠알렌에 더 높아 초임계 용매 사용이 증가하게 되는 문제점이 있었다.On the other hand, in order to improve the extraction yield of supercritical fluid extraction, we tried to increase the solubility by adopting squalene having a similar molecular structure as lycopene as an auxiliary solvent, but in the case of lycopene, the carbon number is 40, and the squalene has 30 carbon atoms. There was a problem that the distribution coefficient of carbon dioxide is higher in squalene than lycopene and the use of supercritical solvent is increased.
게다가 친유성 라이코펜과 스쿠알렌의 극성 파라메타가 유사하여 추출 후 스쿠알렌 제거가 용이하지 않은 문제점이 있었다. In addition, since the polar parameters of the lipophilic lycopene and squalene are similar, there is a problem that the removal of squalene after the extraction is not easy.
또한, 대한민국 공개특허공보 제10-2006-0112346호에는 일반적 유기용매 추출법과 차별성을 두기 위해 식물유만을 이용하여 토마토 라이코펜을 수득하는 방법이 공개되어 있다.
In addition, Korean Patent Laid-Open Publication No. 10-2006-0112346 discloses a method for obtaining tomato lycopene using only vegetable oil in order to distinguish it from the general organic solvent extraction method.
상기와 같은 종래기술의 경우, 식물유의 지방산 조성은 탄소수 4개부터 24개까지의 지방산을 가지며 이 중 주로 탄소수 18개로 이루어진 단일결합, 이중결합, 삼중결합 구조를 가지는데 이중결합을 포함하는 분자구조의 경우 꺽인 직쇄 구조로써 라이코펜과 유사한 분자구조 특성을 가지게 되므로 라이코펜에 대한 용해성이 높아 유기용매보다 다소 높은 용해도를 가지게 된다.In the prior art as described above, the fatty acid composition of the vegetable oil has a fatty acid of 4 to 24 carbon atoms, of which has a single bond, double bond, triple bond structure consisting mainly of 18 carbon atoms, molecular structure including a double bond In the case of a straight chain structure having a molecular structure similar to lycopene, solubility in lycopene is higher than that of an organic solvent.
하지만, 식물유의 경우 유기용매 보다 낮은 확산계수 및 강한 점성으로 인해 원료 분말의 표면 및 내부 침투가 용이하지 않아 추출시간이 상당히 길어지게 되는 문제점이 있었다. 다시 말하면 단위시간당 추출수율로 환산하면 비효율적 추출방식에 해당되는 것이다.
However, in the case of vegetable oil, the extraction time is considerably longer because the surface and internal penetration of the raw material powder are not easy due to the lower diffusion coefficient and stronger viscosity than the organic solvent. In other words, the conversion rate per unit time is equivalent to an inefficient extraction method.
본 발명은 상술한 문제점을 해결하기 위한 것으로, 저온 칼럼 추출법 및 반용매 용출법으로 라이코펜을 추출함으로써, 저온 추출방식을 채택함에도 짧은 단위공정 시간으로 높은 추출 수율을 나타낼 수 있도록 하는 토마토 유래 정제 라이코펜 및 수용성 라이코펜의 수득방법을 제공함을 과제로 한다.
The present invention is to solve the above problems, by extracting lycopene by low temperature column extraction method and anti-solvent elution method, tomato-derived purified lycopene to show a high extraction yield with a short unit process time even when the low temperature extraction method is adopted; An object of the present invention is to provide a method for obtaining water-soluble lycopene.
아울러, 라이코펜을 제외한 카로테노이드류 및 지질 성분을 제거하여 정제 라이코펜을 수득할 수 있도록 함으로써, 천연 항상화제 등을 경제적으로 생산할 수 있도록 하는 토마토 유래 정제 라이코펜 및 수용성 라이코펜의 수득방법을 제공함을 다른 과제로 한다.
In addition, by removing carotenoids and lipid components other than lycopene to obtain purified lycopene, another object is to provide a method for obtaining purified lycopene and water-soluble lycopene derived from tomato to economically produce natural homeotropic agents and the like. .
또한, 수용성 라이코펜으로의 전환을 가능하게 함으로써, 각종 화장조성료로의 사용이 용이하도록 하는 토마토 유래 정제 라이코펜 및 수용성 라이코펜의 수득방법을 제공함을 또 다른 과제로 한다.
It is another object of the present invention to provide a method for obtaining tomato-derived lycopene and a water-soluble lycopene to facilitate the use of various cosmetic compositions by enabling the conversion to water-soluble lycopene.
본 발명은 토마토 유래 정제 라이코펜 및 수용성 라이코펜의 수득방법에 있어서, The present invention provides a method for obtaining purified lycopene and water-soluble lycopene derived from tomato,
40 ~ 60g의 건조 토마토 분말을 글래스 필터(glass filter)가 장착된 칼럼(column)에 충진시킨 후, 추출용매 0.5 ~ 2ℓ를 투입하여 토마토 분말로부터 조추출물(crude extract)을 제조하는 조추출물 제조단계(S1); A crude extract manufacturing step of preparing a crude extract from tomato powder by filling 40 ~ 60 g of dried tomato powder in a column equipped with a glass filter, and then adding 0.5 ~ 2 L of an extraction solvent. (S1);
진공농축기를 이용하여, 상기 조추출물에서 추출용매를 제거한 농축물을 제조하는 농축물 제조단계(S2);Concentrate manufacturing step (S2) for producing a concentrate from the crude extract by using the vacuum condenser extract removed;
반용매 0.5 ~ 2ℓ에 상기 농축물 0.5 ~ 2㎖를 투입, 교반하여 카로테노이드(carotenoid)류를 제거하고 라이코펜(lycopene)을 용출하며, 상기 용출된 라이코펜을 여과, 건조 및 분말화하여 정제 라이코펜을 제조하는 라이코펜 정제단계(S3); 및 0.5-2 mL of the concentrate was added to 0.5-2 L of the anti-solvent, followed by stirring to remove carotenoids, eluting lycopene, and filtering, drying, and powdering the eluted lycopene to produce purified lycopene. Lycopene purification step (S3); And
상기 라이코펜 분말 0.006 ~ 0.008g에 5 ~ 20㎖의 계면활성제를 30 ~ 70℃에서 30분 ~ 2시간 동안 교반, 가열하여 수용성 라이코펜을 제조하는 라이코펜 수용화단계(S4);를 포함하여 구성되는 것을 특징으로 하는 토마토 유래 정제 라이코펜 및 수용성 라이코펜의 수득방법을 과제의 해결 수단으로 한다.
It comprises a; lycopene soluble step (S4) to prepare a water-soluble lycopene by stirring and heating the lycopene powder 0.006 ~ 0.008g 5 ~ 20ml of the surfactant at 30 ~ 70 ℃ for 30 minutes ~ 2 hours; The method of obtaining the tomato-derived purified lycopene and the water-soluble lycopene characterized by the above-mentioned is a solution to the problem.
한편, 상기 추출용매는, 에틸아세테이트(ethyl acetate)를 사용하는 것이 바람직하다.
On the other hand, the extraction solvent, it is preferable to use ethyl acetate (ethyl acetate).
아울러, 상기 반용매는, 0 ~ -20℃의 메탄올(methanol)을 사용하는 것이 바람직하다.
In addition, it is preferable that the anti-solvent uses methanol (methanol) of 0 ~ -20 ℃.
또한, 상기 계면활성제는, 리옥시에틸렌 소르비탄 모노올레이트(Polyoxyethyelene Sorbitan Monooleate: Tween 80)를 사용하는 것이 바람직하다.
In addition, as the surfactant, it is preferable to use lyoxyethylene sorbitan monooleate (Polyoxyethyelene Sorbitan Monooleate: Tween 80).
본 발명에 의하면, 저온 칼럼 추출법 및 반용매 용출법으로 라이코펜을 추출함으로써, 저온 추출방식을 채택함에도 짧은 단위공정 시간으로 높은 추출 수율을 나타낼 수 있으며, 라이코펜을 제외한 카로테노이드류 및 지질 성분을 제거하여 정제 라이코펜을 수득할 수 있도록 함으로써, 천연 항상화제 등을 경제적으로 생산할 수 있을 뿐만 아니라, 수용성 라이코펜으로의 전환을 가능하게 함으로써, 각종 화장조성료로의 사용이 용이하도록 하는 효과가 있다.
According to the present invention, by extracting the lycopene by low temperature column extraction method and anti-solvent elution method, even if the low temperature extraction method is adopted, it can exhibit a high extraction yield with a short unit process time, purification by removing carotenoids and lipids except lycopene By allowing lycopene to be obtained, not only economical production of natural homeotropic agents and the like, but also conversion to water-soluble lycopene can be achieved, thereby making it easy to use in various cosmetic compositions.
도 1은 본 발명의 일 실시예에 따른 토마토 유래 정제 라이코펜 및 수용성 라이코펜의 수득방법을 나타낸 제조 흐름도
도 2는 본 발명의 시험예에 따른 크로마토그램[chromatogram]을 나타낸 도면1 is a manufacturing flowchart showing a method of obtaining tomato-derived lycopene and a water-soluble lycopene according to an embodiment of the present invention.
2 is a diagram showing a chromatogram according to a test example of the present invention.
상기의 효과를 달성하기 위한 본 발명은 토마토 유래 정제 라이코펜 및 수용성 라이코펜의 수득방법에 관한 것으로서, 본 발명의 기술적 구성을 이해하는데 필요한 부분만이 설명되며 그 이외 부분의 설명은 본 발명의 요지를 흩트리지 않도록 생략될 것이라는 것을 유의하여야 한다.
The present invention for achieving the above effect relates to a method for obtaining purified lycopene and a water-soluble lycopene derived from tomato, only the parts necessary for understanding the technical configuration of the present invention will be described, the description of other parts scatter the gist of the present invention. Note that it will be omitted so as not to fall short.
이하, 본 발명에 따른 토마토 유래 정제 라이코펜 및 수용성 라이코펜의 수득방법을 상세히 설명하면 다음과 같다.
Hereinafter, the method of obtaining the tomato-derived lycopene and the water-soluble lycopene according to the present invention will be described in detail.
도 1은 본 발명의 일 실시예에 따른 토마토 유래 정제 라이코펜 및 수용성 라이코펜의 수득방법을 나타낸 제조 흐름도로써, 본 발명은, 조추출물 제조단계(S1), 농축물 제조단계(S2), 라이코펜 정제단계(S3) 및 라이코펜 수용화단계(S4)를 포함하여 구성된다.
1 is a manufacturing flowchart showing a method of obtaining tomato-derived lycopene and water-soluble lycopene according to an embodiment of the present invention, the present invention, crude extract preparation step (S1), concentrate production step (S2), lycopene purification step (S3) and lycopene solubilization step (S4) is configured.
상기 조추출물 제조단계(S1)는, 토마토 분말로부터 조추출물(crude extract)을 제조하는 단계로써, 구체적으로는 40 ~ 60g의 건조 토마토 분말을 글래스 필터(glass filter)가 장착된 칼럼(column)에 충진시킨 후, 추출용매 0.5 ~ 2ℓ를 투입하여 토마토 분말로부터 조추출물을 제조하며, 상기 추출용매로는 에틸아세테이트(ethyl acetate)를 사용하는 것이 바람직하다.The crude extract manufacturing step (S1) is a step of preparing a crude extract (crude extract) from the tomato powder, specifically 40 ~ 60g dry tomato powder in a column equipped with a glass filter (glass filter) After filling, 0.5 ~ 2L of extraction solvent is added to prepare crude extract from tomato powder, and ethyl acetate is preferably used as the extraction solvent.
한편, 상기 건조 토마토 분말 40 ~ 60g에 대하여, 상기 추출용매가 0.5 ~ 2ℓ를 투입하되, 추출 수율 향상을 위해 3회 이상 반복하며, 상기 추출용매의 투입량이 0.5ℓ 미만일 경우, 추출 수율 낮아지는 문제점이 있으며, 2ℓ을 초과할 경우, 용매 소비량이 증가하는 문제점이 있다.
On the other hand, with respect to the dry tomato powder 40 ~ 60g, the extraction solvent is added 0.5 ~ 2L, repeated three or more times to improve the extraction yield, the extraction yield is lowered when the amount of the extraction solvent is less than 0.5ℓ There is a problem that, when it exceeds 2L, solvent consumption increases.
상기 농축물 제조단계(S2)는, 진공농축기를 이용하여 상기 조추출물에서 추출용매를 제거한 농축물을 제조하는 단계로써, 구체적으로는 반용매 0.5 ~ 2ℓ에 상기 농축물 0.5 ~ 2㎖를 투입, 교반하여 카로테노이드(carotenoid)류를 제거하고 라이코펜(lycopene)을 용출하며, 상기 용출된 라이코펜을 여과, 건조 및 분말화하여 정제 라이코펜을 제조하게 되며, 상기 반용매로는 0 ~ -20℃의 메탄올(methanol)을 사용하는 것이 바람직하다.The concentrate preparation step (S2) is a step of preparing a concentrate from which the extraction solvent is removed from the crude extract by using a vacuum concentrator, specifically, 0.5-2 ml of the concentrate is added to 0.5-2 L of the anti-solvent, By stirring, carotenoids are removed, lycopene is eluted, and the eluted lycopene is filtered, dried, and powdered to produce purified lycopene, and the antisolvent is methanol (0-20 C). methanol).
한편, 상기 반용매 0.5 ~ 2ℓ에 대하여, 상기 농축물 0.5 ~ 2㎖가 투입되는데, 상기 농축물의 투입량이 2㎖을 초과할 경우, 라이코펜 정제율이 낮아지는 문제점이 있다.
On the other hand, with respect to 0.5 ~ 2L of the anti-solvent, 0.5 ~ 2mL of the concentrate is added, when the amount of the concentrate exceeds 2mL, there is a problem that the lycopene purification rate is lowered.
상기 라이코펜 수용화단계(S4)는, 상기 분말화된 라이코펜을 수용화시키는 단계로써, 구체적으로는 상기 라이코펜 분말 0.006 ~ 0.008g에 5 ~ 20㎖의 계면활성제를 30 ~ 70℃에서 30분 ~ 2시간 동안 교반, 가열하여 수용성 라이코펜을 제조하며, 상기 계면활성제로는 리옥시에틸렌 소르비탄 모노올레이트(Polyoxyethyelene Sorbitan Monooleate: Tween 80)를 사용하는 것이 바람직하다.The lycopene solubilization step (S4) is a step of solubilizing the powdered lycopene, specifically, the lycopene powder in 0.006 ~ 0.008g 5 ~ 20ml of the surfactant at 30 ~ 70
한편, 상기 라이코펜 분말 0.006 ~ 0.008g에 대하여, 상기 계면활성제가 5 ~ 20㎖ 교반되는데, 상기 계면활성제의 교반량이 5㎖ 미만일 경우, 라이코펜 분말의 용해가 용이하지 않은 문제점이 있다.On the other hand, for the lycopene powder 0.006 ~ 0.008g, the surfactant is stirred 5 ~ 20ml, when the stirring amount of the surfactant is less than 5ml, there is a problem that the lycopene powder is not easy to dissolve.
아울러, 상기 교반 및 가열 조건(30 ~ 70℃에서 30분 ~ 2시간)이 상기 조건을 벗어날 경우, 30℃ 미만의 조건에서는 용해가 용이하지 않으며, 70℃를 초과할 경우, 라이코펜의 열변성 우려가 있다.
In addition, when the stirring and heating conditions (30 minutes to 2 hours at 30 ~ 70 ℃) out of the above conditions, it is not easy to dissolve under the conditions of less than 30 ℃, if the temperature exceeds 70 ℃, lycopene heat deterioration concerns There is.
이하, 본 발명을 실시예, 시험예 및 제형예에 의거하여 더욱 구체적으로 설명하겠는 바, 본 발명이 다음 실시예에 의해 한정되는 것을 아니다.
Hereinafter, the present invention will be described in more detail based on Examples, Test Examples, and Formulation Examples, but the present invention is not limited to the following Examples.
<실시예 1>≪ Example 1 >
50g의 건조 토마토 분말을 글래스 필터가 장착된 칼럼에 충진시킨 후, 에틸아세테이트 1ℓ를 투입하여 토마토 분말로부터 조추출물(crude extract)을 제조한 후, 진공농축기를 이용하여, 상기 조추출물에서 에틸아세테이트를 제거한 농축물을 제조하고, 0 ~ -20℃의 메탄올 1ℓ에 상기 농축물 1㎖를 투입, 교반하여 카로테노이드류를 제거하고 라이코펜을 용출하며, 상기 용출된 라이코펜을 여과, 건조 및 분말화하여 정제 라이코펜을 제조하고, 상기 라이코펜 분말 0.007g에 10㎖의 리옥시에틸렌 소르비탄 모노올레이트(Tween 80)를 40℃에서 1시간 동안 교반, 가열하여 수용성 라이코펜을 제조하였다.
After filling 50 g of dried tomato powder in a column equipped with a glass filter, 1 liter of ethyl acetate was added to prepare a crude extract from tomato powder, and then using a vacuum concentrator, ethyl acetate was extracted from the crude extract. Prepared the removed concentrate, 1 ml of the concentrate was added to 1 L of methanol at 0 ~ -20 ℃, stirred to remove carotenoids, eluting lycopene, and the eluted lycopene is filtered, dried and powdered to purified lycopene To prepare a water-soluble lycopene was prepared by stirring and heating 10 ml of lyoxyethylene sorbitan monooleate (Tween 80) at 40 ℃ for 1 hour to 0.007 g of the lycopene powder.
<시험예 1><Test Example 1>
상기와 같이 수용성 라이코펜의 순도 및 수율을 아래와 조건으로 분석하였으며, 그 결과를 [표 1] 및 도 2에 나타내었다.
As described above, the purity and yield of the water-soluble lycopene were analyzed under the following conditions, and the results are shown in [Table 1] and FIG. 2.
(1) 기기(instrument) : Waters(Waters delta 600, USA)(1) Instrument: Waters (Waters delta 600, USA)
(2) 컬럼(Column) : Alltima C18 5u(250×10㎜) (2) Column: Alltima C18 5u (250 × 10mm)
(3) 이동상(Mobile Phase) : Methanol(3) Mobile Phase: Methanol
(4) 유량(Flow Rate) : 1㎖/min(4) Flow Rate: 1ml / min
(5) 검출기(Detector) : Waters(Waters 2489 UV/Vis Detector, USA)(5) Detector: Waters (Waters 2489 UV / Vis Detector, USA)
(6) 파장(Wave Length) : 472 ㎚(6) Wave Length: 472 nm
(7) 실행시간(RunTime) : 30 min(7) RunTime: 30 min
(8) 추출용매(Elution Solvent) : ethyl acetate(HPLC Assay)(8) Elution Solvent: ethyl acetate (HPLC Assay)
(9) 주입부피(Injection Volume) : 200um
(9) Injection Volume: 200um
상기 [표 1] 및 도 2에 도시된 바와 같이, 9.6분대에서 단일 피크를 보였으며, 총 피크 면적의 98.45%로 높은 정제율을 나타내었다.As shown in Table 1 and FIG. 2, a single peak was observed at 9.6 minutes, and a high purification rate was 98.45% of the total peak area.
따라서, 본 발명은 저온 추출방식을 채택함에도 짧은 단위공정 시간으로 높은 추출 수율을 나타낼 수 있으며, 라이코펜을 제외한 카로테노이드류 및 지질 성분을 제거하여 정제 라이코펜을 수득할 수 있도록 함으로써, 천연 항상화제 등을 경제적으로 생산할 수 있을 뿐만 아니라, 수용성 라이코펜으로의 전환을 가능하게 함으로써, 각종 화장조성료로의 사용이 용이하도록 하는 효과가 있다.
Therefore, the present invention may exhibit a high extraction yield with a short unit process time even when the low temperature extraction method is adopted, and by removing carotenoids and lipids except lycopene to obtain a purified lycopene, economical natural homeostasis, etc. Not only can it be produced, but also by enabling the conversion to water-soluble lycopene, there is an effect to facilitate the use in various cosmetic compositions.
또한, 이상에서 설명한 본 발명은 전술한 실시예 및 첨부된 도면에 의해 한정되는 것은 아니고, 본 고안의 기술적 사상을 벗어나지 않는 범위내에서 여러가지 치환, 변형 및 변경이 가능함은 본 발명이 속하는 기술분야에서의 통상의 지식을 가진 자에게 있어 명백할 것이다.
In addition, the present invention described above is not limited to the above-described embodiments and the accompanying drawings, and various substitutions, modifications, and changes are possible within the scope without departing from the technical spirit of the present invention. It will be apparent to those of ordinary skill in the art.
S1 : 조추출물 제조단계
S2 : 농축물 제조단계
S3 : 라이코펜 정제단계
S4 : 라이코펜 수용화단계S1: crude extract manufacturing step
S2: concentrate production step
S3: Lycopene purification step
S4: lycopene solubilization step
Claims (4)
40 ~ 60g의 건조 토마토 분말을 글래스 필터(glass filter)가 장착된 칼럼(column)에 충진시킨 후, 추출용매 0.5 ~ 2ℓ를 투입하여 토마토 분말로부터 조추출물(crude extract)을 제조하는 조추출물 제조단계(S1);
진공농축기를 이용하여, 상기 조추출물에서 추출용매를 제거한 농축물을 제조하는 농축물 제조단계(S2);
반용매 0.5 ~ 2ℓ에 상기 농축물 0.5 ~ 2㎖를 투입, 교반하여 카로테노이드(carotenoid)류를 제거하고 라이코펜(lycopene)을 용출하며, 상기 용출된 라이코펜을 여과, 건조 및 분말화하여 정제 라이코펜을 제조하는 라이코펜 정제단계(S3); 및
상기 라이코펜 분말 0.006 ~ 0.008g에 5 ~ 20㎖의 계면활성제를 30 ~ 70℃에서 30분 ~ 2시간 동안 교반, 가열하여 수용성 라이코펜을 제조하는 라이코펜 수용화단계(S4);를 포함하여 구성되되,
상기 추출용매는,
에틸아세테이트(ethyl acetate)인 것을 특징으로 하는 토마토 유래 정제 라이코펜 및 수용성 라이코펜의 수득방법
In the method for obtaining purified lycopene and water-soluble lycopene derived from tomato,
A crude extract manufacturing step of preparing a crude extract from tomato powder by filling 40 ~ 60 g of dried tomato powder in a column equipped with a glass filter, and then adding 0.5 ~ 2 L of an extraction solvent. (S1);
Concentrate manufacturing step (S2) for producing a concentrate from the crude extract by using the vacuum condenser extract removed;
0.5-2 ml of the concentrate was added to 0.5-2 L of the antisolvent, followed by stirring to remove carotenoids, eluting lycopene, and filtering, drying, and powdering the eluted lycopene to produce purified lycopene. Lycopene purification step (S3); And
It comprises a; lycopene soluble step (S4) to prepare a water-soluble lycopene by stirring and heating the lycopene powder 0.006 ~ 0.008g 5 ~ 20ml of the surfactant at 30 ~ 70 ℃ for 30 minutes ~ 2 hours;
The extraction solvent,
Method for obtaining purified lycopene and water-soluble lycopene derived from tomato, characterized in that the ethyl acetate (ethyl acetate)
상기 반용매는,
0 ~ -20℃의 메탄올(methanol)인 것을 특징으로 하는 토마토 유래 정제 라이코펜 및 수용성 라이코펜의 수득방법
The method of claim 1,
The anti-solvent,
Method for obtaining purified lycopene and water-soluble lycopene derived from tomato, characterized in that methanol (methanol) of 0 ~ -20 ℃
상기 계면활성제는,
폴리옥시에틸렌 소르비탄 모노올레이트(Polyoxyethyelene Sorbitan Monooleate: Tween 80)인 것을 특징으로 하는 토마토 유래 정제 라이코펜 및 수용성 라이코펜의 수득방법The method of claim 1,
The surfactant is,
Method for obtaining purified lycopene and water-soluble lycopene derived from tomato, characterized in that the polyoxyethylene sorbitan monooleate (Polyoxyethyelene Sorbitan Monooleate: Tween 80)
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| CN116803404A (en) * | 2023-08-24 | 2023-09-26 | 汤臣倍健股份有限公司 | Application of water-soluble tomato concentrate in preparation of hair loss reducing and hair growing products |
| CN116803404B (en) * | 2023-08-24 | 2023-12-15 | 汤臣倍健股份有限公司 | Application of water-soluble tomato concentrate in preparation of hair loss reducing and hair growing products |
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