KR20160149024A - A efficient method for extracting lycopene from plants - Google Patents

A efficient method for extracting lycopene from plants Download PDF

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KR20160149024A
KR20160149024A KR1020150085957A KR20150085957A KR20160149024A KR 20160149024 A KR20160149024 A KR 20160149024A KR 1020150085957 A KR1020150085957 A KR 1020150085957A KR 20150085957 A KR20150085957 A KR 20150085957A KR 20160149024 A KR20160149024 A KR 20160149024A
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lycopene
extract
alcohol
plant
organic solvent
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KR1020150085957A
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KR101745780B1 (en
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김동구
최낙현
이호완
장평익
김병선
나인호
맹진수
김철진
김종태
조용진
박방헌
김태은
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주식회사 조은푸드텍
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Priority to PCT/KR2016/006427 priority patent/WO2016204544A1/en
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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
    • 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
    • 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
    • A23V2200/00—Function of food ingredients
    • A23V2200/30—Foods, ingredients or supplements having a functional effect on health
    • 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
    • A23V2200/30—Foods, ingredients or supplements having a functional effect on health
    • A23V2200/308—Foods, ingredients or supplements having a functional effect on health having an effect on cancer prevention
    • 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
    • A23V2200/30—Foods, ingredients or supplements having a functional effect on health
    • A23V2200/326—Foods, ingredients or supplements having a functional effect on health having effect on cardiovascular health
    • 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
    • A23V2200/30—Foods, ingredients or supplements having a functional effect on health
    • A23V2200/3262—Foods, ingredients or supplements having a functional effect on health having an effect on blood cholesterol
    • 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
    • A23V2250/213—Lycopene
    • 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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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Nutrition Science (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Mycology (AREA)
  • Botany (AREA)
  • Cosmetics (AREA)

Abstract

More particularly, the present invention relates to a method for efficiently extracting lycopene from a plant containing lycopene, which is a fat-soluble cartonoid compound, and more particularly, to a method for efficiently extracting lycopene from a plant containing lycopene, To a method for efficiently extracting lycopene.
The extraction method of the present invention can maximize the extraction efficiency of lycopene by allowing the nonpolar organic solvent to be forcedly mixed with the pulp tissue to penetrate into the fibrous tissue of the tissue. In addition, the extraction method of the present invention can regulate the moisture content to a level that can prevent contact with oxygen in the air through dehydration process by alcohol, thereby minimizing destruction due to oxidation of lycopene in the concentration process.

Description

[0001] The present invention relates to a method for efficiently extracting lycopene from a plant,

The present invention relates to a method for efficiently mass-extracting lycopene from a plant containing lycopene, which is a fat-soluble cartonoid compound, and more particularly, to a method for efficiently extracting lycopene from a plant containing lycopene, And a method for efficiently extracting lycopene by forcedly mixing and impregnating a nonpolar organic solvent.

Lycopene (molecular formula C 40 H 56 ) is a non-cyclic chain-like fat-soluble carnenoid with 11 conjugate double bonds, a pigment component that reddish various fruits. Specifically, it is also contained in watermelons, persimmons, etc. in addition to tomatoes, and is also known as a powerful antioxidant that can prevent cancer and aging. It is well known that lycopene has an antioxidant activity that can effectively defend against cell-damaging free radicals. It is also known that antioxidants and free radicals, together with vitamin E, C and other compounds, It plays a major role. Lycopene has also been shown to interact with low density lipoproteins that reduce the oxidation of cholesterol and other lipids to prevent damage to blood vessels and further evidence of inverse correlation between blood lycopene levels and prostate cancer.

In order to extract lycopene from such a plant, the plant is first dried to remove moisture, and then extracted with a solvent. Korean Patent No. 0849156 discloses a technique for producing lycopene-enriched extracts from watermelon flesh using supercritical carbon dioxide.

On the other hand, it is known to use a mixed solvent of a polar solvent and a non-polar solvent as a method for extracting a non-polar component without drying the plant as described above. Specifically, a mixed solvent of methanol-chloroform or hexane-acetone-ethanol is mixed with the plant to dissolve the nonpolar component, and the solvent is transferred to the mixed solvent. Then, a polar solvent such as water is added to the mixed solvent in an excess amount, ) Is induced to separate the nonpolar solvent, and then the useful nonpolar material eluted in the nonpolar solvent is recovered.

However, this method has a problem in that it is difficult to apply industrially because the extraction cost is high due to the cost of recovering the mixed solvent or the loss of solvent and the economical competitiveness of the extracted product is low.

Therefore, there is a continuing need to develop a new technology capable of efficiently extracting lycopene in large quantities from plants.

Therefore, the present inventors have made efforts to provide a large-scale extraction method of industrially applicable lycopene. As a result, they have found that when a plant containing lycopene is dewatered to a certain level by mixing with alcohol, and a lycopene extract is obtained by forced- The inventors have found that lycopene can be prevented from being oxidized and destroyed, and the extraction efficiency can be enhanced, thereby completing the present invention.

Accordingly, it is an object of the present invention to provide a method for efficiently extracting lycopene from a plant.

According to the present invention,

Mixing the fruit of the lycopene-containing plant with an alcohol of C 1 -C 4 to prepare an alcohol mixture;

Separating the alcohol mixture into a liquid component and a flesh cake by filtration;

Stirring the resultant mixture with stirring in a nonpolar organic solvent having a dielectric constant of 6.0 or less to obtain a first extract;

And extracting the lycopene from the plant, which comprises the step of removing the solvent from the primary extract to obtain a final extract.

Further, the extraction method of the present invention is characterized in that the plant is olive, tomato, papaya or watermelon in autumn, and the alcohol is ethanol.

In addition, the extraction method of the present invention is characterized in that the moisture content of the fleshy foil is dehydrated to 35 to 50% by weight.

The extraction method of the present invention is characterized in that the seeds of the fruit are removed and the fruit juice and the juice are separated, and then the juice is mixed with the C 1 -C 4 alcohol to produce an alcohol mixture.

Further, the extraction method of the present invention is characterized in that the above-mentioned flesh-like foil is stirred and extracted with a non-polar organic solvent at 40 to 70 ° C to obtain a first extract.

In addition, the extraction method of the present invention is characterized in that the above-mentioned flesh and skin foil is stirred with a non-polar organic solvent at 50 to 900 rpm.

The extraction method of the present invention is characterized in that the nonpolar organic solvent is at least one solvent selected from the group consisting of ethyl acetate, hexane, chloroform, toluene, pentane, hexane, heptane, octane, oleic acid and linoleic acid.

In addition, the extraction method of the present invention is characterized in that the primary extract is vacuum-dried to remove the solvent to obtain a final extract.

The extraction method of the present invention can maximize the extraction efficiency of lycopene by allowing the nonpolar organic solvent to be forced into the fibrous tissue of the tissue by forced mixing with the pulp tissue.

In addition, the extraction method of the present invention can regulate the moisture content to a level that can prevent contact with oxygen in the air through dehydration process by alcohol, thereby minimizing destruction due to oxidation of lycopene in the concentration process.

FIG. 1 is a schematic view showing an extraction process of lycopene according to Example 1 of the present invention. FIG.
FIG. 2 is a schematic view showing the extraction process of lycopene according to the second embodiment of the present invention. FIG.

The present invention is a method for extracting lycopene from a plant, wherein a series of steps are as follows.

First, the fruit of a plant containing lycopene is mixed with a C 1 -C 4 alcohol to prepare an alcohol mixture. Plants containing lycopene include tomatoes, watermelons, papaya, or autumn olives ( Elaeagnus umbellata ), preferably autumn olives.

It is advantageous for the fruit of the plant to increase the extraction efficiency and purity of lycopene by removing seeds so that a large amount of oil contained in the seed is not included in the final extract.

When the fruit of the plant is mixed with alcohol, the pulp obtained by separating the pulp from the pulp can be mixed with the alcohol, and the pulp and the juice can be separated using a centrifuge. In addition, it is also possible to prepare an alcohol mixture by mixing the fruit of the plant with the seeds and the alcohol without the separation of the fruit and juice, and in this case, the centrifugation process can be omitted.

As the alcohol to be mixed with the fruit of the plant, C 1 -C 4 alcohol is used, preferably methanol or ethanol, and most preferably ethanol. In this case, the alcohol is preferably used in a weight of 1 to 10 times, more preferably 2 to 5 times, by weight of the fruit or fruit weight of the plant.

Next, the alcohol mixture is filtered to separate into a liquid component and a flesh cake, and the flesh of the flesh is dehydrated to a certain level to remove water contained in the plant fruit in a large amount.

Lycopene exhibits a non-cyclic chain structure and a needle-like crystal structure. The needle-like structure is piled up with fibrin filaments in the plant tissue, and the outer portion of the fibrin is hydrophilic and water is bonded to prevent lycopene from contacting oxygen in the air . When the water is completely removed, the infiltrated lycopene crystal is exposed to air and is destroyed by oxidation. Accordingly, in the present invention, dehydration proceeds only to the extent that lycopene can be prevented from contacting with oxygen in the air by using C 1 -C 4 alcohol, preferably ethanol. The moisture content of the flesh cake obtained through the above process is 35 By weight to 50% by weight.

Next, the flesh-like foil obtained by dehydration and filtration with alcohol is stirred and extracted with a nonpolar organic solvent having a dielectric constant of 6.0 or less to obtain a first extract.

The nonpolar organic solvent may penetrate into the fiber of the dehydrated fleshy foil to maximize extraction efficiency of lycopene. A solvent having a dielectric constant of 6.0 or less, more preferably 5.3 or less, may be applied.

The nonpolar organic solvent may be at least one solvent selected from ethyl acetate, hexane, chloroform, toluene, pentane, hexane, heptane, octane, oleic acid and linoleic acid, preferably ethyl acetate, hexane Or chloroform.

The stirring extraction is preferably carried out at 40 to 70 ° C, more preferably 50 to 60 ° C. When the temperature of the stirring extraction is too high, the antioxidative activity of the extracted lycopene is lowered, and when the stirring extraction temperature is too low, the extraction efficiency is lowered.

The stirring may be performed at a speed of 50 to 900 rpm. In case of a solvent having a relatively high dielectric constant such as ethyl acetate or chloroform, penetration into the flesh of the pulp is easy, so that it is preferably 100 to 500 rpm, more preferably 200 to 400 rpm The extracts can be obtained by stirring at a speed of about 5,000 rpm. However, a solvent having a relatively low dielectric constant such as hexane, heptane, octane or toluene is required to be stirred at 500 rpm or more or a strong agitation with a homogenizer.

The nonpolar organic solvent is preferably used in an amount of 1 to 10 times by weight, more preferably 2 to 5 times by weight, based on the weight of the pulp.

The non-polar organic solvent may be added to the separated extract to further extract the non-polar organic solvent. The extracted extract may be mixed with the first extract.

Finally, the non-polar organic solvent may be removed from the primary extract to obtain a final extract. More specifically, the non-polar organic solvent may be removed through cooling and filtration after stirring and dispersing using a C 1 -C 4 alcohol And preferably in the form of a powder through a drying process.

Through the above process, lycopene of high purity can be obtained, and the final extract of lycopene which is concentrated can be added to food to further enhance its functionality. Examples of the food include fruit, vegetable, dried or cut products thereof, fruit juice, vegetable juice, mixed juice thereof, beverages including acidic beverages, confectionery such as cookies, candy, caramel and gum, baked goods, ice cream products Fermented milk products such as yoghurt, dairy products, condiments, liquor, canned or bottled products, noodles, processed livestock products, processed marine products, fermented microbial foods, cereals, cereals, meat products, licorice , And Herb.

Hereinafter, the present invention will be described in detail with reference to examples. However, this is for the purpose of helping the understanding of the invention, and the present invention should not be construed as being limited thereto.

Example 1

100 kg of autumn olive ( Elaeagnus umbellata ) fruit, which had been washed with water and removed from the surface, was put into a pulp finisher to remove seeds and then centrifuged at 500 rpm for 30 minutes to separate the pulp and the juice. Three times the weight of ethanol was added to 26.5 kg of the separated pulp, and the mixture was stirred at 50 캜 for 20 minutes to obtain an ethanol mixture. Next, the ethanol mixture was cooled at room temperature and then filtered to separate the liquid component and the fleshy foil. The water content of the fleshy foil was determined to be 40% by weight.

Next, 22 kg of the above-mentioned fleshy poultry was placed in an extractor equipped with a stirrer, and 3 times by weight of ethyl acetate preheated to 50 DEG C was added and stirred for 30 minutes at 300 rpm for extraction. The extracted mixture obtained through the stirring and extraction process was separated by filtration, separated into a first extract and an extraction foil. Ethyl acetate, which had been preheated to 50 ° C, was added to the extracted foil, and the mixture was extracted with stirring for 30 minutes. And then filtered again to obtain a second extract.

The first extract and the second extract were mixed to prepare 3.065 kg of the first extract. Next, 1.2 kg of ethanol heated to 50 캜 was added to the first extract, dispersed with stirring, cooled to room temperature, and filtered. Then, as the solvent was completely removed by drying with nitrogen gas, 696 g of powdery final extract having a purity of 35% of lycopene was obtained, and the recovery rate of lycopene was 43.5%.

The lycopene extraction process is shown in FIG. 1, and changes in lycopene content during the extraction process are shown in Table 1 below.

process Quantity (kg) Lycopene content Concentration (mg / kg) Total amount (g) Recovery rate (%) Autumn olive 100 559.6 560 100 Flesh 22 2436.4 536 95.7 Primary extract 3.065 110000 337.2 60.1 Final extract 0.696 350000 243.5 43.5

Example 2

Remove the foreign matter and wash the surface of the fall olive ( Elaeagnus umbellata ) was added to a pulp finisher, to which 3 kg of ethanol was added to 20 kg of the pulp from which the seed had been removed, and the mixture was stirred at 50 ° C for 1 hour to obtain an ethanol mixture. Next, the ethanol mixture was cooled at room temperature and then filtered to separate the liquid component and the fleshy foil. The moisture content of the flesh-like foil was measured to be 45% by weight.

Next, 16 kg of the above-mentioned fleshy poultry was placed in an extractor equipped with a stirrer, and 3-fold by weight of ethyl acetate preheated at 50 DEG C was added and stirred for 30 minutes at 300 rpm for extraction. The extracted mixture obtained through the stirring and extraction process was separated by filtration, separated into a first extract and an extraction foil. Ethyl acetate, which had been preheated to 50 ° C, was added to the extracted foil, and the mixture was extracted with stirring for 30 minutes. And then filtered again to obtain a second extract.

The first extract and the second extract were mixed to prepare 2.95 kg of the first extract. Next, 1.2 kg of ethanol heated to 50 캜 was added to the first extract, dispersed with stirring, cooled to room temperature, and filtered. After drying with nitrogen gas to remove all of the solvent, 650 g of a powdery final extract having a purity of 33% of lycopene was obtained, and the recovery of lycopene was confirmed to be 42%.

The extraction process of the lycopene is shown in FIG. 2, and the separation of the juice and dehydration by ethanol are performed at the same time, so that the centrifugation process required for the separation of the juice can be replaced by the filtration process.

Example 3

Extraction was carried out in the same manner as in Example 1, except that the above-mentioned flesh-like foil was stirred at a speed of 500 rpm for 30 minutes using 3 times by weight hexane. As a result, 665 g of a powdery final extract of 31% purity of lycopene was obtained.

Example 4

Extraction was carried out in the same manner as in Example 2, except that the above-mentioned fleshy foil was stirred at a speed of 500 rpm for 30 minutes using hexane of 3 times the weight. As a result, 610 g of a final powdery powder of 28% purity of lycopene was obtained.

From the above examples, it was confirmed that the extract of lycopene having a purity of 30% or more can be produced at a high recovery rate through the extraction process of the present invention.

While the present invention has been described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. . Accordingly, the true scope of the present invention is to be determined by the following claims.

Claims (9)

Mixing the fruit of the lycopene-containing plant with an alcohol of C 1 -C 4 to prepare an alcohol mixture;
Separating the alcohol mixture into a liquid component and a flesh cake by filtration;
Stirring the resultant mixture with stirring in a nonpolar organic solvent having a dielectric constant of 6.0 or less to obtain a first extract;
And removing the solvent from the primary extract to obtain a final extract.
The method according to claim 1,
Wherein the plant is olive, tomato, papaya or watermelon in autumn.
The method according to claim 1,
Wherein the alcohol is ethanol. ≪ RTI ID = 0.0 > 11. < / RTI >
The method according to claim 1,
Wherein the flesh of the pulp is dehydrated to a moisture content of 35 to 50% by weight.
The method according to claim 1,
Removing the seeds of the fruit, separating the fruit juice and the juice, and then mixing the juice with the C 1 -C 4 alcohol to prepare an alcohol mixture.
The method according to claim 1,
And extracting the lycopene from the plant characterized in that the above-mentioned flesh-like foil is stirred and extracted with a non-polar organic solvent at 40 to 70 DEG C to obtain a first extract.
The method according to claim 1,
Wherein the pulp is stirred with a non-polar organic solvent at 50 to 900 rpm.
The method according to claim 1,
Wherein the nonpolar organic solvent is one or more solvents selected from the group consisting of ethyl acetate, hexane, chloroform, toluene, pentane, hexane, heptane, octane, oleic acid and linoleic acid.
The method according to claim 1,
And extracting the lycopene from the plant, wherein the primary extract is vacuum-dried to remove the solvent to obtain a final extract.
KR1020150085957A 2015-06-17 2015-06-17 A efficient method for extracting lycopene from plants KR101745780B1 (en)

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JP4192215B2 (en) * 2002-07-11 2008-12-10 株式会社望月鉄工所 Method for separating pulp and seeds in fruits
EP1886584A1 (en) * 2006-08-08 2008-02-13 Indena S.P.A. Stable and bioavailable compositions of isomers of lycopene for skin and hair
KR100849156B1 (en) * 2007-01-23 2008-07-30 한국식품연구원 Development of lycopene recovery by supercritical carbon dioxide extraction
KR101112053B1 (en) * 2011-06-20 2012-02-13 신라대학교 산학협력단 Method for obtaining purified lycopene and water-soluble lycopene from tomato
WO2013041935A1 (en) * 2011-09-19 2013-03-28 Omniactive Health Technologies Limited An efficient process for the preparation of lycopene containing oleoresin and lycopene crystals for human consumption
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