WO2016204544A1 - Method for efficiently extracting lycopene from plant - Google Patents

Abstract

The present invention relates to a method for efficiently mass extracting lycopene, which is an oil-soluble carotenoid compound, from a plant containing lycopene and, specifically, to a method for efficiently extracting lycopene by dehydrating a plant containing lycopene such that the plant contains suitable water content, and then forcibly mixing and infiltrating a nonpolar organic solvent thereinto. The extraction method of the present invention forcibly mixes a nonpolar organic solvent with fruit pulp meal tissue such that the nonpolar organic solvent can be infiltrated into the cellulose of the tissue, thereby being capable of maximizing the extraction efficiency of lycopene. In addition, the extraction method of the present invention can control the water content to be at the level capable of blocking contact with oxygen in the air through a dehydration step by means of an alcohol, thereby maximizing the breakage of lycopene caused by oxidation during a concentration step.

Description

How to efficiently extract lycopene from plants

The present invention relates to a method for the efficient mass extraction of lycopene from a plant comprising lycopene, which is a fat-soluble carotenoid-based compound, and specifically, a plant containing lycopene has undergone a process of dehydrating with alcohol to contain appropriate moisture. Thereafter, the present invention relates to a method for extracting lycopene efficiently by forcibly mixing the nonpolar organic solvent.

This application claims priority based on Korean Patent Application No. 10-2015-0085957 filed on June 17, 2015, and all the contents disclosed in the specification and drawings of the application are incorporated in this application.

Lycopene (molecular formula C ₄₀ H ₅₆ ) is a lipophilic carotenoid in the form of an acyclic chain having eleven conjugated double bonds, and is a pigment component that gives a variety of red fruits. Specifically, in addition to tomatoes, watermelon, persimmons, etc. are 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 free radicals that damage cells and, along with vitamins E, C, and other compounds as antioxidants and free-radical phagocytes, has been shown to reduce the antioxidant mechanisms in humans and organisms. Play a major role. Lycopene has also been shown to interact with low-density lipoproteins, which reduce the oxidation of cholesterol and other lipids, to prevent blood vessel damage, further demonstrating the inverse correlation between lycopene levels in the blood and prostate cancer.

In order to extract lycopene from such plants, it is common to first dry the plants to remove moisture and then extract them using a solvent. Meanwhile, Korean Patent No. 0849156 discloses a technique for preparing an extract of lycopene concentrated using supercritical carbon dioxide from watermelon flesh.

On the other hand, it is known to use a mixed solvent of a polar solvent and a nonpolar solvent as a method of extracting the nonpolar component without drying the plant as described above. Specifically, the mixture is forcibly mixed with the plant using methanol-chloroform or hexane-acetone-ethanol mixed solvent, the non-polar component is dissolved and transferred to the mixed solvent, and then phase separation is performed by adding an excessive amount of a polar solvent such as water to the mixed solvent. ) Is used to isolate the nonpolar solvent and then recover the useful nonpolar material eluted in the nonpolar solvent.

However, the method has a high cost of recovering the mixed solvent or the cost of extraction due to the loss of the solvent, so that the economic competitiveness of the extract product is low, which is problematic in industrial application.

Therefore, the development of a new technology that can efficiently extract a large amount of lycopene from the plant is constantly required.

Accordingly, the present inventors have conducted research and efforts to provide an industrially applicable method for mass extraction of lycopene, and as a result, when lycopene-containing plants are mixed with alcohol and dehydrated to a certain level, a non-polar organic solvent is forcedly mixed to obtain lycopene extract. The present invention has been completed by discovering that lycopene is prevented from being oxidized and destroyed and that extraction efficiency can be improved.

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

The present invention,

Preparing an alcohol mixture by mixing the fruit of the plant containing lycopene with an alcohol of C ₁ to C ₄ ;

Filtering the alcohol mixture to separate the liquid component and the cake;

Obtaining a first extract by stirring the pulp cake with a nonpolar organic solvent having a dielectric constant of 6.0 or less;

Characterized by the method of extracting lycopene from the plant comprising the step of removing the solvent from the primary extract to obtain a final extract.

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

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

In addition, the extraction method of the present invention is characterized in that the seed of the fruit is removed, and after separation of the pulp and the juice, the juice is mixed with alcohol of C ₁ ~ C ₄ to prepare an alcohol mixture.

In addition, the extraction method of the present invention is characterized in that the extract obtained by stirring the pulp thin film at 40 ~ 70 ℃ with a non-polar organic solvent.

In addition, the extraction method of the present invention is characterized in that the pulp thin film is stirred with a nonpolar organic solvent at 50 to 900 rpm.

In addition, the extraction method of the present invention is characterized in that the nonpolar organic solvent is one or two or more solvents selected from 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 by obtaining the final extract by removing the solvent by vacuum drying the primary extract.

Extraction method of the present invention by forcibly mixing the non-polar organic solvent with the pulverulent tissue to enable penetration into the fibers of the tissue, it is possible to maximize the extraction efficiency of lycopene.

In addition, the extraction method of the present invention can adjust the moisture content to a level that can prevent contact with oxygen in the air through the dehydration process with alcohol, it is possible to minimize the destruction by oxidization of lycopene during the concentration process.

1 is a schematic diagram showing an extraction process of lycopene according to Example 1 of the present invention.

Figure 2 is a schematic diagram showing the extraction process of lycopene according to Example 2 of the present invention.

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

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

The fruit of the plant is advantageous to increase the lycopene extraction efficiency and purity by removing the seed so that the 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 and the juice in advance may be mixed with the alcohol, and the pulp and the juice may be separated using a centrifuge. In addition, it is also possible to prepare an alcohol mixture by mixing the fruit and the alcohol of the plant from which the seed is removed without undergoing the separation process of the pulp and juice, in which case the centrifugation process can be omitted.

As alcohol mixed with the fruit of the plant, alcohols of C ₁ to C ₄ are used, preferably methanol or ethanol, and most preferably ethanol. At this time, the alcohol is preferably used 1 to 10 times the weight, more preferably 2 to 5 times the weight of the fruit or fruit weight of the plant.

Next, the alcohol mixture is filtered and separated into a liquid component and a pulp cake. The pulp is dehydrated to a certain level to remove moisture contained in a large amount of plant fruit.

Lycopene exhibits acyclic chain structure and needle-like crystal structure, and the needle-like structure is accumulated as fibrillar filament in the plant tissue, and the outside of the fiber is hydrophilic and water is bound to prevent the contact between lycopene and oxygen in the air. . When the water is completely removed, the infiltrating lycopene crystal is exposed to air and destroyed by oxidation. Therefore, in the present invention, dehydration is performed only to the extent that lycopene is prevented from contacting oxygen in the air by using C ₁ to C ₄ alcohols, preferably ethanol, and the moisture content of the pulp obtained through the process is 35 It is preferable to represent -50 wt%.

Next, the pulp 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 primary extract.

The non-polar organic solvent may penetrate into the fiber of the dehydrated pulp to maximize the extraction efficiency of lycopene, and a dielectric constant of 6.0 or less, more preferably 5.3 or less, may be applied.

As the nonpolar organic solvent, one or two or more solvents selected from ethyl acetate, hexane, chloroform, toluene, pentane, hexane, heptane, octane, oleic acid and linoleic acid may be used. Preferably, ethyl acetate, hexane Or chloroform.

The stirring extraction is preferably made at 40 to 70 ° C, more preferably 50 to 60 ° C. If the temperature of the stirring extraction is too high, the antioxidant activity of the lycopene to be extracted is low, and if the temperature of the stirring extraction is too low, there is a problem that the extraction efficiency is lowered.

The agitation may be performed at a rate of 50 to 900 rpm, and in the case of a solvent having a relatively high dielectric constant such as ethyl acetate or chloroform, it is easy to penetrate into the pulp thin film 100 to 500 rpm, more preferably 200 to 400 rpm. The extract can be obtained by stirring at a speed, but 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 to undergo strong stirring with a homogenizer.

In addition, the nonpolar organic solvent is preferably used in an amount of 1 to 10 times the weight of the pulp thin film, and more preferably in an amount of 2 to 5 times the increase.

The extract obtained through the stirring extraction process using the non-polar organic solvent may be filtered, and the non-polar organic solvent may be additionally added to the separated extraction foil, and the stirring extraction may be repeated, and the extract may be mixed with the primary extract.

Finally, the final extract may be obtained by removing the non-polar organic solvent from the primary extract, and more specifically, after stirring and dispersing using an alcohol of C ₁ to C _4, the non-polar organic solvent may be removed through cooling and filtration. And, preferably, it can be obtained in powder form through a drying process.

Through the above process it is possible to obtain a high purity lycopene, the final extract of the lycopene is concentrated can be added to food to further enhance the functionality. The foods include fruits, vegetables, dried or cut products thereof, fruit juices, vegetable juices, mixed juices or beverages containing acidic beverages, cookies, candies, caramels, gums, etc. Fermented dairy foods such as tea, tea, yogurt, dairy foods, condiments, alcoholic beverages, canned or bottled foods, noodles, livestock processed foods, fish processed foods, microbial fermented foods, legumes foods, cereal foods, processed meats, licorice And herbs.

The present invention will be described in detail through the following examples. However, this is only to aid the understanding of the invention, the present invention should not be considered to be limited thereto.

Example 1

Autumn olives removed from foreign bodies and washed with water ( Elaeagnus) 100 kg of the fruit of umbellata ) was put into a pulp finisher to remove seeds, and then centrifuged at 500 rpm for 30 minutes to separate fruit and juice. Three times the weight of ethanol was added to 26.5 kg of the separated flesh and stirred at 50 ° C. for 20 minutes to obtain an ethanol mixture. Next, the ethanol mixture was cooled to room temperature and then filtered to separate the liquid component and the pulp. As a result of measuring the moisture content of the pulp was found to be 40% by weight.

Next, 22 kg of the pulp meal was placed in a sealed extractor equipped with a stirrer, and ethyl acetate, which was preheated to 50 ° C., was added thereto, and extracted by stirring at 300 rpm for 30 minutes. The extraction mixture obtained through the stirring extraction process was filtered and separated into a first extraction solution and an extraction foil, and added to the extraction foil by addition of three times the weight of ethyl acetate preheated to 50 ° C. and extracted with stirring for 30 minutes. It filtered again and obtained the 2nd extract.

The first extract and the second extract were mixed to prepare 3.065 kg of primary extract. Next, 1.2 kg of ethanol heated to 50 ° C. was added to the primary extract, stirred, and dispersed, and then cooled to room temperature and filtered. As the solvent was removed by drying with nitrogen gas, 696 g of a powdery final extract having a lycopene purity of 35% was obtained, and a recovery rate of lycopene was found to be 43.5%.

The extraction process of the lycopene was modeled in Figure 1, the change of the lycopene content in the extraction process is shown in Table 1 below.

process Quantity (kg) Lycopene content Concentration (mg / kg) Gross weight (g) % Recovery Fall olive 100 559.6 560 100 Pulp 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

Autumn olives removed from foreign bodies and washed with water ( Elaeagnus) The fruit of umbellata ) was put into a pulp finisher, and three times the weight of ethanol was added to 20 kg of the pulp from which the seeds were removed and stirred at 50 ° C. for 1 hour to obtain an ethanol mixture. Next, the ethanol mixture was cooled to room temperature and then filtered to separate the liquid component and the pulp. As a result of measuring the moisture content of the pulp was found to be 45% by weight.

Next, 16 kg of the pulp meal was placed in a sealed extractor equipped with a stirrer, and ethyl acetate, which was preheated to 50 ° C., was added thereto, and extracted by stirring at 300 rpm for 30 minutes. The extraction mixture obtained through the stirring extraction process was filtered and separated into a first extraction solution and an extraction foil, and added to the extraction foil by addition of three times the weight of ethyl acetate preheated to 50 ° C. and extracted with stirring for 30 minutes. It filtered again and obtained the 2nd extract.

The first extract and the second extract were mixed to prepare 2.95 kg of the primary extract. Next, 1.2 kg of ethanol heated to 50 ° C. was added to the primary extract, stirred, and dispersed, and then cooled to room temperature and filtered. As the solvent was removed by drying with nitrogen gas, 650 g of a powdery final extract having a lycopene purity of 33% was obtained, and the recovery of lycopene was confirmed to be 42%.

The lycopene extraction process is schematically illustrated in Figure 2, it can be seen that the separation of the fruit juice and dehydration by ethanol at the same time can be replaced by the filtration process centrifugation process required for separation of the fruit juice.

Example 3

The extraction was carried out in the same manner as in Example 1 except that the mixture was stirred at a speed of 500 rpm for 30 minutes using hexane of three times the weight of the pulp. As a result, 665 g of a powdery final extract having a lycopene purity of 31% was obtained.

Example 4

Extraction was carried out in the same manner as in Example 2 except that the mixture was stirred at a speed of 500 rpm for 30 minutes using hexane of three times the weight of the pulp. As a result, 610 g of a powdery final extract having a lycopene purity of 28% was obtained.

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

Although the above description has been made with reference to embodiments of the present invention, this is merely exemplary, and a person skilled in the art to which the present invention pertains will understand that various modifications and equivalent other embodiments are possible. . Therefore, the true technical protection scope of the present invention will be determined by the claims described below.

Claims (9)

Preparing an alcohol mixture by mixing the fruit of the plant containing lycopene with an alcohol of C ₁ to C ₄ ; Filtering the alcohol mixture to separate the liquid component and the cake; Obtaining a first extract by stirring the pulp cake with a nonpolar organic solvent having a dielectric constant of 6.0 or less; Removing lycopene from the plant, characterized in that to obtain a final extract by removing the solvent from the primary extract. The method of claim 1, The plant is a method for extracting lycopene from the plant, characterized in that the autumn olives, tomatoes, papaya or watermelon. The method of claim 1, The alcohol is a method for extracting lycopene from the plant, characterized in that ethanol. The method of claim 1, The pulp gourd is a method for extracting lycopene from the plant, characterized in that the water content is dehydrated by 35 to 50% by weight. The method of claim 1, Removing the seed of the fruit, separating the pulp and juice, and then lycopene extract from the plant, characterized in that for mixing the juice with alcohol of C ₁ ~ C ₄ to prepare an alcohol mixture. The method of claim 1, Method for extracting lycopene from the plant, characterized in that the extract obtained by stirring the pulp gourd with a non-polar organic solvent at 40 ~ 70 ℃. The method of claim 1, A method for extracting lycopene from the plant, characterized in that the pulp gourd is stirred with a non-polar organic solvent at 50 ~ 900 rpm. The method of claim 1, The non-polar organic solvent is a method for extracting lycopene from the plant, characterized in that one or more solvents selected from ethyl acetate, hexane, chloroform, toluene, pentane, hexane, heptane, octane, oleic acid and linoleic acid. The method of claim 1, Method of extracting lycopene from the plant, characterized in that to remove the solvent by vacuum drying the primary extract to obtain a final extract.

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