CN110790628B - Extraction method of lycopene - Google Patents
Extraction method of lycopene Download PDFInfo
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- CN110790628B CN110790628B CN201910923778.2A CN201910923778A CN110790628B CN 110790628 B CN110790628 B CN 110790628B CN 201910923778 A CN201910923778 A CN 201910923778A CN 110790628 B CN110790628 B CN 110790628B
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Abstract
The invention provides a method for extracting lycopene, which comprises the following steps: s1) crushing the dried momordica cochinchinensis pericarp to obtain primary crushed pericarp; s2) mixing the primary broken peel with water to prepare peel dough, and grinding the peel dough by using a three-roller grinder to obtain secondary ground peel; s3) freezing the secondary ground pericarp by liquid nitrogen and then grinding to obtain a tertiary ground pericarp; s4) extracting the three-stage ground pericarp by using supercritical carbon dioxide fluid to obtain lycopene. Compared with the prior art, the method provided by the invention has the advantages that the three-stage crushing is carried out on the pericarp of the momordica cochinchinensis, so that more red tomatoes stored in the cells are dissolved in the supercritical carbon dioxide fluid, and the extraction yield is improved.
Description
Technical Field
The invention belongs to the technical field of pigment extraction, and particularly relates to a method for extracting lycopene.
Background
Lycopene (lycopene) is a yellow/red carotenoid, widely found in nature. Lycopene was first isolated from berries by Hartsen in 1873 and was found to be a crystalline dark red pigment. Millardet extracted lycopene-containing crude extract from tomatoes in 1875, which was called Solanorbin. Schunck in 1903 found that lycopene was different from carotene extracted from carrots through studies on the absorption spectrum of lycopene, and thus named this pigment as lycopene, thereby establishing the name of lycopene. Subsequently, the chemical structure of lycopene was studied, and in 1910, Wllstatter and escherichia first proposed that lycopene is an isomer of carotene and determined to have the molecular formula C40H 56. In 1930 Karrer et al proposed that lycopene has a structural formula of 11 conjugated and 2 non-conjugated planar conjugated polyenes of carbon-carbon double bonds, and was confirmed in 1932 by Kuhn and gundinann. Lycopene, as a functional natural pigment, has various physiological functions of quenching active oxygen, eliminating free radicals of human bodies, slowing down atherosclerosis, preventing various cancers, protecting cardiovascular system and resisting aging, and also has the effects of preventing ultraviolet rays, beautifying and strengthening skin in cosmetics. Lycopene has been recognized as a type a nutrient by the united nations Food and Agriculture Organization (FAO), the food additive council (JECFA) and the World Health Organization (WHO), and has been widely used in the industries of food, health products, cosmetics and the like as a food additive having dual functions of nutrition and coloration in more than 50 countries and regions. At present, the development of lycopene health-related products has become a hot spot of international research on functional foods and new drugs. However, the bioavailability of lycopene is 0.1% -3.0%, and artificial pigments cause many food safety problems, so optimization and utilization rate improvement of natural pigment extraction methods are one of the problems to be solved urgently.
At present, the main source of lycopene is tomato, and common extraction techniques include solvent extraction, ultrasonic-assisted extraction, enzymatic extraction, microwave-assisted extraction and supercritical carbon dioxide fluid extraction.
The solvent extraction method utilizes the principle of similar intermiscibility, lycopene is extracted and separated from tissue fluid due to different solubilities of lycopene in different solvents, raw materials are generally required to be pretreated, then solvent extraction is carried out, then an extracting solution is concentrated to obtain a product, commonly used organic solvents comprise petroleum ether, normal hexane, chloroform, ether, acetone and the like, the extraction efficiency is low, the environment is polluted, and organic solvent residues exist.
The ultrasonic-assisted extraction method refers to the fact that ultrasonic waves can generate strong cavitation, vibration, mechanical stirring and the like, and plant cell walls are prone to being broken, so that active ingredients in plants are accelerated to enter a solvent, the extraction efficiency is greatly improved, however, organic solvents are still used for extraction in the extraction process, and only the extraction efficiency is higher than that of a common solvent extraction method.
The enzymolysis-assisted extraction method is a mild and environment-friendly extraction method, and is characterized in that specific enzyme is used for degrading or destroying pectin, glycoprotein, cellulose and hemicellulose in cell walls or cell membranes, so that bioactive substances are released from the cells, organic solvents can be reduced, the extraction speed is increased, the extraction yield is improved, but the organic solvents are still used for extraction in the extraction process, so that the environment is polluted, and organic solvent residues exist.
The microwave-assisted extraction technology is a novel chemical separation technology which utilizes the multi-stage effects of microwave such as thermal effect, biological effect and the like to assist and strengthen solvent extraction, and microwave is used for heating inside and outside simultaneously through ion conduction and dipole rotation. The heating effect can be improved by adding polar organic solvents (ethanol, methanol and the like) or salts, but the organic solvents are still adopted for extraction in the extraction process, so that the extraction efficiency is low, the environment is polluted, and organic solvent residues exist.
Supercritical fluid extraction is a separation technique in which a fluid is caused to extract a target component in a state higher than a critical temperature and a critical pressure by increasing temperature and pressure. In the supercritical state, the fluid has a density close to that of liquid, a viscosity close to that of gas and a diffusivity between the two. The principle of extraction is to change the density of a supercritical fluid by changing the temperature or pressure, thereby changing the solvency power of the fluid. The extraction method has the advantages of low extraction temperature, effective retention of lycopene activity, high extraction efficiency, no solvent residue in the extract, and environmental friendliness, but the extraction efficiency still needs to be improved, and the extract still needs to be purified.
The lycopene purification method mainly comprises saponification, chromatography, recrystallization and membrane separation. The saponification method comprises adding alkaline solution into crude extract of lycopene to make acidic impurities such as fatty acid react with alkali to generate water-soluble substance, washing the reactant with water to neutrality, and removing water-soluble impurities and excessive alkali to obtain pure lycopene; the chromatography is the main method for separating and purifying lycopene at present, mainly comprises preparative thin-layer chromatography, column chromatography and high performance liquid chromatography, and the preparative thin-layer chromatography has limited separation and purification amount and general separation effect; the high performance liquid chromatography has good separation and purification effects, but the separation amount is relatively small; the column chromatography has low cost, large separation and purification amount and is more common in use; recrystallization is also a more efficient method for purifying lycopene. The method is simple to operate, high in separation efficiency and suitable for the requirement of industrial production, and normal hexane is usually used as a recrystallization solvent; the membrane separation method takes a selective permeation membrane as a separation medium, realizes physical separation, purification and enrichment of a multi-component mixture by utilizing the difference of the permeability of the membrane to each component of the mixture, can be operated at normal temperature, does not damage chemical components to be separated in the separation process, can ensure that the impurity rejection rate in a lycopene extracting solution reaches more than 60 percent, and obviously improves the purity of products. However, lycopene obtained by these purification methods is not separated from organic solvents, is not environment-friendly, and has a risk of organic solvent residue, while obtaining high-purity tomato red is more difficult.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a method for extracting lycopene.
The invention provides a method for extracting lycopene, which comprises the following steps:
s1) crushing the dried momordica cochinchinensis pericarp to obtain primary crushed pericarp;
s2) mixing the primary broken peel with water to prepare peel dough, and grinding the peel dough by using a three-roller grinder to obtain secondary ground peel;
s3) freezing the secondary ground pericarp by liquid nitrogen and then grinding to obtain a tertiary ground pericarp;
s4) extracting the three-stage ground pericarp by using supercritical carbon dioxide fluid to obtain lycopene.
Preferably, the particle size of the primary broken peel is 2-4 mm.
Preferably, the mass ratio of the primary broken peel to water is 1: (0.5 to 1.5).
Preferably, the gap between the middle roller and the rear roller of the three-roller grinding machine is 0.02-0.25 mm; the gap between the middle roller and the front roller is 0.01-0.25 mm.
Preferably, the grain size of the secondary grinding peel is 0.21-0.7 mm; the grain size of the three-stage ground peel is 4-7 mu m.
Preferably, the pressure extracted in the step S3) is 300 to 450 bar; the temperature is 70-90 ℃.
Preferably, the pressure extracted in step S3) is 350 bar; the temperature was 80 ℃.
Preferably, the three-stage ground pericarp is extracted using a supercritical carbon dioxide fluid extraction device; the supercritical carbon dioxide fluid extraction apparatus comprises:
an extraction tank;
a crystal separation tank; the upper end of the crystal separation tank is provided with an inlet, and the lower end of the crystal separation tank is provided with an outlet; the inlet of the crystal separation tank is communicated with the extraction tank through a pressure regulator; a filler is arranged in the crystal separation tank; the tank wall of the crystal separation tank is provided with cooling equipment;
a separator; the separator is communicated with the outlet of the crystal separation tank;
a cooler; the cooler is communicated with the separator;
a carbon dioxide liquefaction unit; the carbon dioxide liquefying device is communicated with the cooler;
a heating device; the carbon dioxide liquefying device is communicated with the extracting tank through a heating device.
Preferably, a first hollow baffle is arranged between the inlet of the crystal separation tank and the filler; a second hollow baffle is arranged between the outlet and the filler.
Preferably, the filler is a spherical filler; the cooling device on the tank wall of the crystal separation tank keeps the temperature in the crystal separation tank between 30 and 32 ℃.
The invention provides a method for extracting lycopene, which comprises the following steps: s1) crushing the dried momordica cochinchinensis pericarp to obtain primary crushed pericarp; s2) mixing the primary broken peel with water to prepare peel dough, and grinding the peel dough by using a three-roller grinder to obtain secondary ground peel; s3) freezing the secondary ground pericarp by liquid nitrogen and then grinding to obtain a tertiary ground pericarp; s4) extracting the three-stage ground pericarp by using supercritical carbon dioxide fluid to obtain lycopene. Compared with the prior art, the method has the advantages that the three-stage crushing is carried out on the pericarp of the momordica cochinchinensis, so that more lycopene stored in cells is dissolved in supercritical carbon dioxide fluid, and the extraction yield is improved.
Drawings
FIG. 1 is a schematic diagram of the procedure of breaking pericarp of Momordica cochinchinensis in example 1 of the present invention;
FIG. 2 is a schematic view of a supercritical carbon dioxide fluid extraction apparatus used in example 1 of the present invention;
FIG. 3 is a schematic view showing the structure of a crystal-separating tank used in example 1 of the present invention;
FIG. 4 is a SEM photograph of the primary crushed pericarp, the secondary ground pericarp and the tertiary ground pericarp of example 1 of the present invention;
FIG. 5 is a graph showing lycopene extraction efficiency curves of materials of different particle sizes in example 1 and comparative examples 1 and 6 to 7 of the present invention;
FIG. 6 is a graph of lycopene extraction efficiency at different extraction temperatures in comparative examples 1 to 3 of the present invention;
FIG. 7 is a graph of lycopene extraction efficiency at different extraction pressures of comparative examples 1 and 4 to 5 of the present invention;
FIG. 8 is a schematic view of a supercritical carbon dioxide fluid extraction apparatus used in comparative example 8 of the present invention;
FIG. 9 is a histogram of tomato red content at different positions in the extraction apparatus of example 1 of the present invention;
fig. 10 is a photograph of different locations in an extraction device according to embodiment 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a method for extracting lycopene, which comprises the following steps: s1) crushing the dried momordica cochinchinensis pericarp to obtain primary crushed pericarp; s2) mixing the primary broken peel with water to prepare peel dough, and grinding the peel dough by using a three-roller grinder to obtain secondary ground peel; s3) freezing the secondary ground pericarp by liquid nitrogen and then grinding to obtain a tertiary ground pericarp; s4) extracting the three-stage ground pericarp by using supercritical carbon dioxide fluid to obtain lycopene.
The present invention is not particularly limited in terms of the source of all raw materials, and may be commercially available.
The invention takes the pericarp of the Momordica cochinchinensis as an extraction raw material, the Momordica cochinchinensis fruit (Momoracia cochinchinensis Spreng) is the fruit with the highest carotenoid content discovered so far, and the aril of the Momordica cochinchinensis fruit contains rich lycopene and beta-carotene, so the Momordica cochinchinensis fruit is known as the fruit from heaven and is valued by many scholars at home and abroad. The fruit of momordica cochinchinensis consists of a pericarp, a mesocarp (pulp), a aril, a seed, and a connective tissue. Aril (seed membrane) is the edible part of Momordica cochinchinensis fruit, and has average mass of 240.26g, accounting for about 24.6% of fresh fruit mass, and is rich in lycopene and beta-carotene. The types and the contents of carotenoid and fatty acid in the momordica cochinchinensis fruit (including seeds) are analyzed by liquid chromatography, and the result shows that the total content of lycopene in the aril is 1546.5-3053.6 mug/g (wet mass) and is about 76 times of the content of lycopene in tomatoes (the content of lycopene in tomatoes is 40-50 mug/g wet mass), and the cis-form lycopene in the momordica cochinchinensis fruit accounts for 2.7-13.2%. Therefore, the momordica cochinchinensis not only contains rich lycopene, but also is a good source of carotene.
As the lycopene is fixedly stored in the cell structure, in order to enable the lycopene to be more easily dissolved in the supercritical carbon dioxide fluid, the cell structure is damaged by adopting a three-stage crushing mode, so that the intracellular lycopene is easily contacted with the supercritical carbon dioxide fluid, and the extraction of the lycopene is facilitated.
Crushing dried cochinchina momordica fruit peels to obtain primary crushed peels; the crushing is preferably carried out by a crusher; the crusher is preferably a horizontal crushing structure (when in operation, the movable knife and the fixed knife on the main shaft are matched with each other for crushing); the rotating speed of a main shaft of the crusher is preferably 300-500 r/min, and more preferably 400 r/min; the power of the crusher is preferably 2-3 kW, and more preferably 2.2 kW; the crushing frequency is preferably 1-4 times, more preferably 2-3 times, and further preferably 3 times; the particle size of the primary broken peel obtained after breaking is preferably 2-4 mm.
Mixing the primary crushed peel with water to prepare peel dough, and grinding by using a three-roller grinding machine to obtain secondary ground peel; the mass ratio of the primary broken peel to water is preferably 1: (0.5 to 1.5), more preferably 1: (0.8 to 1.2), and more preferably 1: 1; the preferred gap between the middle roller and the rear roller of the three-roller grinding machine is 0.02-0.25 mm; the preferred gap between the middle roller and the front roller is 0.01-0.25 mm; the grain size of the secondary grinding peel is preferably 0.21-0.7 mm.
Freezing the second-stage ground pericarp by using liquid nitrogen, and then grinding to obtain a third-stage ground pericarp; the grinding is preferably carried out by a mortar grinder; the secondary ground peel is preferably frozen by liquid nitrogen immersion; the weight ratio of the secondary ground peel to the liquid nitrogen is 1: (0.5 to 1.5), more preferably 1: (0.8-1.2), and preferably 1: 1; the liquid nitrogen is preferably mixed with the secondary ground peel for three times, and grinding is carried out after each mixing; the time for each grinding is preferably 5-20 min, more preferably 10-20 min, and further preferably 15 min; the particle size of the three-stage ground peel is preferably 4-7 μm.
Extracting the three-stage ground pericarp by using supercritical carbon dioxide fluid to obtain lycopene; the pressure of the supercritical carbon dioxide fluid extraction is preferably 300-450 bar, more preferably 320-400 bar, still more preferably 340-360 bar, and most preferably 350 bar; the extraction temperature is preferably 70 to 90 ℃, more preferably 75 to 85 ℃, and still more preferably 80 ℃.
The method is characterized in that the cell structure of the pericarp of the momordica cochinchinensis is physically broken, a three-stage breaking method is adopted, a breaker with a horizontal type breaking structure is adopted for primary breaking, the dried momordica cochinchinensis pericarp is broken into particles with the average particle size of about 1 millimeter through the primary breaking, but the particle size distribution range of the momordica cochinchinensis pericarp is very wide due to the limitation of a machine; the secondary grinding adopts a three-roller grinding machine for grinding, after the powder of the primary broken pericarp is mixed with a proper amount of water, the gap between a middle roller and a rear roller of the three-roller grinding machine is adjusted, and the pericarp powder of the secondary grinding is obtained after grinding, so that the particle size is reduced to 0.5 mm, and the pericarp is basically decomposed into single cells; the third-stage grinding adopts a mortar grinder for grinding after the liquid nitrogen is frozen, the damage of heat generated in the grinding process to the lycopene is reduced under the action of the liquid nitrogen, in addition, the cell walls of cells of the pericarp become brittle due to the rapid reduction of the temperature, and the cell walls of the pericarp cells are more easily damaged under the action of the grinder, so that the lycopene existing in the cell walls is favorably contacted with supercritical carbon dioxide fluid, the pericarp of the momordica cochinchinensis is crushed, the particle size which does not influence the extraction of the supercritical carbon dioxide fluid is obtained (the particle size can cause the powder to run out of an extraction tank and block a pipeline), and the extraction efficiency of the lycopene can be improved.
In the present invention, it is preferable to perform extraction using a supercritical carbon dioxide fluid extraction apparatus; the supercritical carbon dioxide fluid extraction apparatus comprises: an extraction tank; a crystal separation tank; the upper end of the crystal separation tank is provided with an inlet, and the lower end of the crystal separation tank is provided with an outlet; the inlet of the crystal separation tank is communicated with the extraction tank through a pressure regulator; a filler is arranged in the crystal separation tank; the tank wall of the crystal separation tank is provided with cooling equipment; a separator; the separator is communicated with the outlet of the crystal separation tank; a cooler; the cooler is communicated with the separator; a carbon dioxide liquefaction unit; the carbon dioxide liquefying device is communicated with the cooler; a heating device; the carbon dioxide liquefying device is communicated with the extracting tank through a heating device.
The supercritical carbon dioxide fluid extraction device comprises an extraction tank; the wall of the extraction tank is preferably provided with a heating device; the heating equipment is preferably hydrothermal equipment, in the invention, the wall of the extraction tank is preferably of a double-layer structure, a water inlet is arranged below the outer side tank wall, a water outlet is arranged above the outer side tank wall, and hot water is introduced between the double-layer tank walls through the water inlet so as to heat the extraction tank.
The extraction tank is communicated with the inlet of the crystal separation tank through a pressure regulator; the supercritical carbon dioxide fluid is used for dissolving lycopene and the extract of the pericarp oil of the momordica cochinchinensis in the extraction tank, then the pressure can be released through the pressure regulator, the carbon dioxide fluid discharged from the extraction tank is converted into a gas state from a supercritical state after the pressure is released, so that the solubility of the carbon dioxide fluid is reduced, and the extract of the pericarp oil of the momordica cochinchinensis dissolved in the carbon dioxide fluid and the lycopene are separated out. The crystal separation tank preferably comprises a first threaded end socket, a tank body and a second threaded end socket which are sequentially arranged; the first thread sealing head is provided with an inlet; an outlet is formed in the second threaded sealing head; the tank body is internally provided with a filler; the filler is preferably a spherical filler, more preferably glass beads; in order to avoid the situation that the filler is brought out of a blocked pipeline by fluid to cause overlarge local pressure, a first hollow baffle is preferably arranged between the inlet of the crystal separation tank and the filler, and a first hollow baffle is more preferably arranged between the first threaded end socket and the tank body; a second hollow baffle is preferably arranged between the outlet of the crystal separation tank and the filler, and a second hollow baffle is more preferably arranged between the tank body and the second threaded end enclosure; the aperture of the first hollow baffle and the aperture of the second hollow baffle are preferably smaller than the diameter of the filler; the tank wall of the crystal separation tank is provided with cooling equipment; the cooling equipment is preferably water cooling equipment, the tank wall of the crystal separation tank is preferably of a double-layer structure, a water inlet is formed below the tank wall on the outer side, a water outlet is formed above the tank wall on the outer side, and cooling water is introduced between the double-layer tank walls through the water inlet to cool the crystal separation tank. The temperature of the cooling water is preferably 27-29 ℃, and more preferably 28 ℃; the cooling water, i.e. the cooling device preferably keeps the temperature in the crystal separation tank at 30-32 ℃, more preferably at 31 ℃, so that the momordicae cochinchinensis oil extract and the lycopene dissolved in the carbon dioxide fluid are separated out at a lower temperature, and simultaneously, the lycopene dissolved in the momordicae cochinchinensis oil extract is also separated out due to sudden temperature drop, so that the extract stays in the crystal separation tank; the filling material filled in the crystal separation tank can increase the turbulence degree of fluid flow, increase the contact specific surface area so as to realize better heat exchange, finally separate out more lycopene crystals from the fluid and the extract so as to realize separation, simultaneously the separated crystals can also be blocked by the filling material and stay in the crystal separation tank, the momordica cochinchinensis pericarp grease extract is converged at the bottom of the crystal separation tank under the action of gravity, and is carried to the separator for re-separation and convergence under the action of carbon dioxide fluid, so that the lycopene crystals can be collected in the crystal separation tank without being attached to pipelines or other walls, and the high-purity lycopene can be directly obtained after the filling material in the crystal separation tank is centrifuged; the rotation speed of the centrifugation is preferably 5000-20000 rpm, more preferably 8000-15000 rpm, and further preferably 10000 rpm; the centrifugation time is preferably 5-20 min, more preferably 8-15 min, and further preferably 10 min; the centrifugation is preferably performed for 2-4 times, more preferably 3 times, and grease on the surface layer is removed each time, so that a purification step is not required.
The outlet of the crystal separation tank is communicated with the separator; the upper end of the separator is provided with a gas outlet; the lower end of the separator is provided with a liquid outlet, and the extract of the momordica cochinchinensis pericarp grease can be collected from the liquid outlet.
The gas outlet of the separator is communicated with the cooler; the gas is cooled by the cooler, and impurities such as moisture remaining in the gas can be removed.
The cooler is communicated with the carbon dioxide liquefying device; the carbon dioxide liquefying device liquefies the carbon dioxide gas coming out of the cooler for reuse.
The carbon dioxide liquefying device is preferably communicated with the extracting tank sequentially through a pressurizing device and a heating device; preferably, an evacuation valve is arranged between the pressurizing device and the heating device and used for evacuating air in the pressurizing device, so that the pressurizing device is filled with liquid carbon dioxide, and the pressurizing device can be directly pressurized after being started conveniently; in addition, in the process of emptying the carbon dioxide, the temperature of the pressurizing device is reduced after the liquid carbon dioxide is gasified, and the carbon dioxide is favorably stored in the pressurizing device.
According to the present invention, it is preferable to further include a carbon dioxide replenishment tank; the carbon dioxide supplement tank is communicated with the extraction tank through a pressurizing device and a heating device so as to supplement the loss of carbon dioxide in the extraction process.
According to the invention, the pericarp of the momordica cochinchinensis fruit is subjected to three-stage crushing, so that the tomato red color stored in the cell is more dissolved in the supercritical carbon dioxide fluid, and the extraction yield is improved; further, by optimizing the supercritical carbon dioxide fluid extraction process of the cochinchina momordica fruit peel, lycopene with high yield is obtained; and a supercritical carbon dioxide fluid extraction device is further improved, so that the high-purity lycopene can be obtained from the pericarp of the momordica cochinchinensis by a one-step method without adopting a solvent. .
In order to further illustrate the present invention, the following will describe the extraction method of lycopene provided by the present invention in detail with reference to the examples.
The reagents used in the following examples are all commercially available.
Example 1
First stage (steps a to b in FIG. 1): crushing the dried momordica cochinchinensis fruit peel by using a common crusher to obtain primary crushed peel; the crusher is preferably a horizontal crushing structure (when in operation, the movable knife and the fixed knife on the main shaft are matched with each other for crushing); the rotating speed of the main shaft is 400 r/min; the power of the crusher is 2.2 kW; the number of the crushing times was 3. The particle size of the primary broken peel is: 2-4 mm.
Second stage (c-d steps in FIG. 1): then according to the primary breaking peel: water 1: 1(w/w), the primary crushed pericarp is made into dough package. The momordica cochinchinensis pericarp dough is then passed through a three roll grinder to obtain a secondary ground pericarp. (the normal working time of the rollers is within the range of 0.02-0.25 mm of the gap between the middle roller and the rear roller and 0.01-0.25 mm of the gap between the middle roller and the front roller). The grain size of the secondary ground peel is: 0.21 to 0.7 mm.
Third stage (step f in fig. 1): soaking the secondary ground peel in liquid nitrogen, and grinding by using a mortar grinder to obtain a tertiary ground peel; the mass ratio of the secondary grinding peel to the liquid nitrogen is 1: and 1, mixing liquid nitrogen with the secondary grinding peel for three times, and grinding after each mixing, wherein the grinding time is 15 min. The grain size of the tertiary grinding peel is as follows: 4-7 μm.
Extracting with supercritical carbon dioxide fluid at 350bar with the extraction equipment shown in FIG. 2; the temperature is 80 ℃; centrifuging the filler in the crystal separation tank to obtain high-purity lycopene directly, wherein the centrifugation parameter is 10000RPM, the time is 10 minutes, the time is 3, the grease on the surface layer is removed each time, and the purity of the lycopene collected in the crystal separator is 95%; lycopene in the Momordica cochinchinensis fruit peel oil extract in the separator is in a dissolved state, and the specific content can be analyzed by HPLC to obtain the concentration of lycopene in the Momordica cochinchinensis fruit peel oil extract, so that the final yield of lycopene is calculated. In fig. 2, 1 is an extractor, 2 is a back pressure regulator, 3 is a separator, 4 is a cooler, 5 is a carbon dioxide liquefying device, 6 is a carbon dioxide replenishing tank, 7 is a pressurizing device, 8 is an emptying valve, 9 is a heating device, 10 is an outlet of the separating tank, 11 is an outlet of the carbon dioxide, 12 is an emptying pipe, and 13 is a crystal separating tank.
FIG. 3 is a schematic structural view of a crystal separating tank;
the crystal separating tank is divided into a tank body and threaded end sockets at two ends, the upper end of the crystal separating tank is an inlet and is connected with an outlet of a pressure regulator (BPR), and the lower end of the crystal separating tank is an outlet and is connected with an inlet of the original separating tank. The upper end and the lower end of the crystal separating tank are provided with two hollowed-out baffles which are consistent with the inner diameter of the separating tank, and the diameter of the hollowed-out baffles is smaller than that of a glass ball used for filling the crystal separating tank. The crystal separating tank is designed as a double-layer water jacket, and cooling water enters and exits from the crystal separating tank under the cooling water.
The primary crushed peel, secondary ground peel and tertiary ground peel were analyzed by scanning electron microscope to obtain a scanning electron micrograph, which is shown in fig. 4.
Comparative example 1
The extraction method is the same as example 1, except that the secondary ground pericarp is used as the extraction raw material.
Comparative example 2
The extraction method is the same as example 1, except that the secondary ground pericarp is used as the extraction raw material, and the extraction temperature is 60 ℃.
Comparative example 3
The extraction method is the same as example 1, except that the secondary ground pericarp is used as the extraction raw material, and the extraction temperature is 70 ℃.
Comparative example 4
The extraction method is the same as example 1, except that the secondary ground pericarp is used as the extraction raw material, and the extraction pressure is 250 bar.
Comparative example 5
The extraction method is the same as example 1, except that the secondary ground pericarp is used as the extraction raw material, and the extraction pressure is 300 bar.
Comparative example 6
The extraction method was the same as example 1 except that the primary crushed pericarp was used as the extraction raw material.
Comparative example 7
The extraction method is the same as that of example 1, except that crushed pericarp with the particle size of 710-2000 microns (the pericarp powder after primary grinding is respectively obtained by sieving with a sieve with 10 meshes and 25 meshes) is used as an extraction raw material.
The extraction efficiency (calculated by the total amount of lycopene in the crystal separation tank and lycopene in the oil extract of cochinchina momordica fruit peel in the separator) of the lycopene obtained in example 1 and comparative examples 1-7 is shown in fig. 5-7, wherein fig. 5 is a graph of the extraction efficiency of lycopene from materials with different particle sizes; FIG. 6 is a graph of lycopene extraction efficiency at different extraction temperatures; fig. 7 is a graph of lycopene extraction efficiency at different extraction pressures.
As can be seen from fig. 5 to 7, the optimal conditions for extracting lycopene from the pericarp of momordica cochinchinensis by supercritical fluid carbon dioxide fluid are as follows: pressure: 350 bar; temperature: the particle size is 4-7 microns at 80 ℃. The yield of the lycopene is improved from 27.28 percent to 91.96 percent and is improved to 64.62 percent.
Comparative example 8
The extraction apparatus shown in FIG. 8 was used to extract supercritical carbon dioxide fluid, and the other steps were the same as in example 1. In fig. 8, 1 is an extractor, 2 is a back pressure regulator, 3 is a separator, 4 is a cooler, 5 is a carbon dioxide liquefaction device, 6 is a carbon dioxide supplement tank, 7 is a pressurization device, 8 is an evacuation valve, 9 is a heating device, 10 is a separator tank outlet, 11 is a carbon dioxide outlet, and 12 is an evacuation pipe.
The content of tomato red at different positions of the extraction equipment adopted in example 1 and the extraction equipment adopted in comparative example 8 was measured, and the results are shown in table 1, fig. 9 and fig. 10; fig. 9 is a histogram of tomato red content at different positions in the extraction apparatus of example 1, and fig. 10 is a photograph of different positions in the extraction apparatus of example 1, from top to bottom, of the Momordica cochinchinensis pericarp oil extract, the crystal separator, and the Momordica cochinchinensis pericarp powder.
TABLE 1 lycopene content in different positions
Example 2
The procedure of example 1 was followed except that the particle size of the three-stage ground pericarp was: 5 microns, which was compared to the efficiency of other methods of extraction, and the results are shown in table 2.
Table 2 comparison of example 2 with different literature methods
Comparative example 9
Directly grinding the dried Momordica cochinchinensis pericarp by a three-roll grinder to obtain ground powder, and extracting under the same other extraction conditions as in example 1.
The yield of lycopene was 63.57%.
Comparative example 10
Directly grinding the dried cochinchina momordica fruit peel by a three-roll grinder, soaking the ground cochinchina momordica fruit peel in liquid nitrogen, grinding the rinded cochinchina momordica fruit peel to obtain ground powder, and extracting the ground powder under the other extraction conditions the same as those in the example 1.
The yield of lycopene was 72.08%.
Comparative example 11
The primary crushed pericarp of example 1 was soaked in liquid nitrogen and ground to obtain ground powder, and the extraction conditions were the same as in example 1.
The yield of lycopene was 49.33%.
Comparative example 12
The dried pericarp of momordica cochinchinensis is directly soaked in liquid nitrogen and then ground to obtain ground powder for extraction, and the extraction conditions are the same as those in example 1.
The yield of lycopene was 43.35%.
Claims (9)
1. A method for extracting lycopene, which is characterized by comprising the following steps:
s1) crushing the dried momordica cochinchinensis pericarp to obtain primary crushed pericarp;
s2) mixing the primary broken peel with water to prepare peel dough, and grinding the peel dough by using a three-roller grinder to obtain secondary ground peel;
s3) freezing the secondary ground pericarp by liquid nitrogen and then grinding to obtain a tertiary ground pericarp;
s4) extracting the three-stage ground pericarp by using supercritical carbon dioxide fluid to obtain lycopene;
extracting the three-stage ground pericarp by using a supercritical carbon dioxide fluid extraction device; the supercritical carbon dioxide fluid extraction apparatus comprises:
an extraction tank;
a crystal separation tank; the upper end of the crystal separation tank is provided with an inlet, and the lower end of the crystal separation tank is provided with an outlet; the inlet of the crystal separation tank is communicated with the extraction tank through a pressure regulator; a filler is arranged in the crystal separation tank; the tank wall of the crystal separation tank is provided with cooling equipment;
a separator; the separator is communicated with the outlet of the crystal separation tank;
a cooler; the cooler is communicated with the separator;
a carbon dioxide liquefaction unit; the carbon dioxide liquefying device is communicated with the cooler;
a heating device; the carbon dioxide liquefying device is communicated with the extracting tank through a heating device.
2. The extraction process according to claim 1, wherein the primary crushed peel has a particle size of 2 to 4 mm.
3. The extraction method according to claim 1, wherein the mass ratio of the primary broken peel to water is 1: (0.5 to 1.5).
4. The extraction method according to claim 1, wherein the gap between the middle roller and the rear roller of the three-roller mill is 0.02 to 0.25 mm; the gap between the middle roller and the front roller is 0.01-0.25 mm.
5. The extraction method according to claim 1, wherein the secondary ground peel has a particle size of 0.21 to 0.7 mm; the grain size of the three-stage ground peel is 4-7 mu m.
6. The extraction method according to claim 1, wherein the pressure of the extraction in step S3) is 300 to 450 bar; the temperature is 70-90 ℃.
7. The extraction method according to claim 1, wherein the pressure of the extraction in step S3) is 350 bar; the temperature was 80 ℃.
8. The extraction method according to claim 1, wherein a first hollow baffle is arranged between the inlet of the crystal separation tank and the filler; a second hollow baffle is arranged between the outlet and the filler.
9. The extraction method according to claim 1, characterized in that the filler is a spherical filler; the cooling device on the tank wall of the crystal separation tank keeps the temperature in the crystal separation tank between 30 and 32 ℃.
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| CN1364832A (en) * | 2002-02-07 | 2002-08-21 | 山东大学 | Method for extracting and separating lycopene from tamato |
| CN101611878A (en) * | 2009-04-14 | 2009-12-30 | 中国科学院武汉植物园 | The preparation method of carotenoids in the Momordica cochinchiensis fruit |
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| CN1364832A (en) * | 2002-02-07 | 2002-08-21 | 山东大学 | Method for extracting and separating lycopene from tamato |
| CN101611878A (en) * | 2009-04-14 | 2009-12-30 | 中国科学院武汉植物园 | The preparation method of carotenoids in the Momordica cochinchiensis fruit |
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