CN112645919A - Method for extracting flavonoid compounds in plants - Google Patents

Method for extracting flavonoid compounds in plants Download PDF

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CN112645919A
CN112645919A CN202011551946.9A CN202011551946A CN112645919A CN 112645919 A CN112645919 A CN 112645919A CN 202011551946 A CN202011551946 A CN 202011551946A CN 112645919 A CN112645919 A CN 112645919A
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extraction
extracting
eutectic solvent
plants
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邸多隆
王鹏波
刘建飞
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Lanzhou Institute of Chemical Physics LICP of CAS
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Lanzhou Institute of Chemical Physics LICP of CAS
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
    • C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
    • C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
    • C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
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    • A61K36/18—Magnoliophyta (angiosperms)
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    • A61K36/81—Solanaceae (Potato family), e.g. tobacco, nightshade, tomato, belladonna, capsicum or jimsonweed
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
    • C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
    • C07D311/40—Separation, e.g. from natural material; Purification
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    • 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
    • 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
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • 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
    • A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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Abstract

The invention discloses a method for extracting flavonoid compounds in plants, which comprises the steps of cleaning, drying and crushing the plants, and sieving the plants by a 50-mesh sieve to obtain dry plant powder; reacting choline chloride and ethylene glycol at 60-90 ℃ for 1-2 h to obtain transparent uniform liquid, cooling to room temperature, adding purified water, and mixing uniformly to obtain a eutectic solvent; placing the plant dry powder in a high-speed shearing machine, adding a eutectic solvent as an extraction medium, shearing and extracting at normal temperature, centrifuging after extraction is finished, and centrifuging to obtain lower-layer plant residues and a supernatant; and continuously shearing, extracting and centrifuging the plant residues, repeating for multiple times, and combining the supernatants to obtain plant extract which is a flavonoid compound. The method disclosed by the invention is rapid, efficient, environment-friendly, convenient, easy to industrialize, low in operation cost, wide in application range, high in flavone extraction rate and stable in physicochemical properties.

Description

Method for extracting flavonoid compounds in plants
Technical Field
The invention relates to a method for extracting flavonoid compounds in plants, in particular to a method for extracting the flavonoid compounds in the plants by combining flash extraction and eutectic solvent extraction and application, and belongs to the technical field of compound extraction and preparation.
Background
The flavonoid compounds are widely present in natural plants and belong to plant secondary metabolites. The flavonoids are yellow pigments derived from flavone (2-phenylchromone) as a parent nucleus, and comprise isomers of the flavone and hydrogenation and reduction products thereof. It exists in plant in most forms of glycosides or carbo-glycosyl combined with sugar, and in some forms of free form. Many studies have demonstrated that flavonoids are complex in the biosynthetic pathway in plants, being the biosynthetic products of the shikimic acid pathway and the acetate-malonate pathway, and that the basic skeleton of flavones is produced by the biosynthesis of 3 malonyl-coa and one coumaroyl-coa.
The flavonoids have wide distribution and are mostly present in higher plants and ferns. Most intensively distributed in angiosperm, such as more flavonoids in plants of Labiatae, Scrophulariaceae, Acanthaceae, Sonchusaceae, and Compositae; flavonols are widely distributed in dicotyledons, particularly in flowers and leaves of some woody plants; the flavanone is distributed more in Rosaceae, Rutaceae, Leguminosae, Ericaceae, Compositae, and Zingiberaceae; flavanonols are more commonly present in leguminous plants; isoflavones are present in a large amount in plants belonging to subfamily of Leguminosae and Iridaceae. Also exists in gymnosperms, such as biflavonoids which are multiply distributed in gymnosperms, in particular in plants of conidiomycetes, ginkgoceae and pterocarpus; but is less common in lower plants such as fungi, algae, lichens and the like.
The flavonoid compound is an important effective ingredient of the traditional Chinese medicine, has various biological activities and is mainly shown in that:
(1) effect on cardiovascular system: such as radix Puerariae total flavone, puerarin, folium Ginkgo total flavone, etc., has effects of dilating coronary artery blood vessel, and can be used for treating coronary heart disease; rutin, hesperidin, d-catechin, etc. have effects of reducing capillary fragility and abnormal permeability, and can be used as hemostatic for capillary hemorrhage and adjuvant for treating hypertension and arteriosclerosis.
(2) Anti-liver injury effect: such as silymarin, silymarin and silymarin, etc., has liver protection effect, and is clinically used for treating acute and chronic hepatitis, liver cirrhosis, various toxic liver injuries, etc.
(3) Spasmolysis: such as isoliquiritigenin and daidzein, have papaverine-like effect, and can relieve smooth muscle spasm.
(4) Effect on the respiratory system: such as farrerol, nobiletin and quercetin, has antitussive and expectorant effects.
(5) Estrogen-like action: isoflavones such as genistein and daidzein have a female hormone-like effect and may be related to their structural moieties similar to that of diethylstilbestrol.
(6) Antibacterial, antiviral, and antitumor effects. Such as luteolin, baicalin, baicalein, quercetin, morin and the like, has antibacterial and antiviral effects: vitexin, morin, d-catechu and the like have anti-tumor effects.
(7) Has antioxidant effect. Such as ginkgetin, soybean isoflavone, rutin, quercetin, etc., has strong antioxidant capacity. In addition, the flavonoid compound is also an important functional food additive, a natural antioxidant, a natural pigment, a natural sweetener and the like.
At present, the extraction method of the flavonoid compounds has the defects of low extraction rate, long extraction time and unstable physicochemical properties of the extract. Therefore, the invention provides a method for efficiently and quickly extracting the flavonoid compounds from the plants, and the flavonoid compounds are used as main raw materials of medicines, health-care foods, foods and foods with special medical application, and have very important significance.
Disclosure of Invention
The invention aims to solve the technical problem of providing the method for extracting the flavonoid compounds in the plants aiming at the defects in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention firstly provides a method for extracting flavonoid compounds in plants, which comprises the following steps:
(1) preparing an extracting solution: cleaning plant, drying, pulverizing, and sieving with 50 mesh sieve to obtain plant dry powder;
(2) preparing a eutectic solvent: reacting choline chloride and ethylene glycol at 60660 ℃ for 162h to obtain transparent uniform liquid, cooling to room temperature, adding purified water, and mixing uniformly to obtain a eutectic solvent;
(3) extraction: placing the plant body dry powder obtained in the step (1) into a high-speed shearing machine, adding the eutectic solvent obtained in the step (2) as an extraction medium, shearing and extracting at normal temperature, wherein the shearing rotation speed is 6000612000rpm, the shearing time is 367min, centrifuging after the extraction is finished, and centrifuging to obtain lower-layer plant residues and a supernatant;
(4) repeatedly extracting and combining: placing the plant slag obtained in the step (3) into a high-speed shearing machine, adding the eutectic solvent obtained in the step (2) as an extraction medium, continuing shearing, extracting and centrifuging according to the method in the step (3), and continuing to obtain the plant slag and a supernatant; repeating the steps for multiple times, and combining the supernatants obtained in the steps (3) and (4) to obtain plant extract which is a flavonoid compound.
In the above technical scheme, in the step (1), the plant cleaning refers to cleaning with tap water and then cleaning with purified water 263 times.
In the above technical scheme, in the step (1), the drying refers to drying at 40655 ℃ for 8612 h.
In the above technical solution, in the step (1), the pulverization means that the pulverization is 50 meshes.
In the above technical scheme, in the step (2), the mol ratio of choline chloride to ethylene glycol is 1: 161: 4, preferably 1: 2.
in the above technical scheme, in the step (2), the reaction temperature of the choline chloride and the ethylene glycol is preferably 80 ℃, and the reaction time is preferably 1.5 h.
In the above technical solution, in the step (2), the amount of the purified water is 630%, preferably 20%, of the total weight of choline chloride and ethylene glycol.
In the above technical solution, in the step (3), the ratio of the plant body dry powder to the eutectic solvent (weight to volume) is 1:15625, preferably 1: 20.
In the technical scheme, in the step (3), a high-speed desktop centrifuge is adopted for centrifugal separation, the rotating speed is 14000615000rpm, and the time is 15620 min.
The invention also provides a flavonoid compound extracted by the extraction method.
The invention also provides application of the flavonoid compound in preparing food, health-care food, formula food for special medical application or medicines.
In the technical scheme, when the flavonoid compound is used for preparing food, health food, special medical application formula food or medicine, the flavonoid compound is compounded with auxiliary materials or additives which can be accepted in the food, the health food, the special medical application formula food or medicine as an effective component, and the corresponding oral preparation is prepared according to the corresponding preparation method and process.
In the technical scheme, the oral preparation comprises common tablets, effervescent tablets, chewable tablets, buccal tablets, capsules or granules and the like.
In the technical scheme, the auxiliary materials acceptable in the food, the health food, the special medical purpose formula food or the medicine comprise a filling agent, an excipient, a diluent, a disintegrating agent, an adhesive, a flavoring agent, a foaming agent, a lubricant, a solvent, a thickening agent, a cosolvent, a pH regulator, an osmotic pressure regulator, an antioxidant or a swelling agent and the like.
In the technical scheme, the acceptable additives in the food, the health food, the special medical purpose formula food or the medicine comprise trace elements, minerals, vitamins, amino acids or taurine.
The invention has the following remarkable advantages:
(1) the invention applies the high-speed shearing technology to extract the flavonoid compounds in the plants in an auxiliary way, and high-speed shearing breaks away the wax coat and the cell wall on the surface of the plant, so that the flavonoid compounds are released to the maximum extent, the extraction rate of the flavonoid compounds is greatly improved, the extraction time is obviously shortened, and the energy is saved.
(2) The traditional solvent is changed, the eutectic solvent is used for extraction, and hydrogen bond receptors in the eutectic solvent are easy to combine with hydroxyl in the flavonoid compounds, so that the extraction rate of the flavonoid compounds in the plant body is increased.
(3) All steps in the whole process of the invention are carried out at normal temperature, the active structure and the heat-sensitive active ingredients of the flavonoid compound are retained to the maximum extent, and the quality of the flavonoid compound is improved.
Detailed Description
The following detailed description of the embodiments of the present invention is provided, but the present invention is not limited to the following descriptions:
the invention will now be illustrated with reference to specific examples:
example 1:
a method for extracting flavonoid compounds in plants comprises the following steps:
(1) preparing an extracting solution: cleaning 5 kg of high-quality wolfberry fruits by using tap water, cleaning the wolfberry fruits by using purified water for 2 times, drying the wolfberry fruits at 50 ℃ for 10 hours, crushing the wolfberry fruits into 70 meshes, and sieving the wolfberry fruits by using a 50-mesh sieve to obtain plant dry powder;
(2) preparing a eutectic solvent: weighing choline chloride and ethylene glycol (molar ratio is 1:2) and sequentially adding the choline chloride and the ethylene glycol into a round-bottom flask, putting a magnetic rotor, putting the magnetic rotor into an oil bath pot, reacting for 1.5 hours at 80 ℃ to form uniform transparent liquid, putting the liquid on a balance when the temperature of the liquid is reduced to room temperature, adding 20% purified water, and successfully preparing a eutectic solvent (DES) for later use;
(3) extraction: precisely weighing about 3.0g of a medlar sample, placing the medlar sample in a high-speed shearing machine, then adding DES (choline chloride: ethylene glycol, molar ratio of 1:2), wherein the material-liquid ratio is 1:20, processing for 5min at room temperature under the condition of 10000r/min of the high-speed shearing machine, shaking up, placing in a high-speed desk type centrifuge, and centrifuging for 15min under the condition of 15000r/min to obtain plant residues and supernatant;
(4) repeatedly extracting and combining: placing the plant residues obtained in the step (3) into a high-speed shearing machine, adding the eutectic solvent obtained in the step (2) as an extraction medium (the material-liquid ratio is 1:20), continuously performing shearing extraction and centrifugation according to the method in the step (3), and continuously obtaining the plant residues and a supernatant; repeating the steps for 2 times, and combining the supernatants obtained in the steps (3) and (4) to obtain plant extract which is flavonoid compound.
Example 2:
a method for extracting flavonoid compounds in plants comprises the following steps:
(1) preparing an extracting solution: cleaning 8 kg of high-quality wolfberry fruits by using tap water, cleaning the wolfberry fruits by using purified water for 2 times, drying the wolfberry fruits for 12 hours at 45 ℃, crushing the wolfberry fruits into 60 meshes, and sieving the wolfberry fruits by using a 60-mesh sieve to obtain plant dry powder;
(2) preparing a eutectic solvent: weighing choline chloride and ethylene glycol (the molar ratio is 1:1.5) and sequentially adding the choline chloride and the ethylene glycol into a round-bottom flask, putting a magnetic rotor into the round-bottom flask, putting the round-bottom flask into an oil bath kettle, reacting for 2 hours at 75 ℃ to form uniform transparent liquid, putting the liquid on a balance when the temperature of the liquid is reduced to room temperature, adding 20% purified water into the balance, and successfully preparing a eutectic solvent (DES) for later use;
(3) extraction: precisely weighing about 3.0g of a medlar sample, placing the medlar sample in a high-speed shearing machine, then adding DES (choline chloride: ethylene glycol, molar ratio of 1:1.5), material-liquid ratio of 1:25, treating for 3min at room temperature under the condition of 12000r/min of the high-speed shearing machine, shaking uniformly, placing the medlar sample in a high-speed desk type centrifuge, and centrifuging for 20min under the condition of 12000r/min to obtain plant residues and supernatant;
(4) repeatedly extracting and combining: placing the plant residues obtained in the step (3) into a high-speed shearing machine, adding the eutectic solvent obtained in the step (2) as an extraction medium (the material-liquid ratio is 1:25), continuously performing shearing extraction and centrifugation according to the method in the step (3), and continuously obtaining the plant residues and a supernatant; repeating the steps for 2 times, and combining the supernatants obtained in the steps (3) and (4) to obtain plant extract which is flavonoid compound.
Example 3:
a method for extracting flavonoid compounds in plants comprises the following steps:
(1) preparing an extracting solution: taking 10 kg of high-quality cynomorium songaricum, cleaning with tap water, cleaning with purified water for 2 times, drying at 50 ℃ for 12 hours, crushing to 60 meshes, and sieving with a 80-mesh sieve to obtain dry plant powder;
(2) preparing a eutectic solvent: weighing choline chloride and ethylene glycol (molar ratio is 1:2) and sequentially adding the choline chloride and the ethylene glycol into a round-bottom flask, putting a magnetic rotor, putting the magnetic rotor into an oil bath pot, reacting for 1.5 hours at 80 ℃ to form uniform transparent liquid, putting the liquid on a balance when the temperature of the liquid is reduced to room temperature, adding 25% of purified water, and successfully preparing a eutectic solvent (DES) for later use;
(3) extraction: precisely weighing about 5.0g of cynomorium songaricum sample, placing the cynomorium songaricum sample in a high-speed shearing machine, adding DESS (choline chloride: ethylene glycol, molar ratio of 1:2), treating for 5min at room temperature under 12000r/min of the high-speed shearing machine, shaking uniformly, placing the mixture in a high-speed desktop centrifuge, and centrifuging for 20min under 12000r/min to obtain plant residues and supernatant;
(4) repeatedly extracting and combining: placing the plant residues obtained in the step (3) into a high-speed shearing machine, adding the eutectic solvent obtained in the step (2) as an extraction medium (the material-liquid ratio is 1:25), continuously performing shearing extraction and centrifugation according to the method in the step (3), and continuously obtaining the plant residues and a supernatant; repeating the steps for 2 times, and combining the supernatants obtained in the steps (3) and (4) to obtain plant extract which is flavonoid compound.
And (3) verification test: method for measuring content of flavone in Chinese wolfberry
1 experimental materials:
1.1 instruments, drugs and reagents:
an XQ100 g type multifunctional high-speed pulverizer (shanghai guang sand works ltd); a T25 high speed shearer (IKA corporation); BSA224S-CW type electronic analytical balance (Beijing Saedodus Instrument systems, Inc.); a KQ-250DB type numerical control ultrasonic cleaning machine (kunshan ultrasonic instrument ltd); DHG-6140A type electric heating constant temperature air blast drying oven (Shanghai sperm macro experimental facilities Co., Ltd.); h1650 type medical centrifuge (Changshan instrument, Inc.); TI-16 series double-beam UV-Vis spectrophotometer (Beijing Pujingyu general instruments, Inc.).
Rutin control (purity ≧ 68%, lot number 1000800-171130, Cinningtian blue Biotech Co., Ltd.); choline chloride (analytically pure, annagi chemical company); ethylene glycol (analytically pure, linalon bothua (tianjin) pharmaceutical chemistry, ltd.).
1.2 materials:
wolfberry fruit sample: is prepared from Baotou of inner Mongolia, is identified as dry mature fruit of Lycium barbarum L of Solanaceae by professor Thysanopterus Schott of Thysanova, Chinese medicinal university, and is pulverized and sieved with 50 mesh sieve, and is protected from light and stored for use.
2 statistical analysis
The measurement data is expressed by mean plus or minus standard deviation, SPSS17.0 and origin statistical software are used for carrying out one-way variance analysis on experimental data, and P <0.05 is used as a statistical significance index
3. Drawing of standard curve
Precisely absorbing 0.5mL, 1.0mL, 1.5 mL, 2.0mL, 2.5 mL and 3.0mL of rutin reference substance solution, respectively placing in a 10mL volumetric flask, fixing the volume with 60% ethanol, measuring the value of absorbance A according to a sodium nitrite-aluminum nitrate-sodium hydroxide colorimetric method and an ultraviolet-visible spectrophotometry, drawing a rutin concentration (c) -absorbance (A) standard curve by taking the concentration (c) of the rutin reference substance solution as a horizontal coordinate and the absorbance (A) as a vertical coordinate, and calculating a linear regression equation of the rutin standard curve.
4. Measurement of samples
Precisely sucking 1.0mL of sample solution obtained by 2.2 preparation methods, placing in 10.0mL volumetric flasks, adding 0.5mL of 5% NaNO2Shaking the water solution, standing for 6 min; 0.5mL of 10% Al (NO) was added to each of the solutions3)3Shaking the water solution, standing for 6 min; adding 4.0mL of 4% NaOH aqueous solution, adding 70% ethanol to constant volume, shaking, and standing for 15 min. 2.0mL of water is precisely absorbed, and a blank solution without rutin reference substance is prepared as a reference solution in the same way. And respectively taking the reference solution and the sample solution, and measuring the reference solution and the sample solution on an ultraviolet-visible spectrophotometer at an absorption wavelength of 510 nm.
And calculating according to a linear regression equation to obtain the content of the total flavonoids in the solution of the absorbed sample. The content of total flavonoids in the medlar is calculated according to the formula (1.1):
Figure BDA0002858230040000101
in formula (1.1), w: total content of flavonoids, mg/g; c: the concentration of the sample liquid on a standard curve corresponding to the measured light absorption value is mg/mL; v1The volume of the test solution is mL; v2: after the volume is fixed, the volume of the sample liquid to be detected is mL; v3: the volume of the test solution, mL, absorbed when measuring the light absorption value; m: wolfberry quality, g.
5 investigation of extraction of Lycium chinense flavone by different methods
5.1 preparation of sample solution by ethanol reflux method: the specific operation is as follows: precisely weighing about 3.0g of fructus Lycii sample, reflux-extracting with 70% ethanol at a material-liquid ratio of 1:15 for 2 times, each time for 1.5 hr, standing at room temperature, filtering, mixing filtrates, transferring into 100.0mL volumetric flask, adding ethanol with the same concentration to constant volume, and shaking. Centrifuging at 15000r/min for 20min, and collecting supernatant to obtain total flavone extract I.
5.2 preparation of sample solution by high-speed shearing assisted ethanol extraction: the specific operation is as follows: precisely weighing about 3.0g of fructus Lycii sample, treating with 70% ethanol at a ratio of 1:20 at room temperature at 18000r/min for 5min, shaking, centrifuging at 15000r/min for 20min, and collecting supernatant to obtain total flavone extract II.
5.3 ultrasonic assisted DES extraction method sample solution preparation: the method comprises precisely weighing fructus Lycii sample about 3.0g, treating with DES (choline chloride: ethylene glycol, molar ratio 1:2) and feed-liquid ratio 1:20 in an ultrasonic cleaner (power 100W) at room temperature for 30min, shaking, centrifuging at 15000r/min for 20min, and collecting supernatant to obtain total flavone extract III.
5.4 preparation of sample solution by high-speed shearing assisted DES extraction: precisely weighing about 3.0g of fructus Lycii sample, treating with DES (choline chloride: ethylene glycol, molar ratio 1:2) and material-liquid ratio 1:20 at room temperature under 10000r/min with a high speed shearing machine for 5min, shaking, centrifuging at 15000r/min for 20min, and collecting supernatant to obtain total flavone extract IV.
6 results of the experiment
The different methods for extracting fructus Lycii flavone show in Table 1
TABLE 14 comparison of the extraction methods for wolfberry flavonoids (n ═ 3)
Figure BDA0002858230040000111
As can be seen from Table 1: the invention considers 3 different methods of ethanol reflux extraction, ultrasonic-assisted DES extraction and high-speed shearing-assisted ethanol extraction to extract the medlar flavone under the optimal condition, and compares the medlar flavone yield with the medlar flavone yield extracted by high-speed shearing-assisted DES, the high-speed shearing-assisted DES extraction effect is optimal, the ethanol reflux extraction effect is inferior, and the other 2 extraction methods have poor effects by taking the flavone extraction rate as an evaluation index.
The above examples are only for illustrating the technical concept and features of the present invention, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

Claims (10)

1. A method for extracting flavonoid compounds in plants is characterized by comprising the following steps:
(1) preparing an extracting solution: cleaning plant, drying, pulverizing, and sieving with 50 mesh sieve to obtain plant dry powder;
(2) preparing a eutectic solvent: reacting choline chloride and ethylene glycol at 60-90 ℃ for 1-2 h to obtain transparent uniform liquid, cooling to room temperature, adding purified water, and mixing uniformly to obtain a eutectic solvent;
(3) extraction: placing the plant body dry powder obtained in the step (1) into a high-speed shearing machine, adding the eutectic solvent obtained in the step (2) as an extraction medium, shearing and extracting at normal temperature, wherein the shearing rotation speed is 6000-12000 rpm, the shearing time is 3-7 min, centrifuging after the extraction is finished, and centrifuging to obtain lower-layer plant residues and a supernatant;
(4) repeatedly extracting and combining: placing the plant slag obtained in the step (3) into a high-speed shearing machine, adding the eutectic solvent obtained in the step (2) as an extraction medium, continuing shearing, extracting and centrifuging according to the method in the step (3), and continuing to obtain the plant slag and a supernatant; repeating the steps for multiple times, and combining the supernatants obtained in the steps (3) and (4) to obtain plant extract which is a flavonoid compound.
2. The extraction method according to claim 1, characterized in that: in the step (1), the plant cleaning is to clean the plant by using tap water and then clean the plant for 2-3 times by using purified water.
3. The extraction method according to claim 1, characterized in that: in the step (1), the drying refers to drying for 8-12 hours at the temperature of 40-55 ℃.
4. The extraction method according to claim 1, characterized in that: in the step (1), the pulverization refers to the pulverization of 50 meshes.
5. The extraction method according to claim 1, characterized in that: in the step (2), the mol ratio of the choline chloride to the ethylene glycol is 1: 1-1: 4; the addition amount of the purified water is 10-30% of the total weight of choline chloride and glycol.
6. The extraction method according to claim 1, characterized in that: in the step (2), the choline chloride and the ethylene glycol are reacted at the temperature of 80 ℃ for 1.5 h.
7. The extraction method according to claim 1, characterized in that: in the step (3), the feed-liquid ratio of the plant body dry powder to the eutectic solvent is 1: 15-25.
8. The extraction method according to claim 1, characterized in that: in the step (3), a high-speed desktop centrifuge is adopted for centrifugal separation, the rotating speed is 14000-15000 rpm, and the time is 15-20 min.
9. A flavonoid compound obtained by the extraction method according to any one of claims 1 to 8.
10. Use of flavonoids according to claim 9 for the preparation of a food product, a health food product, a food formulation for specific medical use or a pharmaceutical product.
CN202011551946.9A 2020-12-24 2020-12-24 Method for extracting flavonoid compounds in plants Pending CN112645919A (en)

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