CN115894423A - Method for extracting quercetin from folium cortex eucommiae - Google Patents
Method for extracting quercetin from folium cortex eucommiae Download PDFInfo
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- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 title claims abstract description 207
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 title claims abstract description 103
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 0.000 title claims abstract description 103
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 title claims abstract description 103
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- 238000001914 filtration Methods 0.000 claims description 23
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 15
- 230000007062 hydrolysis Effects 0.000 claims description 12
- 238000006460 hydrolysis reaction Methods 0.000 claims description 12
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- 238000000605 extraction Methods 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
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- 238000001179 sorption measurement Methods 0.000 claims description 9
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- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a method for extracting quercetin from eucommia leaves, which comprises the following steps: s1, collecting 100g of eucommia ulmoides leaves, cleaning, S2, putting the smashed eucommia ulmoides leaves into a beaker, adding 60-80% alcohol solution, soaking for 2 hours, extracting for 45 minutes in an ultrasonic mode at 70-90 ℃, S3, adding the crushed eucommia ulmoides leaves into solid residues according to the ratio of 1:8, adding 60-80% of alcoholic solution, extracting for 35 minutes in an ultrasonic mode at 70-90 ℃, and S4, adding the solid residue into the mixture according to the ratio of 1:6, adding 60-80% of alcohol solution, extracting for 20 minutes in an ultrasonic mode in an environment of 70-90 ℃, S5 obtaining final suction filtration liquid, S6, recovering the alcohol solution under reduced pressure to obtain concentrated solution, centrifuging for 30 minutes, S7, evaporating to dryness to obtain a hydrolysate, namely a crude product of the quercetin, and S8, carrying out vacuum drying on the precipitated crystals to obtain a refined quercetin product.
Description
Technical Field
The invention belongs to the field of quercetin extraction, and particularly relates to a method for extracting quercetin from eucommia ulmoides leaves.
Background
Quercetin is a flavonoid compound, also known as quercetin, and is dissolved in glacial acetic acid, the alkaline aqueous solution is yellow and almost insoluble in water, and the ethanol solution is bitter in taste. It can be used as medicine, and has good expectorant, antitussive, and antiasthmatic effects. In addition, it also has effects of lowering blood pressure, enhancing capillary resistance, reducing capillary fragility, reducing blood lipid, dilating coronary artery, and increasing coronary blood flow. Can be used for treating chronic bronchitis. It also has adjuvant treatment effect on coronary heart disease and hypertension.
Through retrieval, a patent with the application number of 201210126236.0 discloses a method for extracting quercetin from eucommia leaves, wherein the eucommia leaves are used as raw materials, the eucommia leaves are crushed and sieved and then are subjected to reflux extraction, concentration and separation by using an alcohol solution, acid hydrolysis is carried out on the crushed eucommia leaves to obtain crude quercetin, and the crude quercetin is purified to obtain the quercetin.
The purity of the quercetin obtained by the scheme is high, and the highest purity of the quercetin obtained in the test data is 91.2%, so that the purity of the quercetin needs to be further improved, and the yield of the quercetin extracted by the scheme is not high.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a method for extracting quercetin from eucommia ulmoides leaves, which comprises the steps of firstly carrying out three ultrasonic extraction processes on a mixed solution of eucommia ulmoides leaf raw materials and an alcohol solution to fully separate quercetin from the eucommia ulmoides leaf raw materials, concentrating a suction filtration liquid obtained by three extraction processes, carrying out centrifugal treatment, carrying out reduced pressure drying, water adding dispersion, resin adsorption, pH value adjustment and hydrolysis treatment to obtain a crude quercetin product, and carrying out crystallization treatment on the crude quercetin product to obtain a refined quercetin product, wherein the refined quercetin product has high yield and high purity, so that the yield of a production enterprise and the quality of the quercetin are improved.
In order to achieve the purpose, the invention provides the following technical scheme: the method for extracting quercetin from eucommia ulmoides leaves comprises the following steps:
s1, collecting eucommia ulmoides leaves, cleaning, drying, mashing the dried eucommia ulmoides leaves, and sieving the smashed eucommia ulmoides leaves with a 80-140-mesh sieve;
s2, adding the smashed eucommia leaves into a mixture according to the material-liquid ratio of 1: adding 60-80% alcohol solution according to the proportion of 10, soaking for 2 hours, and extracting for 45 minutes in an ultrasonic mode at 70-90 ℃ to obtain a primary mixed solution;
s3, filtering the primary mixed solution to obtain primary suction filtration liquid and solid residues, and adding the primary suction filtration liquid and the solid residues into the solid residues according to a mass ratio of 1:8, adding 60-80% of alcohol solution, and extracting for 35 minutes in an ultrasonic mode at 70-90 ℃ to obtain a secondary mixed solution;
s4, filtering the secondary mixed solution to obtain secondary suction filtration liquid and solid residues, fusing the secondary suction filtration liquid and the primary suction filtration liquid together, and adding the fused liquid into the solid residues according to the mass ratio of 1:6, adding 60-80% of alcoholic solution in proportion, and extracting for 20 minutes in an ultrasonic mode at 70-90 ℃ to obtain a third mixed solution;
s5, filtering the third mixed solution to obtain a third suction filtration liquid and solid residues, mixing the third suction filtration liquid into a mixed solution of the first suction filtration liquid and the second suction filtration liquid to obtain a final suction filtration liquid, and completely discarding the residual solid residues;
s6, decompressing the final suction-filtered liquid, recovering an ethanol solution to obtain a concentrated solution, centrifuging for 30 minutes to enable the concentrated solution to be pasty, decompressing and drying in an environment of-0.1 MPa and 60 ℃ to obtain a solid paste, and grinding the paste into powder;
s7, taking a proper amount of the prepared powder, and mixing the powder with the liquid according to a material-liquid ratio of 1:4, adding water for dispersion, adding macroporous resin for adsorption, adding an ethanol solution for eluting quercetin, collecting ethanol eluent, recovering ethanol under reduced pressure, adding 2mol/L hydrochloric acid aqueous solution into the concentrated solution, adjusting the pH to 2-4, carrying out water bath reflux hydrolysis for 2 hours at the temperature of 60-80 ℃, and evaporating to dryness to obtain a hydrolysate, namely a crude product of quercetin;
s8, dissolving the crude quercetin product with methanol, standing for crystallization, crystallizing for two times, and vacuum drying the precipitated crystals to obtain the refined quercetin product.
Preferably, in S1, the washed leaves of eucommia ulmoides are dried to remove moisture on the surface thereof and baked at a temperature of 60 to 80 ℃ for 15 to 30 minutes.
Preferably, in S2, the smashed eucommia ulmoides leaves are placed into the eucommia ulmoides leaves, 1000 ml of 80% alcohol solution is added, the eucommia ulmoides leaves are soaked for 2 hours, and the eucommia ulmoides leaves are extracted in an ultrasonic mode in an environment of 90 ℃ for 45 minutes to obtain a primary mixed solution.
Preferably, in S3, the primary mixed solution is filtered by using a microporous filter membrane with a pore size of 0.45 μm, the filtered solid residue is squeezed to obtain a primary suction filtered liquid, 800 ml of 70% alcohol solution is added to the solid residue, and the mixture is extracted by using an ultrasonic method at 80 ℃ for 35 minutes to obtain a secondary mixed solution.
Preferably, in S4, the secondary mixed solution is filtered by using a microporous filter membrane with a pore size of 0.35 micron, the filtered solid residue is squeezed to obtain a secondary suction-filtered liquid, 600 ml of 60% alcohol solution is added to the solid residue, and the mixture is extracted by using an ultrasonic method at 70 ℃ for 20 minutes to obtain a tertiary mixed solution.
Preferably, in S5, the third mixed solution is filtered by using a microporous filter membrane with a pore size of 0.22 μm, the filtered solid residue is extruded to obtain a third filtered liquid, the first filtered liquid, the second filtered liquid and the third filtered liquid are transferred to a concentration container, and the first filtered liquid, the second filtered liquid and the third filtered liquid are stirred for 3-5 minutes by using a stirring rod and then kept stand for later use.
Preferably, the concentrated solution obtained in S6 is centrifuged at 2500-3000r/min.
Preferably, in S7, the macroporous resin is any one of XDA-1 macroporous resin or X-5 macroporous resin, and when XDA-1 macroporous resin is selected, 80% ethanol solution is added to elute quercetin, and when quercetin is selected, 70% ethanol solution is added to elute quercetin.
Preferably, in S7, the concentrated solution is added with a 2mol/L hydrochloric acid aqueous solution with a volume of 20 ml, the pH value is adjusted to 3, and the solution is hydrolyzed in a water bath under reflux at the temperature of 70 ℃ for 2 hours.
The invention has the technical effects and advantages that: compared with the prior art, the method for extracting quercetin from eucommia ulmoides leaves firstly carries out three ultrasonic extraction processes on a mixed solution of eucommia ulmoides leaf raw materials and an alcohol solution, so that the quercetin in the eucommia ulmoides leaf raw materials is fully separated, suction filtration liquid obtained by the three extraction processes is concentrated and then centrifuged, crude quercetin is obtained after decompression drying, water adding dispersion, resin adsorption, pH value adjustment and hydrolysis, and crude quercetin is obtained after the crude quercetin is crystallized, and the refined quercetin is high in yield and purity, so that the yield of production enterprises and the quality of the quercetin are improved.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention. 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.
Referring to fig. 1, the method for extracting quercetin from eucommia ulmoides leaves includes the following steps:
s1, collecting eucommia ulmoides leaves, cleaning, drying, mashing the dried eucommia ulmoides leaves, and sieving the smashed eucommia ulmoides leaves with a 80-140-mesh sieve;
s2, adding the smashed eucommia leaves into a mixture according to the material-liquid ratio of 1: adding 60-80% alcohol solution according to the proportion of 10, soaking for 2 hours, and extracting for 45 minutes in an ultrasonic mode at 70-90 ℃ to obtain a primary mixed solution;
s3, filtering the primary mixed solution to obtain primary suction filtration liquid and solid residues, and adding the primary suction filtration liquid and the solid residues into the solid residues according to the mass ratio of 1:8, adding 60-80% of alcohol solution, and extracting for 35 minutes in an ultrasonic mode at 70-90 ℃ to obtain a secondary mixed solution;
s4, filtering the secondary mixed solution to obtain secondary suction filtration liquid and solid residues, fusing the secondary suction filtration liquid and the primary suction filtration liquid together, and adding the fused liquid into the solid residues according to the mass ratio of 1:6, adding 60-80% of alcoholic solution in proportion, and extracting for 20 minutes in an ultrasonic mode at 70-90 ℃ to obtain a third mixed solution;
s5, filtering the third mixed solution to obtain third suction filtration liquid and solid residues, mixing the third suction filtration liquid into a mixed solution of the first suction filtration liquid and the second suction filtration liquid to obtain final suction filtration liquid, and completely discarding the residual solid residues;
s6, decompressing the final suction-filtered liquid, recovering an ethanol solution to obtain a concentrated solution, centrifuging for 30 minutes to enable the concentrated solution to be pasty, decompressing and drying in an environment of-0.1 MPa and 60 ℃ to obtain a solid paste, and grinding the paste into powder;
s7, taking a proper amount of the prepared powder, and mixing the powder with the liquid according to a material-liquid ratio of 1:4, adding water for dispersion, adding macroporous resin for adsorption, adding an ethanol solution for eluting quercetin, collecting ethanol eluent, recovering ethanol under reduced pressure, adding 2mol/L hydrochloric acid aqueous solution into the concentrated solution, adjusting the pH to 2-4, carrying out water bath reflux hydrolysis for 2 hours at the temperature of 60-80 ℃, and evaporating to dryness to obtain a hydrolysate, namely a crude product of quercetin;
s8, dissolving the crude quercetin product with methanol, standing for crystallization, crystallizing for two times, and vacuum drying the precipitated crystals to obtain the refined quercetin product.
When quercetin is extracted, 100g of eucommia leaf raw material is taken, cleaned, dried and crushed, sieved by a sieve of 80-140 meshes, the crushed eucommia leaf is placed into a beaker, 1000 ml of 80% alcohol solution is added, soaked for 2 hours, extracted for 45 minutes in an ultrasonic mode in an environment of 90 ℃ to obtain a primary mixed solution, the primary mixed solution is filtered to obtain a primary suction filtration liquid, 800 ml of 70% alcohol solution is added into solid residues, extracted for 35 minutes in an ultrasonic mode in an environment of 80 ℃ to obtain a secondary mixed solution, the secondary mixed solution is filtered to obtain a secondary suction filtration liquid, 600 ml of 60% alcohol solution is added into the solid residues, extracted for 20 minutes in an ultrasonic mode in an environment of 70 ℃ to obtain a third mixed solution, filtering the third mixed solution, transferring the first filtered liquid, the second filtered liquid and the third filtered liquid into a concentration container, performing reduced pressure recovery on an ethanol solution to obtain a concentrated solution, performing centrifugal treatment, performing reduced pressure drying in an environment with the pressure of-0.1 MPa and the temperature of 60 ℃, finally adding water for dispersion, adding macroporous resin for adsorption, adding the ethanol solution for eluting quercetin, adding 2mol/L hydrochloric acid aqueous solution into the concentrated solution, adjusting the pH to 3, performing water bath reflux hydrolysis at the temperature of 60-80 ℃ for 2 hours to obtain a crude quercetin product, crystallizing the crude quercetin product to obtain a refined quercetin product, measuring the content of the quercetin by a liquid chromatograph, calculating the mass of the quercetin to be 0.75g, and detecting the purity of the quercetin to obtain the purity of 92.0%.
In S1, the cleaned eucommia ulmoides leaves are wiped to dry the water on the surfaces of the eucommia ulmoides leaves, and then the eucommia ulmoides leaves are put into a dryer and continuously baked for 15-30 minutes at the temperature of 60-80 ℃. Preferably, the eucommia ulmoides leaves are baked at the temperature of 70 ℃ for 2 minutes, so that the moisture of the eucommia ulmoides leaves can be fully dried, and the chemical structure of the extract is not damaged.
In S2, the smashed eucommia leaves are placed in a beaker, 1000 ml of 80% alcohol solution is added into the beaker, the mixture is soaked for 2 hours and extracted for 45 minutes in an ultrasonic mode in an environment of 90 ℃, and a primary mixed solution is obtained.
In S3, filtering the primary mixed solution by using a microporous filter membrane with the aperture of 0.45 micron, extruding the filtered solid residue to fully obtain primary suction filtration liquid, adding 800 milliliters of 70% alcohol solution into the solid residue, and extracting for 35 minutes in an ultrasonic mode at the temperature of 80 ℃ to obtain a secondary mixed solution.
In S4, filtering the secondary mixed solution by using a microporous filter membrane with the aperture of 0.35 micron, extruding the filtered solid residue to fully obtain secondary suction filtration liquid, adding 600 milliliters of 60% alcohol solution into the solid residue, and extracting for 20 minutes in an ultrasonic mode at 70 ℃ to obtain a tertiary mixed solution.
And in S5, filtering the third mixed solution by using a microporous filter membrane with the aperture of 0.22 micron, extruding the filtered solid residues to fully obtain a third suction filtration liquid, transferring the first suction filtration liquid, the second suction filtration liquid and the third suction filtration liquid into a concentration container, fully stirring for 3-5 minutes by using a stirring rod, and standing for later use.
In S6, the centrifuge is set to be a table-type low-speed centrifuge, the highest rotating speed of the centrifuge is 5000r/min, the maximum capacity of the centrifuge is 1200 milliliters, and when the obtained concentrated solution is centrifugally operated in the centrifuge, the rotating speed of the centrifuge is set to be 2500-3000r/min.
In S7, the macroporous resin is set to be any one of XDA-1 macroporous resin or X-5 macroporous resin, when XDA-1 macroporous resin is selected, 80% ethanol solution is added to elute quercetin, and when quercetin is selected, 70% ethanol solution is added to elute quercetin.
In S7, the volume of 2mol/L hydrochloric acid aqueous solution added to the concentrate was 20 ml, the pH value after adjustment was optimally solved to 3, and hydrolysis was performed in a water bath under reflux at 70 ℃ for 2 hours.
Example 2
Different from the embodiment 1
When the quercetin is extracted, adding an alcohol solution into folium cortex eucommiae, preparing a mixed solution by adopting an ultrasonic method, wherein the adding sequence of the solubility of different alcohol solutions is different, and the temperature environment of ultrasonic extraction is different, concretely, when the quercetin is extracted, 100g of folium eucommiae raw material is taken, cleaned, dried and crushed, sieved by a sieve of 80-140 meshes, the crushed folium eucommiae is put into a beaker, 1000 ml of 60% alcohol solution is added, soaked for 2 hours, extracted for 45 minutes by adopting an ultrasonic method in an environment of 70 ℃ to obtain a primary mixed solution, the primary mixed solution is filtered to obtain a primary suction filtration liquid, 800 ml of 70% alcohol solution is added into solid residues, extracted for 35 minutes by adopting an ultrasonic method in an environment of 80 ℃ to obtain a secondary mixed solution, and the secondary mixed solution is filtered to obtain a secondary suction filtration liquid, adding 600 ml of 80% alcohol solution into the solid residue, extracting for 20 minutes in an ultrasonic manner at 90 ℃ to obtain a third mixed solution, filtering the third mixed solution, transferring the first suction filtered liquid, the second suction filtered liquid and the third suction filtered liquid into a concentration container, recovering the ethanol solution under reduced pressure to obtain a concentrated solution, centrifuging, drying under reduced pressure at-0.1 MPa and 60 ℃, adding water for dispersing, adding macroporous resin for adsorption, adding the ethanol solution for eluting quercetin, adding 2mol/L hydrochloric acid aqueous solution into the concentrated solution, adjusting the pH to 3, carrying out water bath reflux hydrolysis for 2 hours at 60-80 ℃ to obtain a crude quercetin product, crystallizing the crude quercetin product to obtain a refined quercetin product, measuring the content of the quercetin by a liquid chromatograph, and calculating the mass of the quercetin to be 0.71g, and detecting the purity of the quercetin to obtain the purity of 91.2%.
Example 3
Different from the embodiment 1
When extracting quercetin, adding an alcohol solution into folium Eucommiae, preparing a mixed solution by ultrasonic method, wherein the adding sequence of different alcohol solution solubilities is different, specifically, when extracting quercetin, adding an alcohol solution into folium Eucommiae, preparing a mixed solution by ultrasonic method, wherein the adding sequence of different alcohol solution solubilities is different, and the temperature environment of ultrasonic extraction is different, specifically, when extracting quercetin, taking 100g folium Eucommiae raw material, cleaning, drying and crushing, sieving with a 80-140 mesh sieve, placing crushed folium Eucommiae into a beaker, adding 1000 ml of 80% alcohol solution, soaking for 2 hours, extracting for 45 minutes at 70 ℃ by ultrasonic method, obtaining a primary mixed solution, filtering the primary mixed solution, obtaining a primary suction-filtered liquid, adding 800 ml of 70% alcohol solution into solid residue, extracting for 35 minutes by adopting an ultrasonic mode in an environment of 80 ℃ to obtain a secondary mixed solution, filtering the secondary mixed solution to obtain a secondary suction-filtered liquid, adding 600 milliliters of 60 percent alcohol solution into the solid residue, extracting for 20 minutes by adopting an ultrasonic mode in an environment of 90 ℃ to obtain a third mixed solution, filtering the third mixed solution, transferring the primary suction-filtered liquid, the secondary suction-filtered liquid and the third suction-filtered liquid into a concentration container, performing reduced pressure recovery on the ethanol solution to obtain a concentrated solution, performing centrifugal treatment, performing reduced pressure drying in an environment of-0.1 MPa and 60 ℃, finally adding water for dispersion, adding macroporous resin for adsorption, adding the ethanol solution for eluting quercetin, adding 2mol/L hydrochloric acid aqueous solution into the concentrated solution, adjusting the pH value to 3, performing water bath reflux hydrolysis for 2 hours at the temperature of 60-80 ℃, obtaining crude quercetin, crystallizing the crude quercetin to obtain refined quercetin, measuring the content of quercetin by a liquid chromatograph, calculating the mass of quercetin to be 0.73g, and detecting the purity of quercetin to obtain the purity of 91.6%.
Example 4
Different from the embodiment 1
Adding alcohol solution into folium Eucommiae, ultrasonic extracting at different temperature and environment, specifically, taking 100g folium Eucommiae raw material, cleaning, oven drying, crushing, sieving with 80-140 mesh sieve, placing the crushed folium Eucommiae into a beaker, adding 1000 ml 60% alcohol solution, soaking for 2 hr, extracting for 45 minutes in an ultrasonic mode at 90 ℃ to obtain a primary mixed solution, filtering the primary mixed solution to obtain primary suction filtration liquid, adding 800 ml of 70% alcoholic solution into the solid residue, extracting for 35 minutes in an ultrasonic mode at the temperature of 80 ℃ to obtain a secondary mixed solution, filtering the secondary mixed solution to obtain secondary suction filtration liquid, adding 600 ml of 80% alcoholic solution into the solid residue, extracting for 20 minutes in an ultrasonic mode at 70 ℃ to obtain three times of mixed solution, filtering the third mixed solution, transferring the first, second and third filtered liquids to a concentration container, recovering ethanol solution under reduced pressure to obtain concentrated solution, centrifuging, drying under reduced pressure at-0.1 MPa and 60 deg.C, dispersing in water, adsorbing with macroporous resin, eluting quercetin with ethanol solution, adding 2mol/L hydrochloric acid aqueous solution into the concentrated solution, adjusting pH to 3, performing water bath reflux hydrolysis at 60-80 deg.C for 2 hr, obtaining crude quercetin, crystallizing to obtain refined quercetin, measuring quercetin content with liquid chromatograph, and calculating the mass of the quercetin to be 0.72g, and detecting the purity of the quercetin to obtain the purity of 91.4%.
The specific details in the above examples are given in the following table:
| quality of eucommia ulmoides leaves | Quercetin refined product | Purity of Quercetin | |
| Example 1 | 100g | 0.75g | 92.0％ |
| Example 2 | 100g | 0.71g | 91.2％ |
| Example 3 | 100g | 0.73g | 91.6％ |
| Example 4 | 100g | 0.72g | 91.4％ |
In conclusion, the invention firstly carries out three times of ultrasonic extraction processes on the mixed solution of the eucommia leaf raw material and the alcohol solution, so that the quercetin in the eucommia leaf raw material is fully separated, the suction filtration liquid obtained by the three times of extraction is concentrated and then centrifuged, and crude quercetin is obtained after decompression drying, water adding dispersion, resin adsorption, pH value adjustment and hydrolysis treatment, and the crude quercetin is crystallized to obtain refined quercetin, and the refined quercetin has high yield and high purity, so that the yield of production enterprises and the quality of the quercetin are improved.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (9)
1. The method for extracting quercetin from eucommia ulmoides leaves is characterized by comprising the following steps: the method comprises the following steps:
s1, collecting eucommia ulmoides leaves, cleaning, drying, mashing the dried eucommia ulmoides leaves, and sieving the smashed eucommia ulmoides leaves with a 80-140-mesh sieve;
s2, adding the mixture into the smashed eucommia leaves according to the material-liquid ratio of 1: adding 60-80% alcohol solution according to the proportion of 10, soaking for 2 hours, and extracting for 45 minutes in an ultrasonic mode at 70-90 ℃ to obtain a primary mixed solution;
s3, filtering the primary mixed solution to obtain primary suction filtration liquid and solid residues, and adding the primary suction filtration liquid and the solid residues into the solid residues according to a mass ratio of 1:8, adding 60-80% of alcohol solution, and extracting for 35 minutes in an ultrasonic mode at 70-90 ℃ to obtain a secondary mixed solution;
s4, filtering the secondary mixed solution to obtain secondary suction filtration liquid and solid residues, fusing the secondary suction filtration liquid and the primary suction filtration liquid together, and adding the fused liquid into the solid residues according to the mass ratio of 1:6, adding 60-80% of alcohol solution, and extracting for 20 minutes in an ultrasonic mode at 70-90 ℃ to obtain a third mixed solution;
s5, filtering the third mixed solution to obtain a third suction filtration liquid and solid residues, mixing the third suction filtration liquid into a mixed solution of the first suction filtration liquid and the second suction filtration liquid to obtain a final suction filtration liquid, and completely discarding the residual solid residues;
s6, decompressing the final suction filtered liquid, recovering an ethanol solution to obtain a concentrated solution, centrifuging for 30 minutes to enable the concentrated solution to be pasty, decompressing and drying in an environment with the pressure of-0.1 MPa and the temperature of 60 ℃ to obtain a solid paste, and grinding the paste into powder;
s7, taking a proper amount of the prepared powder, and mixing the powder with the liquid-material ratio of 1:4, adding water for dispersion, adding macroporous resin for adsorption, adding an ethanol solution for eluting quercetin, collecting ethanol eluent, recovering ethanol under reduced pressure, adding 2mol/L hydrochloric acid aqueous solution into the concentrated solution, adjusting the pH to 2-4, performing reflux hydrolysis in a water bath at the temperature of 60-80 ℃ for 2 hours, and evaporating to obtain a hydrolysate, namely a quercetin crude product;
s8, dissolving the crude quercetin product with methanol, standing for crystallization, crystallizing for two times, and vacuum drying the precipitated crystals to obtain the refined quercetin product.
2. The method of extracting quercetin from leaves of eucommia ulmoides as claimed in claim 1, wherein: in S1, drying the cleaned folium Eucommiae, and baking at 60-80 deg.C for 15-30 min.
3. The method of claim 1, wherein the extraction of quercetin from eucommia ulmoides leaves comprises: in S2, the smashed eucommia leaves are placed into the eucommia leaves, 1000 ml of 80% alcohol solution is added, soaking is carried out for 2 hours, and ultrasonic extraction is carried out for 45 minutes in an environment of 90 ℃ to obtain a primary mixed solution.
4. The method of extracting quercetin from leaves of eucommia ulmoides as claimed in claim 1, wherein: in S3, filtering the primary mixed solution by using a microporous filter membrane with the aperture of 0.45 micron, extruding the filtered solid residue to fully obtain primary suction filtration liquid, adding 800 ml of 70% alcohol solution into the solid residue, and extracting for 35 minutes in an ultrasonic manner at 80 ℃ to obtain a secondary mixed solution.
5. The method of claim 1, wherein the extraction of quercetin from eucommia ulmoides leaves comprises: in S4, filtering the secondary mixed solution by using a microporous filter membrane with the aperture of 0.35 micron, extruding the filtered solid residue to fully obtain secondary suction filtration liquid, adding 600 ml of 60% alcohol solution into the solid residue, and extracting for 20 minutes in an ultrasonic manner at 70 ℃ to obtain a tertiary mixed solution.
6. The method of claim 1, wherein the extraction of quercetin from eucommia ulmoides leaves comprises: and in S5, filtering the third mixed solution by using a microporous filter membrane with the aperture of 0.22 micron, extruding the filtered solid residues to fully obtain a third suction filtration liquid, transferring the first suction filtration liquid, the second suction filtration liquid and the third suction filtration liquid into a concentration container, fully stirring for 3-5 minutes by using a stirring rod, and standing for later use.
7. The method of claim 1, wherein the extraction of quercetin from eucommia ulmoides leaves comprises: the concentrated solution obtained in S6 is centrifuged at 2500-3000r/min.
8. The method of claim 1, wherein the extraction of quercetin from eucommia ulmoides leaves comprises: in S7, the macroporous resin is set to be any one of XDA-1 macroporous resin or X-5 macroporous resin, when XDA-1 macroporous resin is selected, 80% ethanol solution is added to elute quercetin, and when quercetin is selected, 70% ethanol solution is added to elute quercetin.
9. The method of extracting quercetin from leaves of eucommia ulmoides as claimed in claim 1, wherein: in S7, a 2mol/L aqueous hydrochloric acid solution was added to the concentrate in a volume of 20 ml, the pH value after adjustment was 3, and hydrolysis was carried out in a water bath at 70 ℃ under reflux for 2 hours.
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