CN113563294B - Method for extracting kaempferol from sophora fruit - Google Patents
Method for extracting kaempferol from sophora fruit Download PDFInfo
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- CN113563294B CN113563294B CN202110902868.0A CN202110902868A CN113563294B CN 113563294 B CN113563294 B CN 113563294B CN 202110902868 A CN202110902868 A CN 202110902868A CN 113563294 B CN113563294 B CN 113563294B
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- 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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Abstract
The invention discloses a method for extracting kaempferol from sophora fruit, which comprises the following steps: weighing a proper amount of sophora fruit powder, adding NaOH solution into the sophora fruit powder, and leaching at 50-80 ℃ to obtain a crude extract; filtering the crude extract, collecting filtrate, adding acetic acid to adjust the pH value to 6-7, standing and concentrating to obtain a concentrated extract; adding the concentrated extract into an acid solution for hydrolysis, wherein the hydrolysis temperature is 60-70 ℃, then filtering, and collecting filter residues; washing the filter residue with water until the water solution is neutral, performing thermal extraction on the neutral filter residue by using ethanol with the mass of 3-7 times that of the neutral filter residue, heating and refluxing at 70-80 ℃, filtering, collecting the obtained filtrate, adding activated carbon to perform adsorption decoloration, then filtering, collecting the filtrate again, and concentrating to 1/5-1/7 of the original volume to obtain concentrated filtrate; standing the concentrated filtrate, performing centrifugal separation, drying the precipitate, and crushing to obtain a kaempferol finished product with the content of 98%. The kaempferol extraction method provided by the invention is relatively simple in process and easy to operate, and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of kaempferol extraction, and particularly relates to a method for extracting kaempferol from sophora fruit.
Background
The Sophora fruit is a dry mature fruit of Sophora japonica (Sophora japonica L.) of Leguminosae, also can be called as Sophora fruit, sophora seed, kidney bean, locust bean and the like, is a common Chinese medicinal material in China, and is listed as the top grade in Shennong Ben Cao Jing. With the rapid development of modern science and technology, a plurality of chemical components in the fructus sophorae are separated and identified, wherein the fructus sophorae is mainly composed of flavone and isoflavone compounds, and the fructus sophorae has great significance and value for researching pharmacological efficacy and corresponding effective components of the fructus sophorae.
Kaempferol (Kaempferol) is used as a main flavonol compound in the sophora fruit and becomes a research hotspot in the sophora fruit extract because the Kaempferol has the functions of resisting oxidation and cancer, treating diabetes and osteoporosis, inhibiting fertility and the like. The kaempferol is yellow powder, is slightly soluble in water, is dissolved in hot ethanol, alkali and other liquids, and exists in the form of glucoside in the fructus sophorae, so that the kaempferol can be effectively and efficiently extracted through the physicochemical characteristics of the kaempferol in the fructus sophorae, and the effect of the kaempferol is exerted and applied to the maximum extent.
The existing kaempferol extraction mode generally adopts enzymolysis to decompose kaempferol and adopts macroporous resin and other methods to purify, the extraction cost is high, and the technological operation process is complicated.
Disclosure of Invention
The invention aims to provide a method for extracting kaempferol from sophora fruit, which integrally adopts alkaline liquor for preliminary extraction, then adopts acid hydrolysis to obtain mixed liquor containing kaempferol, and then adopts ethanol for effective extraction so as to solve the problems of higher extraction cost and more complex process operation process caused by the existing modes of decomposition of kaempferol by enzymolysis, macroporous resin and the like for purification.
The invention is realized by the following technical scheme:
the method for extracting the kaempferol from the sophora fruit comprises the following steps:
step 1: weighing a proper amount of sophora fruit powder, adding NaOH solution into the sophora fruit powder, and leaching at the temperature of 50-80 ℃ to obtain a crude extract;
step 2: filtering the crude extract, collecting filtrate, adding acetic acid to adjust the pH value to 6-7, standing and concentrating to obtain a concentrated extract;
and step 3: adding the concentrated extract into an acid solution for hydrolysis at the hydrolysis temperature of 60-70 ℃, then filtering, and collecting filter residues;
and 4, step 4: washing the filter residue with water until the water solution is neutral, performing hot extraction on the neutral filter residue by using ethanol with the mass of 3-7 times of that of the neutral filter residue, heating and refluxing at 70-80 ℃, filtering, collecting the obtained filtrate, adding activated carbon to perform adsorption decoloration, then filtering, collecting the filtrate again, and concentrating the filtrate to 1/5-1/7 of the original volume to obtain concentrated filtrate;
and 5: and standing the concentrated filtrate, performing centrifugal separation, drying the precipitate, and crushing to obtain a kaempferol finished product with the content of 98%.
As a further illustration of the invention, the preparation process of the sophora fruit powder is as follows:
screening and cleaning the sophora fruit raw material, naturally drying in a cool and ventilated place, and crushing the dried sophora fruit raw material.
As a further description of the present invention, the ratio of the sophora fruit powder to the NaOH solution is 1kg.
As a further illustration of the invention, the leaching time in the step 1 is 4-7 h, and the leaching times are 2-3.
As a further explanation of the invention, the standing time in the step 2 is 2 to 6 hours.
As a further explanation of the present invention, the ratio of the amount of the acidic solution used in step 3 to the sophorae fructus powder is 1kg.
As a further explanation of the invention, the hydrolysis time in step 3 is 3 hours, and the hydrolysis times are 2 to 3 times.
As a further explanation of the invention, the time of each heat extraction in the step 4 is 2-4 h, and the number of heat extractions is 3.
As a further illustration of the present invention, the concentration in step 2 and step 4 is performed by vacuum concentration.
As a further illustration of the invention, the recovery rate of the kaempferol finished product obtained in step 5 is 80-85%.
Compared with the prior art, the invention has the following beneficial technical effects:
the method uses alkali liquor for primary extraction, can effectively improve the extraction rate of the kaempferol, and can separate the kaempferol from most of the components of the fructus sophorae in one step.
The kaempferol extraction method provided by the invention is different from other extraction methods, the process flow adopts alkaline liquor for preliminary extraction, the mixed liquor containing kaempferol is obtained through acid hydrolysis, then ethanol is adopted for effective extraction, decomposition of kaempferol is not carried out through enzymolysis, and purification is carried out through methods such as macroporous resin and the like, the cost is reduced, the process is relatively simple and easy to operate, and the method is suitable for industrial production.
Drawings
Fig. 1 is a flow chart of the method for extracting kaempferol from sophora fruit provided by the invention.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, a detailed description of the present invention will be given below with reference to the accompanying drawings and specific embodiments. It should be noted that the embodiments and features of the embodiments of the present invention may be combined with each other without conflict.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Example 1:
step 1: the method comprises the steps of screening and cleaning the raw materials of the fructus sophorae, naturally airing the raw materials in a cool and ventilated place, crushing the aired raw materials of the fructus sophorae, weighing 10kg of the crushed raw materials of the fructus sophorae, adding the crushed raw materials of the fructus sophorae into 70L of 2% NaOH solution for leaching, leaching at the temperature of 50 ℃ for 4 hours, and repeatedly leaching for 2 times to obtain a crude extract.
And 2, step: filtering the obtained crude extract, collecting filtrate, adding acetic acid to adjust pH to 6, standing for 2 hr, and vacuum concentrating to obtain concentrated extract.
And 3, step 3: adding the obtained concentrated extractive solution into 70L of 3% acetic acid solution for hydrolysis at 60 deg.C for 3 hr, repeating hydrolysis for 2 times, filtering, and collecting residue.
And 4, step 4: washing the obtained filter residue with water until the water solution is neutral, performing thermal extraction on the neutral filter residue by using ethanol with the mass of 3 times of that of the neutral filter residue, performing heating reflux at 70 ℃, repeatedly extracting for 3 times, extracting for 2 hours each time, filtering, collecting filtrate, adding activated carbon to perform adsorption decoloration, stirring uniformly, filtering, collecting filtrate, and performing vacuum concentration on the filtrate to 1/5 of the original volume to obtain concentrated filtrate;
and 5: standing the obtained concentrated filtrate, performing centrifugal separation, drying the precipitate, pulverizing, and sieving with 80 mesh sieve to obtain kaempferol finished product with recovery rate of 85% and content of 98.1%.
Example 2:
step 1: screening and cleaning the fructus sophorae raw material, naturally airing in a cool and ventilated place, crushing the aired fructus sophorae raw material, weighing 10kg of the crushed fructus sophorae raw material, adding 70L of 4% NaOH solution for leaching, leaching at 65 ℃ for 5.5h, and repeatedly leaching for 3 times to obtain a crude extract.
Step 2: filtering the obtained crude extract, collecting filtrate, adding acetic acid to adjust pH to 7, standing for 3.5 hr, and vacuum concentrating to obtain concentrated extract.
And step 3: adding the obtained concentrated extractive solution into 75L of 4.5% acetic acid solution, hydrolyzing at 65 deg.C for 3 hr, repeating the hydrolysis for 3 times, filtering, and collecting residue.
And 4, step 4: washing the obtained filter residue with water until the water solution is neutral, performing thermal extraction on the neutral filter residue by using ethanol with the mass of 5 times of that of the neutral filter residue, performing heating reflux at 75 ℃, repeatedly extracting for 3 times, extracting for 3 hours each time, filtering, collecting filtrate, adding activated carbon to perform adsorption decoloration, stirring uniformly, filtering, collecting filtrate, and performing vacuum concentration on the filtrate to 1/6 of the original volume to obtain concentrated filtrate;
and 5: standing the obtained concentrated filtrate, performing centrifugal separation, drying the precipitate, pulverizing, and sieving with 80 mesh sieve to obtain kaempferol finished product with recovery rate of 83% and content of 98.6%.
Example 3:
step 1: screening and cleaning the sophora fruit raw material, naturally airing in a cool and ventilated place, crushing the aired sophora fruit raw material, weighing 10kg of the crushed sophora fruit raw material, adding 70L of 6% NaOH solution into the crushed sophora fruit raw material, leaching for 3 times at the leaching temperature of 80 ℃ for 7 hours, and obtaining a crude extract.
Step 2: filtering the obtained crude extract, collecting filtrate, adding acetic acid to adjust pH to 7, standing for 6h, and vacuum concentrating to obtain concentrated extract.
And 3, step 3: adding the obtained concentrated extractive solution into 80L of 6% phosphoric acid solution, hydrolyzing at 70 deg.C for 3 hr, repeating hydrolysis for 3 times, filtering, and collecting residue.
And 4, step 4: washing the obtained filter residue with water until the water solution is neutral, performing thermal extraction on the neutral filter residue by using 7 times of ethanol, performing heating reflux at 80 ℃, repeatedly extracting for 3 times at the temperature of 4 hours each time, filtering, collecting filtrate, adding activated carbon to perform adsorption decoloration, uniformly stirring, filtering, collecting filtrate, and performing vacuum concentration on the filtrate to 1/7 of the original volume to obtain concentrated filtrate;
and 5: standing the obtained concentrated filtrate, performing centrifugal separation, drying the precipitate, pulverizing, and sieving with 80 mesh sieve to obtain kaempferol finished product with recovery rate of 80% and content of 98.8%.
The method uses alkali liquor for primary extraction, can effectively improve the extraction rate of the kaempferol, and can separate the kaempferol from most of the sophora fruit components in one step.
The kaempferol extraction method provided by the invention is different from other extraction methods, the process flow adopts alkaline liquor for preliminary extraction, the mixed liquor containing kaempferol is obtained through acid hydrolysis, then ethanol is adopted for effective extraction, decomposition of kaempferol is not carried out through enzymolysis, and purification is carried out through methods such as macroporous resin and the like, the cost is reduced, the process is relatively simple and easy to operate, and the method is suitable for industrial production.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. A method for extracting kaempferol from sophora fruit is characterized by comprising the following steps: the method comprises the following steps:
step 1: weighing a proper amount of sophora fruit powder, adding NaOH solution into the sophora fruit powder, and leaching at the temperature of 50-80 ℃ for 4-7 h for 2-3 times to obtain a crude extract; the proportion of the sophora fruit powder to the NaOH solution is 1kg;
and 2, step: filtering the crude extract, collecting filtrate, adding acetic acid to adjust the pH value to 6-7, standing and concentrating to obtain a concentrated extract;
and step 3: adding the concentrated extract into an acid solution for hydrolysis at the hydrolysis temperature of 60-70 ℃, then filtering, and collecting filter residues;
and 4, step 4: washing the filter residue with water until the water solution is neutral, performing hot extraction on the neutral filter residue by using ethanol with the mass of 3-7 times of that of the neutral filter residue, heating and refluxing at 70-80 ℃, filtering, collecting the obtained filtrate, adding activated carbon to perform adsorption decoloration, then filtering, collecting the filtrate again, and concentrating the filtrate to 1/5-1/7 of the original volume to obtain concentrated filtrate;
and 5: and standing the concentrated filtrate, performing centrifugal separation, drying the precipitate, and crushing to obtain a kaempferol finished product with the content of 98%.
2. The method for extracting kaempferol from sophora fruit as claimed in claim 1, wherein: the preparation process of the sophora fruit powder comprises the following steps:
screening and cleaning the raw material of the fructus sophorae, naturally drying in a cool and ventilated place, and crushing the dried raw material of the fructus sophorae.
3. The method for extracting kaempferol from sophora fruit as claimed in claim 1, wherein: and the standing time in the step 2 is 2-6 h.
4. The method for extracting the kaempferol from the sophora fruit as claimed in claim 1, wherein the ratio of the amount of the acidic solution used in the step 3 to the sophora fruit powder is 7L-8L.
5. The method for extracting kaempferol from sophora fruit as claimed in claim 1, wherein the hydrolysis time in step 3 is 3 hours, and the hydrolysis times are 2 to 3.
6. The method for extracting kaempferol from sophora fruit as claimed in claim 1, wherein the time of each heat extraction in step 4 is 2-4 h, and the number of heat extractions is 3.
7. The method for extracting kaempferol from sophora fruit as claimed in claim 1, wherein the concentration in step 2 and step 4 is performed by vacuum concentration.
8. The method for extracting kaempferol from sophora fruit as claimed in claim 1, wherein the recovery rate of the kaempferol finished product obtained in step 5 is 80% -85%.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746265A (en) * | 2011-04-21 | 2012-10-24 | 西安通江生物科技有限责任公司 | Method for extracting high purity kaempferol from sophora fruit extraction waste residue |
| CN102875511A (en) * | 2012-09-04 | 2013-01-16 | 陕西嘉禾植物化工有限责任公司 | Method for comprehensively extracting dye lignin and kaempferol from sophora fruit |
| EP3290044A1 (en) * | 2016-08-30 | 2018-03-07 | SjF Hanse Scientific UG | Antibacterial composition, comprising a plant extract, method for obtaining the extract, pharmaceutical composition and use |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746265A (en) * | 2011-04-21 | 2012-10-24 | 西安通江生物科技有限责任公司 | Method for extracting high purity kaempferol from sophora fruit extraction waste residue |
| CN102875511A (en) * | 2012-09-04 | 2013-01-16 | 陕西嘉禾植物化工有限责任公司 | Method for comprehensively extracting dye lignin and kaempferol from sophora fruit |
| EP3290044A1 (en) * | 2016-08-30 | 2018-03-07 | SjF Hanse Scientific UG | Antibacterial composition, comprising a plant extract, method for obtaining the extract, pharmaceutical composition and use |
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