A plant flavonoid modified extraction method and its application

Abstract

The invention relates to the technical field of plant chemical engineering and natural product extraction, and in particular to a modified plant flavonoid extraction method and application thereof. The method uses an aqueous solution of molybdenum salt, aluminum salt or phosphate as an extraction solvent, heats the solution to 60-99°C, and then adds corresponding plant powder for extraction to obtain an extract rich in plant flavonoids. The process changes the physicochemical properties of flavonoids by chemical complexation, greatly improves the water solubility of flavonoids, is simple and easy to operate, and is used for extracting water-insoluble flavonoids. At the same time, the extracted flavonoid compounds still retain the original biological activity of the flavonoids or exceed the biological activity of the original flavonoids. At the same time, the technology is applied to the extraction and purification process, which can greatly reduce the extraction cost.

Description

Technical Field

[0001] The present invention relates to the field of plant chemical engineering and natural product extraction technology, and more specifically to a flavonoid modified extraction method and application thereof. Background Art

[0002] Vine tea, also known as vine tea, is the tender stems and leaves of Ampelopsis grossedentata of the genus Ampelopsis of the family Vitaceae. It is called vine tea in English and is grown in the mountainous areas of the south of the Yangtze River. It is a folk herbal medicine used by ethnic minorities in southwest my country for generations. The "Compendium of Materia Medica for Famine Relief", "Compendium of Chinese Materia Medica" and "Compendium of Chinese Herbal Medicine" all include vine tea. The main uses are: clearing away heat and detoxifying, reducing heat and promoting body fluid, reducing fat and blood pressure, removing rheumatism, strengthening muscles and bones, and anti-inflammatory and diuretic. Vine tea is a unique vine plant for both medicine and food in my country. The Yao, Bai, Miao, Yi and Tujia people use vine tea to decoct water to treat sore throat, liver disease, beriberi and other diseases, with significant efficacy. Modern research has found that vine tea is rich in flavonoids (dihydromyricetin), amino acids, polysaccharides, polyphenols, vitamins and other effective ingredients. The total flavonoids and dihydromyricetin content are more than 50% and 40% respectively. It is a miracle of flavonoid content in nature and is called the "king of flavonoids". A large number of modern studies have shown that flavonoids from rattan tea have the effects of immunomodulation, anti-oxidation, anti-cancer, hypoglycemic, hypolipidemic, heat-clearing and detoxifying, anti-rheumatic, strengthening bones and muscles, anti-inflammatory, detumescence, diuresis, hemostasis, and treatment of chronic hepatitis and nephritis. In the past decade, domestic and foreign academic circles have published more than 1,000 research papers on the medicinal effects of dihydromyricetin in terms of liver protection, hangover relief, anti-cancer, antibacterial and anti-inflammatory, and more than 100 patent applications related to rattan tea, providing sufficient scientific theoretical basis and technical support for the industrial development of rattan tea.

[0003] In recent years, rattan tea has become an emerging Tujia specialty industry in the southwest region. "Laifeng rattan tea" has obtained the national geographical indication protection product certification. The development of rattan tea industry bases has been rapid, and more than 300,000 mu of rattan tea has been developed in Enshi, Chongqing, Zhangjiajie and other places. However, due to the limitations of rattan tea deep processing technology, rattan tea has only been circulated in a small range as a niche tea product, which has seriously restricted the development of the rattan tea industry. The main reason is that there is no breakthrough in the key technology of large-scale circulation product research and development of rattan tea. That is, rattan tea must develop large-scale circulation products, such as rattan tea beverages, rattan tea skin care soaps, shower gels, etc., to solve the crisis of rattan tea raw materials in excess, so as to guide the healthy development of the rattan tea industry. The technical bottleneck of producing rattan tea beverages or soaps is that rattan tea flavonoids (dihydromyricetin) are hexahydroxyflavonoids, which are difficult to dissolve in water and are very easy to precipitate, making it impossible to produce high-quality rattan tea beverages or washing and skin care products. Ginkgo flavonoids also have similar defects as above. Based on these problems, the present application provides a water-insoluble plant flavonoid modification technology, which not only improves the extraction efficiency of flavonoids from rattan tea, but also solves the problem of flavonoids from rattan tea being insoluble in water, and also improves the health benefits of flavonoids from rattan tea. Summary of the invention

[0004] In order to solve the problems existing in the above-mentioned prior art, the present invention provides the use of soluble molybdenum salts, phosphates or aluminum salts in extracting water-insoluble flavonoid compounds from plants; it also provides a method for extracting water-insoluble plant flavonoids using molybdenum salts, phosphates or aluminum salts, and the use of the method in producing plant flavonoid beverages, food additives or anti-inflammatory skin care daily chemical products. The method has a simple process flow, high production efficiency and low cost.

[0005] In order to achieve the above object, the technical solution adopted by the present invention is:

[0006] The invention relates to the application of soluble molybdenum salt, phosphate or aluminum salt in extracting water-insoluble flavonoid compounds.

[0007] Furthermore, the flavonoid compound is ginseng flavonoids, ginkgo flavonoids and / or sophora japonica flavonoids.

[0008] Furthermore, the molybdenum salt is sodium molybdate, potassium molybdate or ammonium molybdate; the phosphate is trisodium phosphate or tripotassium phosphate; and the aluminum salt is aluminum trichloride.

[0009] The salt ions of the above salts form water-soluble complexes with plant flavonoid compounds, thereby making the water-insoluble flavonoids dissolve in water and exert the efficacy of flavonoids in a water environment.

[0010] The present invention also provides a method for extracting water-insoluble flavonoid compounds from plants using the above-mentioned soluble molybdenum salt, phosphate or aluminum salt, comprising the following steps:

[0011] (1) preparing an aqueous solution of a molybdenum salt, a phosphate or an aluminum salt; the resulting aqueous solution is the extractant;

[0012] (2) The plant powder is added to an extractant heated to 60-99° C. and kept warm for a period of time for extraction. During the warming process, the mixture is continuously stirred until the extraction is complete, and then filtered (in the actual process, at least two extractions are performed according to the actual situation) to obtain an extract containing plant flavonoids.

[0013] Furthermore, the mass percentage concentration of the molybdenum salt, phosphate or aluminum salt in the aqueous solution in step (1) is 0.001%-10%, preferably 0.1%-10%.

[0014] The invention also provides application of the method in preparing flavonoid solid.

[0015] Furthermore, the application steps of the above method in preparing flavonoid solids are as follows:

[0016] (A) adding zinc dihydrogen phosphate or calcium chloride or potassium hydroxide or sodium hydroxide to the extract containing plant flavonoids prepared by the above method to react, stirring slowly during the reaction, and after the reaction is complete, standing at 5-10° C. to precipitate, filtering and collecting the precipitate, drying, and crushing to obtain a dried powder;

[0017] (B) The dried powder is directly purified by chromatography using an organic solvent as a mobile phase to obtain a high-purity flavonoid solid.

[0018] Furthermore, the organic solvent is a mixture of solvent A (solvent A is ethanol, methanol, propanol, butanol or petroleum ether) and solvent B (solvent B is ethanol, methanol, propanol or butanol), and the solvent A and solvent B are different.

[0019] Furthermore, the chromatography purification operation method is carried out with reference to the technical solution recorded in the disclosed invention patent: "Announcement text CN105214333B of ZL201510724254.2, a high-efficiency purification device for plant extracts and a method for purifying plant extracts".

[0020] Specifically, the operation of the chromatography purification is as follows:

[0021] The equipment used is the high-efficiency purification device in the above-mentioned invention patent. During purification, the purification tank cover is first opened, and the dried powder is added into the purification tank, and then the purification tank cover is tightly closed, and then the chromatography solvent is injected into the tank body of the purification tank through the valve until it is full, and then the valve is closed and the purification tank is placed in a heating box for heating, and the heating temperature is 20-50°C higher than the boiling point of the chromatography solvent; the chromatography solvent in the purification tank is evaporated by heat, and the solvent vapor is released through the steam outlet of the cover on the top of the purification tank, and finally the solvent is recovered from the solvent outlet of the heating box; the bottom solvent in the purification tank will also continue to migrate to the surface through the filter sieve plate along the powder layer in the purification tank until the chromatography solvent is completely evaporated; in the process of the chromatography solvent migrating upward through the powder in the purification tank, the flavonoids are dissolved in the solvent and move to the surface, and finally crystallize on the surface, and the subsequent upwardly migrating solvent continues to migrate to the surface through the flavonoid crystals, carrying a small amount of impurities in the flavonoids to the surface and forming impurity crystals; the impurity layer on the surface is removed, and the purified flavonoid solid is collected.

[0022] The invention also provides application of the method in preparing plant flavonoid beverages, food additives or daily chemical products.

[0023] Furthermore, the application steps of the above method in preparing a plant flavonoid beverage are as follows:

[0024] The extract containing plant flavonoids prepared by the above method is diluted to prepare a clear and uniform plant flavonoid beverage (in the process, flavoring agents may be added or not according to production needs).

[0025] Furthermore, the daily chemical products include toothpaste, soap, hand sanitizer, bath and foot bath bags, and shampoo and bath products.

[0026] Furthermore, the application steps in preparing food additives or daily chemical raw materials are as follows:

[0027] The plant flavonoid-containing extract prepared by the method is vacuum concentrated and dried and then used as a food additive or daily chemical raw material.

[0028] Compared with the prior art, the present invention has the following advantages and beneficial effects:

[0029] 1. The present invention is simple to operate, and the equipment used is common equipment. An aqueous solution of molybdenum salt, aluminum salt or phosphate is used as the extraction solvent, and no organic solvent is needed. Therefore, the present invention is low in cost, non-toxic and harmless, and suitable for industrial production.

[0030] 2. Using molybdenum salt aqueous solution as extraction solvent, molybdenum-containing rattan tea flavonoids can be directly used as food raw materials, and the antibacterial and anti-inflammatory effects are significantly improved. Sodium molybdate is a nutritional supplement, so the extract not only solves the problem of nutritional supplements, but also further enhances the efficacy of rattan tea flavonoids.

[0031] 3. The cost of the plant flavonoid beverage produced by the present invention is greatly reduced compared with the traditional process, and the health care effect of the product is also higher than similar products, and it has incomparable competitiveness.

[0032] 4. When the flavonoid extract obtained by the method of the present invention is used to prepare flavonoids, zinc dihydrogen phosphate is used. The waste zinc molybdate generated during the reaction is a highly efficient non-toxic disinfectant, which can be directly used for disinfection in farms, homes, and public places, or as a feed disinfectant for the prevention and treatment of livestock and poultry diseases, thereby further reducing the production cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 The structure schematic diagram of the purification tank used for reverse chromatography described in the embodiment;

[0034] Figure 2 Schematic diagram of the material purification process in reverse chromatography described in the examples. DETAILED DESCRIPTION

[0035] The applicant will further explain the method of the present invention in detail below in conjunction with specific examples. However, it should be understood that the following examples should not be construed as limiting the scope of protection of the claims of the present invention to any extent.

[0036] The chromatography operation principle and method described in the following embodiments refer to another invention patent of the first inventor of this application that has been authorized and announced (a high-efficiency purification device for plant extracts and a method for purifying plant extracts, ZL201510724254.2, see announcement text CN105214333B). The chromatography method is hereinafter referred to as "reverse chromatography".

[0037] The specific operation process of the above reverse chromatography is as follows:

[0038] The equipment used is the high-efficiency purification device in the above invention patent, and its schematic diagram is as follows Figure 1 As shown, first open the lid of the purification tank, add the dried powder into the purification tank, then cover the lid of the purification tank, and then inject the chromatography solvent into the body of the purification tank through the valve until it is full, then close the valve and put the purification tank into the heating box for heating. The heating temperature must be 30°C higher than the boiling point of the chromatography solvent. The chromatography solvent in the purification tank evaporates due to the heat, and the solvent vapor is released through the steam outlet of the lid on the top of the purification tank, and finally the solvent is recovered from the solvent outlet of the heating box. The bottom solvent in the purification tank will also continue to migrate to the surface through the filter screen along the powder layer in the purification tank until the chromatography solvent is completely evaporated (such as Figure 2 As shown in the figure, during the upward migration of the chromatography solvent through the powder in the purification tank, the flavonoids dissolved in the solvent move toward the surface layer and finally crystallize on the surface layer. The solvent that subsequently migrates upwards continues to migrate toward the surface layer through the flavonoid crystals, carrying a small amount of impurities in the flavonoids to the surface layer and forming impurity crystals. In this way, the flavonoids are separated from the solid powder, and the impurities in the flavonoids are also separated. The impurity layer on the surface is removed, and the purified target flavonoids are collected.

[0039] Embodiment 1 A flavonoids modified extraction method, the steps of which are as follows:

[0040] (1) using molybdenum salt, phosphate or aluminum salt, dissolved in water to obtain a clear aqueous solution with a mass percentage concentration of 0.001% to 10% of salt; the obtained clear aqueous solution is used as an extractant to extract flavonoids from plants, including vine tea flavonoids, ginkgo flavonoids, sophora japonica flavonoids or other plant flavonoids that are insoluble in water;

[0041] (2) adding plant powder rich in flavonoids that are poorly soluble in water to an extractant heated to 60-99° C., keeping the temperature for a period of time and stirring continuously, and then filtering, repeating the above extraction process at least once as needed for the obtained residue, combining the filtrate, and obtaining an extract of modified flavonoids from rattan tea;

[0042] Specifically, in this embodiment, 100 grams of dried rattan tea powder was taken, and flavonoids in rattan tea were extracted using a sodium molybdate aqueous solution with a mass percentage concentration of 5% according to the above technical scheme. On the other hand, the extractant in the above step (2) was replaced with water and then extracted to obtain a control extract. The main process data of the two groups of experiments are shown in Table 1:

[0043] Table 1. Comparison of main parameters of dihydromyricetin extracted from rattan tea by two equal solvents: water and molybdenum salt aqueous solution

[0044]

[0045]

[0046] Note: As shown in Table 1 above, the content of dihydromyricetin in the extract was detected by liquid chromatography; the extraction yield was calculated as follows: total content of dihydromyricetin in the extract / dry weight of rattan tea × 100%; solid-liquid ratio = mass of the extract to be extracted / volume of the extractant.

[0047] It can be seen from the above data that the technical solution of the present invention using molybdate aqueous solution to extract rattan tea flavonoids can greatly reduce costs and improve extraction efficiency.

[0048] Embodiment 2 A flavonoids modified extraction method, the steps of which are as follows:

[0049] (1) dissolving sodium molybdate in water to obtain a sodium molybdate aqueous solution with a mass percentage concentration of 5%; the obtained sodium molybdate aqueous solution is used as an extractant to extract rattan tea flavonoids;

[0050] (2) Add 1000 g of dried rattan tea powder to an extractant at 70°C, keep warm for 30 min, and then filter. Stir continuously during the heat preservation. The obtained filter residue is extracted again according to the above process, filtered again, and the filtrates of the two extractions are combined to obtain an extract of modified flavonoids from rattan tea. The solid-liquid ratio of each extraction process is 1 g:5 ml.

[0051] (3) Add zinc dihydrogen phosphate to the extract of modified flavonoids from rattan tea (the actual amount of zinc dihydrogen phosphate added is calculated based on the stoichiometric ratio of zinc dihydrogen phosphate and sodium molybdate in the chemical reaction equation, specifically, the molar ratio of zinc dihydrogen phosphate to sodium molybdate is 1:1), slowly stir thoroughly, let stand at 5-10° C. to precipitate, collect the precipitate after filtration, dry it in vacuum at 60° C., and grind it to obtain a dried powder.

[0052] (4) The dried powder is subjected to reverse chromatography, wherein the chromatography solvent is a mixture of petroleum ether and ethanol (10:1 by volume), to obtain rattan tea flavonoids containing more than 95% dihydromyricetin.

[0053] Embodiment 3 A flavonoids modified extraction method, the steps of which are as follows:

[0054] (1) preparing a sodium molybdate aqueous solution with a mass percentage concentration of 0.1% as an extractant for extracting rattan tea flavonoids;

[0055] (2) Add 200 g of dried rattan tea powder to an extractant at 80°C, keep warm for 30 min, and then filter. Stir continuously during the heat preservation. The obtained filter residue is extracted again according to the above process, filtered again, and the filtrates of the two extractions are combined to obtain an extract of modified flavonoids from rattan tea. The solid-liquid ratio of each extraction process is 1 g:5 ml.

[0056] (3) diluting the extract of step (2) according to production needs to prepare a clear and uniform plant flavonoid beverage.

[0057] The extractant in the above step (2) was replaced with water and then extracted to obtain a control extract. The water extraction temperature was 100°C.

[0058] The antibacterial data of the molybdenum-containing rattan tea beverage and the beverage produced by water-extracted rattan tea flavonoids produced according to the above technical solution are as follows:

[0059] Table 2. Comparison of the main antibacterial parameters of the rattan tea flavonoid beverage obtained by extraction with two equal solvents: water and molybdenum salt aqueous solution after one week of plate culture

[0060] index Molybdenum vine tea beverage Water-extracted rattan tea beverage Escherichia coli colony count (cfu / ml) 2 8 Diameter of inhibition zone (mm) 5.5 3.2 Taste Sweet Bitter Beverage visual inspection Deep red, clear Brownish yellow, turbid precipitate

[0061] It can be seen from the above data that the flavonoid-modified rattan tea beverage produced by the technical solution of the present invention using molybdenum salt aqueous solution has significantly enhanced antibacterial effect, a milder taste, and a beautiful appearance, making it a healthier rattan tea beverage.

[0062] The extract of modified flavonoids from rattan tea in step (2) can be directly sealed and packaged and used as foot bath or bath water after vacuum concentration. It can also be used as a formula for shower gel, soap, or shampoo to produce antibacterial skin care daily chemicals.

[0063] Embodiment 4 A flavonoids modified extraction method, the steps of which are as follows:

[0064] (1) preparing a sodium molybdate aqueous solution with a mass percentage concentration of 5%; the obtained sodium molybdate aqueous solution is used as an extractant to extract ginkgo flavonoids;

[0065] (2) Add 1000 g of dried powdered ginkgo leaves to an extractant at 80° C., keep warm for 30 min with constant stirring, and then filter. The resulting residue is extracted again according to the above process, filtered again, and the filtrates of the two extractions are combined to obtain an extract of modified ginkgo flavonoids. The solid-liquid ratio of each extraction process is 1 g:5 ml.

[0066] (3) Add zinc dihydrogen phosphate (zinc dihydrogen phosphate: sodium molybdate molar ratio of 1:1) to the modified ginkgo flavonoids extract, slowly stir thoroughly, let stand at 5-10° C. to precipitate, collect the precipitate after filtration, dry it in vacuum at 60° C., and grind it to obtain a dried powder.

[0067] (4) Adding a mixture of petroleum ether and ethanol (volume ratio of 10:1) to the dried powder as a mobile phase for reverse chromatography to obtain ginkgo flavonoids with a purity of more than 92%.

[0068] Embodiment 5 A flavonoids modified extraction method, the steps of which are as follows:

[0069] (1) preparing a sodium molybdate aqueous solution with a mass percentage concentration of 0.1%; the obtained sodium molybdate aqueous solution is used as an extractant to extract ginkgo flavonoids;

[0070] (2) Add 200 g of dried powdered ginkgo leaves to an extractant at 80° C., keep warm for 30 min with constant stirring, and then filter. The resulting residue is extracted again according to the above process, filtered again, and the filtrates of the two extractions are combined to obtain an extract of ginkgo modified flavonoids. The solid-liquid ratio of each extraction process is 1 g:5 ml.

[0071] (3) The ginkgo flavonoids extract of step (2) is diluted according to production needs, and necessary flavoring agents and other nutrients are added to prepare a uniform and stable ginkgo flavonoids oral solution.

[0072] Embodiment 6 A flavonoids modified extraction method, the steps of which are as follows:

[0073] (1) preparing an aluminum chloride aqueous solution with a mass percentage concentration of 5%; the obtained aluminum chloride aqueous solution is used as an extractant to extract rattan tea flavonoids;

[0074] (2) Add 1000 g of the dried powder of Ampelopsis ulmoides into an extractant at 60°C, keep warm for 30 min with constant stirring, and then filter. The resulting residue is extracted again according to the above process, filtered again, and the filtrates of the two extractions are combined to obtain a modified flavonoid extract of Ampelopsis ulmoides. The solid-liquid ratio of each extraction process is 1 g:5 ml.

[0075] (3) adding sodium hydroxide to the modified flavonoid extract of rattan tea (the actual amount of sodium hydroxide added is calculated according to the chemical reaction equation of aluminum chloride and sodium hydroxide, and the molar ratio of aluminum chloride to sodium hydroxide is 1:3), slowly stirring while adding, and then standing at 5-10 degrees Celsius to precipitate overnight, then filtering and collecting the precipitate, drying the precipitate, and crushing through 200 mesh to obtain a fine powder.

[0076] (4) The fine powder was subjected to reverse chromatography using a mixture of petroleum ether and ethanol (10:1 volume ratio) as the mobile phase to obtain high-purity rattan tea flavonoids, wherein the content of dihydromyricetin reached 95%.

[0077] The extractant in the above step (2) was replaced with water and then extracted to obtain rattan tea flavonoids. The extraction yields of dihydromyricetin in flavonoids obtained with two different extractants were compared. The results are shown in Table 3.

[0078] Table 3. Comparison of main parameters of extracting dihydromyricetin from rattan tea with two equal solvents: water and aluminum salt aqueous solution

[0079]

[0080] Note: As shown in the above test table, liquid chromatography was used to detect the content of dihydromyricetin in the extract; the extraction yield calculation method is: total content of extracted dihydromyricetin / dry weight of rattan tea × 100%; material-liquid ratio = mass of the extract to be extracted / volume of the extractant.

[0081] Embodiment 7 A flavonoids modified extraction method, the steps of which are as follows:

[0082] (1) preparing a 10% by mass concentration of trisodium phosphate aqueous solution; the obtained aqueous solution is used as an extractant to extract flavonoids from rattan tea;

[0083] (2) Add 1000 g of the dried powder of Ampelopsis ulmoides into an extractant at 80°C, keep warm for 30 min with constant stirring, and then filter. The resulting residue is extracted again according to the above process, filtered again, and the filtrates of the two extractions are combined to obtain a modified flavonoid extract of Ampelopsis ulmoides. The solid-liquid ratio of each extraction process is 1 g:5 ml.

[0084] (3) Add calcium chloride to the modified flavonoid extract of rattan tea (calculate the amount of calcium chloride added according to the stoichiometric ratio of trisodium phosphate and calcium chloride in the chemical reaction equation; the molar ratio of trisodium phosphate to calcium chloride is 2:3), stir slowly, and then allow to settle overnight at 5-10 degrees Celsius, filter the precipitate, dry the precipitate, and then crush it into a 200-mesh fine powder.

[0085] (4) The fine powder was subjected to reverse chromatography using a mixture of petroleum ether and ethanol (10:1 volume ratio) as the mobile phase to obtain high-purity flavonoids, wherein the content of dihydromyricetin reached 95%.

[0086] The extractant in the above step (2) was replaced with water to extract the flavonoids. The extraction yields of dihydromyricetin in the flavonoids obtained from the two different extracting solutions were compared. The results are shown in Table 4.

[0087] Table 4. Comparison of main parameters of extracting dihydromyricetin from rattan tea by two equal solvents: water and trisodium phosphate aqueous solution

[0088]

[0089]

[0090] Note: As shown in the above test table, liquid chromatography was used to detect the content of dihydromyricetin in the extract; the extraction yield calculation method is: total amount of extracted dihydromyricetin / dry weight of rattan tea × 100%; material-liquid ratio = mass of rattan tea powder / volume of extract.

Claims

1. A method for extracting water-insoluble flavonoids from plants using soluble molybdenum salts and preparing flavonoid solids using the extracted water-insoluble flavonoids, wherein the flavonoids are radix ophiopogonis flavonoids, ginkgo biloba flavonoids or radix ophiopogonis flavonoids, comprising the following steps: (1) preparing an aqueous solution of a molybdenum salt, wherein the obtained aqueous solution is the extractant; The molybdenum salt is sodium molybdate, potassium molybdate or ammonium molybdate; (2) adding the plant powder to an extractant at 60-99°C and keeping it warm for a period of time to extract, stirring continuously during the keeping warm process, and then filtering to obtain an extract containing plant flavonoids; (3) adding zinc dihydrogen phosphate to the extract containing plant flavonoids prepared in step (2) to react, stirring slowly during the reaction, and after the reaction is complete, standing at 5-10° C. to precipitate, filtering and collecting the precipitate, drying, and crushing to obtain a dried powder; (4) Purifying the dried powder by chromatography using an organic solvent as a mobile phase to obtain a high-purity flavonoid solid; wherein: The organic solvent is a mixture of solvent A and solvent B, wherein the solvent A and solvent B are different, the solvent A is ethanol, methanol, propanol, butanol or petroleum ether, and the solvent B is ethanol, methanol, propanol or butanol; The operation process of the chromatography purification is as follows: during purification, first open the purification tank cover, add the dried powder into the purification tank, then cover the purification tank cover tightly, and then inject the chromatography solvent into the purification tank body through the valve until it is full, then close the valve and put the purification tank into the heating box for heating, and the heating temperature should be 20-50° C. higher than the boiling point of the chromatography solvent; the chromatography solvent in the purification tank evaporates under the heat, and the solvent vapor is released through the steam outlet of the cover on the top of the purification tank, and finally the solvent is recovered from the solvent outlet of the heating box; the bottom solvent in the purification tank will also continue to migrate to the surface layer along the powder layer in the purification tank through the filter sieve plate until the chromatography solvent is completely evaporated; in the process of the chromatography solvent migrating upward through the powder in the purification tank, the flavonoids are dissolved in the solvent and move to the surface layer, and finally crystallize on the surface layer, and the solvent that subsequently migrates upward continues to migrate to the surface layer through the flavonoid crystals, carrying a small amount of impurities in the flavonoids to the surface layer and forming impurity crystals; The impurity layer on the surface is removed and the purified flavonoid solid is collected.

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