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CN-122005647-A - Method for extracting flavone from astragalus leaves

CN122005647ACN 122005647 ACN122005647 ACN 122005647ACN-122005647-A

Abstract

The invention relates to an extraction method of flavonoids in astragalus leaves, which comprises the steps of mixing astragalus leaf powder and water to obtain a first mixed material, sequentially carrying out first constant-temperature leaching treatment and first solid-liquid separation treatment on the first mixed material to obtain a first liquid-phase product and a first solid-phase product, mixing the first solid-phase product and water to obtain a second mixed material, sequentially carrying out second constant-temperature leaching treatment and second solid-liquid separation treatment on the second mixed material to obtain a second liquid-phase product and a second solid-phase product, mixing the first liquid-phase product and the second liquid-phase product to obtain a liquid-phase product, mixing the liquid-phase product and anhydrous sodium sulfate to obtain a crude impurity-removed liquid, and sequentially carrying out reduced-pressure concentration treatment, first drying treatment and first crushing treatment on the crude impurity-removed liquid to obtain a flavonoids powder product. The invention uses water as extractant, adopts constant temperature leaching combined with secondary leaching technology, and uses anhydrous sodium sulfate to adsorb water and polar impurities in liquid phase product, thus being capable of efficiently extracting flavone in astragalus leaves.

Inventors

  • SHI BAOJUN
  • DU HONGWEI
  • YE ZISHENG

Assignees

  • 内蒙古蒙圣金薯食品科技有限责任公司

Dates

Publication Date
20260512
Application Date
20260324

Claims (10)

  1. 1. The extraction method of the flavone in the astragalus leaves is characterized by comprising the following steps of: (1) Firstly mixing astragalus leaf powder and water to obtain a first mixed material; (2) Sequentially carrying out first constant-temperature leaching treatment and first solid-liquid separation treatment on the first mixed material to obtain a first liquid-phase product and a first solid-phase product; (3) Performing second mixing on the first solid-phase product and water to obtain a second mixed material, sequentially performing second constant-temperature leaching treatment and second solid-liquid separation treatment on the second mixed material to obtain a second liquid-phase product and a second solid-phase product, and performing third mixing on the first liquid-phase product and the second liquid-phase product to obtain a liquid-phase product; (4) Fourth mixing the liquid-phase product and anhydrous sodium sulfate to perform crude impurity removal on the liquid-phase product to obtain a crude impurity-removed liquid; (5) And (3) sequentially carrying out reduced pressure concentration treatment, first drying treatment and first crushing treatment on the crude impurity-removed liquid to obtain a flavone powder product.
  2. 2. The extraction method according to claim 1, wherein the preparation of the astragalus leaf powder comprises sequentially subjecting astragalus leaves to a washing treatment, a second drying treatment, a second pulverizing treatment and a sieving treatment to obtain the astragalus leaf powder; Preferably, the cleaning agent used in the cleaning treatment includes water; Preferably, the temperature of the second drying treatment is 40-60 ℃; preferably, the screening treatment comprises screening treatment by using a 60-120 mesh screen.
  3. 3. The extraction method according to claim 1 or 2, wherein the ratio of the astragalus leaf powder to water in the first mixture is 1g (10-20) mL; preferably, after the first mixing, performing a first standing treatment to obtain a first mixed material; preferably, the time of the first standing treatment is 20-40 min.
  4. 4. The extraction method according to any one of claims 1 to 3, wherein the temperature of the first constant temperature leaching treatment is 80 to 85 ℃; Preferably, the leaching time of the first constant-temperature leaching treatment is 180-210 min; preferably, stirring treatment is carried out every 20-30 min in the first constant temperature leaching treatment; Preferably, the stirring treatment time is more than or equal to 1min.
  5. 5. The extraction method according to claim 3, wherein the ratio of the first solid-phase product to water in the second mixture is 1g (10-15) mL; preferably, the feed ratio in the second mixture is the same as the feed ratio in the first mixture; preferably, the temperature of the second constant-temperature leaching treatment is 80-85 ℃; Preferably, the leaching time of the second constant-temperature leaching treatment is 150-180 min; Preferably, stirring treatment is performed every 20-30 min in the second constant temperature leaching treatment.
  6. 6. The extraction method according to any one of claims 1 to 5, wherein the mass/volume ratio of anhydrous sodium sulfate to liquid phase product in the fourth mixture is (0.005 to 0.01) g/1 mL; preferably, the fourth mixing is performed under agitation; preferably, the stirring time is 5-15 min; Preferably, after the fourth mixing, sequentially performing a second standing treatment and a third solid-liquid separation treatment to obtain a crude impurity-removed liquid; Preferably, the second standing treatment is performed for 10-30 min.
  7. 7. The method according to any one of claims 1 to 6, further comprising purifying the crude purified liquid with a polyamide column before concentrating under reduced pressure, purifying with water, eluting with water, and obtaining an eluent; preferably, the polyamide column is subjected to an activation treatment prior to the purification treatment; preferably, the flow rate of the crude impurity-removed liquid in the purification treatment is 1.5-2.5 BV/h; Preferably, the flow rate of water in the process of purifying on the upper column is 2-2.5 BV/h; Preferably, the flow rate of the water in the elution treatment is 1.5-2.5 BV/h.
  8. 8. The method according to claim 7, wherein the flavone concentrate is obtained after the concentration under reduced pressure; Preferably, the temperature of the reduced pressure concentration treatment is 60-65 ℃; preferably, the vacuum degree of the reduced pressure concentration treatment is 0.06-0.08 MPa; Preferably, stirring is carried out during the reduced pressure concentration treatment; Preferably, the density ratio of the flavone concentrate to the eluent is (1.2-1.25): 1.
  9. 9. The extraction method according to any one of claims 1 to 8, wherein the temperature of the first drying treatment is 50 to 60 ℃; preferably, the average particle size of the flavone powder product is 150-200 mu m.
  10. 10. The extraction method according to any one of claims 1 to 9, characterized in that it comprises the steps of: (1) Sequentially carrying out cleaning treatment, second drying treatment at 40-60 ℃ and second crushing treatment on astragalus leaves, screening by using a screen mesh with 60-120 meshes to obtain astragalus leaf powder, carrying out first mixing on the astragalus leaf powder and water according to a feed-liquid ratio of 1g (10-20) mL, and standing for 20-40 min to obtain a first mixed material; (2) Sequentially carrying out first constant-temperature leaching treatment and first solid-liquid separation treatment on the first mixed material at the temperature of 80-85 ℃ for 180-210 min to obtain a first liquid-phase product and a first solid-phase product; (3) According to the feed-liquid ratio of 1g (10-15) mL, carrying out second mixing on the first solid-phase product and water to obtain a second mixed material, sequentially carrying out second constant-temperature leaching treatment and second solid-liquid separation treatment at the temperature of 80-85 ℃ for 150-180 min on the second mixed material to obtain a second liquid-phase product and a second solid-phase product, and carrying out third mixing on the first liquid-phase product and the second liquid-phase product to obtain a liquid-phase product; (4) Carrying out fourth mixing on anhydrous sodium sulfate and a liquid-phase product according to the mass volume ratio of (0.005-0.01) g to carry out crude impurity removal on the liquid-phase product, sequentially carrying out second standing treatment and third solid-liquid separation treatment for 10-30 min after fourth mixing to obtain a crude impurity-removed liquid, purifying the crude impurity-removed liquid by using a polyamide column, carrying out column-loading impurity removal by using water after the purification treatment, and then carrying out elution treatment by using water to obtain an eluent; (5) And sequentially carrying out reduced pressure concentration treatment, first drying treatment and first crushing treatment on the eluent at the temperature of 60-65 ℃ and the vacuum degree of 0.06-0.08 MPa to obtain a flavone powder product with the average particle size of 150-200 mu m.

Description

Method for extracting flavone from astragalus leaves Technical Field The invention relates to the technical field of traditional Chinese medicine extraction, in particular to a method for extracting flavone from astragalus leaves. Background Astragalus membranaceus is a leguminous astragalus membranaceus, belongs to plants, is a traditional rare traditional Chinese medicinal material, and contains rich flavonoid substances in roots, stems and leaves. The flavonoid compound is taken as an important natural active ingredient, has various biological activities such as antioxidation, anti-inflammatory, immunoregulation, blood fat reduction and the like, has wide application prospect in the fields of medicines, foods, health care products and the like, and continuously increases market demands. At present, the development and utilization of the astragalus root are mainly concentrated at the root, and a large amount of astragalus leaves are discarded as processing waste, so that not only is the serious waste of natural resources caused, but also a certain environmental pressure is brought. Therefore, the flavonoid substances are extracted from the astragalus leaves, the high-value utilization of the astragalus leaf wastes is realized, and the method becomes an important direction of the comprehensive development of the current astragalus resources, and has remarkable economic value and environmental protection significance. In the existing astragalus root leaf flavone extraction technology, the traditional alcohol extraction method is widely applied due to simple and convenient operation and lower cost, but the technology has obvious technical defects that the extraction parameters are not optimized by a system, the flavone extraction rate is lower, the temperature and time control in the extraction process are unreasonable, the oxidation and degradation of flavone substances are easily caused, the bioactivity is lost, the concentration equipment is improper in selection, the concentration process is unstable, the coking and the purity reduction of products are easily caused, and meanwhile, the problems of high energy consumption, complicated operation, difficult large-scale popularization and the like of part of the technology cannot be met, so that the market demands of industrial production and high-quality flavone extracts can not be met. In addition, the variety control of astragalus leaf raw materials in the prior art is not strict enough, so that the quality of the raw materials is uneven, further the flavone extraction effect and the product quality stability are affected, and a part of extraction process is not provided with a reasonable impurity removal and purification link or is unreasonable in impurity removal parameters, so that the impurity content in the extract is too high, and the application of the extract in the high-end field is limited. Aiming at the defects existing in the prior art, a novel extraction method is developed, flavone is extracted from astragalus leaves, and the problem to be solved is to improve the extraction rate of the flavone. Disclosure of Invention In order to solve the technical problems, the invention provides the extraction method of the flavonoids in the astragalus leaves, which uses water as an extracting agent, adopts a constant-temperature leaching combined secondary leaching process, and uses anhydrous sodium sulfate to adsorb water and polar impurities in a liquid-phase product, thereby effectively solving the technical pain points of low extraction efficiency, poor flavone activity retention, high energy consumption, unstable product quality and the like of the existing process, realizing efficient, green and large-scale extraction of the flavonoids in the astragalus leaves, and providing a practical technical scheme for comprehensive utilization of astragalus resources. To achieve the purpose, the invention adopts the following technical scheme: In a first aspect, the present invention provides a method for extracting flavonoids from astragalus leaves, the method comprising the steps of: (1) Firstly mixing astragalus leaf powder and water to obtain a first mixed material; (2) Sequentially carrying out first constant-temperature leaching treatment and first solid-liquid separation treatment on the first mixed material to obtain a first liquid-phase product and a first solid-phase product; (3) Performing second mixing on the first solid-phase product and water to obtain a second mixed material, sequentially performing second constant-temperature leaching treatment and second solid-liquid separation treatment on the second mixed material to obtain a second liquid-phase product and a second solid-phase product, and performing third mixing on the first liquid-phase product and the second liquid-phase product to obtain a liquid-phase product; (4) Fourth mixing the liquid-phase product and anhydrous sodium sulfate to perform crude impurity removal on the liquid-phase