Search

CN-121974923-A - Method for extracting high-purity imperatorin from radix angelicae

CN121974923ACN 121974923 ACN121974923 ACN 121974923ACN-121974923-A

Abstract

The invention discloses a method for extracting high-purity imperatorin from dahurian angelica root, which comprises the steps of compounding dahurian angelica root medicinal materials, carrying out thermal reflux circulation extraction, reducing the degree, carrying out fractional elution, concentrating, dispatching, freezing for impurity removal, reducing the degree, carrying out secondary fractional elution, crystallizing, recrystallizing and carrying out vacuum drying to obtain a imperatorin Hu Suchun product with the purity higher than 99%. The raw materials used in the invention are wide in sources and easy to obtain, the used extraction equipment is common, the cost of the extraction solvent is low, the purification process is convenient, and the organic solvent with strong volatility and irritation is not used, so that a new green and environment-friendly industrial production method is provided for the preparation of the high-purity imperatorin.

Inventors

  • PENG TING
  • ZHANG FAN
  • YANG QIANG
  • WANG YU
  • ZHANG JIBIN
  • XU LANG
  • WANG QIONG
  • CHEN YANG
  • CHEN CUN
  • HU YOUBIAO
  • CHEN ZHIYUAN

Assignees

  • 劲牌有限公司
  • 劲牌持正堂药业有限公司

Dates

Publication Date
20260505
Application Date
20260126

Claims (8)

  1. 1. A method for separating and purifying imperatorin from dahurian angelica root, which is characterized by comprising the following steps: firstly, compounding, extracting and reducing the quality, namely taking the raw materials of angelica dahurica and emblic leafflower fruit decoction pieces according to the mass ratio of 1:1-1:5, carrying out heat reflux circulation extraction, and collecting an extracting solution; step two, fractional elution, namely passing the degradation liquid through nonpolar or weak polar macroporous resin, eluting by using ethanol with different alcohol degrees, collecting high-alcohol eluent, concentrating under reduced pressure, adding ethanol for dispatching, and carrying out solid-liquid separation to obtain alcohol-soluble supernatant and precipitate; step three, freezing and removing impurities, namely putting the alcohol-soluble supernatant into a refrigerator for freezing, then carrying out solid-liquid separation, collecting the frozen supernatant and sediment, and adding purified water into the frozen supernatant to obtain a freezing degradation liquid; Step four, secondary fractional elution, namely passing the frozen degradation liquid through a vinyl ester resin column, performing fractional elution by using ethanol with different alcohol degrees, collecting alcohol washing liquid, and concentrating to obtain extract; step five, crystallization and recrystallization, namely adding 70-95% ethanol solution into the extract for thermal dissolution, filtering, adding a small amount of poor solvent for crystallization, crystal washing and recrystallization to obtain imperatorin crystals with higher purity; And step six, drying and crushing, namely drying and crushing the obtained crystals to obtain the imperatorin dry product with the purity of more than or equal to 95 percent.
  2. 2. The method according to claim 1, wherein in the first step, the ethanol concentration is 40-95%, the volume ratio of the medicinal material to the extraction solvent is 1:7-15, the thermal reflux cycle temperature is 60-85 ℃, the extraction times are 1-2, the extraction time is 1-3 hours, and the alcohol degree of the degradation liquid is 10-70%.
  3. 3. The method according to claim 1, wherein in the second step, the macroporous resin is D101, AB-8, HPD-100, D201, HPD-400 or X-5, the mass volume ratio of the macroporous resin to the filtrate is 1:2-6, the alcohol degree of the low-grade eluent is 10-65%, the alcohol degree of the high-grade eluent is 66-95%, the concentration is reduced to 1/2-1/5 of the original volume, the pressure of reduced pressure drying is-0.08-0.1 MPa, the temperature is 40-65 ℃, and the alcohol degree of the alcohol solution after dispatching is 60-90%.
  4. 4. The method according to claim 1, wherein in the third step, the freezing temperature is 0, -4 ℃, -16 ℃, -20 ℃ or-24 ℃, the freezing time is 12-48 hours, and the alcohol degree of the freezing degradation liquid is 10-70%.
  5. 5. The method according to claim 1, wherein in the fourth step, the vinyl ester resin is novolac epoxy vinyl ester, standard bisphenol A epoxy vinyl ester resin or flame retardant vinyl ester resin, the mass volume ratio of the vinyl ester resin to the filtrate is 1:1-3, the alcohol degree of the eluent is 10-95%, the number of times of fractional elution is 2-6, the alcohol washing liquid with the alcohol degree of more than 70% is collected, the concentration is carried out under reduced pressure to form an extract, the reduced pressure is-0.08-0.1 MPa, and the temperature is 40-65 ℃.
  6. 6. The method of claim 5, wherein the vinyl ester resin is SW901, hetron 970, ADS-17 or Derakane411.
  7. 7. The method according to claim 1, wherein in the fifth step, the ethanol solution is added in an amount of 1-3 times the weight of the extract, the dissolution temperature is 40-65 ℃, the poor solvent is purified water, 10% -30% of low-grade ethanol, the volume ratio of the poor solvent to the good solvent is 1:3-8, the crystallization temperature is-16 ℃ to 5 ℃ for 24-120 hours, the crystallization solvent is purified water, 10% -50% of low-grade ethanol, the solvent temperature is-24-5 ℃, the recrystallization temperature is-16-5 ℃, the recrystallization time is 48-120 hours, and the recrystallization times are 1-3 times.
  8. 8. The method according to claim 1, wherein in the step six, the recrystallized crystals are dried in vacuum or box type, and the drying temperature is less than or equal to 65 ℃.

Description

Method for extracting high-purity imperatorin from radix angelicae Technical Field The invention relates to the technical field of separation and purification of active ingredients of traditional Chinese medicinal materials, in particular to a method for extracting high-purity imperatorin from dahurian angelica root. Background The angelica dahurica is the dry root of the angelica dahurica or the angelica dahurica of the Umbelliferae, is divided into the angelica dahurica, the Sichuan angelica dahurica, the Qi Baizhi and the angelica dahurica according to the variety and the yield, is planted in northeast, north China, sichuan, zhejiang, hunan, hubei, jiangxi, hebei, henan and the like, has the effects of dispelling wind and cold, improving fragrance and removing fishy smell, is widely used in soup and meal, has more outstanding medicinal value as medicinal materials with homology of medicine, has the effects of relieving exterior syndrome and dispelling cold, dispelling wind and relieving pain, freeing nasal orifices, and relieving swelling and expelling pus, and is the clinical common medicine of traditional Chinese medicine. The imperatorin is a furocoumarin, is a characteristic component of angelica dahurica in Chinese pharmacopoeia, and has good application value in the aspects of resisting cancer, resisting inflammation, protecting nerves, reshaping airway of bronchial asthma, relieving non-alcoholic fatty liver injury, improving gouty arthritis and the like. CN01138873.0 discloses a method for extracting imperatorin from dahurian angelica root, the extraction and purification method comprises pulverizing medicinal materials, extracting with 95% ethanol, concentrating until no alcohol, diluting with water, extracting with chloroform, volatilizing chloroform layer, purifying with silica gel column, eluting with petroleum ether-acetone, and refining on the preparation liquid phase by reversed phase high performance liquid chromatography to obtain imperatorin reference (purity not less than 98%). The prepared sample has higher purity, but the used solvent has large environmental pollution, and the refining equipment has high price. CN200610042997.2 discloses a method for extracting the active ingredients of the traditional Chinese medicine cnidium fruit, namely imperatorin and osthole, which adopts a supercritical extraction method to extract the broken medicinal materials of the cnidium fruit, adopts diethyl ether to carry out ultrasonic dissolution, adopts petroleum ether to carry out crystallization and adopts absolute ethyl alcohol to carry out recrystallization. The prepared sample has higher purity, but the extraction equipment has high price, and the used solvent has great environmental pollution. CN200910232660.1 discloses a method for separating imperatorin from hukumquat, which adopts a supercritical extraction method to extract hukumquat crushed medicinal materials, decompresses and concentrates, adopts polyamide resin for purification, adopts hot methanol for saturated dissolution, crystallization and recrystallization, and adopts hot deionized water for crystallization. The prepared sample has higher purity, but the extraction equipment has high price, low polyamide resin adsorption capacity, low flow speed, easy blockage, easy regeneration, quick resin attenuation and high industrial production cost. CN201010531934.X discloses a process for separating imperatorin from osthole extraction waste liquid, wherein 60-80% methanol is used for extraction after medicinal materials are crushed, reduced pressure concentration is adopted for extraction, petroleum ether or n-hexane is used for extraction, low-temperature standing crystallization is adopted for recrystallization, and 98% ethanol is used for recrystallization. The prepared sample has high purity, and the used solvent has great environmental pollution. CN201110329004.0 discloses a method for extracting methoxy imperatorin and imperatorin from cnidium fruit by using inclusion crystallization method, adding benzene into main molecule I and cnidium fruit crude extract to make dissolution, adding petroleum ether to make crystallization, using benzene and petroleum ether to make recrystallization, volatilizing solvent, adding petroleum ether to make overnight, crystallizing, adding acetone overnight so as to obtain imperatorin crystal. The prepared sample has higher purity, but the process is complex, and the used solvent has great environmental pollution. CN201510178901.4 discloses a method for separating and purifying osthole and imperatorin from fructus cnidii, pulverizing fructus cnidii, cold-leaching with absolute ethanol, concentrating under reduced pressure, extracting with petroleum ether, dissolving with methanol, separating by supercritical fluid chromatography, and collecting fractions of different components. The prepared sample has higher purity, but the used solvent has great environmental pollution and the supercritical fluid chr