Method for separating and purifying isoimperatorin and imperatorin from angelica dahurica

A technology for the separation and purification of isoimperatorin and imperatorin, which is applied in the field of separation and purification of isoimperatorin and imperatorin, and can solve problems such as the difficulty in realizing green and clean production, the difficulty in selecting a solvent system, and the large consumption of organic solvents , to achieve the effects of easy automatic control, short process cycle and easy recycling

Inactive Publication Date: 2015-07-29
LIAOCHENG UNIV
View PDF4 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional separation and purification methods of coumarin components in Angelica dahurica mostly use solvent extraction such as ether and petroleum ether, and purification by silica gel column chromatography. This method has complicated steps, large consumption of organic solvents, and many solvent residues in the product.
In recent years, high-speed countercurrent chromatography has been used to separate and purify the coumarin components in Angelica dahurica. Although it has a wide range of applications, does not require solid carriers, and has low requirements for sample pretreatment, it is difficult to choose a solvent system, and there are also organic The disadvantages of large solvent consumption and residual solvents in the product make it difficult to realize green and clean production

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for separating and purifying isoimperatorin and imperatorin from angelica dahurica
  • Method for separating and purifying isoimperatorin and imperatorin from angelica dahurica

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 500 grams of Angelica dahurica, pulverize it with a pulverizer, put it into a glass container, add 3000ml of petroleum ether, heat and reflux for extraction 3 times, each time for 2 hours, combine the extracts, filter, and concentrate under reduced pressure to obtain Angelica dahurica extract.

[0024] The extract of Angelica dahurica was dissolved in methanol, filtered (the filter membrane used was 0.45 μm filter membrane), and separated by supercritical fluid chromatography. The chromatographic column was a C18 chromatographic column, and the chromatographic column temperature was 35°C. The mobile phase is supercritical carbon dioxide, the flow rate is 4 times column volume / min, and the pressure is 12 MPa. The improver is methanol, and its ratio is 1.15%. The separation process is detected by an ultraviolet detector with a detection wavelength of 220nm, and fractions of target components are collected according to detection signals to obtain isoimperatorin and i...

Embodiment 2

[0027] Weigh 500 grams of Angelica dahurica, pulverize it with a pulverizer, put it into a glass container, add 4000ml of petroleum ether, heat and reflux for extraction for 3 hours, and reflux for 1 hour each time, combine the extracts, filter, and concentrate under reduced pressure to obtain Angelica dahurica extract.

[0028] Angelica dahurica extract is dissolved with methanol, and after filtration, carry out supercritical fluid chromatography separation, the chromatographic column is a C18 chromatographic column, and the chromatographic column temperature is 42°C. The mobile phase is supercritical carbon dioxide, the flow rate is 3.5 times column volume / min, and the pressure is 13 MPa. The improver is methanol, and its ratio is 1.35%. The separation process is detected by an ultraviolet detector with a detection wavelength of 220nm, and fractions of target components are collected according to detection signals to obtain isoimperatorin and imperatorin respectively.

Embodiment 3

[0030] Weigh 500 grams of Angelica dahurica, pulverize it with a pulverizer, put it into a glass container, add 2200ml of petroleum ether, heat and reflux for extraction for 3 hours, and reflux for 3 hours each time, combine the extracts, filter, and concentrate under reduced pressure to obtain Angelica dahurica extract.

[0031] Angelica dahurica extract is dissolved with methanol, after filtration, carry out supercritical fluid chromatography separation, the chromatographic column is a C18 chromatographic column, and the chromatographic column temperature is 38 ℃. The mobile phase is supercritical carbon dioxide, the flow rate is 2.5 times column volume / min, and the pressure is 11 MPa. The improver is methanol, and its ratio is 0.95%. The separation process is detected by an ultraviolet detector with a detection wavelength of 220nm, and fractions of target components are collected according to detection signals to obtain isoimperatorin and imperatorin respectively.

[0032]...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention provides a method for separating and purifying isoimperatorin and imperatorin from angelica dahurica. The method comprises the following steps: crude angelica dahurica medicine is ground, petroleum ether is added, the mixture is subjected to backheating and refluxing, and an extracting solution is filtered and subjected to pressure reduction concentration to obtain an angelica dahurica extract; the angelica dahurica extract is dissolved with methanol, the mixture is filtered, a filtering product is subjected to supercritical fluid chromatographic separation, a chromatographic column adopts the C18 chromatographic column, a mobile phase adopts a supercritical fluid, and an improving agent adopts the methanol. An organic solvent harmful to the environment is not used, the production process is environment-friendly, and a product is free of residual hazardous substances; carbon dioxide is easy to recycle, and the energy consumption and the production cost are low.

Description

technical field [0001] The invention belongs to the field of chemical industry and pharmacy, and in particular relates to a method for separating and purifying isoimperatorin and imperatorin from the extract of Angelica dahurica. Background technique [0002] Angelica dahurica is a commonly used traditional Chinese medicine, which has the functions of dispersing wind and dehumidification, clearing orifices, relieving pain, reducing swelling and discharging pus. Coumarin is the main active ingredient in Angelica dahurica, among which imperatorin and isoimperatorin are relatively high in content, and these two substances are also the main indicators for the quality control of Angelica dahurica and its preparations. [0003] The traditional separation and purification methods of coumarin components in Angelica dahurica mostly use ether, petroleum ether and other solvents for extraction, and silica gel column chromatography for purification. This method has complicated steps, co...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/04
CPCC07D493/04Y02P20/54
Inventor 于琳琳孙爱玲李爱峰亢静静柳仁民
Owner LIAOCHENG UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap