Method for preparing daphnetin from daphne giraldii nitsche

A technology of daphnetin and ancestors, applied in the direction of organic chemistry, etc., can solve the problems of low degree of industrialization, low resin resolution rate, large amount of organic reagents, etc.

Inactive Publication Date: 2010-09-08
NANJING ZELANG AGRI DEV
View PDF0 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] 1) The amount of organic reagents is large and there are many types (extraction method);
[0011] 2) low degree of industrialization (liquid chromatography preparation method);
[0012] 3) The resin resolution rate is low

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take Zushima medicinal material, remove impurities and pulverize, weigh 1kg, put it into a flask, add 10L water to reflux for 2 hours to extract, and extract 3 times. Take 500g of the treated D101 resin, put it into a column, add the extract to the resin column after passing through a 300 mesh sieve, control the flow rate to 75L / h, repeat the adsorption 4 times, and elute the resin column with deionized water after the extraction is completed. To sugar-free color, use 3L of 60% ethanol to elute impurities, and then use 3L of 75% ethanol to elute Daphnetin. The elution temperature is controlled at 50-60°C. Collect the eluate and concentrate it with a rotary evaporator. Stop concentrating when there is no alcohol smell. Place the crystals, centrifuge to obtain 20g of crude crystals, reflux with deionized water to dissolve the secondary crystals, centrifuge to obtain 15g of secondary crystals, then reflux with 50%, 70%, and 95% ethanol to dissolve the crystals, and centrifu...

Embodiment 2

[0024] Take Zushima medicinal material, remove impurities and pulverize, weigh 1kg, put it into a flask, add 5L of water and reflux for 3 hours to extract, and extract 3 times. Take 500g of the treated HPD100 resin, put it into a column, add the extract to the resin column after passing through a 300 mesh sieve each time, control the flow rate at 50L / h, repeat the adsorption for 3 times, and elute the resin column with deionized water after the extraction is completed. To sugar-free color, use 2.4L 60% ethanol to elute impurities, then use 2L 75% ethanol to elute Daphnetin, control the elution temperature at 50-60°C, collect the eluate, concentrate it with a rotary evaporator, stop concentrating if there is no alcohol smell , place the crystals, centrifuge to obtain 17g of crude crystals, reflux with deionized water to dissolve the secondary crystals, centrifuge to obtain 13g of secondary crystals, then use 50%, 70%, and 95% ethanol to reflux to dissolve the crystals, and centr...

Embodiment 3

[0026] Take Zushima medicinal material, remove impurities and pulverize, weigh 1kg, put it into a flask, add 10L water to reflux for 2 hours to extract, and extract 3 times. Take 500g of the treated HZ816 resin, put it into a column, add the extract to the resin column after passing through a 300 mesh sieve, control the flow rate at 5L / h, repeat the adsorption for 3 times, and elute the resin column with deionized water after the extraction is completed. To sugar-free color, use 3L of 60% ethanol to elute impurities, and then use 3L of 75% ethanol to elute Daphnetin. The elution temperature is controlled at 50-60°C. Collect the eluate and concentrate it with a rotary evaporator. Stop concentrating when there is no alcohol smell. Place the crystals, centrifuge to obtain 19g of crude crystals, reflux with deionized water to dissolve the secondary crystals, centrifuge to obtain 16g of secondary crystals, then reflux with 50%, 70%, and 95% ethanol to dissolve the crystals, and cent...

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 relates to a method for preparing daphnetin from daphne giraldii nitsche. The method comprises the following steps of: crushing a daphne giraldii nitsche serving as a raw material, adding water into the powder, refluxing and extracting; filtering extract, and quickly adding a macroporous resin column into the extract for adsorption, and repeatedly adsorbing the extract for 2 to 3 times; washing the extract with deionized water until the extract does not have sugar color; eluting impurities with 60 percent ethanol, and eluting active ingredients with 75 percent hot ethanol (50-60 DEG C); concentrating alcohol-free crystal; dissolving secondary crystal with boiling water; recrystallizing with ethanol; and centrifugally drying the crystal to obtain daphnetin crystal. The method for preparing the daphnetin has the advantages of simple process, simple variety of used organic reagents, high product content, and easy industrialization.

Description

Technical field: [0001] The invention relates to a method for preparing daphnetin from zushima, in particular to a method for preparing daphnetin by macroporous resin adsorption and hot ethanol elution. Background technique: [0002] Daphnetin, also known as Zushimajia element, belongs to the flavonoid coumarin. [0003] Molecular formula: C9H6O4 [0004] Molecular weight: 178.14 [0005] Daphnetin is soluble in boiling water, hot dilute ethanol, hot glacial acetic acid, slightly soluble in ether, chloroform and ethyl acetate, and has sublimation property. Daphnetin has pharmacological effects such as dilating capillaries, analgesia, sedation and anti-inflammation. For example, the document "Research Status of Daphnetin Pharmacological Actions" published by Zhang Wenliang et al. lists the pharmacological actions and uses of daphnetin in detail. [0006] Zushima is the root bark or stem bark of Daphne chrysantha, a plant of Daphneaceae, which has the effects of dispelling...

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): C07D311/18
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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