Preparation method of 20-deoxyingenol

A technology of ingenol and euphorbia, which is applied in the field of preparation of ingenol diterpenoids, can solve the problems of poor repeatability, long time-consuming, large consumption of reagents, etc.

Inactive Publication Date: 2021-02-05
SHENYANG PHARMA UNIVERSITY
View PDF1 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the preparation of 20-deoxyingenol is mainly through the traditional extraction and separation method, which has many defects, such as long time-consuming, large reagent consu

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
  • Preparation method of 20-deoxyingenol
  • Preparation method of 20-deoxyingenol
  • Preparation method of 20-deoxyingenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 1.0 kg of dry root tubers of Euphorbiaceae Euphorbi genus Gansui, reflux extraction with 2 L of 75% methanol water for 3 times, each time for 1.5 hours, and combine the extracts; filter the extracts, concentrate under reduced pressure to obtain 109 g of extract a Add 500mL of water to extract a, extract 5 times with ethyl acetate equal to the volume of water, combine the extract phases, concentrate under reduced pressure to obtain 14.2g of extract b; dissolve extract b with 160mL of anhydrous methanol and add 2.2g Potassium carbonate, stirred at room temperature for 8 hours, then added 1N hydrochloric acid at 0°C for neutralization and adjusted the pH to 6-7. Concentrate under reduced pressure, then add 200mL saturated saline to dilute, then add an equal volume of ethyl acetate to extract 3 times, concentrate under reduced pressure to obtain 10.0g extract c; dissolve extract c in 50mL methanol, add 100 mesh HP-20 resin 100g to mix the sample And packed into a colum...

Embodiment 2

[0028]Take 1 kg of dry root tubers of Euphorbiaceae Euphorbi genus Gansui, reflux extract with 2L of 75% ethanol water for 3 times, each time for 2 hours, and combine the extracts; filter the extracts, concentrate under reduced pressure to obtain 158 g of extract a; Add 500mL of water to the extract a to suspend, extract 5 times with ethyl acetate equal to the volume of water, combine the extract phases, and concentrate under reduced pressure to obtain 20.1g of extract b; dissolve extract b with 200mL of anhydrous methanol and add 5.0 g potassium carbonate, stirred at room temperature for 4 hours, then added 1N hydrochloric acid at 0°C for neutralization and adjusted the pH to 6-7. Then concentrate under reduced pressure and add 200mL saturated saline to dilute, then add an equal volume of dichloromethane to extract 5 times, concentrate under reduced pressure to obtain 15.6g of extract c; extract c is mixed with 200mL of 100 mesh HP-20 resin 100g and packed into a column, The ...

Embodiment 3

[0030] Take 1 kg of dry root tuber of Euphorbiaceae Euphorbi genus Gansui, reflux extraction with 75% ethanol water 2L for 5 times, each time for 1.5 hours, and combine the extracts; filter the extracts, concentrate under reduced pressure to obtain 149 g of extract a; Add 500mL of water to extract a to suspend, extract 5 times with ethyl acetate equal to the volume of water, combine the extract phases, concentrate under reduced pressure to obtain 19.0g of extract b; dissolve extract b with 200mL of anhydrous methanol and add 4.0 g barium hydroxide, stirred at room temperature for 6 hours, then added 1N hydrochloric acid at 0°C for neutralization and adjusted the pH to 6-7. After concentrating under reduced pressure, add 200 mL of saturated saline to dilute, then add an equal volume of ethyl acetate to extract 5 times, concentrate under reduced pressure to obtain 14.5 g of extract c; add 150 g of 100 mesh HP-20 resin to dissolve extract c in 50 mL of methanol The sample was pac...

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 the technical field of medicines for extracting and separating effective components in medicinal plants, in particular to a preparation method of ingenane diterpenoid compounds. The preparation method comprises the following steps of by taking dry tuberous roots of euphorbia kansui (Euphorbia kansui T.N.Liou ex T.P.Wang) as a raw material, extracting with an organic solvent, extracting, carrying out alkaline hydrolysis, carrying out macroporous resin column chromatography, and carrying out high performance liquid chromatography separation, thereby obtaining the product. According to the method, the separation efficiency and the yield can be greatly improved, the yield of the 20-deoxyingenol is over 100mg/kg, the yield is high, the repeatability is good, and the requirements of industrial production can be met after process amplification.

Description

technical field [0001] The invention relates to the technical field of medicine for extracting and separating active ingredients in medicinal plants, in particular to a preparation method of ingenane diterpenoids. Background technique [0002] Gansui (Euphorbia kansui T.N.Liou ex T.P.Wang) is the dry root tuber of Euphorbia genus (Euphorbia.) in the family Euphorbiaceae. Gansui is rich in resource reserves, widely distributed in Gansu, Shanxi, Shaanxi, Ningxia, Henan, Qinghai and other provinces. Gansui has the functions of purging water, dispelling swelling, reducing swelling and dissipating stagnation, etc. It is mainly used by folks to induce labor, edema and treat various difficult diseases. And its methanol extract showed obvious activity in the preliminary determination of HIV virus-related activity. Ingenane diterpene is a characteristic component of Gansui, which is composed of a 5-membered ring (A ring) and two 7-membered rings (B ring and C ring) system. The C-8 ...

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
IPC IPC(8): C07C49/727C07C45/64C07C45/78C07C45/79
CPCC07C45/64C07C45/78C07C45/79C07C2603/86C07C49/727
Inventor 宋少江刘庆博李吉翀任会王茹祺
Owner SHENYANG PHARMA UNIVERSITY
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