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Method for extracting tripterine from celastrus orbiculatus root cortex

A technology of triptolide and eucalyptus, applied in the directions of steroids, organic chemistry, etc., can solve the problems of high extraction rate of raw materials and no mention of the preparation of triptolide monomers.

Inactive Publication Date: 2010-02-03
安徽省科学技术研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process adopts 95% ethanol extraction, and the total diterpenes and triterpenoids of the vine cane can be obtained after ethyl acetate extraction. The advantages are high extraction rate of raw materials, low cost, and easy operation, but there is no mention of the monomer preparation of Tripterygium wilfordii

Method used

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  • Method for extracting tripterine from celastrus orbiculatus root cortex
  • Method for extracting tripterine from celastrus orbiculatus root cortex
  • Method for extracting tripterine from celastrus orbiculatus root cortex

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Select 300 g of the coarse powder of the root bark of S. chinensis with a particle size of 20 mesh, add 1,2-dichloroethane at a mass ratio of 1:5, heat and reflux for extraction for 4 hours, and reflux twice. After filtration, the combined filtrates were concentrated under reduced pressure to recover 1,2-dichloroethane to obtain 0.39 g of dark red extract (primary extract) with a red pigment content of 9.2%. Add 50vt% methanol solution to dissolve, a white precipitate precipitates out of the solution, let it stand still, take the supernatant to concentrate and repeat the treatment 2-3 times to obtain the crude extract of tripteryglide, the content of tripteryne is 51.3%. The crude extract was dissolved in methanol and the stationary phase was reversed phase C 18 Separation is carried out on the preparative chromatography, the eluent is 83vt% methanol aqueous solution, the pH is adjusted to 3 with acetic acid, the tripterylide fractions are collected according to the pre...

Embodiment 2

[0033] Select 300 g of the coarse powder of the root bark of S. chinensis with a particle size of 20 mesh, add metatrichloroethane at a mass ratio of 1:7, heat and reflux for extraction for 5 hours, and reflux twice. After filtering, the combined filtrates were concentrated under reduced pressure to recover metatrichloroethane to obtain 0.41 g of dark red extract (initial extract) with tripterine content of 10.3%. Add 60vt% ethanol solution to fully dissolve, white precipitate precipitates out in the solution, take the filtrate after filtration, repeat the same treatment 2-3 times again after concentrating, and obtain tripteryglide crude extract, tripteryne content 48.2%. The crude extract was dissolved in methanol and the stationary phase was reversed phase C 18 Separation is carried out on the preparative chromatography, the eluent is 85vt% methanol solution, the pH is adjusted to 3 with acetic acid, the tripterylide fraction is collected according to the preparative chromat...

Embodiment 3

[0035]Select 300 g of the coarse powder of the root bark of S. chinensis with a particle size of 20 mesh, add chloroform at a mass ratio of 1:10, heat and reflux for extraction for 5 hours, and reflux twice. After filtering, the combined filtrates were concentrated under reduced pressure to recover chloroform to obtain 0.47 g of dark red extract (initial extract) with tripterine content of 10.1%. Add 60vt% methanol solution, the solution is turbid, let it stand, filter and concentrate the filtrate and repeat the same treatment 2-3 times again to obtain the tripterylide crude extract with a tripterylide content of 53.1%. The crude extract was dissolved in methanol and mixed with silica gel to separate the stationary phase into a normal-phase silica gel atmospheric pressure column. The eluent was chloroform / methanol (60:40) isocratic elution, followed by TLC monitoring, and the tripterine fraction was collected and concentrated. After evaporating to dryness, the essence-producin...

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Abstract

The invention discloses a method for extracting tripterine from celastrus orbiculatus root cortex, which uses celastrus orbiculatus root cortex powder as a raw material and comprises the steps of extraction, separation, purification and recrystallization. The extraction step comprises the following steps: firstly using low-level chloralkane as a solvent; heating, reflowing and extracting the solvent, wherein the quality ratio of the root cortex powder and the solvent is 1:(3-20), and the time is not less than 2 hours; desolventizing an extracting liquid to obtain an extractum-type primary extract; adding 50-70 percent by weight of methanol or ethanol solution into the primary extract; sufficiently stirring, standing and extracting; and desolventizing the extracting liquid to obtain a densepaste rough extract. The purification step comprises the following steps: dissolving the mathnol by using the rough extract; carrying out column chromatography separation and purification on a normalphase silica gel or a reverse phase silica gel by using a solid phase; collecting eluent; desolventizing and drying to obtain a powder refined extract; and finally carrying out recrystallization by using the mixed solvent of the ethanol and the water. The method has simple separation and purification processes so as to obtain the tripterine with the purity of 98 percent.

Description

1. Technical field [0001] The invention relates to a method for preparing natural chemicals from plants, in particular to a method for extracting tripterine from root bark of Serpentis vine. 2. Background technology [0002] The molecular formula of tripterine is C 29 h 38 O, also known as Celastrol, is a pentacyclic triterpenoid present in plants such as Tripterygium wilfordii and Celastrol. Its structural formula is shown in the figure. [0003] Previous studies have shown that tripterygium can inhibit the proliferation of various cancer cells, including leukemia, glioma, and prostate cancer. In addition, there is evidence that tripterine can participate in the regulation of pro-inflammatory cytokines, inducible nitric oxide synthase, adhesion molecules, proteasome activity, topoisomerase, potassium channels, and heat shock response. In vivo studies, tripterine can significantly inhibit the proliferation of prostate cancer and pancreatic cancer cell tumor suppressor m...

Claims

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Application Information

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IPC IPC(8): C07J63/00
Inventor 陈龙胜许舒雯吕杨陈兰
Owner 安徽省科学技术研究院
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