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Method for quickly and massively separating high purity triptolide from thunder god vine

A technology of triptolide and triptolide, which is applied in the field of rapid large-scale separation of high-purity triptolide, and achieves the effect of simple process, easy control and few steps

Inactive Publication Date: 2010-10-20
CHENGDU PUSH BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, Tripterygium wilfordii Polyglycoside Tablets are the main preparations on the market with Tripterygium wilfordii as raw material, which are used for rheumatoid arthritis, nephrotic syndrome, Behcet's triad, leprosy reaction, autoimmune hepatitis, etc., but its toxicity Larger, the difference between the effective dose and the toxic dose is very small, and the safety of the drug is difficult to control. The single most effective ingredient, triptolide, can also be used as a precursor for structural modification because it can control the dose well, and its demand is increasing. getting bigger
The content of triptolide in plants is extremely low. At present, it is mainly separated by repeated silica gel column chromatography at atmospheric pressure. The yield is low. Not only is it very toxic to operators, but it also consumes a lot of toxic solvents.

Method used

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  • Method for quickly and massively separating high purity triptolide from thunder god vine
  • Method for quickly and massively separating high purity triptolide from thunder god vine
  • Method for quickly and massively separating high purity triptolide from thunder god vine

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Experimental program
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Effect test

Embodiment 1

[0034] A method for rapidly and massively separating high-purity triptolide from Tripterygium wilfordii is characterized in that it is carried out according to the following process steps:

[0035] A. Heating extraction: select 30kg of tripterygium wilfordii stem and leaf coarse powder with a particle size of 10 mesh, add methanol at a mass ratio of 1:5, heat at 50°C for 3 hours, remove slag by filtration, recover the filtrate under reduced pressure to remove methanol, and obtain water suspension;

[0036] B. Solvent extraction: Take 10 L of the aqueous suspension obtained in step A, first extract with 20 L of petroleum ether, and then extract the aqueous phase with 30 L of dichloromethane, each extraction 3 times. The petroleum ether layer was discarded after recovery of petroleum ether, and the dichloromethane extracts were combined and concentrated at 50°C to obtain 150 g of dark yellow precipitate (density 1.26).

[0037] C. Chromatographic column chromatography: take 20 ...

Embodiment 2

[0042] A method for rapidly and massively separating high-purity triptolide from Tripterygium wilfordii is characterized in that it is carried out according to the following process steps:

[0043] A. Heating extraction: Select 500kg of coarse powder of tripterygium wilfordii with a particle size of 20 mesh, add 95% ethanol at a mass ratio of 1:5, heat at 55°C for 3 hours, filter to remove slag, and recover the filtrate under reduced pressure to remove ethanol After that, an aqueous suspension is obtained;

[0044] B. Solvent extraction: Take 500 L of the aqueous suspension obtained in step A, first extract with 1000 L of petroleum ether, and then extract the aqueous phase with 1500 L of dichloromethane, each extraction 5 times. The petroleum ether layer was discarded after recovery of petroleum ether, and the dichloromethane extracts were combined and concentrated at 55°C to obtain 9000 g of dark yellow precipitate (density 1.26).

[0045] C. Chromatographic column chromatog...

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Abstract

The present invention discloses a technique for separating out and purifying triptolide monomer from common threewingnut root. The technique is carried out according to the following technical steps: (A) heating and extraction: after ethanol or methanol is warmly soaked, dregs are removed; (B) solvent extraction: organic solvent is adopted to extract concentrated solution in order to enrich the product; (C) chromatographic column chromatography: with neutral alumina or silica gel as filler, dichloromethane-methanol or chloroform-methanol is used to carry out gradient elution, and cut fractionis collected by stages; (D) high-efficiency preparation and liquid phase separation; (E) crystallization: two-phase solvent crystallization is adopted to use petroleum ether-ethyl acetate, dichloromethane-methanol or methylene dichloride-ethyl acetate to crystallize the cut fraction collected by stages, so that the colorless spiculate crystal product of triptolide, the purity of which reaches over 99.5 percent, can be obtained. The technique, which has the advantages of simplicity, rapidness, little solvent consumption, economy, environment-friendliness and high yield, can prepare a large amount of the product for one time, thus having high economic and academic values.

Description

technical field [0001] The invention relates to a method for isolating active components from Chinese herbal medicinal materials, in particular, the invention relates to a method for quickly and massively isolating high-purity triptolide from Tripterygium wilfordii. Background technique [0002] Triptolide is the most active epoxidized diterpene lactone compound isolated from Tripterygium wilfordii Hook.f., a plant of the Euonymus family. It is one of the main active ingredients of Triptolide, and its related potency 100-200 times higher than tripterygium total glycosides. Pharmacological and clinical tests show that it has certain biological activities such as immunosuppression, anti-inflammation, anti-fertility and anti-tumor. At present, Tripterygium wilfordii Polyglycoside Tablets are the main preparations on the market with Tripterygium wilfordii as raw material, used for rheumatoid arthritis, nephrotic syndrome, Behcet's triad, leprosy reaction, autoimmune hepatitis,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J73/00A61P29/00A61P13/12A61P1/16
Inventor 张黎杨兵董维臻夏柯
Owner CHENGDU PUSH BIOLOGICAL TECH
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