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Extraction preparation method of triptolide

A technology of triptolide and reflux extraction, applied in the field of medicine, can solve the problems of low enrichment rate of crude extract triptolide, complicated purification process, low efficiency, etc., and achieves simplified follow-up workload, simplified operation steps, The effect of improving economic efficiency

Active Publication Date: 2015-07-22
AKTIN CHEM INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, the extraction and purification methods of triptolide generally have defects such as low enrichment rate of triptolide in the crude extract, complicated purification process, long time consumption, low efficiency, low yield, and high cost.

Method used

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  • Extraction preparation method of triptolide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 300 kilograms of Tripterygium wilfordii medicinal material (after testing, its triptolide content is 0.0043%), pulverize to 20-30 meshes, put into extraction tank, add 3 tons of ethyl acetate, then add 360g ascorbic acid, heat and reflux extraction 3 times, Each time for 5 hours, the extract was filtered and concentrated under reduced pressure to obtain 8.3 kg of extract; 360 liters of dichloromethane was used to dissolve the extract, pour it into the extraction tank, and weigh 17.28 kg of NaOH to prepare 720 liters of 0.6moL / L NaOH solution , put into the extraction tank twice, carry out alkali washing on the dichloromethane solution twice, concentrate the dichloromethane phase to obtain 2 kg of extract after alkali washing; take 10 kg of 200-300 mesh Qingdao ocean column chromatography normal phase silica gel , a 35cm-diameter column in a wet method, after alkaline washing, the extract is loaded and then eluted with dichloromethane, and after the color of the eluent be...

Embodiment 2

[0039]200 kg of Tripterygium wilfordii medicinal material, crushed to 20-30 mesh, put into an extraction tank, add 3 tons of ethyl acetate, heat and reflux for extraction twice, each time for 4 hours, the extract is filtered and concentrated under reduced pressure to obtain 6.0 kg of extract; Dissolve the extract with 300 liters of dichloromethane, put it into the extraction tank, weigh 14.4 kg of NaOH, prepare 450 liters of 0.8moL / L NaOH solution, put it into the extraction tank in 3 times, and wash the dichloromethane solution with alkali for 3 Once, concentrate the dichloromethane phase to obtain 1.2 kg of extract after alkali washing; take 12 kg of 200-300 mesh Qingdao Ocean column chromatography normal phase silica gel, install a column with a diameter of 35 cm in a wet method, and use two Chloromethane elution, after the color of the eluent becomes light, use dichloromethane:methanol=10:1 mixed solvent to elute 2 column volumes, then elute with methanol, concentrate the m...

Embodiment 3

[0041] 250 kg of Tripterygium wilfordii medicinal material (after testing, its triptolide content is 0.0039%), crushed to 20-30 meshes, put into an extraction tank, added 2.5 tons of ethyl acetate, then added 375g of ascorbic acid, heated and refluxed twice, For 4 hours each time, the extract was filtered and concentrated under reduced pressure to obtain 6.3 kg of extract; 220 liters of dichloromethane was used to dissolve the extract, pour it into the extraction tank, and weigh 4.8 kg of NaOH to prepare 240 liters of 0.5moL / L NaOH solution , into the extraction tank in 2 times, 130 liters for the first time, 110 liters for the second time, carry out alkali washing 2 times to the dichloromethane solution, concentrate the dichloromethane phase to obtain 1.6 kg of extract after alkali washing; take 6 kg 200-300 mesh Qingdao ocean column chromatography normal-phase silica gel, wet-packed column diameter 20cm, after alkaline washing, the extract is loaded with dichloromethane and t...

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Abstract

The invention provides an extraction preparation method of triptolide. The method comprises the steps of extracting thunder god vine herbs by utilizing ethyl acetate, dissolving extract by utilizing dichloromethane, then carrying out the alkali wash, carrying out the secondary positive silica-gel column chromatography, carrying out the elution sequentially by utilizing dichloromethane, dichloromethane / methanol mixed solvent and methanol for the primary column chromatography, carrying out the gradient elution by utilizing petroleum ether / ethyl acetate mixed solvent for the secondary column chromatography, and finally preparing a triptolide pure product in a crystallizing manner. The preparation method is fewer in steps and simple to operate, the triptolide product with high purity can be effectively obtained, and the production cost of the triptolide can be greatly reduced.

Description

technical field [0001] The invention relates to a method for extracting and preparing triptolide, which belongs to the technical field of medicine. Background technique [0002] Tripterygium wilfordii Hook f. is a plant of the genus Tripterygium wilfordii Hook f., which is recorded in the Chinese Medicine Dictionary. It has the effects of expelling wind and dampness, dredging collaterals and relieving pain, reducing swelling and pain, detoxifying and killing insects. It is clinically used to treat rheumatoid joints In recent years, it has been used in the anti-rejection treatment of organ transplantation, and has achieved good curative effect. Modern studies have successively found that Tripterygium wilfordii has anti-inflammatory, anti-immune, anti-fertility, anti-tumor, and antibacterial activities. So far, more than 200 chemical monomers have been isolated from Tripterygium wilfordii, among which diterpenoids, sesquiterpene alkaloids, and triterpenoids are the main activ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J73/00
CPCC07J73/003
Inventor 谢相林付书青
Owner AKTIN CHEM INC
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