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Method for extracting tripchlorolide from tripterygium wilfordii front segment

A technology for triptolide wilfordii and chlorinolide is applied in the field of extracting a single component triptolide clololactone alcohol, which can solve the problems of a small amount of triptolide clololactone alcohol, a low extraction yield, and inability to be used in large-scale production, and achieves the Effects of Tripterygium wilfordii clolactone alcohol content increase, simplification of separation and purification process, and simple and easy purification process

Active Publication Date: 2014-03-19
浙江得恩德制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Tripchlorolide is an epoxy diterpene lactone compound isolated from Tripterygium genus Euonymus. Pharmacological tests show that It has strong anti-inflammatory, immunosuppressive and male anti-fertility effects, and its potency is 100-200 times that of the currently clinically used "tripterygium glycosides" preparation. One of the main active monomers, and it has been proven to have no mutagenic effect, but the extraction rate of this compound from the original plant is extremely low
[0003] Chinese Patent No. 89105433.2 discloses the preparation method of tripterydrolactone and its anti-fertility application. Chromatographic separation of the extract after feeding, the process is to adopt the method of multiple chromatography, and after rotating thin layer chromatography, the amount of tripterygium chloride finally obtained is very small, and it cannot be used for large-scale production at all.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Take 4100g of the concentrated extract of the front part of Tripterygium wilfordii, add 4500ml of acetone and 400ml of hydrochloric acid, put it in a 10000ml round bottom flask, put it in a water bath and heat it to reflux at 80°C, and react for 2 hours when it starts to reflux, take it out, add 4500ml of purified water, and use plastic Stir the rod evenly and let it stand overnight; the next day separate the upper acetone solution, filter it with filter paper, put the filtrate on a water bath at 65°C to recover acetone (600ml per 2000ml), then adjust it to 80°C to recover about 1000ml of concentrated solution, pour The filtrate was extracted three times with chloroform, and the extract was dried under reduced pressure after recovering the chloroform to obtain 241.986 g of the transformed product powder. The conversion product was applied to a silica gel column at a ratio of 1:10, ethanol-chloroform gradient elution, T4 was collected, drained, and the dried product was r...

Embodiment 2

[0019] Take 30Kg of the concentrated extract of Tripterygium wilfordii, add ethanol 90Kg, hydrochloric acid 1800ml, heat and reflux with steam in the enamel reaction pot for 6 hours, put it in a plastic storage bucket, add 90Kg of water, turn on the mixer and stir for 15 minutes, and let it stand overnight; the next day vacuum Aspirate the upper layer solution, recover ethanol in the enamel reaction pot, release it when it is concentrated to about 1 / 3, add chloroform to the filtrate and extract three times, the extract is dried under reduced pressure after recovering chloroform to obtain 7.215Kg of crude extract powder (yield 24.05% ). Put the crude extract powder into a large stainless steel column (30×500cm) for silica gel chromatography to obtain 1343.3 g of fine extract powder. The fine extract powder was recrystallized twice with chloroform to obtain 161.2 g of white crystals with a measured content of 98.5% triptolide.

[0020]

Embodiment 3

[0022] Take 100Kg of the concentrated extract of the front part of Tripterygium wilfordii, add methanol 500Kg, hydrochloric acid 20L, steam heat and reflux in the enamel reaction pot for 6 hours, put it in a plastic storage bucket, add 500Kg of water, turn on the mixer and stir for 15 minutes, and let it stand overnight; the next day vacuum Aspirate the upper layer solution, recover methanol in the enamel reaction pot, release it when concentrated to about 1 / 3 of the volume, add chloroform to the filtrate and extract three times, the extract is dried under reduced pressure after recovering chloroform to obtain 20.14Kg of crude extract powder (yield 20.14% ). Put the crude extract powder into a large stainless steel column (30×500cm) for silica gel chromatography to obtain 2348.6 g of fine extract powder. The fine extract powder was recrystallized twice with chloroform to obtain 422.75 g of white crystals with a measured content of 99.01% triptolide.

[0023] The high performa...

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Abstract

The invention discloses a method for extracting tripchlorolide from tripterygium wilfordii front segment extractum. At present, tripchlorolide with little amount is obtained by employing a multi-time chromatography method to perform chromatographic separation on tripterygium glycosides or an extraction product directly extracted from tripterygium wilfordii raw material by ethanol and perform rotating thin layer chromatography, and the method cannot be used to large-scale production at all. The method provided by the invention comprises: utilizing a hydrophilic solvent low alcohol / ketone to perform extraction on the tripterygium wilfordii front segment extractum, separating majority of lipophilic impurities in the front-segment extractum, then extracting with trichloromethane to separate some other non-target products with relatively small solubility in the low alcohol / ketone, then performing chromatographic separation purification, and finally utilizing chloroform to perform recrystallization. The method provided by the invention is simple and practicable in separation and purification technology, is suitable for industrialized large-scale production; and the prepared tripchlorolide is applicable to develop new drugs.

Description

technical field [0001] The invention relates to a method for preparing natural chemicals from plant extracts, in particular to a method for extracting tripterygium chloractone, a single component, from the extracts of tripterygium wilfordii. Background technique [0002] Tripchlorolide is an epoxy diterpene lactone compound isolated from Euonymus genus Tripterygium. Pharmacological tests show that it has strong anti-inflammatory, immunosuppressive and male anti-fertility effects , its potency is 100-200 times that of the currently clinically used "tripterygium glycosides" preparation, and it is one of the main active monomers of tripterygium wilfordii to display anti-inflammatory, immunosuppressive and male anti-fertility effects, and it has been proven that it has no mutagenesis, but the extraction rate of the compound from the original plant is extremely low. [0003] Chinese Patent No. 89105433.2 discloses the preparation method and anti-fertility application of tripte...

Claims

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Application Information

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IPC IPC(8): C07J73/00
Inventor 刘法千金春晖吕文辉
Owner 浙江得恩德制药股份有限公司
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