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A method for preparing high-purity triptolide by membrane separation technology

A technology for triptolide and membrane separation, which is applied in the field of medicine, can solve the problems of high consumption of toxic solvents, complex processes, and long time consumption, and achieve the effects of improving extraction efficiency and yield, protecting personal safety, and reducing production costs

Active Publication Date: 2018-10-16
桂林三棱生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the content of triptolide in Tripterygium wilfordii is extremely low. At present, the main use of medicinal materials is to extract repeatedly, and to separate through silica gel column chromatography at normal pressure, and the yield is also very low. According to literature reports, the plant separation yield is only 0.001%, and the consumption of toxic solvents in the extraction and separation process is large, and it is also very toxic to operators
The current process generally has defects such as complex process, long time-consuming, high cost, and large environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Crush 250Kg of triptolide medicinal material (the content of triptolide is 0.0036%), crush it into 30-50 meshes, put it into the extraction container, add 2000Kg of 80% ethanol solution according to the mass ratio, and reflux extraction for 3 times, 4 hours each time, Filter and combine the extracts;

[0034] Put the Tripterygium wilfordii extract into the concentration tank and concentrate to a relative density of 1.07;

[0035] Centrifuge the concentrated solution and collect the supernatant;

[0036] Filter with a 200nm ceramic membrane filter;

[0037] After fine filtration, the extract of Tripterygium wilfordii is pumped into the membrane filtration system, and under the condition of 0.50-1.0MPa, it is filtered through an ultrafiltration membrane with a molecular weight of 1000 to obtain the dialysate of Tripterygium wilfordii;

[0038] Concentrate Tripterygium wilfordii dialyzate to dryness to obtain extract 0.51Kg, dissolve it in dichloromethane, mix the sample...

Embodiment 2

[0041] Crush 400Kg of triptolide medicinal material (the content of triptolide is 0.0041%), crush it into 30-50 meshes, put it into an extraction container, add 2500Kg of 75% ethanol solution according to the mass ratio, and reflux extraction for 3 times, 5 hours each time, Filter and combine the extracts;

[0042] Put the Tripterygium wilfordii extract into the concentration tank and concentrate to a relative density of 1.06;

[0043] Centrifuge the concentrated solution and collect the supernatant;

[0044] Filter with a 200nm ceramic membrane filter;

[0045] After fine filtration, the extract of Tripterygium wilfordii is pumped into the membrane filtration system, and under the condition of 0.50-1.0MPa, it is filtered through an ultrafiltration membrane with a molecular weight of 1000 to obtain the dialysate of Tripterygium wilfordii;

[0046] Concentrate Tripterygium wilfordii dialyzate to dryness to obtain extract 0.86Kg, dissolve it with ethyl acetate, mix the sample ...

Embodiment 3

[0049]Crush 350Kg of triptolide medicinal material (the content of triptolide is 0.0032%), crush it into 30-50 meshes, put it into the extraction container, add 2100Kg of 80% ethanol solution according to the mass ratio, and reflux extraction for 3 times, 4.5 hours each time, Filter and combine the extracts;

[0050] Put the Tripterygium wilfordii extract into the concentration tank and concentrate to a relative density of 1.08;

[0051] Centrifuge the concentrated solution and collect the supernatant;

[0052] Filter with a 200nm ceramic membrane filter;

[0053] After fine filtration, the extract of Tripterygium wilfordii is pumped into the membrane filtration system, and under the condition of 0.50-1.0MPa, it is filtered through an ultrafiltration membrane with a molecular weight of 1000 to obtain the dialysate of Tripterygium wilfordii;

[0054] Concentrate the dialysate of Tripterygium wilfordii to dryness to obtain 0.62Kg of extract, dissolve it in dichloromethane, mix...

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Abstract

The invention discloses a method for preparing high-purity triptolide by adopting a membrane separation technology. The method comprises the following steps: taking thunder god vine extracted by taking ethanol solution as a solvent as a raw material, carrying out coarse filtration, then carrying out separation and impurity removal by adopting an appropriate membrane, obtaining a triptolide crude product after macromolecular impurities are removed, further concentrating, and passing a silicagel column once, so that the triptolide colorless needle-like crystal product with the purity more than 99% can be obtained. The method disclosed by the invention replaces a method that a large amount of organic solvent is used for extraction firstly and then column chromatography is carried out for multiple times in the traditional technology, technology is simplified, separation at normal temperature can be realized, and thermosensitive substances can not be destroyed; meanwhile, a large amount of a toxic organic solvent is saved, the environment is protected, production cost is reduced, and yield is high and safety and reliability are realized, so that the method has strong economic competitiveness and accords with nationally advocated traditional Chinese medicine green development concept.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a method for preparing high-purity triptolide by adopting membrane separation technology. Background technique [0002] Tripterygium wilfordii Hook. f. (Latin scientific name Tripterygium wilfordii Hook. f.), also known as Huangteng, Huanglateng, vegetable insect medicine, etc., is a traditional Chinese medicine with a long and widely used history. It is the root of Tripterygium wilfordii of the Euonymus family Tripterygium genus. This taste is bitter, pungent, cool in nature, and highly poisonous. Return liver, kidney channel. Efficacy Expelling wind and dampness, dredging collaterals and relieving pain, reducing swelling and pain, detoxifying and killing insects. It is used for damp-heat nodules and cancerous tumors to accumulate poison. It is used clinically to treat leprosy reactions, rheumatoid arthritis, etc., and has anti-tumor and anti-inflammatory effects. The main co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J73/00
CPCC07J73/003
Inventor 毛武德唐荣军张学梅聂元壮
Owner 桂林三棱生物科技有限公司
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