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Process for extracting and purifying podophyllotoxin from Dysosma difformis

A technology of podophyllotoxin and star anise lotus, applied in the direction of organic chemistry, can solve the problems of many separation and purification steps, not enough environmental protection, and complexity, and achieve the effect of simple and feasible process, low cost and simple equipment

Inactive Publication Date: 2012-11-07
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above processes also have the problems of not being environmentally friendly, and the separation and purification steps are numerous and complicated.

Method used

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  • Process for extracting and purifying podophyllotoxin from Dysosma difformis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Take the rhizome of the small star anise and crush it into a coarse powder, use ethanol as an organic solvent, pretreat the small star anise coarse powder, make the small star anise coarse powder be in a strong osmotic and dissolution-promoting environment, and then add 9 times the amount of ethanol with a concentration of 80% Heat reflux extraction in hot water at 90°C for 60 minutes and filter, add 7 times the amount of ethanol with a concentration of 80% to the filter residue, continue heat reflux extraction in hot water at 100°C for 45 minutes, then filter again, combine the two filtrates, and recover ethanol Finally, dilute to volume with appropriate amount of water to obtain podophyllotoxin extract. The podophyllotoxin extract was prepared into a solution containing 0.121 g / mL of the crude drug of the star anise lotus as the sample solution, and the purified LSA5B macroporous adsorption resin was selected as the column resin, and the sample was loaded at a flow rat...

Embodiment 2

[0021] Take the rhizome of the small star anise lotus and crush it into a coarse powder, mix the organic solvent with ethanol and acetone at a ratio of 7:3, and pretreat the small star anise lotus coarse powder, so that the small star anise lotus coarse powder is in a strong osmotic and dissolution-promoting environment, and then add 12 times the amount Concentration is 70% ethanol in the hot water of 95 ℃ hot reflux extraction for 80 minutes and filtered, filter residue is added 15 times the amount of 70% ethanol to continue hot reflux extraction in 95 ℃ hot water for 120 minutes and then filtered again, combined The filtrates were recovered twice, and then the ethanol was recovered and the volume was fixed with an appropriate amount of water to obtain the podophyllotoxin extract. The podophyllotoxin extract was prepared into a solution containing 0.152 g / mL of the crude drug of the star anise lotus as the sample solution, and the purified HPD100 macroporous adsorption resin w...

Embodiment 3

[0023] Take the rhizome of the small star anise lotus and crush it into coarse powder, mix the organic solvent with ethanol and ethyl acetate at a ratio of 9:1, pretreat the small star anise lotus coarse powder, make the small star anise lotus coarse powder in a strong osmotic and dissolution-promoting environment, and then add 15 90% ethanol at 90°C for hot reflux extraction for 60 minutes and filtered, then add 20 times of 90% ethanol to the filter residue and continue hot reflux extraction for 100 minutes at 90°C for hot water and then filter again , combined two filtrates, recovered ethanol and dilute to volume with appropriate amount of water to obtain podophyllotoxin extract. The podophyllotoxin extract was prepared into a solution containing 0.152 g / mL of the crude drug of the star anise lotus as the sample solution, and the purified HPD400 macroporous adsorption resin was selected as the column resin, and the sample was loaded at a flow rate of 3BV / h and fully After ad...

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Abstract

The invention relates to a process for extracting and purifying podophyllotoxin from Dysosma difformis, which comprises the following steps: crushing rhizomes of the Dysosma difformis into coarse powder, pretreating the Dysosma difformis coarse powder with organic solvents, extracting with hot water by reflux, continuously extracting filter residue by hot reflux, filtering again, merging the two filtrates, recovering the organic solvents, adding a defined amount of water to maintain a constant volume so as to obtain a podophyllotoxin extracting solution; and preparing the podophyllotoxin extracting solution into a solution the crude drug content of which is 0.12-0.18g / mL, selecting a purified macroporous adsorptive resin as the adsorption column resin to sufficiently adsorb the solution acting as a sample solution, respectively and sequentially washing off impurities with water and 10% ethanol, eluting with a strippant, collecting the eluted part, recovering the strippant, and adding a defined amount of water to maintain a constant volume so as to obtain a podophyllotoxin purified solution. The organic solvents used in the process are nonpoisonous and can be recovered, and no three wastes polluting the environment are produced. The whole process is green and environment friendly and has the advantages of simple operation and easy industrialization, and the purity of the podophyllotoxin obtained by the process is above 98%.

Description

technical field [0001] The invention relates to a process for extracting and purifying podophyllotoxin from the natural plant Aniseum chinensis. Background technique [0002] Podophyllotoxin belongs to lignans, mainly found in Berberidaceae Podophyllum genus, Chrysanthemum genus, Heliconia genus and Star anise genus. It was recorded in the United States Pharmacopoeia in 1820 and is used to treat condyloma acuminatum. 0.5% tincture of podophyllotoxin is the first-choice medicine recommended by the World Health Organization (WHO) for the treatment of venereal genital warts. Podophyllotoxin can treat almost all warts, and compared with other methods, the course of treatment is shorter, the effect is significant, and the side effects are less. Podophyllotoxin and its similar compounds also have anti-measles, herpes simplex and anti-cytomegalovirus effects, and are also used as biological pesticides. But anti-tumor and anti-virus are its most important functions. Podophyllotoxi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/04
Inventor 张杰周春山
Owner CENT SOUTH UNIV