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 complexity, many separation and purification steps, not enough environmental protection, etc., and achieve the effect of simple equipment, simple and feasible process, and low cost

Inactive Publication Date: 2011-02-16
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

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Experimental program
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Effect test

Embodiment 1

[0019] Take the small octagonal lotus roots and smash it into coarse powder, use ethanol as the organic solvent to pretreat the small octagonal lotus powder to make the small octagonal lotus powder in a strong osmotic and dissolving environment, and then add 9 times the amount of 80% ethanol Heat reflux extraction in hot water at 90°C for 60 minutes and filter, add 7 times the amount of 80% ethanol to the filter residue, continue hot reflux extraction in hot water at 100°C for 45 minutes, filter again, combine the two filtrates, and recover ethanol Then, the volume is fixed with an appropriate amount of water to obtain the podophyllotoxin extract. Take the podophyllotoxin extract to prepare a solution containing 0.121g / mL of the crude drug of the octagonal lotus as the loading solution, select the purified LSA5B macroporous adsorption resin as the upper column resin, and load the sample at a flow rate of 2BV / hr and fully After adsorption, wash away impurities with water and 10%...

Embodiment 2

[0021] The rhizome of the small octagonal lotus is crushed into coarse powder, and the organic solvent is mixed with ethanol and acetone in a ratio of 7:3, and the small octagonal lotus powder is pretreated to make the small octagonal lotus powder in a strong osmotic and dissolving environment, and then add 12 times the amount Ethanol with a concentration of 70% was extracted by refluxing in hot water at 95°C for 80 minutes and filtered. The filter residue was added with 15 times the amount of ethanol with a concentration of 70% and continued to be extracted with hot reflux in hot water at 95°C for 120 minutes and then filtered again and combined After the two filtrates, the ethanol is recovered and the volume is fixed with appropriate amount of water to obtain the podophyllotoxin extract. Take the podophyllotoxin extract and prepare a solution containing 0.152g / mL of the crude drug of the small octagonal lotus as the loading solution, select the purified HPD100 macroporous adso...

Embodiment 3

[0023] The rhizome of the small octagonal lotus is crushed into coarse powder, and the organic solvent is mixed with ethanol and ethyl acetate in a ratio of 9:1, and the small octagonal lotus coarse powder is pretreated so that the small octagonal lotus powder is in a strong osmotic and dissolving environment, and then 15 Ethanol with a doubled concentration of 90% was extracted by refluxing in hot water at 90°C for 60 minutes and filtered. The filter residue was added with 20 times the amount of ethanol with a concentration of 90% and continued to be refluxed in hot water at 90°C for 100 minutes and then filtered again , Combine the two filtrates, recover the ethanol and make the volume with an appropriate amount of water to obtain the podophyllotoxin extract. Take the podophyllotoxin extract to prepare a solution containing 0.152g / mL of the raw medicine of the small octagonal lotus as the sample liquid, select the purified HPD400 macroporous adsorption resin as the upper colum...

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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 small octagonal lotus. Background technique [0002] Podophyllotoxin belongs to the class of lignans, and mainly exists in the plants of the genus Podophyllum, the genus Paleocephalus, the genus Anemone, and the octagonal lotus of the Berberis family. It was included in the United States Pharmacopoeia in 1820 and was used to treat condyloma acuminata. The 0.5% podophyllotoxin tincture is the first choice for the treatment of condyloma acuminatum recommended by the World Health Organization (WHO). Podophyllotoxin can treat almost all warts, and it has a shorter treatment course, significant curative effect and fewer side effects than other methods. Podophyllotoxin and its similar compounds also have anti-measles, herpes simplex and anti-cytomegalovirus effects, and are also used as biological pesticides. However, anti-tumor and anti-virus are its most imp...

Claims

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Application Information

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