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Method for extracting podophyllotoxin from dysosma versipellis

A technique for podophyllotoxin and extraction, applied in directions such as organic chemistry, can solve problems such as no preparation process report, and achieve the effects of stable process, low energy consumption and low production cost

Inactive Publication Date: 2013-01-16
NANJING ZHENGLIANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no report on the preparation process suitable for the large-scale industrial production of high-purity podophyllotoxin

Method used

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  • Method for extracting podophyllotoxin from dysosma versipellis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1 Take 10 kg of star anise lotus, pulverize it, add 15 times its mass and volume of ethanol with a concentration of 80%, put it into a microwave extraction device for microwave extraction, extraction power 300W, extract 2 times, 5 minutes each time, and combine the extracts , filter, recover ethanol under reduced pressure and concentrate, add to D101 macroporous adsorption resin column for adsorption, elute with 50% ethanol, collect 3 times the column volume eluate, recover ethanol under reduced pressure and concentrate, add to polyamide (Polyamide 6) chromatographic column, eluted with a mixed solvent of dichloromethane-methanol at a ratio of 4:1, and the same type of polyamide film was developed with the above eluent as a supporting detection, and the corresponding polyamide film was collected For the fraction with Rf=4-5, the solvent was recovered under reduced pressure, acetone was added to crystallize, the crystals were separated, washed and dried to obtain ...

Embodiment 2

[0021] Example 2 Take 10 kg of star anise lotus, pulverize it, add 85% ethanol with a concentration of 18 times its mass and volume, and put it into a microwave extraction device for microwave extraction. The extraction power is 400W, and the extraction is performed 3 times, each time for 10 minutes, and the extracts are combined , filter, recover ethanol under reduced pressure and concentrate, add to D102 macroporous adsorption resin column for adsorption, elute with 60% ethanol, collect 5 times the column volume eluate, recover ethanol under reduced pressure and concentrate, add to polyamide (Polyamide 66) chromatographic column, eluted with a mixed solvent of dichloromethane-methanol at a ratio of 4:1, and the same type of polyamide film was developed with the above eluent as a supporting detection, and the corresponding polyamide film was collected For the fraction with Rf=4-5, the solvent was recovered under reduced pressure, acetone was added to crystallize, the crystals ...

Embodiment 3

[0022] Example 3 Take 10 kg of star anise lotus, pulverize it, add 20 times its mass and volume of ethanol with a concentration of 90%, put it into a microwave extraction device for microwave extraction, extract power 600W, extract 4 times, each time for 20 minutes, and combine the extracts , filter, recover ethanol under reduced pressure and concentrate, add to AB-8 macroporous adsorption resin column for adsorption, elute with 70% ethanol, collect 8 times the column volume eluate, recover ethanol under reduced pressure and concentrate, add to On a polyamide (polyamide 11) chromatography column, elute with a mixed solvent of dichloromethane-methanol at a ratio of 4:1, use the same type of polyamide film to develop with the above eluent as a supporting detection, and collect the corresponding polyamide For the fraction with Rf=4-5 on the amide film, the solvent was recovered under reduced pressure, crystallized by adding acetone, separated and crystallized, washed and dried to ...

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Abstract

The invention relates to a method for extracting podophyllotoxin from dysosma versipellis. The method comprises the steps as follows: extracting with waveform to obtain extract; adding the extract to macroreticular resin column to absorb; eluting; recovering alcohol in a pressure reduced way; concentrating; adding the concentrate to polyamide chromatographic column; eluting; carrying out support detection with homogenous polyamide film by utilizing the eluant; collecting; recovering the solvent in a pressure reduced way; adding acetone to crystallize; separating and crystallizing; washing; and drying to obtain the product. The method provided by the invention is simple in operation, less in consumption of solvent, low in production cost, stable in technology, low in energy consumption and pollution, and high in purity of the obtained product (99%), and is suitable for experiment and industrial preparation and preparative production.

Description

technical field [0001] The invention relates to a method for extracting podophyllotoxin, in particular to a method for extracting podophyllotoxin from star anise lotus. Background technique [0002] The star anise lotus is the root and rhizome of the Berberidaceae plants star anise lotus, hexagonal lotus and Sichuan star anise lotus. Resolving phlegm and dispelling stagnation; dispelling blood stasis and relieving pain; clearing heat and detoxifying. For cough; sore throat; scrofula; goiter; carbuncle; furunculosis; poisonous snake bites; bruises; Podophyllotoxin is contained in star anise lotus, and its structural formula is: [0003] [0004] Studies have shown that: Podophyllotoxin targets condyloma acuminata, multiple superficial epithelioma (such as multiple superficial or infiltrating basal cell tumor, squamous cell epithelioma and basal squamous cell epithelioma), pre-epithelial tumor Keratosis vulgaris, seborrheic keratosis, actinic keratosis and ray keratosis,...

Claims

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Application Information

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IPC IPC(8): C07D493/04
Inventor 不公告发明人
Owner NANJING ZHENGLIANG MEDICAL TECH
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