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Method for preparing high-purity podophyllotoxin from Chinese podophyllum root

A technology of podophyllotoxin and Taoerqi, which is applied in antiviral agents, organic chemistry, drug combination, etc., can solve the problems of low purity and unstable quality of podophyllotoxin, and achieve complete extraction, easy operation, and superior The effect of large sample volume

Inactive Publication Date: 2009-08-12
SHANGHAI JINHE BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] But the podophyllotoxin refined product purity that above-mentioned method obtains is slightly lower and less stable

Method used

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  • Method for preparing high-purity podophyllotoxin from Chinese podophyllum root

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 5 kg of ultra-finely ground rhizomes with a particle size of less than 10 μm were soaked in 30 L of methanol at 50 ° C, extracted 3 times with a power of 1000 W ultrasonic wave, 3 hours each time, combined and concentrated for 3 times to obtain 4.8 L of reddish-brown infusion with a specific gravity of 1.1. paste, transferred to the extraction tank and added 9.6L of water, shared 15L of dichloromethane for 3 extractions, combined the 3 dichloromethane phases, dried with anhydrous sodium sulfate, filtered, concentrated to dryness, and dried at 60°C to obtain 640g of dichloromethane Crude yellow podophyllotoxin powder. The light yellow podophyllotoxin crude powder is dissolved in 3L of dichloromethane, and the sample is wet loaded onto a 300-400 mesh silica gel high-pressure column. The column pressure of the high-pressure column is 2.5-3.5MPa, and the inner diameter of the high-pressure column is 100mm. The diameter-to-height ratio is 1:12, and it is eluted with a mixed ...

Embodiment 2

[0030] 50kg of ultra-finely ground rhizomes with a particle size of less than 10 μm were soaked in 300L of methanol at 50°C, extracted 3 times with a power of 5000W ultrasonic waves, each time for 3 hours, combined and concentrated for 3 times to obtain 48.6L of reddish-brown infusion with a specific gravity of 1.1. paste, transferred to the extraction tank and added 100L water, shared 150L dichloromethane for 3 extractions, combined 3 dichloromethane phases, dried and filtered with anhydrous sodium sulfate, concentrated to dryness, and dried at 60°C to obtain 6240g light yellow ghost Crude powder of aphyllotoxin. The light yellow podophyllotoxin crude powder is dissolved in 20L of dichloromethane, and the sample is wet loaded onto a 300-400 mesh silica gel high-pressure column. The column pressure of the high-pressure column is 2.5-3.5MPa, and the inner diameter of the high-pressure column is 200mm. The diameter-to-height ratio is 1:12.5, and it is eluted with a mixture of ac...

Embodiment 3

[0032] Soak 5kg of ultra-finely crushed rhizomes of Taoerqi with a particle size below 10 μm in 30L of ethanol at 60°C, extract 3 times with a power of 1000W ultrasonic waves, 3 hours each time, combine the extracts for 3 times and concentrate to obtain 4.82L of reddish-brown infusion with a specific gravity of 1.08. paste, transferred to the extraction tank and added 10L of water, shared 15L of dichloromethane for 3 extractions, combined the 3 dichloromethane phases, dried with anhydrous sodium sulfate, concentrated to dryness, and dried at 60°C to obtain 624g of light yellow ghost Crude powder of aphyllotoxin. The light yellow podophyllotoxin crude powder is dissolved in 3L of dichloromethane, and the sample is wet-loaded onto a 300-400 mesh silica gel high-pressure column, where the column pressure of the high-pressure column is 2.5-3.5MPa, and the inner diameter of the high-pressure column is 100mm. The ratio of layer diameter to height is 1:12, and it is eluted with a mix...

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Abstract

The invention provides a method for preparing high-purity podophyllotoxin from Chinese podophyllum root, consisting of two parts of: extraction of alcohols used for raw materials to obtain extractum and extraction of the extractum to obtain podophyllotoxin crude product, and high-pressure column chromatography of the podophyllotoxin crude product. The method comprises the following specific steps of: after superfine pulverizing rootstalks of the Chinese podophyllum root, heating and extracting the pulverized rootstalks by using alcoholic solvents under the ultrasonic condition for three times, merging extracting solutions in the three times, and concentrating the alcoholic solvents by the merged extracting solutions to obtain red brown extractum with the specific gravity of 1.0-1.2; then adding water with the volume of 1-2 times of that of the extractum to obtain alcohol-water phase of podophyllotoxin; extracting the alcohol-water phase of podophyllotoxin by using methylene dichloride with the volume equal to that of the alcohol-water phase of podophyllotoxin for three times, merging methylene dichloride phases in the three times, and concentrating to obtain yellowish podophyllotoxin crude product with the purity of 40% to 50%; and dissolving the yellowish podophyllotoxin crude product, loading sample to a high-pressure column with silica gel of 300-400 meshes, eluting by using mixed eluent of acetone + methylene dichloride solvent, collecting eluent of product sections, concentrating, filtering, and drying to obtain the podophyllotoxin fine product with the purity of more than 99%.

Description

technical field [0001] The invention relates to a method for extracting podophyllotoxin from plants, in particular to a method for preparing high-purity podophyllotoxin from Rhizoma chinensis. Background technique [0002] Podophyllotoxin, also known as podophyllotoxin, podophyllotoxin, podophyllotoxin, is a natural product with anti-tumor activity, belonging to cyclolignan lactones in lignans. Its chemical name is [5R-(5α, 5αβ, 8aα, 9α)], 5,8,8α, 9-tetrahydro-9-hydroxy-5-(3,4,5-trimethoxyphenyl)furan (3 ',4': 6,7) Naphtho-[2,3-d]-1,3-dioxole-6(5αH)-one. Molecular formula: C22H2208, molecular weight: 414.41, structural formula is general formula I: [0003] [0004] Podophyllotoxin can be used to treat genital warts and inhibit herpes virus. At the same time, since podophyllotoxin was confirmed to have a therapeutic effect on tumor cells in the 1950s, people have strengthened the research on podophyllotoxin and synthesized a large number of podophyllotoxin derivatives....

Claims

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Application Information

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IPC IPC(8): C07D493/04A61P31/22A61P35/00
Inventor 张伟中蔡志香仝泽彬王权勇张爱平高卅
Owner SHANGHAI JINHE BIO TECH
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