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Improved process for preparing podophyllotoxin from Chinese podophyllum root

A technology for podophyllotoxin and podophyllotoxin, which is applied in the field of improved technology for preparing podophyllotoxin, can solve problems such as large consumption of eluent, low product purity, complicated operation, etc., and achieves less solvent consumption, wide industrial application, and operation handy effect

Inactive Publication Date: 2005-03-02
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional chemical extraction method has the advantages of simple operation and large yield, but the toxic solvent—benzene is needed in the extraction and purification process, and the product purity is low; although the traditional column chromatography can obtain high-purity products, the operation is cumbersome , and the yield is low, and a large amount of eluent is consumed

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 1kg of the rhizome of Taoerqi, crush it, add 7kg of 90% ethanol solution, extract under reflux for 3 times, combine the extracts, concentrate under reduced pressure to obtain about 316g of brownish red slurry.

[0020] Weigh 100g of the brownish-red slurry, add 500g of petroleum ether, shake vigorously, extract, let stand to separate layers, discard the lower layer of brownish-red liquid, put the upper layer of light yellow liquid into a 1000mL beaker, and leave it at room temperature for about 12 hours. 2.9 g of white to light yellow crystals were precipitated. As determined by HPLC, the purity of podophyllotoxin is 78.6%.

[0021] Take a certain amount of silica gel for column chromatography (with a particle size of 200-300 mesh), put it into a glass column with an inner diameter of 5 cm, and the height of the silica gel column is 15 cm (the diameter-to-height ratio of the chromatography column is 1:5), so that the bed volume For 300mL, a tee is connected to th...

Embodiment 2

[0023] Weigh 1kg of the rhizome of Taoerqi, crush it, add 10kg of 95% ethanol solution, extract under reflux for 3 times, combine the extracts, concentrate under reduced pressure, and obtain about 396g of brownish-red slurry.

[0024] Weigh 100g of brownish-red slurry, add 800g of petroleum ether, shake vigorously, extract, let stand to separate layers, discard the lower layer of brownish-red liquid, put the upper layer of light yellow liquid into a 1000mL beaker, and let it stand at room temperature for 16 hours. 2.1 g of white to pale yellow crystals were precipitated. As determined by HPLC, the purity of podophyllotoxin is 75.3%.

[0025] Take a certain amount of silica gel (200-300 meshes) for column chromatography, put it into a glass column with an inner diameter of 3 cm, the height of the silica gel column is 15 cm, and the ratio of diameter to height of the chromatography column is (1:5), so that the The volume is 100mL, a tee is connected at the lower end of the glas...

Embodiment 3

[0027] Weigh 1kg of the rhizome of Taoerqi, crush it, add 4kg of 50% ethanol solution, heat reflux extraction 3 times, combine the extracts, concentrate under reduced pressure to obtain about 286g of brownish red slurry.

[0028] Weigh 100g of brownish-red slurry, add 400g of petroleum ether, shake vigorously, extract, let stand to separate layers, discard the lower layer of brownish-red liquid, put the upper layer of light yellow liquid into a 1000mL beaker, and let it stand at room temperature for about 6 hours. 3.4 g of white to light yellow crystals were precipitated. As determined by HPLC, the purity of podophyllotoxin is 71.6%.

[0029] Take a certain amount of silica gel for column chromatography (with a particle size of 200-300 mesh), put it into a glass column with an inner diameter of 10 cm, and the height of the silica gel column is 70 cm (the diameter-to-height ratio of the chromatography column is 1:7), so that the bed volume For 5500mL, a tee is connected at the...

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Abstract

The present invention relates to the extraction and purification technology of podophyllotoxin via solvent crystallization process and compression chromatographic process. The present invention has simple operation, is easy to use in industrial production to obtain podophyllotoxin with purity not lower than 97 %. Podophyllotoxin may be extracted directly from Chinese podophyllum root or may be obtained from refining the extract of Chinese podophyllum root.

Description

technical field [0001] The present invention relates to a kind of preparation method of intermediate, more specifically relate to an improved process for preparing podophyllotoxin from P. chinensis. Background technique [0002] Taoerqi (Podophyllum emodi Wall.var.chinense Sprague), also known as Podophyllum emodi Wall.var.chinense Sprague, is a plant of Berberidaceae. It grows in damp places under forests in mountains and is distributed in Sichuan, Shaanxi, Gansu, Qinghai, In Yunnan, Tibet and other places, the underground part or fruit is used as medicine. It is warm in nature and bitter in taste, and has the effects of harmonizing blood, stopping bleeding, eliminating rheumatism, detoxifying, and reducing swelling. [0003] Podophyllotoxin (podophyllotoxin) can be extracted from the rhizome of peach seven. For a long time, the research on podophyllotoxin has mainly focused on its pharmacological effects in cancer treatment, and its anticancer me...

Claims

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Application Information

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IPC IPC(8): C07D493/04
Inventor 卢艳花魏东芝袁永红
Owner EAST CHINA UNIV OF SCI & TECH
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