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Method for separating preparing tripterygium wilfordii monomer from tripterygium wilfordii by countercurrent flow chromatography

A tripterygium wilfordii alkaloid and countercurrent chromatography technology are applied in the field of separation and preparation of tripterygium wilfordii alkaloid monomers from tripterygium wilfordii by countercurrent chromatography, which can solve the problems of low recovery rate and low purity, and achieve simple operation, easy purchase and high efficiency. high effect

Inactive Publication Date: 2007-02-14
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing literature reports adopt the method separation of column chromatography, but the purity is not high, and the recovery rate is very low

Method used

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  • Method for separating preparing tripterygium wilfordii monomer from tripterygium wilfordii by countercurrent flow chromatography
  • Method for separating preparing tripterygium wilfordii monomer from tripterygium wilfordii by countercurrent flow chromatography
  • Method for separating preparing tripterygium wilfordii monomer from tripterygium wilfordii by countercurrent flow chromatography

Examples

Experimental program
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Effect test

Embodiment 1

[0020] 1. 10kg of Tripterygium wilfordii root bark was percolated with 30L 60% ethanol for 10 hours, the leachate was collected, concentrated under reduced pressure to obtain ethanol extract, the ethanol extract was extracted 3 times with chloroform, and the chloroform extract obtained after concentration under reduced pressure was extracted with 4% hydrochloric acid 6 times, the filtrate was collected after filtration, the filtrate was adjusted to a pH value between 8-11 with sodium hydroxide, and a solid was precipitated. After filtration, the solid was washed 3 times with deionized water, and 30 g of crude total alkaloids were obtained after the solid was dried.

[0021] 2. The crude total alkaloids were fully dissolved with 200 mL of methanol, the filter residue was collected by filtration, and the filter residue was crystallized by heating with methanol to obtain 10 g of pure total alkaloids.

[0022] 3. Separate the pure total alkaloids with a high-speed countercurrent ch...

Embodiment 2

[0026]1. 10kg of tripterygium twig root bark was percolated with 30L 70% ethanol for 10 hours, the leachate was collected, concentrated under reduced pressure to obtain ethanol extract, the ethanol extract was extracted 3 times with chloroform, and the chloroform extract obtained after concentration under reduced pressure was extracted with 20% sulfuric acid 6 times, the filtrate was collected after filtration, and the pH value of the filtrate was adjusted between 8-11 with sodium bicarbonate, and a solid was precipitated. After filtration, the solid was washed 6 times with deionized water, and 32 g of crude total alkaloids were obtained after the solid was dried.

[0027] 2. The crude total alkaloids were fully dissolved with 250 mL of methanol, the filter residue was collected by filtration, and the filter residue was crystallized by heating with methanol to obtain 12 g of pure total alkaloids.

[0028] 3. Separate the pure total alkaloids with a high-speed countercurrent chr...

Embodiment 3

[0032] 1. 10kg of tripterygium twig root bark was percolated with 30L 80% ethanol for 10 hours, the leachate was collected, concentrated under reduced pressure to obtain ethanol extract, the ethanol extract was extracted 3 times with chloroform, and the chloroform extract obtained after concentration under reduced pressure was extracted with 20% acetic acid 6 times, the filtrate was collected after filtration, the filtrate was adjusted to a pH value between 8-11 with sodium carbonate, and a solid was precipitated. After filtration, the solid was washed 6 times with deionized water, and 35 g of crude total alkaloids were obtained after the solid was dried.

[0033] 2. The crude total alkaloids were fully dissolved with 250 mL of methanol, the filter residue was collected by filtration, and the filter residue was crystallized by heating with methanol to obtain 14 g of pure total alkaloids.

[0034] 3. Separate the pure total alkaloids with a high-speed countercurrent chromatograp...

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Abstract

The countercurrent chromatographic process for separating and preparing tripterygium alkaloid monomer from tripterygium material includes the following steps: 1. extracting crude total tripterygium alkaloid, mixing crude total tripterygium alkaloid with methanol, filtering to obtain filter residue and drying, and re-crystallizing in methanol to obtain total tripterygium alkaloid; 2. compounding the fixed phase and the flowing phase of two-phase solvent system; 3. filling the column of countercurrent chromatograph with the fixed phase; 4.pumping the flowing phase into the column of the high speed countercurrent chromatograph; and 5. feeding the total tripterygium alkaloid and collecting different tripterygium alkaloid monomers based on the detector spectral graph. The present invention can obtain different tripterygium alkaloid monomers in purity over 95 %.

Description

technical field [0001] The invention relates to a method for separating and preparing tripterygium wilfordii alkaloid monomer from tripterygium wilfordii by countercurrent chromatography. Background technique [0002] Tripterygium wilfordii Hook.f. (Celastraceae, TWHF) is a traditional Chinese medicine in China, mainly distributed in South China, and has the effects of treating immune diseases, anti-inflammation, and anti-fertility (C.N.Liu, M.Peng, Anticancer Chinese Herb Dictionary, Science and Technology Publishing Co., Hubei, 1994, p.1072). The main active ingredients in Tripterygium wilfordii are tripterygium alkaloids, diterpenes and triterpenoids (Qian Shao Zhen, Xu Ye, Zhangjian Wei. Recent progress in research Tripterygium: A male antiferility plant, Contraception, 1995, 51: 121-129 ). Tripterygium wilforine, tripterygium wilforine, tripterygium wilfortine, tripterygium wilfortine were first isolated from tripterygium wilfordii root (Beroza M.Alkaloids from Tripte...

Claims

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Application Information

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IPC IPC(8): C07D491/22
Inventor 欧阳小琨何潮洪
Owner ZHEJIANG UNIV
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