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Method for separating and purifying amentoflavone

A technology for the separation and purification of biflavonoids from A. spicosa, which is applied in the field of separation and purification of abiflavones from A. spica, which can solve the problems of cumbersome separation steps, easy loss of samples, irreversible adsorption, etc., and achieve large separation volume, no loss of samples, and good repeatability Effect

Inactive Publication Date: 2011-11-02
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above methods are summed up and mainly adopt column chromatography, including silica gel column, macroporous adsorption resin column, and gel column. These column chromatography uses solid packing, which is prone to irreversible adsorption, easy loss of samples, slow speed, and cumbersome separation steps.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] (1) Preparation of Selaginella crude extract:

[0012] Take 1 kg of Selaginella and pulverize it into coarse powder, place it in a 15L extraction tank, reflux extract with 10L of 70% ethanol for 3 times, each time for 1h, combine the extracts, concentrate to a paste, and obtain the crude extract of Selaginella.

[0013] (2) separation and purification:

[0014] Put petroleum ether, ethyl acetate, acetone and water with a volume ratio of 1:5:6:1 in a separatory funnel, shake evenly to make the two phases reach equilibrium, separate after standing for stratification, and the upper phase is fixed. phase, the lower phase is the mobile phase, and after it is ultrasonically degassed for 30 minutes, it is cooled for subsequent use; the crude extract of Selaginella 100mg is dissolved in the solvent (each 10ml) of the upper phase and the lower phase of an equal volume, and filtered to obtain Sample solution; adopt the preparative TBE-1000A high-speed countercurrent chromatograp...

Embodiment 2

[0016] (1) Preparation of Selaginella crude extract:

[0017] Take 1 kg of Selaginella and crush it into coarse powder, place it in a 15L extraction tank, extract twice with 9L of 80% acetone under reflux, each time for 1 hour, combine the extracts, concentrate to a paste, and obtain the crude extract of Selaginella.

[0018] (2) separation and purification:

[0019] Put petroleum ether, ethyl acetate, acetone and water with a volume ratio of 3:4:6:3 in a separatory funnel, shake evenly to make the two phases reach equilibrium, separate after standing and layering, and the upper phase is fixed. phase, the lower phase is the mobile phase, and after it is ultrasonically degassed for 30 minutes, it is cooled for subsequent use; the crude extract of Selaginella 100mg is dissolved in the solvent (each 10ml) of the upper phase and the lower phase of an equal volume, and filtered to obtain Sample solution; adopt the preparative TBE-1000A high-speed countercurrent chromatograph, fill...

Embodiment 3

[0021] (1) Preparation of Selaginella crude extract:

[0022] Take 1kg of Selaginella and grind it into coarse powder, put it in a 15L extraction tank, extract twice with 12L of 75% ethanol under reflux, each time for 1h, combine the extracts, concentrate to a paste, and obtain the crude extract of Selaginella.

[0023] (2) separation and purification:

[0024] Put petroleum ether, ethyl acetate, acetone and water with a volume ratio of 0.5:4:5:2 in a separatory funnel, shake evenly to make the two phases reach equilibrium, separate after standing for stratification, and the upper phase is fixed. phase, the lower phase is the mobile phase, and after it is ultrasonically degassed for 30 minutes, it is cooled for subsequent use; the crude extract of Selaginella 100mg is dissolved in the solvent (each 10ml) of the upper phase and the lower phase of an equal volume, and filtered to obtain Sample solution; adopt the preparative TBE-1000A high-speed countercurrent chromatograph, fi...

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PUM

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Abstract

The invention belongs to the field of traditional Chinese medicine pharmacy, and relates to a method for separating and purifying amentoflavone, in particular, a method for enriching and purifying the amentoflavone through a high speed countercurrent chromatography method. The method is characterized in that: two mutually-immiscible solvent systems are utilized to perform the separation and purification in a mode of high-speed planetary motion in a support pipe; the method is applicable for the countercurrent chromatographies with various types to separate the amentoflavone, and has advantages of no irreversible adsorption, no loss of sample, no pollution, high efficiency and speed, high recovery rate, mild separating environment, high product purity and large quantity separation, and is applicable for industrial production.

Description

Technical field: [0001] The invention relates to a method for isolating and purifying the amiflavonoids from Selaginella chinensis, in particular to a method for separating and purifying the amiflavones from Selaginella chinensis by high-speed countercurrent chromatography. Background technique: [0002] Biflavone is a biflavonoid compound isolated from Selaginella tamariscina (Beauv.) Spring or Selaginella pulvinata (Hook.et Grev.) Maxim. Selaginella is mainly distributed in Guangdong, Guangxi, Fujian, Taiwan, Zhejiang, Jiangsu, Jiangxi, Hunan and other places in China. The biflavonoids of Suicha chinensis have physiological activities such as anti-tumor, anti-inflammatory, anti-bacterial, and vasodilation, and are the characteristic components of Selaginella medicinal materials. Wei Lina established a two-step precipitation process for the preliminary purification of the extract, and used preparative high-performance liquid chromatography, silica gel column chromatography...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/40
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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