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Process for preparing high-purity gentiopicrin

A high-purity technology of gentiopicroside, which is applied in the field of preparation of high-purity gentiopicroside, can solve the problems of easy sample loss, easy pollution, cumbersome separation steps, etc., and achieve the effect of low cost and no loss of samples

Inactive Publication Date: 2007-11-14
赵景辉
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The previously reported extraction and separation of gentiopicroside mainly uses column chromatography, which requires the use of solid fillers, which is prone to irreversible adsorption, and has the disadvantages of easy sample loss, easy contamination, low efficiency, slow speed, and cumbersome separation steps.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] An analytical high-speed countercurrent chromatograph is used, and the solvent is selected from a n-hexane-methanol-water system. Firstly, the above solvent system was placed in a separatory funnel at a volume ratio of 4:5:3:5, shaken evenly and then separated into layers. After equilibrating for a period of time, separate the upper and lower phases, the upper phase is the stationary phase, and the lower phase is the mobile phase. Take an appropriate amount of gentian crude extract and dissolve it in 2ml of the lower phase for later use. The CCC-3000 high-speed countercurrent chromatograph made in the United States is used for separation. The stationary phase is filled with the chromatographic separation column, and the speed controller is turned on. When the predetermined speed is reached, the mobile phase is pumped in at a certain flow rate. When the mobile phase flows out, through The six-port injection valve injects samples. Elute from the head end to the tail end...

Embodiment 2

[0010] A semi-preparative high-speed countercurrent chromatograph is used, and the solvent is selected from the n-hexane-methanol-water system. Firstly, the above solvent system was placed in a separatory funnel at a volume ratio of 7:3:1:3, shaken evenly and then separated into layers. After equilibrating for a period of time, separate the upper and lower phases, the upper phase is the stationary phase, and the lower phase is the mobile phase. Take an appropriate amount of gentian crude extract and dissolve it in 10ml of the lower phase for later use. Use the CCC-1000 high-speed countercurrent chromatograph made in the United States for separation, fill the chromatographic separation column with the stationary phase, turn on the speed controller, and start pumping the mobile phase at a certain flow rate when the predetermined speed is reached. The six-port injection valve injects samples. Elute from the head end to the tail end, the main engine rotates forward, the speed is...

Embodiment 3

[0012] An analytical high-speed countercurrent chromatograph is used, and the solvent is selected from a n-hexane-methanol-water system. Firstly, the above solvent system was placed in a separatory funnel at a volume ratio of 4:3:1:3, shaken evenly and then separated into layers. After equilibrating for a period of time, separate the upper and lower phases, the upper phase is the stationary phase, and the lower phase is the mobile phase. Take an appropriate amount of gentian crude extract and dissolve it in 2ml of the lower phase for later use. The CCC-3000 high-speed countercurrent chromatograph made in the United States is used for separation. The stationary phase is filled with the chromatographic separation column, and the speed controller is turned on. When the predetermined speed is reached, the mobile phase is pumped in at a certain flow rate. When the mobile phase flows out, through The six-port injection valve injects samples. Elute from the head end to the tail end...

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PUM

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Abstract

This invention relates to a method of preparing high-purity gentiopicrin. The invention adopts small scale preparation by analysis mode high speed counter-current chromatography, and large-scale preparation by semipreparing type high speed counter-current chromatography; volume ratio of chloroform, methanol, normal butyl alcohol and water is 4-8:3-6:1-4:3-6; one time separation to gain gentiopicrin. No need solid filling and without irreversible adsorption. The acquired gentiopicrin purity reach 92%upwards, lend itself to prepare gentiopicrin from different kinds of rough gentian crude extract.

Description

Technical field: [0001] The invention relates to a method for preparing high-purity gentiopicroside, which is a method for preparing high-purity gentiopicroside from gentian crude extract by using a high-speed countercurrent chromatography (HSCCC) method. Background technique: [0002] Gentian is the dry root and rhizome of Gentiana manshurica Kitag., Gentiana scabra Bge., Gentiana triflora pall. or Gentiana rigescens Franch. of Gentianaceae. The main active ingredient of the medicinal part is gentiopicroside, which belongs to the iridoid glycoside compound, and has the effects of clearing the liver and detoxifying, digesting food and invigorating the stomach. Gentiopicroside has been used as a quantitative chemical indicator for the content determination of Gentiana HPLC by the Chinese Pharmacopoeia 2005 edition. At the same time, it is also a symbolic component of the fingerprints of gentian and its products. Therefore, high-purity gentiopicroside is widely used and in g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08
Inventor 王艳艳王英平赵景辉刘继永焉石
Owner 赵景辉
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