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Process for preparing high-purity deoxyschizandrin

A high-purity Schizandrin B technology, applied in organic chemistry methods, chemical instruments and methods, purification/separation/stabilization of organic compounds, etc., can solve the problems of easy loss, slow speed, and easy contamination of samples, and achieve sample No loss, low cost effect

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 schisandra B is mainly based on column chromatography, which requires the use of solid fillers, which is prone to irreversible adsorption, and has the disadvantages of easy sample loss, easy pollution, low efficiency, slow speed, and cumbersome separation steps.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] An analytical high-speed countercurrent chromatograph is used, and the solvent is selected from the n-hexane-methanol-water-acetonitrile system. Firstly, the above solvent system was placed in a separatory funnel at a volume ratio of 6:3:3:1, 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 the crude extract of Schisandra chinensis 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. Elut...

Embodiment 2

[0011] A semi-preparative high-speed countercurrent chromatograph is used, and the solvent is selected from the n-hexane-methanol-water-acetonitrile system. Firstly, the above solvent system was placed in a separatory funnel at a volume ratio of 9:4:3:2, 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 the crude extract of Schisandra chinensis 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 eng...

Embodiment 3

[0013] An analytical high-speed countercurrent chromatograph is used, and the solvent is selected from the n-hexane-methanol-water-acetonitrile system. Firstly, the above solvent system was placed in a separatory funnel at a volume ratio of 5:3:2:1, 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 the crude extract of Schisandra chinensis and dissolve it in 2ml of the lower phase for later use. Use the CCC-3000 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. When the mobile phase flows out, pass through The six-port injection valve injects samples. Elute from th...

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PUM

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Abstract

This invention relates to a method of preparing high-purity Schisandrin B. The invention adopts analysis mode high speed counter-current chromatography to proceed small scale preparation, adopt semipreparative type high speed counter-current chromatography to proceed large-scale preparation. The feature is that in solvent system the volume ratio of normal hexane, methanol, water and acetonitrile is 5 - 11 : 3 - 6 : 2 - 5 : 1, and the best volume ratio is 10:5:4:3. The invention does not need solid padding, has no irreversible adsorption and no pollution.The purity of gained Schisandrin B can reach 98%upwards.

Description

Technical field: [0001] The invention relates to a method for preparing high-purity schisandrin, which uses a high-speed countercurrent chromatography (HSCCC) method to prepare high-purity schisandrin from the crude extract of schisandra fruit. Background technique: [0002] Schisandra chinensis (Turcz.) Baill] is a perennial woody vine of Magnoliaceae. The fruit is used as medicine, and the roots and stems can also be used as medicine. It has the functions of astringing the lungs, nourishing the kidneys, stopping sweating, promoting body fluid, stopping diarrhea, and astringent essence. Indications for cough and asthma, body fluid deficiency and thirst, spontaneous sweating, nocturnal emission, chronic diarrhea, neurasthenia. Modern studies have proved that it also has the functions of regulating blood pressure, protecting the liver and "adaptogen". It is an authentic northern precious medicinal material. Schisandrin B is the main active ingredient of Schisandra chinens...

Claims

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Application Information

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IPC IPC(8): C07D317/70C07B63/00
Inventor 刘继永王英平赵景辉焉石
Owner 赵景辉
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