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Process for preparing high-purity deoxyschizandrin

A high-purity Schizandrin A technology, applied in organic chemistry methods, chemical instruments and methods, purification/separation/stabilization of organic compounds, etc., can solve the problems of sample loss, contamination, and low efficiency, and achieve low Cost, no sample loss 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 schisandrin A 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

[0009] 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 5:6:4, 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. Elute from the head e...

Embodiment 2

[0011] 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 3:5:7, 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 engine rotates for...

Embodiment 3

[0013] 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 2:3:4, shaken 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. Elute from the head end to t...

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PUM

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Abstract

This invention relates to a preparation method of high-purity deoxyschizandrin. The process as follows: the solvent system includes normal hexane, methanol and water; the volume ratio of normal hexane, methanol and water is 2 - 6: 3 - 7: 4 - 8; firstly dissolve deoxyschizandrin crude extract perpared by traditional craft in 2ml - 10ml bottom phase; adopt 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 invention does not need solid padding, has no irreversible adsorption and no pollution. The purity of gained deoxyschizandrin can reach 94%upwards.

Description

Technical field: [0001] The invention relates to a method for preparing high-purity schisandrin, which is a method for preparing high-purity schisandrin from the crude extract of schisandra fruit by applying a high-speed countercurrent chromatography (HSCCC) method. 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 A is the main active ingredient...

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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