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Separation method of solanesol-containing eluate

A separation method and a solanesol-containing technology are applied in the field of separation of solanesol-containing eluents, and can solve the problems of low purity of solanesol and the like

Pending Publication Date: 2020-06-05
CHANGDE ZHENGYANG BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a method for separating the eluent containing solanesol, aiming to solve the problem of low purity of the solanesol separated by the existing separation method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The embodiment of the present invention provides a method for separating the eluent containing solanesol, comprising the following steps:

[0027] S1: Concentrate the eluate containing solanesol in vacuum at low temperature at a pressure of 0.085Mpa and a temperature of 50°C to obtain a mixed liquid a with a solanesol content of 70%;

[0028] S2: Pump the mixed liquid a into the first silica gel chromatographic column and the second silica gel chromatographic column connected in series, and absorb the mixed liquid a through the silica gel particles in the first silica gel chromatographic column and the second silica gel chromatographic column, and the first silica gel chromatographic column 200-mesh silica gel particles are installed in the middle column, and 400-mesh silica gel particles are installed in the second silica gel chromatography column;

[0029] S3: pumping an eluent b composed of 99% petroleum ether and 1% ethyl acetate into the first silica gel chromatogr...

Embodiment 2

[0036] The embodiment of the present invention provides a method for separating the eluent containing solanesol, comprising the following steps:

[0037] S1: Concentrate the eluate containing solanesol in vacuum at low temperature at a pressure of 0.09Mpa and a temperature of 55°C to obtain a mixed liquid a with a solanesol content of 60%;

[0038] S2: Pump the mixed liquid a into the first silica gel chromatographic column and the second silica gel chromatographic column connected in series, and absorb the mixed liquid a through the silica gel particles in the first silica gel chromatographic column and the second silica gel chromatographic column, and the first silica gel chromatographic column 100-mesh silica gel particles are installed in the second column, and 300-mesh silica gel particles are installed in the second silica gel chromatography column;

[0039] S3: pumping an eluent b composed of 98% petroleum ether and 2% ethyl acetate into the first silica gel chromatogra...

Embodiment 3

[0046] The embodiment of the present invention provides a method for separating the eluent containing solanesol, comprising the following steps:

[0047] S1: Concentrate the eluate containing solanesol in vacuum at low temperature at a pressure of 0.085Mpa and a temperature of 50°C to obtain a mixed liquid a with a solanesol content of 60%;

[0048] S2: Pump the mixed liquid a into the first silica gel chromatographic column and the second silica gel chromatographic column connected in series, and absorb the mixed liquid a through the silica gel particles in the first silica gel chromatographic column and the second silica gel chromatographic column, and the first silica gel chromatographic column 200-mesh silica gel particles are installed in the middle column, and 300-mesh silica gel particles are installed in the second silica gel chromatography column;

[0049] S3: pumping an eluent b composed of 97% petroleum ether and 3% ethyl acetate into the first silica gel chromatogr...

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PUM

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Abstract

The invention is applicable to the technical field of eluent separation, and provides a separation method of solanesol-containing eluate. Vacuum low-temperature concentration of the solanesol-containing eluate is adopted to remove part of a solvent, and the vacuum low-temperature concentration is faster in solvent removal speed and higher in efficiency compared with the traditional concentration methods; the adsorption efficiency and the subsequent elution effect can be improved by adsorbing a mixed liquid a through silica gel with different fineness; an eluent b prepared from petroleum etherand ethyl acetate according to a certain ratio is used for elution, so that the elution efficiency is relatively high; mixed solid d is dissolved with an acetone solution, and then solanesol is separated out through freezing crystallization, so that the separation effect is better, the separation efficiency is higher, and the purity of the separated solanesol is higher.

Description

technical field [0001] The invention belongs to the technical field of eluent separation, in particular to a method for separating eluent containing solanesol. Background technique [0002] Solanesol is an active ingredient of polyterpenoids contained in tobacco. It is an unsaturated polyprenyl alcohol. It has the function of lipid antioxidant and eliminating free radicals in antibodies. It is a pharmaceutical intermediate of traditional Chinese medicine and can be used for synthesis Vitamin K2, coenzyme Q10, anti-cancer and anti-AIDS drugs. At present, coenzyme Q10, which has been produced and widely used in many developed countries, must rely on high-purity solanesol as a raw material, and solanesol with a content of more than 90% will surely become an important export-earning pharmaceutical intermediate in my country. [0003] The process for extracting solanesol from tobacco mainly includes extracting tobacco leaves with an organic solvent to obtain an extract, concentr...

Claims

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Application Information

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IPC IPC(8): C07C29/78C07C29/76C07C33/02
CPCC07C29/78C07C29/76C07C33/02
Inventor 曾勇黄平易松山杨鸿波陈德亮陈孟军
Owner CHANGDE ZHENGYANG BIOTECH CO LTD