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Method for preparing shionone by utilizing high-speed countercurrent chromatography

A high-speed countercurrent chromatography, asterone technology, applied in steroids, organic chemistry and other directions, can solve the problems of complex process operation, high production cost, poor specificity, etc., to achieve large separation, no sample loss, fast separation speed. Effect

Inactive Publication Date: 2011-11-23
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of preparing high-purity shionone, the technical defect is complex operation and poor specificity. At the same time, silica gel column is used for separation, and a large amount of silica gel waste is generated, which pollutes the environment and has high production costs.

Method used

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  • Method for preparing shionone by utilizing high-speed countercurrent chromatography

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Experimental program
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Effect test

Embodiment 1

[0016] Take the aster medicinal material and crush it, weigh 1kg, add 10L80% methanol to reflux for extraction for 2 hours, extract twice, add 200g of medicinal activated carbon to the combined extract for decolorization, filter out the activated carbon while it is hot, concentrate to an alcohol concentration of 50%, and place it for crystallization for 8 hours. 16 g of crude crystals were obtained by filtration. Take n-hexane, ethyl acetate, methanol, and water, and mix them in a ratio of 5:4:3:3. After standing still and stratifying, take the lower phase and fill it into the high-speed countercurrent chromatography column tube, turn the host at 700rpm, and pump it into the upper phase. , after equilibrium, adjust the flow rate to 3ml / min, and at the same time take the upper phase to dissolve the crude crystals, inject the sample through the injection valve, detect with the ELSD detector, collect the target components according to the spectrum, place the concentrated fraction ...

Embodiment 2

[0018] Take the aster medicinal material and crush it, weigh 1kg, add 8L of 90% methanol to reflux for extraction for 2 hours, extract twice, add 300g of medicinal activated carbon to the combined extract for decolorization, filter out the activated carbon while it is hot, concentrate to an alcohol concentration of 70%, and place it for crystallization for 12 hours. 12 g of crude crystals were obtained by filtration. Take n-hexane, ethyl acetate, methanol, and water, and mix them in a ratio of 3:4:2:3. After standing still and stratifying, take the lower phase and fill it into the high-speed countercurrent chromatography column tube, turn the main engine at a speed of 1000rpm, and pump it into the upper phase. , after equilibrium, adjust the flow rate to 1ml / min, and at the same time take the upper phase to dissolve the crude crystals, inject the sample through the injection valve, detect with the ELSD detector, collect the target components according to the spectrum, place the...

Embodiment 3

[0020] Take the aster medicinal material and crush it, weigh 1kg, add 6L of 90% methanol to reflux for extraction for 1 hour, extract 3 times, add 200g of medicinal activated carbon to the combined extract for decolorization, filter out the activated carbon while it is hot, concentrate to an alcohol concentration of 60%, and place it for crystallization for 16 hours. 13 g of crude crystals were obtained by filtration. Take n-hexane, ethyl acetate, methanol, and water, and mix them in a ratio of 5:5:2:4. After standing for stratification, take the lower phase and fill it into the high-speed countercurrent chromatography column tube, turn the host at a speed of 900rpm, and pump it into the upper phase. , after equilibrium, adjust the flow rate to 3ml / min, and at the same time take the upper phase to dissolve the crude crystals, inject the sample through the injection valve, detect with the ELSD detector, collect the target components according to the spectrum, place the concentra...

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Abstract

The invention discloses a method for preparing shionone by utilizing a high-speed countercurrent chromatography. The method provided by the invention comprises the following steps of: a, crushing Tatarian aster root as a medicinal material and reflowing and extracting by utilizing methanol with the concentration of 80-90%; adding active carbon into an extracted solution to de-color and filtering when the solution is hot; concentrating the solution until the concentration of the alcohol is 50-70%; standing and crystallizing to obtain a rough crystal; b, separating the crystal by utilizing the high-speed countercurrent chromatography; collecting target components according to an ELSD (Evaporative Light Scattering Detector) detector map; and decompressing, concentrating, crystallizing and then drying to obtain a product. The method provided by the invention has the advantages of simplicity for technological operation, short preparation period and high yield; and the method can be used for obtaining the shionone product with the content of more than 98% and is suitable for the industrial production.

Description

Technical field: [0001] The invention relates to a method for preparing shionone from aster, in particular to a method for preparing shionone by high-speed countercurrent chromatography. Background technique: [0002] Shinonen chemical name 2-shinonen-3-one, molecular formula C 30 h 50 O, molecular weight 426.7, molecular structure: [0003] [0004] Shivanone is a colorless crystal, soluble in petroleum ether, benzene, ether, chloroform and other organic solvents, but insoluble in water. The acetic anhydride-concentrated sulfuric acid reaction is positive, and the trichloroacetic acid reaction is positive, with a melting point of 161-162°C. [0005] Aster is the root and rhizome of Aster tataricus L.f. It is warm in nature, bitter and pungent in taste, moistens the lungs and lowers qi, and has the effect of eliminating phlegm and relieving cough. It is often used to treat symptoms of excessive phlegm, wheezing and coughing, persistent cough, and hemoptysis due to ove...

Claims

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Application Information

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IPC IPC(8): C07J63/00
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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