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New method for purifying schisandrin

A technology of schisandra alcohol A and schisandra chinensis, applied in ether separation/purification, organic chemistry, ether preparation, etc., can solve the problems of cost reduction, low purity, long time, etc., and achieve the effect of cost reduction, high purity and simple method

Active Publication Date: 2012-10-17
DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The regeneration of macroporous resin is convenient and rapid, suitable for large-scale production, and the cost is greatly reduced. Most of the pigments and impurities are removed by water elution; The effect is good, and recrystallization is adopted in the later stage, so the product obtained by the present invention has high purity, significantly increases the content of active ingredients, and overcomes the shortcomings of conventional extraction methods such as low purity and long time

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1: a method utilizing microwave countercurrent extraction, macroporous adsorption resin adsorption, and column chromatography to purify Schizandrin A in Schisandra chinensis,

[0022] The steps are as follows:

[0023] (1) Take 500g Schisandra chinensis and crush it to 40 mesh, add 60% ethanol solution, extract microwave countercurrent under 400W, time 10min, 8 times of material-liquid ratio, forward feed, reverse water feed, the flow of material and water is Reverse continuous dynamic flow. The extract is layered with petroleum ether to remove fatty oil;

[0024] (2) reclaim ethanol, the macroporous resin adsorption on the gained solution, model is DA201 resin, and the aspect ratio of resin column is 8: 1;

[0025] (3) Under normal temperature and pressure, with a flow rate of 1BV / h, first elute with distilled water, and the elution volume is 3BV;

[0026] (4) Then use 40%, 50%, 60%, 70%, 85%, 95% ethanol solution for elution at a flow rate of 1BV / h and a...

Embodiment example 2

[0031] (1) Take 500g Schisandra chinensis and crush it to 50 mesh, add 70% ethanol solution, extract microwave countercurrent under the condition of 500W, time 20min, 10 times material-liquid ratio, forward feed, reverse water, the flow of material and water is Reverse continuous dynamic flow. The extract is layered with petroleum ether to remove fatty oil;

[0032] (2) reclaim ethanol, absorb the macroporous resin on the gained solution, the model is D101 resin, and the height-to-diameter ratio of the resin column is 10: 1;

[0033] (3) Under normal temperature and pressure, with a flow rate of 1BV / h, first elute with distilled water, and the elution volume is 4BV;

[0034] (4) Then use 40%, 50%, 60%, 70%, 85%, 95% ethanol solution for elution at a flow rate of 2BV / h and an elution volume of 7BV. The eluent was tracked and monitored by thin-layer chromatography (with schisandrin A as the reference substance);

[0035] (5) Collect ethanol eluate and concentrate, recover eth...

Embodiment example 3

[0039] (1) Get 500g schisandra chinensis and crush it to 60 mesh, add 75% ethanol solution, extract microwave countercurrent under 500W, time 30min, 12 times of material-liquid ratio conditions, forward feed, reverse water, the flow of material and water is Reverse continuous dynamic flow. The extract is layered with petroleum ether to remove fatty oil;

[0040] (2) reclaim ethanol, the macroporous resin adsorption on the gained solution, model is AB-8 resin, and the aspect ratio of resin column is 10: 1;

[0041] (3) Under normal temperature and pressure, with a flow rate of 1BV / h, first elute with distilled water, and the elution volume is 4BV;

[0042] (4) Then use 40%, 50%, 60%, 70%, 85%, 95% ethanol solution for elution at a flow rate of 2BV / h and an elution volume of 7BV. The eluent was tracked and monitored by thin-layer chromatography (with schisandrin A as the reference substance);

[0043] (5) Collect ethanol eluate and concentrate, recover ethanol, and dry under ...

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PUM

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Abstract

The invention belongs to the field of natural organic chemistry, and relates to a purifying method for schisandrin, and particularly to a method for purifying schisandrin in schisandra chinensis by using microwave countercurrent extraction, macroporous resin adsorption, and column chromatography purification. The method has the following advantages that: 1, the microwave extraction is adopted, and ethanol is adopted as a solvent to remove part of fatty oil so as to greatly reduce the extraction time, and improve production efficiency, in addition, the method is simple; 2, the macroporous resin can be conveniently and rapidly regenerated, and is suitable for large-scale production, water elution can remove most of pigments and impurities, and the macroporous resin is easy to operate; 3, the macroporous resin and the silica gel column chromatography are combined so as to provide a good separation and purification effect, at the late stage, recrystallization is adopted so as to greatly improve the product purity. With the present invention, the microwave countercurrent extraction, the macroporous resin separation and purification and the column chromatography are adopted to carry out further purification, such that the product purity is greatly improved, and the semi-finished product schisandrin with the content more than 65% and the final product schisandrin with the content more than 98% are obtained.

Description

Technical field: [0001] The invention belongs to the field of natural organic chemistry, and relates to a method for purifying schisandrin A, in particular to a method for purifying schisandrin A in schisandra chinensis by using microwave countercurrent extraction, macroporous adsorption resin adsorption and column chromatography. Background technique: [0002] Schisandra chinensis, commonly known as mountain pepper, weight dumpling, medicine schisandra, noodle vine, Wumeizi, etc., Tang et al. "Xinxiu Materia Medica" contains "five flavors are sweet and sour in the flesh, hard in the core, and have a salty taste", so it has the name of schisandra. According to medical books, it is called Chuzhu, Xuanji, and Huiji, which were first listed in the top grade of Shennong’s Herbal Classic. The efficacy of traditional Chinese medicine lies in the power of nourishing and strengthening, and its medicinal value is extremely high. The present invention adopts the dry mature fruit comm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/23C07C41/36
Inventor 姚德坤姚德利张亚红万莉
Owner DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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