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A double-column circulation separation system and method for preparing tanshinone compounds

A separation system and compound technology, applied in the field of double-column circulation separation system, can solve the problems of high environmental hazards of solvents, low recovery rate, long separation process, etc., and achieve the effect of saving separation time, saving solvent and wide application range

Active Publication Date: 2015-12-30
ZHEJIANG UNIV
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  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to provide a double column for the preparation of tanshinone compounds that is simple in extraction and separation and can be operated continuously in view of the above-mentioned defects in the existing tanshinone separation and preparation process, such as long separation process, high environmental hazards of the solvent used, and low recovery rate. Circulation separation system and method thereof

Method used

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  • A double-column circulation separation system and method for preparing tanshinone compounds
  • A double-column circulation separation system and method for preparing tanshinone compounds
  • A double-column circulation separation system and method for preparing tanshinone compounds

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Embodiment 1

[0037] A method for preparing tanshinone compounds using a double-column circulation separation system, the tanshinone compounds comprising structural formula (1) dihydrotanshinone I, structural formula (2) trefoil B and structural formula (3) methyl tanshinone ester,

[0038]

[0039] Proceed as follows:

[0040] 1. Extraction and enrichment:

[0041] Take 9.5 kg of dry rhizome of Salvia miltiorrhiza, crush it into a 60-mesh coarse powder, place it in 30 L of ethanol with a volume concentration of 95% at room temperature and extract 3 times, each time for 24 hours, stir regularly, combine the extracts and concentrate under reduced pressure to obtain the crude extract of Salvia miltiorrhiza , take out 30g and mix the sample with normal phase silica gel, then elute with petroleum ether and ethyl acetate, collect the eluate rich in tanshinone compounds, concentrate and freeze-dry under reduced pressure, and obtain The crude product of B and methyl tanshinone ester (HPLC anal...

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Abstract

The invention relates to a double-column circulating separation system and method for preparing a high-purity tanshinone compound. The double-column circulating separation system comprises three counter-current chromatographic columns, three pumps, three detectors, three collectors and three six-way valves. A first counter-current chromatographic column serves as an initial separation column, a second counter-current chromatographic column and a third counter-current chromatographic column serve as mutually independent circulating separation columns, and the multidimensional circulating separation of the tanshinone compound can be realized by adjusting a second six-way valve and a third six-way valve. The tanshinone compound comprises dihydrotanshinone I, triiuganone B and methyl tanshinone ester. The system and method disclosed by the invention are simple in extraction and separation, short in time, high in product purity, capable of being continuously operated, and suitable for industrial production.

Description

technical field [0001] The invention relates to a double-column circulation separation system and a method for preparing tanshinone compounds. Background technique [0002] Counter-current chromatography (CCC) is a liquid-liquid partition chromatography that does not require solid supports, so it can avoid the disadvantages of solid supports, such as sample loss, activity changes, tailing and pollution. Compared with high performance liquid chromatography (High performance liquid chromatography HPLC), CCC has a larger preparation load and better selectivity. Therefore, from microanalysis to preparation separation and even industrial production, CCC is still an important separation and purification technology. However, the resolution of countercurrent chromatography is still much smaller than that of HPLC, gas chromatography (GaschromatographyGC) and capillary electrophoresis (CapillaryelectrophoresisCE). However, researchers have taken many methods to improve this shortcom...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/10C07J73/00
Inventor 吴世华孟杰
Owner ZHEJIANG UNIV
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