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Double-column circulating separation system and method for preparing high-purity tanshinone compound

A separation system and technology of tanshinone, applied in the direction of separation methods, steroids, chemical instruments and methods, etc., can solve the problems of low recovery rate, high environmental hazards of solvents, and long separation process, so as to save solvent and save separation Effects over a wide range of time and applications

Active Publication Date: 2014-04-23
ZHEJIANG UNIV
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Problems solved by technology

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

Method used

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  • Double-column circulating separation system and method for preparing high-purity tanshinone compound
  • Double-column circulating separation system and method for preparing high-purity tanshinone compound
  • Double-column circulating separation system and method for preparing high-purity tanshinone compound

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Embodiment 1

[0037] A method for preparing a high-purity tanshinone compound by utilizing a double-column circulatory separation system, the tanshinone compound comprises structural formula (1) dihydrotanshinone I, structural formula (2) trilobite ketone 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 rhizomes of Salvia miltiorrhiza, pulverize them into 60-mesh coarse powder, place 30 L of 95% ethanol by volume at room temperature to 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 30 g of the sample and mix it with normal phase silica gel, then elute with petroleum ether and ethyl acetate, collect the eluent rich in tanshinone compounds, concentrate under reduced pressure and freeze-dried to obtain rich in dihydrotanshinone I, trilobal urone The cr...

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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 high-purity 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 contamination. 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 lower than that of HPLC, gas chromatography (Gas chromatography GC) and capillary electrophoresis (Capillary electrophoresis CE). However, researchers have taken many methods to imp...

Claims

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Application Information

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IPC IPC(8): B01D15/10C07J73/00
Inventor 吴世华孟杰
Owner ZHEJIANG UNIV
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