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Single-column cyclic separation system for preparing high-purity tanshinone compounds and method thereof

A separation system, tanshinone technology, applied in the direction of steroids, chemical instruments and methods, steroid preparation, etc., can solve the problems of high environmental hazards of solvents, low recovery rate, long separation process, etc., to save separation time, Solvent saving and wide application range

Active Publication Date: 2014-05-07
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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. Single-column circulating separation system and method thereof

Method used

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  • Single-column cyclic separation system for preparing high-purity tanshinone compounds and method thereof
  • Single-column cyclic separation system for preparing high-purity tanshinone compounds and method thereof
  • Single-column cyclic separation system for preparing high-purity tanshinone compounds and method thereof

Examples

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Effect test

Embodiment 1

[0063] A method for preparing high-purity tanshinone compounds using a single-column circulation separation system, the tanshinone compounds include structural formula (1) dihydrotanshinone I, structural formula (2) trilobal ketone B and structural formula (3) methyl tanshinone ester,

[0064]

[0065] Proceed as follows:

[0066] 1. Extraction and enrichment:

[0067] 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 tanshinon...

Embodiment 2

[0075] A method for preparing high-purity tanshinone compounds using a single-column circulation separation system, the prepared tanshinone compounds include structural formula (4) cryptotanshinone, structural formula (5) tanshinone I and structural formula (6) 1,2-dihydrotanshinone,

[0076]

[0077] Proceed as follows:

[0078] 1. Extraction and enrichment:

[0079] 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 under reduced pressure and freeze-dry to obtain cryptotanshinone, tanshinone Ⅰ and 1,2- The cr...

Embodiment 3

[0087] A method for preparing high-purity tanshinone compounds using a single-column circulation separation system, the prepared tanshinone compounds include structural formula (1) dihydrotanshinone I, structural formula (2) trefoil B,

[0088]

[0089] Proceed as follows:

[0090] 1. Extraction and enrichment:

[0091] 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 rich dihydrotanshinone Ⅰ and trilobal ratone The crude product of B (HPLC analysis chart sees...

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Abstract

The invention relates to a single-column cyclic separation system for preparing high-purity tanshinone compounds and a method thereof. The single-column cyclic separation system comprises three countercurrent chromatographic columns, three pumps, three detectors, three collectors and three six-way valves. The first countercurrent chromatographic column is taken as a starting separation column, the second countercurrent chromatographic column and the third countercurrent chromatographic column are used as mutually independent cyclic separation columns, the second six-way valve is used for connecting the first and second countercurrent chromatographic columns, and the third six-way valve is used for connecting the first and third countercurrent chromatographic columns; the multi-dimensional cyclic separation of tanshinone compounds can be realized by regulating the second six-way valve and the third six-way valve. The tanshinone compounds comprise dihydrotanshinone I, triiuganone B, methyl tanshinone ester, cryptotanshinone, tanshinone I and 1, 2-dihydrotanshinone. The single-column cyclic separation system and the method, provided by the invention, have the advantages of simple extraction and separation, short time, high product purity and continuous operation, and are suitable for industrial production.

Description

technical field [0001] The invention relates to a single-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): C07J73/00C07J75/00
Inventor 吴世华孟杰
Owner ZHEJIANG UNIV
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