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Three-column cyclic separation system for preparing high-purity tanshinone compound and method thereof

A separation system and technology for tanshinone, applied in separation methods, steroids, chemical instruments and methods, etc., can solve the problems of long separation process, low recovery rate, and high environmental hazards of solvents, and achieve solvent saving and application scope. The effect of wide and saving separation time

Active Publication Date: 2014-05-07
ZHEJIANG UNIV
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  • 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. Three-column circulating separation system and method thereof

Method used

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  • Three-column cyclic separation system for preparing high-purity tanshinone compound and method thereof
  • Three-column cyclic separation system for preparing high-purity tanshinone compound and method thereof
  • Three-column cyclic separation system for preparing high-purity tanshinone compound and method thereof

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Embodiment 1

[0035] The method for preparing high-purity tanshinone compounds using the three-column circulation separation system of the present invention, the tanshinone compounds include structural formula (1) dihydrotanshinone I, structural formula (2) cryptotanshinone, structural formula (3) tanshinone I, structural formula (4) 1 , 2-dihydrotanshinone, structural formula (5) tanshinone Ⅱ A, structural formula (6) trilobal ketone B, structural formula (7) methyl tanshinone ester and structural formula (8) tanshinone A,

[0036]

[0037] Proceed as follows:

[0038] 1. Extraction:

[0039] Take 9.5 kg of dried salvia miltiorrhiza rhizome, grind 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 tanshinone extracts of dihydrotanshinone Ⅰ, cryptotanshinone, tanshinone Ⅰ, 1,2-dihydrotansh...

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Abstract

The invention relates to a three-column cyclic separation system for preparing a high-purity tanshinone compound and a method thereof. The three-column cyclic separation system comprises three countercurrent chromatographic columns, three pumps, three detectors, three collectors and four six-way valves, wherein the first countercurrent chromatographic column is used as a start separation column; the second countercurrent chromatographic column and the third countercurrent chromatographic column are cyclic separation columns independent from each other; a sample is subjected to first-dimensional separation through the first countercurrent chromatographic column, sequentially enters the second countercurrent chromatographic column for second-dimensional separation by adjusting the three six-way valves, enters the third countercurrent chromatographic column for third-dimensional separation, and enters the first countercurrent chromatographic column again for the next cyclic separation, so that multi-dimensional cyclic separation on the tanshinone compound is realized; the tanshinone compound comprises dihydrotanshinone I, cryptotanshinone, tanshinone I, 1,2-dihydrotanshinone, tanshinone II A, three-leaf sage root ketone B, methyl tanshinone ester and neotanshinone A. The three-column cyclic separation system is simple in extraction and separation, short in time and high in product purity and can realize continuous operation.

Description

technical field [0001] The invention relates to a three-column circulating separation system and 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 improv...

Claims

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Application Information

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IPC IPC(8): B01D11/02B01D15/10C07J73/00C07J75/00C07C50/34C07C46/10
Inventor 吴世华孟杰
Owner ZHEJIANG UNIV
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