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

A separation system and technology for tanshinone, applied in separation methods, steroids, chemical instruments and methods, etc., can solve the problems of low recovery rate, high environmental hazard of solvent, long separation process, etc., and achieve solvent saving and separation saving. Time, wide range of effects

Active Publication Date: 2016-03-02
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 three-column extraction and separation process for the preparation of tanshinone compounds that is simple in extraction and separation and can be operated continuously, aiming at the shortcomings of 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. Circulation separation system and method thereof

Method used

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

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Embodiment 1

[0035] The method for preparing 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) trefoil B, structural formula (7) methyl tanshinone ester and structure

[0036] Formula (8) Salvia quinone A,

[0037]

[0038] Proceed as follows:

[0039] 1. Extraction:

[0040] Take 9.5 kg of dried salvia miltiorrhiza root, 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 it 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-dihydrotanshinone, ta...

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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 circulation separation system and 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 shortcoming...

Claims

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Application Information

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