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SFC separation and purification preparation method of tanshinone IIA

A technology for separation and purification of tanshinone, applied in the production of organic chemistry, steroids, bulk chemicals, etc., can solve the problems of ethanol recovery, concentration, drying process loss, etc., achieve simple post-processing, maintain stability, and simple operation process Effect

Inactive Publication Date: 2014-05-14
江苏汉邦科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to aim at the stability of tanshinone components in the process of extracting tanshinone by ethanol percolation or reflux greatly affected by heat and humidity, tanshinone II A In the problem of serious loss in the process of ethanol recovery, concentration and drying, a semi-preparative SFC separation system is provided to prepare high-purity tanshinone II A A novel method for a monomer, the method comprising the following steps:

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0010] Take 20 mg of the ethanol extract of Salvia miltiorrhiza, dissolve in 95% ethanol, and inject it into the semi-preparative SFC separation system from the autosampler; 2 The flow rate is 0.8~5.0ml / min, the temperature is 40°C, and the back pressure is 15MPa. The detection wavelength of the ultraviolet photometric detector that adopts is 270nm, collects tanshinone II A The peak fraction was analyzed by HPLC with a purity of ≥98.5%.

Embodiment 2

[0012] Take 50mg of the ethanol extract of Danshen, dissolve it in ethanol, and inject it into the semi-preparative SFC separation system from the autosampler; the chromatographic column size is Φ25×250mm, C18 packing, particle size 2 The flow rate is 5.0~20.0ml / min, the temperature is 40°C, and the back pressure is 18MPa. The detection wavelength of the ultraviolet photometric detector that adopts is 270nm, collects tanshinone II A The peak fraction was analyzed by HPLC with a purity of ≥99.2%.

Embodiment 3

[0014] Take 100 mg of the ethanol extract of Danshen, dissolve it in 95% ethanol, and inject it into the semi-preparative SFC separation system from the autosampler; 2 The flow rate is 5.0~40.0ml / min, the temperature is 40°C, and the back pressure is 20MPa. The detection wavelength of the ultraviolet photometric detector that adopts is 270nm, collects tanshinone II A The peak fraction was analyzed by HPLC with a purity of ≥99.5%.

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Abstract

The invention relates to an SFC separation and purification preparation method of tanshinone IIA. With an ethanol extract of salvia miltiorrhiza as a raw material, appropriate separation conditions of a mobile phase proportion, a chromatographic column, a temperature, a pressure and the like are obtained through SFC optimization of conditions and are further enlarged to a semi-preparative SFC separation system, and a tanshinone IIA monomer is obtained. The method has the advantages that the ethanol extract of alvia miltiorrhiza directly adopts the semi-preparative SFC separation system to obtain the tanshinone IIA monomer, high efficiency of the separation process can be realized, and the method has the advantages of simple operation, short cycle, green and environmental protection, and simple subsequent treatment.

Description

technical field [0001] The present invention relates to a kind of supercritical fluid chromatographic separation technology, especially relate to a kind of tanshinone II A SFC separation and purification preparation method. Background technique [0002] Salvia miltiorrhiza is the dry root and rhizome of Salvia miltiorrhiza in the labiatae family. It was first recorded in "Shen Nong's Materia Medica", listed as top grade, and has been recorded in successive dynasties of herbal medicines. Salvia miltiorrhiza is bitter in nature, slightly cold, returns to the heart, liver meridian; has the effect of promoting blood circulation and dispelling blood stasis, dredging menstrual flow and relieving pain, clearing heart-fire and eliminating restlessness, cooling blood and eliminating carbuncle. The main active ingredients in Danshen are fat-soluble tanshinones and water-soluble salvianolic acids. Tanshinone II A , Cryptotanshinone, Tanshinone I, Dihydrotanshinone I, etc. Modern ph...

Claims

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Application Information

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IPC IPC(8): C07J73/00
CPCY02P20/54
Inventor 王冰冰郁万中张大兵
Owner 江苏汉邦科技股份有限公司
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