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Method for extracting and purifying tanshinone monomeric compounds from red sage root

An extract, tanshinone technology, applied in the direction of steroids, quinone separation/purification, organic chemistry, etc., can solve the problems of troublesome operation, low purity of components, etc., and achieves reagent saving, simple method operation, and low content of polar impurities. Effect

Inactive Publication Date: 2011-08-31
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above-mentioned various methods may adopt multi-step separation, and the operation is cumbersome; or only one or a few tanshinone components can be obtained; or the obtained components are not high in purity

Method used

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  • Method for extracting and purifying tanshinone monomeric compounds from red sage root
  • Method for extracting and purifying tanshinone monomeric compounds from red sage root
  • Method for extracting and purifying tanshinone monomeric compounds from red sage root

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-5

[0033] Embodiment 1-5: Method for extracting and purifying tanshinone monomer compounds from salvia miltiorrhiza

[0034] (1) Preparation of the extract: Take 100 g of crushed Danshen medicinal material (through a 25-mesh sieve), add 500 ml of dichloromethane (soaked for 120 min) and reflux extraction three times, the extraction temperature is 40 °C, and the extraction time is 30 h each time . The three extracts were combined, the dichloromethane was recovered, and the Danshen extract was obtained. figure 2 is the high performance liquid chromatogram of salvia miltiorrhiza dichloromethane extract, by figure 2 It can be seen that the main component of the extract is tanshinone compounds, and the amount of impurities is low.

[0035](2) Purification by high-speed countercurrent chromatography: the extract of Salvia miltiorrhiza was dissolved in the lower phase of petroleum ether-n-butanol-methanol-water system as the sample solution for subsequent separation and purificati...

Embodiment 6

[0050] Example 6 The difference from Examples 1-5 is that in the preparation of the extract in step (1), percolation extraction is used, and a double-layer percolation column with a jacket for heating and heat preservation is used. The temperature of the return medium is 43°C, and the percolation The flow rate was 3 column volumes / hour. According to the high performance liquid chromatogram of each compound, calculate through chromatographic area normalization method, the purity of dihydrotanshinone I (compound 1) is 96.6%, 1,2,15,16-tetrahydrodanshinone (compound 2) The purity of tanshinone (compound 3) is 96.3%, the purity of tanshinone I (compound 4) is 99.3%, the purity of ganxixinone (compound 5) is 96.5%, and the purity of tanshinone IIA (compound 5) is 99.4%. 6) was 99.6% pure, and tanshinone (compound 7) was 99.3% pure.

Embodiment 7

[0051] Example 7The difference from Examples 1-5 is that in the preparation of the extract in step (1), ultrasonic extraction is used, the ultrasonic frequency used is 28KHZ, the extraction time is 40 minutes, and the number of extractions is 2 times. According to the high performance liquid chromatogram of each compound, calculate through chromatographic area normalization method, the purity of dihydrotanshinone I (compound 1) is 96.2%, 1,2,15,16-tetrahydrodanshinone (compound 2) The purity of tanshinone is 96.4%, the purity of cryptotanshinone (compound 3) is 96.4%, the purity of tanshinone I (compound 4) is 96.7%, the purity of ganxixinone (compound 5) is 98.4%, and the purity of tanshinone IIA (compound 6) was 98.6% pure, and tanshinone (compound 7) was 96.3% pure.

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Abstract

The invention discloses a method for extracting and purifying tanshinone monomeric compounds from red sage root, which comprises the steps of: (1) preparing an extract: smashing the red sage roots, immersing in dichloromethane, extracting by percolation, ultrasound or refluxing, and recovering solvent from an extracting solution to obtain the extract of the red sage root; and (2) purifying with high-speed countercurrent chromatography: purifying the obtained extract by the high-speed countercurrent chromatography with petroleum ether-n-butyl alcohol-methanol-water as a two-phase solvent system, so as to obtain seven monomeric compounds with purity over 95%, including dihydrotanshinone I, 1,2,15,16-tetrahydrotanshinquinone, cryptotanshinon, tanshinone I, neo-przewaquinone A, tanshinone II A and miltirone.

Description

technical field [0001] The invention belongs to the field of chemical industry, and specifically relates to a method for extracting and purifying various high-purity tanshinone monomer compounds from the traditional Chinese medicine Salvia miltiorrhiza Compounds such as quinone, cryptotanshinone, tanshinone I, ganxixinone, tanshinone IIA, and tanshinone. Background technique [0002] Danshen (Salivia miltiorrihiza Bunge) is a traditional Chinese medicine in my country. It has the effects of dispelling blood stasis and relieving pain, promoting blood circulation and stimulating menstruation, clearing heart and eliminating troubles, and can significantly increase coronary flow. Tanshinone compounds are the main fat-soluble components of Danshen, which have obvious anti-inflammatory effects and have been widely used in the treatment of coronary heart disease. [0003] At present, there are many reports on the methods of extracting and purifying tanshinone compounds from Salvia...

Claims

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Application Information

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IPC IPC(8): C07J73/00C07C50/16C07C46/10C07D493/04
Inventor 孙爱玲柳仁民
Owner LIAOCHENG UNIV
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