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A class of flavonoid lignan compounds and extraction method thereof

An extraction method and compound technology, applied in organic chemistry and other directions, can solve problems such as unreported chemical composition research, and achieve the effects of rich structural types, high purity, and little impact on the ecological environment

Inactive Publication Date: 2019-01-11
LANZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, studies on the chemical constituents of this genus have not been reported.

Method used

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  • A class of flavonoid lignan compounds and extraction method thereof
  • A class of flavonoid lignan compounds and extraction method thereof
  • A class of flavonoid lignan compounds and extraction method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The preparation method of the flavonoid lignans mixture of the present invention is as follows:

[0024] Collect the aboveground part of the weeping grass, dry it in the shade and crush it, and pass it through a 100-mesh sieve to get a fine powder. Take 11.8kg of fine powder and soak it in 3 times of methanol solution at room temperature for 3 times, successively for 3 days, 3 days and 7 days, and distill under reduced pressure to obtain about 980g of crude extract.

[0025] The crude extract was dissolved in 500 mL of water and then extracted three times with ethyl acetate in a volume ratio (1:1) to obtain 190 g of the ethyl acetate phase.

[0026] The ethyl acetate part passed through a macroporous resin (HP-20, Mitsubishi Chemical Corporation), the eluent was methanol-water, the volume ratios were: 30%, 50%, 80%, methanol, 9 L each. Wherein 80% methanol was partially concentrated under reduced pressure and dried in the shade to obtain 40 g.

[0027] Ethyl acetate 8...

Embodiment 2

[0030] The preparation method of compound 1 and 2 of the present invention is as follows:

[0031] The Fr.3d part (12 g) was shaken and washed with 20 mL of methanol solution, the washing solution was concentrated under reduced pressure to obtain Fr.3dr (2 g), and the remaining part was dried in the shade to obtain Fr.3dc.

[0032] A partial sample (0.3 g) of Fr.3dr was subjected to column chromatography on Sephadex LH-20 (Sephadex LH-20, Amersham Pharmacia Biotech) with methanol as eluent (200 mL) to remove compound alfalfalin (20 mg). The remaining parts were combined and purified by silica gel column chromatography, chloroform / methanol=10:1 was used as the eluent for purification, dissolved in methanol, passed through Waters1525 high performance liquid chromatography, the chromatographic solvents were water and acetonitrile, and the chromatographic conditions were: 25% acetonitrile Isocratic, flow rate: 2mL / min, detection wavelength: 340nm, compound 1 (4mg, retention time: ...

Embodiment 3

[0041] The preparation method of compound 3-6 of the present invention is as follows:

[0042] The Fr.3d part (12g) was shaken and washed with 20mL of methanol solution, the washing solution was concentrated under reduced pressure to obtain Fr.3dr (2g), and the remaining insoluble part was dried in the shade to obtain Fr.3dc.

[0043] Take Fr.3dc (10g) by reverse phase (RP-C 18 , Mitsubishi Chemical Corporation), the eluent is acetone / water (volume ratio: 30%, 50%, 70%, 90%), each 2L. The 30% and 50% parts are Fr.3dc1, the 70% part is Fr.3bc2, the 90% part is Fr.3dc3, and the acetone part is Fr.3dc4.

[0044] The Fr.3dc2 part was subjected to silica gel column chromatography with chloroform:methanol, the volume ratio was 20:1, 10:1, 5:1, 300 mL each, gradient elution. Get chloroform: methanol (10:1) part, adopt 20cm * 20cm to prepare silica gel plate, chloroform / methanol=10:1 is eluent, obtain two parts, utilize Sephadex LH-20 column chromatography (with chloroform / methanol ...

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Abstract

Elymus nutans is distributed in a large area in China and is one kind of main native herbs in Tibet plateau, and plant resources are abundant. The invention discloses a method for separating 10 flavone and lignin compounds from elymus nutans. The 3 of the 10 compounds are new compounds, and the purity of 8 of the 10 compounds is 95% or above. The compound has multiple physiological effects of liver protection, blood fat reduction, oxidation resistance and the like. In addition, the overground parts of the elymus nutans are utilized, the production cycle is show, less influence is caused on the ecological environment, the high-purity monomeric compound can be quickly prepared, the economic benefits are remarkable, and the method has very important significance on scientific and reasonable development of the elymus nutans resource.

Description

technical field [0001] The invention belongs to the technical field of biopharmaceuticals, and in particular relates to a method for extracting high-purity flavonoid lignans from Elymus chinensis. Background technique [0002] Elymus is a large genus of the Triticea family, with 150 species of plants. They are widely distributed all over the world, and most of them are important pastures. China is one of the countries where this genus is widely distributed. However, the chemical constituents of this genus have not been reported. [0003] Among them, Elymus pachyrhiza is distributed in a large area in my country, from the Northeast Plain to the Inner Mongolia grassland to the Qinghai-Tibet Plateau, and is rich in plant resources. Especially as one of the main native pasture grasses on the Qinghai-Tibet Plateau, Elymus acarina has adapted to the high altitude of the Qinghai-Tibet Plateau during the long-term evolution process, the large temperature difference between day an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/78C07D311/30C07D311/40
CPCC07D311/30C07D311/40C07D311/78
Inventor 高坤刘权吴成慧
Owner LANZHOU UNIVERSITY
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