Method for preparing hyperin and isorhamnetin-3-0-galactose glycosides reference substance simultaneously

A technology of isorhamnetin and galactoside, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of difficult to find reference substances, high cost of equipment, etc. The effect of short process flow and low cost

Inactive Publication Date: 2004-08-25
ZHEJIANG UNIV
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Problems solved by technology

With the continuous deepening of the basic research on the pharmacodynamic substances of traditional Chinese medicine (natural medicine), the demand for reference substances of traditional Chinese medicine (natural medicine) is also increasing. For example, when using high performance liquid chromatography for qualitative and quantitative analysis of some natural products, It is often impossible to carry out in-depth research due to the difficulty of finding the right amount of reference substances for a while
The current preparation method of reference substance usually adopts preparative high-performance liquid chromatography purification, which is expensive and expensive, and is only suitable for preparing a small amount of samples

Method used

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  • Method for preparing hyperin and isorhamnetin-3-0-galactose glycosides reference substance simultaneously
  • Method for preparing hyperin and isorhamnetin-3-0-galactose glycosides reference substance simultaneously
  • Method for preparing hyperin and isorhamnetin-3-0-galactose glycosides reference substance simultaneously

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preparation example Construction

[0018] The simultaneous preparation method steps of hyperin and isorhamnetin-3-O-galactoside reference substance are as follows:

[0019] (1) Put Evodia rutaecarpa medicinal material in a container, add solvent (methanol or ethanol aqueous solution) to reflux and extract.

[0020] (2) The extract of Evodia rutaecarpa was filtered and concentrated under reduced pressure to obtain the extract. Add appropriate amount of water to dissolve the extract, and extract it with petroleum ether, chloroform, and ethyl acetate accordingly.

[0021] (3) The ethyl acetate part was subjected to polyamide column chromatography twice, the first column chromatography was eluted with water and 10-95% ethanol gradient; the second time was eluted with 20-40% ethanol isocratic.

[0022] (4) The eluates from column chromatography were combined and concentrated, and recrystallized from methanol to obtain two reference substances of hyperin and isorhamnetin-3-O-galactoside respectively.

[0023] Hyper...

Embodiment 1

[0027] Evodia rutaecarpa fruit 800g, methanol reflux extraction 3 times, combined filtrate, concentrated under reduced pressure to obtain extract. The extract was dissolved in water and extracted with petroleum ether, chloroform and ethyl acetate respectively. The ethyl acetate part was subjected to polyamide column chromatography, gradient elution of water, 10% ethanol, 30% ethanol, 50% ethanol, 70% ethanol, 95% ethanol, and identified by polyamide thin-layer chromatography. The same components were combined, then subjected to polyamide column chromatography, eluted with 20% ethanol, and recrystallized from methanol to obtain 30 mg of hyperoside, with a content of 99.5%, and 171 mg of isorhamnetin-3-O-galactoside, with a content of 98.4% (HPLC).

Embodiment 2

[0029] Evodia rutaecarpa fruit 800g, methanol reflux extraction 3 times, combined filtrate, concentrated under reduced pressure to obtain extract. The extract was dissolved in water and extracted with petroleum ether, chloroform and ethyl acetate respectively. The ethyl acetate part was subjected to polyamide column chromatography, gradient elution of water, 10% ethanol, 30% ethanol, 50% ethanol, 70% ethanol, 95% ethanol, and identified by polyamide thin-layer chromatography. The same components were combined, then subjected to polyamide column chromatography, eluted with 30% ethanol, and recrystallized from methanol to obtain 31 mg of hyperoside, with a content of 99.4%, and 175 mg of isorhamnetin-3-O-galactoside, with a content of 98.3% (HPLC).

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Abstract

The present invention discloses a method for simultaneously preparing hyperin and isorhammetin-3-O-galactoside control products. Said method includes the following steps: (1) placing Chinese medicinal material evodia in a container, adding solvent to make extraction with reflux; (2) filtering evodia extract, reduced pressure concentrating to obtain extractum, adding water to dissolve it, then successively using petroleum ether, chloroform and ethyl acetate to make extraction; (3). using column chromatographic process to purify the ethyl acetate extracted portion twice; and (4). combining chromatographic eluents, concentrating, recrystallizing so as to obtain the invented two control products of hyperin and isorhamnetin-3-O-galactoside. Said invention is simple, and can simultaneously prepare hyperin and isorhamnetin-3-O-galactoside pure products whose purity can be above 98%.

Description

technical field [0001] The invention relates to a simultaneous preparation method of hyperin and isorhamnetin-3-O-galactoside reference substances. Background technique [0002] In recent years, under the influence of the trend of returning to nature, traditional Chinese medicine (natural medicine) has developed rapidly. With the continuous deepening of the basic research on the pharmacodynamic substances of traditional Chinese medicine (natural medicine), the demand for reference substances of traditional Chinese medicine (natural medicine) is also increasing. For example, when using high performance liquid chromatography for qualitative and quantitative analysis of some natural products, It is often difficult to conduct in-depth research because it is difficult to find an appropriate amount of reference substance for a while. The current preparation method of the reference substance usually adopts preparative high-performance liquid chromatography ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/08C07H17/07
Inventor 吕秀阳潘浪胜吴平东
Owner ZHEJIANG UNIV
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