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Hosta ventricososide A and preparation method thereof

A technology of violet calyx and new glycosides, applied in the field of biomedicine, can solve the problems of difficult large-scale preparation, difficult separation and purification, complicated operation, etc., and achieves the effects of saving separation time, reducing sample loss and improving separation efficiency.

Inactive Publication Date: 2015-05-13
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the structure of this compound is complex, it is a triglycoside compound, and the types of three sugars are different; and the 25th position is an S configuration, which is prone to configuration transformation under conditions such as acid, alkali, and high temperature; the compound is highly water-soluble, The content in purple calyx is low, less than 0.5%. Purple calyx also contains many other water-soluble components such as carbohydrates, proteins, amino acids, etc., which are difficult to separate and purify
However, the yield of components obtained by this technology is low: the obtained steroidal saponins are less than 6 parts per million; the operation is cumbersome, semi-preparative HPLC is required, and it is difficult to prepare on a large scale

Method used

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  • Hosta ventricososide A and preparation method thereof
  • Hosta ventricososide A and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] This embodiment includes the following steps:

[0036] 1) Take 650g of dried leaves of Calyx aurantiae, crush them into coarse powder, and use 50% ethanol (v / v) solution (solid-to-liquid ratio: 1:8) to reflux extract once for 1 hour each time. Paste 122g, the alcoholic extract is suspended in 1000mL water, after being extracted with ethyl acetate of equal volume successively, the obtained water layer is extracted with n-butanol of equal volume, and each solvent is extracted once respectively, and n-butanol layer is obtained at last, Recover n-butanol to obtain 27 g of n-butanol extract.

[0037] 2) Take the n-butanol extract obtained in step 1) and carry out silica gel column (sample loading is 1:10) chromatography, and use chloroform-methanol solution (100:20~100:40, v / v) gradient elution (diameter The height ratio is 1:6, the flow rate is 3BV / h, and 0.2BV is a fraction). After the eluate was concentrated under reduced pressure, TLC detection (developing solvent: chl...

Embodiment 2

[0041] This embodiment includes the following steps:

[0042] 1) Take 652g of dried leaves of Calyx aurantiae, crush them into coarse powder, use 70% ethanol (v / v) solution (solid-to-liquid ratio: 1:10) to reflux extract twice, each time for 2h, and extract the solution to be filtered and concentrated to obtain alcohol immersion Paste 109g, the alcoholic extract is suspended in 1000mL water, after being extracted with ethyl acetate of equal volume successively, the obtained water layer is extracted with n-butanol of equal volume, and each solvent is respectively extracted twice, and n-butanol layer is obtained at last, Recover n-butanol to obtain 25 g of n-butanol extract.

[0043]2) Take the n-butanol extract obtained in step 1) and carry out silica gel column (sample loading is 1:20) chromatography, and use chloroform-methanol solution (100:20~100:40, v / v) gradient elution (diameter The height ratio is 1:8, the flow rate is 6BV / h, and 0.2BV is a fraction), and the eluate is...

Embodiment 3

[0047] This embodiment includes the following steps:

[0048] 1) Take 650g of dried leaves of Violet Calyx, crush them into coarse powder, and use 90% ethanol (v / v) solution (solid-to-liquid ratio: 1:12) to reflux extract 3 times, each time for 3 hours, and extract the solution to obtain alcohol immersion after filtration and concentration Paste 103g, the alcoholic extract is suspended in 1000mL water, after being extracted with ethyl acetate of equal volume successively, the gained water layer is extracted with n-butanol of equal volume, and each solvent is respectively extracted 3 times, finally gets n-butanol layer, Recover n-butanol to obtain 28 g of n-butanol extract.

[0049] 2) Take the n-butanol extract obtained in step 1) and carry out silica gel column (sample loading: 1:30) chromatography, and use chloroform-methanol solution (100:20~100:40, v / v) gradient elution (diameter The height ratio is 1:10, the flow rate is 9BV / h, and 0.2BV is a fraction), after the eluent ...

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Abstract

The invention provides hosta ventricosa leaf dry powder extractive in the field of biological medicine and particularly relates to hosta ventricososide A. The structural formula of the hosta ventricososide A is shown in the specification. Hosta ventricosa dry powder is subjected to reflux extraction in ethyl alcohol, then alcohol extract is extracted in an organic solvent, an extract obtained after extraction is subjected to silica column chromatography and reverse-phase silica column chromatography and eluted, fraction with hosta ventricososide A as a main ingredient is collected, and finally, the collected fraction is recrystallized to obtain the hosta ventricososide A. The purity of the obtained hosta ventricososide A is larger than 96%. Normal phase and reverse phase are combined, steroid saponin with high purity is obtained through recrystallization, the separation efficiency is improved, and the separation time is saved.

Description

technical field [0001] The present invention relates to a technique in the field of biomedicine, in particular to a violaxin A and a preparation method thereof. Background technique [0002] Purple calyx is the dried leaf of Hosta ventricosa (Salisb.) Stearn, a plant of the genus Hosta in the family Liliaceae. It is a commonly used traditional Chinese medicine in my country. The root, flower, and whole plant of Purple calyx can be used as medicine. It has the effects of dispelling blood stasis, relieving pain, and detoxifying. Its roots are used to treat toothache, red eyes, sore throat, mastitis, otitis media, sores and swelling. Our study found for the first time that there is a novel steroidal saponin A in the leaves of the purple calyx. The role of benign prostatic hyperplasia. However, the structure of this compound is complex, it is a triglycoside compound, and the types of three sugars are different; and the 25th position is an S configuration, which is prone to con...

Claims

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Application Information

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IPC IPC(8): C07J71/00
CPCC07J71/0005
Inventor 李晓波王梦月李雪梅李锐
Owner SHANGHAI JIAO TONG UNIV
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