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Violaside a and its preparation method

A purple calyx and new glycoside technology, applied in the field of biomedicine, can solve the problems of difficult separation and purification, cumbersome operation, difficult large-scale preparation, etc., and achieve the effect of reducing sample loss, improving separation efficiency and saving separation time

Inactive Publication Date: 2016-07-06
SHANGHAI JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Violaside a and its preparation method
  • Violaside a and its preparation method

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Experimental program
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Effect test

Embodiment 1

[0035] This embodiment includes the following steps:

[0036] 1) Take 650g of dried purple calyx leaves, pulverize them into coarse powder, and extract with 50% ethanol (v / v) solution (material-to-liquid ratio 1:8) refluxing once for 1 hour each time. The extract is filtered and concentrated to obtain an alcohol dip After 122 g of the alcohol extract was suspended in 1000 mL of water, successively extracted with an equal volume of ethyl acetate, the resulting aqueous layer was extracted with an equal volume of n-butanol, each solvent was extracted once, and finally the n-butanol layer was obtained. The n-butanol is recovered to obtain 27 g of n-butanol extract.

[0037] 2) Take the n-butanol extract obtained in step 1) for chromatography on a silica gel column (loading amount is 1:10), and use a chloroform-methanol solution (100:20~100:40, v / v) gradient elution (diameter The height ratio is 1:6, the flow rate is 3BV / h, 0.2BV is the first batch). The eluent was concentrated under ...

Embodiment 2

[0041] This embodiment includes the following steps:

[0042] 1) Take 652g dried leaves of purple calyx, crush them into coarse powder, and extract twice with 70% ethanol (v / v) solution (material-to-liquid ratio of 1:10) for 2 hours each time. The extract is filtered and concentrated to obtain an alcohol dip Extract 109g of alcohol extract. Suspend the alcohol extract in 1000 mL of water. After successively extracting with equal volume of ethyl acetate, the resulting aqueous layer is extracted with equal volume of n-butanol, each solvent is extracted twice, and finally the n-butanol layer is obtained. The n-butanol is recovered to obtain 25 g of n-butanol extract.

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

Embodiment 3

[0047] This embodiment includes the following steps:

[0048] 1) Take 650g of dried purple calyx leaves, crush them into coarse powder, reflux and extract 3 times with 90% ethanol (v / v) solution (material-to-liquid ratio is 1:12), each 3h, the extract is filtered and concentrated to obtain alcohol immersion Extract 103 g of the alcohol extract. Suspend the alcohol extract in 1000 mL of water. After successively extracting with an equal volume of ethyl acetate, the resulting aqueous layer is extracted with an equal volume of n-butanol, and each solvent is extracted 3 times. Finally, the n-butanol layer is obtained. The n-butanol is recovered to obtain 28 g of n-butanol extract.

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

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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 invention relates to a technology in the field of biomedicine, in particular to a new glycoside A and a preparation method thereof. Background technique [0002] Purple calyx is the dry leaf of Hostaventricosa (Salisb.) Stearn in the genus Liliaceae. It is a common traditional Chinese medicine in our country. The roots, flowers and whole plant of the purple calyx can be used as medicine. Its root is used to treat toothache, redness and swelling of eyes, sore throat, mastitis, otitis media, sore pain, swelling and poison. Our research found for the first time that purple calyx leaves contain a novel structure of steroidal saponin A. The compound is in the S configuration at the 25th position. It is currently only found in purple calyx leaves. Pharmacological experiments have shown that it has the treatment of testosterone propionate. The role of benign prostatic hyperplasia. However, the compound has a complex structure and contains triglycoside compou...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J71/00
CPCC07J71/0005
Inventor 李晓波王梦月李雪梅李锐
Owner SHANGHAI JIAOTONG UNIV
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