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Method for separating and preparing steroidal saponins from garlic by utilizing high speed countercurrent chromatography

A high-speed countercurrent chromatography, garlic technology, applied in separation methods, chemical instruments and methods, liquid separation of solid adsorbents, etc., can solve problems such as dead adsorption, low yield, and inability to detect online

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

AI Technical Summary

Problems solved by technology

Steroidal saponins in garlic are similar in structure and have no ultraviolet absorption. Traditional chromatographic separation methods cannot achieve efficient and rapid separation of them, and the content of steroidal saponins in garlic is low. In traditional research, multi-step silica gel column chromatography is usually used And the separation and preparation of steroidal saponins in garlic by using the preparation liquid and other methods, not only takes a long time, cannot be detected online, but also causes dead adsorption, large loss, and low yield

Method used

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  • Method for separating and preparing steroidal saponins from garlic by utilizing high speed countercurrent chromatography
  • Method for separating and preparing steroidal saponins from garlic by utilizing high speed countercurrent chromatography
  • Method for separating and preparing steroidal saponins from garlic by utilizing high speed countercurrent chromatography

Examples

Experimental program
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Effect test

Embodiment 1

[0032] (1) Preparation of garlic steroid saponin crude extract

[0033] 1 kg of fresh garlic bulbs was pulverized, extracted three times with garlic (kg) / 90% ethanol (L) (1:3) under reflux, combined the extracts, concentrated under reduced pressure to obtain a crude garlic saponin extract. The crude steroidal saponin extract of garlic was dissolved in water, applied to D101 macroporous adsorption resin, eluted with 30% and 80% ethanol respectively, and the 80% ethanol part was recovered under reduced pressure to dryness to obtain the total steroidal saponins;

[0034] (2) Preparation of garlic steroidal saponins by countercurrent separation

[0035] Mix n-butanol: glacial acetic acid: 6mM ammonium acetate aqueous solution (4:1:5, v / v / v), shake fully, let stand for 12 hours, take the upper phase as the stationary phase, and the lower phase as the mobile phase, respectively The biphasic solvent was ultrasonically degassed for 30 minutes. Put 300 mg of the solvent of the crude ...

Embodiment 2

[0044] (1) Preparation of garlic steroid saponin crude extract

[0045] The preparation of the crude extract of garlic steroidal saponins is the same as in Example 1.

[0046] (2) Preparation of garlic steroidal saponins by countercurrent separation

[0047] Mix n-butanol: glacial acetic acid: 10mM ammonium acetate aqueous solution (3.5:1:4.5, v / v / v), oscillate fully, let stand for 12 hours, take the upper phase as the stationary phase, and the lower phase as the mobile phase, respectively The biphasic solvent was ultrasonically degassed for 30 minutes. Put 350 mg of the solvent of the crude sample in the above (1) in 20 ml of equal volume of stationary phase and mobile phase mixed solution, and filter to obtain a sample solution. Connect the high-speed countercurrent chromatograph and the evaporative light scattering detector, pump the prepared stationary phase into the chromatographic column of the high-speed countercurrent chromatograph, then turn on the high-speed counte...

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Abstract

The invention relates to a separation method of a natural medicament, in particular to a method for separating and preparing four garlic steroidal saponins by utilizing high speed countercurrent chromatography and an evaporative light-scattering detector. The method is characterized in that the high speed countercurrent chromatography and the evaporative light-scattering detector are utilized commonly; fractions are collected according to the spectra of the evaporative light-scattering detector, wherein the stationary phase and mobile phase of the high speed countercurrent chromatography are obtained by mixing n-butanol, glacial acetic acid and ammonium acetate solution and layering, the upper phase is the stationary phase and the lower phase is the mobile phase; and four steroidal saponins are separated from garlic. The method does not use solid carrier and has no irreversible adsorption phenomenon; the sample has no loss; the method for preparing the garlic steroidal saponins has high efficiency, high speed, low cost and no pollution; and the purity of the obtained garlic steroidal saponins is up to more than 90%.

Description

technical field [0001] The invention relates to a method for separating natural medicines, in particular to a method for separating and preparing four allicin steroidal saponins from garlic by using high-speed countercurrent chromatography coupled with an evaporative light scattering detector. Background technique [0002] Garlic is the bulb of Allium sativum L. in the Liliaceae family. It is an indispensable condiment on people's daily table, and it is often used as a health medicine to prevent colds, improve body immunity and prevent cardiovascular disease. systemic disease. It is rich in volatile sulfur-containing compounds and steroidal saponins are the main active ingredients, and has been developed into garlic dry powder, garlic volatile oil capsules and other drugs. Modern people pay more and more attention to their own health care. As a plant with the same origin as medicine and food, garlic has excellent flavor and curative effect, and has no toxic and side effects...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J71/00B01D15/10
Inventor 孔令义马强罗建光
Owner CHINA PHARM UNIV