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A kind of preparation method of garlic ajoene reference substance

A technology of ajoene and reference substance, which is applied in the field of preparation of ajoene reference substance in garlic, and can solve the problems of complicated process and low purity of ajoene

Active Publication Date: 2020-07-10
深圳市阿霍烯生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method of garlic ajoene reference substance, to solve the problem of using too many organic solvents or vegetable oils in the process of extracting ajoene from garlic in the prior art, complex process, low ajoene purity, etc. question

Method used

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  • A kind of preparation method of garlic ajoene reference substance
  • A kind of preparation method of garlic ajoene reference substance
  • A kind of preparation method of garlic ajoene reference substance

Examples

Experimental program
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Effect test

Embodiment 1

[0037] 1. Take 1Kg of garlic cloves, peel them, crush the garlic to 100μm, add 5L of purified water, extract homogeneously under 50MPa high pressure for 1 hour, extract once, and filter to obtain the extract;

[0038] 2. Add ethyl acetate to the extract to extract twice, 1 L each time, let stand to separate layers, take the upper layer, combine the upper layer to obtain the extract; concentrate the extract under reduced pressure at 45-65°C to obtain the extract;

[0039] 3. Take 100g of 200-300 mesh silica gel, put it into a glass column for chromatography, and apply the dry powder of the extract. In terms of volume ratio, use 2BV ethyl acetate: petroleum ether=20:80 mixed solvent to elute and remove impurities at a flow rate of 2BV / h, then use 2BV ethyl acetate: petroleum ether=50:50 mixed solvent to remove impurities at 2BV / h A flow rate of h elutes ajoene;

[0040] 4. After concentrating the eluate under reduced pressure at 45-65°C, add methanol to dissolve. Take 50 μm C ...

Embodiment 2

[0047] 1. Take 1Kg of garlic alone, peel it, crush the garlic to 50μm, add 2L of purified water, 80MPa high-pressure homogeneous extraction for 0.5h, extract once, filter to obtain the extract;

[0048] 2. Add 2L of n-butanol to the extract and extract once, let stand to separate layers, take the upper layer to obtain the extract; concentrate the extract under reduced pressure at 45-65°C to obtain the extract;

[0049] 3. Take 100g of 200-300 mesh silica gel, put it into a glass column for chromatography, and apply the dry powder of the extract. In terms of volume ratio, use 2BV ethyl acetate: petroleum ether=20:80 mixed solvent to elute and remove impurities at a flow rate of 2BV / h, and then use 2BV ethyl acetate: petroleum ether=30:70 mixed solvent to remove impurities at 2BV / h A flow rate of h elutes ajoene;

[0050] 4. After concentrating the eluate under reduced pressure at 45-65°C, add methanol to dissolve. Take 100 μm C 18 Preparative column, using methanol with a vo...

Embodiment 3

[0054] 1. Take 1Kg of garlic cloves, peel them, crush the garlic to 300μm, add 2L of purified water, extract homogeneously under 20MPa high pressure for 2 hours, extract once, and filter to obtain the extract;

[0055] 2. Extract the extract with chloroform for 3 times, 500mL each time, let stand to separate layers, take the upper layer, combine the upper layer to obtain the extract; extract the extract by concentrating under reduced pressure at 45-65°C to obtain the extract;

[0056] 3. Take 100g of 200-300 mesh silica gel, put it into a glass column for chromatography, and apply the dry powder of the extract. In terms of volume ratio, use 2BV ethyl acetate: petroleum ether = 20:80 mixed solvent to elute and remove impurities at a flow rate of 2BV / h, then use 2BV ethyl acetate: petroleum ether = 70:30 mixed solvent to remove impurities at 2BV / h A flow rate of h elutes ajoene;

[0057] 4. After concentrating the eluate under reduced pressure at 45-65°C, add methanol to dissol...

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Abstract

The invention relates to a garlic ajoene reference substance preparation method. The preparation method comprises the following steps: 1) crushing garlic, adding a solvent, performing high- pressure homogeneous extraction, filtering the material to obtain an extract; 2) adding the solvent in the extract for extraction, standing and layering the material, taking an upper layer of the solution to obtain an extract; 3) performing vacuum concentration on the extract, through silica-gel column chromatography, eluting the solvent to obtain an eluate; 4) performing vacuum concentration on the eluate, through separating and purifying a liquid phase to obtain the ajoene-rich eluate; and 5) performing vacuum concentration on the eluate to obtain the ajoene reference substance. Each index of four spectrums and purity determination of the ajoene reference substance can be accorded with a national standard. The method is simple and stable, is used for preparing the garlic ajoene reference substance, and provides the technical support for deep research of ajoene.

Description

technical field [0001] The invention relates to the technical field of separation and purification, in particular to a preparation method of ajoene reference substance in garlic. Background technique [0002] Garlic generally contains about 1% alliin, and the content of alliin in garlic will increase during low-temperature storage. When cutting, smashing, chewing, etc., alliinase (Alliinase) will quickly decompose alliin into thiosulfinate, the main compound of which is allicin (Allicin). Allicin and other thiosulfinates are very unstable at room temperature, and can be decomposed into sulfide forms, vinyl dithiobenzenes (Dithiins), and ajoenes (Ajoene) in a few hours. [0003] After searching the prior art documents and published patents, it was found that the Chinese patent publication number "CN103525878A", titled "A Preparation Method of Ajoene-rich Composition", discloses the following technical scheme: dissolving in buffer solution The alliin is reacted under the cat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/28C07C323/65C12P11/00
CPCC07C319/28C12P11/00C07C323/65
Inventor 黄伟昌
Owner 深圳市阿霍烯生物科技有限公司
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