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Method for preparing hydroxytyrosol by converting oleuropein through ion exchange resin

An ion exchange resin, hydroxytyrosol technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as being unsuitable for factory production, adding acid and cultivating too long, and avoiding acid The effect of pollution, solvent safety and non-toxicity, good application prospect

Inactive Publication Date: 2015-06-24
HEILONGJIANG BAYI AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method of adding acid culture takes too long and is not suitable for industrial production

Method used

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  • Method for preparing hydroxytyrosol by converting oleuropein through ion exchange resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Using 1 kg of lilac twigs as raw material, homogenate extraction with 20% ethanol solution by volume fraction to obtain extract; after removing alcohol by rotating the extract, and using HPD-100B macroporous resin column to absorb the obtained plant extract, The highly polar impurity part is washed away with a low-concentration ethanol solution with a volume fraction of 15%, and is used for the preparation of other products. Then elution was carried out with a high-concentration ethanol solution with a volume fraction of 40%, and the collected eluate was concentrated and dried to obtain crude oleuropein. After dissolving the obtained crude oleuropein in 20% ethanol solution, the super acidic SO 3 - Ion exchange resin 001*7 resin column, then eluted with ethanol solution with a volume fraction of 70%, collected the effluent and eluent, concentrated and recovered ethanol after merging, and obtained 7.5g of hydroxytyrosol extract, and used high performance liquid phase C...

Embodiment 2

[0027] Using 1 kg of Pamarinium leaves as a raw material, it was soaked and extracted with 40% ethanol solution for 120 minutes to obtain an extract; after the extract was rotary-evaporated to remove alcohol, the obtained plant extract was absorbed by a D101 macroporous resin column , with a volume fraction of 20% low-concentration ethanol solution to wash away the highly polar impurity part, and use it for the preparation of other products. Then elution was carried out with a high-concentration ethanol solution with a volume fraction of 45%, and the collected eluate was concentrated and dried to obtain crude oleuropein. After dissolving the obtained crude oleuropein in 20% ethanol solution, the super acidic SO 3 - Ion exchange resin 001*7 resin column, then eluted with ethanol solution with a volume fraction of 80%, collected the effluent and eluent, concentrated and recovered ethanol after merging, and obtained 5.2 g of hydroxytyrosol extract, and used high performance liqu...

Embodiment 3

[0029] Using 1 kg of small-leaf clove sprigs as a raw material, homogenate extraction with a volume fraction of 30% ethanol solution to obtain an extract; after the extract is rotary-evaporated to remove alcohol, after the HPD-100B macroporous resin column is used to absorb the obtained plant extract, The highly polar impurity part is washed away with a low-concentration ethanol solution with a volume fraction of 25%, and is used for the preparation of other products. Then elution was carried out with a high-concentration ethanol solution with a volume fraction of 50%, and the collected eluate was concentrated and dried to obtain crude oleuropein. After dissolving the obtained crude oleuropein in 20% ethanol solution, the super acidic SO 3 - Ion-exchange resin 001*7 resin column, then elute with ethanol solution with a volume fraction of 80%, collect the effluent and eluate, concentrate and recover ethanol after merging, and obtain 9.6g of hydroxytyrosol extract, and use high...

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Abstract

The invention discloses a method for preparing hydroxytyrosol by converting oleuropein through an ion exchange resin. The method comprises the following steps: by taking a plant extract as a raw material, carrying out adsorption separation by a macroporous resin, enriching an oleuropein part in the plant extract through silica-gel column chromatography, then hydrolyzing and converting oleuropein to generate hydroxytyrosol through a strong-acid SO3<-1> ion exchange resin, collecting column-passing effluent and eluent, combining the column-passing effluent and eluent and then concentrating to recover ethanol, so as to obtain a high-concentration hydroxytyrosol extract. The ion exchange resin in the method disclosed by the invention is capable of being repeatedly utilized, moderate in reaction conditions, and good in stability; the used solvent is safe and non-toxic; the hydrolysis conversion rate is not less than 90%; moreover, the problems of acid pollution, difficult separation and the like existing in hydrochloric acid hydrolysis are avoided; the method is good in application prospect, and suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of natural product chemistry, in particular to a method for preparing hydroxytyrosol by converting oleuropein with an ion exchange resin. Background technique [0002] The chemical name of hydroxytyrosol (hydroxytyrosol) is 3,4-dihydroxyphenylethanol, also known as hydrated tyrosine, 4-(2-hydroxyethyl)-1,2-benzenediol, which is a natural polyphenol Compounds whose molecular structure is as follows: [0003] [0004] Originally derived from olive leaf extract, it mainly exists in various parts of olives in the form of esterified oleuropein, and free hydroxytyrosol can be obtained after oleuropein is hydrolyzed. Studies have found that hydroxytyrosol has many biopharmacological activities that are beneficial to human health, and has been paid attention to by the biological and medical circles in recent years. The preparation and chemical synthesis of hydroxytyrosol are the research hotspots of medicinal chemists re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/11C07C37/00C07C37/82
Inventor 刘香萍韩玉静李国良杨智明罗英花曲善民杨伟光
Owner HEILONGJIANG BAYI AGRICULTURAL UNIVERSITY