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A method for preparing hydroxytyrosol by boiling and hydrolyzing

A technology for hydroxytyrosol and ethanol, which is applied in the field of preparing hydroxytyrosol by boiling and hydrolysis, can solve problems such as corrosion of resin equipment, and achieve the effects of improving conversion rate, shortening conversion time and shortening production cycle.

Active Publication Date: 2011-12-14
陕西方舟制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method uses acid solution on the column and acid solution for elution, which will cause corrosion to the resin equipment

Method used

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  • A method for preparing hydroxytyrosol by boiling and hydrolyzing

Examples

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Effect test

Embodiment 1

[0030] Example 1 Preparation of hydroxytyrosol from Ligustrum lucidum, including the following steps:

[0031] 1) Preparation of Ligustrum lucidum extract:

[0032] Take 100 grams of Ligustrum lucidum as a raw material, add water and soak for half an hour, decoct and extract 3 times (the amount of water added each time is 8 times the weight of the raw material, the first time is 1.5 hours, and the second and third times are 1 hour each), combined and decocted. liquid, concentrated to extract shape, the relative density is 1.2, obtains Ligustrum lucidum extract;

[0033] 2) get Ligustrum lucidum extract, add concentrated hydrochloric acid to make its pH 1, boil and hydrolyze for 2 hours under normal pressure, after the gained hydrolyzate is allowed to cool, sodium hydroxide is adjusted to neutrality, filtered, and the supernatant is taken;

[0034] 3) Load the supernatant on DM130 macroporous adsorption resin column chromatography, rinse with water to remove impurities after t...

Embodiment 2

[0036] Example 2 The preparation of hydroxytyrosol from jasmine flower includes the following steps:

[0037] 1) Preparation of the extract of S. japonica:

[0038] Using 100 grams of Shengxinhua as a raw material, add water for decocting and extracting for 3 times (the amount of water added each time is 10 times the weight of the raw material, and each extraction is 1 hour), combine the decoction liquid, and concentrate it to an extract, with a relative density of 1.1. Shengxinhua extract;

[0039] 2) Take the extract of S. japonica, add concentrated hydrochloric acid to make its pH 2, boil and hydrolyze for 3 hours under normal pressure, adjust the pH to neutral (7.0) with sodium hydroxide after the gained hydrolyzate is cooled, filter, and get the supernatant ;

[0040] 3) Load the supernatant on XDA10 macroporous adsorption resin column chromatography, rinse with water to remove impurities after the adsorption is completed until the washing liquid becomes clear, then elu...

Embodiment 3

[0042] Embodiment 3 olive prepares hydroxytyrosol, comprising the following steps:

[0043] 1) Preparation of olive extract:

[0044] Take 200 grams of fresh olive fruit as a raw material, squeeze out the juice, concentrate it to the shape of an extract, the specific gravity is about 1.3, and obtain an olive extract.

[0045] 2) get the olive extract, add concentrated hydrochloric acid to make its pH 2, boil and hydrolyze for 4 hours under normal pressure, adjust the pH to neutrality (7.2) with sodium hydroxide after the gained hydrolyzate is allowed to cool, filter, and get the supernatant;

[0046] 3) Load the supernatant on D101 macroporous adsorption resin column chromatography, rinse with water to remove impurities after the adsorption is completed until the washing liquid becomes clear, then elute with 25% ethanol, and collect the eluate;

[0047]4) The collected eluate was concentrated to dryness and ethanol was recovered to obtain 0.9 g of a hydroxytyrosol extract wit...

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Abstract

The invention discloses a method for preparing hydroxytyrosol by boiling and hydrolyzing. The method comprises the following steps of: firstly, preparing plant extract, adjusting pH of the plant extract to be 1-3, and boiling and hydrolyzing the plant extract for 1-4 h under normal pressure; after cooling, adjusting the pH to be 6.8-7.2, filtering and taking supernate; sampling the supernate on macroporous adsorption resin, after adsorbing, washing and removing impurities by using water, eluting by using 10-90% by volume of methanol or ethanol, and collecting eluent; and condensing and recovering the methanol or the ethanol to obtain hydroxytyrosol extract. According to the method disclosed by the invention, the conversion time of the hydroxytyrosol is greatly shortened; the conversion rate is increased; the production cycle is shortened as a whole; the production cost is saved; after hydrolyzing, adjusting to be neutral and placing the sample on a column, the supernate is washed and purified by using water and then eluted by using the methanol or the ethanol; and, instead of placing the sample on the column and eluting by using acid liquid, the disadvantage that resin equipment can be corroded is overcome.

Description

technical field [0001] The invention belongs to the technical field of preparation of hydroxytyrosol, and relates to a method for preparing hydroxytyrosol by boiling and hydrolysis. Background technique [0002] Hydroxytyrosol was originally found in olive oil, and widely exists in plants such as Ligustrum lucidum, Shengxin, olive, Rhodiola, Scrophulariaceae, Lycium barbarum, clove, etc. It has a wide range of pharmacological effects: it has antioxidant, antiviral, antibacterial It can effectively reduce the occurrence of cardiovascular disease. Japanese scholars have found that hydroxytyrosol can inactivate H1N1, H3N2, H5N1, and H9N2 viruses. Under the guidance of Professor Liu Jiankang, Liu Zhongbo, a doctoral student at Shanghai Institute of Biological Sciences, Chinese Academy of Sciences, cooperated with DSM Company to study the effect of olive oil extract-hydroxytyrosol on retinal pigment epithelial cells. The results showed that olive oil extract hydroxytyrosol (hyd...

Claims

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Application Information

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IPC IPC(8): C07C39/11C07C37/01C07C37/82
Inventor 雷玉萍令华
Owner 陕西方舟制药有限公司
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