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Method for preparing hydroxytyrosol by boiling and hydrolyzing

A technology for hydroxytyrosol and ethanol recovery, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as resin equipment corrosion, and achieve the effects of improving conversion rate, shortening conversion time, and shortening production cycle

Active Publication Date: 2015-07-01
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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  • Method for preparing hydroxytyrosol by boiling and hydrolyzing

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1 The preparation of hydroxytyrosol from Ligustrum lucidum comprises the following steps:

[0031] 1) Preparation of Ligustrum lucidum extract:

[0032] Take 100 grams of Ligustrum lucidum as the raw material, add water to 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, 1.5 hours for the first time, 1 hour for the second and third times), combined and decocted solution, concentrated to extract, with a relative density of 1.2, to obtain Ligustrum lucidum extract;

[0033] 2) Take Ligustrum lucidum extract, add concentrated hydrochloric acid to make the PH to 1, boil and hydrolyze for 2 hours under normal pressure, let the obtained hydrolyzate cool, adjust the pH to neutral with sodium hydroxide, filter, and take the supernatant;

[0034] 3) Apply the supernatant to DM130 macroporous adsorption resin column chromatography. After the adsorption is completed, rinse with water to re...

Embodiment 2

[0036] Example 2 The preparation of hydroxytyrosol from Frangipani Frangipani comprises the following steps:

[0037] 1) Preparation of Frangipani Fructus Extract:

[0038] Take 100 grams of Frangipani japonica as raw material, add water to decoct and extract 3 times (the amount of water added each time is 10 times the weight of the raw material, and extract for 1 hour each), combine the decoction liquid, concentrate to extract, and the relative density is 1.1 to obtain Frangipani extract;

[0039] 2) Take the extract of Frangipani japonica, add concentrated hydrochloric acid to make the PH to 2, boil and hydrolyze for 3 hours under normal pressure, let the obtained hydrolyzate cool, adjust the pH to neutral (7.0) with sodium hydroxide, filter, and take the supernatant ;

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

Embodiment 3

[0042] Embodiment 3 olives prepare hydroxytyrosol, comprising the following steps:

[0043] 1) Preparation of olive extract:

[0044] Take 200 grams of fresh olive fruit as a raw material, press to extract the juice, concentrate to extract, the specific gravity is about 1.3, and the olive extract is obtained.

[0045] 2) Take the olive extract, add concentrated hydrochloric acid to make the pH 2, boil and hydrolyze for 4 hours under normal pressure, let the obtained hydrolyzate cool, adjust the pH to neutral (7.2) with sodium hydroxide, filter, and take the supernatant;

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

[0047]4) Concentrate and dry the collected eluate and recover ethanol to obtain 0.9 g of hydroxytyrosol extract with a purity of 35.9%.

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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 hydrolysis. Background technique [0002] Hydroxytyrosol was originally found in olive oil, and widely exists in plants such as Ligustrum lucidum, Shengxin, olive, Rhodiola rosea, Scrophulariaceae, Lycium barbarum, clove, etc. It has a wide range of pharmacological effects: anti-oxidation, anti-virus, anti-bacterial It can effectively reduce the occurrence of cardiovascular diseases. Japanese scholars found that hydroxytyrosol can inactivate H1N1, H3N2, H5N1, and H9N2 viruses. Under the guidance of Professor Liu Jiankang, Liu Zhongbo, a doctoral student at the Shanghai Institute of Biological Sciences, Chinese Academy of Sciences, cooperated with DSM to study the effect of olive oil extract-hydroxytyrosol on retinal pigment epithelial cells. It was found that olive oil extract hydroxytyrosol (hydroxytyrosol) c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/11C07C37/01C07C37/82
Inventor 王宇杜小英
Owner 陕西方舟制药有限公司
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