Method for purifying hydroxytyrosol

A technology of hydroxytyrosol and purification method, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as unutilized oleuropein, incomplete utilization of resources, etc., and achieves reduction in dosage and catalysis The amount of reaction catalyst, the effect of reducing difficulty and improving economic benefits

Inactive Publication Date: 2011-06-15
天津市尖峰天然产物研究开发有限公司
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

Liu Dailin's patent (CN101298411B) discloses a method for extracting hydroxytyrosol from olive extracts. The method adopts styrene resin column chromatography, ethyl acetate extraction and molecular distillation techniques to extract hydroxytyrosol from olive leaves. Alcohol is purified to 70%, but the oleuropein in its raw material has not been utilized, resulting in incomplete utilization of resources

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  • Method for purifying hydroxytyrosol
  • Method for purifying hydroxytyrosol
  • Method for purifying hydroxytyrosol

Examples

Experimental program
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Embodiment 1

[0037] 1) adding 30 times the mass of deionized water to the crude product powder with oleuropein content of 10% and stirring to dissolve;

[0038] 2) Pass the oleuropein aqueous solution through the AB-8 type macroporous resin column, wash with deionized water 3 times the retained volume, and then elute with 40% ethanol aqueous solution with a volume fraction 3 times the retained volume, and collect the ethanol eluent from aqueous solution;

[0039] 3) Concentrating the collected eluate in vacuum to no alcohol to obtain a refined aqueous solution of oleuropein;

[0040] 4) In the refined oleuropein aqueous solution, add hydrochloric acid to make the pH of the solution = 2, stir at 75°C for 7 hours, add an appropriate amount of saturated sodium hydroxide solution to neutralize until the pH = 7 when the reaction is terminated, and obtain hydroxytyrosol-containing aqueous solution;

[0041] 5) Concentrate the aqueous solution containing hydroxytyrosol to 5 degrees of sugar in ...

Embodiment 2

[0043] 1) adding 10 times the mass of deionized water to the olive leaf extract concentrate with oleuropein content of 1% and hydroxytyrosol content of 0.4% and stirring to dissolve;

[0044]2) The aqueous solution of oleuropein was passed through a D101 type macroporous resin column and a neutral alumina column in series, washed with deionized water 3 times the retained volume, and then eluted with 35% ethanol aqueous solution 3.5 times the retained volume, and collected Ethanol-containing eluent;

[0045] 3) Concentrating the collected eluate in vacuum to no alcohol to obtain a refined aqueous solution of oleuropein;

[0046] 4) In the refined oleuropein aqueous solution, add glycosidase with a solution mass of 1.5%, stir at 45°C for 4 hours, and heat up to 75°C for 30 minutes to inactivate when the reaction is terminated; an aqueous solution containing hydroxytyrosol is obtained;

[0047] 5) Concentrate the aqueous solution containing hydroxytyrosol to a sugar content of 7...

Embodiment 3

[0049] 1) adding 20 mass times of deionized water to the crude product powder with oleuropein content of 25% and stirring to dissolve;

[0050] 2) passing the oleuropein aqueous solution through a neutral alumina chromatography column, washing with 3 times the reserved volume of deionized water, and then eluting with 4 times the reserved volume of 50% ethanol aqueous solution, and collecting the ethanol-containing eluate;

[0051] 3) Concentrating the collected ethanol-containing eluent in vacuum to no alcohol to obtain a refined aqueous solution of oleuropein;

[0052] 4) In the refined oleuropein aqueous solution, add hydrochloric acid to make the pH of the solution = 1, stir at 75° C. for 7 hours, add an appropriate amount of saturated sodium hydroxide solution to neutralize to neutral when the reaction is terminated; obtain an aqueous solution containing hydroxytyrosol;

[0053] 5) Concentrate the aqueous solution containing hydroxytyrosol to a sugar content of 10 degrees ...

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Abstract

The invention discloses a method for purifying hydroxytyrosol. The method for purifying the hydroxytyrosol comprises the following steps of: dissolving an oleuropein crude product by using deionized water under stirring; passing through an adsorption type macroporous resin chromatographic column, washing with the deionized water, performing elution by using ethanol aqueous solution, and collecting eluent; performing vacuum concentration until no alcohol exists to obtain refined oleuropein aqueous solution; adding an inorganic acid to react; adding sodium hydroxide to adjust the pH value to be 7 to obtain hydroxytyrosol-containing aqueous solution; performing vacuum concentration; performing extraction by using equivalent ethyl acetate; and laminating ester and concentrating to remove the ethyl acetate to obtain faint yellow paste hydroxytyrosol with purity of more than or equal to 80 percent. In the method, the characteristic of one-way conversion from the oleuropein in an olive leaf resource to the hydroxytyrosol is completely utilized, so that the conversion rate is high, the current situation that the oleuropein component is blindly separated in the purification process of the oleuropein is changed, the oleuropein is converted into the hydroxytyrosol with high economic value, economic benefit is improved, and difficulty in preparation of high-content hydroxytyrosol is greatly reduced.

Description

technical field [0001] The invention relates to a preparation method of high-content hydroxytyrosol. Background technique [0002] Olive (olive) belongs to Oleaceae (Oleaceae) in botany, and its most famous is Olea europaea L., which is also called foreign olive. Olives are native to Asia Minor, and are mainly distributed in the Mediterranean coastal areas, with Spain, Italy, Portugal and Albania as the concentrated production areas. Now all countries in the world are introducing and cultivating them, and my country is no exception. In the 1970s and 1980s, Gansu Province took the lead in introducing foreign olive varieties. , has been cultivated successfully and has begun to take shape. [0003] There are three main functional components known in olive leaves: simple phenolic compounds (such as hydroxytyrosol, tyrosol); aldehyde derivatives); lignans. These three types of compounds are good antioxidants. Among them, oleuropein is clinically used as a medicine, which can i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/11C07C37/70
Inventor 於洪建孙华庚
Owner 天津市尖峰天然产物研究开发有限公司
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