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Method for performing ultrasonic assisted in-situ extraction on natural hydroxytyrosol

An ultrasound-assisted, hydroxytyrosol technology, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of long separation and purification cycle and low extraction rate of hydroxytyrosol, and achieve easy scale-up production, The effect of shortening the production cycle and simple operation

Inactive Publication Date: 2015-07-15
LANZHOU UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The present invention aims at the defects of the above-mentioned production process, focuses on solving the problems of low extraction rate of hydroxytyrosol and long separation and purification period, and combines the simple and effective separation and purification process to develop a method for rapidly and efficiently preparing high-content hydroxytyrosol The new process, extraction and extraction are carried out simultaneously, the production cycle is short, the extraction efficiency is high, the separation and purification process is simple, it can realize green, environmental protection, reduce production costs, increase the yield of products, and facilitate industrial production

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0027] Take 1 kg of olive leaves, wash them, dry them in the air, crush them through an 80-mesh sieve, soak them in 8 L of sodium hydroxide solution, and soak them for 12 hours. Using ultrasonic extraction equipment, add 12L ethyl acetate to form a two-phase system, and conduct ultrasonic extraction for 4 hours under the conditions of vacuum degree 0.08MPa, power 200W, and temperature 80°C. Stand to separate layers, take the upper extract phase, add 2.5g of activated carbon for decolorization by heating under reflux. After decolorization, the solution was concentrated under reduced pressure at a vacuum degree of 0.07MPa and a temperature of 40°C until the Baume degree was 3, and 0.2L ether was added thereto twice to remove impurities to obtain crude hydroxytyrosol. Dissolve in 0.05L of 30% ethanol, filter while hot, and concentrate the obtained clear solution under reduced pressure at a vacuum of 0.09MPa and a temperature of 55°C. Vacuum freeze-drying is carried out at ℃ to o...

Embodiment 2

[0029] Take 5 kg of olive leaves, wash them, dry them in the air, crush them through an 80-mesh sieve, soak them in 50 L of sodium hydroxide solution, and soak them for 20 hours. Use ultrasonic extraction equipment, add 100L ethyl acetate to form a two-phase system, and conduct ultrasonic extraction for 5 hours under the conditions of vacuum degree 0.08MPa, power 220W, and temperature 90°C. Stand to separate layers, take the upper extract phase, add 13g of activated carbon for decolorization by heating under reflux. After decolorization, the solution was concentrated under reduced pressure at a vacuum degree of 0.07 MPa and a temperature of 40° C. until the Baume degree was 3, and 1 L of ether was added thereto twice to remove impurities to obtain crude hydroxytyrosol. Melt with 0.27L of 40% ethanol, filter it while it is hot, and concentrate the obtained clear solution under reduced pressure at a vacuum of 0.09MPa and a temperature of 55°C. Vacuum freeze-drying was carried o...

Embodiment 3

[0031]Take 10kg of olive leaves, wash them, dry them in the air, crush them through an 80-mesh sieve, soak them in 100L of sodium hydroxide solution for 24 hours. Use ultrasonic extraction equipment, add 200L ethyl acetate to form a two-phase system, and conduct ultrasonic extraction for 6 hours under the conditions of vacuum degree 0.08MPa, power 240W, and temperature 100°C. Stand to separate layers, take the upper extract phase, add 27g of activated carbon for decolorization by heating under reflux. After decolorization, the solution was concentrated under reduced pressure at a vacuum degree of 0.07 MPa and a temperature of 40° C. until the Baume degree was 3, and 2.2 L of diethyl ether was added thereto twice to remove impurities to obtain crude hydroxytyrosol. Dissolve in 0.6L of 50% ethanol, filter while it is hot, and concentrate the obtained clear solution under reduced pressure at a vacuum of 0.09MPa and a temperature of 55°C. Vacuum freeze-drying was carried out at ℃...

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Abstract

The invention discloses a method for preparing natural hydroxytyrosol by taking olive leaves as a raw material and adopting an ultrasonic assisted in-situ extraction process, and belongs to the technical field of extraction and separation of natural product effective components. The method comprises the following steps: (1) pretreating the raw material; (2) performing ultrasonic extraction synchronous leaching on hydroxytyrosol in the olive leaves by using a double-phase system which consists of an organic solvent A and an alkaline solution; (3) performing activated carbon decoloration on an organic solvent extraction phase, then performing compressed concentration, and removing impurities by adopting an organic solvent B; and (4) performing thermal melting on an extract which is obtained by virtue of impurity removal by using an organic solvent C, filtering while heating, and then performing compressed concentration and drying to obtain a high-quality hydroxytyrosol product. According to the process disclosed by the invention, the cavitation effect and mechanical vibration effect produced by ultrasonic waves and an in-situ extraction process are adopted, extraction and leaching can be synchronously performed, and natural hydroxytyrosol with high content can be prepared by using simple separation and purification processes; and the method disclosed by the invention can be used for shortening the production cycle, is high in product yield, mild in separation and purification conditions, small in toxicity and low in production cost, and can be suitable for industrial production.

Description

technical field [0001] The invention relates to a method for extracting and preparing high-purity natural hydroxytyrosol, in particular to a method for ultrasonically assisted in-situ extraction of natural hydroxytyrosol. Background technique [0002] Hydroxytyrosol, also known as 3,4-dihydroxyphenylethanol, was originally a phenolic compound extracted from olive oil. Natural hydroxytyrosol is mainly produced from olive trees, especially its leaves and fruits. Oleuropein exists in the form of oleuropein, which accounts for 6% to 9% (mass fraction) in dry olive tree leaves, and is also the reason why olive fruit has a strong bitter taste. During olive oil processing, in order to remove the sour taste in olive oil, oleuropein is hydrolyzed to obtain polyphenolic compounds, and hydroxytyrosol is the main component of these phenolic compounds. [0003] The nature of oleuropein is unstable, and it is easily degraded into hydroxytyrosol and elemic acid under the action of acid, a...

Claims

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Application Information

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IPC IPC(8): C07C39/11C07C37/70
CPCC07C37/004C07C37/685C07C37/70C07C37/72C07C39/11
Inventor 陈富文史高峰王国英姚瑞星赵国超
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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