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Novel method for rapidly preparing hydroxytyrosol

A technology of hydroxytyrosol and a new method, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as shortened production cycle, low efficiency, and long production process time of high-purity hydroxytyrosol, and achieves The effect of shortening the production cycle, stable process and easy industrial production

Inactive Publication Date: 2013-05-22
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problems of long production process and low efficiency of high-purity hydroxytyrosol, and shorten the production cycle

Method used

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  • Novel method for rapidly preparing hydroxytyrosol
  • Novel method for rapidly preparing hydroxytyrosol
  • Novel method for rapidly preparing hydroxytyrosol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 50g of crude oleuropein extract (containing 38.3% oleuropein), add 1000mL of 0.3mol / L NaOH, stir for 30mins, then add hydrochloric acid to neutralize the pH of the solution to 7, then add 300mL ethyl acetate Ethyl acetate, repeated extraction 3 times, rotary evaporation to remove ethyl acetate, adding 50mL water to dilute and dissolve, then pass through AB-8 macroporous resin, after fully adsorbed, then elute with 40% ethanol aqueous solution, and collect 3-5BV solution , and then through Sephadex LH-20, eluted with 60% ethanol aqueous solution, collected 4-6BV of the solution, and finally recovered ethanol by rotary evaporation, and the concentrated solution was vacuum freeze-dried to obtain a solid content of 7.36g, wherein the hydroxyl The HPLC content of tyrosol reached 93.12%.

[0021]

Embodiment 2

[0023] Weigh 30g of crude oleuropein extract (containing oleuropein 27.93%), add 800mL of 0.2mol / L NaOH, stir for 45mins, then add hydrochloric acid to neutralize the solution to pH=7, then add 150mL ethyl acetate Ethyl acetate, repeated extraction 3 times, rotary evaporation to remove ethyl acetate, adding 35mL water to dilute and dissolve, then pass through AB-8 macroporous resin, after fully adsorbed, then elute with 55% ethanol aqueous solution, and collect 2-4BV solution , and then through Sephadex LH-20, eluted with 50% ethanol aqueous solution, collected 3-4BV of the solution, and finally recovered ethanol by rotary evaporation, and the concentrated solution was dried in vacuum to obtain a solid content of 3.87g, of which hydroxyphenol The HPLC content of alcohol reaches 89.58%.

[0024]

Embodiment 3

[0026] Weigh 80g of dried olive leaves (containing 8.21% oleuropein), crush them to 40-60 mesh, add 2400mL of 0.3mol / L NaOH, stir for 40mins, then add dilute sulfuric acid to neutralize the solution to pH=7, Then add 500mL of ethyl acetate, repeat the extraction 3 times, remove the ethyl acetate by rotary evaporation, add 150mL of water to dilute and dissolve, then pass through HPD-450 macroporous resin, after fully adsorbed, then elute with 55% ethanol aqueous solution, collect 3-5BV solution, and then passed through Sephadex LH-20, eluted with 65% ethanol aqueous solution, collected 3-5BV solution, and finally recovered ethanol by rotary evaporation, and the concentrated solution was vacuum freeze-dried to obtain solid content 5.35g, wherein the HPLC content of hydroxytyrosol reaches 85.12%.

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Abstract

The invention discloses a novel method for rapidly preparing hydroxytyrosol and belongs to the technical field of extraction and separation of active ingredients of natural products. According to the novel method, the olive leaf extract containing oleuropein serves as a raw material, and hydroxytyrosol is prepared by rapid hydrolysis under alkaline conditions. The method comprises the following steps: weighing a certain amount of olive leaf extract, mixing with an alkaline solution, reacting under a certain temperature and time, cooling to room temperature, adding a little amount of acid to neutralize until the pH is equal to 7, centrifuging, collecting the supernatant fluid, adding a proper amount of ethyl acetate for extracting, performing rotary evaporation to remove ethyl acetate, sequentially allowing the obtained concentrated solution to pass through macroporous resin and sephadex resin, and finally carrying out spray freeze-drying or vacuum freeze-drying to obtain high-purity hydroxytyrosol. The purity can be up to over 90 percent. The novel method is easy to operate, short in time, high in efficiency, high in quality and suitable for industrialization.

Description

technical field [0001] The invention relates to the technical field of extraction and purification of chemical active ingredients of natural products, and relates to a process for preparing high-purity hydroxytyrosol. Background technique [0002] Hydroxytyrosol, also known as 3,4-dihydroxyphenylethanol, Hydroxytyrosol in English, is a natural small molecule polyphenolic compound. It was discovered in the form of echinacoside in the traditional Chinese medicine Echinacea angustifolia in 1950. Hydroxytyrosol also exists in olive leaves, but the content is very small, about 0.2%-0.7%. Because it exhibits many biological activities such as anti-oxidation, anti-inflammation, anti-cancer (prostate cancer and breast cancer, etc.), protection against cardiovascular diseases, lowering blood sugar, repairing cartilage damage or inhibiting obesity, etc. Especially its antioxidant properties, hydroxytyrosol is considered to be one of the most free radical scavenging natural antioxida...

Claims

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Application Information

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IPC IPC(8): C07C39/11C07C37/50
Inventor 黄立新谢普军张彩虹游凤张耀雷
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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