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Method for synchronous separation and purification of oleuropein and hydroxytyrosol from olive leaves

A technology for synchronous separation of olive leaves, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of oleuropein and hydroxytyrosol which have not been reported, and achieve low cost and high regeneration performance Good, environment-friendly effect

Active Publication Date: 2022-01-11
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the process of simultaneously separating and purifying oleuropein and hydroxytyrosol from olive leaves has not been reported

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Extraction: Weigh 200g of olive leaves, put them in a 5L round bottom flask, add 3L of water, heat in an electric heating mantle to reflux at normal pressure for 2h, and pour out the extract. Add 2.4 L of water to the slag, reflux at normal pressure for 2 hours, pour out the extract, and discard the slag. Combine the two extracts, cool, filter, concentrate the filtrate under reduced pressure, and finally dilute to 2L with water, so that the concentration is equivalent to 0.1g of olive leaf per liter, and shake well to obtain the sample solution;

[0019] (2) Preparation of eluent: Take 20 mL of n-hexane, 180 mL of ethyl acetate, 20 mL of methanol and 180 mL of water, put them in a 1000 mL separatory funnel, shake for a few minutes, let stand to separate the layers, and put the upper, Separate the lower phase as eluent;

[0020] (3) Separation and purification of macroporous resin: take macroporous resin LSA-21112g, wet-load it into a glass column with an inner diam...

Embodiment 2

[0023] (1) Extraction: same as Example 1;

[0024] (2) Preparation of eluent: Take 20 mL of n-hexane, 160 mL of ethyl acetate, 20 mL of methanol and 160 mL of water, put them in a 1000 mL separatory funnel, shake for several minutes, let stand to separate the layers, and put the upper, Separate the lower phase as eluent;

[0025] (3) Separation and purification of macroporous resin: take 12 g of macroporous resin HPD450, and wet-load it into a glass column with an inner diameter of 1.5 cm and a column height of 27 cm. The diameter-to-height ratio is 1:14, and 1 BV=12 mL. Take 8 BV of the sample solution obtained in step (1) and put it on the column for adsorption, adsorb at a flow rate of 12 BV / h, discard the effluent; then add 6 BV of water to the adsorbed resin column to wash and remove impurities, and discard the water washing solution . Then use the lower phase eluent prepared with 7 BV to elute at a flow rate of 3 BV / h. At this time, hydroxytyrosol is mainly eluted; fin...

Embodiment 3

[0027] (1) Extraction: same as Example 1;

[0028] (2) Preparation of eluent: Take 30 mL of n-hexane, 300 mL of ethyl acetate, 50 mL of methanol and 240 mL of water, put them in a 1000 mL separatory funnel, shake for several minutes, let stand to separate the layers, and put the upper and lower Separate the lower phase as eluent;

[0029] (3) Separation and purification of macroporous resin: take 20 g of macroporous resin LSD001, and wet-load it into a glass column with an inner diameter of 1.5 cm and a column height of 27 cm. The diameter-to-height ratio is 1:14, and 1 BV=20 mL. Take 6 BV of the sample solution obtained in step (1) and put it on the column for adsorption, adsorb at a flow rate of 9 BV / h, discard the effluent; then add 8 BV of water to the adsorbed resin column to wash and remove impurities, and discard the water washing solution . Then use the lower phase eluent prepared with 6 BV to elute at a flow rate of 4 BV / h. At this time, hydroxytyrosol is mainly elu...

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Abstract

The invention provides a method for synchronously separating and purifying oleuropein and hydroxytyrosol from olive leaves. The olive leaves are soaked in water for reflux extraction, and the extract is concentrated as a sample solution; n-hexane, ethyl acetate, methanol and After the water is evenly mixed, let it stand for stratification; then separate the upper phase solution and the lower phase solution, and use them as eluents respectively; Remove the washing solution; then use the lower phase eluent to elute and collect the effluent; finally use the upper phase eluent to elute and collect the effluent. Oleuropein was mainly in the upper phase eluent and hydroxytyrosol was mainly in the lower phase eluent. After the extract of the present invention is treated with resin once, the content of oleuropein reaches more than 45%, and the recovery rate reaches more than 90%; the content of hydroxytyrosol reaches about 3%, and the recovery rate reaches more than 85%.

Description

technical field [0001] The invention relates to a method for synchronously separating and purifying oleuropein and hydroxytyrosol from olive leaves, belonging to the technical field of natural product separation. Background technique [0002] Olive ( Oleaeuropaea L.) As an economic crop, it was mainly planted in Greece, Italy and other countries along the Mediterranean Sea at first, and then introduced into my country, mainly distributed in Yunnan, Sichuan, Gansu, Guizhou and other places. Olive leaves, a major by-product of olive farming, are discarded each year during pruning and fruit harvest. This not only pollutes the environment, but also causes serious waste of resources. Therefore, it is very necessary to carry out comprehensive utilization and development of olive leaves. [0003] The active substances in olive leaves are mainly polyphenols, flavonoids, secoiridoids, biflavones, etc., among which oleuropein (OL) and hydroxytyrosol (Hydroxytyrosol, HT) are the tw...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H1/08C07H17/04C07C37/68C07C39/11
CPCC07C37/68C07H1/08C07H17/04C07C39/11
Inventor 邸多隆刘宝乾黄新异
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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