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Method for separating oleuropein from olive leaves through counter-current chromatographic continuous sampling

A technology of countercurrent chromatography and olive leaves is applied in the field of natural product separation and separation of oleuropein in olive leaves, and can solve the problems of low recovery rate, limited injection volume of preparative instruments, and only oleuropein yield. Improves injection volume and productivity

Pending Publication Date: 2022-02-25
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in this purification method, active carbon is used for decolorization and n-butanol extraction, which consumes more solvent, and the recovery of n-butanol consumes a lot of energy, and the recovery rate is low, and the yield of oleuropein only reaches about 1%.
The methods disclosed in the prior art all use countercurrent chromatography when separating oleuropein, but they are all traditional single injections, and the preparation volume is limited by the injection volume of the instrument

Method used

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  • Method for separating oleuropein from olive leaves through counter-current chromatographic continuous sampling
  • Method for separating oleuropein from olive leaves through counter-current chromatographic continuous sampling

Examples

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Embodiment 1

[0024] Take 100 g of dried olive leaves, add 1000 mL of ethanol aqueous solution, the ethanol aqueous solution is composed of 800 mL of ethanol and 200 mL of water; extract under reflux for 90 min, filter to obtain an extract, and place the extract at a temperature of 55°C and a pressure of -0.08MPa. Concentrate under reduced pressure to solvent-free state under reduced pressure to obtain crude extract of olive leaf. Mix n-butanol, ethyl acetate, methanol, water, and dichloromethane in a volume ratio of 1:19:1:19, shake, stand for layering, and obtain a two-phase solvent system. The original mobile phase was used as the original mobile phase for countercurrent chromatographic separation; then the original mobile phase was divided into two parts; 50 mg of olive leaf crude extract was dissolved in a part of the original mobile phase (100 mL) to prepare a mass-volume concentration of 5 mg / mL. sample solution, another part of the original mobile phase is the mobile phase, and the ...

Embodiment 2

[0030]Take 50 g of dried olive leaves, add 500 g of water, heat under reflux for 120 min, and filter to obtain an extract. The extract is dried under reduced pressure at a temperature of 75 °C and a pressure of -0.08 MPa to obtain crude olive leaf extract. Mix n-butanol, ethyl acetate, methanol, and water in a volume ratio of 1:19:1:19, shake, stand for layering, and obtain a two-phase solvent system; the upper phase of the two-phase solvent system is used as a countercurrent chromatograph Separated stationary phase, the lower phase of this two-phase solvent system was used as the original mobile phase for countercurrent chromatography; then the original mobile phase was divided into two parts; 700 mg of olive leaf crude extract was dissolved in a part of the original mobile phase (70 mL) , to prepare a sample solution with a mass volume concentration of 10 mg / mL; another part of the original mobile phase is the mobile phase; the sample solution is filtered with a 0.45 μm Milli...

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Abstract

The invention discloses a method for separating oleuropein from olive leaves through counter-current chromatographic continuous sampling. The method comprises the following steps: extracting the olive leaves, and conducting concentrating to obtain crude extract of the olive leaves; adopting a solvent system formed by mixing n-butyl alcohol, ethyl acetate, methanol and water as a two-phase solvent for counter-current chromatographic separation, wherein an upper phase of the solvent system is used as a stationary phase, and a lower phase is used as an original mobile phase; and dissolving the crude extract of the olive leaves in one part of the original mobile phase to prepare a sample solution, using the other part of the original mobile phase as a mobile phase, conducting continuous sample introduction and separation of oleuropein in the olive leaves by adopting an elution-extrusion mode to obtain oleuropein monomers, wherein an obtained compound has relatively high purity. According to the separation method disclosed by the invention, a sample introduction amount is increased through continuous sample introduction, solvent consumption can be reduced, a preparation amount is increased, and macro preparation of oleuropein in the olive leaves is facilitated.

Description

technical field [0001] The invention relates to a method for separating oleuropein from olive leaves, in particular to a method for separating oleuropein monomers from olive leaves by continuous sampling using countercurrent chromatography in an elution-extrusion mode, belonging to a method for separating natural products technical field. Background technique [0002] Olive oil (Olea europaea L.) is an evergreen tree of the Oleaceae family, and its leaves are rich in oleuropein. Modern pharmacological studies have shown that oleuropein has good anti-inflammatory, antifungal, antiviral, antioxidant, and anticancer and hypoglycemic effects. At the same time, oleuropein can also reduce the degree of oxidation of low-density lipoprotein, prevent coronary heart disease, atherosclerosis, relieve vascular smooth muscle, and lower blood pressure. In addition, oleuropein is also used in a variety of skin care products to reduce UV damage to skin cells, promote collagen production i...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
CPCC07H17/04C07H1/08
Inventor 黄新异邸多隆孙潇
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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