Method for purifying oleuropein

A technology of oleuropein and olive leaf, applied in chemical instruments and methods, separation methods, organic chemistry, etc., can solve the problems of small separation, long cycle, and small preparation, and achieve high product yield, short cycle, large amount of preparation

Inactive Publication Date: 2012-05-23
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method adopts preparative liquid phase purification, the preparation amount is small, the solvent utilization rate is low, and the cost is high
Document "SephadexLH-20 Purification of Oleuropein", small amount of separation, long cycle

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Olive leaves are crushed, 1kg is taken, 10L of 90% ethanol solution is added to reflux and extracted twice, the combined extract is decolorized by adding 100g of activated carbon to reflux for 1 hour, the activated carbon is filtered out, ethanol is recovered under reduced pressure, the concentrated solution is extracted 3 times by adding 1L of water-saturated n-butanol, The n-butanol layer was collected and recovered under reduced pressure to obtain an extract. Take chloroform, methanol, n-butanol, and water and mix them in a ratio of 3:4:2:1, remove the lower phase to dissolve the extract, use the upper phase as the stationary phase, and separate with a preparative high-speed countercurrent chromatograph, with the speed controlled at 850r / min and the flow rate controlled At 2ml / min, the sample was injected and separated, and the effective components of oleuropein were collected and dried under reduced pressure to obtain 9.1g of oleuropein with a content of 96.7%.

Embodiment 2

[0020] Olive leaves are crushed, 1 kg is taken, 10L of 70% ethanol solution is added to reflux and extracted twice, the combined extract is decolorized by adding 80g of activated carbon to reflux for 1 hour, the activated carbon is filtered out, ethanol is recovered under reduced pressure, the concentrated solution is extracted by adding 500L of water-saturated n-butanol for 5 times, The n-butanol layer was collected and recovered under reduced pressure to obtain an extract. Get chloroform, methanol, n-butanol, water and mix according to 6:3:3:1, remove the phase to dissolve the extract, the above phase is the stationary phase, separate with a preparative high-speed countercurrent chromatograph, the speed is controlled at 1000r / min, and the flow rate is controlled At 3ml / min, the sample was injected and separated, and the effective components of oleuropein were collected and dried under reduced pressure to obtain 9.5g of oleuropein with a content of 95.5%.

Embodiment 3

[0022] Olive leaves are pulverized, 1kg is taken, 5L of 80% ethanol solution is added to reflux and extracted 3 times, the combined extract is decolorized by adding 120g of activated carbon to reflux for 1 hour, the activated carbon is filtered out, ethanol is recovered under reduced pressure, the concentrated solution is extracted 4 times by adding 500L of water-saturated n-butanol, The n-butanol layer was collected and recovered under reduced pressure to obtain an extract. Take chloroform, methanol, n-butanol, and water and mix them in a ratio of 4:3:3:2, remove the lower phase to dissolve the extract, use the upper phase as the stationary phase, and separate with a preparative high-speed countercurrent chromatograph, with the speed controlled at 700r / min and the flow rate controlled At 1ml / min, the sample was separated, and the effective components of oleuropein were collected and dried under reduced pressure to obtain 8.7g of oleuropein with a content of 97.2%.

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Abstract

The invention provides a method for quickly and efficiently purifying oleuropein. The method comprises the following steps of: smashing olive leaves, adding a 70-90 percent ethanol solution in an amount of 5-10 times that of the olive leaves for refluxing and extracting for 2-3 times, adding active carbon into an extracting solution for decoloring, filtering the active carbon out, recovering ethanol, adding water-saturated n-butyl alcohol into a concentrated solution for extracting for 3-5 times, collecting a n-butyl alcohol layer, and recovering under reduced pressure to obtain an extract; and separating the extract with a chloroform-methanol-n-butyl alcohol-water solvent system ((3-6):(2-4):(2-3):(1-2)) by using a preparation type high-speed counter current chromatograph, collecting active ingredients, and drying under reduced pressure to obtain high-content oleuropein. Due to the adoption of the method for purifying the oleuropein, the obtained product has high content, large preparation amount and low cost.

Description

Technical field: [0001] The invention relates to a method for purifying oleuropein, in particular to a method for purifying oleuropein by high-speed countercurrent chromatography. Background technique: [0002] Oleuropein is a phenolic split iridoid glycoside, molecular formula: C 25 h 32 o 13 , molecular weight 540.43, soluble in hot water, methanol, ethanol, ethyl acetate, etc., insoluble in chloroform, petroleum ether and other non-polar organic reagents. [0003] Oleuropein has antioxidant capacity, can reduce the oxidation degree of low-density lipoprotein, prevent the occurrence of coronary heart disease and atherosclerosis, and can also relieve vascular smooth muscle and lower blood pressure. [0004] Oleuropein is mostly extracted from olive leaves and small-leaf cloves, and most of the products are low-content products. [0005] For example, the Chinese patent "Preparation method of olive leaf extract rich in high-purity oleuropein", the method discloses that th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08B01D15/10
Inventor 李法庆杨成东刘东锋
Owner 苏州宝泽堂医药科技有限公司
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