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Preparation method of high-purity wedelolactone

A high-purity technology for wedelide, which is applied in the field of natural medicinal chemistry, can solve the problem of low purity of norwedelide, and achieve the effects of large separation volume, low pollution, and easy operation

Inactive Publication Date: 2014-05-21
SHANGHAI TAUTO BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] CN103265554A discloses a preparation method of norwedelide. Eclipta chinensis is ultrasonically extracted with methanol solution, extracted with ethyl acetate, and then adsorbed with a macroporous resin, and then eluted with methanol solution. However, the obtained norwedelide The purity is not high, still needs further improvement

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  • Preparation method of high-purity wedelolactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Crush the raw material of Eclipta chinensis, weigh 2kg, add 10L50% methanol solution for ultrasonic extraction for 30 minutes each time, extract 3 times, extract the extract under reduced pressure to 1000ml, add an equal volume of water-saturated ethyl acetate to extract 3 times, combine the extracts to recover acetic acid Ethyl ester extract. The extract was mixed with 100-200 mesh silica gel and ethyl acetate, added to silica gel column chromatography, eluted with petroleum ether / ethyl acetate (volume ratio 50:1), and the eluent was concentrated under reduced pressure to obtain a crude extract. For high-speed countercurrent separation. Mix n-hexane, ethyl acetate, ethanol, and water in a volume ratio of 1:3:1:2, shake and let stand to separate layers. Take the upper phase and fill the high-speed countercurrent chromatograph as the stationary phase, turn the main engine at a speed of 800rpm, and pump the lower phase at 2ml / min as the mobile phase. After the dynamic eq...

Embodiment 2

[0019] Crush the raw material of Eclipta chinensis, weigh 2kg, add 20L 60% methanol solution for ultrasonic extraction for 30 minutes each time, extract 3 times, extract the extract under reduced pressure to 1000ml, add an equal volume of water-saturated ethyl acetate to extract 3 times, combine the extracts to recover acetic acid Ethyl ester extract. The extract was mixed with 100-200 mesh silica gel and ethyl acetate, added to silica gel column chromatography, eluted with petroleum ether / ethyl acetate (volume ratio 40:1), and the eluent was concentrated under reduced pressure to obtain a crude extract. For high-speed countercurrent separation. Mix n-hexane, ethyl acetate, ethanol, and water in a volume ratio of 0.5:2:1:3, shake and let stand to separate. Take the upper phase and fill the high-speed countercurrent chromatograph as the stationary phase, turn the main engine at a speed of 800rpm, and pump the lower phase at 2ml / min as the mobile phase. After the dynamic equili...

Embodiment 3

[0021] The raw material of Eclipta chinensis is crushed, weighing 2kg, adding 17L 70% methanol solution for ultrasonic extraction for 30 minutes each time, extracting 3 times, the extract is concentrated under reduced pressure to 1000ml, adding an equal volume of water-saturated ethyl acetate to extract 3 times, and combining the extracts to recover acetic acid Ethyl ester extract. The extract was mixed with 100-200 mesh silica gel and ethyl acetate, added to silica gel column chromatography, eluted with petroleum ether / ethyl acetate (volume ratio 15:1), and the eluent was concentrated under reduced pressure to obtain a crude extract. For high-speed countercurrent separation. Mix n-hexane, ethyl acetate, ethanol, and water in a volume ratio of 0.5:1:1:2, shake and let stand to separate. Take the upper phase and fill the high-speed countercurrent chromatograph as the stationary phase, turn the main engine at a speed of 850rpm, and pump the lower phase at 3ml / min as the mobile ...

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Abstract

The invention relates to a preparation method of high-purity wedelolactone. The preparation method comprises the steps of crushing the raw material eclipta, adding an industrial methanol solution by a quintuple to decuple quantity for ultrasonic extraction 2-3 times, concentrating the extract and then extracting the extract with ethyl acetate, collecting the extract, recovering a reagent and adsorbing the reagent removed extract through a silicagel column, carrying out isocratic elution by using petroleum ether and ethyl acetate in a volume ratio of 5: 1 to 50: 1, concentrating the eluate to obtain a coarse extract, next, separating through a high-speed counter current chromatograph, carrying out online monitoring with an ultraviolet detector, collecting the fraction and carrying out decompression concentration, crystallizing and drying to obtain the high-purity wedelolactone. The preparation method is simple and convenient to operate, high in recovery rate, large in separation quantity and low in pollution due to the adoption of the silicagel column for adsorption and isocratic elution with the petroleum ether and the ethyl acetate, and the obtained wedelolactone is high in purity and has excellent application prospect.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, in particular to a preparation method of high-purity wedelolide. Background technique [0002] Eclipta prostrata L., commonly known as Eclipta prostrata L., is the dry aboveground part of the snakehead intestine of Compositae. It is one of the commonly used traditional Chinese medicines. It has the functions of nourishing liver and kidney, cooling blood and stopping bleeding. According to foreign studies, the main active ingredients of Eclipta japonica for anti-hepatotoxicity are coumarins-wedelide and norwedelide. These two components have an effect on CCl 4 , GalNAc, etc. caused liver injury in rats, all of which have obvious hepatoprotective effects, and the effect of wedelolide is stronger. Wedelotolactone is the main active ingredient of Eclipta chinensis, and it is an important characteristic substance for the quality standard and detection of Eclipta spp. and its extracts. [...

Claims

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Application Information

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IPC IPC(8): C07D493/04
CPCC07D493/04
Inventor 王维娜邓力
Owner SHANGHAI TAUTO BIOTECH CO LTD
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