Method for extracting wedelia lactone by using microwave-assisted technology

A microwave-assisted, wedelolide-based technology, applied in the direction of organic chemistry, can solve the problems of complex production process and high synthesis cost, and achieve the effects of convenient operation, wide industrial application and reduced energy consumption

Inactive Publication Date: 2012-11-14
TIANJIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The preparation of wedelolide in existing patents mainly adopts the method of chemical synthesis, which has the disadvantages of high synthesis cost and complicated production process. The invention patent publication number is CN102020655A, which provides a method for naturally extracting wedelide. Ultrasonic extraction with alkaline water containing borax, macroporous resin is applied to the extract, and the column solution is collected and adjusted to a certain pH value with acid, then washed with macroporous resin until the sugar reaction is negative, eluted with low-carbon alcohol, ethyl acetate Extraction, methanol recrystallization

Method used

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  • Method for extracting wedelia lactone by using microwave-assisted technology
  • Method for extracting wedelia lactone by using microwave-assisted technology

Examples

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Effect test

Embodiment 1

[0026] Take 1 kg of Eclipta whole grass and crush it, add methanol with a volume fraction of 70%, and a solid-to-liquid ratio of 1:5, here the two are measured by kg:l (a solid-to-liquid ratio of 1:5 to 1:8 is also suitable), microwave Extract once, each extraction time is 3min, filter the extract, use a rotary evaporator to concentrate and recover methanol, and control the temperature at 45°C to obtain a black-green extract. Add 3 times the volume of black-green extract, heat in a microwave generator at 70°C for 2 minutes, and filter while hot. The filtrate is successively removed with petroleum ether to remove fat-soluble components such as chlorophyll, extracted twice with 2L ethyl acetate, anhydrous sulfuric acid Sodium dehydration, concentrated under reduced pressure to obtain a yellow-green extract, each time take the extract 1:4 on a silica gel column, the column volume is 1.5L, the diameter-to-height ratio is 1:9, and the ethyl acetate-methanol volume ratio is 20:1 Gra...

Embodiment 2

[0028] Take 1kg of Eclipta whole grass and crush it, add ethanol with a volume fraction of 75%, and the solid-to-liquid ratio is 1:10, here the two are measured by kg:l (solid-to-liquid ratio 1:9~1:13 is also suitable), microwave Extract 2 times, each extraction time is 6min, filter the extract, combine the filtrate, use a rotary evaporator to decompress and concentrate to recover methanol, and the temperature is controlled at 60°C to obtain a black-green extract. Add 2 times the volume of water of the black-green extract, heat in a microwave generator at 75°C for 3 minutes, filter while hot, remove fat-soluble components such as chlorophyll with petroleum ether in turn, extract 3 times with 1.8L ethyl acetate, anhydrous Sodium sulfate dehydration, concentrated under reduced pressure to obtain a yellow-green extract, each time take the extract 1:3 on the silica gel column, the column volume is 1.5L, the diameter-to-height ratio is 1:6, and the ethyl acetate-methanol volume rati...

Embodiment 3

[0030] Take 10kg of Eclipta whole grass and pulverize it, add methanol with a volume fraction of 75%, and the solid-to-liquid ratio is 1:16, here the two are measured by kg:l (the solid-to-liquid ratio is also suitable for 1:14 to 1:17), microwave Extract 2 times, each extraction time is 9min, filter the extract, combine the filtrates, use a rotary evaporator to decompress and concentrate to recover methanol, and control the temperature at 55°C to obtain a black-green extract. Add 3 times the volume of the black-green extract, heat in a microwave generator at 75°C for 2 minutes, and filter while it is hot. The filtrate is successively removed with petroleum ether for fat-soluble components such as chlorophyll, extracted 3 times with 16L ethyl acetate, anhydrous sulfuric acid Sodium dehydration, concentrated under reduced pressure to obtain a yellow-green extract, each time take the extract 1:5 on a silica gel column, the column volume is 15L, the diameter-to-height ratio is 1:9...

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Abstract

The invention relates to a method for extracting wedelia lactone by using microwave-assisted technology, which comprises the following steps of: crushing eclipta grass, adding an organic extractant, extracting with microwave for 2-3 times, filtering the extract, combining filtrate, recovering organic extractant with a rotary evaporator by reduced pressure evaporation to obtain dark green extract, adding 2-5 times the volume of water, heating in a microwave reator of 70-80 DEG C for a period of time, filtering as soon as possible, adding petroleum ether to the filtrate to remove fat-soluble ingredients such as chlorophyll, adding ethyl acetate to extract, adding anhydrous sodium sulfate to remove water, concentrating under reduced pressure to obtain yellow-green extract, taking certain amount of extract on the silica gel column, using ethyl acetate-methanol with polarity ascending for the gradient elution, obtaining off-white solid when the volume ratio of ethyl acetate-methanol is appropriate, and recrystallizing with methanol for 2-4 times to obtain the product. The microwave extracting technology can shorten the time, reduce the solvent dosage and energy consumption, and also can improve the yield and purity of the extract. The technology can meet the requirement of the green environmental protection and has significance of industrialization.

Description

technical field [0001] The invention belongs to the field of separation and purification of natural products, and relates to a method for extracting wedelolide, in particular to a microwave-assisted technology for extracting wedelia lactone. Background technique [0002] Herba Ecliptae (Herba Ecliptae) is the dry above-ground part of the snakehead sausage of the genus Channa in the family Compositae, because when its stems and leaves are rubbed, black juice can be seen flowing out, so it is called "Ecliptae", and it is one of the commonly used traditional Chinese medicines. It has the functions of nourishing liver and kidney, cooling blood and stopping bleeding. It is used for loose teeth, premature graying of beard and hair, dizziness and tinnitus, sore waist and knees, blood heat due to yin deficiency, hematemesis, traumatic bleeding, etc. The main pharmacological active ingredient of Eclipta chinensis is the coumarin ether component wedelolide contained in it. According ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/04
Inventor 丁辉史大静
Owner TIANJIN UNIV
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