Method for preparing wedelolactone monomeric compounds extracted from eclipta

A technology of wedelide and wedelide, which is applied in the direction of organic chemistry, can solve the problems of high production cost, low proportion of wedelide monomer compounds, and many operating procedures, and achieve low cost, high extraction rate and simple process Effect

Active Publication Date: 2014-12-10
THE FIRST AFFILIATED HOSPITAL OF MEDICAL COLLEGE OF XIAN JIAOTONG UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

Since the above-mentioned patents all use a large amount of organic solvents, there are many operating procedures,

Method used

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  • Method for preparing wedelolactone monomeric compounds extracted from eclipta

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Example Embodiment

[0022] Example one:

[0023] The Eclipta prostrata medicinal materials are crushed into 40-60 mesh Eclipta protea powder, 150 grams of Eclipta prostrata powder are weighed, put into a multi-stage countercurrent extraction device, and then 1500ml of 80% ethanol-acetic acid aqueous solution is added for countercurrent extraction for 5 hours After extraction, it is filtered, concentrated under vacuum (0.05-0.1MPa), and concentrated under reduced pressure at about 50°C to obtain 4.5 g of crude Eclipta prostrata extract.

[0024] Take a glass chromatographic column with a column length of 450mm and an inner diameter of 45mm, and install 350ml D101 macroporous adsorption resin. Load the crude extract of Eclipta prostrata on the top of the column, and then use the mobile phase 50% and 60% respectively. , 70%, 80%, 90% ethanol-water solution for gradient elution, TLC plate tracking, concentration under vacuum (0.05-0.1MPa), with absolute ethanol to bring water, the obtained solid is recrys...

Example Embodiment

[0030] Embodiment two:

[0031] The medicinal materials of Eclipta prostrata are crushed into 40-60 mesh Eclipta protea powder, 150g of Eclipta protea powder are weighed and put into a multi-stage countercurrent extraction device, and then 1500ml of 80% methanol-phosphoric acid aqueous solution is added for multi-stage The countercurrent extraction was performed for 4 hours, and the extract was filtered. The filtrate was concentrated under vacuum (0.05-0.1MPa), and concentrated under reduced pressure at about 55°C to obtain 4.2 g of Eclipta prostrata extract crude product.

[0032] Take a glass chromatographic column with a column length of 450mm and an inner diameter of 45mm, and install 250ml of DM301 macroporous adsorption resin. Load the crude extract of Eclipta prostrata on the top of the column, and then use the mobile phase 50% and 60% respectively. , 70%, 80%, 90% ethanol-water solution for gradient elution, TLC plate tracking, concentration under vacuum (0.05-0.1MPa), with...

Example Embodiment

[0033] Embodiment three:

[0034] The Eclipta prostrata medicinal materials are crushed into 40-60 mesh Eclipta protea powder, 150 grams of Eclipta protea powder are weighed, and put into a multi-stage countercurrent extraction device, and then 1500ml of 80% ethanol-glycine aqueous solution is added to the room temperature. Stage countercurrent extraction for 6 hours, take out the extract and filter, the filtrate is concentrated under vacuum (0.05-0.1MPa), and concentrated under reduced pressure at about 30°C to obtain 4.3 g of Eclipta prostrata extract crude product.

[0035] Take a glass chromatographic column with a column length of 450mm and an inner diameter of 45mm, install 350ml D101 macroporous adsorption resin, load the crude Eclipta prostrata extract on the top of the column, and then use the mobile phase 50% and 60% respectively , 70%, 80%, 90% ethanol-water solution for gradient elution, TLC plate tracking, concentration under vacuum (-0.6-0.1MPa), with absolute ethanol...

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Abstract

The invention discloses a method for preparing wedelolactone monomeric compounds extracted and purified from a traditional Chinese medicine eclipta. The method comprises the following steps: grinding the eclipta into powder, adding an alcohol-acid aqueous solution for performing multistage counter-current extraction, filtering the extracting solution, and performing vacuum concentration, thereby obtaining a coarse product of wedelolactone; separating and purifying by virtue of a macroporous resin, performing gradient elute, collecting the eluent, and respectively performing vacuum concentration, thereby respectively obtaining wedelolactone and demethylwedelolactone. By utilizing good and stable physico-chemical properties of wedelolactone compounds under weak acid conditions, the active ingredients of the eclipta are protected in the process of extracting by using the alcohol-acid aqueous solution, the extraction rate of the active ingredients in the eclipta medicinal materials is greatly improved, the macroporous resin can be repeatedly utilized, an ethanol aqueous solution serves as a solvent and is economical and practical, high-purity wedelolactone and demethylwedelolactone compounds can be conveniently and efficiently obtained, the purity of each monomeric compound is over 95 percent, and the method is simple in process, easy and convenient to operate, low in cost and suitable for batch production.

Description

Technical field [0001] The invention relates, in particular, to a preparation method for extracting and purifying wedelia lactone and norwedewede lactone monomer compounds from Chinese medicine Eclipta prostrata, belonging to the technical field of traditional Chinese medicine phytochemistry. Background technique [0002] Eclipta prostrata, also known as Eclipta prostrata and Hogtooth grass, was first published in "Tang Materia Medica". It is the dry aerial part of Eclipta prostrata L. Cool in nature; sweet and sour in taste; in the liver and kidney channels. It has the effects of cooling blood, hemostasis, tonifying the kidney, and replenishing yin. It is mainly used in the clinical treatment of coronary heart disease and bleeding diseases. Modern pharmacological research shows that Eclipta prostrata has anti-tumor, immune regulation, anti-inflammatory and other pharmacological effects. It contains a variety of active molecules, such as triterpene saponins, flavonoids, thioph...

Claims

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Application Information

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IPC IPC(8): C07D493/04
CPCC07D493/04
Inventor 徐德锋
Owner THE FIRST AFFILIATED HOSPITAL OF MEDICAL COLLEGE OF XIAN JIAOTONG UNIV
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