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A preparation method for extracting wedelia lactone monomer compound from Eclipta chinensis

A technology in Werethrin and Werethrin, which is applied in directions such as organic chemistry, can solve the problems of high production cost, many operation procedures, low proportion of the Werethrin-based monomer compound, etc., and achieves low cost, simple process, and improved extraction rate. Effect

Active Publication Date: 2016-05-25
THE FIRST AFFILIATED HOSPITAL OF MEDICAL COLLEGE OF XIAN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • 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, the proportion of available wedelide monomer compounds is low, and the production cost is high. Technical problems

Method used

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  • A preparation method for extracting wedelia lactone monomer compound from Eclipta chinensis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Crush the Eclipta medicinal material into 40-60 mesh Eclipta powder, weigh 150 grams of Eclipta powder, put it into a multi-stage countercurrent extraction device, and then add 1500ml of 80% ethanol-acetic acid aqueous solution for countercurrent extraction for 5 hours , filtered after extraction, concentrated under vacuum (0.05-0.1MPa), and concentrated under reduced pressure at about 50°C to obtain 4.5 grams of crude Eclipta chinensis extract.

[0024] Get column length and be 450mm, inner diameter is the glass chromatographic column of 45mm, dress 350mlD101 macroporous adsorption resin, the above-mentioned Eclipta chinensis extract crude product is loaded on the chromatographic column column top, then use mobile phase 50%, 60%, respectively 70%, 80%, 90% ethanol-water solution for gradient elution, followed by TLC plate, concentrated under vacuum (0.05-0.1MPa), carried water with absolute ethanol, and recrystallized the obtained solid with methanol to obtain 103mg res...

Embodiment 2

[0031] Crush the Eclipta medicinal material into 40-60 mesh Eclipta powder, weigh 150 grams of Eclipta powder, put it into a multistage countercurrent extraction device, add 80% methanol-phosphoric acid aqueous solution of 1500ml, and carry out multistage Countercurrent extraction for 4 hours, the extract was filtered, the filtrate was concentrated under vacuum (0.05-0.1 MPa), and concentrated under reduced pressure at about 55° C. to obtain 4.2 grams of crude Eclipta officinalis extract.

[0032] Get column length and be 450mm, internal diameter is the glass chromatographic column of 45mm, dress 250mlDM301 macroporous adsorption resin, the above-mentioned Eclipta chinensis extract crude product is loaded on the chromatographic column column top, then respectively use mobile phase 50%, 60%, 70%, 80%, 90% ethanol-water solution for gradient elution, followed by TLC plate, concentrated under vacuum (0.05-0.1MPa), carried water with absolute ethanol, and recrystallized the obtaine...

Embodiment 3

[0034] The Eclipta medicinal material is crushed into 40-60 mesh Eclipta powder, 150 grams of Eclipta powder is weighed, packed into a multi-stage countercurrent extraction device, and then 1500ml of 80% ethanol-glycine aqueous solution is added to carry out multiple extraction at room temperature. Stage countercurrent extraction for 6 hours, the extract was taken out and filtered, the filtrate was concentrated under vacuum (0.05-0.1 MPa), and concentrated under reduced pressure at about 30° C. to obtain 4.3 grams of crude Eclipta chinensis extract.

[0035] Get column length and be 450mm, inner diameter is the glass chromatographic column of 45mm, dress 350mlD101 macroporous adsorption resin, the above-mentioned Eclipta chinensis extract crude product is loaded on the chromatographic column column top, then use mobile phase 50%, 60%, respectively 70%, 80%, 90% ethanol-water solution for gradient elution, followed by TLC plate, concentrated under vacuum (-0.6-0.1MPa), carried w...

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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 wedelide and norwedelide monomer compounds from the traditional Chinese medicine Eclipta chinensis, belonging to the technical field of traditional Chinese medicine phytochemistry. Background technique [0002] Eclipta, also known as Eclipta, pigtooth grass, was first recorded in "Tang Materia Medica". Dried aerial part of Channa prostrata L. of Compositae. Cool in nature; sweet and sour in taste; returns to liver and kidney channels. It has the effects of cooling blood, stopping bleeding, nourishing the kidney, and benefiting yin. It is mainly used for the treatment of coronary heart disease and hemorrhagic diseases in clinical practice. Modern pharmacological studies have shown that Eclipta has pharmacological effects such as anti-tumor, immune regulation, and anti-inflammation. It contains a variety of active molecules, such as triterpenoid saponins, flavon...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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