Preparation method for wedelolactone

Abstract

The invention provides a preparation method for wedelolactone. The method is characterized by comprising the following steps: smashing dry herba ecliptae medicinal herb; adding borated alkaline water the amount of which is 8-12 times of that of the smashed dry herba ecliptae medicinal herb, and carrying out ultrasonic extraction for 2-3 times; merging extracting solutions, extracting the merged solution with a macroporous resin column, collecting residual solution, and adding acid to regulate the pH value to 5-7; processing the collected solution with the macroporous resin column, washing with water until sugar reaction is negative, then eluting by utilizing high-concentration low carbon alcohol, and concentrating the eluent until no alcohol flavor exists; and extracting with ethyl acetate the amount of which is 2-3 times of that of the concentrated eluent for 1-3 times, evaporating the extraction liquid to dryness, and recrystallizing by utilizing methanol for 2-4 times, thus obtaining the product, namely the wedelolacton. The method provided by the invention has the advantages that the operation is simple, the preparation quantity is large, and the energy consumption in the production process is low, thereby having industrialization significance.

Description

Technical field: [0001] The invention belongs to the field of natural product separation, and particularly relates to a preparation method of wedelia lactone. Background technique: [0002] Herba Ecliptae (Herba Ecliptae) is the dry above-ground part of Channa intestines, commonly known as Ecliptae, which is commonly known as Ecliptae. It has the functions of nourishing liver and kidney, cooling blood and stopping bleeding. In recent years, studies at home and abroad have found that Eclipta alba has a strong liver protective effect. Pharmacological experiments show that its main pharmacologically active ingredient is Wedelia lactone, such as "Coumestants as the main active principles of the liver drugs Eclipta alba and wedelia" published by Wagner et al. Calendulacea", the literature study shows that wedelia lactone exhibits strong anti-hepatotoxicity and lower transaminase activity both in vivo and in vitro in rats. [0003] Wedelia lactones: Coumarol ethers, soluble in ethyl ace...

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Problems solved by technology

Such as Wu Hongxia's master's degree thesis "Research on Ecliptas quality evaluation method", the method adopted in this document is methanol immersion, the leachate is concentrated to extractum, water bath heating after water dispersion, filtered while hot, and the filtrate is extracted with ethyl acetate. The extract is recovered from ethyl acetate, concentrated to the extract, then applied to a silica gel column, eluted with chloroform-methanol (10:1), evaporated to dryness, and then recrystallized by methanol. This method has many steps, complicated operation, and repeated concentration. Large energy consumption, long methanol immersion cycle and small amount of preparation; for example, "Research on the Chemical Composition of Eclipta" published by Wu Jiang et al., the method disclosed in this document is 70% ethanol reflux extraction, and the extract is concentrated to no alcohol. Ethyl acetate extraction, the extract is separated and purified by silica gel column and SephadexLH-20 gel column respectively. This method obtains the product by repeated loading on the column. The preparation amount is small, the cycle is long, and the reflux process consumes a lot of energy

[0006] The preparation of wedelolide in existing patents mainly adopts the method of chemical total synthesis, which also has the defects of high synthesis cost and complicated production process. The present invention provides a method for naturally extracting wedelolide

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