Method for extracting wedelolactone from yerbadetajo herb

A technology of wedelolide and Eclipta chinensis, which is applied in the field of separation of natural products, can solve the problems of high synthesis cost, small preparation amount, cumbersome operation process, etc., and achieve the effect of short extraction period, low energy consumption and good separation effect

Inactive Publication Date: 2012-07-11
苏州宝泽堂医药科技有限公司
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  • Abstract
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  • Application Information

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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 ...

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0017] Take 1Kg of dried medicinal material of Eclipta chinensis, crush it through a 50-mesh sieve, add it to a supercritical extraction tank for extraction, set the extraction temperature to 60°C, and the extraction pressure to 30Mpa, and introduce CO 2 The flow rate is 22L / h. After the environment in the extraction tank is stable, add 100ml of absolute ethanol solution as an entrainer, extract for 3 hours, adjust the temperature of the first-stage separation ax to 45°C, the pressure to 8Mpa, and the temperature of the second-stage separation ax to 40°C , the pressure is 6Mpa, collect the analytical solution, extract twice with 120ml n-butanol, concentrate the extract to 30ml, mix the sample with 30g100-mesh polyamide resin, evaporate the n-butanol to dryness, put it on the polyamide resin column by dry method, and use 5BV The chloroform-absolute ethanol (8:1) solvent system was used for elution, and the elution rate was controlled at 1.5 BV / h. The eluate was collected and eva...

Embodiment 2

[0019] Take 1Kg of dried medicinal material of Eclipta chinensis, crush it through a 40-mesh sieve, add it to a supercritical extraction tank for extraction, set the extraction temperature to 65°C, and the extraction pressure to 25Mpa, and introduce CO 2 The flow rate is 20L / h. After the environment in the extraction tank is stable, add 120ml of absolute ethanol solution as an entrainer, extract for 2.5 hours, adjust the temperature of the first-stage separation ax to 50°C, the pressure to 9Mpa, and the temperature of the second-stage separation ax to 38°C , the pressure is 6Mpa, collect the analytical solution, extract 3 times with 100ml n-butanol, concentrate the extract to 40ml, mix the sample with 30g120 mesh polyamide resin, evaporate the n-butanol, dry the polyamide resin column, use 4BV The chloroform-absolute ethanol (8:1) solvent system was used for elution, and the elution rate was controlled at 2 BV / h. The eluate was collected and evaporated to dryness to obtain 1.31...

Embodiment 3

[0021] Take 2Kg of dried medicinal material of Eclipta chinensis, crush it through a 40-mesh sieve, add it to a supercritical extraction tank for extraction, set the extraction temperature to 50°C, and the extraction pressure to 35Mpa, and introduce CO 2 The flow rate is 24L / h. After the environment in the extraction tank is stable, add 280ml of absolute ethanol solution as an entrainer, extract for 3.5 hours, adjust the temperature of the first-stage separation ax to 40°C, the pressure to 9Mpa, and the temperature of the second-stage separation ax to 38°C , the pressure is 5.5Mpa, collect the analytical solution, extract twice with 300ml n-butanol, concentrate the extract to 60ml, mix the sample with 50g100-mesh polyamide resin, evaporate the n-butanol, dry the polyamide resin column, use 6BV The chloroform-absolute ethanol (8:1) solvent system was used for elution, and the elution rate was controlled at 2 BV / h. The eluate was collected and evaporated to dryness to obtain 3.28...

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Abstract

The invention relates to a method for extracting wedelolactone from yerbadetajo herb. The method comprises the following steps of: crushing dry yerbadetajo herb, putting the crushed dry yerbadetajo herb in a supercritical fluid extraction kettle for extraction, adding alcohol liquid as an entrainer, collecting analytical liquid, extracting for 2-3 times by using n-butyl alcohol, combining extract liquor, concentrating to be 1/15-1/8 of the original volume, stirring with a little amount of polyamide resin, leading the n-butyl alcohol to be volatilized completely, adopting a dry process for polyamide chromatographic columns, eluting by using a chloroform-absolute ethyl alcohol mixed-solvent system, collecting eluent, evaporating and obtaining a product. The method has the advantages that the operation is simple, the energy consumption is less, and the prepared product is good in quality and high in content.

Description

Technical field: [0001] The invention belongs to the field of separation of natural products, and in particular relates to a method for extracting wedelolide from Eclipta chinensis. Background technique: [0002] Eclipta prostrata L., commonly known as Eclipta prostrata L., is the dry aerial part of Eclipta prostrata L., a commonly used traditional Chinese medicine for treating liver diseases. According to the "Chinese Pharmacopoeia", it has the effects of nourishing the liver and kidney, cooling blood and stopping bleeding. Modern pharmacological studies have shown that Eclipta chinensis and its extracts have strong liver protection and expansion effects. [0003] Wedelolide: Coumarin, easily soluble in ethyl acetate, n-butanol, methanol, is a derivative of coumarins. It mainly exists in the leaves of Eclipta japonica. [0004] Wu Hongxia's master's degree thesis "Research on the Quality Evaluation Method of Eclipta chinensis" pointed out that the main hepatoprotective a...

Claims

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Application Information

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IPC IPC(8): C07D493/04
CPCY02P20/54
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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