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Preparation method of tricin

A technology of alfalfa and alfalfa, applied in the production of bulk chemicals, organic chemistry, etc., can solve the problems of long preparation period, less preparation amount, and large amount of solvent usage, and achieve large processing capacity, easy operation, and high purity Effect

Inactive Publication Date: 2011-11-16
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

As disclosed by Zhang Rui et al. "Preparation of a method for preparing alfalfa from bamboo roots by high performance liquid chromatography", the method used in this document is to extract with ethanol, add water to disperse after concentration, and then extract with ethyl acetate, and the extraction liquid reclaims ethyl acetate To dryness, perform silica gel column chromatography in a dry method, and finally prepare alfalfain by preparing high-efficiency liquid phase. Although this method produces a higher content of alfalfalin, the preparation cycle is long, and the amount of solvent used is large and the amount of preparation is small.

Method used

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  • Preparation method of tricin

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Embodiment 1

[0021] Get 1kg of alfalfa, crush it, add it to the extraction kettle, and use supercritical CO 2 For extraction, set the conditions of the extraction kettle as follows: the extraction temperature is 40°C, the extraction pressure is 25MPa, CO 2 The flow rate is 15L / h, the extraction time is 2.5h, and 100ml of ethanol is introduced as an entrainer to participate in the extraction. The conditions of the separation tank are set as follows: the temperature of the separation tank I is 30 ° C, the pressure is 8 MPa, the temperature of the separation tank II is 22 ° C, the pressure 5MPa, collect the alfalfa extract in the separation kettle II, dissolve it with an appropriate amount of ethanol, add 350g polyamide resin (80 mesh) to mix the sample, evaporate the solvent, pack the column, wash with 2BV water to remove impurities, and then use 3BV containing 1 90% ethanol solution of % hydrochloric acid was used for elution, the eluate was collected, concentrated to a small volume, left t...

Embodiment 2

[0023] Get 10kg of alfalfa, pulverize, add in the extraction kettle, adopt supercritical CO 2 For extraction, set the conditions of the extraction kettle as follows: the extraction temperature is 55°C, the extraction pressure is 35MPa, CO 2 The flow rate is 30L / h, the extraction time is 1h, and 2L of methanol is introduced as an entrainer to participate in the extraction. The conditions of the separation tank are set as follows: the temperature of the separation tank I is 40°C, the pressure is 10MPa, the temperature of the separation tank II is 30°C, and the pressure is 8MPa, collect the alfalfa extract in the separation kettle II, dissolve it with an appropriate amount of ethanol, add 6kg polyamide resin (120 mesh) to mix the sample, evaporate the solvent, pack the column, first wash away the impurities with 3BV water, and then use 7BV containing 1% The 70% ethanol solution of hydrochloric acid was eluted, the eluate was collected, concentrated to a small volume, left to crys...

Embodiment 3

[0025] Get 20kg of alfalfa, pulverize, add in the extraction kettle, adopt supercritical CO 2 For extraction, set the conditions of the extraction kettle as follows: the extraction temperature is 45°C, the extraction pressure is 30MPa, CO 2 The flow rate is 25L / h, the extraction time is 2h, and 3L of ethanol is introduced as an entrainer to participate in the extraction. The conditions of the separation tank are set as follows: the temperature of the separation tank I is 35°C, the pressure is 9MPa, the temperature of the separation tank II is 25°C, and the pressure is 6MPa, collect the alfalfa extract in the separation kettle II, dissolve it with an appropriate amount of ethanol, add 8kg polyamide resin (200 mesh) to mix the sample, evaporate the solvent, pack the column, first wash away the impurities with 4BV water, and then use 6BV containing 1% The 85% ethanol solution of hydrochloric acid was eluted, the eluent was collected, concentrated to a small volume, left to crysta...

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Abstract

The invention relates to a preparation method of tricin. The method comprises the following steps of: crushing lucerne serving as a raw material; adding the crushed lucerne into an extraction kettle; collecting a tricin extract by performing hypercritical CO2 extraction; dissolving with ethanol; adding polyamide resin for sample stirring; vaporizing a solvent; loading on a column; washing impurities away with water; eluting with acid alcohol; collecting an eluent; concentrating to a small volume; standing for crystallizing; and filtering crystals out and recrystallizing with ethyl acetate to obtain a tricin product. The method has the advantages of low energy consumption, short preparation period and high product purity.

Description

Technical field: [0001] The invention belongs to the field of natural product separation, in particular to a method using supercritical CO 2 A method for purifying alfalfa with extraction technology combined with polyamide resin. Background technique: [0002] Alfalfa Medicago sativa L. is a perennial leguminosa herbaceous plant. It is widely used as pasture all over the world. In my country, it is mainly distributed in the northwest, north, northeast and southwest regions. In our country, it is used to treat indigestion, lung heat cough, jaundice, bladder stones and other diseases. Modern medical research has found that alfalfa has the activities of lowering cholesterol and preventing coronary heart disease. Alfalfa mainly contains chemical components such as flavonoids, saponins, coumarins, sterols, monoterpenes and organic acids, among which flavonoids are the main functional component groups. [0003] Tricin, also known as wheat flavin and tricin, is one of the main ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30C07D311/40
CPCY02P20/54
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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