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Preparation process for formononetin with high purity

A kind of formononetin, technology of preparation process

Inactive Publication Date: 2012-07-04
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The column chromatography adsorption capacity of this method is small, the resolution rate is low, and each monomeric isoflavone is not separated
[0005] Chinese patent (application number 200610031716.3) "Preparation method of red clover extract" adopts the aerial part of red clover in a fresh state, after alcohol extraction, concentration, and standing, the obtained precipitate is dried to obtain red clover Grass extract, the method is simple in process, low in yield, low in product purity, and poor in specificity
This method is the preparation of total isoflavones, and monomer products cannot be obtained

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Grind red clover herb, take 1kg, use 3L of 80% ethanol solution, microwave-assisted ultrasonic extraction twice, each time for 1h, microwave power is 30W, ultrasonic frequency is 25KHz, filter, combine extracts, concentrate without alcohol smell , add water to suspend, extract with ethyl acetate, get the extract after desolventizing the extract, use 5% NaCO 3 Dissolve the solution, filter out the insoluble matter, add 1mol / L hydrochloric acid to the filtrate until no precipitation occurs, filter, dissolve the precipitate with an appropriate amount of methanol, add an appropriate amount of macroporous resin, stir evenly, install it on the top of 1LHPD-100 macroporous resin, and use 5L of water, 4L of 10%, 4L of 30%, 4L of 55%, and 3L of 70% ethanol solution for eluting, collecting the eluate, concentrating, placing the crystals, filtering out the crystals and refluxing with ethanol to dissolve them, letting the crystals cool down, filtering out the crystals and drying the...

Embodiment 2

[0024] Grind the red clover herb, take 1kg, use 8 times the amount of 85% ethanol solution, microwave-assisted ultrasonic extraction once, each time 1.5h, microwave power is 30W, ultrasonic frequency is 25KHz, filter, combine extracts, concentrate No alcohol smell, add water to suspend, extract with ethyl acetate, get the extract after desolventizing the extract, use 5% NaCO 3 Dissolve the solution, filter out insoluble matter, add 0.5mol / L sulfuric acid to the filtrate until no precipitation occurs, filter, dissolve the precipitate with an appropriate amount of methanol, add an appropriate amount of macroporous resin, stir evenly, install on the top of 1LS-8 macroporous resin, and then Use 5L water, 4L 20%, 4L 45%, 4L 60%, 4L 75% ethanol solution to elute, collect the eluent, concentrate, place crystals, filter out crystals and dissolve them in ethanol reflux, let cool crystals, filter out crystals and dry to obtain thorn 3.6g of pedicelin, the content is 98.4%.

Embodiment 3

[0026] Grind the red clover herb, take 1kg, use 5 times the amount of 90% ethanol solution, microwave-assisted ultrasonic extraction once, each time 2h, microwave power is 30W, ultrasonic frequency is 25KHz, filter, combine extracts, concentrate without Alcoholic taste, add water to suspend, extract with ethyl acetate, get the extract after desolventizing the extract, use 5% NaCO 3 Dissolve the solution, filter out the insoluble matter, add 1mol / L hydrochloric acid to the filtrate until no precipitation occurs, filter, dissolve the precipitate with an appropriate amount of methanol, add an appropriate amount of macroporous resin, stir evenly, install it on the top of 1LS-8 macroporous resin, and use Elute with 5L water, 5L10, 5L40%, 3L65%, 3L80% ethanol solution, collect the eluate, concentrate, place crystals, filter crystals and dissolve them with ethanol reflux, let cold crystals, filter crystals and dry to obtain Formonibus sinensis Su 4.2g, the content is 97.8%.

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PUM

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Abstract

The invention relates to a preparation process for formononetin with high purity. The method is characterized in comprising the steps of using ethanol water solution as a solvent, carrying out ultrasonic-assisted extraction under the assist of microwaves, concentrating extraction liquid until alcohol smell disappears, adding ethyl acetate for extraction, carrying out desolvation on extraction liquid to obtain extract, dissolving the extract with 5% NaCO3 solution, filtering, precipitating with acid to obtain precipitate, dissolving the precipitate with methanol, purifying with macroporous resin, and then eluting with water and ethanol solution with different concentrations, concentrating eluent and crystallizing, filtering, recrystallizing with ethanol, and then drying crystal to obtain the product. A compound extracted by the method opens a new way for developing and applying new generation of antineoplastic agents with natural resources.

Description

Technical field: [0001] The invention belongs to the field of natural plant extraction and relates to a preparation process of high-purity formononetin. Background technique: [0002] Red clover is the inflorescence and flowering branches and leaves of leguminous plant red clover, which has the effects of antispasmodic, cough and asthma. The whole plant contains formononetin, genistein, daidzein, red clover root, red clover and other isoflavones. [0003] Formononetin, 7-hydroxy-4'-methoxyisoflavone, formononetin, easily soluble in methanol, ethyl acetate, ether, dilute alkali solution, hardly soluble in water. It has anti-cancer effect and can prevent breast cancer, prostate cancer and colon cancer. It has the effect of estrogen, and can increase the weight of the uterus of mice and other animals. In addition, it has the effect of lowering blood lipids on the hyperlipidemia of male albino rats caused by TritonWR-1339, regulating blood lipid metabolism and improving athero...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/36C07D311/40
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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