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Preparation method of homoeriodictyol-7-O-beta-D-glucoside

A technology of glucoside and homo-eriodin, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of low preparation yield, small preparation amount, complicated operation, etc., and achieve high product content , loss reduction, simple operation effect

Inactive Publication Date: 2013-02-06
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 existing solid-packed column chromatographic separation has technical defects such as low preparation yield, small preparation amount, and complicated operation.

Method used

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  • Preparation method of homoeriodictyol-7-O-beta-D-glucoside

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Grind mistletoe medicinal material, take 2kg, add 16L of 60% ethanol solution for microwave extraction twice, each time for 1 hour, combine the extracts after concentration and alcohol-free, add to 1LHZ816 macroporous resin column for adsorption, elute with 5 times the amount of 30% ethanol, collect After the eluate was concentrated, the pH2 was adjusted with hydrochloric acid, filtered, the filtrate was extracted three times with an equal volume of ethyl acetate, and the extract was concentrated to obtain a crude extract. Take chloroform, methanol, and water and mix them fully in a separatory funnel at a ratio of 3:4:2. After standing for stratification, take the lower phase and fill it with a high-speed countercurrent chromatographic column. Turn the main engine at a speed of 700 rpm and pump the upper phase into the mobile phase. After equilibrium, the flow rate of the mobile phase was adjusted to 2ml / min. At the same time, the crude product was dissolved in the upper...

Embodiment 2

[0018] Grind mistletoe medicinal material, take 2kg, add 6L 80% ethanol solution for microwave extraction twice, each time for 1 hour, combine the extracts and concentrate without alcohol, add 1L ADS-21 macroporous resin column for adsorption, wash with 3 times the amount of 50% ethanol After the eluate was collected and concentrated, it was adjusted to pH3 with hydrochloric acid, filtered, and the filtrate was extracted three times with an equal volume of ethyl acetate, and the extract was concentrated to obtain a crude extract. Take chloroform, methanol, and water and mix them fully in a separatory funnel at a ratio of 4:6:3. After standing for stratification, take the lower phase and fill it with a high-speed countercurrent chromatographic column. Turn the host at a speed of 900 rpm, and pump the upper phase into the mobile phase. After equilibrium, the flow rate of the mobile phase was adjusted to 3ml / min. At the same time, the crude product was dissolved in the upper phase...

Embodiment 3

[0020] Grind mistletoe medicinal material, take 2kg, add 5L of 75% ethanol solution for microwave extraction for 3 times, each time for 1 hour, combine the extracts after concentration and alcohol-free, add 1L NKA-9 macroporous resin column for adsorption, wash with 5 times the amount of 50% ethanol After the eluate was collected and concentrated, the pH2 was adjusted with hydrochloric acid, filtered, and the filtrate was extracted three times with an equal volume of ethyl acetate, and the extract was concentrated to obtain a crude extract. Take chloroform, methanol, and water and mix them fully in a separatory funnel at a ratio of 5:7:4. After standing for stratification, take the lower phase and fill it with a high-speed countercurrent chromatographic column, turn the main engine at a speed of 1000 rpm, and pump the upper phase into the mobile phase. After equilibrium, the flow rate of the mobile phase was adjusted to 4ml / min. At the same time, the crude product was dissolved...

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Abstract

The invention discloses a preparation method of homoeriodictyol-7-O-beta-D-glucoside. The method comprises the steps that: (1) a mistletoe medicine material is crushed; a 60-80% ethanol solution is added, and microwave extraction is carried out 2-3 times; an extraction liquid is concentrated until no alcohol is left; the extract is absorbed by using macroporous resin column; 30-50% ethanol is used for eluting; an obtained elution liquid is concentrated, and a pH value is regulated to 2-3; ethyl acetate is added for extraction, and the extraction liquid is concentrated, such that a crude extract is obtained; and (2) chloroform, methanol, and water are mixed and stratified; a lower-phase is used for filling a high-speed countercurrent chromatographic column; a main machine is rotated, and an upper-phase is pumped in as a mobile phase; the crude product dissolved by the mobile phase is fed by using a feeding valve, and is subjected to UV detector detecting; a target component is collected according to a spectrum; and a fraction is subjected to reduced-pressure drying, such that the homoeriodictyol-7-O-beta-D-glucoside is obtained. The method provided by the invention has the advantages of simple operation, large preparation amount, high yield, and suitability for industrialized productions.

Description

technical field [0001] The present invention relates to a preparation method of homoeroticin-7-O-β-D-glucoside, in particular to a method for preparing homoeroticin-7-O-β-D-glucoside by using high-speed countercurrent chromatography method. Background technique [0002] Homoeridin-7-O-β-D-glucoside is a dihydroflavone glycoside compound, melting point: 158-160°C, easily soluble in acetone, soluble in methanol, ethanol, water, insoluble in chloroform, petroleum ether . Molecular formula: C 22 h 2 o 11 , molecular weight: 464, molecular structure: [0003] [0004] Mistletoe is also known as northern parasite, holly, mulberry parasite, willow parasite, yellow parasite, frozen green, and parasite. It usually parasitizes trees in the genus Quercus, Apple, Poplar, and Pinus. Modern studies have shown that mistletoe contains a large amount of flavonoids, alkaloids, and terpenoids, which have effects on the cardiovascular system, anti-platelet aggregation, and anti-tumor e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08
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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