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A kind of dihydroxyphenylethanol glucoside compound and its preparation method

A technology of dihydroxyphenylethanol and glucoside, which is applied in the field of phenylethanol glycosides to achieve the effects of good reproducibility, stable preparation performance and high sample purity

Inactive Publication Date: 2011-12-07
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far there is no report about 2,5-dihydroxyphenylethanol glycosides

Method used

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  • A kind of dihydroxyphenylethanol glucoside compound and its preparation method
  • A kind of dihydroxyphenylethanol glucoside compound and its preparation method
  • A kind of dihydroxyphenylethanol glucoside compound and its preparation method

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Experimental program
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Effect test

Embodiment 1

[0021] Forsythia raw medicinal material was crushed, weighed 1 kg, placed in a 50 liter extraction tank, decocted with 10 liters of water for 2 hours, filtered, and the filtrate was stored for later use. Add 10 liters of water to the filter residue and decocted for 2 hours, filtered, and the filtrate Combine this time and discard the filter residue. Rotary evaporation of the filtrate to obtain 190ml of extract (relative density 1.05). The extract was dissolved in an equal volume of water, added with 653 ml of 95% ethanol, stirred, allowed to stand for 24 hours, filtered, and the filter residue was discarded. The filtrate was concentrated until no alcohol smell, and 142 ml of forsythia alcohol precipitation fraction was obtained.

[0022] The forsythia alcohol precipitation component was made up to 200 ml with water, and 28.4 g of sodium bicarbonate was added, stirred, reacted for 3 hours, and left overnight. Gradually add 56.8 ml of 1:1 hydrochloric acid and 1.4 ml of 1:2 hydroc...

Embodiment 2

[0036] Forsythia raw medicinal materials were crushed, weighed 3 kg, placed in a 100 liter extraction tank, decocted with 30 liters of water for 2 hours, filtered, and the filtrate was stored for later use. Add 30 liters of water to the filter residue and decocted for 2 hours. Combine this time and discard the filter residue. Rotary evaporation of the filtrate to obtain 570ml of extract (relative density 1.05). The extract was dissolved in an equal volume of water, added with 1959 ml of 95% ethanol, stirred, allowed to stand for 24 hours, filtered, and the filter residue was discarded. The filtrate was concentrated until there was no alcohol smell to obtain 426 ml of forsythia alcohol precipitation fraction.

[0037] The forsythia alcohol precipitation component was made up to 600 ml with water, 85.2 g of sodium bicarbonate was added, stirred, reacted for 3 hours, and left overnight. Gradually add 170.4 ml of 1:1 hydrochloric acid and 4.1 ml of 1:2 hydrochloric acid (the pH is a...

Embodiment 3

[0042] Forsythia raw medicinal materials were crushed, weighed 6.8 kg, placed in a 100 liter extraction tank, decocted with 68 liters of water for 2 hours, filtered, and the filtrate was stored for later use. Add 68 liters of water to the filter residue and decocted for 2 hours. Combine this time and discard the filter residue. The filtrate was rotary evaporated to obtain 1292ml of extract (relative density 1.05). The extract was dissolved in an equal volume of water, added 4.44 liters of 95% ethanol, stirred, allowed to stand for 24 hours, filtered, and the filter residue was discarded. The filtrate was concentrated until there was no alcohol smell to obtain 966 ml of forsythia alcohol precipitation.

[0043] The forsythia alcohol precipitation component was made up to 1.36 liters with water, and 193 g of sodium bicarbonate was added, stirred, reacted for 3 hours, and left overnight. Gradually add 386 ml of 1:1 hydrochloric acid and 9.3 ml of 1:2 hydrochloric acid (the pH is ab...

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Abstract

The invention discloses a method for preparing a new compound of dihydroxyphenethyl glucoside from traditional Chinese medicine Forsythia through acid-base treatment and chromatographic separation technology. The compound is systematically named 1-(2,5-dihydroxy)phenethyl- β-D-glucopyranoside. The main process steps are pulverizing the traditional Chinese medicine Forsythia suspensa, decocting and extracting in water, ethanol precipitation, adding a certain amount of sodium bicarbonate or sodium carbonate, reacting, adjusting the pH value to 2-3, and rotary evaporation to obtain the extract; Further isolation gave this compound. The invention is a preparation method of a new compound of (2,5-dihydroxy) phenethyl glucoside with high purity, good reproducibility and short cycle. It is used for the preparation of standard compounds of phenethyl alcohol glycosides and further study of their pharmacological activities.

Description

Technical field [0001] The present invention relates to phenylethanol glycoside compounds, in particular to a new dihydroxyphenylethanol glucoside compound and its preparation and separation method. It is a preparation and separation method from traditional Chinese medicine Forsythia by acid-base treatment and chromatographic separation technology New compounds coming out. Background technique [0002] Phenylethanol glycoside compounds have anti-inflammatory, antibacterial, antiviral, anti-oxidant, and memory-enhancing effects (Jinghui et al. Lishizhen Traditional Chinese Medicine and Materia Medica. 2006, 17(3): 440; Park Jinghua et al. Chinese Pharmacological Bulletin. 2001, 17(6): 625; Hu Kejie et al. Chinese Journal of Traditional Chinese Medicine. 2001, 8(2): 89). [0003] Six phenethyl glycoside compounds have been isolated and identified from the roots of Phu Huanglian in Wang Haoyu (Wang Hao et al. Chinese Traditional Medicine Impurities. 2004, 29(6): 531); Zheng Xiaoke ha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/18
Inventor 梁鑫淼王亚琴丰加涛
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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