Method for separating and preparing epigoitrin

A technology for reporting Yichun and ethanol, applied in the field of separation of natural medicines, can solve the problems of inability to large-scale production, low degree of automation, backward detection methods, etc., and is suitable for large-scale industrial production, with good reproducibility, The effect of small residues of organic solvents

Active Publication Date: 2008-10-22
浙江华谱新创科技有限公司
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

The reports on the extraction and separation preparation of Biaobao Yichun in the literature basically adopt methods such as traditional solvent extraction such as hexane and methylene chloride, silica gel column chromatography, and alumina column chromatography (Liu Haili et al. Shenyang Pharmaceutical Sciences) University Journal, 2002, 19(2)...

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  • Method for separating and preparing epigoitrin
  • Method for separating and preparing epigoitrin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Grind the original medicinal material of Radix isatidis, weigh 2 kg quantitatively, put it in a 50-liter extraction tank, add 20 liters of water to decoct for 2 hours, filter, and save the filtrate for later use, add 20 liters of water to the filter residue and decoct for 2 hours, filter, and the filtrate and the second Once combined, the filter residue was discarded. Concentrate the extract by rotary evaporation to 1000 ml to obtain the extract fraction of Yichun. Add 1750 ml of 95% ethanol to the extract, stir well, refrigerate and stand at 0°C for 24 hours, filter, discard the filter residue, concentrate the filtrate to 500 ml, add 2600 ml of 95% ethanol to the concentrate, stir well, set aside at 0°C Refrigerate and stand for 24 hours, filter, discard the filter residue, concentrate the filtrate until it has no alcohol smell, and the concentrate is centrifuged in a high-speed centrifuge (20,000 rpm) to obtain 600 ml of the alcohol-precipitated fraction of echun.

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Embodiment 2

[0029]Grind the original medicinal material of Radix isatidis, weigh 0.5 kg quantitatively, put it in a 20-liter extraction tank, add 5 liters of water to decoct for 2 hours, filter, and save the filtrate for later use, add 5 liters of water to the filter residue and decoct for 2 hours, filter, and the filtrate and the second Once combined, the filter residue was discarded. The extract was concentrated by rotary evaporation to 250 ml to obtain the extract fraction of Yichun. Add 440 ml of 95% ethanol to the extract, stir well, refrigerate at 0°C for 24 hours, filter, discard the filter residue, concentrate the filtrate to 150 ml, add 800 ml of 95% ethanol to the concentrated solution, stir well, set aside at 0°C Refrigerate and stand for 24 hours, filter, discard the filter residue, concentrate the filtrate until it has no alcohol smell, and the concentrate is centrifuged in a high-speed centrifuge (20,000 rpm) to obtain 200 ml of echun alcohol precipitation fraction.

[0030...

Embodiment 3

[0033] Pulverize the original medicinal material of Radix isatidis, weigh 5 kg quantitatively, put it in a 100-liter extraction tank, add 50 liters of water to decoct for 2 hours, filter, and save the filtrate for later use, add 50 liters of water to the filter residue and decoct for 2 hours, filter, and the filtrate and the second Once combined, the filter residue was discarded. The extract was concentrated by rotary evaporation to 2500 ml to obtain the extract fraction of Yichun. Add 4400 ml of 95% ethanol to the extract, stir well, refrigerate at 0°C for 24 hours, filter, discard the filter residue, concentrate the filtrate to 1500 ml, add 8 liters of 95% ethanol to the concentrated solution, stir well, and set aside at 0°C Refrigerate and stand for 24 hours, filter, discard the filter residue, concentrate the filtrate until it has no alcohol smell, and the concentrated solution is centrifuged in a high-speed centrifuge (20000 rpm) to obtain 1.8 liters of echun alcohol prec...

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Abstract

The invention relates to separation of natural medicines, in particular to a preparation method for separating an epigoitrin. After being ground, radix isatidis plants are decocted in 8 to 12 volumes of water to obtain the extract; then the extract group is obtained by concentration; ethanol is added to precipitate twice; the supernatant fluid above the alcohol precipitation is concentrated; the ethanol is recycled; the concentrated solution is filtered by a high speed centrifuge; the filtrate is separated by a membrane separator; the transmission fluid is chromatograph zed, separated and prepared through a macroporous resin column; the water ethanol is gradient eluted to obtain components and then to be separated and prepared by a highly efficient industrial chromatography column; the water methanol is gradient eluted to collect the eluent; and the epigoitrin is obtained by concentrating, freezing and drying the eluent. The products of the invention which is high in purity, large in preparation amount and reliable and stable in technique is especially suitable for separating and preparing a large amount of the epigoitrin compounds with the high purity from Chinese radix isatidis.

Description

technical field [0001] The present invention relates to the separation of natural medicines, in particular to a method for separating and preparing yichun, which is a preparation method for separating yichun from traditional Chinese medicine Radix Isatidis through industrial chromatographic technology. Background technique [0002] Isatis root is a traditional Chinese medicine. "Pharmacopoeia of the People's Republic of China" (2000 edition) stipulates that it is the dried root of Isatis indigotica Fort., a cruciferous plant. It was first recorded in "Shen Nong's Herbal Classic". Pharyngeal function, commonly used clinically for viral and bacterial infectious diseases. Banlangen has varying degrees of inhibitory effects on influenza virus, hemorrhagic fever with renal syndrome virus (HFRSV), Japanese encephalitis virus, mumps virus, herpes simplex virus, hepatitis B virus and Coxsackie B4 virus (Li Ling et al. . Acta Pharmaceutica Sinica, 1994, 29(2): 128-131; Zhang Chenhao...

Claims

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Application Information

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IPC IPC(8): C07D263/16A61K36/315A61K125/00
Inventor 梁鑫淼丰加涛徐青薛兴亚
Owner 浙江华谱新创科技有限公司
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