Method for separating and preparing tetrandrine and hanfangchin through ion exchange and column chromatography on silica gel

A technology of silica gel column chromatography and tetrandrine, which is applied in the direction of organic chemistry, can solve problems such as easy residue, large environmental pollution, and difficult to handle chloroform, so as to avoid the use of toxic solvents, reduce production costs, and facilitate scale-up production Effect

Active Publication Date: 2017-06-13
CSPC JIANGXI GOLDEN LOTUS PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when tetrandrine is used as medicine, especially when used as an injection, it must have a relatively high purity, which is generally required to reach more than 99%, and must not contain other impurities such as benzene and chloroform, which makes high-purity tetrandrine Vegetarian raw materials are in short supply, which is far from meeting the needs of preparation production
At present, there are two main extraction techniques for tetrandrine in China: one is the cold benzene method, the basic process is to use ethanol as the solvent for reflux extraction, the extract is concentrated and then added with lime for precipitation, and the precipitate is extracted by cold immersion in benzene, and after recovery of benzene , recrystallized with ethanol, the benzene used in this method is extremely toxic, easy to remain, harmful to the human body, unable to adapt to large-scale production, it is difficult to obtain tetrandrine that meets the medicinal requirements; the other is the chloroform extraction method, its The basic process is to use ethanol as a solvent for reflux extraction. The extract i

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. Take 1 kg of Fangji and grind it into coarse powder, add 4L of 85% ethanol for hot reflux extraction, filter the extract, concentrate the filtrate under reduced pressure until it has no alcohol smell, and obtain a liquid extract for later use;

[0027] 2. Dissolve the extract obtained in step 1 with 9L 0.5mol / L hydrochloric acid solution, adjust the pH value to 3, let it stand for 24 hours, filter, and filter the filtrate through the treated cation exchange 001×7 (cation exchange resin volume: Paste weight = 30ml: 1g), repeated loading 3 times;

[0028] 3. Use 5BV deionized pure water, 5BV 60% ethanol, 5BV 0.5 mol / L ammonia 75% ethanol solution, 5BV 2.0mol / L ammonia 90% ethanol solution, and collect 2.0 mol / L ammonia 90% ethanol solution eluate ;

[0029] 4. The above-mentioned eluent in step 3 is recovered under reduced pressure to ethanol, suspended in water, filtered, and the filter residue is washed with deionized water to obtain a crude alkaloid extract;

[00...

Embodiment 2

[0034] 1. Take 1 kg of Fangji and grind it into coarse powder, add 4L of 85% ethanol for hot reflux extraction, filter the extract, concentrate the filtrate under reduced pressure until it has no alcohol smell, and obtain a liquid extract for later use;

[0035] 2. Dissolve the extract obtained in step 1 with 9L 0.5mol / L hydrochloric acid solution, adjust the pH value to 3, let it stand for 24 hours, filter, and filter the filtrate through the treated cation exchange 001×4 (cation exchange resin volume: Paste weight = 30ml: 1g), repeated loading 3 times;

[0036] 3. Use 5BV deionized pure water, 5BV 60% ethanol, 5BV 0.5 mol / L ammonia 75% ethanol solution, 5BV 2.0mol / L ammonia 90% ethanol solution, and collect 2.0 mol / L ammonia 90% ethanol solution eluate ;

[0037] 4. The above-mentioned eluent in step 3 is recovered under reduced pressure to ethanol, suspended in water, filtered, and the filter residue is washed with deionized water to obtain a crude alkaloid extract;

[00...

Embodiment 3

[0042] 1. Take 1 kg of Fangji and grind it into coarse powder, add 4L of 85% ethanol for hot reflux extraction, filter the extract, concentrate the filtrate under reduced pressure until it has no alcohol smell, and obtain a liquid extract for later use;

[0043] 2. Dissolve the extract obtained in step 1 with 9L 0.5mol / L hydrochloric acid solution, adjust the pH value to 3, let it stand for 24 hours, filter, and the filtrate has been treated with cation exchange D001 (cation exchange resin dosage volume: extract weight =30ml: 1g), repeated loading 3 times;

[0044] 3. Use 5BV deionized pure water, 5BV 60% ethanol, 5BV 0.5 mol / L ammonia water 75% ethanol solution, 5BV 2.0 mol / L ammonia water 90% ethanol solution, and collect 2.0 mol / L ammonia water 90% ethanol solution to wash Dehydration;

[0045] 4. The above-mentioned eluent in step 3 is recovered under reduced pressure to ethanol, suspended in water, filtered, and the filter residue is washed with deionized water to obtain...

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Abstract

The invention relates to a method for separating and preparing tetrandrine and hanfangchin through ion exchange and column chromatography on silica gel. Fourstamen stephania root is dried root of a menispermaceae stephania plant stephania tetrandra, an effective ingredient of the fourstamen stephania root is sinomenine, main effective ingredients of sinomenine are tetrandrine and hanfangchin, and the sinomenine has anti-myocardial ischemia, anti-arrhythmia, blood pressure lowering, anti-inflammatory, anti-silicosis, anti-cancer and analgesic effects. When in drug use, the purity requirement of the tetrandrine and hanfangchin reaches more than 99%, and extraction and purification are important reasons limiting the drug use of the tetrandrine and hanfangchin. At present, a technology for extracting and purifying the tetrandrine and hanfangchin applies massive toxic and expensive chloroform and strong base, and the chloroform has great toxic effect on human and the environment and is also strong corrosive on equipment for enlarged production; besides, sample purity is not high, and a technological process is complex. At the current situation, the invention develops a method for obtaining high-purity tetrandrine and hanfangchin through rapid separation and purification by applying ion exchange resin and a C18 bonded silica gel column chromatography and also discloses a method for recrystallizing and purifying the tetrandrine and hanfangchin by utilizing ethyl alcohol. The method provided by the invention has the advantages that a preparation technology does not apply any toxic reagent, column chromatography filler can be recycled, and ethyl alcohol can be recycled.

Description

technical field [0001] The invention relates to a method for separating and preparing active ingredients from traditional Chinese medicines, belonging to the field of traditional Chinese medicines. As a kind of using ion exchange resin and reverse phase C 18 A method for rapidly preparing tetrandrine and tetrandrine simultaneously by bonded silica gel column chromatography. Background technique [0002] Tetrandrine is an alkaloid extracted from the traditional Chinese medicine Fangji. Pharmacological studies in recent years have shown that tetrandrine has anti-myocardial ischemia, anti-arrhythmia, anti-hypertensive, anti-inflammation, anti-silicosis, anti-cancer and analgesic effects. Tablets have been widely used clinically. However, when tetrandrine is used as medicine, especially when used as an injection, it must have a relatively high purity, which is generally required to reach more than 99%, and must not contain other impurities such as benzene and chloroform, whic...

Claims

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Application Information

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IPC IPC(8): C07D491/18
CPCC07D491/18
Inventor 邓胜杨燕欢郜杰
Owner CSPC JIANGXI GOLDEN LOTUS PHARMA CO LTD
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