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

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...

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 is concentrated and then acid-precipitated. After the acid solution is filtered, it is alkalized with ammonia water. The lye is extracted with chloroform. After the chloroform is recovered, it is recrystallized with acetone. The chloroform used in this method is costly and toxic. Large, large corrosion to the sealing ring of the equipment, easy to leak, difficult to dispose of recovered chloroform, difficult to separate chloroform in waste liquid, great environmental pollution, low content of tetrandrine produced, dark color, low melting point, and high cost , Severe organic residues

Tetrandrine extracted by the above two methods all use benzene and chloroform as the extraction solvent, and recrystallize with acetone. Such extraction methods all have residual toxic organic solvents, and it is difficult to combine with tetrandrine during the extraction process. Separation, thus affecting the purity of tetrandrine

In addition, there are no reports of tetrandrine extraction methods that do not use benzene and chloroform as solvents at home and abroad, and tetrandrine that does not contain benzene and chloroform