Method for preparing tetrandrine alkaloids by coupling in-situ conversion-adsorptive separation technology

Abstract

The invention relates to a method for preparing tetrandrine alkaloids by coupling in-situ conversion-adsorptive separation technology, and the preparation process comprises: 1) tetrandrine raw drug is ground and soaked into ethanol water solution for heat preservation and agitation. After the mixed solution is filtered, filtrate is processed by reduced pressure distillation, and ethanol is recovered; acetic acid water solution is added into the processed filtrate which is then filtered, ammonia water is used for adjusting the pH value of the filtrate to be within the range of 10-12, and precipitate is separated out; the obtained precipitate is dissolved into the acetic acid water solution and centrifugated, and supernate is collected and called as adsorption solution for short; 2) after the adsorption solution with the quantity being 3-5 times of bed volume is absorbed by resin column, a resin bed layer is washed by a great quantity of deionized water, and then the tetrandrine alkaloids extract is obtained by the steps such as using the ammonia water to pass through the resin column, etc. In the preparation process, noxious solvent is not used, and other solvents are consumed in a small quantity; meanwhile, resin is not needed to be processed by acid-alkali regeneration after the extraction period of every time, so that the operation technique is greatly simplified, the resin can be reused, a great deal of resources can be saved, the extraction efficiency is improved, and the method is suitable for industrialized large-scale production. The prepared tetrandrine alkaloids have the purity being higher than 70% and the yield being higher than 95%.

Description

【Technical Field】: [0001] The invention relates to the technical field of extraction and separation of effective components of traditional Chinese medicine, in particular to a method for preparing total alkaloids of tetrandrine by in situ conversion-adsorption separation technology combined. 【Background technique】: [0002] Tetrandrine is the root of Stephania tetrandra S.Moore, a plant of the genus Stephania tetrandra S. Moore in the tetrandrine family. It has a long history of clinical use in my country. The main active ingredient is alkaloids, such as tetrandrine (also known as tetrandrine). ), fangchinoline (also known as tetrandrine, demethyltetrandrine), methyl tetrandrine, diberberamine, ring cylinol and so on. Among them, tetrandrine A and tetrandrine B have the highest content, and they are also the main medicinal ingredients in tetrandrine. [0003] The plant of the genus Stephania has long been anti-cancer in our country. Among them, tetrandrine has a preventive effect...

AI Technical Summary

Problems solved by technology

This method has the following main problems: 1) most processes in the extraction need to use a large amount of highly toxic solvents such as benzene and chloroform in an open environment, which is very harmful to operators and the environment; 2) the sample loss is more during activated carbon decolorization; 3 ) method is complicated, operability is poor, and production cost is higher

Wang Mingkui etc. disclose a kind of method (Wang Mingkui, Cui Wenfeng, Bao Ling, Li Fu, the preparation technology of Tetany alkaloids, Chinese invention patent, CN 101288695A) utilizing ion exchange resin to prepare high-purity tetrandrine alkaloids, but in this method The ion exchange resin D72 used needs to be repeatedly treated with acid and alkali after each process is completed to regenerate it before it can be used in the next service cycle. , The generation of alkali-containing wastewater makes the advantages of the resin lost