Process for producing high purity matrine oxide by kuh-seng

Abstract

The invention relates to a method to make oxymatrine from kuhseng that includes the following steps: mixing kuhseng raw material with alcohol acid solution or alkali solution, taking sonic oscillation, concentrating the distilled liquid, separating flavonoid material, adjusting pH value to below 3, degreasing by non-polar solvent; adjusting the pH value to over 11, extracting by organic solvent, adding crystal solvent to dissolve, decoloring, crystallizing, solving by alcohol or methanol adding catalyst to take reaction, filtering to gain raw oxymatrine, adding to crystal solvent to take recrystallizing to gain oxymatrine. The invention simplifies separating process, decreases cost and realizes high purity oxymatrine distillation.

Description

technical field [0001] The invention relates to a method for producing high-purity oxymatrine from Sophora flavescens. technical background [0002] Sophora flavescens is rich in active ingredients of flavescens alkaloids and flavonoids. Current research mainly focuses on flavescens alkaloids. Sophora flavescens is a class of alkaloids with similar chemical structures represented by matrine. 23 alkaloids have been isolated, including matrine, oxymatrine, sophocarpine, oxysophocarpine, sophoryl alcohol, sophoridine, anagerline, bapufoline, matrine, etc. , total alkaloids of matrine have a variety of physiological activities, and have inhibitory effects on hepatitis, viral myocarditis, tumors, etc., and have broad application prospects in the field of biological pesticides. The State Food and Drug Administration has set higher standards for medicinal matrine and oxymatrine, both requiring a purity greater than 98.0%, which poses a challenge to the separation and purification ...

AI Technical Summary

Problems solved by technology

[0003] The invention patent "comprehensive utilization method of bitter beans" (CN85108322A) treats bitter beans with acid to detoxify them, and then uses acid solution to back-extract the alkaloids sequentially, but the physical and chemical properties of various alkaloids are very close, and it is difficult to obtain them only by adjusting the pH value. High-purity product; the invention patent "Method for preparing matrine from sophocarpine by transfer hydrogenation" (ZL00118510.1) prepares matrine by reacting hydrazine hydrate with sophocarpine in the presence of oxygen, but the high-purity sophocarpine itself There are problems in the separation and purification of alkaloids and matrine. Due to the existence of oxymatrine and sophocarpine, the purity of the obtained matrine product must be limited; The total lye of beans is directly extracted to obtain the crude product of aloperine, which is recrystallized to obtain aloperine with a purity greater than 98%. This process is impossible to achieve etc., so the 98% purity should be the content of total biological alkaloids, rather than the product of a single chemical component; the invention patent "Using CO2 supercritical extraction technology to prepare matrine water and matrine powder" ( CN02103757.4) obtained matrine former powder with content less than 50% by supercritical extraction, but Ge Fahuan (Chinese herbal medicine, 2003, 26 (6): 426) et al.'s research showed that under the condition of no entraining agent, supercritical Carbon dioxide can hardly extract matrine, and the extraction effect is not ideal when adding ethanol entrainer. It needs to be alkalized by ammonia water or introduced non-ionic surfactant to obtain a higher yield, but ammonia water has strong corrosion on supercritical devices. role, and the complete separation of surfactants and products is a more complicated issue

Invention patent "a preparation method of sterile high-purity oxymatrine" (CN1687063A) extracts matrine alkaloids with alkaline solution, and then uses supercritical carbon dioxide to directly extract from alkaline solution to obtain total alkaloids of matrine, hydrogenation, oxidation , crystallization, and obtain the product, but practice has proved that the solubility of supercritical carbon dioxide to the alkaloids of Sophora flavescens is extremely limited, and the alkaloids of Sophora flavescens have relatively large solubility in aqueous solution, so the product yield obtained by this method is low, and the introduction of super Critical technology, high process cost, limited output