Process for producing high purity matrine oxide

Abstract

The invention relates to a method to make high purity oxymatrine that includes the following steps: mixing kuhseng or fenugreek raw material with acid solution , taking sonic oscillation, filtering, 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 hydrogenation reaction, hydrogen peroxide oxidation 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. technical background [0002] Sophora flavescens and Sophora flavescens are rich in active ingredients of matrine alkaloids and bioflavonoids. The current research mainly focuses on matrine alkaloids. Sophora flavescens alkaloids are represented by matrine and have similar chemical structures. Alkaloids, 23 kinds of alkaloids have been isolated, including matrine, oxymatrine, sophocarpine, oxysophocarpine, sophoric alcohol, sophoridine, anajiline, baptinine, matrine Alcohol bases, total alkaloids of matrine have a variety of physiological activities, have inhibitory effects on hepatitis, viral myocarditis, tumors, etc., and also have broad application prospects in the field of biological pesticides. The State Food and Drug Administration has put forward higher standards for medicinal matrine and oxymatrine, and both require a purity greater than 98.0%. This is a challenge for the separa...

AI Technical Summary

Problems solved by technology

[0003] The invention patent "comprehensive utilization method of bitter bean" (CN85108322A) treats bitter beans with acid to detoxify, and then uses acid solution to sequentially back-extract alkaloids. However, the physical and chemical properties of various alkaloids are very close, and it is difficult to rely solely on pH adjustment High-purity products are obtained; the invention patent "Method for preparing matrine from sophocarpine by transfer hydrogenation" (ZL00118510.1) prepares matrine by reacting hydrazine hydrate and sophocarpine in the presence of oxygen, but the high-purity sophocarpine itself There are problems in the separation and purification of fruit base and matrine. Due to the existence of oxymatrine and sophocarpine, the purity of the obtained matrine product must be limited; "The preparation process of the total alkaloids of Sophora sophorae" (CN1368502A) directly extracts the total lye of sophora sophora to obtain the crude product of aloperine, and recrystallizes to obtain aloperine with a purity greater than 98%. This process cannot realize matrine and oxypicrine. Separation of ginseng, sophocarpine, oxidized sophocarpine, sophoryl alcohol, etc., so the 98% purity should be the content of total biological alkaloids, not a product of a single chemical component; the invention patent "is prepared by CO2 supercritical extraction technology Method of Matrine Aqua and Matrine Powder" (CN02103757.4) obtains matrine raw powder with a content of less than 50% by supercritical extraction, but Gefahuan (Chinese herbal medicine, 2003, 26 (6): 426) etc. Human studies have shown that under the condition of no entrainer, 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 a strong corrosive effect on supercritical devices, and the complete separation of surfactants and products is a more complicated problem

Invention patent "A kind of matrine and its preparation process" (CN1277202A) is obtained by using pure matrine through hydrogen peroxide oxidation, concentration, industrial ethanol dissolution, evaporation to dryness, absolute ethanol dissolution, evaporation to dryness, acetone reflux, suction filtration, etc. White matrine, although the oxidation process is introduced, but pure matrine is not easy to obtain, and the process engineering is complicated and the operation cost is high

Invention patent "process for preparing oxymatrine from Sophora sophora" (CN1148370) through extraction, organic solvent extraction, acid water stripping, alkali precipitation, catalytic hydrogenation, crystallization, hydrogen peroxide oxidation, crystallization drying, etc., to obtain oxypicrin Sophora flavescens, but the alkaloids of Sophora flavescens have a high solubility in water, and the alkali precipitation in the process is often difficult to obtain. Even if obtained, the yield of flavescens alkaloids is not high; acid water stripping It is also difficult to completely extract the alkaloids in the organic solvent, and using toluene recrystallization, in addition to the low yield, it is also a problem to completely remove the more toxic toluene

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