Process for producing high purity matrine oxide by kuh-seng

A high-purity technology for oxymatrine, applied in organic chemistry and other fields, can solve problems such as limited solubility, high process cost, and limited output, and achieve the effects of easy industrial production, simplified separation process, and reduced production cost

Inactive Publication Date: 2006-06-28
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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 mat

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Add 20ml of ammonia water to 1000ml of 80wt% ethanol to make an extract, add 100g of flavescens powder of 10 to 40 meshes into the extract, ultrasonically extract at 10°C for 60min, let stand, filter, wash the filter residue three times with the above extract, and combine Filtrate and washing liquid; concentrate the extract to a volume of 200ml, add 400ml of water, flavonoids are precipitated, and filter to obtain a solid aqueous solution of total flavonoids and alkaloids of Sophora flavescens.

[0031] (2) Add hydrochloric acid to the alkaloid solution obtained in (1) to adjust the pH value to 3, add 150 ml of ether for extraction and degreasing, and separate the liquids. In this way, the degreasing and liquid separation is performed three times, and the ethers are combined and evaporated for recovery.

[0032](3) Add sodium carbonate to the aqueous phase obtained by (2) liquid separation, stir and dissolve to adjust the pH value to 11, add 60ml of chloroform to ext...

Embodiment 2

[0037] (1) 800ml of 90wt% methanol was added with 10ml of ammonia water to make an extract, 100g of 40-80 mesh Sophora flavescens powder was added to the extract, ultrasonically extracted at 30°C for 40min, left to stand, filtered, the filter residue was washed three times with the above extract, and the filtrate and Washing liquid: concentrated by rotary evaporation to make the volume of the concentrated liquid 150ml, adding 800ml of water, flavonoids are precipitated, and filtered to obtain solid aqueous solution of total flavonoids and alkaloids of Sophora flavescens.

[0038] (2) Add acetic acid to the alkaloid solution obtained in (1) to adjust the pH value to 2, add 200ml of petroleum ether for extraction and degreasing, and separate the liquids. In this way, the degreasing and liquid separation is performed three times, and the petroleum ethers are combined and evaporated for recovery.

[0039] (3) Add sodium bicarbonate to the aqueous phase obtained in (2) and stir to d...

Embodiment 3

[0044] (1) Add 1ml of ammonia water to 500ml of 95wt% ethanol to make an extract, add 100g of Sophora flavescens powder of 80 to 100 meshes into the extract, ultrasonically extract at 50°C for 20min, let stand, filter, wash the filter residue three times with the above extract, and combine Filtrate and washing liquid; concentrated by rotary evaporation so that the volume of the concentrated liquid is 100ml, adding 800ml of water, flavonoids are precipitated, and filtered to obtain a solid aqueous solution of total flavonoids and alkaloids of Sophora flavescens.

[0045] Add nitric acid to the alkaloid solution obtained in (1) to adjust the pH value to 1, add 80 ml of chloroform to extract and degrease, and separate the liquids. In this way, the degreased liquids are separated three times, and the chloroform is combined and evaporated for recovery.

[0046] (2) (2) Add sodium hydroxide to the aqueous phase obtained by liquid separation, stir and dissolve to adjust the pH value t...

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PUM

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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 ...

Claims

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Application Information

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IPC IPC(8): C07D455/00
Inventor 侯相林邓天昇齐永琴杜俊民
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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