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Method for extracting brucine N-oxide from nux vomica

A technology of strychnine and nitrogen oxides, applied in the direction of organic chemistry, etc., can solve the problems of small batch differences of compounds, potential effects to be developed, and applications are rarely researched, etc., to achieve low reagent consumption and short preparation cycle. , the effect of good operability

Inactive Publication Date: 2016-04-27
正源堂(天津)生物科技有限公司
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Problems solved by technology

[0004] The current separation and extraction of strychnine nitrogen oxides is limited by the non-mechanized operation of traditional Chinese medicine. The steps are cumbersome, time-consuming, and labor-intensive. The amount of the compound obtained is small and the difference between batches is large, making it difficult to conduct clinical research.
[0005] In addition, for strychnine nitrogen oxides, due to the low content in plants, its application is rarely studied, so its potential role remains to be developed

Method used

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  • Method for extracting brucine N-oxide from nux vomica
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  • Method for extracting brucine N-oxide from nux vomica

Examples

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Embodiment 1

[0032] Use the fruiting body of Nuxyche as the raw material, grind it into powder, and extract it with ethanol under reflux for 1.5h, filter, take the precipitate and repeat the extraction twice, combine the obtained filtrate, spin evaporate to obtain dry coarse powder of Nuxe nux, weigh 10g, dissolve In 100mL of 55% methanol-water (0.1% acetic acid) solution, a solution of Nuxychia seed extract was prepared with a concentration of 100mg / mL, passed through a 0.45μm microporous membrane, and prepared by one-dimensional liquid chromatography. One-dimensional liquid chromatography adopts InnovelC18150×250mm, 10μm, The mobile phase is a mixture of binary liquid phases, in which the binary liquid phase A is water (containing 0.1% acetic acid), and B phase is methanol. The elution method: B phase concentration 25% isocratic 10min, B phase concentration 35 % isocratic for 20 minutes, phase B concentration 100% isocratic for 10 minutes. Adopt ultraviolet detector, select 210nm absor...

Embodiment 2

[0036] Use the fruiting body of Nuxyche as the raw material, grind it into powder, extract it with ethanol under reflux for 2 hours, filter, take the precipitate and repeat the extraction twice, combine the obtained filtrate, spin evaporate to obtain dry coarse powder of Nuxe officinalis, weigh 15g, dissolve in 100mL of 50% methanol-water (0.1% acetic acid) solution was used to prepare a Nuxychia seed extract solution with a concentration of 150mg / mL, passed through a 0.45μm microporous membrane, and prepared by one-dimensional liquid chromatography. One-dimensional liquid chromatography adopts InnovelC18150×250m, 10μm, The mobile phase is a mixture of binary liquid phases, in which the binary liquid phase A is water (0.1% acetic acid), and B phase is methanol, and the elution method: the concentration of phase B is 25% isocratic for 10 minutes, and the concentration of phase B is 35% Isocratic for 20 minutes, B phase concentration 100% isocratic for 10 minutes. The absorpti...

Embodiment 3

[0040] Use the fruiting body of Nuxyche as the raw material, grind it into powder, soak it in ethanol for 2 hours, filter, take the precipitate and repeat it twice, combine the filtrates, spin evaporate to obtain dry Nuxychnium powder, weigh 5g, dissolve in 100mL60% The methanol-water (0.1% acetic acid) solution was used to prepare the Nuxychia seed extract solution with a concentration of 50 mg / mL, passed through a 0.45 μm microporous membrane, and prepared by one-dimensional liquid chromatography. One-dimensional liquid chromatography adopts InnovelC18150×250mm, 10μm, The mobile phase is a mixture of binary liquid phases, in which the binary liquid phase A is water (0.1% acetic acid), and B phase is methanol, and the elution method: the concentration of phase B is 25% isocratic for 10 minutes, and the concentration of phase B is 35% Isocratic for 20 minutes, B phase concentration 100% isocratic for 10 minutes. The absorption wavelength is selected with a UV detector at 210...

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Abstract

The invention provides a method for extracting brucine N-oxide from nux vomica. The method comprises the following steps: grinding nux vomica into powder, immersing the nux vomica powder with ethanol or carrying out reflux extraction, drying a filtrate by distillation and dissolving with methanol-water solution; carrying out one-dimensional liquid phase separation, adopting a C18 chromatographic column, A phase water and B phase methanol binary liquid phase, carrying out 25% B-phase isocratic elution for 10 min, carrying out 35% B-phase isocratic elution for 20 min, carrying out 100% B-phase isocratic elution for 10 min, collecting 13.5-15.5min eluate, drying by distillation, and dissolving with methanol-water solution; carrying out two-dimensional liquid-phase separation, adopting a C18 chromatographic column, A phase water and B phase methanol binary liquid phase, carrying out 30% B-phase isocratic elution, collecting 17.5-20 min eluate, and drying by distillation to obtain brucine N-oxide with purity being 99%. The method can be directly applied to industrial production and provides source guarantee for potential role development of brucine N-oxide.

Description

technical field [0001] The invention relates to the technical field of extracting traditional Chinese medicines, in particular to a method for extracting strychnine nitrogen oxides from strychnium seeds. Background technique [0002] Strychnine nitrogen oxide is a compound in the traditional Chinese medicine Strychnium, and its structural formula is as follows: [0003] [0004] The current separation and extraction of strychnine nitrogen oxides is limited by the non-mechanized operation of traditional Chinese medicine. The steps are cumbersome, time-consuming, and labor-intensive. The amount of the compound obtained is small and the difference between batches is large, making it difficult to conduct clinical research. [0005] In addition, for strychnine nitrogen oxide, due to the low content in plants, its application is rarely studied, so its potential role remains to be developed. Contents of the invention [0006] The technical problem to be solved in this inventi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/22
CPCC07D491/22
Inventor 张耀洲李上文
Owner 正源堂(天津)生物科技有限公司
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