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A kind of preparation method of 4-hydroxyecaine

A technology of hydroxyecalid and ethanol, which is applied in the field of preparation of 4-hydroxyecatine, can solve the problems such as hindering the progress of 4-hydroxyecatine, cumbersome and other problems, and achieves a feasible separation and purification method, high purity, and automatic instrumentation. high degree of effect

Active Publication Date: 2016-11-23
TIANJIN LANGLI PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] So far, the method of extracting 4-hydroxyecaine from natural product extracts is rarely reported, and it is relatively cumbersome, not to mention the extraction of high-purity or monomeric 4-hydroxyecaine, which is certain To a certain extent, it also hinders the progress of 4-hydroxyecaine in the development of traditional Chinese medicine

Method used

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  • A kind of preparation method of 4-hydroxyecaine
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  • A kind of preparation method of 4-hydroxyecaine

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Effect test

Embodiment 1

[0024] Use the fruiting body of Nuxychonna as raw material, grind it into powder, extract it with ethyl acetate and rotary steam it to get dried Nuxychonna powder, weigh 5g, dissolve it in 100mL 20% ethanol-n-hexane solution, and make Nuxychonium Sub-extract solution, the concentration is 50mg / mL, pass through 0.45μm microporous membrane, prepare by one-dimensional liquid chromatography. One-dimensional liquid chromatography adopts Innovel silica 150×250m, 10μm, The mobile phase is a mixture of organic phases, in which the organic phase A is n-hexane, B is ethanol, and the elution method is: B phase concentration 0% isocratic 5min, B phase concentration 0%-64% gradient 5-35min, B phase concentration 64%-100% gradient 35-45min. Use an ultraviolet detector at 210nm to select the absorption wavelength, the preparation temperature is room temperature, the injection volume is 5000 μL / needle, the flow rate of the mobile phase is 80mL / min, and the fractions collected for 28-33 minu...

Embodiment 2

[0026] Nuxychnium fruiting body is used as raw material, ground into powder, extracted with ethyl acetate and rotary steamed to obtain dry nuxychonium powder, weigh 10g, dissolve in 100mL 30% ethanol-n-hexane solution, and prepare nuxychonium Sub-extract solution, the concentration is 100mg / mL, pass through 0.45μm microporous membrane, and prepare by one-dimensional liquid chromatography. One-dimensional liquid chromatography adopts Innovel silica 150×250mm, 10μm, The mobile phase is a mixture of organic phases, in which the organic phase A is n-hexane, B is ethanol, and the elution method is: B phase concentration 0% isocratic 5min, B phase concentration 0%-64% gradient 5-35min, B phase concentration 64%-100% gradient 35-45min. Use an ultraviolet detector at 210nm to select the absorption wavelength, the preparation temperature is room temperature, the injection volume is 5000 μL / needle, the flow rate of the mobile phase is 80mL / min, and the fractions collected for 28-33 mi...

Embodiment 3

[0028] Take nuxychon fruiting bodies as raw materials, grind them into powder, extract and rotary steam with ethyl acetate to obtain dried nuxychonium powder, weigh 5g, dissolve in 200mL 30% ethanol-n-hexane solution, and prepare nuxychonium The sub-extract solution, the concentration is 25mg / mL, pass through 0.45μm microporous membrane, and prepare by one-dimensional liquid chromatography. One-dimensional liquid chromatography adopts Innovel silica 150×250mm, 10μm, The mobile phase is a mixture of organic phases, in which the organic phase A is n-hexane, B is ethanol, and the elution method is: B phase concentration 0% isocratic 5min, B phase concentration 0%-64% gradient 5-35min, B phase concentration 64%-100% gradient 35-45min. Use an ultraviolet detector at 210nm to select the absorption wavelength, the preparation temperature is room temperature, the injection volume is 5000 μL / needle, the flow rate of the mobile phase is 80mL / min, and the fractions collected for 28-33 m...

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Abstract

The invention relates to a preparation method of vomicine. According to the method, vomicin is extracted from a natural product strychnos nux-vomica fruiting body with a two-dimensional liquid-phase chromatographic technique, the whole separation and purification method is practicable by means of reasonable selection of chromatographic columns, dissolved solutions, mobile phases and the like and optimization of technological conditions such as the flow velocity, the elution mode, the collection sections and the like, the operation is simple and convenient, the automation degree of an instrument is high, preparation can be performed at room temperature and normal temperature and pressure, the repeatability is high, the consistency of batches of obtained material components is high, the operability is high, the purity of the obtained vomicine is high and can be higher than 99%, and the preparation method can be directly applied to industrial production.

Description

technical field [0001] The invention relates to the field of compound production, in particular to a preparation method of 4-hydroxyekaquin. Background technique [0002] Alkaloid compounds are widely distributed in traditional Chinese medicine animal medicines, and their chemical structures are complex and diverse, and their biological activities are remarkable. Some alkaloids with novel structures have remarkable physiological and pharmacological activities, and may be an important source of drugs for the treatment of a series of major human diseases. 4-Hydroxyecaine is such an alkaloid compound, which is an important natural active ingredient widely present in plants. Its structure is as follows: [0003] [0004] At present, it is found that 4-hydroxyekagen has the following effects: first, it has the effect of inhibiting the proliferation, differentiation and cytotoxicity of proliferating and differentiated cells and tumor cells, and inducing apoptosis. Therefore, 4...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D491/22
CPCC07D491/22
Inventor 张耀洲李上文
Owner TIANJIN LANGLI PHARMA CO LTD
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