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Method for extracting 2, 7-dihydroxyapogeissoschizine

An extraction method and dihydroxyl technology, applied in the direction of organic chemistry, etc., can solve the problems that have not yet been discovered, and achieve the effects of reducing the dissolution of impurities, high efficiency and large extraction amount.

Inactive Publication Date: 2012-10-03
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] After searching the literature, no related reports on the industrial extraction and purification method of 2,7-dihydroxyapocalyptus alkaloids have been found

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Marchanaceae Strychnos gossweileri Exell. The root bark is crushed, take 1kg, add 1% hydrochloric acid aqueous solution to soak for 6 hours, ultrasonically treat for 20 minutes, filter to obtain the extract, adjust the pH to 7.5, add ultrafiltration membrane ultrafiltration with a molecular weight cut-off of 2000, and then add Nanofiltration membrane nanofiltration to obtain a concentrated solution, adjust the pH to 10, extract with chloroform, take the organic layer, recover the chloroform, and dry to obtain the crude product. With a volume ratio of 9:6:3 chloroform-methanol-water as a two-phase solvent system, fully mix it, stand still to separate the phases, and ultrasonically degas the two phases for 25 minutes respectively. The upper phase is the stationary phase and the lower phase is the mobile phase. The crude product was dissolved in a mixed solution of two phases (the volume ratio of the upper phase and the lower phase was 1:1), injected into a high-speed cou...

Embodiment 2

[0021] Marchanaceae Strychnos gossweileri Exell. The root bark is crushed, take 1kg, add 0.3% sulfuric acid aqueous solution to soak for 1h, ultrasonically treat for 60min, filter to obtain the extract, adjust the pH to 6, add ultrafiltration membrane ultrafiltration with a molecular weight cut-off of 6000, and then add Nanofiltration membrane nanofiltration to obtain the concentrated solution, adjust the pH to 9, extract with chloroform, take the organic layer, recover the chloroform, and dry to obtain the crude product. With a volume ratio of 4:3:3 chloroform-methanol-water as a two-phase solvent system, fully mix it, let stand to separate the phases, degas the two phases by ultrasonic wave for 25 minutes, the upper phase is the stationary phase, and the lower phase is the mobile phase. Dissolve the crude product in a mixed solution of two phases (the volume ratio of the upper phase and the lower phase is 1:1), inject it into a high-speed countercurrent chromatograph, detec...

Embodiment 3

[0023] Marchanaceae Strychnos gossweileri Exell. The root bark is crushed, take 1kg, add 0.5% sulfuric acid aqueous solution to soak for 4 hours, ultrasonically treat for 40 minutes, filter to obtain the extract, adjust the pH to 7, add ultrafiltration membrane ultrafiltration with a molecular weight cut-off of 4000, and then add Nanofiltration membrane nanofiltration to obtain the concentrated solution, adjust the pH to 9.5, extract with chloroform, take the organic layer, recover the chloroform, and dry to obtain the crude product. With a volume ratio of 7:5:3 chloroform-methanol-water as a two-phase solvent system, fully mix it, stand still and separate the phases, and ultrasonically degas the two phases for 25 minutes respectively. The upper phase is the stationary phase and the lower phase is the mobile phase. Dissolve the crude product in a mixed solution of two phases (the volume ratio of the upper phase and the lower phase is 1:1), inject it into a high-speed counter-...

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Abstract

The invention discloses a method for extracting 2, 7-dihydroxyapogeissoschizine. The method comprises the steps of taking roots and barks of Strychnosgossweileri Exell in Loganiaceae as raw material, crushing the material, adding 0.3 to 1 percent of hydrochloric acid or sulfuric acid aqueous solution in the material for extracting, regulating the PH value of an extraction solution to 6-7.5, adding an ultrafiltration membrane for ultrafiltration, then adding a nanofiltration membrane for nonofiltration, regulating the PH value of the concentration solution to be 9-10, extracting by chloroform, concentrating the extraction solution, drying the concentrated extraction solution to obtain a crude extract, separating and purifying the crude extract by means of high-speed counter-current chromatography, performing online ultraviolet detection, collecting target components, and drying the target components at the low temperature to obtain the 2,7-dihydroxyapogeissoschizine. According to the method provided by the invention, the energy consumption is low, the pollution is few, and the product content is too high to be more than 95 percent, therefore, the method is suitable for small-scale experiments as well as industrialized production.

Description

technical field [0001] The invention belongs to the technical field of extraction and separation of traditional Chinese medicines, and in particular relates to a method for extracting 2,7-dihydroxyapocalyptus. Background technique [0002] 2,7-Dihydroxyapocalypsis Strychnos gossweileri The active ingredient in Exell. root bark is a carboline alkaloid with molecular formula C 21 h 24 N 2 o 4 , molecular weight: 368.43, structural formula: [0003] . [0004] 2,7-Dihydroxy Apocalypse has cytotoxic activity, and at a concentration of 75 μg / ml, it showed low cytotoxic activity to B16 melanoma cells cultured in vitro. [0005] Through literature search, there is no relevant report on the industrial extraction and purification method of 2,7-dihydroxyapocalyptus alkaloid. Contents of the invention [0006] The object of the present invention is to provide a method for extracting 2,7-dihydroxy apocaria japonica. [0007] The present invention is achieved through the fo...

Claims

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Application Information

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IPC IPC(8): C07D455/00
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH