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Method for extracting purification machilin from machilus

A technology for nanmu and lignan, which is applied in the field of extracting and purifying nan lignan A, can solve problems such as the preparation method of nan lignan A that has not been retrieved, and achieve the effects of easy industrialization and simple production process.

Inactive Publication Date: 2012-09-12
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The preparation method report of Phoebenan A has not yet been retrieved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Dry and pulverize 2kg red nan tree bark into the extraction tank, add 4 times the amount of 80% ethanol solution, soak for 4 hours, then ultrasonically extract for 2 hours, add diatomaceous earth and activated carbon to the mixture in a mass ratio of 1:2 The mixture, added in an amount of 5% (w / v) of the extract, was fully stirred and filtered, the filtrate was concentrated to no alcohol, passed through the AB-8 macroporous adsorption resin column, and first eluted with 10% ethanol of 3 times the column volume , The eluate was discarded after recovering the reagent, and then eluted with 4 times the column volume of 85% ethanol, the eluate was collected, concentrated and dried to obtain the crude product. The crude product was prepared into a 20mg / ml solution with methanol, separated by preparative high-performance liquid chromatography, and the preparative column was filled with C18, with methanol-water (63:37) as the mobile phase, and the flow rate was controlled at 45m...

Embodiment 2

[0015] Dry and pulverize 2kg red nan tree bark into the extraction tank, add 3 times the amount of 65% ethanol solution, soak for 3 hours, then ultrasonically extract for 2 hours, add diatomaceous earth and activated carbon to the extract solution in a mass ratio of 1:2 The mixture, added in an amount of 4% (w / v) of the extract, was fully stirred and then filtered, and the filtrate was concentrated to no alcohol, passed through a D101 macroporous adsorption resin column, first eluted with 15% ethanol 4 times the column volume, and washed Remove the liquid to recover the reagent and discard it, then elute with 6 times the column volume of 80% ethanol, collect the eluate, concentrate and dry to obtain the crude product. The crude product was prepared into a 20mg / ml solution with methanol, separated by preparative high-performance liquid chromatography, and the preparative column was filled with C18, with methanol-water (56:44) as the mobile phase, and the flow rate was controlled...

Embodiment 3

[0017] Dry and pulverize 5kg red nan tree bark into the extraction tank, add 6 times the amount of 50% ethanol solution, soak for 6 hours, then ultrasonically extract for 1 hour, add diatomaceous earth and activated carbon to the extract solution in a mass ratio of 1:2 The mixture, added in an amount of 2% (w / v) of the extract, was fully stirred and filtered, the filtrate was concentrated to no alcohol, passed through the AB-8 macroporous adsorption resin column, and first eluted with 20% ethanol of 6 times the column volume , The eluate was discarded after recovering the reagent, and then eluted with 5 times the column volume of 75% ethanol, the eluate was collected, concentrated and dried to obtain the crude product. The crude product was prepared into a 20mg / ml solution with methanol, and separated by preparative high-performance liquid chromatography. The preparative column used C18 as column packing, methanol-water (73:27) as mobile phase, and controlled the flow rate at 2...

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PUM

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Abstract

The invention discloses a method for extracting purification machilin from machilus, which comprises the following steps: airing and crushing machilus barks and soaking for 3-6 hours with 50-95 percent of ethanol after crushing; then carrying out ultrasonic extraction, adding extracting solution into a mixture of kieselguhr and activated carbon, filtering, enabling a concentrated filtrate to pass through a macro-porous adsorption resin column, collecting an eluent, reducing the pressure and recovering a reagent; and separating through a preparative liquid chromatography to obtain the machilin A. The method has the advantages of simple production process, easiness in realization of industrialization, no toxic solvent used in the whole process, safety and environment friendliness.

Description

technical field [0001] The invention belongs to the technical field of extracting traditional Chinese medicines, and relates to a method for extracting and purifying phoenixin A from phobia. Background technique [0002] Machilin A, the molecular formula is C 20 h 22 o 4 , with a molecular weight of 326.39, is a colorless needle crystal, which is obtained from the Lauraceae plant Phoebe Machilus thunbergii A lignan compound isolated from the bark of Sieb. et Zucc. Pharmacological studies have shown that phoenixin A has immunosuppressive activity, and has a strong inhibitory effect on the proliferation of human peripheral blood lymphocytes induced by mitogen (conavalin A), and its IC 50 It is 0.02μg / mL, which is equivalent to prednisolone. In addition, it also has cytotoxic activity against human leukemia cell lines HL-60 and Molt-4 cells. Its IC 50 (ng / ml) were 26 and 54, respectively. [0003] No report on the preparation method of phoenixin A has been retrieved yet. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/50
Inventor 刘东锋郭琴
Owner NANJING ZELANG MEDICAL TECH
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