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Preparation method of castanospermine

A suspension, macroporous resin technology, applied in organic chemistry and other directions, can solve rare problems and achieve the effect of less sample loss, strong separation ability, and time period

Inactive Publication Date: 2013-08-07
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] There are few reports on the extraction of chestnut stigmatine, and there is no chestnut stigmatine for sale in the market. Therefore, it is necessary to provide a preparation method of chestnut stigmatine, which can provide information for its follow-up research. support

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 1kg of dried leaves of Dahuabudou, crush them into coarse powder, mix them with 10kg of 75% ethanol solution, suspend them by cavitation for 30 minutes, perform negative pressure cavitation suspension solid-liquid extraction twice to obtain the extract, and concentrate to density 1.2g / ml to obtain total alkaloid extract, add D101 type macroporous resin to the extract, mix well, dry, then pack into column, wash with water until the color is light, and then wash with 85% ethanol solution of 6 times column volume Detach, TLC detection, collect the target fraction, and concentrate to obtain the crude product.

[0022] Take chloroform-methanol-water and put it in a separatory funnel according to the volume ratio (5:15:6), mix well, let it stand, release the upper layer as the stationary phase, and the lower layer as the mobile phase, dissolve the crude product in the lower phase, and start the preparation Type high-speed countercurrent chromatograph, first pump the stat...

Embodiment 2

[0024] Take 2kg of dried leaves of Dahuabudou, crush them into coarse powder, mix them with 20kg of 75% ethanol solution, suspend them by cavitation for 30 minutes, perform negative pressure cavitation suspension solid-liquid extraction twice to obtain the extract, and concentrate to density 1.2g / ml, to get the total alkaloid extract, add D101 macroporous resin to the extract, mix well, dry and pack into a column, first wash with water until the color is light, and then wash with 85% ethanol solution 5 times the column volume Detach, TLC detection, collect the target fraction, and concentrate to obtain the crude product.

[0025] Take chloroform-methanol-water and put it in a separatory funnel according to the volume ratio (9:17:8), mix well, let it stand still, release the upper layer as the stationary phase, and the lower layer as the mobile phase, dissolve the crude product in the lower phase, and start the preparation Type high-speed countercurrent chromatograph, first pum...

Embodiment 3

[0027] Take 2kg of dried leaves of Dahuabudou, crush them into coarse powder, mix them with 20kg of 75% ethanol solution, suspend them by cavitation for 30 minutes, perform negative pressure cavitation suspension solid-liquid extraction twice to obtain the extract, and concentrate to density 1.1g / ml, to get the total alkaloid extract, add D101 macroporous resin to the extract, mix well, dry and pack into a column, wash with water until the color is light, and then wash with 85% ethanol solution of 6 times the column volume Detach, TLC detection, collect the target fraction, and concentrate to obtain the crude product.

[0028] Take chloroform-methanol-water and place it in a separatory funnel according to the volume ratio (7:16:7), mix well, let it stand still, release the upper layer as the stationary phase, and the lower layer as the mobile phase, dissolve the crude product in the lower phase, and start the preparation Type high-speed countercurrent chromatograph, first pump...

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PUM

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Abstract

The invention provides a preparation method of castanospermine. The preparation method of the castanospermine is characterized by comprising the following steps of: (1), crushing dry leaves of pinto beans, adding an ethanol aqueous solution, carrying out negative-pressure cavitation suspension solid-liquid extraction to obtain extract liquor; recycling reagent from the extract liquor to obtain total alkaloid extract; (2), adding macroporous resin to the total alkaloid extract for packing after uniformly stirring, drying, carrying out alcohol-water solution elution, collecting castanospermine fraction components and concentrating to obtain a castanospermine crude product; and (3), separating and purifying the crude product by high-speed counter-current chromatography to obtain the castanospermine. The preparation method of the castanospermine has the advantages of high product yield, high extracting rate and the like, and is simple to operate.

Description

technical field [0001] The invention belongs to the field of separation of natural products, and in particular relates to a method for separating and purifying chestnut sourine from dried leaves of Dahuabudou by using high-speed countercurrent chromatography. Background technique [0002] Chestnut sourine (Castanospermine) is from the leguminous plant Alexa grandiflora An indole alkaloid active ingredient isolated from the leaves of Ducke. Modern pharmacological studies have shown that sowine can inhibit α-glucoside Ⅰ, Ⅱ and change glycogen metabolism in rats; inhibit the growth of HIV-1 and HIV-2, and inhibit the reproduction of HIV in human cells. AZT combined treatment of AIDS; antiviral effect, the IC50 of murine leukemia virus is 1.0μg / mL; inhibition of tumor metastasis, intraperitoneal injection of 500mg / kg once a day to Lewis lung cancer mice, on the 18th day, the average tumor weight was inhibited by 25% and 40%, the average inhibition of metastatic lesions is...

Claims

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Application Information

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IPC IPC(8): C07D471/04
Inventor 苏刘花万冬梅
Owner NANJING ZELANG AGRI DEV
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