Method for preparing henningsoline

A technology of seeds and chloroform, applied in the field of natural medicines, can solve the problems such as the undiscovered industrial preparation method of Henning Sorling, and achieve the effects of short cycle, good separation and large sample volume

Inactive Publication Date: 2012-12-19
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 relevant reports on the industrial preparation method of Henning Sorling have been found

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Take 3 kg of S. chinensis seeds and crush them, extract twice with a methanol-dichloromethane mixed solvent with a volume ratio of 3:1, concentrate the extract under reduced pressure to obtain a crude extract, suspend the crude extract with water, and then use ethyl acetate to Extract 4 times, collect the ethyl acetate layer, concentrate, load the sample to a 200-300 mesh silica gel high-pressure column with a column pressure of 3.0MPa, a column inner diameter of 230mm, and a column diameter-to-height ratio of 1:15, using chloroform-acetone solvent The system changes the volume ratio from 10:1 to 1:10 for gradient elution, collects the fractions in sections, combines the fractions containing Henning Sorling, recovers the solvent under reduced pressure to a small volume, stands for crystallization, and filters out the crystals , the crude crystals were recrystallized with chloroform-acetonitrile (1:4), the crystals were filtered off, and dried to obtain 1.06 g of Henning ...

Embodiment 2

[0021] Take 5 kg of S. chinensis seeds and crush them, and then extract 3 times with ethanol-dichloromethane mixed solvent with a volume ratio of 2:1, concentrate the extract under reduced pressure to obtain a crude extract, add water to suspend the crude extract, and then use ethyl acetate Extract 6 times, collect the ethyl acetate layer, concentrate, and load the sample to a 300-400 mesh silica gel high-pressure column with a column pressure of 2.6MPa, a column inner diameter of 250mm, and a column diameter-to-height ratio of 1:18, using chloroform-acetone solvent The system changes the volume ratio from 10:1 to 1:10 for gradient elution, collects the fractions in sections, combines the fractions containing Henning Sorling, recovers the solvent under reduced pressure to a small volume, stands for crystallization, and filters out the crystals , the crude crystals were recrystallized with chloroform-acetonitrile (1:4), the crystals were filtered off, and dried to obtain 1.67 g ...

Embodiment 3

[0023] Take 10 kg of S. chinensis seeds, break them, extract 3 times with 85% ethanol, concentrate the extract under reduced pressure to obtain a crude extract, suspend the crude extract with water, then extract 4 times with chloroform, collect the chloroform layer, concentrate, and load the sample to Filled with 300-400 mesh silica gel high-pressure column, the column pressure is 3.4MPa, the inner diameter of the column is 180mm, the ratio of column diameter to height is 1:20, and the gradient washing is carried out by changing the volume ratio of chloroform-acetone solvent system from 10:1 to 1:10. Remove, collect the fractions in sections, combine the fractions containing Henning Sorling, recover the solvent under reduced pressure to a small volume, let it stand for crystallization, filter out the crystals, and rewet the crude crystals with chloroform-acetonitrile (1:4) Crystallized, the crystals were filtered out, and dried to obtain 3.51 g of Henning Sulling, with a conten...

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PUM

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Abstract

The invention discloses a method for preparing henningsoline. The method comprises the following steps of: extracting strychnos cathayensis medicinal materials by a solvent; condensing the extracted liquid; adding water into the extracted liquid to suspend; extracting a mixture by ethyl acetate or chloroform; performing high-pressure silica gel column chromatography on the mixture by an ethyl acetate layer or a chloroform extracting layer, wherein a chloroform-acetone or chloroform-ethyl acetate solvent system is eluent; performing gradient elution on the eluent according to the volume change from 10:1 to 1:10; performing thin-layer chromatography tracking combination on the eluent; collecting target components; and recrystallizing and purifying the target components to acquire a final product. The method is easy to operate and short in period.

Description

technical field [0001] The invention relates to a preparation method of Henning Sulphin, which belongs to the field of natural medicines. Background technique [0002] Henningsoline is a colorless prism, mp.207-209℃, is a carbazole alkaloid with the molecular formula C 22 h 26 N 2 o 5 , the molecular weight is 398.46, and the molecular structure formula is: [0003] . [0004] Mainly distributed in the Marchanaceae plant Huamai Strychnos cathayensis Merr. in seeds. Huama money is produced in Guangxi, Hainan Island and other places in my country, and is used by folks to relieve pain. Modern pharmacological studies have found that Henning Sulling has obvious analgesic effect on mice injected intraperitoneally (500mg / kg). [0005] After searching the literature, no relevant reports on the industrial preparation method of Henning Sulphine have been found. Contents of the invention [0006] The purpose of the present invention is to provide a kind of preparation meth...

Claims

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Application Information

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IPC IPC(8): C07D491/22
Inventor 刘东锋
Owner NANJING ZELANG MEDICAL TECH
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