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Process for purifying swainsonine in Feng grass

A swainsonine and process technology, applied in the field of natural product chemistry research, can solve the problems of inability to mass production, low extraction rate and the like, and achieve the effects of low extraction cost and high product purity

Inactive Publication Date: 2003-02-12
葛鹏斌
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantage is that the extraction rate is low and cannot be mass-produced
There is still a vacancy in the main technical process for the purification of swainsonine in China

Method used

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  • Process for purifying swainsonine in Feng grass
  • Process for purifying swainsonine in Feng grass
  • Process for purifying swainsonine in Feng grass

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: the extraction of swainsonine in Oxytropis gansu

[0031] The first step, extract extraction stage: Gansu Oxytropis hay powder 5kg, cold immersion extraction with 30 liters of industrial methanol 4 times, each cold immersion for 7 days, filtering, merging methanol liquid, recovering methanol under reduced pressure to obtain 680g of total extract, The paste yield was 13.6%.

[0032] The second step, crude alkaloid extraction stage: 680g total extract was ground and dissolved repeatedly with 6800mL 1N hydrochloric acid, and filtered until the last acid water improved bismuth iodide potassium test showed a negative reaction, and the acid water was combined. The obtained acidic aqueous solution was adjusted to a pH of 4-5 with concentrated ammonia water, passed through a hydrogen-type cation exchange resin column, first eluted with 100 times the amount of sample-loaded deionized water until colorless, and then eluted with 20 times the amount of 1N ammonia wate...

Embodiment 2

[0036] Embodiment 2: Extraction of swainsonine in Oxytropis japonica

[0037] The first stage of extraction of extract: 11.5kg of Oxytropis chrysantha hay powder, cold soaked with 70 liters of industrial methanol to extract 6 times, each cold soaked for 7 days, filtered, combined methanol liquid, and recovered methanol under reduced pressure to obtain 1600g of total extract. The paste yield was 13.9%.

[0038] The second step of crude alkaloid extraction stage: 1600g of the total extract was repeatedly ground and dissolved with 16000mL of 1N hydrochloric acid, and filtered until the last test of the improved bismuth iodide potassium iodide showed a negative reaction, and the acid water was combined. The obtained acidic aqueous solution was adjusted to a pH of 4-5 with concentrated ammonia water, passed through a hydrogen-type cation exchange resin column, first eluted with 100 times the amount of sample-loaded deionized water until colorless, and then eluted with 20 times the ...

Embodiment 3

[0042] Embodiment 3: Extraction of swainsonine in Oxytropis gansu

[0043] The first step of extract extraction stage: Gansu Oxytropis hay powder 20kg, cold immersion extraction with 100 liters of industrial methanol 4 times, each cold immersion for 5 days, filtering, merging methanol liquid, and recovering methanol under reduced pressure to obtain 2230g of total extract. The paste rate was 11.2%.

[0044] The second step of crude alkaloid extraction stage: 2230g total extract was repeatedly ground and dissolved with 15000mL 1N hydrochloric acid, and filtered until the last acid water solution improved bismuth potassium iodide test showed a negative reaction, and the acid water solution was combined. The resulting acidic aqueous solution was adjusted to pH 4-5 with concentrated ammonia water, passed through a hydrogen-type cation exchange resin column, and first eluted with 100 times the amount of sample-loaded deionized water until it was colorless, and then eluted with 30 ti...

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Abstract

A process for purifying swainsonic contained in loco weed includes extracting macropolar alkaloid crude product by cationic exchange, further extracting with alkaline chloroform, silica gel chromatography to obtain swainsonic crude product and finally sublimating by steps. Its advantages are low cost and high purity.

Description

[0001] 1. Field [0002] The invention belongs to the field of chemical research of natural products, relates to natural product extraction, separation and identification methods, in particular to a purification process of swainsonine in locoweed. 2. Background technology [0003] Locoweed is the general term for the poisonous plants of the genus Oxytopis and Astragalus in the leguminous family, and it is the most serious poisonous weed that endangers grassland animal husbandry in the world. It is distributed in Russia, Canada, Morocco, Australia, Mexico, Spain, Brazil, Egypt, Iceland and other countries. In my country, there are 44 species of locoweed plants, mainly distributed in Inner Mongolia, Ningxia, Gansu, Qinghai, Xinjiang, Tibet, Shaanxi, Sichuan and other provinces, with a distribution area of ​​more than 4 million hectares, and the economic losses caused by locoweed poisoning every year It is as high as more than 1.2 billion yuan. Therefore, the research on locowee...

Claims

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Application Information

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IPC IPC(8): C07D311/58
Inventor 曹光荣童德文赵宝玉葛鹏斌
Owner 葛鹏斌
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