Technique for spherosinin purification with continuous column chromatography

A technology of swainsonine and column chromatography, which is applied in the field of natural product chemistry research, can solve the problems of low yield, complex process and high cost, and achieve the effects of high extraction rate, simple process flow and low cost.

Inactive Publication Date: 2008-09-24
贺武利 +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a process for purifying swainsonine by continuous column chromatography, so as to overcome the disadvantages of complex process, high cost and low yield in the prior art

Method used

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  • Technique for spherosinin purification with continuous column chromatography
  • Technique for spherosinin purification with continuous column chromatography
  • Technique for spherosinin purification with continuous column chromatography

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Embodiment 1: the extraction of swainsonine in Oxytropis gansu

[0041] (1) Pretreatment of locoweed: Picked Oxytropis gansuensis was naturally air-dried for a week, then dried in an oven at 60°C to completely remove moisture, pulverized into powder with a pulverizer, and stored in a dry place.

[0042] (2) Obtaining of Locoweed extract: 500g of Gansu Oxytropis dry grass was extracted by cold soaking with 3L of edible ethanol 4 times, each time for 7 days, filtered, combined ethanol liquid, and ethanol was recovered under reduced pressure to obtain 64.8g of total extract. The extraction rate is 12.96%.

[0043] (3) Polar macroporous adsorption resin (YWD-06, produced by Yuanwei Chemical Co., Ltd., Cangzhou, Hebei) for the preliminary separation of swainsonine in locoweed extract:

[0044] 1. Pretreatment of Locoweed Extract: Weigh 10.058g of Locoweed Extract obtained and fully dissolve it with 30ml of methanol-water (5:1, v / v), centrifuge, filter, discard the residue, ...

Embodiment 2

[0054] Embodiment 2: Extraction of swainsonine in Oxytropis japonica

[0055] (1) Pretreatment of locoweed: the picked Oxytropis chrysalis is naturally air-dried, dried in an oven to remove moisture completely, pulverized into powder by a pulverizer, and stored in a dry place.

[0056] (2) Acquisition of Locoweed Extract: 500g of Oxytropis japonicus hay was cold soaked and extracted with 5L of 70% methanol for 5 times, each time for 5 days, filtered, combined ethanol solution, and ethanol was recovered under reduced pressure to obtain 59.3g of total extract , The extraction rate is 11.86%.

[0057] (3) Polar macroporous adsorption resin (commercially available D101) for the preliminary separation of swainsonine in the extract of locoweed:

[0058] 1. Pretreatment of Locoweed Extract: Weigh 10.032g of Locoweed Extract obtained and fully dissolve it with 40ml of methanol-water (4:1, v / v), centrifuge, filter, discard the residue, combine the supernatant, Concentrated for later ...

Embodiment 3

[0068] Embodiment 3: Extraction of swainsonine in mutated Astragalus membranaceus

[0069] (1) Pretreatment of locoweed: the picked mutated Astragalus membranaceus was naturally air-dried for a week, then dried in an oven at 60°C to completely remove water, pulverized into powder with a pulverizer, and stored in a dry place.

[0070] (2) Acquisition of Locoweed Extract: Extract 500g of Astragalus mutator with 3L of edible ethanol cold immersion for 6 times, each time for 8 days, filter, combine the ethanol solution, recover ethanol under reduced pressure, and obtain 65.3g of total extract, with an extraction rate of 13.06 %.

[0071] (3) Polar macroporous adsorption resin (YWD-03, produced by Yuanwei Chemical Co., Ltd., Cangzhou, Hebei) for the preliminary separation of swainsonine in locoweed extract:

[0072] 1. Pretreatment of Locoweed Extract: Weigh 10.086g of Locoweed Extract obtained and fully dissolve it with 20ml of methanol-water (5:1, v / v), centrifuge, filter, disca...

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Abstract

Belonging to the field of chemical analyses on natural products, the present invention relates to a method for extracting, separating, purifying and testing natural products, in particular to a technique for extracting swainsonine by continuous column chromatography. The present invention resolves the defects of the prior art, including a complex process, high cost and low yield rate. The solution orderly includes the following steps: (1) the preprocessing of locoweed; (2) the acquisition of locoweed extract; (3) the preparation of a crude product: The extract is roughly separated by polar macroporous adsorption resin and, after TLC test, merged with eluant containing swainsonine to serve as the crude product for later use; (4) the purification of the swainsonine: The crude product is purified by silica gel column chromatography, and by the TLC test and the GC test, the parts of the swainsonine, which have relative content larger than or equal to 10 percent, are respectively collected; (5) the acquisition of a pure swainsonine product by the HPLC test; the parts collected in the step (4) undergo the HPLC test in order to collect eluate in the appearance time period of the swainsonine, and after the solvent is evaporated, the pure swainsonine product can be produced by recrystallization.

Description

1. Technical field [0001] The invention belongs to the field of chemical research of natural products, and in particular relates to extraction, separation, purification and detection methods of natural products, in particular to a process for extracting swainsonine by continuous column chromatography. 2. Background technology [0002] Locoweed is a very common weed in Northwest my country. It is easy to cause poisoning after being eaten by livestock, and it is often regarded as a harmful weed. Studies in recent years have shown that the main toxic component of locoweed - swainsonine, can not only inhibit the growth of cancer cells, but also activate the body's immunity and reduce the side effects of cancer patients caused by chemotherapy. Therefore, it is a promising natural medicine. [0003] There are three main sources of swainsonine (SW): ① Extraction and separation from plants. The currently known plants containing swainsonine are mainly Astragalus and Oxytopis plants...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/04A61K36/48A61P35/00
Inventor 贺武利师宗臣辛发定刘彬慧
Owner 贺武利
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