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Preparation method of colchicumautumnale

A technology for colchicine and alkali aqueous solution, which is applied in the production of bulk chemicals, organic chemistry, separation/purification of carboxylic acid amides, etc., and can solve the problems of long steps, high production cost, and low yield

Active Publication Date: 2009-12-16
YUNNAN XISHUANGBANNA BANNA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the prior art, colchicine is mainly produced by synthesis, which has long steps, low yield and high production cost

Method used

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  • Preparation method of colchicumautumnale

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Effect test

Embodiment 1

[0017] Take colchicum bulb fine powder 10Kg, add in the ammonia solution of pH=10 and soak overnight, dry, place in CO 2 Supercritical extraction in supercritical extraction device, CO 2 The flow rate is 1ml / min / g crude drug, 90% ethanol aqueous solution is selected as the entrainer, the flow rate is 0.1ml / min / g crude drug, the extraction temperature is 20°C, the pressure is 10MPa, and the extraction time is 0.5h; the extract is dissolved by adding 2% hydrochloric acid aqueous solution , filtered, added chloroform to the filtrate for extraction, removed the lower layer, adjusted the pH to 13, added chloroform for extraction, took the chloroform layer, separated it through an AB-8 macroporous adsorption resin column, and used 1% acetic acid aqueous solution as the The eluent was eluted, the eluate was collected, concentrated, recrystallized by adding acetone, washed and dried to obtain 201 mg of colchicine, which was detected by HPLC with a purity of 94.3%.

Embodiment 2

[0019] Take colchicum bulb fine powder 10Kg, add in the triethylamine aqueous solution of pH=14 and soak overnight, dry, place in CO 2 Supercritical extraction in supercritical extraction device, CO 2 The flow rate is 5ml / min / g crude drug, 90% ethanol aqueous solution is selected as the entrainer, the flow rate is 0.8ml / min / g crude drug, the extraction temperature is 80°C, the pressure is 30MPa, and the extraction time is 4h; the extract is dissolved by adding 2% hydrochloric acid aqueous solution, Filtrate, add chloroform to the filtrate for extraction, remove the lower layer, adjust the pH to 13, add chloroform for extraction, take the chloroform layer, separate it through an H-103 macroporous adsorption resin column, wash with 5% hydrochloric acid aqueous solution The eluate was eluted with a solvent, the eluate was collected, concentrated, recrystallized by adding acetone, washed and dried to obtain 238 mg of colchicine, which was detected by HPLC with a purity of 90.4%. ...

Embodiment 3

[0021] Take colchicum bulb fine powder 10Kg, add the triethylamine aqueous solution of pH=12 and soak overnight, dry, place in CO 2 Supercritical extraction in supercritical extraction device, CO 2 The flow rate is 2ml / min / g crude drug, 90% ethanol aqueous solution is selected as the entrainer, the flow rate is 0.4ml / min / g crude drug, the extraction temperature is 40°C, the pressure is 20MPa, and the extraction time is 2h; the extract is dissolved by adding 2% hydrochloric acid aqueous solution, Filtrate, add chloroform to the filtrate for extraction, remove the lower layer, adjust the pH to 13, add chloroform for extraction, take the chloroform layer, separate it through a D-101 macroporous adsorption resin column, wash with 2% hydrochloric acid aqueous solution The eluate was collected, concentrated, recrystallized by adding acetone, washed and dried to obtain 222 mg of colchicine, which was detected by HPLC with a purity of 96.2%.

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Abstract

The invention relates to a preparation method of colchicumautumnale, which is characterized by simple operation and little pollution and comprises the following processing steps: taking raw fine powder, soaking the fine powder in aqueous alkali solution overnight, drying the powder and placing the dried powder in a CO2 supercritical liquid extraction device for supercritical liquid extraction; adding 2% aqueous hydrochloric acid solution to extracts to dissolve the extracts, filtering the extracts, adding chloroform to filtrate for extraction, taking subnatant, adjusting pH value to 13, adding the chloroform for extraction, taking the chloroform layer, carrying out separation by a macroporous resin absorption column, taking aqueous acid as an eluting agent for elution, collecting eluent, concentrating the eluent, adding acetone for recrystallization, washing and drying the crystal, thus obtaining the colchicumautumnale. By adopting the invention to prepare the colchicumautumnale, the product is high in purity and industrialization enlargement is easy to realize.

Description

technical field [0001] The invention relates to a method for preparing colchicine, in particular to a method for extracting colchicine from plants. Background technique [0002] Colchicine (Colchicumautumnale) is an important phenolic alkaloid, which widely exists in a variety of Liliaceae plants. Its structural formula is as follows: [0003] [0004] Colchicine can inhibit cell mitosis and DNA synthesis, and can also inhibit the growth of cancer cells. Clinically, it can be used to treat breast cancer, skin cancer, leukemia, Hodgkin's disease, Mediterranean familial fever, etc., and has a specific effect on primary gout. In agriculture, colchicine is widely used to breed polyploid seeds. It is also a commonly used reagent in cell biotechnology. [0005] In the prior art, colchicine is mainly produced by synthesis, which has long steps, low yield and high production cost. Contents of the invention [0006] The technical problem to be solved by the present invention...

Claims

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Application Information

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IPC IPC(8): C07C233/32C07C231/24
CPCY02P20/54
Inventor 王琳范淦彬
Owner YUNNAN XISHUANGBANNA BANNA PHARMA
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