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A kind of extraction and separation method of cytisine

A separation method, the technology of cytisine, applied in the direction of organic chemistry, etc., can solve the problems of low purity, long cycle and high cost of separating cytisine, and achieve the effect of raw material source method, simple regeneration and easy operation

Active Publication Date: 2016-01-06
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Purpose of the invention: In order to solve the problems of low purity, high cost, heavy pollution and long cycle of extracting and separating cytisine in the prior art, the purpose of the present invention is to provide a low-cost, high-purity and suitable for industrial application of gorse Alkaline extraction and separation method

Method used

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  • A kind of extraction and separation method of cytisine
  • A kind of extraction and separation method of cytisine
  • A kind of extraction and separation method of cytisine

Examples

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Effect test

Embodiment 1

[0027] Take 100kg of the raw material of the herbaceous bean and grind it, pass the raw material obtained through the above-mentioned treatment through a 10-mesh sieve, and use 8 times the mass of ethanol with a concentration of 95% to reflux and extract for 1 hour to obtain an extract. Concentrate the extract to a mass concentration of 1.0g / mL, adjust the pH to 8.0, and put it on a pretreated X-5 macroporous resin column (315×1500mm), with a sample volume of 0.1 times the column volume, let it stand for 30min, and then Elute with 8 times column volume of pure water and 8 times column volume of 10% ethanol aqueous solution, the elution rate is 1.0mL / min, collect the 10% ethanol eluate, and then concentrate to a mass concentration of 1.0g / mL, Adjust the pH to 9.0, put on the pretreated DM18 macroporous resin column (315×1500mm), the loading volume is 0.1 times the column volume, let stand for 30min, then use 5 times the column volume of pure water, 5 times the column volume of ...

Embodiment 2

[0049]Take 100 kg of the raw material of the herbaceous bean and grind it, pass the raw material obtained from the above-mentioned treatment through a 20-mesh sieve, and use 10 times the amount of methanol with a concentration of 35% to reflux extract for 3 hours to obtain an extract. Concentrate the extract to a mass concentration of 0.5g / mL, adjust the pH to 9.0, and put it on a pretreated AB-8 macroporous resin column (315×1500mm), with a sample volume of 0.2 times the column volume, let it stand for 50min, and then Use 10 times column volume of pure water and 10 times column volume of 30% ethanol aqueous solution to elute, the elution rate is 3mL / min, collect the 30% ethanol eluate, then concentrate to a mass concentration of 0.5g / mL, adjust pH to 8.0, on the pretreated DM18 macroporous resin column (315 × 1500mm), the sample volume is 0.2 times the column volume, let stand for 20min, and then use 6 times the column volume of pure water, 6 times the column volume of 10 % e...

Embodiment 3

[0071] Take 100 kg of the raw material of the herba bean and grind it, pass the raw material obtained from the above treatment through a 60-mesh sieve, and reflux extract with 4 times the amount of ethanol with a concentration of 65% for 4 hours to obtain an extract. Concentrate the extract to a mass concentration of 1.5g / mL, adjust the pH to 8.5, and put it on a pretreated X-5 macroporous resin column (315×1500mm), with a sample volume of 0.01 times the column volume, let it stand for 10min, and then Elute with 5 times column volume of pure water and 5 times column volume of 40% ethanol aqueous solution, the elution rate is 5mL / min, collect the 40% ethanol eluate, then concentrate to a mass concentration of 1.5g / mL, adjust pH to 8.5, on the pretreated DM2 macroporous resin column (315 × 1500mm), the sample volume is 0.01 times the column volume, let stand for 40min, followed by 4 times the column volume of pure water, 4 times the column volume of 10 % ethanol water solution, ...

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Abstract

The invention provides a method for extracting and separating cytisine. The method comprises the following steps: extracting, namely grinding thermopsis lanceolata seeds, adding an organic solvent water solution with the mass being 4-10 times that of the ground thermopsis lanceolata seeds, carrying out reflux extraction for 1-4 hours, and concentrating an extracting solution until the mass concentration is 0.5-1.5 g / ml so as to obtain a concentrated solution; carrying out macroporous resin combination separation, namely carrying out primary separation by polystyrene nonpolar resin with the aperture of 130-300 angstroms and the specific surface area of 480-600 m<2> / g, and carrying out secondary separation by polystyrene nonpolar resin with the aperture of 50-80 angstroms and the specific surface area of 800-1100 m<2> / g; re-crystallizing to obtain cytisine. The method is simple in process and easy and convenient to operate, adopts high available raw materials and is low in cost; the separation materials are easy to regenerate, nontoxic and pollution-free; the method is suitable for industrialization mass production.

Description

technical field [0001] The invention belongs to the field of traditional Chinese medicine chemistry, in particular to a method for extracting and separating alkaloids, in particular to a method for extracting and separating cytisine. Background technique [0002] Cytisine, whose molecular formula is C 11 h 14 0N 2 , the molecular weight is 190.24. Cytisine has significant biological activity. It is clinically used for intravenous injection of 0.15% aqueous solution of cytisine to rescue reflex apnea, shock and neonatal asphyxia caused by surgery and various traumas. Recent studies have shown that cytisine also has anti-arrhythmia, anti-microbial infection, anti-ulcer and strong anti-cancer activity. [0003] Most of the existing extraction and purification processes for cytisine are traditional processes. Chinese patent 201010182690.9 discloses a method for extracting cytisine, including CO 2 After supercritical extraction, macroporous resin chromatography separation, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D471/18
CPCC07D471/18
Inventor 廖志新叶润纪兰菊孙洪发胥廉谦施天一
Owner SOUTHEAST UNIV
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