Extraction, separation and purification method of aconitum alkaloid

A technology for separation and purification of alkaloids, applied in the direction of organic chemistry, etc., can solve the problems of easy degradation in the extraction process, large consumption of organic solvents, and low purity of products, and achieve the effect of accelerating separation speed, improving extraction rate, and high purity

Active Publication Date: 2021-04-23
NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these inventions have been improved and perfected compared with previous literatures, there are still problems such as large consumption of organic solvents, high production costs, easy degradation in the extraction process, and low product purity.

Method used

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  • Extraction, separation and purification method of aconitum alkaloid
  • Extraction, separation and purification method of aconitum alkaloid
  • Extraction, separation and purification method of aconitum alkaloid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Extraction: crush the medicinal material containing aconitum alkaloids, and pass through a 100-mesh sieve to obtain medicinal material powder. Take 1.0kg of medicinal material powder, add 2L of acidified ethanol solution, and use ultrasonic power density of 200W / cm at 25°C 2 And ultrasonic frequency 100kHz, ultrasonic extraction for 30min, filter, filter out insoluble matter, use 25mL petroleum ether to degrease and repeat twice, use ammonia water to alkalinize to pH = 9, and distill the solvent under reduced pressure at 40°C to obtain crude alkaloid.

[0041] (2) Separation: Weigh 0.50 g of the crude alkaloid obtained above, select a mixed solvent containing ions doped as the HSCCC solvent system, add 200 mL of the HSCCC solvent system and the crude alkaloid into the separatory funnel, oscillate to fully mix the solution , placed overnight, and separated into upper and lower phases after equilibration. With the upper phase of the solvent system as the stationary p...

Embodiment 2

[0047] (1) Extraction: crush the medicinal material containing aconitum alkaloids, and pass through a 100-mesh sieve to obtain medicinal material powder. Take 1.0kg of medicinal material powder, add 1L of acidified ethanol solution, extraction temperature is 20°C, ultrasonic power density is 150W / cm 2 At an ultrasonic frequency of 10 kHz, ultrasonically extract for 30 min, filter to remove insoluble matter, degrease with 25 mL of petroleum ether and repeat twice, alkalinize with ammonia water to pH=9, and distill off the solvent under reduced pressure at 40°C to obtain a crude alkaloid.

[0048] (2) Separation: Weigh 0.50 g of the crude alkaloid obtained above, select a mixed solvent containing ions as the HSCCC solvent system, add 100 mL of the HSCCC solvent system and the crude alkaloid into the separatory funnel, and oscillate to fully mix the solution , placed overnight, and separated into upper and lower phases after equilibration. With the upper phase of the solvent sys...

Embodiment 3

[0053] (1) Extraction: crush the medicinal material containing aconitum alkaloids, and pass through a 100-mesh sieve to obtain medicinal material powder. Take 1.0kg of medicinal material powder, add 5L of acidified ethanol solution, extraction temperature is 30°C, ultrasonic power density is 10W / cm 2 And ultrasonic frequency 80kHz, ultrasonic extraction for 30min, filter to remove insoluble matter, degrease with 25mL petroleum ether and repeat twice, alkalinize with ammonia water to pH=9, distill off the solvent under reduced pressure at 40°C to obtain crude alkaloid.

[0054] (2) Separation: Weigh 0.50 g of the crude alkaloid obtained above, select a mixed solvent containing ions doped as the HSCCC solvent system, add 500 mL of the HSCCC solvent system and the crude alkaloid into the separatory funnel, oscillate to fully mix the solution , placed overnight, and separated into upper and lower phases after equilibration. With the upper phase of the solvent system as the statio...

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Abstract

The invention discloses an extraction, separation and purification method of aconitum alkaloid, which belongs to the technical field of alkaloid extraction. The method comprises the following steps of by taking plant tubers containing aconitum alkaloid as raw materials, crushing, sieving, performing ultrasonic-assisted extraction by adopting an acidified ethanol solution, and removing a solvent through deesterification, alkalization and reduced pressure distillation to obtain crude alkaloid, then separating by adopting high-speed counter-current chromatography, finally preparing high-content aconitum alkaloid monomers by adopting reversed-phase high-performance liquid-phase semi-preparative chromatography, carrying out ultraviolet online detection, collecting a target object, and carrying out freeze drying to obtain aconitine, aconitine, neoaconitine and aconitine yunnanense with purity greater than 98.0%. By adopting the preparation method disclosed by the invention, the separated product is high in yield, high in purity, short in process, low in cost and easy to industrialize.

Description

technical field [0001] The invention relates to the technical field of extraction, separation and purification of alkaloids, in particular to a method for extraction, separation and purification of aconitum alkaloids. Background technique [0002] Aconitum carmichaeli Debx. is a ranunculaceae plant, and its mother root is called Aconitum, which is an antispasmodic, curative for rheumatism and neuralgia. Lateral roots (zigens) are used as medicine and are called aconite. It has the functions of restoring yang, expelling cold, and dispelling rheumatism. Treatment of profuse sweating and death of yang, Jueni of the limbs, cholera tendons, cold pain in the waist and knees due to weak kidney yang, cold body and limbs, lack of energy, wind-cold damp pain, beriberi and other diseases. Aconitum is cultivated in Sichuan, Shaanxi, Yunnan, Guizhou, Hebei, Hunan, Hubei, Jiangxi, Gansu and other provinces. [0003] In the medicinal materials of the genus Aconitum, the alkaloids are no...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D221/22
CPCC07D221/22
Inventor 金米聪何仟蔡美强张昱周健陈晓红
Owner NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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