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Method for separating and purifying tetrandrine and tetrandrine from tetrandrine

A technology for tetrandrine and tetrandrine, applied in the chemical industry, can solve the problems of inability to meet market demand, small production scale, low product purity, etc., and achieve the effects of shortening separation time, saving reagents, and high purity

Inactive Publication Date: 2011-12-21
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above-mentioned various methods can only obtain single-component products, or the obtained products have low purity, or the systems used are relatively complicated, and some have high production costs and small production scales, which cannot meet market demand.

Method used

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  • Method for separating and purifying tetrandrine and tetrandrine from tetrandrine
  • Method for separating and purifying tetrandrine and tetrandrine from tetrandrine
  • Method for separating and purifying tetrandrine and tetrandrine from tetrandrine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Take 100g of pulverized Fangji medicinal material, add 0.5L 50% ethanol, heat and reflux for 100 minutes, separate the residue and extract; add 0.5L 50% ethanol to the residue and reflux twice, each time for 60 minutes, separate the residue and extract; combine the extracts obtained by the above-mentioned reflux for 3 times, and recover ethanol by distillation under reduced pressure to obtain the crude extract of Fangji.

[0028] Dissolve the extract of Fangji crude extract with 0.2L of 0.5% hydrochloric acid, let it stand for 36 hours, and filter to remove the precipitate to obtain a solution; adjust the pH of the above solution to 8 with ammonia water, let it stand for 24 hours, then filter to obtain a precipitate, and let the precipitate dry in the air dry to obtain the crude extract of Fangji alkaloid.

[0029] Diethyl ether-phosphate buffer was used as a high-speed countercurrent chromatography two-phase solvent system to separate and purify the extract of Fangji. ...

Embodiment 2

[0031] Take 100g of pulverized powdered Tetragalus, add 2L of 55% ethanol, heat and reflux for 90 minutes, separate the residue and extract; add 1L of 55% ethanol to the residue and reflux twice, each time for 50 minutes, separate the residue and extract liquid; the above-mentioned 3 times of reflux obtained extracts were combined, the ethanol was recovered by distillation under reduced pressure, and the crude extract of tetrandrine was obtained.

[0032]Dissolve the extract of Fangji crude extract with 0.16L of 1.0% hydrochloric acid, let it stand for 36 hours, and filter to remove the precipitate to obtain the solution; adjust the pH of the above solution to 10 with ammonia water, let it stand for 36 hours, then filter to obtain the precipitate, and let the precipitate dry in the air dry to obtain the crude extract of Fangji alkaloid.

[0033] Diethyl ether-phosphate buffer was used as a high-speed countercurrent chromatography two-phase solvent system to separate and purify...

Embodiment 3

[0035] Take 100g of pulverized Fangji medicinal material, add 0.5L 60% ethanol, heat and reflux for 80 minutes, separate the residue and extract; add 0.5L 60% ethanol to the residue and reflux twice, each time for 50 minutes, separate the residue and extract; combine the extracts obtained by reflux for the above 3 times, and recover ethanol by distillation under reduced pressure to obtain the crude extract of tetrandrine.

[0036] Dissolve the extract of Fangji crude extract with 0.08L of 4.0% hydrochloric acid, let it stand for 12 hours, and then filter to remove the precipitate to obtain a solution; adjust the pH of the above solution to 8 with ammonia water, let it stand for 24 hours, then filter to obtain a precipitate, and let the precipitate dry in the air dry to obtain the crude extract of Fangji alkaloid.

[0037] Diethyl ether-phosphate buffer was used as a high-speed countercurrent chromatography two-phase solvent system to separate and purify the extract of Fangji. ...

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Abstract

The invention relates a method for separating and purifying fangchinoline and tetrandrine from stephania tetrandra. The stephania tetrandra is taken as a raw material, and the method comprises the following steps of: (1) preparation of crude extract; (2) pre-separation of acid dissolution and alkaline sedimentation; and (3) purification of a high-speed reverse flow chromatograph to obtain the fangchinoline and tetrandrine with purities over 98%. According to the method disclosed by the invention, alkaloid in the stephania tetrandra medicinal material is extracted by alcohol, pre-separated by the acid dissolution and alkaline sedimentation and purified by the high-speed reverse flow chromatograph, and the technical process is green and environemtal-friendly and does not have serious damageto the environment.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for separating and purifying fangchinoline and fangji from traditional Chinese medicine fangji. Background technique [0002] Fenfangji is the root tuber of Phyllostachys chinensis, a plant belonging to the genus Fangji. It is one of the commonly used Chinese herbal medicines in my country. It has the functions of dispelling wind and dampness, diuresis, reducing swelling, promoting qi and relieving pain. The main active ingredient of tetrandrine is alkaloid, such as tetrandrine, fangchinoline and so on. Tetanus alkaloids have extensive physiological activities of antihypertensive, anti-myocardial ischemia and reperfusion injury, anti-arrhythmia, anti-inflammation and immunosuppression, and anti-tumor. [0003] There are existing literature reports on the method of extracting and purifying alkaloid components from Tetradendronae. Li Xingnuo et al. [Isolation...

Claims

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Application Information

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IPC IPC(8): C07D491/18
CPCY02P20/582
Inventor 孙爱玲李霞柳仁民
Owner LIAOCHENG UNIV
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