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Preparation method of acronycine

The invention relates to a preparation-type technology for citrus alkaloids, which is applied in the field of preparation of citron alkaloids, can solve problems such as the extraction and purification method of citron alkaloids, and achieves high economic benefit and academic value, simple operation and short time-consuming. Effect

Inactive Publication Date: 2014-10-01
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there is no report on the extraction and purification method of berberine in China

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Take 1 kg of mountain oil mandarin root, crush it into coarse powder, feed it from the feed inlet of the head of the continuous countercurrent ultrasonic extraction equipment, add 10 times of 95% ethanol solution from the solvent inlet at the tail of the continuous countercurrent ultrasonic extraction equipment, and carry out continuous countercurrent at 55 °C Ultrasonic extraction for 20 minutes, the ultrasonic frequency is 80KHz, to obtain the extract, the extract is decompressed and the reagents are recovered to obtain the extract, add alumina (120 mesh) to the extract, mix well, dry and pack the column, and use 7 times the column volume of chloroform- Acetone (1:1) mixed solution was eluted, TLC detection was performed, and the fraction of berberine was collected and concentrated to obtain a concentrated solution. Add methanol to the concentrated solution until it just dissolves. The dissolved solution is filtered through a 0.45 μm microfiltration membrane to obtain ...

Embodiment 2

[0020] Take 1 kg of mountain oil mandarin root, crush it into coarse powder, feed it from the feed inlet of the head of the continuous countercurrent ultrasonic extraction equipment, add 10 times of 80% ethanol solution from the solvent inlet at the tail of the continuous countercurrent ultrasonic extraction equipment, and carry out continuous countercurrent at 45 °C Ultrasonic extraction for 100min, the ultrasonic frequency is 60KHz, to obtain the extract, the extract is decompressed and the reagent is recovered to obtain the extract, add alumina (80 mesh) and mix well, dry and pack the column, and use 4 times the column volume of chloroform-acetone (1: 1) Elution with the mixed solution, TLC detection, collection of the alkaloid fraction, and concentration to obtain a concentrated solution. Add methanol to the concentrated solution until it just dissolves. The dissolved solution is filtered through a 0.45 μm microfiltration membrane to obtain a sample solution. Take the filtr...

Embodiment 3

[0022] Take 10 kg of mountain oil mandarin root, crush it into coarse powder, feed it from the feed inlet of the head of the continuous countercurrent ultrasonic extraction equipment, add 6 times of 70% ethanol solution from the solvent inlet at the tail of the continuous countercurrent ultrasonic extraction equipment, and carry out continuous countercurrent at 35 °C Ultrasonic extraction for 50min, the ultrasonic frequency is 50KHz, to obtain the extract, the extract is decompressed and the reagent is recovered to obtain the extract, add alumina (100 mesh) and mix well, dry and pack the column, and use 6 times the column volume of chloroform-acetone (1: 1) Elution with the mixed solution, TLC detection, collection of the alkaloid fraction, and concentration to obtain a concentrated solution. Add methanol to the concentrated solution until it just dissolves. The dissolved solution is filtered through a 0.45 μm microfiltration membrane to obtain a sample solution. Take the filtr...

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Abstract

The invention discloses a preparation method of acronycine. The preparation method comprises the following steps of (1) weighting coarse powder of acronychia pedunculata roots, and carrying out continuous countercurrent ultrasonic extraction by using 70-95% ethanol solution to obtain an extracting solution; (2) concentrating the extracting solution, and carrying out aluminum oxide column chromatography; (3) carrying out preparative liquid chromatographic separation; (4) carrying out chloroform and acetone recrystallization to obtain a high-purity acronycine crystal product. The method disclosed by the invention is simple, high in acronycine yield and capable of obtaining high-purity products; in addition, the acronycine has relatively high economic and academic values.

Description

technical field [0001] The invention belongs to the field of natural plant extraction, and in particular relates to a preparation method of caperine. Background technique [0002] Acronycine, molecular formula C 20 h 19 NO 3 , molecular weight 321.36, hardly soluble in water, soluble in organic solvents such as ethanol and chloroform. [0003] Capreline is an alkaloid compound extracted from the root of the Rutaceae plant Acronychia pedunculata (L.) Miq. Experimental studies have shown that caperine can inhibit cell mitosis and reduce the division index of Yoshida ascites tumor cells. It can affect the production of nucleic acid in cancer cells, significantly reduce the RNA content in the spleen of L615 mice, but has no significant effect on the RNA and DNA content in normal animal tissues. It has a broad spectrum of anti-animal cancer. Among the 17 tumor spectrums, it has a significant inhibitory effect on 12 tumor spectrums. It is insensitive to current clinical chemo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/052
CPCC07D491/052
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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