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Method for extracting and separating Huperzine from huperzine serrate

A technology of huperzine A and Melaleuca tower, which is applied in the field of extracting and separating huperzine A from Melaleuca tower, can solve the problems of low yield and high production cost, and achieve reduced production cost, high production efficiency and easy control Effect

Active Publication Date: 2008-03-05
SHAANXI JIAHE PHYTOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a method for extracting and separating huperzine A from the Melaleuca tower, which solves the technical problems of low yield and high production cost in the background technology

Method used

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  • Method for extracting and separating Huperzine from huperzine serrate
  • Method for extracting and separating Huperzine from huperzine serrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] (1) Extraction: select 100 kilograms of Melaleuca tower raw material, the raw material content is: 0.017%, pulverize to 10-20 mesh. Reflux extraction with 80% ethanol for 3 times, 1 hour each time. The extract was concentrated to a specific gravity of 1.10.

[0048] (2) Acid adjustment: add 1 times the amount of water according to the volume, and adjust the pH to 3.0. Filter and discard the filter residue to obtain the filtrate.

[0049] (3) Cation exchange resin chromatography: use the filtrate in step (2) with a cation exchange resin. Wash with water first, and then elute with 8% ammonia water and ethanol. The eluate was collected and concentrated into an extract. Mix the sample with a certain amount of silica gel to obtain a sample mixed with silica gel.

[0050] (4) Silica gel column chromatography: the sample mixed with silica gel and silica gel are wet-packed in a column at a weight ratio of 1:20. Acetone and chloroform were prepared as a mixed eluent at a v...

Embodiment 2

[0053] (1) Extraction: select 100 kg of Melaleuca tower raw material (raw material content: 0.017%), and grind to 20-30 mesh. Reflux extraction with 90% ethanol three times for 2 hours each time. The extract was concentrated to a specific gravity of 1.10.

[0054] (2) Acid adjustment: add 1 times the amount of water according to the volume, and adjust the pH to 4.0. Filter, discard the filter residue, and concentrate the filtrate.

[0055] (3) Cation exchange resin chromatography: the filtrate of step (2) is separated by cation exchange resin chromatography, washed with water first, and then eluted with 10% ammonia water and ethanol. The eluate was collected and concentrated into an extract.

[0056] (4) Silica gel column chromatography: the sample mixed with silica gel and silica gel are wet-filled at a weight ratio of 1:20. Take methanol and petroleum ether at a volume ratio of 1:7 to prepare a mixed eluent for elution, identify by thin-layer plate method, and collect th...

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Abstract

The process of extracting and separating huperzine A from huperzine serrate includes the steps of crushing huperzine serrate, reflux extracting in organic solvent, regulating acidity, filtering, chromatographic separation of the filtrate with cationic exchange resin, eluting, concentrating to obtain extractum, eluting on silica gel column with mixed eluant, collecting the eluted liquid, concentrating, letting stand to separate out huperzine A, and re-crystallizing to obtain refined huperzine A product. The present invention has high yield, low production cost and huperzine A product purity as high as 98 %.

Description

technical field [0001] The invention relates to a method for extracting alkaloids, in particular to a method for extracting and separating huperzine A from a Melaleuca tower. Background technique [0002] At present, there are many separation and extraction methods for huperzine A, but all of them have shortcomings or deficiencies in varying degrees. [0003] The Chinese patent application CN1207285C announced on June 22, 2005 discloses a "method for extracting huperzine A from the Chinese herbal medicine Melaleuca pagoda". Layer tower dried powder, treated with dilute alkali, extracted with chloroform, and concentrated to extract. The main defects of this method are: the method of liquid-liquid extraction used is prone to emulsification, and the loss of huperzine A is relatively serious, resulting in a low yield. [0004] The Chinese patent CN1704405A published on December 7, 2005 "A Method for Analyzing, Separating and Preparing Huperzine A and Huperzine B" and the afore...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D221/22A61K36/36
CPCY02P20/582
Inventor 祁春雷肖红杨军仁高娟邓尚勇王晓莹王春德
Owner SHAANXI JIAHE PHYTOCHEM
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