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Method for purifying huperzine A

A technology for huperzine A and a purification method is applied in the field of purifying huperzine A by membrane separation and medium pressure alumina column, which can solve the problems of low degree of industrialization, high energy consumption, small production volume and the like, and reduce the use of reagents. , low energy consumption, large sample loading effect

Inactive Publication Date: 2010-11-10
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] As mentioned above, existing methods for producing huperzine A have problems such as high energy consumption, small production capacity, and low degree of industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Extraction: Pulverize the melaleuca medicinal materials, take 10kg and 60Lph2 hydrochloric acid aqueous solution, put it into a small extraction tank, heat at 40°C, extract dynamically for 1 hour, extract 4 times, and combine the extracts.

[0032] Membrane filtration: the extract is first treated with a microfiltration membrane, and then added to a hollow cellulose membrane with a molecular weight cut-off of 3000 for ultrafiltration. The pressure is controlled at about 0.5Mpa. The concentrated solution was obtained in 2L.

[0033] Extraction: add ammonia water to the concentrated solution to adjust the pH to 9, add 1L of chloroform, stir and extract, extract 3 times, combine the chloroform layers, and recover the chloroform to 100ml.

[0034] Alumina column chromatography: take 500g basic alumina column, inject 100ml concentrated solution, take 5L methanol and 4L methanol-chloroform mixture (1:1), pressurize and inject the alumina column in sequence to elute impurities...

Embodiment 2

[0037] Extraction: Pulverize the melaleuca medicinal materials, take 10kg and 150Lph3 sulfuric acid aqueous solution, put it into a small extraction tank, heat at 60°C, extract dynamically for 3 hours, extract twice, and combine the extracts.

[0038] Membrane filtration: the extract is first treated with a microfiltration membrane, and then added to a hollow cellulose membrane with a molecular weight cut-off of 6000 for ultrafiltration. The pressure is controlled at about 0.3Mpa. The concentrated solution was obtained in 1.5 L.

[0039] Extraction: add ammonia water to the concentrated solution to adjust the pH to 10, add 700ml of chloroform, stir and extract, extract 5 times, combine the chloroform layers, and recover the chloroform to 100ml.

[0040] Alumina column chromatography: take 600g basic alumina column, inject 100ml concentrated solution, take 5L methanol and 4L methanol-chloroform mixture (1:1), pressurize and inject the alumina column in turn to elute impurities,...

Embodiment 3

[0043] Extraction: Pulverize the melaleuca medicinal materials, take 20kg and 120Lph3 acetic acid aqueous solution, put it into a small extraction tank, heat at 50°C, extract dynamically for 2 hours, extract 3 times, and combine the extracts.

[0044] Membrane filtration: the extract is first treated with a microfiltration membrane, and then added to a hollow cellulose membrane with a molecular weight cut-off of 3000 for ultrafiltration. The pressure is controlled at about 0.4Mpa. The concentrated solution was obtained in 4L.

[0045] Extraction: add ammonia water to the concentrated solution to adjust the pH to 10, add 2L of chloroform, stir and extract, extract 3 times, combine the chloroform layers, and recover the chloroform to 300ml.

[0046] Alumina column chromatography: take 1200g basic alumina column, inject 300ml concentrated solution, take 12L methanol and 9.6L methanol-chloroform mixture (1:1), pressurize and inject into the alumina column to elute impurities, frac...

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Abstract

The invention relates to a method for purifying huperzine A, which is easy for industrialized production. The method comprises the following production steps of: crushing of raw materials, acid water heating and extraction, membrane filtration, impurity removal and condensation, aminated chloroform extraction and condensation, medium-pressure alumina column chromatography, chloroform methanol recrystallization, and drying of a finished product. The method for producing the huperzine A has low energy consumption and short period.

Description

Technical field: [0001] The invention relates to a method for purifying huperzine A, in particular to a method for purifying huperzine A by adopting membrane separation and medium-pressure alumina column. Background technique: [0002] Huperzine A [0003] Molecular weight: 242.32; Molecular formula: C15H18N2O; [0004] Soluble in chloroform, soluble in methanol, ethanol, slightly soluble in water. [0005] Huperzine A is an alkaloid extracted from the unique Chinese plant Melaleuca, and it is a world-class new drug created by China. Belonging to reversible cholinesterase inhibitors, it is currently one of the safest and most effective drugs for the treatment of benign memory impairment and Alzheimer's disease. [0006] Huperzine A, which is a Chinese patent medicine, has many extraction and purification methods. [0007] "Extraction Method Selection of Huperzine A in Melaleuca Tower" published by Li Hongying et al., which discloses the optimization of the extraction eff...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D221/22
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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