Method for preparing annotine

A technology of cenmanine and crude drug, which is applied in the field of preparation of cenmanine extraction from plants, can solve the problems such as the unsuitable industrial production process report of cenmanine, and achieve the advantages of large-scale production operation, low energy consumption and pollution small effect

Inactive Publication Date: 2010-09-22
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the prior art, there is no report on the preparation proces

Method used

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  • Method for preparing annotine

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Embodiment 1

[0017] Take 10Kg of the whole Lycopodium clover, crush it, add hydrochloric acid aqueous solution with pH=2 for percolation, the percolation speed is 5L / min, collect the percolation solution with 5 times the volume of the crude drug, filter, concentrate to 1ml / g crude drug, concentrate Adjust the pH value to 12 with ammonia water, add an equal volume of ethyl acetate to extract twice, combine the ethyl acetate layers, recover the solvent under reduced pressure and dry to obtain the total alkaloids, add them to an alumina chromatography column, elute with methanol, and collect the initial 4 times the column volume of the eluate, recovered the solvent, added acetone to crystallize, separated and dried to obtain 13.5 g of ethanine, which was detected by HPLC with a purity of 99.1%.

Embodiment 2

[0019] Take 10Kg of whole Lycopodium clover, crush it, add pH=5 aqueous hydrochloric acid solution for percolation, the percolation rate is 20L / min, collect 8 times the volume of crude drug quality, filter, concentrate to 1ml / g crude drug, concentrate Adjust the pH value to 14 with ammonia water, add an equal volume of ethyl acetate to extract 4 times, combine the ethyl acetate layers, recover the solvent under reduced pressure and dry to obtain the total alkaloids, add them to an alumina chromatography column, elute with methanol, and collect the initial 4 times the column volume of the eluate, recovered the solvent, added acetone to crystallize, separated and dried to obtain 10.5 g of ethanine, which was detected by HPLC with a purity of 97.9%.

Embodiment 3

[0021] Take 10Kg of whole Lycopodium clover, crush it, add pH=3 aqueous hydrochloric acid solution for percolation, the percolation rate is 10L / min, collect 6 times the volume of the crude drug, filter, concentrate to 1ml / g crude drug, concentrate Adjust the pH value to 13 with ammonia water, add an equal volume of ethyl acetate to extract three times, combine the ethyl acetate layers, recover the solvent under reduced pressure and dry to obtain the total alkaloids, add them to an alumina chromatography column, elute with methanol, and collect the initial 4 times the column volume of the eluate, recovered the solvent, added acetone to crystallize, separated and dried to obtain 14.6 g of ethanine, which was detected by HPLC with a purity of 99.6%.

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Abstract

The invention provides a method for preparing annotine, which has the advantages of easy operation, less pollution and low energy consumption. The method comprises the following process steps of: taking the whole plant of lycopodium annotinum; crushing the lycopodium annotinum, and adding the crushed lycopodium annotinum into aqueous acid with a pH value of 2 to 5 for percolation, wherein the percolation speed is 0.5 to 2ml/g crude medicament.min; collecting percolating solution of which the volume is 5 to 8 times mass of the crude medicament; filtering the percolating solution; condensing the percolating solution to 1ml/g crude medicament; adjusting the pH value of the percolating solution to be 12 to 14 by using strong ammonia water; adding ethyl acetate with equal volume into the mixture and extracting for 2 to 4 times; mixing ethyl acetate layers, and recovering solvents by reducing pressure; drying to obtain total alkaloid and adding the total alkaloid onto an aluminum oxide chromatographic column; eluting the total alkaloid by using methanol; collecting eluting solution of which the volume is 4 times original column volume; recovering the solvents; adding acetone for crystallizing; and separating and drying to obtain the annotine. The annotine prepared by the method has the advantages of high purity of products and easy realization of enlargement of industrial production.

Description

technical field [0001] The invention relates to a preparation method of cadmanine, in particular to a preparation method of extracting cadmanine from plants. Background technique [0002] Annotine, molecular formula: C 16 h 21 NO 3 , Molecular weight: 275.347, CAS accession number: 5096-59-3, mainly found in Lycopodium annotinum L., a plant of the family Lycopodium. Its molecular formula is as follows: [0003] [0004] Modern studies have shown that cenmanine has the functions of lowering blood pressure and antipyretic. [0005] In the prior art, there is no report on the preparation process suitable for the large-scale industrial production of cenmanine. Contents of the invention [0006] The technical problem to be solved by the present invention is to provide a method for preparing cenmanine which is beneficial to large-scale production operations and has high product purity. [0007] In order to solve the problems of the technologies described above, the pres...

Claims

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Application Information

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IPC IPC(8): C07D491/18
Inventor 王峰王琳张发成
Owner SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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