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Method for preparing picrinine

A technology for alkaloid and leaves is applied in the field of preparing alkaloid, which can solve the problems of large amount of organic solvent, serious environmental pollution, complicated process operation and the like, and achieves the effects of simple operation and low energy consumption.

Inactive Publication Date: 2012-06-27
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods have many industrial "three wastes", serious environmental pollution, large amount of organic solvents, high production costs, and cumbersome process operations.

Method used

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  • Method for preparing picrinine

Examples

Experimental program
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Effect test

Embodiment 1

[0017] The leaves of the lampstand are crushed into granules, take 10kg, use 15 times the amount of 1% sulfuric acid aqueous solution to percolate and extract, filter the extract and add a hollow cellulose ultrafiltration membrane with a molecular weight cut off of 2000 for ultrafiltration, and add a hollow fiber with a molecular weight cut off of 300 to the permeate Concentrate with plain nanofiltration membrane, pass the concentrated solution through AB-8 macroporous resin column, elute with appropriate amount of water, collect the lower column liquid and washing liquid, adjust pH9 with ammonia water, place the precipitate, centrifuge, dissolve the precipitate with 90% methanol and reflux to dissolve, add Decolorize with 1% activated carbon in the solution, filter out the activated carbon from the decolorized solution, add 1 / 10 of the volume of petroleum ether, fully stir and refrigerate to crystallize, then recrystallize the crystal with 70% ethanol solution, dry to obtain 15...

Embodiment 2

[0019] The leaves of the lampstand are crushed into granules, take 20kg, use 20 times the amount of 1% sulfuric acid aqueous solution to percolate and extract, filter the extract and add hollow cellulose ultrafiltration membrane with a molecular weight cut off of 6000 for ultrafiltration, and then add hollow fibers with a molecular weight cut off of 200 to the permeate Concentrate with plain nanofiltration membrane, pass the concentrated solution through the ADS-21 macroporous resin column, elute with appropriate amount of water, collect the lower column liquid and washing liquid, adjust the pH10 with ammonia water, place the precipitate, centrifuge, dissolve the precipitate with 99% methanol and reflux to dissolve, add Decolorize with 0.5% activated carbon in the solution, filter out the activated carbon from the decolorized solution, add 1 / 12 volume of petroleum ether, fully stir and refrigerate to crystallize, then recrystallize the crystal with 85% ethanol solution, dry to o...

Embodiment 3

[0021] The leaves of the lampstand are crushed into granules, take 50kg, use 20 times the amount of 1% sulfuric acid aqueous solution to percolate and extract, filter the extract and add hollow cellulose ultrafiltration membrane with a molecular weight cut off of 2000 for ultrafiltration, and add hollow fiber with a molecular weight cut off of 300 to the permeate Concentrate with plain nanofiltration membrane, pass the concentrated solution through NK-9 macroporous resin column, elute with appropriate amount of water, collect the lower column liquid and washing liquid, adjust pH8 with ammonia water, place the precipitate, centrifuge, dissolve the precipitate with 95% methanol and reflux to dissolve, add Decolorize with 0.5% activated carbon in the solution, filter out the activated carbon from the decolorized solution, add 1 / 8 volume of petroleum ether, fully stir and refrigerate to crystallize, then recrystallize the crystals with 95% ethanol solution, dry to obtain 81g of whit...

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Abstract

The invention discloses a method for preparing picrinine. The method comprises the following steps: crushing alstonia leaves; carrying out extraction on the alstonia leaves through percolation with acid water; carrying out ultrafiltration with an ultrafiltration membrane after filtration of an obtained extract; condensing obtained permeate with a nanofiltration membrane; allowing concentrate to pass through a macroporous resin column; carrying out elution with a proper amount of water; collecting eluted liquid and eluting water and adjusting the pH value of obtained mixed liquid to 8 to 10; standing the mixed liquid for deposition; centrifuging the mixed liquid; dissolving an obtained precipitation through reflux dissolving with methanol; decolouring the precipitation with active carbon; adding a proper amount of petroleum ether into decolouring liquid; refrigerating an obtained mixture for crystallization; and carrying out recrystallization on an obtained crystal by using an ethanol solution so as to obtain picrinine. The method has the advantages of simple operation, low energy consumption, a short period and suitability for industrialization.

Description

technical field [0001] The present invention relates to a kind of method for preparing citronine, in particular to a method for preparing cucurbitine by adopting membrane separation technology and macroporous resin. Background technique [0002] Picrinine is an indole monoterpene alkaloid, molecular formula C20H22N2O3, molecular weight 338, molecular structure formula: [0003] [0004] Daffodil has antitussive, asthmatic, expectorant and anti-acetylcholine, histamine and other effects. [0005] The lampstand tree is a plant of the genus Apocynaceae genus Apocynaceae Alstonia scholars (L.) R. Brown, using leaves or twigs as medicine, also known as duck foot tree, fat pig leaf, Dashu Lifei powder, Maidanbie (Dai language), has anti-inflammatory, phlegm-reducing cough, and pain-relieving effects. For the treatment of bronchitis, pertussis, stomach pain, diarrhea, malaria and external treatment of bruises, etc. Dracaena is the main medicinal ingredient of the leaves of th...

Claims

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Application Information

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IPC IPC(8): C07D498/22
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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