Method for separating and purifying dehydroevodiamine from fructus evodiae

A technology for separation and purification of dehydroevodiamine, applied in the direction of organic chemistry, can solve the problems of unsuitability for large-scale preparation, complicated and time-consuming operation, unfriendly environment, etc., and achieve easy large-scale preparation, short separation time and long time-consuming Effect

Active Publication Date: 2018-11-20
JIANGXI UNIVERSITY OF TRADITIONAL CHINESE MEDICINE
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Problems solved by technology

The separation and purification of dehydroevodiamine mainly adopts silica gel column chromatography and macroporous resin separation and purification method (research on the chemical constituents of Evodia rutaecarpa[J]. Chinese Journal of Traditional Chinese Medicine, 2009,34(06):792-794; Chemical composition research [J]. Chinese Journal of Experimental Formulas, 2016,22(08):58-64; preparation method of dehydroevodiamine and its application against agricultural pathogenic bacteria, Chinese patent, CN 106892919A.), due to dehydroevodiamine Evodiamine is easily soluble in water and organic solvents at the same time, leading to the disadvantages of the previous extraction methods such as large loss, low yield, cumbersome and time-consuming operation, the solvent used is not friendly to the environment, and is not suitable for large-scale preparation.

Method used

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  • Method for separating and purifying dehydroevodiamine from fructus evodiae
  • Method for separating and purifying dehydroevodiamine from fructus evodiae
  • Method for separating and purifying dehydroevodiamine from fructus evodiae

Examples

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Embodiment 1

[0028] A method for separating and purifying dehydroevodiamine from Evodia rutaecarpa fruit, the specific steps are:

[0029] (1) Raw materials: take 5g of dried and nearly mature fruit of Evodia rutaecarpa;

[0030] (2) Sour water extraction: Add 10 times the amount of petroleum ether to 5 g of Evodia rutaecarpa fruit, let it stand for 10 hours, drain the petroleum ether, then add 10 times the amount of 2% HCl to extract by reflux extraction, collect the extract and concentrate under reduced pressure Obtain 2.3g extract A, add methanol to dissolve extract A, filter impurities, and concentrate the filtrate under reduced pressure to obtain 0.7g extract B;

[0031] (3) Chromatographic column chromatography: After the extract B is dissolved in 5% ethanol and loaded by wet method, carry out atmospheric pressure chromatographic column chromatography, wherein the column chromatography filler is polyamide resin, and the particle size is 30-60 mesh; 5cm; using 5% ethanol as the eluen...

Embodiment 2

[0034] A method for separating and purifying dehydroevodiamine from Evodia rutaecarpa fruit, the specific steps are:

[0035] (1) Raw materials: take 100g of dry and nearly mature fruit of Evodia rutaecarpa;

[0036] (2) Acidic water extraction: add 5 times the amount of petroleum ether to 100 g of Evodia rutaecarpa fruit, let it stand for 5 hours, drain the petroleum ether, then add 10 times the amount of 2% HCl to extract by reflux extraction, collect the extract and freeze-dry to obtain 40 g Extract A, add methanol to dissolve extract A, filter impurities, freeze-dry the filtrate to obtain 16g extract B;

[0037] (3) Chromatographic column chromatography: Dissolve the extract B with 10% ethanol, and carry out normal pressure chromatographic column chromatography after wet loading, wherein the column chromatography filler is polyamide resin with a particle size of 30-60 mesh; The diameter is 10 cm; using 10% ethanol as the eluent, the semi-finished product is collected in s...

Embodiment 3

[0040] A method for separating and purifying dehydroevodiamine from Evodia rutaecarpa fruit, the specific steps are:

[0041] (1) Raw materials: take 250g of dry and nearly mature fruit of Evodia rutaecarpa;

[0042] (2) Acidic water extraction: add 8 times the amount of petroleum ether to 250 g of Evodia rutaecarpa fruit, place it for 15 hours, drain the petroleum ether, then add 5 times the amount of 2% HCl to extract by reflux extraction, collect the extract and freeze-dry to obtain 98g Extract A, add methanol to dissolve extract A, filter impurities, and freeze-dry the filtrate to obtain 37g extract B;

[0043] (3) Chromatographic column chromatography: Dissolve the extract B with 35% ethanol, and carry out atmospheric pressure chromatographic column chromatography after wet loading, wherein the column chromatography packing material is polyamide resin, and the particle size is 30-60 mesh; The diameter is 15 cm; using 35% ethanol as the eluent, the semi-finished product i...

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Abstract

The invention discloses a method for separating and purifying dehydroevodiamine from fructus evodiae which is a rutaceous plant. The method comprises the following steps: soaking a fructus evodiae fruit by using a petroleum ether to degrease, then extracting with 2% HCl as a solvent through a reflux extraction method, collecting an extracting solution, then carrying out vacuum concentration or freeze-drying to obtain an extractum A, dissolving the extractum A with methyl alcohol, filtering, carrying out vacuum concentration or freeze-drying on a filtrate to obtain an extractum B, taking polyamide resin as a filler to elute the extractum B with water-ethyl alcohol, fractionally collecting a semi-finished product, conducting vacuum concentration or freeze-drying to obtain a solid semi-finished product, taking ethyl alcohol-acetone as a solvent to recrystallize the solid semi-finished product to obtain a dehydroevodiamine powder crystal with the purity more than 98.5%. The yield of the dehydroevodiamine prepared through the method is high, the cost is low, the operation is simple, and the method is environmentally friendly, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of active ingredients of traditional Chinese medicine, in particular to a method for separating and purifying dehydroevodiamine from Rutaceae plant Evodia rutaecarpa. Background technique [0002] Dehydroevodiamine is an alkaloid compound mainly found in the fruit of Rutaceae plant Evodia rutaecarpa, and is a characteristic component of the plant. Dehydroevodiamine has medium polarity, easily soluble in water and organic solvents, melting point 216-218°C, molecular formula C 19 h 15 N 3 O, molecular weight 301.34. [0003] [0004] Dehydroevodiamine is an alkaloid compound with high pharmacological activity isolated from Rutaceae plant Evodia rutaecarpa. Investigation into the stability and reactivity of the pentacyclic alkaloiddehydroevodiamine and the benz-analog thereof [J]. ]. Tetrahedron, 2016, 72:2535-2543.). The separation and purification of dehydroevodiamine mainly adopts silica gel column...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/14
CPCC07D471/14
Inventor 袁金斌董嘉皓何军伟任刚乔日发杨武亮陈海芳
Owner JIANGXI UNIVERSITY OF TRADITIONAL CHINESE MEDICINE
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