Method for preparing catalpol

A technology of catalpol and methanol, which is applied in the field of preparation of catalpol, and can solve problems such as unfavorable large-scale production operations, pollution, and low content of catalpol

Inactive Publication Date: 2010-05-12
南京璇荣贸易有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In the prior art, the extraction and separation of catalpol mainly adopts organic solvent method, etc., but the content of catalpol obtained by these extraction processes is low, the pollution is serious in the production process, and it is unfavorable for large-scale production operations

Method used

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  • Method for preparing catalpol

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Experimental program
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Effect test

Embodiment 1

[0017] Take 10Kg of the fresh root of Rehmannia glutinosa, add methanol 5 times its weight and volume, heat and reflux twice, each time for 0.5 hours, combine the reflux liquid, filter, recover methanol under reduced pressure and concentrate, add an equal volume of water saturated n-butanol to extract 3 times , combined the n-butanol layer, recovered n-butanol under reduced pressure to the end, adsorbed by AB-8 macroporous adsorption resin column, eluted with water to remove impurities, eluted with 5% ethanol, collected 3 times the column volume of the eluate, concentrated And dried, dry added to the silica gel chromatography column, eluted with chloroform-methanol-water (6:4:1), the eluent of each column volume was 1 fraction, and the 3rd-6th stream was collected Parts were combined, the solvent was recovered and concentrated, crystallized by adding absolute ethanol, separated, washed and dried to obtain 6.4 g of catalpol, which was detected by HPLC with a purity of 98.4%.

Embodiment 2

[0019] Take 10Kg of the fresh root of Rehmannia glutinosa, add methanol 10 times its weight, heat and reflux 4 times, 2 hours each time, combine the reflux liquid, filter, recover methanol under reduced pressure and concentrate, add an equal volume of water saturated n-butanol to extract 8 times , combined the n-butanol layer, recovered n-butanol under reduced pressure to the end, adsorbed by H-103 macroporous adsorption resin column, eluted with water to remove impurities, eluted with 30% ethanol, collected 8 times the column volume of the eluate, and concentrated And dried, dry added to the silica gel chromatography column, eluted with chloroform-methanol-water (6:4:1), the eluent of each column volume was 1 fraction, and the 3rd-6th stream was collected Parts were combined, the solvent was recovered and concentrated, crystallized by adding absolute ethanol, separated, washed and dried to obtain 8.4 g of catalpol, which was detected by HPLC with a purity of 98.1%.

Embodiment 3

[0021] Take 10Kg of the fresh root of Rehmannia glutinosa, add methanol 8 times its weight, heat and reflux 3 times, each time for 1 hour, combine the reflux liquid, filter, recover methanol under reduced pressure and concentrate, add an equal volume of water saturated n-butanol to extract 5 times , combined the n-butanol layer, recovered n-butanol under reduced pressure to the end, adsorbed by D101 macroporous adsorption resin column, eluted with water to remove impurities, and eluted with 10% ethanol, collected 5 times the column volume of the eluate, concentrated and dried , added to a silica gel chromatography column by dry method, and eluted with chloroform-methanol-water (6:4:1), the eluent of each column volume was 1 fraction, and the 3rd to 6th fractions were collected, Combined, recovered the solvent and concentrated, added absolute ethanol to crystallize, separated, washed and dried to obtain 9.8 g of catalpol, which was detected by HPLC with a purity of 99.6%.

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Abstract

The invention relates to a method for preparing catalpol, which has simple operation, light pollution and less equipment investment. The method comprises the following processing steps of: taking fresh roots of rehmannia root; adding methanol of which the volume is 5 to 10 times weight of the fresh roots; refluxing for 2 to 4 times, and taking 0.5 to 2 hours for each refluxing; merging backflow liquid; filtering the liquid; recovering the methanol at reduced pressure and condensing the liquid; adding isopyknic water saturation butarol to extract for 3 to 8 times; merging a butarol layer; recovering the butarol at reduced pressure until the butarol is exhausted; adsorbing the butarol with a macroporous adsorbent resin column; carrying out water washing to remove impurities; carrying out elution with 5 to 30 percent ethanol; collecting eluent of which the volume is 3 to 8 times volume of the column; concentrating and drying the eluent; adding the eluent to a silica gel chromatographic column by a dry method; carrying out elution with chloroform-methanol-water (6:4:1); making the eluent in each column volume as one fluid part; collecting 3rd to 6th fluid parts; merging the fluid parts; recovering the solvent and concentrating the fluid parts; and adding anhydrous ethanol to crystallize. The catalpol prepared by the method has high product purity and is easy to realize industrialization expansion.

Description

technical field [0001] The invention relates to a method for preparing catalpol, in particular to a method for extracting catalpol from plants. Background technique [0002] Catalpol, synonym: Catalpinoside, etc. Molecular formula: C 15 h 22 o 10 , molecular weight: 362.333, CAS accession number: 2415-24-9, the structural formula is as follows: [0003] [0004] Catalpol is a natural compound that can enhance immunity and is widely found in a variety of plants. [0005] The traditional Chinese medicine Rehmannia glutinosa is the fresh or dried root tuber of Rehmannia glutinosa Libosch., a plant of the family Scrophulariaceae. [0006] In the prior art, the extraction and separation of catalpol mainly adopts the organic solvent method, etc., but the content of catalpol obtained by these extraction processes is low, the pollution is serious in the production process, and it is unfavorable for large-scale production operations. Contents of the invention [0007] The ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08
Inventor 张发成毛志英范淦彬
Owner 南京璇荣贸易有限公司
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