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Method for extracting and purifying catalpol by use of active carbon column chromatography and crystallization technology

A technology of crystallization and technology, which is applied in the field of medicine, to achieve the effect of comparative source, easy source, multiple similarity and pharmacological activity

Inactive Publication Date: 2012-04-11
THE CHINESE TRADITIONAL HERB MEDICINE RES INST HENAN PROV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] So far, there have been no patent reports involving the separation and purification of rehmannia root tubers by activated carbon column chromatography, and the separation and preparation of catalpol by flexible use of various crystallization techniques

Method used

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  • Method for extracting and purifying catalpol by use of active carbon column chromatography and crystallization technology
  • Method for extracting and purifying catalpol by use of active carbon column chromatography and crystallization technology
  • Method for extracting and purifying catalpol by use of active carbon column chromatography and crystallization technology

Examples

Experimental program
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Effect test

Embodiment 1

[0066] Take 20Kg of fresh rehmannia root, clean, cut into thin slices, immediately mix with 0.5% calcium carbonate, mix well, add 100L of 95% ethanol, crush and extract in a crushing extractor (rotational speed: 3000rpm) for 15min, and centrifuge in a drier to initially separate and remove plants The tissue was crushed, filtered, and the filtrate was decompressed to recover ethanol, and dried in vacuo to obtain 1.12Kg of dry extract. Add 5.0L of water to the dry extract to dissolve, filter, and pass through the treated activated carbon separation column (the granular activated carbon is heat-treated at 150°C for 4.5 hours, then soaked in distilled water for 1 hour, and then wet-packed with distilled water after removing floating powder), First elute with water until the effluent is nearly colorless, the flow rate is 2BV / hour, and the sugar reaction test is negative (molish reaction is negative), combined with TLC inspection until catalpol appears, continue to elute with 75% eth...

Embodiment 2

[0068] Take 100Kg of fresh rehmannia rhizome root, select it, cut it into thin slices, put it into the extraction tank, add 95% ethanol 400L to reflux extraction for 3 times, each time for 1 hour, combine the extracts, filter, recover the ethanol from the filtrate under reduced pressure, and dry it in vacuum to obtain dry extract 8.56Kg. Add 50.0L of water to the dry extract to dissolve, filter, and pass through the treated activated carbon separation column (granular activated carbon is heated at 150°C for 4.5 hours, then soaked in distilled water for 1 hour, and then wet-packed with distilled water after removing floating powder) ), first eluted with water until the effluent is nearly colorless, the flow rate is 3BV / hour, and the sugar reaction test is negative (molish reaction negative) combined with TLC inspection until catalpol appears, continue to elute with 75% ethanol solution until there is no catalpol When alcohol was detected, the flow rate was 3BV / hour, and the alc...

Embodiment 3

[0070] Take 50Kg of fresh rehmannia root, select it, cut it into thin slices with a thickness of 1-2mm, immediately heat it to 40-50°C, keep it warm for 100-120min, crush and extract it in a crushing extractor, add 200L of ethanol and homogenate at 5000rpm for 15min , the centrifugal preliminary separation of the drier to remove the broken plant tissue, the residue is soaked twice at room temperature with 50% ethanol 200L, the homogenate filtrate and the soaking liquid are combined, the ethanol is recovered, concentrated under reduced pressure, and vacuum-dried to obtain 4.87Kg of dry extract. Add 40.0L of water to the dry extract to dissolve, filter, and pass through the treated activated carbon separation column (granular activated carbon is heated at 150°C for 4.5 hours, then soaked in distilled water for 1 hour, and then wet-packed with distilled water after removing floating powder) ), first eluted with water until the effluent is nearly colorless, the flow rate is 2BV / hou...

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Abstract

The invention belongs to the technical field of medicines, and particularly relates to a method for separating and preparing catalpol from the tuberous root of a traditional Chinese medicine radix rehmanniae recens. The method takes the fresh tuberous root of the traditional Chinese medicine radix rehmanniae as a raw material, adopts a separation and purification method of active carbon column chromatography, and flexibly utilizes a solvent extraction method, a silica gel column separation method and various crystallization technologies to prepare catalpol products with different purities. The invention aims to provide a catalpol preparation method which has a simple process, is environment-friendly and energy-saving and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicines, and in particular relates to a method for separating and preparing catalpol from the roots of traditional Chinese medicine rehmannia glutinosa. Background technique [0002] Rehmannia glutinosa is a commonly used traditional Chinese medicine. There are nearly 200 kinds (194 kinds) of prescriptions in the 2010 edition of "Chinese Pharmacopoeia". The fresh or dried tuber root of Rehmannia glutinosa Libosch., a plant of the family Scrophulariaceae, has the effects of clearing heat and cooling blood, nourishing yin, and promoting body fluid [1] . [0003] The members of our research group have long been engaged in the research on the chemical constituents and pharmacology of Rehmannia glutinosa, and have successively undertaken the National Seventh Five-Year Research Project "Research on Varieties and Quality of Commonly Used Chinese Medicinal Rehmannia Rehmanniae", and the National Ninth Five-Yea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08
CPCY02P20/54
Inventor 刘明王慧森李更生
Owner THE CHINESE TRADITIONAL HERB MEDICINE RES INST HENAN PROV
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