Method for preparing dendrobine of which content is more than 95%

A technology for the content of dendrobine, which is applied in the field of natural medicinal chemistry, can solve the problems of high cost of dendrobine extraction consumables, high operation requirements, and high production costs, and achieve the effects of low cost, high purification efficiency, and simple method

Inactive Publication Date: 2015-04-29
GUIZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] One of the purposes of the present invention is to provide a preparation method that is simple, easy to operate, low in cost, environment-friendly and high in purification efficiency to solve the problems of high cost of dendrobine extraction consumables, high operating requirements, time-consuming, and high production costs. More than 95% dendrobine method

Method used

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Examples

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Embodiment

[0025] Take 1kg of dried stem section of Dendrobium nobile and pass through 20 meshes, add 10L of 70% ethanol for reflux extraction for 3 hours, then use 4L of 70% ethanol for reflux extraction for 3 hours, combine the extracts and concentrate to a paste; use twice the volume of 2% HCl solution was stirred to extract dendrobine from the ethanol extract, and the extraction was repeated once; chloroform extracted 2% HCl extract 3 times; the HCl extract was basified to pH 8 with ammonia water, and then chloroform was used to extract dendrobine from the extract; evaporated to dryness After chloroform, add twice the volume of 2% HCl solution to the extract to extract the dendrobine; extract the 2% HCl extract with chloroform to remove impurities; alkalinize the ammonia water to pH 8, extract the dendrobine with chloroform, and evaporate the chloroform again That is, 3.43 g of crude dendrobine with a content of 81.4% was obtained.

[0026] The obtained 3.43 g of crude dendrobine was...

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Abstract

The invention discloses a method for preparing dendrobine of which the content is more than 95%. The method comprises the following steps: step 1, acquiring dendrobium stems, adding an ethanol solution to the dendrobium stems for reflux extraction, adding ethanol solution again for reflux extraction, and combining extraction solutions, and concentrating the combined extraction solutions so as to obtain pasty extracts; step 2, adding an HCl solution to the pasty extracts, stirring the HCl solution and the pasty extracts, extracting dendrobine, and leaching the dendrobine so as to obtain an HCl extraction solution; step 3, repeating the step 2 until no alkaloid is detected in the HCl extraction solution; step 4, performing chloroform extraction on the HCl extraction solution for three times, alkalizing the HCl extraction solution by ammonium hydroxide until the pH value of the HCl extraction solution is 8, and performing chloroform extraction on the alkalized HCI extraction solution to obtain dendrobine; step 5, evaporating the chloroform, and retreating the step 2, step 3 and the step 4, and then evaporating the chloroform again to obtain crude dendrobine; step 6, dissolving the crude dendrobine in a small volume of ethyl ether, placing the ethyl ether with the crude dendrobine under minus 20 DEG C for crystallization, and repeating crystallization on the precipitated dendrobine crystals in the ethyl ether twice so as to obtain refined dendrobine of which the content is more than 95%. The method disclosed by the invention is simple and easy to operate, low in cost, environment-friendly, and high in purification efficiency.

Description

technical field [0001] The invention belongs to the field of natural medicinal chemistry, and in particular relates to a method for purifying dendrobine. Background technique [0002] At present, the preparation of dendrobine in China mostly stays in the optimization of extraction conditions, such as organic solvent extraction, enzyme-assisted extraction, ultrasonic-assisted extraction, carbon dioxide supercritical fluid extraction and other conditions, without further purification work; Method-assisted extraction requires the consumption of expensive biocatalyst enzymes, which increases the cost; ultrasonic or microwave-assisted extraction also has special requirements for equipment and is not easy to scale up; the one-time investment of carbon dioxide supercritical fluid extraction equipment is large, which increases the cost. Some documents and patents involve the further purification technology of dendrobine, but it needs to use ion exchange chromatography and silica gel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/08
CPCC07D491/08
Inventor 洪鲲乙引张宇斌张习敏
Owner GUIZHOU NORMAL UNIVERSITY
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