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Method for separating and extracting cepharanthine

The technology of a steppin and its extraction method, which is applied in the field of extraction and separation of steppin, can solve the problems of large consumption of organic solvent, low recovery rate of stepsteprin, and large loss of stepstephin, so as to improve the purity and process route Green environmental protection, the effect of reducing organic impurities

Active Publication Date: 2011-08-10
YUNNAN HANDE BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the prior art, steppavine is mainly extracted by pure methanol or ethanol, acid-soluble alkali precipitation, silica gel column chromatography or alumina column chromatography, and acetone crystallization. These traditional methods of extraction and separation have a low recovery rate of steppavine, and purification During the process, the loss of patinol is relatively large, the consumption of organic solvent is large, the cost of industrialization is high, and the industrial pollution is serious

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Take 1kg of dry root tubers, crush them to 40 mesh, add 2L water and 3ml mixed biological enzyme solution (pectin lyase: α low-temperature liquefaction enzyme = 1:4), soak at 50°C for 1 hour, add 10 liters of 1% HCL ( mass percentage, the same below) aqueous solution was heated to 90°C for extraction for 3 hours. Separate the medicinal liquid, add 10 liters of 1% HCL aqueous solution to the medicinal dregs and decoct for 3 hours, filter, combine the filtrate twice, use strong acid styrenesulfonic acid-based cation exchange resin 001X7 for exchange adsorption, enrich stepherin, and add hydrogen to oxidize Sodium to 80% (mass percentage, the same below) in ethanol aqueous solution to saturated solution 5L as eluent, elution, flow rate is 10ml / min, collect the eluate from the stephenin section, adjust the pH value to 7, concentrate and recover Ethanol, filtered, and the precipitate was dissolved in absolute ethanol, then purified by an anionic DESE cellulose column, the el...

Embodiment 2

[0015] Take 1kg of dry root tubers, crush them to 60 mesh, add 2L of water and 1ml of mixed biological enzyme solution (snail enzyme: niger enzyme = 3:2), soak at 50°C for 1 hour, add 11 liters of 2% HCL (mass percentage, The same below) aqueous solution was heated to 90°C for extraction for 3 hours. Separate the medicinal liquid, add 11 liters of 2% HCL aqueous solution to the medicinal dregs and decoct for 3 hours, filter, combine the filtrates twice, and use cationic CM cellulose column to absorb, enrich the stephenin, and add sodium hydroxide to 70% ethanol aqueous solution 5L of the solution in the medium to saturated state was used as the eluent for elution, and the flow rate was 10ml / min. Collect the eluate from the stephatrin segment and adjust the pH value to 7, concentrate and recover ethanol, filter, dissolve the precipitate with absolute ethanol, purify it with a 700B anion resin column, collect the eluate, concentrate, and dry it with 60% ethanol water crystalliza...

Embodiment 3

[0017] Take 1 kg of dry ground root tubers, crush them to 40 mesh, add 3 L of water and 5 ml of mixed biological enzyme solution (hemicellulase: α medium temperature liquefaction enzyme = 1:4), soak at 60 ° C for 1 hour, add 9 liters of 1% HCL ( mass percentage, the same below) aqueous solution was heated to 90°C for extraction for 3 hours. Separate the medicinal liquid, add 9 liters of 1% HCL aqueous solution to the medicinal dregs and decoct for 3 hours, filter, combine the filtrates twice, use weakly acidic acrylic acid cation exchange resin 152 to exchange and adsorb alkaloids, enrich stephalin, and add hydrogen Add 5 L of sodium oxide to 90% ethanol aqueous solution to a saturated state as the eluent, and elute with a flow rate of 10 ml / min. Collect the eluate from the stephenin segment and adjust the pH value to 7, concentrate and recover ethanol, filter, dissolve the precipitate with absolute ethanol, use D941 anion column to elution and purify, collect the eluate, conc...

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PUM

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Abstract

The invention relates to a method for separating and extracting cepharanthine, which comprises the following steps of: taking a dry stephania tuberous root, crushing, adding 2 to 3L of water and 0.5 to 5ml of mixed bio-enzyme liquid into each kilogram of crushed material, soaking for 1 hour, adding 9 to 11L of 1 to 2 mass percent aqueous solution of HCL, heating to 90DEG C, and soaking for 3 hours; and separating out a liquid medicine, adding 9 to 11L of 1 to 2 percent aqueous solution of HCL into dregs, decocting for 3 hours, filtering, mixing filtrate, adsorbing by adopting a cation exchange column or cation cellulose column, enriching the cepharanthine, eluting by using solution that sodium hydroxide is added into 60 to 90 percent aqueous solution of ethanol until the saturation state as eluent, collecting eluent of a cepharanthine section, regulating the pH value to be 7, concentrating for recovering ethanol, filtering, dissolving a precipitate by using absolute ethanol, eluting and purifying by using an anion column, collecting eluent of a cepharanthine section, concentrating, crystallizing, and drying to obtain the cepharanthine. The method has the advantages of simple operation, light pollution, low cost, high yield, high purity of cepharanthine, and suitability for industrial production.

Description

technical field [0001] The present invention relates to a method for extracting and separating stephatrin, in particular to a method for extracting stephatrin from plant root. Background technique [0002] Cepharanthine is a biologically active bisbenzyl isoquinoline alkaloid, mainly derived from plants of the family Anthraceae, such as Rhizoma chinensis, Rhizoma glabra, Golden Thread Hanging Turtle, Jiangnan Rhizoma and Taiwan Stephania vine and so on. Due to the influence of geographical environment, climatic conditions and other factors, the quality of the same medicinal material from different sources is often different, and the difference in species and origin results in different levels of paternin in plants. [0003] Stephalin can promote the proliferation of bone marrow tissue, increase the number of white blood cells in the blood, and is suitable for leukopenia; it is also a good anticancer drug synergist, which can improve the curative effect of anticancer drugs, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/056
Inventor 蔡群虎
Owner YUNNAN HANDE BIO TECH
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