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Method for simultaneously preparing vasicine and vasicinone from peganum harmala

A technology of orchidine and orchidine, which is applied in the direction of organic chemistry, can solve the problems of cumbersome process, low alkaloid efficiency, and inability to obtain the content of orchidine, so as to achieve low process cost and simple process Effect

Inactive Publication Date: 2010-12-22
NORTHWEST A & F UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can obtain purer alkaloids, the process is relatively cumbersome, especially the reflux extraction of alkalized resins with organic solvents is difficult to use on a large scale in industry, and the efficiency of lye eluting alkaloids It is very low, so large-scale production cannot be realized; at the same time, this method can only obtain a compound of kaline, and cannot obtain kabione with a large content, which is a huge waste of resources
[0007] If the traditional alkaloid extraction method (organic solution extraction method) is used to separate and purify it, although a large amount of impurities can be removed, many impurities such as neutral and non-polar pigments are difficult to get out, and a large amount of alkaloids will be used in the extraction process Repeated extraction of organic reagents, on the one hand, increases the extraction time and workload, on the other hand, this method is prone to emulsification, which reduces the transfer of active ingredients and reduces the efficiency of separation
Therefore, this method is difficult to be used in industrial production

Method used

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  • Method for simultaneously preparing vasicine and vasicinone from peganum harmala
  • Method for simultaneously preparing vasicine and vasicinone from peganum harmala
  • Method for simultaneously preparing vasicine and vasicinone from peganum harmala

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Take 500g of dry powder of stems and leaves of Camelia punctatus, add 15L of ethanol with a mass fraction of 70%, ultrasonically extract 3 times, each time for 30min, remove the filter residue after filtering the extract, concentrate the filtrate to brown-red viscous extract, and use pH=9 The extract was dissolved in deionized water for 3 times, filtered, and the filtrate was passed through a D101 macroporous resin column at a flow rate of 3 times column volume / hour, adsorbed for 10 hours, and eluted with deionized water at a flow rate of 4 times column volume / hour for 3 hours. Then use 30% ethanol with a mass fraction of pH=5 to elute at a flow rate of 2 times column volume / hour for 4 hours, and then use 50% ethanol with a mass fraction of pH=5 to elute with a flow rate of 2 times column volume / hour for 4 hours, Finally, elute with 95% ethanol at a flow rate of 5 times column volume / hour for 4 hours.

[0039] Concentrate the ethanol eluent with a mass fraction of 30% to ...

Embodiment 2

[0042] Take 500Kg of dried stem and leaf powder of Camelia pontica, add 10L of ethanol with a mass fraction of 80%, ultrasonically extract 3 times, each time for 30min, remove the filter residue after filtering the extract, concentrate the filtrate to brown-red viscous extract, and use pH=10 Dissolve the extract in deionized water for 3 times, filter, and pass the filtrate through a D101 macroporous resin column at a flow rate of 2 times the column volume / hour, absorb for 8 hours, elute with deionized water for 2 hours at a flow rate of 4 times the column volume / hour, and then Elute with 30% ethanol with a mass fraction of pH=5 at a flow rate of 3 column volumes / hour for 4 hours, then use 50% ethanol with a mass fraction of pH=5 for 4 hours at a flow rate of 3 times column volume / hour, and finally Elute with 95% ethanol at a flow rate of 5 times column volume / hour for 4 hours.

[0043] Concentrate the ethanol eluent with a mass fraction of 30% to dryness to obtain 5.8g of extr...

Embodiment 3

[0046] Refer to attached figure 1 , take 1Kg of dry powder of stems and leaves of Camelia punctatus, add 10L of ethanol with a mass fraction of 60%, ultrasonically extract 3 times, each time for 30min, remove the filter residue after filtering the extract, concentrate the filtrate to a brown-red viscous extract, and use pH=9 The extract was dissolved in deionized water for 3 times, filtered, and the filtrate was passed through a D101 type macroporous resin column at a flow rate of 3 times column volume / hour, adsorbed for 12 hours, and eluted with deionized water at a flow rate of 3 times column volume / hour for 6 hours. Then use 30% ethanol with a mass fraction of pH=5 to elute at a flow rate of 3 times column volume / hour for 3 hours, and then use 50% ethanol with a mass fraction of pH=5 to elute with a flow rate of 2 times column volume / hour for 5 hours, Finally, ethanol with a mass fraction of 95% was eluted for 7 hours at a flow rate of 5 times column volume / hour.

[0047]...

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Abstract

The invention discloses a method for simultaneously preparing vasicine and vasicinone from stem leaves of peganum harmala, comprising the steps of ethanol extraction, D101 type macroporous resin enrichment, silicagel column separation and purification, recrystallization and the like. The method of the invention is as follows: extracting the vasicine and the vasicinone from the stem leaves of the peganum harmala by the ultraphonic secondary solvent extraction method; enriching and separating the vasicine and the vasicinone by regulating the concentration and the pH value of an eluent for the macroporous resin; and finally preparing the vasicine and the vasicinone the concentrations of which are greater than 95% by the silicagel column chromatography method and the recrystalization method.

Description

technical field [0001] The invention belongs to the field of preparation of biochemical articles, and relates to a method for simultaneously preparing oracine and oracine from camel succulents. Background technique [0002] Camelina ( Peganum harmala L. ) plant is Tribulus terrestris ( Zygophyllaceae ) in the most primitive groups, a total of six species, distributed in Asia, Europe, North Africa and other places, in our country there are three, that is, camel cape ( Peganum harmala L. ), Artemisia camel ( P. nigelastrum Bge ) and multi-lobed camels ( P. multisectum (maxim.) Bobr. ), which are mainly distributed in desert and semi-desert areas such as Xinjiang, Mongolia, Shaanxi, Gansu, and Ningxia in the northwest, and are very rich in resources. [0003] There are a variety of alkaloids contained in camel ponchos, among which quinazoline alkaloids are a major class of alkaloids, mainly including: alkaloids and alkaloids. These alkaloids are highly active in many wa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04
Inventor 王俊儒杜宏涛任飞苏银芬张君
Owner NORTHWEST A & F UNIV
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