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Method for separation of alkaloids in Kaoyasu by ph-zone refined countercurrent chromatography

A technology of alkaloids and countercurrent chromatography is applied in the field of separation and purification of effective components of traditional Chinese medicines, which can solve the problems of isolating tetrandrine and the like, and achieve the effects of simple operation, low preparation cost and high efficiency.

Active Publication Date: 2017-08-25
SHANDONG ANALYSIS & TEST CENT
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no report on the separation of tetrandrine from gonglao wood, and there is no record of separation of alkaloids in gongo wood by using pH-zone refined countercurrent chromatography

Method used

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  • Method for separation of alkaloids in Kaoyasu by ph-zone refined countercurrent chromatography
  • Method for separation of alkaloids in Kaoyasu by ph-zone refined countercurrent chromatography
  • Method for separation of alkaloids in Kaoyasu by ph-zone refined countercurrent chromatography

Examples

Experimental program
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Embodiment 1

[0028] Such as figure 1 The flow chart of monomer preparation in Gongluo wood is shown.

[0029] Take 2 kg of the medicinal material of Gongluomu, grind it, and extract it with 95% ethanol under reflux for 3 times (2 hours each time), filter, and concentrate the filtrate under reduced pressure until it has no alcohol smell.

[0030] Add hydrochloric acid to the above-mentioned concentrated extract to adjust pH=3, extract petroleum ether 3 to 5 times to remove fat-soluble components, add ammonia water to the extracted water layer to adjust pH=9, and filter to obtain 10.6g of precipitate, which is the desired biological Total alkali.

[0031] Separation and Purification of the Total Alkaloids of S. chinensis Using pH-Zone Refining Countercurrent Chromatography

[0032] The solvent system is chloroform: chloroform: methanol: water = 4:3:3, the column volume of the high-speed countercurrent chromatography is 300mL, the sample volume is 3g, the rotation speed is 800rpm, the uppe...

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Abstract

The invention discloses a method for separating alkaloid compounds in eucalyptus by refining countercurrent chromatography in a pH-zone. The conditions used in the separation are: the solvent system is chloroform:methanol:water=3.5-4.5:2.5- 3.5: 2.5-3.5, pH-zone refined countercurrent chromatography column volume is 200-400, sample loading is 2-5g, rotation speed is 300-1000rpm, upper phase is stationary phase, lower phase is mobile phase, flow rate is 1.5-2.5 mL / min, the stationary phase retention rate is 35.71%, and the detection wavelength is 250-260nm. The preparation cost of the method of the present invention is lower than that of the prior art, and the operation is simple and efficient, and it can separate and prepare jatrorrhizine, berberine, palmatine, and African fangji with a purity greater than 96% from the traditional Chinese medicine Gongluo in large batches. The separation and preparation method of alkali monomer compound, the invention firstly separates tetrandrine from the traditional Chinese medicine Gongluomu.

Description

technical field [0001] The invention relates to a method for separating and purifying the effective components of traditional Chinese medicine, specifically separating alkaloid compounds (jatrorrhizine, berberine, tetrandrine, and palmatine monomer) in Gonglaojiao by using pH-zone refining countercurrent chromatography Methods. Background technique [0002] Gonggongmu is the dry stem of Berberidaceae plant broad-leaved ten merits Mahoniabealei (Fort.) Carr or fine-leaf ten majors Mahoniafortunei (Lindl.) Fedde, and its nature and flavor are bitter, cold, has the effect of clearing away heat and dampness, purging fire and detoxifying. effect. Cure mainly damp-heat diarrhea, jaundice, red urine, red eyes and swelling, stomach fire and toothache, boils and carbuncles. The alkaloid compounds in Gongluo wood are mainly isoquinoline alkaloids, including jatrorrhizine, palmatine and berberine. The research results show that isoquinoline alkaloids can inhibit free radicals and lip...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D455/03
CPCC07D455/03
Inventor 王岱杰耿岩玲王晓赵恒强于金倩段文娟闫慧娇
Owner SHANDONG ANALYSIS & TEST CENT
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