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A Method for Separating Alkaloids in Gongluomu by High Speed ​​Countercurrent Chromatography

A technology of high-speed countercurrent chromatography and alkaloids, which is applied in the field of separation and purification of active ingredients of traditional Chinese medicine, can solve the problems of separating tetrandrine and other problems, and achieve the effect of simple operation, high efficiency and low preparation cost

Active Publication Date: 2017-05-03
SHANDONG ANALYSIS & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, there is no relevant report on the separation of tetrandrine from gonglao wood, and there is no record of separation of alkaloids in gonglao wood by high-speed countercurrent chromatography

Method used

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  • A Method for Separating Alkaloids in Gongluomu by High Speed ​​Countercurrent Chromatography
  • A Method for Separating Alkaloids in Gongluomu by High Speed ​​Countercurrent Chromatography
  • A Method for Separating Alkaloids in Gongluomu by High Speed ​​Countercurrent Chromatography

Examples

Experimental program
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Embodiment 1

[0030] Such as figure 1 The flow chart of monomer preparation in Gongluo wood is shown.

[0031] 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.

[0032] 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.

[0033] Separation and Purification of the Total Alkaloids of Gonglaojiao by High Speed ​​Countercurrent Chromatography

[0034] The solvent system is chloroform: methanol: 0.5mol L -1 Hydrochloric acid solution=4:1.5:2, the column volume of high-speed countercurrent chromatography is 300mL, the sample volume is 300mg, the rotation speed is 800r...

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Abstract

The present invention discloses a method for separating alkaloid compounds in eucalyptus by using high-speed countercurrent chromatography. The conditions used for the separation are: the solvent system is chloroform:methanol:0.5mol L-1 hydrochloric acid solution=3.5-4.5:1- 2: 1.5-2.5, the column volume of high-speed countercurrent chromatography is 200-400, the sample volume is 200-500, the rotation speed is 300-1000rpm, the upper phase is the stationary phase, the lower phase is the mobile phase, the flow rate is 1.5-2.5 mL / min, and the detection Wavelength 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 active ingredients of traditional Chinese medicines, in particular to a method for separating alkaloid compounds (jatrorrhizine, berberine, palmatine, and african tetrandrine monomers) in Gonglaojiao by using high-speed countercurrent chromatography. [0002] technical background [0003] 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 ra...

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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