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Method for separating alkaloids compound in caulis mahoniae by high-speed countercurrent chromatography

A high-speed countercurrent chromatography and alkaloid technology, 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 effects of simple operation, low preparation cost and high efficiency

Active Publication Date: 2016-07-06
SHANDONG ANALYSIS & TEST CENT
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Problems solved by technology

[0007] 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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  • Method for separating alkaloids compound in caulis mahoniae by high-speed countercurrent chromatography
  • Method for separating alkaloids compound in caulis mahoniae by high-speed countercurrent chromatography
  • Method for separating alkaloids compound in caulis mahoniae by high-speed countercurrent chromatography

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Embodiment 1

[0029] Such as figure 1 The flow chart of monomer preparation in Gongluo wood is shown.

[0030] 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.

[0031] 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.

[0032] Separation and Purification of the Total Alkaloids of Gonglaojiao by High Speed ​​Countercurrent Chromatography

[0033] 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 invention discloses a method for separating alkaloids compound in caulis mahoniae by high-speed countercurrent chromatography. The condition for separation includes that the solvent system is chloroform and methyl alcohol in a ratio of 0.5 mol.L-1, hydrochloric solution in a ratio of 3.5-4.5:1-2:1.5-2.5, the size of the high-speed countercurrent chromatographic instrument is 200-400, sampling amount is 200-500, revolving speed is at 300-1000 rpm, the upper phase is fixed phase, and the lower phase is flow phase. Velocity is 1.5-2.5 mL / min, and detection wavelength is 250-260 nm. The method is low in preparation cost, convenient to operate, high in efficiency as compared with the prior art, and can separate jatrorrhizine with purity higher than 96%, berberine, palmatine, columbamine monomer compound from caulis mahoniae. The method successfully separates the columbamine from the caulis mahoniae for the first time.

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. technical background [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 a...

Claims

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Application Information

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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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