Preparation method of high-purity bergapten and psoralen
A technology of bergamot lactone and psoralen, applied in the direction of organic chemistry, can solve the problems of large solvent consumption, sample adsorption, low distribution efficiency, etc. Effect
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Embodiment 1
[0034] The methyl acetate-n-propanol-ethanol-water system was selected to separate and purify bergamotide and psoralen on a semi-preparative countercurrent chromatograph. The suitable temperature for the experiment is 25°C. Firstly, the above-mentioned solvent components are distributed and placed in a separatory funnel according to the volume ratio of 4:0.8:2:6, shaken and allowed to stand for stratification. After equilibrating for a period of time, separate the upper and lower phases. A semi-preparative countercurrent chromatograph is used, equipped with a polytetrafluoroethylene column, a 20ml injection valve, a column volume of 300ml, a TBP-50A pump, a TBD-23 detector and an N2000 chromatographic workstation. Weigh 300mg crude fig sample and dissolve it in a solution composed of 10ml upper phase and 10ml lower phase for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 950rpm, and pump the mobile phase into...
Embodiment 2
[0036] The ethyl acetate-n-butanol-ethanol-water system was selected to separate and purify bergamotide and psoralen on a semi-preparative countercurrent chromatograph. The suitable temperature for the experiment is 30°C. Firstly, the above-mentioned solvent components are distributed and placed in a separatory funnel according to the volume ratio of 3:0.5:1:8, shaken and then allowed to stand for stratification. After equilibrating for a period of time, separate the upper and lower phases. A semi-preparative countercurrent chromatograph is used, equipped with a polytetrafluoroethylene column, a 20ml injection valve, a column volume of 300ml, a TBP-50A pump, a TBD-23 detector and an N2000 chromatographic workstation. Weigh 150mg crude fig sample and dissolve in 10ml upper phase and 10ml lower phase solution for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 650rpm, and pump the mobile phase into the column at...
Embodiment 3
[0038]The butyl acetate-n-propanol-ethanol-water system was selected to separate and purify bergamotide and psoralen on a semi-preparative countercurrent chromatograph. The suitable temperature for the experiment is 22°C. Firstly, the above-mentioned solvent components are distributed in a separatory funnel according to the volume ratio of 4:1:1:6, shaken and allowed to stand to separate into layers. After equilibrating for a period of time, separate the upper and lower phases. A semi-preparative countercurrent chromatograph is used, equipped with a polytetrafluoroethylene column, a 20ml injection valve, a column volume of 300ml, a TBP-50A pump, a TBD-23 detector and an N2000 chromatographic workstation. Weigh 150mg crude fig sample and dissolve in 10ml upper phase and 10ml lower phase solution for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 750rpm, and pump the mobile phase into the column at a flow rate ...
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