Method for preparing high-purity hispidulin and herba lycopi flavone
A technology of high psyllium and zelan flavonoids is applied in the field of preparation of high-purity psyllium and zelan flavonoids, which can solve the problems of large solvent consumption, adsorption of samples, low distribution efficiency and the like, and achieves a large separation amount. , the separation environment is relaxed, the effect of saving solvent
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Embodiment 1
[0036] The trichloromethane-tetrachloromethane-ethanol-water system was selected to separate and purify the flavonoids of Lychee Grass on a semi-preparative countercurrent chromatograph. The suitable temperature for the experiment is 25°C. Firstly, the above-mentioned solvent components are distributed in a separatory funnel according to the volume ratio of 0.5:4:2:6, 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 100mg of Lychee Grass crude 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 ...
Embodiment 2
[0038] Tetrachloromethane-n-butanol-ethanol-water system was selected on a semi-preparative countercurrent chromatograph to separate and purify flavonoids from Lychee Grass. 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 of Lychee Grass crude sample and dissolve in 10ml upper phase and 10ml lower phase solution for later use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 650rpm, and pump the mobile p...
Embodiment 3
[0040] The dichloromethane-chloroform-methanol-water system was selected to separate and purify the flavonoids of Lychee Grass 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 0.5:4:3:2, 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 of Lychee Grass crude sample and dissolve in 10ml upper phase and 10ml lower phase solution for later 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 i...
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