Method for separating and preparing rumicin
A technology of ruminoid and high-speed countercurrent chromatography, which is applied in the field of high-speed countercurrent chromatography to separate and prepare high-purity ruminoid, and achieves the effects of short time, mild conditions and high recovery rate
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Embodiment 1
[0019] Take 150 g of Radix Hibiscus (manufactured in Nanjing), infiltrate with 100 ml of dichloromethane, and extract by percolation until the color of the percolation liquid becomes lighter, and recover the solvent to obtain 16.3 g of a brown crude dry product.
[0020] A high-speed countercurrent chromatograph is used, and the chromatographic separation solvent system is composed of petroleum ether-ethyl acetate-ethanol-water, and the volume ratio is 6:8:4:2. Set layering, take the upper phase as the stationary phase, and the lower phase as the mobile phase, take 1.5 g of the crudely extracted dry matter and dissolve it in the mixed solvent of the upper and lower layers of 30 ml, so that the column of the high-speed countercurrent chromatography is filled with the stationary phase, and then the column The head end is connected with the injection valve, and the speed controller is turned on to make the host rotate until the rotation speed reaches 700rpm, and the mobile phase i...
Embodiment 2
[0022] Take 150 g of Radix Hibiscus (manufactured in Nanjing), infiltrate with 100 ml of dichloromethane, and extract by percolation until the color of the percolation liquid becomes lighter, and recover the solvent to obtain 16.3 g of a brown crude dry product.
[0023] A high-speed countercurrent chromatograph is used, and the chromatographic separation solvent system is composed of petroleum ether-ethyl acetate-ethanol-water, and the volume ratio is 8:10:6:4. The solvent system is arranged in a separatory funnel, fully shaken and static Set layering, take the upper phase as the stationary phase, and the lower phase as the mobile phase, get 2.1 g of the crudely extracted dry matter and dissolve it in the mixed solvent of 40 ml upper and lower layers, so that the column of the high-speed countercurrent chromatograph is filled with the stationary phase, and then the column The head end is connected with the injection valve, and the speed controller is turned on to make the host...
Embodiment 3
[0025] Take 150 g of Radix Hibiscus (manufactured in Nanjing), infiltrate with 100 ml of dichloromethane, and extract by percolation until the color of the percolation liquid becomes lighter, and recover the solvent to obtain 16.3 g of a brown crude dry product.
[0026] A high-speed countercurrent chromatograph is used, and the chromatographic separation solvent system is composed of petroleum ether-ethyl acetate-ethanol-water, and the volume ratio is 5:7:5:3. Place layers, take the upper phase as the stationary phase, and the lower phase as the mobile phase, get 2.5 g of the crudely extracted dry matter and dissolve it in the mixed solvent of the upper and lower layers of 50 ml, so that the column of the high-speed countercurrent chromatography is filled with the stationary phase, and then the column The head end is connected with the injection valve, and the speed controller is turned on to make the host rotate until the rotation speed reaches 900rpm, and the mobile phase is...
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