Method of preparing four active substances such as cycloartenyl ferulate by separation
A technology of pineapple enol ferulate and sitosterol ferulate, which is applied in the field of separating and preparing four active substances of pineapple enol ferulate, and can solve problems such as the inability to obtain extremely high-purity monomers.
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Embodiment 1
[0011] Select n-hexane-acetonitrile on a semi-preparative countercurrent chromatograph GS10AB to separate and purify rice bran extract. First, the above solvent components are prepared in a separatory funnel according to a volume ratio of 1:1, shake well and then stand to separate layers. After equilibrating for a period of time, separate the upper phase and the lower phase, take the lower phase as the stationary phase, and the upper phase as the mobile phase. A semi-preparative high-speed countercurrent chromatograph is used, equipped with an NS-1007 pump, a 20mL injection valve, a polytetrafluoroethylene column with a column volume of 240mL, an 8823A-UV ultraviolet detector, and a Yokogawa3057 portable recorder. Weigh 200mg of rice bran extract and dissolve in 5mL upper phase and 5mL lower phase mixed solution for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 800rpm, and pump the mobile phase into the colum...
Embodiment 2
[0013] Select n-heptane-dichloromethane-acetonitrile on the semi-preparative countercurrent chromatograph GS10A to separate the rice bran extract. Set layers. After equilibrating for a period of time, separate the upper and lower phases, take the lower phase as the stationary phase, and the upper phase as the mobile phase. A semi-preparative high-speed countercurrent chromatograph is used, equipped with NS-1007 pump, 20mL injection valve, polytetrafluoroethylene column with a column volume of 230mL, 8823A-UV ultraviolet detector, and Yokogawa 3057 portable recorder. Weigh 128.5mg of rice bran extract and dissolve in 5mL upper phase and 5mL lower phase mixed solution for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 800rpm, and pump the mobile phase into the column at a flow rate of 2.0mL / min; after the dynamic equilibrium of the entire system is established, inject the sample through the injection valve; the...
Embodiment 3
[0015] Select n-pentane-dichloromethane-acetonitrile on the semi-preparative countercurrent chromatograph EMC-500 to separate and purify the rice bran extract. Let it stand for layering. After equilibrating for a period of time, separate the upper phase and the lower phase, take the lower phase as the stationary phase, and the upper phase as the mobile phase. A semi-preparative high-speed countercurrent chromatograph is used, equipped with NS-1007 pump, 20mL injection valve, polytetrafluoroethylene column with a column volume of 500mL, 8823A-UV ultraviolet detector, and Yokogawa 3057 portable recorder. Weigh 400.2mg of rice bran extract and dissolve in 5mL upper phase and 5mL lower phase mixed solution for use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine to 800rpm, and pump the mobile phase into the column at a flow rate of 2.0mL / min; after the dynamic equilibrium of the entire system is established, inject the sa...
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