Method for simultaneously preparing high-purity podophyllotoxin and deoxidized podophyllotoxin from sabina vulgaris
A technology of deoxypodophyllotoxin and podophyllotoxin, which is applied in the direction of organic chemistry, etc., to achieve the effects of simple operation, high separation efficiency and expansion of column capacity
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Embodiment 1
[0031] In the working drum of the main engine of the countercurrent chromatography in this embodiment, the column capacity of the multi-layer wound polytetrafluoroethylene (PTFE) tube is 2.5 liters. The solvent system adopts carbon tetrachloride: ethyl acetate: methanol: water = 17:6:15:3.5 (volume ratio).
[0032] Take 3.4L of carbon tetrachloride, 1.2L of ethyl acetate, 3.0L of methanol, and 0.7L of water, and mix them thoroughly in a 10L mixing kettle. After standing for stratification, separate the upper and lower phases for later use. The above phase is used as the stationary phase, and the upper phase is pressed into the working drum of the main engine by air pressure. Take by weighing 20 grams of the ethanol extraction extract of Juniper juniper, dissolve with 200mL of the lower phase solution, filter to obtain the ethanol extraction extract solution of Juniper juniper for dissolving, and set aside. Open the countercurrent chromatographic separation device, adjust the ...
Embodiment 2
[0034] In the working drum of the main engine of the countercurrent chromatography in this embodiment, the column capacity of the multi-layer wound polytetrafluoroethylene (PTFE) tube is 2.5 liters. The solvent system adopts carbon tetrachloride: ethyl acetate: methanol: 0.10 mol / L acetic acid aqueous solution = 17:6:15:3.5 (volume ratio).
[0035] Take 3.4 L of carbon tetrachloride, 1.2 L of ethyl acetate, 3.0 L of methanol, and 0.7 L of 0.10 mol / L aqueous acetic acid solution, mix them thoroughly in a 10 L mixing kettle, and separate the upper and lower phases for later use. The above phase is used as the stationary phase, and the upper phase is pressed into the working drum of the main engine by air pressure. Take by weighing 20 grams of the ethanol extraction extract of Juniper juniper, dissolve with 200mL of the lower phase solution, filter to obtain the ethanol extraction extract solution of Juniper juniper for dissolving, and set aside. Open the countercurrent chromato...
Embodiment 3
[0037]The column capacity of the multi-layer wound polytetrafluoroethylene (PTFE) tube in the main machine working drum of the countercurrent chromatography in this embodiment is about 1.2 liters. The solvent system adopts carbon tetrachloride: ethyl acetate: methanol: water = 19:6:16:3 (volume ratio).
[0038] Take 1.9L of carbon tetrachloride, 0.6L of ethyl acetate, 1.6L of methanol, and 0.3L of water, and mix them thoroughly in a 5L mixing kettle. After standing for stratification, separate the upper and lower phases for later use. The above phase is used as the stationary phase, and the upper phase is pressed into the working drum of the main engine by air pressure. Take by weighing 10 grams of the ethanol extraction extract of Juniper juniper, dissolve with 100mL of the lower phase solution, filter to obtain the ethanol extraction extract solution of Juniper juniper for dissolving, and set aside. Open the countercurrent chromatographic separation device, adjust the main ...
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