A method for large-scale preparation of wedelolide chemical reference substance
A technology of wecarolide and lactone chemistry, which is applied in the field of large-scale preparation of chemical reference substances of werethrin, can solve the problems that the output of the reference substance cannot meet the needs of practical application, cannot be scaled up in industrial scale production, and is expensive, and achieves Easy batch preparation, easy processing, low cost effect
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Embodiment 1
[0028] 1) Ethyl acetate extraction:
[0029] Add 3kg of Eclipta alcohol extract (provided by Sichuan Academy of Traditional Chinese Medicine), add 15L of water, heat to dissolve at 40°C, add 4.5L of ethyl acetate for extraction, extract 3 times, combine extracts, concentrate under reduced pressure to 500ml, mix Add 500 grams of 100-200 mesh silica gel, mix well, dry in a fume hood, and grind for later use.
[0030] 2) Medium-pressure silica gel column chromatography purification:
[0031] Pick The stainless steel column is used as a medium-pressure chromatography column, and 1.5kg of 100-200 mesh silica gel is loaded as a separation silica gel, and the ethyl acetate extract sample powder is evenly loaded into the column head, and the packing is tight; Shanghai Tongtian TBP2H10 constant flow pump is used as a medium-pressure column. Pump, petroleum ether: ethyl acetate: acetic acid (7:3:1) mixed solvent as the eluent, the flow rate is controlled at 150ml / min, the pressure is...
Embodiment 2
[0036] 1) Ethyl acetate extraction:
[0037]40kg of Eclipta medicinal material, reflux extraction with 70% ethanol, 480L for the first time, 400L for the second time, each extraction for 1.5 hours, the two extractions were combined to obtain about 7kg of alcohol extract extract; add 35L of water, heat at 40°C Make it dissolve, add 10.5L ethyl acetate for extraction, extract 3 times, combine the extracts, concentrate under reduced pressure to 2L, mix in 2kg of 100-200 mesh silica gel, mix well, dry in a fume hood, and grind for later use.
[0038] 2) Purification by silica gel column chromatography under reduced pressure:
[0039] Pick The stainless steel column is used as a decompression chromatography column, and a 2.5L suction filter bottle is used as a collector; 4.2kg of 200-300 mesh silica gel is loaded as a separation silica gel, and the ethyl acetate extract powder is evenly loaded into the column head, and the packing is tight; Henan Gongyi Yuhua brand circulating v...
Embodiment 3
[0043] 1) Ethyl acetate extraction:
[0044] Add 1kg of Eclipta alcohol extract (provided by Sichuan Academy of Traditional Chinese Medicine), add 5L of water, heat to dissolve at 40°C, add 1.5L of ethyl acetate for extraction, extract 3 times, combine extracts, concentrate under reduced pressure to 200ml, mix Add 200 grams of 100-200 mesh silica gel, mix well, dry in a fume hood, and grind for later use.
[0045] 2) Medium-pressure silica gel column chromatography purification:
[0046] Pick The stainless steel column is used as a medium-pressure chromatography column, and 750 grams of 100-200 mesh silica gel is loaded as a separation silica gel, and the ethyl acetate extract powder is evenly loaded into the column head, and the packing is tight; Shanghai Tongtian TBP2H10 constant flow pump is used as the medium Pressure pump, petroleum ether: ethyl acetate: acetic acid (6:4:1) mixed solvent as the eluent, the flow rate is controlled at 100ml / min, the pressure is about 0.2...
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