Preparation method for extracting cinobufagin and bufalin mixture from venenum bufonis
A technology for chinabufoni-based and bufalin, which is applied in the field of extracting high-purity chinabufoni-based and bufalin mixtures, and can solve the problems of low purity and the like
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Embodiment 1
[0041] (1) Toad venom is crushed into a coarse powder that passes through a 40-mesh sieve, 95% ethanol is added to 30 times the amount of toad venom, heated and refluxed for 3 times, each extraction is 3 hours, the extract is filtered, and the ethanol is recovered from the filtrate until it has no ethanol smell. Ethanol extract A;
[0042] (2) In the extract A, add 5 times the amount of toad venom, silica gel with a particle size of 100-200 mesh, evaporate to dryness, and add the top of the chromatography column that has been filled with silica gel (the diameter-to-height ratio of the silica gel column is 2.5:13.5, and the loading capacity is 20 to 30 times the amount of toad venom in extract A), first use petroleum ether-acetone (9:1) mixed solvent as the eluent, elute, discard the eluent, and then use petroleum ether-acetone (8.5: 1.5) The mixed solvent is used as the eluent, and the eluent B is obtained when the components of the mixture of Cinobufacin and Bufafalin are co...
Embodiment 2
[0046] Toad venom is crushed into a fine powder that passes through a 40-mesh sieve, 80% ethanol is added to 40 times the amount of toad venom, heated and refluxed for 3 times, each extraction is 2 hours, the extract is filtered, and the ethanol is recovered from the filtrate until it has no ethanol smell, and the ethanol extract is obtained A;
[0047] (2) In the extract A, add 5 times the amount of toad venom, silica gel with a particle size of 100-200 mesh, evaporate to dryness, and add the top of the chromatography column that has been filled with silica gel (the diameter-to-height ratio of the silica gel column is 1:10, and the filling volume is 20 to 30 times the amount of toad venom in extract A), first use petroleum ether-acetone (9:1) mixed solvent as the eluent, elute, discard the eluent, and then use petroleum ether-acetone (8.5: 1.5) The mixed solvent is used as the eluent, and the eluent B is obtained when the components of the mixture of Cinobufacin and Bufafalin...
Embodiment 3
[0051] Toad venom is crushed into a fine powder that passes through a 20-mesh sieve, 70% ethanol is added to 20 times the amount of toad venom, heated and refluxed for extraction twice, each time for 4 hours, the extract is filtered, and the ethanol is recovered from the filtrate until it has no ethanol smell, and the ethanol extract is obtained A;
[0052](2) In the extract A, add 5 times the amount of toad venom, silica gel with a particle size of 100-200 mesh, evaporate to dryness, and add the top of the chromatography column that has been filled with silica gel (the diameter-to-height ratio of the silica gel column is 1:3, and the filling volume is 20 to 30 times the amount of toad venom in extract A), first use petroleum ether-acetone (9:1) mixed solvent as the eluent, elute, discard the eluent, and then use petroleum ether-acetone (8.5: 1.5) The mixed solvent is used as the eluent, and the eluent B is obtained when the components of the mixture of cinobufaction base and ...
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