Hairy sepal ponicidin crystallization, preparation method and medicament composition containing the same
A technology of eelin and composition, applied in the field of diterpene compounds, which can solve the problems of poor storage stability, easy moisture absorption, unfavorable industrial production, etc.
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Embodiment 1
[0056] Method 1 for the preparation of echinocetin crystal type I sample:
[0057] Take 100mg of echinacein B sample, heat it at 40°C and dissolve it completely in 50mL of methanol solution, place it at room temperature and pressure for 96 hours for recrystallization, filter and wash the obtained crystal, and dry it under vacuum for 2 hours to prepare the obtained crystal I-type calyxin B solid matter 82mg.
[0058] Method 2 for the preparation of echinocetin crystal type I samples:
[0059] Take 100 mg of eelin B, heat it at 45°C and dissolve it completely in 50 mL of ethanol: acetone = 1: 1 solution, place it under normal temperature and pressure for 72 hours for recrystallization, filter and wash the obtained crystals, and dry under vacuum After 2 hours, 84 mg of crystalline form I eclexin was prepared as a solid substance.
[0060] Problems that need to be explained: Since there are 12 single organic solvents that can be used to prepare samples of crystalline form B, and...
Embodiment 2
[0062] Method 1 for the preparation of echinacein crystal type II samples:
[0063] Take 200 mg of calyxin, and use crystal type I solid sample as the preparation raw material at a temperature of 10-30°C, and use the method of physical and mechanical lattice destruction and molecular rearrangement to crystallize to obtain the solid material of calyxin crystal form 185 mg, or 188 mg of echinacein crystal II solid substance prepared by changing physical pressure conditions and temperature conditions.
[0064] Method 2 for the preparation of echinocetin crystal type II samples:
[0065] Take 200mg of eriocalyxin sample, first use acetone solvent to completely dissolve the eriocalyxin sample at room temperature of 15-25°C, and then quickly prepare 193mg of crystalline type II eriocalyxin as a solid substance by cold spray method.
[0066] Problems that need to be explained: Since there are 12 single organic solvents that can be used to prepare samples of crystalline form B, and t...
Embodiment 3
[0068] The preparation method of echinocetin crystal type III sample:
[0069] Take 100mg of eriocalyxin, heat it at 40°C and dissolve it completely in 50mL of methanol, and then use a rotary evaporator to quickly evaporate the solvent under a vacuum condition at a temperature of 45°C to prepare a solid substance of crystalline type I eriocalyxin 97mg, and then the obtained sample was placed in a 225°C incubator and heated for 30 minutes to transform the crystal to obtain 95mg of the crystalline type III solid sample of calyxin.
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