A kind of swertirolactone compound and its preparation method, preparation and application
A technology of sorghum lactone and compound, which is applied in the field of sorghum lactone compound and its preparation, can solve the problems of thermal instability of alkenyl ether bond, occurrence of decomposition, transformation, hidden danger of clinical safety medication, etc., and achieves easy access to raw materials. The effect of obtaining, simple process and strong operability
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[0024] The preparation method of swertiger lactone compound of the present invention comprises the following steps:
[0025] A. Take swertiamarin, add water with a weight ratio of 3 to 5 times, and reflux at 90 to 100°C for 5 to 7 hours until the swertiamarin completely disappears to obtain the water-soluble part a and the fat-soluble part b;
[0026] B. Take the water-soluble part a, carry out gradient elution with methanol-water solution with a volume ratio of 5:95~100:0 through a reverse column, and collect in sections;
[0027] C. Take the eluate under the methanol-water solution section with a volume ratio of 15:85~30:70, concentrate under reduced pressure to obtain extract a, and extract a through a macroporous adsorption resin column for adsorption, with a volume ratio of 0:100 ~100:0 methanol-water solution for gradient elution, the extract b concentrated under reduced pressure of the eluent, and the extract b is packed with 4~5 times the amount of 160~200 mesh silica ...
Embodiment 1
[0035]Take 5.8 kg of swertiamarin, add 3 times the weight of water, heat to 90°C, and keep the temperature constant for 6 hours, the swertiamarin completely disappears, and the water-soluble part and the fat-soluble part are obtained. The water-soluble part was collected in sections by reverse medium-pressure column, gradient elution with methanol-water (5:95~100:0). Take methanol-water as the eluent under the polar section (15:85~30:70), concentrate under reduced pressure to obtain the extract, and the obtained extract is adsorbed by HPD-100 macroporous adsorption resin, and methanol-water (0: 100-100:0) for gradient elution; and then silica gel column chromatography, using petroleum ether-ethyl acetate (8:1-2:1) for gradient elution to obtain the crude extract of the target compound. After concentration, the crude extract was adsorbed by MCI-gel, and gradient eluted with methanol-water (20:80~100:0), followed by thin-layer chromatography to collect the target components, and...
Embodiment 2
[0037] Take 10 kg of swertiamarin, add 5 times the weight of water, heat to 95°C, keep the temperature for 5 hours, the swertiamarin completely disappears, and the water-soluble part and the fat-soluble part are obtained. The water-soluble part was collected in sections by reverse medium-pressure column, gradient elution with methanol-water (5:95~100:0). Take methanol-water as the eluent under the polar section (15:85~30:70), concentrate under reduced pressure to obtain the extract, and the obtained extract is adsorbed by HPD-300 macroporous adsorption resin, and methanol-water (0: 100-100:0) for gradient elution; and then silica gel column chromatography, using petroleum ether-ethyl acetate (8:1-2:1) for gradient elution to obtain the crude extract of the target compound. After concentration, the crude extract was adsorbed by MCI-gel, and gradient eluted with methanol-water (20:80~100:0), followed by thin-layer chromatography to collect the target components, and the eluate w...
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