A kind of linear furanocoumarin compound and its preparation method and application
A technology of furanocoumarins and coumarins, applied in the field of online furanocoumarins and their preparation, can solve the problems of few chemical components and no pharmacological activity research reports
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[0042] The preparation method of the new linear furocoumarin compound of the present invention comprises the following steps:
[0043] 1) Take a certain quality of Xing’an Duhuo dry root, use ethanol, methanol, 90% ethanol or 90% methanol with a volume of 1 to 8 times the mass of Xing’an Duhuo dry root to heat and reflux near the boiling point for 1 to 5 times, each time 2 After ~4 hours, the combined extracts were recovered under reduced pressure to remove the solvent to obtain the total extract.
[0044]2) Suspend the total extract in water, the volume ratio of the total extract to water is 1:1 to 1:5 to obtain an extract solution, which is sequentially extracted with an equal volume of organic solvent, wherein the first During the first extraction, the extract or concentrated solution is extracted with equal volumes of petroleum ether, and then each extraction is to separate the organic layer after the last extraction, and the remaining water layer is extracted with an equa...
Embodiment 1
[0052] 1. Separation and purification of linear furanocoumarins
[0053] 1) Get 6.5kg of dry roots of Kankura, extract 3 times with 19.5L of ethanol under reflux, each time for 3 hours, at this time, the volume of ethanol is 3 times of the quality of the dry roots of Xing'an Duhuo, and the combined ethanol extracts are decompressed Recover the solvent to obtain the total extract;
[0054] 2) Suspend the total extract in 3 times the volume of water, extract 4 times with petroleum ether and chloroform in equal volume successively, and obtain petroleum ether layer, chloroform layer and the remaining water layer.
[0055] 3) Take 81.1 g of the chloroform extraction layer, apply the sample to silica gel column chromatography, use the chloroform-methanol system as the eluent, and carry out gradient elution according to the volume ratio (v / v) of (100:0) to (0:100) , collected once every 500mL, the solvent was recovered by atmospheric distillation, and the same fractions were merged...
Embodiment 2
[0078] 1) Take 10 kg of dried roots of Kankura, heat and reflux extraction with 30 L of 90% ethanol for 4 times, each time for 3 hours, combine the extracts to recover the solvent under reduced pressure, and obtain the total extract;
[0079] 2) The total extract was suspended in 4 times the volume of water, extracted 4 times with equal volumes of petroleum ether and chloroform, and the organic layer was distilled off under normal pressure or reduced pressure to obtain a petroleum ether layer and a chloroform layer respectively.
[0080] 3) Take 100 g of the chloroform extraction layer, apply it to silica gel column chromatography, use the chloroform-methanol system as the eluent, and carry out gradient elution according to the volume ratio (v / v) of (100:0) to (0:100), Collect once every 500mL, atmospheric distillation reclaims solvent, TLC detects and merges identical fractions, obtains 33 fractions altogether, named as Fr1-Fr33 respectively, gets wherein Fr13 fractions, i.e. ...
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