Effective cardiotonic parts of Chinese silkvine root bark and their preparing method medicine preparation and application
An effective part, the technology of Xiangjiapi, which is applied in the effective part of Xiangjiapi to strengthen the heart, its preparation method and the pharmaceutical preparation containing them, and the application field of medicine for treating acute and chronic congestive heart failure, which can solve the problem of less side effects , control of the content of barley toxin, enrichment of barley toxin, etc., to achieve the effect of simple process
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Embodiment 1
[0032] Embodiment 1 resin adsorption-normal phase column chromatography
[0033] Cypress bark extract 60g, suspended in water, filtered with D 101 Macroporous resin adsorption, first washed with water, then eluted with 10% ethanol, then eluted with 60% ethanol, collected 60% eluent, concentrated to dryness under reduced pressure, and recovered the solvent; the resulting solid was subjected to silica gel column chromatography, Ethyl acetate:methanol=20:1 isocratic elution, each 100mL as a portion, using thin-layer chromatography (developing solvent: chloroform:methanol:water=65:35:10 lower layer, silica gel G thin-layer plate, 3 , 5'-dinitrobenzoic acid reagent for color development) to test the collected fractions, combine the fractions containing barretoxin, concentrate under reduced pressure and carry out another silica gel column chromatography under the same conditions, and the thin layer test (Thin-layer conditions are the same as above), merge the fractions with higher ...
Embodiment 2
[0034] Embodiment 2 Soxhlet extraction-normal phase column chromatography
[0035] 25g of Cyperus cypress extract, mixed with 25g of silica gel, extracted with ethyl acetate for Soxhlet extraction for 12 hours; the extract was concentrated to dryness under reduced pressure, the solvent was recovered, the obtained solid was mixed with 5g of silica gel, and the sample was placed on Silica gel column, first eluted with ethyl acetate, then eluted with ethyl acetate: ethanol = 25: 1, tested by TLC (the TLC conditions are the same as in Example 1), and the fractions with higher glucosinolate content were combined , freeze-dried to obtain 48 mg of the effective part of the heart-tonic effect of Xiangjiapi, and the content of salivatoxin was determined by HPLC to be 58%.
Embodiment 3
[0036] Embodiment 3 reverse phase column chromatography
[0037]Carry out reverse-phase column chromatography with 5 g of Cyperus bark extract, the filler is carbon-octave bonded phase silica gel, and use 10% to 99.5% methanol for gradient elution, and the TLC test (thin-layer condition embodiment 1) collects willow poison Fractions with higher glucoside content were combined, concentrated, and then spray-dried to obtain 10 mg of the effective fraction of Xiangjiapi cardiotonic effect. As determined by HPLC, the content of glucoside was 56%; the fraction with lower glucoside content Reverse-phase column chromatography can be performed again.
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