Method and system for simultaneously extracting three c-glycosylflavone compound monomers from herba desmodii styracifolii
A flavonoid carbon glycoside compound and the technology of Desmodium sativa, applied in the field of phytochemistry, to achieve the effects of simple process operation, high purity and high product yield
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Embodiment 1
[0041] Figure 8 Show the general flow process of the inventive method, comprise following:
[0042] 1. Raw material processing: select 45,000-50,000 parts by weight of the leguminous plant Desmodium glabra, cut into 5-10 cm sections, wash off the sediment with drinking water, drain, and feed.
[0043] 2. Ethanol extraction: 80% ethanol reflux extraction twice, the first time 12 times the amount for 2 hours, the second time 10 times the amount for 1.5 hours; combine the two alcohol extracts, recover the ethanol until it has no alcohol smell.
[0044] 3. Concentration under reduced pressure: add water to dilute the extract concentrate to 5 times the volume of the medicinal material; filter through a 200-mesh filter cloth; get the column liquid; pack the net product resin that has been treated with 95% ethanol in advance, and replace it with purified water; The upper column liquid is pumped into the column for adsorption, and the flow rate is controlled to be 0.5-1 times BV / h. ...
Embodiment 2
[0067] 1. Carry out according to the steps 1-3 of Example 1 to obtain the Guangjin bulk drug.
[0068] 2. Multi-stage chromatographic separation and identification
[0069] (1) 300-400 parts by weight of Guangjin crude drug is separated by AB-8 macroporous resin chromatography, i.e. chromatographic separation I, ethanol-water mixed solvent 25:75, 35:65, 45:55, 65:35 gradient washing Take off, wash each gradient until there is no color, combine the fractions to get 25%, 35%, 45%, and 65% in four parts.
[0070](2) Use ODS reversed-phase medium-pressure chromatography to separate 35% of the chromatogram I, that is, chromatographic separation II. Specifically: the conditions are 8% isocratic for 30 minutes, 8-30% gradient for 200 minutes, and the peak is produced according to the chromatogram Sequentially, collect in fractions, collect one fraction per 100-150 volume fractions, collect a total of 40-50 fractions, combine the same fractions after HPLC detection, and obtain 3 merg...
Embodiment 3
[0078] 1. Carry out according to the steps 1-3 of Example 1 to obtain the Guangjin bulk drug.
[0079] 2. Multi-stage chromatographic separation and identification
[0080] (1) 300-400 parts by weight of Guangjin crude drug is separated by AB-8 macroporous resin chromatography, that is, chromatographic separation I, ethanol-water mixed solvent 20:80, 30:70, 40:60, 60:40 gradient washing Take off, wash each gradient until there is no color, combine the fractions to get 20%, 30%, 40%, and 60% in four parts.
[0081] (2) Separating 30% of the part obtained by chromatography I with ODS reverse-phase medium-pressure chromatography, that is, chromatographic separation II, specifically: use ethanol-water, the condition is 12% isocratic for 30 minutes, and the gradient of 12-30% is eluted for 200 minutes. According to the order of the peaks in the chromatogram, collect in portions, collect one portion per 100-150 volume parts, collect 40-50 fractions in total, combine the same fracti...
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