Method for simultaneously extracting baicalin, baicalein and wogonin from scutellaria baicalensis
A technology for wogonin and baicalein, which is applied in the field of traditional Chinese medicine extraction, can solve the problems of resource waste, component loss, loss and the like, and achieves the effects of less waste liquid, reduced loss, and efficient extraction.
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Embodiment 1
[0038] Step 1. Simultaneous extraction: take Scutellaria baicalensis pieces, add 12 times the mass of water to heat and reflux for extraction for 2 hours, filter the extract, add 10 times the amount of water to the filter residue and extract twice, each time for 1.5 hours, and combine the filtrates to obtain baicalin and baicalein and the mixed crude extract of wogonin.
[0039] Step 2. Separation: Concentrate the crude extract from the previous step under reduced pressure to 0.2 g crude drug per 1 mL, load the sample on a D101 macroporous adsorption resin column at a flow rate of 4 BV / h, the sample volume is 1 BV, and elute with water first Until the effluent is colorless, it is eluted with 10BV 60% ethanol and 6BV 80% ethanol in turn, and the 60% ethanol eluate is collected. The main component is baicalin (see figure 2 ), collect 80% ethanol eluate, the main components are baicalein and wogonin (see image 3 ). Concentrate the baicalin eluate to contain 0.5 g crude drug p...
Embodiment 2
[0041] Step 1. Simultaneous extraction: Take Scutellaria baicalensis slices, add 15 times the amount of mass to heat and reflux for extraction for 1.8 h, filter the extract, add 15 times the amount of water to the filter residue and extract once more, combine the filtrates to obtain baicalin, baicalein and wogonin Combine the crude extracts.
[0042]Step 2. Separation: Concentrate the crude extract from the previous step to 0.5 g crude drug per 1 mL, load the sample on the AB-8 macroporous adsorption resin column at a flow rate of 4 BV / h, and the sample volume is 0.5 BV. Eluted with water until the effluent was colorless, then eluted with 8BV 70% ethanol and 4BV 80% ethanol respectively, collected 70% ethanol eluate, the main component was baicalin, collected 80% ethanol eluate, the main component was Baicalein and Wogonin. Concentrate the baicalin eluate to contain 1 g crude drug per mL, adjust the pH value to 2.1 with 1 mol / L sulfuric acid, incubate at 70 °C for 1 h, let st...
Embodiment 3
[0044] Step 1. Simultaneous extraction: take Scutellaria baicalensis slices, add 20 times the mass of water, heat and reflux for extraction for 1.5 h, filter the extract, add 15 times the amount of water to the filter residue and extract once more, combine the filtrates, and obtain baicalin, baicalein and wogonin Combine the crude extracts.
[0045] Step 2. Separation: Concentrate the crude extract from the previous step under reduced pressure to 0.3 g crude drug per 1 mL, and load the HPD-100 macroporous adsorption resin column at a flow rate of 4 BV / h. The sample volume is 1 BV. Eluted with water until the effluent was colorless, then eluted with 9BV 60% ethanol and 6BV 75% ethanol respectively, collected 60% ethanol eluate, the main component was baicalin, collected 75% ethanol eluate, the main component was Baicalein and Wogonin. The crude extract of baicalin was concentrated under reduced pressure to contain 1.5 g crude drug per mL, the pH value was adjusted to 1.8 with ...
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