Method for separating and purifying fangchinoline and tetrandrine from stephania tetrandra
A technology of fangchinoline and tetrandrine, which is applied in the chemical industry, can solve the problems of not being able to meet market demand, small production scale, and high production cost, and achieve the effects of shortening separation time, saving reagents, and low cost
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Embodiment 1
[0027] Take 100 g of the crushed fangji medicinal material, add 0.5L of 50% ethanol, heat under reflux for 100 minutes, and separate the residue and the extract; add 0.5L of 50% ethanol to the residue and reflux for 2 times, each time for 60 minutes, to separate the residue and extracting liquid; combining the extracting liquid obtained by the above-mentioned 3 times of reflux, and recovering ethanol by vacuum distillation to obtain the extract of powdered fangji crude extract.
[0028] Dissolve the extract of the crude extract of fenugreek with 0.2L of 0.5% hydrochloric acid, stand for 36h, filter to remove the precipitate, and obtain a solution; adjust the pH of the above solution to 8 with ammonia water, stand for 24h, and filter to obtain the precipitate, and the precipitate is aired. Drying to obtain the crude extract of tetrandrine alkaloids.
[0029] The diethyl ether-phosphate buffer solution was used as a high-speed countercurrent chromatography two-phase solvent syst...
Embodiment 2
[0031] Take 100g of the crushed fangji medicinal material, add 2L of 55% ethanol, heat under reflux for 90 minutes, and separate the residue and the extract; add 1L of 55% ethanol to the residue and reflux twice for 50 minutes each time to separate the residue and extract Combine the extracts obtained by the above-mentioned 3 refluxes, and recover ethanol by vacuum distillation to obtain the crude extract of tetrandrine.
[0032]Dissolve the extract of Fangji crude extract with 0.16L of 1.0% hydrochloric acid, let it stand for 36 hours, and filter to remove the precipitate to obtain the solution; adjust the pH of the above solution to 10 with ammonia water, let it stand for 36 hours, then filter to obtain the precipitate, and let the precipitate dry in the air dry to obtain the crude extract of Fangji alkaloid.
[0033] Diethyl ether-phosphate buffer was used as a high-speed countercurrent chromatography two-phase solvent system to separate and purify the extract of Fangji. Th...
Embodiment 3
[0035] Take 100g of pulverized Fangji medicinal material, add 0.5L 60% ethanol, heat and reflux for 80 minutes, separate the residue and extract; add 0.5L 60% ethanol to the residue and reflux twice, each time for 50 minutes, separate the residue and extract; combine the extracts obtained by reflux for the above 3 times, and recover ethanol by distillation under reduced pressure to obtain the crude extract of tetrandrine.
[0036] Dissolve the extract of Fangji crude extract with 0.08L of 4.0% hydrochloric acid, let it stand for 12 hours, and then filter to remove the precipitate to obtain a solution; adjust the pH of the above solution to 8 with ammonia water, let it stand for 24 hours, then filter to obtain a precipitate, and let the precipitate dry in the air dry to obtain the crude extract of Fangji alkaloid.
[0037] Diethyl ether-phosphate buffer was used as a high-speed countercurrent chromatography two-phase solvent system to separate and purify the extract of Fangji. ...
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