Method for preparing high-purity bulleyaconitine A
A kind of aconitin, high-purity technology, applied in the direction of organic chemistry, can solve the problems of high production cost, high consumption of chromatographic column packing, environmental pollution, etc., to shorten the production cycle, reduce production cost and reduce environmental pollution. pollution effect
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Embodiment 1
[0024] Take 10kg of fresh roots of Aconiti officinalis, wash them with water, add 20L 0.1mol / L H 2 SO 4 After soaking in the aqueous solution for 24 hours, put it into a homogenizer, and then add 100L 0.1mol / L H 2 SO 4 The aqueous solution was homogenized and extracted for 10 minutes, filtered, and the filtrate was collected. Add 100L of 0.1mol / L H 2 SO 4 The aqueous solution was subjected to cavitation vortex solid-liquid extraction for 30 min under a negative pressure of 0.06 MPa, and then filtered. This step was repeated 4 times, and the filtrates were combined and concentrated. After passing through 732 type cation exchange resin with a weight of 20kg, first elute with 4 times the column volume of water, then elute with 70% ethanol solution (containing 2% NaOH), collect the eluate, adjust the pH to 7.00, concentrate, and remove ethanol. The concentrated solution was passed through D101 type macroporous adsorption resin with a weight of 3 kg, and was first eluted with...
Embodiment 2
[0026] Take 10kg of fresh roots of Aconitum aconitum, wash them with water, add 40L 0.2mol / L HCl aqueous solution to soak for 24 hours, put them into a homogenizer, add 60L 0.2mol / L HCl aqueous solution to homogenate and extract for 15min, filter, and collect the filtrate . Add 60 L of 0.2 mol / L HCl aqueous solution to the remaining material, perform cavitational vortex solid-liquid extraction for 60 min under a negative pressure of 0.1 MPa, and filter. This step is repeated 4 times, and the filtrates are combined and concentrated. After passing through the 732-type cation exchange resin with a weight of 30 kg, it was first eluted with 4 times the column volume of water, and then eluted with 2% HCl aqueous solution. The eluate was collected, adjusted to pH 7.00, and concentrated. The concentrated solution is passed through the AB-8 type macroporous adsorption resin with a weight of 3 kg, and is first eluted with 4 column volumes of 30% ethanol, and then 7 column volumes of 70%...
Embodiment 3
[0028] Take 10kg of fresh roots of Aconiti fruticosa, wash them with clean water, add 30L of 0.4mol / L HCl aqueous solution to soak for 24 hours, put them into a homogenizer, add 80L of 0.4mol / L HCl aqueous solution to homogenate for 20min, filter and collect filtrate. Add 80 L of 0.4 mol / L HCl aqueous solution to the remaining material, and perform cavitation, mixing, and solid-liquid extraction for 45 minutes under negative pressure of 0.08 MPa and filter. This step was repeated 4 times, and the combined filtrates were concentrated. After passing through 20 kg of 732-type cation exchange resin, it was first eluted with 4 times the column volume of water, and then eluted with 3 mol / L NaCl solution, and the eluate was collected and concentrated. The concentrated solution was passed through D101 type macroporous adsorption resin with a weight of 3 kg, and was first eluted with 3 column volumes of 40% ethanol, and then 5 column volumes of 80% ethanol. The eluate was collected an...
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