Method for preparing high-purity bulleyaconitine A

Abstract

The invention discloses a method for preparing high-purity bulleyaconitine A. The method comprises the following steps of: soaking a fresh radix aconiti agrestis root in acid aqueous solution, performing homogenate extraction and cavitation mixing solid-liquid extraction, collecting and concentrating the filtrate, and respectively performing gradient elution to obtain a crude bulleyaconitine A product through ion exchange resin column chromatography and macroporous adsorption resin column chromatography; and uniformly mixing crude bulleyaconitine A product and ethanol aqueous solution, dissolving in a water bath, cooling the filtrate to room temperature, standing and crystallizing at the temperature of 4 DEG C, repeatedly washing the crystal by using the ethanol aqueous solution, and obtaining a final product. According to the method, crushing and extracting are finished in one step through a homogenization method, and the method has the advantages of zero dust and simple flow. By adoption of a negative-pressure cavitation extraction technology, the mass transfer rate is improved, heating is not required, and the production period is shortened; and moreover, the reagents used in the whole process are ethanol and water, the organic solvent amount is greatly reduced, the production cost can be reduced, the environmental pollution is reduced, and the method has good application prospect.

Description

technical field

[0001] The invention belongs to the technical field of plant purification, and in particular relates to a method for extracting and preparing high-purity aconitin from fresh aconitum aconitum. Background technique

[0002] Aconitum aconitum and aconite are traditional Chinese medicinal materials in the Ranunculaceae family, and are commonly used in the treatment of rheumatism, rheumatoid arthritis, sciatica and other emergencies. Its water decoction has been used to relieve the pain of patients with advanced tumors. Aconitin is one of its main active ingredients, which has dual pharmacological effects of central analgesia and peripheral analgesia, and has the characteristics of long analgesic time and no addiction. Its side effects are small, it has no obvious damage to vital organs, and it has no teratogenic effect. At present, it is mainly used in the treatment of acute and chronic pain diseases such as herpes zoster and advanced cancer pain, rheumatism an...

Examples

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...

technical field

[0001] The invention belongs to the technical field of plant purification, and in particular relates to a method for extracting and preparing high-purity aconitin from fresh aconitum aconitum. Background technique

[0002] Aconitum aconitum and aconite are traditional Chinese medicinal materials in the Ranunculaceae family, and are commonly used in the treatment of rheumatism, rheumatoid arthritis, sciatica and other emergencies. Its water decoction has been used to relieve the pain of patients with advanced tumors. Aconitin is one of its main active ingredients, which has dual pharmacological effects of central analgesia and peripheral analgesia, and has the characteristics of long analgesic time and no addiction. Its side effects are small, it has no obvious damage to vital organs, and it has no teratogenic effect. At present, it is mainly used in the treatment of acute and chronic pain diseases such as herpes zoster and advanced cancer pain, rheumatism an...

Examples

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...