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Preparation method for bulleyaconitine A

A technology for clathrin and methanol, applied in the field of preparation of high-purity clathrate, can solve the problems of high cost, complicated method steps, difficult recovery and reuse, etc., achieves a high degree of fluidization, reduces production costs, The effect of easy recycling

Inactive Publication Date: 2014-07-09
YUNNAN AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The elution solvents involved in these methods are all ternary systems, and the polarity of the solvent changes after recovery, which is not easy to recycle and reuse, and the cost is high and the method steps are complicated

Method used

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  • Preparation method for bulleyaconitine A
  • Preparation method for bulleyaconitine A

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The preparation method of aconitin provided by the invention specifically comprises the following processing steps:

[0015] (1) extract

[0016] Crush the dried roots of Aconitum transsectum Diels., infiltrate them with an appropriate amount of methanol for 24 hours, and use methanol for percolation extraction. The amount of methanol used is 8 to 15 times the amount of medicinal materials. Combine the leachate and concentrate to a paste.

[0017] (2) Extraction and separation

[0018] Dissolve the paste obtained in step (1) with 1.5% hydrochloric acid solution, filter, adjust the pH to 9 with concentrated ammonia water (25%), and extract the lye twice with petroleum ether, then use chloroform or ethyl acetate Extract 3 times, combine chloroform or ethyl acetate and recover chloroform under reduced pressure to a paste to obtain crude total alkali.

[0019] (3) Separation and purification by column chromatography

[0020] The crude total alkali obtained in step (2) wa...

Embodiment 2

[0026] Take 10 kg of dried roots of Aconitum aconitum, crush them, infiltrate them with an appropriate amount of methanol for 24 hours, and use methanol for percolation extraction. The amount of methanol used is 10 times the amount of medicinal materials. Dissolve, filter, adjust pH to 9 with concentrated ammonia water (25%), and extract lye with petroleum ether twice, 5 liters each; Compress and recover to a paste to obtain 110 g of crude total alkali. The crude total alkali was dissolved in 300 ml of chloroform and adsorbed on 164 g of 200-300 mesh silica gel to mix the sample, evaporated to dryness at room temperature, and subjected to silica gel column chromatography, with a gradient of petroleum ether: diethylamine (50:1-20:2) Elution, collect the eluate, use Aconitin as a control with thin-layer chromatography [developing solvent is petroleum ether: acetone: diethylamine (20:1:1)] tracking detection, and combine the main components containing Aconitin Fractions, the sol...

Embodiment 3

[0028] Take 10 kg of dried roots of Aconitum aconitum, crush them, infiltrate them with an appropriate amount of methanol for 24 hours, and use methanol for diafiltration extraction. The amount of methanol used is 8 times the amount of medicinal materials. Combine the leachate, concentrate to paste, and use 1.5% hydrochloric acid solution Dissolve, filter, adjust pH to 9 with concentrated ammonia water (25%), and extract lye with petroleum ether twice, 5 liters each; then extract 3 times with chloroform, 5 liters each time, combine chloroform solution, Recover under reduced pressure to a creamy state to obtain 105 g of crude total alkali. The crude total alkali was dissolved in 300 ml of chloroform and adsorbed on 160 g of 200-300 mesh silica gel to mix the sample, evaporated to dryness at room temperature, and subjected to silica gel column chromatography, with a gradient of petroleum ether: diethylamine (50:1-20:2) Elution, collect the eluate, use Aconitin as a control with ...

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Abstract

A preparation method for high-purity bulleyaconitine A comprises the steps of extraction, extraction separation, column chromatography separation and purification, crystallization and purification. The content of the bulleyaconitine A in the product detected by a high performance liquid chromatography (HPLC) is greater than 98 percent. According to the preparation method, the extraction is realized at room temperature and the bulleyaconitine A is free from hydrolysis; a silica gel column chromatography eluent only uses a binary system, a solvent is recycled more easily and the adjustment on the polarity trends to be consistent more easily, and thus the production cost is greatly reduced. The preparation method is simple, easy for industrial production and high in streamline degree; and the purity of products is high.

Description

Technical field: [0001] The invention belongs to the field of natural medicine preparation, and in particular relates to a preparation method of high-purity aconitin. Background technique: [0002] Bulleyaconitine A (Bulleyaconitine A, molecular formula C 35 h 49 NO 10 , with a molecular weight of 643.77) has strong analgesic and anti-inflammatory pharmacological activities. Experiments have confirmed that aconitin is a central analgesic with strong analgesic activity and no addiction. At present, Aconitin tablets, oral liquids, injections and other dosage forms using Aconitin as raw material are used clinically, mainly for the treatment of advanced cancer pain, rheumatism and rheumatoid arthritis, periarthritis of the shoulder, shoulder and arm pain, Stiff neck, osteoarthritis, benign joint pain, lumbar and extremity joint sprains, contusions, lumbar muscle strain and low back pain, sciatica, myofibritis and costochondritis, herpes zoster, cold headache, toothache, etc. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D221/22
Inventor 沈勇艾洪莲赵大克张丽梅郑丽李晓波字淑慧
Owner YUNNAN AGRICULTURAL UNIVERSITY
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