Preparation method of galanthamine
A technology of galantamine and chloroform, applied in the field of preparation of galantamine, can solve the problems of low galantamine content, unfavorable large production operation, large sewage discharge and the like
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[0016] Example 1
[0017] Take 10Kg of Lycoris radiata bulb fine powder, add it to pH=12 triethylamine aqueous solution, soak overnight, dry, and place in CO 2 Supercritical extraction in supercritical extraction equipment, CO 2 The flow is 2ml / min / g crude drug, 90% ethanol aqueous solution is selected as the entrainer, the flow is 0.4ml / min / g crude drug, the extraction temperature is 60℃, the pressure is 30MPa, and the extraction time is 2h; the extract is dissolved by adding 2% hydrochloric acid aqueous solution, Filter, add CHCl to the filtrate 3 Extract, remove the lower layer, adjust the pH to 13, add CHCl 3 Extraction, take CHCl 3 The layer is separated by an alumina chromatographic column, and the lower layer solution of chloroform-methanol-water (5:3:1) is used as the eluent for elution. The eluent is collected, concentrated, and reconstituted with acetone-ethanol (1:1). After crystallization, washing and drying, 213 mg of galantamine was obtained, and its purity was 94.5%...
Example Embodiment
[0018] Example 2
[0019] Take 10Kg of fine powder of Lycoris radiata bulb, add it to pH=10 ammonia solution, soak overnight, dry, and place in CO 2 Supercritical extraction in supercritical extraction equipment, CO 2 The flow rate is 1ml / min / g crude drug, 90% ethanol aqueous solution is selected as the entrainer, the flow rate is 0.1ml / min / g crude drug, the extraction temperature is 20℃, the pressure is 10MPa, and the extraction time is 0.5h; the extract is dissolved in 2% hydrochloric acid aqueous solution , Filter, add CHCl to the filtrate 3 Extract, remove the lower layer, adjust the pH to 13, add CHCl 3 Extraction, take CHCl 3 The layer is separated by an alumina chromatographic column, and the lower layer solution of chloroform-methanol-water (4:5:1) is used as the eluent for elution. The eluent is collected, concentrated, and added with acetone-ethanol (3:1). After crystallization, washing and drying, 175 mg of galantamine was obtained, and its purity was 92.3% by HPLC.
Example Embodiment
[0020] Example 3
[0021] Take 10Kg of fine powder of Lycoris radiata bulb, add it to pH=13 triethylamine aqueous solution, soak overnight, dry, and place in CO 2 Supercritical extraction in supercritical extraction equipment, CO 2 The flow rate is 5ml / min / g crude drug, 90% ethanol aqueous solution is selected as the entrainer, the flow rate is 0.8ml / min / g crude drug, the extraction temperature is 80℃, the pressure is 50MPa, and the extraction time is 4h; the extract is dissolved by adding 2% hydrochloric acid aqueous solution, Filter, add CHCl to the filtrate 3 Extract, remove the lower layer, adjust the pH to 13, add CHCl 3 Extraction, take CHCl 3 The layer is separated by an alumina chromatographic column, and the lower layer solution of chloroform-methanol-water (2:1:1) is used as the eluent for elution. After crystallization, washing and drying, 235 mg of galantamine was obtained, and its purity was 93.4% by HPLC.
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