Atropine separated and purified from alkaloid extract and preparation method thereof
A technology of separation and purification and alkaloids, applied in the direction of organic chemistry, can solve the problems of sewage treatment pressure, inability to pass chemical synthesis, waste of resources, etc., to reduce waste, promote industrial development, and save resources.
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[0014] On the one hand, the present invention provides a preparation method for separating and purifying atropine from alkaloid extract, comprising the following steps: obtaining alkaloid extract from Huashan ginseng by leaching, extracting alkaloid extract with chloroform, and recovering under reduced pressure Chloroform is used to obtain intermediate 1, and intermediate 1 uses the mixed solution of ethyl acetate / methanol / concentrated ammonia water as a developer to separate out the stock solution, and the stock solution is refluxed at a temperature of 90-100°C for 3-6 hours to obtain intermediate 2, and intermediate Body double crystallization to obtain the crude product, crude product decolorization to obtain atropine.
[0015] Impregnating Huashan ginseng with the extracting solution to extract the effective components in the extracting solution, and then filtering and concentrating to obtain the alkaloid extract. Hyoscyamine is easily soluble in chloroform, so the alkaloi...
Embodiment 1
[0027] The embodiment of the present invention proposes a preparation method for separating and purifying atropine from alkaloid extract, comprising the following steps:
[0028] Extraction of alkaloids: use ethanol with a volume fraction of 80% vol to impregnate Huashan ginseng at a temperature of 40°C, then filter to obtain the filtrate and filter residue, then add the above-mentioned ethanol to the filter residue for impregnation and filter again. Perform extraction.
[0029] Preparation of alkaloid extract: use the above method to extract Huashan ginseng 4 times, then combine the filtrates, concentrate the mixed filtrate under reduced pressure to obtain extracts, adjust the pH of the extracts to 3, let stand for 6 hours, and then adjust After the pH was set to 10 and left to stand for 6 hours, the original solution was obtained, and the original solution was extracted with chloroform, then concentrated under reduced pressure, and the chloroform was recovered to obtain an a...
Embodiment 2
[0034] The embodiment of the present invention proposes a preparation method for separating and purifying atropine from alkaloid extract, comprising the following steps:
[0035] Extraction of alkaloids: use ethanol with a volume fraction of 70% vol to impregnate Huashan ginseng at a temperature of 35°C, then filter to obtain the filtrate and filter residue, then add the above-mentioned ethanol to the filter residue for impregnation and filter again, such a cycle operation is effective for Huashan ginseng Perform extraction.
[0036] Preparation of alkaloid extract: use the above method to leach Huashan ginseng 3 times, then combine the filtrates, concentrate the mixed filtrate under reduced pressure to obtain extracts, adjust the pH of the extracts to 1, let stand for 5 hours, and then adjust The original solution was obtained after the pH reached 9 and left to stand for 5 hours, and the original solution was extracted with chloroform, then concentrated under reduced pressure...
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