Preparation of sinomontanine and its hydrobromide
A technology of urinine and urinine base, which is applied in the field of preparation technology of urinine hydrobromide, can solve the problems of long production cycle and low purity, and achieve the advantages of convenient operation, high purity and simple extraction process Effect
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Embodiment 1
[0027] Example 1. A process for extracting aconitine from Aconitum vulgaris:
[0028] Cut the high aconitum root tuber into sections or crush it, add 30-95% ethanol and heat reflux to extract 3 times, the first and second extraction for 2 hours, the third extraction for 1 hour, combine the alcohol extract to recover the ethanol, and concentrate to dilute leaching Paste to obtain the crude extract of Aconitum; add 1 to 5% hydrochloric acid to adjust the pH value to 1, and mix and stir to prepare an acidified liquid; the acidified liquid is adsorbed through the pretreated cation exchange resin column at a flow rate of 0.8-1ml / min, after all the drug solution has passed through the resin column, the resin column is eluted with water to remove acid-insoluble impurities, and then the resin column is eluted with concentrated ammonia water and the eluate is collected, and the eluate is recovered under reduced pressure, and the alkaline wash is further extracted with chloroform The liqui...
Embodiment 2
[0029] Example 2. A process for extracting aconitine A from Aconitum vulgare:
[0030] Cut or crush the root tuber of high aconitum, extract with ethanol dipping method, and concentrate the extract into a dilute extract to obtain a crude extract of high aconitum; add phosphoric acid to adjust the pH value to 1, mix and stir to make acidified liquid ; Pass the acidified solution through the pretreated weakly polar macroporous adsorption resin column at a flow rate of 0.8-1ml / min. After the drug solution passes through the resin column, the resin column is eluted with water to remove acid-insoluble impurities, and then 1~ 10% sodium carbonate solution is eluted, the alkali eluate is collected, and then the alkali eluate is extracted with chloroform, the chloroform is recovered and concentrated into an extract, and then the extract is dissolved in ethanol, placed overnight, crystallized, and washed with ethanol to obtain Contains Aconitine.
Embodiment 3
[0031] Example 3. A process for extracting aconitine A from Aconitum vulgare:
[0032] Cut the root tuber of high aconitum into sections or crush it, soak it in hydrochloric acid with a concentration of 1 to 5% for 3 to 10 days, and extract it (the amount of hydrochloric acid added is 620 times the weight of the crude medicinal material), filter, and pass the acidified solution through The pretreated AB-8 macroporous adsorption resin column has a flow rate of 0.8-1ml / min. After the drug solution passes through the resin column, the resin column is first eluted with water to remove acid-insoluble impurities, and then 1-10% sodium hydroxide is used. The solution is eluted, and the alkaline eluate is collected, and then the alkaline eluate is extracted with ethanol, and the ethanol is recovered under reduced pressure, placed overnight, crystallized, and washed with ethanol to obtain aconitine.
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