Preparation method of acronycine
The invention relates to a preparation-type technology for citrus alkaloids, which is applied in the field of preparation of citron alkaloids, can solve problems such as the extraction and purification method of citron alkaloids, and achieves high economic benefit and academic value, simple operation and short time-consuming. Effect
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Embodiment 1
[0018] Take 1 kg of mountain oil mandarin root, crush it into coarse powder, feed it from the feed inlet of the head of the continuous countercurrent ultrasonic extraction equipment, add 10 times of 95% ethanol solution from the solvent inlet at the tail of the continuous countercurrent ultrasonic extraction equipment, and carry out continuous countercurrent at 55 °C Ultrasonic extraction for 20 minutes, the ultrasonic frequency is 80KHz, to obtain the extract, the extract is decompressed and the reagents are recovered to obtain the extract, add alumina (120 mesh) to the extract, mix well, dry and pack the column, and use 7 times the column volume of chloroform- Acetone (1:1) mixed solution was eluted, TLC detection was performed, and the fraction of berberine was collected and concentrated to obtain a concentrated solution. Add methanol to the concentrated solution until it just dissolves. The dissolved solution is filtered through a 0.45 μm microfiltration membrane to obtain ...
Embodiment 2
[0020] Take 1 kg of mountain oil mandarin root, crush it into coarse powder, feed it from the feed inlet of the head of the continuous countercurrent ultrasonic extraction equipment, add 10 times of 80% ethanol solution from the solvent inlet at the tail of the continuous countercurrent ultrasonic extraction equipment, and carry out continuous countercurrent at 45 °C Ultrasonic extraction for 100min, the ultrasonic frequency is 60KHz, to obtain the extract, the extract is decompressed and the reagent is recovered to obtain the extract, add alumina (80 mesh) and mix well, dry and pack the column, and use 4 times the column volume of chloroform-acetone (1: 1) Elution with the mixed solution, TLC detection, collection of the alkaloid fraction, and concentration to obtain a concentrated solution. Add methanol to the concentrated solution until it just dissolves. The dissolved solution is filtered through a 0.45 μm microfiltration membrane to obtain a sample solution. Take the filtr...
Embodiment 3
[0022] Take 10 kg of mountain oil mandarin root, crush it into coarse powder, feed it from the feed inlet of the head of the continuous countercurrent ultrasonic extraction equipment, add 6 times of 70% ethanol solution from the solvent inlet at the tail of the continuous countercurrent ultrasonic extraction equipment, and carry out continuous countercurrent at 35 °C Ultrasonic extraction for 50min, the ultrasonic frequency is 50KHz, to obtain the extract, the extract is decompressed and the reagent is recovered to obtain the extract, add alumina (100 mesh) and mix well, dry and pack the column, and use 6 times the column volume of chloroform-acetone (1: 1) Elution with the mixed solution, TLC detection, collection of the alkaloid fraction, and concentration to obtain a concentrated solution. Add methanol to the concentrated solution until it just dissolves. The dissolved solution is filtered through a 0.45 μm microfiltration membrane to obtain a sample solution. Take the filtr...
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