Method for extracting antofine
An extraction method and technology for extracting liquid, which are applied in the field of extraction and separation of traditional Chinese medicines, can solve problems such as an industrial extraction and purification method for antophene that has not yet been found, and achieve the effects of high product purity, reduced impurity dissolution, and large extraction amount.
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Embodiment 1
[0021] Grind the old melon head raw material, take 1kg, add 1% hydrochloric acid aqueous solution to soak for 3 hours, ultrasonically treat for 40 minutes, filter to obtain the extract, adjust the pH to 7.5, add ultrafiltration with a molecular weight cut-off of 3000, and then add a molecular weight cut-off of 200 Nanofiltration membrane nanofiltration to obtain the concentrated solution, adjust the pH to 10, extract with chloroform, take the organic layer, recycle the chloroform, and dry to obtain the crude product; Membrane filtration to obtain the sample solution, the extraction column is filled with C8 bonded phase, the particle size is 10 μm, the column length is 15 cm, and the diameter is 4 cm. Diamine aqueous solution was used as the mobile phase, the volume ratio was 23:77, the flow rate was controlled at 50ml / min, and the ultraviolet on-line detection was performed at a detection wavelength of 258nm. The target components were collected and dried at low temperature to ...
Embodiment 2
[0023] Grind the old melon head raw material, take 1kg, add 0.5% sulfuric acid aqueous solution to soak for 8 hours, ultrasonically treat for 45 minutes, filter to obtain the extract, adjust the pH to 8.5, add ultrafiltration with a molecular weight cut-off of 5000, and then add a molecular weight cut-off of 500 Nanofiltration membrane nanofiltration to obtain the concentrated solution, adjust the pH to 9.5, extract with chloroform, take the organic layer, recycle the chloroform, and dry to obtain the crude product; the crude product is dissolved in 95% ethanol to form a solution with a concentration of 100mg / ml, and the solution is subjected to 0.45 μm microfiltration membrane to obtain the sample solution, the extraction column is filled with C18 bonded phase, the particle size is 20 μm, the column length is 10 cm, and the diameter is 1 cm. The % ethylenediamine aqueous solution was used as the mobile phase, the volume ratio was 23:77, the flow rate was controlled at 10ml / min...
Embodiment 3
[0025] Grind the old melon head raw material, take 5kg, add 0.8% sulfuric acid aqueous solution to soak for 6 hours, ultrasonically treat for 35 minutes, filter to obtain the extract, adjust the pH to 8, add ultrafiltration membrane ultrafiltration with a molecular weight cut-off of 5000, and then add a molecular weight cut-off of 300 Nanofiltration membrane nanofiltration to obtain the concentrated solution, adjust the pH to 11, extract with chloroform, take the organic layer, recycle the chloroform, and dry to obtain the crude product; Membrane filtration to obtain the sample solution, the extraction column is filled with C18 bonded phase, the particle size is 15 μm, the column length is 50 cm, and the diameter is 10 cm. Diamine aqueous solution was used as the mobile phase, the volume ratio was 23:77, the flow rate was controlled at 250ml / min, and the ultraviolet on-line detection was performed at a detection wavelength of 258nm. The target components were collected and drie...
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