Water phase/organic phase two-phase extraction-chromatography purification method for gutta-percha
A purification method and organic phase technology, which is applied in the purification field of Eucommia gum aqueous phase/organic phase two-phase extraction-chromatography, which can solve the problems of large pollution of organic volatiles, failure to remove, and large consumption of solvents, etc.
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Embodiment 1
[0024] 1. Filtration of Eucommia coarse glue solution:
[0025] Use a filter to filter out the residues visible to the naked eye from the extract obtained by extracting eucommia gum with petroleum ether, and let the glue-containing solution stand at 50°C for 6 hours, and then use a finer filter to remove finer residues to obtain light yellow Containing gum solution, as the next purification raw material.
[0026] 2. Aqueous-organic two-phase extraction:
[0027] Mix the aqueous phase containing 1% chelating agent EDTA and 1% ammonium salt with the Eucommia gum organic solvent obtained in the previous step, the aqueous phase: organic phase volume ratio is 0.5:1 (v / v), and stir at 30°C After 3 hours, let stand to separate the liquid, and take the upper organic phase for later use.
[0028] 3. Column purification:
[0029] The organic phase obtained above was pressurized and continuously flowed through the chromatographic equipment, and the flow rate of the organic phase was 1...
Embodiment 2
[0031] 1. Filtration of Eucommia coarse glue solution:
[0032] The extract obtained by extracting eucommia gum with toluene was filtered through a filter to remove visible residues, and the glue-containing liquid was left to stand at 55°C for 8 hours, and finer residues were filtered through a finer filter to obtain a light yellow Glue, as the next purification raw material.
[0033] 2. Aqueous-organic two-phase extraction:
[0034] Mix the aqueous phase containing 2% chelating agent citric acid and 2% NaOH with the Eucommia gum organic solvent obtained in the previous step, the aqueous phase: organic phase volume ratio is 1:1 (v / v), and stir at 60°C After 2 hours, let stand to separate the liquid, and take the upper organic phase for later use.
[0035] 3. Column purification:
[0036] The organic phase obtained above was pressurized and continuously flowed through the chromatographic equipment, and the flow rate of the organic phase was 3BV / h. The chromatography equipme...
Embodiment 3
[0038] 1. Filtration of Eucommia coarse glue solution:
[0039] The extract obtained by extracting eucommia gum with benzene was filtered through a filter to remove visible residues, and the glue-containing liquid was left to stand at 55°C for 7 hours, and finer residues were filtered through a finer filter to obtain a light yellow Glue, as the next purification raw material.
[0040] 2. Aqueous-organic two-phase extraction:
[0041]Mix the aqueous phase containing 3% chelating agent potassium sodium tartrate and 3% KOH with the Eucommia gum organic solvent obtained in the previous step, the aqueous phase: organic phase volume ratio is 1.5:1 (v / v), at 60 ° C Stir for 1 h, let stand for liquid separation, and take the upper organic phase for later use.
[0042] 3. Column purification:
[0043] The organic phase obtained above was pressurized and continuously flowed through the chromatographic equipment, and the flow rate of the organic phase was 2BV / h. The chromatography eq...
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