Method for multi-stage extraction of tetracycline by virtue of imidazolium ionic liquid two-phase aqueous system
A two-phase aqueous system and ionic liquid technology, applied in the separation/purification of carboxylic acid amides, organic chemistry, etc., can solve the problems of low concentration, low extraction rate, and limited effect, so as to avoid waste of resources, increase extraction rate, reduce The effect of usage
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Embodiment 1
[0022] N-level cross-flow extraction experiment: Prepare N 7mL dry and clean centrifuge tubes, add K with a concentration of 50wt% 2 HPO 4 Put 1.6mL of solution, 3.4mL of [Bmim]Cl solution with a concentration of 50wt% and 1mL of tetracycline stock solution with a concentration of 1.2mg / mL into a centrifuge tube, shake it with a vortex shaker at 25°C to mix it evenly, and shake it for 2 minutes Put it into a centrifuge, set it to 10000r / min speed, centrifuge for 20 min, and then use a syringe to separate the upper extract phase, and the lower raffinate phase is the raw material solution, and add K with a concentration of 50wt%. 2 HPO 4 solution and [Bmim]Cl solution for two-stage extraction experiment, after the stratification is stable, separate the upper extraction phase, and then use the lower phase as the raw material solution, and add a concentration of 50wt% K 2 HPO 4 The solution and the [Bmim]Cl solution were subjected to a three-stage extraction experiment. The raf...
Embodiment 2
[0024] N-level countercurrent extraction experiment: Prepare N 7mL dry and clean centrifuge tubes, numbered as 0#, 1#, 2#...N#, and pipette K with a concentration of 50wt% in the 0# centrifuge tube 2 HPO 4 Solution 1.6mL, concentration is the tetracycline stock solution 1mL of the [Bmim]Cl solution 3.4mL of 50wt% and 1.2mg / mL, forms the upper and lower phase volume ratio ( V r =0.7) of the two-phase aqueous system for extraction, shake and centrifuge at 25°C and let it stand still. In 1#, 2#...N# centrifuge tubes, use K with a concentration of 50wt% 2 HPO 4 solution and [Bmim]Cl solution, made into a unified upper and lower phase volume ratio ( V r =0.7) of the aqueous two-phase system. After separating the upper and lower phases of 1#, 2#...N# centrifuge tubes with a syringe, add 1.2mg tetracycline to the lower phase of 1#, 2#...N# centrifuge tubes respectively, Shake to mix well and let stand. Then the upper phase extracted with tetracycline in the 0# centrifuge tube...
Embodiment 3
[0026] When performing multi-stage cross-current two-phase extraction, the volume ratio of the upper and lower phases was controlled at 0.3, 0.5, and 0.7 respectively for extraction experiments; during multi-stage counter-current two-phase extraction, the volume ratio of the upper and lower phases was controlled at 0.5 for extraction experiments After shaking and centrifuging in each stage of the extraction experiment, place them in a constant temperature box at 25°C and let them stand still. After the phase separation is clear, measure the tetracycline content in the upper and lower phases of each stage to obtain the tetracycline extraction efficiency. The result is as figure 1 shown.
[0027] from figure 1It can be seen that under the condition that the upper and lower phase volume ratios are respectively 0.3, 0.5, and 0.7, the extraction rates of tetracycline in the three-stage cross-flow extraction process reach 97.2%, 98.1% and 98.7% respectively; The extraction rate of...
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