Method for separating trace amount tetracycline antibiotics in enrichment environment
A technology for separation and enrichment, tetracyclines, applied in the direction of material separation, measuring devices, analysis materials, etc., to achieve significant separation effect, less reagent consumption and good separation effect
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Embodiment 1
[0023] Accurately pipette samples (2mL each of TC, OTC, and CTC working solutions), and add 5mL1.0×10 to a 100mL beaker -4 mol / L La(NO 3 ) 3 Solution, add pH7.6 Clark-Lubs buffer solution, stir, after standing still for 10 minutes, add about 70mL of 30% NaCl solution, stir evenly, transfer to 100mL flotation cell, continue to add 30% NaCl solution to 100mL, Mix well, add 5mL [Bmim]PF 6 and EA mixed solution (1:1 volume ratio) on the liquid surface, pass N 2 , after 50min, stop ventilation, stand still for a while, after there are no microbubbles in the flotation cell, take out [Bmim]PF with a dropper 6 The mixed layer with EA was placed in a 1cm cuvette, and the absorbance was measured at the maximum wavelength (with the reagent blank as a reference).
[0024] The rare earth element La(III) and TC, OTC, and CTC all form complexes with a composition ratio of 1:2 in weakly alkaline media, with similar spectral characteristics, and the maximum absorption wavelengths are 390, ...
Embodiment 2
[0026] Selection of flotation solvent:
[0027] Air flotation solvent flotation is to add a layer of organic solvent on the surface of the test solution of the substance to be separated. Low density and other characteristics, while the density of ionic liquids is mostly 1.1-1.6g.cm -3 Among them, the viscosity is usually 1-3 orders of magnitude higher than that of traditional organic solvents. The high density and high viscosity of ionic liquids prevent them from being directly used in air flotation solvent flotation. The study found that the addition of organic solvents will reduce the density and viscosity of ionic liquids to varying degrees. The present invention has investigated adding different proportions of organic solvents (this organic solvent itself can not float TCs-La (III) complexes) in the ionic liquid, such as: ethyl acetate (Ethylacetat), acetone (Acetone), acetonitrile ( Acetonitrile), methanol (Methanol), butyl acetate (Butylacetat), Benzene, toluene (Tolue...
Embodiment 3
[0042] Embodiment 3: Comparison with solvent extraction
[0043] At the same time of ionic liquid flotation, we also applied the mixture of ionic liquid and ethyl acetate in the same proportion to extract TCs-La(III) complex, and compared them. The results are shown in Table 1. It can be seen that the ionic liquid solvent flotation The separation and enrichment effect of the extraction method on tetracycline antibiotics was obviously better than that of the solvent extraction method. Its principle is basically the same as that of organic solvent flotation, because solvent flotation does not involve the distribution balance of solvent extraction, as long as the upper phase ionic liquid-ethyl acetate phase is unsaturated, the TCs-La(III) complex floating with the bubbles will can be transferred to the upper phase. Therefore, for the separation and enrichment of TCs-La(III) complex, compared with the solvent extraction method, the ionic liquid solvent flotation method is an effi...
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Abstract
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