将离子液体应用于气浮溶剂浮选,建立了一种分离/富集四环素类(tetracyclines, TCs)抗生素的新方法——离子液体气浮溶剂浮选。最优化浮选条件为:以1-己基-3-甲基咪唑六氟磷酸盐([Hmim]PF6)和乙酸乙酯(EA)的混合溶剂(φ=1/0.9)为浮选剂,以Fe(Ⅲ)为捕集剂,pH值为7.6,气体流速为40 mL·min-1,浮选时间为50 min。富集TCs-Fe(Ⅲ)配合物的[Hmim]PF6-EA相用荧光光谱法直接测定,其线性回归方程为F=246.5c+4.32(c: μg·10 mL-1),相关系数r=0.999 1。实测了鱼塘表面水体和沉积物中四环素类抗生素的含量,加标回收率达到94.2%~100.4%,RSD<3.2%(n=5)。红外光谱分析显示TCs-Fe(Ⅲ)配合物没有和离子液体发生反应,离子液体在气浮溶剂浮选中只起到溶剂作用。该方法适合于环境水样中痕量四环素类抗生素的分离/富集及分析。
It is the first time ionic liquid was applied to gas solvent sublation, which established a new method for separation/en- richment of tetracyclines(TCs) antibiotic based on ionic liquid gas solvent sublation. The optimizing experimental conditions were as follows., the mixture of ionic liquid 1-hexyl-3-methylimidazo lium hexafluorophosphats and ethyl acetate ([Hmim]PF6- EA, φ=1/0.9) can be used as flotation solvent, Fe( Ⅲ ) ion was as trapping agent, pH of test solution was 7.6, the gas flow rate was 40 mL ~ rain ~, and the flotation time was 50 rain. The complexes of TCs- Fe ( Ⅲ ) were pre-eoneentrated in the Y-Hmim]PF6-EA layer and this was used to determine analytes by fluorescence method directly. The linear regression equation was F=246.5c+4.32 (c: μg·10 mL-1 ), and correlation coefficient was 0. 999 1. Recoveries between 94. 2% and 100. 4% were achieved from surface water and sediment samples in ponder by using this method and the relative standard deviation of 5 μg· mL-1 TCs for 5 parallel determinations was less than 3.2%. FTIR spectroscopy demonstrated that no chemical (bonding) in- teractions occurred between the ionic liquid and the complexes functional groups, and the ionic liquid was only solvent. The ex- perimental result indicated that utilizing ionic liquid to float TCs in environmental sample is feasible.