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TCs-Fe(Ⅲ)体系离子液体气浮浮选荧光光谱法分离/富集四环素类抗生素残留的研究

Studies on TCs-Fe(Ⅲ) System Separation/Enrichment of Trace Tetracyclines Antibiotic by Combination Ionic Liquid [Hmim]PF6 Solvent Sublation with Fluorescence Spectroscopy Determination

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摘要

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。

Abstract

It is the first time ionic liquid was applied to gas solvent sublation, which established a new method for separation/enrichment 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 ethy1 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?min-1, and the flotation time was 50 min. The complexes of TCs- Fe(Ⅲ) were pre-concentrated in the [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) interactions occurred between the ionic liquid and the complexes functional groups, and the ionic liquid was only solvent. The experimental result indicated that utilizing ionic liquid to float TCs in environmental sample is feasible.

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中图分类号:O652.6

基金项目:国家自然科学基金项目(20777029, 20676057)和吉林省教育厅基金项目(20070156)资助

收稿日期:2009-03-12

修改稿日期:2009-06-18

网络出版日期:0001-01-01

作者单位    点击查看

王良:吉林师范大学化学学院, 吉林 四平 136000江苏大学化学化工学院, 江苏 镇江 212013
闫永胜:江苏大学化学化工学院, 江苏 镇江 212013
李华明:江苏大学化学化工学院, 江苏 镇江 212013
孙汉文:河北大学化学与环境科学学院, 河北 保定 071000

联系人作者:闫永胜(yys@ujs.edu.cn)

备注:王良, 女, 1974年生, 江苏大学化学化工学院副教授

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引用该论文

WANG Liang,YAN Yong-sheng,LI Hua-ming,SUN Han-wen. Studies on TCs-Fe(Ⅲ) System Separation/Enrichment of Trace Tetracyclines Antibiotic by Combination Ionic Liquid [Hmim]PF6 Solvent Sublation with Fluorescence Spectroscopy Determination[J]. Spectroscopy and Spectral Analysis, 2010, 30(2): 391-394

王良,闫永胜,李华明,孙汉文. TCs-Fe(Ⅲ)体系离子液体气浮浮选荧光光谱法分离/富集四环素类抗生素残留的研究[J]. 光谱学与光谱分析, 2010, 30(2): 391-394

被引情况

【1】付新梅,汪磊,戴树桂. 红外光谱法和量子化学法对离子液体提取水中壬基酚的机理研究. 光谱学与光谱分析, 2011, 31(3): 625-629

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