Department of Chemistry, Faculty of Sciences, Azarbaijan University of Tarbiat Moallem, Tabriz, Iran.
Talanta. 2010 May 15;81(3):778-85. doi: 10.1016/j.talanta.2010.01.012. Epub 2010 Jan 18.
In this research, we combined ionic liquid-based dispersive liquid-liquid micro-extraction (IL-based DLLME) with stopped-flow spectrofluorometry (SFS) to evaluate the concentration of aluminum in different real samples at trace level. 1-Hexylpyridinium hexafluorophosphate [Hpy][PF(6)] ionic liquid and 8-hydroxyquinoline (oxine), which forms a highly fluorescent complex with Al(3+), were chosen as the extraction solvent and chelating agent, respectively. The hydrophobic Al-oxine complex was extracted into the [Hpy][PF(6)] and separated from the aqueous phase. Then, the concentration of the enriched aluminum in the sediment phase was determined by SFS. Some effective parameters that influence the SFS signals and the micro-extraction efficiency, such as the suction and sending time, the concentration of the chelating agent, pH, the amount of the ionic liquid, the type of disperser solvent and diluting agent, ionic strength, extraction time, equilibration temperature and centrifugation time were investigated and optimized. In the optimum experimental conditions, the limit of detection (3s) and enrichment factor were 0.05microgL(-1) and 100, respectively. The relative standard deviation (RSD) for six replicate determinations of 6microgL(-1) Al was 1.7%. The calibration graph using the pre-concentration system was linear in the range of 0.06-15microgL(-1) with a correlation coefficient of 0.9989. The developed method was validated by the analysis of certified reference materials and applied successfully to the determination of aluminum in several water, fruit juice and food samples.
在这项研究中,我们将基于离子液体的分散液液微萃取(IL-based DLLME)与停流荧光光谱法(SFS)相结合,以痕量水平评估不同实际样品中的铝浓度。选择 1-己基吡啶六氟磷酸盐 [Hpy][PF(6)]离子液体和 8-羟基喹啉(oxine)分别作为萃取溶剂和螯合剂,形成与 Al(3+)高度荧光的配合物。疏水性 Al-oxine 配合物被萃取到 [Hpy][PF(6)]中并与水相分离。然后,通过 SFS 测定沉淀相中富集的铝浓度。研究并优化了一些影响 SFS 信号和微萃取效率的有效参数,例如抽吸和发送时间、螯合剂浓度、pH 值、离子液体用量、分散剂溶剂和稀释剂类型、离子强度、萃取时间、平衡温度和离心时间。在最佳实验条件下,检测限(3s)和富集因子分别为 0.05μg L(-1)和 100。6μg L(-1)Al 的 6 次重复测定的相对标准偏差(RSD)为 1.7%。使用预浓缩系统的校准曲线在 0.06-15μg L(-1)范围内呈线性,相关系数为 0.9989。该方法通过对标准参考物质的分析进行了验证,并成功应用于几种水、果汁和食品样品中铝的测定。