Key Laboratory of Eco-environments in Three Gorges Reservoir Region (Ministry of Education), School of Chemistry and Chemical Engineering, Southwest University, Chongqing, China.
Anal Chim Acta. 2012 Feb 17;715:113-9. doi: 10.1016/j.aca.2011.12.004. Epub 2011 Dec 13.
In this paper, 1-hexadecyl-3-methylimidazolium bromide (C(16)mimBr)-coated Fe(3)O(4) magnetic nanoparticles (NPs) as an adsorbent of mixed hemimicelles solid-phase extraction was investigated for the preconcentration of two chlorophenols (CPs) in environmental water samples prior to HPLC with UV detection at 285 nm. The high surface area and excellent adsorption capacity of the Fe(3)O(4) NPs after modification with C(16)mimBr were utilized adequately in the SPE process. By the rapid isolation of Fe(3)O(4) NPs through placing a strong magnet on the bottom of beaker, the time-consuming preconcentration process of loading large volume sample in conventional SPE method with a column can be avoided. A comprehensive study of the adsorption conditions such as the zeta-potential of Fe(3)O(4) NPs, added amounts of C(16)mimBr, pH value, standing time and maximal extraction volume were also presented. Under optimized conditions, two analytes of 2,4-dichlorophenol (2,4-DCP) and 2,4,6-trichlorophenol (2,4,6-TCP) were quantitatively determined. The method was then used to determine the two CPs in real environmental water samples. The accuracy of method was evaluated by recovery measurements on spiked samples. Good recovery results (74-90%) were achieved. It is important to note that satisfactory preconcentration factors and extraction recoveries for the two CPs were obtained with only a small amount of Fe(3)O(4) NPs (40 mg) and C(16)mimBr (24 mg).
本文研究了以 1-十六烷基-3-甲基咪唑溴盐(C(16)mimBr)包覆的 Fe(3)O(4)磁性纳米粒子(NPs)为吸附剂的混合单分子层固-液萃取,用于环境水样中两种氯酚(CPs)的预浓缩,然后采用 HPLC-UV 法在 285nm 处进行检测。经过 C(16)mimBr 修饰后,Fe(3)O(4)NPs 的高表面积和优异的吸附能力在 SPE 过程中得到了充分利用。通过将磁铁置于烧杯底部,快速分离 Fe(3)O(4) NPs,避免了传统 SPE 方法中用柱子加载大体积样品所需的耗时浓缩过程。本文还对 Fe(3)O(4) NPs 的 ζ-电位、C(16)mimBr 的添加量、pH 值、静置时间和最大萃取体积等吸附条件进行了全面研究。在优化条件下,可对 2,4-二氯苯酚(2,4-DCP)和 2,4,6-三氯苯酚(2,4,6-TCP)两种分析物进行定量测定。然后,该方法用于测定实际环境水样中的两种 CP。通过对加标样品的回收率测量评估了方法的准确性。结果表明,回收率良好(74-90%)。值得注意的是,仅使用少量 Fe(3)O(4) NPs(40mg)和 C(16)mimBr(24mg)即可获得两种 CP 的令人满意的浓缩因子和萃取回收率。