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基于十六烷基三甲基溴化铵包覆的纳米磁体Fe3O4的混合半胶束固相萃取用于环境水样中氯酚的测定及液相色谱/分光光度检测联用

Mixed hemimicelles solid-phase extraction based on cetyltrimethylammonium bromide-coated nano-magnets Fe3O4 for the determination of chlorophenols in environmental water samples coupled with liquid chromatography/spectrophotometry detection.

作者信息

Li Jidong, Zhao Xiaoli, Shi Yali, Cai Yaqi, Mou Shifen, Jiang Guibin

机构信息

State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China.

出版信息

J Chromatogr A. 2008 Feb 8;1180(1-2):24-31. doi: 10.1016/j.chroma.2007.12.028. Epub 2007 Dec 23.

Abstract

Mixed hemimicelles solid-phase extraction (SPE) based on cetyltrimethylammonium bromide (CTAB)-coated nano-magnets Fe3O4 was investigated for the preconcentration of four chlorophenols (CPs) in environmental water samples prior to HPLC-spectrophotometry determination in this paper. By the rapid isolating (about 5 min) of Fe3O4 nanoparticles (NPs) through placing a Nd-Fe-B strong magnet on the bottom of beaker, the time-consuming preconcentration process of loading large volume sample in conversional SPE method with a column can be avoided. The unique properties of Fe3O4 NPs such as high surface area and strong magnetism were utilized adequately in the SPE process. This novel separation method produced a high preconcentration rate and factor. A comprehensive study of the adsorption conditions such as the Fe3O4 NPs zeta-potential, CTAB added amounts, pH value, standing time and maximal extraction volume was also presented. Under optimized conditions, four analytes of 2-chlorophenol (2-CP), 2,4-dichlorophenol (2,4-DCP), 2,4,6-trichlorophenol (TCP) and pentachlorophenol (PCP) were quantitatively extracted. The method was then used to determine four CPs in five real environmental water samples. High concentration factors (700) were achieved for each of the analytes, with observed detection limits ranging between 0.11 and 0.15 microg L(-1). The accuracy of method was evaluated by recovery measurements on spiked samples. Good recovery results (83-98%) with satisfactory relative standard deviation (RSD) were achieved. It is important to note that satisfactory preconcentration factors and extraction recoveries for the four CPs were obtained with only a little amount of Fe3O4 NPs (0.1g) and CTAB (60 mg). To the best of our knowledge, this was the first time a mixed hemimicelles SPE method based on Fe3O4 NPs magnetic separation had been used for the pretreatment of environmental water samples.

摘要

本文研究了基于十六烷基三甲基溴化铵(CTAB)包覆的纳米磁体Fe3O4的混合半胶束固相萃取(SPE)方法,用于在高效液相色谱 - 分光光度法测定之前对环境水样中的四种氯酚(CPs)进行预富集。通过将钕铁硼强磁体放置在烧杯底部快速分离(约5分钟)Fe3O4纳米颗粒(NPs),可以避免传统柱式SPE方法中加载大量样品所耗时的预富集过程。在SPE过程中充分利用了Fe3O4 NPs的独特性质如高比表面积和强磁性。这种新型分离方法具有高预富集率和富集因子。还对吸附条件如Fe3O4 NPs的ζ电位、CTAB添加量、pH值、静置时间和最大萃取体积进行了全面研究。在优化条件下,对2 - 氯酚(2 - CP)、2,4 - 二氯酚(2,4 - DCP)、2,4,6 - 三氯酚(TCP)和五氯酚(PCP)这四种分析物进行了定量萃取。然后该方法用于测定五个实际环境水样中的四种CPs。每种分析物都实现了高富集因子(700),观察到的检测限在0.11至0.15 μg L(-1)之间。通过对加标样品进行回收率测量来评估方法的准确性。获得了良好的回收率结果(83 - 98%)以及令人满意的相对标准偏差(RSD)。需要注意的是,仅使用少量Fe3O4 NPs(0.1 g)和CTAB(60 mg)就获得了四种CPs令人满意的预富集因子和萃取回收率。据我们所知,这是首次将基于Fe3O4 NPs磁分离的混合半胶束SPE方法用于环境水样预处理。

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