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基于离子液体的单滴微萃取结合高效液相色谱 - 光电二极管阵列检测法对汞的形态分析

Speciation of mercury by ionic liquid-based single-drop microextraction combined with high-performance liquid chromatography-photodiode array detection.

作者信息

Pena-Pereira Francisco, Lavilla Isela, Bendicho Carlos, Vidal Lorena, Canals Antonio

机构信息

Departamento de Química Analítica y Alimentaria, Area de Química Analítica, Facultad de Química, Universidad de Vigo, Campus As Lagoas-Marcosende s/n, 36310 Vigo, Spain.

出版信息

Talanta. 2009 Apr 30;78(2):537-41. doi: 10.1016/j.talanta.2008.12.003. Epub 2008 Dec 6.

Abstract

Room temperature ionic liquids can be considered as environmentally benign solvents with unique physicochemical properties. Ionic liquids can be used as extractant phases in SDME, being compatible with chromatographic systems. A single-drop microextraction method was developed for separation and preconcentration of mercury species (MeHg(+), EtHg(+), PhHg(+) and Hg(2+)), which relies on the formation of the corresponding dithizonates and microextraction of these neutral chelates onto a microdrop of an ionic liquid. Afterwards, the separation and determination were carried out by high-performance liquid chromatography with a photodiode array detector. Variables affecting the formation and extraction of mercury dithizonates were optimized. The optimum conditions found were: microextraction time, 20 min; stirring rate, 900 rpm; pH, 11; ionic liquid type, 1-hexyl-3-methylimidazolium hexafluorophosphate ([C(6)MIM][PF(6)]); drop volume, 4 microL; and no sodium chloride addition. Limits of detection were between 1.0 and 22.8 microg L(-1) for the four species of mercury, while the repeatability of the method, expressed as relative standard deviation, was between 3.7 and 11.6% (n=8). The method was finally applied to the determination of mercury species in different water samples.

摘要

室温离子液体可被视为具有独特物理化学性质的环境友好型溶剂。离子液体可作为单滴微萃取中的萃取相,与色谱系统兼容。开发了一种单滴微萃取方法用于汞形态(甲基汞离子、乙基汞离子、苯基汞离子和汞离子)的分离和预富集,该方法依赖于相应双硫腙盐的形成以及这些中性螯合物在离子液体微滴上的微萃取。之后,通过配备光电二极管阵列检测器的高效液相色谱进行分离和测定。对影响汞双硫腙盐形成和萃取的变量进行了优化。发现的最佳条件为:微萃取时间20分钟;搅拌速率900转/分钟;pH值11;离子液体类型为1-己基-3-甲基咪唑六氟磷酸盐([C(6)MIM][PF(6)]);液滴体积4微升;且不添加氯化钠。四种汞形态的检测限在1.0至22.8微克/升之间,而该方法的重复性以相对标准偏差表示,在3.7%至11.6%之间(n = 8)。该方法最终应用于不同水样中汞形态的测定。

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