Kannamkumarath Sasi S, Wuilloud Rodolfo G, Jayasinghe Sarath, Caruso Joseph A
Department of Chemistry, University of Cincinnati, Cincinnati, OH 45221-0172, USA.
Electrophoresis. 2004 Jun;25(12):1843-51. doi: 10.1002/elps.200305855.
An analytical methodology for the fast separation and determination of iodophenol species in natural water samples was developed using capillary electrophoresis (CE) coupled to inductively coupled plasma-mass spectrometry (ICP-MS). Based on the element-specific and highly sensitive detection provided by ICP-MS, the methodology has been applied to the analysis of 2-iodophenol, 4-iodophenol, and 2,4,6-triiodophenol. The use of solid-phase microextraction (SPME), after proper optimization, improved the signal by a factor of 100 leading to detection limits in the sub microg.L(-1). Different desorption conditions of iodophenol compounds from the SPME microfiber were studied to achieve the optimum preconcentration factor and best analytical performance. Different CE conditions were studied to achieve complete baseline separation of iodophenols in short migration times. Three different CE buffer systems were evaluated using ICP-MS detection. A buffer solution containing 20 mmol.L(-1) 3-(cyclohexylamino)-1-propanesulfonic acid (CAPS) and an applied potential of +22 kV were finally selected leading to a maximum separation time of 6.6 min. A relative standard deviation (%RSD) of about 5.0% for ten consecutive determinations was obtained. Finally, the speciation methodology developed was utilized for the determination of iodophenol compounds in natural water samples.
开发了一种采用毛细管电泳（CE）与电感耦合等离子体质谱（ICP-MS）联用的分析方法，用于快速分离和测定天然水样中的碘酚类物质。基于ICP-MS提供的元素特异性和高灵敏度检测，该方法已应用于2-碘酚、4-碘酚和2,4,6-三碘酚的分析。经过适当优化后，使用固相微萃取（SPME）使信号提高了100倍，检测限达到亚微克·升⁻¹。研究了碘酚化合物从SPME微纤维上的不同解吸条件，以实现最佳的预浓缩因子和最佳分析性能。研究了不同的CE条件，以在短迁移时间内实现碘酚的完全基线分离。使用ICP-MS检测评估了三种不同的CE缓冲系统。最终选择了含有20毫摩尔·升⁻¹ 3-（环己基氨基）-1-丙烷磺酸（CAPS）的缓冲溶液和+22 kV的施加电位，最大分离时间为6.6分钟。连续十次测定的相对标准偏差（%RSD）约为5.0%。最后，所开发的形态分析方法用于测定天然水样中的碘酚化合物。
