Department of Analytical Chemistry, Faculty of Natural Science, Comenius University in Bratislava, Bratislava 4, Slovak Republic.
J Chromatogr A. 2012 Dec 7;1267:252-8. doi: 10.1016/j.chroma.2012.07.075. Epub 2012 Aug 1.
A new, sensitive, and robust analytical method based on capillary zone electrophoresis with on-line capillary isotachophoresis sample pretreatment (ITP-CZE) using a column-coupling (CC) arrangement of automated capillary electrophoretic analyzer was developed for determination of bromate in different type of drinking water samples. Both columns were provided with contact-less conductivity detectors and in CZE step UV detection at 200 nm wavelength was used. Electroosmotic flow of the buffer solutions was suppressed with the addition of 0.1% or 0.05% (m/v) methylhydroxyethylcellulose into the leading and terminating electrolyte, respectively. Hydrodynamic and electroosmotic flows of the buffer solutions were successfully suppressed and therefore, only the electrophoretic transport of ions was significant. Limit of detection for bromate approaching 0.6 μg/L was achieved. Good repeatabilities of migration time (RSD less than 0.3%) and peak area (RSD less than 4.0%) at concentration level 1 μg/L were obtained. Robustness of proposed ITP-CZE method and validation parameters were evaluated. Developed automated ITP-CZE method was applied to the determination of bromate in drinking water samples with different content of inorganic macroconstituents without the need of further sample preparation.
建立了一种新的、灵敏且稳健的分析方法,基于毛细管区带电泳,采用柱耦合(CC)排列的自动化毛细管电泳分析仪,在线进行毛细管等速电泳样品预处理(ITP-CZE),用于测定不同类型饮用水中的溴酸盐。两个柱子都配备了非接触式电导检测器,在 CZE 步骤中使用 200nm 波长的紫外检测。通过在先导电解质和终止电解质中分别添加 0.1%或 0.05%(m/v)甲基羟乙基纤维素,可以抑制缓冲溶液的电渗流。成功地抑制了缓冲溶液的动力学和电渗流,因此,只有离子的电泳传输是显著的。溴酸盐的检测限接近 0.6μg/L。在 1μg/L 的浓度水平下,迁移时间(RSD 小于 0.3%)和峰面积(RSD 小于 4.0%)的重现性良好。评估了所提出的 ITP-CZE 方法的稳健性和验证参数。开发的自动化 ITP-CZE 方法可用于测定不同无机常量成分含量的饮用水中的溴酸盐,无需进一步的样品制备。