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采用毛细管区带电泳-方波安培检测法同时测定苯二酚的位置异构体。

Simultaneous determination of positional isomers of benzenediols by capillary zone electrophoresis with square wave amperometric detection.

作者信息

Xie Tianyao, Liu Qiwen, Shi Yurong, Liu Qiuying

机构信息

School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275, China.

出版信息

J Chromatogr A. 2006 Mar 24;1109(2):317-21. doi: 10.1016/j.chroma.2006.01.135. Epub 2006 Feb 21.

Abstract

A capillary zone electrophoresis method coupling square wave amperometric detection (SWAD) for the simultaneous determination of positional isomers of benzendiols (i.e. o-, m-, p-benzenediols) has been developed. Effects of several factors, such as the composition of the running buffer, the pH value, separation voltage, injection time and the potential applied to the working electrode, were investigated to acquire the optimum conditions. The efficacy of the boric acid and ascorbic acid in the running buffer were discussed. o-, m-, p-Benzendiols can be well separated within 8 min in a 50 cm length of 50 microm diameter fused-silica capillary at a separation voltage of +15 kV. Operated in a wall-jet configuration, a 100 microm Pt-disk electrode used as the working electrode exhibits good response for the analytes. The relation between peak current and analyte concentration was linear over two orders of magnitude with detection limits (S/N = 3) ranging from 0.5 to 1.5 microM for all analytes. The proposed method has been successfully applied to monitor the o-, m-, p-benzendiols contents in the environmental wastewater samples with satisfactory assay results.

摘要

已开发出一种结合方波安培检测(SWAD)的毛细管区带电泳方法,用于同时测定苯二酚的位置异构体(即邻苯二酚、间苯二酚、对苯二酚)。研究了运行缓冲液组成、pH值、分离电压、进样时间和施加于工作电极的电位等几个因素的影响,以获得最佳条件。讨论了运行缓冲液中硼酸和抗坏血酸的作用。在50 cm长、50 μm内径的熔融石英毛细管中,在+15 kV的分离电压下,邻苯二酚、间苯二酚、对苯二酚可在8分钟内得到良好分离。采用壁喷配置,以100 μm铂盘电极作为工作电极,对分析物表现出良好的响应。峰电流与分析物浓度之间的关系在两个数量级内呈线性,所有分析物的检测限(S/N = 3)为0.5至1.5 μM。该方法已成功应用于监测环境废水样品中邻苯二酚、间苯二酚、对苯二酚的含量,测定结果令人满意。

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