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毛细管区带电泳-安培检测法分离测定硝基苯胺异构体

Separation and determination of nitroaniline isomers by capillary zone electrophoresis with amperometric detection.

作者信息

Guo Xifeng, Lv Jin, Zhang Weidong, Wang Qingjiang, He Pingang, Fang Yuzhi

机构信息

Department of Chemistry, East China Normal University, Shanghai, PR China.

出版信息

Talanta. 2006 Mar 15;69(1):121-5. doi: 10.1016/j.talanta.2005.09.008. Epub 2005 Oct 13.

DOI:10.1016/j.talanta.2005.09.008
PMID:18970542
Abstract

In this paper, capillary zone electrophoresis with amperometric detection (CZE-AD) was firstly applied to the simultaneous separation and determination of nitroaniline positional isomers. The three analytes could be perfectly analyzed by using the buffer of extreme pH. The effects of several important factors were investigated to find optimum conditions. A carbon-disk electrode was used as working electrode. The optimal conditions were 40 mmol/L tartaric acid-sodium tartrate (pH 1.2) as running buffer, 17kV as separation voltage and 1.10V (versus saturated calomel reference electrode, SCE) as detection potential. Under the optimum conditions, o-, m- and p-nitroaniline were separated successfully and good linearity, reproducibility and recovery results were obtained. The detection limit for m-nitroaniline was as low as at 9.06 x 10(-9)mol/L. This proposed method demonstrated long-term stability and reproducibility with relative standard deviations of less than 1.8% for migration time and 1.1% for peak areas. The utility of this method was demonstrated by monitoring dyestuff wastewater and the assay results were satisfactory.

摘要

本文首次将毛细管区带电泳-安培检测法(CZE-AD)应用于硝基苯胺位置异构体的同时分离与测定。使用极端pH值的缓冲液可对三种分析物进行完美分析。研究了几个重要因素的影响以找到最佳条件。使用碳盘电极作为工作电极。最佳条件为:40 mmol/L酒石酸-酒石酸钠(pH 1.2)作为运行缓冲液,17kV作为分离电压,1.10V(相对于饱和甘汞参比电极,SCE)作为检测电位。在最佳条件下,邻、间、对硝基苯胺成功分离,并获得了良好的线性、重现性和回收率结果。间硝基苯胺的检测限低至9.06×10(-9)mol/L。该方法具有长期稳定性和重现性,迁移时间的相对标准偏差小于1.8%,峰面积的相对标准偏差小于1.1%。通过监测染料废水证明了该方法的实用性,测定结果令人满意。

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