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一种基于电生溴的用于毛细管电泳的串联双电极检测器。

A serial dual-electrode detector based on electrogenerated bromine for capillary electrophoresis.

作者信息

Du Fuying, Cao Shunan, Fung Ying-Sing

机构信息

Department of Water Quality Engineering, School of Power and Mechanical Engineering, Wuhan University, Wuhan, China; Department of Chemistry, The University of Hong Kong, Hong Kong SAR, China.

出版信息

Electrophoresis. 2014 Dec;35(24):3556-63. doi: 10.1002/elps.201400257. Epub 2014 Oct 21.

Abstract

A new serial dual-electrode detector for CE has been designed and fabricated for postcolumn reaction detection based on electrogenerated bromine. A coaxial postcolumn reactor was employed to introduce bromide reagent and facilitate the fabrication of upstream generation electrode by simply sputtering Pt film onto the outer surface of the separation capillary. Bromide introduced could be efficiently converted to bromine at this Pt film electrode and subsequently detected by the downstream Pt microdisk detection electrode. Analytes that react with bromine could be determined by the decrease of bromine reduction current at the downstream electrode resulting from the reaction between analytes and bromine. The effects of serial dual-electrode detector working conditions including electrode potentials, bromide flow rate, and bromide concentration on analytical performance were investigated using glutathione (GSH) and glutathione disulfide (GSSG) as test analytes. Under the optimal conditions, detection limits down to 0.16 μM for GSH and 0.14 μM for GSSG (S/N = 3) as well as linear working ranges of two orders of magnitude for GSH and GSSG were achieved. Furthermore, the separation efficiency obtained by our dual-electrode detector design was greatly improved compared with previous reported design. The developed method has been successfully applied to determine the GSH and GSSG impurity in commercial GSH supplement.

摘要

一种用于毛细管电泳(CE)的新型串联双电极检测器已被设计并制造出来,用于基于电生溴的柱后反应检测。采用同轴柱后反应器引入溴化物试剂,并通过简单地在分离毛细管外表面溅射铂膜来便于制造上游生成电极。引入的溴化物可在该铂膜电极上有效地转化为溴,随后由下游的铂微盘检测电极进行检测。与溴反应的分析物可通过分析物与溴之间的反应导致下游电极上溴还原电流的降低来测定。以谷胱甘肽(GSH)和谷胱甘肽二硫化物(GSSG)作为测试分析物,研究了串联双电极检测器工作条件(包括电极电位、溴化物流速和溴化物浓度)对分析性能的影响。在最佳条件下,GSH的检测限低至0.16 μM,GSSG的检测限低至0.14 μM(信噪比=3),并且GSH和GSSG的线性工作范围达到两个数量级。此外,与先前报道的设计相比,我们的双电极检测器设计所获得的分离效率有了很大提高。所开发的方法已成功应用于测定市售GSH补充剂中的GSH和GSSG杂质。

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