Development of a miniaturized injection cell for online electrochemistry–capillary electrophoresis–mass spectrometry
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The elucidation of oxidation or reduction pathways is important for the electrochemical characterization of compounds of interest. In this context, hyphenation of electrochemistry and mass spectrometry is frequently applied to identify products of electrochemical reactions. In this contribution, the development of a novel miniaturized injection cell for online electrochemistry–capillary electrophoresis–mass spectrometry (EC–CE–MS) is presented. It is based on disposable thin-film electrodes, which allow for high flexibility and fast replacement of electrode materials. Thus, high costs and time-consuming maintenance procedures can be avoided, which makes this approach interesting for routine applications. The cell was designed to be suitable for investigations in aqueous and particularly non-aqueous solutions making it a universal tool for a broad range of analytical problems. EC–CE–MS measurements of different ferrocene derivatives in non-aqueous solutions were carried out to characterize the cell. Oxidation products of ferrocene and ferrocenemethanol were electrochemically generated and could be separated from the decamethylferricenium cation. The importance of fast CE–MS analysis of instable oxidation products was demonstrated by evaluating the signal of the ferriceniummethanol cation depending on the time gap between electrochemical generation and detection.
KeywordsCapillary zone electrophoresis Electrochemistry Mass spectrometry Reaction mechanisms
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