Zusammenfassung
Electrochemically assisted injection (EAI) is an attractive injection concept for CE that enables the separation of neutral analytes via electrochemical generation of charged species during the injection process. A new semiautomated EAI configuration was developed and applied in conjunction with CE-MS (EAI-CE-MS). The EAI cell arrangement consists of an integrated buffer reservoir for ...
Zusammenfassung
Electrochemically assisted injection (EAI) is an attractive injection concept for CE that enables the separation of neutral analytes via electrochemical generation of charged species during the injection process. A new semiautomated EAI configuration was developed and applied in conjunction with CE-MS (EAI-CE-MS). The EAI cell arrangement consists of an integrated buffer reservoir for CEseparations and a compartment holding screen-printed electrodes. A drop of sample solution (50 mu L) was sufficient to cover the three-electrode structures. A piezo motor provided a fast and precise capillary positioning over the screen-printed electrode assembly. Using ferrocene methanol as a model system, the EAI arrangement was characterized regarding coulometric efficiency, precision, and sensitivity of electrospray ionization-time-of-flight-MS. The formation of the cationic oxidation product of ferrocene methanol enhanced the sensitivity of CE-MS determination by two orders of magnitude and the electrochemically formed product showed a migration time corresponding to its individual electrophoretic mobility. Preliminary studies of EAI-CE-MS in the field of the analysis of nitroaromatic compounds were carried out. The formation of corresponding hydroxylamines and amines paved the way for selective and sensitive CE-MS determinations without the need of adding surfactants to the electrophoresis buffer.
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