Premium
Development and characterization of a novel semiautomated arrangement for electrochemically assisted injection in combination with capillary electrophoresis time‐of‐flight mass spectrometry
Author(s) -
Palatzky Peter,
Matysik FrankMichael
Publication year - 2012
Publication title -
electrophoresis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.666
H-Index - 158
eISSN - 1522-2683
pISSN - 0173-0835
DOI - 10.1002/elps.201200088
Subject(s) - capillary electrophoresis , chemistry , electrophoresis , mass spectrometry , ferrocene , chromatography , electrospray , analyte , analytical chemistry (journal) , capillary electrophoresis–mass spectrometry , electrospray ionization , cationic polymerization , electrochemistry , capillary action , electrode , materials science , organic chemistry , composite material
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 CE separations and a compartment holding screen‐printed electrodes. A drop of sample solution (50 μL) 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.