Study of Electrochemical Reactions Using Nanospray Desorption Electrospray Ionization Mass Spectrometry

Journal Article · Tue Jul 03 04:00:00 EDT 2012 · Analytical Chemistry, 84(13):5737-5743

DOI:https://doi.org/10.1021/ac300916k· OSTI ID:1047382

Liu, Pengyuan; Lanekoff, Ingela T.; Laskin, Julia; Dewald, Howard D.; Chen, Hao

The combination of electrochemistry (EC) and mass spectrometry (MS) is a powerful analytical tool for studying mechanisms of redox reactions, identification of products and intermediates, and online derivatization/recognition of analytes. This work reports a new coupling interface for EC/MS by employing nanospray desorption electrospray ionization (nano-DESI), a recently developed ambient ionization method. We demonstrate online coupling of nano-DESI-MS with a traditional electrochemical flow cell, in which the electrolyzed solution emanating from the cell is ionized by nano-DESI for MS analysis. Furthermore, we show first coupling of nano-DESI-MS with an interdigitated array (IDA) electrode enabling chemical analysis of electrolyzed samples directly from electrode surfaces. Because of its inherent sensitivity, nano-DESI enables chemical analysis of small volumes and concentrations of sample solution. Specifically, good-quality signal of dopamine and its oxidized form, dopamine ortho-quinone, was obtained using 10 μL of 1 μM solution of dopamine on the IDA. Oxidation of dopamine, reduction of benzodiazepines, and electrochemical derivatization of thiol groups were used to demonstrate the performance of the technique. Our results show the potential of nano-DESI as a novel interface for electrochemical mass spectrometry research.

• Research Organization: Pacific Northwest National Laboratory (PNNL), Richland, WA (US), Environmental Molecular Sciences Laboratory (EMSL)
• Sponsoring Organization: USDOE
• DOE Contract Number: AC05-76RL01830
• OSTI ID: 1047382
• Report Number(s): PNNL-SA-86939; 34920; KP1704020; KC0302020
• Journal Information: Analytical Chemistry, 84(13):5737-5743, Journal Name: Analytical Chemistry, 84(13):5737-5743 Journal Issue: 13 Vol. 84
• Country of Publication: United States
• Language: English

Related Subjects

Ambient ionization
Environmental Molecular Sciences Laboratory
electrochemistry
mass spectrometry
nanospray desorption electrospray ionization (nano-DESI)