Journal
ANALYTICAL CHEMISTRY
Volume 75, Issue 4, Pages 1022-1030Publisher
AMER CHEMICAL SOC
DOI: 10.1021/ac026066p
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It is well-established that electrochemical reactions can occur within the capillary of an electrospray (ES) devise coupled to a mass spectrometer. In fact, such reactions must occur to maintain charge balance during the ES process. However, electrochemical reactions occurring distal to the capillary as a result of the high potential applied to the capillary have not been thoroughly investigated. In the present communication, we show that electrochemical processes can occur on a high performance liquid chromatography (HPLC) column coupled to an ES capillary. On-column solvent electrolysis is proposed to generate free radicals, which can subsequently initiate analyte oxidation. Oxidation of steroid sulfates possessing a reactive double bond between C-5 and C-6 is demonstrated. The possibility of similar reactions occurring within peptides possessing a site of unsaturation is also considered.
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