Bis-pyridinium aldoximes reactivate inhibited cholinesterases poisoned by organophosphorous insecticides; 4-carbamoy 1–2′-hydroximinomethyl-bis (1-pyridinomethyl) ether dichloride is presently being investigated as an antidote for this type of phosphate ester poisoning. Current chromatographic detection methods for this compound and its metabolites, at levels present in biological samples, lack both sensitivity and selectivity. The electrochemical properties of these compounds were studied in both aqueous and non-aqueous media in order to establish a suitable electrochemical detection strategy for use after separation by high pressure liquid chromatography.