Selenonium cations are electron deficient species in which the central selenium atom is bonded to three carbon chains (aryl or alkyl). Trimethylselenonium iodide was synthesized by reaction of methyllithium with metallic selenium to produce methylselenolithium which was, in turn, reacted with the appropriate alkylbromide. The selenide thus formed was further methylated at the selenium atom with methyl iodide in methanol in the presence of sodium tetraphenylborate. After several recrystallizations the selenonium analytes were characterized by AAS, FT-IR, $ sp1$H-NMR, $ sp{13}$C-NMR, FAB-MS and LAMMA spectroscopic techniques and used as standards for analytical methods development. / The analysis was performed by high performance liquid chromatography with atomic absorption detection. The chromatography on a cynopropyl silica bonded phase was optimized for mobile phase composition by response surface analysis. The resulting surface response plots permitted a differentiation between the mechanisms of action of two mobile phase modifiers: triethylamine and trimethylsulfonium iodide. The improvement in chromatographic efficiency resulted in two to three fold decrease in the limit of detection. An extraction procedure with liquefied phenol was evaluated for the determination, by HPLC-AAS, of traces of selenonium cations in biological samples. The advantages and shortcomings of the HPLC-THG-AAS approach are discussed.

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