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An approach to the identification of unknown signals in selenium speciation analysis of yeast by reversed-phase chromatography with ICP-MS detection is described. The analytical strategy was based on: (i), heart-cutting of a Secontaining fraction in the reversed-phase chromatographic eluate followed by its lyophilization; (ii), pneumaticallyassisted electrospray (ESI) MS and ESI tandem MS of the lyophilizate; and (iii) confirmation of the fragmentation pattern obtained using the sulfur analogue of the seleno compound that was expected to have been identified. The approach developed allowed the identification of Seadenosylhomocysteine as the major selenium species in an extract of a selenized yeast sample.

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