Abstract.
An HPLC/MS-MS method was developed for the analysis of selenium species. Tandem mass spectrometry (MS-MS) was chosen as a detector to provide structural and molecular information allowing the identification of species, which are not commercially available as standards. A new separation method for selenium species was developed, based on porous graphitic carbon (PGC) as the stationary phase. The applicability of the optimized HPLC/MS-MS system was demonstrated by the analysis of a mixture containing Se-methyl-selenocysteine, selenomethionine, selenocystine, selenoethionine and selenocystamine. All peaks were baseline-resolved and eluted within 16 min. Positive ionization led to higher intensities than negative ionization. Signal suppression tests showed that electrospray ionization (ESI) is a more effective ionization method than atmospheric pressure chemical ionization (APCI) for selenium species in a matrix containing pentafluoropropionic acid, heptafluorobutyric acid or ammonium formate. Comparative experiments with a triple quadrupole mass spectrometer (Quattro LC) and a time-of-flight instrument (Q-Tof-2) showed a 20 fold higher mass resolution of the latter mass spectrometer (m/Δm=5000) and significantly lower intensities for analyte signals as well as background noise compared to the triple quadrupole instrument. MS-MS spectra of the investigated selenium species including characteristic fragmentation patterns are presented.
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Lindemann, T., Hintelmann, H. Selenium speciation by HPLC with tandem mass spectrometric detection. Anal Bioanal Chem 372, 486–490 (2002). https://doi.org/10.1007/s00216-001-1113-x
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DOI: https://doi.org/10.1007/s00216-001-1113-x