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Please use this identifier to cite or link to this item: http://hdl.handle.net/10271/2910

Title: A new approach in tandem mass spectrometric simultaneous determination of perchlorate, thiocyanate and iodide using their ternary complexes with tris(1,10-phenanthroline) iron(II) chelate
Authors: Minakata, Kayoko
Nozawa, Hideki
Yamagishi, Itaru
Gonmori, Kunio
Hasegawa, Koutaro
Suzuki, Masako
Wurita, Amin
Watanabe, Kanako
Suzuki, Osamu
Keywords: Perchlorate
Tris (1,10-phenanthroline) iron (II)
Tandem mass spectrometry
Elecrospray ionization
Issue Date: Jul-2012
Publisher: Springer Japan
Abstract: A rapid and sensitive method was developed for simultaneous determination of perchlorate (ClO4–), thiocyanate (SCN–) and iodide (I–). They were reacted with tris (1,10-phenanthroline) iron (II) chelating cation, [Fe(phen)3]2+, to produce their ternary complexes, [Fe(phen)2ClO4]+, [Fe(phen)2SCN]+ and [Fe(phen)2I]+ that were extracted together with nitrobenzene. Five micro-liter of the extract was injected directly into an electrospray ionization tandem mass spectrometric instrument. Quantifications of ClO4–, SCN–, and I– were performed by selected reaction monitoring of the product ion [Fe(phen)O2]+ at m/z 268 that derived from the precursor ion [Fe(phen)2ClO4]+ at m/z 515, the product ion [Fe(phen)SCN]+ at m/z 294 that derived from precursor ion [Fe(phen)2SCN]+ at m/z 474, the product ion [Fe(phen)I]+ at m/z 363 that derived from precursor ion [Fe(phen)2I]+ at m/z 543, respectively. ClO4–, SCN–, and I– could be measured in the range of 0.1 – 10 μM with the limit of detection at 0.03 μM, respectively, using 50 μL aliquot of a sample containing three kinds of ions within 10 min. The SCN– level in gastric fluid of a victim ingested NaCN was 137±23 μM, a little increased from that of control subjects (n=7), 72±39 μM.
URI: http://hdl.handle.net/10271/2910
DOI: info:doi/10.1007/s11419-012-0140-y
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