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

作者：Minakata Kayoko^*; Nozawa Hideki; Yamagishi Itaru; Gonmori Kunio; Hasegawa Koutaro; Suzuki Masako; Wurita Amin; Watanabe Kanako; Suzuki Osamu

来源：Forensic Toxicology, 2012, 30(2): 156-161.

DOI：10.1007/s11419-012-0140-y

• Perchlorate
• Thiocyanate
• Iodide
• Tris(1,10-phenanthroline)iron(II)
• Tandem mass spectrometry
• Electrospray ionization

A rapid and sensitive method was developed for simultaneous determination of perchlorate (ClO4 (-)), thiocyanate (SCN-), and iodide (I-). The ions were reacted with tris(1,10-phenanthroline)iron(II) chelating cation, [Fe(phen)(3)](2+), to produce their ternary complexes, [Fe(phen)(2)ClO4](+), [Fe(phen)(2)SCN](+), and [Fe(phen)(2)I](+) that were extracted together with nitrobenzene. Five microliters of the extract was injected directly into an electrospray ionization tandem mass spectrometer. Quantification of ClO4 (-), SCN-, and I- was performed by selected reaction monitoring of the product ion [Fe(phen)O-2](+) at m/z 268 that derived from the precursor ion [Fe(phen)(2)ClO4](+) at m/z 515, the product ion [Fe(phen)SCN](+) at m/z 294 that derived from precursor ion [Fe(phen)(2)SCN](+) at m/z 474, and the product ion [Fe(phen)I](+) at m/z 363 that derived from precursor ion [Fe(phen)(2)I](+) at m/z 543, respectively. Perchlorate, SCN-, and I- were measured in the range of 0.1-10 mu M with the limits of detection at 0.03 mu M by using a 50-mu l sample aliquot containing the three ions within 10 min. The SCN- level in gastric fluid of a victim of NaCN poisoning was 137 +/- A 23 mu M, which is slightly higher than the results from control subjects (n = 7), 72 +/- A 39 mu M.

• 出版日期2012-7