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
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
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利用三(1,10-菲咯啉)铁(II)螯合物的三元络合物串联质谱同时测定高氯酸盐、硫氰酸盐和碘化物的新方法
DOI：
10.1007/s11419-012-0140-y
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发表时间：
2012
影响因子：
2.2
通讯作者：
Hideki Nozawa
中科院分区：
文献类型：
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作者：
Kayoko Minakata;Hideki Nozawa
建立了同时测定高氯酸盐(ClO_4-−)、硫氰酸盐(SCN-−)和碘(I-−)的快速、灵敏的方法。这些离子与三(1，10-邻菲咯啉)铁(II)络合阳离子[Fe(Phen)3]2+反应生成它们的三元络合物[Fe(Phen)2ClO4]+、[Fe(Phen)2SCN]+和[Fe(Phen)2I]+，并与硝基苯一起萃取。将5微升提取物直接注入电喷雾电离串联质谱仪。通过选择性反应监测前体离子[Fe(Phen)2ClO4]+atm/Z515的产物离子[Fe(Phen)2ClO4]+atm/z268、前体离子[Fe(Phen)2SCN]+atm/z474的产物离子[Fe(Phen)−]+atm/z474和前体离子[Fe(Phen)2SCN]+atm/z543的产物离子[Fe(Phen)O2]+atm/z363进行定量测定。高氯酸盐、SCN−和I−的测量范围为0.1-10μM，检出限为0.0 3μM，使用含三种离子的50μL样品等份，在10分钟内进行了测定。1例NaCN中毒患者胃液中SCN-−水平为137.23±2.23μM，略高于对照组(n=17.7)72±0.39μM。
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)2ClO4]+, [Fe(phen)2SCN]+, and [Fe(phen)2I]+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)O2]+atm/z268 that derived from the precursor ion [Fe(phen)2ClO4]+atm/z515, the product ion [Fe(phen)SCN]+atm/z294 that derived from precursor ion [Fe(phen)2SCN]+atm/z474, and the product ion [Fe(phen)I]+atm/z363 that derived from precursor ion [Fe(phen)2I]+atm/z543, respectively. Perchlorate, SCN−, and I−were measured in the range of 0.1–10 μM with the limits of detection at 0.03 μM by using a 50-μl sample aliquot containing the three ions within 10 min. The SCN−level in gastric fluid of a victim of NaCN poisoning was 137 ± 23 μM, which is slightly higher than the results from control subjects (n= 7), 72 ± 39 μM.