Multicapillary gas chromatography coupled to inductively coupled plasma-time-of-flight mass spectrometry for rapid mercury speciation analysis |
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Authors: | Petru Jitaru |
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Institution: | Micro and Trace Analysis Centre, University of Antwerp, Universiteitsplein 1, B-2610 Wilrijk, Belgium |
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Abstract: | A simple, rapid and accurate method on the basis of multicapillary gas chromatography (MCGC) combined with inductively coupled plasma-time-of-flight mass spectrometry (ICP-TOFMS) was developed for speciation analysis of methylmercury (MeHg+) and inorganic mercury (Hg2+). The potential of the ICP-TOFMS for transient multi-isotope detection of very short signals (peak width of 0.4 s at half peak height) was evaluated. Two injection systems (purge-and-trap (PTI) and split (SI) injections) were compared in terms of species separation resolution and transient signal profile. Using purge-and-trap injection, after in situ derivatization of the ionic mercury species with sodium tetraethylborate, a baseline separation of MeHg+ and Hg2+ was achieved within a chromatographic run of <35 s. To correct for matrix-induced ion signal variation and instrumental drift, propylmercury (PrHg+) was used as internal standard. Detection limits of 16 and 257 fg g−1 for MeHg+ (as Hg) and Hg2+, respectively, were achieved. The analytical precision (R.S.D. (%)) for 10 successive injections of a standard mixture containing 10 pg MeHg+ (as Hg) and Hg2+ was 1.2% for MeHg+ and 4.1% for Hg2+. The method was validated by analysis of two biological certified reference materials (CRM): a dogfish muscle (DORM-2) and a freeze-dried tuna fish (CRM 464). |
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Keywords: | Purge-and-trap injection Multicapillary gas chromatography Inductively coupled plasma-time-of-flight-mass spectrometry Mercury speciation analysis Biological certified reference material |
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