On-line solid-phase extraction coupled with liquid chromatography/electrospray ionization mass spectrometry for the determination of trace tributyltin and triphenyltin in water samples
Chen, Zuliang（ Univ S Australia, Ctr Environm Risk Assessment & Remediat, Mawson Lakes, SA 5095, Australia）
Megharaj, Mallavarapu（ Univ S Australia, Ctr Environm Risk Assessment & Remediat, Mawson Lakes, SA 5095, Australia）
Naidu, Ravendra（ Univ S Australia, Ctr Environm Risk Assessment & Remediat, Mawson Lakes, SA 5095, Australia）
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On-line solid-phase extraction (SPE) for pre-concentration and sample cleanup is one strategy to reduce matrix effects and to simultaneously improve detection sensitivity in liquid chromatography/ mass spectrometry (LC/MS). This paper describes an on-line SPE-LC/MS method for the determination of tributyltin (TBT) and triphenyltin (TPhT) at trace levels in water samples. The direct coupling of an on-line C-18 pre-column to LC/MS was used to pre-concentrate TBT and TPhT at trace levels from waters and to remove interfering matrix effects. Pre-concentration was followed by separation of TBT and TPhT on a C-18 column using a mobile phase containing 0.1% (v/v) HCOOH/ 5 mM HCOONH4 and methanol. While both electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) can be interfaced with MS for the detection of TBT and TPhT, ESI-MS was preferred for this application. The calibration curve for the targets was linear in the concentration range 0.1-30 mu g L-1. The detection limit (signal-to-noise (S/N) ratio = 3) was 0.02 mu g L-1 when 3.0 mL of sample was enriched on the C18 pre-column. The recoveries of TBT and TPhT in spiked waters were from 81.0 to 101.9%. The reproducibilities for the analysis of the standard mixture (10 mu g L-1) for TBT and TPhT were 13.1 and 5.0%, respectively. The developed method was an easy and fast way to analyze TBT and TPhT in water samples. Copyright (c) 2009 John Wiley & Sons, Ltd.
出处RAPID COMMUNICATIONS IN MASS SPECTROMETRY，2009，23（23）：3795-3802
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