Abstract

A microwave-assisted extraction method is described for the determination of three butyltin species in National Research Council of Canada Certified Reference Material (NRCC CRM) PACS-2 Sediment using high-performance liquid chromatography (HPLC) in conjunction with inductively coupled plasma mass spectrometry (ICP-MS). Quantitative recoveries of monobutyltin (MBT), dibutyltin (DBT) and tributyltin (TBT) from PACS-2 Sediment were achieved in a closed-vessel microwave extraction system using 5 ml of acetic acid as the extraction medium. Chromatographic separation of MBT, DBT and TBT could be achieved in 7 min with a strong cation-exchange column using an ammonium citrate buffer in a 60∶40 methanol–water mixture as mobile phase. Values of 0.45 ± 0.02, 1.11 ± 0.03 and 0.96 ± 0.02 µg g⁻¹ as tin were obtained for MBT, DBT and TBT in PACS-2, respectively, in excellent agreement with their respective certified values of 0.45 ± 0.05, 1.09 ± 0.15 and 0.98 ± 0.13 µg g⁻¹. The detection limits (3σ), based on a 0.5 g sample, were 0.08, 0.05 and 0.03 µg g⁻¹ for MBT, DBT and TBT, respectively.