Fast sample preparation involving MASE and coupled column normal phase liquid chromatography for the rapid trace analysis of dioxins in air-dust samples from fire catastrophe emissions

• Published in: Talanta (Oxford) 2004-08, Vol.63 (5), p.1183-1191
• Main Authors: van Beuzekom, A.C, Hijman, W.C, Berkhoff, C.J, Stoffelsen, B.H.G, den Boer, A.C, Groenemeijer, G.S, Mooibroek, D, Hoogerbrugge, R, Broekman, M.H, Baumann, R.A, Hogendoorn, E.A
• Format: Article
• Language: English
• Subjects: Air-dust; Column switching; Dioxins; MASE
• ISSN: 0039-9140; 1873-3573
• DOI: 10.1016/j.talanta.2004.05.026

A new approach has been developed and tested for the urgent analysis of dioxins in samples of air-dust filters originating from catastrophe emissions. The procedure consists of a fast extraction of the sample with microwave solvent extraction (MASE) and acetone as solvent followed by a fast cleanup of the extract with normal phase coupled column liquid chromatography (LC/LC). The multi-dimensional LC/LC system employs a 50 mm×4.6 mm i.d. column packed with 3 μm silica and a 150 mm×4.6 mm i.d. column packed with 5 μm PYE as the first and second analytical column, respectively. Iso-hexane is used on both columns to perform cleanup and dichloromethane to perform efficient back-flush elution of the compounds from the second column. The obtained polarity-based separation in the first dimension and molecular-structure based separation in the second dimension provides a fast and powerful cleanup. Validation was done by analysing samples of homemade RIVM air-dust with aged residues ( n=8, spiking level about 15 pg mg −1 per compound) of dioxins/furans and samples of reference Urban Dust SRM 1649a ( n=4) with both the new approach and the existing conventional procedure and were instrumentally analyzed with capillary gas chromatography and high resolution mass spectrometric detection (GC/HRMS). In comparison to the existing conventional procedure, the new approach reduces sample processing from several days to several hours per sample. As regards the aged-residue air-dust samples, the new method shows a good accuracy, precision and high selectivity providing a performance in good agreement with the existing procedure. In SRM air-dust, the concentration of a few compounds obtained by the new method was below (10–50%) the certified value.