Analysis of Polychlorinated Biphenyls, Dibenzodioxins and Dibenzofurans by On-Line Coupled Microcolumn HPLC Capillary GC-MS

Abstract

A multi-dimensional μLC-GC-MS system was developed and used to analyze a sample containing chlorinated aromatic solutes. The electron-acceptor stationary phase, 5-μm 2,4-dinitrophenylmercaptopropylsilica (DNPMP), was packed into a 0.32-mm × 400-mm microcapillary liquid chromatography (μLC) column. Aromatic fractions eluted from the μLC system at 12 μL/min and were then diverted to the gas chromatograph mass spectrometer (GC-MS) by a ten-port switching valve with 50 and 7.6-μL loops. Concurrent cosolvent evaporation occurred in a 0.32-mm × 3-m precolumn ahead of a 0.25-mm × 30-m DB-5 analytical column. Solvent vapors exited through an open-split interface. The μLC-GC-MS system was demonstrated through the analysis of a sample containing polychlorinated biphenyls, 2,7-dichlorodibenzodioxin and 3,6-dichlorodibenzofuran. The precision for the quantitative transfer of an analyte from the μLC to the GC-MS was 16.9% RSD.