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In situ derivatization reaction and determination of ibuprofen in water samples using headspace generation-programmed temperature vaporization-gas chromatography-mass spectrometry

Pérez Pavón, José Luis, Casas Ferreira, Ana María, Fernández Laespada, María Esther, Moreno Cordero, Bernardo
Journal of chromatography 2009 v.1216 no.39 pp. 6728-6734
derivatization, detection limit, gas-chromatography-mass spectrometry, headspace analysis, ibuprofen, mixing, solvents, temperature, wastewater
The aim of the present work is to propose a method for the determination of ibuprofen, as a typical representative of pharmaceutical compounds, in aqueous samples. To do so, an in situ derivatization reaction in aqueous medium was employed in the vial of a headspace sampler (HS), after which instrumental measurements were made with gas chromatography-mass spectrometry (GC-MS). As the injection system we propose a programmed temperature vaporizer (PTV) where, in solvent vent mode, better results can be obtained than with the conventional split and splitless injection modes. Since the derivatization reaction takes place in the HS vial, after the mixing of reagents and the sealing of the vial, the whole process takes place on-line, with no need for intermediate steps. The simplicity and speed of the method - analysis throughput: 10.5min - together with the limit of detection obtained (0.23μg/L), bearing in mind that no preconcentration step or later clean-up step are required, make this a good method for the analysis of ibuprofen in aqueous samples of urban waste water.