Analysis of 35 priority semivolatile compounds in water by stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry I.: Method optimisation

A multiresidue method for the determination of 35 organic micropollutants (pesticides and polycyclic aromatic hydrocarbons) in water has been optimised using stir bar sorptive extraction (SBSE) and thermal desorption coupled to capillary gas chromatography-mass spectrometry (GC-MS). In the present work, the different parameters affecting the extraction of the analytes from the water samples to the PDMS-coated stir bars and optimisation of conditions affecting thermal desorption are investigated. The optimised conditions consist of a 100-ml water sample with 20% NaCI addition extracted with 20 mm length x 0.5 mm film thickness stir bars at 900 rpm during 14 h at ambient temperature. Desorption is carried out at 280 degreesC during 6 min under a helium flow of 75 ml /min in the splitless mode while maintaining a cryofocusing temperature of 20 degreesC in the programmed-temperature vaporisation (PTV) injector of the GC-MS system. Finally, the PTV injector is ramped to a temperature of 280 degreesC and the analytes are separated in the GC and detected by MS using full scan mode (m/z 60-400). Under the described conditions, the good repeatability, high analyte recoveries and robustness, make SBSE a powerful tool for routine quality control analysis of the selected semivolatile compounds in water samples. (C) 2003 Elsevier Science B.V. All rights reserved.