Stir bar sorptive extraction-thermal desorption-capillary GC–MS for profiling and target component analysis of pharmaceutical drugs in urine

Abstract

Stir bar sorptive extraction (SBSE) in combination with thermal desorption (TD) on-line coupled to capillary gas chromatography–mass spectrometry (CGC–MS) was applied to the analysis of pharmaceutical drug compounds and metabolites in urine. SBSE implies stirring of the aqueous sample (urine, blood, etc.) with a glass stir bar coated with a thick layer (24 μl) of polydimethylsiloxane (PDMS) for sorptive enrichment of the analytes of interest. In combination with quantitative TD, on-line coupled with CGC–MS, the technique showed to be very versatile and sensitive for the analysis of a wide range of drug substances. Moreover, the relative high enrichment efficiencies of SBSE allow to use mass spectrometric detection (MSD) in the full scan mode. In situ derivatization of polar compounds before SBSE is demonstrated for the analysis of paracetamol and this resulted in both improved chromatographic behavior and higher sensitivity. The quantitative performance of SBSE–TD–CGC–MS is illustrated with the analysis of some barbiturates in urine.