Determination of steroids, caffeine and methylparaben in water using solid phase microextraction-comprehensive two dimensional gas chromatography–time of flight mass spectrometry

•Automated low-level extraction, separation and detection of drugs in water using SPME-GCxGC–ToFMS.•Analysis of steroids by GC–MS without derivatization or internal standard.•Optimization of SPME conditions using experimental design.•Use of GCxGC and ToFMS to separate and quantitate several very closely eluting analytes.

Analysis of several emerging contaminants (steroids, caffeine and methylparaben) in water using automated solid-phase microextraction with comprehensive two dimensional gas chromatography coupled to time of flight mass spectrometry (SPME-GCxGC–ToF/MS) is presented. Experimental design was used to determine the best SPME extraction conditions and the steroids were not derivatized prior to injection. SPME-GCxGC–ToF/MS provided linear ranges from 0.6 to 1200 μg L−1 and limits of detection and quantitation from 0.02 to 100 μg L−1. A series of river water samples obtained locally were subjected to analysis. SPME-GCxGC–ToF/MS is readily automated, straightforward and competitive with other methods for low level analysis of emerging contaminants