Optimization of Headspace Solid Phase Microextraction Procedure for Trace Analysis of Toluene

This study describes optimization of headspace solid phase microextraction followed by gas chromatography equipped with a flame ionization detector for toluene at trace level in spiked urine. The parameters affecting the extraction and gas chromatographic determination of analytes were studied: extraction time and temperature; desorption time and temperature; addition of NaCl; and pH, volume and agitation of the sample. Optimized headspace extraction was carried out at 30 °C for 6 min in the presence of 0.2 g-m^-1of NaCl in the sample solution. Also, sample volume and sample pH were optimized at 5 ml and 7 (neutral pH), respectively. Desorption of the analytes was carried out at 250 °C for 60 s. The optimized procedure was validated with 3 different pools of spiked urine; it showed good reproducibility over 6 consecutive days and 6 within-day experiments. The study also determined the accuracy, linearity and detection limits of this method.