The possibility of applying headspace microextraction into a single drop for the determination of alcohols in aqueous solutions is demonstrated. A drop of ethylene glycol containing butan-2-one as an internal standard is used for extraction. The analytes are extracted by suspending a 1 μl extracting drop directly from the tip of a microsyringe fixed above an extraction vial with a septum such that the needle passes through the septum and the needle tip appears above the surface of the solution. After the extraction is finished the drop is retracted back into the needle and injected directly into a GC column. Optimization of experimental conditions (sampling time, sampling temperature, stirring rate and ionic strength of the solution) with respect to the extraction efficiency were investigated and the linear range and the precision were examined. This headspace single drop microextraction method was applied to the analysis of beer.
A hollow fibre liquid phase microextraction for gas chromatographic determination of some p-hydroxybenzoic acid esters has been developed. Chlorobenzene containing tetradecane as internal standard was used for the extraction. Optimized extraction was carried out at room temperature for 40 min in the presence of 0.4 g mL−1 NaCl in the sample solution. Calibration was linear up to 30 mg L−1. Correlation coefficients were 0.996–0.998. Enrichment factors were 21, 95 and 154, and detection limits were 0.20, 0.03 and 0.01 μg mL−1 for methylparaben, ethylparaben and propylparaben, respectively. Reproducibility was acceptable with relative standard deviations up to 11.7%. The technique was tested for water and urine analysis.