A rapid and simple derivatization procedure has been developed for gas chromatographic determination of perfluorinated organic acids (PFCAs, C(6)-C(12)), using isobutyl chloroformate (IBCF) to convert the acids into the more volatile isobutyl esters, under catalysis by pyridine. The procedure was optimized in an acetonitrile medium and applied to GC techniques with electron-capture detection (GC-ECD) and mass spectrometry with electron-impact ionization (GC-EI-MS); for the sake of comparison, HPLC with electrospray-ionization MS (HPLC-ESI(-)-MS) was also tested. The LOD and LOQ values obtained for these three techniques were compared, and the lowest LODs were obtained with GC-ECD (0.06-1.80 microg mL(-1)). The procedure was further optimized in an aqueous medium, obtaining the best results in a phosphate buffer (pH 2.5, 50 mmol L(-1)), in which the LOD and LOQ values were measured for GC-ECD a GC-EI-MS. The lowest LODs were found for GC-EI-MS (0.030-0.314 microg mL(-1)). The practical applicability was tested on Vltava river water samples.
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