Ion-pair dynamic liquid-phase microextraction combined with injection-port derivatization for the determination of...

Ion-pair dynamic liquid-phase microextraction coupled to injection-port derivatization has been developed for the determination of long-chain fatty acids in water samples by gas chromatography-mass spectrometry (GC-MS). In this procedure, long-chain fatty acids (C(14), C(16) and C(18)) were converted into their ion-pair complexes with tetrabutylammonium hydrogen sulfate and then extracted by organic solvent (1-octanol) impregnated in the hollow fiber. The dynamic nature of the extraction was represented by the repeated movement of the acceptor phase (organic solvent) in the hollow fiber that was controlled by a syringe pump. Ion pairs of fatty acids quantitatively formed butyl esters in the injection-port of the gas chromatography. Several parameters such as injection temperature, purge-off time, organic solvent, ion-pair reagent, pH, agitation speed, extraction time and the syringe pump parameters (plunger speed and dwell time) have been optimized. The limits of detection were in the range 0.0093-0.015 ng mL(-1) (at a signal-to-noise ratio of 3) under GC-MS-selected ion monitoring mode and the relative standard deviations were between 7.7% and 11.5%. The method was successfully applied to measure long-chain fatty acids in real water samples.