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In this study, a series of ionic liquids (ILs) are evaluated as stationary phases in comprehensive two-dimensional gas chromatography (GC × GC) for the separation of aliphatic hydrocarbons from kerosene. IL-based stationary phases were carefully designed to evaluate the role of cavity formation/dispersive interaction on the chromatographic retention of nonpolar analytes by GC × GC. The maximum allowable operating temperature (MAOT) of the IL-based columns was compared to that of commercial IL-based columns. Evaluation of the solvation characteristics of GC columns guided the selection of the best performing IL-based stationary phases for the resolution of aliphatic hydrocarbons, namely, trihexyl(tetradecyl)phosphonium tetrachloroferrate ([P66614][FeCl4]) and trihexyl(tetradecyl)phosphonium tris(pentafluoroethyl)trifluorophosphate ([P66614][FAP]) ILs. The best performing [P66614][FeCl4] IL-based column exhibited a MAOT of 320 °C, higher than the commercial SUPELCOWAX 10 (MAOT of 280 °C) and commercial IL-based columns (MAOT up to 300 °C). The structurally tuned [P66614][FeCl4] IL stationary phase exhibited improved separation of aliphatic hydrocarbons by GC × GC compared to the commercial columns examined (e.g., OV-1701, SUPELCOWAX 10, SLB-IL60, SLB-IL100, and SLB-IL111).

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Several crosslinked polymeric ionic liquid (PIL)-based sorbent coatings of different nature were prepared by UV polymerization onto nitinol wires. They were evaluated in a direct-immersion solid-phase microextraction (DI-SPME) method in combination with high-performance liquid chromatography (HPLC) and diode array detection (DAD). The studied PIL coatings contained either vinyl alkyl or vinylbenzyl imidazolium-based (ViCnIm- or ViBCnIm-) IL monomers with different anions, as well as different dicationic IL crosslinkers. The analytical performance of these PIL-based SPME coatings was firstly evaluated for the extraction of a group of 10 different model analytes, including hydrocarbons and phenols, while exhaustively comparing the performance with commercial SPME fibers such as polydimethylsyloxane (PDMS), polyacrylate (PA) and polydimethylsiloxane/divinylbenzene (PDMS/DVB), and using all fibers under optimized conditions. Those fibers exhibiting a high selectivity for polar compounds were selected to carry out an analytical method for a group of 5 alkylphenols, including bisphenol-A (BPA) and nonylphenol (n-NP). Under optimum conditions, average relative recoveries of 108% and inter-day precision values (3 non-consecutive days) lower than 19% were obtained for a spiked level of 10µgL(-1). Correlations coefficients for the overall method ranged between 0.990 and 0.999, and limits of detection were down to 1µgL(-1). Tap water, river water, and bottled water were analyzed to evaluate matrix effects. Comparison with the PA fiber was also performed in terms of analytical performance. Partition coefficients (logKfs) of the alkylphenols to the SPME coating varied from 1.69 to 2.45 for the most efficient PIL-based fiber, and from 1.58 to 2.30 for the PA fiber. These results agree with those obtained by the normalized calibration slopes, pointing out the affinity of these PILs-based coatings.