This work concerns the development of a novel and rapid in situ dispersive liquid-liquid microextraction method for magnetic retrieval of ionic liquid as a new approach for the separation of benzophenone type (BP-type) UV filters via quantification using UPLC with PDA detection. The analytes determined in this study were a group of three benzophenones: 2,4-dihydroxybenzophenone (BP1), 2,2′,4,4′-tetrahydroxybenzophenone (BP2) and 2-hydroxy-4-metoxybenzophenone (BP3). The hydrophilic ionic liquid found suitable for use as an extraction solvent of the targeted analytes was didecyldimethylammonium chlorate (DDAC). An anion exchanger, NaClO 4 was added to promote a metathesis reaction and in situ formed the IL, [DDA][ClO 4 ]. The experimental parameters such as the concentration of IL, the molar ratio of DDAC to NaClO 4 , amount of iron oxide added and volume of water sample were investigated and optimised using a step-by-step optimisation process. The optimum experimental parameters were as follows: 30 mL of sample volume, 1% concentration of DDAC, the molar ratio of DDAC to NaClO 4-1:2, and 5 mg of Fe 3 O 4 magnetic nanoparticles. The proposed extraction method is simple and requires no more than 5 min. The detection limit (LOD) obtained for target analytes ranged from 12.320.0 ng L −1 , while the correlation coefficient (r 2) was from 0.9995 to 0.9999. Finally, the developed method was successfully applied to the determination of BP-type UV filters in environmental water samples, and satisfactory results were obtained.
In this study, the dual nature of quaternary ammonium ionic liquid–didecyldimethylammonium perchlorate, [DDA][ClO4], was evaluated. A novel and sensitive in situ ionic liquid dispersive liquid–liquid microextraction method (in situ IL-DLLME) combined with magnetic retrieval (MR) was applied to enrich and separate selected organic micro-pollutants, both polar and non-polar. The magnetic support relied on using unmodified magnetic nanoparticles (MNPs) prepared by the co-precipitation of Fe2+/Fe3+ (Fe3O4). The separation technique was on-lined with high-performance liquid chromatography (HPLC–DAD) verified by inverse gas chromatography. An anion exchanger, NaClO4, was added to form an in situ hydrophobic IL. The fine droplets of [DDA][ClO4], molded in aqueous samples, functioned as an extractant for isolating the studied compounds. Then the carrier MNPs were added to separate the IL from the water matrix. The supernatant-free sample was desorbed in acetonitrile (MeCN) and injected into the HPLC system. The applicability of [DDA][ClO4] as an extraction solvent in the MR in situ IL-DLLME method was checked by the selectivity parameters (Sij∞) at infinite dilution. The detection limit (LOD) ranged from 0.011 to 0.079 µg L−1 for PAHs and from 0.012 to 0.020 µg L−1 for benzophenones. The method showed good linearity with correlation coefficients (r2) ranging from 0.9995 to 0.9999.
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