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A fast gas chromatography/mass spectrometry method was developed and validated for the analysis of the potential endocrine disrupters octinoxate and oxybenzone in swimming pool water samples based on the solvent-free solid-phase microextraction technique. The low-pressure gas chromatography/mass spectrometry method used for the fast identification of UV filter substances was compared to a conventional method in terms of sensitivity and speed. The fast method proposed resulted in 2 min runs, leading to an eightfold decrease in the total analysis time and a sevenfold improvement in detection limits. The main parameters affecting the solid-phase microextraction process were also studied in detail and the optimized conditions were as follows: fiber coating, polyacrylate; extraction mode, direct immersion; extraction temperature, 25°C; sample volume, 5 mL; extraction time 45 min; pH 6.5. Under the optimized conditions, a linear response was obtained in the concentration range of 0.5-25 μg/L with correlation coefficients in the range 0.990-0.999. The limits of detection were 0.17-0.29 μg/L, and the recoveries were 80-83%. Combined method uncertainty was assessed and found to be less than 7% for both analytes for concentrations equal to or higher than 5 μg/L. Pool water samples were analyzed to demonstrate the applicability of the proposed method. Neither octinoxate nor oxybenzone were detected in the swimming pool water samples at concentrations above the respective limits of detection.

This work describes the development of a fast method for speciation analysis of triethyl-lead and tributyl-tin species in urine samples after in situ derivatization by tetraethyl- or tetrapropyl-borate reagents. The alkylation reaction is done in the aqueous and urine medium and the less-polar derivatives are extracted in hexane by liquid-liquid extraction. The species were extracted and the extract was efficiently collected from the aqueous phase after centrifugation. Finally, the organometallic species are separated by gas chromatography and determined from the emission signals of elemental lead and tin. Atomic lead and tin are formed from the organolead and organotin compounds during atomization of the column eluate in a microwave-induced helium plasma source. The simultaneous measurement of lead (Pb) at 405.780 nm and tin (Sn) at 303.419 nm was achieved by an atomic emission detector. Finally, the analytes were determined with satisfactory precision (

A novel monolithic methylsilsesquioxane-based material with hierarchical pore structure was prepared and tested for its applicability as stationary phase for RP-HPLC. The monolithic material is produced using sol-gel chemistry according to a proprietary protocol developed in our working group. A procedure for the production of HPLC columns from the self-contained monolithic material is described. The chromatographic performance and the reproducibility of the column production was tested using the procedures of the widely accepted Tanaka test and suitable parts of the Engelhardt test which were applied to a set of four monolithic columns produced under identical conditions. The test proved the excellent hydrophobic selectivity and silanophilic behaviour of the new stationary phase material. According to the tests on steric and shape selectivity, there are strong indications that this type of material also acts as restricted access material. This assumption is further supported by the presence of a high fraction of micropores as was evidenced by physical characterisation of the material. The novel stationary phase material showed great potential for the separation of small apolar substances and was found to be particularly useful in the separation of basic compounds due its excellent silanophilic interaction.