Selective monitoring of acidic and basic compounds in environmental water by capsule phase microextraction using sol-gel mixed-mode sorbents followed by liquid chromatography-mass spectrometry in tandem.

Nadal, Joan Carles; Borrull, Francesc; Furton, Kenneth G; Kabir, Abuzar; Fontanals, Núria; Marcé, Rosa Maria

In addition to the diverse extraction techniques available, capsule phase microextraction (CPME), which uses a microextraction capsule (MEC), has recently been introduced as a sorptive-based sample preparation technique. In this study, two different MECs (MEC-C18/SAX and MEC-C18/SCX) based on mixed-mode ion-exchange technology were synthesized and evaluated for the selective extraction of a group of ionizable compounds, including acidic and basic analytes. A sulfonic acid was used as the cation-exchange group in MEC-C18/SCX, and a quaternary amine as the anion-exchange group in MEC-C18/SAX. The extraction parameters optimized were sample pH, elution solvent, sample/elution volume and extraction/elution time. The optimized CPME method followed by LC-MS/MS was used to determine the ionizable compounds in environmental water samples, including river water and effluent wastewater, with excellent selectivity and matrix effect values below -30% (except -33% for mephedrone) and apparent recovery results ranging from 40% to 69%, except for ibuprofen (< 35%) and atenolol (< 25%). The analytical method was validated for environmental water samples, and used in the analysis of several samples in which some of the target compounds were found at ng L-1 concentration levels.