Abstract This study focused on developing an analytical method to quantify nineteen selected micropollutants (MPs), including pharmaceuticals and personal care products, in complex wastewater matrices. An online solid-phase extraction system coupled with LC–MS/MS was used, and different mobile phase compositions were tested in the chromatographic method. The validated method was subsequently applied to real influent and effluent samples from an anaerobic biological reactor in order to assess MP occurrence and removal behavior. The best results were achieved using a mixture of acetonitrile and methanol (50:50 v:v) with 0.1% formic acid, offering high resolution, ionization efficiency, and sensitivity. The method demonstrated good linearity, low detection limits (sewage: 12–143 ng L −1 ; effluent: 7–45 ng L −1 ), and RSD 80%), whereas diclofenac and carbamazepine were poorly removed (< 20%). Application to real wastewater samples revealed highly variable influent concentrations and compound-dependent removal efficiencies, highlighting both the analytical challenges posed by complex matrices and the relevance of the method for evaluating biological treatment performance.
Carneiro et al. (Tue,) studied this question.