Optimization of matrix solid-phase dispersion for liquid chromatography tandem mass spectrometry analysis of 12 pharmaceuticals in sediments

The matrix solid-phase dispersion (MSPD) technique accompanied with LC–MS/MS detection for the purpose of determination of 12 pharmaceuticals (sulfaguanidine, sulfadiazine, sulfamethazine, sulfamethoxazole, trimethoprim, roxithromycin, praziquantel, febantel, enrofloxacin, ciprofloxacin, norfloxacin and procaine) applied to sediment samples has been described in this paper. Different parameters, such as the type of solid phase, the elution solvent and its volume have been investigated. The analytes were successfully extracted by C18 as an MSPD sorbent with 5 mL of acetonitrile:5% of oxalic acid = 6:4 (v/v) as an elution solvent. The proposed method provides a linear response over the concentration range of 0.0005–100 μg/g, depending on pharmaceuticals with correlation coefficients above 0.9928 in all cases except for trimethoprim (0.9889). Also, the method has revealed low limits of detection (0.125–500 ng/g), good precision (intra and inter-day), a relative standard deviation below 15% and recoveries above 80%, except for roxithromycin, febantel and enrofloxacin. The method has been successfully applied to analysis of different sediment samples.

► First matrix solid-phase extraction (MSPD) method for determination of pharmaceuticals in sediments samples.
► Optimization of MSPD procedure.
► Validation of developed MSPD–LC–MS/MS method for simultaneous determination of 12 pharmaceuticals in sediments samples.