ABSTRACT The occurrence of pharmaceutical residues in the environment has sparked interest in developing a multi-residue method to analyse a broader range of compounds. This study focuses on the development and validation of a methodology that employs QuEChERS extractions combined with UPLC-MS/MS, enabling simultaneous detection and quantification of pharmaceutical compounds from diverse therapeutic classes (fluoroquinolones, sulphonamides, anticonvulsants, tetracyclines, macrolides, β – blocker, cephalosporins and anti-inflammatory non-steroids) in sediments. The extraction using 0.2 M Na2-EDTA solution and 0.5% acetic acid in MeOH, partitioning by MgSO4/NaOAc (4:1) and cleaning up by C18 sorbent. The analytical performance demonstrated commendable accuracy (trueness and precision), alongside favourable linearity, with MDLs approaching relevant environmental samples, allowing for trace analysis. The MDLs ranged from 0.03 to 2.2 ng/g dried weight (d.w) while slightly lower than IDLs and varied from 0.001 to 0.1 ng/mL. The recovery test yielded satisfactory results (40–120%) for 11 compounds. The optimised method has been effectively applied to quantify the concentration of pharmaceutical residues in surface sediments collected from several locations including Red River (within Hanoi), West Lake and Yen So Lake, with five samples collected at each site. The five compounds (SMZ, TMP, AZM, SOL and DIC) were quantified with the concentration ranged from 1.5 to 56.8 ng/g d.w. in lake sediments, while only CTX was detected in one-fifth river sediments at 10.2 ng/g d.w.
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