Quantification of pharmaceuticals and endocrine disruptors in river sediments: development and validation of a QuEChERS based extraction.

Accessing exposure concentrations can be challenging for the analyst as environmental concentrations and toxicological or eco-toxicological effect induced quantities are often not consistent with analysis capacities. To encounter those limitations analysts use pre-concentration and purification steps like Accelerated Solvent Extraction (ASE) and Solid Phase Extraction (SPE) to extract and analyse pharmaceuticals or hormones at the lower or sub ng/g level from solid matrices. A recent extraction method known as Quick Easy Cheap Effective Rugged and Safe has been developed for the analysis of pesticides in food matrices. This method has already been extended to various matrices like rats' serum and gonads in our laboratory. We developed and validated a multiresidue analytical method with QuEChERS extraction for the screening of multi-families of pharmaceuticals and endocrine disruptors in river sediments. The molecules were chosen among the priority pollutants listed in a prioritisation for French surface waters, in the Water Framework Directive and within the potential or confirmed EDCs. This selection of 13 pharmaceuticals includes β-blockers, anti-inflammatories, antibiotics, anxiolitics, anti-depressants and anti-analgesics 24 EDCs includes pesticides, alkylphenols, hormones and phenolic derivates and. Quantification is performed on a 3200QTrap tandem mass spectrometer (MS/MS) coupled to Liquid Chromatography (LC) Agilent 1200 system with a Kinetex XB-C18 column (100x2.1mm, 1.7μm). Extraction was optimised to get acceptable recoveries (>60%) and the linearity of the method has been verified by statistical means. Acceptable Relative Standard Deviations of both injection and preparation steps (<20 to 30%) were calculated for intraday injections of 3 independent solutions. Repetition of a calibration over three days allowed us to calculate good interday RSD. Limits of quantification were determined by injection of 5 independent standard solutions and were consistent with environmental concentrations.