Determination of 136 pharmaceuticals and hormones in sewage sludge using quick, easy, cheap, effective, rugged and safe extraction followed by analysis with liquid chromatography–time-of-flight-mass spectrometry

The aim of this study was to develop an analytical method for the analysis of a wide range of hormonal steroids and pharmaceutical compounds in sewage sludge. Thus, 136 substances were selected, including 119 pharmaceuticals and 17 hormonal steroids. An innovative sample preparation procedure based on the quick, easy, cheap, effective, rugged and safe (QuEChERS) method was developed. The analysis was then performed using liquid chromatography coupled with time-of-flight mass spectrometry. This analytical procedure was validated by evaluating the specificity, quadratic curve fitting, recovery, reproducibility and limits of detection and quantification. The method allows the analysis of the majority of the target compounds with limits of detection ranging from 1 ng/g to 2500 ng/g, depending on the nature of the substance. The protocol was then successfully applied to various types of sludge (limed, digested, dried, liquid and composted) collected in several sewage works in France. Among the target compounds, 34 were quantified at levels up to 6000 ng/g. Among the most commonly detected pharmaceuticals were the antiemetic domperidone (mean concentration 769 ng/g) and the antiepileptic lamotrigine (mean concentration 31 ng/g) whose presence had, to our knowledge, never been shown in sludge.