Application of a fast and sensitive method for the determination of contaminants of emerging concern in wastewater using a quick, easy, cheap, effective, rugged and safe-based extraction and liquid chromatography coupled to mass spectrometry

Abstract

The inefficiency of wastewater treatment plants (WWTPs) to remove contaminants of emerging concern (CECs) leads to their continuous release to the environment. Consequently, CECs are present at low concentrations in the treated wastewater (TWW), producing unpredicted and unwanted effects on living organisms as they are discharged into water receiving bodies. This work presents a fast and reliable method for the determination of CECs in TWW based on the innovative application of a QuEChERS (quick, easy, cheap, effective, rugged and safe) method for water extraction and determination by sensitive liquid chromatography coupled to quadrupole-linear ion trap tandem mass spectrometry (LC-QqLIT-MS/MS). The scope of the proposed QuEChERS-based method allows the monitoring of 107 CECs, including pharmaceuticals (58), antibiotics (16) and pesticides (33). The proposed method was successfully validated in urban TWW at two concentration levels (50 and 500 ng L−1) and it is a feasible alternative to conventional and time-consuming solid-phase extraction (SPE) methodologies. 89% of the CECs presented mean recovery values in the 70–120% range with relative standard deviations (RSDs) always < 20% (intra and inter-day precision), and limits of quantification (LOQs) in the range 5–500 ng L−1 (89% of the compounds showed a LOQ ≤ 50 ng L−1). The applicability of the method was demonstrated by the analysis of urban TWW samples (7 sampling events). In total, 35 CECs (23 pharmaceuticals, 2 antibiotics and 10 pesticides) were detected in the monitored samples with concentrations ranging from 5 to 677 ng L−1.