High-throughput multi-residue quantification of contaminants of emerging concern in wastewaters enabled using direct injection liquid chromatography-tandem mass spectrometry

Abstract

A rapid quantitative method for 135 contaminants of emerging concern (CECs) in untreated wastewater enabled with direct injection liquid chromatography-tandem mass spectrometry is presented. All compounds were analysed within 5 min on a short biphenyl cartridge using only 10 μL of filtered sample per injection. Up to 76 compounds were monitored simultaneously during the gradient (including mostly two transitions per compound and stable isotope-labelled analogues) while yielding >10 data points per peak. Evaluation of seven solid phase extraction sorbents showed no advantage for wastewater matrix removal. Excellent linearity, range, accuracy and precision was achieved for most compounds. Matrix effects were <11 % and detection limits were <30 ng L−1 on average. Application to untreated wastewater samples from three wastewater treatment works in the UK, USA and Mexico, enabled quantification of 56 compounds. Banned and EU ‘watch-list’ substances are critically discussed, including pesticides, macrolide antibiotics, diclofenac, illicit drugs as well as multiple pharmaceuticals and biocides. This high-throughput method sets a new standard for the speedy and confident determination of over a hundred CECs in wastewater at the part-per-trillion level, as demonstrated by performing over 260 injections per day.