Development and validation of a generic nontarget method based on liquid chromatography - high resolution mass...

A comprehensive workflow for using nontarget approaches as process evaluation tools was implemented, including data acquisition based on a LC-HRMS (QTOF) system using direct injection and data post-processing for the peak recognition in "full scan" data. Both parts of the approach were not only developed and validated in a conventional way using the suspected analysis of a set of spiked known micropollutants but also the nontarget analysis of a wastewater treatment plant (WWTP) effluent itself was utilized to consider a more environmental relevant range of analytes. Hereby, special focus was laid on the minimization of false positive results (FPs) during the peak recognition. The optimized data post-processing procedure reduced the percentage of FPs from 42% to 10-15%. Furthermore, the choice of a suitable chromatography for biological treated wastewater systems was also discussed during the method development. The workflow paid also attention to differences in the performance levels of the LC-HRMS system by implementation of an adaption system for intensity variations comparing different measurements dates or different instruments. The application of this workflow on wastewater samples from a municipal WWTP revealed that more than 91% compounds were eliminated by the biological treatment step and that the received effluent contained 55% newly formed potential transformation products.