Identification of unknowns in industrial wastewater using offline 2D chromatography and non-target screening

• Published in: The Science of the total environment Vol. 706; p. 135835
• Main Authors: Purschke, Kirsten, Zoell, Christian, Leonhardt, Juri, Weber, Markus, Schmidt, Torsten C.
• Format: Journal Article
• Language: English
• Published: Netherlands Elsevier B.V 01.03.2020
• Subjects: High-resolution mass spectrometry (HRMS); Identification; Industrial wastewater; Non-target analysis; Prioritisation; High-resolution mass spectrometry (HRMS); Industrial wastewater; Identification; Prioritisation; Non-target analysis
• ISSN: 0048-9697; 1879-1026
• DOI: 10.1016/j.scitotenv.2019.135835

Industrial wastewater is characterised by a complex composition of trace organic compounds (TrOC) in a difficult matrix. The identification of unknown pollutants is of high interest. On the one hand to ensure protection of the environment by elucidating contaminations and on the other hand to protect the biological treatment step in the wastewater treatment plant (WWTP). Due to the high variability of the matrix, the identification of compounds of interest is very time consuming and often unsuccessful. To overcome this limitation, a prioritisation method was developed to identify so called ‘known unknowns’, i.e. compounds frequently detected but not identified, as prioritised compounds in industrial wastewater. The method based on an offline two-dimensional (offline 2D) liquid chromatography (LC) approach with ultra violet (UV) detection in the first and high-resolution mass spectrometry (HRMS) in the second dimension. As a proof of concept, an identification process of one ‘known unknown’ is described. The compound was identified as a dichlorodinitrophenol isomer by retention time in two dimensions, UV spectrum, exact mass, mass fragmentation and 1H- NMR. As prioritisation method, the offline 2D LC in combination with non-target analysis provides a powerful workflow to determine tentative structures of unknown organic compounds in industrial wastewater. [Display omitted] •Frequently observed contaminants named ‘known unknowns’ serve as prioritised compounds.•2D offline LC-UV/LC-HRMS was used for identification.•1st dimension provides clean-up of interfering signals and UV absorption.•2nd dimension provides HRMS for elucidation of unknown wastewater compounds.