Use of Passive and Grab Sampling and High-Resolution Mass Spectrometry for Non-Targeted Analysis of Emerging Contaminants and Their Semi-Quantification in Water

Abstract

Different groups of organic micropollutants including pharmaceuticals and pesticides have emerged in the environment in the last years, resulting in a rise in environmental and human health risks. In order to face up and evaluate these risks, there is an increasing need to assess their occurrence in the environment. Therefore, many studies in the past couple of decades were focused on the improvements in organic micropollutants’ extraction efficiency from the different environmental matrices, as well as their mass spectrometry detection parameters and acquisition modes. This paper presents different sampling methodologies and high-resolution mass spectrometry-based non-target screening workflows for the identification of pharmaceuticals, pesticides, and their transformation products in different kinds of water (domestic wastewater and river water). Identification confidence was increased including retention time prediction in the workflow. The applied methodology, using a passive sampling technique, allowed for the identification of 85 and 47 contaminants in the wastewater effluent and river water, respectively. Finally, contaminants’ prioritization was performed through semi-quantification in grab samples as a fundamental step for monitoring schemes.

Partially saturated vertical surface flow constructed wetland for emerging contaminants and antibiotic resistance genes removal from wastewater: The effect of bioaugmentation with Trichoderma

“…Sample preparation, chromatographic separation, and mass spectrometry conditions are described in detail elsewhere (Tadić et al, 2022). Briefly, a generic approach was applied that consisted of SPE using OASIS HLB cartridges (200 mg sorbent, 6 cc).…”

“…As the influent was a secondary treated WWTP effluent, transformation products (TPs) were also investigated. A total of 22 TPs were identified by LC-HRMS in the influent following a workflow previously published by our group (see Supplementary Excel file 3 and Tadić et al, 2022). Tramadol N-oxide, valsartan acid, venlafaxine N-oxide, O-desmethylvenlafaxine N-oxide were confirmed with reference standards, whereas the others were confirmed by matching their spectrum with library spectrum data (i.e., mz cloud).…”

Explorative Quantitative Nontarget Analysis Reveals Micropollutants in Danish Groundwater

“…Indeed, the variability among the triplicate measurements might originate from the relative quantification error of the semiquantification approach, which consequently produce concentration results with relatively high standard deviations. 42 Since semiquantification tools require the use of tailoring compounds, standard or labeled internal standards with known concentration, for the estimation of analyte concentration, the contribution due to variability in the detection of the (internal) standard compounds among samples, for example, within the triplicate cannot be avoided. Nonethe- Across all regions, pesticides and their degradation products were found at a higher concentration than other micropollutants.…”

Occurrence of Contaminants of Emerging Concern and Pesticides and Relative Risk Assessment in Tunisian Groundwater

“…For the suspect screening, the analysis was performed following the method described in Tadić et al (2022). Briefly, HPLC Accelera 600 pump coupled to a Q-Exactive Orbitrap mass spectrometer (Thermo Fischer Scientific, Les Ullis, France) with a HESI source was used for detection and the column for the chromatographic separation was a Waters XBridge BEH C18 (2.1 × 150 mm and 2.5 μm particle size).…”

“…For the targeted quantification of the prioritized pesticides, the method used was also developed by Tadić et al (2022) where an Alliance HPLC system (Waters Series 2695) and a reverse-phase column, a Phenomenex Kinetex Polar C18 (100 mm × 4.6 mm I⋅D × 2.6 μm particle size) were used. In this case, the mobile phase consisted of Milli-Q and acetonitrile, both with 0.05 % formic acid, and the flow rate was set at 0.4 mL min − 1 .…”