Multi-residue analysis of emerging pollutants in sediment using QuEChERS-based extraction followed by LC-MS/MS analysis

Abstract

Emerging contaminants are suspected to cause adverse effects in humans and wildlife. Aquatic ecosystems are continuously contaminated by agricultural and industrial sources. To establish a causality relationship between the occurrence of contaminants in the environment and disease, experiments including all environmental matrices must be performed. Consequently, the current analytical tools must be improved. A new multi-residue method for analysing 15 emerging pollutants in sediments based on the Quick, Easy, Cheap, Effective, Rugged and Safe approach is reported. The development of such a multirisque, inter-family method for sediment including pharmaceuticals, pesticides, personal care products and plasticizers is reported for the first time. The procedure involves salting-out liquid-liquid extraction using acetonitrile and clean-up with dispersive solid phase extraction, followed by liquid chromatography coupled with tandem mass spectrometry. The validated analytical procedure exhibited recoveries between 40 and 98% for every target compound. This methodology facilitated the determination of pollutant contents at nanogram-per-gram concentrations.

Improved sample treatment for the determination of 17 strong sorbed quinolone antibiotics from compost by ultra high performance liquid chromatography tandem mass spectrometry

“…PSA resulted the most statistically significant parameter for almost all compounds, with a positive effect for both, its lineal and quadratic terms. These results are according to previous works, because the use of PSA in the determination of quinolones in similar environmental matrices has been already documented [30,33]. PSA demonstrated its ability to selectively remove acidic interferences that are main components of compost, such as humic and fulvic acids, as well as other organic acids, polar pigments, carbohydrates, sugars and fatty acids with hydrogen bonding properties [28].…”

“…After extraction, the organic solvent phase containing the analytes of interest is cleaned up again by adding an SPE sorbent (dispersive SPE, D-SPE) such as primary secondary amine (PSA) or C18, to remove interferences. Recently, some works for the determination of antimicrobial agents using this technique in environmental matrices have been published [30][31][32][33][34], including quinolones [31,34]. However, the extraction procedure led to low recoveries, which is indicative of the need of drastic extraction conditions.…”

Evolution and applications of the QuEChERS method

“…Apart from the comparison between acetate-buffered and citrate-buffered procedures, which has been common in some of these works [110][111][112][113], different authors have compared the efficiency, speed and ease of QuEChERS methods with other well-established procedures [LLE, the Folch method (used in the extraction of lipids), pseudo-modified QuEChERS (avoiding the d-SPE step), microwave-assisted solvent extraction, classical SPE, pressurized liquid extraction (coupled to gel-permeation chromatography or SPE)] for the extraction of miscellaneous compounds [93,97,114]. Although QuEChERS provided better (or comparable) results in the majority of the manuscripts (in terms of not only efficiency and speed but also solvent and reagent consumption and economic cost), there are examples in which QuEChERS methods has been less efficient [97,107].…”

Determination of pharmaceuticals in freshwater sediments using ultrasonic-assisted extraction with SPE clean-up and HPLC-DAD or LC-ESI-MS/MS detection

“…Thus, the use of an SPE step was necessary for purification and for reducing the effects of the matrix interfering substances, resulting in sample enrichment. 26,42,43 The effect of pH manipulation of the diluted UAE extract on SPE recoveries using the optimal elution solvents was tested by adjusting the pH to 2, 4.6 and 10 ( Table 3). The acidification of extracts prior to SPE clean-up increased the recoveries for all pharmaceuticals except cimetidine which showed a low SPE recovery (60.8%) and total recovery of 46.2%.…”