Aleksander Kravos (Author), Helena Prosen (Author)

Abstract

Solid-phase extraction (SPE) has gained an essential role in environmental analytical chemistry. Classic off-line SPE coupled with LC-MS/MS systems creates powerful analytical procedures for ultratrace analysis of contaminants of emerging concern (CECs) in water. But, being associated with tedious work and large consumption of materials, alternative SPE modes are becoming interesting. As so, the study focuses on development, evaluation, and overall comparison of established and novel SPE modes. Off-line SPE, dispersive micro SPE (DMSPE), and ‘fast’ single-pump on-line SPE were explored, using commercially available sorbents. Their efficiency was evaluated on their performance in water analysis of 20 multiclass CECs. Hydrophilic-lipophilic sorbent and mixture of C18/C8 sorbents were the best choice for off-line and DMSPE, respectively. All optimized SPE modes coupled with UHPLC-MS/MS reached environmentally-relevant limits of detection (LODs 0.1− 12 ng L$^{−1}$), acceptable repeatability (<20 % RSD), and exhibited less than ±30 % matrix effects in real river water sample. Among all, on-line SPE showed a potential to fully replace the well-established off-line SPE and even improve analytical performance. This was due to the best repeatability (<10 % RSD), automatization, simplicity, the highest multiplexing capacity, as well as comparable LODs of <2 ng L$^{−1}$. DMSPE is, on the other hand, the most innovative and could be seen as a quick and green alternative to off-line SPE for determination of semi-to-nonpolar CECs, but within sub-10 ng L$^{−1}$ range. Overall, the study shows workflow for the exploration of important and promising sample pretreatment techniques in water analysis. Comparison of the developed three SPE-UHPLC-MS/MS methods suggests that alternative SPE modes can compete with the well-established off-line SPE and can even improve the analysis quality if properly applied.

Keywords

novodobna organska onesnaževala;tehnike priprave vzorca;razvoj analiznih metod;off-line SPE;on-line SPE;disperzivna mikro ekstrakcija na trdno fazo;contaminants of emerging concern;sample pretreatment;method development;dispersive micro solid-phase extraction;

Data

Language: English
Year of publishing:
Typology: 1.01 - Original Scientific Article
Organization: UL FKKT - Faculty of Chemistry and Chemical Technology
UDC: 542.61
COBISS: 201913091 Link will open in a new window
ISSN: 0003-2670
Views: 45
Downloads: 4
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Other data

Secondary language: Slovenian
Secondary keywords: novodobna organska onesnaževala;tehnike priprave vzorca;razvoj analiznih metod;off-line SPE;on-line SPE;disperzivna mikroekstrakcija na trdno fazo;
Type (COBISS): Article
Pages: str. 1-12
Issue: ǂVol. ǂ1319, [article no.] 342955
Chronology: 29 Aug. 2024
DOI: 10.1016/j.aca.2024.342955
ID: 24599389