Exploration of novel solid-phase extraction modes for analysis of multiclass emerging contaminants

Kravos, Aleksander (author), Prosen, Helena (author)

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.

• Language: English
• Keywords: contaminants of emerging concern, sample pretreatment, method development, off-line SPE, on-line SPE, dispersive micro solid-phase extraction
• Work type: Article
• Typology: 1.01 - Original Scientific Article
• Organization: FKKT - Faculty of Chemistry and Chemical Technology
• Publication status: Published
• Publication version: Version of Record
• Year: 2024
• Number of pages: 12 str.
• Numbering: Vol. 1319, art. 342955
• PID: 20.500.12556/RUL-159801
• UDC: 542.61
• ISSN on article: 0003-2670
• DOI: 10.1016/j.aca.2024.342955
• COBISS.SI-ID: 201913091
• Publication date in RUL: 25.07.2024

Record is a part of a journal

• Title: Analytica chimica acta
• Shortened title: Anal. chim. acta
• Publisher: Elsevier
• ISSN: 0003-2670
• COBISS.SI-ID: 5085447

Licences

• License: CC BY 4.0, Creative Commons Attribution 4.0 International
• Link: http://creativecommons.org/licenses/by/4.0/
• Description: This is the standard Creative Commons license that gives others maximum freedom to do what they want with the work as long as they credit the author.

Secondary language

• Language: Slovenian
• Keywords: novodobna organska onesnaževala, tehnike priprave vzorca, razvoj analiznih metod, off-line SPE, on-line SPE, disperzivna mikroekstrakcija na trdno fazo