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Analysis of primary aromatic amines in surface and wastewater using stir bar sorptive extraction with in situ derivatization followed by liquid chromatography-tandem mass spectrometry
| Autoři | |
|---|---|
| Rok publikování | 2026 |
| Druh | Recenzovaný odborný článek |
| Časopis / Zdroj | Microchemical Journal |
| Fakulta / Pracoviště MU | |
| Citace | |
| www | https://www.sciencedirect.com/science/article/pii/S0026265X26017017 |
| Doi | https://doi.org/10.1016/j.microc.2026.118499 |
| Klíčová slova | SBSE; LC-MS/MS; Benzoyl chloride; Surface water; Wastewater; Primary aromatic amines |
| Popis | Primary aromatic amines (PAAs) are toxic and potentially carcinogenic contaminants occurring in wastewater and surface waters. Their quantification in environmental matrices remains challenging due to low concentrations, strong matrix interferences, and poor extractability of underivatized amines. This study presents a selective and sensitive analytical method combining in-situ benzoyl chloride derivatisation with stir bar sorptive extraction (SBSE) and LC-MS/MS analysis for the determination of 22 PAAs in aqueous samples. The derivatisation step efficiently converts PAAs to hydrophobic benzamide derivatives, enabling improved extraction on polydimethylsiloxane (PDMS) and ethylene-glycol silicone (EG) coatings. Extraction and desorption kinetics were systematically evaluated and modelled, to establish optimal conditions of sample processing. Equilibrium was reached within 360 min for PDMS and 120 min for EG, with complete desorption achieved after 1 h in acetonitrile. Sequential extraction experiments allowed estimation of polymer-water distribution coefficients of the derivatives and comparison with predicted loge values. PDMS exhibited superior robustness, low variability, and stable long-term performance, while EG showed higher variability and coating degradation under derivatisation conditions. Matrix-dependent recovery experiments revealed substantial signal suppression in WWTP influent, particularly for high-loge compounds, driven by reduced derivatisation efficiency and competitive sorption. Limits of quantification, determined using standard addition, ranged from low ng/L levels in pure water to tens of ng/L in wastewater matrices. The method provides a miniaturized, solvent-efficient, and selective approach suitable for routine monitoring of PAAs in wastewater and surface waters, offering improved sensitivity and reliability compared to traditional extraction techniques. |
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