Akademik Veri Yönetim Sistemi
Talanta, cilt.308, 2026 (SCI-Expanded, Scopus)
Accurate quantification of trace organic compounds in complex aquatic matrices is frequently limited by matrix effects, analyte losses, and uncertainties associated with conventional calibration strategies. In this study, a quadruple isotope dilution (ID4) approach coupled with Orbitrap high-resolution mass spectrometry was developed as a reference-grade analytical method. The method was applied to wastewater (WW) and river water (RW) samples, using paracetamol as the model analyte. The LC-ESI-ID4-HRMS method demonstrated excellent accuracy, yielding recoveries between 99.7% and 101.7% across three different aqueous matrices. The robustness of the ID4 strategy was evaluated through two targeted pairwise comparisons. At low concentration levels, the values determined using the ID4 strategy (4.04 ± 0.03 μg kg−1 for the effluent WW sample and 3.06 ± 0.05 μg kg−1 for the RW sample) showed close agreement with those obtained by the standard addition calibration method (4.02 ± 0.04 μg kg−1 for the effluent WW sample and 3.26 ± 0.04 μg kg−1 for the RW sample). At high analyte levels in the influent water, results obtained by the LC-ESI-ID4-HRMS and direct infusion NanoESI-ID4-HRMS were in close agreement (1490.6 ± 9.3 μg kg−1 and 1457.6 ± 48.3 μg kg−1, respectively), demonstrating reliable quantification even without chromatographic separation. These results demonstrate that the combination of high-resolution isotope ratio measurements with the ID4 experimental design enables matrix-independent quantification across different concentration levels and analytical configurations.