Abstract
ABSTRACT A dispersive magnetic solid-phase extraction by means of core-shell iron-based metal-organic framework (Fe3O4- SiO2/EN@MIL-101(Fe)) nanospheres coupled with high-performance liquid chromatographic was developed for the determination of pyrene (Pyr) and phenanthrene (Phe) in water samples. Key parameters such as sorbent amount, sample volume, pH, extraction time, type and volume of elution, and desorption time were optimised by response surface methodology (RSM). Under the optimised conditions (sample volume: 5 mL, extraction time: 3 min, eluent: 3 mL acetonitrile: propanol, and desorption time: 3 min), the developed method showed a low detection and quantification limits (0.015 and 0.040 ng mL−1, respectively), good precision (< 9.8% RSD), wide linear range (0.06 - 10,000 ng mL−1, R2 > 0.99), high enrichment factors (49–57), good matrix effect (> 93.2%), high reusability (25 times), short extraction and desorption time (3 and 3 min, respectively), and high extraction recovery (96.5%). The established method was able to recover the Pyr and Phe from spiked real water samples with an extraction efficiency of 95.71% and 96.32%, respectively (RSD ≤ 9.52%).
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