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Sensitive detection of fluoroquinolone antibiotics using Fe3O4@MOF@COFs-based magnetic solid-phase extraction coupled with HPLC

Xiupei Yang,Xin Zhou,Qingying Wang,Qiang Yang,Jiayu Wang,Lianfang Chen

The widespread use of fluoroquinolone antibiotics (FQs) in medical and agricultural applications has raised significant environmental and food safety concerns, necessitating the development of sensitive and reliable detection methods. This study presents an advanced analytical approach combining a novel hierarchical magnetic Metal organic framework@Covalent organic framework (MOF@COF) composite materials, named Fe 3 O 4 @NH₂-MIL-88(Fe)@TpBD (Fe 3 O 4 @MOF@COFs), with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) for trace-level FQ determination. The composite was synthesized via a solvothermal method featuring in situ growth of covalent organic frameworks (COFs) on magnetic metal‒organic frameworks (MOFs) and exhibited exceptional performance in magnetic solid‒phase extraction (MSPE) of three target FQs (enrofloxacin, ciprofloxacin, and norfloxacin). The method achieved outstanding sensitivity (0.23–0.27 ng mL⁻¹), a wide linear range (0.70–1000 ng mL⁻¹), strong correlation (R² = 0.9996), and excellent repeatability (1.6–3.8 % RSD). Successful applications in tap water and chicken samples demonstrated recoveries of 85.8–112.2 %, whereas adsorption studies using pseudo-first-order, pseudo-second-order, Langmuir, and Freundlich models provided mechanistic insights into the extraction process. This work has the following advantages: (1) a graded magnetic adsorbent with good extraction efficiency was designed through the synergistic effect of MOF-COF, (2) a robust detection scheme with convenient and fast performance was established, and (3) the adsorption mechanism of recyclable materials was elucidated, thereby demonstrating excellent practical utilization. In summary, this MOF@COFs-MSPE-HPLC-UV method provides a sensitive, efficient, and sustainable solution for monitoring trace FQ pollutants in complex matrices, which is expected to promote the development of the environment and food safety.