This study involved the development of a novel adsorbent by combining a Zn-based MOF with a melamine-based COF, resulting in the formation of a hybrid material known as Zn-MOF/COF. The adsorbent was characterized using FT-IR, SEM, XRD, EDX, and BET analysis techniques. The resulting Zn-MOF/COF sorbent was employed to prepare solid-phase microextraction (SPME) fibers for the extraction and enrichment of polycyclic aromatic hydrocarbons (PAHs) in contaminated soil samples, after coupling with GC-FID. A Box-Behnken design (BBD) was used to optimize key variables of SPME conditions. Under optimal conditions of 85 °C for 30 min extraction with 23 μL g sample's moisture level, linear responses of six PAHs were ranging from 1 to 20000 ng g⁻ with determination coefficients greater than 0.99. Limits of detection (LODs) were over the ranges of 0.1-1 ng g-1. The RSDs for intra-fiber and inter-fiber analyses were obtained 2.2-6.6% and 5.2-11.6%, respectively. Relative recoveries values for real soil samples were found to be 91.1-110.2%. The results showed lower cost and higher extraction efficiency for the Zn-MOF/COF fiber, compared with commercial and homemade adsorbents.
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