In this study, solid-phase microextraction (SPME) fiber adsorbents were coated with the metal-organic framework ZIF-67 and protected by layered double hydroxides (LDH) nanotubes. The findings unequivocally show that the extraction selectivity is dependent on the surface element composition of coatings produced from ZIF-67. The ZIF-67@NiCo-LDHs coating was chosen for the enrichment and detection of polycyclic aromatic hydrocarbons (PAH) in water samples due to its long-term stability and superior extraction selectivity. The calibration curves were dynamically linear and ranged from 0.00 to 100 g L1 at the optimum circumstances, with correlation values (R2) above 0.996–0.999. LOD values ranged from 0.07 to 0.5 ng L1. Under ideal circumstances, the test compounds’’ repeatability for one fiber (n ¼ 3), expressed as relative standard deviation (RSD%), ranged between 7.5 and 9.2%. Additionally, the synthetic fiber displayed 40 cycles of extraction and desorption and perfectly controlled development.
