Introduction: A new solid-phase microextraction fibre is fabricated through polymerisation of molecularly imprinted polymer on the surface of a layered double hydroxide framework that has been fabricated via the in situ synthesis on a non-porous anodic aluminium oxide/aluminium wire as both the substrate and the aluminium source. Objective: The synthesized SPME fiber was performed to analyze trace digoxin in real samples. Material and method: A one-at-a-time optimization strategy was applied for optimizing the important extraction parameters such as extraction solvent, extraction time, stirring rate, pH, ionic strength, and desorption time. Result: Aluminum surface before and after anodizing and LDH structure reveal that anodizing and preparation LDH increases the surface area and adsorption capacity of aluminum wire. Conclusion: Under optimum conditions, the repeatability for one fibre (n = 3), expressed as relative standard deviation (RSD %), was 5.2%
