New insights into the design of highly sensitive, carbon‐based electrochemical sensors are presented in this work. This was achieved by exploring the interesting properties of conductive (Mg/Al) layered double hydroxide‐dodecyl sulphate/polypyrrole nanocomposites which were synthesized by in‐situ polymerization of pyrrole during the assembly of (Mg/Al) layered double hydroxide, and by employing the anionic surfactant dodecyl sulphate as a modifier. Changes in morphology and surface area of the nanocomposites occured as a result of change in pyrrole percentage. Under optimal conditions, the modified carbon paste electrode successfully achieved detection limits of 0.057 and 0.134 nmol L−1 of Terazosin hydrochloride in pharmaceutical formulation and spiked human serum fluid, respectively. Moreover, the sensors are highly stable, reusable and free of interference by other commonly present excipients in drug formulations.
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