In water samples from industrial regions, the presence
of highly
toxic and nonbiodegradable heavy metal ions (HMI) poses a significant
threat to environmental quality. While analytical methods based on
mercury electrodes are widely recognized for their high performance
in the sensitive and selective quantification of various metal contaminants,
the development of environmentally friendly strategies for the voltammetric
determination of HMI remains a formidable challenge. In this study,
we propose a material utilizing small-size chitosan (CTS) cobalt ferrite
core–shell nanoparticles (CoFe2O4@CTS)
as an electrode modifier for the simultaneous voltammetric determination
of Pb(II) and Cd(II). The magnetic nanoparticles were synthesized
using the solvothermal method and characterized using various techniques
to explore their crystalline structure, magnetic properties, and chemical
composition. The resulting electrochemical sensor, CoFe2O4@CTS/GCE, was generated through a one-step modification
of a glassy carbon electrode (GCE). Utilizing differential pulse adsorptive
stripping voltammetry (DPAdSV), our proposed sensor exhibited high
sensitivity, with low limits of detection (LOD) values of 0.04 and
0.31 μg L–1 (E
d = −1.0 V; t
d = 90 s) for lead
and cadmium, respectively. The exceptional sensitivity observed is
indicative of interactions between HMI and CTS amine groups, leading
to the effective preconcentration of the analytes. Furthermore, our
sensor demonstrated excellent selectivity with an interference response
below 8.93% for Pb(II) and 20% for Cd(II). Accuracy was evaluated
using SRM 1643e (NIST). The application of green analytical chemistry
(GAC) metrics resulted in a score of 0.91, highlighting the environmentally
conscious aspects of our methodology.