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Abstract
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A novel magnetic nano-biocomposite (MNBC) was introduced as an adsorbent for a dispersive magnetic solid-phase extrac-
tion procedure. The synthesis of the MNBC is based on the co-precipitation of Ni(II) and Fe(III) ions as their hydroxide
forms via a simple hydrothermal method, calcination of the obtained Ni–Fe layered double hydroxide, and hybridation
of the resultant NiO–NiFe 2 O 4 MNC with chitosan nanoparticles. After prosperous synthesis and characterization of the
MNBC, it was applied as an effectual adsorbent for the extraction and pre-concentration of cadmium ions (Cd(II)) from
aqueous solutions followed by flame atomic absorption spectrometry detection. The essential factors affecting the extraction
recovery were investigated and optimized. According to the method validation, the method’s linear dynamic range was from
0.2 to 30 ng mL‒1 with a determination coefficient of 0.9996, and the limit of detection was calculated to be 0.02 ng mL‒1 .
The precision of the method in terms of intra-day and inter-day relative standard deviations (n = 6) with a concentration of
20ng mL‒1 Cd(II) were 1.42% and 2.11%, respectively. The developed method’s accuracy was confirmed by analysis of a
certified reference sample. The developed method was applied for the determination of Cd(II) in various water and indus-
trial wastewater samples. The satisfactory relative recovery values between 97.6 and 103.9% were achieved for the spiked
samples, confirming the ignorable matrix effect and successive applicability of the method.
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