Optimization of preconcentration procedure using magnetic nanoparticles for the determination of manganese in cereal samples

In the present study, we developed a magnetic nanoparticle adsorbent that uses iron oxide nanoparticles as the core and 1-(2-pyridylazo)-2-naphthol (PAN) as manganese ion exchange groups in cereal samples. This adsorbent was shown to be quick and efficient for the adsorption of manganese due to higher specific surface area, lower mass removal resistance and the absence of internal diffusion resistance. This method is simple and rapid for the preconcentration and determination of manganese in food samples by inductively coupled plasma optical emission spectrometry (ICP OES). The technical feasibility of magnetic nanoparticles for the removal of manganese was investigated under batch studies. It was based on (PAN)-modified magnetic nanoparticles. Four variables (pH of solution, amount of extractant (E), amount of nanoparticles (N) and time) were regarded as factors in the optimization. Results of the two-level fractional factorial design (2⁴⁻¹) based on an analysis of variance demonstrated that only the pH, amount of extractant (E) and amount of nanoparticles (N) were statistically significant. Optimal conditions for the extraction of manganese were obtained using Box–Behnken design. For optimum recovery of manganese, the variables pH of solution, amount of nanoparticles and amount of extractant values were 9.44, 3.46 mg and 3.91 mg, respectively. In the optimum experimental conditions, the limit of detection and enrichment factor of the proposed method were 0.1 μg L−1 and 28, respectively. The precision as RSD was 3.6% for concentration of 50 μg L−1. The accuracy of the proposed procedure was evaluated by analysis of certified reference material. The method was applied to the determination of manganese in barley, wheat and rice flour samples. The manganese content in the samples analyzed varied from 7.8 to 19.9 μg g−1.