Synthesis and Surface Modification of Iron Oxide Nanoparticles for the Extraction of Cadmium Ions in Food and Water Samples: A Chemometric Study
In this project, a prompt, efficient, and effective method for Cd<sup>2+</sup> ions extraction from different food and water samples using magnetic dispersion-based solid phase extraction by functionalized iron oxide nanoparticles was proposed. Iron oxide nanoparticles were synthesized t...
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MDPI AG
2023-02-01
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author | Faheem Shah Munazza Ghafoor |
author_facet | Faheem Shah Munazza Ghafoor |
author_sort | Faheem Shah |
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description | In this project, a prompt, efficient, and effective method for Cd<sup>2+</sup> ions extraction from different food and water samples using magnetic dispersion-based solid phase extraction by functionalized iron oxide nanoparticles was proposed. Iron oxide nanoparticles were synthesized through the co-precipitation method followed by functionalization with tetraethyl orthosilicate (TEOS) and 3-aminopropyl silane (APTES) to obtain Fe<sub>3</sub>O<sub>4</sub>@SiO<sub>2</sub>@APTES. This composite was characterized through different techniques, including vibrating sample magnetometer, dynamic light scattering, zeta potential, FTIR, SEM, XRD, and BET. Variables studied were pH, temperature, sorbent amount, sonication time, and sample and eluent volume affecting the sorption efficacy of freshly synthesized sorbent. Plackett–Burman design was utilized for the identification of significant factors for microextraction of target analyte, while the central composite design was utilized for the optimization of significant factors. Detection and quantification limits obtained were 0.17 and 0.58 μgL<sup>−1</sup>, respectively, with an enhancement factor of 83.5. Under optimum conditions, Fe<sub>3</sub>O<sub>4</sub>@SiO<sub>2</sub>@APTES showed good stability even after >80 adsorption/desorption cycles run while maintaining over 96% analyte recoveries. The developed method was validated by assessing certified reference materials and standard addition methodology for Cd<sup>2+</sup> detection in real samples. To confirm the precision, repeatability (RSD<sub>r</sub>) and reproducibility (RSD<sub>R</sub>) were calculated and found as <3.0 (<i>n</i> = 7) and <7.5 (<i>n</i> = 15), respectively. Furthermore, in accordance with the ISO/IEC 17025 recommendations, the validation was also confirmed through a “bottom-up” approach while considering all possible uncertainties in data. |
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spelling | doaj.art-5551b42f992c442190081a90ac60b03d2023-11-16T23:14:40ZengMDPI AGSeparations2297-87392023-02-0110212410.3390/separations10020124Synthesis and Surface Modification of Iron Oxide Nanoparticles for the Extraction of Cadmium Ions in Food and Water Samples: A Chemometric StudyFaheem Shah0Munazza Ghafoor1Department of Chemistry, School of Science, King Faisal University, Hofuf 31982, Saudi ArabiaDepartment of Chemistry, COMSATS University Islamabad, Abbottabad Campus, Abbottabad 22060, PakistanIn this project, a prompt, efficient, and effective method for Cd<sup>2+</sup> ions extraction from different food and water samples using magnetic dispersion-based solid phase extraction by functionalized iron oxide nanoparticles was proposed. Iron oxide nanoparticles were synthesized through the co-precipitation method followed by functionalization with tetraethyl orthosilicate (TEOS) and 3-aminopropyl silane (APTES) to obtain Fe<sub>3</sub>O<sub>4</sub>@SiO<sub>2</sub>@APTES. This composite was characterized through different techniques, including vibrating sample magnetometer, dynamic light scattering, zeta potential, FTIR, SEM, XRD, and BET. Variables studied were pH, temperature, sorbent amount, sonication time, and sample and eluent volume affecting the sorption efficacy of freshly synthesized sorbent. Plackett–Burman design was utilized for the identification of significant factors for microextraction of target analyte, while the central composite design was utilized for the optimization of significant factors. Detection and quantification limits obtained were 0.17 and 0.58 μgL<sup>−1</sup>, respectively, with an enhancement factor of 83.5. Under optimum conditions, Fe<sub>3</sub>O<sub>4</sub>@SiO<sub>2</sub>@APTES showed good stability even after >80 adsorption/desorption cycles run while maintaining over 96% analyte recoveries. The developed method was validated by assessing certified reference materials and standard addition methodology for Cd<sup>2+</sup> detection in real samples. To confirm the precision, repeatability (RSD<sub>r</sub>) and reproducibility (RSD<sub>R</sub>) were calculated and found as <3.0 (<i>n</i> = 7) and <7.5 (<i>n</i> = 15), respectively. Furthermore, in accordance with the ISO/IEC 17025 recommendations, the validation was also confirmed through a “bottom-up” approach while considering all possible uncertainties in data.https://www.mdpi.com/2297-8739/10/2/124cadmiummicroextractionsorbentfood sampleschemometrics |
spellingShingle | Faheem Shah Munazza Ghafoor Synthesis and Surface Modification of Iron Oxide Nanoparticles for the Extraction of Cadmium Ions in Food and Water Samples: A Chemometric Study Separations cadmium microextraction sorbent food samples chemometrics |
title | Synthesis and Surface Modification of Iron Oxide Nanoparticles for the Extraction of Cadmium Ions in Food and Water Samples: A Chemometric Study |
title_full | Synthesis and Surface Modification of Iron Oxide Nanoparticles for the Extraction of Cadmium Ions in Food and Water Samples: A Chemometric Study |
title_fullStr | Synthesis and Surface Modification of Iron Oxide Nanoparticles for the Extraction of Cadmium Ions in Food and Water Samples: A Chemometric Study |
title_full_unstemmed | Synthesis and Surface Modification of Iron Oxide Nanoparticles for the Extraction of Cadmium Ions in Food and Water Samples: A Chemometric Study |
title_short | Synthesis and Surface Modification of Iron Oxide Nanoparticles for the Extraction of Cadmium Ions in Food and Water Samples: A Chemometric Study |
title_sort | synthesis and surface modification of iron oxide nanoparticles for the extraction of cadmium ions in food and water samples a chemometric study |
topic | cadmium microextraction sorbent food samples chemometrics |
url | https://www.mdpi.com/2297-8739/10/2/124 |
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