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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Main Authors: Faheem Shah, Munazza Ghafoor
Format: Article
Language:English
Published: MDPI AG 2023-02-01
Series:Separations
Subjects:
Online Access:https://www.mdpi.com/2297-8739/10/2/124
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author Faheem Shah
Munazza Ghafoor
author_facet Faheem Shah
Munazza Ghafoor
author_sort Faheem Shah
collection DOAJ
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
work_keys_str_mv AT faheemshah synthesisandsurfacemodificationofironoxidenanoparticlesfortheextractionofcadmiumionsinfoodandwatersamplesachemometricstudy
AT munazzaghafoor synthesisandsurfacemodificationofironoxidenanoparticlesfortheextractionofcadmiumionsinfoodandwatersamplesachemometricstudy