Magnetic Solid-Phase Extraction using Ionic Liquid-Modified Magnetic Nanoparticles for The Simultaneous Extraction of Cadmium and Lead in Milk Samples; Evaluation of Measurement Uncertainty
DOI:
https://doi.org/10.29356/jmcs.v65i4.1473Keywords:
Pb (II) and Cd (II) analysis, ionic liquid, magnetic solid-phase extraction, measurement uncertainty, milk samplesAbstract
Abstract. In the present study, a new, sensitive, and rapid method was developed for extraction and determination of the trace amounts of Pb (II) and Cd (II) ions in milk samples through magnetic solid-phase extraction using DABCO based-ionic liquid-modified magnetic nanoparticles (Fe3O4/[DABCO-PDO]Cl NPs). Herein, Pb (II) and Cd (II) contents were quantified with flame atomic absorption spectroscopy (FAAS). The effect of different empirical parameters (such as sample pH, adsorbent amount, type and amount of the elution, extraction and desorption times, and the ligand concentration) was evaluated and optimized for simultaneous extraction and pre-concentration Pb (II) and Cd (II) ions. The calibration curve was linear under the optimum condition in the concentration range of 0.4-200 µgL-1 for Cd, and 0.5-120 µgL-1 for Pb, respectively. The pre-concentration factor was 67, with the detection limit of 0.09 and 0.07 µgL-1 for Pb and Cd, respectively. The relative standard deviation values (RSD %) of the proposed method were lower than 2.6 %. The developed method was successfully used to determine lead and cadmium content in milk samples. The information obtained from the method validation has been used to estimate the expanded uncertainty for the determination of Pb (II) and Cd (II) at trace levels in commercial milks.
Resumen. En este trabajo, se ha desarrollado un nuevo, sensible y rápido procedimiento para la extracción y determinación de iones Pb(II) y Cd(II) a nivel de trazas en leche, mediante extracción en fase sólida utilizando nanopartículas magnéticas modificadas con líquido iónico basado en DABCO (Fe3O4/[DABCO-PDO]Cl NPs). La determinación de ambos metales se llevó a cabo por espectrometría de absorción atómica con atomización en llama. Se ha evaluado el efecto de diferentes parámetros empíricos (tales como pH, cantidad de adsorbente, tipo y cantidad de solvente de elución, tiempo de extracción y desorción, y concentración del ligando); estos parametros fueron optimizados enfocándose en la extracción y preconcentración simultanea de ambos iones. Empleando las condiciones establecidas, se obtuvo buena linealidad de las curvas de calibración en el intervalo de concentraciones 0.4-200 µgL-1 para Cd, y 0.5-120 µgL-1 para Pb, respectivamente. Se logró el factor de preconcentración 67, con los límites de detección 0.09 y 0.07 µgL-1 para Pb y Cd, respectivamente. Los valores de desviación estandar relativa (RSD %) en el procedimiento propuesto no sobrepasaron 2.6 %. En el análisis de leche, se obtuvieron resultados satisfactorios. Los datos obtenidos en etapa de validación se utilizaron para estimar la incertidumbre expandida en la determinación de Pb y Cd a nivel de trazas en leche.
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