Speciation, Preconcentration, and Determination of Iron(II) and (III) Using 1,10-Phenanthroline Immobilized on Alumina-Coated Magnetite Nanoparticles as a Solid Phase Extraction Sorbent in Pharmaceutical Products

Authors: Hossein Tavallali, Mohammad Ali Karimi, Gohar Deilamy-Rad

Abstract:

The proposed method for speciation, preconcentration and determination of Fe(II) and Fe(III) in pharmaceutical products was developed using of alumina-coated magnetite nanoparticles (Fe₃O₄/Al₂O₃ NPs) as solid phase extraction (SPE) sorbent in magnetic mixed hemimicell solid phase extraction (MMHSPE) technique followed by flame atomic absorption spectrometry analysis. The procedure is based on complexation of Fe(II) with 1, 10-phenanthroline (OP) as complexing reagent for Fe(II) that immobilized on the modified Fe₃O₄/Al₂O₃ NPs. The extraction and concentration process for pharmaceutical sample was carried out in a single step by mixing the extraction solvent, magnetic adsorbents under ultrasonic action. Then, the adsorbents were isolated from the complicated matrix easily with an external magnetic field. Fe(III) ions determined after facility reduced to Fe(II) by added a proper reduction agent to sample solutions. Compared with traditional methods, the MMHSPE method simplified the operation procedure and reduced the analysis time. Various influencing parameters on the speciation and preconcentration of trace iron, such as pH, sample volume, amount of sorbent, type and concentration of eluent, were studied. Under the optimized operating conditions, the preconcentration factor of the modified nano magnetite for Fe(II) 167 sample was obtained. The detection limits and linear range of this method for iron were 1.0 and 9.0 - 175 ng.mL⁻¹, respectively. Also the relative standard deviation for five replicate determinations of 30.00 ng.mL^-1 Fe²⁺ was 2.3%.

Keywords: Alumina-coated magnetite nanoparticles, magnetic mixed hemimicell solid-phase extraction, Fe(ΙΙ) and Fe(ΙΙΙ), pharmaceutical sample.

Digital Object Identifier (DOI): doi.org/10.5281/zenodo.1125147

References:

[1] S. B. Goldhaber, “Trace element risk assessment: essentiality vs. toxicity,” Regul. Toxico. Pharm., vol. 38, pp. 232–242, 2003.
[2] K. Lee, F. M. Clydesdale, “Iron sources for food fortification and their changes due to food processing,” CRC Cr. Rev. Food Sci., vol. 11, pp. 117–153, 1978.
[3] A. Quinteros, R. Farre´, M.J. Lagarda, “Optimization of iron speciation (soluble, ferrous and ferric) in beans, chickpeas and lentils Food Chemistry,” Food Chem. vol. 75, pp. 365–370, 2001.
[4] J.F. Van Staden, L.V. Mulaudzi, R.I. Stefan, “Speciation of Mn(II) and Mn(VII) by on-line spectrophotometric sequential injection analysis,” Anal. Chim. Acta, vol. 499, pp. 129–137, 2003.
[5] Z. Sabatkova, M. Safarikova, I. Safarik, “Magnetic ovalbumin and egg white aggregates as affinity adsorbents for lectins separation’ Biochem. Eng. J., vol.40, pp. 542–545, 2008.
[6] Z.F. Wang, H.S. Guo, Y.L. Yu, N.Y. He, “Synthesis and characterization of a novel magnetic carrier with its composition of Fe3O4/carbon using hydrothermal reaction,” J. Magn. Magn. Mater, vol. 302, pp. 397-404, 2006.
[7] Y. Li, Y.C. Liu, J. Tang, H.Q. Lin, N. Yao, X.Z. Shen, C.H. Deng, P.Y. Yang, X.M. Zhang, “Fe3O4@Al2O3 magnetic core–shell microspheres for rapid and highly specific capture of phosphopeptides with mass spectrometry analysis,” J. Chromatogr. A, vol. 1172, pp. 57-71, 2007.
[8] D. Creanga, G. Calugaru, “Physical investigations of a ferrofluid based on hydrocarbons,” J. Magn. Magn. Mater. vol. 289, pp. 81–83, 2006.