One-Step Synthesis of Zirconia and Magnetite Nanocomposite Immobilized Chitosan for Micro-Solid-Phase Extraction of Orga
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One-Step Synthesis of Zirconia and Magnetite Nanocomposite Immobilized Chitosan for Micro-Solid-Phase Extraction of Organophosphorous Pesticides from Juice and Water Samples Prior to Gas Chromatography/Mass Spectroscopy Nadereh Rahbar 1,2 & Elnaz Behrouz 1 & Zahra Ramezani 1,2
Received: 21 September 2016 / Accepted: 13 December 2016 # Springer Science+Business Media New York 2017
Abstract In this research, a magnetic sorbent was prepared by immobilizing zirconia and magnetite (Fe3O4) nanoparticles in chitosan, which is characterized and used as an effective nanosorbent in magnetic dispersive micro-solid-phase extraction (MDMSPE) of organophosphorous pesticides (OPPs) from juice and water samples prior to gas chromatographymass detection (GC-MS). The properties and morphology of synthesized sorbent were characterized by scanning electron microscopy (SEM), Fourier transform-infrared spectroscopy (FT-IR), vibrating sample magnetometry (VSM), and differential scanning calorimetric (DSC) analysis. The main experimental parameters including pH level, extraction time, sorbent mass, salt concentration, and desorption conditions were investigated and optimized to maximize extraction efficiency. Under optimized conditions, the calibration curves were obtained in the concentration range of 0.1–500 ng mL−1 with correlation coefficients between 0.9993 and 0.9999. The limits of detection (signal-to-noise ratio (S/N) = 3) and limits of quantification (S/N = 10) of the method ranged from 0.031 to 0.034 ng mL−1 and 0.105–0.112 ng mL−1, respectively. The intra-day and inter-day RSDs were 2.2–5.7 and 2.5–7.5%, respectively. The method was successfully applied to the analysis of OPPs in fruit juices (apple, peach, and cherry) and Electronic supplementary material The online version of this article (doi:10.1007/s12161-016-0769-y) contains supplementary material, which is available to authorized users. * Nadereh Rahbar [email protected]; [email protected]
1
Nanotechnology Research Center, Faculty of Pharmacy, Ahvaz Jundishapur University of Medical Sciences, Ahvaz, Iran
2
Department of Medicinal Chemistry, Faculty of Pharmacy, Ahvaz Jundishapur University of Medical Sciences, Ahvaz, Iran
water (mineral, tap, and river) real samples, with recoveries in the range of 86.0–106.0% for the spiked juice and water samples. The results showed that with combination of high selectivity of zirconia and magnetic property of magnetite as well as immobilizing ability of chitosan, the fabricated sorbent exhibited exceptional extraction ability toward the OPPs. Keywords Zirconia nanoparticles . Magnetite nanoparticles . Organophosphorous pesticides . Magnetic dispersive micro-solid-phase extraction . Gas chromatography . Mass spectroscopy
Introduction Organophosphorous pesticides (OPPs) as relatively low toxic compounds are used worldwide to increase the yield of agricultural products. However, extensive and incorrect use of them has raised public concern of the potential threat to food and environmental safety. Many international or
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