Food Analytical Methods

, Volume 10, Issue 7, pp 2229–2240 | Cite as

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



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 chromatography-mass 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 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.


Zirconia nanoparticles Magnetite nanoparticles Organophosphorous pesticides Magnetic dispersive micro-solid-phase extraction Gas chromatography Mass spectroscopy 


Compliance with Ethical Standards


The financial support of this work was provided by the Research Council of Ahvaz Jundishapur University of Medical Sciences and Nanotechnology Research Center under grant number GP 94108. This paper is an extract from Miss Behrouz’s thesis.

Conflict of Interest

Nadereh Rahbar declares that she has no conflict of interest. Elnaz Behrouz declares that she has no conflict of interest. Zahra Ramezani declares that she has no conflict of interest.

Ethical Approval

This article does not contain any studies with human participants or animals performed by any of the authors.

Informed Consent

Not applicable.

Supplementary material

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Copyright information

© Springer Science+Business Media New York 2017

Authors and Affiliations

  • Nadereh Rahbar
    • 1
    • 2
  • Elnaz Behrouz
    • 1
  • Zahra Ramezani
    • 1
    • 2
  1. 1.Nanotechnology Research Center, Faculty of PharmacyAhvaz Jundishapur University of Medical SciencesAhvazIran
  2. 2.Department of Medicinal Chemistry, Faculty of PharmacyAhvaz Jundishapur University of Medical SciencesAhvazIran

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