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Magnetic dispersive micro-solid-phase extraction integrated with hollow fiber liquid-phase microextraction for preconcentration of trace amounts of chlorpyrifos pesticide in aqueous samples

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Abstract

In the present study, the integration of magnetic dispersive micro-solid-phase extraction (MD-µSPE) with hollow fiber liquid-phase microextraction (HF-LPME) prior to gas chromatography–mass spectrometry (GC/MS) was developed to preconcentrate and determine trace amounts of chlorpyrifos pesticide. Azolla filiculoides fern biomass was loaded by magnetite nanoparticles to prepare magnetic adsorbent (azolla@Fe3O4). The structural characteristics of the produced magnetic nanocomposites (MNCs) were investigated by FESEM, TEM, VSM, FTIR, EDX, and XRD methods. In the proposed MD-µSPE/HF-LPME method, the adsorption/desorption variables in MD-µSPE step were optimized by Taguchi fractional factorial design. After chlorpyrifos adsorption in the optimized condition of MD-µSPE (Vsample = 50 mL, contact time = 15 min, solution pH = 3, adsorbent mass = 0.05 g, ionic strength = 0.01 mol L−1, and eluent type = ethanol), 2.0 mL of the desorbed ethanolic solution was added to 16 mL of 10% (w/v) NaCl aqueous solution for the next HF-LPME method and the final analysis was performed by GC/MS. The developed method showed a limit of detection of 0.05 μg L−1, a limit of quantification of 0.5 μg L−1, a dynamic linear range of 0.5–1000.0 μg L−1, preconcentration factors between 700 and 1050, and a repeatability (RSD%) of 6.9%. The suitability of the MD-µSPE/HF-LPME method was confirmed by measuring chlorpyrifos in real samples with relative recoveries in the range of 97.0–108.5%. The results showed good accuracy and precision of the developed MD-µSPE/HF-LPME method for the preconcentration and determination of trace amounts of chlorpyrifos in the aqueous samples.

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Acknowledgements

The authors are thankful to Rasht Branch, Islamic Azad University and Forensic Medicine Research Center—General Department of Legal Medicine of Guilan Province for their help.

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Authors and Affiliations

  1. Department of Chemistry, Tabriz Branch, Islamic Azad University, Tabriz, Iran

    Reyhaneh Kouchakinejad, Jafar Abolhasani, Ebrahim Ghorbani Kalhor & Mohammad Taghi Vardini

  2. Department of Chemistry, Rasht Branch, Islamic Azad University, Rasht, Iran

    Shahab Shariati

  3. Legal Medicine Research Center, Legal Medicine Organization, Tehran, Iran

    Ameneh Dorri

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  1. Reyhaneh Kouchakinejad
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Correspondence to Shahab Shariati.

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Kouchakinejad, R., Shariati, S., Abolhasani, J. et al. Magnetic dispersive micro-solid-phase extraction integrated with hollow fiber liquid-phase microextraction for preconcentration of trace amounts of chlorpyrifos pesticide in aqueous samples. J IRAN CHEM SOC (2024). https://doi.org/10.1007/s13738-024-03028-4

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