Porous magnetized carbon sheet nanocomposites for dispersive solid-phase microextraction of organophosphorus pesticides prior to analysis by gas chromatography-ion mobility spectrometry

Carbon sheets were attached to magnetite (Fe₃O₄) nanoparticles. The resulting nanocomposite is shown to be a viable sorbent for use in magnetic dispersive solid-phase microextraction of three organophosphorus pesticides. The sorbent was synthesized via the sol-gel process followed by calcination and was characterized by an X-ray diffractometer, field emission scanning electron microscopy and energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, and Raman spectrometry techniques. The affecting parameters in the adsorption and desorption steps were assessed and optimized via response surface methodology. Following desorption with dichloromethane, the OPPs were quantified by gas chromatography along with ion mobility spectrometry detection. Under optimized conditions, the limits of detection were 1.00, 0.46 and 0.85 μg L⁻¹ for fenthion, malathion and chlorpyrifos, respectively. Response is linear in the concentration range of 2–500 μg L⁻¹ for fenthion and malathion, and 2–1000 μg L⁻¹ for chlorpyrifos with the determination coefficient larger than 0.9969. The intra-day and inter-day precision were from 3 to 9% and 5 to 16%, respectively. The enrichment factor was greater than 142 for all the studied pesticides. The sorbent was used for analyze spiked water and vegetable samples and gave relative recovery higher than 82%.

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