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Microextraction in packed syringe by using a three-dimensional carbon nanotube/carbon nanofiber–graphene nanostructure coupled to dispersive liquid-liquid microextraction for the determination of phthalate esters in water samples

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Abstract

Microextraction in packed syringe (MEPS) was combined with dispersive liquid-liquid microextraction (DLLME) for the extraction of phthalate esters (PEs) from water samples prior to their determination by GC with flame ionization detection. A three-dimensional nanomaterial composed of carbon nanotubes, carbon nanofibers and graphene was prepared by chemical vapor deposition (CVD) and employed as a sorbent for MEPS. The porous structure of the sorbent has been revealed by scanning electron microscopy, transmission electron microscopy, and Brunauer-Emmett-Teller adsorption. The effects of various experimental variables on the extraction efficiencies of the following PEs were studied: Dimethyl phthalate, diethyl phthalate, diisobutyl phthalate, di-n-butyl phthalate, and di-2-ethylhexyl phthalate. After extraction, the GC assay gives a linear calibration plot that covers the 0.02 to 200 ng mL−1 PE concentration ranges. The method displays detection limits (at an S/N ratio of 3) in the range from 1 to 10 ng mL−1. Relative standard deviations for intra-day and inter-day precision are between 5.7 and 8.9%, and between 7.6 and 10.1%, respectively. The feasibility of the method was demonstrated by extracting and determining PEs in (spiked) real water samples, whereby recoveries in the range of 90.3–98.8% and RSD% lower than 10.3% were attained.

Schematic of a method for microextraction in packed syringe (MEPS) combined with dispersive liquid-liquid microextraction (DLLME) as a new approach for the extraction and preconcentration of phthalate esters (PEs). They were quantified by gas chromatography (GC) with flame ionization (FID) detection.

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Acknowledgements

The authors thank the Research Council of Hakim Sabzevari University for their financial support.

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Authors and Affiliations

  1. Department of Chemistry, Faculty of Sciences, Hakim Sabzevari University, Sabzevar, 9617976487, Iran

    Amirhassan Amiri

  2. Institute of Tropical Forestry and Forest Products, Universiti Putra Malaysia, 43400 UPM, Serdang, Selangor, Malaysia

    Ferial Ghaemi

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  1. Amirhassan Amiri
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  2. Ferial Ghaemi
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Correspondence to Amirhassan Amiri.

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Amiri, A., Ghaemi, F. Microextraction in packed syringe by using a three-dimensional carbon nanotube/carbon nanofiber–graphene nanostructure coupled to dispersive liquid-liquid microextraction for the determination of phthalate esters in water samples. Microchim Acta 184, 3851–3858 (2017). https://doi.org/10.1007/s00604-017-2416-8

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  • DOI: https://doi.org/10.1007/s00604-017-2416-8

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