Analysis of Polycyclic Aromatic Hydrocarbons Using Magnetic Three-Dimensional Graphene Solid-Phase Extraction Coupled with Gas Chromatography–Mass Spectrometry

In this study, a composite material consisting of three-dimensional graphene aerogel and iron oxide nanoparticles (3DG/Fe<sub>3</sub>O<sub>4</sub>) was created and utilized for the purpose of magnetic solid-phase extraction (MSPE) of thirteen polycyclic aromatic hydrocarbon (...

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Main Authors: Hassan Sereshti, Mahsa Karimi, Sajad Karami, Shokouh Mahpishanian, Mehdi Esmaeili Bidhendi, Shahabaldin Rezania, Amin Mojiri, Hesam Kamyab, Hamid Rashidi Nodeh
Format: Article
Language:English
Published: MDPI AG 2023-11-01
Series:Separations
Subjects:
Online Access:https://www.mdpi.com/2297-8739/10/11/564
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author Hassan Sereshti
Mahsa Karimi
Sajad Karami
Shokouh Mahpishanian
Mehdi Esmaeili Bidhendi
Shahabaldin Rezania
Amin Mojiri
Hesam Kamyab
Hamid Rashidi Nodeh
author_facet Hassan Sereshti
Mahsa Karimi
Sajad Karami
Shokouh Mahpishanian
Mehdi Esmaeili Bidhendi
Shahabaldin Rezania
Amin Mojiri
Hesam Kamyab
Hamid Rashidi Nodeh
author_sort Hassan Sereshti
collection DOAJ
description In this study, a composite material consisting of three-dimensional graphene aerogel and iron oxide nanoparticles (3DG/Fe<sub>3</sub>O<sub>4</sub>) was created and utilized for the purpose of magnetic solid-phase extraction (MSPE) of thirteen polycyclic aromatic hydrocarbon (PAH) compounds via gas chromatography–mass spectrometry/selected ion monitoring (GC-MS/SIM) analysis. The synthesized adsorbent underwent a range of characterization techniques, including scanning electron microscopy, vibrating sample magnetometry, Raman spectroscopy, X-ray diffraction, Brunauer–Emmett–Teller, Fourier transform-infrared spectroscopy, and Barrett–Joyner–Halenda techniques, to examine its properties and morphology. The synthesized adsorbent integrates the benefits of superior adsorption capacity from modified graphene oxide (GO) with the magnetic separability of magnetite microparticles, resulting in a high adsorption capacity with easy separation from sample solutions. The efficiency of the proposed method was optimized and modeled using a central composite design (CCD), which considered the primary factors influencing it. The optimal conditions were obtained as the adsorbent dosage of 10 mg, the extraction time of 4 min, and the salt concentration of 3% <i>w</i>/<i>v</i>. The limit of detection for the target PAHs was established to range from 0.016 to 0.2 ng mL<sup>−1</sup> in optimal conditions, exhibiting a signal-to-noise ratio of 3. The linear dynamic range spanned from 5 to 100 ng mL<sup>−1</sup>, with determination coefficients (R<sup>2</sup>) ranging from 0.9913 to 0.9997. The intra- and inter-day precisions were calculated as relative standard deviations (RSDs) equal to 3.9% and 4.7%, respectively. The proposed method was successfully applied to the determination of PAHs in water samples (tap, river, and rainwater), and recoveries in the range of 71–110% (RSDs < 5.2%, <i>n</i> = 3) were obtained.
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spelling doaj.art-01af0d9ca2dc4b4b9422125b972dc6722023-11-24T15:06:09ZengMDPI AGSeparations2297-87392023-11-01101156410.3390/separations10110564Analysis of Polycyclic Aromatic Hydrocarbons Using Magnetic Three-Dimensional Graphene Solid-Phase Extraction Coupled with Gas Chromatography–Mass SpectrometryHassan Sereshti0Mahsa Karimi1Sajad Karami2Shokouh Mahpishanian3Mehdi Esmaeili Bidhendi4Shahabaldin Rezania5Amin Mojiri6Hesam Kamyab7Hamid Rashidi Nodeh8School of Chemistry, College of Science, University of Tehran, Tehran P.O. Box 14155-6619, IranSchool of Chemistry, College of Science, University of Tehran, Tehran P.O. Box 14155-6619, IranDepartment of Nutrition, Dietetics and Food Sciences, Utah State University, Logan, UT 84322, USASchool of Chemistry, College of Science, University of Tehran, Tehran P.O. Box 14155-6619, IranSchool of Environment, College of Engineering, University of Tehran, Tehran P.O. Box 14155-6619, IranDepartment of Environment and Energy, Sejong University, Seoul 05006, Republic of KoreaEnvirowise Research Associate, Christchurch 8053, New ZealandFaculty of Architecture and Urbanism, UTE University, Calle Rumipamba S/N and Bourgeois, Quito 170129, EcuadorSchool of Chemistry, College of Science, University of Tehran, Tehran P.O. Box 14155-6619, IranIn this study, a composite material consisting of three-dimensional graphene aerogel and iron oxide nanoparticles (3DG/Fe<sub>3</sub>O<sub>4</sub>) was created and utilized for the purpose of magnetic solid-phase extraction (MSPE) of thirteen polycyclic aromatic hydrocarbon (PAH) compounds via gas chromatography–mass spectrometry/selected ion monitoring (GC-MS/SIM) analysis. The synthesized adsorbent underwent a range of characterization techniques, including scanning electron microscopy, vibrating sample magnetometry, Raman spectroscopy, X-ray diffraction, Brunauer–Emmett–Teller, Fourier transform-infrared spectroscopy, and Barrett–Joyner–Halenda techniques, to examine its properties and morphology. The synthesized adsorbent integrates the benefits of superior adsorption capacity from modified graphene oxide (GO) with the magnetic separability of magnetite microparticles, resulting in a high adsorption capacity with easy separation from sample solutions. The efficiency of the proposed method was optimized and modeled using a central composite design (CCD), which considered the primary factors influencing it. The optimal conditions were obtained as the adsorbent dosage of 10 mg, the extraction time of 4 min, and the salt concentration of 3% <i>w</i>/<i>v</i>. The limit of detection for the target PAHs was established to range from 0.016 to 0.2 ng mL<sup>−1</sup> in optimal conditions, exhibiting a signal-to-noise ratio of 3. The linear dynamic range spanned from 5 to 100 ng mL<sup>−1</sup>, with determination coefficients (R<sup>2</sup>) ranging from 0.9913 to 0.9997. The intra- and inter-day precisions were calculated as relative standard deviations (RSDs) equal to 3.9% and 4.7%, respectively. The proposed method was successfully applied to the determination of PAHs in water samples (tap, river, and rainwater), and recoveries in the range of 71–110% (RSDs < 5.2%, <i>n</i> = 3) were obtained.https://www.mdpi.com/2297-8739/10/11/564polycyclic aromatic hydrocarbonsthree-dimensional graphenemagnetic solid-phase extractioncentral composite designgas chromatography–mass spectrometry-selected ion monitoring
spellingShingle Hassan Sereshti
Mahsa Karimi
Sajad Karami
Shokouh Mahpishanian
Mehdi Esmaeili Bidhendi
Shahabaldin Rezania
Amin Mojiri
Hesam Kamyab
Hamid Rashidi Nodeh
Analysis of Polycyclic Aromatic Hydrocarbons Using Magnetic Three-Dimensional Graphene Solid-Phase Extraction Coupled with Gas Chromatography–Mass Spectrometry
Separations
polycyclic aromatic hydrocarbons
three-dimensional graphene
magnetic solid-phase extraction
central composite design
gas chromatography–mass spectrometry-selected ion monitoring
title Analysis of Polycyclic Aromatic Hydrocarbons Using Magnetic Three-Dimensional Graphene Solid-Phase Extraction Coupled with Gas Chromatography–Mass Spectrometry
title_full Analysis of Polycyclic Aromatic Hydrocarbons Using Magnetic Three-Dimensional Graphene Solid-Phase Extraction Coupled with Gas Chromatography–Mass Spectrometry
title_fullStr Analysis of Polycyclic Aromatic Hydrocarbons Using Magnetic Three-Dimensional Graphene Solid-Phase Extraction Coupled with Gas Chromatography–Mass Spectrometry
title_full_unstemmed Analysis of Polycyclic Aromatic Hydrocarbons Using Magnetic Three-Dimensional Graphene Solid-Phase Extraction Coupled with Gas Chromatography–Mass Spectrometry
title_short Analysis of Polycyclic Aromatic Hydrocarbons Using Magnetic Three-Dimensional Graphene Solid-Phase Extraction Coupled with Gas Chromatography–Mass Spectrometry
title_sort analysis of polycyclic aromatic hydrocarbons using magnetic three dimensional graphene solid phase extraction coupled with gas chromatography mass spectrometry
topic polycyclic aromatic hydrocarbons
three-dimensional graphene
magnetic solid-phase extraction
central composite design
gas chromatography–mass spectrometry-selected ion monitoring
url https://www.mdpi.com/2297-8739/10/11/564
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