Preparation of Novel Solid Phase Extraction Sorbents for Polycyclic Aromatic Hydrocarbons (PAHs) in Aqueous Media

In this study, functionalized mesoporous silica was prepared and characterized as a stationary phase using various analytical and solid-state techniques, including a Fourier-transform infrared (FTIR) spectrometer, thermogravimetric analysis, and nitrogen sorption. The results confirmed the successfu...

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Main Authors: Deogratius T. Maiga, Rose W. Kibechu, Bhekie B. Mamba, Titus A. M. Msagati, Terence T. Phadi
Format: Article
Language:English
Published: MDPI AG 2023-08-01
Series:Molecules
Subjects:
Online Access:https://www.mdpi.com/1420-3049/28/16/6129
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author Deogratius T. Maiga
Rose W. Kibechu
Bhekie B. Mamba
Titus A. M. Msagati
Terence T. Phadi
author_facet Deogratius T. Maiga
Rose W. Kibechu
Bhekie B. Mamba
Titus A. M. Msagati
Terence T. Phadi
author_sort Deogratius T. Maiga
collection DOAJ
description In this study, functionalized mesoporous silica was prepared and characterized as a stationary phase using various analytical and solid-state techniques, including a Fourier-transform infrared (FTIR) spectrometer, thermogravimetric analysis, and nitrogen sorption. The results confirmed the successful synthesis of the hybrid stationary phase. The potential of the prepared hybrid mesoporous silica as a solid-phase extraction (SPE) stationary phase for separating and enriching polycyclic aromatic hydrocarbons (PAHs) in both spiked water samples and real water samples was evaluated. The analysis involved extracting the PAHs from the water samples using solid-phase extraction and analyzing the extracts using a two-dimensional gas chromatograph coupled to a time-of-flight mass spectrometer (GC × GC-TOFMS). The synthesized sorbent exhibited outstanding performance in extracting PAHs from both spiked water samples and real water samples. In the spiked water samples, the recoveries of the PAHs ranged from 79.87% to 95.67%, with relative standard deviations (RSDs) ranging from 1.85% to 8.83%. The limits of detection (LOD) for the PAHs were in the range of 0.03 µg/L to 0.04 µg/L, while the limits of quantification (LOQ) ranged from 0.05 µg/L to 3.14 µg/L. Furthermore, all the calibration curves showed linearity, with correlation coefficients (r) above 0.98. Additionally, the results from real water samples indicated that the levels of individual PAH detected ranged from 0.57 to 12.31 µg/L with a total of 44.67 µg/L. These findings demonstrate the effectiveness of the hybrid mesoporous silica as a promising stationary phase for solid-phase extraction and sensitive detection of PAHs in water samples.
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spelling doaj.art-8c41e64bf3fd45f7be8a5e052b9c5aaa2023-11-19T02:25:23ZengMDPI AGMolecules1420-30492023-08-012816612910.3390/molecules28166129Preparation of Novel Solid Phase Extraction Sorbents for Polycyclic Aromatic Hydrocarbons (PAHs) in Aqueous MediaDeogratius T. Maiga0Rose W. Kibechu1Bhekie B. Mamba2Titus A. M. Msagati3Terence T. Phadi4Measurement and Control Division, Council for Mineral Technology (MINTEK), Private Bag X3015, Randburg, Johannesburg 2125, South AfricaDepartment of Chemistry, University of Eswatini, P/Bag 4 Kwaluseni Campus, Kwaluseni 0004, EswatiniInstitute for Nanotechnology and Water Sustainability, College of Science Engineering and Technology, UNISA Science Campus, University of South Africa, Roodepoort, Johannesburg 1710, South AfricaInstitute for Nanotechnology and Water Sustainability, College of Science Engineering and Technology, UNISA Science Campus, University of South Africa, Roodepoort, Johannesburg 1710, South AfricaMeasurement and Control Division, Council for Mineral Technology (MINTEK), Private Bag X3015, Randburg, Johannesburg 2125, South AfricaIn this study, functionalized mesoporous silica was prepared and characterized as a stationary phase using various analytical and solid-state techniques, including a Fourier-transform infrared (FTIR) spectrometer, thermogravimetric analysis, and nitrogen sorption. The results confirmed the successful synthesis of the hybrid stationary phase. The potential of the prepared hybrid mesoporous silica as a solid-phase extraction (SPE) stationary phase for separating and enriching polycyclic aromatic hydrocarbons (PAHs) in both spiked water samples and real water samples was evaluated. The analysis involved extracting the PAHs from the water samples using solid-phase extraction and analyzing the extracts using a two-dimensional gas chromatograph coupled to a time-of-flight mass spectrometer (GC × GC-TOFMS). The synthesized sorbent exhibited outstanding performance in extracting PAHs from both spiked water samples and real water samples. In the spiked water samples, the recoveries of the PAHs ranged from 79.87% to 95.67%, with relative standard deviations (RSDs) ranging from 1.85% to 8.83%. The limits of detection (LOD) for the PAHs were in the range of 0.03 µg/L to 0.04 µg/L, while the limits of quantification (LOQ) ranged from 0.05 µg/L to 3.14 µg/L. Furthermore, all the calibration curves showed linearity, with correlation coefficients (r) above 0.98. Additionally, the results from real water samples indicated that the levels of individual PAH detected ranged from 0.57 to 12.31 µg/L with a total of 44.67 µg/L. These findings demonstrate the effectiveness of the hybrid mesoporous silica as a promising stationary phase for solid-phase extraction and sensitive detection of PAHs in water samples.https://www.mdpi.com/1420-3049/28/16/6129hybrid stationary phase materialsSPE separationorganic pollutantsgas chromatography coupled with time-of-flight mass spectrometry
spellingShingle Deogratius T. Maiga
Rose W. Kibechu
Bhekie B. Mamba
Titus A. M. Msagati
Terence T. Phadi
Preparation of Novel Solid Phase Extraction Sorbents for Polycyclic Aromatic Hydrocarbons (PAHs) in Aqueous Media
Molecules
hybrid stationary phase materials
SPE separation
organic pollutants
gas chromatography coupled with time-of-flight mass spectrometry
title Preparation of Novel Solid Phase Extraction Sorbents for Polycyclic Aromatic Hydrocarbons (PAHs) in Aqueous Media
title_full Preparation of Novel Solid Phase Extraction Sorbents for Polycyclic Aromatic Hydrocarbons (PAHs) in Aqueous Media
title_fullStr Preparation of Novel Solid Phase Extraction Sorbents for Polycyclic Aromatic Hydrocarbons (PAHs) in Aqueous Media
title_full_unstemmed Preparation of Novel Solid Phase Extraction Sorbents for Polycyclic Aromatic Hydrocarbons (PAHs) in Aqueous Media
title_short Preparation of Novel Solid Phase Extraction Sorbents for Polycyclic Aromatic Hydrocarbons (PAHs) in Aqueous Media
title_sort preparation of novel solid phase extraction sorbents for polycyclic aromatic hydrocarbons pahs in aqueous media
topic hybrid stationary phase materials
SPE separation
organic pollutants
gas chromatography coupled with time-of-flight mass spectrometry
url https://www.mdpi.com/1420-3049/28/16/6129
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