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Synthesis and Characterization of a Multi-Walled Carbon Nanotube–Ionic Liquid/Polyaniline Adsorbent for a Solvent-Free In-Needle Microextraction Method

Sample preparation is an essential process when handling complex matrices. Extraction without using a solvent requires the direct transfer of analytes from the sample to the adsorbent either in the gas or liquid phase. In this study, a wire coated with a new adsorbent was fabricated for in-needle mi...

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Autores principales: Ahn, Soyoung, Bae, Sunyoung
Formato: Online Artículo Texto
Lenguaje:English
Publicado: MDPI 2023
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10142705/
https://www.ncbi.nlm.nih.gov/pubmed/37110753
http://dx.doi.org/10.3390/molecules28083517
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author Ahn, Soyoung
Bae, Sunyoung
author_facet Ahn, Soyoung
Bae, Sunyoung
author_sort Ahn, Soyoung
collection PubMed
description Sample preparation is an essential process when handling complex matrices. Extraction without using a solvent requires the direct transfer of analytes from the sample to the adsorbent either in the gas or liquid phase. In this study, a wire coated with a new adsorbent was fabricated for in-needle microextraction (INME) as a solvent-free sample extraction method. The wire inserted into the needle was placed in the headspace (HS), which was saturated with volatile organic compounds from the sample in a vial. A new adsorbent was synthesized via electrochemical polymerization by mixing aniline with multi-walled carbon nanotubes (MWCNTs) in the presence of an ionic liquid (IL). The newly synthesized adsorbent using IL is expected to achieve high thermal stability, good solvation properties, and high extraction efficiency. The characteristics of the electrochemically synthesized surfaces coated with MWCNT–IL/polyaniline (PANI) adsorbents were characterized using Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), thermogravimetric analysis (TGA), and atomic force microscopy (AFM). Then, the proposed HS–INME–MWCNT–IL/PANI method was optimized and validated. Accuracy and precision were evaluated by analyzing replicates of a real sample containing phthalates, showing spike recovery between 61.13% and 108.21% and relative standard deviations lower than 15%. The limit of detection and limit of quantification of the proposed method were computed using the IUPAC definition as 15.84~50.56 μg and 52.79~168.5 μg, respectively. We concluded that HS–INME using a wire coated with the MWCNT–IL/PANI adsorbent could be repeatedly used up to 150 times without degrading its extraction performance in an aqueous solution; it constitutes an eco-friendly and cost-effective extraction method.
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spelling pubmed-101427052023-04-29 Synthesis and Characterization of a Multi-Walled Carbon Nanotube–Ionic Liquid/Polyaniline Adsorbent for a Solvent-Free In-Needle Microextraction Method Ahn, Soyoung Bae, Sunyoung Molecules Article Sample preparation is an essential process when handling complex matrices. Extraction without using a solvent requires the direct transfer of analytes from the sample to the adsorbent either in the gas or liquid phase. In this study, a wire coated with a new adsorbent was fabricated for in-needle microextraction (INME) as a solvent-free sample extraction method. The wire inserted into the needle was placed in the headspace (HS), which was saturated with volatile organic compounds from the sample in a vial. A new adsorbent was synthesized via electrochemical polymerization by mixing aniline with multi-walled carbon nanotubes (MWCNTs) in the presence of an ionic liquid (IL). The newly synthesized adsorbent using IL is expected to achieve high thermal stability, good solvation properties, and high extraction efficiency. The characteristics of the electrochemically synthesized surfaces coated with MWCNT–IL/polyaniline (PANI) adsorbents were characterized using Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), thermogravimetric analysis (TGA), and atomic force microscopy (AFM). Then, the proposed HS–INME–MWCNT–IL/PANI method was optimized and validated. Accuracy and precision were evaluated by analyzing replicates of a real sample containing phthalates, showing spike recovery between 61.13% and 108.21% and relative standard deviations lower than 15%. The limit of detection and limit of quantification of the proposed method were computed using the IUPAC definition as 15.84~50.56 μg and 52.79~168.5 μg, respectively. We concluded that HS–INME using a wire coated with the MWCNT–IL/PANI adsorbent could be repeatedly used up to 150 times without degrading its extraction performance in an aqueous solution; it constitutes an eco-friendly and cost-effective extraction method. MDPI 2023-04-17 /pmc/articles/PMC10142705/ /pubmed/37110753 http://dx.doi.org/10.3390/molecules28083517 Text en © 2023 by the authors. https://creativecommons.org/licenses/by/4.0/Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https://creativecommons.org/licenses/by/4.0/).
spellingShingle Article
Ahn, Soyoung
Bae, Sunyoung
Synthesis and Characterization of a Multi-Walled Carbon Nanotube–Ionic Liquid/Polyaniline Adsorbent for a Solvent-Free In-Needle Microextraction Method
title Synthesis and Characterization of a Multi-Walled Carbon Nanotube–Ionic Liquid/Polyaniline Adsorbent for a Solvent-Free In-Needle Microextraction Method
title_full Synthesis and Characterization of a Multi-Walled Carbon Nanotube–Ionic Liquid/Polyaniline Adsorbent for a Solvent-Free In-Needle Microextraction Method
title_fullStr Synthesis and Characterization of a Multi-Walled Carbon Nanotube–Ionic Liquid/Polyaniline Adsorbent for a Solvent-Free In-Needle Microextraction Method
title_full_unstemmed Synthesis and Characterization of a Multi-Walled Carbon Nanotube–Ionic Liquid/Polyaniline Adsorbent for a Solvent-Free In-Needle Microextraction Method
title_short Synthesis and Characterization of a Multi-Walled Carbon Nanotube–Ionic Liquid/Polyaniline Adsorbent for a Solvent-Free In-Needle Microextraction Method
title_sort synthesis and characterization of a multi-walled carbon nanotube–ionic liquid/polyaniline adsorbent for a solvent-free in-needle microextraction method
topic Article
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10142705/
https://www.ncbi.nlm.nih.gov/pubmed/37110753
http://dx.doi.org/10.3390/molecules28083517
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