Exploring Adsorption Performance of Functionalized Mesoporous Silicas with a Different Pore Structure as Strong Cation-Exchange Sorbents for Solid-Phase Extraction of Atropine and Scopolamine

In this work, mesoporous silicas with two types of mesoporous structures were synthesized and functionalized with sulfonic acid groups: MCM-41-SO<sub>3</sub>H (honeycomb-like hexagonal structure) and MSU-2-SO<sub>3</sub>H (three-dimensional porous structure with wormhole pore...

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Main Authors: Fernando L. Vera-Baquero, Sonia Morante-Zarcero, Damián Pérez-Quintanilla, Isabel Sierra
Format: Article
Language:English
Published: MDPI AG 2025-01-01
Series:Applied Sciences
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Online Access:https://www.mdpi.com/2076-3417/15/2/646
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author Fernando L. Vera-Baquero
Sonia Morante-Zarcero
Damián Pérez-Quintanilla
Isabel Sierra
author_facet Fernando L. Vera-Baquero
Sonia Morante-Zarcero
Damián Pérez-Quintanilla
Isabel Sierra
author_sort Fernando L. Vera-Baquero
collection DOAJ
description In this work, mesoporous silicas with two types of mesoporous structures were synthesized and functionalized with sulfonic acid groups: MCM-41-SO<sub>3</sub>H (honeycomb-like hexagonal structure) and MSU-2-SO<sub>3</sub>H (three-dimensional porous structure with wormhole pores). The synthesized materials were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, nitrogen adsorption–desorption, Fourier-transform infrared spectroscopy, <sup>29</sup>Si solid-state nuclear magnetic resonance spectroscopy, and elemental analysis. The obtained functionalized materials were evaluated as sorbents for strong cation-exchange solid-phase extraction (SPE) to determine their efficiency in the adsorption and desorption of tropane alkaloids (atropine and scopolamine). The loading solvents, loading volume, analyte concentration, and elution volume were studied, using 50 mg of both materials. Analyses were carried out by ultra-high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry. The synthesized MCM-41-SO<sub>3</sub>H material presented the highest recovery efficiency and has proven to be a promising sorbent for strong cation-exchange SPE of atropine and scopolamine in aqueous media. The high degree of functionalization of MCM-41-SO<sub>3</sub>H and the high accessibility of the sulfonic groups for the target analytes, due to the regularity and uniformity of their pores, maximize the contact between the alkaloids and the sorbent, favoring efficient adsorption.
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spelling doaj-art-781cd2092e174e24baaed9e681ab755c2025-01-24T13:20:16ZengMDPI AGApplied Sciences2076-34172025-01-0115264610.3390/app15020646Exploring Adsorption Performance of Functionalized Mesoporous Silicas with a Different Pore Structure as Strong Cation-Exchange Sorbents for Solid-Phase Extraction of Atropine and ScopolamineFernando L. Vera-Baquero0Sonia Morante-Zarcero1Damián Pérez-Quintanilla2Isabel Sierra3Departamento de Tecnología Química y Ambiental, Escuela Superior de Ciencias Experimentales y Tecnología (E.S.C.E.T), Universidad Rey Juan Carlos, C/Tulipán s/n, Móstoles, 28933 Madrid, SpainDepartamento de Tecnología Química y Ambiental, Escuela Superior de Ciencias Experimentales y Tecnología (E.S.C.E.T), Universidad Rey Juan Carlos, C/Tulipán s/n, Móstoles, 28933 Madrid, SpainDepartamento de Tecnología Química y Ambiental, Escuela Superior de Ciencias Experimentales y Tecnología (E.S.C.E.T), Universidad Rey Juan Carlos, C/Tulipán s/n, Móstoles, 28933 Madrid, SpainDepartamento de Tecnología Química y Ambiental, Escuela Superior de Ciencias Experimentales y Tecnología (E.S.C.E.T), Universidad Rey Juan Carlos, C/Tulipán s/n, Móstoles, 28933 Madrid, SpainIn this work, mesoporous silicas with two types of mesoporous structures were synthesized and functionalized with sulfonic acid groups: MCM-41-SO<sub>3</sub>H (honeycomb-like hexagonal structure) and MSU-2-SO<sub>3</sub>H (three-dimensional porous structure with wormhole pores). The synthesized materials were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, nitrogen adsorption–desorption, Fourier-transform infrared spectroscopy, <sup>29</sup>Si solid-state nuclear magnetic resonance spectroscopy, and elemental analysis. The obtained functionalized materials were evaluated as sorbents for strong cation-exchange solid-phase extraction (SPE) to determine their efficiency in the adsorption and desorption of tropane alkaloids (atropine and scopolamine). The loading solvents, loading volume, analyte concentration, and elution volume were studied, using 50 mg of both materials. Analyses were carried out by ultra-high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry. The synthesized MCM-41-SO<sub>3</sub>H material presented the highest recovery efficiency and has proven to be a promising sorbent for strong cation-exchange SPE of atropine and scopolamine in aqueous media. The high degree of functionalization of MCM-41-SO<sub>3</sub>H and the high accessibility of the sulfonic groups for the target analytes, due to the regularity and uniformity of their pores, maximize the contact between the alkaloids and the sorbent, favoring efficient adsorption.https://www.mdpi.com/2076-3417/15/2/646atropinescopolaminefunctionalized mesoporous silicaMCM-41-SO<sub>3</sub>HMSU-2-SO<sub>3</sub>Hstrong cation-exchange solid-phase extraction
spellingShingle Fernando L. Vera-Baquero
Sonia Morante-Zarcero
Damián Pérez-Quintanilla
Isabel Sierra
Exploring Adsorption Performance of Functionalized Mesoporous Silicas with a Different Pore Structure as Strong Cation-Exchange Sorbents for Solid-Phase Extraction of Atropine and Scopolamine
Applied Sciences
atropine
scopolamine
functionalized mesoporous silica
MCM-41-SO<sub>3</sub>H
MSU-2-SO<sub>3</sub>H
strong cation-exchange solid-phase extraction
title Exploring Adsorption Performance of Functionalized Mesoporous Silicas with a Different Pore Structure as Strong Cation-Exchange Sorbents for Solid-Phase Extraction of Atropine and Scopolamine
title_full Exploring Adsorption Performance of Functionalized Mesoporous Silicas with a Different Pore Structure as Strong Cation-Exchange Sorbents for Solid-Phase Extraction of Atropine and Scopolamine
title_fullStr Exploring Adsorption Performance of Functionalized Mesoporous Silicas with a Different Pore Structure as Strong Cation-Exchange Sorbents for Solid-Phase Extraction of Atropine and Scopolamine
title_full_unstemmed Exploring Adsorption Performance of Functionalized Mesoporous Silicas with a Different Pore Structure as Strong Cation-Exchange Sorbents for Solid-Phase Extraction of Atropine and Scopolamine
title_short Exploring Adsorption Performance of Functionalized Mesoporous Silicas with a Different Pore Structure as Strong Cation-Exchange Sorbents for Solid-Phase Extraction of Atropine and Scopolamine
title_sort exploring adsorption performance of functionalized mesoporous silicas with a different pore structure as strong cation exchange sorbents for solid phase extraction of atropine and scopolamine
topic atropine
scopolamine
functionalized mesoporous silica
MCM-41-SO<sub>3</sub>H
MSU-2-SO<sub>3</sub>H
strong cation-exchange solid-phase extraction
url https://www.mdpi.com/2076-3417/15/2/646
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